JPS62278170A - Cubic boron nitride sintered body and manufacture - Google Patents
Cubic boron nitride sintered body and manufactureInfo
- Publication number
- JPS62278170A JPS62278170A JP61118670A JP11867086A JPS62278170A JP S62278170 A JPS62278170 A JP S62278170A JP 61118670 A JP61118670 A JP 61118670A JP 11867086 A JP11867086 A JP 11867086A JP S62278170 A JPS62278170 A JP S62278170A
- Authority
- JP
- Japan
- Prior art keywords
- boron nitride
- cbn
- sintered body
- cubic boron
- powder
- 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 description 19
- 229910052582 BN Inorganic materials 0.000 title claims description 16
- 238000004519 manufacturing process Methods 0.000 title claims description 7
- IJGRMHOSHXDMSA-UHFFFAOYSA-N Atomic nitrogen Chemical compound N#N IJGRMHOSHXDMSA-UHFFFAOYSA-N 0.000 claims description 16
- 238000006243 chemical reaction Methods 0.000 claims description 14
- 238000005245 sintering Methods 0.000 claims description 14
- UFHFLCQGNIYNRP-UHFFFAOYSA-N Hydrogen Chemical compound [H][H] UFHFLCQGNIYNRP-UHFFFAOYSA-N 0.000 claims description 10
- 150000001875 compounds Chemical class 0.000 claims description 10
- 239000001257 hydrogen Substances 0.000 claims description 6
- 229910052739 hydrogen Inorganic materials 0.000 claims description 6
- 229910052757 nitrogen Inorganic materials 0.000 claims description 6
- 239000000203 mixture Substances 0.000 claims description 5
- 239000002994 raw material Substances 0.000 claims description 5
- 229910001873 dinitrogen Inorganic materials 0.000 claims description 4
- 239000000843 powder Substances 0.000 description 17
- 239000007789 gas Substances 0.000 description 10
- UORVGPXVDQYIDP-UHFFFAOYSA-N borane Chemical compound B UORVGPXVDQYIDP-UHFFFAOYSA-N 0.000 description 7
- 238000010438 heat treatment Methods 0.000 description 6
- 238000000034 method Methods 0.000 description 6
- 239000000463 material Substances 0.000 description 5
- 229910000085 borane Inorganic materials 0.000 description 4
- 150000003839 salts Chemical class 0.000 description 4
- PAWQVTBBRAZDMG-UHFFFAOYSA-N 2-(3-bromo-2-fluorophenyl)acetic acid Chemical compound OC(=O)CC1=CC=CC(Br)=C1F PAWQVTBBRAZDMG-UHFFFAOYSA-N 0.000 description 3
- 239000011230 binding agent Substances 0.000 description 3
- 239000003054 catalyst Substances 0.000 description 3
- 230000007423 decrease Effects 0.000 description 3
- 230000000694 effects Effects 0.000 description 3
- 239000002184 metal Substances 0.000 description 3
- 239000002667 nucleating agent Substances 0.000 description 3
- 239000000126 substance Substances 0.000 description 3
- 238000011109 contamination Methods 0.000 description 2
- 229910003460 diamond Inorganic materials 0.000 description 2
- 239000010432 diamond Substances 0.000 description 2
- 238000011049 filling Methods 0.000 description 2
- 239000011812 mixed powder Substances 0.000 description 2
- 239000007858 starting material Substances 0.000 description 2
- QGZKDVFQNNGYKY-UHFFFAOYSA-N Ammonia Chemical compound N QGZKDVFQNNGYKY-UHFFFAOYSA-N 0.000 description 1
- ZOXJGFHDIHLPTG-UHFFFAOYSA-N Boron Chemical compound [B] ZOXJGFHDIHLPTG-UHFFFAOYSA-N 0.000 description 1
- 229910000831 Steel Inorganic materials 0.000 description 1
- 230000004913 activation Effects 0.000 description 1
- 239000000654 additive Substances 0.000 description 1
- 239000000956 alloy Substances 0.000 description 1
- 229910045601 alloy Inorganic materials 0.000 description 1
- 229910052796 boron Inorganic materials 0.000 description 1
- 230000000052 comparative effect Effects 0.000 description 1
- 230000008602 contraction Effects 0.000 description 1
- 238000001816 cooling Methods 0.000 description 1
- 239000013078 crystal Substances 0.000 description 1
- 238000000354 decomposition reaction Methods 0.000 description 1
- 238000007872 degassing Methods 0.000 description 1
- 238000000227 grinding Methods 0.000 description 1
- 238000001000 micrograph Methods 0.000 description 1
- 238000002156 mixing Methods 0.000 description 1
- 230000006911 nucleation Effects 0.000 description 1
- 238000010899 nucleation Methods 0.000 description 1
- 239000002245 particle Substances 0.000 description 1
- 239000011148 porous material Substances 0.000 description 1
- 230000001737 promoting effect Effects 0.000 description 1
- 230000001681 protective effect Effects 0.000 description 1
- 239000011541 reaction mixture Substances 0.000 description 1
- 239000010959 steel Substances 0.000 description 1
- 238000009834 vaporization Methods 0.000 description 1
- 230000008016 vaporization Effects 0.000 description 1
Abstract
(57)【要約】本公報は電子出願前の出願データであるた
め要約のデータは記録されません。(57) [Summary] This bulletin contains application data before electronic filing, so abstract data is not recorded.
