JPS59111981A - Manufacture of silicon nitride-containing fine sintered body - Google Patents
Manufacture of silicon nitride-containing fine sintered bodyInfo
- Publication number
- JPS59111981A JPS59111981A JP57221276A JP22127682A JPS59111981A JP S59111981 A JPS59111981 A JP S59111981A JP 57221276 A JP57221276 A JP 57221276A JP 22127682 A JP22127682 A JP 22127682A JP S59111981 A JPS59111981 A JP S59111981A
- Authority
- JP
- Japan
- Prior art keywords
- sintered body
- silicon oxide
- component
- silicon
- silicon nitride
- 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
- 238000004519 manufacturing process Methods 0.000 title claims description 5
- 229910052581 Si3N4 Inorganic materials 0.000 title description 14
- HQVNEWCFYHHQES-UHFFFAOYSA-N silicon nitride Chemical compound N12[Si]34N5[Si]62N3[Si]51N64 HQVNEWCFYHHQES-UHFFFAOYSA-N 0.000 title description 13
- VYPSYNLAJGMNEJ-UHFFFAOYSA-N Silicium dioxide Chemical compound O=[Si]=O VYPSYNLAJGMNEJ-UHFFFAOYSA-N 0.000 claims description 33
- 229910052814 silicon oxide Inorganic materials 0.000 claims description 31
- HBMJWWWQQXIZIP-UHFFFAOYSA-N silicon carbide Chemical compound [Si+]#[C-] HBMJWWWQQXIZIP-UHFFFAOYSA-N 0.000 claims description 21
- 229910010271 silicon carbide Inorganic materials 0.000 claims description 19
- IJGRMHOSHXDMSA-UHFFFAOYSA-N Atomic nitrogen Chemical compound N#N IJGRMHOSHXDMSA-UHFFFAOYSA-N 0.000 claims description 16
- 239000007789 gas Substances 0.000 claims description 16
- 229910001873 dinitrogen Inorganic materials 0.000 claims description 12
- UGFAIRIUMAVXCW-UHFFFAOYSA-N Carbon monoxide Chemical compound [O+]#[C-] UGFAIRIUMAVXCW-UHFFFAOYSA-N 0.000 claims description 8
- 229910002091 carbon monoxide Inorganic materials 0.000 claims description 8
- 238000006243 chemical reaction Methods 0.000 description 23
- 238000000034 method Methods 0.000 description 14
- 238000005121 nitriding Methods 0.000 description 13
- 229910002090 carbon oxide Inorganic materials 0.000 description 8
- 239000000843 powder Substances 0.000 description 8
- CURLTUGMZLYLDI-UHFFFAOYSA-N Carbon dioxide Chemical compound O=C=O CURLTUGMZLYLDI-UHFFFAOYSA-N 0.000 description 7
- LIVNPJMFVYWSIS-UHFFFAOYSA-N silicon monoxide Chemical compound [Si-]#[O+] LIVNPJMFVYWSIS-UHFFFAOYSA-N 0.000 description 7
- 238000005245 sintering Methods 0.000 description 7
- 239000000203 mixture Substances 0.000 description 6
- 239000011148 porous material Substances 0.000 description 5
- 239000002994 raw material Substances 0.000 description 5
- 239000002245 particle Substances 0.000 description 3
- XKRFYHLGVUSROY-UHFFFAOYSA-N Argon Chemical compound [Ar] XKRFYHLGVUSROY-UHFFFAOYSA-N 0.000 description 2
- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical compound [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 description 2
- MCMNRKCIXSYSNV-UHFFFAOYSA-N Zirconium dioxide Chemical compound O=[Zr]=O MCMNRKCIXSYSNV-UHFFFAOYSA-N 0.000 description 2
- 229910052799 carbon Inorganic materials 0.000 description 2
- 239000013078 crystal Substances 0.000 description 2
- 238000000280 densification Methods 0.000 description 2
- 229910044991 metal oxide Inorganic materials 0.000 description 2
- 150000004706 metal oxides Chemical class 0.000 description 2
- 229910052757 nitrogen Inorganic materials 0.000 description 2
- 235000012239 silicon dioxide Nutrition 0.000 description 2
