JP2004188358A - Manufacturing method for hydrogen separation member - Google Patents

Manufacturing method for hydrogen separation member Download PDF

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Publication number
JP2004188358A
JP2004188358A JP2002361643A JP2002361643A JP2004188358A JP 2004188358 A JP2004188358 A JP 2004188358A JP 2002361643 A JP2002361643 A JP 2002361643A JP 2002361643 A JP2002361643 A JP 2002361643A JP 2004188358 A JP2004188358 A JP 2004188358A
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Prior art keywords
hydrogen separation
hydrogen
separation membrane
pores
metal
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JP3845372B2 (en
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Atsushi Gamachi
厚志 蒲地
Shunsuke Itami
俊輔 伊丹
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Honda Motor Co Ltd
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Honda Motor Co Ltd
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Abstract

<P>PROBLEM TO BE SOLVED: To reduce the number of manufacturing processes of a hydrogen separation member and to improve manufacturing efficiency. <P>SOLUTION: The hydrogen separation member 1 is provided with a metallic hydrogen separation membrane 2 for selectively transmitting hydrogen and a porous base material 4 having a plurality of pores 3 for transmitting the hydrogen. A manufacturing method includes the means for: forming the hydrogen separation membrane 2 on one surface of a resist sheet 6; obtaining the negative model 12 of the porous base material 4 by performing X-ray lithography with the resist sheet 6 as a body to be irradiated; filling a metal 15 by electroforming in a recessed part 11 corresponding to a peripheral wall 5 around each pore of the negative model 4; and obtaining the porous base material 4 composed of the metal 15 by removing a part 10 corresponding to each pore 3 of the negative model 12 and these means are used. <P>COPYRIGHT: (C)2004,JPO&NCIPI

