JPH0347140B2 - - Google Patents
Info
- Publication number
- JPH0347140B2 JPH0347140B2 JP58159362A JP15936283A JPH0347140B2 JP H0347140 B2 JPH0347140 B2 JP H0347140B2 JP 58159362 A JP58159362 A JP 58159362A JP 15936283 A JP15936283 A JP 15936283A JP H0347140 B2 JPH0347140 B2 JP H0347140B2
- Authority
- JP
- Japan
- Prior art keywords
- fine particles
- laser beam
- raw material
- pulse
- gas
- 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 - Lifetime
Links
- 239000010419 fine particle Substances 0.000 claims description 39
- 239000002994 raw material Substances 0.000 claims description 36
- 239000002245 particle Substances 0.000 claims description 21
- 238000006243 chemical reaction Methods 0.000 claims description 18
- 238000000034 method Methods 0.000 claims description 17
- 238000002347 injection Methods 0.000 claims description 14
- 239000007924 injection Substances 0.000 claims description 14
- 238000004519 manufacturing process Methods 0.000 claims description 9
- 239000000919 ceramic Substances 0.000 claims description 4
- 229910052751 metal Inorganic materials 0.000 claims description 3
- 239000002184 metal Substances 0.000 claims description 3
- 230000010355 oscillation Effects 0.000 claims description 3
- 239000000126 substance Substances 0.000 claims description 2
- 230000001360 synchronised effect Effects 0.000 claims description 2
- 239000007789 gas Substances 0.000 description 48
- PXHVJJICTQNCMI-UHFFFAOYSA-N Nickel Chemical compound [Ni] PXHVJJICTQNCMI-UHFFFAOYSA-N 0.000 description 8
- 239000011261 inert gas Substances 0.000 description 7
- CURLTUGMZLYLDI-UHFFFAOYSA-N Carbon dioxide Chemical compound O=C=O CURLTUGMZLYLDI-UHFFFAOYSA-N 0.000 description 6
- XEEYBQQBJWHFJM-UHFFFAOYSA-N Iron Chemical compound [Fe] XEEYBQQBJWHFJM-UHFFFAOYSA-N 0.000 description 6
- FAPWRFPIFSIZLT-UHFFFAOYSA-M Sodium chloride Chemical compound [Na+].[Cl-] FAPWRFPIFSIZLT-UHFFFAOYSA-M 0.000 description 6
- XKRFYHLGVUSROY-UHFFFAOYSA-N Argon Chemical compound [Ar] XKRFYHLGVUSROY-UHFFFAOYSA-N 0.000 description 4
- 239000011572 manganese Substances 0.000 description 4
- 235000002639 sodium chloride Nutrition 0.000 description 4
- 239000011780 sodium chloride Substances 0.000 description 4
- 229910002092 carbon dioxide Inorganic materials 0.000 description 3
- 239000001569 carbon dioxide Substances 0.000 description 3
- 238000007796 conventional method Methods 0.000 description 3
- 238000010438 heat treatment Methods 0.000 description 3
- 239000000203 mixture Substances 0.000 description 3
- 229910052750 molybdenum Inorganic materials 0.000 description 3
- 229910052759 nickel Inorganic materials 0.000 description 3
- 229910052721 tungsten Inorganic materials 0.000 description 3
- ZOKXTWBITQBERF-UHFFFAOYSA-N Molybdenum Chemical compound [Mo] ZOKXTWBITQBERF-UHFFFAOYSA-N 0.000 description 2
- 229910021417 amorphous silicon Inorganic materials 0.000 description 2
- 229910052786 argon Inorganic materials 0.000 description 2
- 229910017052 cobalt Inorganic materials 0.000 description 2
- 239000010941 cobalt Substances 0.000 description 2
- GUTLYIVDDKVIGB-UHFFFAOYSA-N cobalt atom Chemical compound [Co] GUTLYIVDDKVIGB-UHFFFAOYSA-N 0.000 description 2
- 229910052742 iron Inorganic materials 0.000 description 2
- 230000001678 irradiating effect Effects 0.000 description 2
- 229910052748 manganese Inorganic materials 0.000 description 2
- 239000011859 microparticle Substances 0.000 description 2
- 239000011733 molybdenum Substances 0.000 description 2
- 238000011017 operating method Methods 0.000 description 2
- WFKWXMTUELFFGS-UHFFFAOYSA-N tungsten Chemical compound [W] WFKWXMTUELFFGS-UHFFFAOYSA-N 0.000 description 2
