JPS63224732A - Production of ultrafine particles - Google Patents
Production of ultrafine particlesInfo
- Publication number
- JPS63224732A JPS63224732A JP62056781A JP5678187A JPS63224732A JP S63224732 A JPS63224732 A JP S63224732A JP 62056781 A JP62056781 A JP 62056781A JP 5678187 A JP5678187 A JP 5678187A JP S63224732 A JPS63224732 A JP S63224732A
- Authority
- JP
- Japan
- Prior art keywords
- ultrafine particles
- reactive gas
- gas
- vacuum vessel
- laser beams
- 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
- 239000011882 ultra-fine particle Substances 0.000 title claims abstract description 24
- 238000004519 manufacturing process Methods 0.000 title claims description 7
- 239000012495 reaction gas Substances 0.000 claims description 15
- 238000010574 gas phase reaction Methods 0.000 claims description 6
- 239000002245 particle Substances 0.000 abstract description 22
- 239000007789 gas Substances 0.000 abstract description 15
- 238000009826 distribution Methods 0.000 abstract description 10
- BLRPTPMANUNPDV-UHFFFAOYSA-N Silane Chemical compound [SiH4] BLRPTPMANUNPDV-UHFFFAOYSA-N 0.000 abstract description 3
- 238000006243 chemical reaction Methods 0.000 abstract description 3
- 229910052581 Si3N4 Inorganic materials 0.000 abstract description 2
- 239000007792 gaseous phase Substances 0.000 abstract 2
- 239000008246 gaseous mixture Substances 0.000 abstract 1
- 239000000376 reactant Substances 0.000 description 4
- 230000000694 effects Effects 0.000 description 3
- 230000008020 evaporation Effects 0.000 description 3
- 238000001704 evaporation Methods 0.000 description 3
- 238000000034 method Methods 0.000 description 3
- 239000000126 substance Substances 0.000 description 3
- ATJFFYVFTNAWJD-UHFFFAOYSA-N Tin Chemical compound [Sn] ATJFFYVFTNAWJD-UHFFFAOYSA-N 0.000 description 2
- 238000007796 conventional method Methods 0.000 description 2
- 239000000203 mixture Substances 0.000 description 2
- UFHFLCQGNIYNRP-UHFFFAOYSA-N Hydrogen Chemical compound [H][H] UFHFLCQGNIYNRP-UHFFFAOYSA-N 0.000 description 1
- 238000005054 agglomeration Methods 0.000 description 1
- 230000002776 aggregation Effects 0.000 description 1
- 238000000889 atomisation Methods 0.000 description 1
- 239000003054 catalyst Substances 0.000 description 1
- 239000000919 ceramic Substances 0.000 description 1
- 230000007423 decrease Effects 0.000 description 1
- 239000010419 fine particle Substances 0.000 description 1
- 229910052739 hydrogen Inorganic materials 0.000 description 1
- 239000001257 hydrogen Substances 0.000 description 1
- 230000001678 irradiating effect Effects 0.000 description 1
- 239000000463 material Substances 0.000 description 1
- 239000002184 metal Substances 0.000 description 1
- 230000003287 optical effect Effects 0.000 description 1
- 239000000843 powder Substances 0.000 description 1
- 239000007787 solid Substances 0.000 description 1
- 239000013076 target substance 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
-
- 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
- B01J12/00—Chemical processes in general for reacting gaseous media with gaseous media; Apparatus specially adapted therefor
- B01J12/02—Chemical processes in general for reacting gaseous media with gaseous media; Apparatus specially adapted therefor for obtaining at least one reaction product which, at normal temperature, is in the solid state
Abstract
Description
【発明の詳細な説明】 〔産業上の利用分野〕 この発明は、超微粒子の製造方法に関するものである。[Detailed description of the invention] [Industrial application field] The present invention relates to a method for producing ultrafine particles.
一般に金属又はセラミックスの粉末のうち、粒径がｌ／
Ｌｍ以下の固体粒子を超微粒子と呼ぶが、比表面積（容
積に対する表面積の割合）が太きいため、一般の微粒子
には認められない特異な性質を有する。即ち、超微粒子
は化学的活性が強いばかりでなく、熱的、電気的、磁気
的、光学的にも興味深い性質を示し、触媒、電子素子、
磁気素子、生物医学機能素子への応用が考えられている
。Generally, among metal or ceramic powders, the particle size is l/
Solid particles of Lm or less are called ultrafine particles, but because they have a large specific surface area (ratio of surface area to volume), they have unique properties not found in general fine particles. In other words, ultrafine particles not only have strong chemical activity, but also exhibit interesting thermal, electrical, magnetic, and optical properties, and are useful for catalysts, electronic devices,
Applications to magnetic elements and biomedical functional elements are being considered.
