ISO 9001 certified © JOANNEUM RESEARCH Forschungsgesellschaft mbH Laser Center Leoben SLONANO 2007...

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ISO 9001 certified © JOANNEUM RESEARCH Forschungsgesellschaft mbH Laser Center Leoben SLONANO 2007 10-12 October 2007, Ljubljana, Slovenia The Austrian and Styrian activities in nano Surface Engineering: Development of nanostructured coatings for the design of multifunctional surfaces Wolfgang Waldhauser Laser Center Leoben [email protected]
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Transcript of ISO 9001 certified © JOANNEUM RESEARCH Forschungsgesellschaft mbH Laser Center Leoben SLONANO 2007...

Page 1: ISO 9001 certified © JOANNEUM RESEARCH Forschungsgesellschaft mbH Laser Center Leoben SLONANO 2007 10-12 October 2007, Ljubljana, Slovenia The Austrian.

ISO

9001

cert

ified

© JOANNEUM RESEARCH Forschungsgesellschaft mbH

Laser Center Leoben

SLONANO 200710-12 October 2007, Ljubljana, Slovenia

The Austrian and Styrian activities in nano Surface Engineering:

Development of nanostructured coatings for the design of multifunctional surfaces

Wolfgang Waldhauser

Laser Center Leoben

[email protected]

Page 2: ISO 9001 certified © JOANNEUM RESEARCH Forschungsgesellschaft mbH Laser Center Leoben SLONANO 2007 10-12 October 2007, Ljubljana, Slovenia The Austrian.

ISO

9001

cert

ified

© JOANNEUM RESEARCH Forschungsgesellschaft mbH

Laser Center Leoben

Outline

The Austrian NANO Initiative Research Project Cluster NANOCOAT

The Styrian Activities in Nanotechnology nanoSurface Engineering Center Leoben (nSEC)

Research Activities at JOANNEUM RESEARCH Collaboration with Jozef Stefan Institute

Conclusions

ISO

9001

cert

ified

Laser Center Leoben

Page 3: ISO 9001 certified © JOANNEUM RESEARCH Forschungsgesellschaft mbH Laser Center Leoben SLONANO 2007 10-12 October 2007, Ljubljana, Slovenia The Austrian.

ISO

9001

cert

ified

© JOANNEUM RESEARCH Forschungsgesellschaft mbH

Laser Center Leoben

Austrian NANO Initiative

A multi-annual funding programme for Nanoscale Sciences and Nanotechnologies in Austria

Coordination of NANO measures on the national and regional levels

Supported by several Ministries, Federal provinces and Funding institutions

The programme is managed by FFG (Austrian Research Promotion Agency) on behalf of the BMVIT (Federal Ministry for Transport, Innovation and Technology)

ISO

9001

cert

ified

Laser Center Leoben

Page 4: ISO 9001 certified © JOANNEUM RESEARCH Forschungsgesellschaft mbH Laser Center Leoben SLONANO 2007 10-12 October 2007, Ljubljana, Slovenia The Austrian.

ISO

9001

cert

ified

© JOANNEUM RESEARCH Forschungsgesellschaft mbH

Laser Center Leoben

Objectives of the Austrian NANO Initiative 1/2

Orientation and the structure have been developed jointly with scientists, entrepreneurs and intermediaries

Strengthening and networking the Austrian NANO players in science and industry

Building critical masses for positioning the Austrian NANO players in international competition

Supported by several Ministries, Federal provinces and Funding institutions

Using NANO for industry and society by developing research results further and implementing them

ISO

9001

cert

ified

Laser Center Leoben

Page 5: ISO 9001 certified © JOANNEUM RESEARCH Forschungsgesellschaft mbH Laser Center Leoben SLONANO 2007 10-12 October 2007, Ljubljana, Slovenia The Austrian.

ISO

9001

cert

ified

© JOANNEUM RESEARCH Forschungsgesellschaft mbH

Laser Center Leoben

Objectives of the Austrian NANO Initiative 2/2

Providing a sufficient number of qualified employees through education and training

Building and expanding infrastructure as well as building centres in basic research and in application-oriented special fields

ISO

9001

cert

ified

Laser Center Leoben

Page 6: ISO 9001 certified © JOANNEUM RESEARCH Forschungsgesellschaft mbH Laser Center Leoben SLONANO 2007 10-12 October 2007, Ljubljana, Slovenia The Austrian.

ISO

9001

cert

ified

© JOANNEUM RESEARCH Forschungsgesellschaft mbH

Laser Center Leoben

Austrian NANO Initiative

Target GroupsNANO players from University and non-University research, as well as enterprises located in Austria

International partners are welcome to participate in all Programme Action Lines

Public BudgetFor 2004 to 2006: 35 MEuro

For 2007: 12 MEuro

ISO

9001

cert

ified

Laser Center Leoben

Page 7: ISO 9001 certified © JOANNEUM RESEARCH Forschungsgesellschaft mbH Laser Center Leoben SLONANO 2007 10-12 October 2007, Ljubljana, Slovenia The Austrian.

