Book of Abstracts 2013 kompakt

BOOK OFABSTRACTS

Organisati on

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Sponsors andConferenceSupporti ng

Organisati ons

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34th Internati onal Conference on Fundamentals and Industrial Applicati ons of HIPIMS – Braunschweig 2013 – Book of Abstracts

PrefaceThin fi lm technology and surface engineering are nowadays key components for numerous innovati ve products like effi cient windows, fl at screens, sensors or hard coati ngs used in tool coati ng and automoti ve applicati ons, as well as products for everyday life. In line with the demands of surface technology, coati ng technology is also evolving and improving. The latest major technology jump was the intro-ducti on of pulse technology in physical vapor depositi on. High power impulse magnetron sputt ering is the most re-cent development of pulse sputt ering. Aft er approximately a decade of intense academic investi gati on and develop-ment we observe today a transfer of this new technology towards industrial processes.

As well as several internati onal acti viti es the internati onal conference on fundamentals and applicati ons of HIPIMS conti nues the success story of the HIPIMS days, initi ated in 2004 at Sheffi eld Hallam University, UK. Becoming the only internati onal conference especially dedicated to HIPIMS the HIPIMS conference is a venue for industrial and academic exchange on the latest developments in this fast evolving new technology. As a joint undertaking of Sheffi eld Hallam University SHU, Network of Competence for Indus-trial Plasma Surface Technology INPLAS and Fraunhofer Insti tute for Surface Engineering and Thin Films IST the HIPIMS conference was launched in 2010 in Sheffi eld, UK. With 120 delegates the impact of the new conference was underlined. The growing importance of HIPIMS technology was connected with a growth to more than 160 parti cipants in the following two years in Braunschweig, DE and Sheffi eld, UK 2012 and 2013, respecti vely. The parti cipants were made up of equal numbers from research and develop-ment (university and research institutes) and industry. Being a global conference representati ves from 25 diff erent countries from all conti nents att ended.

The HIPIMS conference 2013 is linked with the Final Event of the COST Acti on MP0804 Highly Ionized Pulse Plasma Processes (www.hipp-cost.eu). COST (European Coopera-ti on in Science and Technology) is one of the longest-run-ning European frameworks supporti ng cooperati on among scienti sts and researchers across Europe (www.cost.eu).

The COST Acti on MP0804 HIPP processes focuses on the fundamentals and the industrial implementati on of highly ionized pulse plasmas, where HIPIMS is the most promi-nent and most mature technology, today. Within the Acti on representati ves from 23 COST countries, one near neigh-bor country, and 4 NON-COST partners linked to create a unique forum to successfully accompany the transiti on of HIPP processes from fundamental science to applicati ons.

The HIPIMS Conference 2013 and Final Event of COST MP0804 gathers world leading experts in the fi eld of high power impulse magnetron sputt ering (HIPIMS), on equal shares from academia and industry within more than 60 topical contributi ons. More than 70% of the contributi ons involve partners from the COST Acti on MP0804 and under-line the close connecti on of the COST Acti on and the HIPIMS society, meeti ng annually at the HIPIMS conference.The talks from internati onal experts covered a range from fundamental physics, experimental investi gati ons, theoreti -cally modeling to several applicati ons and made the COST Acti on and this internati onal conference on fundamentals and applicati ons a success story to be conti nued in the following years.

Dr. Ralf Bandorf and Prof. A. Ehiasarian(Conference Chairmen and Co-Chairman of HIPIMS 2013)

4 54th Internati onal Conference on Fundamentals and Industrial Applicati ons of HIPIMS – Braunschweig 2013 – Book of Abstracts 4th Internati onal Conference on Fundamentals and Industrial Applicati ons of HIPIMS – Braunschweig 2013 – Book of Abstracts

Contents page Contents page

Preface . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 3

HIPIMS as a tool to understand the ti me-domain and energeti c bombardment eff ects on the nucleati on and coalescence of thin metal fi lms on amorphous substratesD. Magnfält, V. Elofsson, G. Abadias, U. Helmersson, K. Sarakinos . . . . . . 8

High ionizati on triple: An innovati ve PVD process for advanced coati ng architectures based on HIPIMS and ArcJ. Vett er, J. Mueller, T. Krienke, M. Schmidt-Mauer, G. Erkens . . . . . . . . . . 9

Advances in process technology and depositi on equipment for HIPIMS coati ngs for cutti ng toolsT. Leyendecker, O. Lemmer, W. Kölker, C. Schiff ers . . . . . . . . . . . . . . . . . . . 9

TiN for forming applicati onsJ. Alami, Z. Maric . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 10

Infl uence of Ion bombardment energy on the growth of CrN fi lms by reacti ve magnetron sputt ering and high power impulse magnetron sputt eringA. P. Ehiasarian, B. Howe, I. Petrov . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 10

Corrosion protecti on by HIPIMS+ deposited CrN-based coati ngsM. Eerden, F. Papa, R. Tietema, G. Aresta, T. Krug . . . . . . . . . . . . . . . . . . 11

HIPIMS process with oscillatory voltage pulse shapes for directi onal sputt ering applicati onsR. Chistyakov, B. Abraham . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 12

Electrical characteristi cs of S3p™ HIPIMS dischargeS. Krassnitzer, D. Kurapov, H. Rudigier . . . . . . . . . . . . . . . . . . . . . . . . . . . . 12

New development of HIPIMS power supply with best in class technology and new featuresP. Ozimek, A. Klimczak, P. Rozanski, W. Glazek, P. Lesiuk . . . . . . . . . . . . . 13

Depositi on rates and oxygen negati ve ion energy distribu-ti ons during reacti ve HIPIMS of ti tanium in Ne /O2, Ar/O2, Kr/O2 and Xe/O2 gas mixturesM. Bowes, J. W. Bradley. . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 13

Plasma characterisati on of the HIPIMS instabiliti es by energy resolved mass spectrometryY. Aranda Gonzalvo, A. Hecimovic, J. Winter, T. de los Arcos . . . . . . . . . . 14

A novel, depositi on-tolerant, Langmuir probe suitable for plasma parameter measurement in HIPIMS dischargesD. Gahan, P. Scullin, D. O’ Sullivan, M. B. Hopkins . . . . . . . . . . . . . . . . . . . 15

Fe2O3 thin fi lms for water splitti ng applicati on prepared by high power pulsed magnetron and pulsed hollow cathode systemsZ. Hubička, Š. Kment, M. Čada, J. Olejníček . . . . . . . . . . . . . . . . . . . . . . . . 16

Can HIPIMS CrxN serve as alternati ve for hard chromium?Truijen I., Cosemans P. . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 16

Correlati on between the Rockwell indentati on test and the progressive load scratch test for assessment of coati ng adhesionN. Randall, G. Favaro, M. Hess . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 17

Target implantati on and re-depositi on processes during high power impulse magnetron sputt ering of aluminiumT. de los Arcos, A. Will, C. Corbella, A. Hecimovic, A. von Keudell,

J. Winter . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 17

Mechanical properti es of TiSiN coati ngs processed by HIPIMS-pulsed DC hybrid processM. Arab Pour Yazdi, F. Lomello, F. Sanchett e, F. Schuster, A. Billard . . . . . . 18

Gyrokineti c descripti on of technical plasmasR. P. Brinkmann, S. Gallian, B. Schröder, D. Eremin . . . . . . . . . . . . . . . . . . 19

Infl uence of the Y-doping on the oxidati on and mechanical properti es of AlCrN-based coati ngsF. Lomello, M. Arab Pour Yazdi, F. Sanchett e, P. Steyer, F. Schuster,

A. Billard . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 19

Study of wear mechanism of chromium doped DLC coati ng by Raman spectroscopy in boundary lubricati on conditi onP. Mandal, A. P. Ehiasarian, P. E. Hovsepian . . . . . . . . . . . . . . . . . . . . . . . 20

Correlati on between mass-spectrometer measurements and thin fi lm characteristi cs using HIPIMS dischargesA. Ferrec, S. Jacq, J. Kenardel, F. Schuster, M.-C. Fernandez, P.-Y. Jouan,

A. Djouadi . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 21

The study of ti tanium nitride fi lms deposited using a hybrid system combining cathodic arc depositi onand high power impulse magnetron sputt eringC.-L. Chang, W.-Y. Wu, C.-T. Ho, P.-H. Chen, W.-C. Chen, D.-Y. Wang . . . . . . 22

Time-resolved opti cal emission spectroscopy of a vanadium HIPIMS plasmaB. Treverrow, D. McKenzie, M. Bilek . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 22

HIPIMS vs DCMS technology to produce tungsten coati ngs for fusion applicati onsS. M. Deambrosis, E. Miorin, F. Agresti , F. Montagner, V. Zin,

M. Fabrizio . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 23

HIPIMS depositi on of TiAlN fi lms on microforming die and its tribological properti es in progressive micro-deep drawingT. Shimizu, H. Komiya, T. Watanabe, Y. Teranishi, H. Nagasaka,

M. Yang . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 24

Titanium carbide oxide and nitride HIPIMS and DCMS processes compared from the OES point of viewA. Patelli, M. Colasuonno, M. Bazzan, G. Matt ei, V. Rigato . . . . . . . . . . . . 24

Chromium nitride (CrN) thin fi lms deposited by MPPMS for protecti on of diff erent steel substratesL. Mendizabal, U. Ruiz de Gopegui, X. Fernandez, J. Barriga . . . . . . . . . . 25

Investi gati ons of very short pulse sequences in HIPIMS mode for reacti ve depositi on of SilicaH. Gerdes, R. Bandorf, T. Preller, G. Bräuer . . . . . . . . . . . . . . . . . . . . . . . . 26

Nb coati ngs for superconducti ng RF applicati ons by HIPIMSG. Terenziani, S. Calatroni, A. P. Ehiasarian . . . . . . . . . . . . . . . . . . . . . . . . 26

The structure and tribological properti es of tungsten containing hydrogenated diamond-like carbon coati ngsZheng Jun . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 27Titanium-doped MoS2 lubricati ng coati ngs for space precision ball bearingsR.-P. Sang . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 27

Overcoming HIPIMS depositi on rate limitati ons by hybrid RF / HIPIMS co-sputt ering and its relevance for NbSi fi lmsN.Holtzer, O. Antonin, T. Minea, S. Marnieros . . . . . . . . . . . . . . . . . . . . . . 28

The structure and mechanical properti es of Cr2N coati ngs deposited by HIPIMS technologyZhou Hui . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 29

ZrSiN and NbN coati ngs deposited by HIPIMS for hard coati ng corrosion protecti on on aluminumM. Colasuonno, A. Patelli, G. Matt ei, V. Rigato . . . . . . . . . . . . . . . . . . . . . 29

Tungsten coati ngs by HIPIMS as plasma facing material for nuclear fusion reactor applicati onsN. Gordillo, M. Panizo-Laiz, I. Fernandez-Marti nez, E. Tejado, A. Rivera,

F. Briones, J. Y. Pastor, J. M. Perlado, R. Gonzalez-Arrabal . . . . . . . . . . . . . . 30

Opti mizati on of HIPIMS photocatalyti c ti tania coati ngs on polymeric substratesP. J. Kelly, M. Ratova, G. T. West . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 31


Growth of carbon – tungsten nanocomposites by high power impulse magnetron sputt ering from compound targetsG. Abrasonis, R. Y. Kumar, F. Munnik, R. Heller, R. Hübner, W. Möller,

J. Neidhardt . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 31

Ellipsometric characterizati on of transparent nickel oxide deposited by reacti ve DC magnetron sputt ering and HIPIMSD. T. Nguyen, A. Ferrec, J. Keraudy, M. Richard-Plouet, A. Goullet, L. Catti n,

L. Brohan, P-Y. Jouan . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 32

The reacti ve high power impulse magnetron sputt ering process for the synthesis of CFx thin fi lms using CF4 and C4F8

S. Schmidt, C. Goyenola, G. K. Gueorguiev, J. Jensen, G. Greczynski,

Z. Czigány, L. Hultman . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 33

Compressive stress generati on through adatom inserti on into grain boundaries in low mobility metal fi lms de-posited by high power impulse magnetron sputt eringD. Magnfält, G. Abadias, K. Sarakinos . . . . . . . . . . . . . . . . . . . . . . . . . . . . 33High power impulse magnetron sputt er depositi on of ITO and AZO thin fi lmsA. Ecis, E. Macevskis, M. Zubkins, A. Kalinko, R. Kalendarevs, K. Vilnis,

A. Azens, V. Kozlovs, J. Purans . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 34

Uniform, adhesive, robust Cu/TiO2 DCP and HIPIMS sputt ered fi lms inducing fast bacterial/viral inacti vati on under low intensity solar irradiati onJ. Kiwi, S. Rti mi, C. Pulgarin, R. Sanjines . . . . . . . . . . . . . . . . . . . . . . . . . . . 34

Opti cal emission spectroscopy of aluminum nitride thin fi lms deposited by pulsed laser depositi onJ. A. Pérez, L. P. Vera, H. Riascos, J. C. Caicedo . . . . . . . . . . . . . . . . . . . . . . 35

Carbon ion producti on using a high-power impulse magnetron sputt ering (HIPIMS) glow plasmaK. Yukimura, H. Ogiso, S. Nakano . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 36

Contents page Contents page

The blood platelet behavior of ti tanium-copper fi lms by high power pulsed magnetron sputt eringF. Jing, Y. Tai, K. Yukimura, H. Sun, L. Yao, Y. Leng, H. Nan . . . . . . . . . . . . . 36

Depositi on of nickel by inducti vely coupled impulse sputt ering (ICIS)D. A. L. Loch, A. P. Ehiasarian . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 37

Film depositi on using a 1 inch-sized HIPIMS systemH. Ogiso, K. Yukimura, S. Nakano . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 38

Time- and space-resolved laser-induced fl uorescence spectroscopy in a short-pulse HIPIMS dischargeN. Britun, M. Palmucci, S. Konstanti nidis, R. Snyders . . . . . . . . . . . . . . . . 38

Angle- and ti me-resolved ion velocity distributi ons in HIPIMSM. Cada, P. Adamek, V. Stranak, J. Olejnicek, S. Kment, Z. Hubicka,

R. Hippler . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 39

Depositi on rate enhancement in HIPIMS without compromising the ionized fracti on of the depositi on fl uxJ. Capek, M. Hala, O. Zabeida, J. E. Klemberg-Sapieha, L. Marti nu . . . . . . . 40

Amorphous carbon matrix – carbon nanotube nano-compositesV. A. Meliksetyan, A. P. Ehiasarian . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 40Ionizati on zones, plasma fl ares, self-organizati on, and the asymmetric ejecti on of parti cles in high power impulse magnetron sputt eringA. Anders, P. Ni, M. Panjan . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 41

Mechanism of the instabiliti es in HIPIMS dischargeA. Hecimovic, T. de los Arcos, V. Schulz-von der Gathen, M. Böke,

J. Winter . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 41

Global modeling of the azimuthally rotati ng structure in HIPIMSS. Gallian, R. P. Brinkmann, W. N. G. Hitchon . . . . . . . . . . . . . . . . . . . . . . . 42

Dynamics of the fast – HIPIMS discharge during FINEMET-type fi lms depositi onV. Tiron, I.-L. Velicu, C. Costi n, G. Popa . . . . . . . . . . . . . . . . . . . . . . . . . . . 43

Spokes modelling by pseudo 3D PIC MCCA. Revel, C. Costi n, T. M. Minea . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 43

Kineti c modelling of an Ar-Cu preionized HIPIMS dischargeJ. Bretagne, C. Vitelaru, P. Fromy, T. Minea . . . . . . . . . . . . . . . . . . . . . . . . 44

Balance of powers delivered to magnetrons and balance of depositi on rates in reacti ve bipolar pulsed HIPIMS of aluminum oxideS. Kadlec, J. Čapek, J. Kousal, J. Vyskočil . . . . . . . . . . . . . . . . . . . . . . . . . . . 45

Reacti ve high-power impulse magnetron sputt ering of opti cally transparent zirconium dioxide fi lmsJ. Rezek, J. Vlcek, J. Houska, R. Cerstvy, T. Kozak, J. Kohout . . . . . . . . . . . 46

Reacti vely grown TiN and Ti-Si-N fi lms with high depositi on rate using chopped HIPIMSP. M. Barker, E. Lewin, J. Patscheider . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 46

High-power impulse magnetron sputt ering of CNx

C. Nouvellon, M. Michiels, A. Roobroeck, S. Konstanti nidis,

R. Snyders . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 47

Depositi on of highly insulati ng aluminium nitride (AlN) by DC and HIPIMS technique: comparison of the two tech-niques according to plasma investi gati ons and physical analysisJ. Camus, K. Ait Aissa, Q. Simon, P.-Y. Jouan, L. Le Brizoual,

M. A. Djouadi . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 48

Eff ect of nitrogen fl ow rate on the corrosion resistance of ZrN coati ngs deposited by HIPIMS technologyY. P. Purandare, A. P. Ehiasarian, P. E. Hovsepian . . . . . . . . . . . . . . . . . . . . 48

List of authors . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . .50 – 53


��

HIPIMS as a tool to understand the ti me-domain and energeti cbombardment eff ects on the nucleati on and coalescence of thin metal fi lms on amorphous substrates

D. M��1, V. E��1, G. A��2, U. H��1, K. S��1*

1 P�� C�� P�� D��,IFM-M�� P��, L�� U��,SE-58183, L��, S��

2 I�� P’, D�� P�� M�� M��, U�� P��-CNRSENSMA,SP2MI, T�� 2, B� M. �� P. C��,F-86962 C��-F��, F��-��: ��.��.��

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In the course of the past decade, HIPIMS has been established as an advanced ionized PVD method and extensive research has been performed to understand the fundamentals of HIPIMS process and plasmas and their implicati ons for fi lm growth1-7.

We embark on the next era of HIPIMS by using its unique features as a science tool to improve our understanding offundamental mechanisms during fi lm formati on. In the current contributi on, we uti lize the ti medependent character of the HIPIMS process along with its high degree of ionizati on to study their eff ect on the nucleati on and coalescence of thin metal fi lms on amorphous substrates. Pulsed, ionized vapor fl uxes, generated from high power impulse magnetron sputt ering (HIPIMS) discharges, are employed Ag fi lms on SiO2 substrates. In situ plasma diagnosti cs and parti cle transport simulati ons show that

vapor fl ux pulses with a width of ~200 μs, a frequency in the range 50 to 1.000 Hz and energies up to ~50 eV are provided to the growing fi lm. Moreover, it is shown that the ti me-domain of the depositi on fl ux and its energy can be controlled independently which allows for studying their eff ect on fi lm growth separately. This is done by in situmonitoring of the fi lm growth, by means of wafer curvature measurements and spectroscopic ellipsometry, determining the fi lm thickness where a conti nuous fi lm is formed (dcoal). The results reveal that dcoal decreases from ~210 to ~140 Å when either increasing the pulsing frequency for aconstant pulse amplitude or the pulse amplitude of the material fl ux and the energy of the fi lm forming species for a constant pulsing frequency. Esti mati ons of adatom lifeti mes and the coalescence ti mes show that there are conditi ons at which these ti mes are within the range of themodulati on of the vapor fl ux. Thus, by changing the tempo-ral profi le of the vapor fl ux, nucleati on and coalescence processes can be manipulated. It is suggested that, other than for elucidati ng the atomisti c mechanisms that control pulsed growth processes, the interplay between the ti me scales for diff usion, coalescence and vapor fl ux pulsing can be used as a tool to determine characteristi c surface diff usion and island coalescence parameters.

References[1] V. Kouznetsov, K. Macak, J. M. Schneider, U. Helmersson, and I. Petrov, Surf.

Coat. Technol. 122, 290 (1999).

[2] U. Helmersson, M. Latt emann, J. Bohlmark, A. P. Ehiasarian, and

J. T. Gudmundsson, Thin Solid Films 513, 1 (2006).

[3] A. P. Ehiasarian, Plasma Surface Engineering Research and its practi cal

applicati ons (R. Wei, ed.), 2008, pp.35 – 86.

[4] K. Sarakinos, J. Alami, S. Konstanti nidis, Surf. Coat. Technol. 204, 1661 (2010).

[5] A. Anders, Surf. Coat. Technol. 205, S1 (2010).

[6] D. Lundin and K. Sarakinos, J. Mat. Res 27, 780 (2012).

[7] J. T. Gudmnundsson, N. Brenning, D. Lundin, and U. Helmersson,

J. Vac. Sci. Technol. A 30, 030801 (2012).

Example: Smooth gradient of the morphologyFrom coarse columnar growth to pure amorphous top layer

��

High ionizati on triple:An innovati ve PVD process for advanced coati ng architectures based on HIPIMS and Arc

J. V��, J. M��, T. K��, M. S��-M��, G. E��

A new class of advanced PVD-coaters, the METAPLAS.DOMINO series , for dedicated coating applications comprise both improved vacuum arc evaporators (APA, Advanced Plasma Assisted) and high power impulse magnetron sputtering (HIPIMS) sources (HIPAC – High Ionized Plasma Assisted Coating). The ion cleaning is based on the (AEGD, Arc Enhanced Glow Discharge) process. This combination of the three highly ionized processes is named HI3 (High Ionization Triple). It’s possible to run the processes in different modes, e.g. pure APA arc evaporation or pure HIPAC magnetron sputtering. However the combination of the two high ionized deposition processes to generate multilayer, nanomultilayers and nanocomposite layers opens new horizons in tailoring of coating architectures.

