JPS63134661A - Method for synthesizing high hardness boron nitride - Google Patents
Method for synthesizing high hardness boron nitrideInfo
- Publication number
- JPS63134661A JPS63134661A JP27935986A JP27935986A JPS63134661A JP S63134661 A JPS63134661 A JP S63134661A JP 27935986 A JP27935986 A JP 27935986A JP 27935986 A JP27935986 A JP 27935986A JP S63134661 A JPS63134661 A JP S63134661A
- Authority
- JP
- Japan
- Prior art keywords
- boron nitride
- gas
- substrate
- atoms
- boron
- 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
- 229910052582 BN Inorganic materials 0.000 title claims abstract description 32
- PZNSFCLAULLKQX-UHFFFAOYSA-N Boron nitride Chemical compound N#B PZNSFCLAULLKQX-UHFFFAOYSA-N 0.000 title claims abstract description 32
- 238000000034 method Methods 0.000 title claims description 18
- 230000002194 synthesizing effect Effects 0.000 title claims description 7
- 239000007789 gas Substances 0.000 claims abstract description 34
- 239000000758 substrate Substances 0.000 claims abstract description 29
- 239000011261 inert gas Substances 0.000 claims abstract description 19
- 125000004433 nitrogen atom Chemical group N* 0.000 claims abstract description 18
- 125000004429 atom Chemical group 0.000 claims abstract description 6
- 229910052739 hydrogen Inorganic materials 0.000 claims abstract description 3
- UFHFLCQGNIYNRP-UHFFFAOYSA-N Hydrogen Chemical compound [H][H] UFHFLCQGNIYNRP-UHFFFAOYSA-N 0.000 claims abstract 2
- 239000001257 hydrogen Substances 0.000 claims abstract 2
- ZOXJGFHDIHLPTG-UHFFFAOYSA-N Boron Chemical group [B] ZOXJGFHDIHLPTG-UHFFFAOYSA-N 0.000 claims description 20
- 229910052796 boron Inorganic materials 0.000 claims description 14
- 229910052757 nitrogen Inorganic materials 0.000 claims description 12
- 238000001308 synthesis method Methods 0.000 claims description 2
- 239000012495 reaction gas Substances 0.000 claims 1
- 238000006243 chemical reaction Methods 0.000 abstract description 6
- 230000001105 regulatory effect Effects 0.000 abstract 1
- 239000010408 film Substances 0.000 description 18
- 238000005520 cutting process Methods 0.000 description 10
- IJGRMHOSHXDMSA-UHFFFAOYSA-N Atomic nitrogen Chemical compound N#N IJGRMHOSHXDMSA-UHFFFAOYSA-N 0.000 description 6
- 238000000576 coating method Methods 0.000 description 4
- 238000004519 manufacturing process Methods 0.000 description 4
- 239000002994 raw material Substances 0.000 description 4
- 239000011248 coating agent Substances 0.000 description 3
- 238000000151 deposition Methods 0.000 description 3
- 230000000694 effects Effects 0.000 description 3
- ZOKXTWBITQBERF-UHFFFAOYSA-N Molybdenum Chemical compound [Mo] ZOKXTWBITQBERF-UHFFFAOYSA-N 0.000 description 2
- 238000004458 analytical method Methods 0.000 description 2
- 230000015572 biosynthetic process Effects 0.000 description 2
- ILAHWRKJUDSMFH-UHFFFAOYSA-N boron tribromide Chemical compound BrB(Br)Br ILAHWRKJUDSMFH-UHFFFAOYSA-N 0.000 description 2
- 239000011247 coating layer Substances 0.000 description 2
- 238000010884 ion-beam technique Methods 0.000 description 2
- -1 iron group metals Chemical class 0.000 description 2
- 239000000463 material Substances 0.000 description 2
- 229910052751 metal Inorganic materials 0.000 description 2
- 239000002184 metal Substances 0.000 description 2
- 229910052750 molybdenum Inorganic materials 0.000 description 2