Description
【発明の詳細な説明】
３、発明の詳細な説明
（産業上の利用分野）
本発明は反応焼結によって製造する実質的に立方晶窒化
硼素からなる多結晶焼結体及びその製造法に関するもの
である。[Detailed Description of the Invention] 3. Detailed Description of the Invention (Field of Industrial Application) The present invention relates to a polycrystalline sintered body made essentially of cubic boron nitride produced by reaction sintering, and a method for producing the same. It is.
（従来の技術）
立方晶窒化硼素（以下ｃＢＮと略記する）は、硬度、耐
摩耗性及び熱伝導率がダイヤモンドについですぐれ、切
削、研削用材料として、あるいはヒートシンク材として
有用な物質である。特に鋼材の高速切削加工用工具とし
てのｃＢＮはダイヤモンド工具よも熱的、化学的に安定
しており、耐摩耗性もすぐれているので用途が急激に増
加している。(Prior Art) Cubic boron nitride (hereinafter abbreviated as cBN) has hardness, wear resistance, and thermal conductivity that are second only to diamond, and is a useful substance as a material for cutting and grinding or as a heat sink material. In particular, the use of cBN as a tool for high-speed cutting of steel materials is rapidly increasing because it is thermally and chemically more stable than diamond tools and has excellent wear resistance.
従来、ｃＢＮ焼結材やその製造法に関して数多くの発明
がなされている。それらの−例はｃＢＮを結合材となる
金属あるいは化合物と混合し高圧高温処理によりｃＢＮ
焼結体とするものであり、例えば特公昭５７−４９６２
１号に記載されているように、ＣＢＮ粉末、耐熱性化合
物粉末及び金属またはその合金、化合物の粉末を混合し
て成形し、高圧高温下で焼結させた高硬度工具用焼結体
およびその製造法がある。他の１つは出発原料に大方晶
窒化硼素を用い、触媒となる金属あるいは化合物を混合
し、高圧高温処理を行なって、大方晶窒化硼素（以下ｈ
ＢＮと略記する）をｃＢＮに転換すると同時に焼結体を
製造するものであり、例えば特公昭５）−１６１９９号
に記載されているように、ｈＢＮに触媒となるＣｏを加
え、高圧高温反応により、ｃＢＮに転換させると同時に
焼結させる方法がある。Conventionally, many inventions have been made regarding cBN sintered materials and methods for producing the same. For example, cBN is mixed with a metal or compound as a binder and processed by high pressure and high temperature.
For example, Japanese Patent Publication No. 57-4962
As described in No. 1, a sintered body for high-hardness tools and its sintered body formed by mixing CBN powder, heat-resistant compound powder, metal or its alloy, or compound powder and sintering it under high pressure and high temperature. There is a manufacturing method. The other method uses orthogonal boron nitride as a starting material, mixes a metal or compound as a catalyst, and performs high-pressure and high-temperature treatment.
In this method, a sintered body is produced at the same time as BN (abbreviated as BN) is converted into cBN. , there is a method of converting to cBN and sintering at the same time.
