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7-th Symposium on Vacuum based Science and Technology
in conjunction with the
12-th Annual Meeting of the German Vacuum Society (DVG)
organized by
Institute of Technology
and Education
Koszalin University
of Technology
Clausius
Tower
Society
in cooperation with
BalticNet PlasmaTec Association Society of Vacuum Coaters
under the auspices of
Polish Vacuum Society PTP
German Vacuum Society DVG
November 19-21, 2013
Kołobrzeg, Poland
Marshal’s Office of the Westpomeranian Region
The publication was financially supported by the Westpomeranian Region
- 2 -
ISBN 978-83-7365-318-4
Chairman of Editorial Board
Mirosław Maliński
Editor
Roman Olik
Cover design
Justyna Horków
© Copyright by Wydawnictwo Uczelniane Politechniki Koszalińskiej
Koszalin 2013
Wydawnictwo Uczelniane Politechniki Koszalińskiej
75-620 Koszalin, ul. Racławicka 15-17
Koszalin 2013, 1st Edition, No. of quires: 4,53, B-5, No. of copies: 100
Printed by: INTRO-DRUK Koszalin
- 3 -
SYMPOSIUM CHAIRS
Chair
Witold Gulbiński, Koszalin University of Technology
Institute of Technology and Education
e-mail: [email protected]
phone: + 48 94 34 78 626
Co-Chair
Michael Kopnarski, Institute for Surface and Thin Film Analysis, Kaiserslautern
President of the German Vacuum Society (DVG)
e-mail: [email protected]
phone: +49 631 20573 3000
Co-Chair
Leszek Markowski, University of Wroclaw
President of the Polish Vacuum Society (PTP)
e-mail: [email protected]
phone: +48 71375 9307
- 4 -
SCIENTIFIC AND PROGRAM COMMITTEE
Prof. David Cameron, Lappeenranta University of Technology, FI
Prof. Elżbieta Czerwosz, Tele & Radio Research Institute, Warsaw, PL
Prof. Jürgen Fassbender, Helmholtz-Zentrum Dresden-Rossendorf, DE
Prof. Axel Groß, Ulm University, DE
Prof. Ulf Helmerson, Linköping University, SE
Prof. Rainer Hippler, Ernst Moritz Arndt University of Greifswald, DE
Prof. Michael Kopnarski, Institute for Surface and Thin Film Analysis, Kaiserslautern, DE
Prof. Leszek Markowski, University of Wroclaw, Wroclaw, PL
Prof. Jerzy Morgiel, Institute of Metallurgy and Materials Science, Kraków, PL
Prof. Witold Posadowski, Wrocław University of Technology, PL
Prof. Frank Richter, Chemnitz University of Technology, DE
Prof. Petr Spatenka, University of South Bohemia, Ceske Budejovice, CZ
Prof. Marian Szczerek, Institute for Sustainable Technologies, Radom, PL
Prof. Jacek Szuber, Silesian University of Technology, Gliwice, PL
Priv.-Doz. Sven Ulrich, Karlsruhe Institute of Technology, DE
Prof. Jan Walkowicz, Koszalin University of Technology, PL
Prof. Klaus-Dieter Weltmann, INP Greiswald, DE
Prof. Bogdan Wendler, Łódź University of Technology, PL
Prof. Jan Walkowicz, Koszalin University of Technology, PL
Prof. Klaus-Dieter Weltmann, INP Greiswald, DE
Prof. Bogdan Wendler, Łódź University of Technology, PL
LOCAL ORGANIZING COMMITTEE Koszalin University of Technology
Institute of Technology and Education
Prof. Andrzej Czyżniewski
Prof. Bogdan Warcholiński
Dr Roman Olik
Ms Karina Grześkowiak
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7-th Symposium on Vacuum based Science and Technology November 19-21, 2013, Koszalin - Kołobrzeg, Poland Preface
Dear Colleagues,
it is my exceptional pleasure to welcome you again in Kołobrzeg during the 7th
Symposium
on Vacuum based Science and Technology, organized by the Institute of Technology and
Education, the unit of the Koszalin University of Technology, under auspices of the Polish
Vacuum Society (PTP) and the German Vacuum Society (DVG) and held in conjunction with
the 12th Annual Meeting of the DVG. The Symposium organization is also supported by the
Clausius Tower Association and the Baltic-Net Plasma-Tec Association.
For the first time, the Symposium is organized in collaboration with the Society of Vacuum
Coaters (SVC).
Mission of the Symposium is to foster cooperation links within the European plasma science
community and to provide a forum for discussion of research results as well as exchange
of expertise in the field of vacuum and plasma based science.
This year, the Rudolf-Jaeckel Prize, awarded by the DVG for outstanding achievements in the
field of vacuum based sciences, will be presented to Dr Ute Bergner, the member of our
community.
The Clausius session, already traditionally organized during the Symposium is addressed this
year to young generation. We invited our young colleagues to attend a series of educational
lectures reporting on achievements in graphene science, scanning probe microscopy and
offering an adventure with the fascinating world of plasma.
During the Symposium, a special emphasis is placed on the following topics:
Plasma physics and techniques
Vacuum science, techniques and trends
Protective coatings and thin films
Characterization of surfaces and thin films
Thin films for solar cells and sensors
Plasma based surface treatment technologies
New trends and concepts of plasma based deposition processes
The meeting is accompanied by an industry exhibition attended by the representatives of
leading companies offering vacuum equipment, complete solutions for plasma based
technologies as well as advanced research equipment.
This Book of Abstracts will guide you through the Symposium topics and sessions. You are
welcome to attend invited lectures, oral presentations and the poster session.
I wish you fruitful discussions and good time spent in Kołobrzeg where I hope to meet you
again.
Witold Gulbiński
Symposium Chairman
- 6 -
List of Exhibitors 7-th Symposium on Vacuum based Science and Technology
November 19-21, 2013, Koszalin - Kołobrzeg, Poland
Zakład Techniki Próżniowej TEPRO SA
www.tepro.com.pl
Kurt J. Lesker Company
www.lesker.com
VAT Vacuum Valves
www.vatvalve.com
VAK-POL & GAZ
www.vakpol.com
Scientific Instrument and Equipment Design,
Development and Manufacturing from Hiden
Analytical
www.hidenanalytical.com
ITL
www.instech.co.uk
Edwards Ltd
www.edwardsvacuum.com
- 7 -
UniExport
www.uni-export.com.pl
7-th Symposium on Vacuum based Science and Technology November 19-21, 2013, Koszalin - Kołobrzeg, Poland Contents
Invited Speakers
INV1 C. Mitterer Interface and stress design of hard coatings
INV2 U. Janson Magnetron sputtering of Me-B-C films
INV3 G. Abadias, A. Fillon, J. J. Colin, A. Michel, C. Jaouen
Real-time stress evolution during sputter-deposition of metal films: influence of adatom mobility
INV4 M. Fenker, M. Balzer, H. Kappl Challenges and progress in the corrosion protection of steel with hard coatings
INV5 K.-D. Weltmann, Th. von Woedtke, R. Bussiahn Recent Development of Atmospheric Plasma Sources for Life Science
INV6 S. Zhou Ion beam synthesis of ferromagnetic semiconductors
INV7 H. Kersten, S. Bornholdt, J. Rutscher, T. Trottenberg, V. Schneider Diagnostics of particle fluxes and sputter effects by non-conventional methods
INV8 K. Zdunek, K. Nowakowska-Langier, R. Chodun, S. Okrasa Pulsed plasma processes for surface engineering
DVG1 - Honorific speech: Ton van de Kerkhof
Contamination Risk and Contamination Control Strategy DVG2 - Lecture of the laureate DVG Rudolf Jaeckel Award: Ute Bergner
Innovation into Emptiness
- 8 -
Contents 7-th Symposium on Vacuum based Science and Technology
November 19-21, 2013, Koszalin - Kołobrzeg, Poland
Oral presentations O1 Z. Stryhal, A. Bergmann, A. Sendzik, S. Berg, F. Richter
Fluorinated amorphous carbon coatings for polymer-on-polymer tribological applications
O2 K. Jousten
Recent steps toward traceability for partial pressure measurements
O3 M. Wahl, J. Lösch, S. Gutsch, H. Gnaser, W. Bock, M. Zacharias, M. Kopnarski P-doped Si nanocrystals in silicon for tandem solar cells characterized by 3d atom probe tomography
O4 K. Marszałek, P. Winkowski, J. Jaglarz, M. Perzanowski, M. Marszałek Studies of structure and antireflective properties of LaF3/HfO2/SiO2 and LaF3/HfO2/MgF2 trilayers for UV applications
O5 A. Kamińska, M. Kozłowski, P. Dłużewski, E. Czerwosz
C-Pd films obtaining by PVD method and influence of annealing time on their structure and sensing properties
O6 A. Clausner, F. Richter New results on mechanical characterisation of thin films
O7 Ł. Szparaga, J. Ratajski, R. Olik
On polyoptimization of gradient coatings
O8 F. Bernsmann, H. Busch, M. Castellucci
Diffusion-tight multilayer coatings for the encapsulation of implants O9 A. Kruth, S. Müller, S. Peglow, S. Hansen, T. Beweries, N. Rockstroh, H. Junge,
M.-M. Pohl, V. Brüser, K-D. Weltmann Plasma-enhanced synthesis of visible light-active photocatalyst nanostructures for water splitting and other solar applications
O10 U. Helmersson, I. Pilch, D. Söderström, R. Gunnarsson, N. Brenning
A high power pulsed plasma process for nanoparticle synthesis O11 G. Greczynski, J. Lu, J. Jensen, I. Petrov, J.E. Greene, W. Kölker, S. Bolz,
Ch. Schiffers, O. Lemmer, L. Hultman Controlled growth of transition metal nitride films via selection of metal ion irradiation during hybrid HIPIMS/magnetron co-sputtering
O12 T. Leyendecker, O. Lemmer, W. Kölker, Ch. Schiffers
Advances in Process Technology and Deposition Equipment for HiPIMS Coatings for Cutting Tools
O13 K. Jousten
- 9 -
New standard to test the dynamics of vacuum gauges in the ms range
7-th Symposium on Vacuum based Science and Technology November 19-21, 2013, Koszalin - Kołobrzeg, Poland Contents
O14 S. Rosendahl, E. Brown, I. Cristescu, A. Fieguth, Ch. Huhmann, M. Murra,
Ch. Weinheimer A cryogenic distillation column for the XENON1T experiment
O15 G. Baldsiefen, N.Laube Flexible DLC Coatings to prevent Crystalline Biofilm formation on Urinary Tract Implants
O16 J. Koprowska, E. Dobruchowska, K. Reszka
Polypropylene nonwoven shields against electromagnetic fields obtained by plasma deposition of CuSn alloy
O17 A. Gilewicz, B. Warcholiński
The surface assessment and the properties of selected multilayer coatings
Poster Session P1 J. Baranowska, S. Fryska
The influence of deposition parameters on s phase coatings obtained by reactive magnetron sputtering
P2 D. Caffrey, K. Fleischer and I.V. Shvets Deposition and characterisation of magnesium doped Cr2O3 grown via magnetron sputtering
P3 F. Danneil, M. Stüber, S. Ulrich, K. Seemann, H. Leiste, A. Welle Control of wettability of amorphous carbon based coatings by adjustment of surface chemistry and surface topography
P4 E. Dobruchowska, J. Koprowska, K. Reszka Preparation and characterization of EMI nonwoven shields obtained by plasma deposition of CuSn alloy
P5 S. Gogler, B. Budner, J. Mierczyk, M. Szymanska, M. Kalisz
Characterisation of anti-reflective diamond-like carbon coatings for infrared aplications P6 E. Kowalska, A. Kamińska, E. Czerwosz, M. Kozłowski, K. Sobczak, B. Witkowski
Influence of CVD duration process on morphology, structure, and sensing properties of carbonaceous-palladium thin films
P7 S. Krawczyk, A. Kamińska , M. Kozłowski, J. Radomska, P. Dłużewski, E. Czerwosz
Nanocomposite carbonaceous-palladium thin films for ammonia sensing P8 K. Labisz, T. Tański, M. Bilewicz
PVD surface treatment of heat treated cast aluminium alloys P9 K. Marszałek, W. Doros
Sputtering line for the photovoltaic coating deposition
- 10 -
Contents 7-th Symposium on Vacuum based Science and Technology
November 19-21, 2013, Koszalin - Kołobrzeg, Poland
P10 P. Myśliński
Dilatometric method of thermomechanical effects detection of substrate – PVD coating systems
P11 S. Passlack, B. Suksut, J. Meyer, A. Brodyanski, B. Reuscher, L. Lin,
G. Niedner-Schatteburg, A. Schlarb, M. Kopnarski Magnetron sputtered metallic nanoparticles for reinforcement of polymer materials
P12 S. Peglow, A. Kruth, V. Brüser
Nanostructured gold/titanium dioxide catalysts for light-driven water splitting P13 M. Rinke, M. Stüber, C. Ziebert, M. Lattemann, S. Ulrich
Constitution, microstructure and mechanical properties of magnetron-sputtered TiC/a-C nanocomposite coatings
P14 S. Rosendahl and the KATRIN collaboration
Venting of the KATRIN Main Spectrometer with Ultra-clean Argon keeping the activation of the non-evaporable Getters
P15 M. Strafela, J. Fischer, M. Rinke, T. Bergfeldt, H.J. Seifert, S. Ulrich Constitution and microstructure of magnetron sputtered Li-Ni-Mn-Co-O thin film cathodes for lithium-ion batteries as a function of working gas pressure
P16 T. Suszko, V. Jahodowa, W. Gulbiński Plasma optical emission spectroscopy (OES) as a monitoring tool for deposition of expanded austenite (s phase) layers by magnetron sputtering
P17 A. Śliwa, J. Mikuła. W. Kwaśny, T.Tański, K. Golombek
FEM modelling of internal stresses in PVD coated tool composites
P18 Ł. Tomaszewski, A. Urbanowicz, W.K. Gulbiński, T. Suszko, A. Lewandowski, W. Gulbiński TiAlN based wear resistant coatings modified by molybdenum co-deposition
P19 B.G. Wendler, I.F. Progalskiy, T. Moskalewicz, W. Pawlak, A. Rylski, P. Nolbrzak,
K. Włodarczyk, M. Makówka XRD, TEM and HRTEM investigations of nanostructured superhard TiN/Si3N4 coatings deposited by means of a novel gas pulsed reactive magnetron sputtering
P20 V. Zavaleyev, J. Walkowicz
Investigation of the properties of thin amorphous ta-C coatings deposited by combined DC impulse vacuum-arc method using the linear Venetian blind plasma filter
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7-th Symposium on Vacuum based Science and Technology November 19-21, 2013, Koszalin - Kołobrzeg, Poland INV 1
INTERFACE AND STRESS DESIGN OF HARD COATINGS
Christian Mitterer
Department of Physical Metallurgy and Materials Testing, Montanuniversität Leoben,
Franz-Josef-Strasse 18, A-8700 Leoben, Austria
e-mail: [email protected]
Hard coatings deposited by plasma-assisted vapor deposition are widely used to
reduce friction and wear of tools and engineering components. During application,
mechanical and thermal loads vary over a wide range and might place extreme
demands on coating systems, requiring their application-based tailoring. Advanced
hard coatings are characterized by multi-functional properties like age-hardening by
spinodal decomposition of metastable phases and self-lubrication. In addition to these
properties, retardation of cracks for increased toughness and even thermal
management abilities to reduce local flash temperatures are required. This multi-
functionality requires a multi-phase coating design, with layers fulfilling different
tasks and well defined interfaces and stresses. Within this talk a survey of
achievements in advanced hard coatings is given, covering fracture toughness
measurements by bending of free-standing coating cantilevers and the possible
reduction of local tribological flash temperatures by embedded phase-change
materials. Finally, an approach based on modeling and experimental methods for
formation of interfaces in dual-phase coatings is presented, which could be the basis
for a knowledge based interface design of coating systems.
