JPH03215309A - Boron carbide fine particle manufacturing method - Google Patents
Boron carbide fine particle manufacturing methodInfo
- Publication number
- JPH03215309A JPH03215309A JP2006562A JP656290A JPH03215309A JP H03215309 A JPH03215309 A JP H03215309A JP 2006562 A JP2006562 A JP 2006562A JP 656290 A JP656290 A JP 656290A JP H03215309 A JPH03215309 A JP H03215309A
- Authority
- JP
- Japan
- Prior art keywords
- fine particles
- reaction
- particle size
- laser
- 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.)
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Classifications
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- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01B—NON-METALLIC ELEMENTS; COMPOUNDS THEREOF; METALLOIDS OR COMPOUNDS THEREOF NOT COVERED BY SUBCLASS C01C
- C01B32/00—Carbon; Compounds thereof
- C01B32/90—Carbides
- C01B32/914—Carbides of single elements
- C01B32/991—Boron carbide
-
- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01P—INDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS
- C01P2002/00—Crystal-structural characteristics
- C01P2002/80—Crystal-structural characteristics defined by measured data other than those specified in group C01P2002/70
- C01P2002/82—Crystal-structural characteristics defined by measured data other than those specified in group C01P2002/70 by IR- or Raman-data
-
- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01P—INDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS
- C01P2004/00—Particle morphology
- C01P2004/51—Particles with a specific particle size distribution
-
- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01P—INDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS
- C01P2004/00—Particle morphology
- C01P2004/60—Particles characterised by their size
- C01P2004/61—Micrometer sized, i.e. from 1-100 micrometer
-
- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01P—INDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS
- C01P2004/00—Particle morphology
- C01P2004/60—Particles characterised by their size
- C01P2004/62—Submicrometer sized, i.e. from 0.1-1 micrometer
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- Chemical & Material Sciences (AREA)
- Organic Chemistry (AREA)
- Inorganic Chemistry (AREA)
- Physical Or Chemical Processes And Apparatus (AREA)
- Carbon And Carbon Compounds (AREA)
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】
（産業上の利用分野）
本発明は、レーザーによる炭化ホウ素（以下、Ｂ．Ｃ
と言う）微粒子の製造に係わり、詳しくは、ガスブレー
クダウンを利用したレーザーによるＢ．Ｃ微粒子の製造
方法に関する。DETAILED DESCRIPTION OF THE INVENTION (Industrial Field of Application) The present invention is directed to the production of boron carbide (hereinafter referred to as B.C.
Regarding the production of microparticles (B. The present invention relates to a method for producing C fine particles.
（従来技術）
一般に物質の粒径が１μｍ（原子数にして１０１０個）
以下のものは微粒子と呼ばれ、焼結原料、触媒、生物工
学等の用途に用いられる新素材として関心がもたれてい
る。この場合、用いられる微粒子に望ましい条件は、化
学的純度が高いこと、球状かつ粒径が小さいこと、粒径
が均一であること等である。このような微粒子の製造方
法としては、固相反応法、液相反応法、気相反応法等が
あるが、上配の条件に適合した微粒子の製造方法として
は気相反応法が最適である。(Prior art) Generally, the particle size of a substance is 1 μm (1010 atoms)
The following are called fine particles and are of interest as new materials for use in applications such as sintering raw materials, catalysts, and biotechnology. In this case, desirable conditions for the fine particles used include high chemical purity, spherical shape and small particle size, and uniform particle size. There are solid phase reaction methods, liquid phase reaction methods, gas phase reaction methods, etc. for producing such fine particles, but the gas phase reaction method is the most suitable method for producing fine particles that meet the above conditions. .
従来、気相反応法とレーザー誘起反応とを組み合わせた
微粒子生成法〔セラミックス：１９（１９８４）、Ｎα
６ ｐ４８２）により、ＳｔｓＳｉＣＳＳｉｓＮｉの
微粒子が得られていた。Conventionally, a fine particle generation method combining a gas phase reaction method and a laser-induced reaction [Ceramics: 19 (1984), Nα
6 p482), fine particles of StsSiCSSisNi were obtained.
