JPS60177198A - Production of thin film-like porous body of al2o3 - Google Patents
Production of thin film-like porous body of al2o3Info
- Publication number
- JPS60177198A JPS60177198A JP3214784A JP3214784A JPS60177198A JP S60177198 A JPS60177198 A JP S60177198A JP 3214784 A JP3214784 A JP 3214784A JP 3214784 A JP3214784 A JP 3214784A JP S60177198 A JPS60177198 A JP S60177198A
- Authority
- JP
- Japan
- Prior art keywords
- porous
- layer
- thin film
- al2o3
- aluminum
- 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.)
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Abstract
Description
【発明の詳細な説明】
ａ 産業上の利用分野
本発明は厚味の薄い多孔質体の製造方法に関する。更に
詳しくは、薄膜状ＡＡ’２０３多孔質体の多孔方体に関
する。DETAILED DESCRIPTION OF THE INVENTION a. Field of Industrial Application The present invention relates to a method for producing a thin porous body. More specifically, the present invention relates to the porous parallelepiped of the thin film-like AA'203 porous body.
ｂ 従来技術
今日、７ミクロン（μ）以下の大きさの細孔を有する多
孔質体が注目され、具体的には海水の脱塩を目的とした
逆浸透膜、各種酵素の固定化等生化学への応用、自動車
排気ガス用触媒などの担体。b. Prior art Today, porous materials with pores of 7 microns (μ) or less in size are attracting attention, and specifically, they are used in biochemical applications such as reverse osmosis membranes for the purpose of desalinating seawater, immobilization of various enzymes, etc. applications, carriers for automobile exhaust gas catalysts, etc.
気体−気体の分離膜、あるいはその比表面積の大きさを
利用し種々の物質に対する吸着剤としての輯利用など多
くの方面で新しい機能性材料としての開発が進められて
いる。。The development of new functional materials is progressing in many fields, such as gas-gas separation membranes and their use as adsorbents for various substances by taking advantage of their large specific surface area. .
多孔質体の材料としてはセラミックスやガラスなどの無
機材料の他、ポリアクリルアミド、アガロース、セルロ
ース系物質など有機材料についても材料開発が進められ
ている。このうち有機材料については（１１大規模な工
業レベルでの使用にｉえる充分な強度がないこと。（２
）膨張・収縮を起し易い。（３）高温で使用できない。In addition to inorganic materials such as ceramics and glass, the development of porous materials is also progressing on organic materials such as polyacrylamide, agarose, and cellulose materials. Among these, organic materials (11) do not have sufficient strength for use on a large-scale industrial level. (2)
) Easily expands and contracts. (3) Cannot be used at high temperatures.
等の難点があることから、近年特に無機材料についての
開発に力が注がれている。Due to these difficulties, in recent years, efforts have been particularly focused on the development of inorganic materials.
無機系材料では多孔質セラミックスとしてＡｌｚ０３ｍ
’ｒｉｏ２．５ｉ０２ ｅ Ｔｉ０２−Ａｊ？２０３
、 ｚｒｏ２が既ニツくられ実用に供されている。一
方、多孔質ガラスも早くから研究され、例えばＮａ２０
−Ｂ２Ｏ３−８ｉ０２から成る。ホウケイ酸ガラスをｒ
ｏｏ”ｃ以上に加熱してＮａ２０−Ｂ２Ｏ３と５ｉ０２
の２相に分相させ、その後同ガラスを酸性液中に浸すこ
とで目Ｊ溶成分のＮａ２０−Ｂ２Ｏ３相を抽出し、後ｖ
ｃ Ｓｉｏ２の多孔質層を残すという方法も開発されて
いる。Among inorganic materials, Alz03m is used as porous ceramics.
'rio2.5i02 e Ti02-Aj? 203
, ZRO2 has already been developed and put into practical use. On the other hand, porous glasses were also studied early on, such as Na20
-B2O3-8i02. borosilicate glass
Heating to oo”c or higher produces Na20-B2O3 and 5i02
After separating the glass into two phases, the same glass is immersed in an acidic solution to extract the Na20-B2O3 phase, which is the soluble component of the glass.