（発明が解決しようとする問題点）
しかしながらこれらの焼結体及びその製造方法では、結
合剤あるいは触媒が焼結体中に存在するため、硬度が低
くなって、耐摩耗性が低下し、熱的化学的安定性の点で
もｃＢＮ本来の特性より劣ることが避けられない。(Problems to be Solved by the Invention) However, in these sintered bodies and their manufacturing methods, since the binder or catalyst is present in the sintered bodies, the hardness decreases, the wear resistance decreases, and the heat resistance decreases. It is unavoidable that cBN is inferior to the original properties of cBN in terms of chemical stability as well.
さらにこれらの欠点を改良するため触媒に分解気化する
ものを用い、高圧高温処理により転換と焼結を同時に行
なわせる方法が提案されている。Furthermore, in order to improve these drawbacks, a method has been proposed in which a catalyst capable of decomposition and vaporization is used and conversion and sintering are performed simultaneously through high pressure and high temperature treatment.
例えば特公昭５３−１０２９００号に記載されているよ
うに、アンモニアガスを含有したｈＢＮに高圧高温を印
加してｃＢＮ焼結体を製造する方法である。しかしなが
らこの方法では、ｈＢＮの充填率の悪さやｈＢＮがｃＢ
Ｎに転換する場合の体積収縮が大きいことな、 どの
ため実用化が困難である。For example, as described in Japanese Patent Publication No. 53-102900, a cBN sintered body is produced by applying high pressure and high temperature to hBN containing ammonia gas. However, with this method, the filling rate of hBN is poor and hBN is cB.
It is difficult to put it into practical use because of the large volumetric contraction when converting to N.
本発明は上記の問題を解決するためになされたものであ
り、ｃＢＮを核としてｈＢＮをｃＢＮに転換させると同
時に焼結させることができれば、ｃＢＮのみからなる焼
結体が形成できるのではないかという着想に基づき研究
を行ない、本発明に到ったものである。ｃＢＮを転換の
核発生剤にできれば結合剤を含まない焼結体が形成でき
、ｈＢＮがｃＢＮへ転換する場合の体積収縮量を小さく
することができる。The present invention was made to solve the above problem, and it is believed that if hBN can be converted into cBN using cBN as a core and sintered at the same time, a sintered body made only of cBN can be formed. Based on this idea, we conducted research and arrived at the present invention. If cBN can be used as a nucleating agent for conversion, a sintered body containing no binder can be formed, and the amount of volumetric shrinkage when hBN is converted to cBN can be reduced.
（問題点を解決するための手段）
本発明の立方晶窒化硼素焼結体は、立方晶窒化硼素を含
有する大方晶窒化硼素粉末を原料とし、反応焼結により
製造した実質的に立方晶窒化硼素からなることを特徴と
するものである。(Means for Solving the Problems) The cubic boron nitride sintered body of the present invention is substantially cubic boron nitride produced by reaction sintering using bulk boron nitride powder containing cubic boron nitride as a raw material. It is characterized by being made of boron.
また、本発明の立方晶窒化硼素焼結体の製造法は、立方
晶窒化硼素を含有する六方晶窒化硼素粉末を真空加熱脱
気した後、窒素ガスと水素ガスの混合雰囲気中で加熱し
、１００℃以上で分解気化する水素及び窒素を含む化合
物を添加し、該混合物を圧力４ＧＰａ以上温度１０００
℃以上の高圧高温のもとで反応焼結することを特徴とす
るものである。In addition, the method for producing a cubic boron nitride sintered body of the present invention includes vacuum heating and degassing of hexagonal boron nitride powder containing cubic boron nitride, and then heating in a mixed atmosphere of nitrogen gas and hydrogen gas. A compound containing hydrogen and nitrogen that decomposes and vaporizes at 100°C or higher is added, and the mixture is heated at a pressure of 4GPa or higher and a temperature of 1000°C.
It is characterized by reaction sintering under high pressure and high temperature of ℃ or higher.
