EP1922354A2 - Widerstandsfähiges keramikmaterial und herstellungsverfahren dafür - Google Patents

Widerstandsfähiges keramikmaterial und herstellungsverfahren dafür

Info

Publication number: EP1922354A2
Authority: EP; European Patent Office
Prior art keywords: sic; ceramic material; solid solution; resistant ceramic; aln
Prior art date: 2005-08-15
Legal status (The legal status is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the status listed.): Withdrawn

Application number

EP06780403A

Other languages

English (en)

French (fr)

Inventor

Avigdor Zangvil

Michael Katz

Current Assignee (The listed assignees may be inaccurate. Google has not performed a legal analysis and makes no representation or warranty as to the accuracy of the list.)

Carboshield Ltd

Original Assignee

Carboshield Ltd

Priority date (The priority date is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the date listed.)

2005-08-15

Filing date

2006-08-15

Publication date

2008-05-21

2006-08-15 Application filed by Carboshield Ltd filed Critical Carboshield Ltd

2008-05-21 Publication of EP1922354A2 publication Critical patent/EP1922354A2/de

Status Withdrawn legal-status Critical Current

Links

238000000034 method Methods 0.000 title claims abstract description 40
229910010293 ceramic material Inorganic materials 0.000 title claims abstract description 39
239000006104 solid solution Substances 0.000 claims abstract description 81
239000000843 powder Substances 0.000 claims abstract description 58
230000015572 biosynthetic process Effects 0.000 claims abstract description 31
238000003786 synthesis reaction Methods 0.000 claims abstract description 24
238000007596 consolidation process Methods 0.000 claims abstract description 19
239000011230 binding agent Substances 0.000 claims abstract description 18
238000003801 milling Methods 0.000 claims abstract description 18
238000005469 granulation Methods 0.000 claims abstract description 9
230000003179 granulation Effects 0.000 claims abstract description 9
238000005191 phase separation Methods 0.000 claims abstract description 8
238000012545 processing Methods 0.000 claims abstract description 7
229910010271 silicon carbide Inorganic materials 0.000 claims description 44
239000000463 material Substances 0.000 claims description 36
238000005245 sintering Methods 0.000 claims description 36
239000010936 titanium Substances 0.000 claims description 32
OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical compound [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 claims description 28
238000010438 heat treatment Methods 0.000 claims description 24
IJGRMHOSHXDMSA-UHFFFAOYSA-N Atomic nitrogen Chemical compound N#N IJGRMHOSHXDMSA-UHFFFAOYSA-N 0.000 claims description 22
229910052799 carbon Inorganic materials 0.000 claims description 18
239000007791 liquid phase Substances 0.000 claims description 15
238000002360 preparation method Methods 0.000 claims description 15
238000001272 pressureless sintering Methods 0.000 claims description 14
238000003825 pressing Methods 0.000 claims description 12
230000008569 process Effects 0.000 claims description 11
229910052723 transition metal Inorganic materials 0.000 claims description 11
150000003624 transition metals Chemical class 0.000 claims description 10
229910052782 aluminium Inorganic materials 0.000 claims description 9
238000007731 hot pressing Methods 0.000 claims description 9
229910001873 dinitrogen Inorganic materials 0.000 claims description 8
238000009740 moulding (composite fabrication) Methods 0.000 claims description 8
229910052710 silicon Inorganic materials 0.000 claims description 8
229910052719 titanium Inorganic materials 0.000 claims description 8
RTAQQCXQSZGOHL-UHFFFAOYSA-N Titanium Chemical compound [Ti] RTAQQCXQSZGOHL-UHFFFAOYSA-N 0.000 claims description 7
239000000654 additive Substances 0.000 claims description 7
230000001681 protective effect Effects 0.000 claims description 7
229910052761 rare earth metal Inorganic materials 0.000 claims description 7
150000002910 rare earth metals Chemical class 0.000 claims description 7
238000009694 cold isostatic pressing Methods 0.000 claims description 6
XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims description 6
238000001513 hot isostatic pressing Methods 0.000 claims description 5
230000001902 propagating effect Effects 0.000 claims description 5
ZOXJGFHDIHLPTG-UHFFFAOYSA-N Boron Chemical compound [B] ZOXJGFHDIHLPTG-UHFFFAOYSA-N 0.000 claims description 4
QCWXUUIWCKQGHC-UHFFFAOYSA-N Zirconium Chemical compound [Zr] QCWXUUIWCKQGHC-UHFFFAOYSA-N 0.000 claims description 4
229910052796 boron Inorganic materials 0.000 claims description 4
150000001639 boron compounds Chemical class 0.000 claims description 4
150000004767 nitrides Chemical class 0.000 claims description 4
229910052726 zirconium Inorganic materials 0.000 claims description 4
LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 claims description 3
238000002485 combustion reaction Methods 0.000 claims description 2
238000010316 high energy milling Methods 0.000 claims description 2
