JPH03242378A - Production of raw material for sintered body of cubic boron nitride - Google Patents
Production of raw material for sintered body of cubic boron nitrideInfo
- Publication number
- JPH03242378A JPH03242378A JP2037154A JP3715490A JPH03242378A JP H03242378 A JPH03242378 A JP H03242378A JP 2037154 A JP2037154 A JP 2037154A JP 3715490 A JP3715490 A JP 3715490A JP H03242378 A JPH03242378 A JP H03242378A
- Authority
- JP
- Japan
- Prior art keywords
- boron nitride
- powder
- sintered body
- raw material
- alkaline earth
- 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
- PZNSFCLAULLKQX-UHFFFAOYSA-N Boron nitride Chemical compound N#B PZNSFCLAULLKQX-UHFFFAOYSA-N 0.000 title claims abstract description 34
- 229910052582 BN Inorganic materials 0.000 title claims abstract description 31
- 239000002994 raw material Substances 0.000 title claims abstract description 23
- 238000004519 manufacturing process Methods 0.000 title claims description 7
- 239000000843 powder Substances 0.000 claims abstract description 38
- 229910052784 alkaline earth metal Inorganic materials 0.000 claims abstract description 30
- -1 alkaline earth metal boron nitride Chemical class 0.000 claims abstract description 18
- 238000010438 heat treatment Methods 0.000 claims abstract description 11
- 239000011812 mixed powder Substances 0.000 claims abstract description 7
- 239000012298 atmosphere Substances 0.000 claims abstract description 5
- 230000001590 oxidative effect Effects 0.000 claims description 3
- 150000001342 alkaline earth metals Chemical class 0.000 abstract description 12
- 150000004767 nitrides Chemical class 0.000 abstract description 5
- 239000000203 mixture Substances 0.000 abstract description 3
- 239000000463 material Substances 0.000 abstract description 2
- 238000000465 moulding Methods 0.000 abstract 2
- 239000003054 catalyst Substances 0.000 description 20
- 238000000034 method Methods 0.000 description 14
- 238000009792 diffusion process Methods 0.000 description 11
- 238000005470 impregnation Methods 0.000 description 10
- IJGRMHOSHXDMSA-UHFFFAOYSA-N Atomic nitrogen Chemical compound N#N IJGRMHOSHXDMSA-UHFFFAOYSA-N 0.000 description 7
- 229910052749 magnesium Inorganic materials 0.000 description 7
- 239000011777 magnesium Substances 0.000 description 7
- 238000006243 chemical reaction Methods 0.000 description 6
- 238000005245 sintering Methods 0.000 description 6
- 229910052791 calcium Inorganic materials 0.000 description 5
- 239000002245 particle Substances 0.000 description 5
- 238000010532 solid phase synthesis reaction Methods 0.000 description 5
- QVGXLLKOCUKJST-UHFFFAOYSA-N atomic oxygen Chemical compound [O] QVGXLLKOCUKJST-UHFFFAOYSA-N 0.000 description 4
- 229910052751 metal Inorganic materials 0.000 description 4
- 239000002184 metal Substances 0.000 description 4
- 229910052760 oxygen Inorganic materials 0.000 description 4
- 239000001301 oxygen Substances 0.000 description 4
- 229910052788 barium Inorganic materials 0.000 description 3
- 229910052757 nitrogen Inorganic materials 0.000 description 3
- 229910052712 strontium Inorganic materials 0.000 description 3
- FYYHWMGAXLPEAU-UHFFFAOYSA-N Magnesium Chemical compound [Mg] FYYHWMGAXLPEAU-UHFFFAOYSA-N 0.000 description 2
- 238000002441 X-ray diffraction Methods 0.000 description 2
- 238000005520 cutting process Methods 0.000 description 2
- 230000000694 effects Effects 0.000 description 2
- 238000005121 nitriding Methods 0.000 description 2
- 239000012299 nitrogen atmosphere Substances 0.000 description 2
- 239000012808 vapor phase Substances 0.000 description 2
- 241001197925 Theila Species 0.000 description 1
- 238000005229 chemical vapour deposition Methods 0.000 description 1
- 230000000052 comparative effect Effects 0.000 description 1