（作 用）
上述した構成において、本発明の特徴はｃＢＮを含むｈ
ＢＮ粉末を用いることによりｃＢＮを核発生剤として反
応焼結を行なわしめるところにあり、そのために前処理
と分解気化する水素及び窒素を含む化合物、好ましくは
塩またはボラン類の添加による活性化が重要な役割を果
す。ｃＢＮを含むｈＢＮ粉末を原料とする別の利点は、
高温高圧装置に充填する粉末の量が多くなって試料に加
わる圧力の効率が向上し、ざらにｈＢＮがｃＢＮに転換
する場合の体積変化も小さくすることができることにあ
る。(Function) In the above-described configuration, the feature of the present invention is that h containing cBN
By using BN powder, reaction sintering is performed using cBN as a nucleating agent, and for this purpose, pretreatment and activation by adding a compound containing hydrogen and nitrogen that decomposes and vaporizes, preferably salt or borane, are important. play a role. Another advantage of using hBN powder containing cBN as a raw material is that
The amount of powder packed into the high-temperature and high-pressure apparatus is increased, which improves the efficiency of the pressure applied to the sample, and also reduces the volume change when hBN is converted to cBN.
前処理の作用はｃＢＮを含有するｈＢＮ粉末の表面に吸
着している異物を真空加熱により除き、次に水素ガスと
窒素ガスの混合雰囲気中で加熱することにより該粉末の
表面を活性し、ｈＢＮのＣＢＮ Ｉ＋２−換への核発生
を容易にすると同時に焼結を促進させることにある。The effect of pretreatment is to remove foreign substances adsorbed on the surface of hBN powder containing cBN by vacuum heating, and then activate the surface of the powder by heating in a mixed atmosphere of hydrogen gas and nitrogen gas, The objective is to facilitate nucleation into CBN I+2- conversion and at the same time promote sintering.
前処理した粉末を高温高圧装置に充填する場合、いかに
迅速に処理しても前処理により活性化した試料が大気に
晒されることは避けられず、その結果活性化した表面が
汚染される。その汚染を取り除くために低温で分解気化
する水素及び窒素を含む化合物、好ましくは塩、または
ボラン類を添加する。低温で分解気化する水素及び窒素
を含む化合物、好ましくは塩またはボラン類は高圧高温
処理の昇温中に分解気化し、粉末の表面活性に役立つと
共にｂＢＮがｃＢＮに転換し焼結する反応焼結における
保護雰囲気の作用も果す。When filling a pretreated powder into a high-temperature, high-pressure device, no matter how quickly the powder is processed, it is inevitable that the sample activated by the pretreatment will be exposed to the atmosphere, resulting in contamination of the activated surface. To remove the contamination, compounds containing hydrogen and nitrogen, preferably salts, or boranes, which decompose and vaporize at low temperatures, are added. Compounds containing hydrogen and nitrogen that decompose and vaporize at low temperatures, preferably salts or borane, decompose and vaporize during the temperature increase during high-pressure and high-temperature treatment, and serve for surface activity of the powder, as well as reaction sintering in which bBN is converted to cBN and sintered. It also acts as a protective atmosphere.
（実施例）
本発明において立方晶窒化硼素焼結体を得るには、まず
、出発原料としてｃＢＮを含有するｈＢＮ粉末を用意し
、その粉末を真空加熱により脱気した後、水素ガスと窒
素ガスの混合雰囲気中で温度４００℃以上に加熱する。(Example) In order to obtain a cubic boron nitride sintered body in the present invention, first, hBN powder containing cBN is prepared as a starting material, the powder is degassed by vacuum heating, and then hydrogen gas and nitrogen gas are Heating to a temperature of 400°C or higher in a mixed atmosphere.
冷却後１００℃以上で分解気化する水素及び窒素を含む
化合物、好ましくは塩またはボラン類を添加し、該混合
物を適当な高圧高温装置により圧力４ＧＰａ、温度１０
００℃以上所定時間保持し、予め存在するｃＢＮを核発
生剤としてｈＢＮをｃＢＮに転換すると同時に焼結させ
る反応焼結により、実質的にｃＢＮからなる多結晶焼結
体を形成するものである。After cooling, a compound containing hydrogen and nitrogen that decomposes and vaporizes at 100°C or higher, preferably salt or borane, is added, and the mixture is heated at a pressure of 4 GPa and a temperature of 10
A polycrystalline sintered body substantially consisting of cBN is formed by reaction sintering in which hBN is converted into cBN and sintered at the same time by holding the reaction mixture at 00° C. or higher for a predetermined period of time using pre-existing cBN as a nucleating agent.