229910052727 yttrium Inorganic materials 0.000 claims description 2
VWQVUPCCIRVNHF-UHFFFAOYSA-N yttrium atom Chemical compound [Y] VWQVUPCCIRVNHF-UHFFFAOYSA-N 0.000 claims description 2
229910018540 Si C Inorganic materials 0.000 claims 1
229910052769 Ytterbium Inorganic materials 0.000 claims 1
NAWDYIZEMPQZHO-UHFFFAOYSA-N ytterbium Chemical compound [Yb] NAWDYIZEMPQZHO-UHFFFAOYSA-N 0.000 claims 1
239000000243 solution Substances 0.000 abstract description 4
238000011068 loading method Methods 0.000 abstract description 3
HBMJWWWQQXIZIP-UHFFFAOYSA-N silicon carbide Chemical compound [Si+]#[C-] HBMJWWWQQXIZIP-UHFFFAOYSA-N 0.000 description 43
PMHQVHHXPFUNSP-UHFFFAOYSA-M copper(1+);methylsulfanylmethane;bromide Chemical compound Br[Cu].CSC PMHQVHHXPFUNSP-UHFFFAOYSA-M 0.000 description 30
239000000203 mixture Substances 0.000 description 30
238000006243 chemical reaction Methods 0.000 description 24
239000002245 particle Substances 0.000 description 20
239000000047 product Substances 0.000 description 20
239000000919 ceramic Substances 0.000 description 14
229910002804 graphite Inorganic materials 0.000 description 13
239000010439 graphite Substances 0.000 description 13
239000007795 chemical reaction product Substances 0.000 description 10
238000001816 cooling Methods 0.000 description 10
229910052757 nitrogen Inorganic materials 0.000 description 10
PNEYBMLMFCGWSK-UHFFFAOYSA-N aluminium oxide Inorganic materials [O-2].[O-2].[O-2].[Al+3].[Al+3] PNEYBMLMFCGWSK-UHFFFAOYSA-N 0.000 description 9
239000008367 deionised water Substances 0.000 description 9
238000002156 mixing Methods 0.000 description 9
KFZMGEQAYNKOFK-UHFFFAOYSA-N Isopropanol Chemical compound CC(C)O KFZMGEQAYNKOFK-UHFFFAOYSA-N 0.000 description 8
229910000831 Steel Inorganic materials 0.000 description 8
XAGFODPZIPBFFR-UHFFFAOYSA-N aluminium Chemical compound [Al] XAGFODPZIPBFFR-UHFFFAOYSA-N 0.000 description 8
TWNQGVIAIRXVLR-UHFFFAOYSA-N oxo(oxoalumanyloxy)alumane Chemical compound O=[Al]O[Al]=O TWNQGVIAIRXVLR-UHFFFAOYSA-N 0.000 description 8
239000010959 steel Substances 0.000 description 8
PEDCQBHIVMGVHV-UHFFFAOYSA-N Glycerine Chemical compound OCC(O)CO PEDCQBHIVMGVHV-UHFFFAOYSA-N 0.000 description 6
XUIMIQQOPSSXEZ-UHFFFAOYSA-N Silicon Chemical compound [Si] XUIMIQQOPSSXEZ-UHFFFAOYSA-N 0.000 description 6
238000002441 X-ray diffraction Methods 0.000 description 6
239000012300 argon atmosphere Substances 0.000 description 6
239000010703 silicon Substances 0.000 description 6
239000002002 slurry Substances 0.000 description 6
SIWVEOZUMHYXCS-UHFFFAOYSA-N oxo(oxoyttriooxy)yttrium Chemical compound O=[Y]O[Y]=O SIWVEOZUMHYXCS-UHFFFAOYSA-N 0.000 description 5
239000012071 phase Substances 0.000 description 5
229910000760 Hardened steel Inorganic materials 0.000 description 4
239000004372 Polyvinyl alcohol Substances 0.000 description 4
238000004320 controlled atmosphere Methods 0.000 description 4
238000002425 crystallisation Methods 0.000 description 4
230000008025 crystallization Effects 0.000 description 4
229920002451 polyvinyl alcohol Polymers 0.000 description 4
239000002994 raw material Substances 0.000 description 4
239000010935 stainless steel Substances 0.000 description 4
229910001220 stainless steel Inorganic materials 0.000 description 4
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239000002131 composite material Substances 0.000 description 3
235000011187 glycerol Nutrition 0.000 description 3
229920001903 high density polyethylene Polymers 0.000 description 3
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238000012986 modification Methods 0.000 description 3
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238000012360 testing method Methods 0.000 description 3
WFKWXMTUELFFGS-UHFFFAOYSA-N tungsten Chemical compound [W] WFKWXMTUELFFGS-UHFFFAOYSA-N 0.000 description 3
RUDFQVOCFDJEEF-UHFFFAOYSA-N yttrium(III) oxide Inorganic materials [O-2].[O-2].[O-2].[Y+3].[Y+3] RUDFQVOCFDJEEF-UHFFFAOYSA-N 0.000 description 3
PIGFYZPCRLYGLF-UHFFFAOYSA-N Aluminum nitride Chemical compound [Al]#N PIGFYZPCRLYGLF-UHFFFAOYSA-N 0.000 description 2
LTPBRCUWZOMYOC-UHFFFAOYSA-N Beryllium oxide Chemical compound O=[Be] LTPBRCUWZOMYOC-UHFFFAOYSA-N 0.000 description 2
239000002202 Polyethylene glycol Substances 0.000 description 2
239000007864 aqueous solution Substances 0.000 description 2
150000001875 compounds Chemical class 0.000 description 2
239000002270 dispersing agent Substances 0.000 description 2
238000007580 dry-mixing Methods 0.000 description 2
238000001035 drying Methods 0.000 description 2
239000007789 gas Substances 0.000 description 2
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239000004570 mortar (masonry) Substances 0.000 description 2
239000004014 plasticizer Substances 0.000 description 2
229920001223 polyethylene glycol Polymers 0.000 description 2
230000035939 shock Effects 0.000 description 2
-1 transition metal carbon nitrides Chemical class 0.000 description 2
229910052721 tungsten Inorganic materials 0.000 description 2
239000010937 tungsten Substances 0.000 description 2