- 150000001875 compounds Chemical class 0.000 description 1
- 230000007423 decrease Effects 0.000 description 1
- 229910003460 diamond Inorganic materials 0.000 description 1
- 239000010432 diamond Substances 0.000 description 1
- 229910001873 dinitrogen Inorganic materials 0.000 description 1
- 239000007789 gas Substances 0.000 description 1
- 150000002739 metals Chemical class 0.000 description 1
- 230000000737 periodic effect Effects 0.000 description 1
- 229910052705 radium Inorganic materials 0.000 description 1
- 239000004065 semiconductor Substances 0.000 description 1
- 239000007858 starting material Substances 0.000 description 1
- 239000000126 substance Substances 0.000 description 1
- 229910052717 sulfur Inorganic materials 0.000 description 1
- 230000002194 synthesizing effect Effects 0.000 description 1
Landscapes
- Ceramic Products (AREA)
Abstract
Description
【発明の詳細な説明】
〔産業上の利用分野〕
本発明はヒートシンクおよび切削工具に適した立方晶窒
化ほう素（ｃＢＮ）焼結体を合成するための原料の製造
方法、特に出発物質の熱分解窒化ほう素（Ｐ−ＢＮ）成
型体もしくは六方晶窒化ほう素（ｈＢＮ）焼結体に、ｃ
ＢＮ転換触媒であるアルカリ土類金属ほう窒化物を拡散
含浸させた原料を効率よく製造する方法に関するもので
ある。Detailed Description of the Invention [Field of Industrial Application] The present invention relates to a method for producing raw materials for synthesizing cubic boron nitride (cBN) sintered bodies suitable for heat sinks and cutting tools, and in particular to A decomposed boron nitride (P-BN) molded body or hexagonal boron nitride (hBN) sintered body is
The present invention relates to a method for efficiently producing a raw material diffused and impregnated with an alkaline earth metal bonitride, which is a BN conversion catalyst.
ｃＢＮはダイヤモンドに次ぐ硬さおよび熱伝導率を有す
る材料で、特にその高純度焼結体は切削工具および半導
体素子用ヒートシンクとしての応用が期待されている。cBN is a material with hardness and thermal conductivity second only to diamond, and its high-purity sintered bodies are particularly expected to be used as cutting tools and heat sinks for semiconductor devices.
高純度ｃＢＮ焼結体を製造する方法としては、Ｐ−ＢＮ
成型体（特開昭６２−１０８７７２号公報、特開昭６３
〜２６０８６５号公報）あるいはｈＢＮ焼結体（特公昭
６０−２８７１３２号公報）の表面にそれぞれ、ｃＢＮ
転換触媒であるアルカリ土類金属ほう窒化物などを拡散
含浸させ、これらを立方晶窒化ほう素の熱力学的安定条
件下に高温高圧で焼結する方法が知られている。これら
の方法によって、ｃＢＮ粒子が互に直接結合した高純度
焼結体が製造可能であり、特に前者のＰ−ＢＮ成型体を
出発物質とする方法では高熱伝導率の焼結体が得られる
。As a method for producing a high-purity cBN sintered body, P-BN
Molded body (JP-A-62-108772, JP-A-63
~260865) or hBN sintered body (Japanese Patent Publication No. 60-287132).
A method is known in which a conversion catalyst such as an alkaline earth metal bonitride is diffused and impregnated, and these are sintered at high temperature and pressure under thermodynamically stable conditions of cubic boron nitride. By these methods, it is possible to produce a high-purity sintered body in which cBN particles are directly bonded to each other, and in particular, the former method using a P-BN molded body as a starting material yields a sintered body with high thermal conductivity.
アルカリ土類金属ほう窒化物を拡散含浸させる方法とし
ては、
１． Ｐ−ＢＮ成型体あるいはｈＢＮ焼結体に、アル
カリ土類金属窒化物及び／又はほう窒化物の粉末を接触
させて、非酸化性雰囲気中で反応拡散させる方法（固相
法）、
２、 ｈＢＮ焼結体を窒化ほう素るつぼに入れ、アル
カリ土類金属窒化物及び／又はほう窒化物の粉末と非接
触状態とし、窒素ガス中で気相拡散させる方法（気相法
）、
等が知られているが、拡散条件を簡便に制御できる上述
の方法１（固相法）が−船釣である。As a method for diffusion impregnation with alkaline earth metal bonitride, 1. A method of bringing a P-BN molded body or hBN sintered body into contact with alkaline earth metal nitride and/or boron nitride powder and reacting and diffusing it in a non-oxidizing atmosphere (solid phase method), 2. hBN There are known methods such as placing the sintered body in a boron nitride crucible, keeping it in a non-contact state with powder of alkaline earth metal nitride and/or boron nitride, and performing vapor phase diffusion in nitrogen gas (vapor phase method). However, the above-mentioned method 1 (solid phase method) that allows easy control of diffusion conditions is - boat fishing.
