JPH06339625A - Preparation of particle thin film - Google Patents
Preparation of particle thin filmInfo
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- JPH06339625A JPH06339625A JP12984093A JP12984093A JPH06339625A JP H06339625 A JPH06339625 A JP H06339625A JP 12984093 A JP12984093 A JP 12984093A JP 12984093 A JP12984093 A JP 12984093A JP H06339625 A JPH06339625 A JP H06339625A
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- thin film
- particle
- film
- particles
- liquid
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Abstract
Description
【０００１】[0001]
【産業上の利用分野】この発明は、粒子薄膜の製造法に
関するものである。さらに詳しくは、この発明は、エレ
クトロニクス、バイオマテリアル、セラミック、金属材
料等の諸分野において、新たな機能性材料の創製と、物
理化学プロセスの新しい展開等にとって有用な、新しい
粒子薄膜の製造法に関するものである。BACKGROUND OF THE INVENTION 1. Field of the Invention The present invention relates to a method for producing a particle thin film. More specifically, the present invention relates to a method for producing a new particle thin film, which is useful for the creation of new functional materials and the new development of physicochemical processes in various fields such as electronics, biomaterials, ceramics and metallic materials. It is a thing.
【０００２】[0002]
【従来の技術とその課題】従来より、原子、分子レベル
の物質や微粒子の集積構造を制御する技術として各種の
方法が知られており、たとえば、物質を原子、分子レベ
ルで面方向に二次元的に配設する方法としては、真空蒸
着法、スパッタリング法、電気メッキ、ＬＢ薄膜形成法
などが知られており、また、微粒子（タンパク質、酸化
物、金属、ラテックス、ポリマー）のレベルでは微粒子
エマルジョンを平面に塗布する方法（スピンコート法
等）や、微粒子を粉末として平面に散布する方法（噴霧
法等）、分散媒から気液界面、液々界面に微粒子を析出
する方法等が知られており、工業的にも重要な手段とし
て様々な工夫、改良が試みられてきてる。しかしなが
ら、実際には、従来の技術によっては、微粒子について
その集積構造を高精度に、かつ迅速に形成及び制御する
ことはそれほど簡単なことではなかった。2. Description of the Related Art Conventionally, various methods have been known as techniques for controlling the integrated structure of substances or fine particles at the atomic or molecular level. Vacuum deposition, sputtering, electroplating, LB thin film formation, and the like are known as methods for arranging the particles in a uniform manner, and at the level of fine particles (protein, oxide, metal, latex, polymer), fine particle emulsion. Is known to be applied on a flat surface (spin coating method, etc.), a method of spraying fine particles as a powder on a flat surface (spraying method, etc.), a method of depositing fine particles from a dispersion medium on a gas-liquid interface or a liquid-liquid interface Therefore, various ideas and improvements have been tried as industrially important means. However, in reality, according to the conventional technique, it is not so easy to form and control the integrated structure of the fine particles with high precision and speed.
【０００３】そこで、この発明の発明者は、従来技術の
限界を克服し、一粒子の層を、規則正しく一様に並べ、
かつ、この構造化を迅速に行うことのできる全く新しい
高精度、高効率な微粒子２次元構造の形成・制御方法を
提案した。これは、微粒子分散液を平坦な固体基板上に
展開し、分散液を構成する液状媒体の厚みを制御し、メ
ニスカス力を生成させて、微粒子を二次元で凝集制御す
ることを特徴としている。この方法は、これまでにない
全く新しい方法として、科学的、そして技術的に注目さ
れるものであるが、この方法の場合には、対象となる粒
子の大きさの下限が固体基板の表面粗さで限定されてお
り、たとえばガラス基板等では、小さな粒径の微粒子
（０．１μｍ以下）をきれいな二次元膜として凝集制御
することができないという課題があった。Therefore, the inventor of the present invention overcomes the limitations of the prior art and arranges layers of one particle in a regular and even manner.