The arc evaporation itself is limited to specific cathode material properties (mostly metal alloys). HIPAC magne-tron sputtering processes can be used to atomize and ionize materials which are difficult to evaporate or not evaporable by cathodic arc, e.g. Si, SiC, WC, TiB2 and others. Specific features of the PVD system equipped with APA arc evaporators and HIPAC magnetron sources will be shown. Selected results of hybrid coatings will be presented. Two advanced coating systems were suc-cessfully realized by the HI3 process: a coating architec-ture based on SiBX by HIPAC to increase the oxidation stability and, a coating type based on VXN by HIPAC to decrease the high temperature friction. Coatings were analysed by SEM, chemical analysis, nano-indentation hardness measurement and oxidation tests. Selected ap-plication results will be presented too. The enclosed fig-ure shows the outstanding tailored coating architecture of SiBX coatings: from columnar to amorphous growth.

��

Advances in process technology and depositi on equipment for HIPIMS coati ngs for cutti ng tools

T. L��, O. L��, W. K��, C. S��

C��C�� AG, A�� 20A4, 52146 W��, G��.��.��

HIPIMS is characterised by short power pulses with an extremely short signal rise ti me.The design of the coati ng equipment need to take this characteristi c into ac-count with regard to feeding the electrical energy into the sputt ering cathodes and fi nally into the plasma.

This paper will present recent results on the correlati on of the hardware design of the machine and the coati ng process. Fundamental research about the effi ciency of the pulse transfer and about methods to transmit an undistorted pulse shape and wave form into the process was done. The end user of a cutti ng tool sets its focus to the properti es of the coati ng and, most important, to the machining characteristi cs of the fi lm. Examples and fi eld data will show how the most up-to-date HIPIMS coati ngs boost both producti vity and quality. SEM images reveal a dense morphology of HIPIMS coati ngs. To this feature can be att ributed that HIPIMS fi lms combine high hardness and


��

Corrosion protecti on by HIPIMS+ deposited CrN-based coati ngs

M. E��*, F. P��, R. T��, G. A��, T. K��

H�� T�� C��, V�� H�� 225928 LL V��, T�� N��

*C�� : +31 77 3559 704 | ��: +31 77 3969 798��.��

Because of the restricti ons for use of hexavalent chrome, companies acti ve in galvanic surface treatments are exten-sively using trivalent chrome. The corrosion protecti on of this surface treatment is not as good as for hexavalent chrome. For certain high-end applicati ons, alternati ve treatments are required.

One advantage of HIPIMS technology is the possibility to make dense coati ngs with low defect density. In theory, this should result in improved corrosion resistance compared to arc and magnetron sputt ered coati ngs. For the study, HIPIMS+ deposited CrN-based coati ngs have been depos-ited on steel substrates. The corrosion protecti on has been determined by salt-spray testi ng and will be discussed.

a relati vely low Young’s modulus indicati ng a high coati ng toughness in a way most favourable for metal cutti ng.

Super smooth coati ngs, free from any droplets, and low compressive stress are the most benefi cial characteristi cs of sputt er coati ngs for cutti ng tools. The eff ecti ve bom-bardment of the growing fi lm with highly ionized species further improves the surface of HIPIMS coati ngs.

��

TiN for forming applicati ons

J. A��, Z. M��

INI �� , M�� 32, 53619 R��, G��

TiN is one of the most used coatings for a number of different cutting and forming applications. The best TiN is typically produced by arc evaporation. However, for many precise forming applications, the abundance of droplets leads to high roughness at the surface of the coated part which necessitates after-treatment of the surface prior to the usage of the part. A large effort has been put in the last years to minimize the number and the size of the emitted droplets during the arc process. Nevertheless, extensive after-treatment of the coated parts is necessary in order to obtain the needed functionality. Recently, a lot of attention has been paid to high-density coating deposition by magne-tron sputtering, especially highly charged techniques.

In the present work, TiN is produced by highly ionized magnetron sputtering where the charge Ti ions are abundant, reaching up to 90 % of the total Ti spe-cies, in the discharge, and the dissociation of the N2

gas is increased. The coatings mechanical properties, including hardness, elastic modulus, surface rough-ness, and morphology are investigated both for paral-lel and angled depositions on the substrate. It is found that, compared to other conventional techniques, dense coatings are produced on all surfaces with much enhance coating homogeneity and properties.

��

Infl uence of Ion bombardment energy on the growth of CrN fi lms by reacti ve magnetron sputt ering and high power impulse magnetron sputt ering

A. P. E��1, B. H��2, I. P��3

1J�� S�� H�� U��,F�� IST | HIPIMS R�� C��, M�� E�� R�� I��, S�� H�� U��, S��, S1 1WB, UK �.��.��.��

2A�� F�� R�� L��, US

3U�� I�� U��-C��, US

Producti on of transiti on metal nitrides with dense structures in industrially relevant conditi ons well below the homo-logous temperature requires assistance by ion bombarding fl ux with energy additi onal to that of a sputt er process. In conventi onal direct current magnetron sputt ering (DCMS) the metal species remain in a non-ionised state and have low energies. Thus, even at high ion-to-neutral rati os of 30, microstructures can be porous if ion energy is not augmented.

Recently, fully dense CrN fi lms have been deposited at low temperature without substrate bias by high power impulse magnetron sputt ering (HIPIMS) technology which ionizes the metal fl ux and dissociates nitrogen molecules within its plasma. It is not clear if the additi onal ionizati on provided by HIPIMS can outweigh a simple additi on of energy by substrate biasing in DCMS. Therefore we compare fl oati ng and biased growth of CrN fi lms by DCMS and HIPIMS technologies as shown in the cross secti onal micrograph in the fi gure.

Mass spectroscopic analyses showed that HIPIMS depositi on produces a factor of 10 higher fl ux of dissociated N1+ compared

to DCMS. A rati o of N1+ : N21+ = 0.4 in the HIPIMS plasma is

factor 5 greater than in DCMS. The crystallinity of the DCMS layers improved with ion energy to a certain extent.How-ever, a step change was observed when ionizati on degree increased in HIPIMS-process. The texture evolved from ran-dom towards (200) as energy and ionisati on increased. (220) growth was eliminated altogether. In HIPIMS layers nuclea-ti on and competi ti ve growth were resolved very quickly and the fi lm structure was very dense. HIPIMS depositi on on top of DCMS layers resulted in rapid closure of voids and establishing of a fully dense structure within 50 nm.Growth of DCMS layers on HIPIMS layers was unable to sustain textured growth because of the low ionizati on of the DCMS process. Results from DCMS-deposited fi lms in-dicate that ion energy alone may be insuffi cient to promote a dense structure and a dominant (200) texture if N1+ : N2

1+

rati o is too low. The HIPIMS results show that elevati ng the N1+ : N2

1+ rati o to a moderate amount promotes the growth of (100) surfaces. Complementi ng this with moderate ion energy produces highly textured fi lms with a fully dense structure.


��

HIPIMS process with oscillatory voltage pulse shapes for direc-ti onal sputt ering applicati ons

R. C��*, B. A��

Z�� I��. /Z�� LLC, 20 C�� B��. S�� 300M��, MA 02048

*C�� : (508)-618-1266 | ��: (508)-618-1265��.��

HIPIMS / HPPMS is a fairly new technology that was devel-oped in early 1990s. One of the important features of high power pulse magnetron sputt ering is the ability to gener-ate IMP (ionized metal plasma) in the most simple and cost eff ecti ve way. The biggest applicati ons of pulsed I-PVD technology could be directi onal sputt ering processes to deposit Cu seed layers into diff erent sized high aspect rati o features (trenches, vias and etc.) for integrated circuit fabricati on.

In this presentati on the experimental data such as the cross-secti onal SEM images, voltage pulse shapes, pulse target power densiti es for directi onal sputt ering of Ta and Cu in diff erent sizes and aspect rati os trenches and vias will be presented. The experiments were performed with Zpulser CypriumTM pulse plasma generator that can generate oscil-latory voltage pulse shapes (oscillati ons frequency is about 20 – 60 kHz) and deliver up to 2 – 3 MW during the oscillati on.

It was found that substrate ion current is a functi on of the voltage oscillati ons frequency and durati on in the pulse. The substrates during all these experiments either had fl oati ng potenti al or were connected to the substrate bias power supply. DC power supply or RF power supply were used as a bias power supply. The RF bias is an important feature for the directi onal sputt ering process for noncon-ducti ve substrates. The DC bias and RF voltage as a func-ti on of RF power at diff erent level of peak power will be presented, as well as the experimental data about fi eld, side and bott om coverage for trenches and vias.

��

Electrical characteristi cs of S3p™ HIPIMS discharge

S. K��*, D. K��, H. R��

OC O�� B��, L��

*C�� .��.��

The new HIPIMS process S3p™ from Oerlikon Balzers allows opti mizing high ionized sputt er processes with regard to depositi on rate, material fl ux ionizati on or hysteresis behavior in reacti ve sputt ering. The full fl exibility in pulse durati on and pulse power density is a unique tool, opening up a wide range of possibiliti es in coati ng process develop-ment. Pulse length of 50 μs to 100 milliseconds and power density from 500 W/cm2 to 2.000 W/cm2 can be applied on a variety of sputt er materials. A magnetron discharge is commonly described by the voltage – current characteristi cs. The characteristi c is aff ected mostly by the gas rarefacti on eff ect, current density, secondary electrons, compound formati on or the target material.

The present work will give examples of Voltage-current density characteristi cs by S3p™ HIPIMS discharge, in com-parison with the work of other research groups. Infl uence of pulse durati on, gas pressure and reacti ve gas will be discussed in detail.

��

New development of HIPIMS power supply with best in class technology and new features

P. O��, A. K��, P. R��, W. G��, P. L��*

HUETTINGER E�� S�. � �.�., M�� 47, 05-220 Z��, P��

*C�� P��.L��.��.��

Our HIPIMS power supply developed years ago, is the first device, which enables sputtering materials with HIPIMS technology on an industrial scale. Based on the long experience in HIPIMS research as well as in indus-trial applications, like tool coating, medical, microelec-tronics, optical, photovoltaic, TruPlasma Highpulse 4000 New HIPIMS power supply has been developed. In the paper new features enabling improving process param-eters and quality of deposited layers are presented.

Especially highlights like: arc management with a various arc detection conditions, optimizing arc management, arc quenching circuit (CLC) minimizing arc energy, full water cooled platform providing high level of compactness, advanced control and monitoring circuits facilitating optimization of process parameters, are discussed.

Finally applicati on of new features and their infl uence on parameters of HIPIMS processes is shown.

��

Depositi on rates and oxygen negati ve ion energy distributi ons during reacti ve HIPIMS of ti tanium in Ne /O2, Ar/O2, Kr/O2 and Xe/O2

gas mixtures

M. B��*, J. W. B��

D�� E�� E�� E��, U�� L��, L��, L69 3GJ, UK

*C�� : +44 (0) 151 794 4572 | �.��.��.��

Reacti ve sputt er depositi on, parti cularly in the presence of electronegati ve gases such as oxygen, oft en leads to the formati on of high energy negati ve ions. These energeti c negati ve ions are formed at, or close to, the target surface and can be detected at the substrate with energies close to the applied target potenti al. The impingement of energeti c negati ve ions onto the substrate has been shown to have detrimental eff ects on the structural1 and electrical2

properti es of the growing fi lm and in some applicati ons it is desirable to miti gate this bombardment while maintaining a high depositi on rate.

In this contributi on, the depositi on rates of reacti ve HIPIMS of Ti in a gas mixture of oxygen and diff erent rare gases (Ne, Ar, Kr and Xe) have been measured using a quartz-crystal microbalance (QCM). The QCM was positi oned above the racetrack directly facing the target surface at diff erent axial positi ons (50 and 100 mm above the target surface). The HIPIMS discharge was operated with a pulse on-ti me ton = 100 μs, a pulse frequency fp = 100 Hz andat a constant average discharge power Pavg = 100 W. The parti al pressure of oxygen was maintained constant at 0.2 pt where pt is the total pressure; pt was varied from 0.4 to 1.2 Pa. By means of energy-resolved mass spectro-metry, the energy distributi on of oxygen negati ve ions (O-) was also measured at the same positi ons and using the same HIPIMS discharge parameters.


It was found that for reacti ve HIPIMS using oxygen mixed with heavier rare gases (i.e. Kr and Xe), the measured intensiti es of high energy O- ions was reduced signifi cantly when compared with those in lighter gas mixtures (i.e. Ne/O2

and Ar/O2). Furthermore, the normalized stati c depositi on rates of reacti ve HIPIMS in Kr/O2 and Xe/O2 were found to be higher than those measured when using Ne/O2 or Ar/O2

gas mixtures at low pressures. It is proposed that this reducti on in the intensity of high energy negati ve ions is due to a combinati on of a larger collisional cross-secti on during the gas transport phase as well as a lower ion-induced secondary electron emission coeffi cient for the Kr/O2 and Xe/O2 gas mixtures, which has previously been shown to be correlated with high energy negati ve (O-) ion emission during reacti ve magnetron sputt ering.3

References[1] Seeger S., Harbauer K. and Ellmer K. 2009 J. Appl. Phys.105, 053305

[2] Ellmer K. and Welzel T. 2012 J. Mater. Res. 27, 765–79

[3] Mahieu S. and Depla D 2007 Appl. Phys. Lett . 90, 121117

��

Plasma characterisati on of the HIPIMS instabiliti es by energy resolved mass spectrometry

Y. A�� G��1*, A. H��2, J. W��2, T. �� A��2

1 P�� S�� D��, H�� A�� L��., 420 E�� B��, W��, WA5 7UN, UK

2 R�� D�� P�� C�� I��, R��-U�� B��, G��

*C�� : +44 1925 445225 | F��: +44 1925 416518��.��.��

HIPIMS plasma discharges are characterised by high plasma densiti es and high ionised parti cle fl uxes. These are the key plasma parameters for the growing fi lm quality in the ion-assisted depositi on process and characterisati on of the

plasma is essenti al to understand and improve the depo-siti on process.

Recently instabiliti es have been observed in HIPIMS [1-2] that show the plasma formed is highly complex and inho-mogeneous. The instabiliti es are well – defi ned bright and dark regions of plasma arranged periodically along the full length of the racetrack of a circular HIPIMS magnetron [2]. The instabiliti es result in intermitt ent enhanced parti cle transport away from the cathode which may be of signifi -cant technological importance [2]. These add complexity to the understanding of the spati al and temporal dynamics of the parti cle fl uxes (ions, neutrals and radicals) and it is of great importance to investi gate this phenomenon in detail to build a bett er understanding of the HIPIMS discharge. In parti cular, we have seen that the instabiliti es behave diff er-ently for diff erent values of the peak current value, changing from a stochasti c situati on to a periodic rotati on situati on [2].

The present work reports the results of an investi gati on with QMS for diff erent values of the peak current. The energy distributi ons of ions and neutral-metal species, »energeti c neutrals«, from a target surface have been measured using a Hiden EQP energy/mass resolved spectrometer. The be-haviour of the HIPIMS discharge was investi gated for many diff erent voltage conditi ons ranging from 400 to 900 V in a pure Ar atmosphere for a copper and chromium target. The integrati on of the ion energy distributi on functi on (IEDF from the neutral-metal »energeti c neutrals» gave a relati ve neu-tral fl ux of both targets at diff erent current conditi ons. The results obtained are shown in Figure 1 and it was found that the represented values as a functi on of the applied current to the target follow the trend of the Voltage-Current charac-teristi cs.

Figure 1: Relati ve neutral fl ux of Cu and Cr target at diff erent current target values

References[1] A. P. Ehiasarian, A. Hecimovic, T. de los Arcos, R. New, V. Schulz-von der Gathen,

M. Böke and J. Winter, Appl. Phys. Lett . 100 114101 (2012)

[2] Instabiliti es in High Power Pulsed Magnetron Plasmas: from Stochasti city to

Periodicity. J Winter, A Hecimovic, T de los Arcos, M Böke , and V Schulz-von der

Gathen. Accepted for J. Phys. D (special issue HIPIMS.)

Expected online publicati on January 2013.

��

A novel, depositi on-tolerant, Langmuir probe suitable for plasma parameter measurement in HIPIMS discharges

D. G��, P. S��, D. O’ S��, M. B. H��

I�� L��., U�� 8 W�� C��, W�� B�� P��, S��, D�� 9, I��

Conventi onal Langmuir probes are diffi cult to operate eff ecti vely in depositi on plasma processes, such as HIPIMS, especially when insulati ng layers are deposited. A novel radio-frequency (rf) biased Langmuir probe (Plato) has been developed to overcome the issues that arise when insulati ng layers are present.

Traditi onal Langmuir probes are cleaned through dc bias induced electron bombardment of the probe ti p. This method is not possible in the presence of an insulati ng layer. Time resolved plasma measurements, through the HIPIMS pulse, using the standard ‘boxcar’ technique is diffi cult since the plasma can change from pulse to pulse. Changes in the work functi on of the standard Langmuir probe ti p material due to contaminati on can also become problemati c over ti me. Our novel rf biased probe provides a soluti on which overcomes most of these issues. Cleaning is not required since the rf bias will penetrate any layers deposited. A probe scan is performed in one rf period which takes place on the order of a micro-second. There-fore, the plasma parameters in individual HIPIMS pulses can be resolved with micro-second ti me resoluti on. The »boxcar« method is therefore not needed. Problems due

to changes in the work functi on are avoided since the rf bias is not sensiti ve to dc fl uctuati ons.

The Plato probe consists of an aluminium disk to which a rf bias is applied since the dc bias sweep can not penetrate the insulati ng layers. Experiments are compared for insu-lated probes (coated with a hard-anodized layer and con-ducti ng probes to validate the technique.

This technique relies on accurate measurement of the rf current and voltage waveforms at the electrode surface. The measured radio-frequency current consists of parti cle fl uxes (real) as well as displacement current (imaginary) – due to the charge stored in the capaciti ve sheath that necessarily forms in front of the planar electrode. The radio-frequency voltage applied to the capaciti ve sheath and real ti me dependant parti cle current are determined to enable the computati on of the plasma parameters.

A novel algorithm is described which allows the real parti -cle current to be derived from the measured waveforms. Plotti ng the real current versus the sheath voltage yields the real current-voltage (IV) characteristi c similar to that of a standard Langmuir probe. Analysis of this characteristi c gives the plasma parameters in the usual way.

Plasma parameters determined with the radio-frequency biased depositi on-tolerant probe (with and without the insulati ng layer) are shown to be in excellent agreement with independent, standard Langmuir probe measurements taken in non reacti ve plasmas. This method conti nues to operate well when additi onal layers are deposited by plasma process.


��

Fe2O3 thin fi lms for water splitti ng applicati on prepared by high power pulsed magnetron and pulsed hollow cathode systems

Z. H��*, Š. K��, M. Č��, J. O��

I�� P��, ASCR �.�.�., N� S�� 2, 182 21 P�� 8, C�� R��

*C�� .��

Fe2O3 semiconductor material was recently found very promising as a photoanode for water splitti ng applicati on. Semiconductor oxide thin fi lms of Fe2O3 were deposited by reacti ve sputt ering in a high power pulse magnetron and in a pulsed hollow cathode plasma jet sputt ering system without external heati ng of the substrate. It was possible to prepare by both methods nanocrystalline or polycrystalline thin fi lms of hemati te Fe2O3. HIPIMS condi-ti ons were capable to deposit smooth, dense nanocrys-talline hemati te. Applicati on of diff erent magnitudes of duty cycle was tested in the range 1 % – 50 %. Quite diff erent preferred orientati on of crystallites relati ve to the substrate surface was observed in dependence on the duty cycle. This texture was apparent at as deposited fi lms and also at thin fi lms annealed aft er depositi on on 600 °C. Hemati te Fe2O3 thin fi lms were deposited also by the low pressure DC pulsed hollow cathode system. The metallic hollow cathode with internal diameter 5 mm and length 30 mm was sputt ered in argon plasma fl ow and reacti ve gas oxygen was supplied directly to the reactor. The hollow cathode discharge was generated by the DC pulsed power supply working in high power pulsed mode. The maximum att ained pulsed current density in our hollow cathode discharge was approximately ≈ 3 A/cm2. The main advantage of this system was the high deposi-ti on rate which was nearly independent on the amount of used oxygen in the plasma. Fe2O3 hemati te thin fi lms were deposited with this system. Surface roughness of fi lms was much higher for the pulsed hollow cathode system

than for pulsed magnetron system. Photoconducti vity and photoelectrochemistry under 1AM illuminati on was measured on deposited on Fe2O3 thin fi lms. IPCE (induced photocurrent effi ciency) was obtained for these samples.

��

Can HIPIMS CrxN serve as alternati ve for hard chromium?

T�� I.*, C�� P.

S��, S�� C�� A�� L�� W�� 3, 3590 D��, B��

*C�� : +32 491 34 53 77 | ��.��.��

Electroplated hard chromium is a common surface fi nishing approach in many engineering industries due to its high hardness and excellent corrosion resistance. However, environmental and health regulati ons on chromates drive the explorati on of alternati ve coati ng methods, among which physical vapor depositi on looks very promising.

This study aims to evaluate PVD CrxN as a viable replace-ment for hard chromium. A way to achieve an increased performance of PVD coati ngs in terms of wear and corrosion resistance is the use of High Power Impulse Magnetron Sputt ering. The HIPIMS technology is believed to allow for denser coati ngs with superior mechanical, tribological and wear resistant properti es compared to DC-MS.

CrxN coati ngs are deposited by means of DC-MS, HIPIMS and combined DC-MS/HIPIMS. Mechanical (Calo test, Nanoindentati on test, Scratch test, 3D Profi lometry, Taber Abrasion test) and tribological (Pin-on-disc test) proper-ti es and corrosion resistance (Salt spray test) of the diff er-ent coati ngs are studied and compared to electroplated hard chromium.