ISO

9001

cert

ified

© JOANNEUM RESEARCH Forschungsgesellschaft mbH

Laser Center Leoben

Programme Action Lines

PL1 Research and Technology Development Project Clusters

PL2 Networks and Confidence Building

PL3 Training and Education Measures

PL4 Accompanying Measures

Transnational Projects

Individual Projects

ISO

9001

cert

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Laser Center Leoben

Page 8: ISO 9001 certified © JOANNEUM RESEARCH Forschungsgesellschaft mbH Laser Center Leoben SLONANO 2007 10-12 October 2007, Ljubljana, Slovenia The Austrian.

ISO

9001

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ified

© JOANNEUM RESEARCH Forschungsgesellschaft mbH

Laser Center Leoben

Partners of the Austrian NANO Initiative Austria Business Service GmbH (aws)

Austrian Research Promotion Agency (FFG)

Federal Ministry for Education, Science and Culture (BMBWK)

Federal Ministry for Transport, Innovation and Technology (BMVIT)

Federal Ministry of Economics and Labour (BMWA)

Austrian Science Fund (FWF)

Office of the Austrian Council for Research and Technology Development

Federal Province of Carinthia

Federal Province of Lower Austria

Federal Province of Upper Austria

Federal Province of Salzburg

Federal Province of Styria

Federal Province of Tyrol

Federal Province of Vorarlberg

City of Vienna

Page 9: ISO 9001 certified © JOANNEUM RESEARCH Forschungsgesellschaft mbH Laser Center Leoben SLONANO 2007 10-12 October 2007, Ljubljana, Slovenia The Austrian.

ISO

9001

cert

ified

© JOANNEUM RESEARCH Forschungsgesellschaft mbH

Laser Center Leoben

PL1 RTD project clusters

NaDiNe “Nano Diamond Network”

NANO-HEALTH “Nanostructured Material for Drug Targeting, Release and Imaging”

ISOTEC “Integrated Organic Sensor and Optoelectronics Technologies”

NANOCOAT “Development of Nanostuctured Coatings for the Design of Multifunctional Surfaces”

NSI "Nanostructured Surfaces and Interfaces"

Page 10: ISO 9001 certified © JOANNEUM RESEARCH Forschungsgesellschaft mbH Laser Center Leoben SLONANO 2007 10-12 October 2007, Ljubljana, Slovenia The Austrian.

ISO

9001

cert

ified

© JOANNEUM RESEARCH Forschungsgesellschaft mbH

Laser Center Leoben

PL2 Networks

The Austrian NANO Forum is the information- and communication platform for all Austrian NANO Experts

The existing Austrian NANO Networks: NANONET-STYRIA

MNA Micro@Nano-Fabrication-Austria Networking

w-Inn West Austrian Initiative for NANO Networking

Page 11: ISO 9001 certified © JOANNEUM RESEARCH Forschungsgesellschaft mbH Laser Center Leoben SLONANO 2007 10-12 October 2007, Ljubljana, Slovenia The Austrian.

ISO

9001

cert

ified

© JOANNEUM RESEARCH Forschungsgesellschaft mbH

Laser Center Leoben

Transnational RTD Projects

MNT ERA-Net Call 2007 (Call is closed now!) The European Network MNT ERA-Net opened its second call for transnational,

product oriented research projects in the field of Micro and Nano Technologies (MNT)

ERA-SPOT Call 2007 (Deadline for pre-proposal 26th November 2007) The European Network ERA-SPOT "Strengthening Photonics and Optical

Technologies for Europe" is a multi-annual initiative comprising representatives of photonic and optical technologies related funding programmes in six EU Member States

Page 12: ISO 9001 certified © JOANNEUM RESEARCH Forschungsgesellschaft mbH Laser Center Leoben SLONANO 2007 10-12 October 2007, Ljubljana, Slovenia The Austrian.

RPC NANOCOAT

RPC NANOCOATDevelopment of Nanostructured Coatings

for the

Design of Multifunctional Surfaces

2005 20122007 2009 201120102006 2008

Call 1RPC Start

Call 2BI

project added

Call 3BI, BII projects

prolonged,BII projects

added

Page 13: ISO 9001 certified © JOANNEUM RESEARCH Forschungsgesellschaft mbH Laser Center Leoben SLONANO 2007 10-12 October 2007, Ljubljana, Slovenia The Austrian.

