JPH03264610A - Manufacture of super fine particles - Google Patents
Manufacture of super fine particlesInfo
- Publication number
- JPH03264610A JPH03264610A JP2065419A JP6541990A JPH03264610A JP H03264610 A JPH03264610 A JP H03264610A JP 2065419 A JP2065419 A JP 2065419A JP 6541990 A JP6541990 A JP 6541990A JP H03264610 A JPH03264610 A JP H03264610A
- Authority
- JP
- Japan
- Prior art keywords
- fine particles
- super fine
- plasma
- ultrafine particles
- carrier 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.)
- Granted
Links
- 238000004519 manufacturing process Methods 0.000 title claims description 9
- 239000010419 fine particle Substances 0.000 title abstract 5
- 229910052751 metal Inorganic materials 0.000 claims abstract description 14
- 239000002184 metal Substances 0.000 claims abstract description 14
- 239000000178 monomer Substances 0.000 claims abstract description 13
- 238000000034 method Methods 0.000 claims abstract description 11
- 239000011882 ultra-fine particle Substances 0.000 claims description 39
- 229910045601 alloy Inorganic materials 0.000 claims description 4
- 239000000956 alloy Substances 0.000 claims description 4
- 150000002736 metal compounds Chemical class 0.000 claims description 4
- 239000012808 vapor phase Substances 0.000 claims description 4
- 238000006116 polymerization reaction Methods 0.000 claims description 3
- 239000012159 carrier gas Substances 0.000 abstract description 11
- 238000006243 chemical reaction Methods 0.000 abstract description 5
- 239000011248 coating agent Substances 0.000 abstract description 3
- 238000000576 coating method Methods 0.000 abstract description 3
- 238000011109 contamination Methods 0.000 abstract description 3
- 230000005684 electric field Effects 0.000 abstract description 3
- 238000010438 heat treatment Methods 0.000 abstract description 3
- 230000006698 induction Effects 0.000 abstract description 3
- 230000003647 oxidation Effects 0.000 abstract description 3
- 238000007254 oxidation reaction Methods 0.000 abstract description 3
- 230000000379 polymerizing effect Effects 0.000 abstract 1
- 238000001947 vapour-phase growth Methods 0.000 abstract 1
- 239000007789 gas Substances 0.000 description 23
- 239000002245 particle Substances 0.000 description 15
- 150000002739 metals Chemical class 0.000 description 10
- XKRFYHLGVUSROY-UHFFFAOYSA-N Argon Chemical compound [Ar] XKRFYHLGVUSROY-UHFFFAOYSA-N 0.000 description 8
- PPBRXRYQALVLMV-UHFFFAOYSA-N Styrene Chemical compound C=CC1=CC=CC=C1 PPBRXRYQALVLMV-UHFFFAOYSA-N 0.000 description 6
- 239000012071 phase Substances 0.000 description 6
- VGGSQFUCUMXWEO-UHFFFAOYSA-N Ethene Chemical compound C=C VGGSQFUCUMXWEO-UHFFFAOYSA-N 0.000 description 5
- 239000005977 Ethylene Substances 0.000 description 5
- QGZKDVFQNNGYKY-UHFFFAOYSA-N Ammonia Chemical compound N QGZKDVFQNNGYKY-UHFFFAOYSA-N 0.000 description 4
- 229910021529 ammonia Inorganic materials 0.000 description 4
- 229910052786 argon Inorganic materials 0.000 description 4
- 230000000694 effects Effects 0.000 description 4
