JPH04357187A - Sintered silicon nitride and its production - Google Patents
Sintered silicon nitride and its productionInfo
- Publication number
- JPH04357187A JPH04357187A JP3131146A JP13114691A JPH04357187A JP H04357187 A JPH04357187 A JP H04357187A JP 3131146 A JP3131146 A JP 3131146A JP 13114691 A JP13114691 A JP 13114691A JP H04357187 A JPH04357187 A JP H04357187A
- Authority
- JP
- Japan
- Prior art keywords
- silicon nitride
- sintered body
- nitride sintered
- yttrium
- sintered silicon
- 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.)
- Withdrawn
Links
- 229910052581 Si3N4 Inorganic materials 0.000 title claims abstract description 45
- HQVNEWCFYHHQES-UHFFFAOYSA-N silicon nitride Chemical compound N12[Si]34N5[Si]62N3[Si]51N64 HQVNEWCFYHHQES-UHFFFAOYSA-N 0.000 title claims abstract description 44
- 238000004519 manufacturing process Methods 0.000 title claims description 7
- BPQQTUXANYXVAA-UHFFFAOYSA-N Orthosilicate Chemical compound [O-][Si]([O-])([O-])[O-] BPQQTUXANYXVAA-UHFFFAOYSA-N 0.000 claims abstract description 8
- SIWVEOZUMHYXCS-UHFFFAOYSA-N oxo(oxoyttriooxy)yttrium Chemical compound O=[Y]O[Y]=O SIWVEOZUMHYXCS-UHFFFAOYSA-N 0.000 claims abstract description 8
- 229910052727 yttrium Inorganic materials 0.000 claims abstract description 8
- VWQVUPCCIRVNHF-UHFFFAOYSA-N yttrium atom Chemical compound [Y] VWQVUPCCIRVNHF-UHFFFAOYSA-N 0.000 claims abstract description 7
- AKTQKAXQEMMCIF-UHFFFAOYSA-N trioxido(trioxidosilyloxy)silane;yttrium(3+) Chemical compound [Y+3].[Y+3].[O-][Si]([O-])([O-])O[Si]([O-])([O-])[O-] AKTQKAXQEMMCIF-UHFFFAOYSA-N 0.000 claims abstract description 4
- 238000000034 method Methods 0.000 claims description 13
- 239000010408 film Substances 0.000 claims description 10
- 239000000843 powder Substances 0.000 claims description 8
- 238000010438 heat treatment Methods 0.000 claims description 6
- 238000005245 sintering Methods 0.000 claims description 5
- 239000010409 thin film Substances 0.000 claims description 3
- 239000000654 additive Substances 0.000 claims description 2
- TWNQGVIAIRXVLR-UHFFFAOYSA-N oxo(oxoalumanyloxy)alumane Chemical compound O=[Al]O[Al]=O TWNQGVIAIRXVLR-UHFFFAOYSA-N 0.000 claims description 2
- 230000003647 oxidation Effects 0.000 abstract description 15
- 238000007254 oxidation reaction Methods 0.000 abstract description 15
- 238000000151 deposition Methods 0.000 abstract description 2
- -1 yttrium compound Chemical class 0.000 abstract description 2
- VYPSYNLAJGMNEJ-UHFFFAOYSA-N Silicium dioxide Chemical compound O=[Si]=O VYPSYNLAJGMNEJ-UHFFFAOYSA-N 0.000 description 23
- 239000010410 layer Substances 0.000 description 17
- 229910052681 coesite Inorganic materials 0.000 description 12
- 229910052906 cristobalite Inorganic materials 0.000 description 12
- 239000000377 silicon dioxide Substances 0.000 description 12
- 229910052682 stishovite Inorganic materials 0.000 description 12
- 229910052905 tridymite Inorganic materials 0.000 description 12
- 235000012239 silicon dioxide Nutrition 0.000 description 11
- RUDFQVOCFDJEEF-UHFFFAOYSA-N yttrium(III) oxide Inorganic materials [O-2].[O-2].[O-2].[Y+3].[Y+3] RUDFQVOCFDJEEF-UHFFFAOYSA-N 0.000 description 9
- 239000011521 glass Substances 0.000 description 6
- 238000005470 impregnation Methods 0.000 description 6
- 229910052760 oxygen Inorganic materials 0.000 description 6
- 239000001301 oxygen Substances 0.000 description 6
- 229910007277 Si3 N4 Inorganic materials 0.000 description 5
- QVGXLLKOCUKJST-UHFFFAOYSA-N atomic oxygen Chemical compound [O] QVGXLLKOCUKJST-UHFFFAOYSA-N 0.000 description 5
