INSTITUTE OF MATERIALS RESEARCH OF SASINSTITUTE OF MATERIALS RESEARCH OF SASKOKOŠŠICE, SLOVAKIAICE, SLOVAKIA

Jan Jan DuszaDuszajdusza@imr.saske.skjdusza@imr.saske.sk

PROJECTPROJECT--GERERATION WORKSHOPGERERATION WORKSHOP““9.2.2007, 9.2.2007, IMR SASIMR SAS, Watsonova 47, Ko, Watsonova 47, Koššiceice

RESEARCH IN RESEARCH IN NANOTECHNOLOGY NANOTECHNOLOGY &&NANOMATERIALS NANOMATERIALS

IN KOIN KOŠŠICEICE

EUROPE & SLOVAKIAEUROPE & SLOVAKIA

Nano - research in Slovakia/Kosice• Institutes of Slovak Academy of Sciences

• Institutes of Universities

EUROPE

SlovakRepublic

SAS IndustryUniversities

•• From From ccacca 19951995•• Main areas:Main areas:

-- Bulk Bulk nanostructurednanostructured materials (metallic, ceramic, materials (metallic, ceramic, composites, etc.);composites, etc.);

-- NanoNano –– powder, powder, nanotubesnanotubes, , nanowiresnanowires;;-- Polymers and bio Polymers and bio –– materials;materials;-- Thin films and coatings;Thin films and coatings;For electro/functional, structural and bioFor electro/functional, structural and bio--medical medical applications. applications.

-- Education, standardization, application.Education, standardization, application.

NANO NANO –– RESEARCH / SCIENCERESEARCH / SCIENCEIN SLOVAKIAIN SLOVAKIA

SLOVAK NETWORKSSLOVAK NETWORKS

INSTITUTE OF INORGANIC CHEMISTRY, SAS DEPARTMENT OF CERAMICS

INSTITUTE OF EXPERIMENTAL PHYSICS, SAS DEPARTMENT OF MAGNETISM

INSTITUTE OF GEOTECHNICS, SAS DEPARTMENT OF MECHANOCHEMISTRY

INSTITUTE OF MATERIALS and MACHINE MECHANICS, SAS DEPARTMENT OFMICROSTRUCTURE OF COATINGS and BOUNDARIES

INSTITUTE OF PHYSICS, SAS DEPARTMENT OF METAL PHYSICS

INSTITUTE OF MATERIALS RESEARCH, SAS DEPARTMENT OF STRUCTURALCERAMICS - Coordinator

ELECTRICAL INSTITUTE OF SAS

Centre of Excellence of SASNANOSTRUCTURED MATERIALS – NANOSMART

2003 – 2006, 2006 - 2010

SLOVAK NETWORKSSLOVAK NETWORKS

NANOSMARTNANOSMART+ +

Laboratories from SASLaboratories from SAS++

Laboratories from UniversitiesLaboratories from Universities

NATIONAL CENTRE OF EXCELLENCEfor

Nano-science & nano-technology

2006

•• NanoSciNanoSci –– ERAERA•• MINAEASTMINAEAST•• NENAMAT Network for Nanostructured NENAMAT Network for Nanostructured

Materials of Associate Candidate Countries Materials of Associate Candidate Countries •• NANOMATNANOMAT--targeted action to encourage the targeted action to encourage the

participation of SMEs in the 6FP, in the participation of SMEs in the 6FP, in the Nanotechnologies and knowledge based Nanotechnologies and knowledge based multifunctional materrials fieldsmultifunctional materrials fields

INTERNATIONAL ACTIVITIESINTERNATIONAL ACTIVITIES

INTERNATIONAL ACTIVITIESINTERNATIONAL ACTIVITIES

Network for Network for NanostructuredNanostructured Materials of ACC Materials of ACC (NENAMAT, INCO(NENAMAT, INCO--CTCT--20032003--510363), 510363), 2004 2004 –– 20062006

• to mobilize in ACC existing human and material resources in the field of nano-structured materials;

