JPH04275982A - Boron nitride-aluminum nitride combined sintered body and its production - Google Patents
Boron nitride-aluminum nitride combined sintered body and its productionInfo
- Publication number
- JPH04275982A JPH04275982A JP3058210A JP5821091A JPH04275982A JP H04275982 A JPH04275982 A JP H04275982A JP 3058210 A JP3058210 A JP 3058210A JP 5821091 A JP5821091 A JP 5821091A JP H04275982 A JPH04275982 A JP H04275982A
- Authority
- JP
- Japan
- Prior art keywords
- sintered body
- aluminum nitride
- boron nitride
- sintering
- weight
- 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
- 238000004519 manufacturing process Methods 0.000 title claims description 7
- ZOXJGFHDIHLPTG-UHFFFAOYSA-N Boron Chemical compound [B] ZOXJGFHDIHLPTG-UHFFFAOYSA-N 0.000 title abstract 2
- 229910052796 boron Inorganic materials 0.000 title abstract 2
- 238000005245 sintering Methods 0.000 claims abstract description 41
- PMHQVHHXPFUNSP-UHFFFAOYSA-M copper(1+);methylsulfanylmethane;bromide Chemical compound Br[Cu].CSC PMHQVHHXPFUNSP-UHFFFAOYSA-M 0.000 claims abstract description 33
- 229910052582 BN Inorganic materials 0.000 claims abstract description 30
- PZNSFCLAULLKQX-UHFFFAOYSA-N Boron nitride Chemical compound N#B PZNSFCLAULLKQX-UHFFFAOYSA-N 0.000 claims abstract description 30
- 238000010438 heat treatment Methods 0.000 claims abstract description 13
- 239000002131 composite material Substances 0.000 claims description 31
- 239000000843 powder Substances 0.000 claims description 16
- QVGXLLKOCUKJST-UHFFFAOYSA-N atomic oxygen Chemical compound [O] QVGXLLKOCUKJST-UHFFFAOYSA-N 0.000 claims description 11
- 239000001301 oxygen Substances 0.000 claims description 11
- 229910052760 oxygen Inorganic materials 0.000 claims description 11
- 239000002245 particle Substances 0.000 claims description 10
- 239000000203 mixture Substances 0.000 claims description 9
- 238000000137 annealing Methods 0.000 abstract description 2
- 238000000034 method Methods 0.000 description 12
- 238000010292 electrical insulation Methods 0.000 description 11
- 239000000463 material Substances 0.000 description 7
- 230000000694 effects Effects 0.000 description 6
- 239000002994 raw material Substances 0.000 description 6
- 239000012298 atmosphere Substances 0.000 description 4
- 230000000052 comparative effect Effects 0.000 description 4
- JKWMSGQKBLHBQQ-UHFFFAOYSA-N diboron trioxide Chemical compound O=BOB=O JKWMSGQKBLHBQQ-UHFFFAOYSA-N 0.000 description 4
- 239000007789 gas Substances 0.000 description 4
- 239000011261 inert gas Substances 0.000 description 4
- 230000006866 deterioration Effects 0.000 description 3
- 238000002156 mixing Methods 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
- CURLTUGMZLYLDI-UHFFFAOYSA-N Carbon dioxide Chemical compound O=C=O CURLTUGMZLYLDI-UHFFFAOYSA-N 0.000 description 2
- ODINCKMPIJJUCX-UHFFFAOYSA-N calcium oxide Inorganic materials [Ca]=O ODINCKMPIJJUCX-UHFFFAOYSA-N 0.000 description 2
- 238000000280 densification Methods 0.000 description 2
- 238000000151 deposition Methods 0.000 description 2
- 229910002804 graphite Inorganic materials 0.000 description 2
- 239000010439 graphite Substances 0.000 description 2
- 239000011810 insulating material Substances 0.000 description 2