従来の超微粒子の製造方法としては、ガス中蒸発法、プ
ラズマ蒸発法、水素プラズマ反応法、アトマイゼイショ
ンなどがある。Conventional methods for producing ultrafine particles include in-gas evaporation, plasma evaporation, hydrogen plasma reaction, and atomization.
しかし、上述したような従来の製造方法においては、生
成粒子の凝集が起り易いために粒子の平均粒径が大きく
且つ粒度分布が広い。さらに、目的物質を含んだ適切な
蒸発源材料が必要となるため（−１製造可能々超微粒子
の種類が限定され、しかも、均質且つ高純度の超微粒子
を製造することが困難である。However, in the conventional manufacturing method as described above, agglomeration of the produced particles tends to occur, so that the average particle size of the particles is large and the particle size distribution is wide. Furthermore, since an appropriate evaporation source material containing the target substance is required (-1), the types of ultrafine particles that can be produced are limited, and it is difficult to produce homogeneous and highly pure ultrafine particles.
従って、この発明の目的は、平均粒径が小さく且つ粒度
分布が狭く、しかも、均質且つ高純度の超微粒子の製造
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 ultrafine particles having a small average particle size and a narrow particle size distribution, and which are homogeneous and highly pure.
この発明は、真空容器内に反応ガスを、前記真空容器内
の圧力を所定圧力に維持しながら導入し、レーザビーム
を前記真空容器内の反応ガスにパルス的に照射して気相
反応を起こさせ、かくして、超微粒子を得ることに特徴
を有するものである。In this invention, a reaction gas is introduced into a vacuum container while maintaining the pressure inside the vacuum container at a predetermined pressure, and a laser beam is irradiated to the reaction gas in the vacuum container in a pulsed manner to cause a gas phase reaction. This method is characterized in that ultrafine particles are obtained.
次に、この発明の一実施態様を図面を参照しながら説明
する。Next, one embodiment of the present invention will be described with reference to the drawings.
第１図は、この発明の一実施態様の概略断面図である。FIG. 1 is a schematic cross-sectional view of one embodiment of the present invention.
第１図に示すように、真空容器１内に、例えば、５ｉｎ
４とＮＨ３とからなる混合ガス２を反応ガスとして真空
容器１内を所定圧力に維持しながら導入し、そして、前
記反応ガスに、例えば、ＣＯ２レーザビーム３を第２図
に示すようにパルス的に照射する。As shown in FIG. 1, for example, a 5 inch
A mixed gas 2 consisting of 4 and NH3 is introduced as a reaction gas into the vacuum vessel 1 while maintaining a predetermined pressure, and then a CO2 laser beam 3 is applied to the reaction gas in a pulsed manner as shown in FIG. irradiate.
即ち、ｔ１時間出力Ｐ１ のレーザビームを反応ガス
に照射して反応ガスをこれが反応しない程度に加熱し、
次に、ｔ２ 時間出力Ｐ２のレーザビームを反応ガス
に照射して反応ガスに気相反応を起こさせる。かくして
、Ｓｉ３Ｎ４からなる超微粒子４が製造される。次（−
１このようにして得られた超微粒子を、次のｔ５時間の
間に未反応ガスと共に真空容器ｌ内から回収（排気装置
及び回収装置は図示せず）ｔ１時間の間、レーザの出力
がＰｌと低いために、反応ガスは気相反応を起こさず、
ガス温度は低下する。従って、製造された超微粒子は凝
集を起こさず、粒径が小さく、粒度分布の狭いものとな
る。That is, the reactant gas is heated to such an extent that it does not react by irradiating the reactant gas with a laser beam having an output of P1 for a time t1,
Next, the reactant gas is irradiated with a laser beam having an output of P2 for a time t2 to cause a gas phase reaction in the reactant gas. In this way, ultrafine particles 4 made of Si3N4 are produced. Next (−
1 The ultrafine particles obtained in this way are collected from the vacuum vessel l together with the unreacted gas during the next time t5 (exhaust equipment and collection equipment are not shown). During the time t1, the laser output is Because of the low
Gas temperature decreases. Therefore, the produced ultrafine particles do not agglomerate, have a small particle size, and have a narrow particle size distribution.
上記レーザビームの照射サイクルは、次の通りが好まし
い。The irradiation cycle of the laser beam is preferably as follows.