229910052984 zinc sulfide Inorganic materials 0.000 description 2
VBICKXHEKHSIBG-UHFFFAOYSA-N 1-monostearoylglycerol Chemical compound CCCCCCCCCCCCCCCCCC(=O)OCC(O)CO VBICKXHEKHSIBG-UHFFFAOYSA-N 0.000 description 1
229910000838 Al alloy Inorganic materials 0.000 description 1
238000007088 Archimedes method Methods 0.000 description 1
XKRFYHLGVUSROY-UHFFFAOYSA-N Argon Chemical compound [Ar] XKRFYHLGVUSROY-UHFFFAOYSA-N 0.000 description 1
RYGMFSIKBFXOCR-UHFFFAOYSA-N Copper Chemical compound [Cu] RYGMFSIKBFXOCR-UHFFFAOYSA-N 0.000 description 1
DCXXMTOCNZCJGO-UHFFFAOYSA-N Glycerol trioctadecanoate Natural products CCCCCCCCCCCCCCCCCC(=O)OCC(OC(=O)CCCCCCCCCCCCCCCCC)COC(=O)CCCCCCCCCCCCCCCCC DCXXMTOCNZCJGO-UHFFFAOYSA-N 0.000 description 1
WHXSMMKQMYFTQS-UHFFFAOYSA-N Lithium Chemical compound [Li] WHXSMMKQMYFTQS-UHFFFAOYSA-N 0.000 description 1
239000006057 Non-nutritive feed additive Substances 0.000 description 1
239000004698 Polyethylene Substances 0.000 description 1
VYPSYNLAJGMNEJ-UHFFFAOYSA-N Silicium dioxide Chemical compound O=[Si]=O VYPSYNLAJGMNEJ-UHFFFAOYSA-N 0.000 description 1
229910002795 Si–Al–O–N Inorganic materials 0.000 description 1
239000002253 acid Substances 0.000 description 1
150000007513 acids Chemical class 0.000 description 1
229910052786 argon Inorganic materials 0.000 description 1
239000012298 atmosphere Substances 0.000 description 1
239000011324 bead Substances 0.000 description 1
238000010296 bead milling Methods 0.000 description 1
INAHAJYZKVIDIZ-UHFFFAOYSA-N boron carbide Chemical compound B12B3B4C32B41 INAHAJYZKVIDIZ-UHFFFAOYSA-N 0.000 description 1
150000003841 chloride salts Chemical class 0.000 description 1
229910052802 copper Inorganic materials 0.000 description 1
239000010949 copper Substances 0.000 description 1
229910001610 cryolite Inorganic materials 0.000 description 1
230000007423 decrease Effects 0.000 description 1
230000007812 deficiency Effects 0.000 description 1
238000000280 densification Methods 0.000 description 1
238000001739 density measurement Methods 0.000 description 1
238000011161 development Methods 0.000 description 1
229910003460 diamond Inorganic materials 0.000 description 1
239000010432 diamond Substances 0.000 description 1
238000009792 diffusion process Methods 0.000 description 1
239000006185 dispersion Substances 0.000 description 1
238000000227 grinding Methods 0.000 description 1
230000007062 hydrolysis Effects 0.000 description 1
238000006460 hydrolysis reaction Methods 0.000 description 1
238000011065 in-situ storage Methods 0.000 description 1
238000001746 injection moulding Methods 0.000 description 1
150000002500 ions Chemical class 0.000 description 1
238000004093 laser heating Methods 0.000 description 1
239000007788 liquid Substances 0.000 description 1
229910052744 lithium Inorganic materials 0.000 description 1
238000005461 lubrication Methods 0.000 description 1
238000005259 measurement Methods 0.000 description 1
229910052751 metal Inorganic materials 0.000 description 1
239000002184 metal Substances 0.000 description 1
150000002739 metals Chemical class 0.000 description 1
239000011812 mixed powder Substances 0.000 description 1
239000003607 modifier Substances 0.000 description 1
238000000465 moulding Methods 0.000 description 1
239000012299 nitrogen atmosphere Substances 0.000 description 1
239000003921 oil Substances 0.000 description 1
238000000879 optical micrograph Methods 0.000 description 1
230000008520 organization Effects 0.000 description 1
UZLYXNNZYFBAQO-UHFFFAOYSA-N oxygen(2-);ytterbium(3+) Chemical compound [O-2].[O-2].[O-2].[Yb+3].[Yb+3] UZLYXNNZYFBAQO-UHFFFAOYSA-N 0.000 description 1
230000035515 penetration Effects 0.000 description 1
229920000573 polyethylene Polymers 0.000 description 1
229920000642 polymer Polymers 0.000 description 1
238000001556 precipitation Methods 0.000 description 1
239000002243 precursor Substances 0.000 description 1
238000003672 processing method Methods 0.000 description 1
238000005086 pumping Methods 0.000 description 1
238000009717 reactive processing Methods 0.000 description 1
230000009467 reduction Effects 0.000 description 1
230000003014 reinforcing effect Effects 0.000 description 1
150000003839 salts Chemical class 0.000 description 1
238000004062 sedimentation Methods 0.000 description 1
238000007873 sieving Methods 0.000 description 1
238000002791 soaking Methods 0.000 description 1
238000001330 spinodal decomposition reaction Methods 0.000 description 1
238000001694 spray drying Methods 0.000 description 1
238000006467 substitution reaction Methods 0.000 description 1
239000004094 surface-active agent Substances 0.000 description 1
230000002195 synergetic effect Effects 0.000 description 1
230000007704 transition Effects 0.000 description 1
238000011282 treatment Methods 0.000 description 1
UONOETXJSWQNOL-UHFFFAOYSA-N tungsten carbide Chemical compound [W+]#[C-] UONOETXJSWQNOL-UHFFFAOYSA-N 0.000 description 1
238000009736 wetting Methods 0.000 description 1
229940075624 ytterbium oxide Drugs 0.000 description 1
229910003454 ytterbium oxide Inorganic materials 0.000 description 1

