JP3902495B2 - Method for forming fine particle fixing film - Google Patents

Method for forming fine particle fixing film Download PDF

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JP3902495B2
JP3902495B2 JP2002087677A JP2002087677A JP3902495B2 JP 3902495 B2 JP3902495 B2 JP 3902495B2 JP 2002087677 A JP2002087677 A JP 2002087677A JP 2002087677 A JP2002087677 A JP 2002087677A JP 3902495 B2 JP3902495 B2 JP 3902495B2
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film
electric field
particles
fixed
conductor
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JP2003282626A (en
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正彦 阿部
浩之 山崎
政紀 織田
晋也 塚本
俊郎 酒井
有朋 山口
秀樹 酒井
信幸 桃澤
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    • H—ELECTRICITY
    • H01—ELECTRIC ELEMENTS
    • H01L—SEMICONDUCTOR DEVICES NOT COVERED BY CLASS H10
    • H01L24/00—Arrangements for connecting or disconnecting semiconductor or solid-state bodies; Methods or apparatus related thereto
    • H01L24/01—Means for bonding being attached to, or being formed on, the surface to be connected, e.g. chip-to-package, die-attach, "first-level" interconnects; Manufacturing methods related thereto
    • H01L24/02—Bonding areas ; Manufacturing methods related thereto
    • H—ELECTRICITY
    • H01—ELECTRIC ELEMENTS
    • H01L—SEMICONDUCTOR DEVICES NOT COVERED BY CLASS H10
    • H01L2224/00—Indexing scheme for arrangements for connecting or disconnecting semiconductor or solid-state bodies and methods related thereto as covered by H01L24/00
    • H01L2224/01—Means for bonding being attached to, or being formed on, the surface to be connected, e.g. chip-to-package, die-attach, "first-level" interconnects; Manufacturing methods related thereto
    • H01L2224/10—Bump connectors; Manufacturing methods related thereto
    • H01L2224/1012—Auxiliary members for bump connectors, e.g. spacers
    • H01L2224/10122—Auxiliary members for bump connectors, e.g. spacers being formed on the semiconductor or solid-state body to be connected
    • H01L2224/10125—Reinforcing structures
    • H01L2224/10126—Bump collar
    • H—ELECTRICITY
    • H01—ELECTRIC ELEMENTS
    • H01L—SEMICONDUCTOR DEVICES NOT COVERED BY CLASS H10
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    • H01L2924/00—Indexing scheme for arrangements or methods for connecting or disconnecting semiconductor or solid-state bodies as covered by H01L24/00
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    • H01L2924/00—Indexing scheme for arrangements or methods for connecting or disconnecting semiconductor or solid-state bodies as covered by H01L24/00
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    • H01L2924/01029—Copper [Cu]