- 239000000463 material Substances 0.000 description 5
- 239000011248 coating agent Substances 0.000 description 4
- 238000000576 coating method Methods 0.000 description 4
- 238000006243 chemical reaction Methods 0.000 description 3
- 238000010587 phase diagram Methods 0.000 description 3
- 229910018404 Al2 O3 Inorganic materials 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
- 229910021486 amorphous silicon dioxide Inorganic materials 0.000 description 2
- 239000011247 coating layer Substances 0.000 description 2
- 238000009792 diffusion process Methods 0.000 description 2
- 230000000694 effects Effects 0.000 description 2
- 238000005566 electron beam evaporation Methods 0.000 description 2
- 238000004453 electron probe microanalysis Methods 0.000 description 2
- 238000004544 sputter deposition Methods 0.000 description 2
- 238000007740 vapor deposition Methods 0.000 description 2
- 229910006360 Si—O—N Inorganic materials 0.000 description 1
- 238000002441 X-ray diffraction Methods 0.000 description 1
- 230000004913 activation Effects 0.000 description 1
- 238000004458 analytical method Methods 0.000 description 1
- 239000003795 chemical substances by application Substances 0.000 description 1
- 150000001875 compounds Chemical class 0.000 description 1
- 239000013078 crystal Substances 0.000 description 1
- 230000007547 defect Effects 0.000 description 1
- 238000010586 diagram Methods 0.000 description 1
- 239000000203 mixture Substances 0.000 description 1
- 239000002245 particle Substances 0.000 description 1
- 229910002059 quaternary alloy Inorganic materials 0.000 description 1
- 239000002994 raw material Substances 0.000 description 1
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- Ceramic Products (AREA)
Abstract
Description
【０００１】0001
【産業上の利用分野】本発明は耐熱性、耐酸化性と高強
度を必要とする高温構造材料や高温部品に好適な窒化珪
素質焼結体及びその製造方法に関する。BACKGROUND OF THE INVENTION 1. Field of the Invention The present invention relates to a silicon nitride sintered body suitable for high-temperature structural materials and high-temperature parts requiring heat resistance, oxidation resistance and high strength, and a method for manufacturing the same.
【０００２】0002
【従来の技術】窒化珪素質焼結体は耐熱および耐摩耗性
材料として期待されているが、難焼結性物質であるため
、焼結助剤としてＡｌ２ Ｏ３ ，Ｙ２ Ｏ３ 等を添
加して１７００〜１９００℃の温度で焼結する方法によ
り製造されている。しかしながら高温では大気中で保持
すると次第に酸化され、表面に酸化スケールが生成し、
重量が増える等の問題がある。この時、酸化により生成
した酸化スケールは主として高ＳｉＯ２ 濃度の多成分
系ガラス中にＳｉＯ２ やＹ２ Ｏ３ ・２ＳｉＯ２
等の結晶が分散した構造をもっており、このため酸素イ
オンの拡散が高温のＳｉＯ２ 質ガラス中では早くなり
、窒化珪素の酸化が防止できない等の問題点がある。[Prior Art] Silicon nitride sintered bodies are expected to be heat-resistant and wear-resistant materials, but since they are difficult to sinter, sintering agents such as Al2 O3 and Y2 O3 are added to make them It is manufactured by a method of sintering at a temperature of ~1900°C. However, when kept in the atmosphere at high temperatures, it gradually oxidizes and forms oxide scale on the surface.
There are problems such as increased weight. At this time, the oxide scale generated by oxidation is mainly SiO2 and Y2O3 ・2SiO2 in the multicomponent glass with high SiO2 concentration.
It has a structure in which crystals such as, etc. are dispersed, and as a result, oxygen ions diffuse quickly in high-temperature SiO2 glass, causing problems such as oxidation of silicon nitride cannot be prevented.
【０００３】0003
【発明が解決しようとする課題】本発明は上記技術水準
に鑑み、耐酸化性を付与した窒化珪素質焼結体及びその
製造方法を提供しようとするものである。SUMMARY OF THE INVENTION In view of the above state of the art, it is an object of the present invention to provide a silicon nitride sintered body having oxidation resistance and a method for manufacturing the same.