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- C04B35/591—Shaped ceramic products characterised by their composition; Ceramics compositions; Processing powders of inorganic compounds preparatory to the manufacturing of ceramic products based on non-oxide ceramics based on borides, nitrides, i.e. nitrides, oxynitrides, carbonitrides or oxycarbonitrides or silicides based on silicon nitride obtained by reaction sintering
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- C04B35/00—Shaped ceramic products characterised by their composition; Ceramics compositions; Processing powders of inorganic compounds preparatory to the manufacturing of ceramic products
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- C04B35/584—Shaped ceramic products characterised by their composition; Ceramics compositions; Processing powders of inorganic compounds preparatory to the manufacturing of ceramic products based on non-oxide ceramics based on borides, nitrides, i.e. nitrides, oxynitrides, carbonitrides or oxycarbonitrides or silicides based on silicon nitride
- C04B35/593—Shaped ceramic products characterised by their composition; Ceramics compositions; Processing powders of inorganic compounds preparatory to the manufacturing of ceramic products based on non-oxide ceramics based on borides, nitrides, i.e. nitrides, oxynitrides, carbonitrides or oxycarbonitrides or silicides based on silicon nitride obtained by pressure sintering
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- C04B35/632—Organic additives
- C04B35/634—Polymers
- C04B35/63404—Polymers obtained by reactions only involving carbon-to-carbon unsaturated bonds
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- C04B35/638—Removal thereof
- F—MECHANICAL ENGINEERING; LIGHTING; HEATING; WEAPONS; BLASTING
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- F41H—ARMOUR; ARMOURED TURRETS; ARMOURED OR ARMED VEHICLES; MEANS OF ATTACK OR DEFENCE, e.g. CAMOUFLAGE, IN GENERAL
- F41H5/00—Armour; Armour plates
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- F41H5/0414—Layered armour containing ceramic material
- F—MECHANICAL ENGINEERING; LIGHTING; HEATING; WEAPONS; BLASTING
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- F41H5/04—Plate construction composed of more than one layer
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Definitions