    • H—ELECTRICITY
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    • H01L—SEMICONDUCTOR DEVICES NOT COVERED BY CLASS H10
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    • H01L2924/0105—Tin [Sn]
    • H—ELECTRICITY
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    • H01L2924/01079—Gold [Au]

Description

【０００１】
【発明の属する技術分野】
本発明は、微小粒子固着被膜の形成方法に関し、更に詳細には、電極表面上に膜状に配列された微小粒子を固着する微小粒子固着被膜の形成方法に関する。
【０００２】
【従来の技術】
純粋な金属表面は反応性が高いことが多く、そのままの状態では、空気中の酸素により酸化されて酸化皮膜が形成されたり、空気中に浮遊する各種成分が付着し、汚れてしまうことがある。
【０００３】
このような問題を解決するためには、適当な物質で金属表面を被覆することが考えられ、一般的には、有機成分皮膜を形成する塗料等が使用されている。
【０００４】
しかしながら、上記の塗料は、噴霧または塗布あるいは浸漬することにより有機成分の皮膜を形成するものであるが、塗布後の皮膜の厚みは不均一であったり、あるいは極めて厚いものになってしまうという問題があった。
【０００５】
また塗料は、塗布後、塗布物上で反応し、皮膜を形成するものであるため、その成分は限られており、希望の有機材料で金属を被覆できるというものではなかった。
【０００６】
【発明が解決しようとする課題】
本発明は、上記現状においてなされたものであり、金属等の電導体の表面上に、目的とする有機材料の微小粒子を極めて薄い膜状に接着、固定化させるための技術の提供をその課題とするものである。
【０００７】
【課題を解決するための手段】
本発明者らは、上記課題を解決すべく鋭意研究を行った結果、微小粒子を電極表面上で膜状に配列させた後、これにパルス的な電場を印加することにより、膜状に配列した微小粒子同士が固着され、微小粒子の固着被膜が得られることを見出し、本発明を完成した。
【０００８】
すなわち本発明は、電導体を電極とし、これに電場を印加して微小粒子を膜状に配列せしめた後、更にパルス的に電場を印加せしめることを特徴とする電導体表面上での微小粒子固着皮膜の形成方法を提供するものである。
【０００９】
【発明の実施の形態】
本発明の微小粒子固着皮膜は、まず、電導体を電極とし、この上で微小粒子を膜状に配列し、次いで、この状態の微小粒子にパルス的な電場を印加することにより形成される。
【００１０】
本発明において、固着皮膜を形成する微小粒子としては、種々の電荷を有する粒子が挙げられるが、その形状が均一な形状の、ほぼ１０ｎｍから数ｍｍの範囲の粒径を有する粒子が好ましい。ここで、「均一な形状」とは、使用される粒子が配列されたときに規則的な構造体となる形状であることを意味し、特にその形状が制限されるものではないが、大きさや形状が揃っていることが重要であり、球状や、棒状、板状等の粒子が使用される。また、この微小粒子の材質については、特に制約はないが、有機物微小粒子が使用され、例えば、ポリスチレンラテックス粒子、ポリアクリレート粒子、ポリメチルメタクリレート粒子、ポリウレタン粒子等の高分子樹脂粒子が好ましい。
【００１１】
また、上記微小粒子固着皮膜が形成される電導体としては、電極として用いることができるものであれば特に制約はなく、白金、金、銀、銅、鉄、マンガン、モリブデン、亜鉛等の金属やそれらの合金あるいは各種の導電性プラスチック等が用いられる。この電導体を電極とする場合の電極間の距離については特に制約はなく、０.１から５００ｍｍ程度とすればよい。
【００１２】
本発明の微小粒子固着皮膜の形成に当たっては、上記微小粒子を電極である電導体上で膜状に配列させることが必要であるが、微小粒子を配列させるための方法については特に制約はない。しかしながら、簡単に微小粒子を配列させる手段としては、２枚の電極を有するセル中に、水もしくは他の水溶性物質を含有した分散媒に分散させた微小粒子を入れ、ここに交流ないし直流の電場を印加する方法が挙げられる。
【００１３】
微小粒子を膜状に配列するために必要な電場は、交流の場合は、０.５から１０００Ｖｒｍｓ程度であり、直流の場合は、０.５から３Ｖ程度である。また、電場の印加時間は、共に、２から５分程度である。なお、この電場の印加において、交流を用いた場合の方が膜状配列が広く大きなため好ましい。
【００１４】
上記のようにして電導体上に膜状に配列された微小粒子は、次にパルス的な電場の印加により固着される。微粒子の固着のために印可される電場は、直流によるパルス的なものであることが好ましい。例えば、このパルス電場として、３から１０００Ｖ程度の直流電圧を、例えば、３×１０-6から５秒程度の短時間、０.１から１回／秒程度の間隔で印可させればよい。
【００１５】
かくすることにより、電導体上に微小粒子固着皮膜が形成される。この微小粒子固着皮膜は、電導体上に強固に固着したものであるため、電極である電導体を、例えば高分子の微小粒子で被覆することができ、電導体に新たな性質を付与することができる。例えば、金属に疎水性表面を付与することができる。
【００１６】
また、金属上に規則的に規則的にコロイド粒子を配列させ、これを固着させることにより、オパールのような輝きを放つ皮膜を形成することができ（遊色現象）、特徴のある金属表面外観を得ることができる。
【００１７】
【実施例】
次に実施例および参考例を挙げ、本発明を更に詳しく説明するが、本発明はこれら実施例に何ら制約されるものではない。
【００１８】
参 考 例 １
観察用セルの作製：
