JPS61117107A - Amorphous boron niride powder and its preparation - Google Patents
Amorphous boron niride powder and its preparationInfo
- Publication number
- JPS61117107A JPS61117107A JP59238550A JP23855084A JPS61117107A JP S61117107 A JPS61117107 A JP S61117107A JP 59238550 A JP59238550 A JP 59238550A JP 23855084 A JP23855084 A JP 23855084A JP S61117107 A JPS61117107 A JP S61117107A
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- powder
- boron nitride
- spherical
- nitride powder
- amorphous boron
- Prior art date
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Abstract
Description
【発明の詳細な説明】
［発明の技術分野］
本発明は、粒子がＷ１＃１球状である非晶質窒化ホウ素
（以下、ａ−ＢＮという）粉末とその製造方法に関し、
更に詳しくは、この粉末を用いて焼結体を製造したとき
、その焼結体が空孔の少ない緻密構造体になり１組織も
均一になる球状ａ−ＢＮとその製造方法に関する。Detailed Description of the Invention [Technical Field of the Invention] The present invention relates to amorphous boron nitride (hereinafter referred to as a-BN) powder whose particles are W1#1 spherical and a method for producing the same.
More specifically, the present invention relates to spherical a-BN in which when a sintered body is manufactured using this powder, the sintered body becomes a dense structure with few pores and has a uniform structure, and a method for manufacturing the same.
［発明の技術的背景とその問題点］
窒化ホウ素の焼結体は、ファインセラミックスの１つと
して最近とみに注目を集めている。これらの焼結体とし
ては、立方晶窒化ホウ素（以下、ｃ−ＢＮという）焼結
体、ウルツ型窒化ホウ素（以下、ｗ−ＢＮという）の各
焼結体があり、他に大方晶窒化ホウ素（以下、ｈ−ＢＮ
という）焼結体が知られている。これらのうちとくに、
Ｃ−ＢＨの焼結体は高硬度、耐摩耗性に優れた素材とし
て脚光を浴び工具用材料の用途分野への展望が開けてい
る。また、これは一方では極めて高い熱伝導性と電気抵
抗を兼ね備えているため、高密度集積回路におけるヒー
トシンク材料として大きな期待がもたれている。[Technical background of the invention and its problems] Sintered bodies of boron nitride have recently attracted a lot of attention as a type of fine ceramics. These sintered bodies include cubic boron nitride (hereinafter referred to as c-BN) sintered bodies, wurtzian boron nitride (hereinafter referred to as w-BN) sintered bodies, and large cubic boron nitride (hereinafter referred to as w-BN) sintered bodies. (Hereinafter, h-BN
) sintered bodies are known. Among these, especially
C-BH sintered bodies are attracting attention as a material with high hardness and excellent wear resistance, and are opening up prospects for application as materials for tools. Furthermore, since it has both extremely high thermal conductivity and electrical resistance, it holds great promise as a heat sink material for high-density integrated circuits.
このｃ−ＢＮ焼結体は大別して次の２つの方法で製造さ
れている。その第１の方法は、Ｃ−ＢＮの粉末を耐圧、
耐熱性の型内に充填して超高圧・高温下（例えば、 ５
ＧＰａ以上、Ｉ２００℃以上）で焼結したり、又は、ｃ
−ＢＮの粉末と Ｔｉ。This c-BN sintered body is manufactured by the following two methods. The first method is to apply C-BN powder to a pressure-resistant
It is filled into a heat-resistant mold and placed under ultra-high pressure and high temperature (for example, 5
GPa or higher, I200℃ or higher), or c
- BN powder and Ti.
Ｓｉ、 Ａｎ、 ＡＩＮなどの触媒若しくはこの触
媒とＴｉＮ、 Ａｎ ２０３を主体とする結合材とを混
合し、この混合粉末を同じく耐圧、耐熱性の型内に充填
して超高圧・高温下で焼結したりする。いわゆるＣ−Ｂ
Ｎ粉末を原料とする方法である。第２の方法は、ｃ−Ｂ
Ｎ以外の窒化ホウ素の粉末、すなわち前述したｈ−ＢＮ
又はａ７ＢＮの粉末を出発原料とし、これを上記したよ
うな結合材と混合したのち、超高圧・高温下で処理して
、窒化ホウ素なｃ−ＢＮに転換すると同時に全体を焼結
するという方法である。A catalyst such as Si, An, AIN, or this catalyst is mixed with a binder mainly composed of TiN or An 203, and this mixed powder is filled into a pressure-resistant and heat-resistant mold and sintered under ultra-high pressure and high temperature. or tie a knot. So-called C-B
This method uses N powder as a raw material. The second method is c-B
Boron nitride powder other than N, i.e. the above-mentioned h-BN
Alternatively, a7BN powder is used as a starting material, mixed with the above-mentioned binder, and then treated under ultra-high pressure and high temperature to convert it into c-BN, which is boron nitride, and simultaneously sinter the entire product. be.