- 239000010937 tungsten Substances 0.000 description 2
- IJGRMHOSHXDMSA-UHFFFAOYSA-N Atomic nitrogen Chemical compound N#N IJGRMHOSHXDMSA-UHFFFAOYSA-N 0.000 description 1
- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical compound [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 description 1
- 229910001111 Fine metal Inorganic materials 0.000 description 1
- PWHULOQIROXLJO-UHFFFAOYSA-N Manganese Chemical compound [Mn] PWHULOQIROXLJO-UHFFFAOYSA-N 0.000 description 1
- 229910003902 SiCl 4 Inorganic materials 0.000 description 1
- 229910004298 SiO 2 Inorganic materials 0.000 description 1
- XUIMIQQOPSSXEZ-UHFFFAOYSA-N Silicon Chemical compound [Si] XUIMIQQOPSSXEZ-UHFFFAOYSA-N 0.000 description 1
- 229910052782 aluminium Inorganic materials 0.000 description 1
- XAGFODPZIPBFFR-UHFFFAOYSA-N aluminium Chemical compound [Al] XAGFODPZIPBFFR-UHFFFAOYSA-N 0.000 description 1
- 229910052799 carbon Inorganic materials 0.000 description 1
- 238000000354 decomposition reaction Methods 0.000 description 1
- 238000010586 diagram Methods 0.000 description 1
- 229910001873 dinitrogen Inorganic materials 0.000 description 1
- 230000005284 excitation Effects 0.000 description 1
- 229930195733 hydrocarbon Natural products 0.000 description 1
- 150000002430 hydrocarbons Chemical class 0.000 description 1
- 230000003993 interaction Effects 0.000 description 1
- WPBNNNQJVZRUHP-UHFFFAOYSA-L manganese(2+);methyl n-[[2-(methoxycarbonylcarbamothioylamino)phenyl]carbamothioyl]carbamate;n-[2-(sulfidocarbothioylamino)ethyl]carbamodithioate Chemical compound [Mn+2].[S-]C(=S)NCCNC([S-])=S.COC(=O)NC(=S)NC1=CC=CC=C1NC(=S)NC(=O)OC WPBNNNQJVZRUHP-UHFFFAOYSA-L 0.000 description 1
- 239000002923 metal particle Substances 0.000 description 1
- 150000002739 metals Chemical class 0.000 description 1
- 230000006911 nucleation Effects 0.000 description 1
- 238000010899 nucleation Methods 0.000 description 1
- 230000003287 optical effect Effects 0.000 description 1
- 239000011164 primary particle Substances 0.000 description 1
- 239000010453 quartz Substances 0.000 description 1
- 229910052710 silicon Inorganic materials 0.000 description 1
- 239000010703 silicon Substances 0.000 description 1
- VYPSYNLAJGMNEJ-UHFFFAOYSA-N silicon dioxide Inorganic materials O=[Si]=O VYPSYNLAJGMNEJ-UHFFFAOYSA-N 0.000 description 1
- 239000002210 silicon-based material Substances 0.000 description 1
Classifications
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01J—CHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
- B01J19/00—Chemical, physical or physico-chemical processes in general; Their relevant apparatus
- B01J19/08—Processes employing the direct application of electric or wave energy, or particle radiation; Apparatus therefor
- B01J19/12—Processes employing the direct application of electric or wave energy, or particle radiation; Apparatus therefor employing electromagnetic waves
- B01J19/121—Coherent waves, e.g. laser beams
Landscapes
- Physics & Mathematics (AREA)
- Chemical & Material Sciences (AREA)
- Health & Medical Sciences (AREA)
- Electromagnetism (AREA)
- General Health & Medical Sciences (AREA)
- Toxicology (AREA)
- Optics & Photonics (AREA)
- Organic Chemistry (AREA)
- Chemical Kinetics & Catalysis (AREA)
- Silicon Compounds (AREA)
- Physical Or Chemical Processes And Apparatus (AREA)
- Carbon And Carbon Compounds (AREA)
- Manufacture Of Metal Powder And Suspensions Thereof (AREA)
Description
【発明の詳細な説明】
本発明はレーザービームを用いた微粒子の製造
方法、およびその装置に関する。DETAILED DESCRIPTION OF THE INVENTION The present invention relates to a method for producing fine particles using a laser beam and an apparatus therefor.
