JPH05148034A - Production of sintered silicon nitride - Google Patents
Production of sintered silicon nitrideInfo
- Publication number
- JPH05148034A JPH05148034A JP3335547A JP33554791A JPH05148034A JP H05148034 A JPH05148034 A JP H05148034A JP 3335547 A JP3335547 A JP 3335547A JP 33554791 A JP33554791 A JP 33554791A JP H05148034 A JPH05148034 A JP H05148034A
- Authority
- JP
- Japan
- Prior art keywords
- sintering
- silicon nitride
- gas
- pressure
- 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.)
- Granted
Links
- HQVNEWCFYHHQES-UHFFFAOYSA-N silicon nitride Chemical compound N12[Si]34N5[Si]62N3[Si]51N64 HQVNEWCFYHHQES-UHFFFAOYSA-N 0.000 title claims abstract description 26
- 229910052581 Si3N4 Inorganic materials 0.000 title claims abstract description 24
- 238000004519 manufacturing process Methods 0.000 title claims description 7
- 238000005245 sintering Methods 0.000 claims abstract description 46
- 239000007789 gas Substances 0.000 claims abstract description 28
- 239000000843 powder Substances 0.000 claims abstract description 9
- IJGRMHOSHXDMSA-UHFFFAOYSA-N Atomic nitrogen Chemical compound N#N IJGRMHOSHXDMSA-UHFFFAOYSA-N 0.000 claims abstract description 8
- QJGQUHMNIGDVPM-UHFFFAOYSA-N nitrogen group Chemical group [N] QJGQUHMNIGDVPM-UHFFFAOYSA-N 0.000 claims abstract description 6
- 239000011261 inert gas Substances 0.000 claims abstract description 5
- 239000000203 mixture Substances 0.000 claims abstract description 5
- 239000012298 atmosphere Substances 0.000 claims description 8
- 229910052757 nitrogen Inorganic materials 0.000 claims description 3
- 238000000465 moulding Methods 0.000 claims description 2
- 238000000034 method Methods 0.000 abstract description 13
- 239000000463 material Substances 0.000 abstract description 8
- 238000006243 chemical reaction Methods 0.000 abstract description 5
- 229910010271 silicon carbide Inorganic materials 0.000 abstract description 5
- HBMJWWWQQXIZIP-UHFFFAOYSA-N silicon carbide Chemical compound [Si+]#[C-] HBMJWWWQQXIZIP-UHFFFAOYSA-N 0.000 abstract description 4
- 229910001873 dinitrogen Inorganic materials 0.000 abstract description 3
- 230000015572 biosynthetic process Effects 0.000 abstract 1
- 238000005452 bending Methods 0.000 description 6
- 239000011148 porous material Substances 0.000 description 4
- QVGXLLKOCUKJST-UHFFFAOYSA-N atomic oxygen Chemical compound [O] QVGXLLKOCUKJST-UHFFFAOYSA-N 0.000 description 3
- 238000010304 firing Methods 0.000 description 3
- 239000001301 oxygen Substances 0.000 description 3
- 229910052760 oxygen Inorganic materials 0.000 description 3
- 238000005979 thermal decomposition reaction Methods 0.000 description 3
- LTPBRCUWZOMYOC-UHFFFAOYSA-N Beryllium oxide Chemical compound O=[Be] LTPBRCUWZOMYOC-UHFFFAOYSA-N 0.000 description 2
- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical compound [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 description 2
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 description 2
- CPLXHLVBOLITMK-UHFFFAOYSA-N Magnesium oxide Chemical compound [Mg]=O CPLXHLVBOLITMK-UHFFFAOYSA-N 0.000 description 2
- VYPSYNLAJGMNEJ-UHFFFAOYSA-N Silicium dioxide Chemical compound O=[Si]=O VYPSYNLAJGMNEJ-UHFFFAOYSA-N 0.000 description 2
- MCMNRKCIXSYSNV-UHFFFAOYSA-N Zirconium dioxide Chemical compound O=[Zr]=O MCMNRKCIXSYSNV-UHFFFAOYSA-N 0.000 description 2
- PNEYBMLMFCGWSK-UHFFFAOYSA-N aluminium oxide Inorganic materials [O-2].[O-2].[O-2].[Al+3].[Al+3] PNEYBMLMFCGWSK-UHFFFAOYSA-N 0.000 description 2
- 239000012752 auxiliary agent Substances 0.000 description 2