- 238000002844 melting Methods 0.000 description 2
- 230000008018 melting Effects 0.000 description 2
- SIWVEOZUMHYXCS-UHFFFAOYSA-N oxo(oxoyttriooxy)yttrium Chemical compound O=[Y]O[Y]=O SIWVEOZUMHYXCS-UHFFFAOYSA-N 0.000 description 2
- 230000000704 physical effect Effects 0.000 description 2
- -1 rare earth compounds Chemical class 0.000 description 2
- 239000002904 solvent Substances 0.000 description 2
- IJGRMHOSHXDMSA-UHFFFAOYSA-N Atomic nitrogen Chemical compound N#N IJGRMHOSHXDMSA-UHFFFAOYSA-N 0.000 description 1
- 239000004215 Carbon black (E152) Substances 0.000 description 1
- 230000002411 adverse Effects 0.000 description 1
- 229910052786 argon Inorganic materials 0.000 description 1
- 229910052810 boron oxide Inorganic materials 0.000 description 1
- 229910002092 carbon dioxide Inorganic materials 0.000 description 1
- 239000001569 carbon dioxide Substances 0.000 description 1
- 239000000919 ceramic Substances 0.000 description 1
- 150000001875 compounds Chemical class 0.000 description 1
- 229910001873 dinitrogen Inorganic materials 0.000 description 1
- 239000001307 helium Substances 0.000 description 1
- 229910052734 helium Inorganic materials 0.000 description 1
- SWQJXJOGLNCZEY-UHFFFAOYSA-N helium atom Chemical compound [He] SWQJXJOGLNCZEY-UHFFFAOYSA-N 0.000 description 1
- 238000007731 hot pressing Methods 0.000 description 1
- 229930195733 hydrocarbon Natural products 0.000 description 1
- 150000002430 hydrocarbons Chemical class 0.000 description 1
- 238000000462 isostatic pressing Methods 0.000 description 1
- 238000000465 moulding Methods 0.000 description 1
- 239000012299 nitrogen atmosphere Substances 0.000 description 1
- 230000001737 promoting effect Effects 0.000 description 1
- 229910052761 rare earth metal Inorganic materials 0.000 description 1
- 238000003826 uniaxial pressing Methods 0.000 description 1
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 description 1
Abstract
Description
【０００１】0001
【産業の利用分野】本発明は、高純度でかつ高温での電
気絶縁性に優れる窒化ほう素・窒化アルミニウム複合焼
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 boron nitride/aluminum nitride composite sintered body having high purity and excellent electrical insulation properties at high temperatures, and a method for producing the same.
【０００２】0002
【従来の技術及び発明が解決しようとする課題】従来よ
り、機械加工が可能なセラミックスとして窒化ほう素と
窒化アルミニウムとの複合焼結体が知られており、この
複合焼結体は、窒化ほう素、窒化アルミニウムともに難
焼結性物質であることから緻密な焼結体を得るために焼
結助剤を用いて焼結製造することが行われている。[Prior Art and Problems to be Solved by the Invention] Composite sintered bodies of boron nitride and aluminum nitride have been known as ceramics that can be machined. Since aluminum nitride and aluminum nitride are both difficult to sinter, sintering is carried out using a sintering aid in order to obtain a dense sintered body.
【０００３】この場合、焼結助剤としては、Ｙ２Ｏ３等
の希土類化合物の他にＢ２Ｏ３、ＣａＯ等も使用される
が、通常焼結助剤として用いられるものは低融点化合物
であり、これらが焼結体中に残存すると、高温下での強
度、電気絶縁性の低下といった焼結体の高温特性を低下
させる原因となる。In this case, in addition to rare earth compounds such as Y2O3, B2O3 and CaO are also used as sintering aids, but the ones normally used as sintering aids are low melting point compounds; If it remains in the sintered body, it causes deterioration in the high-temperature properties of the sintered body, such as a decrease in strength and electrical insulation at high temperatures.