RPC NANOCOATMontanuniversität Leoben Prof. Christian Mitterer

Karl Franzens Universität Graz Prof. Falko Netzer

Technische Universität Wien Prof. Josef Redinger

Universität Wien Prof. Raimund Podloucky

Österreichische Akademie der Wissenschaften Prof. Gerhard DehmProf. Reinhard PippanDr. Jozef Keckes

Materials Center Leoben Forschung GmbH Prof. Reinhold EbnerDr. Mariann Lovonyak

Joanneum Research Forschungsgesellschaft mbH Dr. Wolfgang WaldhauserDr. Jürgen Lackner

BOEHLERIT GmbH & Co KG Dr. Arno Köpf

Rübig GmbH & Co KG Dipl.-Ing. Thomas Müller

IonBond Austria GmbH Ing. Johann Kiefer

Böhler Edelstahl GmbH Dr. Devrim Caliskanoglu

SECAR Technologie GmbH Karl-Heinz Semlitsch

NANOCOAT Consortium

Page 14: ISO 9001 certified © JOANNEUM RESEARCH Forschungsgesellschaft mbH Laser Center Leoben SLONANO 2007 10-12 October 2007, Ljubljana, Slovenia The Austrian.

RPC NANOCOAT

Nanoscale surface science & technology is a fast growing scientific branch (rapidly increasing number of publications)

Nanoscale surface technology is seen as an important economic factor in Europe, and explicitly addressed in FP6 and FP7, in USA and Japan

Nanoscale Science & Technology is also named as Key Target by the Austrian Research Council and the County of Styria

Role in science and technology:

Why nano-surfaces?

State of the Art

Page 15: ISO 9001 certified © JOANNEUM RESEARCH Forschungsgesellschaft mbH Laser Center Leoben SLONANO 2007 10-12 October 2007, Ljubljana, Slovenia The Austrian.

RPC NANOCOAT

                         

                    

Lotus flower effect

Easy-to-clean wear-resistant surfaces(multi-functional properties)

Easy-to-clean wear-resistant surfaces(multi-functional properties)

State of the Art: Examples

Superhard and tough nanostructured coatings

Page 16: ISO 9001 certified © JOANNEUM RESEARCH Forschungsgesellschaft mbH Laser Center Leoben SLONANO 2007 10-12 October 2007, Ljubljana, Slovenia The Austrian.

RPC NANOCOAT

Self-adaptive low-friction coatingsSelf-adaptive low-friction coatings

State of the Art: Examples

Solidified V2O5 film on top of the AlCrVN coating

Al1-xCrxN

AlCrVN

Arc evaporated AlCrN and AlCrVN coatingsArc evaporated AlCrN and AlCrVN coatings

T=700°C

Page 17: ISO 9001 certified © JOANNEUM RESEARCH Forschungsgesellschaft mbH Laser Center Leoben SLONANO 2007 10-12 October 2007, Ljubljana, Slovenia The Austrian.

RPC NANOCOAT

Key technologies in nanoscalesurface science & technologyKey technologies in nanoscalesurface science & technology

State of the Art

StructuringVacuum- /plasma-

technologies

• Evaporation• Sputtering• Arc Evaporation• Pulsed Laser Deposition

Coating

Chemicaltechnologies

• organic• inorganic

• electrochemical• colloidal

CVD PACVD

Self organisation

Lithographictechnologies

• UV• Electron• Ion

Ion beamtechnologies

Modification• Alloying• Mixing

Structuring• Ion beam machining

FIB

Available to RPC

Page 18: ISO 9001 certified © JOANNEUM RESEARCH Forschungsgesellschaft mbH Laser Center Leoben SLONANO 2007 10-12 October 2007, Ljubljana, Slovenia The Austrian.

RPC NANOCOAT Goals: Scientific and Technological

Fundamental understanding of surface response on all length scales in the targeted areas

• Tools• Engineering Components• Functional Components

Fundamental understanding of surface response on all length scales in the targeted areas

• Tools• Engineering Components• Functional Components

Design rules and strategies for multifunctional surfacesDesign rules and strategies for multifunctional surfaces

Technological realisation of multifunctional surfacesTechnological realisation of multifunctional surfaces

Transfer of results to industrial useTransfer of results to industrial use

Page 19: ISO 9001 certified © JOANNEUM RESEARCH Forschungsgesellschaft mbH Laser Center Leoben SLONANO 2007 10-12 October 2007, Ljubljana, Slovenia The Austrian.

RPC NANOCOAT

Env

ironm

ent

indi

catio

n

Str

ain

indi

catio

n

Col

our

chan

ges

Col

our

mec

hani

sms

Mu

ltif

un

ctio

nal

Co

atin

gs/

Su

rfac

esM

ult

ifu

nct

ion

al C

oat

ing

s/S

urf

aces

Tribolog. coatingsTribolog. coatings

Chemically resistant coatingsChemically resistant coatings

Sensor coatingsSensor coatings

2005 20122007 2009 201120102006 2008

Coatings with designed optical propertiesCoatings with designed optical properties