以下、実際の例について説明する。An actual example will be explained below.
実施±
０．５〜１μｍのｃＢＮを２０〜５０％含有させた平均
粒径２ｐｍのｈＢＮ粉末を１０− ’ ｔｏｒｒ程度で
１０００℃、６０分真空加熱後、Ｎ２ガスとＮ２ガスの
混合ガス中で１０００℃、６０分の前処理を行ない、そ
のまま冷却した混合粉末に１％の硝酸アンモニウムを添
加し、ガードル型の高圧高温装置により圧カフＧＰａ、
温度１７００℃、３０分の高圧高温処理を施した（Ａ、
Ｂ。Implementation ± hBN powder with an average particle size of 2 pm containing 20-50% cBN of 0.5-1 μm was heated in vacuum at 1000°C for 60 minutes at about 10-' torr, and then heated in a mixed gas of N2 gas and N2 gas. After pretreatment at 1000°C for 60 minutes, 1% ammonium nitrate was added to the cooled mixed powder, and a pressure cuff GPa,
High pressure and high temperature treatment was performed at a temperature of 1700°C for 30 minutes (A,
B.
Ｃ試料）。同条件で前処理した混合粉末中に２％のトリ
アンモニアデカボランを添加し、同条件で高温高圧処理
した（Ｄ試料）。比較例としてｃＢＮを３０％含有させ
たｈＢＮを脱気後、Ｎ２ガスとＡｒガスの混合ガスで（
Ｅ試料）、あるいはＮ２ガスで（Ｆ試料）前処理を行っ
た場合、およびＢ試料において硝酸アンモニウムを加え
ない（Ｃ試料）条件でＡ−Ｃ試料と同一の高圧高温処理
を行ない、焼結体を作製して焼結体中のｃＢＮ ｉｉ、
密度、硬さを測定した。その結果を第１表に示す。C sample). 2% triammonium decaborane was added to the mixed powder pretreated under the same conditions, and the mixture was subjected to high temperature and high pressure treatment under the same conditions (Sample D). As a comparative example, hBN containing 30% cBN was degassed and then treated with a mixed gas of N2 gas and Ar gas (
The same high-pressure and high-temperature treatment as for A-C samples was performed in the case of pretreatment with N2 gas (Sample E) or with N2 gas (Sample F), and without the addition of ammonium nitrate in Sample B (Sample C). cBN ii produced and in a sintered body,
Density and hardness were measured. The results are shown in Table 1.
第１表から明らかなように予めｃＢＮを含有させること
によりｈＢＮのｃＢＮへの転換率は向上し、さらにＮ２
ガスとＮ２ガスの混合ガス中における前処理及び硝酸ア
ンモニウムまたはトリアンモニアデカポラン添加により
転換率が向上し、これらの添加物及び前処理は焼結促進
に有効な役割を果していることが明白である。第１図は
Ｂｇ＆料の研摩面写真である。気孔がほとんど見られず
、１０００ｇ荷重のビッカース硬度は５１００ｋｇ／
龍２であった。As is clear from Table 1, by pre-containing cBN, the conversion rate of hBN to cBN is improved, and N2
It is clear that the pretreatment in a mixture of gas and N2 gas and the addition of ammonium nitrate or triammonium decaporane improve the conversion rate, and that these additives and pretreatment play an effective role in promoting sintering. FIG. 1 is a photograph of the polished surface of Bg&material. Almost no pores are seen, and the Vickers hardness under a load of 1000g is 5100kg/
It was Dragon 2.
（発明の効果）
以上詳細に説明したところから明らかなように、本発明
の立方晶窒化硼素焼結体及びその製造法によれば、ｃＢ
Ｎを含有するｈＢＮ粉末を原料として反応焼結によりｃ
ＢＮ焼結体を製造しているので、極めて高純度な多結晶
焼結体を得ることができる。(Effects of the Invention) As is clear from the detailed explanation above, according to the cubic boron nitride sintered body and the manufacturing method thereof of the present invention, cB
c by reaction sintering using hBN powder containing N as a raw material.