電場印加のために、図１に示す装置を作成した。また、観察用セルは、図２に模式的に示すように、ＩＴＯ（Indium Tin Oxide）製の透明電極をスライドグラスに取り付け、この透明電極を内側にし、電極に配線を行ったものであり、中に試料を充填した後、密閉できるようになっている。また、電場印加下での粒子の挙動は微分干渉光学顕微鏡により観察した。
【００１９】
実 施 例 １
交流電場を用いる固着皮膜の形成：
直径が５μｍのポリスチレンラテックス（Duke Scientific Corporation社製；以下、「ＰＳＬ」という）を、蒸留水中に０.５ｗｔ％で加えて懸濁液とし、これを参考例１の観察用セル中に充填した。この観察用セルに、３Ｖｒｍｓ、１ｋＨｚの交流電場を２分間印加したところ、ＰＳＬは膜状に配列した。
【００２０】
次いで、３Ｖｒｍｓ、１ｋＨｚの交流電場を印加した状態で、更に３〜５Ｖのパルス的なバイアス電圧（直流）を印加した。このパルス的なバイアス電圧は、１秒間隔で５回印加した。この結果、膜状に配列したＰＳＬは、観察用セルの電極面に固着した（図３）。この固着皮膜は、電場を印加しない状態にしても、また、逆の電場を印加しても変化はなく、更に、蒸留水を除去しても、蒸留水をかけても壊れるものでなかった。
【００２１】
実 施 例 ２
直流電場を用いる固着被膜の形成：
直径が５μｍのＰＳＬを、蒸留水中に０.５ｗｔ％で加えて懸濁液とし、これを参考例１の観察用セル中に充填した。この観察用セルに、３Ｖの直流電場を２分間印加したところ、ＰＳＬは＋電極側に膜状に配列した。
【００２２】
次いで、上記観察セルに、単独で３〜５Ｖのパルス電圧（パルス時間１ｓｅｃ；パルス間隔１ｓｅｃ）を５回印加した。この結果、膜状に配列したＰＳＬは、観察用セルの電極面に固着した。この固着皮膜は、電場を印加しない状態にしても、また、逆の電場を印加しても変化はなく、更に、蒸留水を除去しても、蒸留水で洗浄しても剥がれないものであった。
【００２３】
実 施 例 ３
固着皮膜のＡＦＭ観察：
直径が１５５ｎｍのＰＳＬ（Duke Scientific Corporation社製）を、蒸留水中に０.５ｗｔ％で加えて懸濁液とし、これを参考例１の観察用セル中に充填した。この観察用セルに、３Ｖの直流電場を５分間印加し、その後合わせて３〜５Ｖの直流パルス（パルス時間１ｓｅｃ；パルス間隔１ｓｅｃ）を２０回印加した。
【００２４】
観察用セル中から水を除去し、＋電極側に膜状に固着したＰＳＬを、原子間力顕微鏡（Atomic Force Microscopy；ＡＦＭ）（セイコー電子工業株式会社製）で観察した。この結果、電極上の吸着膜は、１層ないし６層の厚みを持つものであることが確認された。
【００２５】
実 施 例 ４
固着皮膜の接触角測定：
直径が２μｍのＰＳＬを用い、実施例１に従って固着皮膜を形成した。次いで、この固着皮膜の水との接触角をコンタクト−アングルメーター Ｃ-Ａ型（協和界面化学（株）製）を用いて測定したところ、６５°であった。これに対し、同じＰＳＬを用い、移流集積法により形成した吸着膜は、外観的には上記固着皮膜と極めて類似していたが、形成される膜形状が異なるため、その接触角は、０°と大きく異なっていた。
【００２６】
【発明の効果】
以上説明した本発明によれば、電導体上に微小粒子の膜を形成することができる。そして、この微小粒子皮膜は、電導体表面を撥水加工したり、表面の導電性を低下させる等の表面改質技術として利用することができるものである。
【図面の簡単な説明】
【図１】 電場印加装置のブロック図
【図２】 実施例で使用する観察用セルの模式図
【図３】 固着した微小粒子の光学顕微鏡写真（倍率４００倍）
【符号の説明】
１ … … スライドグラス
２ … … ＩＴＯ膜
３ … … 顕微鏡
以 上[0001]
BACKGROUND OF THE INVENTION
The present invention relates to a method for forming a fine particle fixed film, and more particularly to a method for forming a fine particle fixed film for fixing fine particles arranged in a film form on an electrode surface.
[0002]
[Prior art]
Pure metal surfaces are often highly reactive, and if left as they are, they may be oxidized by oxygen in the air to form an oxide film, or various components floating in the air may adhere and become dirty. .
[0003]
In order to solve such a problem, it is conceivable to coat the metal surface with an appropriate substance, and generally a paint or the like for forming an organic component film is used.
[0004]
However, although the above-mentioned paint forms a film of organic components by spraying, coating or dipping, the film thickness after coating is not uniform or becomes extremely thick. was there.
[0005]
In addition, since the paint reacts on the coated material after application to form a film, its components are limited and the metal cannot be coated with a desired organic material.