一方、本発明者等は、上記の００２レーザーの熱反応法
に代わって、気体の誘電破壊（ガスブレークダウン）、
すなわち、パルス発振レーザーを基体に照射するとレー
ザー光の時間的、空間的な高輝度のために生じる現象を
利用した微粒子生成方法を見い出し、既に、特開平１−
２５２５１５号：炭化ケイ素の微粒子製造方法、特開平
１一２５２５１７号：ホウ素の微粒子製造方法、特開平
１−２５２５１８号：チタン化ホウ素の微粒子製造方法
を提案した。特に、ホウ素（Ｂ）の微粒子製造方法の場
合には、原料気体にハロゲン化ホウ素ＢＸ３ （Ｘ＝Ｆ
ＳＣｌｌＳＢｒ）及び水素の混合気体を用い、
Ｂ Ｘ ｓ ＋ Ｈ ２→Ｂ＋ＨＸ−！−ＢＨＸ２の反
応により平均粒子が０．０８μｍのホウ素の微粒子を製
造するものであり、また、チタン化ホウ素（ＴＩＢ２）
の場合には、原料気体にＴｉｉ４とハロゲン化ホウ素Ｂ
Ｘ．（Ｘ＝ＦＳＣｌ、Ｂｒ）を用い、
ＴｉＣＬ＋ ２ ＢＸ３＋ ５ Ｈ２→ＴＩＢ２＋ １
０ ＨＸの反応により平均粒子が０．１６μｍのチタ
ン化ホウ素の微粒子を製造するものであった。On the other hand, the present inventors have developed a method using gas dielectric breakdown (gas breakdown) instead of the thermal reaction method of the 002 laser described above.
That is, we have discovered a method of generating fine particles that utilizes the phenomenon that occurs due to the temporal and spatial high brightness of laser light when a substrate is irradiated with a pulsed laser, and has already published a method for generating fine particles in Japanese Patent Application Laid-Open No.
No. 252515: A method for producing fine particles of silicon carbide, JP-A-1-252517: A method for producing fine particles of boron, and JP-A-1-252518: A method for producing fine particles of boron titanide. In particular, in the case of the method for producing fine particles of boron (B), boron halide BX3 (X=F
SCllSBr) and hydrogen, B X s + H 2 → B + HX-! - Boron fine particles with an average particle size of 0.08 μm are produced by the reaction of BHX2, and boron titanide (TIB2)
In the case of , Tii4 and boron halide B are added to the raw material gas.
X. Using (X=FSCl, Br), TiCL+ 2 BX3+ 5 H2→TIB2+ 1
By the reaction of 0 HX, fine particles of boron titanide having an average particle size of 0.16 μm were produced.
（発明が解決しようとする課題）
上記方法の特長は次のようなものである。（１）照射光
の波長領域に吸収帯を有しない物質も原料として用いる
ことができる。（２）光の吸収効率が良い。(Problems to be Solved by the Invention) The features of the above method are as follows. (1) Substances that do not have an absorption band in the wavelength region of the irradiated light can also be used as raw materials. (2) Good light absorption efficiency.
（３）揉作圧が高く、反応は連鎖的なので収量が多い。(3) The cropping pressure is high and the reaction is chain-like, so the yield is high.
（４）器壁からの不純物の混入がない。（５）常温の反
応容器で高融点物質が得られる。（６）粒径分布の狭い
微粒子が得られる。（７）反応装置が単純で容易に行う
ことができる。(4) There is no contamination of impurities from the vessel wall. (5) A high melting point substance can be obtained in a reaction vessel at room temperature. (6) Fine particles with a narrow particle size distribution can be obtained. (7) The reaction apparatus is simple and the reaction can be carried out easily.
