JPH01230472A - Sintered silicon carbide and production thereof - Google Patents
Sintered silicon carbide and production thereofInfo
- Publication number
- JPH01230472A JPH01230472A JP63057883A JP5788388A JPH01230472A JP H01230472 A JPH01230472 A JP H01230472A JP 63057883 A JP63057883 A JP 63057883A JP 5788388 A JP5788388 A JP 5788388A JP H01230472 A JPH01230472 A JP H01230472A
- Authority
- JP
- Japan
- Prior art keywords
- silicon carbide
- spinel
- sintering
- sintered
- sintered body
- Prior art date
- 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.)
- Pending
Links
- HBMJWWWQQXIZIP-UHFFFAOYSA-N silicon carbide Chemical compound [Si+]#[C-] HBMJWWWQQXIZIP-UHFFFAOYSA-N 0.000 title claims abstract description 28
- 229910010271 silicon carbide Inorganic materials 0.000 title claims abstract description 27
- 238000004519 manufacturing process Methods 0.000 title claims description 5
- 238000005245 sintering Methods 0.000 claims abstract description 32
- PNEYBMLMFCGWSK-UHFFFAOYSA-N aluminium oxide Inorganic materials [O-2].[O-2].[O-2].[Al+3].[Al+3] PNEYBMLMFCGWSK-UHFFFAOYSA-N 0.000 claims abstract description 16
- 229910052596 spinel Inorganic materials 0.000 claims abstract description 16
- 239000011029 spinel Substances 0.000 claims abstract description 16
- 239000013078 crystal Substances 0.000 claims abstract description 9
- 239000012298 atmosphere Substances 0.000 claims abstract description 5
- 239000000203 mixture Substances 0.000 claims abstract description 4
- 230000001590 oxidative effect Effects 0.000 claims abstract description 4
- CPLXHLVBOLITMK-UHFFFAOYSA-N Magnesium oxide Chemical compound [Mg]=O CPLXHLVBOLITMK-UHFFFAOYSA-N 0.000 claims description 22
- 239000000395 magnesium oxide Substances 0.000 claims description 11
- 239000000463 material Substances 0.000 claims description 2
- 239000007858 starting material Substances 0.000 claims description 2
- 238000000034 method Methods 0.000 abstract description 14
- 239000002245 particle Substances 0.000 abstract description 9
- 239000000919 ceramic Substances 0.000 abstract description 2
- 238000001746 injection moulding Methods 0.000 abstract description 2
- 238000005266 casting Methods 0.000 abstract 1
- 229910052593 corundum Inorganic materials 0.000 abstract 1
- 238000009740 moulding (composite fabrication) Methods 0.000 abstract 1
- 238000003825 pressing Methods 0.000 abstract 1
- 229910001845 yogo sapphire Inorganic materials 0.000 abstract 1
- 238000000465 moulding Methods 0.000 description 5
- 238000001272 pressureless sintering Methods 0.000 description 5
- XKRFYHLGVUSROY-UHFFFAOYSA-N Argon Chemical compound [Ar] XKRFYHLGVUSROY-UHFFFAOYSA-N 0.000 description 4
- 239000007791 liquid phase Substances 0.000 description 4
- ZOXJGFHDIHLPTG-UHFFFAOYSA-N Boron Chemical compound [B] ZOXJGFHDIHLPTG-UHFFFAOYSA-N 0.000 description 3
- XAGFODPZIPBFFR-UHFFFAOYSA-N aluminium Chemical compound [Al] XAGFODPZIPBFFR-UHFFFAOYSA-N 0.000 description 3
- 229910052782 aluminium Inorganic materials 0.000 description 3
- 229910052796 boron Inorganic materials 0.000 description 3
- 238000000280 densification Methods 0.000 description 3
- 239000006104 solid solution Substances 0.000 description 3
- IJGRMHOSHXDMSA-UHFFFAOYSA-N Atomic nitrogen Chemical compound N#N IJGRMHOSHXDMSA-UHFFFAOYSA-N 0.000 description 2
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 description 2
- XUIMIQQOPSSXEZ-UHFFFAOYSA-N Silicon Chemical compound [Si] XUIMIQQOPSSXEZ-UHFFFAOYSA-N 0.000 description 2
- 229910052786 argon Inorganic materials 0.000 description 2
- 238000006243 chemical reaction Methods 0.000 description 2