In addition, we have proposed a completely new method of forming and controlling a two-dimensional fine particle structure with high precision and efficiency, which enables rapid structuring. This is characterized in that the fine particle dispersion is spread on a flat solid substrate, the thickness of the liquid medium constituting the dispersion is controlled, a meniscus force is generated, and the fine particles are two-dimensionally aggregated and controlled. This method has attracted scientific and technical attention as a completely new method that has never existed before.However, in the case of this method, the lower limit of the particle size of interest is the surface roughness of the solid substrate. However, there is a problem that fine particles (0.1 μm or less) having a small particle diameter cannot be aggregated and controlled as a clean two-dimensional film on a glass substrate or the like.
【０００４】この点を解決するためには、水銀を展開基
板とし、水銀面のなめらかさによって微粒子からより大
きな粒径の粒子に至るまでの任意の大きさの粒子の薄膜
を作成することが可能でもある。この方法も、この発明
者らによって提案されている。しかしながら、一方で、
水銀を用いる方法には、 １）人体に有害な物質であるため、健康上の問題が発生
すること、 ２）清浄面作りが難しいこと、 ３）作られた粒子薄膜を他の固体基板に転写することが
必要であること、 等の欠点があった。In order to solve this point, it is possible to use mercury as a developing substrate and to form a thin film of particles of any size from fine particles to particles having a larger particle diameter due to the smoothness of the mercury surface. But also. This method is also proposed by the inventors. However, on the other hand,
In the method using mercury, 1) there is a health problem because it is a harmful substance to the human body, 2) it is difficult to make a clean surface, 3) the formed particle thin film is transferred to another solid substrate It was necessary to do so.
【０００５】この発明は、以上の通りの事情に鑑みてな
されたものであり、前記の欠点を解消し、水銀を展開基
板とすることなく、健康上の害もなく、簡便に清浄面に
任意の粒径の粒子を薄膜として形成することのできる新
しい粒子薄膜の製造法を提供することを目的としてい
る。The present invention has been made in view of the above circumstances, solves the above-mentioned drawbacks, does not use mercury as a developing substrate, has no health hazard, and can be easily and conveniently cleaned. It is an object of the present invention to provide a new method for producing a particle thin film capable of forming particles having the same particle size as a thin film.
【０００６】[0006]
【課題を解決するための手段】この発明は、上記の課題
を解決するものとして、担持用基板上に液体膜を配設し
た後にこの液体膜上に粒子分散液を液体膜と混合するこ
となく展開し、分散媒と液体膜とを蒸発させて担持用基
板上に粒子薄膜を形成することを特徴とする粒子薄膜の
製造法を提供する。In order to solve the above-mentioned problems, the present invention provides a liquid film on a supporting substrate without mixing a particle dispersion liquid with the liquid film on the liquid film. Provided is a method for producing a particle thin film, which comprises developing and evaporating a dispersion medium and a liquid film to form a particle thin film on a supporting substrate.
【０００７】[0007]
【作用】すなわち、この発明の製造法においては、従来
法のように、基板表面上に直接粒子分散液を展開するこ
とや、もしくは水銀基板上に粒子分散液を展開し、次い
で固体基板に粒子を転写担持させることもなく、固体基
板上にあらかじめ配設した液体膜の作用によって、より
簡便に、精度よく、かつ、効率的に粒子の二次元凝集薄
膜を形成する。That is, in the production method of the present invention, as in the conventional method, the particle dispersion is directly spread on the surface of the substrate, or the particle dispersion is spread on the mercury substrate and then the particles are spread on the solid substrate. A two-dimensional aggregated thin film of particles can be formed more simply, accurately, and efficiently by the action of a liquid film previously arranged on a solid substrate without transferring and carrying.