��

Correlati on between the Rock-well indentati on test and the progressive load scratch test for assessment of coati ng adhesion

N. R��, G. F��, M. H��

CSM I��,R�� G�� 4,CH-2034 P��,S��

In recent years it has become current practi ce to employ a wide range of test methods to assess the adhesive properti es of thin fi lms and coati ngs, ranging from the simple tape-peel test to the more advanced pull-off and 3-point bending tests. Many such methods have high operator subjecti vity, high data variability and in many cases are unsuitable for in-dustrial Quality Control (QC) use where assessment is done regularly and oft en by several operators. The Rockwell inden-tati on test (ISO 26443 and VDI 3198) has become common for evaluati ng the adhesion of hard coati ngs deposited on various substrates, but the applied load (1472 N) is oft en too high causing the 200 µm radius diamond indenter to plunge too deeply into the substrate making it diffi cult to classify the resultant coati ng damage around the edges. The pro-gressive load scratch test (ASTM C1624, ISO EN 1071-3, ISO 20502) is now widely used to characterize the adhesion of thin hard coati ngs with high repeatability. However, a direct correlati on between these two methods has never been att empted.

It has been proposed that a smaller radius diamond indenter (possibly 50 µm radius) could be employed with the Rockwell indentati on test, using a lower applied load, in order to con-centrate the maximum stress nearer to the sample surface causing more focused failure of the coati ng-substrate inter-face. The objecti ve of this study is to fabricate samples representati ve of the 6 failure categories of the standard Rockwell test, to then evaluate the same coati ngs with lower load and smaller indenter radius, and thirdly to test the same samples with the progressive load scratch test. It is hoped

that this could lead to bett er correlati on of data obtained with all such methods and aid industry in bett er QC control of their coati ngs.

��

Target implantati on and re-depositi on processes during high power impulse magnetron sputt ering of aluminium

T. �� A��*, A. W��, C. C��, A. H��, A. �� K��, J. W��

R�� D�� P�� , R�� U�� B��U��. 150,D-44801 B��

*C�� T�� A��: +49(0) 234 3227095 | ��: +49(0) 234 3214171

The processes of argon retenti on by the target and re-depositi on of target material were investi gated by X-ray photoelectron spectroscopy (XPS) as functi on of radial positi on for diff erent plasma conditi ons in high power impulse magnetron sputt ering (HIPIMS) of aluminium targets. Signifi cant diff erences in Ar radial concentrati on profi les were observed for diff erent discharge conditi ons. Since the presence of a permanent reservoir of gas within the target can infl uence the characteristi cs of the sputt ered material fl ux (in terms of angular and energy distributi on, for example), it is important to understand the plasma conditi ons for which Ar retenti on by the target takes place and in what magnitude. Inside the racetrack area, Ar ion fl ux-dominated implantati on is compensated by radiati on-enhanced diff usion loss terms. Outside the racetrack, the role of ion implantati on is diminished, and Ar retenti on by the target may stem from a balance between gett er-ing by redeposited Al and ion-induced Ar desorpti on.


This work is funded by the DFG within the framework of the SFB-TR 87.

��

Mechanical properti es of TiSiN coati ngs processed by HIPIMS-pulsed DC hybrid process

M. A�� P�� Y��1, F. L��2,3, F. S��4,5, F. S��6, A. B��1,2

1 IRTES-LERMPS, �� M��, UTBM, 90010 B�� , F��

2 LRC CEA-IRTES-LERMPS, �� M��, UTBM, 90010 B�� , F��

3 DEN/DANS/DPC/SEARS/LISL CEA S��, 91191 G��-��-Y��, F��

pulsed-DC was studied owing the comparison of the fi nal properti es – i.e. microstructural, morphological, mechanical and tribological.

References[1] S. Veprek et al. Thin Solid Films 1 (2005) 476.

[2] J. Patscheider et al. Surf. Coat. Technol.146-147 (2001) 201.

[3] A. Mège-Revil et al. Thin Solid Films 518 (2010) 5932.

[4] F. Sanchett e et al. Surf. Coat. Technol. 205 (2011) 205.

[5] J. B.Choi et al. Thin Solid Films 447-448 (2004) 365.

��

Gyrokineti c descripti on of technical plasmas

R. P. B��*, S. G��, B. S��, D. E��

T�� E�� E��R��-U�� B��44630 B��, G��

*C�� : +49-234-3226336��-��.��.��.��

Many technical plasma processes, like magneti cally en-hanced reacti ve ion etching (MERIE), plasma ion assisted depositi on (PIAD), and of course conventi onal and high-power impulse magnetron sputt ering (dcMS/HIPIMS) employ (parti ally) magneti zed high density plasmas at relati vely low pressures. (Typical values are p ≈ 0.01 – 1 Pa, B ≈ 100 mT, ne ≈ 1016 – 1019 m-3.) These plasmas are, at least in their acti ve regions, characterized by a peculiar ordering of the dynamic length and corresponding ti me scales. Using λD, s, rL, L, λ, and λ* to denote the Debye length, the sheath thickness, the gyrati on radius, the system length, and the elasti c and inelasti c electron mean free paths, respecti vely, the length scales obey

λD << s << rL << L <~ λ << λ*. 1

It is well-known that discharges of this regime are hard to analyze. Conventional fluid models do not apply, and kinetic methods must be used. Numerical simulation

Photo of a 2 inch Al magnetron target exposed to a HIPIMS discharge for 3 minutes.

Superposed are the points where XPS characterizati on was performed, in order to

obtain the radial concentrati on profi le of Ar gas retained by the target

4 I�� C�� D��, L�� S�� M�� ’I�� S�� – UTT, A�� N��-52, P�� T�� H��-C��, 52800 N��, F��

5 LRC CEA-ICD LASMIS, N�� I�� C�� CVD I�� (N��), UTT, A�� N��, �� C��, 52800 N��, F��

6 CEA C��-C�� A�� M�� S��, 91191 G��-��-Y��, F��

*C�� M�� A�� P�� Y�� : +33 3 84 58 37 33 | ��:+33 3 84 58 37 37 E��: ��.��-��-��.��

Superhard TiSiN coati ngs att racts great interested since they exhibit high hardness > 50 GPa1. The reason of the enhanced properti es is att ributed to the possibility of tailoring the TiN size – in the nanometer range – by the content of the amorphous SiNx located at grain boundaries1, 2.

In additi on, it presents an improvement in terms of oxida-ti on resistance if compared with TiN which allows the applicati on on high speed cutti ng tools3. The reason is att ri-buted to the segregati on of SiNx on the grain boundaries which acts as a shield, able to protect the corrosion-prone nitride grains from an aggressive oxidizing atmosphere4. As a matt er of fact, during oxidati on the migrati on of Si to the surface accompanied by the formati on of SiO2 barrier lead to improve the refractory character5.

Several works were devoted to TiSiN nanocomposites thin fi lms processed by chemical and physical vapour deposi-ti on processes. Among the physical vapour depositi on processes, several studies centered the att enti on on the conventi onal DC or RF sputt ering and/or arc evaporati on. However, a lack of informati on regarding the depositi on by using High Power Impulse Magnetron Sputt ering (HIPIMS) was found.

In this study, samples were fabricated by co-sputt ering of Ti and Si targets in order to investi gate the eff ect of nitro-gen fl ow rate and bias voltage on the depositi on of TiN by HIPIMS. Hence, the eff ect of silicon content introduced into the coati ng by co-sputt ering the Si target using conventi onal

using an explicit particle-in-cell scheme (PIC), however, is extremely costly: Its effort number N = ωpeT (L / λD)3

(timesteps × gridpoints at 3D) may exceed 1018.

Our contribution investigates an alternative kinetic description known as gyrokinetics. This approach – actually not one theory but rather a family of theories – very was successfully used in the field of high temperature plasmas1,2. It is based on the insight that the fast gyro motion of the charged particles in magnetized plasmas can be mathe-matically separated from the slower drift motion and »integrated out«, leaving only an effective dynamics which describes the longer time and larger length scales.

Our manuscript will present a transfer of this idea to technical plasmas. It will in particular focus on the ques-ti ons how technical (i.e., low temperature) plasmas diff er from their high temperature cousins, and how those differences – different field topology, magnetization of only the electrons, presence of material walls, presence of neutral gas, etc. – are reflected in the mathematical description.

References[1] Rutherford, P. H., and E. A. Frieman, 1968, Phys. Fluids 11, 569.

[2] A. J. Brizard and T.S. Hahm, Rev. Modern Physics 79, PPPL-4153, 2006.

��

Infl uence of the Y-doping on the oxidati on and mechanical pro-perti es of AlCrN-based coati ngs

F. L��*1,2, M. A�� P�� Y��3, F. S��4,5, P. S��6, F. S��7, A. B��1,3

1 LRC CEA-IRTES-LERMPS, �� M��, UTBM, 90010 B�� , F��

2 DEN/DANS/DPC/SEARS/LISL CEA S��, 91191 G��-��-Y��, F��


measured by pin-on-disc test under dry and boundary lubricati ng conditi ons. Highly viscous commercially avail-able engine oil (Mobil1 10W-60) was used as lubricant. The Raman spectroscopy and X-Ray Diff racti on were used to characterise the wear products to understand the wear mechanism.

It was found that compared to dry sliding conditi on, under lubricati ng conditi on the fricti on coeffi cient of the coat-ing reduces from µ = 0.21 to µ = 0.18 (~ 14.3 %). Raman spectrum was collected from diff erent positi ons of the wear track aft er dry and oil lubricated sliding to investi gate the wear products and in turn to understand the wear mechanism. Raman spectrum indicates that in dry sliding conditi on chromium and iron oxide peaks were present, which was expected due to the operati on of the oxidati ve wear mechanism. However, no oxide wear parti cles were detected when the sliding took place in oil lubricati ng conditi on. Unlike dry sliding conditi on, the wear product found in the wear track was a mixture of chromium car-bide, chromium chloride and chromium sulphide. The XRD anlyses confi rmed the presence of these compounds. The most intensive peak in the XRD patt ern was assigned to chromium sulphide whereas comparati vely lower intensity peaks were recorded for chromium carbide and chromium chloride. Based on these fi ndings, the wear meachnism can be described in the following way. In boundary lubricati on conditi on, the carbon, chlorine and sulphur compounds from the oil react with the metal dopant of the coati ng (Cr) due to high fl ash tempeartures (~ 800 ˚C) at the asperity contacts. The reacti on product is mainly chromium sulphide and comparati vely less amount of chromium chloride and chromium carbide. These com-pounds are adhered to the wear track by forming a thin layer. Among these compounds, chromium chloride has a graphite-like layer-by-layer (low shear strength atomic planes) structure, which acts as a solid lubricant.

Therefore it could be speculated that in boundary lubri-cati on conditi on, the reducti on in fricti on coeffi cient is achieved due to the formati on of solid lubricants such as chromium chloride via tribochemical reacti on mechanism.

3 IRTES-LERMPS, �� M��, UTBM, 90010 B�� , F��

4 I�� C�� D��, L�� S�� M�� ’I�� S�� – UTT, A�� N��-52, P�� T�� H��-C��, 52800 N��, F��

5 LRC CEA-ICD LASMIS, N�� I�� C�� CVD I�� (N��), UTT A�� N��, �� C��, 52800 N��, F��

6 MATEIS, INSA-L��, 21 A�. J�� C��, F69621 V�� C��, F��

7 CEA C��-C�� A�� M��, S��, 91191 G��-��-Y��, F��

*C�� :��: +33 1 69 08 44 08 | ��: +33 1 69 08 77 38��.��.��

The study AlCrN hard layers for high speed machining applicati ons increased during the last years, as commer-cially available coati ngs present high abrasion and oxidati on resistance over 800 °C, thus increasing the tool lifeti mes. Recently, the additi on of alloying elements such as ytt rium are believed to be suitable for enhancing the oxidati on resistance at high temperatures, as reviewed by several authors1.

In this study, AlCrN coati ngs have been deposited by high-power impulse magnetron sputt ering (HIPIMS). This innovati ve technique has been chosen due to its enhanced fi nal properti es in order to improve the current coati ngs usually processed by cathodic arc evaporati on technique.

The results were discussed taking into account the role played by the ytt rium content in AlCrN coati ngs. For this purpose, thermogravimetric measurements were performed in order to evaluate the role of the ytt rium doping if compared with the non-doped material.

It is believed that surface and bulk oxides are suffi ciently plasti c to sustain abrasive wear at high temperatures without spalling eff ects2. Furthermore, they are supposed to increase the wear resistance as they reduce the

fricti on coeffi cients due to the oxides’ formati on which act as protecti ve layer3.

Microstructures and morphology of the deposited coati ngs, before and aft er tests, have been investi gated by means of X-ray diff racti on and scanning electron microscopy (SEM). Nonetheless, the coati ngs’ oxidati on as a functi on of temperature and ti me was quanti fi ed by glow dis-charge opti cal emission spectroscopy (GD-OES).

Finally, samples were submitt ed to mechanical (nanoindentati on) and tribological characteriza-ti on with the aim of correlati ng the fi nal micro-structures to the mechanical behavior.

References[1] Endrino et al., Surf. Coat. Technol. 201 (2007) 4505.

[2] Wright et al., Oxid. Met. 25 (1986) 175.

[3] Ducros et al. Surf. Coat. Technol. (2006) 1045.

��

Study of wear mechanism of chromium doped DLC coati ng by Raman spectroscopy in bound-ary lubricati on conditi on

P. M��*, A. P. E��, P. E. H��

N�� C�� PVD R��, HIPIMS R�� C��, S�� H�� U��, C�� C��, H�� S��, S�� S1 1WB, U�� K��

*C�� 200712��.��

The aim of this work is to study the wear mechanism of chromium doped DLC coati ng (Cr-C) in dry sliding and boundary lubricati on conditi on. The amorphous Cr-C coat-ing was deposited by High Power Impulse Magnetron Sput-tering (HIPIMS) process on hardened (62 HRC) high speed steel substrate. The fricti on coeffi cient of the coati ng was

��

Correlati on between mass-spectrometer measurements and thin fi lm characteristi cs using HIPIMS discharges

A. F��1, S. J��1, J. K��1, F. S��2, M.-C. F��1, P.-Y. J��1, A. D��1

1 U�� N��, UMR CNRS 6502I�� M�� J�� R��, 2 �� H��44322 N��, F��

2 L�� C�� MATPERF CEA-M��, R�� ’A��, 72320 V��, F��

In this work, chromium and chromium nitride thin fi lms were deposited using HIPIMS technology [1]. This IPVD tech-nique provides a lot of interest and is used in the coati ng community since last decade. Inject the power on a short ti me allows us to apply a very high power density on the target. Thus, we achieve a high ionizati on of the metal vapor and by this way, we can enhance the adhesion, the crystal-linity and the hardness, controlling the ion fl ux toward the substrate. That’s why we att empt here to establish the link between plasma and coati ng properti es. Numerous experimental parameters can be used to drive the ion fl ux i.e. the thin fi lm properti es. Among them, duty cycle, pulse width, are studied to bett er understand their real eff ect. One way to esti mate the number and the energy of the ion species consists in mass-spectro-metry measure-ments. Here we use for the plasma diagnosti c a mass-spec-trometer resolved in energy from Hiden (EQP 1000). We choose to associate it with a multi channel analyzer (Ortec) to obtain a ti me resoluti on of 2 µs. Thereby, the delay of arriving species, decay ti me in the post discharge can be analyzed precisely.A correlati on between the in situ diagnosti cs and material analysis will be made. Classical techniques such as XRD, SEM, TEM and XPS were carried out for the material analysis.

References[1] V. Kouznetsov et al. / Surf. Coat. Technol., 122 (1999), 290


��

The study of ti tanium nitride fi lmsdeposited using a hybrid systemcombining cathodic arc depositi onand high power impulse magnetron sputt ering

C.-L. C��1,2, W.-Y. W�1,2*, C.-T. H�2, P.-H. C��2, W.-C. C��2, D.-Y. W��1,2

1 D�� M�� S�� E��, M��D�� U��, 369 W�� R��, P��, C��H��, T��, R.O.C.

2 S�� E�� R�� C��, M��D�� U��, 369 W�� R��, P��, C��H��, T��, R.O.C.

*C�� .��.��

It was known that cathodic arc depositi on (CAD) has been widely used in industry for high quality thin fi lm coati ngs. An extremely high current density (~1012 A/m2) was cre-ated to evaporate and ionize the target material rapidly. However, the CAD also produces macro parti cles or drop-lets along with the depositi on process leading to degrade the fi lm properti es. Magneti c fi lter with diff erent design was therefore adopted to reduce the macro parti cles or droplets. However, the macro parti cles or droplets sti ll can’t be fully eliminated. Lately, a newly developed PVD process known as high power magnetron sputt ering (HIPIMS) was found to have the capability of yielding highly ionized fl ux of both gas and sputt ered materials by applying a high power in short pulses to the target. High plasma density in the order of 1017 to 1019 m-3, which is three orders of magnitude higher than the conventi onal dc magnetron sputt er (dcMS), can therefore be achieved from the large fl uxes of energeti c ions in HIPIMS technique. As a result, a smoother and denser thin fi lm with bett er adhesion to the substrate can be obtained, leading to enhanced mechani-cal, electrical, and opti cal properti es. However, it was also

found the depositi on rate of the HIPIMS process was much slower than conventi onal dcMS. Therefore, a hybrid depo-siti on system combining CAD and HIPIMS was studied in this paper. Furthermore, ti tanium nitride (TiN) fi lm was deposited in such hybrid system to investi gate their micro-structure and the mechanical properti es such as surface roughness, hardness and fricti on coeffi cient. A rectangular and two round Ti targets were used in HIPIMS and CAD techniques, respecti vely. A mixture gas of argon and nitro-gen was introduced to reach the depositi on pressure of 2 × 10-2 torr. Besides, the alternati ng and simultaneous pro-cess of these two depositi on techniques was also investi -gated in this paper.

��

Time-resolved opti cal emission spectroscopy of a vanadium HIPIMS plasma

B. T��*, D. M�K��, M. B��

S�� P�� A28U�� S��NSW 2006A��

*C�� : 02 9114 0846 | F��: 9351 7726�.��.��.��.��

HIPIMS is a sputt ering technique that enables ionised dep-ositi on in the absence of macroparti cles and is therefore att racti ve for applicati ons seeking to improve fi lm quality through ion bombardment. Due to the pulsed mode opera-ti on the plasma properti es vary strongly with ti me. Opti -mising the producti on of ions and the charge state distribu-ti on requires knowledge of how these properti es evolve through the pulse and how they are aff ected by changes in operati ng conditi ons. In this study, we use opti cal emis-sion spectroscopy to examine the evoluti on of the charge states present as a functi on of ti me and pulse voltage. As described in a previous publicati on [1], highly spectrally and temporally resolved Opti cal Emission Spectroscopy (OES)

using a large number of spectral lines can be used to inves-ti gate the underlying plasma processes and relate them to the system parameters. In [1] it was shown that the opti -mum energy effi ciency of producti on of ti tanium ions in HIPIMS depositi on occurred when the voltage was just high enough to enter the highly ionised depositi on regime. In this work, we compare the ti me evoluti on of vanadium HIPIMS plasma with the previous results for ti tanium. Infor-mati on about the ti me evoluti on of electron temperature and charge states is presented.

The introducti on of spati ally resolved sampling enhances understanding of processes underlying the ti me evoluti on observed. The results are used as a foundati on for a model that could be used to fi nd opti mum regimes for depositi on.

Reference[1] A. E. Ross, R. Sangines, B. Treverrow, M.M.M. Bilek, and D.R. McKenzie:

Opti mizing effi ciency of Ti ionized depositi on in HIPIMS. Plasma Sources Sci.

Technol. 20, 035021 (2011)

��

HIPIMS vs DCMS technology to produce tungsten coati ngs for fusion applicati ons

S. M. D��, E. M��*, F. A��, F. M��, V. Z��, M. F��

CNR-I�� E�� I��, C�� S�� U�� 4, 35127 P��, I��

*C�� : +39 049 82958770 | F��: +39 049 8295853�.��.��.��

Carbon-based materials have been used in thermonuclear fusion devices for a long period. The major drawback of a plasma-facing wall with carbon armour, such as graphite or Carbon Fiber Composite (CFC), is their chemical erosion and dust formati on under hydrogen bombardment. Moreover the re-depositi on of carbon layers containing triti um represents a serious safety concern. The use of W

coati ngs deposited on carbon based materials can allow to overcome these problems. The employment of Tungsten as an armour material is convenient because of its high melti ng temperature, good thermal conducti vity, low triti um reten-ti on, low sputt ering rate. W fi lms were deposited by various methods on carbon substrates: Vacuum Plasma Spray (VPS), Chemical Vapor Depositi on (CVD) and Physical Vapor Deposi-ti on (PVD) techniques. However, because of the extreme working conditi ons (neutron bombardement, thermal cyclic fati gue, carbon diff usion, plasma erosion) at present none of the proposed depositi on techniques is completely success-ful. Among the diff erent technologies, HIPIMS seems to be the most promising because it permits to deposit high qual-ity and ultra-dense coati ngs with highly controlled micro-structure and residual stress. This work gives a comparison between the properti es of several W coati ngs obtained by the conventi onal Direct Current Magnetron Sputt ering (DCMS) and High Power Impulse Magnetron Sputt ering (HIPIMS). The used depositi on systems have been custom designed and built. In parti cular, the used HIPIMS generator is the Huetti nger TruPlasma Highpulse one. In front of the 4 inches HIPIMS cathode a single rotati ng tree was mounted provi-ding diff erent target substrate distance (TSD) positi on bet-ween 50 and 200 mm. The substrate can be heated up to 800 °C and biased up to 1200 V. The W coati ngs have been grown on graphite, metal sheets and Si substrates changing progressively the sputt ering parameters to opti mize the pro-cess to obtain the desired thermodynamically stable body-centered-cubic form of metallic tungsten (alfa-W). The tung-sten coati ng fi nal phase depends on substrate bias and tem-perature, depositi on pressure, residual gas species. Multi lay-ered fi lms were produced using Mo as a glue layer because tungsten and carbon can form metallic britt le carbide phases.Furthermore Mo compensates possible thermal expansion mismatch. The crystalline structure and orientati on of the obtained fi lm is analyzed by X-ray diff racti on. The crystallo-graphic parameters are evaluated using MAUD (Material Analysis Using Diff racti on).Their morphology and thickness were determined by elec-tron scanning microscopy. Adhesion properti es were eva-luated by scratch tests and thermal shock tests. Hardness was esti mated by Vickers indentati on.