しかし、上記の固相法によりアルカリ土類金属ほう窒化
物を拡散含浸させたｃＢＮ焼結体用原料を製造する場合
には、拡散含浸のための熱処理と同時に、Ｐ−ＢＮ成型
体もしくはｈＢＮ焼結体と接触させたアルカリ土類金属
窒化物及び／又はほう窒化物の粉末の焼結も同時に進行
し、Ｐ−ＢＮ成型体もしくはｈＢＮ焼結体の表面に形成
されたアルカリ土類金属ほう窒化物Ｎ（触媒層）と、周
囲のアルカリ土類金属窒化物及び／又はほう窒化物の粉
末とが固着する現象がしばしば発生する。このため、触
媒を拡散含浸させたＰ−ＢＮ成型体もしくはｈＢＮ焼結
体（ｃＢＮ焼結体用原料）を回収する際に、その表面の
触媒層が周囲の焼結したアルカリ土類金属窒化物及び／
又はほう窒化物に付着して、ｃＢＮ焼結体用原料の表面
から脱落することが多く、歩留りを低下させる大きな原
因となっていた。However, when producing a raw material for a cBN sintered body diffused and impregnated with an alkaline earth metal bonitride by the above-mentioned solid-phase method, at the same time as the heat treatment for diffusion impregnation, the P-BN molded body or the hBN sintered body is Sintering of the alkaline earth metal nitride and/or bonitride powder that has been brought into contact with the body also proceeds at the same time, and the alkaline earth metal bonitride formed on the surface of the P-BN molded body or the hBN sintered body is sintered. A phenomenon in which the substance N (catalyst layer) and the surrounding alkaline earth metal nitride and/or boronitride powder stick together often occurs. For this reason, when recovering a P-BN molded body or hBN sintered body (raw material for cBN sintered body) that has been diffused and impregnated with a catalyst, the catalyst layer on the surface of the body is removed from the surrounding sintered alkaline earth metal nitride. as well as/
Otherwise, it often adheres to boronitride and falls off from the surface of the raw material for cBN sintered body, which is a major cause of lowering the yield.
良質のｃＢＮ焼結体を得るためには、Ｐ−ＢＮ成型体も
しくはｈＢＮ焼結体に触媒層が均一に形成されている原
料が望まれるが、そのためには接触させるアルカリ土類
金属窒化物及び／又はほう窒化物の粉末の粒度が細かい
方が好ましい。しかし粒度の細かい粉末は焼結・付着も
起こし易い。このため、触媒層が均一に形成されている
良質のｃＢＮ焼結体用原料の合成と、高い歩留りでの該
原料の製造とを両立させることが困難であった。In order to obtain a high-quality cBN sintered body, it is desirable to use a P-BN molded body or hBN sintered body with a raw material in which a catalyst layer is uniformly formed. It is preferable that the grain size of the boronitride powder is fine. However, fine-grained powder tends to cause sintering and adhesion. For this reason, it has been difficult to simultaneously synthesize a raw material for a high-quality cBN sintered body in which a catalyst layer is uniformly formed and manufacture the raw material at a high yield.
本発明の目的は、従来の固相法におけるこのような問題
を解決し、ｃＢＮ焼結体用原料を高い歩留りで製造する
ことにある。すなわち、本発明の目的は、従来の固相法
で起きていた、拡散含浸のための熱処理時に、焼結した
アルカリ土類金属窒化物及び／又はほう窒化物の粉末が
、Ｐ−ＢＮ成型体もしくはｈＢＮ焼結体の表面に生成し
た触媒層に固着し、原料回収時に触媒層を脱落させると
いう問題を解消し、ｃＢＮ焼結体用原料を工業的に高歩
留りで製造する方法を提供することにある。An object of the present invention is to solve these problems in the conventional solid-phase method and to produce raw materials for cBN sintered bodies at a high yield. That is, an object of the present invention is to prevent sintered alkaline earth metal nitride and/or boron nitride powder from forming a P-BN molded body during heat treatment for diffusion impregnation, which occurs in the conventional solid phase method. Or, to provide a method for industrially producing a raw material for a cBN sintered body at a high yield by solving the problem of adhesion to a catalyst layer formed on the surface of an hBN sintered body and causing the catalyst layer to fall off when recovering the raw material. It is in.
