JPH0699144B2 - Agglomerate composed of boron, carbon and nitrogen and method for producing the same - Google Patents
Agglomerate composed of boron, carbon and nitrogen and method for producing the sameInfo
- Publication number
- JPH0699144B2 JPH0699144B2 JP63079089A JP7908988A JPH0699144B2 JP H0699144 B2 JPH0699144 B2 JP H0699144B2 JP 63079089 A JP63079089 A JP 63079089A JP 7908988 A JP7908988 A JP 7908988A JP H0699144 B2 JPH0699144 B2 JP H0699144B2
- Authority
- JP
- Japan
- Prior art keywords
- carbon
- boron
- nitrogen
- film
- substrate
- 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 - Fee Related
Links
- IJGRMHOSHXDMSA-UHFFFAOYSA-N Atomic nitrogen Chemical compound N#N IJGRMHOSHXDMSA-UHFFFAOYSA-N 0.000 title claims description 31
- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical compound [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 title claims description 29
- 229910052799 carbon Inorganic materials 0.000 title claims description 24
- 229910052796 boron Inorganic materials 0.000 title claims description 18
- ZOXJGFHDIHLPTG-UHFFFAOYSA-N Boron Chemical compound [B] ZOXJGFHDIHLPTG-UHFFFAOYSA-N 0.000 title claims description 17
- 229910052757 nitrogen Inorganic materials 0.000 title claims description 16
- 238000004519 manufacturing process Methods 0.000 title description 4
- 239000007789 gas Substances 0.000 claims description 20
- 239000000758 substrate Substances 0.000 claims description 20
- 238000006243 chemical reaction Methods 0.000 claims description 14
- 239000000463 material Substances 0.000 claims description 12
- 238000002441 X-ray diffraction Methods 0.000 claims description 6
- 229910052751 metal Inorganic materials 0.000 claims description 6
- 239000002184 metal Substances 0.000 claims description 6
- 239000012159 carrier gas Substances 0.000 claims description 4
- 238000000034 method Methods 0.000 claims description 3
- 239000010408 film Substances 0.000 description 30
- 229910052582 BN Inorganic materials 0.000 description 12
- PZNSFCLAULLKQX-UHFFFAOYSA-N Boron nitride Chemical compound N#B PZNSFCLAULLKQX-UHFFFAOYSA-N 0.000 description 12
- 239000000843 powder Substances 0.000 description 10
- PXHVJJICTQNCMI-UHFFFAOYSA-N Nickel Chemical compound [Ni] PXHVJJICTQNCMI-UHFFFAOYSA-N 0.000 description 8
- 238000005229 chemical vapour deposition Methods 0.000 description 7
- XEEYBQQBJWHFJM-UHFFFAOYSA-N Iron Chemical compound [Fe] XEEYBQQBJWHFJM-UHFFFAOYSA-N 0.000 description 6
- 230000000704 physical effect Effects 0.000 description 6
- 239000000126 substance Substances 0.000 description 6
- 238000000921 elemental analysis Methods 0.000 description 5
- 239000010453 quartz Substances 0.000 description 5
- VYPSYNLAJGMNEJ-UHFFFAOYSA-N silicon dioxide Inorganic materials O=[Si]=O VYPSYNLAJGMNEJ-UHFFFAOYSA-N 0.000 description 5
- 230000007797 corrosion Effects 0.000 description 4
- 238000005260 corrosion Methods 0.000 description 4
- 229910002804 graphite Inorganic materials 0.000 description 4
- 239000010439 graphite Substances 0.000 description 4
- 238000005259 measurement Methods 0.000 description 4
- 229910052759 nickel Inorganic materials 0.000 description 4
- 239000002994 raw material Substances 0.000 description 4
- RYGMFSIKBFXOCR-UHFFFAOYSA-N Copper Chemical compound [Cu] RYGMFSIKBFXOCR-UHFFFAOYSA-N 0.000 description 3