[0006]
[Problems to be solved by the invention]
The present invention has been made under the above circumstances, and it is an object of the present invention to provide a technique for adhering and immobilizing fine particles of an organic material of interest on a surface of an electric conductor such as a metal in an extremely thin film shape. It is what.
[0007]
[Means for Solving the Problems]
As a result of intensive research to solve the above problems, the present inventors have arranged microparticles in a film shape on the electrode surface, and then applied a pulsed electric field thereto to arrange the microparticles in a film shape. It was found that the fine particles adhered to each other and a fixed coating of fine particles was obtained, and the present invention was completed.
[0008]
That is, the present invention provides a microparticle on the surface of a conductor characterized in that an electric field is applied to the conductor, and an electric field is applied thereto to arrange the microparticles in a film shape, and then the electric field is further applied in a pulsed manner. A method for forming a fixed film is provided.
[0009]
DETAILED DESCRIPTION OF THE INVENTION
The fine particle fixing film of the present invention is formed by first using an electric conductor as an electrode, arranging the fine particles in a film shape thereon, and then applying a pulsed electric field to the fine particles in this state.
[0010]
In the present invention, the fine particles forming the fixed film include particles having various charges, and particles having a uniform shape and a particle size in the range of about 10 nm to several mm are preferable. Here, the “uniform shape” means a shape that becomes a regular structure when the particles to be used are arranged, and the shape is not particularly limited. It is important that the shapes are uniform, and spherical, rod-like, plate-like, etc. particles are used. The material of the fine particles is not particularly limited, but organic fine particles are used. For example, polymer resin particles such as polystyrene latex particles, polyacrylate particles, polymethyl methacrylate particles, and polyurethane particles are preferable.
[0011]
In addition, the conductor on which the fine particle fixing film is formed is not particularly limited as long as it can be used as an electrode, such as platinum, gold, silver, copper, iron, manganese, molybdenum, and zinc, Those alloys or various conductive plastics are used. There is no restriction | limiting in particular about the distance between electrodes when making this conductor into an electrode, What is necessary is just to be about 0.1-500 mm.
[0012]
In forming the fine particle fixing film of the present invention, it is necessary to arrange the fine particles in the form of a film on an electric conductor as an electrode, but there is no particular restriction on the method for arranging the fine particles. However, as a means for easily arranging microparticles, microparticles dispersed in a dispersion medium containing water or other water-soluble substance are placed in a cell having two electrodes, and AC or DC There is a method of applying an electric field.
[0013]
The electric field required to arrange the microparticles in the form of a film is about 0.5 to 1000 Vrms for alternating current and about 0.5 to 3 V for direct current. The electric field application time is about 2 to 5 minutes. In addition, in the application of this electric field, the case where alternating current is used is preferable because the film arrangement is wide and large.
[0014]
The fine particles arranged in a film shape on the conductor as described above are then fixed by applying a pulsed electric field. The electric field applied to fix the fine particles is preferably pulsed by direct current. For example, as this pulse electric field, a DC voltage of about 3 to 1000 V may be applied at a time interval of about 0.1 to 1 time / second for a short time of about 3 × 10 −6 to about 5 seconds.
[0015]
Thus, a fine particle fixed film is formed on the conductor. Since this fine particle fixed film is firmly fixed on the conductor, the electrode conductor can be covered with, for example, polymer fine particles, and a new property is imparted to the conductor. Can do. For example, a hydrophobic surface can be imparted to the metal.
[0016]
In addition, colloidal particles are regularly and regularly arranged on the metal, and this is fixed to form an opal-like shining film (play-color phenomenon), which has a distinctive metal surface appearance. Can be obtained.
[0017]
【Example】
EXAMPLES Next, although an Example and a reference example are given and this invention is demonstrated in more detail, this invention is not restrict | limited at all by these Examples.
[0018]
Reference example 1
Production of observation cell:
The apparatus shown in FIG. 1 was created for applying an electric field. In addition, as schematically shown in FIG. 2, the observation cell is obtained by attaching a transparent electrode made of ITO (Indium Tin Oxide) to a slide glass, setting the transparent electrode inside, and wiring the electrode. After filling the sample, it can be sealed. Moreover, the behavior of the particles under the application of an electric field was observed with a differential interference optical microscope.
