JP2828375B2 - Two-dimensional agglomeration forming device for fine particles - Google Patents

Two-dimensional agglomeration forming device for fine particles

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Publication number
JP2828375B2
JP2828375B2 JP30086992A JP30086992A JP2828375B2 JP 2828375 B2 JP2828375 B2 JP 2828375B2 JP 30086992 A JP30086992 A JP 30086992A JP 30086992 A JP30086992 A JP 30086992A JP 2828375 B2 JP2828375 B2 JP 2828375B2
Authority
JP
Japan
Prior art keywords
fine particles
cell
dimensional
forming apparatus
substrate
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 - Fee Related
Application number
JP30086992A
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Japanese (ja)
Other versions
JPH06210158A (en
Inventor
国昭 永山
ディー デンコフ ニコライ
Current Assignee (The listed assignees may be inaccurate. Google has not performed a legal analysis and makes no representation or warranty as to the accuracy of the list.)
Kagaku Gijutsu Shinko Jigyodan
Original Assignee
Kagaku Gijutsu Shinko Jigyodan
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Filing date
Publication date
Application filed by Kagaku Gijutsu Shinko Jigyodan filed Critical Kagaku Gijutsu Shinko Jigyodan
Priority to JP30086992A priority Critical patent/JP2828375B2/en
Priority to US08/113,664 priority patent/US5437892A/en
Priority to DE69310057T priority patent/DE69310057T2/en
Priority to EP93306851A priority patent/EP0586215B1/en
Publication of JPH06210158A publication Critical patent/JPH06210158A/en
Application granted granted Critical
Publication of JP2828375B2 publication Critical patent/JP2828375B2/en
Anticipated expiration legal-status Critical
Expired - Fee Related legal-status Critical Current

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Description

【発明の詳細な説明】DETAILED DESCRIPTION OF THE INVENTION

【0001】[0001]

【産業上の利用分野】この発明は、微粒子の2次元凝集
形成装置に関するものである。さらに詳しくは、この発
明は、リソグラフィー、マイクロエレクトロニクス、イ
メージ処理分野、バイオマテリアル、セラミック、金属
材料等の諸野において新たな機能性材料の創製において
有用な微粒子の2次元凝集形成装置に関するものであ
る。
BACKGROUND OF THE INVENTION 1. Field of the Invention The present invention relates to an apparatus for forming two-dimensional aggregates of fine particles. More particularly, the present invention relates to a two-dimensional agglomeration forming apparatus for fine particles useful in the creation of new functional materials in various fields such as lithography, microelectronics, image processing, biomaterials, ceramics, and metal materials. .

【0002】[0002]

【従来の技術とその課題】従来より、微粒子(たん白
質、酸化物、金属、ラテックス、ポリマー)等を2次元
的に展開し、これを制御して集合構造を形成するための
方法と装置が検討され、工夫されてきている。たとえば
そのための方法として、微粒子分散液の気液界面、ある
いは液々界面に微粒子を析出させてこれを凝集させる方
法等が試みられている。
2. Description of the Related Art Conventionally, a method and an apparatus for two-dimensionally developing fine particles (protein, oxide, metal, latex, polymer) and the like and controlling them to form an aggregated structure have been proposed. It has been considered and devised. For example, as a method therefor, a method of depositing fine particles at a gas-liquid interface or a liquid-liquid interface of a fine particle dispersion and aggregating the fine particles has been attempted.

【0003】しかしながら、微粒子の凝集構造を、高精
度に、かつ迅速に形成および制御することはそれほど簡
単なことではない。そして実際に、これまでに試みられ
ている方法や装置では限界があった。たとえば従来の析
出方法の場合には粒子一層の2次元膜を作ることは比較
的可能であるが、膜質の均一化が得られないという問題
がある。
[0003] However, it is not so easy to form and control the agglomerated structure of fine particles with high precision and speed. And indeed, the methods and devices that have been attempted to date have limitations. For example, in the case of a conventional deposition method, it is relatively possible to form a two-dimensional film having one layer of particles, but there is a problem in that uniform film quality cannot be obtained.