the present invention relates to a method of preparing a resistant ceramic material by consolidation of SiC-AlN solution powder, and to novel resistant ceramic material comprising primarily a homogeneous SiC-AlN solid solution or a homogeneous SiC-AlN solid solution that underwent phase separation, used for military and civil armor, and products that can withstand dynamic loading and are also wear resistant.
SiC silicon carbide
AlN aluminum nitride
Al 2 O 3 aluminum oxide
B 4 C boron carbide
Aluminum Nitride is resistant to attack by most molten metals, most notably aluminum, lithium and copper. AlN is resistant to attack from most molten salts including chlorides and cryolite; it has high thermal conductivity for a ceramic material (second only to beryllia); AlN has high electrical resistivity; and has high dielectric strength; AlN may be attacked by acids and alkalis; and in the powder form is susceptible to hydrolysis by water or humidity.
Silicon Carbide is highly wear resistant and also has good mechanical properties, including high temperature strength and thermal shock resistance.
Bulk SiC as a technical ceramic, is produced in two main ways. Reaction bonded SiC is made by infiltrating compacts made of mixtures of SiC and Carbon with liquid Silicon. The Silicon reacts with the Carbon forming SiC. The reaction product bonds the SiC particles.
Sintered SiC is produced from pure SiC powder with oxide or non-oxide sintering aids. Conventional ceramic forming processes are used and the material is sintered in an inert atmosphere at temperatures up to 2000 0 C or higher.
the aim of the present invention is the development of an impact resistant ceramic material, which is applicable for manufacture of inexpensive, uniform, controllable and lightweight armor tiles and other articles.
this invention provides a method of preparing a resistant ceramic material by consolidation of a SiC-AlN solid solution powder comprising a. synthesis of a SiC-AlN solid solution, followed by b. processing steps comprising part or all of: crushing, milling, sinter-aid addition, binder addition, granulation (if cold-pressed or hot-pressed), cold forming, consolidation and heat treatment.
this invention provides a resistant ceramic material comprising primarily a homogeneous SiC-AlN solid solution. [009] hi one embodiment, this invention provides a resistant ceramic material comprising primarily a homogeneous SiC-AlN solid solution, which underwent phase separation.
Fig. 1 is an X-ray diffraction pattern of the synthesized and milled SiC-AlN solution powder, similar to that obtained in EXAMPLE 3 below, but with a 1 :1 ratio of SiC:AlN in the solid solution. It shows the typical peaks (at the correct locations and relative intensities) of a SiC-AlN solid solution with approximately 50% SiC and 50% AlN.
Fig. 2 is an X-ray diffraction pattern of the synthesized and milled SiC-AlN solution powder with Ti(QN) particles, similar to that obtained in EXAMPLE 2 below. It shows the typical peaks (at the correct locations and relative intensities) of a SiC-AlN solid solution with approximately 60% SiC and 40% AlN and also of Ti(QN).
Fig. 3 is an optical micrograph of a polished and etched sample from a tile, similar to that obtained in EXAMPLE 3 below. It shows a dense, fined grained microstructure of the solid solution without visible porosity.
Fig. 4 shows square and hexagonal SiC-AlN sintered armor tiles, similar to those described in EXAMPLE 3, on an aluminum alloy block.
the present invention relates to a method of preparing a resistant ceramic material by consolidation of SiC-AlN solid solution powder, and to novel resistant ceramic material comprising primarify a homogeneous SiC-AlN solid solution or a homogenous SiC-AlN solid solution that underwent phase separation, that may be used for military and civil armor, and products that can withstand dynamic loading and are also wear resistant.
SiC and AlN are promising armor materials, although AlN has been of much less interest.
SiC is a highly covalent compound (82%), while AlN is less covalent (57%).
Solid solutions and composites of the two materials have several important advantages for ballistic applications.
the sintering temperature necessary for densification is lower for a SiC-AlN solid solution than for SiC alone.
AlN can help reduce the amount of additives necessary for pressureless sintering (AlN itself can be used a sintering aid to SiC).
SiC and AlN allow good control of the microstructure (e.g., size and shape of crystallites, structure modulation), both during the initial formation of the microstructure and in subsequent treatments.
the SiC-AlN system is among only a few ceramic systems (another important one is the Si-Al-O-N system) where extensive solid solutions can form.
the SiC-AlN system possesses a miscibility gap, where precipitation or spinodal decomposition can occur by soaking the solid solution at certain temperatures, thus improving mechanical properties.
the addition of AlN can potentially improve antiballistic performance, because it is known to possess a structural transition at high shock wave velocity. Because of all these reasons, materials in the SiC-AlN system can have superior ballistic performance (a synergistic effect), if engineered properly, in spite of the fact that AlN itself has lower performance than that of SiC. At the same time, these materials can be processed more easily and more effectively than SiC itself.
the formation of the SiC-AlN solid solution from SiC and AlN requires temperatures of 2100° to 2300 0 C. if powders having particle sizes in the order of micrometers or larger are used. TWs can be achieved only by hot-pressing, because pressureless sintering is not practical at such temperatures due to material loss. Hot-pressing is a very expensive process, and renders the articles produced by it unaffordable for many armor or wear applications. In addition, hot-pressing does not allow the production of large or complicated parts. In addition, even at such high temperatures, the solid solution that is obtained is inhomogeneous: it contains regions with considerably variable SiC: AlN ratios, a fact that makes it extremely difficult to obtain reproducible microstructures and properties.
such homogeneous solid solution powders are produced by an in situ reactive process from certain precursors, rather than from mixtures of SiC and AlN.
the resulting solid solution product undergoes processing steps such as milling, sinter- aid addition, binder addition, granulation, cold forming, and final consolidation.
processing steps such as milling, sinter- aid addition, binder addition, granulation, cold forming, and final consolidation.