[0019]
Example 1
Formation of a fixed film using an alternating electric field:
A polystyrene latex having a diameter of 5 μm (manufactured by Duke Scientific Corporation; hereinafter referred to as “PSL”) was added to distilled water at 0.5 wt% to form a suspension, which was filled in the observation cell of Reference Example 1. . When an alternating electric field of 3 Vrms and 1 kHz was applied to this observation cell for 2 minutes, the PSL was arranged in a film shape.
[0020]
Next, in the state where an AC electric field of 3 Vrms and 1 kHz was applied, a pulsed bias voltage (DC) of 3 to 5 V was further applied. This pulsed bias voltage was applied 5 times at 1 second intervals. As a result, the PSL arranged in the form of a film adhered to the electrode surface of the observation cell (FIG. 3). This fixed film did not change even when an electric field was not applied or when a reverse electric field was applied, and even when distilled water was removed, it was not broken even when distilled water was applied.
[0021]
Example 2
Formation of a fixed film using a direct current electric field:
PSL having a diameter of 5 μm was added to distilled water at 0.5 wt% to form a suspension, and this was filled in the observation cell of Reference Example 1. When a DC electric field of 3 V was applied to this observation cell for 2 minutes, the PSL was arranged in a film on the + electrode side.
[0022]
Next, a pulse voltage of 3 to 5 V (pulse time 1 sec; pulse interval 1 sec) was applied to the observation cell 5 times. As a result, the PSL arranged in a film form was fixed to the electrode surface of the observation cell. This fixed film does not change even when an electric field is not applied or when a reverse electric field is applied, and it does not peel off even if distilled water is removed or washed with distilled water. It was.
[0023]
Example 3
AFM observation of fixed film:
PSL (manufactured by Duke Scientific Corporation) having a diameter of 155 nm was added to distilled water at 0.5 wt% to make a suspension, and this was filled in the observation cell of Reference Example 1. A 3V DC electric field was applied to the observation cell for 5 minutes, and then 3 to 5 V DC pulses (pulse time 1 sec; pulse interval 1 sec) were applied 20 times.
[0024]
Water was removed from the observation cell, and the PSL fixed in the form of a film on the + electrode side was observed with an atomic force microscope (AFM) (manufactured by Seiko Denshi Kogyo Co., Ltd.). As a result, it was confirmed that the adsorption film on the electrode had a thickness of 1 to 6 layers.
[0025]
Example 4
Contact angle measurement of fixed film:
A fixed film was formed according to Example 1 using PSL having a diameter of 2 μm. Subsequently, the contact angle of this fixed film with water was measured using a contact-angle meter C-A type (manufactured by Kyowa Interface Chemical Co., Ltd.) and found to be 65 °. On the other hand, the adsorption film formed by the advection accumulation method using the same PSL was very similar in appearance to the above-described fixed film, but the contact angle was 0 ° because the formed film shape was different. It was very different.
[0026]
【The invention's effect】
According to the present invention described above, a film of fine particles can be formed on a conductor. The fine particle coating can be used as a surface modification technique such as water repellent treatment of the surface of the conductor or reduction of the surface conductivity.
[Brief description of the drawings]
1 is a block diagram of an electric field application device. FIG. 2 is a schematic diagram of an observation cell used in the examples. FIG. 3 is an optical micrograph of a fixed microparticle (400 × magnification).
[Explanation of symbols]
1…… Slide glass 2…… ITO film 3…… Microscope or higher

Claims (4)

電導体を電極とし、これに電場を印加して粒子を膜状に配列せしめた後、更にパルス的に電場を印加せしめることを特徴とする電導体表面上での粒子固着皮膜の形成方法。  A method for forming a particle-fixing film on a surface of an electric conductor, comprising using an electric conductor as an electrode, applying an electric field to the electric conductor to arrange particles in a film, and further applying an electric field in pulses. 交流電場を印加することにより粒子を電極表面上に膜状に配列せしめるものである請求項第１項記載の粒子固着皮膜の形成方法。  2. The method for forming a fixed particle coating according to claim 1, wherein the particles are arranged in a film form on the electrode surface by applying an alternating electric field. パルス的に印加される電場が、直流電圧により得られる電場である請求項第１項または第２項記載の粒子固着皮膜の形成方法。  3. The method for forming a particle fixed film according to claim 1, wherein the pulsed electric field is an electric field obtained by a DC voltage. 粒子がポリスチレン粒子である請求項第１項ないし第３項の何れかの項記載の粒子固着皮膜の形成方法。  4. The method for forming a particle fixing film according to any one of claims 1 to 3, wherein the particles are polystyrene particles.
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