【0004】このような状況において、この発明の発明
者はまったく新しい方法として、微粒子を高精度で迅速
に凝集する方法をすでに発明している。この方法は、こ
の発明の発明者が新たに見出したメニスカス力等によっ
て誘起される微粒子の凝集を高度に制御するものであ
る。すなわち、たとえば図1に例示したように、液状分
散媒体(I)に分散した微粒子(A)(B)を表面平坦
な基板(III) に供給し、液状分散媒体(I)の膜厚
(d)を蒸発等によって微粒子(A)(B)の粒径程
度、特にその径以下にまで制御すると、微粒子(A)
(B)には、大きな吸引力(F)が作用し、微粒子の核
凝集が形成される。
In such a situation, the inventor of the present invention has already invented, as a completely new method, a method of rapidly and precisely aggregating fine particles. This method highly controls the aggregation of fine particles induced by the meniscus force or the like newly found by the inventor of the present invention. That is, as illustrated in FIG. 1, for example, fine particles (A) and (B) dispersed in a liquid dispersion medium (I) are supplied to a substrate (III) having a flat surface, and the thickness (d) of the liquid dispersion medium (I) is increased. ) Is controlled to about the particle size of the fine particles (A) and (B) by evaporation or the like, and particularly to the particle size or less, the fine particles (A)
A large suction force (F) acts on (B), and a nucleus aggregation of fine particles is formed.

【0005】このような吸引力(F)として発生するメ
ニスカス力は、微粒子と液状分散媒体(I)とのぬれ角
(θ)、液状分散媒体(I)の充分遠方での厚さ
(d),および微粒子(A)(B)の径(2r),そし
て液状分散媒体(I)と媒体(II)の界面張力(液状分
散媒体(I)が空気の時は表面張力)、液状分散媒体
(I)と媒体(II)の密度差に依存することが理論的に
予測される。またメニスカス力は極めて長距離的な力
で、微粒子間の距離(l)の逆数に比例すると考えられ
る。このような長距離故に相当遠方の粒子間にも引力が
作用する。
The meniscus force generated as such a suction force (F) is determined by the wetting angle (θ) between the fine particles and the liquid dispersion medium (I) and the thickness (d) of the liquid dispersion medium (I) at a sufficiently long distance. And the diameter (2r) of the fine particles (A) and (B), the interfacial tension between the liquid dispersion medium (I) and the medium (II) (surface tension when the liquid dispersion medium (I) is air), and the liquid dispersion medium ( It is theoretically predicted to depend on the density difference between I) and the medium (II). The meniscus force is an extremely long-distance force, and is considered to be proportional to the reciprocal of the distance (l) between the fine particles. Because of such a long distance, an attractive force acts between particles at a considerably far distance.

【0006】以上のようなメニスカス力等により、表面
平坦基板(III) 上に、微粒子の2次元凝集が形成され
る。しかしながら、この新しい方法によって微粒子の2
次元凝集を形成する場合、その再現性を向上し、広域的
な2次元凝集を得るためには、蒸発速度およびメニスカ
ス力を有効に制御することが必要となる。しかしながら
これらのファクターを制御するための装置はいまだに技
術的に確立していなかった。このため、2次元凝集は必
ずしも均質とならず、その生成効率の向上には制約があ
った。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、液状分散媒体の膜厚およびメニスカス力の制
御を高精度で効率よく行うことを可能とする2次元凝集
形成装置を提供することを目的としている。
[0006] Due to the meniscus force and the like as described above, two-dimensional aggregation of fine particles is formed on the flat surface substrate (III). However, this new method does not
When forming dimensional aggregation, it is necessary to effectively control the evaporation rate and the meniscus force in order to improve the reproducibility and obtain two-dimensional aggregation over a wide area. However, a device for controlling these factors has not been technically established yet. For this reason, the two-dimensional aggregation is not always uniform, and there is a restriction on the improvement of the production efficiency. The present invention has been made in view of the above circumstances, and an object of the present invention is to provide a two-dimensional agglomeration forming apparatus capable of controlling a film thickness and a meniscus force of a liquid dispersion medium with high accuracy and efficiency. The purpose is.