本発明者らは、固相法によりＰ−ＢＮ成型体もしくはｈ
ＢＮ焼結体に、アルカリ土類金属ほう窒化物を拡散含浸
させる際に、Ｐ−ＢＮ成型体もしくはｈＢＮ焼結体に接
触させるアルカリ土類金属窒化物及び／又はほう窒化物
の粉末にｈＢＮ粉末を混合すると、拡散含浸のための熱
処理時にアルカリ土類金属窒化物及び／又はほう窒化物
の粉末の焼結が抑止され、Ｐ−ＢＮ成型体もしくはｈＢ
Ｎ焼結体の表面の触媒層との固着が起きないことを見い
だし、本発明に至ったものである。The present inventors have developed a P-BN molded body or h
When diffusing and impregnating alkaline earth metal bonitride into the BN sintered body, hBN powder is added to the alkaline earth metal nitride and/or boronitride powder that is brought into contact with the P-BN molded body or the hBN sintered body. When mixed, sintering of alkaline earth metal nitride and/or boronitride powder during heat treatment for diffusion impregnation is suppressed, and P-BN molded body or hB
It was discovered that the surface of the N sintered body does not adhere to the catalyst layer, leading to the present invention.
すなわち、本発明は、ｃＢＮ焼結体用原料の製造方法に
関するもので、熱分解窒化ほう素成型体もしくは六方晶
窒化ほう素焼結体に、アルカリ土類金属ほう窒化物を拡
散含浸させた立方晶窒化ほう素焼結体用原料を製造する
にあたり、熱分解窒化ほう素成型体もしくは立方晶窒化
ほう素焼結体を、０．５〜５０重量％の六方晶窒化ほう
素粉末と、９９．５〜５０重量％のアルカリ土類金属窒
化物及び／又はほう窒化物の粉末とからなる混合粉末に
接触させて、非酸化性雰囲気中で加熱することを特徴と
するものである。That is, the present invention relates to a method for producing a raw material for a cBN sintered body, in which a cubic boron nitride molded body or a hexagonal boron nitride sintered body is diffused and impregnated with an alkaline earth metal boron nitride. In producing a raw material for a boron nitride sintered body, a pyrolytic boron nitride molded body or a cubic boron nitride sintered body is mixed with 0.5 to 50% by weight of hexagonal boron nitride powder and 99.5 to 50% by weight of hexagonal boron nitride powder. It is characterized in that it is brought into contact with a mixed powder consisting of powder of an alkaline earth metal nitride and/or boron nitride in an amount of % by weight, and heated in a non-oxidizing atmosphere.
拡散含浸処理に用いる粉末中のｈＢＮ粉末の含有量は、
０．５〜５０重量％が好ましい。０．５％以下ではｈＢ
Ｎ粉末の添加効果が現れず、拡散含浸処理時の粉末の焼
結が抑止されないので、ｃＢＮ焼結体用原料の製造歩留
りが低下する。また５０％を越えると、Ｐ−ＢＮ成型体
もしくはｈＢＮ焼結体に接触するアルカリ土類金属窒化
物及び／又はほう窒化物の濃度が低下するために、Ｐ−
ＢＮ成型体もしくはｈＢＮ焼結体中へのほう窒化物の拡
散速度が遅く、触媒の拡散含浸に長時間を要するので実
用的でない。なお、粉末の粒度ば均一な拡散含浸を達成
するために５００μｍ以下が好ましく、３００μｍ以下
が一層好ましい。The content of hBN powder in the powder used for diffusion impregnation treatment is
0.5 to 50% by weight is preferred. hB below 0.5%
Since the effect of adding N powder is not exhibited and sintering of the powder during the diffusion impregnation treatment is not suppressed, the production yield of the raw material for the cBN sintered body is reduced. Moreover, if it exceeds 50%, the concentration of alkaline earth metal nitrides and/or boronitrides in contact with the P-BN molded body or hBN sintered body decreases.
The rate of diffusion of boronitride into the BN molded body or the hBN sintered body is slow, and it takes a long time to diffuse and impregnate the catalyst, so it is not practical. The particle size of the powder is preferably 500 μm or less, more preferably 300 μm or less in order to achieve uniform diffusion and impregnation.
