JPH04362066A - Production of ceramic sintered body - Google Patents
Production of ceramic sintered bodyInfo
- Publication number
- JPH04362066A JPH04362066A JP3137549A JP13754991A JPH04362066A JP H04362066 A JPH04362066 A JP H04362066A JP 3137549 A JP3137549 A JP 3137549A JP 13754991 A JP13754991 A JP 13754991A JP H04362066 A JPH04362066 A JP H04362066A
- Authority
- JP
- Japan
- Prior art keywords
- sintered body
- hafnium
- ceramic sintered
- hafnium oxide
- sialon
- 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
- 239000000919 ceramic Substances 0.000 title claims abstract description 24
- 238000004519 manufacturing process Methods 0.000 title claims description 20
- WIHZLLGSGQNAGK-UHFFFAOYSA-N hafnium(4+);oxygen(2-) Chemical compound [O-2].[O-2].[Hf+4] WIHZLLGSGQNAGK-UHFFFAOYSA-N 0.000 claims abstract description 24
- 229910052581 Si3N4 Inorganic materials 0.000 claims abstract description 23
- 229910000449 hafnium oxide Inorganic materials 0.000 claims abstract description 23
- HQVNEWCFYHHQES-UHFFFAOYSA-N silicon nitride Chemical compound N12[Si]34N5[Si]62N3[Si]51N64 HQVNEWCFYHHQES-UHFFFAOYSA-N 0.000 claims abstract description 20
- 229910052735 hafnium Inorganic materials 0.000 claims abstract description 19
- 239000000203 mixture Substances 0.000 claims abstract description 16
- -1 hafnium alkoxide Chemical class 0.000 claims abstract description 6
- 229910052761 rare earth metal Inorganic materials 0.000 claims abstract description 4
- 239000002994 raw material Substances 0.000 claims description 14
- VBJZVLUMGGDVMO-UHFFFAOYSA-N hafnium atom Chemical compound [Hf] VBJZVLUMGGDVMO-UHFFFAOYSA-N 0.000 claims description 13
- 238000005245 sintering Methods 0.000 claims description 11
- 150000002894 organic compounds Chemical class 0.000 claims description 10
- 239000007788 liquid Substances 0.000 claims description 8
- PMHQVHHXPFUNSP-UHFFFAOYSA-M copper(1+);methylsulfanylmethane;bromide Chemical compound Br[Cu].CSC PMHQVHHXPFUNSP-UHFFFAOYSA-M 0.000 claims description 3
- 230000035939 shock Effects 0.000 abstract description 3
- 239000007858 starting material Substances 0.000 abstract description 2
- XAGFODPZIPBFFR-UHFFFAOYSA-N aluminium Chemical compound [Al] XAGFODPZIPBFFR-UHFFFAOYSA-N 0.000 abstract 1
- 229910052782 aluminium Inorganic materials 0.000 abstract 1
- 238000000034 method Methods 0.000 description 10
- 239000011159 matrix material Substances 0.000 description 8
- 230000000694 effects Effects 0.000 description 6
- 239000000843 powder Substances 0.000 description 6
- 239000000463 material Substances 0.000 description 5
- 238000000465 moulding Methods 0.000 description 5
- IJGRMHOSHXDMSA-UHFFFAOYSA-N Atomic nitrogen Chemical compound N#N IJGRMHOSHXDMSA-UHFFFAOYSA-N 0.000 description 4
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 description 4
- 229910001873 dinitrogen Inorganic materials 0.000 description 4
- 239000011812 mixed powder Substances 0.000 description 4
- 239000002245 particle Substances 0.000 description 4
- 239000012071 phase Substances 0.000 description 4
- 230000003647 oxidation Effects 0.000 description 3
- 238000007254 oxidation reaction Methods 0.000 description 3
- 239000011230 binding agent Substances 0.000 description 2
- 230000000052 comparative effect Effects 0.000 description 2