従来、レーザーを用いて焼結性を有するセラミ
ツク微粒子を合成する場合、連続的な原料ガス流
と連続発振型のレーザーとを組合せて行つてい
る。この方法では原料ガスの流れる方向とレーザ
ー光軸とが直交しており、原料ガスの流速を制御
する事により連続照射するレーザービーム中での
原料ガスの滞留時間を制御して、均一且つ微小の
粒子を製造する際の化学反応、温度を制御してい
る。 Conventionally, when sinterable ceramic particles are synthesized using a laser, a continuous flow of raw material gas and a continuous wave laser are used in combination. In this method, the flow direction of the raw material gas and the laser optical axis are perpendicular to each other, and by controlling the flow rate of the raw material gas, the residence time of the raw material gas in the continuously irradiated laser beam is controlled. The chemical reaction and temperature during particle production are controlled.
しかしながら、この方式のセラミツク微粒子の
製造法では実用上原料ガスの流速に限界があつて
速くできず、従来では遅い傾向にある。また、レ
ーザービームは連続照射であるため、強度の強い
レーザービームを得にくい。あまり強くないレー
ザービームと比較的低速の原料ガスとの相互作用
による微粒子の粒子核生成条件に幅があるため、
粒子核の生成にゆらぎが生じ、一次粒子の粒径分
布に拡がりが生じる。 However, in this method of producing ceramic fine particles, there is a practical limit to the flow rate of the raw material gas, and the flow rate cannot be increased, and conventional methods tend to be slow. Furthermore, since the laser beam is continuously irradiated, it is difficult to obtain a strong laser beam. There is a wide range of conditions for particle nucleation of fine particles due to the interaction between a not very strong laser beam and a relatively slow source gas.
Fluctuations occur in the generation of particle nuclei, and the particle size distribution of primary particles expands.
従つて、本発明の目的は、上記従来技術の問題
点を解消した、粒径の小さく且つ粒径分布の狭い
微粒子の製造方法を提供することにある。 Therefore, an object of the present invention is to provide a method for producing fine particles having a small particle size and a narrow particle size distribution, which solves the problems of the prior art described above.
本発明の他の目的は、上記製造方法に使用する
装置を提供することにある。 Another object of the present invention is to provide an apparatus for use in the above manufacturing method.
本発明者は、上記目的が従来のレーザービーム
を用いる微粒子の製造法において、原料ガスの供
給およびレーザービームの照射をパルス的に行う
ことにより達成されることを見出し、本発明を完
成するに至つた。 The present inventor discovered that the above object can be achieved by supplying a raw material gas and irradiating a laser beam in a pulsed manner in a conventional method for producing fine particles using a laser beam, and was able to complete the present invention. Ivy.
即ち、本発明の方法は、所定圧の反応容器内に
原料ガスを所定の噴射圧にパルス的に供給し、一
方該原料ガスにレーザービームをパルス的に照射
することにより、該原料ガスから生成される物質
の微粒子を同時に多数個生成させることを特徴と
する。 That is, in the method of the present invention, a raw material gas is supplied in pulses at a predetermined injection pressure into a reaction vessel at a predetermined pressure, and on the other hand, the raw material gas is irradiated with a laser beam in a pulsed manner. It is characterized by simultaneously producing a large number of fine particles of the substance.
