JPS63267431A - Preparation of ultrafine particles - Google Patents
Preparation of ultrafine particlesInfo
- Publication number
- JPS63267431A JPS63267431A JP9982487A JP9982487A JPS63267431A JP S63267431 A JPS63267431 A JP S63267431A JP 9982487 A JP9982487 A JP 9982487A JP 9982487 A JP9982487 A JP 9982487A JP S63267431 A JPS63267431 A JP S63267431A
- Authority
- JP
- Japan
- Prior art keywords
- ultrafine particles
- arc
- raw material
- pure water
- electrode
- 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 50
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims abstract description 24
- 239000002994 raw material Substances 0.000 claims abstract description 22
- 239000007788 liquid Substances 0.000 claims abstract description 10
- 238000004519 manufacturing process Methods 0.000 claims description 8
- 239000007864 aqueous solution Substances 0.000 claims description 7
- 238000000034 method Methods 0.000 claims description 7
- 235000014113 dietary fatty acids Nutrition 0.000 claims description 6
- 229930195729 fatty acid Natural products 0.000 claims description 6
- 239000000194 fatty acid Substances 0.000 claims description 6
- 150000004665 fatty acids Chemical class 0.000 claims description 6
- 239000002245 particle Substances 0.000 abstract description 14
- 238000009826 distribution Methods 0.000 abstract description 8
- 230000015572 biosynthetic process Effects 0.000 abstract description 2
- LNCDZGSESVBWGF-UHFFFAOYSA-N octadecanoic acid;hydrate Chemical compound O.CCCCCCCCCCCCCCCCCC(O)=O LNCDZGSESVBWGF-UHFFFAOYSA-N 0.000 abstract 1
- 239000007789 gas Substances 0.000 description 14
- 238000005054 agglomeration Methods 0.000 description 5
- 230000002776 aggregation Effects 0.000 description 5
- 238000001816 cooling Methods 0.000 description 3
- 230000000694 effects Effects 0.000 description 3
- 229910052751 metal Inorganic materials 0.000 description 3
- 239000002184 metal Substances 0.000 description 3
- XKRFYHLGVUSROY-UHFFFAOYSA-N Argon Chemical compound [Ar] XKRFYHLGVUSROY-UHFFFAOYSA-N 0.000 description 2
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 description 2
- 239000012159 carrier gas Substances 0.000 description 2
- 239000000919 ceramic Substances 0.000 description 2
- 238000010586 diagram Methods 0.000 description 2
- 238000005516 engineering process Methods 0.000 description 2
- VBICKXHEKHSIBG-UHFFFAOYSA-N 1-monostearoylglycerol Chemical compound CCCCCCCCCCCCCCCCCC(=O)OCC(O)CO VBICKXHEKHSIBG-UHFFFAOYSA-N 0.000 description 1
- RYGMFSIKBFXOCR-UHFFFAOYSA-N Copper Chemical compound [Cu] RYGMFSIKBFXOCR-UHFFFAOYSA-N 0.000 description 1
- DCXXMTOCNZCJGO-UHFFFAOYSA-N Glycerol trioctadecanoate Natural products CCCCCCCCCCCCCCCCCC(=O)OCC(OC(=O)CCCCCCCCCCCCCCCCC)COC(=O)CCCCCCCCCCCCCCCCC DCXXMTOCNZCJGO-UHFFFAOYSA-N 0.000 description 1
- 241000238413 Octopus Species 0.000 description 1
- 241000277269 Oncorhynchus masou Species 0.000 description 1
- 241000287530 Psittaciformes Species 0.000 description 1
- 235000021355 Stearic acid Nutrition 0.000 description 1
- 229910000831 Steel Inorganic materials 0.000 description 1
- ATJFFYVFTNAWJD-UHFFFAOYSA-N Tin Chemical compound [Sn] ATJFFYVFTNAWJD-UHFFFAOYSA-N 0.000 description 1
- 239000002253 acid Substances 0.000 description 1
- 239000000654 additive Substances 0.000 description 1