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INV 2 7-th Symposium on Vacuum based Science and Technology
November 19-21, 2013, Koszalin - Kołobrzeg, Poland
MAGNETRON SPUTTERING OF Me-B-C FILMS
Ulf Jansson
Department of Chemistry – Angstrom Laboratory, Uppsala University
Box 538, SE-75121 Uppsala, Sweden
Me-B-C thin films (Me = early transition metal) have interesting mechanical and
tribological properties. Only one ternary phase, Mo2BC, is known and predicted to
exhibit a unique combination of stiffness and ductility. The thermodynamically most
stable phase combination in all other Me-B-C systems is a mixture of binary phases.
During magnetron sputtering at lower temperatures, the high quenching rate combined
with low diffusion rates make it difficult to form these crystalline binary phases and
amorphous growth is therefore frequently observed. A general overview of this
behaviour will be discussed for different early transition metals and some trends will
demonstrated based on the structure of the crystalline binary phases. Furthermore, a
general overview of structure and properties of Me-B-C films with Me= Ti, Cr, Nb
and Mo will be presented and differences in chemical bonding will be discussed based
on e.g. x-ray photoelectron spectroscopy (XPS) and X-ray diffraction (XRD) . In
particular, the importance of chemical composition on hardness and tribological
properties will be discussed.
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7-th Symposium on Vacuum based Science and Technology November 19-21, 2013, Koszalin - Kołobrzeg, Poland INV 3
REAL-TIME STRESS EVOLUTION DURING SPUTTER-
DEPOSITION OF METAL FILMS: INFLUENCE OF ADATOM
MOBILITY
G. Abadias, A. Fillon, J. J. Colin, A. Michel, C. Jaouen
Institut P’, Département Physique et Mécanique des Matériaux, Université de
Poitiers-CNRS-ENSMA, SP2MI, Téléport 2, F86962 Chasseneuil-Futuroscope cedex
Corresponding author: [email protected]
The understanding of the physical origins of stress development during growth of
polycrystalline thin films has been the subject of intense investigations. Significant
progress has been made in the last decade thanks to the potentiality offered by in situ,
real-time stress measurement during deposition, enabling one to probe the growth
dynamics with sub-monolayer sensitivity.
We present here an overview of the typical stress evolutions during the early growth
stages of a large class of sputter-deposited metal (Me) films, using a real-time multi-
beam optical stress sensor (MOSS). For high-mobility fcc (Ag, Au, Pd) metals, a
typical compressive-tensile-compressive (CTC) behavior is observed, characteristic of
a Volmer-Weber growth mode. A correlation between the homologous temperature
(Ts/Tm), tensile stress peak position, grain size and steady-state compressive stress in
the post-coalescence stage is presented.
For low-mobility bcc (Mo, W, Ta) metals (Ts/Tm 0.10) deposited on a-Si, kinetic
limitations result in a 2D growth mode highly influenced by interfacial effects. The
film force is initially dominated by change in surface stress, which scales with the
surface energy difference = Me a-Si. For both Mo and W, a stress transient is
observed in the 2-4 nm range, followed by the development of unexpectedly large
tensile stress, ascribed to a phase transition towards their equilibrium -Mo and -W
structure. Such transient is not evidenced during Ta growth for which a compressive
stress regime is steadily established and related to the growth of its metastable -Ta
structure. For all low-mobility metals, the final stress regime is controlled by the
energetics of the incoming species and intrinsic mechanical properties of the material.
- 14 -
INV 4 7-th Symposium on Vacuum based Science and Technology
November 19-21, 2013, Koszalin - Kołobrzeg, Poland
ION BEAM SYNTHESIS OF FERROMAGNETIC
SEMICONDUCTORS
Shengqiang Zhou
Helmholtz - Zentrum Dresden - Rossendorf,
Institute of Ion Beam Physics and Materials Research, Bautzner Landstr. 400, 01328
Dresden, Germany
Corresponding author: [email protected]
are under intensive investigation in last decade. Until now, III-Mn-V based compound
semiconductors are the only well accepted family. The prototype ferromagnetic
semiconductor GaMnAs has revealed a variety of unique features induced by the
combination of its magnetic and semiconducting properties. To prepare ferromagnetic
semiconductors, one needs to dope the host with up to 5-10% Mn, which is far beyond
the solid solubility of Mn in III-V compounds. As a non-equilibrium process, ion
implantation can introduce enough dopants as required. However, the activation of
dopants remains challenging due to the clustering of implanted ions during post-
annealing. The solubility limit is a fundamental barrier for dopants incorporated into a
specific semiconductor. On the other hand, one notes that the solubility limit in the
liquid phase is generally much larger than that in the solid phase. Short-time annealing
in the millisecond or nanosecond regime allows the epitaxial growth from a liquid
phase. The mature development and commercialization of ion implantation promise
the versatility. The approach combining ion implantation and pulsed laser melting
allows us to prepare ferromagnetic semiconductors covering the full spectrum of III-V
compound semiconductors. We have successfully synthesized ferromagnetic Mn
doped III-V from InAs to GaP with different bandgaps. The results of magnetization,
magnetic anisotropy, resistivity, anomalous Hall effect, magnetoresistance and x-ray
magnetic circular dichroism obtained from the synthesized samples confirm the
intrinsic origin and the carrier-mediated nature of the ferromagnetism. These results
could allow a panorama-like understanding of III-V:Mn based ferromagnetic
semiconductors.
- 15 -
7-th Symposium on Vacuum based Science and Technology November 19-21, 2013, Koszalin - Kołobrzeg, Poland INV 5
CHALLENGES AND PROGRESS IN THE CORROSION
PROTECTION OF STEEL WITH HARD COATINGS
Martin Fenker1, Martin Balzer
1, Herbert Kappl
1
1fem Forschungsinstitut Edelmetalle und Metallchemie,
Katharinenstr. 17, 73525 Schwäbisch Gmünd, Germany
Corresponding author: [email protected]
The high corrosion resistance of hard coatings used for decorative and / or wear
protection applications is well known. However, when deposited on less noble
materials like steel, the coated parts suffer from severe corrosive attack due to inherent
coating defects or inhomogeneities (cracks, pores, transient grain boundaries). They
open possible paths for the corrosive media to reach the substrate. In the case of a less
noble substrate material galvanic corrosion at the substrate will occur. A lot of
research has been undertaken to get rid of this problem. There are several ways to
improve the corrosion resistance of coated parts: thicker coatings, dense coatings (fine
grained or amorphous), elimination of droplets, multilayers, duplex coatings,
intermediate etching, alloying of the hard coating with less noble elements.
In this work the challenges and the progress in the corrosion protection with hard
nitride coatings on steel in NaCl-containing media will be presented. The corrosion
studies have been performed with polarisation tests, open-circuit potential
measurements and neutral salt spray tests. More detailed characterisations before and
after the corrosion tests have been employed by confocal microscopy and scanning
electron microscopy (SEM). Additionally, for an in depth understanding of the
corrosion mechanism cuts and step-by-step removal of surface coating material has
been utilised with the focused ion beam (FIB) technique.
The investigations comprise single layered nitride coatings, multilayered coatings,
DLC coatings, intermediate etching of nitride coatings and the alloying of NbN
coatings with oxygen and of TiN coatings with Mg. Finally the benefit of duplex
treatments (PVD + ALD) on the corrosion behaviour will be demonstrated.
- 16 -
INV 6 7-th Symposium on Vacuum based Science and Technology
November 19-21, 2013, Koszalin - Kołobrzeg, Poland
RECENT DEVELOPMENT OF ATMOSPHERIC PLASMA
SOURCES FOR LIFE SCIENCE
Weltmann, Klaus-Dieter,1 von Woedtke, Thomas
1, Bussiahn, René
1
1INP Greifswald, Felix-HAusdorffstrasse 2, 17489 Greifswald
Plasma Medicine is currently emerging worldwide as a new independent field of
scientific research, that can be subdivided into three main components: plasma surface
modification,
plasma bio-decontamination, and – as the central field – therapeutic plasma
application.
The use of physical plasmas for bio-decontamination or sterilization, just as first
surgical plasma applications such as argon-plasma coagulation or coblation are mainly
based on lethal plasma effects on living systems. However, there is an additional huge
potential of low temperature plasma application for therapeutic fields, which will be
based on selective, at least partially non-lethal, possibly stimulating plasma effects on
living cells and tissue.
The scientific basis of plasma medicine is a fundamental knowledge of the
mechanisms of plasma interaction with living cells and tissue. In the areas of plasma
surface modification and plasma bio-decontamination, plasma is used to treat surfaces
and products to improve their bio-applicability or bio-performance to use it for
therapeutic purposes.
Whereas in these fields, both low-pressure and atmospheric pressure plasmas can be
used, for direct therapeutic plasma applications preferably atmospheric pressure
plasma sources can be used. Especially from the point of practical manageability,
atmospheric pressure plasma jets (APPJ) and dielectric barrier discharges (DBD) are
of special interest for medical applications. The contracted and comparably cold
plasmas allow focused small-spot treatments, even of small size objects, as well as
large-scale treatments.
An overview about the ongoing research on low-temperature atmospheric pressure
plasma sources designed for biomedical applications will be given. Plasma Medicine
as an independent field is growing worldwide - comparable to the development of
laser technology decades ago.
- 17 -
7-th Symposium on Vacuum based Science and Technology November 19-21, 2013, Koszalin - Kołobrzeg, Poland INV 7
DIAGNOSTICS OF PARTICLE FLUXES AND SPUTTER
EFFECTS BY NON-CONVENTIONAL METHODS
H. Kersten, S. Bornholdt, J. Rutscher, T. Trottenberg, V. Schneider
Institute for Experimental and Applied Physics, University of Kiel,
Leibnizstrasse 19, D-24098 Kiel, Germany
Corresponding author: [email protected]
For an optimization of plasma-based thin film deposition suitable diagnostics are
required. In addition to well-established plasma diagnostic methods (e.g. emission
spectroscopy, mass spectrometry, Langmuir probes etc.) we perform selected
examples of “non-conventional” and low-cost diagnostics which are applicable in
technological plasma processes. Examples are i) the determination of energy fluxes by
calorimetric probes [1-3], ii) the measurement of momentum transfer due to sputtered
particles by SPIN [4].
i) The total energy influx from plasma to substrates can be measured by special
calorimetric sensors (thermal probes) based on the determination of the temporal slope
of the substrate surface temperature in the course of the plasma process. By
comparison with model assumptions on the involved plasma-surface mechanisms the
different energetic contributions to the total energy influx can be separated. The
method will be demonstrated for magnetron sputtering and ion beam source operation.
ii) For a variety of thin film applications (e.g. sputtering) it is essential to determine
the sputtering yield as well as the angular distribution of sputtered atoms. Therefore,
in addition to model calculations (TRIM, TRIDYN etc.) an experimental
determination of the related quantities is highly demanded. For this purpose we
propose a novel and rather simple method, the so-called sputtering-propelled
instrument (SPIN). The SPIN, which is stack nearly without friction and exposed to a
vertical ion beam, starts to rotate due to momentum transfer by the released particles,
i.e. sputtered target atoms and recoiled ions.
[1] Kersten,H., Deutsch,H. Steffen,H., Kroesen,G.M.W., Hippler,R., Vacuum
63(2001), 385.
[2] Bornholdt,S., Itagaki,N., Kuwahara,K., Wulff,H., Shiratani,M., Kersten,H.,
Plasma Sourc. Sci. Technol. 22(2013), 025019.
[3] Bornholdt,S., Kersten,H., Eur. Phys. J. D 67(2013), 176.