- 239000002612 dispersion medium Substances 0.000 description 2
- CJNBYAVZURUTKZ-UHFFFAOYSA-N hafnium(iv) oxide Chemical compound O=[Hf]=O CJNBYAVZURUTKZ-UHFFFAOYSA-N 0.000 description 2
- 239000007791 liquid phase Substances 0.000 description 2
- 238000013001 point bending Methods 0.000 description 2
- 229910002795 Si–Al–O–N Inorganic materials 0.000 description 1
- LTBRWBUKPWVGFA-UHFFFAOYSA-N butan-1-olate;hafnium(4+) Chemical compound [Hf+4].CCCC[O-].CCCC[O-].CCCC[O-].CCCC[O-] LTBRWBUKPWVGFA-UHFFFAOYSA-N 0.000 description 1
- 150000001875 compounds Chemical class 0.000 description 1
- 239000000470 constituent Substances 0.000 description 1
- 230000007797 corrosion Effects 0.000 description 1
- 238000005260 corrosion Methods 0.000 description 1
- 239000013078 crystal Substances 0.000 description 1
- 238000000280 densification Methods 0.000 description 1
- 239000006185 dispersion Substances 0.000 description 1
- BFIMXCBKRLYJQO-UHFFFAOYSA-N ethanolate;hafnium(4+) Chemical compound [Hf+4].CC[O-].CC[O-].CC[O-].CC[O-] BFIMXCBKRLYJQO-UHFFFAOYSA-N 0.000 description 1
- 238000010304 firing Methods 0.000 description 1
- 239000011521 glass Substances 0.000 description 1
- 230000005484 gravity Effects 0.000 description 1
- KIXLEMHCRGHACT-UHFFFAOYSA-N hafnium(4+);methanolate Chemical compound [Hf+4].[O-]C.[O-]C.[O-]C.[O-]C KIXLEMHCRGHACT-UHFFFAOYSA-N 0.000 description 1
- 238000007731 hot pressing Methods 0.000 description 1
- 239000011261 inert gas Substances 0.000 description 1
- 238000002156 mixing Methods 0.000 description 1
- 239000011368 organic material Substances 0.000 description 1
- TWNQGVIAIRXVLR-UHFFFAOYSA-N oxo(oxoalumanyloxy)alumane Chemical compound O=[Al]O[Al]=O TWNQGVIAIRXVLR-UHFFFAOYSA-N 0.000 description 1
- SIWVEOZUMHYXCS-UHFFFAOYSA-N oxo(oxoyttriooxy)yttrium Chemical compound O=[Y]O[Y]=O SIWVEOZUMHYXCS-UHFFFAOYSA-N 0.000 description 1
Landscapes
- Ceramic Products (AREA)
Abstract
Description
【０００１】0001
【産業上の利用分野】本発明は、機械的強度、破壊靭性
値、耐熱衝撃性等に優れた窒化ケイ素を主成分とするセ
ラミックス焼結体の製造方法に関する。BACKGROUND OF THE INVENTION 1. Field of the Invention The present invention relates to a method for manufacturing a ceramic sintered body containing silicon nitride as a main component and having excellent mechanical strength, fracture toughness, thermal shock resistance, etc.
【０００２】0002
【従来の技術】Ｓｉ−Ａｌ−Ｏ−Ｎを主構成元素とする
サイアロン系のセラミックス焼結体は、熱膨脹係数が小
さく、耐熱性、耐酸化特性、耐食性等に優れており、Ｓ
ｉ３ Ｎ ４ 系焼結体や ＳｉＣ系焼結体と共に構造
用材料として使用することが試みられている。このよう
なサイアロン系焼結体は、Ｓｉ３ Ｎ ４ 系焼結体に
比べて高温域での強度低下が小さく、かつ耐酸化性に優
れる等の特徴を有する半面、靭性が十分でないという欠
点が存在しているため、構造用材料として使用するには
、信頼性の点で劣っていた。[Prior Art] Sialon-based ceramic sintered bodies whose main constituent elements are Si-Al-O-N have a small coefficient of thermal expansion and are excellent in heat resistance, oxidation resistance, corrosion resistance, etc.
Attempts have been made to use it as a structural material together with i3N4-based sintered bodies and SiC-based sintered bodies. Although such sialon-based sintered bodies have characteristics such as less strength loss in high temperature ranges and excellent oxidation resistance compared to Si3N4-based sintered bodies, they have the disadvantage of insufficient toughness. Therefore, it was not reliable enough to be used as a structural material.
