JPH0342933B2 - - Google Patents
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- Publication number
- JPH0342933B2 JPH0342933B2 JP58072654A JP7265483A JPH0342933B2 JP H0342933 B2 JPH0342933 B2 JP H0342933B2 JP 58072654 A JP58072654 A JP 58072654A JP 7265483 A JP7265483 A JP 7265483A JP H0342933 B2 JPH0342933 B2 JP H0342933B2
- Authority
- JP
- Japan
- Prior art keywords
- cbn
- hbn
- licabn
- powder
- catalyst
- 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.)
- Expired
Links
- 239000003054 catalyst Substances 0.000 claims description 17
- 238000000034 method Methods 0.000 claims description 17
- 229910052582 BN Inorganic materials 0.000 claims description 12
- PZNSFCLAULLKQX-UHFFFAOYSA-N Boron nitride Chemical compound N#B PZNSFCLAULLKQX-UHFFFAOYSA-N 0.000 claims description 12
- 239000000654 additive Substances 0.000 claims description 12
- 230000000996 additive effect Effects 0.000 claims description 8
- 230000002194 synthesizing effect Effects 0.000 claims description 8
- 229910052782 aluminium Inorganic materials 0.000 claims description 5
- 229910052796 boron Inorganic materials 0.000 claims description 5
- ZOXJGFHDIHLPTG-UHFFFAOYSA-N Boron Chemical compound [B] ZOXJGFHDIHLPTG-UHFFFAOYSA-N 0.000 claims 1
- XAGFODPZIPBFFR-UHFFFAOYSA-N aluminium Chemical compound [Al] XAGFODPZIPBFFR-UHFFFAOYSA-N 0.000 claims 1
- 239000000843 powder Substances 0.000 description 19
- 230000015572 biosynthetic process Effects 0.000 description 4
- 238000006243 chemical reaction Methods 0.000 description 4
- 230000000052 comparative effect Effects 0.000 description 4
- 238000004519 manufacturing process Methods 0.000 description 4
- 238000003786 synthesis reaction Methods 0.000 description 4
- 229910003460 diamond Inorganic materials 0.000 description 3
- 239000010432 diamond Substances 0.000 description 3
- 239000002994 raw material Substances 0.000 description 3
- 230000000694 effects Effects 0.000 description 2
- 239000011888 foil Substances 0.000 description 2
- 238000000465 moulding Methods 0.000 description 2
- 239000003082 abrasive agent Substances 0.000 description 1
- 229910052783 alkali metal Inorganic materials 0.000 description 1
- 150000001340 alkali metals Chemical class 0.000 description 1
- 229910052784 alkaline earth metal Inorganic materials 0.000 description 1
- -1 alkaline earth metal nitrides Chemical class 0.000 description 1
- 239000012298 atmosphere Substances 0.000 description 1
- 239000013078 crystal Substances 0.000 description 1
- 230000002542 deteriorative effect Effects 0.000 description 1
- 230000005496 eutectics Effects 0.000 description 1
- 239000011261 inert gas Substances 0.000 description 1
- IDBFBDSKYCUNPW-UHFFFAOYSA-N lithium nitride Chemical compound [Li]N([Li])[Li] IDBFBDSKYCUNPW-UHFFFAOYSA-N 0.000 description 1
- 239000011812 mixed powder Substances 0.000 description 1
- 239000012299 nitrogen atmosphere Substances 0.000 description 1
- 239000002245 particle Substances 0.000 description 1
- 239000000126 substance Substances 0.000 description 1
Landscapes
- Catalysts (AREA)
Description
【発明の詳細な説明】
本発明は、六方晶窒化ほう素から立方晶窒化ほ
う素を合成する方法に関し、特にその収率をあげ
ることを目的とした立方晶窒化ほう素合成法に関
する。DETAILED DESCRIPTION OF THE INVENTION The present invention relates to a method for synthesizing cubic boron nitride from hexagonal boron nitride, and particularly to a method for synthesizing cubic boron nitride aimed at increasing its yield.