the parameters of each of these steps are specifically determined so as to fit the solid solution composition, and are generally different from parameters used for processing of SiC, AlN, or SiC+ AlN mixtures.
the present invention provides a method of preparing a resistant ceramic material by consolidation of a SiC-AlN solid solution powder comprising a) synthesis of a SiC-AlN solid solution, followed by b) processing steps comprising part or all of: crushing, milling, sinter-aid addition, binder addition, granulation (if cold-pressed or hot-pressed), cold forming, consolidation and heat treatment.
carbide, nitride, or carbo-nitride of a transition metal is embedded in step (a) or step (b).
the transition metal is Titanium or Zirconium.
the SiC-AlN solid solution may be homogeneous.
homogeneous solid solution of non-modulated structure includes SiC:AlN constant ratios within 10% error.
homogeneous solid solution of modulated structure includes SiC: AlN constant ratios within 10% error, when local composition is measured over areas larger than the modulation wavelength.
the microstructure of a SiC-AlN solid solution may consist of single- phase crystallites, homogeneous, without large deviation of composition from point to point within each crystallite; in another embodiment crystallites that exhibit a phase-separated structure, including modulation of compositions, with alternating regions that are richer and poorer in AlN content. In another embodiment, such modulated structures have been reported to contribute to the fracture toughness of the material.
the average crystallite size (or grain size) of a SiC-AlN solid solution is between about 0.1 micrometers and 10 micrometers.
a SiC-AlN solid solution constitutes between 60 and 99% of the weight of the article.
LQ another embodiment the method of preparation of homogeneous SiC-AlN solid solution including self propagating high temperature synthesis (SHS) via combustion nitridation of aluminum, silicon and carbon (Al-Si-C) or aluminum and silicon carbide (Al-SiC) under nitrogen gas pressure of up to 50 bar.
SHS high temperature synthesis
the raw dry-mixed powder of aluminum, silicon and carbon or aluminum and SiC is poured into a carbon felt-lined perforated stainless steel reactor or a similar gas-permeable reactor, then pressed or shaken to achieve a desirable bulk density and the reactor placed in a pressure chamber, where nitrogen gas pressure is applied.
ignition of the powder is achieved by tungsten wire heating, graphite strip heating, laser heating or similar means; the reaction propagates downwards and complete reaction is achieved.
the reactor and reaction propagation is in horizontal direction.
the SHS method of solid solution can be described by the following two exothermic reaction paths: xAl +x/2.N 2 (g) + (l-x)Si + (l-x)C ⁇ xAlN + (l-x)SiC (1) xAl +x/2.N 2 (g) + (l-x)SiC ⁇ xAIN + (l-x)SiC (2)
a transition metal powder is added and mixed with the Al-Si-C powders, to obtain, for example, Ti(C 5 N) as separate particles along with or embedded in the SiC-AlN solid solution particles.
This additional reaction path is:
Addition of a transition metal powder provides (a) the formation of TiC from Ti and C is more exothermic than the formation of SiC from Si and C, although less exothermic than the formation of AlN from Al and N 2 .
the addition of Ti allows to obtain a stable reaction with higher Si: Al ratios,
the Ti carbonitride particles can act as a toughening phase.
the molecular ratio (which is also close to the weight ratio) of the SiC-AlN solid solution obtained is between about 92:8 to about 50:50.
the solid solution can be processed in water, in contrast to mixtures containing AlN powder (not in solid solution), which react with water.
the reaction product of (a) (sponge-like product, SiC-AlN solid solution in the SHS process) is crushed in a jaw crusher or by other means, and sieved to ⁇ 250 ⁇ m size powder.
the powder particles themselves are composed of micrometer-sized crystallites, and this fine grained material is easy (relative to SiC) to further comminute.
milling includes wet-vibration-milling in cylindrical rubber-lined steel containers with water or alcohol, and either tungsten carbide or SiC or SiC-AlN milling media such as WC, SiC or SiC-AlN.
the water is de-ionized water
the alcohol is isopropanol.
the containers are mounted on a vibrating plate, activated by a vibratory motor, for a time sufficient to reduce the average particle size to around 1 micrometer.
milling is done in rubber-lined containers or in SiC containers on an attrition miller.
wet bead milling with 1-2 mm ceramic beads is used.
sub-micron powder is obtained by a high energy milling method, such as those mentioned above.
sintering aids for liquid phase sintering are a mixture of oxides of aluminum and yttrium and/or a rare earth (RE) element which are added to the powder.
the mixture is homogenized in a ball mill using steel balls and de-ionized water.
total quantities of oxide additives for liquid phase sintering ranges between 4wt% and 25wt%, or smaller amounts (usually ⁇ 2%) of oxides, carbon, boron and/or boron compounds are added for non-liquid phase sintering.
the final materials contain oxide or oxynitride intergranular phases, which are essentially products of the oxide sintering aid.
the weight ratio between alumina and the sum of [yttria + RE] is between 2 and 0.4.
a binder is added if cold-pressing follows this step.
a binder mixture based on polyethylene glycol (PEG) or polyvinyl alcohol (PVA) is added.
a plasticizer such as glycerin is included in the binder mixture; in another embodiment, additional minor additives are included in the binder mixture to improve lubrication.
the weight percent of binder mixture, relative to powder weight can be from about 2% to about 14%.
granulation includes squeezing a moisture controlled mixture through mesh, in another embodiment it includes palletizing, in another embodiment it includes a spray drying process, in another embodiment achieving a granulated ready-to-press material with free pouring density of about 600-800 kg/m 3 and a tap density of about 800-1200 kg/m 3 .
granule sizes are generally between 40 and 400 micrometers.
uniaxial cold pressing in hardened steel dies (which may be equipped with harder inserts to reduce wear) is performed at pressures in the order of 1 ,000 bar.
cold isostatic pressing at up to 4,000 bar may be added if higher final properties are desired.
usable molding compositions include, in addition to the ceramic powder and major binder component, several minor organic components such as plasticizers for the main polymer which are intended as flow modifiers, and in another embodiment processing aids which are supposed to act as surfactants, to the ceramic and improve particle wetting.