References[1] C. Ruset et al. / Fusion Engineering and Design 86 (2011) 1677–1680.

[2] G. Piazza et al. / Journal of Nuclear Materials 367–370 (2007) 1438–1443.

[3] H Maier et al. / Phys. Scr. T138 (2009) 014031 (5pp).

[4] H. Maier et al. / Journal of Nuclear Materials 415 (2011) S310–S312.


��

HIPIMS depositi on of TiAlN fi lms on microforming die and its tribological properti es in progressive micro-deep drawing

T. S��1*, H. K��2, T. W��2, Y. T��2, H. N��2, M. Y��1

1 D�� H�� M�� S��, T�� M�� U��, T��, J��

2 T�� M�� I�� T�� R�� I��, T��, J��

*C�� 6-6 A��, H��-��, T�� 191-0065, J��: +81- 042-585-8650 | F��: +81-042-585-5119��-��.��.��

Over the last two decades, microforming technology has been contributi ng on reducing the cost of mass producti on for micro to sub-millimeter range components. In view of the remarkable increase of surface area to volume rati o with miniaturizati on of the process dimension, the fricti on-al behavior appears to become more dominant for the forming process. Especially, from the standpoint of dirt han-dling, contaminati on of products, and unstable formability, dry forming process is strongly required. Thus, the acti viti es to applying the hard fi lm coati ngs on micro-forming die substrates are gradually increasing.

Technical issues on the hard fi lm coati ngs for microforming are the remarkable improvement of the tool life to reduce the cost of maintenance. In general, to enhance the tool life, suffi cient high wear toughness and low fricti on are required. However, additi onally in micro scale forming die, the dimensional accuracy and the uniformity of the fi lm thickness and mechanical properti es also strongly infl uences on the durability of the forming tool. Moreover, to obtain the good tribological performance and stable formability, fi ne smooth surface would be required for the microforming die surface fi nishing.

As overviewed by many researchers, high power impulse magnetron sputt ering (HIPIMS) depositi on fi lms has the ad-vantageous features for the forming tool life, such as dense and smooth surface, and three-dimensional uniformity on complex-shaped substrates. Furthermore, since the number of the process parameter of HIPIMS enhances the control-lability of the fi lm property, the opti mizati on, which corres-ponds to the diff erent kind of die shape and forming process, could be possible. However, the availability and practi cal advantages of HIPIMS depositi on fi lms for the microfor-ming die is not well discussed.

Within this background, this study aims to clarify the applicability and practi cal performance of HIPIMS coati ng fi lms for microforming die. The fundamental studies on the eff ect of pulsing characteristi cs, such as pulsing frequency and durati on, process gas pressure, and bias voltage, on the uniformity of the fi lm properti es are investi gated. Based on this investi gati on, TiAlN fi lm depositi on using HIPIMS is applied to the practi cal micro-deep drawing die. Furthermore, in order to investi gate the practi cal durability of this fi lm, the progressive micro-deep drawing tests up to 1000 shots are carried out with the ultra-thin stainless steel foils of 50μm thickness. By the evaluati on of the transiti on of forming force and the forming die surface, applicability of HIPIMS depositi on fi lms on microforming dies are discussed.

��

Titanium carbide oxide and nitride

HIPIMS and DCMS processes com-

pared from the OES point of view

A. P��1, M. C��1, M. B��2, G. M��2, V. R��3

1 V�� N�� S.C.�.A., V�� S�� C�� 106, 35129, P��, I��

2 U�� P��, D�� F��V�� M�� 8, 35131, P��, I��

3 L�� N�� L�� – INFN, V�� ‘U�� 2, 35020 L��, P��, I��

The aim of this study is to relate the eff ect of high power impulse (HiPI) and direct current (DC) power supplies in the depositi on via magnetron sputt ering (MS) of ti tanium composites such as TiC, TiO2 and TiN on compositi on, structure and mechanical properti es with opti cal emission spectroscopy in industrial conditi ons (target size 12” × 4.9”).

Titanium carbide HIPIMS depositi on process from a ti tanium target in acetylene (C2H2) reacti ve atmosphere shows the presence of Hi emission line in opti cal emission spectra that increases in intensity as a functi on of peak power and acetylene fl ux. No hydrogen lines can be observed in DC process. Moreover HIPIMS coati ngs show lower oxygen content. On the other side the hydrogen content in HIPIMS fi lms for the same C/Ti rati o is always lower than for DC and hardness and conducti vity are higher (ρ < 400 µΩ cm). Titanium oxide HIPIMS depositi on process in oxygen reac-ti ve atmosphere shows the presence of double charged oxygen ions emission lines that are increasing in the hyster-esis going from metal to poisoned mode. On the other side the HIPIMS coati ngs show a refracti ve index always higher than DC and the possibility to obtain ruti le and anatase phases in a controllable way. Also in the case of ti tanium nitride the HIPIMS depositi on process presents very diff er-ent emission line spectra and allows to obtain hard coa-ti ngs with no substrate biasing.

These results will be presented and discussed and the relati on with coati ngs properti es with opti cal emission spectra will be further investi gated through tailored experiments. In parti cular the presence of reacti ve gas ions as strictly related to the sputt ered species will be pointed out comparing OES in HIPIMS and DC sputt er-ing of a ti tanium target in oxygen and nitrogen reacti ve atmospheres to that of a carbon target sputt ering. Hydro-gen dissociati on will be evaluated comparing OES of C2H2, CH4 and H2 reacti ve atmospheres with a carbon target. Furthermore, changes in electrical conducti vity of a-C/TiC depending on the reacti ve gas C2H2 and CH4 will be shown. Oxygen content in ti tanium carbide and nitride HIPIMS and DC coati ngs will be compared.

��

Chromium nitride (CrN) thin fi lms deposited by MPPMS for protec-ti on of diff erent steel substrates

L. M��1*, U. R�� G��1, X. F��2, J. B��1

1 IK4 – T��, S�� P�� T�� U��, I�� G��, 5, 20600 E��, S��

2 IK4 – T��, T�� U��, I�� G��, 5, 20600 E��, S��

*C�� .��.��

Chromium nitride (CrN) thin fi lms are extensively used for steel protecti on due to their high wear resistance, low coeffi cient of fricti on and good corrosion resistance. During the last decades, transiti on metal nitrides have been commonly deposited by either cathodic arc evaporati on (CAE) or dc – magnetron sputt ering (dcMS) techniques providing good quality coati ngs for diff erent applicati ons. However, the emission of macroparti cles (during CAE discharge) or the low ionizati on degree of the sputt ered parti cles (during dcMS discharge) leads to a defecti ve and porous fi lm structure which can compromise the fi nal coati ng properti es. To overcome these problems, recently developed modulated pulsed power magnetron sputt ering (MPPMS) technique has been used for coati ng depositi ons.

CrN fi lms were reacti vely sputt ered in Ar/N2 atmosphere by MPPMS and deposited on high speed steel (M3:2) and AISi 316L stainless steel disks and silicon wafers. N2/Ar rati o was varied from 0.1 – 1.5, in order to obtain diff erent morphologies and crystal phases.

Microstructure and thickness analysis were performed by scanning electron microscopy (SEM). Diff erent crystal-lographic structures were determined by X-ray diff racti on (XRD) using a Cr Kα radiati on. SRV Tribometer was used to simulate reciprocati ng sliding moti on for the evaluati on


of fricti on coeffi cient and wear resistance of diff erent deposited coati ngs. Corrosion tests were carried out by potenti odynamic polarizati on and electrochemical impedance spectroscopy (EIS) techniques in NaCl (0.06M) soluti on.

��

Investi gati ons of very short pulse sequences in HIPIMS mode for reacti ve depositi on of Silica

H. G��*, R. B��, T. P��, G. B��

F�� I�� S�� E�� T�� F�� IST, B�� W�� 54 E, B��, G��

*C�� A��:��.��.��.��: +49 531 2155 576 | F��: +49 531 2155 900

Silica coati ngs are used besides opti cal applicati ons as insulator for electric and sensor applicati ons. For these applicati ons it is most important to produce defect-free fi lms with high fi eld strength. Since reacti ve sputt ering of silica needs a process control and leads to a low deposi-ti on rate, a PECVD-process was investi gated. Preferably for PECVD processes the power supply is connected to the substrate, but in the case of depositi ng an insulator mid frequency or rf–sputt ering is mostly used. In the pre-sented case the plasma source is a HIPIMS driven target.

For high rate depositi on of silica a PECVD-process a Cypri-um power supply (oscillatory plasma) was used. The investi gati ons were carried out using TMS as precursor, a carbon target as plasma source. The peak current density for the processes was in the range of 0.1 A/cm2. The Cur-rent-voltage characteristi cs for diff erent pulse sequences and charging voltages are discussed as well as the deposi-ti on rate in dependence of the working conditi ons (gas fl ow, working pressure, and average power). The insulati ng properti es of the fi lms were characterized by their criti cal leakage fi eld strength.

��

Nb coati ngs for superconducti ng RF applicati ons by HIPIMS

G. T��*, S. C��, A. P. E��

*C�� C��B�� 0019/R-0027T�� D��-V�� S�� C��, S�� C�� C�� (TE-VSC/SCC)

High Energy parti cle accelerators such as the LHC at CERN are essenti ally based on two key elements: RF caviti es to accelerate the parti cles, and magnets to steer the beams. In order to achieve state of the art performance, these devices are oft en made with superconducti ng materials. RF accelerati ng caviti es are usually made of bulk niobium, which guarantees excellent performances with the draw-back of high material cost and requiring very sophisti cated manufacturing technologies. CERN has developed since the 1980s the technology of producing accelerati ng caviti es made of a copper substrate coated with a thin niobium fi lm, which is suffi cient to carry the superconducti ng RF surface currents. The coati ng is usually performed by magnetron sputt ering in UHV, and caviti es produced this way are currently em-ployed in the LHC. Nb/Cu caviti es suff er however from the drawback that their quality factor decreases (ie the power losses increase more than quad-rati cally) with increasing the accelerati ng fi eld, contrary to theoreti cal predicti ons and what is actually seen in bulk niobium caviti es. The origin of this phenomenon is unclear at present, but one possible cause is related to the imper-fect microstructure of magnetron sputt ered fi lms. Nb coat-ings by HIPIMS may thus improve the RF quality of acceler-ati ng caviti es, using substanti ally similar coati ng hardware.

Test coati ngs have been performed at Sheffi eld Hallam Universti ty, in order to study the correlati on between coat-ing parameters such as the current density and the pulse durati on with ionizati on effi ciency. Characterisati on by SEM, TEM, and XRD showed the development of stronger texture, improved crystallinity and smoother coati ng morphology with higher ionisati on. In parallel, RF caviti es and test samples have been coated at CERN using appropri-

ately scaled coati ng parameters, and their superconducti ng properti es, microstructure and texture have been character-ized. The fi rst results of this study are reported in this paper.

��

The structure and tribological properti es of tungsten containing hydrogenated diamond-like carbon coati ngs

Z�� J��*

S�� T�� S�� E�� L��, L�� I�� P��, L�� 730000, P. R. C��

*C�� A��1983�163.��

Tungsten containing hydrogenated diamond-like carbon coati ngs were deposited with unbalanced magnetron sput-tering technology. The eff ect of WC target power on the structure and tribological properti es of W-C:H coati ngs were studied. Microstructure of the coati ngs were analyzed by Raman spectroscopy. Hardness and Young’s modulus were tested on CSM Nano-hardness tester. Tribological properti es of the coati ngs with diff erent WC target power were studied on ball-on-disk tester. The result show that all of the coati ngs have typical diamond-like structure. The hardness of the coati ngs increase gradually as increase of WC target power at fi rst, and then it decrease. Fricti on coeffi cient and wear lifeti me also changed obviously with increase of WC target power. The mechanical and tribo-logical properti es of W-C:H coati ngs were strongly infl u-enced by WC target power. It is important to control WC target power at a proper value to prepare coati ngs with excellent properti es.

��

Titanium-doped MoS2 lubrica-ti ng coati ngs for space precision ball bearings

R.-P. S��*

S�� T�� S�� E�� L��, L�� I�� P��, L�� 730000, P. R. C��

*C�� :��163.��

708C Ball bearings were made of 9Cr18 steel which had precision of class 4, MoS2-Ti composite coati ngs were deposited on inner and outer races of ball bearings by unbalanced magnetron sputt ering system, and bearing cages were made of PTFE-based self-lubricati ng polymers. Bearing’s tribological torques as a functi on of storage ti me in high humidity environment were studied by using LHU-2 thermal & humidity test chamber and Bearing 2000 torque measurement device. Developing bearing vacuum performance test rig to research bearing’s torque as a functi on of running ti me, bearings were dismantled aft er test and using XPS to analyze the surfaces of bear-ing’s races and balls. The results show that storied in the environment of 30 ˚C, 85 % RH, bearing’s running torques increased proporti onally as the storage ti me went on.

When run-in the bearings which were storied for 440 days, the start and average running torques of bearings could come back to the level which was the same as the test start, but the fl uctuati on of bearing’s average running torque increased. Running in one directi on at the speed of 650 r/min, in vacuum environment (~10 – 4 Pa) and ambient temperature, tested bearings showed good running performance with low fricti on torque varied only between 1 g • cm ~ 2 g • cm unti l to the test ended at 1.872 × 108 revoluti ons. XPS analysis showed that astable and sustainable solid lubricati on system was established among bearing’s races, balls andcages.


��

Overcoming HIPIMS depositi on rate limitati ons by hybrid RF / HIPIMS co-sputt ering and its relevance for NbSi fi lms

N.H��1*, O. A��2, T. M��2, S. M��1

1 CSNSM, CNRS – U�� P��-S��, B��. 108, F91405 O��, F��

2 LPGP, CNRS – U�� P��-S��, B��. 210 F91405 O��, F��

*C�� N��.��.��2�3.��: +33 1 69 15 52 80 | F��: +33 1 69 15 50 08

NbSi is an Anderson isolator widely used in low tempera-ture applicati ons such as bolometers and far-infrared detector cameras.[1] It is a very interesti ng system due to its adjustable criti cal temperature Tc that can be regulated between a few mK and a few Kelvin. The criti cal tempera-ture of the NbxSi1-x alloy can be easily controlled through the Nb compositi on x during the co-depositi on process of Nb and Si.

The major requirements of NbSi depositi on process are its reproducibility and uniformity on large area substrates, since the bolometers’ complexity is conti nuously growing with increased number of the microstructured pixels need-ed for THz-range cameras. Furthermore, thicker and denser fi lms might be of interest for next generati on cameras.

Successful NbSi depositi on can be achieved by magnetron co-sputt ering leading to highly controlled plasma thin fi lm processing. The resulti ng samples are amorphous alloys commonly obtained operati ng the magnetrons at very low pressures, as low as 0.06 Pa. Enhancing the depositi on rate at such low pressure is challenging for both conventi onal and HIPIMS driven magnetrons. An alternati ve soluti on is the use of hybrid RF / HIPIMS co-sputt ering, on which focuses this communicati on. The dual magnetron plasma

reactor designed at CNRS-IEF presents excellent charac-teristi cs in conventi onal PVD operati on. Implementi ng the HIPIMS power supply with pre-ionizati on system [2] instead of a DC power supply proved undoubtedly its effi ciency in the same reactor. The pre-ionizati on appears criti cal at very low pressure when only one target is HIPIMS driven.

Moreover, extremely interesti ng results are obtained when the hybrid HIPIMS/RF co-sputt ering is used showing a benefi cial alternati ve to conventi onal depositi on of NbSi fi lms. The low temperature measurements demonstrated surprisingly sharp transiti ons with excellent responses. Moreover, from the set of experiments performed by keep-ing constant the HIPIMS average power, pulse width and repeti ti on rate on one cathode, and by changing the RF power on the other magnetron cathode, it gave new insights into the elementary mechanisms sustaining the plasma at very low pressure. Comparisons with con-venti onal magnetron RF /DC co-sputt ering showed the interest of the hybrid RF / HIPIMS soluti on with equiva-lent depositi on rates but improved fi lm properti es.

These successful results open new ways for further appli-cati ons in cryo-material depositi on.

References[1] “Low temperature NbSi thin fi lm thermometers on Silicon Nitride membranes

for bolometer applicati ons” Ph. Camus, L. Bergé, L. Dumoulin, S. Marnieros and

J. P. Torre, Nuclear Instruments and Methods in Physics Research Secti on A:

Accelerators, Spectrometers, Detectors and Associated Equipment Volume 444,

Issues 1–2, 7 April 2000, Pages 419–422

[2] M. Ganciu, M. Hecq, S. Konstanti nidis, J.P. Dauchot, M. Touzeau,

L. de Poucques et J.Bretagne: World Patent N_WO 2005/090632, 2005

��

The structure and mechanical properti es of Cr2N coati ngs deposited by HIPIMS technology

Z�� H��*

S�� T�� S�� E�� L��, L�� I�� P��, L�� 730000, P. R. C��

*C�� 510��.��

Cr2N coati ngs were deposited by HIPIMS technology. The compositi ons, morphology, mechanical and tribological properti es of Cr2N coati ngs were studied. The composi-ti ons and morphology of the coati ngs were analysed by XRF and SEM. The hardness and Young’s modulus of the caoti ngs were measured with CSM nanohardness tester. The tribological properti es of the coati ngs were evaluated by CSM ball-on disk tester. The result shows Cr2N coat-ings deposited by HIPIMS are more denser, harder that that deposited by dcMS. The hardness of the coati ngs reach 24.6 GPa. The sliding wear tests of Cr2N coati ngs sliding against diff erent ballmaterials shows the lowest COF of 0.48 when sliding against Al2O3 ball and extremely low wear rate of 10-8 mm3 N-1m-1 against 100Cr6 ball.

��

ZrSiN and NbN coati ngs deposited

by HIPIMS for hard coati ng corrosion

protecti on on aluminum

M. C��1*, A. P��1, G. M��2, V. R��3

1 V�� N�� S.C.�.A.V�� S�� C�� 106, 35129, P��, I��

2 U�� P��, D�� F��V�� M�� 8, 35131, P��, I��

3 L�� N�� L�� – INFN, V�� ‘U�� 2, 35020 L�� (P��), I��

*C�� .��.��

The aim of this work is to analyze the main diff erences in the coati ng obtained by two diff erent magnetron sputt er-ing methods: the conventi onal Direct Current Magnetron Sputt ering (DCMS), and the recently developed High Power Impulse Magnetron Sputt ering (HIPIMS) used to deposit single NbN and ZrSiN layers and nano-structured NbN – ZrSiN multi layers. These innovati ve nitrides fi lms deposited in a reacti ve sputt ering atmosphere have been used to cover the aluminum 7075 alloy substrate for hard corrosion resistance applicati on. Many samples have been deposited, varying nitrogen fl ux and substrate polariza-ti on. OES and current waveform were used to highlight the diff erent reacti ve regimes and in the hysteresis.

Compositi onal analysis were carried out by RBS and cross-secti on SEM investi gati on was used to highlight coati ng morphology and the presence of defects. Moreover the diff erences between the HIPIMS and DC and between the substrate bias values were observed on crystal structure by XRD, on coating resistivity by four point probes measurement and on mechanical properties by nano-indentation and microscratch test. Electrochemical impedance spectroscopy and salt-spray test were used to evaluate the corrosion resistance of the diff erent coati ngs.


��

Tungsten coati ngs by HIPIMS as

plasma facing material for nuclear

fusion reactor applicati ons

N. G��1,2, M. P��-L��1, I. F��-M��3,4, E. T��5, A. R��1, F. B��4, J. Y. P��5, J. M. P��1, R. G��-A��1

1 I�� F�� N��, ETSII �� I��, U�� P�� M��, C/ J�� G�� A��, 2, E-28006 M��, S��

2 CEI C�� M��, UCM-UPM

3 I�� E�� S�� (IES), U�� P�� M��, A�� C�� /�, E-28040 M��, S��

4 I�� M�� M��, IMM-CNM-CSIC, I�� N�� 8 PTM, E-28760 T�� C��, M��, S��

5 D��. C�� M��. CISDEM, ETSI �� C��, U�� P�� M��, E-28040 M��, S��

The constant increase in the world populati on and in the development degree leads to a high energy consumpti on. The energy soluti on is a long standing problem which requires innovati ve soluti ons. Nowadays, in combinati on with other sustainable sources of energy, fusion energy can become within the next two decades a real alternati ve to fossil fuels. However, the lack of materials able to withstand the severe radiati on conditi ons (high thermal loads and atomisti c damage) expected in such reactors is a bott le neck for fusion to become a reality.