【０００３】そこで、原料混合物中にＨｆの酸化物を添
加し、液相焼結を促進して焼結体密度を向上させると共
に、焼結体の破壊靭性値を高めることが試みられている
。酸化ハフニウムは、サイアロンの結晶粒中に固溶しな
いため、母相組織中に単独で粒子形態で存在し、分散相
を構成する。これによって、破壊靭性値の向上を図るこ
とができる。また、酸化ハフニウムは、窒化ケイ素系の
セラミックス焼結体を製造する際にも、焼結助剤の一部
として使用されており、窒化ケイ素系焼結体においても
同様な効果が得られている。これらにおいて、酸化ハフ
ニウムは粉末として原料混合物中に添加している。[0003] Therefore, attempts have been made to add Hf oxide to the raw material mixture to promote liquid phase sintering to improve the density of the sintered body and to increase the fracture toughness value of the sintered body. Since hafnium oxide is not solidly dissolved in the crystal grains of Sialon, it exists alone in the form of particles in the matrix structure and constitutes a dispersed phase. This makes it possible to improve the fracture toughness value. Hafnium oxide is also used as a sintering aid when manufacturing silicon nitride-based ceramic sintered bodies, and similar effects have been obtained with silicon nitride-based sintered bodies. . In these, hafnium oxide is added as a powder to the raw material mixture.
【０００４】0004
【発明が解決しようとする課題】しかしながら、上述し
たような酸化ハフニウムを用いたサイアロン系または窒
化ケイ素系焼結体の製造方法では、酸化ハフニウムによ
る焼結体の破壊靭性値の向上等が期待できるものの、製
造ロット間による特性のばらつき、特に高温強度のばら
つきが大きく、製品特性を安定して保障することができ
ないという問題があった。[Problem to be Solved by the Invention] However, in the method for producing a sialon-based or silicon nitride-based sintered body using hafnium oxide as described above, it is expected that the fracture toughness of the sintered body will be improved by hafnium oxide. However, there was a problem in that there were large variations in properties between production lots, particularly in high-temperature strength, and that product properties could not be stably guaranteed.
【０００５】本発明は、このような課題に対処するため
になされたもので、酸化ハフニウムを用いた際に、高温
強度、破壊靭性値、耐熱衝撃性等の特性を安定に付与す
ることを可能にした、サイアロン系または窒化ケイ素系
のセラミックス焼結体の製造方法を提供することを目的
とするものである。[0005] The present invention was made to address these problems, and it is possible to stably impart properties such as high temperature strength, fracture toughness, and thermal shock resistance when using hafnium oxide. An object of the present invention is to provide a method for manufacturing a sialon-based or silicon nitride-based ceramic sintered body.
【０００６】[0006]
【課題を解決するための手段と作用】本発明における第
１のセラミックス焼結体の製造方法は、希土類元素酸化
物、窒化アルミニウムおよび酸化ハフニウムを含有する
窒化ケイ素系のセラミックス焼結体を製造するにあたり
、原料混合物中に前記酸化ハフニウムを、ハフニウムを
含む常温液状の有機化合物として添加することを特徴と
している。[Means and effects for solving the problems] A first method for manufacturing a ceramic sintered body according to the present invention includes manufacturing a silicon nitride-based ceramic sintered body containing a rare earth element oxide, aluminum nitride, and hafnium oxide. The method is characterized in that the hafnium oxide is added to the raw material mixture as an organic compound containing hafnium that is liquid at room temperature.
【０００７】また、第２のセラミックス焼結体の製造方
法は、酸化ハフニウムを含有するサイアロン系のセラミ
ックス焼結体を製造するにあたり、原料混合物中に前記
酸化ハフニウムを、ハフニウムを含む常温液状の有機化
合物として添加することを特徴としている。[0007] In addition, in the second method for producing a ceramic sintered body, when producing a sialon-based ceramic sintered body containing hafnium oxide, the hafnium oxide is added to a room temperature liquid organic material containing hafnium in a raw material mixture. It is characterized by being added as a compound.
