JPH086128B2 - How to make an ultrafine particle suspension - Google Patents
How to make an ultrafine particle suspensionInfo
- Publication number
- JPH086128B2 JPH086128B2 JP2172985A JP17298590A JPH086128B2 JP H086128 B2 JPH086128 B2 JP H086128B2 JP 2172985 A JP2172985 A JP 2172985A JP 17298590 A JP17298590 A JP 17298590A JP H086128 B2 JPH086128 B2 JP H086128B2
- Authority
- JP
- Japan
- Prior art keywords
- suspension
- particles
- make
- particle suspension
- ultrafine particle
- 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
- 239000011882 ultra-fine particle Substances 0.000 title claims description 17
- 239000000725 suspension Substances 0.000 title claims description 16
- 238000000034 method Methods 0.000 claims description 17
- 239000007791 liquid phase Substances 0.000 claims description 6
- 239000002904 solvent Substances 0.000 claims description 6
- 239000011343 solid material Substances 0.000 claims description 4
- 239000000919 ceramic Substances 0.000 claims description 2
- 239000007769 metal material Substances 0.000 claims description 2
- 239000002245 particle Substances 0.000 description 11
- 239000007787 solid Substances 0.000 description 8
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 description 4
- 239000011521 glass Substances 0.000 description 4
- 238000006243 chemical reaction Methods 0.000 description 3
- 238000007796 conventional method Methods 0.000 description 3
- 238000001816 cooling Methods 0.000 description 3
- 230000000694 effects Effects 0.000 description 3
- 238000001704 evaporation Methods 0.000 description 3
- 230000008020 evaporation Effects 0.000 description 3
- 238000010574 gas phase reaction Methods 0.000 description 3
- 239000012535 impurity Substances 0.000 description 3
- 238000004519 manufacturing process Methods 0.000 description 3
- MCMNRKCIXSYSNV-UHFFFAOYSA-N Zirconium dioxide Chemical compound O=[Zr]=O MCMNRKCIXSYSNV-UHFFFAOYSA-N 0.000 description 2
- 150000001875 compounds Chemical class 0.000 description 2
- 239000012798 spherical particle Substances 0.000 description 2
- 239000000126 substance Substances 0.000 description 2
- 239000012808 vapor phase Substances 0.000 description 2
- 238000001947 vapour-phase growth Methods 0.000 description 2
- 229910001369 Brass Inorganic materials 0.000 description 1
- 150000004703 alkoxides Chemical class 0.000 description 1
- 230000015572 biosynthetic process Effects 0.000 description 1
- 239000010951 brass Substances 0.000 description 1
- 239000003054 catalyst Substances 0.000 description 1
- 238000005234 chemical deposition Methods 0.000 description 1
- 238000009388 chemical precipitation Methods 0.000 description 1
- 238000000975 co-precipitation Methods 0.000 description 1
- 239000000356 contaminant Substances 0.000 description 1
- 238000011109 contamination Methods 0.000 description 1
- 238000010586 diagram Methods 0.000 description 1
- 239000010419 fine particle Substances 0.000 description 1
- 230000007062 hydrolysis Effects 0.000 description 1
- 238000006460 hydrolysis reaction Methods 0.000 description 1
- 230000001678 irradiating effect Effects 0.000 description 1
- 230000001788 irregular Effects 0.000 description 1
- 239000007788 liquid Substances 0.000 description 1
- 239000000696 magnetic material Substances 0.000 description 1
- 239000008204 material by function Substances 0.000 description 1
- 239000012071 phase Substances 0.000 description 1
- 230000000704 physical effect Effects 0.000 description 1
- 238000000053 physical method Methods 0.000 description 1
- 239000000843 powder Substances 0.000 description 1
- 238000001556 precipitation Methods 0.000 description 1
- 238000002360 preparation method Methods 0.000 description 1
- 150000003839 salts Chemical class 0.000 description 1
- 239000010409 thin film Substances 0.000 description 1
Landscapes
- Glanulating (AREA)
- Manufacture Of Metal Powder And Suspensions Thereof (AREA)
Description
【発明の詳細な説明】 産業上の利用分野 粒径の極めて小さな（１μｍ以下）超微粒子は、磁性
体、触媒、センサーなどの機能性材料として利用されて
いる。本発明はこのような超微粒子の懸濁液を作成する
方法に関するものである。DETAILED DESCRIPTION OF THE INVENTION Industrial field Ultrafine particles having an extremely small particle size (1 μm or less) are used as functional materials such as magnetic materials, catalysts and sensors. The present invention relates to a method for producing such a suspension of ultrafine particles.