これら２つの方法のうち、後者の方法の場合には、窒化
ホウ素からｃ−ＢＮへの転換率が１００％ではなく、未
転換の窒化ホウ素が残留し、得られた焼結体の特性を著
しく低下せしめるという問題が避けられない。Of these two methods, in the latter method, the conversion rate from boron nitride to c-BN is not 100%, and unconverted boron nitride remains, significantly affecting the properties of the obtained sintered body. The problem of deterioration is unavoidable.
そのため、実際には前者の方法で主としてＣ−ＢＮ焼結
体は製造されている。Therefore, in reality, C-BN sintered bodies are mainly produced by the former method.
この前者の方法にあっては、出発原料はＣ−ＢＮである
。したがって、前提問題としてＣ−ＢＮの合成が重要な
ファクターとなる。In the former method, the starting material is C-BN. Therefore, the synthesis of C-BN becomes an important factor as a prerequisite problem.
現在のところ、ｃ−ＢＮの合成に関しては、主に、ｈ−
ＢＮを超高圧Φ高温下で処理してＣ−ＢＮに転換すると
いう方法が採られている。At present, regarding the synthesis of c-BN, mainly h-
A method has been adopted in which BN is converted to C-BN by treating it at ultra-high pressure Φ and high temperature.
しかしながら、その転換率は一般に低い、それは、ｈ−
ＢＮに物理的φ化学的に吸着している酸素又は化学的に
結合している酸素成分の影響に起因するためであること
が明らかとなっている。However, the conversion rate is generally low, as h-
It has been revealed that this is due to the influence of oxygen chemically adsorbed to BN or chemically bonded oxygen components.
ｈ−ＢＮからｃ−ＢＮの転換率を高めるために１種々の
研究が重ねられているが１本発明者らは、ｈ−ＢＮから
ｃ−ＢＮを合成する際に合成触媒としての窒化アルミニ
ウムを介在せしめるとその転換率が向上するとの事実を
見出しこれを既に発表した（粉体粉末冶金協会、昭和５
７年度秋季大会講演概要集、 １００〜１０１頁参照）
。Although various studies have been conducted to increase the conversion rate of c-BN from h-BN, the present inventors have investigated the use of aluminum nitride as a synthesis catalyst when synthesizing c-BN from h-BN. We have already announced the fact that the conversion rate improves when it is interposed (Powder Metallurgy Association, 1930).
(See 7th Autumn Conference Lecture Summary Collection, pages 100-101)
.
更に研究を進め、ｈ−ＢＮの結晶性と転換率との関係に
つき研究を重ねた結果、ｈ−ＢＮの結晶化度が小さいも
のほどｃ−ＢＮへの転換率が高くなることを確認し、そ
れを既に発表した（粉体粉末冶金協会、昭和５８年度春
季大会講演概要集、８６頁〜８７頁参照）。As a result of further research on the relationship between h-BN crystallinity and conversion rate, we confirmed that the lower the crystallinity of h-BN, the higher the conversion rate to c-BN. This has already been announced (see Powder and Powder Metallurgy Association, 1985 Spring Conference Lecture Abstracts, pages 86-87).
このようなことから、ｃ−ＢＮの合成に関しては、結晶
化度の小さいｈ−ＢＮを出発原料として用いてもよいが
、そのこと以上に、出発原料がａ−ＢＮである場合には
、更に高い転換率でＣ−ＢＮを合成できることが明らか
となった。For this reason, in the synthesis of c-BN, h-BN with a low degree of crystallinity may be used as a starting material, but moreover, when the starting material is a-BN, It has become clear that C-BN can be synthesized at a high conversion rate.