[4] Rutscher,J., Trottenberg,T., Kersten,H., Nucl. Instrum. Meth. Phys. Res. B
30(2013), 47.
- 18 -
INV 8 7-th Symposium on Vacuum based Science and Technology
November 19-21, 2013, Koszalin - Kołobrzeg, Poland
IMPULSE PLASMA PROCESSES FOR SURFACE
ENGINEERING
Krzysztof Zdunek1,2)
, Katarzyna Nowakowska-Langier2)
, Rafal Chodun1)
, Sebastian
Okrasa1)
1) Warsaw University of Technology, Warsaw, Poland 2) National Centre for Nuclear Research, Otwock-Swierk, Poland
It is obvious that the surface engineering is a one of the most important tool for
today’s technological progress. The possibilities of using the specially prepared vapor
phase of deposited materials enables to produce coatings with awaiting properties that
are different form core material properties. In this way one can obtain a specific
composite fulfilled required useful feature of the whole product. Also the surface
engineering has become the only method for producing a simple or complicated
construction of semiconductor devices.
Implementation of plasma instead of neutral vapor during coatings deposition
changes dramatically the mechanism of both: gas phase distribution and product phase
nucleation. First of all it makes possible to use the electric field for acceleration the
vapor particles. The kinetic aspect of plasma implementation is resulted in changes in
coatings morphology. These changes could be clearly expressed by comparison of
very well-known structures models of coatings (eg. Movchan-Demchishin vs
Thornton models).
It seems however that the probably most important aspect of using the plasma
in surface engineering is the dependence of electric energy not only on morphology of
coatings but also on the phase composition of the product material (es. synthetized and
deposited by the use of the plasma surface engineering methods).
Our own experiments proved that by the use of plasma, especially the non-
thermal impulse plasma is very useful for producing and depositing the phase with
high nucleation barrier and nanocrystalline structure. Elaborated by us in the end of
80’s last century the Impulse Plasma Deposition method (known in the literature as
the IPD) was used not only for producing the DLC coatings but also for deposition the
other high melting interstitial phases as well as alloy metallic coatings. The coatings
of non-equilibrium materials are characterized by the globular nanocrystalline or
amorphous-nanocrystalline and good adhesion for cold substrates (non-heated form
any external heat source).
Recently we have introduced a new, very promising way to control the plasma
generation process caused by injecting of the working gas into the plasma source.
Such a way was implemented with success both in the case of the IPD and the case of
very well know magnetron sputtering (the last one was called by us as a Gas Injection
Magnetron Sputtering – GIMS). TiN coatings deposited in this manner showed
particularly good antiwear properties.
- 19 -
DVG1
7-th Symposium on Vacuum based Science and Technology
November 19-21, 2013, Koszalin - Kołobrzeg, Poland Honorific speech:
DVG Rudolf Jaeckel Award
CONTAMINATION RISK AND
CONTAMINATION CONTROL STRATEGY
Ton van de Kerkhof
ASML Netherlands B.V. Veldhoven (NL)
Corresponding author: [email protected]
The ASML EUV lithography application is very sensitive for hydrocarbons and
metals used in daily life and in production processes. In the first part of the talk the
risk of hydrocarbon and metal contamination will be presented. HV and UHV is a part
of contamination control strategy as well as definition of cleanliness standards.
Experience with the described contamination control strategy as well as cleanliness
grades and experiences at suppliers will be presented.
Ton van de Kerkhof achieved his expertise in vacuum technology and semiconductor
manufacturing during his work with Philips Semiconductors since 1984, e. g. as
Chairman of Vacuforce. In 2006 he started his work as supply chain engineer for
vacuum technology with ASML and is responsible for the qualification of NXE
products at selected suppliers. In addition Ton van de Kerkhof is Chairman of the
Product Family Team: Environmental control and infrastructure components.
- 20 -
DVG2
7-th Symposium on Vacuum based Science and Technology
November 19-21, 2013, Koszalin - Kołobrzeg, Poland Lecture of the laureate:
DVG Rudolf Jaeckel Award
INNOVATION INTO EMPTINESS
Ute Bergner
VACOM Vakuum Komponenten & Messtechnik GmbH, Gabelsbergerstr. 9,
07749 Jena (DE)
Besides a great idea itself, the transfer of the idea into a beneficial use for mankind is
a premise in order to make it a true innovation. In the past, brilliant minds spent years
or even centuries to discover the secrets of emptiness. The interesting thing is that
revolutionary physical theories were close related to the penetration of the mist by
lowering the gas density. A well-known example is the Maxwell theory of kinetic gas.
Modern high tech processes require not only an extreme low gas density but even
ultraclean vacuum conditions. The question one could raise is: When will we speak of
nanoparticles instead of large gas molecules and how can we describe the processes
involved? Cleanliness and purity need a clear definition to pave the way from the
existing knowledge into further innovation.
Moreover – measuring purity and emptiness is a huge challenge at present. The
complexity of gas species and the unmet requirement for comparability reveal the
actual limits in their determination. In analogy to quantum mechanics the sensor itself
may affect the measurement at very low pressures as XHV which induce new
challenges to the scientific vacuum community.
We investigated theoretically and experimentally the XHV. In its resultant, well-
known effects as the negative X-ray effect in Bayard Alpert gauges or the ignition
characteristics of cold cathodes at low pressures, led to a simple Bayard-Alpert gauge
that measures down to XHV and a cold cathode gauge that ignites within seconds at
these low pressures.
As always in science: During our investigations new questions have arisen and the old
ones were not fully answered. Yet, we strongly believe that answering these questions
will open a new innovative era in vacuum science.
- 21 -
7-th Symposium on Vacuum based Science and Technology November 19-21, 2013, Koszalin - Kołobrzeg, Poland O 1
FLUORINATED AMORPHOUS CARBON COATINGS FOR
POLYMER-ON-POLYMER TRIBOLOGICAL APPLICATIONS
Z. Stryhal1, A. Bergmann
2, A. Sendzik
1, S. Berg
1 and F. Richter
1
1TU Chemnitz, Institut für Physik, 09107 Chemnitz, Germany
2TU Chemnitz, Fakultät Maschinenbau, 09107 Chemnitz, Germany
Corresponding author: [email protected]
Fluorinated amorphous carbon (a-C:F) thin film was used as low-friction and low-
wear coating of polymer material (PBT - Polybutylene terephthalate) that is often used
in conveyor technology. a-C:F coatings were deposited by magnetron sputtering in Ar
+ CF4 gas mixture. The amount of fluorine incorporated into amorphous carbon was
controlled by the ratio of CF4 in the gas mixture. Composition of coatings was
determined by EDX and ERDA methods. Friction properties of coated polymer
samples were tested using a self-made tribo-tester with reciprocating plate-on-plate
arrangement. The surface energy of the films was determined from contact angle of
special liquids. Well adherent wear resistant coatings with up to 40 at.% of fluorine
were deposited. All coatings showed no perceptible wear after friction experiment. No
significant tendency in final friction coefficient after 24 hours for various a-C:F
coatings was found. The coefficient of friction during early hours of the test showed
that the more fluorine in the coating the lower the coefficient of friction is.
- 22 -
O 2 7-th Symposium on Vacuum based Science and Technology
November 19-21, 2013, Koszalin - Kołobrzeg, Poland
RECENT STEPS TOWARD TRACEABILITY FOR PARTIAL
PRESSURE MEASUREMENTS
Karl Jousten
PTB, Berlin
Partial pressure measurement in vacuum by quadrupole mass spectrometer (QMS) is
an important tool to control and monitor processes in industry. It is, however, difficult
to obtain reliable results with quadrupole mass spectrometers, since its calibration is
ill-defined and at present there is no traceability to any national primary standard.
The European project EMRP IND12 has taken steps to provide traceability for both
QMS calibrations. It also a goal of the project to prepare Technical Specifications for
the calibration of QMS. This is done in cooperation with ISO TC 112, the committee
for international standardization in vacuum.
Recently, the TC 112 published the standard ISO 14291 "Definitions and
specifications of quadrupole mass spectrometers" as a first step towards calibrations of
QMS. The European project EMRP IND12 is now performing extensive
investigations on the characterization of QMS including their long-term instability in
preparation of the next step, the definition of a helpful calibration procedure of QMS
and to trace their values to the SI with reasonable accuracy. This also will be a
prerequisite for traceability of outgassing rate measurements.
The talk will focus on the work performed within EMRP IND12, the calibration
standards that have been built, the investigations that are underway and planned, and
the perspectives from there.
Support through the EMRP IND12 project is gratefully acknowledged. The EMRP is
jointly funded by the EMRP participating countries within EURAMET and the
European Union.
- 23 -
7-th Symposium on Vacuum based Science and Technology November 19-21, 2013, Koszalin - Kołobrzeg, Poland O 3
P-DOPED Si NANOCRYSTALS IN SILICON FOR TANDEM
SOLAR CELLS
CHARACTERIZED BY 3D ATOM PROBE TOMOGRAPHY
M. Wahl1, J. Lösch
1, S. Gutsch
2, H. Gnaser
1, W. Bock
1, M. Zacharias
2,
M. Kopnarski 1
1)
Institut für Oberflächen- und Schichtanalytik IFOS, Kaiserslautern 2)
Labor für Nanotechnologie am IMTEK an der Universität Freiburg
Due to shifting the bandgap of Si nanocrystals (SiNC) embedded in an oxide matrix
up to 1.8 eV by varying the size and density of the crystals, this system becomes an
ideal candidate for tandem solar cells based on Si technology.
The SiNC’s we investigate here are generated by the annealing of a SiOx/SiO2
multilayer system which is deposited by PECVD. Phase separation which occurs
during the heating process results in forming the SiNC´s. Electrical properties required
for operation as a solar cell can be achieved by doping the multilayer system with
phosphorus.
The determination of the actual dopant concentration and localization in such SiNC`s
with a size of only a few nm is a very challenging task. We use a CAMECA LEAP
HR 4000X system with its near-atomic resolution to investigate in a 3D volume the
chemical composition and the distribution of size and density of the SiNC’s.
We find that the distribution of the SiNC diameter has a mean value of about 4 nm.
The P concentration is enhanced inside the NCs. Looking at the radial concentration
profile we particularly recognise the boundary between NC and the silicon oxide
matrix as the preferred position for the dopant atoms. In addition the APT data denote
the crystalline nature of the Si nanoparticles.
- 24 -
O 4 7-th Symposium on Vacuum based Science and Technology
November 19-21, 2013, Koszalin - Kołobrzeg, Poland
STUDIES OF STRUCTURE AND ANTIREFLECTIVE
PROPERTIES OF LaF3/HfO2/SiO2 AND LaF3/HfO2/MgF2
TRILAYERS FOR UV APPLICATIONS
K.Marszałek
1, P.Winkowski
2, J.Jaglarz
3, M.Perzanowski
4, M.Marszałek
4
1AGH - University of Science and Technology, 30-059 Krakow, Mickiewicza 30, Poland
2PEVIN, Piaskowa 55, 31-341 Krakow, Poland
3TU, Warszawska 55, Krakow, Poland
4The H. Niewodniczański Institute of Nuclear Physics, 31-342 Krakow, Radzikowskiego 152,
Poland
The aim of this paper is to study antireflective properties of trilayer systems
LaF3/HfO2/SiO2 and LaF3/HfO2/MgF2 deposited on heated optical glass substrates.
The films were evaporated in mixed techniques. Oxide films were prepared by means
of e-gun evaporation, fluoride films by means of thermal source evaporation.
Simulation of reflectance was performed for 1M2H1L (Quarter Wavelength Optical
Thickness) film stack on optical quartz glass with refractive index n= 1,46. The layer
thickness was optimized to achieve the lowest light scattering from glass surface
covered with dioxide and fluoride films. The values of layer thicknesses and interface
roughness were determined through X-ray reflectometry measurements. The essence
of performed calculation was to find minimum reflectance of light in wide ultraviolet
region. The spectral dispersion of the refractive index needed for calculations was
determined from ellipsometric measurements using the spectroscopic ellipsometer
M2000. Additionally, the total reflectance measurements in integrating sphere coupled
with Perkin Elmer 900 spectrophotometer were performed. These investigations
allowed to define the influence of such film features like surface and interface
roughness on light scattering.
Key words: thin film deposition, antireflective coatings, LaF3/HfO2/SiO2, LaF3/HfO2/MgF2,
optical measurements
The authors acknowledge financial support from the project POIG01.03.01-30-056/12.
- 25 -
7-th Symposium on Vacuum based Science and Technology November 19-21, 2013, Koszalin - Kołobrzeg, Poland O 5
C-Pd FILMS OBTAINING BY PVD METHOD AND INFLUENCE
OF ANNEALING TIME ON THEIR STRUCTURE AND SENSING
PROPERTIES
Anna Kamińska
1, Mirosław Kozłowski
1, Piotr Dłużewski
2, Elżbieta Czerwosz
1,*
1Tele and Radio Research Institute, Ratuszowa 11, 03-450 Warsaw, Poland
2Institiute of Physics, Polish Academy of Science, Al. Lotników 32/46,02-668 Warsaw, Poland
*Corresponding author: e-mail: [email protected]
The form and structure of thin palladium film composed of nanograins of palladium
and carbon (C-Pd film) have crucial role in sensing properties of these films on many
gases (hydrogen, ammonia, methane, LPG gases). It was shown in our previous papers
[1,2] that preparation method strongly influence on properties of the film and then on
its sensing properties . In the presentation we want to show the method of obtaining of
such film and discuss their properties as a function of technological process.