Mec

hani

cal

stab

ility

The

rmal

stab

ility

Oxidation

kinetics

Controlled

reaction

Controlled

rinterface

formation

Self-

healing

Sel

f-ha

rden

ing

Sel

f-lu

bric

atio

n

Sel

f-cl

eani

ng

Sel

f-re

pair

Tem

pera

ture

indi

catio

n

Mechanical

stability

Therm

al

stability

Therm

al

changes

Stress

changes

Environm

ental

changes

Active coatingsActive coatings

Coloured drycutting tool

Anti-adhesivemould

Low-frictionvalve needle

Colour-changing tool

Self-repairingturbine blade

MEMS

Anti-adhesivefood cutter

Goals: Roadmap

Page 20: ISO 9001 certified © JOANNEUM RESEARCH Forschungsgesellschaft mbH Laser Center Leoben SLONANO 2007 10-12 October 2007, Ljubljana, Slovenia The Austrian.

RPC NANOCOAT The projects of the RPC

BI.1 StressDesignBI.2 LowFrictionCoatingsBI.3 OxideNanolayersBI.4 NanoInterfacesBII.1 AntiadhesiveLayersBII.2 ColouredCoatingsBII.3 PolymerMetalCoatingBII.4 HIPIMSBII.5 LowTempPACVD

Year 1 (02/2005 - 01/2006) Call 2004 (Call 1)Year 2 (02/2006 - 01/2007) Call 2005 (Call 2)Year 3 (02/2007 - 01/2008) Call 2005 (Call 3)Year 4 (02/2008 - 01/2009)Year 5 (02/2009 - 01/2010)Year 6 (02/2110 - 01/2011)Year 7 (02/2011 - 01/2012)Year 8 (02/2012 - 01/2013)

Year 8Project: Year 5 Year 6 Year 7Year 1 Year 2 Year 3 Year 4

October 2007

Running projects

Page 21: ISO 9001 certified © JOANNEUM RESEARCH Forschungsgesellschaft mbH Laser Center Leoben SLONANO 2007 10-12 October 2007, Ljubljana, Slovenia The Austrian.

RPC NANOCOAT The projects of the RPC

Basic Research (BI)

BI.1: StressDesign

▬ Engineering of residual stresses and nanostructure in thermally-cycled coatings on various substrates.

▬ Goals:

To deeply understand the thermally-induced degradation phenomena

To develop hard coatings with significantly improved thermal fatigue behaviour

Page 22: ISO 9001 certified © JOANNEUM RESEARCH Forschungsgesellschaft mbH Laser Center Leoben SLONANO 2007 10-12 October 2007, Ljubljana, Slovenia The Austrian.

RPC NANOCOAT The projects of the RPC

BI.2: LowFrictionCoatings

▬ Development of a new class of medium-temperature to high-temperature low-friction coatings, which are based on Magnéli-Phases.

▬ Approach:

To apply oxides of the type MenO2n-1 (Me=Mo, Ti, V, W), which exhibit easy deformable crystallographic shear planes that are responsible for low friction coefficients in some of these oxides.

BI.3: OxideNanolayers

▬ To study the oxidation behaviour of multiphase hard coatings

▬ To investigate the formation of oxide nanolayers on functional hard coating surfaces with atomic precision resolved in time and space

Page 23: ISO 9001 certified © JOANNEUM RESEARCH Forschungsgesellschaft mbH Laser Center Leoben SLONANO 2007 10-12 October 2007, Ljubljana, Slovenia The Austrian.

RPC NANOCOAT The projects of the RPC

BI.4: NanoInterfaces

▬ To investigate interfaces and surfaces as well as diffusion and oxidation processes in multilayers and superlattices by combining modelling and experimental approaches

▬ To develop a fundamental understanding of the atomic processes controlling the functionally of self-lubricating TiN / VN multilayers

Page 24: ISO 9001 certified © JOANNEUM RESEARCH Forschungsgesellschaft mbH Laser Center Leoben SLONANO 2007 10-12 October 2007, Ljubljana, Slovenia The Austrian.

RPC NANOCOAT The projects of the RPC

BI.5: FlexibleFilms (planned, call 4)

▬ To build up a basic understanding and guidelines for optimization for the realisation of thin metallic films grown on elastomer substrates which can be repeatedly folded without failure.

▬ Approach:

Interfacial shear strength, defects, and mechanical size effects will be explored across the nano-length scales from atomic dimensions (bonding) to several hundred nm (film thickness, grain size)

Page 25: ISO 9001 certified © JOANNEUM RESEARCH Forschungsgesellschaft mbH Laser Center Leoben SLONANO 2007 10-12 October 2007, Ljubljana, Slovenia The Austrian.

RPC NANOCOAT The projects of the RPC

BI.6: NanoToughening (planned, call 4)

▬ Investigation of the adaptability and benefit of the so-called transformation toughening mechanism to hard and wear-resistant coatings

▬ Approach:

To counteract crack propagation by a local nanoscale stress-induced phase transformation

To exert a crack-closing force by a volume expansion

Page 26: ISO 9001 certified © JOANNEUM RESEARCH Forschungsgesellschaft mbH Laser Center Leoben SLONANO 2007 10-12 October 2007, Ljubljana, Slovenia The Austrian.