以上の知見の上に立って１本発明者らはａ−ＢＮの原料
になり得る化合物を追究したところ。Based on the above knowledge, the present inventors have investigated compounds that can be used as raw materials for a-BN.
ボラジン又はボラジン誘導体を加圧子熱分解するとｃ−
ＢＮへの転換率の高いａ−ＢＮを得ることができるとの
事実を見出し、その方法を既に特願昭５１−１００８８
２号として出願した。When borazine or borazine derivatives are pyrolyzed with an indenter, c-
It was discovered that it was possible to obtain a-BN with a high conversion rate to BN, and the method was already published in patent application No. 51-10088.
I applied as No. 2.
ところで、ａ−ＢＮをｃ−ＢＮに転換し、得られたｃ−
ＢＮを用いてその焼結体を製造する際には、このｃ−Ｆ
ＩＮ粉末を所定の型内に充填して焼結する。このとき、
得られる焼結体が空孔のない緻密質のものになるか否か
又は偏析がなく均一な組織構造になるか否かという問題
には、適用する焼結条件と合わせてｃ−ＢＮ粉末の特性
又は形状も重要な因子として作用する。By the way, the c-BN obtained by converting a-BN to c-BN
When manufacturing the sintered body using BN, this c-F
IN powder is filled into a predetermined mold and sintered. At this time,
The question of whether or not the obtained sintered body will be dense without pores, or whether it will have a uniform structure without segregation, depends on the c-BN powder, together with the sintering conditions to be applied. Characteristics or shape also act as an important factor.
また、ａ−ＢＮ粉末を直接型の中に充填し、高圧ｅ高温
下において、ａ−ＢＮをｃ−ＢＮに転換しながら焼結す
る場合にも、上記したと同様の理由によって、用いるａ
−ＢＮ粉末は個々の粒子が微細な球状体であることが好
ましい。Also, when a-BN powder is directly filled into a mold and sintered under high pressure and high temperature while converting a-BN to c-BN, the a-BN powder used is
- It is preferable that each particle of the BN powder is a fine spherical body.
一方、ｈ−ＢＮ焼結体は軟質ではあるが、しかし軟質で
あるがゆえに機械加工性、潤滑性が優れ、そしてまた化
学安定性、高熱伝導性、高電気絶縁性という特性を備え
ている。従来、ｈ−ＢＮ焼結体は、ｈ−ＢＮ粉末を出発
原料とし潤滑剤及び焼結助剤と共に焼結して製造されて
いるが、このような焼結体は高密度ではなく、せいぜい
理論密度の８０〜８５％程度のものでしかない。On the other hand, the h-BN sintered body is soft, but because it is soft, it has excellent machinability and lubricity, and also has properties such as chemical stability, high thermal conductivity, and high electrical insulation. Conventionally, h-BN sintered bodies have been manufactured by using h-BN powder as a starting material and sintering it together with lubricants and sintering aids, but such sintered bodies do not have high density and are at most theoretically sintered. It is only about 80-85% of the density.
ｈ−ＢＮ焼結体の製造時にあっ°ても、上記したｃ−Ｂ
Ｎ焼結体の製造の場合と同様に、その原料粉末は微細で
かつ球状であることが好ましい。Even if the h-BN sintered body is manufactured, the above-mentioned c-B
As in the case of manufacturing the N sintered body, the raw material powder is preferably fine and spherical.
しかしながら、現在までのところそのような機側球状の
ａ−ＢＮ粉末は開示されていないし、また、その製造方
法も知られていない。However, to date, such machine-side spherical a-BN powder has not been disclosed, nor is a method for producing the same known.
［発明の目的］
本発明は、木発明者らが開発した前記特願昭５９−１０
０８８２号の方法を基礎にして製造される窒化ホウ素の
粒子が微細で球状のａ−ＢＮ粉末とその製造方法の提供
を目的とする。[Object of the Invention] The present invention is based on the aforementioned patent application developed by the inventors of Wood
The present invention aims to provide a-BN powder having fine and spherical boron nitride particles produced based on the method of No. 0882, and a method for producing the same.