ここで使用するｈＢＮ粉末は、酸素含有量が１％以下の
高純度粉末であるのが好ましく、また粒度は１００μｍ
以下の粉末がアルカリ土類金属窒化物及び／又はほう窒
化物の粉末の焼結を抑止する上で好ましい。The hBN powder used here is preferably a high purity powder with an oxygen content of 1% or less, and a particle size of 100 μm.
The following powders are preferred in terms of suppressing sintering of alkaline earth metal nitride and/or boronitride powders.
アルカリ土類金属とは周期律表のＩｌａ属、即ちＢｅ、
Ｍｇ、 Ｃａ、 Ｓｒ、 Ｂａ、 Ｒａであるが、こ
のうち本発明方法では取扱の容易なＭｇ、 Ｃａ、 Ｓ
ｒ、 Ｂａの窒化物及び／又はほう窒化物を通常用いる
。窒化物はそれぞれ、Ｍｇ３Ｎｚ 、Ｃａ３Ｎｚ 、５
ｒＪｚ （あるいは５ｒ２Ｎ＋ＳｒＮ ） 、ＢａＪｚ
が一般的であるが、この他にも金属対窒素の化学量論比
が、２：１．１１：８．３：４．１：６などの化合物の
存在が知られており、これらのいずれによっても、本発
明の目的を達成することができる。これらの窒化物は通
常、各金属を窒素と高温で反応させることにより製造す
ることができる。反応速度が適度に速くしかも窒化反応
の熱暴走が起きにくい工業的に好ましい窒化反応温度・
時間条件の例は、Ｍｇ、 Ｃａ、 Ｓｒ、 Ｂａの場合
には、それぞれ７００〜８００°Ｃ１８５０〜９５０°
Ｃ１５００〜６００°Ｃ１４５０〜５５０ ’Ｃの温度
において５〜１０時間の加熱である。なお、Ｍｇおよび
Ｃａの場合には、前記の温度において金属が溶融するの
で、それぞれ６００°Ｃ，７５０°Ｃ前後で４時間程度
の加熱によりあらかじめ金属表面を予備窒化してお（の
が好ましい。ほう窒化物はＭｅ３８Ｎ＋もしくはＭｅ、
Ｂ、Ｎ４（Ｍｅはアルカリ土類金属を示す）で表わされ
、前記の各窒化物と窒化ほう素とを所定量づつ混合して
、窒素中で加熱することにより製造することができる。Alkaline earth metals are members of the Ila genus of the periodic table, namely Be,
Mg, Ca, Sr, Ba, and Ra, among which Mg, Ca, and S are easy to handle in the method of the present invention.
nitrides and/or boronitrides of Ba are commonly used. The nitrides are Mg3Nz, Ca3Nz, and 5, respectively.
rJz (or 5r2N+SrN), BaJz
However, it is known that there are other compounds with a metal to nitrogen stoichiometric ratio of 2:1.11:8.3:4.1:6, and none of these The object of the present invention can also be achieved. These nitrides can usually be produced by reacting each metal with nitrogen at high temperatures. Industrially preferable nitriding reaction temperature where the reaction rate is moderately fast and thermal runaway of the nitriding reaction is less likely to occur.
Examples of time conditions are 700 to 800°C and 1850 to 950° for Mg, Ca, Sr, and Ba, respectively.
Heating at a temperature of 1500-600'C and 1450-550'C for 5-10 hours. In the case of Mg and Ca, since the metals melt at the above-mentioned temperatures, it is preferable to pre-nitridize the metal surfaces by heating at around 600° C. and 750° C. for about 4 hours, respectively. Boronitride is Me38N+ or Me,
B, N4 (Me represents an alkaline earth metal), and can be produced by mixing predetermined amounts of each of the above nitrides and boron nitride and heating the mixture in nitrogen.
その条件は、Ｍｇ、 Ｃａ、 Ｓｒ、 Ｂａの場合には
、それぞれ１１００〜１３００°Ｃ１６５０〜８５０
”Ｃ１５００〜８００°Ｃ１７００〜１０００°Ｃの温
度において１５５時間程である。The conditions are 1100-1300°C 1650-850°C for Mg, Ca, Sr, and Ba, respectively.
155 hours at a temperature of 1500-800°C and 1700-1000°C.