- 238000012360 testing method Methods 0.000 description 2
- UFHFLCQGNIYNRP-UHFFFAOYSA-N Hydrogen Chemical compound [H][H] UFHFLCQGNIYNRP-UHFFFAOYSA-N 0.000 description 1
- BPQQTUXANYXVAA-UHFFFAOYSA-N Orthosilicate Chemical compound [O-][Si]([O-])([O-])[O-] BPQQTUXANYXVAA-UHFFFAOYSA-N 0.000 description 1
- 230000002411 adverse Effects 0.000 description 1
- PNEYBMLMFCGWSK-UHFFFAOYSA-N aluminium oxide Inorganic materials [O-2].[O-2].[O-2].[Al+3].[Al+3] PNEYBMLMFCGWSK-UHFFFAOYSA-N 0.000 description 1
- 229910052786 argon Inorganic materials 0.000 description 1
- QVGXLLKOCUKJST-UHFFFAOYSA-N atomic oxygen Chemical compound [O] QVGXLLKOCUKJST-UHFFFAOYSA-N 0.000 description 1
- 239000011248 coating agent Substances 0.000 description 1
- 238000000576 coating method Methods 0.000 description 1
- 229910052681 coesite Inorganic materials 0.000 description 1
- 239000002131 composite material Substances 0.000 description 1
- 238000007796 conventional method Methods 0.000 description 1
- 229910052906 cristobalite Inorganic materials 0.000 description 1
- 230000000694 effects Effects 0.000 description 1
- 239000003779 heat-resistant material Substances 0.000 description 1
- 239000000463 material Substances 0.000 description 1
- 238000002844 melting Methods 0.000 description 1
- 230000008018 melting Effects 0.000 description 1
- 230000003647 oxidation Effects 0.000 description 1
- 238000007254 oxidation reaction Methods 0.000 description 1
- 230000001590 oxidative effect Effects 0.000 description 1
- 239000001301 oxygen Substances 0.000 description 1
- 229910052760 oxygen Inorganic materials 0.000 description 1
- 238000013001 point bending Methods 0.000 description 1
- 238000012545 processing Methods 0.000 description 1
- 238000010992 reflux Methods 0.000 description 1
- 238000011160 research Methods 0.000 description 1
- RMAQACBXLXPBSY-UHFFFAOYSA-N silicic acid Chemical compound O[Si](O)(O)O RMAQACBXLXPBSY-UHFFFAOYSA-N 0.000 description 1
- 239000000377 silicon dioxide Substances 0.000 description 1
- XUIMIQQOPSSXEZ-NJFSPNSNSA-N silicon-30 atom Chemical compound [30Si] XUIMIQQOPSSXEZ-NJFSPNSNSA-N 0.000 description 1
- 229910052682 stishovite Inorganic materials 0.000 description 1
- 239000000126 substance Substances 0.000 description 1
- 239000010409 thin film Substances 0.000 description 1
- 229910052905 tridymite Inorganic materials 0.000 description 1
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 description 1
Landscapes
- Ceramic Products (AREA)
Abstract
(57)【要約】本公報は電子出願前の出願データであるた
め要約のデータは記録されません。(57) [Summary] This bulletin contains application data before electronic filing, so abstract data is not recorded.
Description
【発明の詳細な説明】
本発明は窒化けい素を含む緻密な焼結体の製造法、更に
詳しくは１２００℃以上の高温でも高い強度を示す緻密
な焼結体の製造法に関する。DETAILED DESCRIPTION OF THE INVENTION The present invention relates to a method for manufacturing a dense sintered body containing silicon nitride, and more particularly to a method for manufacturing a dense sintered body that exhibits high strength even at high temperatures of 1200° C. or higher.
窒化けい素糸焼結体、または窒化けい素を１成分とし、
炭化けい素などを含む焼結体は高い硬度と化学的安定性
にすぐれ、高温においても剛性をために、耐熱材料とし
て期待されている。Silicon nitride thread sintered body or silicon nitride as one component,
Sintered bodies containing silicon carbide have high hardness and excellent chemical stability, and are expected to be used as heat-resistant materials because of their rigidity even at high temperatures.