本発明の方法は例えばアモルフアスシリコン；
SiC、Si3N4等のケイ素系化合物；SiO2等の酸化
物のようなセラミツクスの微粒子；および例えば
鉄、コバルト、ニツケル、マンガン、モリブデ
ン、タングステン等の金属微粒子の製造に適用し
得る。本発明方法を適用するのに特に適した目的
微粒子はSi3N4、SiCおよびアモルフアスシリコ
ンである。 The method of the present invention includes, for example, amorphous silicon;
It can be applied to the production of silicon-based compounds such as SiC and Si 3 N 4 ; fine particles of ceramics such as oxides such as SiO 2 ; and fine particles of metals such as iron, cobalt, nickel, manganese, molybdenum, and tungsten. Particularly suitable target particles for applying the method of the invention are Si 3 N 4 , SiC and amorphous silicon.
上記原料ガスは、目的とする微粒子により適当
に選ばれた、反応又は分解により目的微粒子を生
成することができる１種類のガス又は２種類以上
のガス混合物である。原料ガスは目的とする微粒
子に応じて、公知の反応式に基づいて適宜選び得
る。例えば、Si3N4微粒子の製造には、原料ガス
としてNH3とSiH4との混合ガス、通常５：１〜
15：１、好ましくは約12：１の体積比の混合ガス
を用いることができる。またSiC微粒子の製造に
は例えば炭素源としてCH4、C2H4等の炭化水素、
そしてケイ素源としてSiH4、又はSiCl4を原料ガ
スとして用いることができる。更にまた、ニツケ
ル（Ni）、鉄（Fe）、コバルト（Co）、マンガン
（Mn）、モリブデン（Mo）およびタングステン
（Ｗ）の各金属微粒子の製造には、原料ガスとし
てそれぞれNi（CO）4、Fe（CO）5、Co2（CO）8、
Mn2（CO）10、Mo（CO）6およびＷ（CO）6の各気化
ガスを用いることができる。 The raw material gas is one type of gas or a mixture of two or more types of gas, which is appropriately selected depending on the target fine particles and is capable of producing the target fine particles through reaction or decomposition. The raw material gas can be appropriately selected based on a known reaction formula depending on the target fine particles. For example, in the production of Si 3 N 4 fine particles, a mixed gas of NH 3 and SiH 4 , usually 5:1 to
A gas mixture with a volume ratio of 15:1, preferably about 12:1, can be used. In addition, for the production of SiC fine particles, for example, hydrocarbons such as CH 4 and C 2 H 4 are used as a carbon source,
As a silicon source, SiH 4 or SiCl 4 can be used as a raw material gas. Furthermore, in the production of fine metal particles of nickel (Ni), iron (Fe), cobalt (Co), manganese (Mn), molybdenum (Mo), and tungsten (W), Ni (CO) 4 is used as a raw material gas, respectively. , Fe(CO) 5 , Co 2 (CO) 8 ,
Vaporized gases of Mn 2 (CO) 10 , Mo(CO) 6 and W(CO) 6 can be used.
反応容器内は通常不活性ガス、例えばアルゴン
ガス、チツ素ガス等、を導入して所定の圧力（正
圧又は負圧）に設定する。 Usually, an inert gas such as argon gas or nitrogen gas is introduced into the reaction vessel to set a predetermined pressure (positive pressure or negative pressure).
原料ガスの噴射は通常絶対圧で0.3〜2.5Kg／
cm2、好ましくは1.5〜２Kg／cm2の噴射圧にて、通
常0.1〜２回／秒、好ましくは0.5〜0.8回／秒のパ
ルスにて、即ち間欠的に繰返し行う。 The injection of raw material gas is usually 0.3 to 2.5 kg/absolute pressure.
cm 2 , preferably 1.5 to 2 Kg/cm 2 , and pulses of usually 0.1 to 2 times/second, preferably 0.5 to 0.8 times/second, ie, repeated intermittently.