- 239000000956 alloy Substances 0.000 description 1
- 229910045601 alloy Inorganic materials 0.000 description 1
- 229910052786 argon Inorganic materials 0.000 description 1
- 239000003795 chemical substances by application Substances 0.000 description 1
- 239000011248 coating agent Substances 0.000 description 1
- 238000000576 coating method Methods 0.000 description 1
- 150000001875 compounds Chemical class 0.000 description 1
- 238000009833 condensation Methods 0.000 description 1
- 230000005494 condensation Effects 0.000 description 1
- 238000007796 conventional method Methods 0.000 description 1
- 229910052802 copper Inorganic materials 0.000 description 1
- 239000010949 copper Substances 0.000 description 1
- 238000001035 drying Methods 0.000 description 1
- 235000013399 edible fruits Nutrition 0.000 description 1
- 238000010891 electric arc Methods 0.000 description 1
- 235000019441 ethanol Nutrition 0.000 description 1
- 239000000945 filler Substances 0.000 description 1
- 239000010419 fine particle Substances 0.000 description 1
- -1 first Substances 0.000 description 1
- 239000011261 inert gas Substances 0.000 description 1
- 230000001788 irregular Effects 0.000 description 1
- 239000000463 material Substances 0.000 description 1
- 150000002739 metals Chemical class 0.000 description 1
- 239000000203 mixture Substances 0.000 description 1
- QIQXTHQIDYTFRH-UHFFFAOYSA-N octadecanoic acid Chemical compound CCCCCCCCCCCCCCCCCC(O)=O QIQXTHQIDYTFRH-UHFFFAOYSA-N 0.000 description 1
- OQCDKBAXFALNLD-UHFFFAOYSA-N octadecanoic acid Natural products CCCCCCCC(C)CCCCCCCCC(O)=O OQCDKBAXFALNLD-UHFFFAOYSA-N 0.000 description 1
- 239000002244 precipitate Substances 0.000 description 1
- 238000001556 precipitation Methods 0.000 description 1
- 239000008213 purified water Substances 0.000 description 1
- 230000005855 radiation Effects 0.000 description 1
- 239000008117 stearic acid Substances 0.000 description 1
- 239000010959 steel Substances 0.000 description 1
- 208000024891 symptom Diseases 0.000 description 1
- PHYFQTYBJUILEZ-IUPFWZBJSA-N triolein Chemical compound CCCCCCCC\C=C/CCCCCCCC(=O)OCC(OC(=O)CCCCCCC\C=C/CCCCCCCC)COC(=O)CCCCCCC\C=C/CCCCCCCC PHYFQTYBJUILEZ-IUPFWZBJSA-N 0.000 description 1
- WFKWXMTUELFFGS-UHFFFAOYSA-N tungsten Chemical compound [W] WFKWXMTUELFFGS-UHFFFAOYSA-N 0.000 description 1
- 229910052721 tungsten Inorganic materials 0.000 description 1
- 239000010937 tungsten 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
- B01J19/087—Processes employing the direct application of electric or wave energy, or particle radiation; Apparatus therefor employing electric or magnetic energy
- B01J19/088—Processes employing the direct application of electric or wave energy, or particle radiation; Apparatus therefor employing electric or magnetic energy giving rise to electric discharges
Abstract
Description
【発明の詳細な説明】
〔産業上の利用分野〕
本発明は、各種金属９合金、セラミックスを含む化付物
の超微粒子７ａ−Ｒ造する方法に係り、符に超微粒子の
粒径分布の良好な超微粒子を製造するのに好適な方法に
関する。Detailed Description of the Invention [Industrial Field of Application] The present invention relates to a method for producing ultrafine particles 7a-R of additives containing various metal 9 alloys and ceramics, and particularly to The present invention relates to a method suitable for producing good ultrafine particles.