【０００４】0004
【課題を解決するための手段】上記問題点を解決するた
め、本発明者らは種々の研究を行った結果、以下の方法
で窒化珪素質焼結体の表面に緻密な結晶質のイットリア
シリケート層をコーティングすることにより耐酸化性を
付与した窒化珪素質焼結体が製造できることを見出し、
本発明を完成した。[Means for Solving the Problems] In order to solve the above-mentioned problems, the present inventors conducted various studies and found that dense crystalline yttria silicate was applied to the surface of a silicon nitride sintered body by the following method. We discovered that it is possible to produce silicon nitride sintered bodies with oxidation resistance by coating them with a layer.
The invention has been completed.
【０００５】すなわち、本発明は
（１）窒化珪素質焼結体の表面に、イットリウムダイシ
リケート質の膜が形成されていることを特徴とする窒化
珪素質焼結体。Specifically, the present invention provides (1) a silicon nitride sintered body, characterized in that a yttrium disilicate film is formed on the surface of the silicon nitride sintered body.
【０００６】（２）窒化珪素質焼結体が、焼結助剤とし
て１〜７重量％の酸化イットリウムと、１〜５重量％の
酸化アルミニウムを含み全助剤添加量が３〜１０重量％
であることを特徴とする上記（１）記載の窒化珪素質焼
結体。(2) The silicon nitride sintered body contains 1 to 7% by weight of yttrium oxide and 1 to 5% by weight of aluminum oxide as sintering aids, and the total amount of additives is 3 to 10% by weight.
The silicon nitride sintered body according to (1) above, characterized in that:
【０００７】（３）窒化珪素質焼結体を酸化イットリウ
ムおよび／またはイットリウムシリケートの粉末中で１
２００〜１５００℃の温度で熱処理することを特徴とす
る上記（１）または（２）記載の窒化珪素質焼結体の製
造方法。(3) A silicon nitride sintered body is dissolved in yttrium oxide and/or yttrium silicate powder.
The method for producing a silicon nitride sintered body according to (1) or (2) above, characterized in that heat treatment is performed at a temperature of 200 to 1500°C.
【０００８】（４）窒化珪素質焼結体表面に酸化イット
リウムおよび／またはイットリウムシリケート質の薄膜
を蒸着させた後、１２００〜１５００℃の温度で熱処理
することを特徴とする上記（１）または（２）記載の窒
化珪素質焼結体の製造方法。である。(4) The above (1) or (1) characterized in that a thin film of yttrium oxide and/or yttrium silicate is deposited on the surface of the silicon nitride sintered body, and then heat-treated at a temperature of 1200 to 1500°C. 2) The method for producing the silicon nitride sintered body. It is.
【０００９】[0009]
【作用】本発明において、窒化珪素質焼結体を酸化イッ
トリウム（Ｙ２ Ｏ３ ）および／またはイットリウム
シリケート（Ｙ２ Ｏ３ ・ｎＳｉＯ２ ）粉末中に埋
め込み、１２００〜１５００℃で熱処理するか、または
窒化珪素焼結体の表面にＹ２ Ｏ３ および／またはＹ
２ Ｏ３ ・ｎＳｉＯ２ 薄膜を高周波スパッタ法、電
子ビーム蒸着法により蒸着した後、大気中で１２００〜
１５００℃の温度で熱処理することにより窒化珪素質焼
結体の表面にイットリウムシリケート（Ｙ２ Ｏ３ ・
ｎＳｉＯ２ で通常ｎ＝２が多い）層が形成されるが、
これは大気中の酸素が侵入することにより窒化珪素質焼
結体表面が酸化されて生じたＳｉＯ２ とＹ２ Ｏ３
またはＹ２ Ｏ３ ・ｎＳｉＯ２ とが反応して、窒化
珪素質焼結体母材と強く結合したイットリウムダイシリ
ケート（Ｙ２ Ｏ３ ・２ＳｉＯ２ ）層を形成するか
らである。[Operation] In the present invention, a silicon nitride sintered body is embedded in yttrium oxide (Y2 O3) and/or yttrium silicate (Y2 O3 .nSiO2) powder and heat treated at 1200 to 1500°C, or silicon nitride sintered Y2 O3 and/or Y on the surface of the body
2 O3 ・nSiO2 thin film was deposited by high frequency sputtering method or electron beam evaporation method, and then heated in the atmosphere for 1200~
Yttrium silicate (Y2 O3 ・
A layer of nSiO2 (usually n = 2) is formed, but
This is caused by the oxidation of the surface of the silicon nitride sintered body due to the intrusion of oxygen from the atmosphere, resulting in SiO2 and Y2O3.