- UHOVQNZJYSORNB-UHFFFAOYSA-N Benzene Chemical compound C1=CC=CC=C1 UHOVQNZJYSORNB-UHFFFAOYSA-N 0.000 description 3
- QVGXLLKOCUKJST-UHFFFAOYSA-N atomic oxygen Chemical compound [O] QVGXLLKOCUKJST-UHFFFAOYSA-N 0.000 description 3
- 239000000919 ceramic Substances 0.000 description 3
- 239000012535 impurity Substances 0.000 description 3
- 239000001301 oxygen Substances 0.000 description 3
- 229910052760 oxygen Inorganic materials 0.000 description 3
- 239000011253 protective coating Substances 0.000 description 3
- IJGRMHOSHXDMSA-UHFFFAOYSA-N Atomic nitrogen Chemical compound N#N IJGRMHOSHXDMSA-UHFFFAOYSA-N 0.000 description 2
- CURLTUGMZLYLDI-UHFFFAOYSA-N Carbon dioxide Chemical compound O=C=O CURLTUGMZLYLDI-UHFFFAOYSA-N 0.000 description 2
- 229910000727 Fe4N Inorganic materials 0.000 description 2
- UFHFLCQGNIYNRP-UHFFFAOYSA-N Hydrogen Chemical compound [H][H] UFHFLCQGNIYNRP-UHFFFAOYSA-N 0.000 description 2
- BAPJBEWLBFYGME-UHFFFAOYSA-N Methyl acrylate Chemical compound COC(=O)C=C BAPJBEWLBFYGME-UHFFFAOYSA-N 0.000 description 2
- -1 SiH4 Chemical class 0.000 description 2
- 230000004075 alteration Effects 0.000 description 2
- 238000004581 coalescence Methods 0.000 description 2
- 238000010586 diagram Methods 0.000 description 2
- 238000010894 electron beam technology Methods 0.000 description 2
- 239000011261 inert gas Substances 0.000 description 2
- 239000002923 metal particle Substances 0.000 description 2
- VNWKTOKETHGBQD-UHFFFAOYSA-N methane Chemical compound C VNWKTOKETHGBQD-UHFFFAOYSA-N 0.000 description 2
- XDTMQSROBMDMFD-UHFFFAOYSA-N Cyclohexane Chemical compound C1CCCCC1 XDTMQSROBMDMFD-UHFFFAOYSA-N 0.000 description 1
- OTMSDBZUPAUEDD-UHFFFAOYSA-N Ethane Chemical compound CC OTMSDBZUPAUEDD-UHFFFAOYSA-N 0.000 description 1
- 229910017061 Fe Co Inorganic materials 0.000 description 1
- 229910001030 Iron–nickel alloy Inorganic materials 0.000 description 1
- 229910005091 Si3N Inorganic materials 0.000 description 1
- BLRPTPMANUNPDV-UHFFFAOYSA-N Silane Chemical compound [SiH4] BLRPTPMANUNPDV-UHFFFAOYSA-N 0.000 description 1
- XTXRWKRVRITETP-UHFFFAOYSA-N Vinyl acetate Chemical compound CC(=O)OC=C XTXRWKRVRITETP-UHFFFAOYSA-N 0.000 description 1
- VVTSZOCINPYFDP-UHFFFAOYSA-N [O].[Ar] Chemical compound [O].[Ar] VVTSZOCINPYFDP-UHFFFAOYSA-N 0.000 description 1
- HSFWRNGVRCDJHI-UHFFFAOYSA-N alpha-acetylene Natural products C#C HSFWRNGVRCDJHI-UHFFFAOYSA-N 0.000 description 1
- 230000005540 biological transmission Effects 0.000 description 1
- 229910002092 carbon dioxide Inorganic materials 0.000 description 1
- 239000001569 carbon dioxide Substances 0.000 description 1
- UUAGAQFQZIEFAH-UHFFFAOYSA-N chlorotrifluoroethylene Chemical group FC(F)=C(F)Cl UUAGAQFQZIEFAH-UHFFFAOYSA-N 0.000 description 1
- 229910052804 chromium Inorganic materials 0.000 description 1
- 229910052802 copper Inorganic materials 0.000 description 1
- 238000002003 electron diffraction Methods 0.000 description 1
- GCSJLQSCSDMKTP-UHFFFAOYSA-N ethenyl(trimethyl)silane Chemical compound C[Si](C)(C)C=C GCSJLQSCSDMKTP-UHFFFAOYSA-N 0.000 description 1
- 125000002534 ethynyl group Chemical group [H]C#C* 0.000 description 1