レーザービームは通常原料ガスの噴射方向と交
差する方向、好ましくは直交する方向から、原料
ガスの噴射パルスと同期させてパルス的に（即
ち、間欠的に）繰返し照射する。レーザービーム
源は系の反応に必要な波長、エネルギーに応じて
適宜選ぶことができる。例えばNH3とSiH4の混
合ガスからSi3N4微粒子の製造には炭酸ガスレー
ザー、F2−エキシマ−レーザー等；C2H4とSiH4
の混合ガスからSiC微粒子の製造には炭酸ガスレ
ーザー、F2−エキシマ−レーザー等；Ni（CO）4、
Fe（CO）5、Co2（CO）8、Mn2（CO）10、Mo（CO）6お
よびＷ（CO）6からそれぞれNi、Fe、Co、Mn、
MoおよびＷの金属微粒子の製造にはCOレーザ
ー、N2Oレーザー等が通常使用される。レーザ
ービームの１パルスの照射時間は原料ガスおよび
目的生成物等により変化するが、通常0.1〜10μ
秒、好ましくは0.2〜0.5μ秒である。またレーザ
ービームの照射強度は、パルス的であるため0.2
〜50MW程度の強い強度となり得る。 The laser beam is usually repeatedly irradiated in a pulsed manner (that is, intermittently) from a direction intersecting, preferably perpendicular to, the injection direction of the source gas in synchronization with the injection pulse of the source gas. The laser beam source can be appropriately selected depending on the wavelength and energy required for the reaction of the system. For example, carbon dioxide laser, F 2 -eximer laser, etc. are used to produce Si 3 N 4 fine particles from a mixed gas of NH 3 and SiH 4 ; C 2 H 4 and SiH 4
Carbon dioxide laser, F2 -excimer laser, etc. are used to produce SiC fine particles from a mixed gas of Ni(CO) 4 ,
Fe(CO) 5 , Co2 (CO) 8 , Mn2 (CO) 10 , Mo(CO) 6 and W(CO) 6 respectively yield Ni, Fe, Co, Mn,
CO laser, N 2 O laser, etc. are usually used to produce Mo and W metal fine particles. The irradiation time of one pulse of the laser beam varies depending on the raw material gas and target product, but it is usually 0.1 to 10μ.
seconds, preferably 0.2 to 0.5 microseconds. In addition, the irradiation intensity of the laser beam is 0.2
It can be as strong as ~50MW.
かかる原料ガスおよびレーザービームのパルス
的供給又は照射により、原料ガスを高速度にて供
給し且つレーザービームを高強度にて短時間照射
できるので、該原料ガスから多数個の微粒子が同
時に生成され、またこの短い照射時間により生成
微粒子が短時間しか加熱されず、従つて該微粒子
の成長が抑えられて、粒径が小さく且つ粒径分布
の狭い微粒子が得られる。 By supplying or irradiating the raw material gas and laser beam in a pulsed manner, the raw material gas can be supplied at high speed and the laser beam can be irradiated with high intensity for a short time, so that a large number of fine particles can be generated from the raw material gas at the same time. Further, due to this short irradiation time, the generated fine particles are heated for only a short time, and therefore, the growth of the fine particles is suppressed, and fine particles having a small particle size and a narrow particle size distribution can be obtained.
本発明の方法により得られる微粒子は通常粒径
約80〜100Åであり、粒径分布も平均粒径から数
％の範囲にあるものを得ることができる。 The fine particles obtained by the method of the present invention usually have a particle size of about 80 to 100 Å, and the particle size distribution can also be within several percent of the average particle size.
次に本発明方法の操作手順およびその方法に使
用する装置を、図面をもつて具体的に説明する。 Next, the operating procedure of the method of the present invention and the apparatus used in the method will be specifically explained with reference to the drawings.
第１図は、本発明方法の操作手順を示すフロー
シートである。即ち、本発明の方法は通常下記
〜の手順に従つて行われる。 FIG. 1 is a flow sheet showing the operating procedure of the method of the present invention. That is, the method of the present invention is usually carried out according to the following steps.
気密な反応容器の内圧を所定圧（正圧又は負
圧）とする。 The internal pressure of the airtight reaction vessel is set to a predetermined pressure (positive pressure or negative pressure).
該容器内に不活性ガスを導入する。 An inert gas is introduced into the container.