【０００８】より具体的には、この発明では、まず各種
の固体基板上に、液体膜を配設する。次いでこの液体膜
の上に粒子分散液を展開し、その後、分散液の分散媒と
液体膜そのものを蒸発させる。その結果、固体基板、つ
まりこの発明の担持用固体基板上に凝集された粒子の薄
膜を形成させる。この方法においては、液体膜を、従来
法の水銀と同様のものとして代替させ、かつ、水銀とは
本質的に相異して、粒子薄膜形成後には蒸発させてしま
うことになる。More specifically, in the present invention, first, a liquid film is provided on various solid substrates. Next, the particle dispersion liquid is spread on the liquid film, and then the dispersion medium of the dispersion liquid and the liquid film itself are evaporated. As a result, a thin film of agglomerated particles is formed on the solid substrate, that is, the solid substrate for carrying of the present invention. In this method, the liquid film is replaced with the same one as the mercury used in the conventional method, and it is essentially different from mercury, and is evaporated after the formation of the particle thin film.
【０００９】このため、液体膜は、粒子分散液の媒体と
相溶性のないもの、あるいは相溶性の乏しいものであっ
て、かつ、分散媒よりも比重の大きなものが使用され
る。そして易蒸発性のものを使用する。粒子そのもの
は、金属、無機、有機、それらの複合物からなる任意の
粒子が使用でき、分散媒としても水、有機溶媒等の各種
のものが適宜に使用されることから、粒子と分散媒との
組合わせに応じて、この液体膜を構成することができ
る。For this reason, the liquid film is used that is incompatible with the medium of the particle dispersion liquid or is poor in compatibility and has a larger specific gravity than the dispersion medium. And the one that is easily evaporated is used. As the particles themselves, any particles made of metal, inorganic, organic, or a composite thereof can be used, and as the dispersion medium, various things such as water and organic solvent are appropriately used. This liquid film can be configured according to the combination of
【００１０】たとえば、より具体的に例示すると、各種
の分散媒に対して汎用なものとして、液体膜には弗化炭
化水素またはそれらの誘導体が使用できる。（ポリ）フ
ルオロハイドロカーボン、（ポリ）フルオロエーテル、
（ポリ）フルオロエステル、（ポリ）フルオロ（ポリ）
クロロハイドロカーボン、（ポリ）フルオロ（ポリ）ク
ロロエーテル等の各種のものが例示される。For example, more specifically, fluorocarbons or derivatives thereof can be used for the liquid film as a general-purpose liquid for various dispersion media. (Poly) fluorohydrocarbon, (poly) fluoroether,
(Poly) fluoroester, (poly) fluoro (poly)
Examples include various substances such as chlorohydrocarbon and (poly) fluoro (poly) chloroether.
【００１１】これらは単一または複数種の混合物として
使用してもよいし、分散媒との濡れ性を向上するため
に、（ポリ）フルオロアミン、（ポリ）フルオロエーテ
ルアミン、フルオロエステルスルホネート等の弗化界面
活性剤やフルオロアルコール等をさらに添加してもよ
い。液体膜の膜厚については、特に限定されることはな
いが、微粒子薄膜の形成時には、通常は、１mm以下程度
とするのが好ましい。These may be used alone or as a mixture of two or more kinds, and in order to improve the wettability with a dispersion medium, (poly) fluoroamine, (poly) fluoroetheramine, fluoroester sulfonate, etc. may be used. A fluorinated surfactant or fluoroalcohol may be further added. The thickness of the liquid film is not particularly limited, but it is usually preferable to set it to about 1 mm or less when forming the fine particle thin film.