C-Pd films were obtained by Physical Vapor Deposition (PVD) method or by
annealing of these initial PVD films at temperature 650°C at different time (5, 10 and
30 min) in xylene flow. These C-Pd films were characterized by Scanning Electron
Microscopy (SEM), Transmission Electron Microscopy (TEM) and FTIR
spectroscopy. The sensing properties of films were studied in specially prepared
chamber allowing for measurements of the changes of resistivity as a function of gas
composition changes. It was found that annealing change films’ morphology,
topography and structure, and then change their sensing properties.
ACKNOWLEDGMENT
This project is co-financed by the European Regional Development Fund within the
Innovative Economy Operational Programme 2007-2013 (title of the project “Development of
technology for a new generation of the hydrogen and hydrogen compounds sensor for
applications in above-normative conditions”) No UDA-POIG.01.03.01-14-071/08-08.
1. E.Kowalska, E.Czerwosz, A.Kamińska, M.Kozłowski, Investigation of Pd content in C-
Pd films for hydrogen sensor applications, J. Therm. Anal. Calorim. 108 (2012) pp.
1017-1023
2. K.Sobczak, P.Dłużewski, M.T.Klepka, B.Kurowska, E.Czerwosz, Transmission
electron microscopy studies of the Pd-C films obtained by physical and chemical
vapor deposition, International Journal of Hydrogen Energy 37 (2012) pp.18556-
185623
- 26 -
O 6 7-th Symposium on Vacuum based Science and Technology
November 19-21, 2013, Koszalin - Kołobrzeg, Poland
NEW RESULTS ON MECHANICAL CHARACTERISATION
OF THIN FILMS
André Clausner1 and Frank Richter
2
1Fraunhofer IZFP-D, Maria-Reiche-Straße 2, 01109 Dresden, Germany
2TU Chemnitz, Institut für Physik, 09107 Chemnitz, Germany
Corresponding author: [email protected]
Critical load during scratch test as well as indentation hardness are frequently used to
characterise the mechanical behaviour of solid materials. These parameters, however,
are no quantities per se but have always to be referred to the particular way of their
determination (measuring method and procedure). In contrast, Young´s modulus and
yield stress. are physical quantities and therefore not related to a certain measuring
technique. Different methods are suited to measure them and shall – within the error
of measurement – deliver the same quantitative values. This establishes the
importance of Young´s modulus and yield stress which can be used to develop
predictive models of the mechanical behaviour of solids and structures.
The subject of this presentation is the determination of yield stress and Young´s
modulus in small vertical and lateral dimensions by means of indentation methods.
Two approaches are discussed and compared: The utilisation of spherical indenters as
well as pointed indenters (three-sided pyramids). For the latter, during the last 15
years the concept of the effectively shaped indenter (EI) has been developed and
successfully applied to the mechanical characterisation of bulk samples and thin films.
However, from fundamental considerations as well as experimental data it was
obvious, that the adequateness of the EI concepts is limited to special classes of
materials.
The main part of this presentation is dedicated to the results of an extensive study
about the determination of yield strength by means of nanoindentation. The study is
based on a large choice of materials covering a wide range of E/Y from < 10 up to
about 1000 (E – Young´s modulus, Y – yield stress) as well as a multitude of
alternative measuring methods. The results are reviewed and conclusions are drawn
for the reliable determination of Y and E for bulk materials and thin films.
- 27 -
7-th Symposium on Vacuum based Science and Technology November 19-21, 2013, Koszalin - Kołobrzeg, Poland O 7
ON POLYOPTIMIZATION OF GRADIENT COATINGS
Łukasz Szparaga, Jerzy Ratajski, Roman Olik
Koszalin University of Technology, Institute of Technology and Education, Materials and
Processes Design Facility, Śniadeckich 2 St., 75-453 Koszalin, Poland
Corresponding author: [email protected]
The polyoptimization procedure of geometry and properties of TiAlN/TiN gradient
coatings was created. For physical modelling purposes Cr, TiN and TiAlN layers were
treated as a continuous medium, thus in mathematical description of the stress and
strain states in the coating a classical theory of stiffness was used. In computer model
gradient coatings were represented by continuous transition functions. Using these
functions change of layers materials' parameters ie. Young's modulus, Poisson
coefficient, thermal expansion coefficient and density was described. Polioptimization
procedure was carried out on the gradient coatings subjected to constant external loads
(Hertzian contact). Decisional criteria used in procedure were functions of the stress
and strain fields in the coating and substrate. Utilizing created procedure, Pareto sets
of optimal values of transition functions parameters were obtained. Additionally three
methods of analysis of Pareto-optimal sets were created and discussed.
- 28 -
O 8 7-th Symposium on Vacuum based Science and Technology
November 19-21, 2013, Koszalin - Kołobrzeg, Poland
DIFFUSION-TIGHT MULTILAYER COATINGS FOR THE
ENCAPSULATION OF IMPLANTS
Falk Bernsmann1, Heinz Busch
1, Mattia Castellucci
2
1NTTF Coatings GmbH, Maarweg 32, 53619 Rheinbreitbach, Germany
2Università degli Studi di Trieste, via Alfonso Valerio 6A, 34127 Trieste, Italy
Corresponding author: [email protected]
Thanks to the progress of medical technology, more and more sophisticated implants
like in-situ blood-pressure sensors, cardiac pacemakers or retinal implants are
developed. Many of the materials employed to build these devices, for example
silicon, do not withstand the corrosive body environment, or they can leach toxic
substances, for example heavy-metal ions. Therefore it is necessary to encapsulate the
implants for their proper functioning and biocompatibility. Yet, a too thick
encapsulation can hinder the functionality of the implants or alter their surface
topography to an undesired extent, leading to the need for very thin barrier coatings.
Traditional polymers and even common high barrier coatings like poly-p-xylylenes
(Parylenes) are often not sufficient to provide the necessary diffusion-tightness.
We have developed multilayer systems with a total thickness between 0.2 µm and
0.8 µm made of amorphous hydrogenated carbon and Parylene layers. Both types of
coatings are deposited by standardised procedures in industrial scale coating devices
at substrate temperatures below 40 °C. Therefore the multilayer systems can easily be
applied to a wide range of implant materials. The combination of the two types of
coatings leads to a strong reduction of water diffusion through coated poly-imide foils
by a factor of up to fourteen.
In addition to the multilayer system, we will present two complementary methods to
measure their efficacy as diffusion barriers. The first one is a very simple and quick
test based on the attack of coated silicon substrates by potassium hydroxide solution.
The second one is more sophisticated but still quite rapid. The diffusion of various
gases from a high pressure chamber through a coated foil to a vacuum chamber is
measured in a custom-built device using a mass spectrometer. The advantages and
limits of our measuring methods in comparison to other methods and commercial
measuring devices will be discussed.
- 29 -
7-th Symposium on Vacuum based Science and Technology November 19-21, 2013, Koszalin - Kołobrzeg, Poland O 9
PLASMA-ENHANCED SYNTHESIS OF VISIBLE LIGHT-
ACTIVE PHOTOCATALYST NANOSTRUCTURES FOR WATER
SPLITTING AND OTHER SOLAR APPLICATIONS
A. Kruth 1, S. Müller
1, S. Peglow
1, S. Hansen
2, T. Beweries
2, N. Rockstroh
2, H.
Junge2, M.-M. Pohl
2, V. Brüser
1, K-D. Weltmann
1
1 Leibniz Institute for Plasma Science and Technology (INP), Greifswald, Germany
2 Leibniz Institute for Catalysis (LIKAT), Rostock, Germany
Corresponding author: [email protected]
Hydrogen is considered to be the main future energy carrier. Its carbon-free
production is one of the main challenges for the breakthrough in sustainable energy
conversion technologies. Semiconductor photocatalysis for solar hydrogen generation
from water has attracted an enormous amount of research interest. Main research
target is the development of stable core candidate materials that are able to perform
under the abundant visible light in the solar spectrum, for which there are two main
approaches, i.e. the development of visible light-sensitive semiconductors and
sensitisation of wide band-gap semiconductors. In materials synthesis, plasma-
enhanced surface modification and layer deposition methods are based on the
presence of non-equilibrium states of reactive species in a plasma environment. They
are therefore able to overcome limitations of traditional catalyst synthesis methods,
giving rise to new reaction pathways and resulting in unique properties of
nanomaterials.
In this work, our current approaches to improve nanomaterials properties through
plasma-enhanced PVD and CVD methods are demonstrated. Firstly, highly
homogenous and stable nanostructured anatase layers were synthesised on TCO by a
DC magnetron sputtering process. Subsequent process routes for surface modification
in order to achieve visible light-sensitisaton involved (i) nitrogen doping by RF
plasma-enhanced surface modification, (ii) MW induced plasma-enhanced CVD
process for synthesis of functional polymer-encapsulations for Ru or Ir dye adsorbers,
(iii) RF magnetron sputtering of Au nanoparticles for surface plasmon enhancement
and (iv) deposition of polymer-encapsulated PbS quantum dots by a dual CVD/PVD
process.
- 30 -
O 10 7-th Symposium on Vacuum based Science and Technology
November 19-21, 2013, Koszalin - Kołobrzeg, Poland
A HIGH POWER PULSED PLASMA PROCESS FOR
NANOPARTICLE SYNTHESIS
Ulf Helmersson1, Iris Pilch
1, Daniel Söderström
1,
Rickard Gunnarsson1, Nils Brenning
1,2
1Linköping University, IFM-Materials Physics, SE-581 83 Linköping, Sweden
2Royal Institute of Technology, School of Electrical Engineering,
Division Space & Plasma Physics, SE-100 44 Stockholm, Sweden
Pulsed high-power plasmas open the possibility to utilize ionized material for the
formation and growth of nanoparticles including core-shell structures with a high
precision and productivity. The advantage of ionizing the source material is that it
increases the trapping of positively charged ions onto the negatively charged
nanoparticles in the plasma resulting in a significant increase in growth rate. In this
work a hollow cathode was used where sputtering of metals is performed from the
inside of the cylindrical cathode. The sputtered material of ions and neutrals is ejected
by a gas flow through the cathode, augmented both by the pressure buildup by the
plasma pulse and an outwards directed ambipolar electric field structure at the hollow
cathode opening. This results in an expansion leading to nucleation and growth of
nanoparticles. A range of materials has been used for nanoparticle syntheses including
Cu, Ti, Ag, Mo, and In. Several process parameters have been identified to affect the
size, size distribution, and structure of the particles. These parameters include pulse
power, pulse frequency, sputtering gas composition, and geometry of the setup. By
tuning the process parameters, the particle size can range from approximately 5 to 700
nm in diameter. Depending on process parameters used, the synthesized nanoparticles
vary in structure from being single crystals with well-defined crystallographic faces to
being amorphous-looking consisting of randomly oriented agglomerates of nano-
crystals.
- 31 -
7-th Symposium on Vacuum based Science and Technology November 19-21, 2013, Koszalin - Kołobrzeg, Poland O 11
CONTROLLED GROWTH OF TRANSITION METAL NITRIDE
FILMS VIA SELECTION OF METAL ION IRRADIATION
DURING HYBRID HIPIMS/MAGNETRON CO-SPUTTERING
G. Greczynski,1 J. Lu,
1 J. Jensen,
1 I. Petrov,
1,2 J.E. Greene,
1,2
W. Kölker,3 S. Bolz,
3 Ch. Schiffers,
3 O. Lemmer
3 and L. Hultman
1
1 Thin Film Physics Division, Department of Physics (IFM), Linköping University, SE-581 83
Linköping, Sweden 2 Frederick Seitz Materials Research Laboratory, University of Illinois
3 CemeCon AG, Adenauerstr. 20 A4, D-52146 Wűrselen, Germany
Corresponding author: [email protected]
Thin films of transition metal nitrides Ti-M-N (where M = Al, Si) are grown from
elemental targets by high-power pulsed magnetron (HIPIMS) and dc magnetron
(DCMS) co-sputtering. Unique film properties are obtained through (i) selection of
metal ion irradiation assisting film growth and (ii) advanced substrate-biasing
schemes. Time-resolved in-situ mass spectrometry is used to analyze composition and
energy distributions of ion fluxes incident at the film surface during growth. The
distinctly different flux distributions obtained from targets driven in HIPIMS vs.
DCMS modes allow the effects of Aln+
, Sin+
and Tin+
(n = 1, 2, 3) ion irradiation on
resulting film properties to be investigated separately.1 Markedly different film growth
pathways are obtained depending upon which target is powered by HIPIMS. For Ti1-
xAlxN layers grown with Vs = 60 V and HIPIMS applied to the Al target, Al+ ion
irradiation of the growing film results in alloys (0.55 ≤ x ≤ 0.60) which exhibit high
hardness, H 30 GPa, and low stress, 0.2-0.7 GPa tensile. On contrary, films with
corresponding AlN concentrations grown with HIPIMS applied to the Ti target, giving
rise to Tin+
ion irradiation (with a significant Ti2+
component) are two phase (cubic
(Ti,Al)N and hexagonal AlN) with low hardness, H = 18-19 GPa, and high
compressive stress ranging up to 2.7 GPa.2 Further advantage is made of the fact that
intensity of metal and gas ion fluxes at the substrate position varies with time. By
using the pulsed substrate bias synchronized with the metal-ion-rich phase of the
HIPIMS pulses, Ar+ ion irradiation is minimized in favor of metal ion irradiation,
which is predominantly by target ions.3 This drastically decreases the concentration of
trapped gas ions and the associated compressive stresses are greatly reduced.