Alternatively, the yttrium disilicate (Y2 O3 .2SiO2) layer is formed by reacting with Y2 O3 .nSiO2 and strongly bonded to the silicon nitride sintered body base material.
【００１０】熱処理温度が１２００℃以下ではＹ２ Ｏ
３ ・２ＳｉＯ２ を形成する反応が遅く、１５００℃
以上では焼結体自身の欠陥が多くなる等の問題点が生ず
るので、好ましくは１３００〜１４００℃の範囲が良好
な結果を与える。なお、熱処理時間は温度により異なる
が、０．５〜２０時間の間で選ぶことにより目的とする
膜厚に調節することが好ましい。[0010] When the heat treatment temperature is below 1200°C, Y2O
3.The reaction to form 2SiO2 is slow and at 1500℃
If the temperature is higher than this, problems such as an increase in defects in the sintered body itself will occur, so preferably a temperature in the range of 1300 to 1400°C gives good results. Although the heat treatment time varies depending on the temperature, it is preferable to adjust the desired film thickness by selecting it between 0.5 and 20 hours.
【００１１】なお、埋め込む粉末としてはＹ２ Ｏ３
が最も簡単であるが、Ｙ２ Ｏ３ ・ＳｉＯ２ やＹ２
Ｏ３ とＳｉＯ２ の混合物でもさしつかえなく（こ
こではこれを一般にＹ２ Ｏ３ ・ｎＳｉＯ２ と表記
）、熱処理によってこれらは反応し、最終的には主とし
てＹ２ Ｏ３ ・２ＳｉＯ２ 層（ｎ＝２の化合物）と
してコーティングされる。[0011] The powder to be embedded is Y2O3
is the simplest, but Y2 O3 ・SiO2 and Y2
A mixture of O3 and SiO2 can also be used (generally referred to here as Y2 O3 .nSiO2), which react with each other through heat treatment and are finally coated as a mainly Y2 O3 .2SiO2 layer (compound with n=2). .
【００１２】以上は含浸法であるが、Ｙ２ Ｏ３ ・２
ＳｉＯ２ 層の形成はスパッタ法や電子ビーム蒸着法に
より窒化珪素質焼結体表面に膜厚２〜３μｍのＹ２ Ｏ
３ ，Ｙ２ Ｏ３ ・ＳｉＯ２ ，Ｙ２ Ｏ３ ・２Ｓ
ｉＯ２ 等をコーティングした後、大気中で１２００〜
１５００℃の温度で反応させる方法でも窒化珪素質焼結
体表面にＹ２ Ｏ３ ・２ＳｉＯ２ 層が形成される。
蒸着により得られたＹ２ Ｏ３ 膜等を高温に加熱した
場合、表面に亀裂が発生することがある。この場合でも
亀裂から侵入した酸素と窒化珪素の反応が生成した非晶
質のＳｉＯ２ とＹ２ Ｏ３ とが反応し、Ｙ２ Ｏ３
・２ＳｉＯ２ を形成することにより緻密な膜が形成
されるので問題はない。なお、膜厚が厚い場合、蒸着膜
は剥離等の問題を生ずるので厚いコーティング層は形成
できない。[0012] The above is an impregnation method, but Y2 O3 .2
The SiO2 layer is formed by depositing Y2O with a thickness of 2 to 3 μm on the surface of the silicon nitride sintered body by sputtering or electron beam evaporation.
3, Y2 O3 ・SiO2 , Y2 O3 ・2S
After coating with iO2 etc., 1200 ~
A Y2 O3 .2SiO2 layer is also formed on the surface of the silicon nitride sintered body even when the reaction is carried out at a temperature of 1500°C. When a Y2O3 film etc. obtained by vapor deposition is heated to a high temperature, cracks may occur on the surface. Even in this case, Y2 O3 reacts with amorphous SiO2 produced by the reaction between oxygen that entered through the crack and silicon nitride, and Y2 O3
- There is no problem because a dense film is formed by forming 2SiO2. Note that if the film is thick, the vapor-deposited film will cause problems such as peeling, so a thick coating layer cannot be formed.