- 239000011733 molybdenum Substances 0.000 description 2
- 239000000126 substance Substances 0.000 description 2
- 239000010409 thin film Substances 0.000 description 2
- 229910015845 BBr3 Inorganic materials 0.000 description 1
- 229910001018 Cast iron Inorganic materials 0.000 description 1
- 238000001069 Raman spectroscopy Methods 0.000 description 1
- XUIMIQQOPSSXEZ-UHFFFAOYSA-N Silicon Chemical compound [Si] XUIMIQQOPSSXEZ-UHFFFAOYSA-N 0.000 description 1
- 238000002441 X-ray diffraction Methods 0.000 description 1
- JZKFIPKXQBZXMW-UHFFFAOYSA-L beryllium difluoride Chemical compound F[Be]F JZKFIPKXQBZXMW-UHFFFAOYSA-L 0.000 description 1
- 229910001633 beryllium fluoride Inorganic materials 0.000 description 1
- 238000009835 boiling Methods 0.000 description 1
- 238000007796 conventional method Methods 0.000 description 1
- 229910003460 diamond Inorganic materials 0.000 description 1
- 239000010432 diamond Substances 0.000 description 1
- 239000012776 electronic material Substances 0.000 description 1
- 238000005516 engineering process Methods 0.000 description 1
- 238000005530 etching Methods 0.000 description 1
- 230000005281 excited state Effects 0.000 description 1
- 239000012535 impurity Substances 0.000 description 1
- 230000001678 irradiating effect Effects 0.000 description 1
- 230000008018 melting Effects 0.000 description 1
- 238000002844 melting Methods 0.000 description 1
- 150000004767 nitrides Chemical class 0.000 description 1
- 230000001376 precipitating effect Effects 0.000 description 1
- 230000035939 shock Effects 0.000 description 1
- 229910052710 silicon Inorganic materials 0.000 description 1
- 239000010703 silicon Substances 0.000 description 1
- 239000007787 solid Substances 0.000 description 1
- 230000008016 vaporization Effects 0.000 description 1
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 description 1
- 239000002023 wood Substances 0.000 description 1
Landscapes
- Chemical Vapour Deposition (AREA)
Abstract
Description
【発明の詳細な説明】
く産業上の利用分野〉
この発明は高硬度な立方晶窒化硼素の合成法に係り、詳
しくは非常に高硬度を有するだけでなく、熱伝導率に富
み、化学的に安定で加えてダイヤモンドとは異なり、鉄
族金属に対する耐性にもすぐれていることから切削工具
、耐摩工具などの工具材料、さらにはヒートシンクなど
の電子材料として用いられる立方晶窒化硼素を気相より
基材表面に析出させる方法に関するものである。[Detailed description of the invention] Industrial application field> This invention relates to a method for synthesizing highly hard cubic boron nitride. Specifically, it not only has very high hardness, but also has high thermal conductivity and chemical resistance. In addition, unlike diamond, cubic boron nitride is used as tool materials such as cutting tools and wear-resistant tools, as well as electronic materials such as heat sinks because it has excellent resistance to iron group metals. This relates to a method of depositing on the surface of a substrate.
〈従来の技術〉
従来、窒化硼素の製造法としては、
（１１ｉＩ素を含有する燕発源から基体上に硼素分子を
蒸着させるとともに、少なくとも窒素を含むイオン種を
発生せしめるイオン発生源から基体上に該イオン種を照
射して、該基体上に窒化硼素を析出せしめる窒化硼素膜
の製造方法（特公昭６０−１８１２６２号公報）。<Prior Art> Conventionally, boron nitride has been produced by depositing boron molecules onto a substrate from a swallow source containing 11iI element, and depositing boron molecules onto the substrate from an ion source that generates ionic species containing at least nitrogen. A method for producing a boron nitride film (Japanese Patent Publication No. Sho 60-181262), in which boron nitride is deposited on the substrate by irradiating the ion species with the ion species.