［発明の概要コ
本発明のａ−ＢＮ粉末は粉末粒子の形状が球状であるこ
とを特徴とし、例えばその球状のａ −ＢＮは、ボラジ
ン又はボラジン誘導体の群から選ばれる少なくとも１種
の化合物を、圧力ｌＯ〜１００ＭＰａ、温度２００−３
５０℃２時間５〜３０分の条件で加圧子熱分解すること
によって得ることができる。[Summary of the Invention] The a-BN powder of the present invention is characterized in that the shape of the powder particles is spherical. For example, the spherical a-BN contains at least one compound selected from the group of borazine or borazine derivatives. , pressure lO~100MPa, temperature 200-3
It can be obtained by thermally decomposing an indenter at 50° C. for 2 hours and 5 to 30 minutes.
本発明のａ−ＢＮ粉末は粒子形状が球状である。その粒
径は、通常ｌ〜４ｐｍと微細である。The a-BN powder of the present invention has a spherical particle shape. The particle size is usually as fine as 1 to 4 pm.
したがって、流動性に富むため焼結体の製造時には型内
への充填性が優れ、他の添加物との混合性も良好なので
作業性も良好である。また焼結時にあっては、微細で水
素を含有しているのでそれ自体が焼結の促進効果を備え
ていて１ｗｋ密で均一な組織の焼結体となり得る。Therefore, since it has high fluidity, it has excellent filling properties into a mold during production of a sintered body, and also has good mixability with other additives, resulting in good workability. Further, during sintering, since it is fine and contains hydrogen, it itself has the effect of promoting sintering, and can become a sintered body with a 1wk dense and uniform structure.
このａ−ＢＮ粉末は次のようにして製造することができ
る。This a-BN powder can be manufactured as follows.
まず、原料は１次式：
で示されるボラジン若しくは後述のボラジン誘導体の１
種又はこれらを２種以上適宜に混合して成る混合物であ
る。これらのうち、
ボラジン誘導体としては、例えば１次式：で示されるボ
ラシナフタリン、次式：
で示されるボラノビ２エニル５次式：
で示される２、４−ジアミノボラ０ジンをあげることが
できる。好ましい原料はボラジンである。First, the raw material is borazine represented by the linear formula: or one of the borazine derivatives described below.
It is a species or a mixture formed by appropriately mixing two or more of these. Among these, examples of the borazine derivatives include boracinaphthalene represented by the linear formula: and boranobi-2enyl represented by the following formula: 2,4-diaminoborozine represented by the quintic formula: A preferred raw material is borazine.
これらの原料は、酸素、炭素を含有していないことが重
要である。なぜならば酸素は前述したようにｃ−ＢＮへ
の転換率を低下せしめる因子として作用するからであり
、また、炭素は後述の条件下で熱分解処理を施したとき
にａ−ＢＨ内に残留するからである。このような炭素を
含有するａ−ＢＮを原料として高圧・高温下でｃ−ＢＮ
を合成した場合、この炭素が黒鉛に転換してｃ−ＢＨ内
に残留し、モしてｃ−ＢＮ焼結体の特性低下をもたらす
からである。It is important that these raw materials do not contain oxygen or carbon. This is because, as mentioned above, oxygen acts as a factor that reduces the conversion rate to c-BN, and carbon remains in a-BH when thermal decomposition is performed under the conditions described below. It is from. Using a-BN containing such carbon as a raw material, c-BN is produced under high pressure and high temperature.
This is because when synthesized, this carbon converts to graphite and remains in c-BH, resulting in deterioration of the properties of the c-BN sintered body.
本発明方法にあっては、上記した原料を密閉式の圧力容
器の中にいれ、加圧子熱分解を施す、このときの加圧子
熱分解反応は、まずその初期段階において原料のボテジ
ン環の開ａｍ合厘応が気相と液相の共存下で進行しつつ
水素含有量の多い球状のａ−ＢＮを生成する。その後１
時間の経過とともに更に水素が放出されていき、水゛素
含有量の少ない球状のａ−ＢＨに転化していく。In the method of the present invention, the above-mentioned raw material is placed in a closed pressure vessel and subjected to indenter thermal decomposition. In the initial stage of the indenter thermal decomposition reaction, the botegin ring of the raw material is opened. The am synthesis reaction proceeds in the coexistence of a gas phase and a liquid phase, producing spherical a-BN with a high hydrogen content. then 1
As time passes, more hydrogen is released, and it is converted into spherical a-BH with a low hydrogen content.