- 230000008020 evaporation Effects 0.000 description 1
- 238000001704 evaporation Methods 0.000 description 1
- 229920001002 functional polymer Polymers 0.000 description 1
- 229910052737 gold Inorganic materials 0.000 description 1
- NEXSMEBSBIABKL-UHFFFAOYSA-N hexamethyldisilane Chemical compound C[Si](C)(C)[Si](C)(C)C NEXSMEBSBIABKL-UHFFFAOYSA-N 0.000 description 1
- UQEAIHBTYFGYIE-UHFFFAOYSA-N hexamethyldisiloxane Chemical compound C[Si](C)(C)O[Si](C)(C)C UQEAIHBTYFGYIE-UHFFFAOYSA-N 0.000 description 1
- 239000001257 hydrogen Substances 0.000 description 1
- 229910052739 hydrogen Inorganic materials 0.000 description 1
- 150000002500 ions Chemical class 0.000 description 1
- JEIPFZHSYJVQDO-UHFFFAOYSA-N iron(III) oxide Inorganic materials O=[Fe]O[Fe]=O JEIPFZHSYJVQDO-UHFFFAOYSA-N 0.000 description 1
- 229910052748 manganese Inorganic materials 0.000 description 1
- 239000012528 membrane Substances 0.000 description 1
- 229910044991 metal oxide Inorganic materials 0.000 description 1
- 150000004706 metal oxides Chemical class 0.000 description 1
- 229910052759 nickel Inorganic materials 0.000 description 1
- 150000004767 nitrides Chemical class 0.000 description 1
- 229910052757 nitrogen Inorganic materials 0.000 description 1
- 239000011146 organic particle Substances 0.000 description 1
- 230000000704 physical effect Effects 0.000 description 1
- 229910052697 platinum Inorganic materials 0.000 description 1
- 239000002994 raw material Substances 0.000 description 1
- 229910052709 silver Inorganic materials 0.000 description 1
- 229910052718 tin Inorganic materials 0.000 description 1
- UHUUYVZLXJHWDV-UHFFFAOYSA-N trimethyl(methylsilyloxy)silane Chemical compound C[SiH2]O[Si](C)(C)C UHUUYVZLXJHWDV-UHFFFAOYSA-N 0.000 description 1
- 229910052721 tungsten Inorganic materials 0.000 description 1
- 229910052720 vanadium Inorganic materials 0.000 description 1
- 230000008016 vaporization Effects 0.000 description 1
Landscapes
- Physical Or Chemical Processes And Apparatus (AREA)
- Manufacture Of Metal Powder And Suspensions Thereof (AREA)
- Powder Metallurgy (AREA)
Abstract
Description
【発明の詳細な説明】
〔産業上の利用分野〕
本発明は、超微粒子の製造方法に関する。更に詳しくは
、金属類からの気相生成法による超微粒子の製造方法に
関する。DETAILED DESCRIPTION OF THE INVENTION [Field of Industrial Application] The present invention relates to a method for producing ultrafine particles. More specifically, the present invention relates to a method for producing ultrafine particles from metals using a gas phase production method.
金属、合金、金属化合物などの金属類を種々の熱源によ
って蒸発させ、原子状態またはクラスター状態となし、
それがキャリヤーガスによって冷却される過程で凝集し
、超微粒子を形成する気相生成法が従来から行われてお
り、その際不活性ガス中で蒸発させると金属超微粒子が
、また反応性ガス中で蒸発させると各種セラミックス超
微粒子がそれぞれ生成する。Evaporates metals such as metals, alloys, and metal compounds using various heat sources to form atomic or cluster states,
A gas phase generation method has traditionally been used in which metal particles coagulate during the process of being cooled by a carrier gas and form ultrafine particles, and when evaporated in an inert gas, ultrafine metal particles can be When evaporated, various types of ultrafine ceramic particles are generated.