この反応容器内に噴孔を臨ましたインジエク
ターから原料ガスを所定の噴射圧でパルス的に
供給しつつ、この原料ガス噴射時に対応してレ
ーザービームをパルス的に該原料ガスに照射
し、同時に原料ガスとレーザービームのパルス
を同期制御する。 While supplying raw material gas in pulses at a predetermined injection pressure from an injector with a nozzle hole facing into this reaction vessel, a laser beam is irradiated to the raw material gas in pulses corresponding to the injection of this raw material gas, and at the same time the raw material gas is Synchronous control of gas and laser beam pulses.
原料ガスの供給及びレーザービームの照射を
パルス的にかつ繰返して、レーザービームの照
射により原料ガスから生成する微粒子を多層同
時に生成させ、一方パルス的なレーザービーム
の照射によりレーザーによる加熱時間を短くし
て粒子の成長を抑える事により、微粒子を製造
する。 The supply of the raw material gas and the irradiation of the laser beam are repeated in a pulsed manner to simultaneously generate multiple layers of fine particles generated from the raw material gas by the irradiation of the laser beam, while the heating time by the laser is shortened by the irradiation of the pulsed laser beam. Fine particles are produced by suppressing particle growth.
生成微粒子をフイルター補集する。 The generated fine particles are collected by a filter.
第２図は、本発明の方法に使用し得る装置の一
態様を示すものである。この装置は、内圧を所定
圧に保持する定圧保持手段を備えた気密な反応容
器１と、この容器内に噴孔を臨ましかつ原料ガス
供給源に連通して原料ガスを所定の噴射圧でパル
ス的に供給するパルスインジエクター２と、前記
原料ガスの供給に対応してレーザービームをパル
ス的に該原料ガスに照射するパルスコントローラ
４を介したパルス発振型レーザー３とから本質的
に成る。 FIG. 2 shows one embodiment of an apparatus that can be used in the method of the invention. This device includes an airtight reaction vessel 1 equipped with a constant pressure holding means for keeping the internal pressure at a predetermined pressure, and a nozzle hole facing into this vessel and communicating with a raw material gas supply source to inject raw material gas at a predetermined injection pressure. It essentially consists of a pulse injector 2 that supplies the raw material gas in a pulsed manner, and a pulse oscillation type laser 3 via a pulse controller 4 that irradiates the raw material gas with a laser beam in a pulsed manner in response to the supply of the raw material gas.
該反応容器１は通常、中空円筒状の形体であ
り、そして容器の両端およびその他の部分はＯリ
ングにより、気密に保たれるように閉止されてい
る。容器１の一方の端にはレーザー光を導入する
窓として岩塩（NaCl）板５が、それに向い合つ
た他方の端にはのぞき窓として石英板６が備えら
れている。 The reaction vessel 1 usually has a hollow cylindrical shape, and both ends and other parts of the vessel are hermetically closed with O-rings. A rock salt (NaCl) plate 5 is provided at one end of the container 1 as a window for introducing laser light, and a quartz plate 6 is provided at the opposite end as a viewing window.
反応容器１内を所定圧に保つ手段として、該容
器１には真空ポンプ７と連結する排気口８と不活
性ガス導入口９、およびそれぞれに連通してガス
排気量、不活性ガス導入量を調整するための真空
バルブ１０とニードルバルブ１１を有し、更に容
器内圧力を測定するための圧力計１２が備えられ
ている。 As a means for maintaining the inside of the reaction vessel 1 at a predetermined pressure, the vessel 1 has an exhaust port 8 and an inert gas inlet 9 connected to a vacuum pump 7, and an inert gas inlet 9 communicating with each other to control the amount of gas exhausted and the amount of inert gas introduced. It has a vacuum valve 10 and a needle valve 11 for adjustment, and is further equipped with a pressure gauge 12 for measuring the pressure inside the container.
パルス発振型レーザービーム３は円筒状の反応
容器１と同軸方向から、パルスインジエクタ２の
噴孔間際の原料ガスを照射するように配置されて
いる。得られた微粒子は排気口８に設けられたフ
イルタ１３により捕集される。 The pulsed laser beam 3 is arranged so as to irradiate the raw material gas near the nozzle hole of the pulse injector 2 from the same axis as the cylindrical reaction vessel 1 . The obtained fine particles are collected by a filter 13 provided at the exhaust port 8.