従来の方法は、特公昭５５−４４１２３号公報に記載の
工９にアーク熱源などを用いてガス気中で超微粒子原材
料の蒸気を発生δせ、搬送ガスで冷却装置へ運び、そし
て超微粒子を捕集するようになっていた。In the conventional method, vapor of ultrafine particle raw material is generated in gas atmosphere using an arc heat source, etc. in step 9 described in Japanese Patent Publication No. 55-44123, and the ultrafine particles are transported to a cooling device using a carrier gas. It was supposed to be collected.
上記従来技術は、超微粒子の原材料から蒸気を発生させ
てから超＃粒子化し、冷却して捕集するまでの過程にお
ける超微粒子の粒成長、凝集について配慮がちれておら
ず、捕集した超微粒子の粒径が不揃いでかつ凝集したも
のが多いという問題があった。すなわち、原材料から発
生した蒸気及び超微粒子は高温でかつ活性であるため、
搬送ガスによって冷却装置に達するまでにお互いに接触
し１粒成長、凝果金起こす。荷にアーク熱源による超微
粒子の生成法ではアーク放電するための雰囲気ガス圧力
は通常数十’ｆｏｒｒ〜大気圧で平均自由行程も小さく
、生成量も比収的多いのでこの傾向が顕者であり、一般
的に第３図に示すような粒径分布となる。The above conventional technology does not pay much attention to the grain growth and agglomeration of ultrafine particles during the process from generating steam from the ultrafine particle raw material to ultrafine particle formation, cooling, and collection. There was a problem that the particle sizes of the fine particles were irregular and many of them were aggregated. In other words, since the steam and ultrafine particles generated from raw materials are hot and active,
By the time the carrier gas reaches the cooling device, they come into contact with each other, causing single grain growth and condensation. In the method of generating ultrafine particles using an arc heat source in a load, the atmospheric gas pressure for arc discharge is usually several tens of forr to atmospheric pressure, the mean free path is small, and the amount produced is relatively large, so this tendency is obvious. Generally, the particle size distribution is as shown in FIG.
本発明の目的は、上記問題点に鑑みなされたものであり
、各種金属、せ金、セラミックスを含む化合物の超微粒
子をアーク熱源τ用いて効率よく生成すると共に、その
粒径分布が良好でかつ凝集の少ない超微粒子を得る方法
を提供することにある。The object of the present invention was made in view of the above-mentioned problems, and it is an object of the present invention to efficiently generate ultrafine particles of compounds containing various metals, fillers, and ceramics using an arc heat source τ, and to have a good particle size distribution. The object of the present invention is to provide a method for obtaining ultrafine particles with little agglomeration.
上ｉ己目的は、超微粒子の原材料と電極とを液中に設け
て電極の回９からシールドガスを流し、かつ、シールド
ガスの回りから脂肪酸を含む水溶液を円筒状に流し、原
材料と電極との間にアークを発生させることによって達
成でれる。The purpose is to place the raw material of ultrafine particles and the electrode in a liquid, flow the shielding gas from the electrode point 9, and flow the aqueous solution containing fatty acids in a cylindrical shape from around the shielding gas to connect the raw material and the electrode. This can be achieved by generating an arc between the
即ち本発明の特徴はアーク熱源を用いて超微粒子を製造
するに際し１ｇ、中に設けた超微粒子の原材料と電極と
の間にアークを発生δせて超微粒子を生成することｆｔ
ｔ＋！ｊ徴とする。That is, the feature of the present invention is that when producing ultrafine particles using an arc heat source, an arc is generated δ between the ultrafine particle raw material provided inside and an electrode to generate ultrafine particles.
T+! J symptoms.
この際、超微粒子の原材料と電極とは共に水中に設ける
ことが望ましい。また電極の回りから７−ルドガスを流
し、かつこのシールドガスの回りから液体を円筒状に流
すことが好ましい。更にこの場合には脂肪酸を言む水溶
液を円筒状に流すことが特に有効である。At this time, it is desirable that both the raw material of the ultrafine particles and the electrode be placed in water. Further, it is preferable to flow a shielding gas from around the electrode and to flow a liquid from around this shielding gas in a cylindrical shape. Furthermore, in this case, it is particularly effective to flow the aqueous solution containing the fatty acid in a cylindrical shape.