A method of leaving a porous layer of c Sio2 has also been developed.
しかしながら、これらの多孔質体においては、脱塩用逆
浸透膜、酵素固定用、気体分離膜のように貫通細孔を必
要とし、かつ細孔中を気体・液体などの媒体が通過する
ような場合、媒体の透過性を高めるために高圧で圧送す
る必要が生じる。このため多孔質体を支持管などに圧力
封着するにも少なからぬ問題があった。あるいは気体分
離において気体の種類によっては高圧にすることで分離
効率が低下するという問題があった。However, these porous materials require through-pores, such as reverse osmosis membranes for desalination, enzyme immobilization, and gas separation membranes, and media such as gases and liquids pass through the pores. In some cases, it may be necessary to pump at high pressure to increase the permeability of the medium. For this reason, there were considerable problems in pressure-sealing the porous body to a support tube or the like. Alternatively, in gas separation, depending on the type of gas, there is a problem that the separation efficiency decreases due to high pressure.
Ｃ発明の目的
本発明は、新規な薄膜状ＡＡ２０３多孔質体の製造方法
を提供することを目的とし、圧力損失の少ない多孔質体
の製造方法を提供することを目的とする。C.Object of the Invention The present invention aims to provide a novel method for manufacturing a thin film-like AA203 porous body, and an object of the present invention is to provide a method for manufacturing a porous body with little pressure loss.
ｄ 発明の構成
本発明は、陽極酸化処理によりアルミニウム物体の表面
に多孔質の酸化アルミニウム層を形成せしめ、しかる稜
線多孔質層被覆アルミニウム物体を陰極還元処理して該
多孔質層を母体アルミニウム物体から分離させることを
特徴とする薄膜状Ａｌ２Ｏ３多孔質体の製造方法である
。d.Structure of the Invention The present invention involves forming a porous aluminum oxide layer on the surface of an aluminum object by anodizing treatment, and then cathodically reducing the ridgeline porous layer-coated aluminum object to separate the porous layer from the base aluminum object. This is a method for producing a thin film-like Al2O3 porous material, which is characterized by separation.
陽極酸化法によりアルミニウムの表面に酸化アルミニウ
ム層を形成することは古くから行なわれ、また酸化アル
ミニウム層が多孔質構造を有することも早くから知られ
ていた。しかしながら、従来のアルミニウムの陽極酸化
被膜は主としてアルミニウム表面への装飾的効果の付与
や、化学的耐久性の向上を目的としたもので、近年その
多孔質構造が注目され、エレクトロクロミック素子、磁
性記録拐料など電子材料への応用も研究されているがい
ずれもアルミニウム表面の多孔質酸化アルミニウム層と
しての利用を図ろうとするものであった。本発明はこれ
ら多孔質層をアルミニウム母体からハク熱させ、薄膜型
の多孔質体を提供する処に特徴がある。Forming an aluminum oxide layer on the surface of aluminum by anodic oxidation has been practiced for a long time, and it has also been known for a long time that the aluminum oxide layer has a porous structure. However, conventional anodic oxide coatings on aluminum were mainly used to add decorative effects to the aluminum surface and improve chemical durability; however, in recent years, its porous structure has attracted attention, and it has been used for electrochromic devices, magnetic recording devices, etc. Applications to electronic materials such as nanoparticles have also been studied, but in all cases the aim has been to use it as a porous aluminum oxide layer on the aluminum surface. The present invention is characterized in that these porous layers are heated from an aluminum matrix to provide a thin film type porous body.
アルミニウムを陽極酸化するには、硫酸、シーウ酸、ク
ロム酸、リン酸、スルファミン酸、ベンゼンスルポン酸
などの二塩基酸中にアルミ阜つムを陽４ｉＭとして浸清
し、陰極として鉛、鉄、黒鉛。To anodize aluminum, aluminum is immersed in a dibasic acid such as sulfuric acid, sulfuric acid, chromic acid, phosphoric acid, sulfamic acid, or benzenesulfonic acid as a positive 4iM, and lead or iron is used as a negative electrode. ,graphite.