【０００４】一方、窒化ほう素・窒化アルミニウム複合
焼結体は、優れた耐熱性を有することから高温下で用い
られることが多いが、この場合上記焼結助剤による高温
強度や高温電気絶縁性の低下は、その応用範囲を制限す
る原因になっている。On the other hand, boron nitride/aluminum nitride composite sintered bodies are often used at high temperatures because of their excellent heat resistance, but in this case, the high-temperature strength and high-temperature electrical insulation properties are The decrease in the amount of carbon dioxide has become a cause of limiting its range of application.
【０００５】本発明は、上記事情に鑑みなされたもので
、高純度でかつ高温強度や高温電気絶縁性といった高温
特性に優れ、種々の用途に応用可能な窒化ほう素・窒化
アルミニウム複合焼結体及びその製造方法を提供するこ
とを目的とする。The present invention was made in view of the above circumstances, and provides a boron nitride/aluminum nitride composite sintered body that is highly pure and has excellent high temperature properties such as high temperature strength and high temperature electrical insulation, and can be applied to various uses. The purpose is to provide a method for producing the same.
【０００６】[0006]
【課題を解決しようとする手段及び作用】本発明者は、
上記目的を達成するため鋭意検討を行った結果、窒化ほ
う素と窒化アルミニウムとを混合焼結する際に、焼結助
剤、特に低融点の焼結助剤を用いて焼結体の緻密化を促
進させ、焼結後に焼結体を高温加熱処理してアニールす
ることにより、焼結体中の過剰な焼結助剤を気散させ、
又は焼結体表面に析出させた後に取り除くことによって
純度及び高温下での電気絶縁性を改善し得ることを見出
した。[Means and effects for solving the problem] The present inventors:
As a result of intensive studies to achieve the above objectives, we found that when boron nitride and aluminum nitride are mixed and sintered, a sintering aid, especially a low melting point sintering aid, is used to densify the sintered body. By promoting the sintering process and annealing the sintered body by high-temperature heat treatment after sintering, the excess sintering aid in the sintered body is diffused.
Alternatively, it has been found that purity and electrical insulation properties at high temperatures can be improved by depositing on the surface of a sintered body and then removing it.
【０００７】そして更に、本発明者は上記純度及び高温
電気絶縁性の改善効果が良好に発揮される焼結材料及び
加熱処理条件を見出すべく更に検討を進めた結果、焼結
材料としては、平均粒子径１０μｍ以下の窒化アルミニ
ウム粉末を５〜９０重量％、平均粒子径２０μｍ以下の
窒化ほう素粉末を５〜９０重量％及び焼結助剤を１〜１
０重量％の範囲でそれぞれ含有し、これらの合計が１０
０重量％となる組成物が好適であり、また加熱処理条件
としては、不活性ガス雰囲気下において常圧又は減圧下
に１７００〜２３００℃の温度で熱処理する条件が良好
な結果を与え、上記焼結材料を焼結して得られた複合焼
結体を上記条件で加熱処理することにより、残存酸素量
が１重量％以下で１０００℃における体積抵抗率が２×
１０８Ωｃｍ以上である高純度で良好な高温電気絶縁性
を有する窒化ほう素・窒化アルミニウム複合焼結体が得
られることを知見し、本発明を完成するに至ったもので
ある。[0007] Further, the present inventor conducted further studies in order to find a sintering material and heat treatment conditions that would exhibit the above-mentioned purity and high-temperature electrical insulation improvement effects favorably. As a result, as a sintered material, the average 5-90% by weight of aluminum nitride powder with a particle size of 10 μm or less, 5-90% by weight of boron nitride powder with an average particle size of 20 μm or less, and 1-1% of a sintering aid.
They each contain within the range of 0% by weight, and the total of these is 10% by weight.
A composition in which the concentration is 0% by weight is suitable, and as the heat treatment conditions, heat treatment at a temperature of 1700 to 2300°C under an inert gas atmosphere at normal pressure or reduced pressure gives good results. By heat-treating the composite sintered body obtained by sintering the sintering material under the above conditions, the volume resistivity at 1000°C is 2x with a residual oxygen amount of 1% by weight or less.
It was discovered that a boron nitride/aluminum nitride composite sintered body having a high purity of 108 Ωcm or more and good high-temperature electrical insulation properties can be obtained, and the present invention was completed.