本発明は、選択された原料気体を用いて、上記のような
特長を有するレーザーによるブレークダウンを利用して
Ｂ．Ｃ の微粒子を製造する方法を提供することを目的
とする。The present invention utilizes selected raw material gases and laser breakdown having the above-mentioned features to produce B.I. An object of the present invention is to provide a method for producing C fine particles.
（課題を解決するための手段）
上記の課題は、ハロゲン化ホウ素、炭化水素、及び水素
とを含む混合気体、またはハロゲン化ホウ素、四塩化炭
素、及び水素を含む混合気体にパルス発振Ｃ Ｏ ２
レーザー光を照射して、ガスプレークダウン現象により
炭化ホウ素の微粒子を生成する本方法によって達成する
ことができる。(Means for Solving the Problem) The above problem is achieved by applying pulse oscillation CO2 to a mixed gas containing a boron halide, a hydrocarbon, and hydrogen, or a mixed gas containing a boron halide, carbon tetrachloride, and hydrogen.
This can be achieved by the present method in which fine particles of boron carbide are generated by irradiation with laser light and a gas breakdown phenomenon.
（作 用） 以下に本発明を詳しく説明する。(for production) The present invention will be explained in detail below.
粒径の揃った特性の良い微粒子の製法としては、気体原
料を用いた気相法が適しているが、Ｂ．Ｃの気体原料と
して、ハロゲン化ホウ＊ Ｂ Ｘ ｓＣＸ＝ＦＸＣｌ、
Ｂｒ，■〕、炭化水素Ｃ．Ｈ．、水素Ｈ２から成る混合
気体、またはハロゲン化ホウ素ＢＸ３、四塩化炭素ＣＩ
Ｊ．、水素Ｈ２から成る混合気体を用いる。ここで、炭
化水素Ｃ．Ｈ．とは、鎮式炭化水素であるＣ ． Ｈ
２．，。２、Ｃ − Ｈ ２ ，，、及びＣＲＨ２１１
−２（ｎは整数）、または環式炭化水素であるＣ．Ｈ．
．，、ＣｈＨ．ｌ，−２、及びＣ＋，Ｈｚｈ−ｓ （ｎ
は整数）で表わきれる化合物である。好ましい混合気体
の範囲は、気体原料として・、ハロゲン化ホウ素、炭化
水素、及び水素Ｈ２を用いる場合には、ハロゲン化ホウ
素：炭化水素：水素の比率が（２〜１０）：ｌ： （
１００以下）であり、気体原料？して、ハロゲン化ホウ
素、四塩化炭素、及び水素を用いる場合には、ハロゲン
化ホウ素二四塩化炭素：水素の比率が（２〜１０）：ｌ
： （１００以下）である。また、これらの混合気体
の全圧は２００〜１ ０ ０ ０Ｔｏｒｒであることが
好ましい。この原料に室温でＣＯ■レーザーのパルス光
を照射すると、レーザー光の単位断面積当たりのエネル
ギー（フルエンス）が小さい場合には、レーザー光のエ
ネルギーは混合ガスにほとんど吸収されないが、ある程
度以上の強さのレーザー光の場合、原料気体内でブレー
クダウンが起こって、照射されたレーザーエネルギーの
ほとんどが吸収される。As a method for producing fine particles with uniform particle size and good properties, a gas phase method using gaseous raw materials is suitable, but B. As a gaseous raw material for C, boron halide* B X sCX=FXCl,
Br, ■], hydrocarbon C. H. , hydrogen H2, or boron halide BX3, carbon tetrachloride CI
J. , hydrogen H2 is used. Here, hydrocarbon C. H. C. is a hydrocarbon. H
2. ,. 2, C-H2,, and CRH211
-2 (n is an integer), or C.I.-2 (n is an integer), or a cyclic hydrocarbon. H.
