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Research Project Sputtering Deposition

Gruppe UHV Lab

 


Polycrystalline sputtered coatings are essential for everyday life today: they are found as anti-reflection coatings on eyeglass lenses, active layers in sensor chips, or hard coatings to extend the life of tools and medical implants.
Depending on the application of the coating, different material properties are required which are directly related to its microstructure. However, the microstructure produced during the film formation is still only predictable to a limited extent.
In situ X-ray measurements (=X-ray measurements during film growth) can help: they provide direct insight into the formation of the microstructure during the sputtering process.

 

Objectives

The main aim of our research is advance the understanding of structure formation in sputter deposited thin films and nanostructures. This includes several tasks:

  • Development of synchrotron-based methods for monitoring the interface formation, crystal growth, and phase formation during deposition
  • Application of these methods to various material systems and structures
  • Derivation of growth models
  • Examination of the interplay between microstructure and microscopic material properties
  • Application of research results: production of specific layers with the desired properties

Methods

  • Reactive and non-reactive rf and dc magnetron sputtering
  • In situ X-ray diffraction and reflectivity experiments during thin film growth
  • Scattering methods (X-ray diffraction, pole figure measurements, X-ray reflectivity, RHEED)
  • Spectroscopic methods (XPS, EXAFS, XANES)
  • Microscopy (AFM, TEM, optical microscopy)

Model systems

  • Hard coating materials based on nitrides and carbides of transition metals (e.g. CrAlN, VN)
  • Silicides and Germanides (e.g. MoSi, WSi)

 

 

Team
Portrait title name function e-mail
Sunil Kotapati PhD student sunil kotapatiGvd1∂kit edu
Bärbel Krause Dr. Head of UHV Analysis Lab and Research Project Sputtering Depostition baerbel krauseCxm5∂kit edu

Former Members
name function
Phd student  
bachelor student Einfuss der Sputtergeometrie auf die Mikrostruktur lateral ausgedehnter Proben (2015)
master student (univ. Poitiers, France), Growth and Characterization of Sputter-Deposited Thin Films (2015)
bachelor student Wachstum und Analyse von CrAlN dünnen Schichten (2014)
PhD student Monitoring the film formation during sputter deposition of vanadium carbide by in situ X-ray reflectivity measurements (2014)
bachelor student Einuss des Depositionswinkels auf die Strukturbildung von Vanadiumcarbid während des Magnetronsputterns (2013)
PhD student Microstructure Analysis of (V,Al)(C,N) Hard Coatings by X-Ray Diffraction and X-Ray Absorption Fine Structure Spectroscopy (2012)
bachelor student Simulation von Wachstumsprozessen während des Magnetron-Sputterns (2012)

Chamber

In-situ experiments during film formation require very special instrumentation, fulfilling the demands of both the X-ray experiment and the film formation process. The heart of our experiment is a portable, modular growth chamber with the following main features:

  • RF and DC magnetron sputter deposition with target diameter up to 3"
  • Multilayer growth and alloy codeposition
  • Variable deposition angle
  • Fully automated deposition process and process data logging
  • Two beryllium windows with a large angular range for X-ray measurements
  • Compatible with simultaneous optical stress monitoring

The sputtering chamber can be docked to the UHV cluster in the UHV analysis laboratory. It can also be installed at various stations at ANKA for in situ X-ray experiments. For detailed information on the sputtering chamber see Krause et al., J. Synchr. Rad.19 (2012), 216-222.

 

 

Fig: Sputter chamber in codeposition geometry, installed at the MPI beamline of ANKA. On top of the chamber, a setup for simultaneous optical stress measurement (G. Abadias, Univ. Poitiers) is mounted.

Motivation

 

Structure formation during growth: crystalline structure

Projekt 1
In situ powder diffraction experiments during the RF and DC magnetron sputtering of transition metal carbides and nitrides.

 

The crystalline microstructure of a coating greatly depends on the growth conditions (e.g. plasma, substrate temperature) and the layer thickness. In situ diffraction experiments give insight into the crystalline phase, crystallite size, strain and texture during film deposition. Growth models based thereon allow selective adjustment of the microstructure.
In-situ reflectivity measurements: observation of growth

 

Projekt 2
Observation of the change in layer material distribution, which depends on the growth parameters and time.