このようにして行われる超微粒子の気相生成法において
は、超微粒子の生成後期または捕集時に超微粒子の表面
活性により粒子同志が合体したり、あるいは大気中に取
り出されたときに酸化されたり、汚染されたりするとい
う問題がみられる。In the gas phase generation method of ultrafine particles carried out in this way, particles may coalesce together due to surface activity of the ultrafine particles during the late stage of generation or during collection, or may be oxidized when taken out into the atmosphere. There are problems such as contamination.
本発明の目的は、超微粒子同志の合体を防止しかつそれ
が大気中に取り出されたとき酸化、汚染などの変質を生
じさせない超微粒子の製造方法を提供することにある。An object of the present invention is to provide a method for producing ultrafine particles that prevents coalescence of ultrafine particles and does not cause alteration such as oxidation or pollution when the particles are taken out into the atmosphere.
かかる本発明の目的は、気相生成した超微粒子の表面を
有機物モノマーのプラズマ重合膜で被覆することにより
達成されることが見出された。It has been found that the object of the present invention can be achieved by coating the surfaces of ultrafine particles produced in a vapor phase with a plasma polymerized film of an organic monomer.
従って、本発明は超微粒子の製造方法に係り、超微粒子
の製造は、金属、合金または金属化合物から気相生成法
で超微粒子を生成させるに際し、有機物モノマーのプラ
ズマ重合雰囲気中で超微粒子を気相生成させることによ
り行われる。Therefore, the present invention relates to a method for producing ultrafine particles, and the production of ultrafine particles involves vaporizing ultrafine particles in an atmosphere of plasma polymerization of organic monomers when producing ultrafine particles from metals, alloys, or metal compounds by a gas phase generation method. This is done by phase generation.
超微粒子形成原料となる金属としては、例えばＦｅ、
Ｃｏ、 Ｎｉ、 Ａｇ、 Ａｕ、 Ｓｎ、 Ｗ、 Ｖ、
Ｃｒ、 Ｍｎ、 Ａｎ、Ｃｕ、 Ｐｔなどが、合金と
しては例えばＦｅ−Ｎｉ、Ｆｅ−Ｃｏ、Ｇｏ−Ｎｉなど
が、また金属化合物としては例えばＳｉＨ４，ＴｉＣＱ
４、ＩｎＣ（１３、ＳｉＣＱ ４． Ａ Ｄ、 ＣＱ
３．５ｎＣｆｌ、、 Ｖ（１，、ＭｏＣＱ、、Ｆｅ
（Ｇｏ） 、、Ｃｒ（Ｃｏ）、。Examples of metals used as raw materials for forming ultrafine particles include Fe,
Co, Ni, Ag, Au, Sn, W, V,
Cr, Mn, An, Cu, Pt, etc., alloys such as Fe-Ni, Fe-Co, Go-Ni, etc., metal compounds such as SiH4, TiCQ, etc.
4, InC (13, SiCQ 4. A D, CQ
3.5nCfl,,V(1,,MoCQ,,Fe
(Go), Cr(Co),.
Ｆｅ（ＣｓＨｓ）ｚなどがそれぞれ用いられる。Fe(CsHs)z, etc. are used, respectively.