RPC NANOCOAT The projects of the RPC

Applied Research (BII)

BII.1: AntiadhesiveCoatings

▬ Development of new multiphase anti-adhesive wear resistant coatings and suitable technologies to deposit these coatings on tools for cutting of soft materials like wood or wrought aluminium alloys

▬ Coating concepts:

Multilayer coatings with layer thicknesses as low as 3 nm

Nanocomposite coatings with crystals in the nanometer range

Layers with thin antiadhesive top layers

Page 27: ISO 9001 certified © JOANNEUM RESEARCH Forschungsgesellschaft mbH Laser Center Leoben SLONANO 2007 10-12 October 2007, Ljubljana, Slovenia The Austrian.

RPC NANOCOAT The projects of the RPC

BII.2: ColouredCoatings

▬ Development of new wear resistant decorative coatings and coating processes for achieving colour effects on various cutting tools made of cemented carbide

▬ Application of two colour concepts:

inherent colours

interference colours

BII.3: PolymerMetalCoating

▬ Gathering of knowledge about the adhesion and growth mechanisms of pulsed laser deposited (PLD) coatings on various polymer materials

▬ To understanding of the changes in the polymer surface due to the deposition process

Page 28: ISO 9001 certified © JOANNEUM RESEARCH Forschungsgesellschaft mbH Laser Center Leoben SLONANO 2007 10-12 October 2007, Ljubljana, Slovenia The Austrian.

RPC NANOCOAT The projects of the RPC

BII.4: HIPIMS

▬ Development of coating technology for wear-resistant low-friction coatings for automotive applications

▬ Two project phases:

Implementation of pulsed and high power impulse magnetron sputtering (HIPIMS) power supplies at existing laboratory-scale and production-scale sputtering systems

Development of nanocomposite low-friction coatings within the system CrC/a-C:H

BII.5: LowTempPACVD

▬ Development of nanostructured hard coatings deposited by plasma-assisted CVD below temperatures of 300°C

▬ Two major strategies:

Using metal halogenide precursors

PACVD based on metalorganic precursors

Page 29: ISO 9001 certified © JOANNEUM RESEARCH Forschungsgesellschaft mbH Laser Center Leoben SLONANO 2007 10-12 October 2007, Ljubljana, Slovenia The Austrian.

RPC NANOCOAT

Small scale vacuum & plasma coating equipment: Small scale vacuum & plasma coating equipment:

Unbalanced DC magnetron sputtering

Pulsed laser deposition system

Methods: Technology

Page 30: ISO 9001 certified © JOANNEUM RESEARCH Forschungsgesellschaft mbH Laser Center Leoben SLONANO 2007 10-12 October 2007, Ljubljana, Slovenia The Austrian.

RPC NANOCOAT

Industrial coating equipment: Industrial coating equipment:

PACVD coating system

Arc / Sputtering coating system( 6 arc/sputter sources)

Methods: Technology

Another industrial sputter system will be installed in August 2007

Page 31: ISO 9001 certified © JOANNEUM RESEARCH Forschungsgesellschaft mbH Laser Center Leoben SLONANO 2007 10-12 October 2007, Ljubljana, Slovenia The Austrian.

RPC NANOCOAT

Industrial coating equipment: Industrial coating equipment:

Process control(plasma emission,

gas analytics)

4 pu

lsd

lase

rs(N

d:Y

AG

)

Vacuum chamber(height 650 mm)

VacuumpumpGas flow

control(Ar, O2, N2,...)

Linearion source

PLD evaporator(rotating target)

Magnetron sputter source(pulsed) & bias voltage supply

Substrates

Substrate mounting(heating, cooling)

Rotary table (Ø 560 mm)for substrate movement

Substraterotation

P l a s m a

Hybrid PLD / Sputter Coating System

Sputtering source

DC-

SputteringPlasma

Multi-

beam

PLD

Methods: Technology

Another industrial PLD / plasma polymerization system will be installed in August 2007

Page 32: ISO 9001 certified © JOANNEUM RESEARCH Forschungsgesellschaft mbH Laser Center Leoben SLONANO 2007 10-12 October 2007, Ljubljana, Slovenia The Austrian.

RPC NANOCOAT Methods: Characterization

Evaluation of micro- and nanostructure:Evaluation of micro- and nanostructure:

GDOESGDOES

HT-XRDHT-XRD

XRDXRD

SAXSSAXS

EDXEDX

WDXWDX

Non-imaging Non-imaging techniquestechniques SAEDSAED

AESAES XPSXPS

RamanRaman

Imaging Imaging techniquestechniques

SEMSEM

TEMTEM

AFMAFM

FIBFIB

ProfilometryProfilometry

PEEMPEEMLEEDLEED

Page 33: ISO 9001 certified © JOANNEUM RESEARCH Forschungsgesellschaft mbH Laser Center Leoben SLONANO 2007 10-12 October 2007, Ljubljana, Slovenia The Austrian.