【００１２】たとえばこのような液体膜の使用によっ
て、水銀表面と同様の平坦さを確保することができ、固
体基板の表面粗さに依存することなく、各種粒径の粒子
の薄膜形成が可能となる。蒸発は自然蒸発、もしくは加
熱によってもよい。図１および図２は、この発明の方法
による薄膜製造を例示した概念図であって、図１は、弗
化炭化水素（フッ化オイル）液体膜上に展開した分散媒
中の粒子が凝集していく様子を示したものである。フッ
化オイルは、水や有機溶媒に不溶であるため、粒子分散
媒中の粒子は、異なる２つの媒体にはさまれることによ
って、毛管力や蒸発による粒子凝集が起こり、薄膜が生
成される。この凝集の原理については、すでにこの発明
者が報告している。また、フッ化オイルは、高い蒸発性
を持つため、その蒸発によって、図２のように、担持用
固体基板上に粒子薄膜が形成、担持される。For example, by using such a liquid film, it is possible to secure the same flatness as the surface of mercury, and it is possible to form a thin film of particles of various particle sizes without depending on the surface roughness of the solid substrate. Become. Evaporation may be natural evaporation or heating. 1 and 2 are conceptual views illustrating thin film production by the method of the present invention. In FIG. 1, particles in a dispersion medium spread on a fluorohydrocarbon (fluorinated oil) liquid film are aggregated. It shows how it goes. Since the fluorinated oil is insoluble in water or an organic solvent, the particles in the particle dispersion medium are sandwiched between two different media, which causes particle aggregation due to capillary force or evaporation to form a thin film. The inventor has already reported the principle of this aggregation. Further, since the fluorinated oil has a high evaporative property, a thin film of particles is formed and carried on the carrying solid substrate by the evaporation as shown in FIG.
【００１３】なお、上記フッ化オイルは、生物学的に不
活性であるため、人体への影響はない。もちろん、上記
の弗化炭化水素（フッ化オイル）を用いる場合でも、図
１に示した媒体、すなわち媒体Ｉ、媒体II（粒子分散液
媒体）、媒体III （フッ化オイル他）と基板との組合わ
せについては各種可能であって、たとえば表１に示すこ
ともできる。Since the fluorinated oil is biologically inactive, it does not affect the human body. Of course, even when the above-mentioned fluorohydrocarbon (fluorinated oil) is used, the medium shown in FIG. 1, that is, medium I, medium II (particle dispersion medium), medium III (fluorinated oil, etc.), and the substrate Various combinations are possible and can be shown in Table 1, for example.
【００１４】[0014]
【表１】 [Table 1]
【００１５】また、この発明において固体基板上に形成
担持された粒子薄膜は、加熱、光照射、化学反応等の各
種手段によって基板と、そして粒子相互とも固定するこ
とができ、これを各種応用することや、さらには、三次
元の粒子薄膜の積層形成も可能とする。粒子分散液の混
合比については、特に限定されないが、通常は、容積比
で０．１〜０．００１程度とするのが好ましい。In the present invention, the particle thin film formed and supported on the solid substrate can be fixed to the substrate and to each other by various means such as heating, light irradiation, chemical reaction, etc. In addition, it is possible to form a three-dimensional particle thin film laminated layer. The mixing ratio of the particle dispersion is not particularly limited, but it is usually preferable to set the volume ratio to about 0.1 to 0.001.
【００１６】そして、この発明者がすでに提案している
ように、粒径の異なる粒子による所定の面パターンの粒
子凝集からなる薄膜もこの発明の方法によって形成され
る。以下実施例を示し、さらにこの発明について詳しく
説明する。As already proposed by the present inventor, a thin film formed by agglomeration of particles having a predetermined surface pattern by particles having different particle sizes is also formed by the method of the present invention. Hereinafter, the present invention will be described in detail with reference to examples.
【００１７】[0017]
【実施例】図３は、この発明の方法を実施するための装
置概念図の一例を示したものである。たとえばこの図３
に例示したように、この装置では、担持用固体基板
（３）の上に液体膜（２）を塗布等の手段によって薄く
配設し、さらにその上に、水性粒子分散液（１）を展開
する。その後、支持台（５）によって支えられたテフロ
ンセル（４）とセルカバー（６）とで囲われた中の窒素
ガス等の雰囲気ガス（７）のガス圧、及び水蒸気圧を適
度に制御することによって、分散液（１）の媒体の蒸発
によって液膜厚を減少させて粒子を凝集させ、粒子の薄
膜を形成するとともに液体膜（２）の蒸発によって、転
写担持用固体基板（３）に粒子薄膜を形成担持する。DETAILED DESCRIPTION OF THE PREFERRED EMBODIMENTS FIG. 3 shows an example of an apparatus conceptual diagram for carrying out the method of the present invention. For example, this Figure 3
In this device, as illustrated in FIG. 2, the liquid film (2) is thinly arranged on the supporting solid substrate (3) by means such as coating, and the aqueous particle dispersion liquid (1) is further spread thereon. To do. Thereafter, the gas pressure of the atmospheric gas (7) such as nitrogen gas surrounded by the Teflon cell (4) supported by the support table (5) and the cell cover (6) and the water vapor pressure are controlled appropriately. As a result, the liquid film thickness is reduced by the evaporation of the medium of the dispersion liquid (1) to agglomerate the particles to form a thin film of the particles, and the liquid film (2) is evaporated to form the solid substrate for transfer transfer (3). Form and support a particle thin film.