これらの金属類を種々の熱源で加熱蒸発させ、それを冷
却して超微粒子を形成させ、同時にプラズマ重合膜を形
成させる際に用いられるキャリヤーガスとしては、アル
ゴン、窒素、水素などの不活性ガスあるいはアルゴン−
酸素混合ガス、水素−アンモニア混合ガス、水素−アン
モニアー二酸化炭素混合ガスなどの反応性ガスが、それ
ぞれ全圧的１〜１００Ｐａで用いられる。反応性ガスの
場合、例えばアルゴン−酸素混合ガスでは酸素の分圧が
全圧の約５〜５部のとき、Ｆｅ２Ｏ３、ＳｎＯ□、■ｎ
２０３．１ｌＩＯ３、Ｍ２Ｏ３、ＣｒＯ□、ＳｉＯ□、
ＡＱ２０３などの金属酸化物（セラミックス）超微粒子
を、また水素−アンモニア混合ガスではアンモニアの分
圧が全圧の約１０％以上のとき、Ｆｅ４Ｎ、 Ｓｉ３Ｎ
４’、 Ａ Ｑ Ｎなどの金属窒化物（セラミックス）
超微粒子をそれぞれ生成させる。Inert gases such as argon, nitrogen, and hydrogen are used as carrier gases to heat and evaporate these metals using various heat sources, cool them to form ultrafine particles, and simultaneously form plasma polymerized films. Or argon
Reactive gases such as oxygen mixed gas, hydrogen-ammonia mixed gas, and hydrogen-ammonia carbon dioxide mixed gas are used at a total pressure of 1 to 100 Pa, respectively. In the case of reactive gases, for example, in the case of argon-oxygen mixed gas, when the partial pressure of oxygen is about 5 to 5 parts of the total pressure, Fe2O3, SnO□, ■n
203.1lIO3, M2O3, CrO□, SiO□,
Ultrafine particles of metal oxides (ceramics) such as AQ203, or in hydrogen-ammonia mixed gas, when the partial pressure of ammonia is about 10% or more of the total pressure, Fe4N, Si3N
4', Metal nitrides (ceramics) such as AQN
Generate ultrafine particles.
この際の有機物モノマーのプラズマ重合雰囲気中での超
微粒子の気相生成は、次のようにして行われる。即ち、
キャリヤーガスを流しながら反応容器内を真空排気し、
０．１Ｔｏｒｒ程度に減圧したキャリヤーガスに高周波
電源から電界を印加すると、キャリヤーガスはイオン化
してプラズマを形成する。そのプラズマ発生域内にセッ
トした金属類蒸気はイオンと衝突して冷却され、合体し
て粒成長し、超微粒子を形成する。それと同時に、プラ
ズマ発生域内に有機物モノマーを導入すると、生成した
超微粒子の表面はプラズマ重合膜によって被覆される。At this time, the gas phase generation of ultrafine particles in the plasma polymerization atmosphere of organic monomers is performed as follows. That is,
Evacuate the inside of the reaction vessel while flowing carrier gas,
When an electric field is applied from a high frequency power source to the carrier gas whose pressure has been reduced to about 0.1 Torr, the carrier gas is ionized to form plasma. The metal vapor set within the plasma generation area collides with ions, is cooled, coalesces, and grows into grains to form ultrafine particles. At the same time, when an organic monomer is introduced into the plasma generation area, the surfaces of the generated ultrafine particles are covered with a plasma polymerized film.
図面の第１図は、本発明方法の一態様の概要図であり、
真空計１を備えた反応容器２内にキャリヤーガスボンベ
３からキャリヤーガスを流しながら真空排気し、減圧し
たキャリヤーガスに高周波３
電源４から電界を印加してプラズマを発生させ、それと
同時に有機物モノマータンク５から有機物子ツマ−を導
入すると、加熱用誘導コイル６によって加熱されたルツ
ボ７内に収容されていた金属類８は蒸発すると共にプラ
ズマ重合膜によって被覆され、真空排気系９側の捕集系
１０でプラズマ重合膜被覆超微粒子として捕集される。FIG. 1 of the drawings is a schematic diagram of one embodiment of the method of the present invention,
A reaction vessel 2 equipped with a vacuum gauge 1 is evacuated while flowing a carrier gas from a carrier gas cylinder 3, and an electric field is applied to the reduced pressure carrier gas from a high frequency power source 4 to generate plasma, and at the same time, an organic monomer tank 5 When the organic particles are introduced from the heating induction coil 6, the metals 8 housed in the crucible 7 are evaporated and covered with a plasma polymerized film, and the metals 8 are heated by the heating induction coil 6 and are covered with a plasma polymerized film. The particles are collected as ultrafine particles coated with plasma polymerized membrane.