．． ,,ChH. l, -2, and C+, Hzh-s (n
is an integer). When using boron halide, hydrocarbon, and hydrogen H2 as gaseous raw materials, the preferred range of the mixed gas is such that the ratio of boron halide:hydrocarbon:hydrogen is (2 to 10):l: (
100 or less) and gaseous raw material? When boron halide, carbon tetrachloride, and hydrogen are used, the ratio of boron halide carbon ditetrachloride:hydrogen is (2 to 10):l
: (100 or less). Moreover, it is preferable that the total pressure of these mixed gases is 200 to 1000 Torr. When this raw material is irradiated with pulsed CO laser light at room temperature, if the energy per unit cross-sectional area (fluence) of the laser light is small, the energy of the laser light is hardly absorbed by the mixed gas, but if the energy of the laser light exceeds a certain level, In the case of laser light, breakdown occurs within the source gas and most of the irradiated laser energy is absorbed.
これは、原料気体分子の光エネルギーによるイオン化及
びそれによって生じた電子の光エネルギー吸収に続くイ
オン化の繰り返しによって、それぞれ以下に示す反応が
引き起こされる。The following reactions are caused by the ionization of raw material gas molecules by light energy and the subsequent ionization of the resulting electrons following absorption of light energy.
４ ｎＢＸ３ＴＣｎＨｍ＋ Ｉ！Ｈ， →ｎＢ４Ｃ＋
１２ｎ｝ＩＸ４８Ｘ３ ＋ＣＣｊ！ａ ＋ ８Ｈ２
→Ｂ４Ｃ ＋１２ＨＸ ＋４ＨＣｌこの場合、照射に使
用するレーザーの波長は、原料気体の吸収波長に関係な
く、できるだけパルスエネルギーの強い発振波長がよい
。好ましくは９．６μｍである。またＣ０２レーザーの
他にＨＦ，Ｃｏ、ＹＡＧ，エキシマレーザーを用いるこ
ともできる。上記反応によって得られるＢ．Ｃは気相で
均一核生成とその成長によって得られるので、原理的に
球状で粒径も揃う。微粒子の粒径は０．３μｍ以下のも
のが得られ、生成条件の制御によっては得られる微粒子
の特性を変えることも可能である。具体的には微粒子の
粒径は、試料圧力に依存し、圧力増大と共に粒径は比例
的に大きくなる。レーザー光のエネルギーを増加しても
粒径は一定であるが収量は比例して大きくなる。4 nBX3TCnHm+ I! H, →nB4C+
12n}IX48X3 +CCj! a + 8H2
→B4C +12HX +4HCl In this case, the wavelength of the laser used for irradiation is preferably an oscillation wavelength with as strong a pulse energy as possible, regardless of the absorption wavelength of the raw material gas. Preferably it is 9.6 μm. In addition to the C02 laser, HF, Co, YAG, and excimer lasers can also be used. B. obtained by the above reaction. Since C is obtained by uniform nucleation and growth in the gas phase, it is in principle spherical and has a uniform particle size. Fine particles having a particle size of 0.3 μm or less can be obtained, and the characteristics of the obtained fine particles can be changed by controlling the production conditions. Specifically, the particle size of the fine particles depends on the sample pressure, and as the pressure increases, the particle size increases proportionally. Even if the energy of the laser beam is increased, the particle size remains constant, but the yield increases proportionally.
実際の微粒子の製造には、回分式または連続流通式の照
射セルを使用し、生成した微粒子の補集にはフィルター
やその他の補集装置を用いることができる。For actual production of fine particles, a batch type or continuous flow type irradiation cell can be used, and a filter or other collection device can be used to collect the generated fine particles.
