1. Joint Glass Centre Vitrum Laugaricio (VILA)
Trečnín, Slovak Republic
Dušan Galusek

2. The Centre is not legal entity
VILA
Joint venture of 3 partners:
Institute of Inorganic Chemistry, SAS
Alexander Dubček University of Trenčín
Slovak University of Technology, Bratislava
Location:
Premises of TnUAD in Trenčín
Personnel:
18 researchers + 8 PhD students
The Centre is not legal entity

3. Scope:
C E R A M I C S:
Composition, structure, and properties of ceramics:
Amorphous grain boundary phase in polycrystalline ceramic materials, with special attention paid to nanostructured materials and nanocomposites ceramics/ceramics.
Oxide ceramics:
Submicron alumina ceramics
Nanocomposites Al2O3-SiC, Al2O3-CNT
Wear resistance of Al2O3-based materials
Corrosion:
chemical and corrosion resistance of structural ceramics in aqueous environment
refractories in glass-forming melts
dental materials  mechanical properties

4. Scope:
G L A S S:
Relations between composition, structure, and properties of glass, with special attention paid to oxide, and silicate glass.
Relations between composition, structure, and properties of glass
Developed of new compositions of glass for industry
Leaching kinetics of glass in aqueous media
Electric and impedance characteristics of glass and glass-formig melts at high temperatures
Direct observation of processes in glass forming melts, melting, fining
Aluminate glasses with photoluminiscence properties

5. Strategy in establishing the Centre
Building of methodical and experimental infrastructure
All fundamental experimental techniques required for a materials research laboratory:
Materials preparation
Materials characterization
Independence from the point of view of fundamental experimental techniques
Removal of „bottlenecks“ influencing the work efficiency
Intensification of cooperation with:
partner academic institutions
with industries
Making the laboratory more attractive from the point of view of submitting joint grant proposals with foreign partners
Utilization of the infrastructure for education (master and PhD study)

6. BUILDING THE INFRASTRUCTURE

7. CERAMOGRAPHIC LABORATORY:
Diamond saw for rough cutting of hard materials
Bühler Abrasimatic 300
Vibration mill
Fritsch Pulversiette 0
Polishing machine
Bühler Ecomet 300/Automet 300
Precise diamond was for cutting og hrad materials
Bühler Izomet 5000
Laping machine
Bühler EcoMet 300Pro

8. LABORATORY OF COLLOIDAL PROCESSES:
Reometry/viscometry Haake MARS III
Measurement of flow properties of liquids in the ciscosity range 0,5 mPas to 106 mPas
Rheoscopic module
Particle size analysis and zeta potentiometry
Brookhaven 90Plus
Planetary mill
Fritsch Pulversiette 6
Helium pycnometry
Ultrapyc 1200e

9. LABORATORY OF CORROSION TESTS:
Climatic chamber Angelantoni Discovery DY110
Laboratory oven up to 350 oC
Autoclave Büchi CC075
Hot water baths with shaking supplements Memmert

10. ICP OES Varian Vista MPX MW combustion Berghof Speedwave 4
LABORATORY OF CHEMICAL ANALYSIS:
ICP OES Varian Vista MPX
MW combustion Berghof Speedwave 4 +
ICP OES Agilent 5100 SVDV
IC Dionex™ ICS-5000+,
ICP MS Agilent 7900 ICP-MS
LSX-213 G2+ Nd:YAG Laser Ablation System

11. X-ray diffractometer Bruker Tiger
X-RAY FLUORESCENCE:
X-ray diffractometer Bruker Tiger
Semi-quantitative and quantitative chemical analysis
Analysis of solids and liquids
All elements from B upwards
Including sample preparation laboratory
Certified measurements

12. FURNACE LABORATORY: Gradient furnace Tube furnace 1300°C
Chamber furnaces, ambient atmosphere 1800°C
Hot press
Glass melting furnaces with mixing 1800 oC
Tube furnace, vacuum, controlled atmosphere, 1800°C

13. JEOL JSM-7600 F/EDS/WDS/EBSD
ELECTRON MICROSCOPY
JEOL JSM-7600 F/EDS/WDS/EBSD
Detailed microstructure and chemical analysis of solids
Resolution:
1-2 nm at 15kV
Analytical modules:
1 x WDS detector
1 x SDD detector
1 x EBSD detector
database SW for evaluation of EBSD spectra
JEOL JFC „AUTO Sputter Coater“, JEOL JEC-520 „Carbon Coater“
Sputtering of non- conductive specimens for SEM
CP Polisher JEOL IB-0901CP