1 G. Greczynski, J. Lu, M. Johansson, J. Jensen, I. Petrov, J.E. Greene, and L. Hultman, “Role of Tin+ and Aln+ ion irradiation (n = 1, 2) during Ti1-xAlxN alloy film growth in a hybrid HIPIMS/magnetron mode”, Surf. Coat. Technol. 206 (2012) 4202 2 G. Greczynski, J. Lu, M. Johansson, J. Jensen, I. Petrov, J.E. Greene, and L. Hultman “Selection of metal ion irradiation for controlling Ti1-xAlxN alloy growth via hybrid HIPIMS/magnetron co-sputtering”, Vacuum 86 (2012) 1036 3 G. Greczynski, J. Lu, J. Jensen, I. Petrov, J.E. Greene, S. Bolz, W. Kölker, Ch. Schiffers, O. Lemmer and L. Hultman, “Metal vs. Rare-gas Ion Irradiation during Ti1-xAlxN Film Growth by Hybrid HIPIMS/DCMS Co-sputtering using Synchronized Pulsed Substrate Bias”, J. Vac. Sci. Technol. A 30 (2012) 061504-1
- 32 -
O 12 7-th Symposium on Vacuum based Science and Technology
November 19-21, 2013, Koszalin - Kołobrzeg, Poland
ADVANCES IN PROCESS TECHNOLOGY AND DEPOSITION
EQUIPMENT FOR HIPIMS COATINGS FOR CUTTING TOOLS
Toni Leyendecker1, Oliver Lemmer
1, Werner Kölker
1, Christoph Schiffers
1
1CemeCon AG, Adenauerstrasse 20A4, 52146 Würselen, Germany
HiPIMS is characterised by short power pulses with an extremely short signal rise
time. The design of the coating equipment need to take this characteristic into account
with regard to feeding the electrical energy into the sputtering cathodes and finally
into the plasma. This paper will present recent results on the correlation of the
hardware design of the machine and the coating process. Fundamental research about
the efficiency 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 cutting tool sets its focus to the properties of the coating and, most
important, to the machining characteristics of the film. Examples and field data will
show how the most up-to-date HiPIMS coatings boost both productivity and quality.
SEM images reveal a dense morphology of HiPIMS coatings. To this feature can be
attributed that HiPIMS films combine high hardness and a relatively low Young’s
modulus indicating a high coating toughness in a way most favourable for metal
cutting.
Super smooth coatings, free from any droplets, and low compressive stress are the
most beneficial characteristics of sputter coatings for cutting tools. The effective
bombardment of the growing film with highly ionized species further improves the
surface of HiPIMS coatings.
- 33 -
NEW STANDARD TO TEST THE DYNAMICS OF VACUUM
GAUGES IN THE MS RANGE
Karl Jousten
PTB, Berlin
In several industrial applications, such as leak testing, CD metallization or coating
processes, fast processes are often involved, requiring rapid changes of pressures in
the vacuum regime. Vacuum load locks are typically being used for coating processes,
where the pressure changes from atmospheric to medium vacuum within 1 s or less.
The control of such vacuum systems is triggered by vacuum gauge readings.
Therefore, vacuum gauge manufacturers are interested to know how fast their gauges
can follow such rapid changes of pressures.
In order to study the response time of vacuum gauges to rapid pressure changes, the
Physikalisch-Technische Bundesanstalt has developed a dynamic vacuum standard
where the pressure may change from 100 kPa to 100 Pa within 20 ms in a step-like
function or in a predictable manner on a longer time scale but still within 1 s or less.
This is accomplished by an expansion of gas at 100 kPa from a very small volume of
less than 0.1 L into a large volume of 180 L through a well defined orifice. The
process is started after the activation of a fast opening gate valve DN40, reaching its
final state within less than 5 ms. The temperature inside the small volume may drop to
about 160 K.
Simulations have been performed to calculate the pressures and temperatures by a
hybrid continuum particle solver. This is a challenging task, due to the fact that the
low pressure dictates an approach based on the kinetic theory of gases, but also due to
the non-stationary nature and extreme characteristics of the flow, such as the
geometrical features and Mach numbers.
First results of tests regarding the response time of fast vacuum gauges are presented
and discussed.
Support through the EMRP IND12 project is gratefully acknowledged. The EMRP is
jointly funded by the EMRP participating countries within EURAMET and the
European Union.
7-th Symposium on Vacuum based Science and Technology November 19-21, 2013, Koszalin - Kołobrzeg, Poland O 13
- 34 -
A CRYOGENIC DISTILLATION COLUMN FOR THE XENON1T
EXPERIMENT Stephan Rosendahl
1, Ethan Brown
1, Ion Cristescu
2, Alexander Fieguth
1, Christian
Huhmann1, Michael Murra
1 and Christian Weinheimer
1
1Institut für Kernphysik, Wilhelm-Klemm Strasse 9, 48149 Münster, Germany
2Karlsruher Institut für Technologie, Tritium Laboratory,, Hermann Von Helmholtz-Platz 1,
76344 Eggenstein-Leopoldshafen, Germany
Corresponding author: [email protected]
The XENON1T experiment is the next generation experiment for the direct detection
of dark matter particles, especially WIMPS (weakly interacting massive particles). For
this purpose a dual-phase TPC, filled with Xenon is used, aiming for a fiducial volume
of 1ton detector mass. To increase the sensitivity of WIMPS-nucleon cross sections,
the radioactive background has to be extremely low.
One source of radioactive contamination in the Xenon is coming from the beta-decay
of Kr-85 with an endpoint energy of 687keV. The Kr-85 originating from nuclear
waste management and nuclear weapon tests in natural Krypton amounts to about
2*10-11
. To reach the final sensitivity of XENON1T, the Xenon has to be purified to a
concentration of <0.1ppt (parts per trillion) natural Krypton in Xenon. For this
purpose the technique of cryogenic distillation is used.
At the University of Münster a distillation column has been designed and built to
reach this level of purity with a process flow of 3kg/h at an operation temperature of -
100°C. To avoid contaminations of the Xenon during the process, the whole system
has to fulfil the same standards in terms of leak tightness and surface cleanness as
ultra-high vacuum systems. All connections are either VCR or CF connections and all
the piping is done using orbital-welding technique. Most of the parts have been
electro-polished and all of them have been cleaned using an ultra-sonic bath. To
evacuate the system an oil-free turbo-molecular pump with scroll pump is used and
the main components are bakeable like it is common in vacuum applications. This
system is also connected to a quadrupole mass spectrometer behind a LN2 cold trap to
enhance the sensitivity to measure the concentration of Krypton in Xenon down to 40
ppt. In addition a new radioactive tracer method based on Kr-83m has been developed
to online monitor and to optimize the separation of Krypton from Xenon in the
cryogenic distillation column.
This presentation gives a status report of the commissioning of the phase 1 version of the
cryogenic distillation column (3m total height) and an outlook of the full phase 5m high
distillation column to be installed at the XENON1T experiment at the Italian underground
laboratory LNGS in 2014.
O 14 7-th Symposium on Vacuum based Science and Technology
November 19-21, 2013, Koszalin - Kołobrzeg, Poland
- 35 -
FLEXIBLE DLC COATINGS TO PREVENT CRYSTALLINE
BIOFILM FORMATION ON URINARY TRACT IMPLANTS.
G. Baldsiefen1, N.Laube
2
1 Institute of Thin Film Technology of the TU-Kaiserslautern,
MAARWEG 32, D-53619 RHEINBREITBACH 2 NTTF Coatings GmbH, Maarweg 32, D-53619 Rheinbreitbach
Corresponding author: [email protected]
Formations of crystalline bacterial biofilms (encrustations) on urological implants
remain a major complication in patient care. Recently, it was shown that amorphous
carbon (a-C:H) coatings deposited on polyurethane (PU) stents provide a distinct
reduction in biofilm formation.
Each implant placed into the urinary tract is vulnerable to the formation of crystalline
bacterial biofilms. These biofilms are the source of partly serious concomitant
deseases. The hitherto applied strategies for the reduction of these complications using
material- and surface-modifications did not show the expected results. The Institute of
Thin Film Technology of the TU Kaiserslautern and the NTTF Coatings GmbH have
shown within a common project that amorphous diamond like carbon coatings (a-C:H,
DLC) reduce the formation of crystalline biofilms on urological catheters and
implants. These carbon coatings are especially well tolerated by the human body.
Plasma deposited amorphous carbon coatings are distinguished by particularly
physical and chemical properties and by their excellent biocompatibility. The
primarily chemically inert coatings are built up from low-molecular carbon
compounds. They arrange themselves in a certain near-order within an otherwise
disordered matrix.
Dependent on their production methods the coatings can be varied in density and
composition. By the integration of dopant atoms they can in addition be specific
modified in their surface properties so that they fulfill versatile requirements in
different fields of application.
7-th Symposium on Vacuum based Science and Technology November 19-21, 2013, Koszalin - Kołobrzeg, Poland O 15
- 36 -
POLYPROPYLENE NONWOVEN SHIELDS AGAINST
ELECTROMAGNETIC FIELDS OBTAINED BY PLASMA
DEPOSITION OF CUSN ALLOY
ed
O 16 7-th Symposium on Vacuum based Science and Technology
November 19-21, 2013, Koszalin - Kołobrzeg, Poland
- 37 -
7-th Symposium on Vacuum based Science and Technology November 19-21, 2013, Koszalin - Kołobrzeg, Poland O 17
THE SURFACE ASSESSMENT AND THE PROPERTIES OF
SELECTED MULTILAYER COATINGS
A. Gilewicz1, B. Warcholinski
1
1Koszalin University of Technology, Institute of Technology and Education, Śniadeckich 2 St.,
75-453 Koszalin, Poland
Corresponding author: [email protected]
One the most widely used method of thin coatings deposition is the cathodic arc
evaporation. This method is characterized by a high degree of ionization of the
plasma, and high energy ions - up to 100 eV, which leads to high efficiency of coating
deposition. The coatings obtained using this method are characterized by high
hardness, good adhesion to the substrate, high density, uniformity, and are greater than
the films obtained using magnetron sputtering method. The disadvantage of this
method is the relatively high roughness of the coating, resulting from the large number
of macroparticles on the surface.
The paper presents the evaluation of the surface quality and properties of
multilayer coatings, obtained by cathodic arc evaporation, of the same structure in
which the top layer is a CrN chromium nitride layer. The second component of double
layer module with a thickness of 400 nm and a thickness of each layer about 200 nm
are two component TiN, Mo2N systems and three component TiAlN and CrCN
systems. In studies by scanning electron microscopy and optical microscopy the
surface density of macroparticles of the coating and their dimensions were estimated.
The adhesion to steel substrates using scratch test and Rockwell test and wear were
also investigated. The results indicate that melting point of cathode material directly
affects the number and size of macroparticles on the surface of the growing coating.
Number of macroparticles increases with lowering of the melting point of the cathode
material. All coatings show good adhesion with the critical load Lc2, greater than 60 N
and hardness above 20 GPa. The Mo2N/CrN coating despite the relatively low critical
load compared with the other tested coatings have the best wear resistant properties,
which is probably due to Mo2N → MoO3 transformation.
- 38 -
- 39 -
7-th Symposium on Vacuum based Science and Technology November 19-21, 2013, Koszalin - Kołobrzeg, Poland P 1
THE INFLUENCE OF DEPOSITION PARAMETERS ON S-
PHASE COATINGS OBTAINED BY REACTIVE MAGNETRON
SPUTTERING
Jolanta Baranowska, Sebastian Fryska
Institute of Materials Science and Engineering, West Pomeranian University of Technology,
70-310 Szczecin, al. Piastow 19, Poland
S-phase (expanded austenite) is a metastable phase with very high hardness and good
corrosion resistance which demonstrates a large potential for many practical
applications. This phase can be obtained using various methods, including gas and
plasma nitriding of austenitic stainless steel as the most common ones. It is considered
as supersaturated nitrogen solution in austenitic matrix. The paper presents the results
of investigations on the influence of deposition parameters on the formation of S-
phase coatings by reactive magnetron sputter deposition. The morphology and
properties of S-phase depends on different parameters eg. deposition parameters,
conditions of the substrate surface, etc. During the process the presence of plasma
elements was measured by mass spectrometer. The phase composition was evaluated
using X-ray diffraction (XRD and GXRD). EMPA (EDS and WDS) techniques were
used to study element composition of the layers. Microstructure was investigated by
means of scanning electron microscope (SEM).
Keywords: S-phase, reactive magnetron deposition, coating texture, microstructure
- 40 -
P 2 7-th Symposium on Vacuum based Science and Technology
November 19-21, 2013, Koszalin - Kołobrzeg, Poland
DEPOSITION AND CHARACTERISATION OF MAGNESIUM
DOPED Cr2O3 GROWN VIA MAGNETRON SPUTTERING
David Caffrey1*, Karsten Fleischer1 and Igor V. Shvets1
1Cleaner Energy Laboratory, School of Physics, Trinity College Dublin, Dublin 2, Ireland
Corresponding author: [email protected]
P type Transparent Conducting Oxides are key materials for the development of
transparent electronics. However, p-type TCOs have always exhibited poorer
performances than their n-type counterparts. As a result, new materials remain an
important area of research. Previous work has indicated Cr2O3 as an appropriate
material, with Mg and N doped samples displaying high p-type conductivities while
maintaining transparencies of up to 65%.
Here, we present the growth of Mg doped Cr2O3 films via Magnetron Sputtering.
Samples were grown via co-deposition from Cr and MgO targets in a reactive Ar + O2
atmosphere. The optoelectronic properties of the material were analysed and are
discussed as a function of the growth parameters. The effects of growth temperature,
Cr/Mg ratio and oxygen flow rate were investigated. Electrical properties were
analysed via 4-point probe. Optical properties were investigated via UV-Visible
measurements and Raman spectroscopy. Crystallographic data was obtained by XRD.
Elemental composition was obtained via EDX. Magnetron grown samples will be
compared to the currently best performing samples grown by spray pyrolysis.