【０００８】従って、本発明は、残存酸素量が１重量％
以下で１０００℃における体積抵抗率が２×１０８Ωｃ
ｍ以上であることを特徴とする窒化ほう素・窒化アルミ
ニウム複合焼結体、及び平均粒子径１０μｍ以下の窒化
アルミニウム粉末を５〜９０重量％、平均粒子径２０μ
ｍ以下の窒化ほう素粉末を５〜９０重量％及び焼結助剤
を１〜１０重量％の範囲でそれぞれ含有し、これらの合
計が１００重量％となる組成物を焼結してなる複合焼結
体を不活性ガス雰囲気下において常圧又は減圧下に１７
００〜２３００℃の温度で熱処理することにより上記窒
化ほう素・窒化アルミニウム複合焼結体を得ることを特
徴とする窒化ほう素・窒化アルミニウム複合焼結体の製
造方法を提供するものである。Therefore, in the present invention, the amount of residual oxygen is 1% by weight.
Below, the volume resistivity at 1000℃ is 2×108Ωc
A boron nitride/aluminum nitride composite sintered body characterized by having a particle size of 5 to 90% by weight and an average particle size of 20 μm or less, and an aluminum nitride powder having an average particle size of 10 μm or less.
A composite sintered product obtained by sintering a composition containing boron nitride powder of 5 to 90% by weight and a sintering aid in a range of 1 to 10% by weight, the total of which is 100% by weight. The aggregate is heated under normal pressure or reduced pressure under an inert gas atmosphere.
The present invention provides a method for manufacturing a boron nitride/aluminum nitride composite sintered body, characterized in that the boron nitride/aluminum nitride composite sintered body is obtained by heat treatment at a temperature of 00 to 2300°C.
【０００９】以下、本発明につき更に詳述すると、本発
明の窒化ほう素・窒化アルミニウム複合焼結体は、上述
したように残存酸素量が１重量％以下で、１０００℃に
おける体積抵抗率が２×１０８Ωｃｍ以上のものである
が、この場合、残存酸素量が１重量％を超えたり、体積
抵抗率が２×１０８Ωｃｍ未満であると、高温電気特性
などの高温物性が低下し、本発明の目的を達成すること
ができず、また１０００℃を超えるような高温下に晒さ
れる高温炉用の絶縁材や処理物容器として用いた場合、
ガスの発生などにより炉内の処理物に悪影響を与える場
合がある。なお、より好ましい残存酸素量は０．５重量
％以下、より好ましい体積抵抗率は１０１０Ωｃｍ以上
、特に１０１２〜１０１６Ωｃｍである。The present invention will be described in more detail below. As mentioned above, the boron nitride/aluminum nitride composite sintered body has a residual oxygen content of 1% by weight or less and a volume resistivity of 2 at 1000°C. x 108 Ωcm or more, but in this case, if the residual oxygen amount exceeds 1% by weight or the volume resistivity is less than 2 x 108 Ωcm, high-temperature physical properties such as high-temperature electrical properties deteriorate, and the object of the present invention is When used as an insulating material or processing material container for a high-temperature furnace that is exposed to high temperatures exceeding 1000°C,
The production of gas may have an adverse effect on the processed material in the furnace. In addition, a more preferable residual oxygen amount is 0.5% by weight or less, and a more preferable volume resistivity is 1010 Ωcm or more, particularly 1012 to 1016 Ωcm.
【００１０】このような窒化ほう素・窒化アルミニウム
複合焼結体は、上述したように窒化アルミニウム粉末、
窒化ほう素粉末及び焼結助剤からなる混合物を焼結して
得た複合焼結体を高温加熱処理することにより、焼結体
中の過剰な焼結助剤を気散させ、又は焼結体表面に析出
させた後に取り除くことによって得ることができる。[0010] Such a boron nitride/aluminum nitride composite sintered body is made of aluminum nitride powder, aluminum nitride powder,
By heating a composite sintered body obtained by sintering a mixture consisting of boron nitride powder and a sintering aid at a high temperature, excess sintering aid in the sintered body is diffused or sintered. It can be obtained by depositing it on the body surface and then removing it.