超微粒子の原材料と−憔との間にアークを発生さぞ、こ
のアーク熱により、原材料から蒸気全発生させ、超微粒
子を生成ａせゐ。この時磁極の回Ｖから流すシールドガ
ス及び円筒状に流す液体は電極、原材料２よひアーク全
周囲の液体から遮断するように作用する。それによって
アークはカス気中で発生させた時と同様に、女定して発
生するので、連続的に原材料の超微粒子を生成すること
ができる。−万、超微粒子は生成直後に円筒状に流れて
いる液体によって急冷却ちれるので２粒成長することが
なく、このため粒径分布の良好な超微粒子を得ることが
できる。’ｉｆｃ、脂肪酸を宮む水浴液を円筒状に流す
ことによって、超微粒子は急冷却されると同時に、脂肪
酸が被覆される。このため１枚径分布が良好でかつ凝集
のない超微粒子を製造することができる。An arc is generated between the raw material of the ultrafine particles and the gas, and the heat of the arc causes all the steam to be generated from the raw material, producing ultrafine particles. At this time, the shielding gas flowing from the magnetic pole V and the liquid flowing in a cylindrical shape act to cut off the electrode, the raw material 2, and the liquid all around the arc. As a result, the arc is generated in the same way as when it is generated in the air, so ultrafine particles of the raw material can be continuously generated. - Immediately after the ultrafine particles are generated, they are rapidly cooled down by the liquid flowing in a cylindrical shape, so that two particles do not grow, and therefore ultrafine particles with a good particle size distribution can be obtained. 'ifc, by flowing a water bath containing fatty acids in a cylindrical shape, the ultrafine particles are rapidly cooled and at the same time coated with fatty acids. Therefore, it is possible to produce ultrafine particles with a good single-particle diameter distribution and no agglomeration.
し実施例〕
以下１本発明の一実施例を第１図及び第２図にＬｖ説明
する。第１図におい°Ｃ，１は超微粒子原材料、２は電
極、３は鋼ルツボ、４はアーク放′１用を源、５はアー
ク、６は水槽、７は純水、８は２重シールドノズル、９
はシールドガス導入口。Embodiment] An embodiment of the present invention will be explained below with reference to FIGS. 1 and 2. In Figure 1, °C, 1 is an ultrafine particle raw material, 2 is an electrode, 3 is a steel crucible, 4 is a source for arc radiation 1, 5 is an arc, 6 is a water tank, 7 is pure water, 8 is a double shield Nozzle, 9
is the shield gas inlet.
１０は水浴液導入口、１１は純水導入、排出口である。10 is a water bath liquid inlet, and 11 is a pure water inlet and outlet.
超微粒子の生成は、１ず、シールドガス導入口９から不
活性ガスを、水溶液導入口１０から５％ステアリン戚氷
水溶液流し、その後、純水導入口１１から純水７を水槽
６に２重シールドノズル８の端面よシも上まで満たす。To generate ultrafine particles, first, inert gas is flowed through the shield gas inlet 9 and a 5% stearin ice aqueous solution is flowed through the aqueous solution inlet 10, and then pure water 7 is poured into the water tank 6 from the pure water inlet 11. Fill the end face of the shield nozzle 8 to the top.
この方法によシ、超微粒子原材料１及び電極２が純水７
と接触するのを防ぐことができる。すなわち１円筒状に
流した水ｇ液は純水７に対してカーテンの役目を果たし
。By this method, ultrafine particle raw material 1 and electrode 2 are purified water 7
contact can be prevented. That is, the water g liquid flowing in a cylindrical shape acts as a curtain for the pure water 7.