- 41 -
7-th Symposium on Vacuum based Science and Technology November 19-21, 2013, Koszalin - Kołobrzeg, Poland P 3
CONTROL OF WETTABILITY OF AMORPHOUS CARBON
BASED COATINGS BY ADJUSTMENT OF SURFACE
CHEMISTRY AND SURFACE TOPOGRAPHY
F. Danneil
1, M. Stüber
2, S. Ulrich
2, K. Seemann
2, H. Leiste
2, A. Welle
3
1 Karlsruhe Institute of Technology, Service Unit Personnel Development (PEBA), 76021
Karlsruhe (Germany) 2 Karlsruhe Institute of Technology (KIT), Institute for Applied Materials – Applied Materials
Physics (IAM-AWP), 76021 Karlsruhe (Germany) 3 Karlsruhe Institute of Technology (KIT), Institute for Biological Interfaces (IBG), 76021
Karlsruhe (Germany)
corresponding author: [email protected]
Adjustment of surface chemistry as well as of surface topography enables to influence
and control wettability, especially of amorphous carbon based coatings. Different
kinds of amorphous carbon coatings were deposited by d.c. magnetron sputtering of a
graphite target at a power of 500 W in different plasma atmospheres consisting of pure
argon, argon and hydrogen, argon and nitrogen, as well as argon and oxygen.
Deposition takes place on single-crystalline, double-sided polished Si-substrates of
<100>-orientation with and without r.f. substrate bias and no additional substrate
heating. These coatings are modified by post-deposition reactive ion etching in an
oxygen atmosphere and micro-patterning by photo-lithography. Geometry of micro-
patterning is 25 µm square wells, 75 µm apart from each other. All these coatings are
characterized with respect to their bonding structure by Visible Raman spectroscopy
analysis. Their wettability is investigated by dynamic contact angle measurement of a
sessile drop of distilled water. Deposition without r.f. substrate bias in pure argon
plasma results in a contact angle by distilled water of about 60°, which is lowered
down to 20° by subsequent reactive ion etching in an argon/oxygen mixture. In
addition to post-deposition reactive ion etching in-situ modification by changing
plasma chemistry by adding hydrogen, oxygen or nitrogen into the argon plasma leads
to contact angles by distilled water of about 55°, 35° and 45°, respectively. As another
in-situ modification an r.f. substrate bias of -100 V was applied to increase ion
bombardment during film growth followed by post-deposition reactive ion etching
results in a contact angle by distilled water of about 50°. Furthermore, an additional
micro-patterning of all considered coatings leads to an increase of contact angles.
Generally, the obtained results show that a smart combination of optimized plasma
chemistry, deposition parameters, reactive ion etching, and micro-patterning allows to
tailor contact angles in a range from 20° to 100°.
A graphic overview of the work is given in Fig. 1.
- 42 -
Fig. 1: Schematic representation of this work.
- 43 -
7-th Symposium on Vacuum based Science and Technology November 19-21, 2013, Koszalin - Kołobrzeg, Poland P 4
PREPARATION AND PROPERTIES CHARACTERIZATION OF
EMI NONWOVEN SHIELDS OBTAINED BY PLASMA
DEPOSITION OF CuSn ALLOY
E. Dobruchowska1 J. Koprowska
2, K. Reszka
1
1 Koszalin University of Technology, Institute of Technology and Education,
ul. Śniadeckich 2, 75-453 Koszalin, Poland 2 Textile Research Institute, ul. Brzezinska 5/15, 92-103 Lodz, Poland
Textiles, due to their specific properties like large surface area relative to volume,
network structure, flexibility and portability, have a great potential to be employed as
components in electromagnetic interference (EMI) shields. In this work, in order to
obtain effective protection against electromagnetic fields, we have used melt-blown
polypropylene (PP) nonwoven which served as a substrate for CuSn deposition.
Nonwoven metallisation was carried out using DC magnetron sputtering process of
CuSn (4:1) alloy target in argon ambient.
The studies aimed at determining the effect of process parameters (power dissipated in
the target, velocity of the substrate drift, number of cycles) on the surface morphology
of PP nonwoven modified by the metallic deposition, the crystalline/amorphous
structure of the CuSn thin layers and the effectiveness of shielding a flat
electromagnetic wave by the two-component CuSn/PP composites. The morphology
studies, performed using metallographic optical microscopy and scanning electron
microscopy, revealed that the metallic layers possess smooth surface, dense structure
and very good adhesion to the substrate. Further, the crystalline character of the CuSn
component was examined in the grazing-incidence angle X-ray diffraction
experiments. It has been found that the composites with the crystalline structure of the
metallic layers exhibit the highest values of the shielding effectiveness (45 dB at
27 MHz and 39 dB at 1795 MHz).
The research was carried out within the key project – PO IG no. 01.03.01-00-006/08
co-financed from the funds of European Regional Development Fund within the
framework of the Operational Programme Innovative Economy
- 44 -
P 5 7-th Symposium on Vacuum based Science and Technology
November 19-21, 2013, Koszalin - Kołobrzeg, Poland
CHARACTERISATION OF ANTI-REFLECTIVE DIAMOND-
LIKE CARBON COATINGS FOR INFRARED APLICATIONS
Slawomir Gogler1, Boguslaw Budner
1, Jadwiga Mierczyk
1, Magdalena
Szymanska2,3
, Malgorzata Kalisz2,3
1Institute of Optoelectronics, Military University of Technology,2 Kaliskiego str.,
00-908 Warsaw 2Institute of Microelectronics and Optoelectronics,Warsaw University of Technology,75
Koszykowa str., 00-662 Warsaw 3 Centre for Material Testing and Mechatronics, Motor Transport Institute,
80 Jagiellonska str., 03-301 Warsaw, Poland
Corresponding author: [email protected]
Many papers have already been presented on diamond-like carbon amorphous layers
deposited by various method. Among papers on layers deposited by PECVD method
those from methane and acetylene prevail. In the presentation diamond-like
amorphous carbon layers deposited by PECVD process from n-hexane vapour as
precursor gas will be characterised. Layers are deposited by a commercial coating
plant - Leybold Optics DLCcs designed specifically for depositing DLC monolayers.
The coating plant is equipped with liquid container and a vapour delivery system that
allows liquid precursors to be used. All gas supplies can be either constant in flow or
PID controlled, so can be bias voltage and RF power supply. Deposited layers are
mainly used as anti-reflective coatings for Long- and Mid- wave Infrared in military
applications as a front lens outer coating due to their high environmental and
mechanical durability. Because such coatings have to adhere to military and domestic
optical norms regarding, for example, their adhesion, scratch resistance and optical
transmission there is a need for evaluation of their tribological and optical properties.
Basic characterisation of deposited layers in the presentation is given: optical/material
properties: FTIR and Raman spectra, tribological: hardness and adhesion tests, surface
morphology: SEM and AFM images.
- 45 -
7-th Symposium on Vacuum based Science and Technology November 19-21, 2013, Koszalin - Kołobrzeg, Poland P 6
INFLUENCE OF CVD DURATION PROCESS ON
MORPHOLOGY, STRUCTURE, AND SENSING PROPERTIES
OF CARBONACEOUS-PALLADIUM THIN FILMS
E.Kowalska1, A.Kamińska
1, E.Czerwosz
1, M.Kozłowski
1, K.Sobczak
2, B.Witkowski
2
1Tele
& Radio Research Institute, Ratuszowa 11 Street, 3-450 Warsaw, Poland
2 Institute of Physics PAS, Al. Lotników 32/46, 02-668 Warsaw, Poland
Corresponding author: [email protected]
We present the nanocomposite carbonaceous-palladium thin films prepared by
physical vapor deposition (PVD) and chemical vapor deposition (CVD) methods.
Scanning electron microscope (SEM) and TEM (transmission electron microscope)
methods were used to study the topography, morphology and structure of carbon and
palladium nanograins contained in these films. The initial PVD films were modified in
a CVD quartz reactor using xylene as a modifying factor at different time (5, 10 and
30 minutes) at a constant temperature ~650°C in atmospheric pressure. It was
observed that the average size of palladium nanograins increases with an increasing
duration of modification process. An amount of xylene was also increased, what
caused the growth of thickness of graphite shells around Pd nanograins. In all samples
Pd nanograins with the size above 300 nm were found regardless of CVD duration
process. These large nanograins in TEM studies were not screened by electron beam.
The differences in microstructures observed in the CVD films modified at different
times, affect their response in measurements of resistance changes in the gas
containing H2 in various concentrations. All samples were measured by
cathodoluminescence (CL) method. In CL studies a large amount of objects with high
intensity of CL was found. Some of them show the emission bands both at 450 nm
and 750 nm. Other reveals emission band only at 450 nm. CL observations show that
Pd nanograins coated by graphite shells exhibit optical activity.
- 46 -
P 7 7-th Symposium on Vacuum based Science and Technology
November 19-21, 2013, Koszalin - Kołobrzeg, Poland
NANOCOMPOSITE CARBONACEOUS-PALLADIUM THIN
FILMS FOR AMMONIA SENSING
Sławomir Krawczyk*1, Anna Kamińska
1 , Mirosław Kozłowski
1, Joanna
Radomska1, Piotr Dłużewski
2, Elżbieta Czerwosz
1
1Tele and Radio Research Institute, Ratuszowa 11, 03-450 Warsaw, Poland
2Institute of Physics, Al. Lotników 32/46 02-668 Warsaw, Poland
*Corresponding author: e-mail: [email protected]
Nanocomposite carbonaceous-palladium (C-Pd) films, which were synthesized
in two steps new method based on Physical Vapor Deposition and Chemical Vapor
Deposition (PVD/CVD) processes. Films were deposited on alundum substrate.
Investigated films were obtained at different parameters of CVD process but at the
same conditions in PVD process.
These films are promising materials for ammonia sensor applications. Films
were characterized by SEM (after PVD and PVD/CVD process), TEM (after
PVD/CVD process) and sensing properties on ammonia for all these films were also
measured.
Our SEM investigations of initial film obtained from PVD process reflect
substrate surface’s shape and are composed of angular grains few hundred nm in size.
Microscopically studies of PVD/CVD films show that topography and morphology of
the film strongly depends on the temperature of CVD process. Sensing properties of
these films are connected to their structural and morphological properties.
ACKNOWLEDGMENT
This project is co-financed by the European Regional Development Fund within the
Innovative Economy Operational Programme 2007-2013 (title of the project “Development of
technology for a new generation of the hydrogen and hydrogen compounds sensor for
applications in above-normative conditions”) No UDA-POIG.01.03.01-14-071/08-08.
- 47 -
7-th Symposium on Vacuum based Science and Technology November 19-21, 2013, Koszalin - Kołobrzeg, Poland P 8
PVD SURFACE TREATMENT OF HEAT TREATED CAST
ALUMINIUM ALLOYS
Krzysztof Labisz 1, Tomasz Tański
1, Marcin Bilewicz
1
1Division of Materials Processing Technology, Management and Computer Techniques in
Materials Science, Institute of Engineering Materials and Biomaterials, Silesian University of
Technology, Konarskiego Str 18A, 44-100 Gliwice, Poland
Corresponding author: [email protected]
Well prepared coatings on surface layer of structural materials is one of the most
important issue in the up to date material engineering, where vacuum techniques are
often used for improvement of t mechanical properties of the surface.
Gradient/monolithic coatings (Cr/CrN-gradient/TiN), Cr/CrN-gradient/CrN) were
deposited onto aluminium alloy (Al-Si-Cu) substrate by cathodic arc evaporation
method. A thin metallic layer (Cr) was deposited prior to deposition of gradient
coatings to improve adhesion. In this work there are presented the investigation results
concerning microstructure and mechanical properties especially microhardness of the
bi-layer coatings (gradient/ multicompound) coated using the PVD method (electric
arc evaporation) onto the aluminium alloy substrate. Investigations of the CrN/CrN
and CrN/TiN coating type were performed, using transmission (TEM) and scanning
electron microscope (SEM). Change of the chemical composition was measured on
the basis of the glow discharge optical emission spectrometer (GDOS). The
investigated coatings reveal a compact structure, without visible defoliations and
defects, it is coated uniformly and tightly bound to the substrate. The fracture
morphology is characterised with a lack of columnar structures. The metallographic
examinations carried out give grounds to state that the coatings were deposited
uniformly onto the investigated substrate materials and that they are characteristic of
the depending on the coating type employed, and that the particular layers adhere
tightly to themselves and to the substrate. In general the following should be pointed
out, that the surface layer has a polycrystalline structure consisting of nanoscale
crystallites. This investigation with appliance of the PVD method makes it possible to
obtain, interesting solutions very attractive for automobile and aviation industry.
- 48 -
P 9 7-th Symposium on Vacuum based Science and Technology
November 19-21, 2013, Koszalin - Kołobrzeg, Poland
SPUTTERING LINE FOR THE PHOTOVOLTAIC COATING
DEPOSITION
K.Marszałek1, W.Doros
2
1AGH - University of Science and Technology, 30-059 Krakow, Mickiewicza 30, Poland
2DAGlass, Warszawska 55, Rzeszow, Poland
The design and technical descriptions of the sputtering line is presented.
Vacuum system is composed of 5 vacuum chambers divided by 4 isolating valves into
3 vacuum sections. All the chambers are made of low carbon mild steel welded
together reinforced by steel bars with fore-buffer chamber, post-buffer chamber and
sputtering deposition chamber in the middle separated by several gas isolating settings
formed several stages of vacuum pressure differentials by diffusion pumps, Pumping
system is composed of Roots pumps, mechanical pumps and diffusion pumps and all
the vacuum valves are e-control pneumatic valves under auto control by vacuum data
and signals with self-lock and inter-lock functions to prevent damages from sudden
failures or mal-operation. Max. vacuum pressure: better than 1×10-3
Pa.Gas inflation
system: 6 sets “Seven Star” MFC (mass flow controller) equipped to set and control
gas flow with throttle valves. It is available to set and control gas flow for sputtering
deposition chambers under pressure range 1×100Pa~1×10
-1Pa. Maximum deposition
size available: 1200X3000mm, thickness 3~8mm.