【００１１】この場合、上記焼結原料混合物中の窒化ア
ルミニウム粉末としては、平均粒子径１０μｍ以下、好
ましくは０．５〜５μｍのものが５〜９０％（重量％、
以下同じ）、好ましくは３５〜６０％配合され、また窒
化ほう素粉末としては、平均粒子径２０μｍ以下、好ま
しくは０．５〜１０μｍのものが５〜９０％、好ましく
は３５〜６０％配合され、更に焼結助剤としては、Ｙ２
Ｏ３、Ｂ２Ｏ３、ＣａＯ、等が１〜１０％、好ましくは
３〜５％配合され、これらの３成分の合計が１００％と
なる組成物を焼結原料とする。この組成物は上記３成分
を混合することにより調製され、この場合の混合方法は
乾式で行ってもよいが、特に湿式で行うことが好ましく
、湿式で行う場合に用いられる分散媒としては、アルコ
ール類、炭化水素系溶媒を用いることが適当であり、水
は窒化アルミニウムを分解する恐れがあるので用いるべ
きではない。In this case, 5 to 90% (by weight,
The same applies below), preferably 35 to 60%, and boron nitride powder with an average particle size of 20 μm or less, preferably 0.5 to 10 μm, is 5 to 90%, preferably 35 to 60%. , Furthermore, as a sintering aid, Y2
A composition in which O3, B2O3, CaO, etc. are blended in an amount of 1 to 10%, preferably 3 to 5%, and the total of these three components is 100% is used as a sintering raw material. This composition is prepared by mixing the above three components, and although the mixing method in this case may be carried out in a dry manner, it is particularly preferable to carry out in a wet manner. It is appropriate to use hydrocarbon-based solvents such as the like, and water should not be used since it may decompose aluminum nitride.
【００１２】なお、上記焼結原料組成物中の窒化アルミ
ニウム粉末の配合量が９０％を超えると、得られる複合
焼結体の機械加工性が極度に低下してしまい、窒化ほう
素粉末の配合量が９０％を超えると、機械加工性は優れ
るものの緻密化が困難になり、強度の低下を招くことに
なる。また、この組成物中の窒化アルミニウムと窒化ほ
う素との好ましい配合比率は、重量比で６０：４０〜８
０：２０である。[0012] If the amount of aluminum nitride powder in the sintering raw material composition exceeds 90%, the machinability of the resulting composite sintered body will be extremely reduced, and the amount of boron nitride powder will be reduced. If the amount exceeds 90%, although machinability is excellent, densification becomes difficult, resulting in a decrease in strength. Further, the preferred blending ratio of aluminum nitride and boron nitride in this composition is 60:40 to 8 by weight.
It was 0:20.
【００１３】この焼結原料から複合焼結体を得る方法と
しては、一軸加圧成形、静水圧加圧成形などの通常の成
形法で所望の形状に成形した後、成形体を不活性ガス雰
囲気中で焼結する通常の方法が用いられる。この場合、
焼結温度は通常１７００〜２１００℃とされ、１７００
℃未満では緻密な焼結体が得られにくく、一方２１００
℃を超える温度にしても焼結体の緻密化効果に変わりは
なく、経済的に不利となる。なお、成形法や焼結法は、
上記の方法に限定されず、例えば原料粉末を黒鉛製金型
に充填し、加熱と加圧を同時に行う熱間加圧法やＨＩＰ
など、粉末原料の焼結に通常用いられる他の方法を採用
することは差し支えない。[0013] The method for obtaining a composite sintered body from this sintered raw material is to mold it into a desired shape by a normal forming method such as uniaxial pressing or isostatic pressing, and then place the molded body in an inert gas atmosphere. The usual method of sintering in a container is used. in this case,
The sintering temperature is usually 1700-2100℃,
Below 2100°C, it is difficult to obtain a dense sintered body;
Even if the temperature exceeds .degree. C., there is no change in the densification effect of the sintered body, which is economically disadvantageous. In addition, the molding method and sintering method are
Not limited to the above methods, for example, hot pressing method in which raw material powder is filled into a graphite mold and heated and pressurized at the same time, HIP
There is no problem in adopting other methods commonly used for sintering powder raw materials.