【００１３】通常、窒化珪素の酸化により生成したＳｉ
Ｏ２ を主成分とする非晶質の酸化スケール中の酸素の
拡散速度は速いので、窒化珪素の酸化を抑制することは
できない。これに対し、結晶質の緻密なＹ２ Ｏ３・２
ＳｉＯ２ 膜の酸素の拡散の活性化エネルギーは非晶質
ＳｉＯ２ と比較すると、はるかに大きく酸素を透過し
にくいので、Ｙ２ Ｏ３ ・２ＳｉＯ２ 層を形成させ
ることにより、酸化がほとんど抑制される。[0013] Usually, Si produced by oxidation of silicon nitride
Since the diffusion rate of oxygen in the amorphous oxide scale mainly composed of O2 is fast, oxidation of silicon nitride cannot be suppressed. On the other hand, dense crystalline Y2O3.2
The activation energy for oxygen diffusion in the SiO2 film is much greater than that in amorphous SiO2, making it difficult for oxygen to pass through the film, so oxidation is almost suppressed by forming the Y2O3.2SiO2 layer.
【００１４】ここで重要なことはＡｌ２ Ｏ３ −Ｙ２
Ｏ３ −ＳｉＯ２ −Ｓｉ３ Ｎ４ 擬４元系の状態
図から判断して、Ｓｉ３ Ｎ４ とＹ２ Ｏ３ ・２Ｓ
ｉＯ２ はＡｌ−Ｙ−Ｓｉ−Ｏ−Ｎ系のガラス相と平衡
状態にあることである。
特に、焼結助剤の添加量３〜１０重量％（Ａｌ２ Ｏ３
は１〜５重量％、Ｙ２ Ｏ３ は１〜７重量％の範囲
で調整）の場合は、状態図上でＳｉ３ Ｎ４ ＋Ｙ２
Ｏ３ ・２ＳｉＯ２ ＋ガラス相が１３００℃程度の高
温で共存する状態を利用するので、窒化珪素焼結体の表
面にＹ２ Ｏ３ ・２ＳｉＯ２ 層を形成させた材料は
熱的にも安定であり、長時間の使用にも安定に耐酸化性
を維持する作用を有している。[0014] What is important here is that Al2 O3 -Y2
O3 -SiO2 -Si3 N4 Judging from the phase diagram of the quaternary system, Si3 N4 and Y2 O3 ・2S
iO2 is in equilibrium with the Al-Y-Si-O-N glass phase. In particular, the amount of sintering aid added is 3 to 10% by weight (Al2O3
(adjusted in the range of 1 to 5% by weight and Y2 O3 in the range of 1 to 7% by weight), on the phase diagram Si3 N4 + Y2
Since the state in which O3 ・2SiO2 + glass phase coexists at a high temperature of about 1300°C is utilized, the material in which the Y2 O3 ・2SiO2 layer is formed on the surface of the silicon nitride sintered body is thermally stable and can be used for a long time. It has the effect of stably maintaining oxidation resistance even when used in
【００１５】[0015]
（例１）以下、本発明の一実施例を図１によって説明す
る。図１中、１は窒化珪素質焼結体、２はＹ２ Ｏ３
またはＹ２ Ｏ３・ｎＳｉＯ２ 粉末、３はアルミナる
つぼである。図１に示すように、体積５×５×１０ｍｍ
３ の窒化珪素質焼結体１をアルミナるつぼ３中でＹ２
Ｏ３ またはＹ２ Ｏ３ ・ｎＳｉＯ２ 粉末２中に
埋め込み、１４００℃で１０時間熱処理した。得られた
試料のＸ線回折および試料断面のＥＰＭＡで分析した結
果、膜厚５〜１５μｍのＹ２ Ｏ３ ・２ＳｉＯ２ 層
が形成されていることが判明した。(Example 1) An embodiment of the present invention will be described below with reference to FIG. In Figure 1, 1 is a silicon nitride sintered body, 2 is Y2O3
or Y2O3.nSiO2 powder, 3 is an alumina crucible. As shown in Figure 1, the volume is 5 x 5 x 10 mm
3 silicon nitride sintered body 1 in an alumina crucible 3 Y2
It was embedded in O3 or Y2 O3 .nSiO2 powder 2 and heat treated at 1400°C for 10 hours. As a result of X-ray diffraction analysis of the obtained sample and EPMA analysis of the cross section of the sample, it was found that a Y2 O3 .2SiO2 layer with a thickness of 5 to 15 μm was formed.