プラズマ重合膜被覆形成に用いられる有機物モノマーと
しては、例えばエチレン、アセチレン、ベンゼン、スチ
レン、メタン、エタン、シクロヘキサン、酢酸ビニル、
メチルアクリレート、ヘキサメチルジシラン、テトラメ
チルジシロキサン、ヘキサメチルジシロキサン、ビニル
トリメチルシラン、クロロトリフルオロエチレンなどが
用いられ、生成した超微粒子の表面に約２０Å以上の被
膜を形成させる。Examples of organic monomers used to form a plasma-polymerized film include ethylene, acetylene, benzene, styrene, methane, ethane, cyclohexane, vinyl acetate,
Methyl acrylate, hexamethyldisilane, tetramethyldisiloxane, hexamethyldisiloxane, vinyltrimethylsilane, chlorotrifluoroethylene, etc. are used to form a film of about 20 Å or more on the surface of the produced ultrafine particles.
本発明方法においては、次のような効果が奏せられる。 The method of the present invention provides the following effects.
（１）超微粒子は、それの生成時の状態のままで、− 表面保護被覆を形成させることができる。(1) Ultrafine particles remain in the state in which they were created, - A surface protective coating can be formed.
（２）形成された表面保護被覆は、超微粒子同志の合体
を防止しかつ大気中に取り出されても酸化や汚染などの
変質を起さない。(2) The formed surface protective coating prevents coalescence of ultrafine particles and does not cause alteration such as oxidation or contamination even when taken out into the atmosphere.
（３）一般の気相法による超微粒子の生成では、粒径の
コントロールが殆んど不可能で、数１００人程度迄粒成
長してしまうが、本発明方法によれば、表面保護被覆膜
が粒成長を抑える効果をも示すため、金属類の蒸発速度
とモノマーの流量とをコントロールすることにより、数
１０〜数１００人の範囲内で粒径をコントロールするこ
とができる。このような粒径範囲では、超微粒子の物性
が粒径によっては大きく左右される。(3) In the production of ultrafine particles using a general vapor phase method, it is almost impossible to control the particle size and the particles grow to about several hundred particles, but according to the method of the present invention, the surface protective coating can be applied. Since the film also exhibits the effect of suppressing grain growth, by controlling the evaporation rate of metals and the flow rate of monomer, the grain size can be controlled within the range of several tens to several hundred. In such a particle size range, the physical properties of the ultrafine particles are greatly influenced by the particle size.
（４）機能性重合膜で表面被覆することにより、超微粒
子表面に種々の機能を付与することができる。(4) By coating the surface with a functional polymer film, various functions can be imparted to the surface of the ultrafine particles.
次に、実施例について本発明を説明する。 Next, the present invention will be explained with reference to examples.
実施例１
第１図に示された装置を用い、まず装置内の全混合ガス
圧力を約１０Ｐａに制御する。混合ガスは、酸素分圧４
Ｐａのアルゴンガスで、それを約１０ｍＱ１分の流量で
流している。そこに、周波数１３．５６ＭＨｚの高周波
を有効電力１０１Ｎで印加してプラズマ放電させ、その
状態でスチレンモノマーガスを約５ｍｕ１分の流量で流
しなからＳｎを蒸発させると、膜厚約２０Å以上のスチ
レンプラズマ重合膜で表面被覆された、粒径約１００Å
以上のＳｎＯ□超微粒子が得られた。得られた超微粒子
は合体せず、それぞれが孤立粒子として存在していた。Example 1 Using the apparatus shown in FIG. 1, first, the total mixed gas pressure in the apparatus was controlled to about 10 Pa. The mixed gas has an oxygen partial pressure of 4
Argon gas of Pa is flowing at a flow rate of about 10 mQ1 minute. A high frequency wave with a frequency of 13.56 MHz and an effective power of 101 N is applied to create a plasma discharge, and in this state, styrene monomer gas is flowed at a flow rate of about 5 μl to evaporate Sn, resulting in a styrene film with a thickness of about 20 Å or more. Particle size approximately 100 Å, surface coated with plasma polymerized film
The above SnO□ ultrafine particles were obtained. The obtained ultrafine particles did not coalesce and each existed as an isolated particle.