【００１８】実際に、この装置を用い、 perfluorometh
yldecaline（ＰＦＭＤ）（〜１００μｌ）を使用して液
体膜（〜１mm）とし、粒子として、１．７μｍのポリエ
チレン球を使用して、その容積比０．０１〜０．００１
程度の水性分散液（〜５０μｌ）を使用して粒子薄膜を
形成した。液体膜のための前記ＰＦＭＤ（ローンプーラ
ンＳ．Ａ．，pp−７）の物性は次の通りであった。Actually, using this device, perfluorometh
yldecaline (PFMD) (~ 100 μl) was used as a liquid film (~ 1 mm), 1.7 μm polyethylene spheres were used as particles, and the volume ratio was 0.01-0.001.
A particle thin film was formed using about 50 μl of the aqueous dispersion. The physical properties of the PFMD (Lone Poulin SA, pp-7) for the liquid film were as follows.
【００１９】ρ25°＝ １．９４ｇ／cm3 Ｔｂ ＝ １４１℃ Ｔｍ ＝ −１０℃ Ｍｗ ＝ ５１２．０７Ｄａ 表面張力（空気）＝ １９．２ｍＮ／ｍ 表面張力（水） ＝ ５３．４ｍＮ／ｍ また、ガス雰囲気として窒素（Ｎ2 ）を使用し、その圧
力は１気圧とした。自然蒸発によって粒子薄膜を形成し
た。Ρ 25 ° = 1.94 g / cm 3 Tb = 141 ° C Tm = -10 ° C Mw = 512.07 Da Surface tension (air) = 19.2 mN / m Surface tension (water) = 53.4 mN / m Nitrogen (N 2 ) was used as the gas atmosphere, and the pressure was 1 atm. A particle thin film was formed by spontaneous evaporation.
【００２０】図４は、１．７μｍポリスチレン球が島状
の凝集体としてＰＦＭＤ上の水分散液中に形成されてい
く様子を示した光学顕微鏡写真像図（×５１０）であ
り、また、図５は、ガラス基板上に担持した後の粒子薄
膜の形成状態を示した光学顕微鏡写真像図（×５１０）
である。１．７μｍポリスチレン球粒子の二次元凝集し
た粒子一層の薄膜がガラス基板上に形成された。FIG. 4 is an optical micrograph (× 510) showing how 1.7 μm polystyrene spheres are formed as island-like aggregates in an aqueous dispersion on PFMD. 5 is an optical microscope photographic image diagram (× 510) showing the formation state of the particle thin film after being supported on the glass substrate.
Is. A two-dimensional aggregated thin film of 1.7 μm polystyrene sphere particles was formed on the glass substrate.
【００２１】同様にして、３．５μｍ、５．５μｍの各
々のポリスチレン球粒子の二次元凝集薄膜も製造した。Two-dimensional aggregated thin films of polystyrene sphere particles of 3.5 μm and 5.5 μm, respectively, were similarly prepared.
【００２２】[0022]
【発明の効果】以上詳しく説明した通り、この発明の製
造法によって、従来使用していた水銀を用いることな
く、粒子薄膜の平坦さを保ちつつ、また、粒子薄膜を他
の転写基板に移すことなく、精度よく、効率的に粒子薄
膜を固体基板に形成担持させることが可能となる。As described in detail above, according to the manufacturing method of the present invention, it is possible to transfer the particle thin film to another transfer substrate while maintaining the flatness of the particle thin film without using mercury which has been used conventionally. Therefore, it becomes possible to form and support the particle thin film on the solid substrate accurately and efficiently.