立方晶窒化ほう素（以下CBNという）は、ダ
イヤモンドに近い固さを有し、しかも化学的安定
性がダイヤンモドより優れているため、研削材と
しての需要が増大しつつある。 Cubic boron nitride (hereinafter referred to as CBN) has a hardness close to that of diamond, and its chemical stability is superior to that of diamond, so demand for it as an abrasive is increasing.
従来、上記のようなCBNの工業的な製造方法
としては、六方晶窒化ほう素（以下HBNとい
う）の粉末と、触媒粉末とを混合し、これを1300
〜1600℃の高温下で、40〜60kbarの高圧を加え、
HBNをCBNに変換する方法が行なわれている。
この方法に使用される触媒としては、アルカリ金
属或いはアルカリ土類金属の窒化物、Ca3B2N4
やLi3BN2等が知られている。このような方法は
HBNを触媒融液に溶け込ませ、合成条件下での
共晶体への溶解度がHBNよりCBNの方が小さい
ことを利用してCBNを析出させるものである。
ところで、研削材としてのCBN粒子は、緻密で
透明性がよく、自形粒で圧壊強度の高い良質なも
のであることが要求される。しかし上記従来の
CBN製造方法においては、必ずしも充分な機械
的強度、良好な形状を有する良質なCBNを得る
ことができるとは限らないのが実情であつた。 Conventionally, the industrial method for producing CBN as described above involves mixing hexagonal boron nitride (hereinafter referred to as HBN) powder and catalyst powder,
Under high temperature of ~1600℃, high pressure of 40~60kbar is applied,
Methods are being used to convert HBN to CBN.
Catalysts used in this method include alkali metal or alkaline earth metal nitrides, Ca 3 B 2 N 4
and Li 3 BN 2 are known. This kind of method
HBN is dissolved in the catalyst melt and CBN is precipitated by taking advantage of the fact that CBN has a lower solubility in the eutectic than HBN under synthesis conditions.
By the way, CBN particles used as an abrasive material are required to be dense, transparent, euhedral grains, and of high quality with high crushing strength. However, the above conventional
The reality is that in CBN manufacturing methods, it is not always possible to obtain high-quality CBN with sufficient mechanical strength and a good shape.
本発明者らは先にHBNに混合する触媒とし
て、LiCaBN2，LiBaBN2を用いて良質なCBNを
得る方法を発明した（特願昭56−181391（特開昭
58−84106号公報）、57−122973（特開昭59−18105
号公報）参照）。 The present inventors previously invented a method for obtaining high-quality CBN using LiCaBN 2 and LiBaBN 2 as catalysts to be mixed with HBN (Japanese Patent Application No. 181391/1989).
58-84106), 57-122973 (Japanese Unexamined Patent Publication No. 59-18105)
(Reference).
これら特願昭にはそれぞれLiCaBN2、
LiBaBN2の合成法が記載されている。これら
LiCaBN2又はLiBaBN2を用いる上記方法は、良
質のCNBが得られるがHBNのCNBへの変換率
（収率）があまりよくない欠点があつた。 These patent applications include LiCaBN 2 ,
A method for synthesizing LiBaBN 2 is described. these
The above method using LiCaBN 2 or LiBaBN 2 can obtain CNB of good quality, but has the drawback that the conversion rate (yield) of HBN to CNB is not very good.
本発明者らは上記の事情を考慮して鋭意研究し
た結果、LiCaBN2又はLiBaBN2触媒とともに添
加物としてAl又はＢを用いると、CBNの質が悪
くならないで、収率が上がることを発見した。 As a result of intensive research in consideration of the above circumstances, the present inventors discovered that when Al or B is used as an additive together with LiCaBN 2 or LiBaBN 2 catalyst, the yield can be increased without deteriorating the quality of CBN. .