【0007】[0007]

【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、セル構造体とこのセル構造体を
覆う密閉性容器体とを備えた装置であって、セル構造体
は、表面平坦基板上に当接もしくは近接する環状壁体を
有し、基板とともに環状壁体によって保持した微粒子分
散液体の液膜厚を制御することで微粒子の2次元凝集を
形成することを特徴とする微粒子の2次元凝集形成装置
を提供する。
Means for Solving the Problems The present invention solves the above-mentioned problems, and is an apparatus provided with a cell structure and a closed container covering the cell structure. It has an annular wall that is in contact with or close to a flat surface substrate, and forms two-dimensional aggregation of fine particles by controlling the liquid film thickness of the fine particle dispersion liquid held by the annular wall together with the substrate. Provided is a two-dimensional aggregation forming apparatus for fine particles.

【0008】また、さらに、この発明においては、密閉
性容器体内に温度制御手段を配設することや、セル環状
壁体の基板対向内壁端に傾斜部を設けること、さらに
は、セル環状壁体の基板対向端に空隙を設け、この空隙
をセル内に連通させてセル内の液膜圧力を制御すること
等を好ましい態様としてもいる。この発明の微粒子の2
次元凝集形成装置は、たとえば、図2に示した装置とし
て示すことができる。
Further, according to the present invention, it is possible to dispose temperature control means in the airtight container, to provide an inclined portion at the end of the inner wall of the cell annular wall facing the substrate, and to further provide a cell annular wall. In a preferred embodiment, a gap is provided at the opposite end of the substrate, and the gap is communicated with the cell to control the liquid film pressure in the cell. 2 of the fine particles of the present invention
The dimensional agglomeration forming apparatus can be shown, for example, as the apparatus shown in FIG.

【0009】この装置は、表面平坦基板(11)に当接
もしくは近接する環状壁体(12)を有するセル構造体
(1)を固定板(2)を介して顕微鏡等のセル固定台
(3)に鋲(4)等を用いて固定し、全体をフード
(5)で覆う密閉性容器体の構造を持っている。このフ
ード(5)は、外部からの不純物がセル内に混入するの
を防ぐだけでなく、リング内の液状分散媒体(6)の蒸
発を制御する役割を有している。
In this apparatus, a cell structure (1) having an annular wall (12) abutting on or close to a flat surface substrate (11) is fixed via a fixing plate (2) to a cell fixing base (3) such as a microscope. ) Is fixed using a stud (4) or the like, and has a structure of a hermetically sealed container body entirely covered with a hood (5). The hood (5) has a role not only to prevent impurities from the outside from entering the cell, but also to control evaporation of the liquid dispersion medium (6) in the ring.

【0010】そして、この円形、多角形等の環状壁体
(12)内に、微粒子と液状分散媒体(6)を装入し、
その後、液状分散媒体(6)の膜厚を制御することによ
って、メニスカス力を発生させて、2次元凝集を形成さ
せる。このとき、たとえば光学顕微鏡(7)等により、
この過程を観察することもできる。また、この発明にお
いては、図2の拡大図に例示したように、表面平坦基板
(11)に対向する環状壁体(12)の内壁端に傾斜部
を設け、液状分散媒体に接するリングの内壁と表面平坦
基板との角度(α)を鋭角にすることが有効でもある。
こうすることにより、液状分散媒体とセル壁との接触角
(β)を小さく保つことができ、メニスカス力をより安
定化させることが可能となる。この結果、さらに精度の
よい2次元凝集を形成することが可能となる。
Then, fine particles and a liquid dispersion medium (6) are charged into the circular or polygonal annular wall (12).
Thereafter, by controlling the film thickness of the liquid dispersion medium (6), a meniscus force is generated to form two-dimensional aggregation. At this time, for example, with an optical microscope (7) or the like,
You can also observe this process. Further, in the present invention, as exemplified in the enlarged view of FIG. 2, an inclined portion is provided at the inner wall end of the annular wall body (12) facing the flat surface substrate (11), and the inner wall of the ring in contact with the liquid dispersion medium is provided. It is also effective to make the angle (α) between the substrate and the flat surface substrate an acute angle.
By doing so, the contact angle (β) between the liquid dispersion medium and the cell wall can be kept small, and the meniscus force can be further stabilized. As a result, more accurate two-dimensional aggregation can be formed.