The main requisite for plasma facing materials (PFM) is to have excellent structural stability since severe cracking or mass loss would hamper their protecti on role which turns out to be unacceptable. Additi onal practi cal requirements for PFM are among others: (i) high thermal shock resist-ance, (ii) high thermal conducti vity (iii) high melti ng

point (iv) low physical and chemical sputt ering, and (v) low triti um retenti on.

W has been proposed to be one of the best candidates for PFM for both laser (IC) and magneti c (MC) confi nement fusion approaches. However, works carried out up to now have identi fi ed some limitati ons for W which have to be defeated in order to fulfi ll specifi cati ons [1, 2, 3]. Nowa-days, the capabiliti es of ultrafi ne grain and nanostructured materials for nuclear fusion reactor applicati ons are being investi gated [4].

We report on the opti mizati on of the HIPIMS parameters for depositi on of nanostructured tungsten coati ngs with a thickness in the micro-meter range. To this aim, we study the infl uence of HIPIMS parameters (target potenti al and pulse frequency) on the W coati ngs morphology, stress state and mechanical properti es. For opti mized parameters, Scanning electron microscope (SEM) images show that coati ngs consist of nano-columns with an average diameter of around 70 nm and a cylindrical shape that grows per-pendicular to the surface substrate. X-Ray diff racti on (XRD) studies show that coati ngs are pure α-phase and polycrys-talline. Opti mized coati ngs show good adhesion to the substrate. Nanoindentati on tests evidence that the coati ngs hardness is as high as ~ 14 GPa.

References[1] Takeshi Hirai, Koichiro Ezato and Patrick Majerus, Materials Transacti ons, 46,

(2005) 412-424

[2] Kajita S., Sakaguchi W., Ohno N., Yoshida N., Saeki T. 2009. Nucl. Fus. 49, 095005

[3] Sharafat S., Takahashi A., Hu Q., Ghoniem N.M. 2009. J. Nucl. Mat. 386-388, 900

[4] M. Rieth et al. private comunicati on

��

Optimization of HIPIMS photo-catalytic titania coatings on polymeric substrates

P. J. K��, M. R��, G. T. W��

S�� E�� G��M�� M�� U��, J�� D�� B��, C�� S��,M�� M1 5GD, UK

Titanium dioxide in its anatase form is widely used in photo-catalyti c applicati ons due to its high photocatalyti c acti vity, stability and low cost. Titania coati ngs directly deposited by conventi onal magnetron sputt ering tend to have an amor-phous microstructure. For the anatase structure to devel-op, substrate heati ng or post-depositi on thermal treatment is usually required, with the anatase crystal phase generally forming at temperatures in excess of 400 °C. This precludes the choice of thermally sensiti ve substrate materials for the photoacti ve coati ng.

Depending on the nature of the driving voltage waveform, high power impulse magnetron sputt ering (HIPIMS) has been shown to deliver a relati vely low thermal fl ux to the substrate, whilst sti ll allowing the direct depositi on of crystalline ti tania coati ngs. Consequently, this technique of-fers the potenti al to deposit photocatalyti cally acti ve ti tania coati ngs directly onto polymeric substrates and, therefore, open up a range of new applicati ons. In the present work a range of ti tanium dioxide thin fi lms were deposited by HIPIMS onto glass substrates in order to study the infl u-ence of various process parameters, such as pressure, pulse frequency and pulse durati on on coati ng structure and photocatalyti c properti es. The photocatalyti c properti es of the coati ngs were assessed by their ability to degrade the organic dye methylene blue under UV and fl uorescent light irradiati on. The degradati on rate of methylene blue was calculated by measuring its absorpti on peak height at 665 nm in conti nuous mode under UV / fl uorescent light source. The hydrophilic properti es of the coati ngs were also investi gated by measuring the contact angle of water drop-lets on the coati ng surfaces.

Opti mised coati ngs then were deposited onto a range of polymeric substrates, such as polyethylene terephthalate (PET), polycarbonate, polypropylene, etc. to assess the suitability of using this method for high-energy, low-temperature depositi on of photoacti ve ti tania coati ngs.

��

Growth of carbon – tungsten nanocomposites by high power impulse magnetron sputt ering from compound targets

G. A��1, R. Y. K��1, F. M��1, R. H��1, R. H��1, W. M��1, J. N��2

1 I�� I�� B�� P�� M�� R��, H��-Z�� D��-R�� .V., P.O. B�� 51 01 19, 01314 D��, G��

2 VON ARDENNE A�� G��H, P�� 19/29, 01324 D��, G��

High power impulse magnetron sputt ering (HIPIMS) ena-bles the implementati on of the advantages of the Ionized Physical Vapour Depositi on paradigm (high proporti on of ionized species and control over parti cle energy) for con-venti onal MS setups. Therefore it triggers not only scienti fi c but also industrial interest.

Here we present a basic study of the processing-structure relati ons of C-W nanocomposite fi lms grown in pulsed direct current (DC) MS and HIPIMS modes. A 3” C-W (~ 10 at. %) compound target has been chosen over single component targets for the investi gati on of principal target surface inter-acti ons initi ated by HIPIMS. Carbon reference fi lms have been grown from pure carbon targets for comparison. The depositi on ti me for all fi lms was identi cal for easy compari-son of growth rates. The fi lm areal density has been determined by Rutherford backscatt ering spectrometry and nuclear reacti on analysis. The fi lm structure has been studied by Raman spectroscopy, X-ray diff racti on and transmission electron microscopy.


For pure carbon targets the duty cycle for a fi xed power was limited by extensive arcing. In contrast, a stable HIPIMS regime can be established for the compound target with a duty cycle as low as ~ 1 %. Resulti ng fi lms consist of WC nanoparti cles embedded in a carbon matrix. The fi lm areal density of tungsten in the C-W fi lms shows only a small drop with decreasing duty cycle (transiti on from pulsed DC to HIPIMS mode). Despite diff erent sputt ering modes (by Ar ions in pulsed DC, by a mixture of Ar/W ions in HIPIMS), the fi lm areal density of carbon does not ex-hibit any signifi cant changes and the typical drop in growth rate going from pulsed DC to a HIPIMS discharge has not been observed. Collisional computer simulati ons using TRIDYN, which take into account changes in surface chem-istry and compositi on during sputt ering, demonstrate a considerable sputt er yield amplifi cati on of carbon when irradiated with a mixture of Ar/W ions. This is in-line with the observed stable carbon fi lm areal density, which can be att ributed to the compensati on of the change in sputt ering ion compositi on by sputt er yield amplifi cati on due to W-enrichment of the target surface.

��

Ellipsometric characterizati on of transparent nickel oxide deposi-ted by reacti ve DC magnetron sputt ering and HIPIMS

D. T. N��, A. F��, J. K��, M. R��-P��, A. G��, L. C��, L. B��, P-Y. J��*

I�� M�� J�� R�� (UMR 6502), 2 �� H��, BP 32229, 44322 N��,C�� 3, F��

*C�� : 00 33 (0)2 40 37 63 24 | F��: 00 33 (0)2 40 37 39 59��-��.��-��.��

The organic photovoltaic cells (OPV) up to now convert 5 % of the solar spectrum and last reports predict that effi cien-cies as high as 10 % can be achieved. For the classical OPV,

charge carrier transport from the photosensiti ve polymer is performed by incorporati on of organic semiconductors which are in contact with metallic electrodes. The inter-faces between metal and organic components as well as the nature of organic semiconductors play an important role for the eff ecti ve charge transport and degradati on processes. Limitati ng the sensiti vity of polymer materials becomes the path for development of hybrid OPV. One possible way is to use inorganic semiconductors. Metal oxide semiconductors as protecti ve layers between metal electrodes and polymers, are interesti ng candidates for achieving charge transport and avoiding the organic-metal interfaces. We propose the NiO as p-type semi-conductor to ensure charge carriers and electron/hole blocking layers. The characteristi c wide gap energy permits one to achieve high transparency for thin fi lms of NiO.

We have deposited transparent p-type semiconducti ve NiO thin fi lms on the conducti ve glass by reacti ve DC magne-tron sputt ering and HIPIMS.

In a previous work1 we have shown that depending on the oxygen content, NiO grows along preferenti al orientati ons: either the most dense [111] directi on for low oxygen percent or [200] for higher oxygen content. We have also highlighted the same behaviour by HIPIMS which can be managed by the frequency and/or the pulse durati on2,3.In this study, we have investi gated the dependence of opti -cal properti es of NiO fi lms using spectroscopic ellipsometry (1.5 – 5.0 eV range). NiO fi lms were obtained when the oxygen content was 15 % in DC case and 9 % in HIPIMS case. Refracti ve index n, exti ncti on coeffi cient k, and gap energy of the NiO fi lms were determined with a refracti ve index gradient changed along the fi lm growth directi on whereas the NiO dispersion functi ons were described using the Tauc Laurentz model…

The general trends identi fi ed for a NiO fi lm with a typical thickness range from 150 to 250 nm shows a decrease of the refracti ve index and an increase of the transparency range when going from the bott om to the top of the layer 4.

References[1] A. Karpinski et al, Vol. 520, Issue 9, 3609–3613 (2012)

[2] A. Ferrec et al, 2nd Internati onal Conference on High Power Impulse Magnetron

Sputt ering (HIPIMS) Braunschweig (2011)

[3] D. T. Nguyen et al, PSE‘12 Garmischpartenkirchen (2012)

[4] G. E. Jellison and F. A. Modine, Appl. Phys. Lett ., 69, 371-374 (1996)

��

The reacti ve high power impulse magnetron sputt ering process for the synthesis of CFx thin fi lms using CF4 and C4F8

S. S��1*, C. G��1, G. K. G��1, J. J��1, G. G��1, Z. C��2, L. H��1

1 T�� F�� P�� D��., D�� P�� (IFM), L�� U��, SE-581 83, S��

2 R�� I�� T�� P�� M�� S��, H�� A�� S��, P.O. B�� 49, H-1525 B��, H��

*�� : +46 13 288 974 | ��: +46 13 137 568��.��.�� (S. S��)

Reacti ve high power impulse magnetron sputt ering (HIPIMS) processes have been explored for the growth of fl uorine-containing amorphous carbon thin fi lms (CFx, 0.15 ≤ x ≤ 0.35) comparing the precursor gases tetrafl uoro-methane (CF4) and octafl uorocyclobutane (c-C4F8). The fl uorine content of the thin fi lms was controlled by varying the parti al pressure of the F-containing gases between 0 mPa and 110 mPa, while keeping the depositi on pressure of 400 mPa and the substrate temperature of 110 °C constant.

The HIPIMS processes were investi gated with ti me averaged positi ve ion mass spectrometry and the resulti ng thin fi lms were characterized regarding their compositi on, chemical bonding and microstructure as well as mechanical proper-ti es. The experimental results are compared to results ob-tained by fi rst-principles calculati ons based on DFT. The calculati ons on the most abundant precursor fragments provide data on their relati ve stability, abundance, and reacti vity. Positi ve ion mass spectrometry on the C4F8 plasma showed, next to inert gas ions, an abundance of CF+, C+, CF2

+

and CF3+ (in this order), whereas only CF3

+ exceeded the Ar+

signal in case CF4 was used. Judged by TEM, all synthesized CFx fi lms are amorphous. Results from X-ray photoelectron

spectroscopy indicate a graphiti c nature for fi lms with fl uo-rine contents below 24 at % and a polymeric structure for fi lms with fl uorine contents above 26 at %.

This is mirrored in their mechanical properti es as the hard-nesses decreases steeply for these CFx thin fi lms exhibiti ng a polymeric structure.

��

Compressive stress generati on through adatom inserti on into grain boundaries in low mobility metal fi lms deposited by high power impulse magnetron sputt ering

D. M��1*, G. A��2, K. S��1

1 P�� C�� P�� D��, D�� P��, C�� B�� (IFM), L�� U��, SE-58183, L��, S��

2 I�� P’, D�� P�� M�� M��, U�� P��-CNRS-ENSMA, SP2MI, T�� 2, B� M. �� P. C��, F-86962 C��-F��, F��

*C�� .��.��

High power impulse magnetron sputt ering has proven to be a versati le ionized PVD technique where coati ng micro-structures and properti es can be tuned by changing the bombarding conditi on through changing the pulse power. In this work we use this versati lity to investi gate the causes of intrinsic stresses in polycrystalline fi lms. Generati on of intrinsic stresses in refractory metals or other high melti ng temperature materials deposited at low temperature have previously been considered originate from two additi ve stress sources; tensile stresses generated from att racti on


between grains over underdense grain boundaries and compressive stresses generated by point defects introduced by energeti c bombardment. Compressive intrinsic stresses has also been suggested to be generated by adatom diffusion into grain boundaries for deposition conditions with highly mobile adatoms, i.e. homologous tempera-tures > ~ 0.2. HIPIMS discharges where used to tune the energeti c bombardment conditi ons during depositi on Mo fi lms at low homologous temperatures and achieve atom mobility in the near surface layers while sti ll freezing the state of the bulk of the fi lm. This allowed us to investi gate the stress-microstructure relati onship post depositi on.

We found that the fi lm stresses ranged from -3 to +0.2 GPa while maintaining a nearly constant stress free latti ce para-meter. This implies that the compressive fi lm stress is not caused by defect creati on in the grains but primarily by grain boundary densifi cati on, a scenario also supported by a correlati on between large compressive fi lm stresses and high fi lm densiti es. Based on this we suggest a growth mechanism acti ve during the energeti c bombardment conditi ons present in HIPIMS fi lm depositi on leading to smooth dense fi lms exhibiti ng compressive stresses.

��

High power impulse magnetron sputter deposition of ITO and AZO thin films

A. E��¹, E. M��², M. Z��¹, A. K��¹, R. K��¹, K. V��¹, A. A��¹, V. K��², J. P��¹*

¹ I�� S�� S�� P��, U�� L��

² A/S S�� R��

*C�� .��.��

High power impulse magnetron sputt ering (HIPIMS) is a promising physical vapour depositi on (PVD) technique with a number of unique properti es, such as an ultra-dense plas-

ma and a high degree of ionizati on of the sputt ered atoms. In this work, HIPIMS was used to deposit In2O3:Sn (ITO) and ZnO:Al (AZO) thin fi lms on polyester substrate rolls. The process was controlled by varying the electrical pa-rameters and the oxygen fl ow based on the opti cal emis-sion line intensiti es measured by Plasma Opti cal Emission Spectroscopy. A photodiode with an oscillograph was used to study the kineti cs within a single power pulse. It was found that HIPIMS reduces the mechanical tension of the fi lms and increases the fl exibility, compared to the fi lms deposited by regular DC sputt ering. There was no oxide growth in the erosion zone of the target, which is an advantage for long depositi on processes. The challenge sti ll to be solved is the relati vely low dynamic depositi on speed, arising from the inability of the power source to provide stable arc-free sputt ering conditi ons at suffi ciently high power levels.

��

Uniform, adhesive, robust Cu/TiO2

DCP and HIPIMS sputt ered fi lms inducing fast bacterial/viral inacti vati on under low intensity solar irradiati onJ. K��1, S. R��1, C. P��1, R. S��2

1 E�� P�� F�� L��EPFL-SB-ISIC-GPAO, S�� 6, CH-1015, L��S��

2 E�� P�� F�� L��EPFL-SB-IPMC-LNNME, B�� PH, S�� 3, CH-1015L��, S��

Sputt ering of Cu1-2 and TiO2/Cu3-4 fi lms on texti le by conventi onal pulsed direct current magnetron sputt er-ing (DCP) and highly ionized pulsed plasma magnetron sputt ering (HIPIMS) was performed to inacti vate E. coli (Gram-negati ve) and methicillin resistant staphylococcus aureus (MRSA, Gram-positi ve). Low intensity sunlight with an intensity of 0.5 – 1 % of solar irradiati on AM1 were

able to accelerate the bacterial inacti vati on. This is impor-tant when precluding the formati on of biofi lms pumping infecti ous bacteria in hospitals, schools and other public places since biofi lms remain acti ve for long-ti mes and are a source of pathogens. Film surface characterizati on was carried out by X-ray fl uorescence (XRF), profi lometry, electron microscopy (HRTEM), AFM, contact angle CA and X-ray photoelectron spectroscopy (XPS). By highly ionized pulsed plasma magnetron sputt ering (HIPIMS) inducing an increased M+-ions energy and high charge density of ~1018-19 e-/m3, a coati ng ~38 nm thick inacti -vated E. coli within 10 minutes by way of a TiO2 60/Cu 40 atomic percent target. By DCP sputt ering the bacte-rial inacti vati on ti me was similar to the one induced by HIPIMS ti mes but a coati ng ~ 600 nm thick was required. Under acti nic light radiati on, samples deposited by pulsed magnetron sputt ering ti me of 150 s induced short inacti -vati on ti mes of ~10 min. This sample presents the most suitable structure-reacti vity for the Cu-clusters on the TiO2. The bactericide acti on under light was due to a synergic eff ect in the TiO2/Cu layers since longer inacti vati on ti mes were observed when sputt ering separately TiO2 or Cu.

DCP sputt ering leads to M+ ionizati on >> 5% and a charge density ~1016 e-/m3 HIPIMS leads to Cu ionizati on of ca. 70 % with a charge density ~1018-19 e-/m3 and with a power per pulse of 1750 W/100 microseconds compared to the DCP power per pulse of 62.3 W/10 microseconds.

The eff ecti ve anti bacterial acti on by the HIPIMS fi lm was possible due to the higher applied V since a higher V increases the transiti on M → M+.

References[1] Osorio, P., Sanjines, R., Ruales, C., Castro, C., Pulgarin, C., Rengifo, J-C. Lavanchy,

Kiwi, J. (2011): Anti microbial Cu-functi onalized surfaces prepared by bipolar

asymmetric DCP- sputt ering. J. Photochem. Photobiol. A, 220, 70-7

[2] Rio, L., Kusiak, E., Kiwi, J., Pulgarin, C., Trampuz C., Bizzini, A (2012): Comparati ve

methods to evaluate the bactericidal acti vity of copper-sputt ered surfaces

against methicillin-resistant Staphylococcus aureus, J. Appl. Microbiol,

78, 8176-8182.

[3] Baghriche, O., Sanjines, R., Pulgarin, C., Rti mi, S., Kiwi, J. (2013): Eff ect of the

spectral properti es of TiO2, Cu, TiO2/Cu sputt ered fi lms on the bacterial

inacti vati on under low intensity acti nic light, Photochem. Photobiol.

A. 251, 50-56.

[4] Rti mi, S., Baghriche, O., Pulgarin, C., Sanjines, R., Kiwi, J (2012): Innovati ve

TiO2/Cu surfaces inacti vati ng bacteria <5 min under low intensity visible/acti nic

light TiO2/Cu surfaces, ACS Appl. Mater. & Interf. 4, 5234-5240.

��

Opti cal emission spectroscopy of aluminum nitride thin fi lms depo-sited by pulsed laser depositi on

J. A. P��*, L. P. V��, H. R��, J. C. C��

*C�� .��

In this work we study the Aluminium Nitride plasma produced by Nd:YAG pulsed laser, (λ = 1064 nm, 500 mJ, τ = 9 ns) with repleti on rate of 10 Hz. The laser interacti on on Al target (99.99 %) under nitrogen gas atmosphere generate a plasma which is produced at room temperature; with variati on in the pressure work from 0.53 Pa to 0.66 Pa matching with a applied laser fl uence of 7 J/cm2 The fi lms thickness measured by profi lometer was 150 nm. The plasma generated was at diff erent pressures was character-ized by Opti cal Emission Spectroscopy (EOS) From emission spectra obtained ionic and atomic species were observed. The plume electronic temperature has been determined by assuming a local thermodynamic equilibrium of the emitti ng species.

Finally the electronic temperature was calculated with Boltzmann plot from relati ve intensiti es of spectral lines. Moreover Surface Acousti c Wave (SAW) devices with a Mo/AlN/Si3N4 confi gurati on have been fabricated, employing AlN-buff er and Mo Channel.


��

Carbon ion producti on using a high-power impulse magnetron sputt ering (HIPIMS) glow plasma

K. Y��1*, H. O��2, S. N��2

1 N�� R�� I��N�� I�� A�� I�� S�� T�� (AIST)AIST T�� C�� 2, T��, I�� 305-8568, J��

2 A�� M�� R�� I��N�� I�� A�� I�� S�� T�� (AIST)1-2-1 N��, T��, I�� 305-8564, J��

*C�� .��.��.��

Carbon ions are signifi cantly produced in a HIPIMS glow plasma by using a self-made magnetron sputt ering plasma source with a target diameter of 150 mm. The magneti c fl ux density on the target and its distributi on are changed by arranging the confi gurati on of the permanent magnet, which is formed as a concentric circle, and the set of the magnet is unbalanced. The important issues to signifi cantly produce carbon ions are (1) a high target voltage so as to obtain a signifi cantly high argon energy, (2) a high density argon plasma and (3) no arc transiti on. In order to enhance the ionizati on of the sputt ered carbon-target species, fi rst of all, magneti c fl ux confi gurati on is varied so as to fi nd a stable glow plasma in HIPIMS, and second, a pulsed source voltage with a short durati on is applied to the target in order to apply high voltage to the target without transiti ng to an arc discharge. Thus, a source voltage over 2000 V can be applied to the target and a glow voltage over 1200 V at the end of the pulse of 5.5 μs. The plasma positi on moves outward on the target by increasing the number of the inner magnet. As a result, the plasma edge approaches to the grounded plate set around the of target. Hence, an arc easily occurs at a lower voltage with an increased number of the inner magnet. In order to confi rm the carbon ion producti on, the opti cal emissions near at the target are

observed using a spectrometer; typically, wavelengths of carbon ions and argon ions of 388 nm and 435 nm, are observed, respecti vely. The increase in the intensity of the opti cal emission is brought by the increases of the consumed power density in the target. The emission intensiti es of argon and carbon ions have a proporti onal relati onship to the consumed power.