しかし、これらの焼結体は現状においては、期待されて
いる程の特性を示していない。その原因は原料粉末を焼
結体として固化させる際に焼結助剤として添加する成分
が高温における焼結体の強度を低下させるように働くた
めである。即ち、焼結体原料中に含まれている酸化けい
素が焼結助剤甲□
で１、ある例えばＭｇＯ、Ｙ２Ｏ３，ＯａＯと結合し、
低融点の漬化物相を形成するために高温強度を低下させ
化によって比較的純粋な窒化けい素焼給体を作る方法も
あるが、この方法で得られた焼結体は、焼結体中に残留
する空孔が多いため充分な強度となし得ない欠点がある
。However, these sintered bodies do not currently exhibit the expected characteristics. The reason for this is that the component added as a sintering aid when solidifying the raw material powder into a sintered body acts to reduce the strength of the sintered body at high temperatures. That is, silicon oxide contained in the sintered body raw material is combined with 1, for example, MgO, Y2O3, OaO, by the sintering aid A□,
There is a method of reducing high-temperature strength and creating a relatively pure silicon nitride sintered body by oxidation to form a pickled phase with a low melting point, but the sintered body obtained by this method has Since there are many remaining pores, there is a drawback that it cannot be achieved with sufficient strength.
本発明はこれらの従来法の欠点を解消し、高温における
強度の低下を来たす原因となる成分が焼結体中に残留せ
ず、且つ充分に緻密で高い高温強度を有する焼結体を製
造する方法を提供するにあるＯ
本発明者は前記目的を達成すべく研究の結果、焼結助剤
として酸化けい素を一定量使用し、一定比の炭化けい素
を含有させた焼結体を作り、この焼結体を高圧窒素ガス
下において高温処理し、酸化けい素成分を窒化けい素と
し、生成する一酸化炭素を排除すると酸化けい素成分の
ない高温強度に優れ、高緻密な焼結体が得られることを
知見し得率発明を完成した。The present invention eliminates the drawbacks of these conventional methods, and produces a sintered body that is sufficiently dense and has high high-temperature strength, without any components that cause a decrease in strength at high temperatures remaining in the sintered body. To provide a method, as a result of research to achieve the above object, the present inventor used a certain amount of silicon oxide as a sintering aid and created a sintered body containing a certain ratio of silicon carbide. When this sintered body is treated at high temperature under high-pressure nitrogen gas, the silicon oxide component is changed to silicon nitride, and the generated carbon monoxide is eliminated, a highly dense sintered body with excellent high-temperature strength and no silicon oxide component is obtained. He discovered that this could be obtained and completed the invention.
本発明の要旨は、
酸化けい素成分１〜３２．５重量％、炭化けい素：成ｊ
分１．５ｉ量％以上で、且つ酸化けい素成分対炭化けい
素成分の重量比が３対２またはこの比より炭化けい素成
分が多い組成物を用いて焼結体を作り、この焼結体を１
０〜３０００に２／ｃｖＬ２の窒素ガス中で１５００〜
２３００℃の温度に保持すると共に、焼結体近傍の気体
の一酸化炭素ガス分圧を窒化反応の平衡分圧以下に保持
することを特徴とする緻密な焼結体の製造法にある。The gist of the present invention is that silicon oxide component: 1 to 32.5% by weight, silicon carbide: composition
A sintered body is made using a composition in which the weight ratio of silicon oxide component to silicon carbide component is 3 to 2 or more than this ratio, and the weight ratio of silicon oxide component to silicon carbide component is 3 to 2 or more than this ratio. body 1
0 to 3000 to 1500 to 2/cvL2 nitrogen gas
The present invention provides a method for producing a dense sintered body, characterized by maintaining the temperature at 2300° C. and maintaining the partial pressure of carbon monoxide gas in the vicinity of the sintered body below the equilibrium partial pressure of the nitriding reaction.
本発明の方法においては、原料の酸化けい素成分；１と
しては酸化けい素粉末を使用するが、けい酸薯の粉末で
もよい。In the method of the present invention, silicon oxide powder is used as the raw material silicon oxide component (1), but silicic acid powder may also be used.