１２３ Ｎ２ ＋ Ｎ２プラズマによる硼素の化学輸
送を行なうことによって立方晶窒化硼素を生成させる方
法（ｊｏｕｒｎａｌ ｏｆ ｍａｔｅｒｉａｌ ５ｃｉ
ｅｎｃｅ １ｅｔｔｅｒｓ ４、（１９８５） 、ｐ５
１〜５４）。123 Method of producing cubic boron nitride by chemical transport of boron by N2 + N2 plasma (journal of material 5ci
ence 1etters 4, (1985), p5
1-54).
ｆ３１ ＨＣＤ ｇｕｎで力木を蒸発させながら、Ｈ
ｏｌｌｏｗＡｎｏｄｅからＮ２をイオン化して基板に放
射し、基板には高周波を印加して５ｅｌｆ ｂｉａｓ効
果をもたせて立方晶窒化硼素を生成する方法
（Ｐｒｏｃｅｅｄｉｎｇ、 ９ ｔｈ ５ｙｉｐｏｓｉ
ｕｎ ｏｎ Ｉｏｎ ５ｏｕｒｃｅＩｏｎ Ａｓ１ｓ
ｔｅｄ Ｔｅｃｈｎｏｌｏｇｙ Ａｎｏｄｅ ８
５ 、 Ｔｏｋｙ。While vaporizing the strength wood with f31 HCD gun, H
A method of generating cubic boron nitride by ionizing N2 from the hollowAnode and emitting it to the substrate, and applying high frequency to the substrate to have a 5elf bias effect (Proceeding, 9th 5yiposi)
un on Ion 5sourceIon As1s
ted Technology Anode 8
5, Tokyo.
（１９８５））。(1985)).
（４）硼素原子含有固体にＥＢを当てることにより、硼
素を蒸発させ、それに窒素原子含有ガスを流し込み、理
水１＞よび窒素を同時にイオン化することにより、基材
表面に立方晶窒化硼素を生成する方法（真空、第２８巻
、第７号、１９８５）。(4) Boron is evaporated by applying EB to a solid containing boron atoms, and a gas containing nitrogen atoms is poured into it, and cubic boron nitride is generated on the surface of the substrate by simultaneously ionizing water and nitrogen. (Vacuum, Vol. 28, No. 7, 1985).
などが知られている。etc. are known.
〈発明が解決しようとする問題点〉
しかしながら上記（１）の方法はイオンビームを発生す
る装置および集束装置が高価であることが欠点とされ、
（２）の方法は高出力のＲＦプラズマを成躾に利用して
いることにより、反応系からの不純物が混入しやすい。<Problems to be Solved by the Invention> However, the method (1) above has the disadvantage that the ion beam generating device and focusing device are expensive.
Since the method (2) uses high-power RF plasma for formation, impurities from the reaction system are likely to be mixed in.
（３）の方法は（１）の方法と同じくイオンビームを発
生する装置およびその集束装置が高価であることと、不
活性ガスの原子が析出した窒化硼素に取り込まれる欠点
がある。また（４）の方法においては、ＴｎｉＡは融点
と沸点が近いため、ＥＢを当てることにより、突沸しや
すく制御が困難であるという欠点を有しているのである
。Method (3), like method (1), has the drawbacks that the ion beam generating device and its focusing device are expensive, and that inert gas atoms are incorporated into the precipitated boron nitride. In addition, in the method (4), since the melting point and boiling point of TniA are close to each other, when EB is applied, it tends to cause bumping and is difficult to control.
〈問題点を解決するための手段〉
この発明は上記した従来法の欠点を解消した窒化硼素の
合成法を得るべく検討の結果見出されたものである。<Means for Solving the Problems> The present invention was discovered as a result of studies aimed at obtaining a method for synthesizing boron nitride that eliminates the drawbacks of the conventional methods described above.