As a result, the emission intensity of the carbon ions is pro-porti onal to that of the argon ions. This suggests that the producti on of the carbon ions is based on the electron impact ionizati on occurs to produce the carbon ions in the HIPIMS glow plasma.

��

The blood platelet behavior of ti tanium-copper fi lms by high power pulsed magnetron sputt ering

F. J��1, Y. T��1, K. Y��2*, H. S��1, L. Y��1, Y. L��1, H. N��1*

1 K�� L��. �� A�� M�� T��, M�� E��, S�� J�� U��, C�� 610031, C��

2 N�� R�� I��, N�� I�� A�� I�� S�� T�� (AIST), AIST T�� C�� 2, T��, I�� 305-8568, J��

*C�� .��.��.��

Surface modifi cati on with high-power glow discharges is a promising physical vapor depositi on (PVD) technology for industrial usage. A metal ion density higher than 1018 m-3

can be obtained due to a high power input in the plasma.

This arti cle reports the ti tanium-copper fi lms generated in a high power pulsed sputt ering (HPPS) plasma with a

magnetron sputt ering system, where a substrate is set nearby the target for positi ons of 90 mm. The copper ion release behavior were investi gated via a typical immer-sion test. The electrical- and opti ca characteristi cs are investi gated. The phase compositi on, structure, and concentrati on of elements were investi gated via X-ray diff racti on and X-photoelectron energy spectrum. The blood compati bility is investi gated using in vitro releasing of nitric oxide experiment and blood platelet adhesion.

The results are compared with characteristi cs by direct current magnetron sputt ering (DCMS) process.

��

Depositi on of nickel by inducti vely

coupled impulse sputt ering (ICIS)

D. A. L. L��*, A. P. E��

HIPIMS T�� C��, S�� H�� U��, S��, UK

*C�� : +44 (0) 114 225 2971 | F��: +44 (0) 114 225 3501�.��.��.��

Inducti vely coupled impulse sputt ering (ICIS) is the latest development in the fi eld of highly ionised plasma processes. ICIS combines the advantages of RF-ICP, in that it can sput-ter materials that are typically challenging in conventi onal magnetron based systems such as magneti c materials, with the advantages of highly ionised metal plasma.

By generati ng the plasma inside a high power pulsed-RF coil in combinati on with a magnet free high voltage pulsed cathode it is possible to eliminate the need for a magnetron. This feature enables the generati on of high density highly ionised metal plasma of magneti c material.

This paper gives an overview of the plasma properti es and magneti c properti es of the coati ng. The setup comprises of a 13.56 MHz pulsed RF coil operati ng at a frequency of 500 Hz and a pulse width of 150 µs, which results in a duty cycle of 7.5 % . A pulsed DC voltage of 1900 V was applied

to the cathode to att ract Argon ions and initi ate sputt ering.Opti cal emission spectra (OES) for argon and nickel species sputt ered at a constant pressure of 14 Pa, show a linear in-tensity increase for peak RF powers of 1000 W – 4800 W. The infl uence of pressure on the process was studied at a con-stant peak RF power of 3000 W for pressures of 6 – 26 Pa. Argon neutrals rise linearly with increasing pressure.

Energy resolved Mass Spectroscopy results for Ni1+ show a non-maxwellian ion energy distributi on with a peak at 20 eV. This represents a good value for ion surface mobility without inducing latti ce defects. This can be useful for depositi on onto high aspect rati o structures.

The Nickel depositi on rate is 50 nmh-1 for a RF-power of 3000 W and a pressure of 14 Pa. The microstructure of the coati ngs shows globular growth. For lower process pressure the microstructure changes to dense columnar structures with dendriti c features. Bott om coverage of unbiased vias with width 0.300 µm and aspect rati o of 3.3:1 was 15 % and for an aspect rati o of 1.5:1 was 47.5 %. Perpendicular growth can also be seen on side walls with densifi cati on on the bott om. Parameters for this coati ng are mean valuesfrom a power and pressure matrix. EDX measurements have shown that it is possible to deposit Nickel coati ngs that are not contaminated by inducti on coil material.

The magneti c properti es have been examined by magneto opti cal kerr-eff ect spectroscopy MOKE. This techniqueuti lises the kerr-rotati on of a non-polarised laser to measure the hysteresis loop. For a 200 nm thick ICIS deposited coati ng the results are very close to that of bulk material.

The current work has given an overview of the plasma properti es and depositi on of nickel in an ICIS plasma. These results are very promising for the depositi on of materials that have been diffi cult to uti lise in conventi onal mag-netron sputt ering, specifi cally for magneti c materials.

The authors would like to thank Prof. Olinda Conde and Nikolay Polushkin from the University of Lisbon for their cooperati on in the MOKE measurements.


��

Film depositi on using a 1 inch-sized HIPIMS system

H. O��1, K. Y��2*, S. N��1

1 A�� M�� R�� I��, N�� I�� A�� I�� S�� T�� (AIST),1-2-1 N��, T��, I�� 305-8564, J��

2 N�� R�� I��, N�� I�� A�� I�� S�� T�� (AIST), AIST T�� C�� 2, T��, I�� 305-8568, J��

*C�� .��.��.��

Hard fi lm coati ng with excellent tribological characteristi cs has been tried out and realized using HIPIMS technology. We have been engaging in a development of a coati ng process using a small-scaled magnetron sputt ering source with a target size of 1 inch in diameter. This would be incor-porated in a newly-developed semi-conductor producti on system, which is called »minimal-fabricati on producti on system« [1]. The base of this technology is a fi lm deposi-ti on on a half-inch sized substrate with a small-scaled plasma producti on method. In order to realize the plasma system, the issues below are considered;

1. The plasma generati on system with a water cooling system

2. Suppression of the plasma radial expansion on the sputt ering target, and

3. Facilitati on of the expansion of the sputt ered metallic species (atoms and ions) to the substrate.

A high magneti c fl ux density over 1000 G on the target at a source voltage less than 600 V at a gas pressure as low as 0.6 Pa, where no arc transiti on is observed. Copper fi lms are prepared under these conditi ons. In order to enhance the depositi on rate of the prepared fi lms, a pulse durati on as long as 600 μs at a repeti ti on frequency of 100 Hz is

employed. As a result, the depositi on rate as high as 2.5 μm/min on a 0.5 inch silicon wafer is realized.

References[1] htt p://staff .aist.go.jp/shiro-hara/minimalfab.html

��

Time- and space-resolved laser-induced fl uorescence spectro-scopy in a short-pulse HIPIMS discharge

N. B��1*, M. P��1, S. K��1, R. S��1, 2

1 C�� I�� P��-S�� (C�IPS), CIRMAP, U�� M��,23 P�� P��, B-7000 M��, B��

2 M�� N�� R�� C��, P�� I��, B-7000 M��, B��

*C�� : 0032 65 55 49 56 | ��: 0032 65 55 49 41��.��.��.��

The velocity distributi on functi on of the sputt ered parti clesin the directi on parallel to the planar magnetron cathode is studied by spati ally- and ti me- resolved laser-induced fl uo-rescence spectroscopy in a short-durati on (20 μs) high-power impulse magnetron sputt ering discharge.

The experimental evidence for the neutral and ionized sputt ered parti cles to have a constant (saturated) velocity at the end of the plasma on-ti me is demonstrated. For Ti atoms and ions, the velocity component parallel to the target surface reaches the values of about 5 km/s, which is higher that the values typically measured in the direct cur-rent sputt ering discharges before. This points out on the presence of a strong gas rarefacti on signifi cantly reducing the sputt ered parti cles energy dissipati on during a certain ti me at the end of the plasma pulse, referred to as »rare-

facti on window« in this work. The obtained results are in line with the data collected during the analysis of the plasma off -ti me previously carried out in Britun et al. Appl. Phys. Lett ., 99 (2011) 131504.

The results are compared to the velocity distributi on functi on width corresponding to the Ar metastable atoms present in the HIPIMS discharge (measured in the same directi on), as well as to the recent ti me-resolved mass spectrometry results (measured perpendicularly to the target surface).

��

Angle- and ti me-resolved ion velocity distributi ons in HIPIMS

M. C��1*, P. A��1, V. S��2, J. O��1, S. K��1, Z. H��1, R. H��2

1 I�� P�� ASCR, �. �. �., N� S�� 2, 182 21 P�� 8, C�� R��

2 I�� P��, U�� G��, F��-H��-S��. 6, 17489 G��, G��

*�� : +420 266052418 | ��: +420 286581448��.��

The High Power Impulse Magnetron Sputt ering System (HIPIMS) equipped with 2” in diameter target has been investi gated by means of ti me-resolved mass- and energy-resolved analyser (plasma monitor) from Hiden Ltd., grid-ded retarding fi eld energy analyser (RFEA) from Impedans Ltd. and so called modifi ed Katsumata probe. All the meth-ods allow to determine ion velocity distributi on functi ons (IVDF) in forward directi on to substrate as a functi on of retarding electric fi eld. However, except plasma monitor latt er methods are not able to resolve the mass of parti cles. The newly developed modifi ed Katsumata probe uses astati c magneti c fi eld created by Sm-Co permanent magnets to intercept the most of plasma electron and pull them away back to the plasma bulk. Furthermore, the plasma monitor and the modifi ed Katsumata probe are character-

ized in very small angular acceptance in comparison with the gridded RFEA. The high power impulse magnetron sputt ering system was equipped with pure metallic targets (ti tanium or iron). As working gas a mixture of Ar and O2

was used. The working gas pressure was ranging between 0.5 Pa to 5 Pa. All the diagnosti c instruments were placed at positi on of substrate. All the measurements were carried out under the same conditi ons as the thin oxide fi lms TiO2

and Fe2O3 were deposited. A comparati ve study of all the aforementi oned methods has been carried out.

Results clearly demonstrate an infl uence of angular resolu-ti on on measured IVDF. Unlike gridded RFEA the modifi ed Katsumata probe was able to disti nguish diff erent groupsof ions coming on the substrate in diff erent ti mes of plasma pulse. The gridded RFEA has angular acceptance more than 70 °C and ions reaching its input orifi ce originate from diff erent directi on unlike the modifi ed Katsumata probe which accepts ions only from cone of a small solid angle. The temporally resolved investi gati on with plasma monitor revealed that sputt ered parti cles reach a substrate later on. All the plasma diagnosti c methods revealed sig-nifi cantly enhanced energy tail in ion velocity distributi ons measured in HIPIMS in contrast to dc magnetron or mid-frequency pulsed-dc magnetron. An infl uence of working gas pressure on velocity distributi ons of argon, metallic and reacti ve gas ions specifi cally on presence of high-energy tail is discussed. The plasma monitor proved that under certain plasma conditi ons appearance of double ionized sputt ered and working gas parti cles can beobserved.

The work was supported by the Ministry of Educati on, Youth, and Sports of the Czech Republic through projectLD120012, by the Czech Science Foundati on through projects P205/11/0386, P108/12/2104 and by the COSTActi on MP0804 through the grant STSM 11182.


��

Depositi on rate enhancement in HIPIMS without compro-mising the ionized fracti on of the depositi on fl uxJ. C��1, M. H��2, O. Z��2, J. E. K��-S��2, L. M��2

1 D�� P��, U�� W�� B��, U�� 22, 30614 P��, C�� R��

2 D�� E�� P��, É�� P��-�� M��, P.O. B�� 6079, S�� D��, M��, Q�� H3C 3A7, C��

We systemati cally investi gate and quanti fy diff erent physi-cal phenomena infl uencing the depositi on rate, aD, of Nb coati ngs prepared by High Power Impulse Magnetron Sput-tering (HIPIMS), and propose a straightf orward approach for depositi on rate enhancement through the control of the magnetron’s magneti c fi eld. The magneti c fi eld strength at the target surface, B, of a 50 mm diameter magnetron was controlled by the applicati on of paramagneti c spacers with diff erent thicknesses in between the magnetron sur-face and the target. We found that lowering B achieved by the applicati on of a 2.8 mm thick spacer led to an increase of aD by a factor of ~4.5 (from 10.6 to 45.2 nm min-1) when the discharge was operated at a fi xed average pulse target power density (2.5 kW cm-2). However, the ionized fracti on of the depositi on fl ux onto the substrate was found to be comparable, despite of a large diff erence in B-dependent discharge characteristi cs (magnetron voltage and discharge current). We show that the decrease in aD commonly observed in HIPIMS (ranging from 33 % to 84 % in com-parison with DC magnetron sputt ering in the presented experiments) is governed by diff erent physical processes, depending on the value of B: For high B, the back-att racti on of the target ions towards the target is the dominant eff ect, while for low B the ion back-att racti on, the sub-linear dependence of the sputt ering yield on the ion energy, and the variati on in material transport eff ects are all important.

Finally, we off er a theoreti cal explanati on for the observed results, demonstrati ng that the here-presented conclusions are applicable to all HIPIMS discharges in general.

��

Amorphous carbon matrix – carbon nanotube nanocomposites

V. A. M��1, A. P. E��2

1 Y�� S�� U��, Y��, A��

2 S�� H�� U��, S��, UK

*C�� .��

Developing new sensors on the basis of nanocomposite materials is highly promising. Materials comprising diff er-ent nanostructures may be especially interesti ng due to the diversity of their functi onal possibiliti es. Carbon nanotubes (CNT) incorporated in a diamond-like carbon (DLC) matrix are a promising material because of its high electrical and thermal conducti vity which will enhance the sensiti vity of corresponding semiconductor devices. Nanotechnology research and development can enhance security capabili-ti es by introducing new concepts and improvement the functi onality of existi ng ones. However there is limited knowledge related to mechanisms of the corresponding nanostructure formati on. The ability of varying growth con-diti ons will contribute to advancing the functi onal diversity of materials for specifi c applicati ons. Diamond like carbon (DLC) coati ngs consisti ng of carbon atoms are biocompat-ible due to their high corrosion- resistant properti es, and therefore are an appropriate material for matrix (platf orm).

Nanotube-DLC matrix composite materials have been prepared from the gas phase by a direct current, glow-dis-charge plasma, whereby nanotubes formed spontaneously within the DLC matrix. At various stages of the growth the control of technological processes and plasma compositi on was conducted in real ti me. In contrast to the case of composites with specially-embedded defi ned nanotubes, in our case it is necessary to determine the qualitati ve compositi on of the obtained nanotubes. Thus the treat-

ment of methods used for the growth of the nanocompo-site is very ti mely, moreover such methods are not suffi -ciently developed.

We propose an approach whereby CNT and other nano-structures may be formed using a relati vely simple and cost-eff ecti ve technique of plasma-chemical depositi on. The approach has a great potenti al as it enhances the con-venti onal magnetron sputt ering technology with an addi-ti onal ion source, which off ers a high fl exibility in materials microstructure design. The equipment has a fully comput-erized control for supplying additi onal agents within the plasma thus allowing high experimental precision, which is crucial. Especially interesti ng is the possibility to improve the growth of nanotubes by using additi onal short high power magnetron impulses to inject within the plasma metal species such as Ni and Fe to promote CNT formati on.

The multi tude of nanostructures, their possible arrange-ment, and peculiariti es of processes taking place on the nanostructure-matrix interface all give an opportunity for systemati c experimentati on with the objecti ve of further development of advanced technology.

��

Ionizati on zones, plasma fl ares, self-organizati on, and the asymmetric ejecti on of parti cles in high power impulse magnetron sputt ering

A. A��1*, P. N�1, M. P��2

1 L�� B�� N�� L��1 C�� R��, B��, C�� 94530, USA

2 on leave of absence from the Jožef Stefan Insti tute, Jamova 39, 1000 Ljubljana, Slovenia

*C�� : +1-510-486-6745 | ��.��

Over the last couple of years, several groups reported on self-organized, traveling patt erns observed in the plasma of magnetrons operati ng in high power impulse magnetron sputt ering (HIPIMS) mode. Sideon fast framing and streak camera images indicate that each of the ionizati on zones, a.k.a. plasma spokes, emit a plasma fl are away from the target. A model emerges where the large current seen in HIPIMS can be explained by locally breaking electron confi nement at the edge of an ionizati on zone. The self-organizati on of ionizati on zones is aff ected by both the presence of atoms available for ionizati on, and electrons suffi ciently energeti c to cause ionizati on. Sputt ered atoms as well as gas atoms contributed to the inventory of atoms available for ionizati on, and their presence is aff ected by the locati on and intensity of ionizati on zones. Such positi ve feedback mechanism and energy dissipati on are typical ingredients for self-organized systems, which show features of chaos conditi onally evolving into spati ally symmetric and temporally periodic structures. Associated with those structures are current and parti cle transport, not only to the substrate but also near the plane of the sputt ering target. We report on measurements of azimuthally asym-metric parti cle fl uxes exhibiti ng patt erns associated with traveling ionizati on zones. Side-on image of a Nb HIPIMS discharge in 0.3 Pa Ar, taken with an exposure ti me of 10 ns, 5 cm diameter target, 500 A peak current, 50 Hz. False color indicates intensity of emitt ed light, integrated over the visible spectrum.

For more informati on see P. A. Ni, et al. Appl. Phys. Lett ., 101 (2012) 224102.

��

Mechanism of the instabiliti es in HIPIMS discharge

A. H��, T. �� A��, V. S��-�� G��, M. B��, J. W��

I�� E�� II, R�� D�� P��, R��-U�� B��, 44780 B��, G��


Recently an inhomogenity of the HIPIMS discharge has been reported[1,2]. In our previous papers we demonstrated and explained the infl uence of the power and pressure on the instabiliti es. Furthermore we investi gated transiti on form stochasti c to periodic behaviour[3]. In this contributi on an explanati on of the shape and mechanism of the instabiliti es is presented, based on the experimental observati ons. The experimental results of a 4 camera setup, photomulti plier tube data correlated with the biased fl at probe are pre-sented. A heuristi c model combines a parti cle approach together with a global approach demonstrati ng that both violati on of the β limit and a modifi ed Rayleigh-Taylor instability could be responsible for the mechanism of the instability. Opti cal emission spectroscopy provides an understanding on the diff erent emission profi les for diff erent cathode materials.

References[1] Ehiasarian AP, Hecimovic A, et al., Appl. Phys. Lett . 2012 Mar 12;100(11).

[2] Anders A., Applied Physics Lett ers. 2012 May 31;100(22):224104–224104–5.

[3] Winter J., Hecimovic A. et al, J. Phys. D: Appl. Phys. 45 (2012) 000000 (8pp)

This work is funded by the DFG within the framework of the SFB-TR 87.

��

Global modeling of the azimuthally rotati ng structure in HIPIMS

S. G��1*, R. P. B��1, W. N. G. H��2

1 Ruhr-Universität Bochum, L�� T�� E��, R��-U�� B��, G�� ID, R�� ID 1/124, Universitätsstraße 150, 44801 Bochum, Germany

2 D�� E�� C�� E��, U�� W��-M��

*C�� : +49 (0) 234 32-27294��.��.��, ��.��.��.��

High Power Impulse Magnetron Sputt ering (HIPIMS) is a novelIonized Physical Vapor Depositi on technique, able to achieve an ultra dense plasma with a high ionizati on degree among the sputt ered atoms. This is accomplished by app-lying a large bias voltage to the target in short pulses with low duty cycle.

HIPIMS discharges are characterized by high density plasma (peak electron density 1018 – 1020 m-3) in a strong magneti c eld (100 mT), with highly energeti c secondary electrons (500 – 1000 eV). The combinati on of these factors results in a discharge showing a vast range of instabiliti es ranging from MHz (i.e. modied two stream instability1) to 10 – 100 kHz range. Here we att empt the descripti on of ionizati on zones breaking the azimuthal symmetry of the set up and rotati ngwith about 10 % the E × B drift velocity in the same direc-ti on. This phenomenon has been observed by severalauthors2, 3, 4 in dierent experimental set up. It is argued that these spoke-like structures determine the overall plasma density, carry most of the discharge current and are re-sponsible for anomalous cross eld electron transport. It is therefore fundamental to understand their formati on and relevance in order to characterize the system behavior.

During the on ti me of the bias, the current increases unti l it reaches a maximum then remains constant. Experi-mental observati ons5 show the formati on of a number of features rotati ng, that decrease in number unti l only one spoke remains. It is moreover observed that this spoke rotates with a constant angular velocity. We theorize that the congurati on with one or more spokes depending on the power coupled to the discharge is indeed a »periodic equilibrium« congurati on, to which the system relaxes to when it switches from Conventi onal DC Magnetron Sputt ering to HIPIMS mode. We assume there is a single structure that rotates with a constant speed, during the plateau period of the current. These conditi on are ex-perimentally observed by Hecimovic et al.6 for a 0.17 Pa pressure Ar-Al discharge with -800 V bias and 100 A peak discharge current: the single structure shows stati onary behavior aft er 170 s and rotates with Ω ≈ 80 kHz.

Since the discharge is sustained by very energeti c second-aries and the electrons are far from equilibrium, we de-velop a global model that evolves the electron energy dis-tributi on functi on self-consistently with the rate equati ons for background gas and metal species. The volume average is performed only in the structure region and a net neutral

fl ux term is imposed to model the spoke rotati on at speed Ω r. Within the spoke region the species densiti es ne(Θ) and nn(Θ) are given a shape taken from a simple equilibrium 1D fl uid model: this allows us to specify the net fl ux of neutrals even if the global model does not have an explicit spati al dependence.

The system consisti ng of the Boltzmann equati on for the electron energy distributi on functi on and rate equati onsfor Ar and Al species is evolved in ti me through a pseudo-transit using a sti equati on solver. The tracked densiti es ne(t); nAr(t) and nAl(t) reach a steady state at physically meaningful values aft er only a few periods T = 1/Ω.