- 239000001307 helium Substances 0.000 description 2
- 229910052734 helium Inorganic materials 0.000 description 2
- SWQJXJOGLNCZEY-UHFFFAOYSA-N helium atom Chemical compound [He] SWQJXJOGLNCZEY-UHFFFAOYSA-N 0.000 description 2
- 238000001953 recrystallisation Methods 0.000 description 2
- 229910052710 silicon Inorganic materials 0.000 description 2
- 239000010703 silicon Substances 0.000 description 2
- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical compound [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 description 1
- 229910052790 beryllium Inorganic materials 0.000 description 1
- ATBAMAFKBVZNFJ-UHFFFAOYSA-N beryllium atom Chemical compound [Be] ATBAMAFKBVZNFJ-UHFFFAOYSA-N 0.000 description 1
- 230000015572 biosynthetic process Effects 0.000 description 1
- 229910052799 carbon Inorganic materials 0.000 description 1
- 230000000052 comparative effect Effects 0.000 description 1
- 230000006378 damage Effects 0.000 description 1
- 238000000354 decomposition reaction Methods 0.000 description 1
- 230000007423 decrease Effects 0.000 description 1
- 230000002542 deteriorative effect Effects 0.000 description 1
- 230000000694 effects Effects 0.000 description 1
- 238000005516 engineering process Methods 0.000 description 1
- -1 etc. can be used Substances 0.000 description 1
- 235000019441 ethanol Nutrition 0.000 description 1
- 238000001125 extrusion Methods 0.000 description 1
- 239000007789 gas Substances 0.000 description 1
- 238000010438 heat treatment Methods 0.000 description 1
- 239000012535 impurity Substances 0.000 description 1
- 239000000155 melt Substances 0.000 description 1
- 239000011812 mixed powder Substances 0.000 description 1
- 238000002156 mixing Methods 0.000 description 1
- 229910052757 nitrogen Inorganic materials 0.000 description 1
- 230000003287 optical effect Effects 0.000 description 1
- 238000000879 optical micrograph Methods 0.000 description 1
- 239000012071 phase Substances 0.000 description 1
- 239000000843 powder Substances 0.000 description 1
- 238000009700 powder processing Methods 0.000 description 1
- 239000002994 raw material Substances 0.000 description 1
- 238000001878 scanning electron micrograph Methods 0.000 description 1
- 238000003756 stirring Methods 0.000 description 1
- 239000000126 substance Substances 0.000 description 1
Classifications
-
- C—CHEMISTRY; METALLURGY
- C04—CEMENTS; CONCRETE; ARTIFICIAL STONE; CERAMICS; REFRACTORIES
- C04B—LIME, MAGNESIA; SLAG; CEMENTS; COMPOSITIONS THEREOF, e.g. MORTARS, CONCRETE OR LIKE BUILDING MATERIALS; ARTIFICIAL STONE; CERAMICS; REFRACTORIES; TREATMENT OF NATURAL STONE
- C04B35/00—Shaped ceramic products characterised by their composition; Ceramics compositions; Processing powders of inorganic compounds preparatory to the manufacturing of ceramic products
- C04B35/515—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
- C04B35/56—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 carbides or oxycarbides
- C04B35/565—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 carbides or oxycarbides based on silicon carbide
Landscapes
- Engineering & Computer Science (AREA)
- Chemical & Material Sciences (AREA)
- Ceramic Engineering (AREA)
- Manufacturing & Machinery (AREA)
- Materials Engineering (AREA)
- Structural Engineering (AREA)
- Organic Chemistry (AREA)
- Ceramic Products (AREA)
Abstract
Description
【発明の詳細な説明】 〔産業上の利用分野〕 本発明は、常圧焼結法により得られる高密度。[Detailed description of the invention] [Industrial application field] The present invention provides high-density products obtained by pressureless sintering.