- 229910052802 copper Inorganic materials 0.000 description 3
- 239000010949 copper Substances 0.000 description 3
- 238000010304 firing Methods 0.000 description 3
- 229910052742 iron Inorganic materials 0.000 description 3
- 239000000203 mixture Substances 0.000 description 3
- 239000000047 product Substances 0.000 description 3
- 230000035939 shock Effects 0.000 description 3
- 238000005245 sintering Methods 0.000 description 3
- XKRFYHLGVUSROY-UHFFFAOYSA-N Argon Chemical compound [Ar] XKRFYHLGVUSROY-UHFFFAOYSA-N 0.000 description 2
- UFHFLCQGNIYNRP-UHFFFAOYSA-N Hydrogen Chemical compound [H][H] UFHFLCQGNIYNRP-UHFFFAOYSA-N 0.000 description 2
- 239000000956 alloy Substances 0.000 description 2
- 229910045601 alloy Inorganic materials 0.000 description 2
- 229910052739 hydrogen Inorganic materials 0.000 description 2
- 239000010409 thin film Substances 0.000 description 2
- 239000004215 Carbon black (E152) Substances 0.000 description 1
- 230000002411 adverse Effects 0.000 description 1
- HSFWRNGVRCDJHI-UHFFFAOYSA-N alpha-acetylene Natural products C#C HSFWRNGVRCDJHI-UHFFFAOYSA-N 0.000 description 1
- 229910052786 argon Inorganic materials 0.000 description 1
- -1 boron halide Chemical class 0.000 description 1
- 239000003054 catalyst Substances 0.000 description 1
- 239000007795 chemical reaction product Substances 0.000 description 1
- 238000009841 combustion method Methods 0.000 description 1
- 150000001875 compounds Chemical class 0.000 description 1
- 238000001816 cooling Methods 0.000 description 1
- 230000006866 deterioration Effects 0.000 description 1
- 229910001873 dinitrogen Inorganic materials 0.000 description 1
- 230000000694 effects Effects 0.000 description 1
- 125000002534 ethynyl group Chemical group [H]C#C* 0.000 description 1
- 239000000835 fiber Substances 0.000 description 1
- 238000010438 heat treatment Methods 0.000 description 1
- 229930195733 hydrocarbon Natural products 0.000 description 1
- 150000002430 hydrocarbons Chemical class 0.000 description 1
- 239000001257 hydrogen Substances 0.000 description 1
- 239000011159 matrix material Substances 0.000 description 1
- 239000011812 mixed powder Substances 0.000 description 1
- 238000002156 mixing Methods 0.000 description 1
- 230000009257 reactivity Effects 0.000 description 1
- 239000006104 solid solution Substances 0.000 description 1
- 238000002230 thermal chemical vapour deposition Methods 0.000 description 1
- 229910052723 transition metal Inorganic materials 0.000 description 1
- 150000003624 transition metals Chemical class 0.000 description 1
- 238000002834 transmittance Methods 0.000 description 1
Landscapes
- Carbon And Carbon Compounds (AREA)
Description
【発明の詳細な説明】 ［産業上の利用分野］ 本発明はホウ素、炭素、窒素からなる塊状体およびその
製造法に関し、耐熱性、化学的安定性、耐熱衝撃性等に
優れた窒化ホウ素の物性とグラファイトの耐薬品性、高
導電性等の物性を併わせ持ち、高温耐食材料、導電性耐
食材料等として各種用途に供すことのできるものであ
る。TECHNICAL FIELD The present invention relates to an agglomerate composed of boron, carbon, and nitrogen, and a method for producing the same, and relates to a boron nitride excellent in heat resistance, chemical stability, thermal shock resistance, and the like. It has both physical properties and chemical resistance of graphite, high electrical conductivity and the like, and can be used for various applications as a high temperature corrosion resistant material, a conductive corrosion resistant material and the like.