次に本発明を、実施例をもつてより具体的に説
明する。 Next, the present invention will be explained in more detail with reference to Examples.
実施例
気密な反応容器１を真空ポンプ７にて
10-3Torrの真空まで排気したのち、反応容器内
の圧力を不活性ガス（アルゴンガス）の導入量と
真空バルブ１０の微調整により、圧力計１２を用
いて一定圧、760Torrに設定する。Example: Airtight reaction vessel 1 is used with vacuum pump 7
After evacuating to a vacuum of 10 -3 Torr, the pressure inside the reaction vessel is set to a constant pressure of 760 Torr using the pressure gauge 12 by introducing the amount of inert gas (argon gas) and finely adjusting the vacuum valve 10.
予じめ組成の調整された原料ガス（体積比
NH3／SiH4＝12）を1.5〜２Kg／cm2絶対圧の噴射
圧でインジエクター２から間欠的に繰返して供給
しつつ、パルスコントローラ４を用いて該原料ガ
ス噴射時に対応させて、横励起型炭酸ガスレーザ
ー３のレーザービームをパルス的に岩塩（NaCl）
製の窓板５を通して該原料ガスに0.2μsec照射す
る。レーザービーム照射を受けて該原料ガスから
生成する微粒子を多数同時に生成させる事と、こ
の短い照射時間に対応するレーザーによる短い加
熱時間により、粒子の成長が抑えられ、粒径80〜
100ÅのSi3N4微粒子がフイルター１３上に捕集
された。 Raw material gas whose composition has been adjusted in advance (volume ratio
NH 3 /SiH 4 = 12) is intermittently and repeatedly supplied from the injector 2 at an injection pressure of 1.5 to 2 Kg/cm 2 absolute pressure, and the pulse controller 4 is used to perform lateral excitation corresponding to the injection of the raw material gas. Rock salt (NaCl) is pulsed with the laser beam of type carbon dioxide laser 3.
The raw material gas is irradiated for 0.2 μsec through a window plate 5 made of aluminum. By simultaneously generating a large number of fine particles from the raw material gas when irradiated with a laser beam, and by short heating times by the laser corresponding to this short irradiation time, particle growth is suppressed and the particle size is reduced to 80~
Si 3 N 4 fine particles of 100 Å were collected on the filter 13 .
本発明によれば、レーザービーム中での原料ガ
ス滞留時間が短く、このレーザー照射により数多
くの微粒子が同時に生成し、かつレーザー照射時
間が短いためにレーザーによる加熱時間も短く、
その結果粒子の成長が抑えられるため、従来法に
比べて製造される微粒子の粒径は小さく、かつ粒
径分布も狭いものになる。 According to the present invention, the residence time of the raw material gas in the laser beam is short, many fine particles are simultaneously generated by this laser irradiation, and the laser irradiation time is short, so the heating time by the laser is also short.
As a result, the growth of particles is suppressed, so the particle size of the fine particles produced is smaller and the particle size distribution is narrower than in the conventional method.
反応容器の容器内圧力、レーザー照射時間、パ
ルスインジエクターの噴射圧の少くとも一つを制
御する事により、微粒子の粒径も制御できるの
で、高品質の微粒子が製造できる。 By controlling at least one of the internal pressure of the reaction vessel, the laser irradiation time, and the injection pressure of the pulse injector, the particle size of the microparticles can be controlled, so high-quality microparticles can be produced.
第１図は本発明方法を示すフローシートであ
り、そして第２図は本発明装置の概略模式図であ
る。
１……１反応容器、２……パルスインジエク
タ、３……パルス発振型レーザー、４……パルス
コントローラ、９……不活性ガス導入口。
FIG. 1 is a flow sheet showing the method of the present invention, and FIG. 2 is a schematic diagram of the apparatus of the present invention. 1...1 reaction vessel, 2...pulse injector, 3...pulse oscillation type laser, 4...pulse controller, 9...inert gas inlet.