この粉末に接触させるＰ−ＢＮ成型体もしくはｈＢＮ焼
結体は、ｃＢＮ焼結体を得るためには高純度のものであ
ることが必要である。ＣＶＤ法により気体から直接製造
されるＰ−ＢＮ成型体は非常に高純度であるので特に好
ましく、特別の前処理無しに用いることができる。一方
、ｈＢＮ焼結体はｈＢＮ粉末に酸化物助剤を添加して焼
結したものであるが、酸素がｃＢＮへの転換を阻害する
ので、これを用いる場合には、特公昭６０−２８７８２
号公報などに示されているように、予め高温処理により
酸素を除去しておくことが必要である。The P-BN molded body or hBN sintered body that is brought into contact with this powder needs to be of high purity in order to obtain a cBN sintered body. P-BN molded bodies produced directly from gas by the CVD method are particularly preferred because they have very high purity and can be used without special pretreatment. On the other hand, the hBN sintered body is made by adding an oxide aid to hBN powder and sintering it, but since oxygen inhibits the conversion to cBN, when using this, it is necessary to use the
As shown in the above publication, it is necessary to remove oxygen in advance by high-temperature treatment.
Ｐ−ＢＮ成型体もしくはｈＢＮ焼結体にアルカリ土類金
属窒化物及び／又はほう窒化物の粉末を接触させる方法
としては、粉末中にＰ−ＢＮ成型体もしくはｈＢＮ焼結
体を軽く埋め込むのが一般的である。A method of bringing the alkaline earth metal nitride and/or boronitride powder into contact with the P-BN molded body or hBN sintered body is to lightly embed the P-BN molded body or hBN sintered body in the powder. Common.
拡散含浸のための熱処理は通常１１００〜１３００°Ｃ
の温度で行なわれるので、Ｐ−ＢＮ成型体、ｈＢＮ焼結
体、アルカリ土類金属窒化物及び／又はほう窒化物の酸
化を防ぐために、窒素、希ガスなどのような非酸化性雰
囲気中で加熱する必要がある。Heat treatment for diffusion impregnation is usually 1100-1300°C
The process is carried out at a temperature of Needs to be heated.
本発明方法によって製造された原料は、引続き高温超高
圧処理することによりｃＢＮ焼結体に転換されるが、そ
の条件としては１３００″Ｃ以上で４万気圧以上のｃＢ
Ｎの熱力学的安定域が選ばれ、またこのような高温高圧
を発生する装置としては、ベルト型、ガードル型などの
装置が一般的である。The raw material produced by the method of the present invention is subsequently converted into a cBN sintered body by high-temperature and ultra-high pressure treatment.
The thermodynamic stability range of N is selected, and belt-type, girdle-type, and other devices are commonly used to generate such high temperature and pressure.
（実施例〕
次に、本発明を実施例および比較例についてさらに詳細
に説明する。(Examples) Next, the present invention will be described in more detail with reference to Examples and Comparative Examples.
１〜９および １〜３
密度２．１６ｇ／ｃｍ’の熱分解窒化ほう素（電気化学
工業■製、商品名「デンカＰ−ＢＮＪ ）の板から、厚
さ１ｍｍＸ直径７閣の円板を超音波加工機により打ち抜
いた。この円板を各５０枚づつ、表１に示すアルカリ土
類金属窒化物もしくはほう窒化物の粉末とｈＢＮ粉末（
電気化学工業■製、グレードＧＰ、粒度３２５メツシユ
以下）との混合粉末中に埋め、窒素雰囲気中で１２００
″Ｃにおいて２０時間保持して、アルカリ土類金属ほう
窒化物触媒をＰ−ＢＮ円板表面に拡散含浸させ、含浸後
のアルカリ土類金属窒化物もしくはほう窒化物の粉末と
ｈＢＮ粉末との混合粉末の状態、触媒含浸量、触媒層の
脱落なく回収できた含浸済みＰ−ＢＮ円板の割合（良品
率）を調べた。結果を表１に示す。なお、アルカリ土類
金属ほう窒化物がＰ−ＢＮ円板に含浸されたことは、そ
れぞれＸ線回折法により確認した。また触媒含浸量は熱
処理前後のＰ−ＢＮ円板の重量変化から求めた。1 to 9 and 1 to 3 From a plate of pyrolytic boron nitride (manufactured by Denki Kagaku Kogyo ■, trade name ``Denka P-BNJ'') with a density of 2.16 g/cm', a disk with a thickness of 1 mm and a diameter of 7 mm was made. The disks were punched out using a sonic processing machine. Fifty disks each were mixed with alkaline earth metal nitride or boronitride powder and hBN powder (shown in Table 1).