- 229910052799 carbon Inorganic materials 0.000 description 2
- 230000000052 comparative effect Effects 0.000 description 2
- 238000000280 densification Methods 0.000 description 2
- 238000005259 measurement Methods 0.000 description 2
- 238000003825 pressing Methods 0.000 description 2
- 239000002344 surface layer Substances 0.000 description 2
- RUDFQVOCFDJEEF-UHFFFAOYSA-N yttrium(III) oxide Inorganic materials [O-2].[O-2].[O-2].[Y+3].[Y+3] RUDFQVOCFDJEEF-UHFFFAOYSA-N 0.000 description 2
- 238000007088 Archimedes method Methods 0.000 description 1
- 238000002441 X-ray diffraction Methods 0.000 description 1
- 229910021417 amorphous silicon Inorganic materials 0.000 description 1
- 239000003575 carbonaceous material Substances 0.000 description 1
- 238000005266 casting Methods 0.000 description 1
- CETPSERCERDGAM-UHFFFAOYSA-N ceric oxide Chemical compound O=[Ce]=O CETPSERCERDGAM-UHFFFAOYSA-N 0.000 description 1
- 229910000422 cerium(IV) oxide Inorganic materials 0.000 description 1
- PMHQVHHXPFUNSP-UHFFFAOYSA-M copper(1+);methylsulfanylmethane;bromide Chemical compound Br[Cu].CSC PMHQVHHXPFUNSP-UHFFFAOYSA-M 0.000 description 1
- 229910021419 crystalline silicon Inorganic materials 0.000 description 1
- 230000007423 decrease Effects 0.000 description 1
- 230000000694 effects Effects 0.000 description 1
- 238000007731 hot pressing Methods 0.000 description 1
- 238000001746 injection moulding Methods 0.000 description 1
- 229910010272 inorganic material Inorganic materials 0.000 description 1
- 239000011147 inorganic material Substances 0.000 description 1
- 239000011810 insulating material Substances 0.000 description 1
- 239000000395 magnesium oxide Substances 0.000 description 1
- 239000011812 mixed powder Substances 0.000 description 1
- 238000002156 mixing Methods 0.000 description 1
- 239000012299 nitrogen atmosphere Substances 0.000 description 1
- -1 nitrogen-containing silane compound Chemical class 0.000 description 1
- 238000013001 point bending Methods 0.000 description 1
- 239000002994 raw material Substances 0.000 description 1
- 229910000077 silane Inorganic materials 0.000 description 1
- 239000000377 silicon dioxide Substances 0.000 description 1
Landscapes
- Ceramic Products (AREA)
Abstract
Description
【０００１】[0001]
【産業上の利用分野】本発明は、高温構造用材料として
有用な窒化珪素質焼結体の製造法に関する。BACKGROUND OF THE INVENTION 1. Field of the Invention The present invention relates to a method for producing a silicon nitride sintered body which is useful as a high temperature structural material.
【０００２】[0002]
【従来技術及びその問題点】窒化珪素質焼結体は、高温
での機械的特性が優れていることから高温構造材料とし
て有望視されている。この窒化珪素質焼結体を高密度に
製造するには、主成分である窒化珪素が難焼結性材料で
あり、しかも高温で熱分解するおそれがあるために、ホ
ットプレス法、熱間静水圧プレス法、雰囲気加圧焼結法
等の高温高圧下で成形体を焼結することが不可欠であ
る。このうち、雰囲気加圧焼結法は製品形状に制約を受
けることなく、少量の焼結助剤で緻密な焼結体を量産す
るのに最適な手段である。2. Description of the Related Art Silicon nitride sintered bodies are regarded as promising high-temperature structural materials because of their excellent mechanical properties at high temperatures. In order to produce this silicon nitride-based sintered body at a high density, since the main component, silicon nitride, is a material that is difficult to sinter, and there is a risk of thermal decomposition at high temperatures, the hot pressing method and hot It is indispensable to sinter the compact under high temperature and high pressure such as a hydraulic pressing method and an atmosphere pressure sintering method. Of these, the atmosphere pressure sintering method is the most suitable means for mass-producing a dense sintered body with a small amount of a sintering aid without being restricted by the product shape.