即ち、この発明は硼素原子含有ガス、窒素原子含有ガス
、および不活性ガスをマイクロ波無極放電中を通過させ
たのち、３００〜１３００℃に加熱した基板表面に導入
して立方晶窒化硼素を析出させることを特徴とする高硬
度窒化硼素の合成法を提供することを目的とするもので
ある。That is, in this invention, a boron atom-containing gas, a nitrogen atom-containing gas, and an inert gas are passed through a microwave non-polar discharge and then introduced onto a substrate surface heated to 300 to 1300°C to precipitate cubic boron nitride. The object of the present invention is to provide a method for synthesizing high hardness boron nitride, which is characterized by the following.
〈作用〉
この発明は硼素原子含有ガス、窒素原子含有ガスおよび
不活性ガスをマイクロ波無極放電に通過せしめることに
より、励起状の硼素原子含有ガス、窒素原子含有ガス、
不活性ガスを生成せしめる。<Operation> The present invention allows a boron atom-containing gas, a nitrogen atom-containing gas, and an inert gas to pass through a microwave nonpolar discharge, thereby generating excited boron atom-containing gas, nitrogen atom-containing gas,
Generates inert gas.
この励起状態の硼素原子含有ガスおよび窒素原子含有ガ
スが加熱された基板表面において互いに反応し、基板表
面上に８Ｎｌ膜を生成する。The boron atom-containing gas and the nitrogen atom-containing gas in the excited state react with each other on the heated substrate surface to form an 8Nl film on the substrate surface.
しかし、加熱した基板上においては、硼素原子と窒素原
子が互いにｓ ｐ ３結合を起すのに不十分であり、基
板表面においてＣＢＮ簿躾のみでなく、ｈ−ＢＮ膜やα
−８Ｎ膜を混在した薄膜が生成されている。そのため、
ｈ−ＢＮやα−ＢＮを除去し、ＣＡＮ膜のみを残す必要
がある。励起した不活性ガスは、膜中に混入することも
なく、また大きなエネルギーを有しているため、ＣＢＮ
のｓ ｐ３結合より弱いｈ−ＢＮのｓ ｐ ！結合、お
よびα−８ＮのＢ−Ｎ間結合を切断し、ｈ−ＢＮやα−
ＢＮを膜中より除去し、ＣＡＮのみを残すことが可能と
なり、選択エッヂング的な働きを有する。However, on a heated substrate, it is insufficient for boron atoms and nitrogen atoms to form sp3 bonds with each other, and not only CBN film but also h-BN film and α
A thin film containing -8N film was produced. Therefore,
It is necessary to remove h-BN and α-BN and leave only the CAN film. The excited inert gas does not mix into the film and has large energy, so CBN
The sp3 bond of h-BN is weaker than the sp3 bond of h-BN! bond, and the B-N bond of α-8N, resulting in h-BN and α-
It becomes possible to remove BN from the film and leave only CAN, and has a selective etching function.
硼素原子数および窒素原子数と不活性ガス原子数の比は
、０．０１ ＜ （！１１本原子数＋窒素原子数）／不
活性ガス原子数＜１００の範囲が好ましい。The ratio of the number of boron atoms and the number of nitrogen atoms to the number of inert gas atoms is preferably in the range of 0.01<(!11 atoms+number of nitrogen atoms)/number of inert gas atoms<100.
この値が０．０１より小さい時は不活性ガスの分圧が大
きくなりすぎ、窒化硼素ＮＷＡが析出しにくくなる。ま
た１００より大きくなると、不活性ガスの割合が非常に
小さいため、析出する窒化硼素薄膜中のα−ＢＮ−Ｆｈ
−８Ｎを除去するのには不足である。When this value is smaller than 0.01, the partial pressure of the inert gas becomes too large, making it difficult for boron nitride NWA to precipitate. If it exceeds 100, the proportion of inert gas is very small, so α-BN-Fh in the deposited boron nitride thin film
This is insufficient to remove -8N.