【００１４】本発明の窒化ほう素・窒化アルミニウム複
合焼結体は、上記焼結原料を上記成形，焼結方法で焼結
して複合焼結体を得た後、これを高温加熱処理すること
により、高温電気絶縁性などの高温下での物性を低下さ
せる原因となる過剰な焼結助剤を該複合焼結体から除去
することにより得ることができる。[0014] The boron nitride/aluminum nitride composite sintered body of the present invention can be obtained by sintering the above-mentioned sintering raw material by the above-described forming and sintering method to obtain a composite sintered body, and then subjecting this to high-temperature heat treatment. This can be obtained by removing from the composite sintered body excess sintering aid that causes deterioration of physical properties at high temperatures, such as high-temperature electrical insulation.
【００１５】この場合、加熱処理条件としては、窒素ガ
ス、アルゴンガス、ヘリウムガス等の不活性ガス雰囲気
下において常圧下又は減圧下に１７００〜２３００℃、
好ましくは１９００〜２１００℃の温度で１時間以上、
特に３〜２４時間程度熱処理する条件とされる。処理温
度が１７００℃未満では焼結助剤を良好に除去すること
が困難であり、一方２３００℃を超える温度で処理を行
っても炉材の消耗が激しくなるだけで焼結助剤の除去効
果は向上せず、不経済である。また、処理時間が１時間
未満であると、過剰の焼結助剤が残留してしまう場合が
あり、十分な高温特性が得られない場合がある。なお、
減圧下に処理を行う場合は、処理温度が２０００℃を超
えると窒化アルミニウム及び窒化ほう素が分解してしま
う恐れがあるので、この場合は処理温度を２０００℃以
下とすることが好ましい。この加熱処理により、過剰な
焼結助剤が気散又は焼結体表面に析出するが、この場合
焼結体表面に析出した焼結助剤は機械的又は表面に析出
した成分を溶解することが可能な溶媒を用いて化学的に
除去するものである。In this case, the heat treatment conditions are 1700 to 2300° C. under normal pressure or reduced pressure in an inert gas atmosphere such as nitrogen gas, argon gas, helium gas, etc.
Preferably at a temperature of 1900 to 2100°C for 1 hour or more,
In particular, the conditions are such that the heat treatment is performed for about 3 to 24 hours. If the treatment temperature is less than 1700°C, it is difficult to remove the sintering aid properly, while if the treatment is performed at a temperature higher than 2300°C, the furnace material will only be consumed more rapidly and the removal effect of the sintering aid will be reduced. is not improved and is uneconomical. Furthermore, if the treatment time is less than 1 hour, excessive sintering aid may remain and sufficient high temperature properties may not be obtained. In addition,
If the treatment is carried out under reduced pressure, aluminum nitride and boron nitride may decompose if the treatment temperature exceeds 2000°C, so in this case the treatment temperature is preferably 2000°C or less. Due to this heat treatment, excessive sintering aid is diffused or precipitated on the surface of the sintered compact, but in this case, the sintering aid precipitated on the surface of the sintered compact cannot be mechanically or dissolved the components precipitated on the surface. It is chemically removed using a solvent that allows for
【００１６】[0016]
【実施例】以下、実施例，比較例を示して本発明を具体
的に説明するが、本発明は下記実施例に制限されるもの
ではない。EXAMPLES The present invention will be specifically explained below with reference to Examples and Comparative Examples, but the present invention is not limited to the following Examples.