【０００８】本発明のセラミックス焼結体の製造方法は
、窒化ケイ素系焼結体の製造方法とサイアロン系焼結体
の製造方法とに大別されるが、基本的には原料混合物中
に酸化ハフニウムを、ハフニウムを含む常温液状の有機
化合物として添加することを特徴とするものである。The method for producing a ceramic sintered body according to the present invention is roughly divided into a method for producing a silicon nitride-based sintered body and a method for producing a sialon-based sintered body, but basically, oxidation is added to the raw material mixture. This method is characterized in that hafnium is added as an organic compound containing hafnium that is liquid at room temperature.
【０００９】上記酸化ハフニウムは、焼結過程で液相を
形成し、焼結を促進して焼結体の高密度化に寄与すると
共に、焼結後は分散粒子として焼結体の機械的強度や破
壊靭性値の向上等に寄与するものである。ここで、本発
明においては酸化ハフニウムを、ハフニウムを含む常温
液状の有機化合物として添加している。これによって、
ハフニウムをより均質に原料混合物中に存在させること
が可能となるため、上記した酸化ハフニウムによる効果
を、有効かつ均一に発現させることが可能となり、製造
ロット間のばらつきを大幅に減少させることが可能とな
る。[0009] The above hafnium oxide forms a liquid phase during the sintering process, promotes sintering, and contributes to increasing the density of the sintered body, and also improves the mechanical strength of the sintered body as dispersed particles after sintering. This contributes to improvements in fracture toughness and fracture toughness. Here, in the present invention, hafnium oxide is added as an organic compound containing hafnium that is liquid at room temperature. by this,
Since hafnium can be present more homogeneously in the raw material mixture, the effects of hafnium oxide described above can be effectively and uniformly expressed, and variations between production lots can be significantly reduced. becomes.
【００１０】上記ハフニウムを含む常温液状の有機化合
物としては、例えばハフニウムテトラメトキシド、ハフ
ニウムテトラエトキシド、ハフニウムテトラブトキシド
等のハフニウムアルコキシドを使用することができる。
これらハフニウムを含む有機化合物は、セラミックス焼
結体の母相形成材料 １００重量部に対し、酸化ハフニ
ウムに換算して０．０５〜３０重量部の範囲で添加する
ことが好ましい。ハフニウムを含む有機化合物の添加量
が酸化ハフニウムに換算して０．０５重量部未満では、
緻密化向上効果があまり期待できず、３０重量部を超え
ると逆に焼結性を阻害したり、比重の増大を招いてしま
う。As the organic compound containing hafnium which is liquid at room temperature, for example, hafnium alkoxides such as hafnium tetramethoxide, hafnium tetraethoxide, and hafnium tetrabutoxide can be used. These hafnium-containing organic compounds are preferably added in an amount of 0.05 to 30 parts by weight in terms of hafnium oxide, based on 100 parts by weight of the matrix forming material of the ceramic sintered body. If the amount of the organic compound containing hafnium added is less than 0.05 parts by weight in terms of hafnium oxide,
The effect of improving densification cannot be expected to be significant, and if it exceeds 30 parts by weight, sinterability will be inhibited or the specific gravity will increase.
【００１１】本発明の窒化ケイ素系焼結体の製造方法に
おいては、窒化ケイ素そのものが母相形成材料となり、
これに焼結助剤として酸化イットリウムのような希土類
元素酸化物と窒化アルミニウムとを添加混合し、原料混
合物を調整する。これら焼結助剤は、窒化ケイ素 １０
０重量部に対して １〜１５重量部の範囲で添加するこ
とが好ましい。[0011] In the method for producing a silicon nitride-based sintered body of the present invention, silicon nitride itself serves as the matrix forming material;
A rare earth element oxide such as yttrium oxide and aluminum nitride are added and mixed as sintering aids to prepare a raw material mixture. These sintering aids are silicon nitride 10
It is preferable to add in an amount of 1 to 15 parts by weight relative to 0 parts by weight.