このように本発明の加圧子熱分解反応は、熱分解時の圧
力、温度１時間が基本的な制御因子であり、これら因子
によって、得られるａ−ＢＮ粉末の状態が左右される。As described above, in the presser pyrolysis reaction of the present invention, the pressure and temperature 1 hour during pyrolysis are the basic control factors, and these factors influence the state of the a-BN powder obtained.
まず、圧力は１０〜ｌｏＯＭＰａの範囲に設定される。First, the pressure is set in the range of 10 to loOMPa.
この圧力が１ 、’ＯＭ Ｐ ａより低い場合には、原
料が熱分解処理中に放出する水素を押え込む圧力として
は不充分であり、ａ−ＢＮの収率は低くなる。また、圧
力が１００＞ＩＰａより高い場合には、得られたａ−Ｂ
Ｎが相互に融合してしまい球状粒子にはならず、この合
体球が帯状に広がった塊状の白色固体となってしまう、
圧力の好ましい範囲は２５〜１００ＭＰａテある。If this pressure is lower than 1,'OM Pa, the pressure is insufficient to suppress the hydrogen released by the raw material during the thermal decomposition treatment, and the yield of a-BN will be low. Moreover, when the pressure is higher than 100>IPa, the obtained a-B
N fuses with each other and does not form spherical particles, but the fused spheres become a lumpy white solid that spreads out in a band-like shape.
The preferred range of pressure is 25 to 100 MPa.
温度は２００〜３５０℃の範囲に設定される。一般に、
熱分解温度が高くなるにつれて得られたａ−ＢＮの水素
含有量は減少していくが、この残存水素の多少がａ−Ｂ
Ｎからｃ−ＢＮへの転換率の大小に１ｌｌ＝Ｊｉな影響
を及ぼすことからして、Ｃ−ＢＮへの転換率を高位に維
持するためには熱分解温度を ３５０℃以下にする。し
かし、熱分解温度が ２００℃よりも低くなると、得ら
れたａ−ＢＮの活性が高くなりすぎて、全体の取扱いを
Ｎ２又は不活性ガス雰囲気中で行なうことが必要になる
ので２００℃未満とする。好ましくは、２５０〜３５０
℃である。The temperature is set in the range of 200-350°C. in general,
As the thermal decomposition temperature increases, the hydrogen content of the obtained a-BN decreases, but some of this residual hydrogen
Considering that 1 liter = Ji influences the magnitude of the conversion rate from N to c-BN, the thermal decomposition temperature is set to 350° C. or lower in order to maintain the conversion rate to C-BN at a high level. However, if the thermal decomposition temperature is lower than 200°C, the activity of the obtained a-BN will be too high, making it necessary to carry out the entire handling in an N2 or inert gas atmosphere. do. Preferably 250-350
It is ℃.
時間は５〜３０分の範囲に設定される。上記した２因子
の設定範囲内にあっては、加圧子熱分解の時間が３０分
を超えると、ａ−ＢＮにおける水素含有量が非常に減少
してしまい、ｃ−ＢＮへの転換率も低下する。逆に時間
が５分より短い場合には、残存する水素量が多すぎてａ
−ＢＮの活性は高くなりすぎ、加水分解を起しやすくな
るというような不都合な問題を生ずる。The time is set in the range of 5 to 30 minutes. Within the setting range of the above two factors, if the indenter pyrolysis time exceeds 30 minutes, the hydrogen content in a-BN will decrease significantly and the conversion rate to c-BN will also decrease. do. On the other hand, if the time is shorter than 5 minutes, the amount of remaining hydrogen is too large.
-The activity of BN becomes too high, leading to disadvantageous problems such as easy hydrolysis.
このようにして、粒ａ！１〜４）ｉｎで球状のａ −Ｂ
Ｎ粉末が得られる。この粉末を例えば真空中又は非酸化
性雰囲気中、高温下で処理すれば、高純度のｈ−ＢＮ粉
末を得ることができ、また、ホットプレスすればｈ−Ｂ
Ｎ焼結体が得られる。更に例えば５．０〜Ｂ、５ＧＰａ
の超高圧、 １１００〜１８５０℃の高温下で処理すれ
ばｃ−ＢＮ焼結体を得ることができる。In this way, grain a! 1-4) Spherical a-B in
N powder is obtained. High purity h-BN powder can be obtained by processing this powder at high temperatures in a vacuum or non-oxidizing atmosphere, and h-BN powder can be obtained by hot pressing.