での結果、アークはガス気中で発生した場合と同様の状
態となる。次に超微粒子原材料１と電極２との間に放電
用電源４から電流を供給し、アーク５を発生名せる。こ
のアーク熱により原材料１が浴融し、蒸気が発生し、超
微粒子が生成さγしるが。As a result, the arc will be in the same state as if it were generated in a gas atmosphere. Next, a current is supplied from a discharge power source 4 between the ultrafine particle raw material 1 and the electrode 2 to generate an arc 5. The raw material 1 is melted in the bath by this arc heat, steam is generated, and ultrafine particles are generated.
この時この超微粒子は円筒状に流した水溶液の中を必ず
通り、純水７へ放出ちれる。At this time, the ultrafine particles always pass through the cylindrical aqueous solution and are released into the pure water 7.
−例としてスズの原材料をシールドガスとしてアルゴン
ガス１０ｔ／馴、水浴／ｇ、３ｔ／馴、シールドガスノ
ズル内径１０４１１１φ、水溶液ノズル内径０．５ｍφ
１条件１５０Ａ−２６Ｖでアークを発生させた場＆、そ
の生成ｉは１２０ ｇ／Ｈであり、得られた超微粒子の
粒径分布は第２図の二うになり、その平均粒径は約２Ｏ
ｎＩｎ′ｔ′あった。- For example, using tin raw material as shielding gas, argon gas 10t/g, water bath/g, 3t/stamping, shield gas nozzle inner diameter 104111φ, aqueous solution nozzle inner diameter 0.5mφ
When an arc was generated under one condition of 150A-26V, the generation i was 120 g/H, and the particle size distribution of the obtained ultrafine particles was as shown in Figure 2, and the average particle size was about 2O
There was nIn't'.
筐たこの超微粒子をエチルアルコールと混什し。Mix ultrafine particles of octopus with ethyl alcohol.
超音波で分散して直径１５ａｍφ、昼ざ１５０鵡の試験
管に入れ、超微粒子が沈澱する様子を観察した所、１８
０日独逸しても沈澱は認められなかった。When dispersed with ultrasonic waves and placed in a test tube with a diameter of 15 amφ and 150 parrots at daytime, the precipitation of ultrafine particles was observed.
No precipitate was observed even after 0 days of drying.
尚、脂肪酸としてステアリン酸の他にオレーイン敵、ラ
ワリンハ、ミリスチンは、バルミチル酸でも同様の効果
がある。In addition to stearic acid as fatty acids, olein, rawinha, myristic, and valmicylic acid have similar effects.
本矢施例に工ｔＬば、平均粒匝２０ ｎ ｒｎの粒径分
布が良好でかつ凝集のない金属超微板子が得られる効果
かめる。In this example, we can see the effect of obtaining ultrafine metal plates with a good particle size distribution of an average grain size of 20 nm and no agglomeration.
なおアーク源としてはタングステン４極アークの他にプ
ラズマアークでも開鎖の幼果が侍すれる。In addition to the tungsten quadrupole arc, a plasma arc can also be used as an arc source.
本発明方法によれば、Ａ！ｉ倣枚子を生成した直仮に急
ｒｖ却し、同時に六−乞肩慎物で被覆することかでさる
ので、筏径分布が良好で凝集のない安定な超微粒子を得
０ことかでさる。ｌｆｃ装置を非常に簡略化することが
できる。According to the method of the present invention, A! It is possible to obtain stable ultrafine particles with a good raft diameter distribution and no agglomeration by immediately discarding the imitated particles and simultaneously coating them with a six-layered material. . The IFC device can be greatly simplified.