RPC NANOCOAT

Evaluation of surface response:Evaluation of surface response:

Methods: Application

ChemicalChemical

PhasePhasetransformationtransformation

ThermalThermalshockshock

ThermalThermalfatiguefatigue

Thermal /Thermal /chemicalchemical

OxidationOxidation

Heat capacityHeat capacity

ThermalThermalstabilitystability

ThermalThermalexpansionexpansion

ThermalThermalconductivityconductivity

PhysicalPhysicalpropertiesproperties

Electric Electric conductivityconductivity

AbrasionAbrasion

AdhesionAdhesion

Rolling contactRolling contactfatiguefatigue

Tribo chemicalTribo chemicalteststests

SurfacesSurfacesin contactin contact

Load-bearingLoad-bearingcapacitycapacity

Page 34: ISO 9001 certified © JOANNEUM RESEARCH Forschungsgesellschaft mbH Laser Center Leoben SLONANO 2007 10-12 October 2007, Ljubljana, Slovenia The Austrian.

RPC NANOCOAT Results

Achievements and highlights on Coating CharacterizationAchievements and highlights on Coating Characterization

Micromechanical testing

FIB machining of thin film cantilevers

enables determination of thin film stress profiles

Page 35: ISO 9001 certified © JOANNEUM RESEARCH Forschungsgesellschaft mbH Laser Center Leoben SLONANO 2007 10-12 October 2007, Ljubljana, Slovenia The Austrian.

RPC NANOCOAT

Temperature (°C)

0 100 200 300 400 500 600

Res

idua

l Str

ess

(GP

a)

-2.5

-2.0

-1.5

-1.0

-0.5

0.0

0.5

CrN/Cr/HSS

In-situ determination of the temperature-dependence of residual stresses in the Cr and CrN layers

Results

Achievements and highlights on Coating ApplicationAchievements and highlights on Coating Application

Response of coated surfaces to• mechanical loads• thermal loads

1 µm CrN

2 µm Cr

HSS

FIB-machined cross-section through wear track of a CrN/Cr coating on HSS indicating plastic deformation of the Cr interlayer

Page 36: ISO 9001 certified © JOANNEUM RESEARCH Forschungsgesellschaft mbH Laser Center Leoben SLONANO 2007 10-12 October 2007, Ljubljana, Slovenia The Austrian.

RPC NANOCOAT Results

Achievements and highlights on Coating ApplicationAchievements and highlights on Coating Application

Functionalization of surfaces for• optical effects• activation of polymers• wetting behaviour

M300(polished)

CrN ZrN Cr2N TiCN

Contact angles (deionized water)

Anodized Ti layer on TiN/Al2O3

Page 37: ISO 9001 certified © JOANNEUM RESEARCH Forschungsgesellschaft mbH Laser Center Leoben SLONANO 2007 10-12 October 2007, Ljubljana, Slovenia The Austrian.

ISO

9001

cert

ified

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Laser Center Leoben

Joint Venture - nSEC

nanoSURFACE ENGINEERING CenterCenter for Nanostructured Multi-functional Coatings and Deposition Technologies

nanoSURFACE ENGINEERING CenterCenter for Nanostructured Multi-functional Coatings and Deposition Technologies

Lead partner of the nSEC Lead partner of the nSEC

University ofLeoben

JOANNEUMRESEARCH

Location of the nSEC: Leoben, Styria, AustriaLocation of the nSEC: Leoben, Styria, Austria

Page 38: ISO 9001 certified © JOANNEUM RESEARCH Forschungsgesellschaft mbH Laser Center Leoben SLONANO 2007 10-12 October 2007, Ljubljana, Slovenia The Austrian.

ISO

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Laser Center Leoben

Form of organisation

ForschungsschwerpunktLaserdünnschichttechnik

LeadpartnerLeadpartner

„Marke NCC“

mit dem Laserzentrum Leobenmit dem Department Metallkunde

und Werkstoffprüfung

Working group nanoSURFACE ENGINEERING CENTER

Arbeitsgruppe Dünne Schichten, CD- Labor für Hard Coatings

ForschungsschwerpunktLaserdünnschichttechnik

LeadpartnerLeadpartner

„Marke NCC“

mit dem Laserzentrum Leoben

Research Group Surface Engineering, CD-Lab Advanced Hard Coatings

Research AreaLaser-assisted Thin Film Technology

Lead partnerLead partner

Trademark nSE

Laser Center LeobenDepartment Physical Metallurgy

and Materials Testing

nSEC

Page 39: ISO 9001 certified © JOANNEUM RESEARCH Forschungsgesellschaft mbH Laser Center Leoben SLONANO 2007 10-12 October 2007, Ljubljana, Slovenia The Austrian.