［従来技術］ 窒化ホウ素は耐熱性、化学的安定性、耐熱衝撃性等には
優れているものの導電性等が劣り、用途によってはこれ
らの物性を併わせ持つものが要求されているにもかかわ
らず、満足できるものが得られていないのが現状であ
る。窒化ホウ素粉末に炭素粉末を添加混合し、焼結によ
り導電性を有する窒化ホウ素物品を得る方法も考えられ
るが、このような例は報告されたことがなく、また、窒
化ホウ素は焼結しにくい材料であり、各種の焼結助剤を
添加する必要があり、物性の低下が避けられない等の問
題がある。また、化学気相析出法（以下CVD法という）
によりホウ素、炭素、窒素からなる均一物を得る試みも
おこなわれており、例えばA.R.Badzinら（Proc.Int.Con
f.Chem.Vap.Dep.3rd.1972,747〜753）はBCl3、CCl3、N2、H
2を用い、CVD法により得ているが、生成物は粉状で得ら
れる。一般にCVD炉内では温度勾配があり、異なった生
成温度域では組成の異なった粉末が生成するため、得ら
れる粉体は組成の異なった粉の混合物となるため、均質
さが要求されるような用途には供すことができず、ま
た、これらの粉は非常に成形するのが困難であり、実用
に供すことができないものであった。[Prior Art] Boron nitride is excellent in heat resistance, chemical stability, thermal shock resistance, etc., but is inferior in conductivity etc., and although it is required to have both of these physical properties depending on the application. The current situation is that no satisfactory product has been obtained. A method of adding carbon powder to boron nitride powder and mixing and obtaining a boron nitride article having conductivity by sintering is also conceivable, but such an example has not been reported, and boron nitride is difficult to sinter. Since it is a material, it is necessary to add various sintering aids, and there is a problem in that the deterioration of physical properties cannot be avoided. In addition, chemical vapor deposition method (hereinafter referred to as CVD method)
Attempts have also been made to obtain a uniform product of boron, carbon, and nitrogen by, for example, ARBadzin et al. (Proc. Int. Con.
f.Chem.Vap.Dep.3rd.1972,747~753) is BCl 3, CCl 3, N 2 , H
2 is obtained by the CVD method, but the product is obtained in powder form. Generally, there is a temperature gradient in the CVD furnace, and powders with different compositions are produced in different production temperature regions, so the obtained powder is a mixture of powders with different compositions, so homogeneity is required. It could not be put to practical use, and these powders were very difficult to mold and could not be put to practical use.
［問題点を解決するための手段］ 本発明者らは、かかる従来の問題点に鑑み、鋭意検討の
結果、CVD法において、基体として特定の材料を選ぶこ
とにより、ホウ素、炭素、窒素からなる均一な塊状物を
得ることに成功し、本発明に至ったものである。[Means for Solving Problems] The inventors of the present invention have made earnest studies in view of the problems of the related art, and as a result, in the CVD method, by selecting a specific material as a substrate, boron, carbon, and nitrogen are formed. The present invention has been succeeded in obtaining a uniform lump.
すなわち本発明は、本質的にホウ素、炭素、窒素からな
り、CuKα線によるＸ線回折測定による２θが20〜30°
の範囲に回折ピークを有することを特徴とする塊状体で
あり、その製造法は、ホウ素源ガス、炭素源ガス、窒素
源ガスおよびキャリャーガスからなる混合ガスを金属基
体を保持した反応容器内に導入して反応させ、基体上に
本質的にホウ素、炭素、窒素からなり、CuKα線による
Ｘ線回折測定による２θが20〜30°の範囲に回折ピーク
を有する塊状体を形成する方法である。本発明の塊状物
は窒化ホウ素と炭素の固溶体であるか、窒化ホウ素マト
リックス中に炭素が均一に分散した連続相からなるもの
であるのかは定かでないところであるが、いずれにして
も連続相となっているのが特徴であり、窒化ホウ素と炭
素との混合粉末を焼結したものとは全く異なるものであ
る。また、本発明の塊状物は本質的にホウ素、炭素、窒
素からなるものであるが、原料ガスに由来する水素が含
まれるるものとなる。ホウ素、炭素、窒素の比は原子比
でホウ素、窒素はほぼ1:1であり、残部が炭素である。
炭素量は特に制限されないが、導電性を付与するために
は実用上0.1％（重量）以上が好ましく、また、炭素含
有量があまりに大きくなりすぎると窒化ホウ素の物性が
十分に発揮されないため、80％（重量）以下が好まし
い。That is, the present invention consists essentially of boron, carbon, and nitrogen, and has a 2θ of 20 to 30 ° measured by X-ray diffraction using CuKα ray.
It is a lump that is characterized by having a diffraction peak in the range of, and its manufacturing method is to introduce a mixed gas consisting of a boron source gas, a carbon source gas, a nitrogen source gas and a carrier gas into a reaction vessel holding a metal substrate. And reacting on the substrate to form a lump consisting essentially of boron, carbon and nitrogen, which has a diffraction peak in the range of 20 to 30 ° in 2θ by X-ray diffraction measurement by CuKα ray. It is not clear whether the agglomerates of the present invention are a solid solution of boron nitride and carbon, or consist of a continuous phase in which carbon is uniformly dispersed in a boron nitride matrix, but in any case it becomes a continuous phase. The feature is that it is completely different from the one obtained by sintering a mixed powder of boron nitride and carbon. Further, the agglomerate of the present invention essentially consists of boron, carbon and nitrogen, but it also contains hydrogen derived from the raw material gas. The atomic ratio of boron, carbon, and nitrogen is about 1: 1 for boron and nitrogen, and the balance is carbon.
