7-th Symposium on Vacuum based Science and...

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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

Transcript of 7-th Symposium on Vacuum based Science and...

Page 1: 7-th Symposium on Vacuum based Science and Technologyitie.dev.tu.koszalin.pl/svbst2013/images/7-th_SVBST_Kolobrzeg_2013... · 7-th Symposium on Vacuum based Science and Technology

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

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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

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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

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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

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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

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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

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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

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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

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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

[email protected]

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.

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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.

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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.

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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

[email protected]

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.

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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.

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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.

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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.

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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.

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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.

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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.

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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.

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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.

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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

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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.

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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.

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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.

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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.

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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.

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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

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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

[email protected]

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.

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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

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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

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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

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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

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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.

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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

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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.

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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.

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Fig. 1: Schematic representation of this work.

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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

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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.

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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.

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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.

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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.

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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.

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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.

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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.

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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.

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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.

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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.

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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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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

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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