高強度且つ高靭性の炭化けい素質焼結体及びその製造方
法に関する。The present invention relates to a high-strength and high-toughness silicon carbide sintered body and a method for producing the same.
従来、高温構造材料として化学的に安定で、耐摩耗性に
優れ、高温強度が高い等の多くの利点を有する炭化けい
素質焼結体は、再結晶法１反応焼結法、常圧焼結法、加
圧焼結法等の焼結法によって製造されて来た。Conventionally, silicon carbide sintered bodies, which have many advantages as high-temperature structural materials such as chemical stability, excellent wear resistance, and high high-temperature strength, have been processed using recrystallization, one-reaction sintering, and pressureless sintering. It has been manufactured by sintering methods such as sintering method and pressure sintering method.
上記の各種製造方法の中で、再結晶法による焼結体は、
高純度であるが密度が小さく、一般に強度が劣る。反応
焼結法による焼結体では、焼結体中に遊離のシリコンが
存在するた約、高温強度はシリコンの溶融に伴い、急激
に低下する欠点がある。また、加圧焼結法では、特性の
優れた焼結体が得られるが、焼結体の形状は比較的単純
なものに限定され量産性に劣るという欠点がある。Among the various manufacturing methods mentioned above, the sintered body by the recrystallization method is
It has high purity but low density and generally poor strength. A sintered body produced by the reaction sintering method has the disadvantage that the high-temperature strength rapidly decreases as the silicon melts due to the presence of free silicon in the sintered body. Further, in the pressure sintering method, a sintered body with excellent properties can be obtained, but the shape of the sintered body is limited to a relatively simple one, and mass productivity is poor.
そのため、高温で強度が高く、比較的複雑な形状の焼結
体を得ることができる点から常圧焼結法の適用が、現在
、炭化けい素質焼結体製造の主流となっている。Therefore, the application of the pressureless sintering method is currently the mainstream in the production of silicon carbide sintered bodies because it is possible to obtain sintered bodies with high strength and relatively complex shapes at high temperatures.
この常圧焼結法の適用に際しては、硼素、アルミニウム
、ベリリウム等の焼結助剤が用いられるが、これらの焼
結助剤を用いて得られた焼結体は、破壊靭性を示す臨界
応力拡大係数（Ｋ、、） か約３ＭＰａｍ”２ と小
さく、非常に脆いという欠点がある。When applying this pressureless sintering method, sintering aids such as boron, aluminum, beryllium, etc. are used, and the sintered bodies obtained using these sintering aids have a critical stress that indicates fracture toughness. The disadvantage is that the magnification factor (K,...) is small, about 3 MPam''2, and it is very fragile.
このため、炭化けい素の焼結助剤として、無加圧の下で
、比較的低温で焼結が可能なように、アルミナ・マクネ
ンヤのスピネルと酸化イツトリウム表の固溶体形成過程
で生成する液相を使用することが特開昭５８−１９９７
７９号公報、特開昭６０−１８０９６１号公報に開示さ
れている。For this reason, it is used as a sintering aid for silicon carbide to enable sintering at relatively low temperatures without pressure. To use JP-A-58-1997
It is disclosed in Japanese Patent Application Laid-open No. 79 and Japanese Patent Application Laid-open No. 180961/1983.
ところが、上記各公報に記載のものは、比較的低温で液
相が生成するため炭化けい素本来の高温での優れた緒特
性を劣化させ、高温強度７ 高温クリープ特性等は期待
てきない。However, in the products described in the above-mentioned publications, a liquid phase is generated at a relatively low temperature, which deteriorates the excellent properties of silicon carbide at high temperatures, and high temperature strength, high temperature creep properties, etc. cannot be expected.
本発明の目的は、炭化けい素本来の高温での優れた緒特
性を劣化することなく、常圧焼結法により破壊靭性の高
い炭化けい素焼結体を得ることにある。An object of the present invention is to obtain a silicon carbide sintered body with high fracture toughness by an atmospheric pressure sintering method without deteriorating the excellent properties of silicon carbide at high temperatures.