References[1] D. Lundin, U. Helmersson, S. Kirkpatrick, S. Rohde, and N. Brenning,

Plasma Sources Science and Technology 17, 025007 (2008).

[2] 2A. Kozyrev, N. Sochugov, K. Oskomov, A. Zakharov, and A. Odivanova,

Plasma Physics Reports 37, 621 (2011).

[3] A. Anders, P. Ni, and A. Rauch. J. of Applied Physics, 111, 5 (2012).

[4] A. P. Ehiasarian, A. Hecimovic, T. de los Arcos, R. New, V. S. von der Gathen,

M. Böke, and J. Winter. Applied Physics Lett ers, 100, 11 (2012).

[5] A. Hecimovic et al., 3rd HIPIMS Conference, Sheeld UK (2012)

[6] A. Hecimovic et al., 65th Gaseous Electronics Conference, Austi n TX (2012) 1

The authors gratefully acknowledge funding by the Deutsche Forschungsgemeinschaft within the frame of SFBTR 87.

��

Dynamics of the fast – HIPIMS discharge during FINEMET-type fi lms depositi on

V. T��*, I.-L. V��, C. C��, G. P��

F�� P��, A�� I�� C�� U��, B��. C�� I ��. 11, I��-700506, R��

*C�� : +40 232 201188 | ��: +40 232 201150��.��.��

The kineti c of the transient plasma parti cles remains an interesti ng fi eld of study for understanding of the com-plex physico-chemical mechanisms involved in the sputt ering and thin fi lms depositi on processes by sput-tering method. The space and ti me evoluti on of the sputt ered parti cles during the pulse plasma and in the aft erglow period is of crucial interest for understanding of the HIPIMS mechanism of sputt ering and depositi on of various materials. The onset of the self-sputt ering regime and the parti cles transport were investi gated using electric measurements (cold and emissive probe), fast imaging, ti me-resolved opti cal emission spectros-copy and space- and ti me-resolved laser spectroscopy. Fe73.5Cu1Nb3Si15.5B7 amorphous thin fi lms have been depos-ited using the HIPIMS technique. The pulse voltage was set to a constant value of -1 kV, for relati vely short pulses (4-20 µs) with a repeti ti on frequency in the range of 0.1 to 2 kHz, att aining a maximum cathode power density of about 5 kW/cm2. The infl uence of certain depositi on conditi ons as working gas pressure, pulse durati on, average power and target-to-substrate distance on the parti cle transport, which is related to depositi on rate, plasma compositi on and thin fi lms properti es, have been studied.

The used plasma diagnosti c methods provide valuable and complementary informati on about the parti cles kineti cs and plasma-target and plasma-substrate interacti on, respecti vely. They were successfully correlated for a bett er understanding of the processes that occur during fi lms depositi on and also for establishing an opti mal set of discharge parameters for obtaining amorphous FINEMET-type thin fi lms with excellent soft magneti c properti es.

��

Spokes modelling by pseudo 3D PIC MCC

A. R��1, C. C��2, T. M. M��3

1 L�� P�� G�� P�� – LPGP, UMR 8578, CNRS – U�� P��-S��,91405 O��, F��


2 A�� I�� C�� U��, F�� P��,B�. C�� I ��. 11, 700506 I��, R��

3 L�� P�� G�� P��, CNRS - U�� P��-S�� 91405 O�� C��, F��

Recently it has been found that spokes are rotati ng around the magnetron axis following the race-track of the target, especially in HIPIMS operati on mode [1]. Many theories have been advanced to explain the origin of these struc-tures based on ion impact onto the target, ionizati on waves, plasma instabiliti es, and the release of electron burst from the cathode. However, the comprehension of this phenomenon is very sparsely and self-consistent modelling can bring new insights, which is the purpose of this communicati on. In the last years we developed a Parti cle-in-Cell code dealing with plasma kineti cs treated by Monte Carlo. Due to the fast variati on of the voltage during the pulse, the reduced ti me-step required by the electron gyro-frequency and the stabil-ity criteria, the model was reduced to 2D. However, the spokes are intrinsic 3D phenomena and hence the third dimension has to be taken into account.

Numerical simulati ons show that the velocity drift E × B/B² combined with the space charge repulsion lead to a non uniformity of the magnetron plasma along the azimuthal directi on resulti ng in the creati on of spokes [2]. To over-come full 3D models, a novel algorithm has been developed and successfully tested.

Indeed, all the test parti cles trajectories in PIC-MCC simula-ti on are calculated in the real 3D space. Hence, the limiti ng point is the knowledge of the electric fi eld in the azimuthal (y) directi on. Using the electric fi eld map obtained at a steady state by 2D modelling of the magnetron discharge in (x, z) plane, it is possible to self-consistently follow the parti cles in (x, y) and (y, z) planes, assuming that E(x, z) is constant (plateau of the pulse). This highly reduces the computati on ti me and produces good qualitati ve results.

The obtained results, such as ion and electron 3D density maps and their projecti on along the azimuthal directi on will be presented and discussed, as well as the eff ect of the ion mass.

References[1] Anders A, Ni P, and Rauch A, Journal of Applied Physics 111, 053304 (2012

[2] N. Brenning, D. Lundin, T. Minea, C. Costi n, and C. Vitelaru, J. Phys. D:

Appl. Phys, 46 (2013) 084005

��

Kineti c modelling of an Ar-Cu preionized HIPIMS discharge

J. B��1*, C. V��1,2, P. F��3, T. M��1

1 L�� P�� G�� P��, CNRS – U�� P��-S��, 91405 O�� C��, F��

2 N�� I�� O��, M��-B��, RO 077125, R��

3 D�� I��, U�� P��-S��, 91405 O�� C��, F��

*C�� .��-��.��

High Power Impulse Magnetron Sputt ering discharges are currently studied for advanced processing parti cularly for the depositi on of thin fi lm materials. In parallel to experi-mental studies and development of novel technologies and industrial applicati ons a great deal of att enti on is focused on modelling and simulati on of this type of discharge.

Monte-Carlo and Parti cle-In-Cell Monte-Carlo-Collision (PIC-MCC) numerical techniques are acti vely used to simu-late the parti cle transport in the discharge, parti cularly, for studying its dynamics. It could be interesti ng for the under-standing of the charged species organizati on, such as spoke instabiliti es which are acti vely studied in the last years. An important aspect of HIPIMS discharges is that they are characterised by non-equilibrium processes in parti cular for what concerns the electron energy distributi on which pre-sents a highly non-maxwellian tail despite the relati vely high α ionizati on rati o which can be as high as 10-2 – 10-1.

The eff ect of this non-maxwellian and non-equilibrium cha-

racter of the eedf (electron energy distributi on functi on) in the magneti zed part of the discharge and its consequences on the kineti c behaviour of the discharge can be captured by a non-equilibrium model associati ng the numerical reso-luti on of the Boltzmann Equati on (BE) for the magneti zed part of the discharge (that we usually call magneti zed nega-ti ve glow) with a Collisional-Radiati ve Model (CRM) for neutral and ionic species created in the plasma. This type of model was already successfully used for the modelling of DC non reacti ve [1,2] and reacti ve discharges [3] and was demon-strated to be eff ecti ve through the comparison of the CRM model results with experimental ones. This approach coupling BE and CRM within one model named OB-ELIX (Orsay Boltzman for Electrons and Excited Spe-cies) is also perti nent in order to emphasize the role of specifi c processes resulti ng from the high density of charged parti cles in HIPIMS plasma. In parti cular, it was established that electron-ion Coulomb collisions play an important role on the electron diff usion current to the anode which was considered as being of Bohm type. At the same ti me, the calculated cathode current is con-sistent with the experimental discharge parameters.

The use of the OBELIX code for the study of temporal beha-viour of a pre-ionized HIMPIS discharge working with a Cop-per cathode in an Argon gas will be presented and compari-son of model data with experimental ones will be made.

References[1] F. Guimarães, J. B. Almeida and J. Bretagne, J. Vac. Sci.Technol. (1991) A 9 133

[2] F. Guimarães and J. Bretagne J, Plasma Sources Sci. Technol. 2 (1993) 127

[3] F Debal, J Bretagne, J P Dauchot, M Hecq and M Wautelet,

Plasma Sources Sci. Technol. 10 (2001) 30–37

��

Balance of powers delivered to magnetrons and balance of depositi on rates in reacti ve bipolar pulsed HIPIMS of aluminum oxide

S. K��1*, J. Č��2, J. K��3, J. V��1

1 HVM P�� L��., N� H�� 2,158 00 P�� 5, C�� R��

2 D�� P��, U�� W�� B��, U�� 22, 30614 P��, C�� R��

3 D�� M�� P��, F�� M�� P��, C�� U��, V H�� 2, 180 00 P�� 8, C�� R��

*�� .��.��

Dielectric fi lms can be deposited by reacti ve bipolar pulsed sputt ering from two metallic targets. The power balance of both magnetrons is important, as it can infl uence magnetron lifeti mes, fi lm thickness homogeneity and fi lm compositi on. Unequal power dissipati on in both magnetrons can some-ti mes be observed. Recently, we have shown [1] that the balance of power delivered to both magnetrons in case of reacti ve sputt ering of Al in O2 depends on the on-ti mes of both magnetrons and on the oxygen parti al pressure. The unequal magnetron power dissipati on can be compensated by unequal rati o of on-ti mes. Moreover, working in the transiti on mode resulted in some negati ve feedback on the power dissipati on in case of reacti ve sputt ering of Al in O2.

Dielectric Al2O3 fi lms have been deposited by reacti ve bipolar pulsed sputt ering from two metallic Al targets in Ar + O2

gas mixture using a MAGPULS BP 1000/100/200 unit. A pair of 2-inch round magnetrons were arranged obliquely in load-lock sputt ering system. The substrate holder enabled splitti ng the sputt ered fl ux of material from each magnetron to one of two substrates. Power input for each magnetron was evaluated from oscilloscopic data of voltage and current.

The bipolar HIPIMS regime used frequency range 1 to 10 kHz, relati vely short on-ti mes and high off -ti mes. The peak mag-netron current was up to 10 A, that is about 350 W/cm2

over the enti re target area at about 250 W average power. Voltage control was used to stabilize the reacti ve working point in the transiti on mode. The on-ti me rati o of both magnetrons has been varied bet-ween 75 % and 125 %. The eff ects on the power balance of both magnetrons are compared with the depositi on rates and properti es of fi lms, measured mainly by spectroscopic ellipsometry. The fi lms deposited close to 100 % on-ti me rati o have refracti ve indices between 1.60 and 1.68 and absorp-


ti on coeffi cients below 0.005. Less balanced powers in magnetrons result in diff erent rate of target oxida-ti on of both magnetrons and to modifi ed depositi on rates. This also aff ects the opti cal properti es of fi lms.

Preliminary results of processes depositi ng Al2O3 fi lms by bipolar pulsed reacti ve sputt ering in a larger scale machine equipped with two rectangular magnetrons are also shown.

References[1] S.Kadlec and J. Vyskočil, “Balance of power delivered to magnetrons in bipolar

pulsed sputt ering of aluminum oxide in high frequency mode and HIPIMS”,

Internati onal Conference on Reacti ve Sputt ering Depositi on (RSD2011)

Dec. 8-9,2011 Linköping, Sweden; online: Vacuum Coati ng

Info: htt p://www.vacuumcoati ng.info/?p=40010

��

Reacti ve high-power impulse magnetron sputt ering of opti cally transparent zirconium dioxide fi lms

J. R��1, J. V��2, J. H��1, R. C��2, T. K��1, J. K��2

1 NTIS – E�� C�� E��, U�� W�� B��, U�� 22, 306 14 P��, C�� R��

2 D�� P��, U�� W�� B��, U�� 22, 306 14 P��, C�� R��

*C�� +420 377632269 | �� +420 377632202��.��.��

High-power impulse magnetron sputt ering with a pulsed reacti ve gas fl ow control, was used for the reacti ve deposi-ti on of opti cally transparent zirconium dioxide fi lms. The depositi ons were performed using a strongly unbalanced magnetron with a planar zirconium target of 100 mm dia-meter in argon-oxygen gas mixtures at the argon pressure of 2 Pa. Two diff erent locati ons of the oxygen gas inlets

above the target with opposite orientati ons (to the target or to the substrate surface) were used. The repeti ti on frequency of a pulsed dc power supply (HMP 2/1, Huet-ti nger Elektronic) was 500 Hz at the average target power density from 5 Wcm-2 to 50 Wcm-2 in a period with duty cycles from 2.5 % to 10 %. Typical substrate temperatures were less than 130 °C during the depositi ons of fi lms on a fl oati ng substrate at the distance of 100 mm from the target. Usual depositi on rates, being around 10 nm/min, were achieved for the target power density of 5 Wcm-2. An opti mized locati on of the oxygen gas inlets above the target and their orientati on to the substrate surface made it possible to improve quality of the fi lms due to mini-mized arcing at the sputt ered target and to enhance their depositi on rates up to 120 nm/min for the target power density of 50 Wcm-2 in a period at the duty cycle of 10 %. This is due to benefi ts of the high-power impulse mag-netron sputt ering discharges. The zirconium dioxide fi lms were found to be crystalline with a predominant monoclinic structure. Their exti ncti on coeffi cient was between 1×10-4

and 5×10-3 (at 550 nm) and hardness between 9 GPa and 16 GPa. Details of the depositi on process, including an energy-resolved mass spectrometry at the substrate positi on (energy distributi on functi ons of positi ve and negati ve ions, and compositi ons of the integral fl uxes of positi ve ions), and measured properti es of the fi lms will be presented.

��

Reacti vely grown TiN and Ti-Si-N fi lms with high depositi on rate using chopped HIPIMS

P. M. B��, E. L��, J. P��

S�� F�� L�� M�� S�� T��L�� N�� M�� S��Ü�� 129, 8600 D��, S��

Chopped HIPIMS, (c-HIPIMS), a modifi ed version of high power impulse magnetron sputt ering (HIPIMS) has been used to deposit ti tanium nitride and ti tanium silicon nitride fi lms. Chopped HIPIMS is a variant of HIPIMS,

where a single pulse is decomposed into several indi-vidual pulses and tailored through soft ware control in the HIPIMS pulse generator to produce pulse sequences. The fi lms grown by this technique were characterised using XRD, XPS and SEM. Mechanical properti es of the fi lms have been assessed using nano-indentati on. The depositi on rate, when using c-HIPIMS depends upon the choice of c-HIPIMS pulse sequence with system-ati c changes for both pulse-on and pulse-off ti mes. In parti cular, depositi on rates are higher than for conven-ti onal HIPIMS, with an increase of 50 % for TiN growth at comparable parameters, whilst maintaining the dense microstructure typical for HIPIMS. The deposi-ti on rates are comparable to direct current magnetron sputt ering (DCMS). The increase in depositi on rate is ascribed to a combinati on of reduced gas rarefac-ti on, less self-sputt ering and reduced ion trapping.Comparison of the fi lms grown by c-HIPIMS to those when using HIPIMS shows microstructure improve-ments when using c-HIPIMS. XPS analysis showed that minimal oxygen contents of less than 1 atomic % are found below 10 nm from the top surface, signifi cantly bett er than for comparable DCMS fi lms. Hysteresis ef-fects and electrical characteristi cs at the target during the running process have been investi gated with vari-ous pulse sequences for c-HIPIMS, i.e. varying pulse-on and pulse-off ti mes. The c-HIPIMS fi lms exhibit similar or enhanced properti es compared to standard HIPIMS fi lms whilst their depositi on rates are increased.

��

High-power impulse magnetron sputt ering of CNx

C. N��1*, M. M��1, A. R��1, S. K��2, R. S��1,2

1 M�� N�� R�� C�� – P�� I��, 1, A�� C��, B-7000 M��, B��

2 C�� I�� P��-S��, CIRMAP, U�� MONS – 20, P�� P��, B-7000 M��, B��

*C�� : +32 65 55 49 37 | F�� : +32 65 55 49 41��.��.��

CNx, referring to under-stoichiometric C3N4 coati ngs, are extensively studied for tribological applicati ons because of their high hardness and low fricti on coeffi cient. Neverthe-less, it is believed that the best properti es would be reached for the ideal βC3N4 compositi on of the coati ng material. Considering magnetron sputt ering-based methods and the need to increase the nitrogen content in the CNx fi lms, increasing the dissociati on and the ionisati on rate of the nitrogen molecules in the plasma could be a promising strategy to achieve this goal. Compared to other magnetron techniques used for thin fi lms depositi on, HIPIMS (High Power Impulse Magnetron Sputt ering) enables a high ioni-zati on of the sputt ered material as well as a strong disso-ciati on and ionisati on of reacti ve molecules.In this work, we are aiming at evaluati ng the relati onship between the pulse parameters, the plasma chemistry, and the incorporati on of N atoms in the CNx fi lms.

CNx fi lms have been synthesized using reacti ve HIPIMS of a graphite target (450 × 150 mm) in pure N2 (2.7 10-2 mbar). The results are compared to those obtained with a conven-ti onal DC reacti ve magnetron discharge (DCMS) at identi cal mean power (PD). In HIPIMS, the discharge voltage VD is set to 1400 V and the pulse durati on τ is varied between 10 and 40 µs. PD is kept constant at 1 kW by adjusti ng the frequency accordingly. We discuss the infl uence of the pulse durati on (τ) and therefore of the peak current (Ipeak) on the chemistry of the fi lm which is determined by X-Ray Photoelectron Spectroscopy (XPS). Opti cal emission spec-troscopy (OES) is performed in order to address the evolu-ti on of the plasma chemistry with respect to the increase of the pulse durati on.

In HIPIMS, the depositi on rate (RD) decreases by increasing Ipeak and τ. Comparing the HIPIMS data with those recorded for DCMS, it is found that, for τ = 10 µs, RD is slightly higher than in DCMS. For all deposited fi lms, the chemical analysis reveals, a low oxygen content (3-6 % at.) and a N/C rati o close to 0.5 which is slightly higher than the rati o obtained in DCMS. The OES data reveal that, for a given value of PD, the N2

+* emission band intensity is increased as compared to the DCMS discharge likely as a result of increased ioni-zati on rate of the N2 gas.


��

Depositi on of highly insulati ng

aluminium nitride (AlN) by DC and

HIPIMS technique: comparison of

the two techniques according to

plasma investi gati ons and physical

analysis

J. C��1, K. A�� A��1, Q. S��1, P.-Y. J��, L. L� B��1, M. A. D��1

1 U�� N��, UMR CNRS 6502,I�� M�� J�� R��,2 �� H��B.P. 32229 – 44322 N�� 3 – F��1

Using DC reacti ve magnetron sputt ering, good crystalline quality AlN fi lms were deposited on silicon substrate (Rock-ing curve FWHM around 2 °C) and even epitaxial growth of AlN on AlGaN [1] and ZnO [2] substrates was achieved. These results were obtained thanks to opti mizati on of ion/neutral rati o and the energy of impinging species [3].

In this work, Magnetron DC but also HIPIMS techniques were used for depositi on of Aluminium nitride (AlN) thin fi lms. The process was opti mized for working with Alumini-um target in reacti ve atmosphere (Ar-N2). As the plasma characterisati on of the ionized species is necessary in order to bett er understand such a specifi c plasma process, ti me-resolved investi gati ons were carried out using Langmuir probe measurements, Opti cal Emission Spectroscopy and Mass Spectrometry. Physical and chemical properti es of the as deposited fi lms are then characterized.

Well crystallised, textured (Rocking curve FWHM around 1°) and thick AlN fi lms were obtained on silicon substrate. Using appropriate substrate for epitaxial growth, some trials have been done by both techniques. The results of such trials will be presented, discussed and a correlati on between the fi lms and plasma properti es will be made.

References[1] C. Duquenne, M. A. Djouadi, P. Y. Tessier, P. Y. Jouan, M. P. Besland, C. Brylinski,

R. Aubry, and S. Delage Applied Phys. Lett . 93 (2008) 052905

[2] Omar Elmazria, Sergei Zhgoon, Laurent Le Brizoual, Frédéric Sarry,

Dmitry Tsimbal and M.A. Djouadi Applied Phys. Lett ers 95, 233503 _2009_

[3] C. Duquenne, P. Y. Tessier, M. P. Besland, B. Angleraud, P. Y. Jouan, R. Aubry, S.

Delage, and M. A. Djouadi, J. Appl. Phys. 104 (2008) 063301

��

Effect of nitrogen flow rate on the corrosion resistance of ZrN coatings deposited by HIPIMS technology

Y. P. P��*, A. P. E��, P. E. H��

N�� C�� PVD R��, S�� H�� U��, S��, U�� K��

*C�� : +44 (0)114 225 3469 | ��: +44 (0) 114 225 3501�.��.��.��.

Monolayer ZrN coati ngs were deposited in an industrial scale PVD machine (HTC-1000-4 target system) by uti lising HIPIMS technique. Only two cathodes furnished with zir-conium targets and with HIPIMS power supplies (Hütti nger Electronic Sp. z o.o., Warsaw, Poland) were operated to deposit the coati ngs on to 1 micron polished M2 High speed steel (HSS), 304 L Stainless steel (SS) specimens and on Si (100) specimens. Prior to depositi on, HIPIMS plasma sustained on a Zirconium (Zr) target was uti lised to pretreat the specimens in order to achieve good adhesion. Follow-ing pretreatment, coati ngs were deposited in a mixed N2

and Ar atmosphere at 400 °C. To analyse the eff ect of nitro-gen fl ow rate on the stoichiometry and hence on the prop-erti es of ZrN coati ngs, following gas fl ow rati os (N2 : Ar) 1 : 2, 1 : 3, 1 : 6 (denoted henceforth as process-P1, P2 and P3 respecti vely) were employed. All coati ngs were depos-ited at -75 V bias with the help of a dedicated bias power supply suitable for HIPIMS (HBP, Hütti nger Electronic) while other depositi on parameters were maintained constant.