繰返し周波数 ：ｌ−１０００Ｈｚ
ピーク比（Ｐ２／Ｐｌ） ： Ｐ＋ が０〜３ ／
４ Ｐ ２、Ｄｕｔｙ（ｔ、ｚ／ｉ＋＋ｔ２） ；
１０〜９０％。Repetition frequency: l-1000Hz Peak ratio (P2/Pl): P+ is 0 to 3 /
4 P 2, Duty (t, z/i++t2);
10-90%.
〔実施例１〕
真空容器内にＳｉＨ４とＮＨ３とからなる反応ガスを、
真空容器内をｌ ５ Ｔｏｒｒ の圧力に維持しなが
ら導入し、そして、前記反応ガスにＣＯ２レーザビーム
を、繰返し周波数： ２００ ）ＬＺ 、 Ｄｕｔｙ（
ｔ、２／ｌｌ＋ｔ２） ： ５０チ、Ｐ２：２００Ｗに
設定し、Ｐ、を０〜１５０Ｗに変化させて、前記反応ガ
スに下式に示す気相反応を起こさせた。[Example 1] A reaction gas consisting of SiH4 and NH3 was placed in a vacuum container.
A CO2 laser beam is introduced into the vacuum container while maintaining a pressure of l 5 Torr, and a CO2 laser beam is applied to the reaction gas at a repetition frequency: 200 ) LZ , Duty (
t, 2/ll+t2): 50 cm, P2: set at 200 W, P was changed from 0 to 150 W, and the reaction gas was caused to undergo a gas phase reaction as shown in the following formula.
３ Ｓ ｉＨ４−１−４ＮＨ３→５１３Ｎ４＋１２Ｈ２
このようにして、８１３Ｎ４からなる超微粒子を製造し
た。この超微粒子の粒度分布および生産効率ノ結果ヲ、
２００Ｗの００２レーザビームを連続照射した結果と合
わせて第１表に示す。なお、本発明法によって得られた
超微粒子は、所定の化学組成（５ｉ３Ｎ４）からなり、
純度も９９．９％であった。3 S iH4-1-4NH3→513N4+12H2
In this way, ultrafine particles made of 813N4 were produced. The results of the particle size distribution and production efficiency of these ultrafine particles are
The results are shown in Table 1 together with the results of continuous irradiation with a 200W 002 laser beam. The ultrafine particles obtained by the method of the present invention have a predetermined chemical composition (5i3N4),
The purity was also 99.9%.
第１表
ただし Ｐ２＝２００（Ｗ）、 Ｄｕｔｙ（ｔ２／ｌ＋
＋ｔ２）＝５０％繰返し周波数 ２００ Ｈｚ
第１表から明らかなよう（二、本発明法は、レーザビー
ムを連続照射した場合に比べて生産効率は若干劣るが、
粒度分布の面で優れていることがわかる。Table 1 However, P2=200(W), Duty(t2/l+
+t2) = 50% repetition frequency 200 Hz As is clear from Table 1 (2. The production efficiency of the method of the present invention is slightly inferior to that of continuous laser beam irradiation, but
It can be seen that the particle size distribution is excellent.
〔実施例２〕
真空容器内にＳｉＨ４とＣ２Ｈ４とからなる反応ガスを
、真空容器内を２５ Ｔｏｒｒ の圧力に維持し表か
ら導入し、そして、前記混合ガスにＣ０２レーザビーム
を、第２表に示す種々の条件で照射して、前 □記反
応ガスに下式に示す気相反応を起こさせた。[Example 2] A reaction gas consisting of SiH4 and C2H4 was introduced into a vacuum container from the front while maintaining the pressure inside the vacuum container at 25 Torr, and a C02 laser beam was applied to the mixed gas as shown in Table 2. Irradiation was performed under the various conditions shown to cause the gas phase reaction shown in the following formula to occur in the reaction gas described above.
２８ｉ Ｈ４＋Ｃ２Ｈ４→２ Ｓ ＩＣ＋ ６ Ｈ２第
２表
このようにしてＳｉＣからなる超微粒子を製造し６一
た。第２表に示した全ての条件において、超９粒子の平
均粒径は小さく且つ粒度分布は１２〜２５μｍであり、
従来法によって製造した場合の粒度分布５０〜２００μ
ｍと比べて著しく狭かった。28i H4+C2H4→2 S IC+ 6 H2 Table 2 In this manner, ultrafine particles made of SiC were produced. Under all conditions shown in Table 2, the average particle size of Super 9 particles was small and the particle size distribution was 12 to 25 μm,
Particle size distribution when manufactured by conventional method: 50-200μ
It was significantly narrower than m.