(manufactured by Denki Kagaku Kogyo ■, grade GP, particle size 325 mesh or less) and buried in a mixed powder of
"C" for 20 hours to diffuse and impregnate the alkaline earth metal bonitride catalyst onto the P-BN disk surface, and mix the alkaline earth metal nitride or bonitride powder and hBN powder after impregnation. The state of the powder, the amount of catalyst impregnated, and the percentage of impregnated P-BN disks that could be recovered without falling off of the catalyst layer (good product rate) were investigated.The results are shown in Table 1.It should be noted that alkaline earth metal bonitride It was confirmed by X-ray diffraction that the P-BN disks were impregnated with each catalyst.The amount of catalyst impregnated was determined from the change in weight of the P-BN disks before and after heat treatment.
１０〜１４および ４〜６
密度１．９ｇ／ｃｍ３のｈＢＮ焼結（電気化学工業■製
、グレードＮ−１）を窒素雰囲気中で２１００°Ｃの温
度で２時間処理した。処理後の酸素含存量は０．１重量
％以下であった。この板から、厚さ１ｍｍＸ直径７ｍｍ
の円板を超音波加工機により打ち抜いた。10-14 and 4-6 Sintered hBN (manufactured by Denki Kagaku Kogyo ■, grade N-1) having a density of 1.9 g/cm3 was treated at a temperature of 2100° C. for 2 hours in a nitrogen atmosphere. The oxygen content after treatment was 0.1% by weight or less. From this board, thickness 1mm x diameter 7mm
A disk was punched out using an ultrasonic processing machine.
この円板を各５０枚づつ、表２に示すＭｇ３Ｎｚ粉末と
ｈＢＮ粉末（電気化学工業■製、グレードＧＰ、粒度３
２５メソシユ以下）との混合粉末中に埋め、窒素雰囲気
中で１１６０°Ｃにおいて８時間保持して、マグネシウ
ムほう窒化物（Ｍｇ３ＢＪ）触媒をＰ−ＢＮ円板表面に
拡散含浸させ、含浸後のＭｇＪｚ粉末とｈＢＮ粉末との
混合粉末の状態、触媒含浸量、触媒層の脱落なく回収で
きた含浸済みｈＢＮ焼結体の割合（良品率）を調べた。Fifty disks each were prepared using Mg3Nz powder and hBN powder (manufactured by Denki Kagaku Kogyo ■, grade GP, particle size 3) shown in Table 2.
The P-BN disc surface was diffused and impregnated with a magnesium boronitride (Mg3BJ) catalyst by burying it in a mixed powder with a P-BN disk (less than 25 mesosinus) and holding it at 1160 °C for 8 hours in a nitrogen atmosphere. The state of the mixed powder of powder and hBN powder, the amount of catalyst impregnated, and the percentage of impregnated hBN sintered bodies that were recovered without falling off of the catalyst layer (good product rate) were investigated.
結果を表２に示す。なお、マグネシウムほう窒化物が含
浸されたことは、それぞれＸ線回折法により確認した。The results are shown in Table 2. In addition, impregnation with magnesium bonitride was confirmed by X-ray diffraction.
また触媒含浸量は熱処理前後のｈＢＮ焼結体円板の重量
変化から求めた。Further, the amount of catalyst impregnated was determined from the change in weight of the hBN sintered disk before and after heat treatment.
〔発明の効果］
本発明によれば、高純度かつ高熱伝導率の立方晶窒化ほ
う素焼結体用原料を高い歩留りで製造する事ができる。[Effects of the Invention] According to the present invention, a raw material for a cubic boron nitride sintered body having high purity and high thermal conductivity can be manufactured at a high yield.