As anti cipated, EDX analysis showed that the eff ect of N2

fl ow rate on stoichiometry of the coati ngs was very pro-nounced. The thicknesses of the coati ngs were found to be 1.88 µm, 1.96 µm and 5.2 µm for the processes P1, P2 and P3 respecti vely. P1 coati ngs were found to be over stoichio-metric whereas P2 coati ngs were near stoichiometric and P3 sub-stoichiometric. Coati ng adhesion was measured by progressive loading scratch tests (CSEM REVETEST) and the criti cal load (Lc2) of coati ng failure was observed under opti cal microscope. Dry sliding wear rates were measured with a pin on disk apparatus (CSM TRIBOMETER) by sliding a 6 mm Al2O3 ball under a load of 5 N at a linear speed of 0.1 ms-1 for a total distance of 3500 laps (220 m). Nano hardness values were calculated from the loading-unloading curves obtained from a CSM nanoindentati on tester. All coati ngs exhibited high adhesion (LC2 > 100 N), high hardness (in the range of 31-36 GPa) and dry sliding wear coeffi cient (in the range of KC = 4 – 6 × 10-14 m3N-1m-1).

Eff ect of nitrogen fl ow rate was also very pronounced on the corrosion resistance of the coati ngs. The samples were polarised from -1000 mV to +1000 mV in a 3.5 % NaCl solu-ti on with the help of a Potenti ostat (Gill AC-ACM instru-ments). Though P1 and P2 coati ngs were found to have similar ECorr values of 422 mV and 425 mV respecti vely, in the anodic range of - 320 mV to +100 mV the corrosion current density of P1 (2.9 × 10-7 Acm-2) was an order of magnitude higher than P2 (1.6 × 10-8 Acm-2). Overall, of all the three coati ngs, P2 coati ngs have the lowest current density in the anodic range of -320 mV to +400 mV sug-gesti ng a superior corrosion resistance. Even though P3 coati ngs (sub-stoichiometric) showed the highest (noble) ECorr value of -363 mV they were almost 3 ti mes thicker than the other two coati ngs. The eff ect of N2 fl ow rate on the microstructure observed by cross-secti onal Scanning Electron Microscopy (FEI NOVA-NANOSEM 200) and its infl uence on the corrosion resistance are discussed.


List of authors List of authors

Abadias, G. Insti tut P’, Département Physique et Mécanique des

Matériaux, Université de Poiti ers-CNRS-ENSMA | F

Abraham, B. Zond Inc. /Zpulser LLC | USA

Abrasonis, G. Insti tute of Ion Beam Physics and Materials Research,

Helmholtz-Zentrum Dresden-Rossendorf e.V. | D

Adamek, P. Insti tute of Physics ASCR, v. v. i. | CZ

Agresti , F. CNR-Insti tute for Energeti cs and Interphases | I

Ait Aissa, K. Université de Nantes, UMR CNRS 6502,

Insti tut des Matériaux Jean Rouxel | F

Alami, J. INI coati ngs ltd | D

Anders, A. Lawrence Berkeley Nati onal Laboratory | USA

Antonin, O. LPGP, CNRS – Université Paris-Sud | F

Arab Pour Yazdi, M. IRTES-LERMPS, UTBM | F

Aranda Gonzalvo, Y. Plasma & Surface Division, Hiden Analyti cal Ltd. | UK

Aresta, G. Hauzer Techno Coati ng | NL

Azens, A. Insti tute of Solid State Physics, University of Latvia | LV

Bandorf, R. Fraunhofer Insti tute for Surface Engineering and Thin

Films IST | D

Barker, P. M. Swiss Federal Laboratories for Materials Science and

Technology, Laboratory for Nanoscale Materials Science | CH

Barriga, J. IK4 – Tekniker, Surface Physics and Technology Unit | E

Bazzan, M. Università di Padova, Diparti mento di Fisica | I

Bilek, M. School of Physics A28, University of Sydney | AUS

Billard, A. IRTES-LERMPS, UTBM and LRC CEA-IRTES-LERMPS, UTBM | F

Böke, M. Insti tute for Experimental physics II, Research Department

Plasma, Ruhr-Universität Bochum | D

Bowes, M. Department of Electrical Engineering and Electronics,

University of Liverpool | UK

Bradley, J. W. Department of Electrical Engineering and Electronics,

University of Liverpool | UK

Bräuer, G. Fraunhofer Insti tute for Surface Engineering and Thin

Films IST | D

Bretagne, J. Laboratoire de Physique des Gaz et Plasmas,

CNRS – Université Paris-Sud | F

Brinkmann, R. P. Theoreti cal Electrical Engineering,

Ruhr-University Bochum | D

Briones, F. Insti tuto de Microelectrónica de Madrid, IMM-CNM-CSIC | E

Britun, N. Chimie des Interacti ons Plasma-Surface (ChIPS), CIRMAP,

Université de Mons | B

Brohan, L. Insti tut des Matériaux Jean Rouxel (UMR 6502) | F

Čada, M. Insti tute of Physics, ASCR v.v.i. | CZ

Caicedo, J. C. Insti tute of Microelectronics of Madrid | E

Calatroni, S. Cern, Technology Department-Vacuum Surface and Coati ngs,

Surface Chemistry and Coati ngs group (TE-VSC/SCC) | CH

Camus, J. Université de Nantes, UMR CNRS 6502,


Čapek, J. Department of Physics, University of West Bohemia | CZ

Catti n, L. Insti tut des Matériaux Jean Rouxel (UMR 6502) | F

Cerstvy, R. Department of Physics, University of West Bohemia | CZ

Chang, C.-L. Department of Materials Science and Engineering,

Ming Dao University and Surface Engineering Research Center,

Ming Dao University | TW

Chen, P.-H. Department of Materials Science and Engineering,


Chen, W.-C. Department of Materials Science and Engineering,


Chistyakov, R. Zond Inc. /Zpulser LLC | USA

Colasuonno, M. Veneto Nanotech S.C.p.A. | I

Corbella, C. Research Department Plasmas with complex interacti ons,

Ruhr Universität Bochum | D

Cosemans P. Sirris, Smart Coati ng Applicati on Lab | B

Costi n, C. Faculty of Physics, Alexandru Ioan Cuza University | RO

Czigány, Z. Research Insti tute for Technical Physics and Materials Science,

Hungarian Academy of Sciences | H

de los Arcos, T. Research Department Plasmas with complex interacti ons,

and Insti tute for Experimental physics II, Research

Department Plasma, Ruhr Universität Bochum | D

Deambrosis, S. M. CNR-Insti tute for Energeti cs and Interphases | I

Djouadi, A. Université de Nantes, UMR CNRS 6502,


Ecis, A. Insti tute of Solid State Physics, University of Latvia | LV

Eerden, M. Hauzer Techno Coati ng | NL

Ehiasarian, A. P. Nanotechnology Centre for PVD Research,

HIPIMS Research Centre, SHU | UK

Elofsson, V. Plasma and Coati ngs Physics Division, IFM-Material Physics,

Linköping University | S

Eremin, D. Theoreti cal Electrical Engineering,


Erkens, G. Sulzer Metaplas | D

Fabrizio, M. CNR-Insti tute for Energeti cs and Interphases | I

Favaro, G. CSM Instruments | CH

Fernandez, M.-C. Université de Nantes, UMR CNRS 6502,


Fernandez, X. IK4 – Tekniker, Tribology Unit | E

Fernandez-Marti nez, I. Insti tuto de Microelectrónica de Madrid, IMM-CNM-CSIC

and Insti tuto de Energía Solar (IES),

Universidad Politécnica de Madrid | E

Ferrec, A. Université de Nantes, UMR CNRS 6502,


Fromy, P. Directi on Informati que, Université Paris-Sud | F

Gahan, D. Impedans Ltd. | IRL

Gallian, S. Theoreti cal Electrical Engineering,


Gerdes, H. Fraunhofer Insti tute for Surface Engineering and Thin

Films IST | D

Glazek, W. HUETTINGER Electronic Sp. z o.o. | PL

Gonzalez-Arrabal, R. Insti tuto de Fusión Nuclear, ETSII de Industriales,


Gordillo, N. Insti tuto de Fusión Nuclear, ETSII de Industriales,

Universidad Politécnica de Madrid and CEI Campus Moncloa,

UCM-UPM | E

Goullet, A. Insti tut des Matériaux Jean Rouxel (UMR 6502) | F

Goyenola, C. Thin Film Physics Div., Department of Physics (IFM),


Greczynski, G. Thin Film Physics Div., Department of Physics (IFM),


Gueorguiev, G. K. Thin Film Physics Div., Department of Physics (IFM),


Hala, M. Department of Engineering Physics,

École Polytechnique de Montréal | CDN

Hecimovic, A. Research Department Plasmas with complex interacti ons


Department Plasma ,Ruhr Universität Bochum | D

Heller, R. Insti tute of Ion Beam Physics and Materials Research,


Helmersson, U. Plasma and Coati ngs Physics Division, IFM-Material Physics,


Hess, M. CSM Instruments | CH

Hippler, R. Insti tute of Physics, University of Greifswald | D

Hitchon, W. N. G. Department of Electrical and Computer Engineering,

University of Wisconsin-Madison | USA

Ho, C.-T. Department of Materials Science and Engineering,


Holtzer, N. CSNSM, CNRS – Université Paris-Sud | F

Hopkins, M. B. Impedans Ltd. | IRL

Houska, J. NTIS – European Centre of Excellence,

University of West Bohemia | CZ

Hovsepian, P. E. Nanotechnology Centre for PVD Research,


Howe, B. Air Force Research Lab | USA

Hubička, Z. Insti tute of Physics, ASCR v.v.i. | CZ

Hübner, R. Insti tute of Ion Beam Physics and Materials Research,


Hui, Z. Science and Technology on Surface Engineering Laboratory,

Lanzhou Insti tute of Physics | P. R. China

Hultman, L. Thin Film Physics Div., Department of Physics (IFM),


Jacq, S. Université de Nantes, UMR CNRS 6502,


Jensen, J. Thin Film Physics Div., Department of Physics (IFM),


Jing, F. Key Lab. of Advanced Materials Technology, Ministry of

Educati on, Southwest Jiaotong University | P. R. China

Jouan, P.-Y. Université de Nantes, UMR CNRS 6502,


Jun, Z. Science and Technology on Surface Engineering Laboratory,


Kadlec, S. HVM Plasma Ltd. | CZ

Kalendarevs, R. Insti tute of Solid State Physics, University of Latvia | LV

Kalinko, A. Insti tute of Solid State Physics, University of Latvia | LV

Kelly, P. J. Surface Engineering Group, Manchester Metropolitan

University | UK

Kenardel, J. Université de Nantes, UMR CNRS 6502,


Keraudy, J. Insti tut des Matériaux Jean Rouxel (UMR 6502) | F

Kiwi, J. Ecole Polytechnique Fédérale de Lausanne,

EPFL-SB-ISIC-GPAO | CH

Klemberg-Sapieha, J. E. Department of Engineering Physics,


Klimczak, A. HUETTINGER Electronic Sp. z o.o. | PL

Kment, Š. Insti tute of Physics, ASCR v.v.i. | CZ

Kohout, J. Department of Physics, University of West Bohemia | CZ

Kölker, W. CemeCon AG | D

Komiya, H. Tokyo Metropolitan Industrial Technology Research Insti tute | J

Konstanti nidis, S. Chimie des Interacti ons Plasma-Surface (ChIPS), CIRMAP,

Université de Mons | B

Kousal, J. Department of Macromolecular Physics, Faculty of

Mathemati cs and Physics, Charles University | CZ

Kozak, T. NTIS – European Centre of Excellence,


Kozlovs, V. A/S Sidrabe Riga | LV

Krassnitzer, S. OC Oerlikon Balzers | LI

Krienke, T. Sulzer Metaplas | D

Krug, T. Hauzer Techno Coati ng | NL

Kumar, R. Y. Insti tute of Ion Beam Physics and Materials Research,


Kurapov, D. OC Oerlikon Balzers | LI


List of authors List of authors

le Brizoual, L. Université de Nantes, UMR CNRS 6502,


Lemmer, O. CemeCon AG | D

Leng, Y. Key Lab. of Advanced Materials Technology, Ministry of


Lesiuk, P. HUETTINGER Electronic Sp. z o.o. | PL

Lewin, E. Swiss Federal Laboratories for Materials Science and Tech-

nology, Laboratory for Nanoscale Materials Science | CH

Leyendecker, T. CemeCon AG | D

Loch, D. A. L. HIPIMS Technology Centre, Sheffi eld Hallam University | UK

Lomello, F. LRC CEA-IRTES-LERMPS, UTBM and DEN/DANS/DPC/

SEARS/LISL CEA Saclay | F

Macevskis, E. A/S Sidrabe Riga | LV

Magnfält, D. Plasma and Coati ngs Physics Division, Department of Physics,

Chemistry and Biology (IFM), Linköping University | S

Mandal, P. Nanotechnology Centre for PVD Research,


Maric, Z. INI coati ngs ltd | D

Marnieros, S. CSNSM, CNRS – Université Paris-Sud | F

Marti nu, L. Department of Engineering Physics,


Matt ei, G. Università di Padova, Diparti mento di Fisica | I

McKenzie, D. School of Physics A28, University of Sydney | AUS

Meliksetyan, V. A. Yerevan State University | AM

Mendizabal, L. IK4 – Tekniker, Surface Physics and Technology Unit | E

Michiels, M. Materia Nova Research Center – Parc Initi alis | B

Minea, T. LPGP, CNRS – Université Paris-Sud | F

Minea, T. Laboratoire de Physique des Gaz et Plasmas,

CNRS – Université Paris-Sud | F

Miorin, E. CNR-Insti tute for Energeti cs and Interphases | I

Möller, W. Insti tute of Ion Beam Physics and Materials Research,


Montagner, F. CNR-Insti tute for Energeti cs and Interphases | I

Mueller, J. Sulzer Metaplas | D

Munnik, F. Insti tute of Ion Beam Physics and Materials Research,


Nagasaka, H. Tokyo Metropolitan Industrial Technology Research Insti tute | J

Nakano, S. Advanced Manufacturing Research Insti tute, Nati onal Insti tute

of Advanced Industrial Science and Technology (AIST) | J

Nan, H. Key Lab. of Advanced Materials Technology, Ministry of


Neidhardt, J. VON ARDENNE Anlagentechnik GmbH | D

Nguyen, D. T. Insti tut des Matériaux Jean Rouxel (UMR 6502) | F

Ni, P. Lawrence Berkeley Nati onal Laboratory | USA

Nouvellon, C. Materia Nova Research Center – Parc Initi alis | B

O’ Sullivan, D. Impedans Ltd. | IRL

Ogiso, H. Advanced Manufacturing Research Insti tute,

Nati onal Insti tute of Advanced Industrial Science and

Technology (AIST) | J

Olejnicek, J. Insti tute of Physics ASCR, v. v. i. | CZ

Ozimek, P. HUETTINGER Electronic Sp. z o.o. | PL

Palmucci, M. Chimie des Interacti ons Plasma-Surface (ChIPS),

CIRMAP, Université de Mons | B

Panizo-Laiz, M. Insti tuto de Fusión Nuclear, ETSII de Industriales,


Panjan, M. Jožef Stefan Insti tute | SLO

Papa, F. Hauzer Techno Coati ng | NL

Pastor, J. Y. Dept. Ciencia Mat. CISDEM, ETSI de Caminos,


Patelli, A. Veneto Nanotech S.C.p.A. | I

Patscheider, J. Swiss Federal Laboratories for Materials Science and Technology,

Laboratory for Nanoscale Materials Science | CH

Pérez, J. A. Insti tute of Microelectronics of Madrid | E

Perlado, J. M. Insti tuto de Fusión Nuclear, ETSII de Industriales,


Petrov, I. University of Illinois at Urbana-Champaign | USA

Popa, G. Faculty of Physics, Alexandru Ioan Cuza University | RO

Preller, T. Fraunhofer Insti tute for Surface Engineering and Thin

Films IST | D

Pulgarin, C. Ecole Polytechnique Fédérale de Lausanne,


Purandare, Y. P. Nanotechnology Centre for PVD Research,

Sheffi eld Hallam University | UK

Purans, J. Insti tute of Solid State Physics, University of Latvia | LV

Randall, N. CSM Instruments | CH

Ratova, M. Surface Engineering Group, Manchester Metropolitan

University | UK

Revel, A. Laboratoire de Physique des Gaz et des Plasmas – LPGP,

UMR 8578, CNRS – Université Paris-Sud | F

Rezek, R. NTIS – European Centre of Excellence,


Riascos, H. Insti tute of Microelectronics of Madrid | E

Richard-Plouet, M. Insti tut des Matériaux Jean Rouxel (UMR 6502) | F

Rigato, V. Laboratori Nazionali di Legnaro – INFN | I

Rivera, A. Insti tuto de Fusión Nuclear, ETSII de Industriales,


Roobroeck, A. Materia Nova Research Center – Parc Initi alis | B

Rozanski, P. HUETTINGER Electronic Sp. z o.o. | PL

Rti mi, S. Ecole Polytechnique Fédérale de Lausanne,


Rudigier, H. OC Oerlikon Balzers | LI

Ruiz de Gopegui, U. IK4 – Tekniker, Surface Physics and Technology Unit | E

Sanchett e, F. Insti tut Charles Delaunay, Laboratoire des Systèmes

Mécaniques et d’Ingénierie Simultanée – UTT and LRC

CEA-ICD LASMIS, Nogent Internati onal Center for CVD

Innovati on (Nicci), UTT | F

Sang, R.-P. Science and Technology on Surface Engineering Laboratory,


Sanjines, R. Ecole Polytechnique Fédérale de Lausanne,

EPFL-SB-IPMC-LNNME | CH

Sarakinos, K. Plasma and Coati ngs Physics Division, IFM-Material Physics,


Schiff ers, C. CemeCon AG | D

Schmidt, S. Thin Film Physics Div., Department of Physics (IFM),


Schmidt-Mauer, M. Sulzer Metaplas | D

Schröder, B. Theoreti cal Electrical Engineering, Ruhr-University Bochum | D

Schulz-von der Gathen, V. Insti tute for Experimental physics II, Research Department

Plasma, Ruhr-Universität Bochum | D

Schuster, F. CEA Cross-Cutti ng program on Advanced Materials | F

Scullin, P. Impedans Ltd. | IRL

Shimizu, T. Division of Human Mechatronics Systems,

Tokyo Metropolitan University | J

Simon, Q. Université de Nantes, UMR CNRS 6502,


Snyders, R. Chimie des Interacti ons Plasma-Surface (ChIPS), CIRMAP,

Université de Mons an Materia Nova Research Center | B

Steyer, P. MATEIS, INSA-Lyon | F

Stranak, V. Insti tute of Physics, University of Greifswald | D

Sun, H. Key Lab. of Advanced Materials Technology, Ministry of


Tai, Y. Key Lab. of Advanced Materials Technology, Ministry of


Tejado, E. Dept. Ciencia Mat. CISDEM, ETSI de Caminos,


Teranishi, Y. Tokyo Metropolitan Industrial Technology Research Insti tute | J

Terenziani, G. Cern, Technology Department-Vacuum Surface and Coati ngs,

Surface Chemistry and Coati ngs group (TE-VSC/SCC) | CH

Tietema, R. Hauzer Techno Coati ng | NL

Tiron, V. Faculty of Physics, Alexandru Ioan Cuza University | RO

Treverrow, B. School of Physics A28, University of Sydney | AUS

Truijen I. Sirris, Smart Coati ng Applicati on Lab | B

Velicu, I.-L. Faculty of Physics, Alexandru Ioan Cuza University | RO

Vera, L. P. Insti tute of Microelectronics of Madrid | E

Vett er, J. Sulzer Metaplas | D

Vilnis, K. Insti tute of Solid State Physics, University of Latvia | LV

Vitelaru, C. Laboratoire de Physique des Gaz et Plasmas, CNRS

– Université Paris-Sud |F and

Nati onal Insti tute for Optoelectronics | RO

Vlcek, J. Department of Physics, University of West Bohemia | CZ

von Keudell, A. Research Department Plasmas with complex interacti ons,


Vyskočil, J. HVM Plasma Ltd. | CZ

Wang, D.-Y. Department of Materials Science and Engineering, Ming Dao

University and Surface Engineering Research Center,

MingDao University | TW

Watanabe, T. Tokyo Metropolitan Industrial Technology Research Insti tute | J

West, G. T. Surface Engineering Group, Manchester

Metropolitan University | UK

Will, A. Research Department Plasmas with complex interacti ons,


Winter, J. Research Department Plasmas with complex interacti ons


Department Plasma, Ruhr Universität Bochum | D

Wu, W.-Y. Department of Materials Science and Engineering,

Ming Dao University and Surface Engineering Research

Center, MingDao University | TW

Yang, M. Division of Human Mechatronics Systems,

Tokyo Metropolitan University | J

Yao, L. Key Lab. of Advanced Materials Technology, Ministry of


Yukimura, K. Nanoelectronics Research Insti tute, Nati onal Insti tute of

Advanced Industrial Science and Technology (AIST) | J

Zabeida, O. Department of Engineering Physics,


Zin, V. CNR-Insti tute for Energeti cs and Interphases | I

Zubkins, M. Insti tute of Solid State Physics, University of Latvia | LV

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