〔実施例３〕
真空容器内にＴ ｉ Ｃ４とＮＨ３とからなる反応ガス
を、真空容器内を２０ Ｔｏｒｒ の圧力に維持しな
がら導入し、そして、前記反応ガスにＣＯ２レーザビー
ムを、ｐ、： ５０Ｗ、Ｐ２： １５０Ｗ、繰返し周波
数： ２００ Ｈｚ 、 Ｄｕｔｙ ： ５０％の条件
に従って照射して、前記反応ガスに下式に示す気相反応
を起こさせた。[Example 3] A reaction gas consisting of T i C4 and NH3 was introduced into a vacuum container while maintaining the pressure inside the vacuum container at 20 Torr, and a CO2 laser beam was applied to the reaction gas, p: The reaction gas was irradiated under the following conditions: 50 W, P2: 150 W, repetition frequency: 200 Hz, and duty: 50% to cause a gas phase reaction shown in the following formula.
ＴＩＣ、Ｉ−４＋ ＮＨｓ ＋ １／ ２Ｈ２→ＴｉＮ
＋４ＨＣｆこのようにしてＴｉＮからなる超微粒子を製
造した。この超微粒子の純度は９９．９９％以上で、且
つ粒度分布は１５〜２５μｍであった。又、化学組成に
ついては化学量論的なＴｉＮであった。TIC, I-4+ NHs + 1/2H2→TiN
+4HCf In this way, ultrafine particles made of TiN were produced. The purity of the ultrafine particles was 99.99% or more, and the particle size distribution was 15 to 25 μm. Furthermore, the chemical composition was stoichiometric TiN.
以上説明したように、この発明によれば、平均粒径が小
さく且つ粒度分布が狭く、しかも、均質且つ高純度の超
微粒子を製造することができるといったきわめて有用な
効果がもたらされる。As explained above, the present invention brings about extremely useful effects such as being able to produce ultrafine particles with a small average particle size and narrow particle size distribution, and which are homogeneous and highly pure.
第１図は、この発明の一実施態様を示す概略断面図、第
２図は、レーザ出力と時間との関係を示すグラフである
。図面において、
１・・・真空容器、 ２・・・反応ガス、３・・
・レーザビーム、 ４・・・超微粒子。FIG. 1 is a schematic sectional view showing one embodiment of the present invention, and FIG. 2 is a graph showing the relationship between laser output and time. In the drawings, 1... vacuum container, 2... reaction gas, 3...
・Laser beam, 4...Ultrafine particles.
Claims (1)
圧力に維持しながら導入し、レーザビームを前記真空容
器内の反応ガスによるパルス的に照射して気相反応を起
こさせ、かくして、超微粒子を得ることを特徴とする、
超微粒子の製造方法。A reaction gas is introduced into a vacuum container while maintaining the pressure in the vacuum container at a predetermined pressure, and a laser beam is irradiated with the reaction gas in the vacuum container in a pulsed manner to cause a gas phase reaction, thus, characterized by obtaining ultrafine particles,
Method for producing ultrafine particles.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| JP62056781A JPS63224732A (en) | 1987-03-13 | 1987-03-13 | Production of ultrafine particles |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| JP62056781A JPS63224732A (en) | 1987-03-13 | 1987-03-13 | Production of ultrafine particles |
Publications (1)
| Publication Number | Publication Date |
|---|---|
| JPS63224732A true JPS63224732A (en) | 1988-09-19 |
Family
ID=13036971
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| JP62056781A Pending JPS63224732A (en) | 1987-03-13 | 1987-03-13 | Production of ultrafine particles |
Country Status (1)
| Country | Link |
|---|---|
| JP (1) | JPS63224732A (en) |
Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| FR2877591A1 (en) * | 2004-11-09 | 2006-05-12 | Commissariat Energie Atomique | SYSTEM AND PROCESS FOR PRODUCING CONTINUOUS FLOW OF NANOMETRIC OR SUB-MICROMETRIC POWDERS UNDER LASER PYROLYSIS |
-
1987
- 1987-03-13 JP JP62056781A patent/JPS63224732A/en active Pending
Cited By (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| FR2877591A1 (en) * | 2004-11-09 | 2006-05-12 | Commissariat Energie Atomique | SYSTEM AND PROCESS FOR PRODUCING CONTINUOUS FLOW OF NANOMETRIC OR SUB-MICROMETRIC POWDERS UNDER LASER PYROLYSIS |
| WO2006051233A1 (en) * | 2004-11-09 | 2006-05-18 | Commissariat A L'energie Atomique | System and method for continuous flow production of nanometric or sub-micrometric powders by the action of a pyrolytic laser |
| US8822878B2 (en) | 2004-11-09 | 2014-09-02 | Commissariat A L'energie Atomique | Production of nanometric or sub-micrometric powders in continuous flux |
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