硼素原子含有ガス中の硼素原子数および窒素原子含有ガ
ス中の窒素原子数の比はＢ／Ｎ＝ ０．１〜１０の範囲
が好ましい。これはＢ／Ｎ＜０．１の時は非晶質状の窒
化硼素膜が析出されやすく、Ｂ／Ｎ〉１０の時は硼素が
過剰となり、非晶質状のｌｌＩ素が形成されやすいため
である。The ratio of the number of boron atoms in the boron atom-containing gas to the number of nitrogen atoms in the nitrogen atom-containing gas is preferably in the range of B/N=0.1 to 10. This is because when B/N<0.1, an amorphous boron nitride film is likely to be deposited, and when B/N>10, boron is excessive and amorphous llI element is likely to be formed. It is.
この発明においては、安定に放電を持続させるため、マ
イクロ波無極放電を採用するものである。In this invention, microwave non-polar discharge is employed in order to sustain stable discharge.
マイクロ波出力は１００Ｗ〜１．５ｋＷの範囲が最適で
ある。この出力が１００ｗより小さい時は不活性ガスが
α−ＢＮやｈ−ＢＮを選択除去するのにエネルギーが不
足であり、また１、５ｋｗより大きいと、励起不活性ガ
スのエネルギーが大きくなりすぎるためα−ＢＮやｈ−
ＢＮだけでなくＣＡＮをも除去してしまうおそれがあり
好ましくない。The optimum microwave output is in the range of 100W to 1.5kW. When this output is smaller than 100W, there is insufficient energy for the inert gas to selectively remove α-BN and h-BN, and when it is larger than 1.5kW, the energy of the excited inert gas becomes too large. α-BN and h-
This is not preferable since there is a risk that not only BN but also CAN will be removed.
基板温度は３００℃以下では励起硼素原子および励起窒
素原子が基板上で互いに反応するエネルギーに不足し、
また１３００℃以上では析出した立方晶窒化硼素から窒
素が抜け、非立方晶窒化硼素になりやすいため３００〜
１３００℃の範囲が好ましい。When the substrate temperature is below 300°C, there is insufficient energy for the excited boron atoms and excited nitrogen atoms to react with each other on the substrate.
In addition, at temperatures above 1,300°C, nitrogen is easily released from the precipitated cubic boron nitride, resulting in non-cubic boron nitride.
A range of 1300°C is preferred.
マイクロ波無極放電を発生する管内の圧力は放電安定を
維持するために０．０５〜４００Ｔｏｒｒの範囲が望ま
しい。The pressure inside the tube that generates microwave non-polar discharge is preferably in the range of 0.05 to 400 Torr in order to maintain discharge stability.
原料ガスのうち、硼素原子含有ガスとしてＢ、ＨいＢ
ＣＦ ｓ 、Ｂ Ｂｒ ３ 、Ｂ−Ｎ−Ｈｉ等が挙げら
れ、窒素原子含有ガスとしてＮ２、Ｎ８３等が、また不
活性ガスとしてはＨｅ、 Ｍｅ、 ｋ等が用いられる。Among the raw material gases, B and HB are used as boron atom-containing gases.
Examples include CFs, BBr3, B-N-Hi, etc. N2, N83, etc. are used as the nitrogen atom-containing gas, and He, Me, K, etc. are used as the inert gas.
なおこの発明で高硬度窒化硼素合成に際しては第１図に
概略図として示す製造装置を用いるものであり、同図に
おいて、１はｇ素原子含有ガス供給装置、２は窒素原子
含有ガス供給装置、３は不活性ガス供給８置、４はウェ
ーブガイド、５はマイクロ波発振器、６は反応室、７は
排気装置、８は基板、９は基板支持台、１０はコック、
１１は排気口である。In the present invention, when synthesizing high-hardness boron nitride, a manufacturing apparatus schematically shown in FIG. 3 is an inert gas supply 8 position, 4 is a wave guide, 5 is a microwave oscillator, 6 is a reaction chamber, 7 is an exhaust device, 8 is a substrate, 9 is a substrate support stand, 10 is a cock,
11 is an exhaust port.