ケイ素鉄等を用い、両極間で電解操作を行なうのが通常
である。この場合、二塩基酸溶液の濃度。Usually, silicon iron or the like is used and electrolysis is performed between the two electrodes. In this case, the concentration of the dibasic acid solution.
１’ｉ１Ｍ度、電流密度および浴電圧が重要で、一般に
は液温か低く、電流密度が大きく、また液の濃度が低い
ほど多孔度が小さくなる。望ましい条件ぼ電解液の種類
によって異なり、硫酸浴の場合は濃度１０−２０％、電
流密度０．乙〜ｚＡ／ｄｍ２．電圧１０〜２ｔ（Ｖ）＋
温湿１ｓ−２ｓ″Ｃが好ましいとされている。その他、
よく用いられる電解液としてシュウ酸系浴、クロム酸系
浴があり、シュウ酸系の場合、概ね濃度λ〜Ｓ％、電流
密度／〜３Ａ／ｄｍ２．′ｉｉ１圧ｑ。1'i1M degrees, current density, and bath voltage are important; generally, the lower the liquid temperature, the higher the current density, and the lower the concentration of the liquid, the smaller the porosity. Desirable conditions vary depending on the type of electrolyte; in the case of a sulfuric acid bath, the concentration is 10-20% and the current density is 0. Otsu~zA/dm2. Voltage 10~2t(V)+
It is said that a temperature and humidity of 1s-2s''C is preferable.Others:
Commonly used electrolytes include oxalic acid baths and chromic acid baths, and in the case of oxalic acid baths, the concentration is approximately λ~S% and the current density is /~3A/dm2. 'ii1 pressure q.
〜ｘＯ（ｖ）、液１１Ｉｉ ２０〜３０″Ｃの条件が用
いられ、クロム酸系浴の場合濃度２〜３％、電流密度０
．／〜０．３Ａ／ｄｍ２１ 電圧１１０〜ｊＯ（’Ｖ）
、浴ｆ、３０〜’ｉｏ”ｃが適当とされている。この
ようにして多孔質構造を有するアルミニウムの陽極酸化
被膜が得られるが、孔の大きさは１００〜１Ｉｏｏｈで
あり、多孔質層の厚さは電解時間や電流密度の大きさと
ともに厚くなり、条件によっては数７００μにもなる。~xO(v), liquid 11Ii 20~30''C conditions are used, and in the case of a chromic acid bath, the concentration is 2~3%, and the current density is 0.
．． /~0.3A/dm21 Voltage 110~jO('V)
, bath f, 30~'io''c is considered to be appropriate.In this way, an anodic oxide film of aluminum having a porous structure is obtained, but the pore size is 100~1Iooh, and the porous layer The thickness increases with the electrolysis time and current density, and can reach several 700 μm depending on the conditions.