従来の技術 超微粒子の作成方法としては、化学的な反応を利用す
る方法と物理的方法の二種類に大きく分けることができ
る。化学的方法には液相からの超微粒子製造法として共
沈法、アルコキシド加水分解法等が知られているが、共
存塩が不純物として混入すること、沈澱形成時に特定成
分が分離あるいは溶解するなどの問題点がある。気相折
出法をはじめとする物理的生成法、あるいは気相での化
学反応を用いる気相化学折出法は、生成物が高純度であ
ること、あるいは雰囲気による反応条件の制御ができる
ことなど多くの特徴を有するが、生成した粒子の補集方
法の問題を解決する必要がある。すなわち粒子の融合や
粗大化が起こりやすく、一度集めた微粒子を再び個々の
粒子にまで完全に分散させることは困難である。超微粒
子の工業的応用においては、粉体自体としてではなく、
懸濁液として、たとえば薄膜形成等に使用されるが、超
微粒子の表面エネルギーが大きいために、懸濁液の作成
に困難をともなうことが多い。2. Description of the Related Art Conventional methods for producing ultrafine particles can be broadly classified into two types: a method utilizing a chemical reaction and a physical method. Co-precipitation method, alkoxide hydrolysis method, etc. are known as chemical methods for producing ultrafine particles from a liquid phase, but coexisting salts are mixed as impurities, and specific components are separated or dissolved during precipitation formation. There is a problem. Physical production methods such as vapor phase deposition method, or vapor phase chemical deposition method using chemical reaction in vapor phase, the product has high purity, or the reaction conditions can be controlled by the atmosphere. Although it has many features, there is a need to solve the problem of how to collect the particles produced. That is, the particles are likely to be fused or coarsened, and it is difficult to completely disperse the once-collected fine particles into individual particles. In industrial application of ultrafine particles, not as the powder itself,
As a suspension, it is used, for example, for forming a thin film, but it is often difficult to prepare a suspension because the surface energy of ultrafine particles is large.
発明が解決しようとする問題点 本発明は、真空装置、あるいは気相反応装置のような
複雑な装置を用いることなく簡便に、しかも混入不純物
の少ない、また多様な展開が可能な超微粒子懸濁液の作
成方法を提供することを目的とするものである。DISCLOSURE OF THE INVENTION Problems to be Solved by the Invention The present invention is an ultrafine particle suspension that can be easily and without a complicated apparatus such as a vacuum apparatus or a gas phase reaction apparatus, has few impurities, and can be developed in various ways. It is intended to provide a method for preparing a liquid.
問題点を解決するための手段 本発明者は、高密度のレーザー光を液相中で試料に照
射することにより、超微粒子懸濁液を作成することが可
能であることを見出し、この知見に基づいて本発明を成
すに至った。Means for Solving Problems The present inventors have found that it is possible to prepare an ultrafine particle suspension by irradiating a sample with a high-density laser beam in a liquid phase, and based on this finding The present invention has been completed based on this.
すなわち、本発明は、金属材料、セラミックス焼結体
をはじめとする固体試料を、液相中に保持し、高密度の
レーザー光を照射することにより、固体試料を蒸発、プ
ラズマ化し、液相中で急激に冷却することにより、超微
粒子の懸濁液を作成する方法を提供するものである。こ
の方法によれば、溶媒および試料以外の不純物、あるい
は汚染源を導入することなく懸濁液を作成することが可
能となる。また、化学的沈殿法で必要な特殊な化合物、
あるいは気相法で必要となる真空装置や気相反応装置を
用いることなく、直接的に液相で懸濁液を作成可能とな
り、多くの固体材料と溶媒の組み合わせによる超微粒子
の懸濁液作成方法となる。That is, the present invention holds a solid sample such as a metal material or a ceramics sintered body in a liquid phase and irradiates it with a high-density laser beam to evaporate the solid sample into a plasma, thereby making it in the liquid phase. It provides a method for preparing a suspension of ultrafine particles by rapidly cooling with. According to this method, a suspension can be prepared without introducing impurities other than the solvent and the sample, or a contamination source. In addition, special compounds required for chemical precipitation,
Alternatively, it is possible to directly create a suspension in the liquid phase without using a vacuum device or a gas phase reaction device, which is required in the gas phase method, and create a suspension of ultrafine particles by combining many solid materials and solvents. Be the way.