易１図は本発明の超微粒子の製造方法の一実施例に係る
製造装置の模式断面図、第２図は同実施例による粒径と
粒子数比との関係を示す特性図。
第３図μ従来技術による粒儀と粒子数比との関係を示す
特性図である。
１・・・超微粒子原材料、２・・・電極、３・・・銅ル
ツボ。
ドノズル。
ノ ・″・ゝ・１、・□ ′ｊ５１
代理人 升埋士 小川勝男 （、二′Ｌ、、１弔 ／
Σ
） 二車シールトノス゛ル
Ｉ！Ｊ ２ 起
第３ＥFIG. 1 is a schematic cross-sectional view of a manufacturing apparatus according to an embodiment of the method for producing ultrafine particles of the present invention, and FIG. 2 is a characteristic diagram showing the relationship between particle size and particle number ratio according to the same embodiment. FIG. 3 μ is a characteristic diagram showing the relationship between grain size and particle number ratio according to the prior art. 1... Ultrafine particle raw material, 2... Electrode, 3... Copper crucible. Do nozzle.
ノ ・″・ゝ・1,・□ ′j51 Agent: Masu buryer Katsuo Ogawa (,2′L,,1 condolence /
Σ) Motorcycle seal nozzle I! J 2 Ki No. 3E
Claims (1)
て、液中に設けた超微粒子の原材料と電極との間にアー
クを発生させて超微粒子を生成することを特徴とする超
微粒子の製造方法。 ２、超微粒子の原材料と前記電極とを水中に設けること
を特徴とする特許請求の範囲第１項記載の超微粒子の製
造方法。 ３、前記電極の回りからシールドガスを流し、かつ該シ
ールドガスの回りから液体を円筒状に流すようにしたこ
とを特徴とする特許請求の範囲第１項または第２項記載
の超微粒子の製造方法。 ４、脂肪酸を含む水溶液を円筒状に流すようにしたこと
を特徴とする特許請求の範囲第３項記載の超微粒子の製
造方法。[Claims] 1. A method for producing ultrafine particles using an arc heat source, characterized by generating ultrafine particles by generating an arc between an electrode and a raw material for ultrafine particles provided in a liquid. A method for producing ultrafine particles. 2. The method for producing ultrafine particles according to claim 1, characterized in that the raw material for the ultrafine particles and the electrode are provided in water. 3. Production of ultrafine particles according to claim 1 or 2, characterized in that a shielding gas is caused to flow from around the electrode, and a liquid is caused to flow from around the shielding gas in a cylindrical shape. Method. 4. The method for producing ultrafine particles according to claim 3, characterized in that the aqueous solution containing fatty acids is caused to flow in a cylindrical shape.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| JP9982487A JPS63267431A (en) | 1987-04-24 | 1987-04-24 | Preparation of ultrafine particles |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| JP9982487A JPS63267431A (en) | 1987-04-24 | 1987-04-24 | Preparation of ultrafine particles |
Publications (1)
| Publication Number | Publication Date |
|---|---|
| JPS63267431A true JPS63267431A (en) | 1988-11-04 |
Family
ID=14257573
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| JP9982487A Pending JPS63267431A (en) | 1987-04-24 | 1987-04-24 | Preparation of ultrafine particles |
Country Status (1)
| Country | Link |
|---|---|
| JP (1) | JPS63267431A (en) |
Cited By (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US5460701A (en) * | 1993-07-27 | 1995-10-24 | Nanophase Technologies Corporation | Method of making nanostructured materials |
| WO2003037553A1 (en) * | 2001-10-29 | 2003-05-08 | Phild Co., Ltd. | Method and apparatus for the production of metal powder |
| JP2009519125A (en) * | 2005-12-13 | 2009-05-14 | コミッサリア タ レネルジー アトミーク | Devices and methods for producing nanometer and submicrometer scale particulate suspensions |
| US8128789B2 (en) | 2001-10-12 | 2012-03-06 | Phiten Co., Ltd. | Method for producing ultrafine dispersion water of noble metal ultrafine particles |
-
1987
- 1987-04-24 JP JP9982487A patent/JPS63267431A/en active Pending
Cited By (7)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US5460701A (en) * | 1993-07-27 | 1995-10-24 | Nanophase Technologies Corporation | Method of making nanostructured materials |
| US5874684A (en) * | 1993-07-27 | 1999-02-23 | Nanophase Technologies Corporation | Nanocrystalline materials |
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