【0011】さらに、この発明においては、図3に例示
するように、液状分散媒体の膜厚の制御精度を向上する
ために、温度制御装置(8)をセル構造体(1)付近に
付設することも有効である。温度制御装置(8)として
は、電熱線等を利用したヒータ、温水等を循環させる細
管等の適宜なものを使用することができる。この発明に
おいては、毛細管(9)を付設し、液状分散媒体(6)
の膜厚を制御してもよい。この場合、たとえば、図3に
例示するように、基体(11)対向端に空隙(30)を
持つセル環状壁体(12)の一部に、この空隙とセル外
部を連通するチャネル(40)を設け、さらに空隙とセ
ル内との間を連通するスリット(50)を設け、チャネ
ル(40)を通して毛細管(9)を空隙(30)に挿入
固定し、空隙(30)に存在する、液状分散媒体をこの
毛細管を用いて吸引または加圧し、スリット(50)を
介して、空隙(30)と、液状分散媒体(6)の膜厚を
制御している。
Further, in the present invention, as exemplified in FIG. 3, in order to improve the control accuracy of the film thickness of the liquid dispersion medium, a temperature control device (8) is provided near the cell structure (1). It is also effective. As the temperature control device (8), an appropriate device such as a heater using a heating wire or a thin tube for circulating hot water or the like can be used. In the present invention, a capillary (9) is provided, and a liquid dispersion medium (6) is provided.
May be controlled. In this case, for example, as illustrated in FIG. 3, a channel (40) that communicates the space with the outside of the cell is formed in a part of the cell annular wall (12) having a space (30) at the end facing the base (11). And a slit (50) communicating between the gap and the inside of the cell is provided, and the capillary (9) is inserted and fixed into the gap (30) through the channel (40), and the liquid dispersion existing in the gap (30) is provided. The medium is sucked or pressurized by using the capillary to control the gap (30) and the film thickness of the liquid dispersion medium (6) through the slit (50).

【0012】この液状分散媒体の膜厚の制御により、よ
り高精度な2次元凝集の形成が可能となる。この発明に
よって形成された2次元凝集に、化学的修飾、あるいは
レーザー等の光による加工、修飾等を施すことにより、
さらに機能性に優れた凝集体(結晶)に変換することも
できる。また、この凝集を層状にすることによって、微
粒子層の多層化を施すこともできる。エレクトロニク
ス、バイオマテリアル、セラミック、金属、ポリマー等
の諸分野の新しい機能材料の創製に、さらには、新しい
物理・化学処理プロセス、計測装置等への応用も可能と
なる。
By controlling the thickness of the liquid dispersion medium, it is possible to form a two-dimensional aggregation with higher precision. By subjecting the two-dimensional aggregation formed by the present invention to chemical modification, or processing and modification with light such as laser,
Further, it can be converted into an aggregate (crystal) having excellent functionality. Further, by forming this aggregation into a layer, a multilayer of the fine particle layer can be provided. It will be possible to create new functional materials in various fields such as electronics, biomaterials, ceramics, metals, and polymers, as well as to apply to new physical and chemical processing processes, measurement devices, and the like.

【0013】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。
Hereinafter, the present invention will be described in detail with reference to Examples.

