spark plasma sintering of ultra high temperature ceramics

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Spark Plasma Sintering of Ultra High Temperature ceramics. Lili Nadaraia , Nikoloz Jalabadze , Levan Khundadze , Levan Lortkipanidze and Givi Sharashenidze. Georgian Technical University, Republic Center for Structure Researches (RCSR). [email protected]. UHTC. Application. Armor. - PowerPoint PPT Presentation

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Lili Nadaraia, Nikoloz Jalabadze, Levan Khundadze, Levan Lortkipanidze and Givi SharashenidzeSpark Plasma Sintering of Ultra High Temperature ceramics

Georgian Technical University, Republic Center for Structure Researches (RCSR)[email protected]

1UHTCApplicationUHTCArmor

Nozzles

Abrasives

Nuclear applicationsRefractory applications

Manufacturing methods of UHTCAdvantages and disadvantages of spark plasma sinteringAdvantages of spark plasma sintering:

Fastsinteringprocess;Uniform sintering;Lowgraingrowth (nano-grain materials may be prepared);Compaction and sintering stages are combined in one operation;Binders are not necessary;Better purification and activation of the powder particles surfaces;Different materials (Metals,Ceramics, composites) may be processed;High energy efficiency;Easy operation.

Disadvantages of spark plasma sintering:

Only simple symmetrical shapes may be prepared;Expensive pulsed DC generator is required.

Expensive SPS device

Fig.1. Scheme of the SPS the process of sintering PDC - pulsed DC, GD - graphite die, S powder sample, P pressure loading, EC- electric current, s spark, sp spark plasma and p- powder particles.SPS mechanism by SPS SYNTEX INC Company; (a) I- Flow direction of electrons during DC current,(b) I- Flow directions of electrons during AC current.Spark plasma between powder particleDC current shapes

Pulse DC current Shape in the developed device: a- at the frequency of 400 Hz, b- during different frequencies (T), different duration pulses (t) and different duration pauses (T-t); Current Shapes to be used after retrofitting the SPS device: during different frequencies (T), different duration pulses (t) and different duration pauses (T-t); SPS Device

Press molds for synthesize nanopowder (a) and sintering dense bodies (b) of composite materials 1-upper plug, 2-lower plug, 3-Matrix.

Sintering process a: Self-Propagating High-Temperature Synthesis (SHS), b: SPS accompanied with poly SHS.

A. G. Merzhanov. 2006, Advances in Science and Technology, 45, 36- 44. Self-propagating high-temperature synthesis (SHS), (combustion synthesis CS)Poly SHS BoridesTiB2 ZrB2HfB2 Titanium Diboride

X-Ray and SEM images of Titanium Diboridesa- TiB2 powder synthesis at 10000C 1h,b- sintered via SPS at 16000C ;C- SEM image of sintered via SPS at 16000CTiB2 Zirconium Diborides

ZrB2X-Ray and SEM images of Zirconium Diboridesa- ZrB2 powder synthesis at 10000C 1h,b- sintered via SPS at 16000C ;C- sintered via SPS at 17000CSEM images of Zirconium Diborides sintered via SPS at 17000CHafnium Diborides

X-Ray and SEM images of Hafnium Diborides sintered via SPS at 18000C ;HfB2 CarbidesTiC SiCB4CCarbides

TiC

SiCX-Ray images of Titanium Carbide sintered via SPS at 14000C -3 min;X-Ray images of Silicium Carbide sintered via SPS at 18000C -1 min;Boron Carbide

a- XRD pattern of B4C powder (SPS 14000C-3 min) b- SEM image of B4C bulk material (SPS 17000C-10min)

A-XRD patterns of B4C powder materials obtained by standard (a), SPS methods (b) ; B- SEM image of nanopowder B4C obtained by SPS method (14000C-3min).B4CComposition

SPS sintered B4C SiC (17000C-5min): a-X-ray diffraction pattern; c- SEM image B4C SiC Sintered via SPS b- SEM image of B4C SiC powder produce via SPS.

17Composition

X Ray of Ti3SiC2 composition of sintered via SPS at 14500C Composition

TiCTiB2X Ray and SEM images of TiB2 - TiC composition of sintered via SPS at 14500C Vickers hardness 29.5 Gpa Sample#Regime SPS-B4CpowderSPS-B4CSPSHfB2SPSTiB2SPS-B4C-SiCSPS- TiB2- TiC

SPS Ti3SiC2

SPSCurrent (V/A)9/13709.2/206010/27009/27009.5/230010/27009/2700Temp. (0C)1600170018001600170017001450Holding Time (min)51055556Pressure MPa0202025203030Density(% of theoretical)-948592959897SPS OPERATING MODES WITH RELATIVELY DENSITY

Shapes of materials sintered via SPSBallistic TestingSize of the plate -120x120mm; Size of the plate fragments 60x60mm; Weight - 50-100g.The plate presented a package armored with ballistic textile (Kevlar, tvarin, denima); Weight of the package was 0,6 0,8 kg; Fire tests were provided by shooting from the Mosins Rifle;Bullets - armor-piercingBullet Mass 10.80,1;Bullet speed - 86910 m/sec.Standard shooting method, distance - 10m towards a plasticine target.Backing material Plastic (Ti-6Al-4V)/textile Hard Blend (B4C, SiC, B4C-TiB2, B4C-SiC )Bullet directionTest is conducting according Standards of National Institute of Justice (NIJ) (type-IV)

Additional energy is absorbed by each successive layer of material in the ballistic panel.http://www.bodyarmornews.com/

Ballistic testing

120mmNIJ requirements - Max Back face signature (BFS) depth is 44mmBFS 40mmConclusionThere was developed new technology for manufacturing of nanocrystalline composite materials.Poly SHS process were detect during SPS and were use for UHTC materials fabricationDiborides of transaction metals Ti, Zr, Hf, were producedNanocrystalline Powders of carbides of metals Ti, Si, and B were obtain after Poly SHS processEffective composition materials TiB2 - TiC, Ti3SiC2, B4C - SiC were developed.Ballistic testing gives promising results and further effort will be directed to improve the characteristics. Modernization of SPS device is undergoing process (replacing of pulse DC current unit with pulse AC current unit). Further work will be directed to detect impacte of DC current at the sintering process and at the materials properties.

The part of research described in this presentation was made possible in scope of projects funded by Shota Rustaveli National Science Foundation. Project # 12/34 Presidential Grants for Young Scientists.

Acknowledgement

Thank you for attention

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