【０００３】しかし、製品が相当大きくなると、雰囲気
加圧焼結法によっても焼結過程で焼結体中に気孔が残存
して、緻密な焼結体を得ることが困難となる。これを改
善する方法として、特開昭５９−１８１６５号公報や同
６２−１１３７６９号公報には窒化珪素を主成分とする
成形体を加圧窒素雰囲気中で一次焼結し、次いで一次焼
結よりも高圧下で二次焼結する二段焼結方法が提案され
ている。However, when the product is considerably large, even in the atmosphere pressure sintering method, pores remain in the sintered body during the sintering process, making it difficult to obtain a dense sintered body. As a method for improving this, JP-A-59-18165 and JP-A-62-113769 disclose that a compact containing silicon nitride as a main component is subjected to primary sintering in a pressurized nitrogen atmosphere and then subjected to primary sintering. A two-stage sintering method has been proposed in which secondary sintering is performed under high pressure.
【０００４】しかしながら、雰囲気加圧焼結法では、通
常ヒーターや断熱材等の炉材がカーボン製の材料で形成
されている焼成炉を用いるために、助剤から揮発した酸
素含有成分と炉材のカーボンとの反応によってＣＯガス
が発生し、このＣＯガスと窒化珪素が反応して炭化珪素
が生成する結果、焼結体中に有害なポアが残存して、焼
結体の強度が低下するという問題があった。However, in the atmospheric pressure sintering method, since a firing furnace in which a furnace material such as a heater or a heat insulating material is usually made of a carbon material is used, the oxygen-containing component volatilized from the auxiliary agent and the furnace material are used. CO gas is generated by the reaction with the carbon, and the CO gas reacts with silicon nitride to generate silicon carbide. As a result, harmful pores remain in the sintered body and the strength of the sintered body decreases. There was a problem.
【０００５】[0005]
【発明の目的】本発明の目的は、前記問題点を解決し、
機械的強度が優れた緻密な窒化珪素質焼結体の製造法を
提供するものである。The object of the present invention is to solve the above problems,
It is intended to provide a method for producing a dense silicon nitride-based sintered body having excellent mechanical strength.
【０００６】[0006]
【問題点を解決するための手段】本発明は、窒化珪素粉
末と焼結助剤との混合物を成形し、該成形体を焼結する
に際し、窒素又は窒素含有不活性ガスを１．０〜２０kg
／cm2 のガス圧で流通しながら、１６５０〜１９５０℃
で一次焼結して、気孔率０．５〜５％の焼結体とした
後、一次焼結の圧力の５〜５０倍のガス圧で１６５０〜
１９５０℃で二次焼結することを特徴とする窒化珪素質
焼結体の製造法に関するものである。According to the present invention, when a mixture of silicon nitride powder and a sintering aid is molded and the molded body is sintered, nitrogen or a nitrogen-containing inert gas is added in an amount of 1.0 to 1.0%. 20 kg
1650 to 1950 ° C while flowing at a gas pressure of / cm 2.
Primary sintering to obtain a sintered body having a porosity of 0.5 to 5%, and then a gas pressure of 1650 to 5 to 50 times the pressure of primary sintering.
The present invention relates to a method for producing a silicon nitride-based sintered body, which is characterized by secondary sintering at 1950 ° C.
【０００７】本発明における窒化珪素粉末としては、特
に制限はないが、非晶質窒化珪素粉末及び／又は含窒素
シラン化合物を窒素含有不活性ガス雰囲気下又は窒素含
有還元性ガス雰囲気下に焼成することにより得られる結
晶質窒化珪素粉末が好ましく用いられる。The silicon nitride powder in the present invention is not particularly limited, but the amorphous silicon nitride powder and / or the nitrogen-containing silane compound is fired in a nitrogen-containing inert gas atmosphere or a nitrogen-containing reducing gas atmosphere. The crystalline silicon nitride powder thus obtained is preferably used.
【０００８】本発明における焼結助剤としては、マグネ
シア、アルミナ、イットリア、ベリリア、セリア、ジル
コニア、シリカ、窒化アルミニウム及びこれらの混合物
が挙げられる。焼結助剤の配合量は、窒化珪素粉末に対
して１〜１５重量％、好ましくは４〜９重量％が望まし
い。Examples of the sintering aid in the present invention include magnesia, alumina, yttria, beryllia, ceria, zirconia, silica, aluminum nitride and mixtures thereof. The mixing amount of the sintering aid is 1 to 15% by weight, preferably 4 to 9% by weight based on the silicon nitride powder.