The amount of carbon is not particularly limited, but 0.1% (by weight) or more is preferable for practical use in order to impart conductivity, and since the physical properties of boron nitride are not sufficiently exhibited when the carbon content becomes too large, 80 % (Weight) or less is preferable.
かかる本発明の塊状物はCVD法において特定の基体を選
ぶことによりはじめて得られるものであり、基体として
は、金属、特に遷移金属が好ましく銅、ニッケル等およ
びこれらの合金が挙げられる。合金のうち鉄を含むもの
は塊状物形成には有効であるものの、鉄分が塊状物へ移
行する傾向があるため、鉄分の存在により悪影響を受け
るような用途の場合には使用を避けるべきである。基体
として、CVD法においてはグラファイト、石英が、用い
られるが、グラファイトの場合、得られる化合物は全く
膜状態となることがなく、粉末物質しか得られない。ま
た石英の場合には、反応の初期において、極めて薄い膜
が該基体上に生成するが、せいぜい１μｍ程度の厚みし
かなく、これ以上厚み方向へ成長することなく、反応生
成物は粉体として得られる。The agglomerate of the present invention can be obtained only by selecting a specific substrate in the CVD method, and the substrate is preferably a metal, particularly a transition metal, preferably copper, nickel or the like and alloys thereof. Although alloys containing iron are effective in forming lumps, iron tends to migrate to lumps, so use should be avoided in applications where the presence of iron is adversely affected. . As the substrate, graphite and quartz are used in the CVD method, but in the case of graphite, the obtained compound does not form a film at all, and only a powder substance is obtained. In the case of quartz, an extremely thin film is formed on the substrate at the initial stage of the reaction, but it has a thickness of at most about 1 μm, and the reaction product is obtained as powder without further growth in the thickness direction. To be
このように従来においても石英基板を用いることによ
り、基体上に極めて薄い膜を形成することは可能であっ
たが、10μｍ以上もの厚みのある塊状物と呼べるものは
得られない。また、石英基体からの剥離が困難であり、
独立膜とすることができないため、この材料をさらに、
他の材料の表面に適用して、表面物性の改善を図るとい
う、この種の材料に要求される使用法が適用できないも
のであった。これに対し、本発明によれば、10μｍ以上
の均一連続相からなる塊状物が容易に得られるものであ
る。金属、特に銅あるいはニッケル系の材料が本発明に
おいて特異的に優れている理由は必ずしも定かではない
が、これらの材料が触媒的な作用をし、厚み方向への成
長が図られるものと考えられる。As described above, it has been possible to form an extremely thin film on a substrate by using a quartz substrate in the related art, but it is not possible to obtain a lump that has a thickness of 10 μm or more. Also, it is difficult to peel from the quartz substrate,
This material is further
The usage required for this type of material, which is to apply it to the surface of another material to improve the physical properties of the surface, cannot be applied. On the other hand, according to the present invention, a lump comprising a uniform continuous phase of 10 μm or more can be easily obtained. The reason why the metal, particularly copper or nickel-based material is specifically excellent in the present invention is not always clear, but it is considered that these materials act as a catalyst and grow in the thickness direction. .
本発明で用いる原料ガスとしては、特に限定されない
が、ホウ素源としてBCl3等のハロゲン化ホウ素、窒素源
としてはNH3等の反応性の高いガスが好ましく、炭素源
としては、炭化水素、特に不飽和結合を有するガスが好
ましく、反応性等からアセチレンが最も好ましい。ま
た、均一な膜を効率よく、且つ再現性よく得るために
は、これら原料ガスに加えてキャリャーガスの使用が好
ましく、水素ガス、アルゴン等を用いることができる。
また、これら原料ガスの量的関係については特に制限さ
れないが、ホウ素源ガスと窒素源ガスは少なくとも原子
比で、1:2以上が好ましい。これ以下ではホウ素源ガス
としてBCl3を用いた場合、膜中にC1が残る等の不都合が
ある。The raw material gas used in the present invention is not particularly limited, but a boron halide such as BCl 3 as a boron source, a highly reactive gas such as NH 3 as a nitrogen source is preferable, and a hydrocarbon is particularly preferable as a carbon source. A gas having an unsaturated bond is preferable, and acetylene is most preferable because of reactivity and the like. Further, in order to obtain a uniform film efficiently and with good reproducibility, it is preferable to use a carrier gas in addition to these raw material gases, and hydrogen gas, argon or the like can be used.