【００１７】［実施例１，比較例１］平均粒子径３μｍ
の窒化アルミニウム粉末、平均粒子径３μｍの窒化ほう
素粉末及び焼結助剤として酸化イットリウムを表１に示
した割合で混合し、１９００℃、２００ｋｇ／ｃｍ２の
圧力で１時間熱間加圧成形し、３種類の複合焼結体を得
た。[Example 1, Comparative Example 1] Average particle diameter 3 μm
Aluminum nitride powder, boron nitride powder with an average particle size of 3 μm, and yttrium oxide as a sintering aid were mixed in the proportions shown in Table 1, and the mixture was hot-pressed at 1900°C and a pressure of 200 kg/cm2 for 1 hour. , three types of composite sintered bodies were obtained.
【００１８】得られた複合焼結体をそれぞれ５０ｍｍ×
５０ｍｍ×１０ｍｍに加工し、黒鉛容器内で窒素雰囲気
下に常圧２０００℃で１０時間加熱した。処理後、それ
ぞれの複合焼結体から試験片を採取し、残存酸素量及び
１０００℃での体積抵抗率を測定した。結果を表１に示
す。なお、残存酸素量は非分散赤外分光器を用いて測定
した。また、比較のため上記加熱処理を行わなかった以
外は同様にして得た複合焼結体からも試験片を採取し、
同様に残存酸素量及び体積抵抗率を測定した。結果を表
１に併記する。なお、表中％はすべて重量％である。[0018] Each of the obtained composite sintered bodies has a size of 50 mm×
It was processed into a size of 50 mm x 10 mm and heated in a graphite container under a nitrogen atmosphere at normal pressure of 2000° C. for 10 hours. After the treatment, test pieces were taken from each composite sintered body, and the residual oxygen amount and volume resistivity at 1000°C were measured. The results are shown in Table 1. Note that the amount of residual oxygen was measured using a non-dispersive infrared spectrometer. For comparison, test pieces were also collected from composite sintered bodies obtained in the same manner except that the heat treatment was not performed.
The residual oxygen amount and volume resistivity were measured in the same manner. The results are also listed in Table 1. Note that all percentages in the table are percentages by weight.
【００１９】[0019]
【表１】[Table 1]
【００２０】［実施例２，比較例２］焼結助剤として酸
化イットリウムに代えて酸化ほう素を用いた以外は実施
例１及び比較例１と同様にして６種類の窒化ほう素・窒
化アルミニウム複合焼結体を得、これらについて上記と
同様にして残存酸素量及び体積抵抗率を測定した。結果
を表２に示す。[Example 2, Comparative Example 2] Six types of boron nitride and aluminum nitride were prepared in the same manner as in Example 1 and Comparative Example 1, except that boron oxide was used instead of yttrium oxide as a sintering aid. Composite sintered bodies were obtained, and the residual oxygen amount and volume resistivity were measured in the same manner as above. The results are shown in Table 2.
【００２１】[0021]
【表２】
表１及び表２の結果から、本発明の窒化ほう素・窒化ア
ルミニウム複合焼結体は残存酸素量が少ないことからＹ
２Ｏ３、Ｂ２Ｏ３の残存量が非常に少ないものであり、
従って十分な高純度化が達成され、しかもその体積抵抗
率をみると高温での電気絶縁性が改善されていることが
確認された。[Table 2] From the results in Tables 1 and 2, it is clear that the boron nitride/aluminum nitride composite sintered body of the present invention has a small amount of residual oxygen.
The remaining amount of 2O3 and B2O3 is very small,
Therefore, it was confirmed that a sufficiently high degree of purity was achieved, and that the electrical insulation properties at high temperatures were improved when looking at the volume resistivity.