【００１２】また、サイアロン系焼結体の製造方法にお
いては、窒化ケイ素、酸化アルミニウムおよび窒化ケイ
素等を組み合わせて母相形成材料とする。ここで、本発
明により得ようとするサイアロン系焼結体の母相は、ほ
ぼサイアロン組成を満足するものであればよく、必ずし
も全てサイアロンである必要はない。すなわち、母相の
９０％以上がサイアロンであれば、本発明の効果が得ら
れるため、他にガラス相等の粒界相を微量含んでいても
よい。なお、サイアロンにはβ型サイアロン組成とα型
サイアロン組成とが存在するが、本発明のサイアロン系
焼結体の母相は、実質的にはβ型サイアロンである。[0012] Furthermore, in the method for producing a sialon-based sintered body, silicon nitride, aluminum oxide, silicon nitride, and the like are combined as a matrix forming material. Here, the matrix of the sialon-based sintered body to be obtained by the present invention may be one that substantially satisfies the sialon composition, and does not necessarily need to be entirely sialon. That is, if 90% or more of the parent phase is sialon, the effects of the present invention can be obtained, and therefore a small amount of grain boundary phase such as a glass phase may also be included. Although sialon has a β-sialon composition and an α-sialon composition, the matrix of the sialon-based sintered body of the present invention is substantially β-sialon.
【００１３】本発明のセラミックス焼結体の製造方法に
おいては、まず上述したような原料混合物中に、ハフニ
ウムを含む常温液状の有機化合物を添加し、十分に混合
した後、これをプレス成形法等の公知の成形法によって
所要の形状に成形する。また、スリップキャスト成形を
用いることも可能である。この後、上記成形体を不活性
ガス雰囲気中にて、１７００℃〜１９００℃程度の温度
で焼結させることにより、目的とするサイアロン系また
は窒化ケイ素系のセラミックス焼結体が得られる。本発
明の製造方法によれば、非加圧焼結によってもサイアロ
ン系または窒化ケイ素系焼結体の緻密化を図ることがで
き、かつ破壊靭性値の向上を図ることが可能であるが、
その他の焼成法、例えば雰囲気加圧焼結法、ホットプレ
ス法、熱間静水圧焼結法（ＨＩＰ）等の適用を妨げるも
のではない。In the method for producing a ceramic sintered body of the present invention, first, a room temperature liquid organic compound containing hafnium is added to the above-mentioned raw material mixture, and after thorough mixing, this is subjected to press molding or the like. It is molded into the desired shape using a known molding method. It is also possible to use slip cast molding. Thereafter, the molded body is sintered at a temperature of about 1700° C. to 1900° C. in an inert gas atmosphere to obtain the desired sialon-based or silicon nitride-based ceramic sintered body. According to the manufacturing method of the present invention, it is possible to densify the sialon-based or silicon nitride-based sintered body by non-pressure sintering, and it is also possible to improve the fracture toughness value.
This does not preclude the application of other firing methods, such as atmospheric pressure sintering, hot pressing, and hot isostatic pressure sintering (HIP).
【００１４】[0014]
【実施例】以下、本発明を実施例によって説明する。[Examples] The present invention will be explained below with reference to Examples.
【００１５】実施例１
まず、平均粒径 ０．７μｍ のＳｉ３ Ｎ ４ 粉末
に対してＡｌ２ ０ ３ 粉末を１０重量％添加し、さ
らにこれらの混合物 １００重量部に対して Ｈｆ（Ｏ
Ｃ３ Ｈ ７ ）４ を ４重量部添加し、これらをエ
タノールを分散媒として２４時間混合した後、乾燥して
原料混合粉末を調整した。次に、上記原料混合粉末 １
００重量部にバインダを約 ５重量部添加して造粒した
後、 １ｔｏｎ／ｃｍ２ の成形圧で長さ５０ｍｍ×幅
５０ｍｍ×厚さ ５ｍｍの板状成形体を作製した。Example 1 First, 10% by weight of Al203 powder was added to Si3N4 powder with an average particle size of 0.7 μm, and Hf(O) was added to 100 parts by weight of the mixture.
4 parts by weight of C3H7)4 were added, and these were mixed for 24 hours using ethanol as a dispersion medium, and then dried to prepare a raw material mixed powder. Next, the above raw material mixed powder 1
After adding about 5 parts by weight of a binder to 00 parts by weight and granulating the mixture, a plate-shaped molded body having a length of 50 mm, a width of 50 mm, and a thickness of 5 mm was produced under a molding pressure of 1 ton/cm2.