（発明の効果）
このように、゛本発明によって得られたＢ．Ｃ微粒子は
、ほぼ球状でしかも均一であり、また高硬度・高融点セ
ラミックスとして種々の有用な素材に利用できる。現在
、Ｂ．Ｃ微粒子は粉砕法によって製造されているが、硬
度が大であるため能率が悪く、球状の微粒子が得られに
くく、また、粉砕機からの不純物の混入も避けられない
。本法は生成原理も簡単なものであり、現行法よりも著
しく有利である。Ｂ．Ｃ粒子は研磨材、耐摩耗材、電子
材料、原子炉の制御材や遮蔽材等への用途が具体的であ
り、特に高品質が要求される原子炉材として好適である
。(Effects of the Invention) As described above, the B. C fine particles are substantially spherical and uniform, and can be used as a variety of useful materials as high hardness and high melting point ceramics. Currently, B. C fine particles are manufactured by a pulverization method, but due to their high hardness, the efficiency is low and it is difficult to obtain spherical fine particles, and contamination with impurities from the pulverizer is unavoidable. This method has a simple generation principle and is significantly more advantageous than the current method. B. Specific applications of C particles include abrasive materials, wear-resistant materials, electronic materials, nuclear reactor control materials and shielding materials, and they are particularly suitable as nuclear reactor materials that require high quality.
（実施例） 本発明に使用した装置の概略を第１図に示す。(Example) FIG. 1 shows an outline of the apparatus used in the present invention.
適切な波数の００２レーザー１１のパルス光１２をＢａ
Ｆ２レンズ１３で集光し、照射反応容器１４内のＢ Ｂ
ｒ３とＣＨ．とＨ２の混合気体である試料気体１５に照
射する。尚、図中１６は絞り、１７はＫＢ，窓板、１８
は補集容器をそれぞれ示す。レーヂー照射後、残留及び
生成された副産物のガスを排気除去し、不活性ガスで容
器内を充たした後生成した微粒子を補集容器から取り出
す。Pulse light 12 of 002 laser 11 with appropriate wave number is Ba
The F2 lens 13 collects the light, and the B B inside the irradiation reaction vessel 14
r3 and CH. The sample gas 15, which is a mixed gas of and H2, is irradiated. In the figure, 16 is the aperture, 17 is the KB, window plate, and 18
indicate collection containers. After radiation irradiation, residual and generated by-product gases are removed by exhaust, and after filling the container with inert gas, the generated fine particles are taken out from the collection container.
（実施例１）
反応容器内を４ Ｘ １ ０−’Ｔｏｒｒの真空度にし
た後、５ ０ＴｏｒｒのＢ Ｂｒ，と１３ＴｏｒｒのＣ
Ｈ．と２ ０ ０ＴｏｒｒのＨ２の混合ガスを導入した
。これに、Ｃ Ｏ ２ レーザーの ９．６μｍ帯のＰ
（２４）、すなわち１ ０ ４ ３ｃｍ−’のパルス光
を、４時間、繰り返し数８００回で照射した。この時の
パルスエネルギーは約２． ５ Ｊ ／ｐｕｌｓｅ ，
使用したレンズの焦点距離は２０ｃｍである。反応式は
、
４ＢＢｒ，＋Ｃ｝Ｉ４＋ ４Ｈ２ →Ｂ４Ｃ ＋１２
ＨＢｒのように表わすことができる。(Example 1) After creating a vacuum level of 4 x 10-' Torr in the reaction vessel, 50 Torr of B Br, and 13 Torr of C were applied.
H. A mixed gas of H2 and 200 Torr was introduced. In addition, P of the 9.6 μm band of the CO 2 laser
(24), that is, pulsed light of 1043 cm-' was irradiated for 4 hours with a repetition rate of 800 times. The pulse energy at this time is approximately 2. 5 J/pulse,
The focal length of the lens used was 20 cm. The reaction formula is 4BBr,+C}I4+ 4H2 →B4C +12
It can be expressed as HBr.
この反応で０．２ｇの８４Ｃが生成した。This reaction produced 0.2 g of 84C.
生成した微粒子のＸ線回折図形を第２図に示す。The X-ray diffraction pattern of the produced fine particles is shown in FIG.