【0014】[0014]

【実施例】ガラスからなる表面平坦基板上に有する径
1.4cmの円形セル構造体のテフロンリング壁の端部
を当接し、流通させる温水の温度によって、液状分散媒
体の蒸発速度を制御する温度制御装置と、液状分散媒体
の圧力を制御するための毛細管を前記の図3に示したよ
うに備えた2次元凝集形成装置を用い、そのセル内部に
直径1.70μmのポリスチレン球の分散水(濃度は1
wt%、温度は25℃)を満たし、2次元凝集を形成さ
せた。
DETAILED DESCRIPTION OF THE PREFERRED EMBODIMENTS A temperature at which the end of a Teflon ring wall of a circular cell structure having a diameter of 1.4 cm on a flat surface substrate made of glass is brought into contact with the substrate and the evaporation rate of a liquid dispersion medium is controlled by the temperature of the hot water to be circulated. A two-dimensional agglomeration forming apparatus provided with a control device and a capillary for controlling the pressure of the liquid dispersion medium as shown in FIG. 3 is used, and dispersed water of polystyrene spheres having a diameter of 1.70 μm ( The concentration is 1
wt%, the temperature was 25 ° C.) to form two-dimensional aggregation.

【0015】その際、セル内のポリスチレン球の分散水
の水面は、蒸発させることにより減少させた。図4は2
次元凝集の形成過程の観察結果である。図4(a)は、
液状分散媒体の蒸発により、微粒子が濃縮し始めた状態
を示し、図4(b)は、さらに、蒸発を継続した結果、
一方向への水の流れが生じ、その流れに乗って微粒子が
凝集し2次元凝集が成長していく状態を示し、図4
(c)は、2次元凝集の成長が完了し、微粒子が一層の
2次元凝集となった状態を示している。
At this time, the water level of the dispersion water of the polystyrene spheres in the cell was reduced by evaporation. FIG.
It is an observation result of a formation process of dimensional aggregation. FIG. 4 (a)
FIG. 4B shows a state in which the fine particles have started to be concentrated by the evaporation of the liquid dispersion medium, and FIG.
FIG. 4 shows a state in which a flow of water in one direction is generated, and fine particles aggregate on the flow and two-dimensional aggregation grows.
(C) shows a state in which the growth of the two-dimensional aggregation has been completed, and the fine particles have been further two-dimensionally aggregated.

【0016】この図が示すように、形成された2次元凝
集は均質で、高精度で効率よく微粒子の固体表面上の2
次元凝集(結晶)を形成することができた。
As shown in this figure, the formed two-dimensional agglomeration is homogeneous, highly precise and efficiently formed on the solid surface of fine particles.
Dimensional aggregation (crystals) could be formed.

【0017】[0017]

【発明の効果】以上詳しく説明した通り、この発明によ
り、液状分散媒体の膜厚およびメニスカス力の制御を行
い、高精度で効率よく2次元凝集を形成することが可能
となる。
As described in detail above, according to the present invention, it is possible to control the film thickness and the meniscus force of the liquid dispersion medium to form two-dimensional aggregation with high precision and efficiency.

【図面の簡単な説明】[Brief description of the drawings]

【図1】メニスカス力を説明した模式図である。FIG. 1 is a schematic diagram illustrating a meniscus force.

【図2】この発明の装置の一例を示した断面図である。FIG. 2 is a sectional view showing an example of the device of the present invention.

【図3】この発明の装置の別の一例を示した断面図であ
る。
FIG. 3 is a sectional view showing another example of the device of the present invention.

【図4】(a)(b)(c)は、この発明の実施例を示
した光学顕微鏡像図である。
FIGS. 4 (a), (b) and (c) are optical microscope images showing an embodiment of the present invention.