A N sintered body is obtained. Furthermore, for example, 5.0~B, 5GPa
A c-BN sintered body can be obtained by processing at an ultra-high pressure of 1,100 to 1,850°C.
［発明の実施例］
実施例１
（＋）ａ−ＢＮの調製
β−トリクロロボラジンを還元してボラジンを製造した
。このボテジン（液体）を金カプセルの中に封入し、カ
プセルをコーン密閉式圧力容器内にセットした。[Examples of the Invention] Example 1 Preparation of (+)a-BN Borazine was produced by reducing β-trichloroborazine. This botedine (liquid) was sealed in a gold capsule, and the capsule was set in a cone-tight pressure vessel.
容器内圧力、温度、処理時間を表に示したように変化さ
せて加圧下熱分解処理を施した。いずれの場合も白色固
体が得られた。これらや固体につさ粉末Ｘ線回折法によ
り結晶構造を観察したところ、いずれも非晶質であるこ
とが確認された。Pyrolysis treatment under pressure was performed while changing the pressure, temperature, and treatment time in the container as shown in the table. A white solid was obtained in each case. When the crystal structures of these and solids were observed by powder X-ray diffraction, it was confirmed that they were all amorphous.
また、これら白色固体につき赤外吸収（！Ｒ）スペクト
ル分析を行なったところ、 ３４００ｃｍ−’の位置に
Ｎ−Ｈ伸縮による吸収、２５２０ ｃ ｍ−’の位置に
Ｂ−Ｈ伸縮による吸収、１４００ｃ■４の位置にＢ−Ｎ
伸縮による吸収が認められた。In addition, when infrared absorption (!R) spectrum analysis was performed on these white solids, absorption due to N-H stretching at the position of 3400 cm-', absorption due to B-H stretching at the position of 2520 cm-', and absorption due to B-H stretching at 1400 cm-'. B-N in position 4
Absorption due to expansion and contraction was observed.
各場合につき、Ｂ−Ｈ及びＢ−Ｎの各伸縮振動に基づく
吸収強度の比を算出し、その値を表に併記した。また、
各白色固体を顕微鏡観察し、その形状等も併記した。更
に、得られた各ａ−ＢＮの粉末に窒化アルミニウム２０
モル％添加して混合し、コノ混合粉末を、圧力８．５Ｇ
Ｐａ、温度１２００℃の条件下で１０分間処理して焼結
した。For each case, the ratio of absorption intensities based on each stretching vibration of BH and BN was calculated, and the values are also listed in the table. Also,
Each white solid was observed under a microscope, and its shape etc. were also recorded. Furthermore, 20% of aluminum nitride was added to each of the obtained a-BN powders.
Add mol% and mix, and mix the Kono mixed powder at a pressure of 8.5G.
It was sintered by processing for 10 minutes under conditions of Pa and temperature of 1200°C.
得られた各焼結体につき、Ｘ線回折法でそのＣ−ＢＨの
存在割合を測定し、各ａ−ＢＮの転換率を算出した。そ
の結果も表に併記した。For each of the obtained sintered bodies, the abundance ratio of C-BH was measured by an X-ray diffraction method, and the conversion rate of each a-BN was calculated. The results are also listed in the table.
実施例２ 粒径的ｌ終ｍの本発明ａ−ＢＮ粉末ａｏｌ量％。Example 2 Amount % of a-BN powder aol of the present invention with particle size end m.
５ｉ０２粉末５重量％、Ａ文粉末５１ｆＵ量％を混合し
、得られた混合粉末を真空雰囲気中において、１８００
℃、４０分、 １０ＭＰａの条件下でホットプレスした
。5i02 powder (5% by weight) and A-text powder (51fU) were mixed, and the resulting mixed powder was heated to 1800% by weight in a vacuum atmosphere.
Hot pressing was carried out at 10 MPa for 40 minutes at ℃.
得られた焼結体はｈ−ＢＮ焼結体であり、その密度は理
論密度の８５％であった。The obtained sintered body was an h-BN sintered body, and its density was 85% of the theoretical density.