【０００９】混合した粉末原料は金型プレス成形法、泥
しょう鋳込法、ラバープレス法、射出成形法等により所
望の形状に成形される。The mixed powder raw materials are molded into a desired shape by a die press molding method, a mud casting method, a rubber pressing method, an injection molding method or the like.
【００１０】次いで、この成形体を、窒素又は窒素含有
不活性ガスを１．０〜２０kg／cm2 のガス圧で流通しな
がら、一次焼結し、気孔率０．５〜５％の焼結体とす
る。Next, the compact was subjected to primary sintering while flowing nitrogen or a nitrogen-containing inert gas at a gas pressure of 1.0 to 20 kg / cm 2 , and sintering with a porosity of 0.5 to 5%. The body.
【００１１】雰囲気ガスの圧力は１．０〜２０kg／c
m2 、好ましくは１．５〜１０kg／cm2 である。圧力が
１．０kg／cm2 よりも低いと、窒化珪素の熱分解を抑制
する効果が発揮されず、また、圧力が２０kg／cm2 より
も高いと、焼結体中の閉気孔内に閉じ込められたガスが
高圧化して、緻密化が促進されないので好ましくない。The pressure of the atmosphere gas is 1.0 to 20 kg / c.
It is m 2 , preferably 1.5 to 10 kg / cm 2 . If the pressure is lower than 1.0 kg / cm 2, the effect of suppressing the thermal decomposition of silicon nitride is not exerted, and if the pressure is higher than 20 kg / cm 2 , it is trapped in the closed pores in the sintered body. The pressure of the generated gas is increased and the densification is not promoted, which is not preferable.
【００１２】また、焼成温度は、１６５０〜１９５０℃
の範囲である。焼成温度が１６５０℃よりも低いと焼結
体の緻密化が不十分となり、１９５０℃よりも高くなる
と窒化珪素の熱分解が起こってしまうので好ましくな
い。The firing temperature is 1650 to 1950 ° C.
The range is. If the firing temperature is lower than 1650 ° C, the densification of the sintered body will be insufficient, and if it is higher than 1950 ° C, thermal decomposition of silicon nitride will occur, which is not preferable.
【００１３】本発明においては、一次焼結の間に、雰囲
気ガスを流通させることが重要である。これにより、助
剤から揮発した酸素含有成分と炉材のカーボンとの反応
によって発生するＣＯガスを炉外に流出させて、雰囲気
ガス中のＣＯガス濃度を０．２％以下に抑制することが
でき、ＣＯガスと窒化珪素との反応による炭化珪素の生
成を抑制できる。In the present invention, it is important to pass the atmospheric gas during the primary sintering. As a result, the CO gas generated by the reaction between the oxygen-containing component volatilized from the auxiliary agent and the carbon of the furnace material is allowed to flow out of the furnace, and the CO gas concentration in the atmospheric gas can be suppressed to 0.2% or less. Therefore, generation of silicon carbide due to the reaction between CO gas and silicon nitride can be suppressed.
【００１４】次に、得られた焼結体を、一次焼結の圧力
の５〜５０倍のガス圧で１６５０〜１９５０℃で二次焼
結する。二次焼結のガス圧は、例えば、一次焼結のガス
圧が２．０kg／cm2 の場合には、１０〜１００kg／cm2
となり、一次焼結のガス圧が１０kg／cm2 の場合には、
５０〜５００kg／cm2 となる。また、二次焼結の温度は
１６５０〜１９５０℃の範囲内であれば、一次焼結の温
度よりも高くても低くてもよい。Next, the obtained sintered body is subjected to secondary sintering at 1650 to 1950 ° C. under a gas pressure of 5 to 50 times the pressure of primary sintering. The gas pressure of the secondary sintering is, for example, 10 to 100 kg / cm 2 when the gas pressure of the primary sintering is 2.0 kg / cm 2.
When the gas pressure for primary sintering is 10 kg / cm 2 ,
It becomes 50 to 500 kg / cm 2 . Further, the temperature of the secondary sintering may be higher or lower than the temperature of the primary sintering as long as it is in the range of 1650 to 1950 ° C.