〈実施例〉 以下実施例によりこの発明の詳細な説明する。<Example> The present invention will be explained in detail below with reference to Examples.
実施例１
第１図に示す製造装置を用い、基板としてモリブデン基
板を使用して原料ガスはＢ、Ｈ，、Ｎ２、ｋを夫々５ｃ
ｃ／１ｉｎ、 ５ｃｃ／１ｎ、 １０ｃｃ／ｌｉｎ流し
た。反応管内圧力は３０Ｔｏｒｒに調整し、マイクロ波
出力５００Ｗ１基板＠ ｌ１１０００℃、成膜時間は４
時間とした。Example 1 Using the manufacturing apparatus shown in Fig. 1, a molybdenum substrate was used as the substrate, and the raw material gases were 5c each of B, H, N2, and k.
The flow rates were c/1in, 5cc/1n, and 10cc/lin. The pressure inside the reaction tube was adjusted to 30 Torr, the microwave output was 500W, 1 substrate @ 11000℃, and the film formation time was 4
It was time.
その結果、基板表面に３μｍの窒化ｉｌｌ素膜を析出し
た。解析手段としてラマン分析法を用いた結果ＣＢＮの
ピークである１０５５ｃ、−１および１３１０ｃ、−１
付近に鋭いピークを検出し、立方晶窒化硼素であると同
定した。As a result, a 3 μm thick nitride ill film was deposited on the substrate surface. As a result of using Raman analysis as an analysis method, the CBN peaks were 1055c, -1 and 1310c, -1.
A sharp peak was detected in the vicinity and it was identified as cubic boron nitride.
実施例２
第１図の装置を使用した。基板としてシリコンウェハー
を使用し、原料ガスとしてＢｅＦ２、ＮＨ３、ｋを夫々
１ ＱＣＣ／ ＩＩ ｊ ｎ １３０ｃ Ｃ／ ＩＩ
ｉ ｎ Ｎ ５ ＣＣ／ Ｉｌｌ ｊ ｎＫ Ｌ／た。Example 2 The apparatus shown in FIG. 1 was used. A silicon wafer is used as the substrate, and BeF2, NH3, and k are each used as raw material gases.
i n N 5 CC/ Ill j nK L/ta.
反応管内圧力を１０Ｔｏｒｒに調整し、マイクロ波出力
８００ｗ １基板湿度を１２００℃、成膜時間は３時間
とした。The pressure inside the reaction tube was adjusted to 10 Torr, the microwave output was 800 W, the humidity per substrate was 1200° C., and the film forming time was 3 hours.
その結果、基板表面に４μ而の厚みを有する窒化硼素膜
を析出した。解析手段としてＸ線回折を用いた結果、Ｃ
ＢＮのピークである４３．２度付近に鋭いピークを検出
し、立方晶窒化硼素と同定した。As a result, a boron nitride film having a thickness of 4 μm was deposited on the surface of the substrate. As a result of using X-ray diffraction as an analytical means, C
A sharp peak was detected near 43.2 degrees, which is the peak of BN, and it was identified as cubic boron nitride.
実施例３
第１図の装置を用い、モリブデン基板を使用した。原料
ガスは不活性ガスを使用せず、Ｂ、ＮｊＨ４のみとし、
その流量は８ｃｃ／ｎｉｎとした。反応管内圧力は５０
Ｔｏｒｒに調整し、マイクロ波出力６００ｗ １基板湿
度１３００℃、成膜時間は５時間とした。Example 3 The apparatus shown in FIG. 1 was used, and a molybdenum substrate was used. The raw material gas does not use inert gas, only B and NjH4,
The flow rate was 8 cc/nin. The pressure inside the reaction tube is 50
Torr, microwave output was 600 W, 1 substrate humidity was 1300° C., and film forming time was 5 hours.