また、その超微粒子は、ＴＥＭ （透過型電子顕微鏡）
観察および電子線回折により、不純物を含んでいないこ
とが確認された。In addition, the ultrafine particles can be seen using a TEM (transmission electron microscope)
It was confirmed by observation and electron diffraction that it contained no impurities.
実施例２
実施例１において、混合ガスの代わりに同圧のアルゴン
ガスを、スチレンモノマーガスの代わりに同量のエチレ
ンモノマーガスを、またＳｎの代わりにＦｅをそれぞれ
用いると、膜厚約２０人のエチレンプラズマ重合膜で表
面被覆された、粒径約１００人のＦｅ超微粒子が得られ
た。得られた超微粒子は合体せず、それぞれが孤立粒子
として存在していた。その超微粒子は、ＴＥＭ観察、電
子線回折および磁気的特性により、不純物を含んでいな
いこと、また大気中に取り出しても酸化されないことが
確認された。Example 2 In Example 1, if the same pressure of argon gas was used instead of the mixed gas, the same amount of ethylene monomer gas was used instead of the styrene monomer gas, and Fe was used instead of Sn, the film thickness was approximately 20 mm. Fe ultrafine particles with a particle size of approximately 100 μm were obtained, the surface of which was coated with an ethylene plasma polymerized film. The obtained ultrafine particles did not coalesce and each existed as an isolated particle. It was confirmed by TEM observation, electron beam diffraction and magnetic properties that the ultrafine particles did not contain any impurities and were not oxidized even when taken out into the atmosphere.
実施例３
第１図に示された装置を用い、まず装置内の全混合ガス
圧力を約１００Ｐａに制御する。混合ガスは、アンモニ
ア分圧２２．５Ｐａ、二酸化炭素分圧２．５Ｐａの水素
ガスで、それを約１０Ｏｎ＋ Ｉｌ／分の流量で流して
いる。そこに、周波数１３．５６ＭＨｚの高周波を有効
電力９０Ｗで印加してプラズマ放電させ、その状態でエ
チレンモノマーガスを約５０ｍ ｎ ／分の流量で流し
ながらＦｅ （Ｃ５Ｈ，）、、を蒸発させると、膜厚約
２０Å以上のエチレンプラズマ重合膜で表面被覆された
、粒径約１００Å以上のＦｅ４Ｎ超微粒子が得られた。Example 3 Using the apparatus shown in FIG. 1, first, the total mixed gas pressure in the apparatus was controlled to about 100 Pa. The mixed gas is hydrogen gas with an ammonia partial pressure of 22.5 Pa and a carbon dioxide partial pressure of 2.5 Pa, which is flowed at a flow rate of about 10 On+Il/min. A high frequency wave with a frequency of 13.56 MHz and an effective power of 90 W is applied thereto to cause plasma discharge, and in this state, Fe (C5H,) is evaporated while flowing ethylene monomer gas at a flow rate of about 50 m n /min. Fe4N ultrafine particles with a particle size of about 100 Å or more were obtained whose surface was coated with an ethylene plasma polymerized film with a film thickness of about 20 Å or more.