本発明はこの発見に基づいて完成されたもの
で、その要旨は六方晶窒化ほう素を合成する方法
において、触媒としてLiCaBN2、又はLiBaBN2
を用い、さらに添加物としてAl又はＢを六方晶
窒化ほう素に対し５重量％以下用いることを特徴
とする立方晶窒化ほう素の合成法にある。 The present invention was completed based on this discovery, and its gist is a method for synthesizing hexagonal boron nitride using LiCaBN 2 or LiBaBN 2 as a catalyst.
A method for synthesizing cubic boron nitride, characterized in that Al or B is used as an additive in an amount of 5% by weight or less based on hexagonal boron nitride.
以下本発明の方法を説明する。 The method of the present invention will be explained below.
本発明は、HBNに触媒としてLiCaBN2、又は
LiBaBN2および添加物としてAl又はＢを所定量
加えて、CBNの安定域である40〜60kbar、1300
〜1600℃の条件に保持してHBNをCBNに変換す
る方法である。 The present invention uses LiCaBN 2 as a catalyst in HBN, or
By adding LiBaBN 2 and a predetermined amount of Al or B as an additive, the temperature is 40 to 60 kbar, which is the stable range of CBN, and 1300 kbar.
This method converts HBN to CBN by maintaining the temperature at ~1600°C.
上記LiCaBN2およびLiBaBN2は合成する原料
も入手し易く、それらの製造も容易である。 The raw materials for synthesizing LiCaBN 2 and LiBaBN 2 are easily available, and their production is also easy.
上記LiCaBN2、LiBaBN2の製法は、上記特願
昭に記載されているが、改めてLiCaBN2を代表
例として説明する。先ず、原料としてLi3N、
Ca3N2、HBNの粉末を用いる。これらの粉末を
モル比でLi3N：Ca3N2：HBN＝１〜1.4：１〜
1.4：３の割合に混合し、約1000℃に40分程度保
持した後冷却して、凝固したLiCaBN2を得る。
これを不活性ガス雰囲気中で150メツシユ以下に
粉砕してCBN合成触媒に使用する。また
LiBaBN2も同様にして製造することができる。 The method for producing LiCaBN 2 and LiBaBN 2 is described in the above patent application, but will be explained again using LiCaBN 2 as a representative example. First, Li 3 N as a raw material,
Ca 3 N 2 and HBN powders are used. The molar ratio of these powders is Li3N : Ca3N2 :HBN=1~1.4:1~
They are mixed at a ratio of 1.4:3, kept at about 1000°C for about 40 minutes, and then cooled to obtain solidified LiCaBN 2 .
This is crushed to 150 mesh or less in an inert gas atmosphere and used as a CBN synthesis catalyst. Also
LiBaBN 2 can also be produced in a similar manner.
上記LiCaBN2、又はLiBaBN2（以下触媒とい
う）の使用量は原料HBNに対し（触媒／
HBN）、５〜50重量％、望ましくは10〜30重量
％である。５％以下又は50％以上では、良質の
CBNが得られない。 The amount of LiCaBN 2 or LiBaBN 2 (hereinafter referred to as catalyst) used is based on the raw material HBN (catalyst/
HBN), 5 to 50% by weight, preferably 10 to 30% by weight. Less than 5% or more than 50% indicates good quality.
I can't get CBN.
Al又はＢ（以下添加物という）は150メツシユ
以下の粉末或は箔として使用する。混合割合は、
HBNに対し0.1〜５重量％がよい。５重量％以上
とするとCBNの形状が悪くなり、0.1重量％以下
だとCBNの収率上昇の効果が少ない。 Al or B (hereinafter referred to as additive) is used in the form of powder or foil of 150 mesh or less. The mixing ratio is
It is preferably 0.1 to 5% by weight based on HBN. If it is more than 5% by weight, the shape of CBN will deteriorate, and if it is less than 0.1% by weight, the effect of increasing the yield of CBN will be small.
上記触媒、添加物を原料HBNに添加するに
は、次のような方法がある。 The following methods can be used to add the above catalyst and additives to raw HBN.
HBNを150メツシユ以下の粉末として、こ
れに所定量の触媒および添加物の粉末を添加混
合し、この混合した粉末を圧粉成形する。 HBN is made into a powder of 150 mesh or less, a predetermined amount of catalyst and additive powder is added and mixed, and the mixed powder is compacted.