その結果、基板表面に５μｍの窒化硼素膜を析出した。As a result, a 5 μm thick boron nitride film was deposited on the substrate surface.
解析手段として×４１回折を用いた結果、ｈ−ＢＮのピ
ークである２６．７度付近に鋭いピーク、ＣＢＮのピー
クである４３．２度付近になだらかなピークを検出し、
ＣＢＮとｈ−ＢＮが混在し、かつｈ−ＢＮの含有率の大
きい窒化硼素膜と同定できた。As a result of using ×41 diffraction as an analytical means, we detected a sharp peak near 26.7 degrees, which is the peak of h-BN, and a gentle peak near 43.2 degrees, which is the peak of CBN.
It was identified as a boron nitride film in which CBN and h-BN were mixed and the content of h-BN was high.
実施例４
上記実施例１〜３の条件を用いてＷＣＣ超超硬合金ある
ＳＮＭＧ４３２をチップとして、該チップにコーティン
グを行ない切削テストを行なった。Example 4 Using the conditions of Examples 1 to 3 above, a cutting test was conducted using SNMG432, a WCC cemented carbide, as a chip by coating the chip.
比較としてコーティングを行なわないチップ、およびＣ
ＶＤ法を用いてｆｉｌ ２０ｇコーティングを行なった
チップの切削テストをも行なった。For comparison, chips without coating and C
A cutting test was also conducted on a chip coated with 20 g of fil using the VD method.
コーティングは何れも被覆層厚３μｍとした。All coatings had a coating layer thickness of 3 μm.
切削テスト条件は第１表に示した。また切削テストの結
果は第２表に示した。The cutting test conditions are shown in Table 1. The results of the cutting test are shown in Table 2.
第 １ 表
第 ２ 表
上表から立方晶窒化硼素を被覆層としてチップに使用し
た場合、この発明の実施例はすべて耐摩耗性にすぐれて
いることが認められた。From Table 1 and Table 2, it was found that all the examples of the present invention had excellent wear resistance when cubic boron nitride was used as a coating layer in the chip.
また、この発明の方法にて得たＣＢＮコートチップの鋳
鉄旋削における切削性能を切削速度と寿命時間との関係
で調べたところ第２図の結果を得た。また欠損までの切
削時間と！ｆｉ撃回数回数関係で調べたところ第３図の
結果を得た。Further, the cutting performance of the CBN-coated insert obtained by the method of the present invention in cast iron turning was investigated in terms of the relationship between cutting speed and life time, and the results shown in FIG. 2 were obtained. Also, the cutting time until breakage! When we investigated the relationship between the number of fi shots, we obtained the results shown in Figure 3.
〈発明の効果〉
以上説明したように、この発明は耐熱衝撃性、熱伝導性
、硬度、耐摩耗性および高温における鉄族金属に対する
耐性にもすぐれる立方晶窒化ｎ素膜を気相から析出する
新規な合成法であり、切削部材、耐摩耗部材および耐熱
部品の被覆膜として用いた場合、第２図および第３図に
示すように多大の効果を示すことが認められた。<Effects of the Invention> As explained above, the present invention provides a cubic n-nitride film that is superior in thermal shock resistance, thermal conductivity, hardness, wear resistance, and resistance to iron group metals at high temperatures by precipitating it from the gas phase. This is a novel synthesis method, and when used as a coating film for cutting members, wear-resistant members, and heat-resistant parts, it was found to have great effects as shown in FIGS. 2 and 3.