【００１６】Ｙ２ Ｏ３ ・２ＳｉＯ２ 層を形成させ
た窒化珪素質焼結体を１３００℃で４８時間大気中で酸
化した時の重量増を従来材と比較して表１中に示す。こ
の結果、表面にコーティング処理を行うことにより耐酸
化性が飛躍的に向上することがわかった。なお含浸に用
いた原料粉末はいずれも平均粒径０．３〜１μｍ程度の
微粉末である。コーティングされたＹ２ Ｏ３ ・２Ｓ
ｉＯ２ 層とＳｉ３ Ｎ４ 焼結体の間に介在する層は
ＥＰＭＡやＳＥＭでは観察されず、両者は粒界ガラス相
と同程度の非常に薄いガラス相を通して互いに強く結合
していると考えられる。Table 1 shows the weight increase when a silicon nitride sintered body having a Y2 O3 .2SiO2 layer formed thereon was oxidized in the air at 1300° C. for 48 hours in comparison with a conventional material. As a result, it was found that oxidation resistance was dramatically improved by coating the surface. Note that the raw material powders used for impregnation are all fine powders with an average particle size of about 0.3 to 1 μm. Coated Y2 O3 ・2S
The layer intervening between the iO2 layer and the Si3N4 sintered body was not observed by EPMA or SEM, and it is thought that both are strongly bonded to each other through a very thin glass phase comparable to the grain boundary glass phase.
【表１】[Table 1]
【００１７】（例２）次に、例２として、窒化珪素質焼
結体上に厚さ２μｍのＹ２ Ｏ３ 層を形成させるか、
Ｙ２ Ｏ３ ・ＳｉＯ２ またはＹ２ Ｏ３ ・２Ｓｉ
Ｏ２ 層を２μｍ形成させた後、大気中で１３００℃に
加熱してＹ２ Ｏ３ ・２ＳｉＯ２ 層を形成させる方
法を実施した。得られた試料を１３００℃で４０時間酸
化した時の重量増を表２に示す。(Example 2) Next, as Example 2, a Y2O3 layer with a thickness of 2 μm is formed on the silicon nitride sintered body, or
Y2 O3 ・SiO2 or Y2 O3 ・2Si
After forming an O2 layer of 2 μm, a method of forming a Y2 O3 .2SiO2 layer was carried out by heating to 1300° C. in the atmosphere. Table 2 shows the weight increase when the obtained sample was oxidized at 1300° C. for 40 hours.
【表２】[Table 2]
【００１８】以上の結果、状態図上でＳｉ３ Ｎ４ と
共存状態にあり、熱力学的にも安定なＹ２ Ｏ３ ・２
ＳｉＯ２ 層を形成させることにより窒化珪素質焼結体
の耐酸化性が向上することがわかったが、コスト的には
蒸着法よりも含浸法の方がはるかに安く、また膜厚も十
分な厚さにまで形成させることができるので、含浸法の
方がより好ましい態様である。As a result of the above, Y2 O3 .2 which coexists with Si3 N4 on the phase diagram and is thermodynamically stable.
It was found that the oxidation resistance of silicon nitride sintered bodies was improved by forming a SiO2 layer, but the impregnation method was much cheaper than the vapor deposition method in terms of cost, and the film was not thick enough. The impregnation method is a more preferable embodiment because it can be formed up to a maximum of 100%.
【００１９】[0019]
【発明の効果】本発明により、熱的に安定なＹ２ Ｏ３
・２ＳｉＯ２ 層をＳｉ３ Ｎ４ 焼結体の表面にコ
ーティングすることにより、高温での耐酸化性、耐熱性
に優れた窒化珪素質焼結体が得られ、エンジン、ボイラ
ー等の高温部品として好適である。[Effect of the invention] According to the present invention, thermally stable Y2O3
・By coating the surface of the Si3 N4 sintered body with a 2SiO2 layer, a silicon nitride sintered body with excellent oxidation resistance and heat resistance at high temperatures can be obtained, making it suitable for high-temperature parts such as engines and boilers. .