Deposit functions: available to coat single layer or multi-layers of metal films, solar-
control films and aluminum mirror films.
Praca współfinansowana przez Unię Europejską ze Środków Europejskiego Funduszu
Rozwoju Regionalnego w ramach Programu Operacyjnego Innowacyjna Gospodarka,
Działanie ‘Wsparcie projektów B+R na rzecz przedsiębiorców realizowanych przez jednostki
naukowe’ projekt POIG.01.03.01-30-056/12.
- 49 -
7-th Symposium on Vacuum based Science and Technology November 19-21, 2013, Koszalin - Kołobrzeg, Poland P 10
DILATOMETRIC METHOD
OF THERMOMECHANICAL EFFECTS DETECTION
OF SUBSTRATE – PVD COATING SYSTEMS
Piotr Myśliński
Koszalin University of Technology
Institute of Technology and Education
Intensive development of technologies of wear resistant PVD coatings deposition
on working surfaces of tools for metal and wood treatments and the increasing
requirements against tools, extort the use of different diagnostic tests of newly formed
coatings. In this regard, anticipating knowledge of the thermal stability of coating
properties relevant to the durability of the tools is a very important factor in the
selection of process parameters for creation of newly designed structures.
PVD coatings deposition takes place in thermally unbalanced conditions, hence the
use of tools in the complex tribological junctions often results in thermal activation of
a series of micro–and macroscopic processes. These are mainly stress relaxation,
growth of the coating material grains, the mechanisms of diffusion as well as chemical
and mechanical degradation of the coating structure. The result of these processes and
their synergy are among others the changes of stresses in the coatings. In the
developed method, during the programming annealing of physical model of the
substrate – PVD coating system, the thermal effects in the film, that take place under
real operating conditions of wear resistant PVD structures, are reproduced.
Distinguishing features of the developed method consist in the fact that monitoring of
the changes in the state of stress in the coating is performed during the course of
applied heat treatment and the subject of measurements are the changes in temperature
and linear displacement of the substrate, recorded by the measuring device –
compensative dilatometer. The proper resolution of the measurements was obtained
by application the dilatometry with modulated temperature.
The content of this article is the presentation of the work realized by the author, the
results of which can be used to implement into research practice a new
thermomechanical method of testing the thermal stability of PVD coatings.
- 50 -
P 11 7-th Symposium on Vacuum based Science and Technology
November 19-21, 2013, Koszalin - Kołobrzeg, Poland
MAGNETRON SPUTTERED METALLIC NANOPARTICLES
FOR REINFORCEMENT OF POLYMER MATERIALS
S. Passlack1, B. Suksut
2, J. Meyer
3, A. Brodyanski
1, B. Reuscher
1, L. Lin
2, G.
Niedner-Schatteburg3, A. Schlarb
2, M. Kopnarski
1
1)
Institut für Oberflächen- und Schichtanalytik IFOS, Kaiserslautern 2)
Lehrstuhl für Verbundwerkstoffe, TU Kaiserslautern, Kaiserslautern 3)
AG Clusterchemie, TU Kaiserslautern, Kaiserslautern
The physical properties and the application characteristics of polymers are strongly
dependent on their morphological structure. Although nanocomposites show
remarkable property improvements compared to virgin polymers the underlying
interaction between the nanoparticles and the resulting polymer morphology could so
far not be explained at a satisfactory level. In an earlier work we investigated the
microstructure of PP containing different loads of nano-SiO2. The small-scale
dispersion and the nature of the used nanoparticles originating from the multistep
compounding process are crucially influencing the super molecular morphology. In a
new approach we used magnetron sputtering and a gas-aggregation technique to
prepare and provide metallic and suboxidic nanoclusters with controllable cluster sizes
and size distributions. The magnetron sputtering gas aggregation source will be
presented and the output of this particle source was analyzed with regard to chemical
and structural composition, lateral homogeneity and size distribution of the deposited
clusters. Furthermore a new approach for the embedding of the nanoparticles in the
polymer matrix is presented.
- 51 -
7-th Symposium on Vacuum based Science and Technology November 19-21, 2013, Koszalin - Kołobrzeg, Poland P 12
NANOSTRUCTURED GOLD/TITANIUM DIOXIDE CATALYSTS
FOR LIGHT-DRIVEN WATERSPLITTING
S. Peglow, A. Kruth, V. Brüser
Leibniz Institute for Plasma Science and Technology (INP), Greifswald, Germany)
Corresponding author: [email protected]
Hydrogen has proven to be an attractive storage medium for energy. Depending on the
nature of its production, it can be an emission-free alternative to fossil fuels. Solar
energy maybe employed in order to to split water into to form hydrogen by the means
of photocatalysis.
Nanoparticular precious metals such as Au, Ag or Cu maybe deposited onto TiO2
semiconductor layers in order to extend the photocatalytic activity of TiO2 from the
UV region into the visible light region by means of plasmon resonance for a more
efficient use of the solar spectrum.
In this work, nanostructured Au particles are deposited onto TiO2-layers on TCO by
means of a plasma-enhanced PVD process. The TiO2-layers were synthesised by a DC
magentron sputtering process on TCO. Process parameters were optimised with regard
to size and nanostructure of the Au, as well as resulting photocatalytic properties at
visible wavelengths. The new materials were characterised using XRD, XPS, electron
micropscopy, UV/Vis spectroscopy and photoelectrochemical measurements.
- 52 -
P 13 7-th Symposium on Vacuum based Science and Technology
November 19-21, 2013, Koszalin - Kołobrzeg, Poland
CONSTITUTION, MICROSTRUCTURE AND MECHANICAL
PROPERTIES OF MAGNETRON-SPUTTERED TIC/A-C
NANOCOMPOSITE COATINGS
M. Rinke1, M. Stüber
1, C. Ziebert
1, M. Lattemann
2, S. Ulrich
1
1Karlsruhe Institute of Technology (KIT), Institute for Applied Materials (IAM), Hermann-
von-Helmholtz-Platz 1, 76344 Eggenstein-Leopoldshafen, Germany 2Department of Physics, Chemistry, and Biology (IFM), Linköping University, SE-581 83
Linköping, Sweden; Sandvik Coromant, Lerkrogsvägen 13, SE-126 80 Stockholm, Sweden
Corresponding author: [email protected]
Carbon-based nanostructured composite coatings wih promising properties like wear
protection and low friction often consist of nanocrystalline phases or clusters
homogeneously dispersed in an amorphous carbon matrix or covered by an
amorphous carbon grain boundary phase. A segmented sputtering target composed of
plates of bulk ceramic TiC and graphite was applied in order to individually adjust the
Ti:C elemental concentration ratio of 6 coatings deposited in one experiment in 6
different positions related to the target. The experiments were carried out in a Leybold
Z 550 PVD machine under systematic variation of the R.F. substrate bias. Results on
the constitution and microstructure are obtained from Electron probe microanalysis
(EPMA), Raman spectroscopy, X-ray diffraction (XRD), and transmission electron
microscopy (TEM). The hardness and Young`s modulus were characterized and the
evolution of microstructure and properties of the coatings are discussed as a function
of the Ti:C ratio and Raman bands. A correlation between constitution, microstructure
and mechanical properties of non-reactively magnetron sputtered TiC/a-C
nanocomposite coatings is given.
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7-th Symposium on Vacuum based Science and Technology November 19-21, 2013, Koszalin - Kołobrzeg, Poland P 14
VENTING OF THE KATRIN MAIN SPECTROMETER WITH
ULTRA-CLEAN ARGON KEEPING THE ACTIVATION OF THE
NON-EVAPORABLE GETTERS
Stephan Rosendahl1 and the KATRIN collaboration
1Institut für Kernphysik, Wilhelm-Klemm Straße 09, 48149 Münster, Germany
Corresponding author: [email protected]
The KATRIN (KArlsruhe TRItium Neutrino) experiment aims to determine the average mass
of the electron antineutrino with a sensitivity of 200meV/c2 by precisely measuring the
electron spectrum of the tritium beta decay near its endpoint. This will be done using a
windowless gaseous molecular tritium source and a spectrometer of MAC-E-Filter type, the
so-called KATRIN main spectrometer.
The KATRIN main spectrometer is the largest ultra-high vacuum chamber in the world. It is
24m long and a diameter of 10m and comprises a volume of 1240m3. It has to be maintained
at a pressure in the 10-11
mbar range for background reasons. This low pressure is reached by a
system of 6 turbo-molecular pumps (Leybold MAG-W-2800) backed by another turbo-
molecular pump system as well as by a huge non-evaporable getter (NEG) pump system
(3000m of stripes SAES St707). The latter should remove the residual hydrogen and other
getterable gases from the spectrometer. A bake-out phase at 300°C had been performed to
further clean the vessel and to activate the NEG pumps before the comissioning of the system
started. The residual gas in the spectrometer can be monitored using a residual gas analyser
(RGA).
During the comissioning phase a severe problem with a vacuum valve occured and therefore
the venting of the main spectrometer was necessarry. The aim was to avoid repeating the
lengthly out-baking and activation process. To keep the activitation of the NEG pump system
a venting with ultra-clean Argon gas has been realized, which allows to open the vacuum
vessel, repair the broken valve and pump down the system again without reactivitating the
getter.
Since commercial Argon is limited in its purity (e.g. purity of Argon 6.0 > 99,9999%), it is
not feasible to vent the spectrometer without saturating the NEP pump by water, oxygen and
other impurities within the Argon gas. Therefore a system has been set up to further clean the
Argon gas using a hot circonium-oxide getter (SAES PS4-MT50-R-2) with a high flow rate of
close to 100 slpm (standard liter per minutes) before it is led into the spectrometer. Such hot
circonium getters are being used to clean noble gases to the ppb level. E.g. at the XENON100
experiment aiming for the direct detection of dark matter particles purities of O2/Xe < 1ppb
have been reached routinely. After venting the KATRIN main spectrometer with this ultra-
clean Argon and pumping it down again a pressure in the 10-11
mbar range was successfully
reached within weeks without baking and re-activating the NEG getters.
This presentation will introduce the vacuum system of the KATRIN experiment and will focus
on providing and venting the KATRIN main specrometer with ultra-clean Argon.
- 54 -
P 15 7-th Symposium on Vacuum based Science and Technology
November 19-21, 2013, Koszalin - Kołobrzeg, Poland
CONSTITUTION AND MICROSTRUCTURE OF MAGNETRON
SPUTTERED Li-Ni-Mn-Co-O THIN FILM CATHODES FOR
LITHIUM-ION BATTERIES AS A FUNCTION OF WORKING
GAS PRESSURE
M. Strafela, J. Fischer, M. Rinke, T. Bergfeldt, H.J. Seifert, S. Ulrich
Karlsruhe Institute of Technology (KIT), Institute for Applied Materials (IAM), Hermann-von-
Helmholtz-Platz 1, 76344 Eggenstein-Leopoldshafen, Germany
Corresponding author: [email protected]
Li-Ni-Mn-Co-O thin film cathodes have been deposited onto Si substrates by non-
reactive r.f. magnetron sputtering from a ceramic Li(Ni1/3Mn1/3Co1/3)O2 target at
various argon working gas pressures from 0.2 to 20 Pa. Coating thickness is about 1.5
µm. Composition and microstructure were investigated comprehensively. The
elemental composition varies with argon gas pressure and was determined by
inductively coupled plasma optical emission spectroscopy (ICP-OES) in combination
with carrier gas hot extraction (CGHE). The microstructure of the films was
characterized by X-ray diffraction (XRD) and by unpolarized micro-Raman
spectroscopy at room temperature. The as-deposited films are nanocrystalline and
show their highest crystallinity in the range between 0.2 Pa to 0.5 Pa and at 7 Pa.
Correlations between process parameter, constitution and microstructure are discussed
in detail.
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7-th Symposium on Vacuum based Science and Technology November 19-21, 2013, Koszalin - Kołobrzeg, Poland P 16
PLASMA OPTICAL EMISSION SPECTROSCOPY (OES) AS
A MONITORING TOOL FOR DEPOSITION OF EXPANDED
AUSTENITE (S-PHASE) LAYERS BY MAGNETRON
SPUTTERING
Tomasz Suszko
1, Vera Jahodowa
2, Witold Gulbiński
1
1Koszalin University of Technology, ul. Śniadeckich 2, 75-453, Koszalin, Poland
2Technical University of Liberec, 1402/2 Studentska, 461 17, Liberec, CZ
Corresponding author:[email protected]
Numerous attempts to improve hardness and wear resistance of austenitic stainless
steel by nitriding or carburizing led to identification of so called S-phase (expanded
austenite).
Presently S-phase is obtained not only by nitriding/carburizing but also by physical
vapour deposition (PVD). The aim of presented work was to verify whether the
deposition can be monitored with use of plasma optical emission spectroscopy (OES).
A set of processes was performed.
The possibility was confirmed. Specific atomic lines were chosen and basic
dependencies between their intensities and other parameters are presented.
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P 17 7-th Symposium on Vacuum based Science and Technology
November 19-21, 2013, Koszalin - Kołobrzeg, Poland
FEM MODELLING OF INTERNAL STRESSES IN PVD
COATED TOOL COMPOSITES
A. Śliwa, J. Mikuła. W. Kwaśny, T.Tański, K. Golombek
Institute of Engineering Materials and Biomaterials, Silesian University of Technology,
Konarskiego St. 18A, 44-100 Gliwice, Poland
Corresponding author. E-mail address: [email protected]
The aim of work is the investigation of the internal stresses in PVD coated
sintered tool composites, determined with use of finite element method in ANSYS
environment. The reason of undertaking the work is necessity of develop the
researches of internal stresses, occurring on the surface of coated materials, as well as
in the adhesion zone where coating meets the substrate, which makes it possible to
draw valuable conclusions concerning engineering process of the advisable structure
and chemical composition of coatings. The investigations were carried out on cutting
tool’s models containing defined zones differing in chemical composition.