Claims (1)
圧にてパルス的に供給し、一方該原料ガスにレー
ザービームをパルス的に照射することにより、該
原料ガスから生成される物質の微粒子を同時に多
数個生成させることを特徴ととする、微粒子の製
造方法。 ２ 生成される微粒子がセラミツク微粒子である
特許請求の範囲第１項記載の方法。 ３ 生成される微粒子が金属微粒子である特許請
求の範囲第１項記載の方法。 ４ 原料ガスがNH3−SiH4混合ガスであり、生
成される微粒子がSi3N4微粒子である特許請求の
範囲第２項記載の方法。 ５ 生成される微粒子が粒径80〜200Åの範囲に
ある特許請求の範囲第１項又は第４項記載の方
法。 ６ 原料ガス噴射のパルスとレーザービームのパ
ルスとをパルスコントローラにより同期させる特
許請求の範囲第１項記載の方法。 ７ 内圧を所定圧に保持する定圧保持手段を備え
た気密な反応容器と、該容器内に噴孔を臨まし
た、原料ガスを所定の噴射圧にてパルス的に供給
するためのパルスインジエクタと、前記原料ガス
の供給パルスに対応してレーザービームをパルス
的に該原料ガスに照射するパルスコントローラを
介したパルス発振型レーザーとから成ることを特
徴とする、レーザービームを用いる微粒子製造用
装置。[Scope of Claims] 1. A source gas is supplied in pulses at a predetermined injection pressure into a reaction vessel at a predetermined pressure, and a laser beam is irradiated to the source gas in pulses to produce a product from the source gas. A method for producing fine particles, characterized by simultaneously producing a large number of fine particles of a substance. 2. The method according to claim 1, wherein the fine particles produced are ceramic fine particles. 3. The method according to claim 1, wherein the fine particles produced are metal fine particles. 4. The method according to claim 2, wherein the raw material gas is a NH 3 -SiH 4 mixed gas, and the generated fine particles are Si 3 N 4 fine particles. 5. The method according to claim 1 or 4, wherein the fine particles produced have a particle size in the range of 80 to 200 Å. 6. The method according to claim 1, wherein the pulse of the source gas injection and the pulse of the laser beam are synchronized by a pulse controller. 7. An airtight reaction vessel equipped with a constant pressure holding means for keeping the internal pressure at a predetermined pressure, and a pulse injector for supplying raw material gas in pulses at a predetermined injection pressure, with an injection hole facing into the container. An apparatus for producing fine particles using a laser beam, comprising: a pulse oscillation type laser via a pulse controller that irradiates the source gas with a laser beam in pulses in response to the supply pulse of the source gas.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| JP58159362A JPS6051539A (en) | 1983-08-31 | 1983-08-31 | Method and apparatus for preparing fine particle by laser beam |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| JP58159362A JPS6051539A (en) | 1983-08-31 | 1983-08-31 | Method and apparatus for preparing fine particle by laser beam |
Publications (2)
| Publication Number | Publication Date |
|---|---|
| JPS6051539A JPS6051539A (en) | 1985-03-23 |
| JPH0347140B2 true JPH0347140B2 (en) | 1991-07-18 |
Family
ID=15692179
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| JP58159362A Granted JPS6051539A (en) | 1983-08-31 | 1983-08-31 | Method and apparatus for preparing fine particle by laser beam |
Country Status (1)
| Country | Link |
|---|---|
| JP (1) | JPS6051539A (en) |
Families Citing this family (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| JPS62123244U (en) * | 1986-01-23 | 1987-08-05 | ||
| KR20010016692A (en) * | 1999-08-02 | 2001-03-05 | 최만수 | Method for manufacturing fine spherical particles by controlling particle coalescence using laser beam heating |
| FR2865671B1 (en) * | 2004-01-30 | 2007-03-16 | Commissariat Energie Atomique | CERAMIC NANOPOUDRE SUITABLE FOR SINTING AND METHOD OF SYNTHESIS |
| FR2916193B1 (en) * | 2007-05-18 | 2009-08-07 | Commissariat Energie Atomique | LASER PYROLYSIS SYNTHESIS OF SILICON NANOCRYSTALS. |
-
1983
- 1983-08-31 JP JP58159362A patent/JPS6051539A/en active Granted
Also Published As
| Publication number | Publication date |
|---|---|
| JPS6051539A (en) | 1985-03-23 |
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