binder removal (also called debinding or dewaxing) is done in flowing Nitrogen gas by slow heating at 10° to 100 0 C per hour to temperatures between 450° and 600 0 C, holding up to 4 hours at the maximum temperature, and cooling down at a controlled slow rate or cooling down naturally with the furnace.
pressureless sintering is performed in Argon or Nitrogen atmosphere in a controlled atmosphere furnace at temperatures from 1850° to 2000 0 C and non-flowing gas pressure of less than 1 bar.
the temperature is preferably between 1870° and 1950 0 C.
the "green" tiles are enclosed in covered graphite containers; in another embodiment the "green” tiles are embedded in coarse SiC or SiC + Al 2 O 3 powder in covered graphite containers.
the heating rate is between 150° and 900 0 C per hour.
the holding time at the maximum temperature is between 10 minutes and 6 hours, preferably 30 minutes to 4 hours.
Green tiles refer to cold formed tiles before final consolidation.
phase separation is optionally performed in the last step of the sintering of the solid solution powder, while reducing the sintering temperature to 1500-1900 0 C for 1 to 24 hours or more, resulting in a modulated structure.
the phase separation may be performed as a separate step after the sintering step, by heating the sintering product to 1500-1900 0 C for 1-24 hours or more, resulting in a modulated structure.
a key to the success of this process is the homogeneity of the solid solution obtained in the preparation of a SiC-AlN solid solution.
hot isostatic pressing can be performed after the sintering step to provide higher density and better performance.
hot pressing of the homogeneous solid solution powder may be performed.
Hot isostatic pressing is done at high temperature under high gas pressure.
Hot pressing is a mechanical uniaxial pressure under heating conditions.
the ceramic bodies may be used as-sintered (and heat-treated, if applicable), or may undergo diamond wheel grinding to achieve more accurate shape and dimensions.
the consolidation of the SiC-AlN solid solution and Ti(C,N) powder into resistant ceramic material includes cold pressing and/or cold isostatic pressing followed by liquid phase assisted pressureless sintering or non-liquid-phase sintering.
the consolidation of the SiC-AlN solid solution and Ti(C 5 N) powder into resistant ceramic material comprises hot pressing.
the consolidation comprises cold- pressing and/or cold-isostatic-pressing followed by non-liquid-phase-assisted pressureless sintering.
the sintering additives may comprise small amounts of alumina, carbon, boron and boron compounds, and the sintering temperature may be higher than in liquid phase sintering.
the consolidation of the SiC-AlN solid solution powder into a resistant ceramic material is achieved by sintering followed by hot isostatic pressing.
the cold forming process comprises cold pressing and/or cold isostatic pressing followed by non-liquid-phase assisted pressureless sintering.
this invention provides a resistant ceramic material comprising primarily a homogeneous SiC-AlN solid solution.
the SiC-AlN solid solution may comprise carbide, nitride or carbo-nitride of a transition metal, in anther embodiment the transition metal is titanium or zirconium.
another way to improve fracture toughness and ballistic performance is to include reinforcing titanium carbo- nitride particles.
a resistant ceramic material of this invention may be used for the preparation of an armor material, in another embodiment for the preparation of a protective personal waistcoats, in another embodiment for the preparation of antiballistic resistance, in another embodiment for the preparation of a resisting to armor piercing bullets or in another embodiment for the preparation of an armor for light vehicles.
a resistant ceramic material comprising 65 to 94 wt % of a highly homogeneous SiC-AlN solid solution (wherein AlN content is from about 8 wt % to about 50 wt %).
a resistant ceramic composite material comprise 0.5 to 18 wt% titanium carbonitride Ti(C,N).
a resistant composite ceramic material comprise up to 25 wt % of multiphase product of reaction and crystallization of melt of the following oxides mixture: aluminum oxide (AI2O3), yttrium oxide (Y 2 O 3 ), a negligible amount of silica (SiO 2 ), and optionally ytterbium oxide (Yb2 ⁇ 3 ) or another rare earth (RE) oxide.
AI2O3 aluminum oxide
Y 2 O 3 yttrium oxide
SiO 2 a negligible amount of silica
Yb2 ⁇ 3 optionally ytterbium oxide
RE rare earth
the shapes and dimensions of the components can be: tiles in sizes from about 2" x 2" (about 50mm x 50mm) to 300mm x 300mm or more, with or without curvatures; hexagonal tiles; rods; spheres; or more complex shapes.
Example 1 Preparation of ceramic armor tiles including Ti (CN) EXAMPLE 1 [0055]
the tiles had a square shape with nominal dimensions 50 x 50 mm and thickness of 6 to 6.5 mm.
the armor tiles were manufactured from a material with the following nominal content of components:
SHS Self Propagating High-temperature Synthesis. Poured 37.5g of the powder mixture layer by layer into a cylindrical perforated stainless steel reactor (lined with graphite felt; inner diameter about 25 mm, height 70mm) and lightly tapped layer by layer to obtain a uniform bulk density of about 900 kg/m 3 . Mounted the reactor in the pressure chamber and sealed the chamber. Pressurized with nitrogen gas at 35 bar. Ignited using a tungsten filament at a distance of about 1 mm above the surface of the powder.
Reaction front downwards propagation was videotaped through the view port in the chamber wall, and temperatures were measured and recorded using 4 Type C thermocouples (one near the filament and 3 along the reaction path, inserted horizontally about 2mm deep into the powder). Ignition temperature was about 1350 0 C and the temperatures along the reaction path reached between 2000 and 2300 0 C. The reaction was complete within about 2 minutes.
Crushing of the reaction product The SHS reaction product was removed as one piece of a porous body from the carbon felt insulator. It was then crushed in a mortar and pestle, and sieved to obtain ⁇ 250 micrometer particles. d) Steps (b) and (c) were repeated for 2 more batches of 37.5g each.
the net weight of the product for each of the three runs was about 42 grams (the error being about 0.3 g due to some product adhering to the carbon felt insulation).
the weight addition of about 4.3-4.5 g (from the original 37.5 g) represents the added nitrogen, theoretically about
Vibratory milling was done in a rubber-lined steel container, having a volume of about 225cc.
the 3 batches of powder were loaded into the container, together with isopropyl alcohol (about 70cc) and about 600 grams of 8mm WC-6wt.°/ ⁇ Co balls as milling media.