本発明は、炭化けい素を主体とする出発原料に焼結助剤
としてアルミナ・マグネシア・スピネル単味を添加して
得た焼結体は、板状結晶の交叉した強固な微細組織を構
成し、破壊靭性が向上するという知見に基づいて完成し
た。In the present invention, a sintered body obtained by adding alumina, magnesia, and spinel as a sintering aid to a starting material mainly composed of silicon carbide has a strong microstructure with intersecting plate crystals. This was completed based on the knowledge that fracture toughness was improved.
その理由については詳細に解明されてはいないが、次の
ように考えられる。Although the reason for this has not been elucidated in detail, it is thought to be as follows.
すなわち、アルミナ・マグネシア・スピネル単味を焼結
助剤とした場合、焼結中アルミナ・マグネシア・スピネ
ル粒子表面からはマグネシアが優先的に蒸発し、表面は
アルミナで覆われる。このためアルミナ層に接するアル
ミナ・マグネシア・スピネル相中ではマグネシア／アル
ミナのモル比が異なり、マグネシア、アルミナの濃度勾
配が生じたスピネル固溶体が形成される。このスピネル
固溶体と表面に形成されたアルミナの系において液相が
形成され、この液相下で炭化けい素粒子の粒成長が起こ
ると同時に緻密化が進行し、最終的には粒成長により形
成された板状結晶の交叉した強固な微細組織が形成され
る。このような微細組織が形成された焼結体の破壊は、
粒内破壊よりは粒界破壊が主体となり、クラックの分岐
が生じ易く、また伝播径路が複雑になり、破壊に要する
エネルギーは増大する。このため、臨界応力拡大係数（
Ｋ、）値が増大して破壊靭性が向上するものと考えられ
る。また、焼結時に形成されるスピネル固溶体とアルミ
ナの液相形成温度は１９００℃以上であるため、炭化け
い素本来の高温での優れた緒特性を劣化させることが少
ない。That is, when alumina, magnesia, and spinel alone are used as a sintering aid, magnesia is preferentially evaporated from the surfaces of alumina, magnesia, and spinel particles during sintering, and the surfaces are covered with alumina. Therefore, the molar ratio of magnesia/alumina is different in the alumina/magnesia/spinel phase in contact with the alumina layer, and a spinel solid solution with a concentration gradient of magnesia and alumina is formed. A liquid phase is formed in the system of this spinel solid solution and alumina formed on the surface, and silicon carbide particles grow under this liquid phase, and at the same time, densification progresses, and finally, silicon carbide particles are formed due to grain growth. A strong microstructure with intersecting plate-shaped crystals is formed. The destruction of a sintered body with such a microstructure is caused by
Intergranular fracture is more prevalent than intragranular fracture, and crack branching is more likely to occur, the propagation path becomes complicated, and the energy required for fracture increases. Therefore, the critical stress intensity factor (
It is thought that the fracture toughness is improved by increasing the K, ) value. Further, since the liquid phase formation temperature of the spinel solid solution and alumina formed during sintering is 1900° C. or higher, the excellent properties inherent to silicon carbide at high temperatures are less likely to be degraded.
本発明において使用する炭化けい素原料としては、α形
、β形いずれの結晶形のものも使用できる。またその純
度は９５％以上で、平均粒径が０．５ｐ以下のものを用
いるのが望ましい。As the silicon carbide raw material used in the present invention, either the α-form or the β-form crystal form can be used. Further, it is desirable to use one having a purity of 95% or more and an average particle size of 0.5p or less.
焼結助剤として添加するスピネルは、純度が９８％以上
のものが好ましく、粒径は０３虜以下が好ましい。The spinel added as a sintering aid preferably has a purity of 98% or more, and a particle size of 0.3 mm or less.
アルミナ・マグネシア・スピネルと炭化けい素との合量
におけるアルミナ・マグネシア・スピネルの配合割合は
０．３〜３５重量％である。これは、０．３重量％未満
であると焼結時に緻密化が充分に進まずに理論密度の９
０％以上の高密度焼結体が得られす、また、逆に３５重
量％を超えると、１９００〜２３００℃での焼結時の分
解が多く多孔化するためである。The blending ratio of alumina/magnesia/spinel in the total amount of alumina/magnesia/spinel and silicon carbide is 0.3 to 35% by weight. If it is less than 0.3% by weight, densification will not proceed sufficiently during sintering and the theoretical density will be 9.