この酸化けい素粉末は炭化けい素粉の表面に均一に付着
した状態で存在させるのが好ましい。例えば炭化けい素
粉末を酸化し、粒子表面が酸化けい素の薄膜で被覆され
た粉体が好ましい。このようにすると、組成むらによっ
て生ずる焼結体中の微細な焼結きずを少くすることがで
きる。酸化けい素成分量は１〜３２．５重量％で、炭化
けい素成分、は１．５重量％以上であることが好ましい
。酸化けい素成分量が１重量％未満では緻密化し難く、
３２．５重量％を超える量は緻密化に不必要であり、ま
た後処理の窒化処理時間が大きくなり悪影響を及ぼす。This silicon oxide powder is preferably present in a state in which it is uniformly adhered to the surface of the silicon carbide powder. For example, a powder obtained by oxidizing silicon carbide powder and coating the particle surface with a thin film of silicon oxide is preferable. In this way, fine sintering flaws in the sintered body caused by compositional unevenness can be reduced. The amount of silicon oxide component is preferably 1 to 32.5% by weight, and the amount of silicon carbide component is preferably 1.5% by weight or more. If the amount of silicon oxide component is less than 1% by weight, it is difficult to densify.
An amount exceeding 32.5% by weight is unnecessary for densification, and also increases the time required for the nitriding treatment in the post-treatment, which has an adverse effect.
炭化けい素１．５重量％未満では未反応５ｉ０２が残り
、また酸化けい素成分対炭化けい素成分比（重量）は３
対２、またはこの比よりも炭化けい素成分が多いことが
必要である。それは後記の５ｉｎ２． 、ＳｉＯ及びＮ
２との反応を完遂し、ＳｉＯ２が焼結体中に残らずＳｉ
Ｏは残ってもよいようにするだめである。If silicon carbide is less than 1.5% by weight, unreacted 5i02 remains, and the silicon oxide component to silicon carbide component ratio (weight) is 3.
2 or more silicon carbide component than this ratio. It is 5in2 which will be mentioned later. , SiO and N
The reaction with 2 is completed, and no SiO2 remains in the sintered body.
O should be allowed to remain.
焼結体製造原料である粉体組成物中には酸化けい素成分
、炭化けい素成分以外に必要に応じて窒化けい素やアル
ミナ、ジルコニア等の金属酸化物を混合してもよい。In addition to the silicon oxide component and the silicon carbide component, metal oxides such as silicon nitride, alumina, and zirconia may be mixed into the powder composition that is the raw material for producing the sintered body, if necessary.
これらを焼結するには、そのまま焼結してもよいが、水
分を含有した水素ガス雰囲気中で行うと焼結が進行し易
いので好ましい。このような条件下では酸化けい素に水
分が１１０００ＰＰ程度まで溶解４．して酸化けい素成
分の粘性を低下させ、焼結の、進１行を容易にする。そ
の焼結の緻密化の程度は、焼結１体中の空孔が独立気泡
の状態になっている程度ると
涯軒ましい。その空孔が独立気泡になってい昏鴫、この
焼結体を高温高圧の窒素ガス中で窒化処理する際、空孔
は圧縮され消滅してしまう。Although these may be sintered as they are, it is preferable to sinter them in a hydrogen gas atmosphere containing moisture, since this facilitates sintering. Under such conditions, water dissolves in silicon oxide to a level of about 11,000 PP4. This reduces the viscosity of the silicon oxide component and facilitates the progress of sintering. The degree of densification of the sintered body is excellent if the pores in the sintered body are in the state of closed cells. The pores become closed cells, and when this sintered body is nitrided in high-temperature, high-pressure nitrogen gas, the pores are compressed and disappear.
得られた焼結体を１０〜３０００ Ｑ／ｃｍ２の窒素ガ
ス中で１５００〜２３００℃の温度で保持すると、焼結
体中に含まれる酸化けい素成分、炭化けい素成分とは、
高圧の窒素ガスと高温において反応する。その化学反応
式を示すと次の通りである。When the obtained sintered body is held at a temperature of 1500 to 2300°C in nitrogen gas of 10 to 3000 Q/cm2, the silicon oxide component and silicon carbide component contained in the sintered body are
Reacts with high pressure nitrogen gas and high temperatures. The chemical reaction formula is as follows.