HBN粉末および触媒粉末をそれぞれ圧粉成
形して薄板とし、これらの薄板と添加物の箔又
は粉末を圧粉した薄板とを所定の比率となるよ
うに積層する。 The HBN powder and the catalyst powder are each compacted into thin plates, and these thin plates and a thin plate made by compacting additive foil or powder are laminated at a predetermined ratio.
上記触媒および添加物が所定の割合で添加され
た成形体或は積層体は、ダイヤモンド合成に使用
される周知の高圧高温反応器に装填され、所定の
条件に保持されてCBNが合成される。 The molded body or laminate to which the catalyst and additives have been added at a predetermined ratio is loaded into a well-known high-pressure, high-temperature reactor used for diamond synthesis, and maintained under predetermined conditions to synthesize CBN.
この方法は、添加物を添加しない場合に比して
30〜60％CBNの生成量が上り、CBNの大幅なコ
ストダウンを可能とする方法である。 This method is more effective than when no additives are added.
This method increases the amount of CBN produced by 30 to 60% and makes it possible to significantly reduce the cost of CBN.
なお、CBNの合成には、結晶成長の該として
CBN種子を添加することがあるが、当然のこと
ながら、これは本発明に含まれる。この場合、上
記種子を上記添加する触媒および添加物で被覆す
ることも可能である。 In addition, in the synthesis of CBN, as a matter of crystal growth,
CBN seeds may be added and are, of course, included in the invention. In this case, it is also possible to coat the seeds with the added catalyst and additives.
次に実施例および比較例により本発明の作用効
果を示す。 Next, the effects of the present invention will be illustrated by Examples and Comparative Examples.
150メツシユ下のLi3N粉末、Ca3N2粉末、
HBN粉末をモル比で１：１：３の割合で混合
し、850℃、N2雰囲気中で１時間反応させた後冷
却し、凝固した生成物をＸ線によつて解析し、
LiCaBN2であることを確認して、これを触媒と
した。 Li 3 N powder, Ca 3 N 2 powder under 150 mesh,
HBN powder was mixed at a molar ratio of 1:1:3, reacted at 850°C in a N2 atmosphere for 1 hour, cooled, and the solidified product was analyzed by X-rays.
It was confirmed that it was LiCaBN 2 , and this was used as a catalyst.
実施例 １
150メツシユ下のHBN、LiCaBN2，Alの粉末
を重量比で10：１；0.02の割合で混合し、成形圧
1.5t／cm2で26mmφ×32mmｈの圧粉成形体とした。
この圧粉成形体の成形密度は、1.7ｇ／cm3であつ
た。これを、高圧高温反応器に装填し、圧力：
50kbar、温度：1450℃の条件で10分間処理し
CBNを合成した。HBNのCBNへの変換率（収
率）は41％であつた。Example 1 150 meshes of HBN, LiCaBN 2 and Al powder were mixed at a weight ratio of 10:1; 0.02, and the molding pressure was
A powder compact of 26 mmφ x 32 mmh was made at 1.5 t/cm 2 .
The compacting density of this powder compact was 1.7 g/cm 3 . This is loaded into a high-pressure, high-temperature reactor, and the pressure:
Processed for 10 minutes at 50kbar and temperature: 1450℃.
CBN was synthesized. The conversion rate (yield) of HBN to CBN was 41%.
実施例 ２
実施例１のAlの代りにＢを用い、HBN：
LiCaBN2：Ｂ＝10：１：0.1とした外は実施例１
と全く同じにしてCBNを合成した。CBNの収率
は41％であつた。Example 2 Using B instead of Al in Example 1, HBN:
Example 1 except that LiCaBN 2 :B=10:1:0.1
CBN was synthesized in exactly the same manner. The yield of CBN was 41%.