一方、これらの多孔質層をアルミニウム母体からハク熱
させるためには酸性液中へ同多孔体を浸漬するのみでも
よいが、簡単には多孔質膜を作成した処理洛中で同多孔
質体何アルミニウムを陰極とし、別に鉛、黒鉛、鉄など
の陽極を準備し、両極間で電解操作することで実現でき
る。すなわち陰極還元処理を施すことで多孔質薄膜をア
ルミニウム母体からハク熱させることができる。この場
合、浸漬液のＰＨ１′ｌｉＡ度、電流密度が重要でそれ
ぞれ６．０≧ＰＨ、浴温度ｔＳ〜３０°Ｃ１電流密度０
．！；−／ＪＡ／ ｄｍ ２ が望ましい。ここでＰＨ
＞ｔ、０ではアルカリにより得られた膜が溶解するおそ
れがあり、／Ｓ°Ｃ未満の浴温度では膜のハク熱が起こ
りにくく、又ハク熱に長時間を要し、３０″Ｃより高い
浴温度ではハク熱する膜が細片化し、又Ｈ２ガスが多量
に発生する失点となる。又電流密度がＯ’、 ３Ａ／ｃ
ｉｍ ２未満ではハク熱が起こらず／、 ＳＡ／ｄｍ２
より高いとハク熱する膜が細片化する。On the other hand, in order to heat these porous layers from the aluminum matrix, it is sufficient to simply immerse the same porous body in an acidic solution, but it is easy to immerse the same porous body in the process used to create the porous membrane. This can be achieved by preparing a separate anode made of lead, graphite, iron, etc., and performing electrolysis between the two electrodes. That is, by performing cathodic reduction treatment, it is possible to heat the porous thin film from the aluminum matrix. In this case, the PH1'liA degree and current density of the immersion liquid are important, each being 6.0 ≧PH, bath temperature tS~30°C1 current density 0
．． ! ;-/JA/dm 2 is desirable. Here PH
> t, 0, there is a risk that the film obtained with alkali will dissolve, and a bath temperature of less than /S °C will hardly cause the film to heat up, and it will take a long time for the film to heat up, and if the temperature is higher than 30"C. At the bath temperature, the heated film becomes fragmented and a large amount of H2 gas is generated, which is a disadvantage.Also, the current density is O', 3A/c.
Haku fever does not occur below im 2/, SA/dm2
If the temperature is higher, the hot film will break into pieces.
このようにして得られた多孔質酸化アルミニウム薄膜は
孔径１００〜ＩＩｏｏ７ｙの孔を無数に有しており、同
薄膜をメソシュ状の担体ではさみ込むことにより、超微
細な濃過能力を有するフィルターを得ることができ、こ
のようなフィルターは塩類溶液の逆浸透膜、ガス分離膜
などに極めて有用である。The porous aluminum oxide thin film obtained in this way has countless pores with a pore diameter of 100 to IIoo7y, and by sandwiching the same thin film between mesoche-like carriers, a filter with ultrafine concentration ability can be created. Such a filter is extremely useful for reverse osmosis membranes for saline solutions, gas separation membranes, etc.
以下に本発明の詳細な説明する。The present invention will be explained in detail below.
ｅ 実施例
寸法！；ＣｍＸ！；Ｃｍ ｉ厚味２ｍ／ｍのアルミニウ
ム板を濃度１０％のＮａＯＨ水溶液中へ１分浸漬し、次
いで水洗い後濃度／３％のＨ，ＮＯ３水溶液中へ７分浸
漬し、更にその後水洗い後乾燥した。e Example dimensions! ;CmX! ; Cm i An aluminum plate with a thickness of 2 m/m was immersed in a 10% concentration NaOH aqueous solution for 1 minute, then washed with water, then immersed in a 3% concentration H, NO3 aqueous solution for 7 minutes, and then washed with water and dried. .
このような前処理を施したアルミニウム板を濃度／Ｓ％
の硫酸水溶液中へｌｌ５４ｉ１として浸漬し、これと向
い合って浸漬している黒鉛板（陰極）との間Ｋｍ電流密
度、 ｊ、Ａ／ｄｍ２ 、電圧２０（■）の直流電圧を
２０分間印加した。この間硫酸水溶液の温度は２２°Ｃ
に保持した。その後、同じ浴中で今度はアルミニウム板
を陰極、黒鉛板を陽極として直流電圧２０ｖを印加した
。この時の電流密度は７．０Ａ／ｄｍ２ であり、浴温
は先と同様、２２℃であった。Concentration/S% of aluminum plate subjected to such pretreatment
A DC voltage of Km current density, j, A/dm2, and voltage of 20 (■) was applied for 20 minutes between this and the graphite plate (cathode) immersed in the sulfuric acid solution for 20 minutes. . During this time, the temperature of the sulfuric acid aqueous solution was 22°C.
was held at Thereafter, in the same bath, a DC voltage of 20 V was applied, using the aluminum plate as a cathode and the graphite plate as an anode. The current density at this time was 7.0 A/dm2, and the bath temperature was 22°C as before.