 

The microstructure of hard coatings can vary widely, from amorphous to crystalline, from homogenous to porous. In situ powder diffraction only gives insight into the crystalline microstructure, while in-situ reflectivity measurements give information on all layers.

Microstructure and geometrical effects
Projekt 3

In situ studies of inclined crystallites, zigzag structures and biaxially oriented layers.



 

 

Many material properties, such as refractive index, hardness, and magnetic properties are dependent on the crystallite orientation. Epitaxial, highly oriented layers are very expensive compared to polycrystalline films. The orientation of polycrystalline films, however, can be significantly improved by appropriate deposition geometries.

Effect of the chemical composition on microstructure

Projekt 4

Study of the crystalline and amorphous phases in simultaneously deposited TM-Al-C-N (TM = transition metal)

 

Materials composed of several chemical elements offer many possibilities to optimize the microstructure for specific applications. Depending on the chemical composition and growth conditions, both metastable mixed phases and nanocomposites of coexisting stable phases can form.
Publications
Title Author Source Date Link

A. Seiler, S. Ibrahimkutty, P. Wochner, R. Pradip, O Waller, B. Krause, A. Plech, T. Baumbach, M. Fiederle, S. Stankov

J. Phys. Chem. C 2016, 120, 7365−7372

2016

M. Kaufholz, B. Krause, S. Kotapati, M. Köhl, M.F. Mantilla, M. Stüber, S. Ulrich, R. Schneider, D. Gerthsen and T. Baumbach

J. Synchrotron Rad. (2015). 22, 76–85

2015

B. Krause, M. Kaufholz, S. Kotapati, R. Schneider, E.Müller, D. Gerthsen, P.Wochner, T. Baumbach

Surface & Coatings Technology 277 (2015) 52–57

2015
O. Bauder, A. Seiler, S. Ibrahimkutty, D.G. Merkel, B. Krause, R. Rüffer, T. Baumbach, S. Stankov Journal of Crystal Growth 400, 61-66 2014

PDF

A. Cecilia, V. Jary, M. Nikl, E. Mihokova, D. Hänschke, E. Hamann, P.-A. Douissard, A. Rack, T. Martin, B. Krause,T. Baumbach, M. Fiederle 

Radiation Measurements 62, 28–34 2014 PDF

B. Krause, B. Miljevic, T. Aschenbrenner, E. Piskorska-Hommel, C. Tessarek, M. Barchuk, G. Buth, R. Donfeu Tchana, S. Figge, J. Gutowski, D. Hänschke, J. Kalden, T. Laurus, S. Lazarev, R. Magalhaes-Paniago, K. Sebald, A. Wolska, D. Hommel, J. Falta, V. Holý, T. Baumbach 

Journal of Alloys and Compounds 585, 572-579 

2014 PDF

B. Krause, S. Darma, M. Kaufholz, S. Mangold, S. Doyle, S. Ulrich, H. Leiste, M. Stüber, T. Baumbach 

Journal of Applied Crystallography 46, 1064-1075 

2013 PDF

T. Marszalek, A. Nosal, R. Pfattner, J. Jung, J, S. Kotarba, M. Mas-Torrent, B. Krause, J. Veciana, M. Gazicki-Lipman, C. Crickert, G. Schmidt, C. Rovira, J. Ulanski 

Organic Electronics 13 (1) 121-128 

2012 PDF

D. Saez de Jauregui, T. Baumbach, S. Casalbuoni, A. Grau, S. Gerstl, M. Hagelstein, C. Heske, T. Holubek, B. Krause, A. Seiler, S. Stankov, L. Weinhardt, C. Boffo, C. Antoine, Y. Boudigou 