A high-density sintered body with a content of 0% or more can be obtained. Conversely, if the content exceeds 35% by weight, a large amount of decomposition occurs during sintering at 1900 to 2300°C, resulting in porosity.
成形方法としては、プレス成形、鋳込成形、射出成形、
押出成形等、通常のセラミックスの成形に使用される方
法がすべて適用できる。Molding methods include press molding, cast molding, injection molding,
All methods commonly used for molding ceramics, such as extrusion molding, can be applied.
焼結は非酸化性雰囲気中、無加圧、１９００〜２３００
℃で行うことが必要で、好ましくは１９００〜２１００
℃である。焼結温度が１９００℃より低いと緻密化が充
分に進まないために、高密度焼結体が得られず、２３０
０℃より高いと成形体の分解が激しく多孔化する。Sintering is done in a non-oxidizing atmosphere, without pressure, at 1900~2300
It is necessary to carry out at a temperature of 1900 to 2100°C, preferably
It is ℃. If the sintering temperature is lower than 1900°C, densification will not proceed sufficiently, making it impossible to obtain a high-density sintered body.
When the temperature is higher than 0°C, the molded product decomposes violently and becomes porous.
非酸化性雰囲気としては、窒素、アルゴン、ヘリウム等
が使用できるが、とくに、アルゴン、ヘリウムが好まし
い。As the non-oxidizing atmosphere, nitrogen, argon, helium, etc. can be used, and argon and helium are particularly preferred.
焼結時間は通常１ ＝２４時間必要であるが、好ましく
は１〜１０時間である。これは時間が短すぎると緻密化
せず、長すぎると分解しすぎて多孔化するた続である。The sintering time is usually 1 = 24 hours, preferably 1 to 10 hours. If the time is too short, it will not become densified, and if it is too long, it will decompose too much and become porous.
純度９７％、平均粒径約０．４ｐの炭化けい素粉束に平
均粒径約０３虜のアルミナ・マク不ンア・スピネル粉末
を第１表に示す割合で添加し、エチルアルコールを媒体
としてボールミルで撹拌混合した。続いて、この混合粉
末を静水圧プレス成形して１０ Ｘ２０ Ｘ５０ｍｍの
テスト用成形体を得た。この成形体をアルコンガス通気
中で表に示す条件により焼結して、炭化けい素焼給体を
製造した。得られた各焼結体の特性を第１表に示す。ま
た、比較例として焼結助剤に硼素と炭素を用いた市販品
の炭化けい素焼給体の特性も併せて表に示す。To a silicon carbide powder bundle with a purity of 97% and an average particle size of about 0.4p, alumina spinel powder with an average particle size of about 0.03p was added in the proportions shown in Table 1, and the mixture was milled in a ball mill using ethyl alcohol as a medium. Stir and mix. Subsequently, this mixed powder was subjected to isostatic press molding to obtain a molded body for testing measuring 10 x 20 x 50 mm. This molded body was sintered under the conditions shown in the table in an atmosphere of Alcon gas to produce a silicon carbide fired body. Table 1 shows the characteristics of each of the obtained sintered bodies. Additionally, as a comparative example, the characteristics of a commercially available silicon carbide sintering body using boron and carbon as sintering aids are also shown in the table.
（以下余白）
第１表
第１図、第２図は実施例Ｎｏ、 ５の焼結体の走査型電
子顕微鏡及び光学顕微鏡写真である。これらの写真から
、本発明に係る焼結体は発達した板状の炭化けい素結晶
粒子が交叉した強固な微細組織で構成されていることが
判る。(The following are blank spaces) Table 1, Figures 1 and 2 are scanning electron microscope and optical microscope photographs of the sintered bodies of Examples No. 5. From these photographs, it can be seen that the sintered body according to the present invention is composed of a strong microstructure in which developed plate-shaped silicon carbide crystal grains intersect.