【００２２】[0022]
【発明の効果】本発明の窒化ほう素・窒化アルミニウム
複合焼結体は、高純度で高温電気絶縁性等の高温特性に
優れ、１０００℃以上の高温においても電気絶縁性の低
下が比較的少ない。また、２０００℃付近の高温下でも
焼結体からのガス発生が少なく、従って従来高温特性の
低下から用いることが困難であった高温炉の絶縁材や処
理物容器などの高温下に晒される用途にも利用すること
ができ、窒化ほう素・窒化アルミニウム複合焼結体の応
用範囲を拡大するものである。Effect of the invention: The boron nitride/aluminum nitride composite sintered body of the present invention has high purity and excellent high-temperature properties such as high-temperature electrical insulation, and shows relatively little decrease in electrical insulation even at high temperatures of 1000°C or higher. . In addition, there is little gas generation from the sintered compact even at high temperatures around 2000°C, so it is suitable for applications that are exposed to high temperatures, such as insulating materials for high-temperature furnaces and containers for processed materials, which were previously difficult to use due to deterioration of high-temperature properties. This expands the range of applications of boron nitride/aluminum nitride composite sintered bodies.
【００２３】また、本発明の製造方法によれば、上記窒
化ほう素・窒化アルミニウム複合焼結体を確実に得るこ
とができる。Furthermore, according to the manufacturing method of the present invention, the boron nitride/aluminum nitride composite sintered body can be reliably obtained.
Claims (2)
℃における体積抵抗率が２×１０８Ωｃｍ以上であるこ
とを特徴とする窒化ほう素・窒化アルミニウム複合焼結
体。[Claim 1] 1000 with residual oxygen amount of 1% by weight or less
A boron nitride/aluminum nitride composite sintered body having a volume resistivity of 2×10 8 Ωcm or more at °C.
ニウム粉末を５〜９０重量％、平均粒子径２０μｍ以下
の窒化ほう素粉末を５〜９０重量％及び焼結助剤を１〜
１０重量％の範囲でそれぞれ含有し、これらの合計が１
００重量％となる組成物を焼結してなる複合焼結体を不
活性ガス雰囲気下において常圧又は減圧下に１７００〜
２３００℃の温度で熱処理することにより請求項１記載
の窒化ほう素・窒化アルミニウム複合焼結体を得ること
を特徴とする窒化ほう素・窒化アルミニウム複合焼結体
の製造方法。2. 5-90% by weight of aluminum nitride powder with an average particle size of 10 μm or less, 5-90% by weight of boron nitride powder with an average particle size of 20 μm or less, and 1-1% by weight of a sintering aid.
Contains each in the range of 10% by weight, and the total of these is 1
A composite sintered body obtained by sintering a composition with a concentration of
A method for producing a boron nitride/aluminum nitride composite sintered body, which comprises obtaining the boron nitride/aluminum nitride composite sintered body according to claim 1 by heat treatment at a temperature of 2300°C.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| JP3058210A JPH04275982A (en) | 1991-02-28 | 1991-02-28 | Boron nitride-aluminum nitride combined sintered body and its production |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| JP3058210A JPH04275982A (en) | 1991-02-28 | 1991-02-28 | Boron nitride-aluminum nitride combined sintered body and its production |
Publications (1)
| Publication Number | Publication Date |
|---|---|
| JPH04275982A true JPH04275982A (en) | 1992-10-01 |
Family
ID=13077687
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| JP3058210A Pending JPH04275982A (en) | 1991-02-28 | 1991-02-28 | Boron nitride-aluminum nitride combined sintered body and its production |
Country Status (1)
| Country | Link |
|---|---|
| JP (1) | JPH04275982A (en) |
Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| WO2002042241A1 (en) * | 2000-11-22 | 2002-05-30 | Ibiden Co., Ltd. | Aluminum nitride sintered body, method for producing aluminum nitride sintered body, ceramic substrate and method for producing ceramic substrate |
| JP2002220282A (en) * | 2001-01-24 | 2002-08-09 | Tokuyama Corp | Aluminum nitride sintered compact and method of manufacture |
-
1991
- 1991-02-28 JP JP3058210A patent/JPH04275982A/en active Pending
Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| WO2002042241A1 (en) * | 2000-11-22 | 2002-05-30 | Ibiden Co., Ltd. | Aluminum nitride sintered body, method for producing aluminum nitride sintered body, ceramic substrate and method for producing ceramic substrate |
| JP2002220282A (en) * | 2001-01-24 | 2002-08-09 | Tokuyama Corp | Aluminum nitride sintered compact and method of manufacture |
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