Conference proceedings of the IPAC12, 723-725 

2012 PDF

B. Krause, S. Darma, M. Kaufholz, H. Gräfe, S. Ulrich, M. Mantilla, R. Weigel, S. Rembold, T. Baumbach 

Journal of Synchrotron Radiation 19, 216-222 

2012 PDF

M. Barchuk, V. Holý, B. Miljević, B. Krause, T. Baumbach 

Applied Physics Letters 98 (2), 021912-1-3 

2011 PDF

M. Barchuk, V. Holý, B. Miljević, B. Krause, T. Baumbach, J. Hertkorn, F. Scholz 

Journal of Applied Physics 108 (4), 043521 

2010

C. Mocuta, K. Mundboth, J. Stangl, B. Krause, A. Malachias, T. Scheller, T. Cornelius, R. Paniago, A. Diaz, M. Rodrigues, J. Chevrier,O. Dhez, T. H. Metzger, G. Bauer, A. Barbier,A. V. Ramos, M. J. Guittet, J. B. Moussy, S. Stanescu, R. Mattana,C. Deranlot, F. Petroff 

Revue de Métallurgie 107 (10-11), 433-439 

2010

A. Malachias, C. Deneke, B. Krause, C. Mocuta, S. Kiravittaya, T. H. Metzger, O. G. Schmidt 

Physical Review B 79 (3), 035301 

2009

C. Reich, M. R. Horton, B. Krause, A. P. Gast, J. O. Rädler, B. Nickel 

Biophysical Journal 95 (2), 657-668 

2008

L. Wang, A. Rastelli, S. Kiravittaya, R. Songmuang, O. G. Schmidt, B. Krause, T. H. Metzger 

Nanoscale Research Letters 1 (1), 74-78 

2006

B. Krause, C. Mocuta, T. H. Metzger, C. Deneke, O. G. Schmidt 

Physical Review Letters 96 (16), 165502 

2006

P. Miskiewicz, M. Mas-Torrent, J. Jung, S. Kotarba, I. Glowacki, E. Gomar-Nadal, D. B. Amabilino, J. Veciana, B. Krause, D. Carbone, C. Rovira, J. Ulanski 

Chemistry of Materials 18 (20), 4724-4729 

2006

M. B. Hochrein, C. Reich, B. Krause, J. O. Rädler, B. Nickel 

Langmuir 22 (2), 538-545 

2006

O. Caha, P. Mikulik, J. Novak, V. Holy, S. C. Moss, A. Norman, A. Mascarenhas, J. L. Reno, B. Krause 

Physical Review B 72 (3), 035313 

2005

E. Piskorska, V. Holy, M. Siebert, B. Krause B, T. H. Metzger. T. Schmidt, J. Falta, T. Yamaguchi, D. Hommel 

Physica Status Solidi C - Current Topics in Solid State Physics 3 (6), 1662–1666 

2005

B. Krause, T. H. Metzger, A. Rastelli, R. Songmuang, S. Kiravittaya, O. G. Schmidt 

Physical Review B 72 (8), 085339 

2005

C. Reich, M. B. Hochrein, B. Krause, B. Nickel 

Review of Scientific Instruments 76 (9), 095103 

2005

B. Krause, A. C. Dürr, F. Schreiber, H. Dosch, O. H. Seeck 

Surface Science 572 (2-3), 385-395 

2004

B. Krause, F. Schreiber, H. Dosch, A. Pimpinelli, O. H. Seeck 

Europhysics Letters 65 (3), 372-378 

2004

B. Krause, A. C. Dürr, F. Schreiber, H. Dosch, O. H. Seeck 

Journal of Chemical Physics 119 (6), 3429-3435 

2003

B. Krause, A. C. Dürr, K. Ritley, F. Schreiber, H. Dosch, D. Smilgies 

Physical Review B 66 (23), 235404 

2002

A. C. Dürr, F. Schreiber, M. Münch, N. Karl, B. Krause, V. Kruppa, H. Dosch 

Applied Physics Letters 81 (12), 2276-2278 

2002

B. Krause, A. C. Dürr, K. A. Ritley, F. Schreiber, H. Dosch, D. Smilgies 

Applied Surface Science 175, 332-336 

2001

K. A. Ritley, B. Krause, F. Schreiber, H. Dosch 

Review of Scientific Instruments 72 (2), 1453-1457 

2001

B. Krause, K. Theis-Bröhl 

Journal of Physics - Condensed Matter 12 (22), 4675-4686 

2000