Modelled materials was characteristic of chemical composition corresponding
to the HS6-5-2 high-speed steel at the core, reinforced with the WC and TiC type hard
carbide phases with the growing portions of these phases in the outward direction
from the core to the surface and additionally coated with (Ti,Al)N or Ti(C,N)
functionally graded PVD coatings.
Results of determined internal stresses were compared with the experimental
results of stresses calculated using the X-ray sin2ψ method. Obtained results was also
related to other important properties of tool materials, such as microhardness and
adhesion of coatings measured experimentally.
It has been demonstrated, that the presented model meets the initial criteria,
which gives ground to the assumption about its utility for determining the stresses in
coatings as well as in functionally graded sintered materials. The computer simulation
results correlate with the experimental results.
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7-th Symposium on Vacuum based Science and Technology November 19-21, 2013, Koszalin - Kołobrzeg, Poland P 18
TiAlN BASED WEAR RESISTANT COATINGS MODIFIED BY
MOLYBDENUM CO-DEPOSITION
Ł. Tomaszewski 12
, A. Urbanowicz 2, W.K. Gulbiński
2, T. Suszko
2, A. Lewandowski
2,
W. Gulbiński 2
1 Lodz University of Technology, Stefanowskiego 1/15, Łódź
2 Koszalin University of Technology, Śniadeckich 2, Koszalin
Corresponding author: [email protected]
TiAlN based thin films already traditionally belong to the group of wear resistant
coatings which among others, single- or multi-component transition metal nitrides, are
used when an improvement of performance and life time of cutting tools is expected.
Dependent on elemental and phase composition their hardness is in the range 25-
30GPa. Due to Al content in TiAlN coatings their oxidation resistance is higher than
that of traditional TiN layer. It is a reason why they are widely used as a protective
layer deposited at tools for high speed machining. The presence of Al in TiAlN
coatings overcomes the oxidation problems due to the presence of a superficial layer
of Al2O3 formed at high temperature.
Presence of this layer restricts oxygen diffusion and oxidative wear. Simultaneously,
dry friction coefficient versus steel, registered for that type of coatings is high,
reaching 0.9-1.0 at room temperature up to 1.5 at 400oC. Due to high cutting forces it
contributes to undesirable increase of tool temperature and promotes wear processes.
Reduction of friction forces is possible by an appropriate modification of chemical
composition of these coatings by introduction of components which form oxides able
to play a role of solid lubricant. Titanium, vanadium and molybdenum are known to
form a series of oxides belonging the group of so called Magnelli phases, were
ordering of oxygen vacancies leads to formation of easy shear planes. It results in low
friction properties of these oxygen deficient compounds. Also the highest oxides of
vanadium (V2O5) and molybdenum (MoO3), due to their lamellar structure, show
interesting lubricating properties, especially at elevated temperature.
In the course of this study Mo doped TiAlN coatings have been deposited at HSS
substrates. Their structure, adhesion, hardness, friction and wear as well as corrosion
resistance were studied.
- 58 -
P 19 7-th Symposium on Vacuum based Science and Technology
November 19-21, 2013, Koszalin - Kołobrzeg, Poland
XRD, TEM AND HRTEM INVESTIGATIONS OF
NANOSTRUCTURED SUPERHARD TiN/Si3N4 COATINGS
DEPOSITED BY MEANS OF A NOVEL GAS PULSED REACTIVE
MAGNETRON SPUTTERING
Wendler B.G.1, Progalskiy I.F.
1, Moskalewicz T.
2, Pawlak W.
1, Rylski A.
1, Nolbrzak
P.1, Włodarczyk K.
1, Makówka M.
1
1Institute of Materials Science and Engineering, Lodz University of Technology (LUT), 90-924
Lodz, Stefanowskiego St. 1/15 2AGH-UST
University of Technology, Chair of Materials Science and Powder Metallurgy in
Krakow, Mickiewicza Alley 30, 30-059 Krakow
Corresponding author: [email protected]
Beginning from the paper of Kuznetsov et al. in 1999 the High Power Impulse Magnetron
Sputtering (HIPIMS) deposition technique has attracted much interest due to high plasma
ionisation degree and a high uniformity of the deposited layer (no microdroplets). On the
other hand, the deposition rate offered by the method was in general lower than that
encountered in the DC MS one. In 2010-2011 a novel method was proposed – a Gas Pulsed
Magnetron Sputtering (GPMS) one [1,2] - in which the deposition rate of approximately 10
μm/hour in case of superhard TiN/Si3N4 coating on metallic substrates was achieved. In the
first papers the deposition technique and the basic properties of the coating were described. It
was the aim of the present work to investigate more thoroughly the phase composition and the
micro-/nanostructure of the deposited coating with use of XRD, TEM and HRTEM
techniques. As a result it turned out that:
the superhard TiN/Si3N4 coating is composed of 3 phases: 1) δ-TiN with fcc elementary cell;
2) α-Si3N4 with trigonal primitive one and 3) β-Si3N4 of a hexagonal symmetry;
- there is no amorphous phase in the deposited coating;
- there is a strong (111) axial texture of the TiN phase in the coating with the axis of the
texture normal to the substrate surface.
It looks like that the very dynamic deposition conditions during the GPMS process (as, e.g.,
considerable changes of the gas pressure from ~10-3
Pa to several dozen Pa at a frequency of ~
1 Hz) are conducive to nucleation of different phases including the metastable ones as, e.g.,
the β-Si3N4.
Later on the novel method was successfully used for deposition of other coatings as well [3,4].
References:
1. Wendler B. et al.: Hard and superhard nanolaminate and nanocomposite coatings for machine
elements based on Ti6Al4V alloy. Journal of Achievements in Materials and Manufacturing
Engineering 43 (1), 2010, 455-462. ISSN 1734-8412.
2. Wendler B.: Section 8.1 in Functional coatings by CVD and PVD methods. Printing House of the
National Research Institute in Radom. Copyright by Wendler B., TUL, 2011 Lodz, Poland. ISBN
978-83-7789-0001-1.
3. Nowakowska-Langier et al.: The effect of the specific features of two PAPVD methods - Impulse
Plasma Deposition (IPD) and Pulsed Magnetron Sputtering (PMS) - on the structure of Fe-Cu alloy
layers. Applied Surface Science 275 (2012) 14-18.
4. Zdunek K.et al.: Gas injection as a tool for plasma process control during coating deposition.
Surface and Coatings Technology 228 (2013) S367-S373.
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7-th Symposium on Vacuum based Science and Technology November 19-21, 2013, Koszalin - Kołobrzeg, Poland P 20
INVESTIGATION OF THE PROPERTIES OF THIN
AMORPHOUS TA-C COATINGS DEPOSITED BY COMBINED
DC IMPULSE VACUUM-ARC METHOD USING THE LINEAR
VENETIAN BLIND PLASMA FILTER
V. Zavaleyev, J. Walkowicz
Institute of Technology and Education, Koszalin University of Technology,
ul. Sniadeckich 2, 75-453 Koszalin, Poland
Vacuum-Arc Deposition is one of physical vapour deposition (PVD)
techniques, which are most often used in the industrial practice. The rapid
development of vacuum-arc methods in the last decade has led to the emergence of
new combined methods of deposition, one of which is DC vacuum-arc with
superimposed high-current arc pulses. To date, much of the research on the deposition
of thin amorphous ta-C coatings is based on the use of different designs of magnetic
filters based on bent solenoids. The use of electromagnetic linear Venetian blind
plasma filter for deposition of thin ta-C coatings opens up new possibilities for the
design of such filters. The advantage of this filter design is simplicity of operation and
possibility of the device modernization without additional structural changes as well
as without reducing the useful volume within the vacuum chamber and the deposition
zone. We have studied amorphous ta-C coatings of the thickness from 40 to 270 nm,
deposited by combined DC impulse vacuum-arc method using water-cooled
electromagnetic linear Venetian blind plasma filter. The carried out investigations of
internal stresses, adhesion, hardness and Young's modulus of deposited amorphous ta-
C coatings show an almost linear dependency on the thickness of the studied coatings.
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- 61 -
7-th Symposium on Vacuum based Science and Technology November 19-21, 2013, Koszalin - Kołobrzeg, Poland Authors
Abadias G., A. 13
Gnaser H. , 23
Baldsiefen G. 35
Gogler S. 44
Balzer M. 14
Golombek K. 56
Baranowska J. 39
Greczynski G. 31
Berg S. 21
GreeneJ.E. 31
Bergfeldt T. 54
Gulbiński W. 55, 57
Bergmann A. 21
Gulbiński W.K. 57
Bergner U. 20
Gunnarsson R. 30
Bernsmann F. 28
Gutsch S. 23
Beweries T. 29
Hansen S. 29
Bilewicz M. 47
Helmersson U. 30
Bock W. 23
Huhmann Ch. 34
Bolz S. 31
Hultman L. 31
Bornholdt S. 17
Jaglarz J. 24
Brenning N. 30
Jahodowa V. 55
Brodyanski A. 50
Janson U. 12
Brown E. 34
Jaouen C. 13
Brüser V. 29, 51
Jensen J. 31
Budner B. 44
Jousten K. 22, 33
Busch H. 28
Junge H. 29
Bussiahn R. 15
Kalisz M. 44
Caffrey D. 40
Kamińska A. 25, 45, 46
Castellucci M. 28
Kappl H. 14
Clausner A. 26
Kerkhof T. 19
Colin J.J. 13
Kersten H. 17
Cristescu I. 34
Kölker W. 31, 32
Czerwosz E. 25, 45, 46
Kopnarski M. 23, 50
Danneil F. 41
Koprowska J. 36, 43
Dłużewski P. 25, 46
Kowalska E. 45
Dobruchowska E. 36, 43
Kozłowski M. 25, 45, 46
Doros W. 48
Krawczyk S. 46
Fenker M. 14
Kruth A. 29, 51
Fieguth A. 34
Kwaśny W. 56
Fillon A., 13
Labisz K. 47
Fischer J. 54
Lattemann M. 52
Fleischer K. 40
Laube N. 35
Fryska S. 39
Leiste H. 41
Gilewicz A. 37
Lemmer O. 31, 32
- 62 -
Authors 7-th Symposium on Vacuum based Science and Technology
November 19-21, 2013, Koszalin - Kołobrzeg, Poland
Lewandowski A. 57
Schiffers Ch. 31, 32
Leyendecker T. 32
Schlarb A. 50
Lin L. 50
Schneider V. 17
Lösch J. 23
Seemann K. 41
Lu J. 31
Seifert H.J. 54
Makówka M. 58
Sendzik A. 21
Marszałek K. 24, 48
Shvets I.V. 40
Marszałek M. 24
Sobczak K. 45
Meyer J. 50
Söderström D. 30
Michel A. 13
Strafela M. 54
Mierczyk J. 44
Stryhal Z. 21
Mikuła J. 56
Stüber M. 41, 52
Mitterer C. 11
Suksut B. 50
Moskalewicz T. 58
Suszko T. 55, 57
Müller S. 29
Szparaga Ł. 27
Murra M. 34
Szymanska M. 44
Myśliński P. 49
Śliwa A. 56
Niedner-Schatteburg G. 50
Tański T. 47, 56
Nolbrzak P. 58
Tomaszewski Ł. 57
Olik R. 27
Trottenberg T. 17
Passlack S. 50
Ulrich S. 41, 52, 54
Pawlak W. 58
Urbanowicz A. 57
Peglow S. 29, 51
von Woedtke Th. 15
Perzanowski M. 24
Wahl .M. 23
Petrov I. 31
Walkowicz J. 59
Pilch I. 30
Warcholiński B. 37
Pohl M.-M. 29
Weinheimer Ch. 34
Progalskiy I.F. 58
Welle A. 41
Radomska J. 46
Weltmann K.-D. 15, 29
Ratajski J. 27
Wendler B.G. 58
Reszka K. 36, 43
Winkowski P. 24
Reuscher B. 50
Witkowski B. 45
Richter F. 21, 26
Włodarczyk K. 58
Rinke M. 52, 54
Zacharias M. 23
Rockstroh N. 29
Zavaleyev V. 59
Rosendahl S. 34, 53
Zdunek K. 18
Rutscher J. 17
Zhou S. 16
Rylski A. 58
Ziebert C. 52
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7-th Symposium on Vacuum based Science and Technology November 19-21, 2013, Koszalin - Kołobrzeg, Poland Notes
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Notes 7-th Symposium on Vacuum based Science and Technology
November 19-21, 2013, Koszalin - Kołobrzeg, Poland
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7-th Symposium on Vacuum based Science and Technology November 19-21, 2013, Koszalin - Kołobrzeg, Poland Notes
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Notes 7-th Symposium on Vacuum based Science and Technology
November 19-21, 2013, Koszalin - Kołobrzeg, Poland
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7-th Symposium on Vacuum based Science and Technology November 19-21, 2013, Koszalin - Kołobrzeg, Poland Notes
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Notes 7-th Symposium on Vacuum based Science and Technology
November 19-21, 2013, Koszalin - Kołobrzeg, Poland
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7-th Symposium on Vacuum based Science and Technology November 19-21, 2013, Koszalin - Kołobrzeg, Poland Notes
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Notes 7-th Symposium on Vacuum based Science and Technology
November 19-21, 2013, Koszalin - Kołobrzeg, Poland
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7-th Symposium on Vacuum based Science and Technology November 19-21, 2013, Koszalin - Kołobrzeg, Poland Notes
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Notes 7-th Symposium on Vacuum based Science and Technology
November 19-21, 2013, Koszalin - Kołobrzeg, Poland