【００１５】本発明においては、一次焼結により、二次
焼結時に排出し難いような成形体内部のガスを排出し、
表面部と内部の密度差の小さい気孔率０．５〜５％の焼
結体とした後、雰囲気圧力の更に高い二次焼結におい
て、内部に残存するポアを排出する。これにより、均質
な焼結体が得られる。In the present invention, by the primary sintering, the gas inside the compact, which is difficult to discharge during the secondary sintering, is discharged,
After forming a sintered body having a porosity of 0.5 to 5% with a small density difference between the surface portion and the inside, the pores remaining inside are discharged in the secondary sintering with a higher atmospheric pressure. Thereby, a homogeneous sintered body is obtained.
【００１６】[0016]
【実施例】以下に実施例及び比較例を示し、本発明をさ
らに具体的に説明する。 実施例１〜６ 窒化珪素粉末（宇部興産（株）製：比表面積１１m2／
ｇ、酸素含有量１．３ｗｔ％）９２．５重量％に、イッ
トリア（信越化学（株）製）５重量％及びアルミナ（住
友化学（株）製：ＡＫＰ−３０）２．５重量％を添加し
た配合粉を、媒体としてエタノールを用いて４８時間湿
式混合した後、減圧乾燥した。EXAMPLES The present invention will be described more specifically by showing Examples and Comparative Examples below. Examples 1 to 6 Silicon nitride powder (manufactured by Ube Industries, Ltd .: specific surface area 11 m 2 /
g, oxygen content 1.3 wt%) 92.5 wt%, yttria (Shin-Etsu Chemical Co., Ltd.) 5 wt% and alumina (Sumitomo Chemical Co., Ltd .: AKP-30) 2.5 wt% were added. The compounded powder was wet mixed using ethanol as a medium for 48 hours and then dried under reduced pressure.
【００１７】得られた混合物を断面が５０×８０mm角の
金型を用いて矩形状に予備成形した後、圧力１．５ton/
cm2 でラバープレスした。得られた成形体を雰囲気加圧
焼結炉に装入し、表１に記載の温度−窒素ガス圧力条件
下で二段焼結を行った。一次焼結時に５ｌ／分の流量で
ガスを流通させることにより、炉内のＣＯガス濃度は
０．１％以下であった。また、保持時間は、一次焼結、
二次焼結共に１．５時間とした。The mixture thus obtained was preformed into a rectangular shape using a die having a cross section of 50 × 80 mm, and the pressure was 1.5 ton /
Rubber pressed at cm 2 . The obtained molded body was charged into an atmosphere pressure sintering furnace and subjected to two-stage sintering under the temperature-nitrogen gas pressure conditions shown in Table 1. By flowing the gas at a flow rate of 5 l / min during the primary sintering, the CO gas concentration in the furnace was 0.1% or less. In addition, the holding time is
The secondary sintering time was 1.5 hours.
【００１８】得られた焼結体の嵩密度及び曲げ強度の測
定結果を表１に示す。嵩密度はアルキメデス法により測
定した。また、曲げ強度は、作製した焼結体から３×４
×４０mmのテストピースを切り出し、これを外スパン３
０mm、内スパン１０mmの４点曲げ試験治具にセットし
て、室温及び１３００℃における曲げ強度を測定した。
室温における曲げ強度はテストピース４０本の平均値、
１３００℃おける曲げ強度はテストピース１０本の平均
値で求めた。Table 1 shows the measurement results of the bulk density and bending strength of the obtained sintered body. The bulk density was measured by the Archimedes method. The bending strength is 3 × 4 from the produced sintered body.
Cut out a test piece of × 40mm and use it for outer span 3
It was set in a 4-point bending test jig having 0 mm and an inner span of 10 mm, and the bending strength at room temperature and 1300 ° C. was measured.
The bending strength at room temperature is the average value of 40 test pieces,
The bending strength at 1300 ° C. was calculated as the average value of 10 test pieces.
【００１９】比較例１〜６ 一次焼結時に窒素ガスを流通させなかった以外は、実施
例１〜６と同様の操作を繰り返した。一次焼結時に炉内
のＣＯガス濃度は５％以上に上昇した。得られた焼結体
の嵩密度及び曲げ強度の測定結果を表１に示す。得られ
た焼結体の表層部は緑灰色に変色していた。Ｘ線回折測
定によれば、焼結体の表層部にはβ−ＳｉＣのピークが
検出された。Comparative Examples 1 to 6 The same operations as in Examples 1 to 6 were repeated except that nitrogen gas was not passed during the primary sintering. During the primary sintering, the CO gas concentration in the furnace increased to 5% or more. Table 1 shows the measurement results of the bulk density and bending strength of the obtained sintered body. The surface layer of the obtained sintered body was discolored in greenish gray. According to X-ray diffraction measurement, a β-SiC peak was detected in the surface layer portion of the sintered body.