The quantitative relationship of these source gases is not particularly limited, but the boron source gas and the nitrogen source gas are preferably at least 1: 2 in atomic ratio. Below this, when BCl 3 is used as the boron source gas, there is an inconvenience such as C 1 remaining in the film.
また、炭素源の量は大きくすればするほど生成膜の炭素
量が増大するが、ホウ素源に対して原子比で６倍以上と
なると、粉体が生成しやすくなり、このましくない。本
発明においては大気圧下での反応が好ましい。減圧下で
は、連続状の膜が得られにくく、粉末あるいは繊維（ウ
ィスカー状）が得られるため、500mmHgより大とするこ
とが好ましい。Further, as the amount of carbon source increases, the amount of carbon in the produced film increases, but when the atomic ratio is 6 times or more that of the boron source, powder is likely to be produced, which is not preferable. In the present invention, the reaction under atmospheric pressure is preferable. Under reduced pressure, it is difficult to obtain a continuous film, and powder or fibers (whiskers) are obtained.
反応温度は特に限定的ではないが、600℃以上が好まし
い。これ以下では反応速度が極端に小さくなる。反応速
度の面からは反応温度は高い方が好ましいが、本発明に
おいては、基体として金属を用いており、この金属の耐
熱温度に依存し、1200℃程度以下での反応が推奨され
る。The reaction temperature is not particularly limited, but is preferably 600 ° C or higher. Below this, the reaction rate becomes extremely low. From the viewpoint of reaction rate, it is preferable that the reaction temperature is high, but in the present invention, a metal is used as the substrate, and a reaction at about 1200 ° C. or lower is recommended depending on the heat resistant temperature of the metal.
本発明の塊状物は少量の炭素量で、導電性を飛躍的に向
上させることができ、例えば、窒化ホウ素単体では、そ
の比抵抗は1013Ωcm程度であるのに対して、重量基準で
１％程度炭素が存在するものでは105Ωcm程度である。The agglomerate of the present invention can remarkably improve the conductivity with a small amount of carbon. For example, the specific resistance of boron nitride alone is about 10 13 Ωcm, whereas it is 1 by weight. When carbon is present in about%, it is about 10 5 Ωcm.
以下、実施例により本発明を具体的に説明する。Hereinafter, the present invention will be specifically described with reference to examples.
実施例１ 内径40mm長さ1000mmの石英管からなる熱CVD装置の中央
に500mm×20mm×3mmの銅基板を設置し、BCl3、C2H2およ
びNH3を原料とし、H2をキャリャーガスとして、反応管
中央を750℃に加熱した炉内に導入した。それぞれのガ
ス流量は次のとおりである。Example 1 A 500 mm × 20 mm × 3 mm copper substrate was placed in the center of a thermal CVD apparatus consisting of a quartz tube having an inner diameter of 40 mm and a length of 1000 mm, and BCl 3 , C 2 H 2 and NH 3 were used as raw materials, and H 2 was used as a carrier gas. The reaction tube was introduced into the furnace whose center was heated to 750 ° C. The respective gas flow rates are as follows.
BCl3 15cc/min NH3 30cc/min C2H2 8cc/min H2 144cc/min 炉内圧力は大気圧でおこなった。BCl 3 15cc / min NH 3 30cc / min C 2 H 2 8cc / min H 2 144cc / min The furnace pressure was atmospheric pressure.
以上の条件で６時間反応をおこなったのち、ガス導入と
基板加熱をやめ、炉内を真空排気、冷却した。基板上に
は、全幅（20mm）にわたり、ガス導入側より約50mm、の
範囲で膜が形成された。冷却により基板上の膜は簡単に
剥離し、得られた膜は黒色〜茶かっ色であり、厚さ約0.
3mmの膜であり、自由に取り扱える程度の強度を有して
いた。この膜（生成膜）の元素分析の結果および比抵抗
の測定結果を第１表に示した。After reacting for 6 hours under the above conditions, gas introduction and substrate heating were stopped, and the inside of the furnace was evacuated and cooled. A film was formed on the substrate over the entire width (20 mm) within a range of about 50 mm from the gas introduction side. Upon cooling, the film on the substrate was easily peeled off, the resulting film was black to brownish brown and had a thickness of about 0.