５ｉｎ２＋ ２３ｉＯ＋ ２ Ｎ２→Ｓｉ、Ｎ４＋ ２
００ ・・・・・・・・・・・・（１）２ＳｉＯ２＋
２ＳｉＯ＋２Ｎ２→２Ｓｉ２Ｎ２０ ＋ ２００ ・
・−・・・・・（２）ＳｉＮＯ＋ＳｉＯ＋Ｎ−＋Ｓｉ、
Ｎ４＋ＣＯ・・・−・・・・・・・・・・・（５ン２
２ ２
これらの反応式において、酸化けい素成分はＳ’ｉ０２
で会表している。焼結原料粉末の組成によっては酸化け
い素成分はけい酸塩として他の金属酸化物として化合し
ている場合もあるが、これも含めてＳｉＯとして表わし
た。酸化けい素成分が窒化によシ生成する生成相は窒化
けい素（５ｉ３Ｎ４）に限らず複合酸窒化物となる場合
も多いが、これも含めてＳｉ Ｎ 及び５ｉ２Ｎ２０と
して表わしだ。なお、本４
発明において言う窒化けい素とはＳｉ３Ｎ４と５ｉ２Ｎ
２０を粛めたものを言う。5in2+ 23iO+ 2 N2→Si, N4+ 2
00 ・・・・・・・・・・・・(1)2SiO2+
2SiO+2N2→2Si2N20 + 200 ・
・−・・・・・・(2) SiNO+SiO+N−+Si,
N4+CO・・・−・・・・・・・・・・・・(5n2
2 2 In these reaction equations, the silicon oxide component is S'i02
We are holding a meeting at Depending on the composition of the sintering raw material powder, the silicon oxide component may be combined as a silicate with other metal oxides, but this is also expressed as SiO. The phase produced by silicon oxide components by nitridation is not limited to silicon nitride (5i3N4), but often becomes composite oxynitrides, and these are also expressed as Si N and 5i2N20. In addition, silicon nitride referred to in this 4th invention refers to Si3N4 and 5i2N.
Say something with the number 20 suppressed.
この反応式で示すように、焼結体中の酸化けい素成分中
の酸素が焼結体中に混在しているＳｉ０粒子の炭素と結
合して一酸化炭素ガスを生成する。As shown in this reaction formula, oxygen in the silicon oxide component in the sintered body combines with carbon in Si0 particles mixed in the sintered body to generate carbon monoxide gas.
他方窒素はＳｉと結合して窒化けい素となる。On the other hand, nitrogen combines with Si to form silicon nitride.
従来、焼結体の■工Ｐ処理、即ち高温高圧の気体を用い
て焼結体中の気孔を圧縮除去する方法は知られている。BACKGROUND ART Conventionally, a method of processing a sintered body by compressing and removing pores in the sintered body using high temperature and high pressure gas is known.
この方法において使用する気体としては通常アルゴンガ
スを使用しているが、窒素ガスを使用する場合もある。The gas used in this method is usually argon gas, but nitrogen gas may also be used.
本発明の方法で行う窒化処理は焼結体のＨＩＰ処理とは
次の点で相違する。The nitriding treatment performed by the method of the present invention differs from the HIP treatment of sintered bodies in the following points.
１）第１に本発明の方法では被処理焼結体中に予め酸化
けい素成分を１重量％以上の多くの成分を含有させてお
く点である。酸化けい素成分は高温強度が低いので、こ
れを多く含む焼結体は高温材料として適しないので、こ
のように多くの酸化けい素成分を含ませない。本発明に
おい世は炭化けい素成分と共存させてこれを窒化は緊素
に変え高温強度を高めるので、１重量％以り
夛含ませておくことが必要である。1) First, in the method of the present invention, the sintered body to be treated contains in advance a silicon oxide component of 1% by weight or more. Since the silicon oxide component has low high-temperature strength, a sintered body containing a large amount of the silicon oxide component is not suitable as a high-temperature material, so such a large amount of the silicon oxide component is not included. In the present invention, it is necessary to contain silicon carbide in an amount of 1% by weight or more because nitriding converts it to nitrogen and increases high-temperature strength by coexisting with the silicon carbide component.
２）第２に本発明の方法では窒化反応によって生ずる一
酸化炭素を除去して、焼結体近傍の一酸化炭素ガス分圧
を化学反応の平衡−酸化炭素ガス分圧よシ低く保持する
点である。もしこのようにしなければ、前記反応式に示
した反応が進行しなくなり、窒化反応を完結させること
ができない。この平衡−酸化炭素ガス分圧を窒化反応温
度の関数として示すと第１図の通りである。2) Second, in the method of the present invention, carbon monoxide produced by the nitriding reaction is removed, and the partial pressure of the carbon monoxide gas near the sintered body is kept lower than the equilibrium of the chemical reaction - the partial pressure of the carbon oxide gas. It is. If this is not done, the reaction shown in the above reaction formula will not proceed and the nitriding reaction will not be completed. This equilibrium carbon oxide gas partial pressure is shown in FIG. 1 as a function of the nitriding reaction temperature.