第１図はこの発明の方法で用いる製造装置の概略説明図
、第２図および第３図はこの発明の方法で得られる立方
晶窒化硼素を被覆膜としたチップの切削性能を示す図表
である。
１・・・ａ素原子含有ガス供給装置
２・・・窒素原子含有ガス供給装置
３・・・不活性ガス供給装置
５・・・マイクロ波発振器Figure 1 is a schematic illustration of the manufacturing equipment used in the method of the present invention, and Figures 2 and 3 are charts showing the cutting performance of chips coated with cubic boron nitride obtained by the method of the present invention. be. 1...A element-containing gas supply device 2...Nitrogen atom-containing gas supply device 3...Inert gas supply device 5...Microwave oscillator
Claims (3)
性ガスをマイクロ波無極放電中を通過させたのち、３０
０〜１３００℃に加熱した基板表面に導入して立方晶窒
化硼素を析出させることを特徴とする高硬度窒化硼素の
合成法。(1) After passing a boron atom-containing gas, a nitrogen atom-containing gas, and an inert gas through a microwave nonpolar discharge,
A method for synthesizing high-hardness boron nitride, which comprises introducing cubic boron nitride onto the surface of a substrate heated to 0 to 1300°C.
ガス中の窒素原子数との比をＢ／Ｎ＝０．１〜１０の範
囲として反応ガスに水素を用いない特許請求の範囲第１
項記載の高硬度窒化硼素の合成法。(2) A claim in which the ratio of the number of boron atoms in the boron atom-containing gas to the number of nitrogen atoms in the nitrogen atom-containing gas is in the range of B/N = 0.1 to 10, and hydrogen is not used as the reaction gas. 1
Synthesis method of high hardness boron nitride as described in .
の比を０、０１〜１００の範囲とする特許請求の範囲第
１項記載の高硬度窒化硼素の合成法。(3) The method for synthesizing high hardness boron nitride according to claim 1, wherein the ratio of (number of boron atoms + number of nitrogen atoms)/number of inert gas atoms is in the range of 0.01 to 100.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| JP27935986A JPS63134661A (en) | 1986-11-22 | 1986-11-22 | Method for synthesizing high hardness boron nitride |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| JP27935986A JPS63134661A (en) | 1986-11-22 | 1986-11-22 | Method for synthesizing high hardness boron nitride |
Publications (1)
| Publication Number | Publication Date |
|---|---|
| JPS63134661A true JPS63134661A (en) | 1988-06-07 |
Family
ID=17610067
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| JP27935986A Pending JPS63134661A (en) | 1986-11-22 | 1986-11-22 | Method for synthesizing high hardness boron nitride |
Country Status (1)
| Country | Link |
|---|---|
| JP (1) | JPS63134661A (en) |
Cited By (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US5463901A (en) * | 1991-09-27 | 1995-11-07 | Sumitomo Electric Industries, Ltd. | Stacked piezoelectric surface acoustic wave device with a boron nitride layer in the stack |
| FR2726834A1 (en) * | 1994-11-07 | 1996-05-15 | Neuville Stephane | Hard protective coating prodn. by PECVD or PVD process |
| WO1996014448A1 (en) * | 1994-11-07 | 1996-05-17 | Neuville Stephane | Method for depositing a hard protective coating |
-
1986
- 1986-11-22 JP JP27935986A patent/JPS63134661A/en active Pending
Cited By (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US5463901A (en) * | 1991-09-27 | 1995-11-07 | Sumitomo Electric Industries, Ltd. | Stacked piezoelectric surface acoustic wave device with a boron nitride layer in the stack |
| FR2726834A1 (en) * | 1994-11-07 | 1996-05-15 | Neuville Stephane | Hard protective coating prodn. by PECVD or PVD process |
| WO1996014448A1 (en) * | 1994-11-07 | 1996-05-17 | Neuville Stephane | Method for depositing a hard protective coating |
| US5846613A (en) * | 1994-11-07 | 1998-12-08 | Neuville; Stephane | Method for depositing a hard protective coating |
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