It was a film with a thickness of 3 mm and had a strength that could be handled freely. Table 1 shows the results of elemental analysis and the measurement results of specific resistance of this film (generated film).
また、生成膜を窒素ガス中2000℃で１時間熱処理し（焼
成膜）、元素分析、比抵抗の測定をおこない、結果を第
１表に示した。生成膜と焼成膜とをCuKα線によるＸ線
回折測定をおこない、この回折パターンを第１図（生成
膜）、第２図（焼成膜）に示した。第１図において、２
θが20〜30℃においてブロードなピークを有し、無定形
BNと無定形Ｃの002の回折ピークが重なりあったもので
ある。この生成膜は、結晶化度が低く、ブロードなパタ
ーンとなることが特徴であり、窒化ホウ素、炭素の粉末
由来のものと明確に区別できる。生成膜を焼成して得た
膜は第２図に示したとおり、２θが26°においてBNとＣ
の002の回折ピークが重なりあったピークとなるが、こ
れはｈ−BN、ｈ−Ｃの002の回折ピーク（２θが26.5
°）よりも低角度であることが特徴であり、焼成によっ
ても回折ピークが顕著には鋭くならないものである。な
お、元素分析において、Ｃ、Ｈ、Ｎは燃焼法により、Ｂ
はアルカリ分解させたのちICPにより定量分析をおこな
った。Further, the produced film was heat-treated in nitrogen gas at 2000 ° C. for 1 hour (baked film), elemental analysis and measurement of specific resistance were performed, and the results are shown in Table 1. The produced film and the fired film were subjected to X-ray diffraction measurement by CuKα ray, and the diffraction patterns are shown in FIG. 1 (generated film) and FIG. 2 (fired film). In FIG. 1, 2
Amorphous with a broad peak at θ of 20 to 30 ° C
The BN and amorphous 002 diffraction peaks overlap each other. This produced film is characterized by having a low crystallinity and a broad pattern, and can be clearly distinguished from those derived from boron nitride and carbon powder. As shown in Fig. 2, the film obtained by firing the formed film was BN and C at 2θ of 26 °.
The 002 diffraction peak of No. 002 is an overlapping peak. This is the 002 diffraction peak of h-BN and hC (2θ is 26.5
The angle is smaller than the angle (°), and the diffraction peak does not become sharply sharp even by firing. In the elemental analysis, C, H, and N were measured by the combustion method to obtain B.
Was alkali-decomposed and then quantitatively analyzed by ICP.
実施例２ 基板として、ニッケルを用い、反応温度を800℃とした
以外は実施例１と同様にして、反応をおこなった。この
結果、淡褐色で透光性を有する約0.1mmの厚みの膜（20m
m×40mm）を得た。Example 2 A reaction was performed in the same manner as in Example 1 except that nickel was used as the substrate and the reaction temperature was 800 ° C. As a result, a light brown, translucent film with a thickness of about 0.1 mm (20 m
m × 40 mm) was obtained.
実施例１と同様にして膜の元素分析、比抵抗の測定をお
こなった。この結果を第１表に示した。In the same manner as in Example 1, the elemental analysis of the film and the measurement of the specific resistance were performed. The results are shown in Table 1.
なお、4000cm-1における透過率を測定したところ約50％
であった。The transmittance at 4000 cm -1 was about 50%.
Met.
実施例３ 基板として、ニッケルを用い、基板温度を650℃とした
以外は実施例１と同様にして、反応をおこなった。この
結果、黒色で約1mmの厚みの膜（20mm×60mm）を得た。
実施例１と同様にして元素分析、比抵抗の測定をおこな
った。この結果を第１表に示した。また、Ｘ線回折測定
をおこない、その回折パターンを第３図（生成膜）、第
４図（焼成膜）に示した。Example 3 A reaction was performed in the same manner as in Example 1 except that nickel was used as the substrate and the substrate temperature was 650 ° C. As a result, a black film (20 mm × 60 mm) having a thickness of about 1 mm was obtained.
Elemental analysis and measurement of specific resistance were performed in the same manner as in Example 1. The results are shown in Table 1. Further, X-ray diffraction measurement was carried out, and the diffraction patterns thereof are shown in FIG. 3 (generation film) and FIG. 4 (baked film).