【００２０】[0020]
【表１】 [Table 1]
【００２１】[0021]
【発明の効果】本発明によれば、ＣＯガスと窒化珪素と
の反応による炭化珪素の生成を抑制できるので、機械的
強度が優れた緻密な窒化珪素質焼結体を製造することが
できる。According to the present invention, since the generation of silicon carbide due to the reaction between CO gas and silicon nitride can be suppressed, it is possible to manufacture a dense silicon nitride-based sintered body having excellent mechanical strength.
フロントページの続き (72)発明者 寺井 健二 山口県宇部市大字小串1978番地の５ 宇部 興産株式会社無機材料研究所内Front Page Continuation (72) Inventor Kenji Terai 5 1978, Kozugushi, Ube City, Yamaguchi Prefecture Ube Industries Ltd. Inorganic Materials Research Laboratory
Claims (2)
形し、該成形体を焼結するに際し、窒素又は窒素含有不
活性ガスを１．０〜２０kg／cm2のガス圧で流通しなが
ら、１６５０〜１９５０℃で一次焼結して、気孔率０．
５〜５％の焼結体とした後、一次焼結の圧力の５〜５０
倍のガス圧で１６５０〜１９５０℃で二次焼結すること
を特徴とする窒化珪素質焼結体の製造法。1. When molding a mixture of silicon nitride powder and a sintering aid and sintering the molded body, nitrogen or a nitrogen-containing inert gas is passed under a gas pressure of 1.0 to 20 kg / cm 2. Meanwhile, the primary sintering was performed at 1650 to 1950 ° C., and the porosity was 0.
5 to 50% of the pressure of the primary sintering after forming a 5 to 5% sintered body
A method for producing a silicon nitride sintered body, which comprises performing secondary sintering at 1650 to 1950 ° C. under double gas pressure.
が０．２％以下であることを特徴とする請求項１の窒化
珪素質焼結体の製造法。2. The method for producing a silicon nitride sintered body according to claim 1, wherein the CO gas concentration in the atmosphere gas of the primary sintering is 0.2% or less.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| JP3335547A JP2696734B2 (en) | 1991-11-26 | 1991-11-26 | Manufacturing method of silicon nitride sintered body |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| JP3335547A JP2696734B2 (en) | 1991-11-26 | 1991-11-26 | Manufacturing method of silicon nitride sintered body |
Publications (2)
| Publication Number | Publication Date |
|---|---|
| JPH05148034A true JPH05148034A (en) | 1993-06-15 |
| JP2696734B2 JP2696734B2 (en) | 1998-01-14 |
Family
ID=18289802
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| JP3335547A Expired - Lifetime JP2696734B2 (en) | 1991-11-26 | 1991-11-26 | Manufacturing method of silicon nitride sintered body |
Country Status (1)
| Country | Link |
|---|---|
| JP (1) | JP2696734B2 (en) |
Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| JP2001181051A (en) * | 1999-12-28 | 2001-07-03 | Ngk Spark Plug Co Ltd | Silicon nitride-based sintered product, tool and sliding member using the same, and method for producing silicon nitride-based sintered product |
| US6359261B1 (en) | 1999-10-29 | 2002-03-19 | Ngk Spark Plug Co., Ltd. | Silicon nitride sintered body, process for producing the same, ceramic heater employing the silicon nitride sintered body and glow plug containing the ceramic heater |
-
1991
- 1991-11-26 JP JP3335547A patent/JP2696734B2/en not_active Expired - Lifetime
Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US6359261B1 (en) | 1999-10-29 | 2002-03-19 | Ngk Spark Plug Co., Ltd. | Silicon nitride sintered body, process for producing the same, ceramic heater employing the silicon nitride sintered body and glow plug containing the ceramic heater |
| JP2001181051A (en) * | 1999-12-28 | 2001-07-03 | Ngk Spark Plug Co Ltd | Silicon nitride-based sintered product, tool and sliding member using the same, and method for producing silicon nitride-based sintered product |
Also Published As
| Publication number | Publication date |
|---|---|
| JP2696734B2 (en) | 1998-01-14 |
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