【００１６】この後、上記成形体に対して窒素ガス雰囲
気中で脱脂を施した後、常圧の窒素ガス雰囲気中におい
て１８５０℃× ２時間の条件で焼結を行い、サイアロ
ンを母相とするセラミックス焼結体を、 １００個作製
した。[0016] After that, the above molded body is degreased in a nitrogen gas atmosphere, and then sintered at 1850°C for 2 hours in a nitrogen gas atmosphere at normal pressure to make Sialon the matrix. 100 ceramic sintered bodies were produced.
【００１７】また、本発明との比較として、ハフニウム
アルコキシドに代えて酸化ハフニウム粉末を用いる以外
は、上記実施例と同一条件でサイアロン系焼結体を １
００個作製した。In addition, as a comparison with the present invention, a sialon-based sintered body was prepared under the same conditions as in the above example except that hafnium oxide powder was used instead of hafnium alkoxide.
00 pieces were produced.
【００１８】このようにして得た実施例および比較例に
よる各サイアロン系焼結体の焼結密度と、 ３点曲げ強
度試験による高温強度およびマイクロインデンテ―ショ
ン法による破壊靭性値ＫＩＣとをそれぞれ測定した。そ
れらの結果を表１に示す。The sintered densities of the sialon-based sintered bodies obtained in the Examples and Comparative Examples thus obtained, the high-temperature strength determined by the three-point bending strength test, and the fracture toughness value KIC determined by the microindentation method were determined, respectively. It was measured. The results are shown in Table 1.
【００１９】[0019]
【表１】[Table 1]
【００２０】表１の結果から明らかなように、酸化ハフ
ニウムの出発原料としてハフニウムアルコキシドを用い
ることにより、各特性の向上を図ることができると共に
、それらのバラツキを大幅に低下させることができるこ
とが分る。[0020] As is clear from the results in Table 1, by using hafnium alkoxide as a starting material for hafnium oxide, it is possible to improve each property and to significantly reduce their dispersion. Ru.
【００２１】実施例２
まず、平均粒径 ０．７μｍ のＳｉ３ Ｎ ４ 粉末
１００重量部に対して、 Ｙ２ ０ ３ を粉末５重量
部、 ＡｌＮ粉末を ５重量部、 Ｈｆ（ＯＣ３ Ｈ
７ ）４ を ２重量部添加し、これらをエタノールを
分散媒として２４時間混合した後、乾燥して原料混合粉
末を調整した。次いで、上記原料混合粉末 １００重量
部にバインダを約 ５重量部添加して造粒した後、 １
ｔｏｎ／ｃｍ２ の成形圧で長さ５０ｍｍ×幅５０ｍｍ
×厚さ ５ｍｍの板状成形体を作製した。Example 2 First, to 100 parts by weight of Si3N4 powder with an average particle size of 0.7 μm, 5 parts by weight of Y203 powder, 5 parts by weight of AlN powder, and Hf(OC3H
7) 2 parts by weight of 4 were added, mixed for 24 hours using ethanol as a dispersion medium, and then dried to prepare a raw material mixed powder. Next, about 5 parts by weight of a binder was added to 100 parts by weight of the raw material mixed powder and granulated, and then 1
Length 50mm x width 50mm with molding pressure of ton/cm2
A plate-shaped molded body having a thickness of 5 mm was produced.
【００２２】この後、上記成形体に対して窒素ガス雰囲
気中で脱脂を施した後、常圧の窒素ガス雰囲気中におい
て１８５０℃× ２時間の条件で焼結を行い、窒化ケイ
素を母相とするセラミックス焼結体を、 １００個作製
した。[0022] After that, the above-mentioned compact was degreased in a nitrogen gas atmosphere, and then sintered at 1850°C for 2 hours in a nitrogen gas atmosphere at normal pressure, thereby converting silicon nitride into a matrix. 100 ceramic sintered bodies were manufactured.