このような操作を７０分間続けたところ、硫酸水溶液中
に半透明な薄片が浮遊しているのが認められた。この薄
片の中から大きさが約ｊ’ｃｍＸ／Ｃｍのものを硫酸水
溶液から取出し、蒸留水中へ入れゆるく攪拌の後、再度
取出し１０メツシーのフルイ上で自然乾燥した。When this operation was continued for 70 minutes, translucent flakes were observed floating in the sulfuric acid aqueous solution. Among these flakes, those having a size of about j'cmX/Cm were taken out from the sulfuric acid aqueous solution, put into distilled water, and stirred gently, then taken out again and air-dried on a 10 mesh sieve.
この後同薄片を２つに折半し、７つはＸ線マイクロアナ
ライザーによる定性分析に供した。その結果、薄片が殆
んどＡＡ！２０３から成っていることが判明した。一方
もう一つの薄片は電子顕微鏡による薄片の表面構造・断
面構造の観察に供した。その結果、表面・断面いずれの
構造も多孔質のスポンジ状構造から成り、孔径はｔ’ｏ
ｏ−ｓｏｏＸ 、Ｎ片の厚味は約にμであることが判明
した。Thereafter, the same thin section was divided into two halves, and seven were subjected to qualitative analysis using an X-ray microanalyzer. As a result, most of the flakes were AA! It turns out that it consists of 203. On the other hand, the other thin section was used for observation of the surface structure and cross-sectional structure of the thin section using an electron microscope. As a result, both the surface and cross-sectional structure consist of a porous sponge-like structure, and the pore size is t'o
The thickness of the o-sooX and N pieces was found to be approximately μ.
発明の効果
本発明によれば、薄膜状の多孔質体をＩＭｆ単な方法で
得ることができる。又上記実施例によりあきらかな通り
、本発明により作成した薄膜状多孔質、膜はＡＩ！２０
３からなり、多孔質体として使用出来る特性を有する物
である。Effects of the Invention According to the present invention, a thin film-like porous body can be obtained by a simple IMf method. Furthermore, as is clear from the above examples, the thin film-like porous membrane prepared according to the present invention is AI! 20
3, and has characteristics that allow it to be used as a porous body.
Claims (1)
葛酸□ア７１．−ウ４層ｔｔＪＩ、ワ、い、５カ、る稜
線多孔質層被覆アルミニウム物体を陰極還元処理して該
多孔質層を母体アルミニウム物体から盆離させることを
特徴とする薄膜状ＡＩ！２０３多孔質体の多孔方体。・Porous katric acid□A71. - Thin film-like AI characterized by cathodic reduction treatment of an aluminum object coated with a 4-layer ttJI, 5-layer ridgeline porous layer to separate the porous layer from the base aluminum object! 203 Porous parallelepiped of porous body.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| JP3214784A JPS60177198A (en) | 1984-02-22 | 1984-02-22 | Production of thin film-like porous body of al2o3 |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| JP3214784A JPS60177198A (en) | 1984-02-22 | 1984-02-22 | Production of thin film-like porous body of al2o3 |
Publications (1)
| Publication Number | Publication Date |
|---|---|
| JPS60177198A true JPS60177198A (en) | 1985-09-11 |
Family
ID=12350788
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| JP3214784A Pending JPS60177198A (en) | 1984-02-22 | 1984-02-22 | Production of thin film-like porous body of al2o3 |
Country Status (1)
| Country | Link |
|---|---|
| JP (1) | JPS60177198A (en) |
Cited By (12)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| JPS60187320A (en) * | 1984-03-07 | 1985-09-24 | Toyo Soda Mfg Co Ltd | Gas separation using anodized aluminum film |
| JPS62185898A (en) * | 1986-02-03 | 1987-08-14 | アルカン・インタ−ナシヨナル・リミテツド | Porous anodic oxidation aluminum film and its production |
| US4973435A (en) * | 1987-11-03 | 1990-11-27 | Alcan International Limited | Method of producing porous membranes of sinterable refractory metal oxides |
| US5112449A (en) * | 1989-03-22 | 1992-05-12 | Alcan International Limited | Two phase metal/oxide films |
| US5218472A (en) * | 1989-03-22 | 1993-06-08 | Alcan International Limited | Optical interference structures incorporating porous films |