８４Ｃの既知のデータ値（Ｎａｔ， Ｂｕｒ．Ｓｔａｎ
ｄ， （Ｕ．Ｓ．）Ｍｏｎｏｇｒ，，２１， （１９
８４））と測定したＸ線回折図形を対比し、この図形の
解析から得られる面定数と元素分析の結果から、生成微
粒子はＢ．Ｃであることを確認した。更に、本方法によ
って得られたＢ．Ｃは平均粒径が０．３μｍの比較的均
一な分布を示し、しかも、ほぼ球状の微粒子であること
が走査型電子顕微鏡写真によって確認された。84C known data values (Nat, Bur. Stan
d, (U.S.) Monogr., 21, (19
84)) and the measured X-ray diffraction pattern, and from the surface constant obtained from the analysis of this pattern and the results of elemental analysis, it was determined that the produced fine particles were B. It was confirmed that it was C. Furthermore, the B. It was confirmed by scanning electron micrographs that C showed a relatively uniform distribution with an average particle size of 0.3 μm, and was found to be approximately spherical fine particles.
本実施例では、炭化水素ＣｎＨｍにメタンＣ Ｈ ４を
用いたが、この他エチレンＣ ２ Ｈ − 、アセチレ
ンＣ ２ Ｈ−プロパンＣ ｓ Ｈ ａ、ベンゼンＣ．
Ｈｇ等を用いても良い。In this example, methane C H 4 was used as the hydrocarbon CnHm, but in addition, ethylene C 2 H -, acetylene C 2 H-propane C s H a, benzene C.
Hg or the like may also be used.
（実施例２）
反応容器内を約４ Ｘ １ ０−’Ｔｏｒｒの真空度に
した後、１ ０ ０ＴｏｒｒのＢＣｊ’ｓと２５＝Ｔｏ
ｒｒのＣＣｊ！４と３ ０ ０ＴｏｒｒのＨ２の混合ガ
スを導入した。これに、ＣＯ２Ｌ／−ザーの９．６μｍ
帯のＰ（２４）、すなわち１０４３ｃｍ−’のパルス光
を、２時間、繰り返し数４， ０ ０ ０回で照射した
。この時のパルスエネルギーは約２． ５ Ｊ ／ｐｕ
ｌｓｅ 、使用したレンズの焦点距離は２０ｃｍである
。反応式は、
４Ｂｉｓ＋ＣＣｌ４；８Ｈ２ → ｅ４ｃ ＋１６Ｈ
Ｃｊ！のように表わすことができる。(Example 2) After creating a vacuum level of about 4 x 10-'Torr in the reaction vessel, BCj's of 100Torr and 25=Torr
CCj of rr! A mixed gas of 4 and 300 Torr of H2 was introduced. In addition to this, CO2L/-zer's 9.6 μm
Pulsed light at band P(24), ie, 1043 cm-', was irradiated for 2 hours with a repetition rate of 4,000 times. The pulse energy at this time is approximately 2. 5 J/pu
lse, the focal length of the lens used is 20 cm. The reaction formula is 4Bis+CCl4;8H2 → e4c +16H
Cj! It can be expressed as
この反応で０．１ｇのＢ．Ｃが生成した。In this reaction, 0.1 g of B. C was generated.
生成した微粒子のＸ線回折図形をＢ ４ Ｃの既知のデ
ータ値（Ｎａｔ．Ｂｕｒ．Ｓｔａｎｄ．（Ｕ．Ｓ，）Ｍ
ｏｎｏｇｒ，，２１，（１９８４））と測定したＸ線回
折図形を対比し、この図形の解析から得られる面定数と
元素分析の結果から、生成微粒子は８４Ｃであることを
確認した。更に、本方法によって得られたＢ４Ｃ は平
均粒径が０．３μｍの比較的均一な分布を示し、しかも
、ほぼ球状の微粒子であることが走査型電子顕微鏡写真
によって確認された。The X-ray diffraction pattern of the generated fine particles was compared with the known data value of B 4 C (Nat. Bur. Stand. (U.S.) M
Onogr., 21, (1984)) was compared with the measured X-ray diffraction pattern, and from the surface constant obtained from analysis of this pattern and the results of elemental analysis, it was confirmed that the produced fine particles were 84C. Furthermore, it was confirmed by scanning electron micrographs that the B4C obtained by this method showed a relatively uniform distribution with an average particle size of 0.3 μm, and was found to be approximately spherical fine particles.