• significantly improve the communication and collaboration between centers working in this area of research in individual ACC and between the Centers in ACC, Member States, Russia & New Independent States (NIS) and Southeast European Countries, (SEEC);

• to disseminate scientific information as well as results of the research in the field of nanotechnology and nanostructuredmaterials;

• to consolidate, network and strengthen the RTD potential in the area of ACC;

• to create a common platform for coordination of the research, education and training activities in ACC in the field of nano-structured materials;

• to contribute to the building of ERA ;

INTERNATIONAL ACTIVITIES INTERNATIONAL ACTIVITIES --AIMS of NENAMATAIMS of NENAMAT

• Institute of Materials Research of the Slovak Academy of Sciences, Košice, Slovak Republic

• Institute of Electrochemistry and Energy Systems of the Bulgarian Academy of Sciences, Sofia, Bulgaria

• Faculty of Mechanical Engineering of the Brno University of Technology, Brno, Czech Republic

• Institute of Materials Technology, Tallin Technical University, Tallin, Estonia• Research Institute for Technical Physics and Materials Science of the

Hungarian Academy of Sciences, Budapest, Hungary• Institute of Inorganic Chemistry of the Riga Technical University, Riga, Latvia• Faculty of Materials Science and Engineering, Warsaw University

of Technology, Warszaw, Poland• National Institute of Research and Development for Technical Physics Rumania• “Jožef Stefan” Institute, Department of Engineering Ceramics, University of

Ljubljana, Ljubljana, Slovenia• Isik University, Maslaki, Istambul, Turkey

INTERNATIONAL ACTIVITIES INTERNATIONAL ACTIVITIES --CONSORCIUM of NENAMATCONSORCIUM of NENAMAT

• NANOVED ‘03 – Bratislava;• NANOVED ’04 - Košice in cooperation

with MINAEAST- NET;• MOBILIZATION WORKSHOP -

NENAMAT ’05 - High Tatras;• CAMIN ‘05 Smolenice Castle;• NANOVED ’06 / NENAMAT-High Tatras.

WORKSHOPS & CONFERENCESWORKSHOPS & CONFERENCES

RecentlyRecently•• Processing :Processing :

Different mills for powder preparation;ECAP systems;Rapid solidification facilities;Hot presses, GPS furnaces ;PVD; thermogravimeter, calorimeter, etc.

•• Characterization & testingCharacterization & testingOM, SEM, TEM, AEM, HREM – 200kV ;SEM – JEOL 7000, NanoScanSQUID, AFM, X – ray, static and dynamic laser scattering equipments;Micro-nano indentation facilities, mechanical & creep tests, etc;

FACILITIESFACILITIESAwaiting

HRTEM – 300kV

Nano - hardness, scratch, tribology

impact, 2007, NCE

Spark plasma sintering furnace;

Advanced PVD;

Auger spectroscopy, etc, 2008-9

European Structural Funds

2007-2013, 800 mill Euro for Resarch & Development

Ing. Juraj Ďurišin, CSc. – durisin@imrnov.saske.sk

Research topic in Nano

• Preparation of the nanocrystalline copper powder mixtures (Cu-Al2O3, Cu-MgO ...)by different methods based on the combination of mechanical milling with phasetransformations of the precursors and their compaction into bulk dispersionstrengthened materials

• Study of dispersoid effect on the nanocrystalline matrix grain stability at elevatedtemperatures

• Analyse of mechanical properties in relation to the material microstructure

Recent project

Evolution and microstructure stability of nanocrystalline grain (No. 2/4172/06)

Institute of Materials ResearchSlovak Academy of Sciences

Watsonova 47, 043 53 Košice, Slovak Republichttp://www.imrnov.saske.sk

Institute of Materials ResearchSlovak Academy of Sciences

0

30

60

90

120

150

180

0 200 400 600 800 1000Temperature (oC)