【００２３】また、本発明との比較として、ハフニウム
アルコキシドに代えて酸化ハフニウム粉末を用いる以外
は、上記実施例と同一条件でサイアロン系焼結体を １
００個作製した。In addition, as a comparison with the present invention, a sialon-based sintered body was prepared under the same conditions as in the above example except that hafnium oxide powder was used instead of hafnium alkoxide.
00 pieces were produced.
【００２４】このようにして得た実施例および比較例に
よる各窒化ケイ素系焼結体の焼結密度と、 ３点曲げ強
度試験による高温強度およびマイクロインデンテ―ショ
ン法による破壊靭性値ＫＩＣとをそれぞれ測定した。そ
れらの結果を表２に示す。[0024] The sintered density of each silicon nitride-based sintered body according to the Examples and Comparative Examples thus obtained, the high-temperature strength by the three-point bending strength test, and the fracture toughness value KIC by the microindentation method were calculated. Each was measured. The results are shown in Table 2.
【００２５】[0025]
【表２】[Table 2]
【００２６】[0026]
【発明の効果】以上説明したように、本発明のセラミッ
クス焼結体の製造方法によれば、高温強度や破壊靭性値
の向上を図ることができると共に、これら特性のばらつ
きを抑制することができ、よって再現性よく優れた特性
を有するサイアロン系焼結体や窒化ケイ素系焼結体を提
供することが可能となる。[Effects of the Invention] As explained above, according to the method for producing a ceramic sintered body of the present invention, it is possible to improve high-temperature strength and fracture toughness values, and to suppress variations in these properties. Therefore, it is possible to provide a sialon-based sintered body or a silicon nitride-based sintered body having excellent properties with good reproducibility.
Claims (3)
および酸化ハフニウムを含有する窒化ケイ素系のセラミ
ックス焼結体を製造するにあたり、原料混合物中に前記
酸化ハフニウムを、ハフニウムを含む常温液状の有機化
合物として添加することを特徴とするセラミックス焼結
体の製造方法。1. In producing a silicon nitride-based ceramic sintered body containing a rare earth element oxide, aluminum nitride, and hafnium oxide, the hafnium oxide is added to a raw material mixture as a room-temperature liquid organic compound containing hafnium. A method for producing a ceramic sintered body, characterized by:
系のセラミックス焼結体を製造するにあたり、原料混合
物中に前記酸化ハフニウムを、ハフニウムを含む常温液
状の有機化合物として添加することを特徴とするセラミ
ックス焼結体の製造方法。2. Ceramic sintering, characterized in that in producing a sialon-based ceramic sintered body containing hafnium oxide, the hafnium oxide is added to a raw material mixture as a room temperature liquid organic compound containing hafnium. How the body is manufactured.
ックス焼結体の製造方法において、前記ハフニウムを含
む有機化合物は、ハフニウムアルコキシドであることを
特徴とするセラミックス焼結体の製造方法。3. The method for producing a ceramic sintered body according to claim 1 or 2, wherein the hafnium-containing organic compound is a hafnium alkoxide.