【００２０】また、本発明の中で特に含浸法を採用した
場合、複雑形状品にもそのまま含浸処理によりコーティ
ング層を形成できるので、コスト的にも大幅なコスト増
をもたらすことなく耐酸化性を付与でき産業上の利用価
値が大きい。[0020] In addition, when the impregnation method is particularly adopted in the present invention, a coating layer can be formed on products with complex shapes by the impregnation treatment, so oxidation resistance can be improved without causing a significant increase in cost. It has great industrial utility value.
【図１】本発明の窒化珪素質焼結体の含浸法の実施例の
説明図。FIG. 1 is an explanatory diagram of an embodiment of the method of impregnating a silicon nitride sintered body according to the present invention.
Claims (4)
ウムダイシリケート質の膜が形成されていることを特徴
とする窒化珪素質焼結体。1. A silicon nitride sintered body, characterized in that a yttrium disilicate film is formed on the surface of the silicon nitride sintered body.
１〜７重量％の酸化イットリウムと、１〜５重量％の酸
化アルミニウムを含み全助剤添加量が３〜１０重量％で
あることを特徴とする請求項１記載の窒化珪素質焼結体
。2. The silicon nitride sintered body contains 1 to 7% by weight of yttrium oxide and 1 to 5% by weight of aluminum oxide as sintering aids, and the total amount of additives is 3 to 10% by weight. The silicon nitride sintered body according to claim 1, characterized in that:
および／またはイットリウムシリケートの粉末中で１２
００〜１５００℃の温度で熱処理することを特徴とする
請求項１または請求項２記載の窒化珪素質焼結体の製造
方法。3. A silicon nitride sintered body is mixed with yttrium oxide and/or yttrium silicate powder.
3. The method for producing a silicon nitride sintered body according to claim 1 or 2, wherein the heat treatment is performed at a temperature of 00 to 1500°C.
ウムおよび／またはイットリウムシリケート質の薄膜を
蒸着させた後、１２００〜１５００℃の温度で熱処理す
ることを特徴とする請求項１または請求項２記載の窒化
珪素質焼結体の製造方法。4. A thin film of yttrium oxide and/or yttrium silicate is deposited on the surface of the silicon nitride sintered body, and then heat-treated at a temperature of 1200 to 1500°C. A method for manufacturing the silicon nitride sintered body described above.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| JP3131146A JPH04357187A (en) | 1991-06-03 | 1991-06-03 | Sintered silicon nitride and its production |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| JP3131146A JPH04357187A (en) | 1991-06-03 | 1991-06-03 | Sintered silicon nitride and its production |
Publications (1)
| Publication Number | Publication Date |
|---|---|
| JPH04357187A true JPH04357187A (en) | 1992-12-10 |
Family
ID=15051081
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| JP3131146A Withdrawn JPH04357187A (en) | 1991-06-03 | 1991-06-03 | Sintered silicon nitride and its production |
Country Status (1)
| Country | Link |
|---|---|
| JP (1) | JPH04357187A (en) |
Cited By (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| JPH07172958A (en) * | 1993-12-22 | 1995-07-11 | Kyocera Corp | Surface-coated silicon nitride heat-resistant material |
| CN110892507A (en) * | 2017-07-13 | 2020-03-17 | 应用材料公司 | Method and apparatus for depositing yttrium-containing films |
| JP2020534684A (en) * | 2017-09-14 | 2020-11-26 | コミコ カンパニー リミテッドＫｏｍｉｃｏ Ｃｏ．，Ｌｔｄ． | Members for plasma etching equipment with improved plasma resistance and manufacturing method thereof |
-
1991
- 1991-06-03 JP JP3131146A patent/JPH04357187A/en not_active Withdrawn
Cited By (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| JPH07172958A (en) * | 1993-12-22 | 1995-07-11 | Kyocera Corp | Surface-coated silicon nitride heat-resistant material |
| CN110892507A (en) * | 2017-07-13 | 2020-03-17 | 应用材料公司 | Method and apparatus for depositing yttrium-containing films |
| CN110892507B (en) * | 2017-07-13 | 2023-07-18 | 应用材料公司 | Method and equipment for depositing yttrium-containing film |
| JP2020534684A (en) * | 2017-09-14 | 2020-11-26 | コミコ カンパニー リミテッドＫｏｍｉｃｏ Ｃｏ．，Ｌｔｄ． | Members for plasma etching equipment with improved plasma resistance and manufacturing method thereof |
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