14. X-ray diffractometer Panalytical Empyrean
X-RAY DIFFRACTION:
X-ray diffractometer Panalytical Empyrean
Qualitative and semi-quantitative phase analysis
goniometer with Θ-2Θ geometry and diameter 240 mm
X-ray lamp with Cu anode
Reflexion and transmission
3D Pixcel® detector
High temperature cell Anton Paar up to °C
Cryogenic and humidity cell Anton Paar to 400 °C
SAXS
Microdiffraction

15. THERMAL ANALYSIS: Simultaneous thermal analysis
Netzsch STA 449 F1 Jupiter TG/DTA/DSC
DTA and TG up to 2000°C
DSC up to 1600°C
Differential scanning calorimetry Perkin Elmer DSC 8500
Thermomechanical analyser
Netzsch TMA 402 F1 Hyperion

16. High temperature rotation viscometry
LABORATORY OF PHYSICAL PROPERTIES:
Hot stage microscope
Max. temperature 1500 oC
Leitz
High temperature rotation viscometry
Max. temperature 1550 oC
Viscosity range 101 – 107,5 dPas
Bähr
Microhardness tester
WIKI 200

17. SPECTROSCOPIC LABORATORY
Fluorescence spectrometer
Fluorolog 3: FL 3-21 (Horiba)
Fiber spectrometer for near infrared wavelengths
Ocean Optics NIRQUEST
UV-VIS-NIR spectrometer
Cary 5000 (Agilent Technologies)

18. LABORATORY OF RAMAN SPECTROSCOPY
Measurement of Raman and photoluminiscence spectra
laser excitation sources
488 nm
514 nm
457 nm
633 nm
Hot stage up to 600 oC
DSC coupled
AFM coupled
TERS

19. LABORATORY OF ELECTRICAL PROPERTIES
Potentiostat with frequency analyser
Solartron Analytical Modulab ESC-MTS
Tmax = 1500 oC
TSDC System Concept 90 + QUATRO, Novocontrol

20. Aluminate Glasses Luminescent materials
Crystallisation  eutectic microstructures
Hollow YAG microspheres

21. Luminescent materials for LEDs
Systems:
Binarny:
Al2O3–RE2O3 RE = Y, Yb, La
Ternary:
Al2O3–RE12O3-RE22O3 RE1 = Y, Yb, La RE2 = Nd, Er (1, 3, 5 mol%)
Al2O3–RE2O3-SiO2
Al2O3–RE2O3-ZrO2
Qaurternary:
Al2O3–RE12O3-SiO2-RE22O3
Al2O3–RE12O3-ZrO2-RE22O3

22. Luminescence properties
Er-doped Y2O3–Al2O3-SiO2 glasses
Excitation spectra:
Maximum intensity in near UV region
λ = 378 nm
Emission spectra:
Maximum intensity in green-yellow area
λ = 548 nm
Intensity decreases with increasing Er content
Concentration quenching
A. Prnová, A. Domanická, R. Klement, J. Kraxner, M. Polovka, M. Pentrák, D. Galusek, P. Šimurka, Optical Materials, (2011)

23. Study of thermal behaviour of Y2O3-Al2O3 glass microspheres
Ea  980 kJ/mol
Nucleation + growth
Ea  1840 kJ/mol
Crystal growth

24. Luminescence properties
Ce-doped Y2O3–Al2O3 glasses: luminescence vs. crystallization

25. pressure-assisted sintering of glass microspheres:
Bulk ceramics or glass-ceramics with ultra fine YAG/Al2O3 eutectic microstructure
HP 1600 oC/0’
HP 1600 oC/40’
pressure-assisted sintering of glass microspheres:
by viscous flow /lower temperatures ≈ °C/
by diffusion flow /higher temperatures ≈ °C

26. Hollow glass and polycrystalline microspheres
Many applications:
Excellent heat insulation properties and low density
Medical applications
Radiation shielding
Hydrogen and nitrogen storage
YAG hollow microspheres:
Stable chemical and physical properties
Promising structural materials for high temperature engineering:
insulating, refractory coatings (high chemical stability, low electrical conductivity and high creep resistance)
Yttrium glass microspheres for cancer treatment