Since a BN sintered body is manufactured, a polycrystalline sintered body of extremely high purity can be obtained.
また、原料粉末を活性化させて反応焼結させているので
、実質的にｃＢＮ １００％からなる高密度で強固な焼
結体を得ることができる。Further, since the raw material powder is activated and subjected to reaction sintering, a high-density and strong sintered body made of substantially 100% cBN can be obtained.
【図面の簡単な説明】
第１図は本発明の一実施例における研磨面の結晶構造を
示す顕微鏡写真である。
特許出願人 株式会社豊田中央研究所
同 出願人日本碍子株式会社BRIEF DESCRIPTION OF THE DRAWINGS FIG. 1 is a micrograph showing the crystal structure of a polished surface in one embodiment of the present invention. Patent applicant: Toyota Central Research Institute Co., Ltd. Patent applicant: Nippon Insulators Co., Ltd.
Claims (1)
料とし、反応焼結により製造した実質的に立方晶窒化硼
素からなることを特徴とする多結晶焼結体。 ２、立方晶窒化硼素を含有する六方晶窒化硼素粉末を真
空加熱脱気した後、窒素ガスと水素ガスの混合雰囲気中
で加熱し、１００℃以上で分解気化する水素及び窒素を
含む化合物を添加し、該混合物を圧力４ＧＰａ以上温度
１０００℃以上の高圧高温のもとで反応焼結することを
特徴とする実質的に立方晶窒化硼素からなる多結晶焼結
体の製造法。[Scope of Claims] 1. A polycrystalline sintered body substantially consisting of cubic boron nitride produced by reaction sintering using hexagonal boron nitride powder containing cubic boron nitride as a raw material. 2. Hexagonal boron nitride powder containing cubic boron nitride is vacuum heated and degassed, then heated in a mixed atmosphere of nitrogen gas and hydrogen gas, and a compound containing hydrogen and nitrogen that decomposes and vaporizes at 100°C or higher is added. A method for producing a polycrystalline sintered body substantially consisting of cubic boron nitride, characterized in that the mixture is reacted and sintered under high pressure and high temperature of 4 GPa or higher and 1000° C. or higher.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| JP61118670A JPS62278170A (en) | 1986-05-23 | 1986-05-23 | Cubic boron nitride sintered body and manufacture |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| JP61118670A JPS62278170A (en) | 1986-05-23 | 1986-05-23 | Cubic boron nitride sintered body and manufacture |
Publications (2)
| Publication Number | Publication Date |
|---|---|
| JPS62278170A true JPS62278170A (en) | 1987-12-03 |
| JPH0329024B2 JPH0329024B2 (en) | 1991-04-22 |
Family
ID=14742305
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| JP61118670A Granted JPS62278170A (en) | 1986-05-23 | 1986-05-23 | Cubic boron nitride sintered body and manufacture |
Country Status (1)
| Country | Link |
|---|---|
| JP (1) | JPS62278170A (en) |
Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| JP2006169080A (en) * | 2004-12-20 | 2006-06-29 | Sumitomo Electric Ind Ltd | Method of manufacturing cubic boron nitride polycrystal |
| JP2015529611A (en) * | 2012-08-03 | 2015-10-08 | 燕山大学 | Ultra-hard nano-twinned boron nitride bulk material and synthesis method thereof |
Citations (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| JPS4930357A (en) * | 1972-06-13 | 1974-03-18 |
-
1986
- 1986-05-23 JP JP61118670A patent/JPS62278170A/en active Granted
Patent Citations (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| JPS4930357A (en) * | 1972-06-13 | 1974-03-18 |
Cited By (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| JP2006169080A (en) * | 2004-12-20 | 2006-06-29 | Sumitomo Electric Ind Ltd | Method of manufacturing cubic boron nitride polycrystal |
| JP2015529611A (en) * | 2012-08-03 | 2015-10-08 | 燕山大学 | Ultra-hard nano-twinned boron nitride bulk material and synthesis method thereof |
| US9422161B2 (en) | 2012-08-03 | 2016-08-23 | Yanshan University | Ultrahard nanotwinned boron nitride bulk materials and synthetic method thereof |
Also Published As
| Publication number | Publication date |
|---|---|
| JPH0329024B2 (en) | 1991-04-22 |
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