the mill was operated for 48 hours at a frequency of 50Hz (3,000 R.P.M.) and amplitude of about 5mm.
the materials were then removed and dried in air at room temperature.
the dried powder was then dispersed in de-ionized water with 0.4% addition of DARV AN-C® dispersant, using an ultrasonic bath for 30 minutes.
X-ray diffraction has shown that the milled reaction products were 2H (wurtzite)-SiC-AlN solid solution, sometimes with a minor amount of residual silicon, depending on initial composition. The peak intensities are in agreement with reported values for the solid solution. No peaks of SiC or AlN are seen, and there is no indication of any deviation from a homogeneous solid solution. In addition, peaks of cubic titanium carbo-nitride [Ti(C 5 N)] are observed. g) Sintering aids addition. In this example, 7.2 grams (6wt%) of alumina and 4.8 grams
the "green” tiles were loaded into a covered graphite container, separated from each other with graphite felt sheets.
the sintering cycle was as follows: Heating to 1,000 0 C at 400 °C/h heating rate, then to 1900 0 C at 900 0 CZh, then to 1920 0 C at 50 0 CZIi; holding 1 hour at 1920 0 C; cooling at 600 0 CZIi to room temperature.
Example 2 the tiles had a square shape with nominal dimensions 50 x 50 mm and thickness of between 6mm and 7mm.
the armor tiles have been manufactured from material with following nominal content of components: (a) 85.4wt% of SiC-AlN solid solution, wherein AlN content was 30wt%; (b) 6.6wt% of Ti(C,N) particles; (c) 8wt % of multiphase product of crystallization of the melt of oxide mixture with the following composition: AI2O3 — 40wt %, and Y2O3 - 40wt%.
Steps (b) and (c) were repeated for 2 more batches of 33.0g each.
Vibratory milling, powder dispersion and XRD were done as in EXAMPLE 1, Item 5, with similar results.
4.52 grams (4wt%) of alumina and 4.52 grams (4wt%) of yttria both with particle size of 0.5-1.0 micrometers were added to 104 grams of the SiC-AlN solid solution + Ti(CN) powder (in aqueous slurry), then mixed-homogenized in a ball mill using alumina cylinders as mixing media and de- ionized water for 16 hours.
Binder addition and granulation were used for 2 more batches of 33.0g each.
the tiles had a square shape with nominal dimensions 50 x 50 mm and thickness of between 6mm. and 9mm.
the armor tiles have been manufactured from material with the following nominal content of components:
Ig of the powder mixture layer by layer into an oval perforated stainless steel reactor (lined with carcon felt, inner cross section about 18cm 2 , height 100mm) and lightly pressed layer by layer to obtain a uniform bulk density of about 900kg/m 3 . Mounted the reactor in the pressure chamber and sealed the chamber. Pressurized with nitrogen gas at 35 bar.
the net weight of the product for each of the three runs was between 185 and 186 grams (the error being about 0.5 g due to some product adhering to the carbon felt insulation).
the weight addition of 25-26g represents the added nitrogen, theoretically 25.7g for a full reaction (1) shown above.
the yield of SiC-AlN solid solution could be determined by dividing the added weight by 25.7, showing values from 99 to 100%. This means that practically all the aluminum reacted with nitrogen (and all the Si with carbon) to form the solid solution, and also that practically no materials were lost as gaseous phases.
the bulk density of the sponge-like product was approximately 1,000 kg/m 3 . e) Vibratory milling to obtain micron-size particles.
Vibratory milling was done in 2 rubber-lined steel containers, having a volume of about 450cc each, attached vertically on the vibrating plate.
the 3 batches of powder were manually mixed in a bowl, divided into two equal parts (about 27Og each) and loaded into the two vibratory mill containers, together with isopropyl alcohol (about 200cc) and 8mm WC-6wt.%Co balls (about 1,300 grams).
the mill was operated for 54 hours at a frequency of 50Hz and amplitude of about 5mm. The materials were then removed and dried in air at room temperature.
X-ray diffraction has shown that the milled reaction products were 2H (wurtzite)-SiC-AlN solid solution, sometimes with a minor amount of residual silicon, depending on initial composition. The peak intensities are in agreement with reported values for the solid solution. No peaks of SiC or AlN are seen, and there is no indication of any deviation from a homogeneous solid solution.
Sedimentation was done by adding de-ionized water to the powder and adding 0.4% (relative to powder weight) of Darvan-C® as a dispersant, dispersing and mixing for 60 minutes in an ultrasonic bath, poured into a 400mm tall 2 liter measuring cylinders, then letting settle for 100 minutes and pumping out the top 95% of the volume of the slurry for use in the following steps.
Sintering aids addition was done by adding de-ionized water to the powder and adding 0.4% (relative to powder weight) of Darvan-C® as a dispersant, dispersing and mixing for 60 minutes in an ultrasonic bath, poured into a 400mm tall 2 liter measuring cylinders, then letting settle for 100 minutes and pumping out the top 95% of the volume of the slurry for use in the following steps.
Sintering aids addition was done by adding de-ionized water to the powder and adding 0.4% (relative to powder weight) of Darvan-C® as a dis
the RTP material was weighed (in an amount corresponding to the desired tile thickness) and manually poured into the die and pressed at 1 ,200 bar pressure, held for 90 seconds, and the green tile released from the die.
the sintering cycle was as follows: Heating to 1,000 0 C at 400 °C/h heating rate, then to 1900 0 C at 900 0 CZh, then to 1930 0 C at 60 0 CZh; holding 3 hours at 1930 0 C; cooling at 400 0 CZh to 1800 0 C, holding 4 hours at 1800 0 C for phase separation; cooling at 60O 0 CZh to room temperature.
Density measurements by the Archimedes method showed values from about 3200 to 3260 kgZm 3 , depending on additives and other processing parameters. These values corresponded to 98- 100% of the theoretical density.
Vickers micro-hardness tests (using 5N and ION loads) show mat the solid solution phase itself has hardness values of 2400 to over 2600 kgZm 3 . Vickers hardness using IOON load showed values of over 2000 kgZm 3 .
Ballistic tests were performed at a professional testing laboratory, by shooting 7.62 mm diameter 51mm long and 9.5 grams in weight Armor Piercing bullets (7.62x51 AP Type 61 IMI), at speeds of 830 to 860 mZsecond.
the tiles were lightly glued on Al 2024-T3 backing block, 30 mm thick. All tiles of thickness 6 mm to 9 mm stopped the bullets completely, as evidenced by the fact that no penetration of the bullet core into the Al backing block (witness block) occurred.

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