Priority Applications (4)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| JP3137549A JPH04362066A (en) | 1991-06-10 | 1991-06-10 | Production of ceramic sintered body |
| US07/764,302 US5238885A (en) | 1990-09-25 | 1991-09-24 | Sialon type sintered bodies and method of producing the same |
| DE69107760T DE69107760T2 (en) | 1990-09-25 | 1991-09-25 | Sialon type sintered body. |
| EP91308759A EP0479485B1 (en) | 1990-09-25 | 1991-09-25 | Sialon type sintered bodies |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| JP3137549A JPH04362066A (en) | 1991-06-10 | 1991-06-10 | Production of ceramic sintered body |
Publications (1)
| Publication Number | Publication Date |
|---|---|
| JPH04362066A true JPH04362066A (en) | 1992-12-15 |
Family
ID=15201302
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| JP3137549A Pending JPH04362066A (en) | 1990-09-25 | 1991-06-10 | Production of ceramic sintered body |
Country Status (1)
| Country | Link |
|---|---|
| JP (1) | JPH04362066A (en) |
Citations (6)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| JPS61251578A (en) * | 1985-04-30 | 1986-11-08 | 住友電気工業株式会社 | Manufacture of silicon nitride sintered body |
| JPS62162673A (en) * | 1986-01-09 | 1987-07-18 | 三菱マテリアル株式会社 | Manufacture of sialon base ceramic tool for cutting cast iron |
| JPS6416791A (en) * | 1987-06-19 | 1989-01-20 | Solvay | Guanidine related compound containing substituted tetraphenylborate ion and its production |
| JPS6469569A (en) * | 1987-09-11 | 1989-03-15 | Mitsubishi Heavy Ind Ltd | Production of sintered material of silicon nitride |
| JPH01126276A (en) * | 1987-11-11 | 1989-05-18 | Inax Corp | Production of ceramic sintered body |
| JPH02248365A (en) * | 1989-02-21 | 1990-10-04 | Hoechst Ag | Silicon nitride ceramic composition |
-
1991
- 1991-06-10 JP JP3137549A patent/JPH04362066A/en active Pending
Patent Citations (6)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| JPS61251578A (en) * | 1985-04-30 | 1986-11-08 | 住友電気工業株式会社 | Manufacture of silicon nitride sintered body |
| JPS62162673A (en) * | 1986-01-09 | 1987-07-18 | 三菱マテリアル株式会社 | Manufacture of sialon base ceramic tool for cutting cast iron |
| JPS6416791A (en) * | 1987-06-19 | 1989-01-20 | Solvay | Guanidine related compound containing substituted tetraphenylborate ion and its production |
| JPS6469569A (en) * | 1987-09-11 | 1989-03-15 | Mitsubishi Heavy Ind Ltd | Production of sintered material of silicon nitride |
| JPH01126276A (en) * | 1987-11-11 | 1989-05-18 | Inax Corp | Production of ceramic sintered body |
| JPH02248365A (en) * | 1989-02-21 | 1990-10-04 | Hoechst Ag | Silicon nitride ceramic composition |
Similar Documents
| Publication | Publication Date | Title |
|---|---|---|
| KR101470322B1 (en) | Aluminum Nitride ceramics with high strength and the method of low temperature sintering thereof | |
| JP4348429B2 (en) | Porous silicon nitride and method for producing the same | |
| KR102565344B1 (en) | Aluminium nitride ceramics composition and manufacturing method thereof | |
| JPH04362066A (en) | Production of ceramic sintered body | |
| JP3454994B2 (en) | Silicon nitride sintered body and method for producing the same | |
| JP3145519B2 (en) | Aluminum nitride sintered body | |
| JP3271123B2 (en) | Method for producing composite of silicon nitride and boron nitride | |
| KR102216429B1 (en) | Cordierite based ceramic composition for use of ceramic heater | |
| JP2534213B2 (en) | Method for producing silicon nitride based sintered body | |
| JPH06263544A (en) | Sialon-based composite sintered compact and its production | |
| JP2980342B2 (en) | Ceramic sintered body | |
| JPH04132668A (en) | Ceramic sintered compact and production thereof | |
| JP2671539B2 (en) | Method for producing silicon nitride sintered body | |
| JPH08198664A (en) | Alumina-base sintered body and its production | |
| JP2541150B2 (en) | Aluminum nitride sintered body | |
| JP2581128B2 (en) | Alumina-sialon composite sintered body | |
| JP2001322874A (en) | Aluminum nitride sintered body and method for manufacturing the same | |
| JP2687634B2 (en) | Method for producing silicon nitride sintered body | |
| JPH05339061A (en) | Silicon nitride sintered body and its production | |
| JPH04951B2 (en) | ||
| JP2536448B2 (en) | Aluminum nitride sintered body | |
| JPH05117041A (en) | Production of sialon-based sintered compact | |
| JP2687633B2 (en) | Method for producing silicon nitride sintered body | |
| JP2001139379A (en) | Method of producing highly thermal conductive aluminum nitride sintered compact | |
| JPH06219852A (en) | Particle dispersed sialon sintered compact |
Legal Events
| Date | Code | Title | Description |
|---|---|---|---|
| A02 | Decision of refusal |
Free format text: JAPANESE INTERMEDIATE CODE: A02 Effective date: 19950131 |