比較のために、粒径的１ｇｍの市販ｈ−ＢＮ粉末３０重
量％、 ５ｉ０２粉末５重量％、Ａ交粉末５重量％の混
合粉末につき、同様の条件下でホットプレスして焼結体
を得た。このｈ−ＢＮ焼結体の密度は理論密度の８０％
であった。For comparison, a mixed powder of 30% by weight of commercially available h-BN powder, 5% by weight of 5i02 powder, and 5% by weight of A-cross powder with a grain size of 1 gm was hot pressed under the same conditions to obtain a sintered body. Ta. The density of this h-BN sintered body is 80% of the theoretical density.
Met.
［発明の効果〕
以丘の説明で明らかなように１本発明の球状ａ−ＢＮ粉
末は微細で水素を含有し、しかもＣ−ＢＮへの転換率が
高いことがらｃ−ＢＮ焼結体の原料として使用すると緻
密で均一組織のｃ−ＢＮ焼結体になり、高硬度、高熱伝
導性、高電気絶縁性が一層優れ、切削用工具、耐摩耗用
工具、ヒートシンクをはじめとする電気部品として応用
でき、また、ｃ−ＢＮ粉末にするとそれは砥石又は砥粒
として研削工具又は研摩材料として応用できる。[Effects of the Invention] As is clear from the above explanation, the spherical a-BN powder of the present invention is fine and contains hydrogen, and has a high conversion rate to C-BN, which makes it suitable for c-BN sintered bodies. When used as a raw material, it becomes a c-BN sintered body with a dense and uniform structure, which has excellent hardness, high thermal conductivity, and high electrical insulation properties, making it suitable for use as cutting tools, wear-resistant tools, heat sinks, and other electrical components. Also, when made into c-BN powder, it can be applied as a grinding wheel or abrasive grain as a grinding tool or abrasive material.
更に１本発明の球状のａ−ＢＮ粉末は微細で活性がある
ためにｈ−ＢＮ焼結体の原料として使用すると、緻密で
均一組織のｈ−ＢＮ焼結体になり、化学安定性、耐食性
９機械加工性、高熱伝導性、高電気絶縁性が一層優れ、
機械加工性もよいので溶融金属若しくは薬品用の容器、
高温域での潤滑材料、７４気部品材料として応用できる
産業上有用な材料である。Furthermore, since the spherical a-BN powder of the present invention is fine and active, when used as a raw material for h-BN sintered bodies, it becomes h-BN sintered bodies with a dense and uniform structure, and has good chemical stability and corrosion resistance. 9 Excellent machinability, high thermal conductivity, and high electrical insulation properties.
It has good machinability, so it can be used for containers for molten metal or chemicals,
It is an industrially useful material that can be applied as a lubricating material in high temperature ranges and as a material for 74 gas parts.
Claims (1)
とする非晶質窒化ホウ素粉末。 ２、前記窒化ホウ素が水素を含有している特許請求の範
囲第１項記載の非晶質窒化ホウ素粉末。 ３、ボランジン又はボラジン誘導体の群から選ばれる少
なくとも１種の化合物を、圧力１０〜１００ＭＰａ、温
度２００〜３５０℃、時間５〜３０分の条件で加圧下熱
分解することを特徴とする非晶質窒化ホウ素粉末の製造
方法。[Claims] 1. An amorphous boron nitride powder characterized in that the boron nitride powder particles have a spherical shape. 2. The amorphous boron nitride powder according to claim 1, wherein the boron nitride contains hydrogen. 3. An amorphous material characterized by thermally decomposing at least one compound selected from the group of borandine or borazine derivatives under pressure at a pressure of 10 to 100 MPa, a temperature of 200 to 350°C, and a time of 5 to 30 minutes. Method for producing boron nitride powder.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| JP59238550A JPS61117107A (en) | 1984-11-14 | 1984-11-14 | Amorphous boron niride powder and its preparation |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| JP59238550A JPS61117107A (en) | 1984-11-14 | 1984-11-14 | Amorphous boron niride powder and its preparation |
Publications (2)
| Publication Number | Publication Date |
|---|---|
| JPS61117107A true JPS61117107A (en) | 1986-06-04 |
| JPH0510282B2 JPH0510282B2 (en) | 1993-02-09 |
Family
ID=17031907
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| JP59238550A Granted JPS61117107A (en) | 1984-11-14 | 1984-11-14 | Amorphous boron niride powder and its preparation |
Country Status (1)
| Country | Link |
|---|---|
| JP (1) | JPS61117107A (en) |