酸化炭素ガス分圧は１５００℃で２００にシー２．２０
００℃で４１０ Ｋｇ／ｃｍ２−ｃあり、温度カ高イト
平衡−酸化炭素ガス分圧も高くなる傾向がある。The partial pressure of carbon oxide gas is 2.20 at 1500℃.
It is 410 Kg/cm2-c at 00°C, and the temperature carbon oxide gas partial pressure also tends to increase.
−酸化炭素ガス分圧を低く保つには、被処理焼結体近傍
の気体を流動させ、−ｍ化炭素ガス分圧の低い窒素ガス
を流入させることによって行うことができる。酸化けい
素成分と炭化けい素成分とが反応して窒化する過程は前
記化学反応式（２）、（５）に示す２段階に進行する場
合がある。- To keep the partial pressure of the carbon oxide gas low, it can be done by flowing the gas near the sintered body to be treated and flowing nitrogen gas having a low partial pressure of the carbon oxide gas. The process of nitriding caused by the reaction between the silicon oxide component and the silicon carbide component may proceed in two stages as shown in the chemical reaction equations (2) and (5).
即ち前記化学反応式（１）によって反応する場合の他、
先ず（２）式によって酸窒化物が生成し、次いで（５）
式のように酸窒化物が窒化される経過をたどることがあ
る。後者の場合は、−酸化炭素ガスの排除が速かでない
場合に起シやすく、先ず（２）式の反応が速かに進行し
、（３）式の反応は一酸化炭素ガス分圧を充分に低く保
たないと進行しない。ただし、（２）式の段階で止め５
１２Ｎ２０を主成分とする焼結体を用いてもよい。（５
）式の反応を進行させ窒化を完了させるには窒素ガス分
圧ｊ５： １０００ Ｋｙ／Ｃｍ２の場合、−ｍ化炭素
ｉ、ｌ）圧を０．５に２／ｃｍ２、望ましくハ０．１に
２／ｃＩＩＬ２以下ニ保持して反応速度を高めることが
望ましい。窒化反応の処理温度は１５００〜２３００℃
であること゛が℃より低いと窒化反応が起り難く、好ま
しく□は″１７００℃以上である。２３００℃を超える
と窒化短縮される。しかし温度が高すぎると、被処理焼
結体中の結晶粒の粗大化が生ずる。That is, in addition to the reaction according to the chemical reaction formula (1),
First, oxynitride is generated according to equation (2), and then (5)
Oxynitrides may follow the nitriding process as shown in the equation. The latter case is likely to occur if -carbon oxide gas is not removed quickly, and first the reaction of equation (2) proceeds quickly, and the reaction of equation (3) occurs when the partial pressure of carbon monoxide gas is sufficiently increased. It will not progress unless it is kept low. However, it should be stopped at the stage of equation (2).
A sintered body containing 12N20 as a main component may also be used. (5
) To proceed with the reaction of the formula and complete nitriding, the partial pressure of nitrogen gas j5: In the case of 1000 Ky/Cm2, the -m carbon i, l) pressure should be reduced to 0.52/cm2, preferably Ha to 0.1. It is desirable to maintain the reaction rate below 2/cIIL2 to increase the reaction rate. The treatment temperature for nitriding reaction is 1500-2300℃
If ゛ is lower than °C, the nitriding reaction is difficult to occur, and preferably □ is 1700 °C or higher. If the temperature exceeds 2300 °C, nitriding will be shortened. However, if the temperature is too high, the crystal grains in the sintered body to be treated will coarsening occurs.
結晶粒の粗大化を阻止するには、炭化けい素成分の添加
量を酸化けい素成分の４よりも過剰に使用し、焼結体中
に炭化けい素が残留するようにすればよい。一般に処理
時間を３０分以上と長くし、処理温度を低くすることが
品質のよい焼結体を得るのに適している。In order to prevent coarsening of crystal grains, the amount of silicon carbide component to be added may be in excess of 4 parts of the silicon oxide component so that silicon carbide remains in the sintered body. In general, increasing the treatment time to 30 minutes or more and lowering the treatment temperature are suitable for obtaining a sintered body of good quality.