実施例 次に添付図面に従って本発明の実施例を説明する。第
１図は本発明の実施方法の１例の要部を示すものであ
る。固体試料:1はガラス容器:2のなかの溶媒:3中に保持
される。レーザー光:4はガラス容器の下から、レンズ:5
で集光され、固体試料に照射される。固体試料は特定位
置のみが蒸発することをさけるためにモーター:7で回転
運動を行う様にする。Embodiments Next, embodiments of the present invention will be described with reference to the accompanying drawings. FIG. 1 shows an essential part of an example of a method for carrying out the present invention. Solid sample: 1 is kept in solvent: 3 in glass container: 2. Laser light: 4 from under the glass container, lens: 5
It is focused on and irradiated onto a solid sample. The solid sample is rotated by a motor: 7 to prevent evaporation only at a specific position.
以下の実施例は第１図の装置を用いて行ったものであ
る。レーザーにはＱ−スイッチのNd:YAGレーザーを使用
した。The following examples were carried out using the apparatus of FIG. A Q-switched Nd: YAG laser was used as the laser.
第２図は、エタノール中に保持したしんちゅうから本
発明により作成した、超微粒子懸濁液を、スライドガラ
ス上で乾燥し、走査型電子顕微鏡（SEM）で観測して得
た粒子構造を示す。数百ナノメートルの球状粒子が観測
できる。従来法における気相折出法では、しんちゅうの
構成元素である銅と亜鉛の高温における蒸気圧が大きく
異なるために、特殊な手法（小田正明、表面科学、８、
337（1987））が必要とされるが、本法では蒸発が瞬時
に起こるため、分別蒸発等による影響は少ない。FIG. 2 shows a particle structure obtained by observing with a scanning electron microscope (SEM) an ultrafine particle suspension prepared by the present invention from brass held in ethanol and dried on a slide glass. . Spherical particles of several hundred nanometers can be observed. In the conventional vapor phase deposition method, a special method (Masada Oda, Surface Science, 8 ,
337 (1987)) is required, but in this method, evaporation occurs instantaneously, so the effect of fractional evaporation is small.
第３図は、エタノール中に保持したジルコニア焼結体
から作成した、懸濁液を第２図と同様の方法で観測した
粒子構造である。球状の粒子とともに不定形粒子が多く
見出される。この結果においては、従来法では、冷却時
間が比較的長いため、結晶性の粒子が形成されやすいこ
とと比較して、急激な冷却に基づくアモルファスな粒子
の形式がかなりあることが特徴として示される。FIG. 3 is a particle structure of a suspension prepared from a zirconia sintered body held in ethanol and observed by the same method as in FIG. Many irregular particles are found with spherical particles. The results show that the conventional method is characterized by the fact that there are a considerable number of amorphous particle types due to rapid cooling, as compared with the tendency that crystalline particles are easily formed due to the relatively long cooling time. .
発明の効果 本発明は、前記したように特殊な化合物や真空装置、
あるいは気相反応装置等を用いることなく固体試料から
直接的に超微粒子懸濁液を作成する方法であり、各種の
固体試料と溶媒の組み合わせにより多様な懸濁液を簡便
に、しかも混入不純物がほとんど入りこまない条件で作
成できる方法である。また、本法により生成する超微粒
子は従来法とは異なった、アモルファス形状のものも多
く含まれており、特異な化学的、物理的特性を示すこと
が期待できる。超微粒子の工業的応用は大きな広がりも
みせているが、本発明による懸濁液作成法は、このよう
な応用において、生成可能な系の多様化、あるいは製造
法の簡便化に大きな効果をもたらす。EFFECTS OF THE INVENTION The present invention, as described above, uses a special compound or a vacuum device,
Alternatively, it is a method of directly producing an ultrafine particle suspension from a solid sample without using a gas phase reaction device, etc., and various suspensions can be easily prepared by combining various solid samples with a solvent, and contaminants can be easily mixed. It is a method that can be created under conditions that hardly enter. In addition, the ultrafine particles produced by this method include many amorphous particles, which are different from the conventional methods, and can be expected to show unique chemical and physical properties. Although the industrial application of ultrafine particles is widespread, the suspension preparation method according to the present invention has a great effect on the diversification of the system capable of producing or the simplification of the production method in such applications. .