本発明における炭化けい素焼給体は、従来の硼素、アル
ミニウム、べＩＪ ＩＪウム等の焼結助剤を添加して常
圧焼結法により得られる焼結体と同程度の特性を有する
と同時に、板状結晶の交叉した強固な微細組織のため、
臨界応力拡大係数（Ｋ、、）の高い焼結体となる。この
ため、炭化けい素焼給体としての適用範囲が大幅に拡が
る。また、焼結助剤に関しても従来の常圧焼結法では、
純度、添加量を厳密に制御しないと充分な特性の焼結体
が得られないのに対して、本発明では焼結助剤添加量の
範囲が広く、更に粉体処理中に不可避的に混入する不純
物に対しても大きな影響を受けない。The silicon carbide sintered body of the present invention has properties comparable to those of conventional sintered bodies obtained by atmospheric pressure sintering by adding sintering aids such as boron, aluminum, aluminum, etc. , due to the strong microstructure of intersecting plate crystals,
This results in a sintered body with a high critical stress intensity factor (K, .). Therefore, the scope of application as a silicon carbide heating element is greatly expanded. In addition, regarding sintering aids, in the conventional pressureless sintering method,
Whereas it is not possible to obtain a sintered body with sufficient properties unless the purity and amount added are strictly controlled, the present invention allows a wide range of the amount of sintering aid added, and furthermore, the amount of sintering aid added is unavoidably mixed during powder processing. It is not significantly affected by impurities.
第１図及び第２図は、本発明に係る焼結体の粒＝８−
子構造を示す走査型電子顕微鏡写真及び光学顕微鏡写真
である。FIG. 1 and FIG. 2 are a scanning electron micrograph and an optical micrograph showing the grain = octad structure of the sintered body according to the present invention.
Claims (2)
合量に対し０．３〜３５重量％添加してなり、且つ板状
結晶の交叉した微細組織からなる高密度，高強度且つ高
靭性の炭化けい素質焼結体。1. A high-density, high-strength, and high-toughness silicon carbide material made by adding 0.3 to 35% by weight of alumina, magnesia, and spinel based on the total amount of silicon carbide, and consisting of a microstructure with intersecting plate-like crystals. Sintered body.
てアルミナ・マグネシア・スピネルを炭化けい素との合
量に対し０．３〜３５重量％添加した混合物を形成後、
非酸化性雰囲気中、無加圧、１９００〜２３００℃の温
度で焼結することを特徴とする炭化けい素質焼結体の製
造方法。2. After forming a mixture in which 0.3 to 35% by weight of alumina, magnesia, and spinel are added as a sintering aid to the starting material mainly consisting of silicon carbide, based on the total amount of silicon carbide,
A method for producing a silicon carbide sintered body, which comprises sintering in a non-oxidizing atmosphere without pressure at a temperature of 1900 to 2300°C.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| JP63057883A JPH01230472A (en) | 1988-03-10 | 1988-03-10 | Sintered silicon carbide and production thereof |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| JP63057883A JPH01230472A (en) | 1988-03-10 | 1988-03-10 | Sintered silicon carbide and production thereof |
Publications (1)
| Publication Number | Publication Date |
|---|---|
| JPH01230472A true JPH01230472A (en) | 1989-09-13 |
Family
ID=13068388
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| JP63057883A Pending JPH01230472A (en) | 1988-03-10 | 1988-03-10 | Sintered silicon carbide and production thereof |
Country Status (1)
| Country | Link |
|---|---|
| JP (1) | JPH01230472A (en) |
Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| WO1991006515A1 (en) * | 1989-10-26 | 1991-05-16 | Western Mining Corporation Limited | DENSE SiC CERAMIC PRODUCTS |
-
1988
- 1988-03-10 JP JP63057883A patent/JPH01230472A/en active Pending
Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| WO1991006515A1 (en) * | 1989-10-26 | 1991-05-16 | Western Mining Corporation Limited | DENSE SiC CERAMIC PRODUCTS |
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