【図１】この発明の製造法の概要を、分散液中の粒子の
凝集状態として例示した概念図である。FIG. 1 is a conceptual diagram illustrating the outline of the production method of the present invention as an aggregated state of particles in a dispersion liquid.
【図２】図２の状態に続く、基板上への粒子薄膜の形成
状態を例示した概念図である。FIG. 2 is a conceptual diagram exemplifying a formation state of a particle thin film on a substrate following the state of FIG.
【図３】この発明の製造法の実施のための装置例を示し
た断面図である。FIG. 3 is a sectional view showing an example of an apparatus for carrying out the manufacturing method of the present invention.
【図４】実施例としての水分散液中のポリスチレン粒子
の凝集を示した光学顕微鏡写真像図である。FIG. 4 is an optical micrograph image diagram showing aggregation of polystyrene particles in an aqueous dispersion as an example.
【図５】実施例としての基板上へのポリスチレン粒子の
薄膜形成を示した光学顕微鏡写真像図である。FIG. 5 is an optical micrograph image showing formation of a thin film of polystyrene particles on a substrate as an example.
１ 粒子分散液 ２ 液体膜 ３ 転写担持用固体基板 ４ テフロンセル ５ 支持台 ６ セルカバー ７ 雰囲気ガス 1 Particle Dispersion Liquid 2 Liquid Film 3 Transfer Support Solid Substrate 4 Teflon Cell 5 Support 6 Cell Cover 7 Atmosphere Gas
Claims (3)
の液体膜上に粒子分散液を液体膜と混合することなく展
開し、分散媒と液体膜とを蒸発させて担持用基板上に粒
子薄膜を形成することを特徴とする粒子薄膜の製造法。1. A liquid film is provided on a supporting substrate, and then a particle dispersion liquid is developed on the liquid film without being mixed with the liquid film to evaporate the dispersion medium and the liquid film to form on the supporting substrate. A method for producing a particle thin film, comprising forming a particle thin film on a substrate.
体とからなる請求項１の製造法。2. The method according to claim 1, which comprises a liquid film having poor compatibility and a medium for the particle dispersion liquid.
を含有するものからなる請求項１の製造法。3. The method according to claim 1, wherein the liquid film contains a fluorocarbon or a derivative thereof.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| JP12984093A JP2828384B2 (en) | 1993-05-31 | 1993-05-31 | Manufacturing method of particle thin film |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| JP12984093A JP2828384B2 (en) | 1993-05-31 | 1993-05-31 | Manufacturing method of particle thin film |
Publications (2)
| Publication Number | Publication Date |
|---|---|
| JPH06339625A true JPH06339625A (en) | 1994-12-13 |
| JP2828384B2 JP2828384B2 (en) | 1998-11-25 |
Family
ID=15019540
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| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| JP12984093A Expired - Lifetime JP2828384B2 (en) | 1993-05-31 | 1993-05-31 | Manufacturing method of particle thin film |
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| Country | Link |
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| JP (1) | JP2828384B2 (en) |
Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| GB2575867A (en) * | 2018-07-27 | 2020-01-29 | Murata Manufacturing Co | Variable DC-DC converter and no-load clamp |
-
1993
- 1993-05-31 JP JP12984093A patent/JP2828384B2/en not_active Expired - Lifetime
Cited By (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| GB2575867A (en) * | 2018-07-27 | 2020-01-29 | Murata Manufacturing Co | Variable DC-DC converter and no-load clamp |
| GB2575867B (en) * | 2018-07-27 | 2020-12-30 | Murata Manufacturing Co | Variable DC-DC converter and no-load clamp |
| US11901824B2 (en) | 2018-07-27 | 2024-02-13 | Murata Manufacturing Co., Ltd. | Variable DC-DC converter and no-load clamp |
Also Published As
| Publication number | Publication date |
|---|---|
| JP2828384B2 (en) | 1998-11-25 |
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