| JPH0967173A (en) * | 1995-08-31 | 1997-03-11 | Univ Tohoku | Production of porous alumina tube |
| US6139713A (en) * | 1996-08-26 | 2000-10-31 | Nippon Telegraph And Telephone Corporation | Method of manufacturing porous anodized alumina film |
| KR100502554B1 (en) * | 1998-09-03 | 2005-10-19 | 한국타이어 주식회사 | Manufacturing method of cylindrical separator with improved durability |
| JP2007070126A (en) * | 2005-09-02 | 2007-03-22 | Japan Organo Co Ltd | Method for producing filtering membrane for capturing particulate, filtering membrane for capturing particulate, and method for measuring particulate in ultrapure water |
| JP2011500969A (en) * | 2007-10-26 | 2011-01-06 | ユニヴェルシテ ポール サバティエ トゥールーズ トロワ | Method for producing a regular porous structure from an aluminum substrate |
| US8147621B2 (en) * | 2002-05-14 | 2012-04-03 | Infineon Technologies Ag | Method for producing a metal article intended for at least partially coating with a substance |
| JP2022530694A (en) * | 2019-06-17 | 2022-06-30 | ナノペック， インコーポレイテッド | Nanoporous anodized aluminum membrane for healthcare and biotechnology |
Citations (1)
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|---|---|---|---|---|
| JPS5331883A (en) * | 1976-09-06 | 1978-03-25 | Honda Senriyouten Kk | Rotary screen apparatus for flat screen printing machine |
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| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| JPS5331883A (en) * | 1976-09-06 | 1978-03-25 | Honda Senriyouten Kk | Rotary screen apparatus for flat screen printing machine |
Cited By (12)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| JPS60187320A (en) * | 1984-03-07 | 1985-09-24 | Toyo Soda Mfg Co Ltd | Gas separation using anodized aluminum film |
| JPS62185898A (en) * | 1986-02-03 | 1987-08-14 | アルカン・インタ−ナシヨナル・リミテツド | Porous anodic oxidation aluminum film and its production |
| US4973435A (en) * | 1987-11-03 | 1990-11-27 | Alcan International Limited | Method of producing porous membranes of sinterable refractory metal oxides |
| US5112449A (en) * | 1989-03-22 | 1992-05-12 | Alcan International Limited | Two phase metal/oxide films |
| US5218472A (en) * | 1989-03-22 | 1993-06-08 | Alcan International Limited | Optical interference structures incorporating porous films |
| JPH0967173A (en) * | 1995-08-31 | 1997-03-11 | Univ Tohoku | Production of porous alumina tube |
| US6139713A (en) * | 1996-08-26 | 2000-10-31 | Nippon Telegraph And Telephone Corporation | Method of manufacturing porous anodized alumina film |
| KR100502554B1 (en) * | 1998-09-03 | 2005-10-19 | 한국타이어 주식회사 | Manufacturing method of cylindrical separator with improved durability |
| US8147621B2 (en) * | 2002-05-14 | 2012-04-03 | Infineon Technologies Ag | Method for producing a metal article intended for at least partially coating with a substance |
| JP2007070126A (en) * | 2005-09-02 | 2007-03-22 | Japan Organo Co Ltd | Method for producing filtering membrane for capturing particulate, filtering membrane for capturing particulate, and method for measuring particulate in ultrapure water |
| JP2011500969A (en) * | 2007-10-26 | 2011-01-06 | ユニヴェルシテ ポール サバティエ トゥールーズ トロワ | Method for producing a regular porous structure from an aluminum substrate |
| JP2022530694A (en) * | 2019-06-17 | 2022-06-30 | ナノペック， インコーポレイテッド | Nanoporous anodized aluminum membrane for healthcare and biotechnology |
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