Claims (1)
焼結体に、アルカリ土類金属ほう窒化物を拡散含浸させ
た立方晶窒化ほう素焼結体用原料を製造するにあたり、 熱分解窒化ほう素成型体もしくは六方晶窒 化ほう素焼結体を、０．５〜５０重量％の六方晶窒化ほ
う素粉末と９９．５〜５０重量％のアルカリ土類金属窒
化物及び／又はほう窒化物の粉末とからなる混合粉末に
接触させて、非酸化性雰囲気中で加熱することを特徴と
する立方晶窒化ほう素焼結体用原料の製造方法。1. In producing a raw material for a cubic boron nitride sintered body, which is a pyrolytic boron nitride molded body or a hexagonal boron nitride sintered body diffused and impregnated with an alkaline earth metal boron nitride, a pyrolyzed boron nitride molded body is used. Or a hexagonal boron nitride sintered body consisting of 0.5 to 50% by weight of hexagonal boron nitride powder and 99.5 to 50% by weight of alkaline earth metal nitride and/or boron nitride powder. A method for producing a raw material for a cubic boron nitride sintered body, which comprises bringing the raw material into contact with a mixed powder and heating it in a non-oxidizing atmosphere.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| JP2037154A JP2938500B2 (en) | 1990-02-20 | 1990-02-20 | Method for producing raw material for cubic boron nitride sintered body |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| JP2037154A JP2938500B2 (en) | 1990-02-20 | 1990-02-20 | Method for producing raw material for cubic boron nitride sintered body |
Publications (2)
| Publication Number | Publication Date |
|---|---|
| JPH03242378A true JPH03242378A (en) | 1991-10-29 |
| JP2938500B2 JP2938500B2 (en) | 1999-08-23 |
Family
ID=12489686
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| JP2037154A Expired - Fee Related JP2938500B2 (en) | 1990-02-20 | 1990-02-20 | Method for producing raw material for cubic boron nitride sintered body |
Country Status (1)
| Country | Link |
|---|---|
| JP (1) | JP2938500B2 (en) |
-
1990
- 1990-02-20 JP JP2037154A patent/JP2938500B2/en not_active Expired - Fee Related
Also Published As
| Publication number | Publication date |
|---|---|
| JP2938500B2 (en) | 1999-08-23 |
Similar Documents
| Publication | Publication Date | Title |
|---|---|---|
| US5942455A (en) | Synthesis of 312 phases and composites thereof | |
| JP2907315B2 (en) | Production of polycrystalline cubic boron nitride | |
| KR0134958B1 (en) | Method for preparing a self support having controlled pores and graded properties | |
| WO1997018162A9 (en) | Synthesis of 312 phases and composites thereof | |
| JPH11246271A (en) | Cubic boron nitride sintered body and its production | |
| JPH0472792B2 (en) | ||
| JPS6256104B2 (en) | ||
| JPS62274034A (en) | Manufacture of polycrystalline diamond sintered compact by reaction sintering | |
| JPH03242378A (en) | Production of raw material for sintered body of cubic boron nitride | |
| JP2799426B2 (en) | Method for producing boron nitride composite | |
| JPH0510282B2 (en) | ||
| JPH04500497A (en) | Improving thermal conductivity of aluminum nitride through pre-densification treatment | |
| JPH0345561A (en) | Sintered material of cubic boron nitride and production thereof | |
| JPH08509691A (en) | Silicon carbide object and manufacturing method thereof | |
| JPH0438685B2 (en) | ||
| JP2721525B2 (en) | Cubic boron nitride sintered body and method for producing the same | |
| JP2628668B2 (en) | Cubic boron nitride sintered body | |
| JPS59217608A (en) | Method for synthesizing cubic boron nitride | |
| JPS5891060A (en) | Manufacture of silicon carbide sintered body | |
| JPH07121835B2 (en) | Cubic boron nitride coating | |
| JPH0455144B2 (en) | ||
| JP2774386B2 (en) | Method for producing cubic boron nitride sintered body | |
| JPS5915112B2 (en) | Method for manufacturing high-density silicon carbide sintered body | |
| JP3452741B2 (en) | Method for producing aluminum nitride based composite material | |
| JPH024550B2 (en) |
Legal Events
| Date | Code | Title | Description |
|---|---|---|---|
| R250 | Receipt of annual fees |
Free format text: JAPANESE INTERMEDIATE CODE: R250 |
|
| R250 | Receipt of annual fees |
Free format text: JAPANESE INTERMEDIATE CODE: R250 |
|
| R250 | Receipt of annual fees |
Free format text: JAPANESE INTERMEDIATE CODE: R250 |
|
| FPAY | Renewal fee payment (event date is renewal date of database) |
Free format text: PAYMENT UNTIL: 20080611 Year of fee payment: 9 |
|
| FPAY | Renewal fee payment (event date is renewal date of database) |
Free format text: PAYMENT UNTIL: 20090611 Year of fee payment: 10 |
|
| LAPS | Cancellation because of no payment of annual fees |