実施例１の膜（第１図）、（第２図）と同様のことがい
え、特に焼成によっても２θが42.5°におけるBNとＣの
10に相当する回折ピークはほとんどシャープにならない
ものであった。The same can be said for the films of Example 1 (Fig. 1) and (Fig. 2), and in particular, BN and C at 2θ of 42.5 ° were also obtained by firing.
The diffraction peak corresponding to 10 was almost not sharp.
［発明の効果］ 本発明の塊状物は、耐熱性、化学的安定性、耐熱衝撃性
等に優れた窒化ホウ素の物性とグラファイトの耐薬品
性、高導電性等の物性を併わせ持つものであり、高温耐
食材料、導電性耐食材料等として各種用途に供すことの
できるものであり、CVD法により容易に得られるもので
ある。 [Effects of the Invention] The lump of the present invention has physical properties of boron nitride excellent in heat resistance, chemical stability, thermal shock resistance and the like, chemical properties of graphite, and high electrical conductivity. Therefore, it can be used for various purposes as a high temperature corrosion resistant material, a conductive corrosion resistant material, etc., and can be easily obtained by the CVD method.
第１図、第２図、第３図および第４図は、それぞれ実施
例１の生成膜、焼成膜、実施例３の生成膜、焼成膜のＸ
線回折パターンを示すものである。1, FIG. 2, FIG. 3 and FIG. 4 show X of the produced film of Example 1, the fired film, the produced film of Example 3, and the fired film, respectively.
It shows a line diffraction pattern.
Claims (2)
Kα線によるＸ線回折測定による２θが20〜30°の範囲
に回折ピークを有することを特徴とする塊状体。1. A material consisting essentially of boron, carbon, nitrogen, Cu
An agglomerate characterized by having a diffraction peak in the range of 20 to 30 at 2θ by X-ray diffraction measurement by Kα ray.
よびキャリャーガスからなる混合ガスを金属基体を保持
した反応容器内に導入して反応させ、基体上に本質的に
ホウ素、炭素、窒素からなり、CuKα線によるＸ線回折
測定による２θが20〜30°の範囲に回折ピークを有する
塊状体を形成する方法。2. A mixed gas consisting of a boron source gas, a carbon source gas, a nitrogen source gas and a carrier gas is introduced into a reaction vessel holding a metal substrate to cause a reaction, and essentially boron, carbon and nitrogen are introduced onto the substrate. And a method of forming a lump having a diffraction peak in the range of 2θ of 20 to 30 ° by X-ray diffraction measurement using CuKα ray.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| JP63079089A JPH0699144B2 (en) | 1988-03-31 | 1988-03-31 | Agglomerate composed of boron, carbon and nitrogen and method for producing the same |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| JP63079089A JPH0699144B2 (en) | 1988-03-31 | 1988-03-31 | Agglomerate composed of boron, carbon and nitrogen and method for producing the same |
Publications (2)
| Publication Number | Publication Date |
|---|---|
| JPH01252519A JPH01252519A (en) | 1989-10-09 |
| JPH0699144B2 true JPH0699144B2 (en) | 1994-12-07 |
Family
ID=13680155
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| JP63079089A Expired - Fee Related JPH0699144B2 (en) | 1988-03-31 | 1988-03-31 | Agglomerate composed of boron, carbon and nitrogen and method for producing the same |
Country Status (1)
| Country | Link |
|---|---|
| JP (1) | JPH0699144B2 (en) |
Families Citing this family (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| JP3346496B2 (en) * | 1992-11-06 | 2002-11-18 | 独立行政法人産業技術総合研究所 | Polycrystalline BCN material and method for producing the same |
| US6759128B1 (en) * | 2002-07-05 | 2004-07-06 | The Regents Of The University Of California | Bulk superhard B-C-N nanocomposite compact and method for preparing thereof |
| JP5804852B2 (en) * | 2011-09-01 | 2015-11-04 | 電気化学工業株式会社 | Mixture of hexagonal boron nitride and hexagonal boron carbonitride, method for producing the same and composition |
-
1988
- 1988-03-31 JP JP63079089A patent/JPH0699144B2/en not_active Expired - Fee Related
Also Published As
| Publication number | Publication date |
|---|---|
| JPH01252519A (en) | 1989-10-09 |
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