【符号の説明】[Explanation of symbols]

1 セル構造体 11 表面平坦基板 12 環状壁体 2 セル固定板 3 セル固定台 4 鋲 5 フード 6 液状分散媒体 7 光学顕微鏡 8 温度制御装置 9 毛細管 30 空隙 40 チャネル 50 スリット REFERENCE SIGNS LIST 1 cell structure 11 flat surface substrate 12 annular wall 2 cell fixing plate 3 cell fixing base 4 tack 5 hood 6 liquid dispersion medium 7 optical microscope 8 temperature control device 9 capillary 30 void 40 channel 50 slit

───────────────────────────────────────────────────── フロントページの続き (58)調査した分野(Int.Cl.6,DB名) B01J 19/00 B05D 5/02──────────────────────────────────────────────────続 き Continued on front page (58) Field surveyed (Int.Cl. 6 , DB name) B01J 19/00 B05D 5/02

Claims (6)

(57)【特許請求の範囲】(57) [Claims] 【請求項1】 セル構造体とこのセル構造体を覆う密閉
性容器体とを備えた装置であって、セル構造体は、表面
平坦基板上に当接もしくは近接する環状壁体を有し、基
板とともに環状壁体によって保持した微粒子分散液体の
液膜厚を制御することで微粒子の2次元凝集を形成する
ことを特徴とする微粒子の2次元凝集形成装置。
1. An apparatus comprising a cell structure and an airtight container covering the cell structure, wherein the cell structure has an annular wall abutting on or close to a flat surface substrate. A two-dimensional agglomeration forming apparatus for fine particles, wherein two-dimensional agglomeration of fine particles is formed by controlling the liquid film thickness of a fine particle-dispersed liquid held by an annular wall together with a substrate.
【請求項2】 密閉性容器体内に温度制御装置を配設し
てなる請求項1の微粒子の2次元凝集形成装置。
2. The two-dimensional agglomeration forming apparatus for fine particles according to claim 1, wherein a temperature control device is provided in the airtight container.
【請求項3】 セル環状壁体の基板対向内壁端に傾斜部
を設けてなる請求項1の微粒子の2次元凝集形成装置。
3. The two-dimensional agglomeration forming apparatus for fine particles according to claim 1, wherein an inclined portion is provided at an end of the inner wall of the cell annular wall facing the substrate.
【請求項4】 セル環状壁体の基板対向端に空隙を設
け、この空隙をセル内に連通させてセル内の液膜圧力を
制御する請求項1の微粒子の2次元凝集形成装置。
4. The two-dimensional agglomeration forming apparatus for fine particles according to claim 1, wherein a gap is provided at an end of the cell annular wall facing the substrate, and the gap is communicated with the inside of the cell to control the liquid film pressure in the cell.
【請求項5】 スリットにより空隙とセル内部とを連通
させてなる請求項5の微粒子の2次元凝集形成装置。
5. The two-dimensional agglomeration forming apparatus for fine particles according to claim 5, wherein the slit communicates the gap with the inside of the cell.
【請求項6】 セル外部より空隙に連通させた毛細管に
より液膜圧力を制御する請求項5の微粒子の凝集形成装
置。
6. The fine particle agglomeration forming apparatus according to claim 5, wherein the liquid film pressure is controlled by a capillary tube communicated from the outside of the cell to the gap.
JP30086992A 1992-08-31 1992-11-11 Two-dimensional agglomeration forming device for fine particles Expired - Fee Related JP2828375B2 (en)

Priority Applications (4)

Application Number Priority Date Filing Date Title
JP30086992A JP2828375B2 (en) 1992-11-11 1992-11-11 Two-dimensional agglomeration forming device for fine particles
US08/113,664 US5437892A (en) 1992-08-31 1993-08-31 Method for manufacturing a fine-particles two-dimensional aggregate from a liquid dispersion of fine particles
DE69310057T DE69310057T2 (en) 1992-08-31 1993-08-31 Method and device for producing a two-dimensional arrangement of fine particles
EP93306851A EP0586215B1 (en) 1992-08-31 1993-08-31 Method for manufacturing a fine-particle two-dimensional assembly and apparatus therefor

Applications Claiming Priority (1)

Application Number Priority Date Filing Date Title
JP30086992A JP2828375B2 (en) 1992-11-11 1992-11-11 Two-dimensional agglomeration forming device for fine particles

Publications (2)

Publication Number Publication Date
JPH06210158A JPH06210158A (en) 1994-08-02
JP2828375B2 true JP2828375B2 (en) 1998-11-25

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