27. Hollow YAG glass microspheres: results

28. Hollow YAG glass microspheres: cross sections~
As-recieved
Crystallized ~ 900 oC

29. Alumina-based ceramics
Transparent alumina with submicron microstructure
Transparent armours
Al2O3-SiC nanocomposites with high creep resistance

30. Two-stage sintering of Al2O3
Preparation of PCA with excellent mechanical properties transparent in VIS region
Losses:
Interface Al2O3-air
Pores
Grain boundaries
What we need:
Clean grain boundaries
Porosity < 0.01 %
Grain size < 300 nm
R. APETZ, M. Van BRUGGEN: J. Am. Ceram. Soc., 2003

31. Two-stage sintering of Al2O3
State of the art:
Addition of dopants (Y2O3, ZrO2)
Grain size < 500 nm
Relative density > 99,5 %

32. … followed by HIP SSS + HIP TSS + HIP dopant MGS (nm) SD/n (nm/-) Nd
SSS + HIP
TSS + HIP
dopant
MGS (nm)
SD/n (nm/-) Nd
510 60
570 80 Eu
400 50
430 Er
360
350 40
Mean grain size of rare earth doped aluminas after HIP (1280°C / 3 h)

33. Luminescence
Al2O3:Nd3+
Al2O3:Eu3+

34. Transparent armours Protection of air and land vehicles
STANAG 4569 Level 3
Max. thickness 60 mm
Significant reduction of weight
Projekt NATO SfP “Light weight and transparent armours”

35. Projectile: caliber: 7,62 x 51 mm Type: AP8 (WC core)
Producer: NAMMO, Sweden
Velocity: 930  20 m/s
Layered armour system with lamelar protection system after multiple hit. Front and rear view.
5 500 60
2 500 40
Glass/Sapphire stripe
31 000
8 000
Glass/Sapphire
2 000
125
1 250 85
Glass
Price [EUR]
Thickness [mm]
7,62x51 AP8 (WC core)
7,62 x 54R B-32 API
Size
500x500 mm

36. Nanocomposites Al2O3-SiC
Organosilicon polymers as the source of SiC
Conventional preparation
Increased resistance against:
wear
creep

37. Corrosion Dental materials Historical glass
Glass fibres in nuclear power plants

38. Mechanisms of dissolution:
Lithium disilicate glass ceramics
Mechanisms of dissolution:
LiDis
+ nucleophylic attack of OH on Si at high pH
White et al.
J Am Cer Soc (1987)
alkaline solution
1 m
Michalske et Bunker,
J. Appl. Phys. (1984)
nl (Si)
100 nm
acidic solution
1 m

39. Leucite glass ceramics
Results: Tribological measurements
Leucite – based glass ceramics
Dynamic test: 12h cyclus N
100 µm
Microhardness (Vickers indentation)
not corroded sp.
LiDis
[HV0.2]
Leucit [HV0.2]
before test
643 ± 9
640 ± 50
citric acid
636 ± 14
590 ± 20
acetic acid
618 ± 14
595 ± 43
ISO standard test
610 ± 9
581 ± 30
Alkaline solution
624 ± 10
553 ± 21 N

40. Historical Glass copper surface before corrosion test
Preparation of model glasses with compositions similar to historical glasses
Study the influence of musei environment on glass and glass-metal joints
Corrosion and acellerated aging tests of glass and glass- metal joints
Identification of corrosion products
Propose the mechanisms
Propose protective measures for protection of historical artifacts
globular precipitate on a corroded Cu tape
metal/glass joint area after corrosion test
new crystaline phase in the metal/joint area

41. Glass fibers in NPP
Approx kg of glass fibrous insulation falls tothe bottom of reactor containment.
Fibers block recirculation of coolant solution.
Glass dissolves in coolant solution and new products are formed.
alkali-depleted layer formed on the surface
Inter-diffusion of alkaline ions and hydroxonium ions
pH value increases
Surface layer dissolves
soluble silicates, borates and aluminates formed
Crystalline alumino-silicates precipitate
Fibers Leached in the pH 10 Borated Containment Water:
 Top part of the fibrous bed

42. Joint Glass Centre Vitrum Laugaricio (VILA)
CONTACT:
Joint Glass Centre Vitrum Laugaricio (VILA)
Študentská 2, Trenčín
Head: Prof. Dušan Galusek, DSc.
Tel. :
Fax :
E:-mail:

43. Thank you for your attention