ISO

9001

cert

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© JOANNEUM RESEARCH Forschungsgesellschaft mbH

Laser Center Leoben

nanoSurface Engineering Center

The nSEC is

a „think tank“ through the interaction with other institutions in the Materials Innovation Center Leoben,

a co-operative platform for its partners,

attractive for international scientists,

one of the internationally leading R&D institutions in its scientific and technological areas.

The nSEC is

a „think tank“ through the interaction with other institutions in the Materials Innovation Center Leoben,

a co-operative platform for its partners,

attractive for international scientists,

one of the internationally leading R&D institutions in its scientific and technological areas.

Materials Innovation Center Leoben

nSEC

To

ols

Co

mp

on

en

ts

Fu

nc

tio

na

l d

ev

ice

s

CD LabsCompetencecenters

Other R&D institutions

Universitydepartments

Companies

Materials Cluster

Goals nSEC for 2008:45 employeesInfrastructure ~2.2 Mio. € (Styria, EFRE)Start: 2005

Page 40: ISO 9001 certified © JOANNEUM RESEARCH Forschungsgesellschaft mbH Laser Center Leoben SLONANO 2007 10-12 October 2007, Ljubljana, Slovenia The Austrian.

ISO

9001

cert

ified

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Laser Center Leoben

Materials Innovation Center Leoben

Total floor space: 5400 m2 Workstations: 231 Construction Costs: 10 MEUR

Organisations: The University of Leoben, Materials Center Leoben,Polymere Competence Center Leoben, Joanneum Research, nanoSurface Engineering Center (approx. 1000 m2)

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nSEC - R&D Topics„Nano-structured Multi-functional Coatings“

available Expertise to be establishedavailable Expertise to be established

Area 1:Tools: steel, ceramics,cemented carbide (Tribological coatings)

Self-hardeningSelf-hardening

Self-lubricatingSelf-lubricating

Anti-adhesiveAnti-adhesive

Self-cleaningSelf-cleaning

Self-repairSelf-repair

R&D growth rate ~20%

Area 2:Components: metal, polymers(active, chemically-resistant coatings)

Self-lubricatingSelf-lubricating

Anti-adhesiveAnti-adhesive

Self-cleaningSelf-cleaning

Self-repairSelf-repair

ColouredColoured

R&D growth rate ~50%

Design, synthesis, characterization, and application are cross-sectional topics

Self-adaptation by tailored surface reactions

Area 3:Functional Devices: metals, polymers(Sensor coatings, optical coatings)

Self-lubricatingSelf-lubricating

Anti-adhesiveAnti-adhesive

Bio-compatibleBio-compatible

Bio-activeBio-active

Indicator coatingsIndicator coatings

R&D growth rate >50%

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Laser Thin Film Technology

Scientific and technological goals:

Development: - Functional thin films (anorganic, organic)

- Room-temperature deposition techniques (Pulsed Laser Deposition (PLD))

- Hybrid PVD techniques (e.g. PLD + Sputtering, Ion beam techniques)

Coating of forming tools

Transfer to industrial applications:- Tribological, wear-resistant and functional

coatings on polymer substrates

- Functional coatings for medical and biological applications

- Sensor coatings

- Laser and plasma-assisted coating processes

Biocompatiblecoatings

Coated tools

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Laser Thin Film Technology

Equipment for Film Deposition Laboratory PLD coating plant (PLD, DC Sputtering, RF

Sputtering, Diameter of sputtering cathodes 76 mm) Demonstration PLD coating plant (PLD employing 4 laser

beams, rectangular sputtering cathode 73.6 mm x 431,8 mm, recipient diameter 740 mm, coating height 300 mm)

Q-switched laser systems 1000 mJ Nd:YAG laser 1200 mJ Nd:YAG laser

Projected (nSEC Leoben) Multi-functional PLD coating plant Excimer laser (248 nm)

560 mm

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Deposition of DLC by Employing an Anode Layer Source (ALS)

Idea in the 1960's: to construct an ion propulsion system for space satellites Kaufmann ion source (USA) : Anode layer ion source (USSR)

outer cathode

inner cathodeslit

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Background of the experimental technique (ALS)

Cross-section of the anode layer source

Detail of the slit

Geometry in the chamber

ion

sour

ce

ion

jet

grow

ing

film

sam

ples

sam

ple

hold

er

Expected benefits:- easy, robust- no target needed- no droplets- no contaminants- good adhesion

Possible drawbacks:- unexplored area- large internal stress

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Film deposition by ALSParameters to be varied

- where to feed the C2H2 gas- ratio Ar : C2H2 (or none Ar at all?)- total flow of the gases - cathode voltage- sample movement: rotation, oscilation, static- deposition time

- constant parameters / two sets / periodic changing

Objectives- a reasonable deposition rate- acceptable adhesion- other parameters for particular application