Hard

ness

HB

Cu-MgO Cu-Al2O3

Al2O3

Al2O3

MgO

Homogeneous Cu – Al2O3 microstructure Bimodal Cu – MgO microstructure

MECHANICAL PROPERTIES

Yield

strength (MPa)

Tensile strength (MPa)

Ductility

(%)

Brinnel hardness

HB Cu – 3 vol.% MgO 145 240 22 90

Cu – 3 vol.% Al2O3 397 436 2 160

coarse-grained Cu 100 135 22 62

Head: Dr. Ivan Škorvánek, Inst. Exp. Physics SAS, 043 53 Kosice, Slovakiaskorvi@saske.sk tel. +421 55 7922235

Group of Nanostructured Magnetic Materials

Research interests :• composition-structure-property relationship in nanostructured magnetic systems• soft magnetic materials with bcc-Fe, Fe(Si) and FeCo nanoparticles embedded

in a residual amorphous matrix • magnetic nanoparticles and nanocapsules with core/shell structure• materials for magnetic refrigeration

Selected research projects:Volkswagen Foundation VW-I/75961 Soft Magnetic Nanocrystalline Materials with Improved Combination of Application Oriented Properties (2000-2003)NATO PST.EAP.CLG 981072 - Science for security Novel soft magnetic nanocrystalline alloys with high critical temperatures (2004 - 2006)COST 523 Structural and functional properties of soft magnetic nanocrystalline materials (2001-2004VEGA 2/4065 Structure and magnetic properties of transition metal based nanocrystalline materialsprepared by controlled crystallization from amorphous precursors (2004-2006)APVT-20-018402 New multiphase materials with defined microstructure and extraordinary physicalproperties (2004-2006)APVT-20-018402 Synthesis and characterization of nanomaterials prepared by non-traditional methods from metals and raw materials precursors (2002-2005)

Group of Nanostructured Magnetic MaterialsSelected results

HRTEM of Fe-based nanocapsules

-3000 -2000 -1000 0 1000 2000 3000-200

-150

-100

-50

0

50

100

150

200 Zero field Longitudinal field

(20 kAm-1) Transverse field

(640 kAm-1)

(FeCo)81Nb7B12 annealed at 500 °C/1h

Mag

netis

atio

n [A

m2 /k

g]

H [A/m]

Improved soft magnetic properties of nanocrystallineFeCoNbB after heat treatment in external magnetic field

Magnetization curves for Dy/Dy2O3 nanoparticles at low temperatures

skorvi@saske.sk

GroupGroup: : CeramicCeramic SuperconductorsSuperconductors and and NanomaterialsNanomaterialsInstitute of Experimental Physics, SAS

Head: Pavel Diko, dikos@saske.sk

Research field: - nano-pining centers in singlegrain REBCO bulk superconductors

- synthesis of nanoparticles stable at high temperatures - trapping of nanoparticles by growing crystal

Projects: SCENET, THE EUROPEAN NETWORK FOR SUPERCONDUCTIVITY , GROWTH 5 RP 2003-2006EFFORT , The European Forum for Processors of Large Grain (RE)BCO Funded by the UK goverment and by European Commission 2003-2007NENAMAT, NANOSMART

SCENETThe European Network for Superconductivity

REBCO Effort

20µm

Y2Ba4CuUOx particles

trapped in YBa2Cu3Ox

crystal at 1000 oC

5 µm

10

10

20

n

d211

[μm]dUbp [µm] 1

YBa2Cu3O7 Y2O3

CeO2 After milling

STRUCTURAL CERAMICS DEPARTMENT,STRUCTURAL CERAMICS DEPARTMENT,CENTRE OF EXCELLENCE FOR NANOSTRUCTURED CENTRE OF EXCELLENCE FOR NANOSTRUCTURED

MATERIALS OF SASMATERIALS OF SASATAT

INSTITUTE OF MATERIALS RESEARCHINSTITUTE OF MATERIALS RESEARCH

www@imrnov.saske.skwww@imrnov.saske.sk

Prof. Dr. Jan Prof. Dr. Jan DuszaDusza, , Dr.ScDr.Sc., ., -- jdusza@imr.saske.skjdusza@imr.saske.sk