第１図は、本発明の実施方法の一例を示す説明図、第２
図及び第３図は第１図の装置を用いて作成した超微粒子
の粒子構造のSEM観察例を示す。 １……固体試料、２……ガラス容器、３……溶媒、４…
…レーザー光、５……レンズ、６……直角プリズム、７
……モータを示す。FIG. 1 is an explanatory diagram showing an example of a method for carrying out the present invention, and FIG.
FIG. 3 and FIG. 3 show SEM observation examples of the particle structure of ultrafine particles prepared by using the apparatus of FIG. 1 ... Solid sample, 2 ... Glass container, 3 ... Solvent, 4 ...
… Laser light, 5 …… Lens, 6 …… Right angle prism, 7
...... Indicates a motor.
Claims (1)
料を液相中に保持し、この固体材料表面に高密度、高出
力のレーザー光を照射することにより、固体材料を蒸
発、プラズマ化する。生成した高温のガス、溶融体を周
囲の溶媒によって急激に冷却、固化することにより超微
粒子として捕集し、懸濁液を作成する方法。1. A solid material such as a metal material or a ceramics sintered body is held in a liquid phase, and the surface of the solid material is irradiated with a high-density, high-power laser beam to evaporate the solid material into plasma. To do. A method in which the generated high-temperature gas and melt are rapidly cooled and solidified by the surrounding solvent to be collected as ultrafine particles to form a suspension.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| JP2172985A JPH086128B2 (en) | 1990-06-29 | 1990-06-29 | How to make an ultrafine particle suspension |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| JP2172985A JPH086128B2 (en) | 1990-06-29 | 1990-06-29 | How to make an ultrafine particle suspension |
Publications (2)
| Publication Number | Publication Date |
|---|---|
| JPH0463203A JPH0463203A (en) | 1992-02-28 |
| JPH086128B2 true JPH086128B2 (en) | 1996-01-24 |
Family
ID=15952038
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| JP2172985A Expired - Lifetime JPH086128B2 (en) | 1990-06-29 | 1990-06-29 | How to make an ultrafine particle suspension |
Country Status (1)
| Country | Link |
|---|---|
| JP (1) | JPH086128B2 (en) |
Families Citing this family (9)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| JP4832668B2 (en) * | 2001-06-13 | 2011-12-07 | トヨタ自動車株式会社 | Manufacturing method of manganese material and manganese material |
| KR100441886B1 (en) * | 2002-04-19 | 2004-07-27 | 학교법인 포항공과대학교 | Method and apparatus for generating nanoparticles |
| WO2004080586A1 (en) * | 2003-03-07 | 2004-09-23 | Hamamatsu Photonics K.K. | Fine particles, method and device for preparation thereof, and agent for parenteral injection and method for production thereof |
| JP4846248B2 (en) * | 2004-02-27 | 2011-12-28 | 学校法人東京理科大学 | A method for producing fine crystal grains, a method for producing a solid obtained by dispersing the fine crystal grains, a transparent luminescent liquid for biosensing, and a transparent luminescent solid. |
| JP4943851B2 (en) * | 2004-09-15 | 2012-05-30 | 国立大学法人京都大学 | Method for producing metal fine particles |
| KR100759286B1 (en) * | 2005-04-06 | 2007-09-17 | 한국지질자원연구원 | Method for preparing zirconium-iron-vanadium alloy nanopowder using laser ablation |
| WO2007106444A2 (en) * | 2006-03-13 | 2007-09-20 | University Of Alabama At Birmingham Research Foundation | Electrically pumped broadly tunable mid-infrared lasers based on quantum confined transition metal doped semiconductors |
| CN100457335C (en) * | 2006-12-19 | 2009-02-04 | 浙江工业大学 | Device of preparing metal nanometer particle colloid by liquid phase medium pulse laser ablation |
| US8246714B2 (en) * | 2009-01-30 | 2012-08-21 | Imra America, Inc. | Production of metal and metal-alloy nanoparticles with high repetition rate ultrafast pulsed laser ablation in liquids |
Family Cites Families (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| JPS61136606A (en) * | 1984-12-06 | 1986-06-24 | Toyobo Co Ltd | Production of ultrafine powder |
-
1990
- 1990-06-29 JP JP2172985A patent/JPH086128B2/en not_active Expired - Lifetime
Also Published As
| Publication number | Publication date |
|---|---|
| JPH0463203A (en) | 1992-02-28 |
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Legal Events
| Date | Code | Title | Description |
|---|---|---|---|
| EXPY | Cancellation because of completion of term |