得られた超微粒子は合体せず、それぞれが孤立粒子とし
て存在していた。その超微粒子は、ＴＥＭ観察、電子線
回折および磁気的特性により、不純物を含んでいないこ
と、また大気中に取り出しても酸化されないことが確認
された。The obtained ultrafine particles did not coalesce and each existed as an isolated particle. It was confirmed by TEM observation, electron beam diffraction and magnetic properties that the ultrafine particles did not contain any impurities and were not oxidized even when taken out into the atmosphere.
第１図は、本発明方法の一態様の概要図である。 （符号の説明） ２・・・・・反応容器 ３・・・・・キャリヤーガスボンベ ４・・・・・高周波電源 ５・・・・・有機物モノマータンク ７・・・・・ルツボ ８・・・・・溶融金属類 １０・・・・・超微粒子捕集系 − FIG. 1 is a schematic diagram of one embodiment of the method of the present invention. (Explanation of symbols) 2...Reaction container 3...Carrier gas cylinder 4...High frequency power supply 5...Organic monomer tank 7... Crucible 8... Molten metals 10...Ultrafine particle collection system −
Claims (1)
粒子を生成させるに際し、有機物モノマーのプラズマ重
合雰囲気中で超微粒子を気相生成させることを特徴とす
る超微粒子の製造方法。1. A method for producing ultrafine particles, which is characterized in that when ultrafine particles are generated from a metal, alloy, or metal compound by a vapor phase generation method, the ultrafine particles are generated in a vapor phase in an atmosphere of plasma polymerization of an organic monomer.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| JP2065419A JP3008433B2 (en) | 1990-03-15 | 1990-03-15 | Ultrafine particle manufacturing method |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| JP2065419A JP3008433B2 (en) | 1990-03-15 | 1990-03-15 | Ultrafine particle manufacturing method |
Publications (2)
| Publication Number | Publication Date |
|---|---|
| JPH03264610A true JPH03264610A (en) | 1991-11-25 |
| JP3008433B2 JP3008433B2 (en) | 2000-02-14 |
Family
ID=13286518
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| JP2065419A Expired - Lifetime JP3008433B2 (en) | 1990-03-15 | 1990-03-15 | Ultrafine particle manufacturing method |
Country Status (1)
| Country | Link |
|---|---|
| JP (1) | JP3008433B2 (en) |
Cited By (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US5560800A (en) * | 1994-08-31 | 1996-10-01 | Mobil Oil Corporation | Protective coating for pressure-activated adhesives |
| WO2005075132A1 (en) * | 2004-02-04 | 2005-08-18 | Ebara Corporation | Composite nanoparticle and process for producing the same |
| JP2007522347A (en) * | 2004-02-16 | 2007-08-09 | クライマックス・エンジニアード・マテリアルズ・エルエルシー | Method and apparatus for producing silver nanoparticles |
| JP2011524245A (en) * | 2008-05-19 | 2011-09-01 | エボニック デグサ ゲーエムベーハー | Phase transition method of matter |
-
1990
- 1990-03-15 JP JP2065419A patent/JP3008433B2/en not_active Expired - Lifetime
Cited By (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US5560800A (en) * | 1994-08-31 | 1996-10-01 | Mobil Oil Corporation | Protective coating for pressure-activated adhesives |
| WO2005075132A1 (en) * | 2004-02-04 | 2005-08-18 | Ebara Corporation | Composite nanoparticle and process for producing the same |
| US7799425B2 (en) | 2004-02-04 | 2010-09-21 | Ebara Corporation | Composite nanoparticles method for producing the same |
| JP2007522347A (en) * | 2004-02-16 | 2007-08-09 | クライマックス・エンジニアード・マテリアルズ・エルエルシー | Method and apparatus for producing silver nanoparticles |
| JP2011524245A (en) * | 2008-05-19 | 2011-09-01 | エボニック デグサ ゲーエムベーハー | Phase transition method of matter |
Also Published As
| Publication number | Publication date |
|---|---|
| JP3008433B2 (en) | 2000-02-14 |
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