実施例 ３
150メツシユ以下のHBN、LiBaBN2、Ｂを重
量比で10：１：0.1の割合で混合し、成形圧1.5t／
cm2で、26mmφ×32mmｈの圧粉成形体とした。Example 3 150 meshes or less of HBN, LiBaBN 2 and B were mixed at a weight ratio of 10:1:0.1, and a molding pressure of 1.5t/
cm 2 and a powder compact of 26 mmφ×32 mmh.
この圧粉成形体の成形密度は、1.65ｇ／cm3であ
つた。これを高圧高温反応器に製填し、圧力
50Kbar、温度1450℃の条件で10分間処理し、
CBNを合成した。この際HBNのCBNへの変換
率（収率）38％であつた。 The compacting density of this powder compact was 1.65 g/cm 3 . This is packed into a high-pressure, high-temperature reactor, and the pressure
Treated for 10 minutes at 50Kbar and 1450℃,
CBN was synthesized. At this time, the conversion rate (yield) of HBN to CBN was 38%.
比較例 １
ｂ族元素を用いないで、HBN：LiCaBN2＝
10：１の重量比で圧粉成形体をつくり、実施例１
と同じ条件でCBNを合成した。その収率は28％
であつた。Comparative example 1 HBN:LiCaBN 2 = without using group b elements
A powder compact was made at a weight ratio of 10:1, and Example 1
CBN was synthesized under the same conditions. Its yield is 28%
It was hot.
比較例 ２
添加物Ｂを添加しない以外は実施例３と同じに
してCBNを合成した。その結果圧粉体の成形密
度は1.65ｇ／cm3、HBNのCBNへの変換率は、26
％であつた。Comparative Example 2 CBN was synthesized in the same manner as in Example 3 except that Additive B was not added. As a result, the density of the green compact was 1.65 g/cm 3 , and the conversion rate of HBN to CBN was 26
It was %.
なお、実施例、比較例共に生成したCBNは良
質であつた。 Note that the CBN produced in both Examples and Comparative Examples was of good quality.
Claims (1)
成する方法において、触媒としてLiCaBN2、又
はLiBaBN2を用い、さらに添加物としてアルミ
ニウム又はほう素を六方晶窒素化ほう素に対して
５重量％以下用いることを特徴とする立方晶窒化
ほう素の合成法。1 In a method for synthesizing cubic boron nitride from hexagonal boron nitride, LiCaBN 2 or LiBaBN 2 is used as a catalyst, and aluminum or boron is added as an additive in an amount of 5% by weight based on the hexagonal boron nitride. A method for synthesizing cubic boron nitride, characterized in that it is used as follows.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| JP58072654A JPS59199513A (en) | 1983-04-25 | 1983-04-25 | Synthesis of boron nitride of cubic system |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| JP58072654A JPS59199513A (en) | 1983-04-25 | 1983-04-25 | Synthesis of boron nitride of cubic system |
Publications (2)
| Publication Number | Publication Date |
|---|---|
| JPS59199513A JPS59199513A (en) | 1984-11-12 |
| JPH0342933B2 true JPH0342933B2 (en) | 1991-06-28 |
Family
ID=13495579
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| JP58072654A Granted JPS59199513A (en) | 1983-04-25 | 1983-04-25 | Synthesis of boron nitride of cubic system |
Country Status (1)
| Country | Link |
|---|---|
| JP (1) | JPS59199513A (en) |
Families Citing this family (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| FR2686101A1 (en) * | 1992-01-14 | 1993-07-16 | Centre Nat Rech Scient | Process for the preparation of single crystals of cubic boron nitride |
| US5869015A (en) * | 1998-05-04 | 1999-02-09 | General Electric Company | Method for producing cubic boron nitride using melamine as a catalyst |
| JPWO2004061040A1 (en) * | 2003-01-06 | 2006-05-11 | 昭和電工株式会社 | Cubic boron nitride abrasive, method for producing the same, grindstone using the same, and abrasive cloth |
-
1983
- 1983-04-25 JP JP58072654A patent/JPS59199513A/en active Granted
Also Published As
| Publication number | Publication date |
|---|---|
| JPS59199513A (en) | 1984-11-12 |
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