0

1

2

3

4

5

6

7

8

9

10

0 2 4 6 8 10 12 14 16batch no.

de

po

sitio

n r

ate

[n

m/m

in]

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Chemical bonds of carbon

Hybridisation

Graphite

Diamond

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Diamond-like Carbon (DLC)Ternary phase diagram of amorphous C-H alloys

sp3

H

ta-C:H

a-C:H

polymers (CHx)

no solids

sp2

graphite, soot, fulerenes, nanotubes

ta-C

a-C(:H)

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Structure of DLC

Tetrahedral C (ta-C)

▬ sp3-content > 40 to 60 %

▬ short range order with sp2 and sp3 bonds

▬ no long range order

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RAMAN Spectroscopy of DLC films deposited by ALS

Typical spectrum of hydrogenated tetrahedral DLCG-peak: bond stretching of all pairs of sp2 sites in rings and chains

D-peak: breathing modes of rings

Spectrometer: LAbRam-HR 800 from Jobin Yvon, laser excitation wavelenth 532 nm

Film deposition: ALS 340 from Veeco, 1 kV, 20 sccm acetylene M. Kahn, M. Cekada, R. Berghauser, W. Waldhauser, C. Bauer,

C. Mitterer, E. Brandstätter; Diamond 2007, 9-14 September 2007, Berlin

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Properties of DLC deposited by ALS

Intensity ratio ID/IG (measured with 532 nm, calculated with the peak amplitudes) and compressive stress

M. Kahn, M. Cekada, R. Berghauser, W. Waldhauser, C. Bauer, C. Mitterer, E. Brandstätter; Diamond 2007, 9-14 September 2007, Berlin

high sp3 low sp3

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Biocompatible coatingsDetachment kinetics of D. discoideum cells from biocompatible PVD coatings

Stainless steel upper disc

1.5 mm hole in upper disc

Sample withattached cells

decreasing shear flow

liquid flow

Cell preparation:• Growth in axenic medium in agitated suspension• Pelletation (107 cells) & washing in Sörensen phosphate buffer• Cell storage on ice and use within 8 h

Cell type:Dictyostelium discoideum Ax-2

0.1

mm

Shear flow test realization:• Attaching cells to sample• Assembling of test device• Liquid flow (Sörenson buffer, 21°C) for specified test duration (5, 10 min)• Counting of cells on sample in dependency on distance to centre (different occuring shear stress) by fluorescence microscopySetup according to Lauffenburger et al.

“Adina” FEM calculation of occurring shear stresses in the slit

J.M. Lackner, W. Waldhauser, R. Berghauser, M. Kahn, F. Bruckert, R. Major, B. Major, SVC 2007, Kentucky, Louisville, 28 April - 3 May , 2007

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Biocompatible coatings -Cell adhesion

J.M. Lackner, W. Waldhauser, R. Berghauser, M. Kahn, F. Bruckert, R. Major, B. Major, SVC 2007, Kentucky, Louisville, 28 April - 3 May , 2007

10 20 30 40 50 6020

30

40

50

60

70

80%

of d

eta

che

d c

ells

[1]

Shear stress [Pa]

Ti substrate

TiN

TiCxN

y (low C)

TiCxN

y (high C)

DLC

critical shear stress

(50 % cell detachment)

(r) = 3 D / ( r e²)

Flow rate

Dynamic viscosity (Sörensen buffer)

Radius from centre hole

Disc spacing

Cell type: Dictyostelium discoideum Ax-2

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Biocompatible coatings -Critical shear flow

J.M. Lackner, W. Waldhauser, R. Berghauser, M. Kahn, F. Bruckert, R. Major, B. Major, SVC 2007, Kentucky, Louisville, 28 April - 3 May , 2007

(for 50 % cell detachment)

0

10

20

30

40

50

60

70

80

Ti substr. TiN mag TiCN 0_ 5 TiCN 2_ 5 DLC

crit

ical

shear

str

ess

(50%

of

cell

s d

eta

ched)

Higher carbon content=> Higher cell adhesion

Decreased adhesion for TiCN low C

low C high C

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ConclusionsThe Austrian government, federal provinces and funding institutions are supporting an Austrian programme für Nanoscale Sciences and Nanotechnologies

Basic and applied research is performed in Research Project Clusters (RPC)

In Styria there are intense activities in nano surface engineering

Two centers for Nanoscale Sciences have been established in Styria nanoSURFACE ENGINEERING Center Leoben Nano Tec Center Weiz

New functional nano coatings will enable new fields of applications and will develop new markets

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Thank you for your attention!

Acknowledgements:Financial support by • Forschung Austria (Grant programme within the brainpower Austria initiative)• Austrian Federal Ministry of Traffic, Innovation and Technology• Austrian Industrial Research Promotion Fund (FFG)• Government of Styria• Slovenian Research Agency• European Union is highly acknowledged.