実施例
炭化けい素４０重量％、酸化けい素３０重量％、窒化け
い素３０重量％、粒径各１ミクロンからなる粉体組成物
を１７００ ℃、３０１９７ｃｍ２テ１０ 分間加熱焼
成して、空孔率１体積％以下の焼結体を作った。この焼
結体から断面４酩角、長さ４０ｍの角柱状試験片を切り
出し１５００ Ｋｙ／ｃｍ２の窒素ガス圧、２０００℃
で、窒素ガス還流下で２０時間保持した。得られた焼結
体は２８Ｈ型の窒化けい素の゛ ・二）
Ｊ光ら′る焼結体１ありた・じ試験片３点曲げ強：度は
１３００℃で５２Ｋｙ／１ａｎ２であった。Example A powder composition consisting of 40% by weight of silicon carbide, 30% by weight of silicon oxide, and 30% by weight of silicon nitride, each having a particle size of 1 micron, was fired at 1700°C for 10 minutes at 30197 cm2 to determine the porosity. A sintered body containing 1% by volume or less was produced. A prismatic test piece with a cross section of 4 mm and a length of 40 m was cut out from this sintered body and heated at 2000°C under a nitrogen gas pressure of 1500 Ky/cm2.
The mixture was maintained under nitrogen gas reflux for 20 hours. The obtained sintered body was a 28H type silicon nitride sintered body.The 3-point bending strength of the same test piece was 52 Ky/1an2 at 1300°C.
−１，・“−；ｉ
巳、以ｊ上のように、本発明の方法によると、高温強度
が高く、高緻密な焼結体を製造し得られる。−1,・“−;i As described above, according to the method of the present invention, a highly dense sintered body with high high temperature strength can be manufactured.
図面は酸化けい素成分、炭化けい素及び窒素ガスが反応
して窒化けい素と一酸化炭素が生成する反応における平
衡−酸化炭素分圧を温度の関数として示した図である。The drawing shows the equilibrium carbon oxide partial pressure as a function of temperature in a reaction in which silicon oxide components, silicon carbide, and nitrogen gas react to produce silicon nitride and carbon monoxide.
Claims (1)
の焼結体を１０〜３０００ Ｋｐｍ２の窒素ガス中世１
５００〜２３００℃の温度に保持すると共に、焼ｉ体近
傍の気体の一酸化炭素ガス分圧を蟹化反、（ −３ｐ平衡分圧以下に保持することを特徴とする緻密な
焼結体の製造法。[Claims] Silicon oxide component 1 to 32.5% by weight, silicon carbide, and this sintered body are heated with nitrogen gas at 10 to 3000 Kpm2.
A dense sintered body characterized by being maintained at a temperature of 500 to 2300°C and maintaining the partial pressure of carbon monoxide gas near the sintered body to below the equilibrium partial pressure (-3p). Manufacturing method.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| JP57221276A JPS59111981A (en) | 1982-12-17 | 1982-12-17 | Manufacture of silicon nitride-containing fine sintered body |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| JP57221276A JPS59111981A (en) | 1982-12-17 | 1982-12-17 | Manufacture of silicon nitride-containing fine sintered body |
Publications (2)
| Publication Number | Publication Date |
|---|---|
| JPS59111981A true JPS59111981A (en) | 1984-06-28 |
| JPH0250074B2 JPH0250074B2 (en) | 1990-11-01 |
Family
ID=16764236
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| JP57221276A Granted JPS59111981A (en) | 1982-12-17 | 1982-12-17 | Manufacture of silicon nitride-containing fine sintered body |
Country Status (1)
| Country | Link |
|---|---|
| JP (1) | JPS59111981A (en) |
Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| JPS62148373A (en) * | 1985-12-23 | 1987-07-02 | 工業技術院長 | Heat treatment of silicon nitride base sintered body |
| US4747984A (en) * | 1985-11-18 | 1988-05-31 | Ngk Insulators, Ltd. | Production of silicon nitride sintered body |
-
1982
- 1982-12-17 JP JP57221276A patent/JPS59111981A/en active Granted
Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US4747984A (en) * | 1985-11-18 | 1988-05-31 | Ngk Insulators, Ltd. | Production of silicon nitride sintered body |
| JPS62148373A (en) * | 1985-12-23 | 1987-07-02 | 工業技術院長 | Heat treatment of silicon nitride base sintered body |
Also Published As
| Publication number | Publication date |
|---|---|
| JPH0250074B2 (en) | 1990-11-01 |
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