Development of structural ceramic nanocomposites – characterization of microstructure and testing of mechanical properties

•• 5FP5FP-- Structural integrity of ceramic multilayers and coatingsStructural integrity of ceramic multilayers and coatings(SICMAC, RTN2(SICMAC, RTN2--20012001--00488), 00488), 20022002--20062006

•• 6FP 6FP –– Knowledge based Multicomponent Materials, Knowledge based Multicomponent Materials, ( KMM( KMM--NoE, 502243NoE, 502243--2), 2), 20042004--20082008 20082008

•• 6FP 6FP –– Network for Network for NanostructuredNanostructured Materials of ACC Materials of ACC (NENAMAT, INCO(NENAMAT, INCO--CTCT--20032003--510363), 510363), 2004 2004 –– 20062006

• High - temperature materials, high thermal efficiency and lower exhaustemission;

• Sintering additives/Intergranular phase• Si3N4 + SiC nanocomposite• HT properties: strength, creep, fatigue

SiSi33NN44 + + SiCSiCnanocompositesnanocomposites

PROCESSING PROCESSING –– SiSi33NN44+SiC+SiCPolysilazane

[MeSiH-NH]m[Me2SiNH]n

Pyrolysis, 1000 0C, Ar

Silicon CarbonitrideSixCyNz

+ Y2O3 + Al2O3Milling/Pressing

Sintering1750 - 1900 0C, N2

β-Si3N4 + β-SiCComposite

α-Si3N4 Powder + [(Me2Si)m(MePhSi)]n

+ Y2O3+Al2O3

Milling/Pressing

Pyrolysis1000 0C, Air

Sintering1750 0C -1900 0C, N2

β-Si3N4 + β-SiCComposite

α-Si3N4 Powder + amorphous Si-C-N

+ Y2O3+Al2O3

Milling/Pressing

Sieving/Drying

CIP, GPS/HT

β-Si3N4 + β-SiCComposite

Si3N4

Si3N4

Si3N4Si3N4

Si3N4

Si3N4

Si3N4

Si3N4SiC

SiC

SiC

CREEP DAMAGE IN SiCREEP DAMAGE IN Si33NN44 AND AND SiSi33NN44+SiC+SiC

J.Dusza et al J. Am. Ceram. Soc., 87, (2005),2113-2117

5,6 5,8 6,0 6,2 6,4 6,6 6,8 7,01E-10

1E-9

1E-8

1E-7

SiCN-derivedCarbon derivedlmixed Si3N4+SiCmonolithic Si3N4,

104/T[K-1]

Cre

ep R

ate

[s-1]

Y2O3

Nano

com

posit

CREEP RESISTANCE IMPROVEMENT OF SiCREEP RESISTANCE IMPROVEMENT OF Si33NN44 CERAMICS CERAMICS BY INTERCORPORATING BY INTERCORPORATING SiCSiC NANOPARTICLESNANOPARTICLES

INTO THE SiINTO THE Si33NN44 / Si/ Si33NN44 BOUNDARIESBOUNDARIESCOOPERATION: IMR SAS, IACH SAS, QM University of London

100 nm

SiC

Si3N4

Si3N4

6.6 A

CHANGED CREEP MECHANISMSIMPROVED CREEP RESISTANCE

nc - MeN/ kov Me = W, Crnc - MeC/a – Cnc - MeC/a – C:Hnc - MeC/DLCnc - MeC/a – CNxnc - MeC/a-C+a-nitridnc - MeN/DLCnc - MeN/a – nitrid

Hardness of the WC/C coat is 40 GPameasured by nanoindentation

0,00

2,00

4,00

6,00

8,00

10,00

12,00

0,00E+00 5,00E-02 1,00E-01 1,50E-01

h [?m]

F [m

N]

THANK YOUTHANK YOU