Cited By (8)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| WO1988000934A1 (en) * | 1986-08-07 | 1988-02-11 | Kabushiki Kaisha Kouransha | Boron nitride sinter and process for its production |
| JPS6345178A (en) * | 1986-08-07 | 1988-02-26 | 株式会社 香蘭社 | Boron nitride sintering raw material powder |
| EP0314807A1 (en) * | 1987-05-12 | 1989-05-10 | Kabushiki Kaisha Kouransha | Molten metal container |
| JPH02296706A (en) * | 1989-05-02 | 1990-12-07 | Rhone Poulenc Chim | Amorphous or irregular- laminate and spherical in particular boron nitride and its production method |
| US5230873A (en) * | 1988-09-10 | 1993-07-27 | Firna Siegfried Golz | Process for producing amorphous boron nitride of high hardness |
| WO1999061391A1 (en) * | 1998-05-22 | 1999-12-02 | Sumitomo Electric Industries, Ltd. | Cubic system boron nitride sintered body cutting tool |
| WO2011021366A1 (en) * | 2009-08-20 | 2011-02-24 | 株式会社カネカ | Process for production of spheroidized boron nitride |
| CN107161960A (en) * | 2017-06-06 | 2017-09-15 | 哈尔滨工业大学深圳研究生院 | A kind of high pressure vapor prepares the method and apparatus of boron nitride spherical powder |
Citations (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| JPS58181707A (en) * | 1982-04-15 | 1983-10-24 | Natl Inst For Res In Inorg Mater | Manufacture of boron nitride |
| JPS60155508A (en) * | 1984-08-02 | 1985-08-15 | Res Dev Corp Of Japan | Noncrystalline boron nitride having improved stability |
-
1984
- 1984-11-14 JP JP59238550A patent/JPS61117107A/en active Granted
Patent Citations (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| JPS58181707A (en) * | 1982-04-15 | 1983-10-24 | Natl Inst For Res In Inorg Mater | Manufacture of boron nitride |
| JPS60155508A (en) * | 1984-08-02 | 1985-08-15 | Res Dev Corp Of Japan | Noncrystalline boron nitride having improved stability |
Cited By (12)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| WO1988000934A1 (en) * | 1986-08-07 | 1988-02-11 | Kabushiki Kaisha Kouransha | Boron nitride sinter and process for its production |
| JPS6345178A (en) * | 1986-08-07 | 1988-02-26 | 株式会社 香蘭社 | Boron nitride sintering raw material powder |
| EP0314807A1 (en) * | 1987-05-12 | 1989-05-10 | Kabushiki Kaisha Kouransha | Molten metal container |
| US5308044A (en) * | 1987-05-12 | 1994-05-03 | Kabushiki Kaisha Kouransha | Boron nitride ceramics and molten metal container provided with members made of the same ceramics |
| US5230873A (en) * | 1988-09-10 | 1993-07-27 | Firna Siegfried Golz | Process for producing amorphous boron nitride of high hardness |
| JPH02296706A (en) * | 1989-05-02 | 1990-12-07 | Rhone Poulenc Chim | Amorphous or irregular- laminate and spherical in particular boron nitride and its production method |
| WO1999061391A1 (en) * | 1998-05-22 | 1999-12-02 | Sumitomo Electric Industries, Ltd. | Cubic system boron nitride sintered body cutting tool |
| US6737377B1 (en) | 1998-05-22 | 2004-05-18 | Sumitomo Electric Industries, Ltd. | Cutting tool of a cubic boron nitride sintered compact |
| WO2011021366A1 (en) * | 2009-08-20 | 2011-02-24 | 株式会社カネカ | Process for production of spheroidized boron nitride |
| US8617503B2 (en) | 2009-08-20 | 2013-12-31 | Kaneka Corporation | Process for production of spheroidized boron nitride |
| JP5673539B2 (en) * | 2009-08-20 | 2015-02-18 | 株式会社カネカ | Method for producing spheroidized boron nitride |
| CN107161960A (en) * | 2017-06-06 | 2017-09-15 | 哈尔滨工业大学深圳研究生院 | A kind of high pressure vapor prepares the method and apparatus of boron nitride spherical powder |
Also Published As
| Publication number | Publication date |
|---|---|
| JPH0510282B2 (en) | 1993-02-09 |
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