第１図は、本発明の実施例に用いた装置の概略図であり
、
第２図は、本発明の実施例１で得られたＢ，Ｃ微粒子の
Ｘ線回折図形である。
（符号の説明）
１１・・・・ＣＣｈレーザー
１２・・・・レーザー光、
１３・・・・ＢａＦ２レンズ、
１４・・・・照射反応容器、 １５・・・・試料気体
、１６・・・・絞り、 １７、１９・・・・ＫＢｒ窓
板、１８・・・・補集容器、 ２０・・・・コック
。
手
続
補
正
書FIG. 1 is a schematic diagram of an apparatus used in an example of the present invention, and FIG. 2 is an X-ray diffraction pattern of B and C fine particles obtained in Example 1 of the present invention. (Explanation of symbols) 11... CCh laser 12... Laser light, 13... BaF2 lens, 14... Irradiation reaction vessel, 15... Sample gas, 16... Aperture, 17, 19...KBr window plate, 18...Collection container, 20...Cook. Procedural amendment
Claims (1)
体、またはハロゲン化ホウ素、四塩化炭素、及び水素と
を含む混合気体にレーザー光を照射して炭化ホウ素の粒
径０．５μｍ以下の微粒子を製造する方法。A gas mixture containing boron halide, hydrocarbon, and hydrogen, or a gas mixture containing boron halide, carbon tetrachloride, and hydrogen is irradiated with laser light to form fine particles of boron carbide with a particle size of 0.5 μm or less. How to manufacture.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| JP2006562A JP2561866B2 (en) | 1990-01-16 | 1990-01-16 | Method for producing fine particles of boron carbide |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| JP2006562A JP2561866B2 (en) | 1990-01-16 | 1990-01-16 | Method for producing fine particles of boron carbide |
Publications (2)
| Publication Number | Publication Date |
|---|---|
| JPH03215309A true JPH03215309A (en) | 1991-09-20 |
| JP2561866B2 JP2561866B2 (en) | 1996-12-11 |
Family
ID=11641771
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| JP2006562A Expired - Lifetime JP2561866B2 (en) | 1990-01-16 | 1990-01-16 | Method for producing fine particles of boron carbide |
Country Status (1)
| Country | Link |
|---|---|
| JP (1) | JP2561866B2 (en) |
Cited By (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| GB2515735A (en) * | 2013-07-01 | 2015-01-07 | Metal Nanopowders Ltd | Hard Materials |
| RU2648421C2 (en) * | 2016-07-06 | 2018-03-26 | Акционерное общество "Производственное объединение Электрохимический завод" (АО "ПО ЭХЗ") | Plasma-chemical method of producing boron carbide |
| CN112897528A (en) * | 2021-03-24 | 2021-06-04 | 云南华谱量子材料有限公司 | Method for synthesizing boron carbide/carbon powder material by laser sintering |
-
1990
- 1990-01-16 JP JP2006562A patent/JP2561866B2/en not_active Expired - Lifetime
Cited By (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| GB2515735A (en) * | 2013-07-01 | 2015-01-07 | Metal Nanopowders Ltd | Hard Materials |
| RU2648421C2 (en) * | 2016-07-06 | 2018-03-26 | Акционерное общество "Производственное объединение Электрохимический завод" (АО "ПО ЭХЗ") | Plasma-chemical method of producing boron carbide |
| CN112897528A (en) * | 2021-03-24 | 2021-06-04 | 云南华谱量子材料有限公司 | Method for synthesizing boron carbide/carbon powder material by laser sintering |
| US12384725B2 (en) | 2021-03-24 | 2025-08-12 | Yunnan Huapu quantum Material Co., Ltd | Method for preparing boron carbide material |
Also Published As
| Publication number | Publication date |
|---|---|
| JP2561866B2 (en) | 1996-12-11 |
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