Description

【０００１】
【発明の属する技術分野】
本発明は，水素分離部材，特に，水素を選択的に透過させる金属製水素分離膜と，その水素分離膜を支持し，且つ水素を通過させる複数の細孔を持つ多孔質基材とを有する水素分離部材の製造方法に関する。
【０００２】
【従来の技術】
水素分離部材は，例えば，水素を含む混合ガスから高純度の水素を取出すために用いられる。この場合，水素分離膜としては薄いもの程水素透過速度が速いことから，その膜形成に当ってはスパッタリング等の薄膜形成技術が採用されている。
【０００３】
ところが，多孔質基材の水素分離膜形成面には複数の細孔の開口が存在するため，膜形成時に水素分離膜が部分的に細孔の開口内に陥没し，その膜が薄いことから陥没部分が裂けてピンホールが発生したり，陥没部分が厚くなって水素に対する選択透過性が不十分となる，等の問題があった。
【０００４】
そこで，前記問題を解決すべく，次のような方法が開発されている。即ち，（１）金属板の一面に電解メッキ処理を施して水素分離膜を形成する，（２）水素分離膜の表面にホトレジスト層を形成する，（３）ホトレジスト層に，ホトリソグラフィを適用して，複数の細孔に対応する部分を残置し，且つ細孔の周壁に対応する部分を除去された，多孔質基材のネガティブモデルを得る，（４）ネガティブモデルに電解メッキを施して，細孔の周壁に対応する部分に金属を充填する，（５）ネガティブモデルの細孔に対応する部分を除去して金属よりなる多孔質体を得る，（６）金属板を水素分離膜から分離する，といった手段を採用するものである。この場合，前記ホトリソグラフィをＸ線リソグラフィに代えることが可能である（例えば，特許文献１参照）。
【０００５】
【特許文献１】
特開平１１−１０４４７２号公報，［００１０］，図３
【０００６】
【発明が解決しようとする課題】
しかしながら前記従来法においては，金属板を電極として用いて電解メッキにより水素分離膜および多孔質基材を形成しているので，最終的に金属板を水素分離膜から分離しなければならず，またホトリソグラフィの実施に当りホトレジスト層の形成も必須工程となるもので，水素分離部材の製造工程数が多く製造能率が悪い，という問題があった。また金属板の分離作業中に薄い水素分離膜を傷付けるおそれもあった。
【０００７】
【課題を解決するための手段】
本発明は，水素分離部材の製造工程数を少なくして製造能率を向上させると共に健全な水素分離膜を備えた水素分離部材を得ることが可能な前記製造方法を提供することを目的とする。
【０００８】
前記目的を達成するため本発明によれば，水素を選択的に透過させる金属製水素分離膜と，その水素分離膜を支持し，且つ水素を通過させる複数の細孔を持つ多孔質基材とを有する水素分離部材を製造するに当り，レジストシートの一面に前記水素分離膜を形成する工程と，前記レジストシートを被照射体とする，Ｘ線リソグラフィおよびＸ線ドライエッチングの一方を行って，複数の前記細孔に対応する部分を残置され，且つ各細孔回りの周壁に対応する部分を除去された，前記多孔質基材のネガティブモデルを得る工程と，前記ネガティブモデルの，各細孔回りの周壁に対応する凹部に電鋳によって金属を充填する工程と，前記ネガティブモデルの各細孔に対応する部分を除去して前記金属よりなる前記多孔質基材を得る工程，とを用いる水素分離部材の製造方法が提供される。
【０００９】
前記方法によれば，４工程にて水素分離部材を得ることができ，これは従来法の６工程に比べて製造工数が少なく，したがって製造能率の向上を図ることができる。一方，水素分離膜に関係する作業は，電鋳に先立って行われるマスキングおよび電極として用いるためのリード線の接続，といったものであるから，この作業による水素分離膜の損傷を回避することは容易である。
【００１０】
また本発明によれば，水素を選択的に透過させる金属製水素分離膜と，その水素分離膜を支持し，且つ水素を通過させる複数の細孔を持つ多孔質基材とを有する水素分離部材を製造するに当り，前記多孔質基材を得るためのレジストシートの一面に前記水素分離膜を形成する工程と，前記レジストシートを被照射体とする，Ｘ線リソグラフィおよびＸ線ドライエッチングの一方を行って前記複数の前記細孔を形成することにより前記多孔質基材を得る工程と，を用いる水素分離部材の製造方法が提供される。
【００１１】
このようにして得られた水素分離部材は，多孔質基材がレジストシートを製造材料としていることから，その使用温度を，例えば１００〜１５０℃に限定される。この場合にも製造工程数は２工程といったように少なく，したがって製造能率の向上を図ることができる。
【００１２】
Ｘ線リソグラフィとＸ線ドライエッチングを比べると，Ｘ線ドライエッチングの場合は現像が不要であることからＸ線リソグラフィに比べて能率的である。
【００１３】
【発明の実施の形態】
〔第１実施例〕
図１〜３において，水素分離部材１は，水素を選択的に透過させる金属製水素分離膜２と，その水素分離膜２を支持し，且つ水素を通過させる複数の六角形細孔３を持つハニカム構造の多孔質基材４とを有する。水素分離膜２はＰｄまたはＰｄ−Ａｇ合金等のＰｄ合金より構成され，その厚さは０．１〜２．０μｍ，例えば０．２μｍである。多孔質基材４はＮｉ，Ｃｕ等の金属より構成され，その厚さは２５〜２００μｍ，例えば１００μｍである。六角形細孔３の対向角部間の長さａは，例えば５μｍ，また細孔３回りの周壁５において，相隣る両六角形細孔３間の厚さｂは，例えば３μｍである。水素分離膜２の形成に当ってはＰＶＤ，例えば，スパッタリング，イオンプレーティング，イオンビーム蒸着等が採用されるが，メッキ法，プラズマＣＶＤ等の適用も可能である。
【００１４】
水素分離部材１は次のような方法で製造される。
【００１５】
（１）図４（ａ）に示すように，例えばＰＭＭＡよりなるレジストシート６の一面にＰｄよりなる水素分離膜２を，例えばスパッタリングにより形成する。
【００１６】
（２）図４（ｂ）に示すように，レジストシート６を被照射体とするＸ線リソグラフィを行うべく，そのレジストシート６の他面に図５に示すＸ線マスク７を載せる。このＸ線マスク７は，複数の六角形細孔３に対応する六角形部分８をＸ線を透過させない材料，例えばＡｕ，Ｔａ，Ｗ−Ｔｉ等より構成され，また各六角形細孔３回りの周壁５に対応する部分９をＸ線を透過させる材料，例えばＳｉＣ，Ｓｉ3 Ｎ4 ，ダイヤモンド等より構成されている。Ｘ線マスク７の上方より，シンクロトロン放射（ＳＲ）光装置から直進性の良いＸ線，つまりＳＲ光Ｘ線を照射する。これによりレジストシート６のＸ線被照射部分，つまり各六角形細孔３回りの周壁５に対応する部分は高分子の連鎖が切断されて分子量が減少し，一方，Ｘ線未照射部分，つまり各六角形細孔３に対応する部分は未変化である。
【００１７】
（３）図４（ｃ）に示すように，レジストシート６に現像液を付与すると，各六角形細孔３に対応する部分１０を残置され，且つ各六角形細孔３回りの周壁５に対応する部分を溶解除去されて凹部１１にされたもの，つまり多孔質基材４のネガティブモデル１２が得られる。
【００１８】
図４（ｄ）に示すように，水素分離膜２を電気絶縁性マスク１３により被覆し，またネガティブモデル１２の周面を電気絶縁性型枠１４により囲んだ状態にて，ネガティブモデル１２の，各六角形細孔３回りの周壁５に対応する凹部１１に電鋳によって金属１５，例えばＮｉを充填する。
【００１９】
（５）図４（ｅ）に示すように，ネガティブモデル１２の各六角形細孔３に対応する部分１０，マスク１３および型枠１４を除去して金属１５よりなる多孔質基材４を得る。前記部分１０の除去に当っては，溶剤による溶解，ＳＲ光Ｘ線照射後現像液の付与等が行われる。
【００２０】
〔第２実施例〕
図６〜８に示す水素分離部材１は，前記同様にＰｄ等より構成された金属製水素分離膜２と，前記同様の形態を持つ多孔質基材４とを有する。ただし，多孔質基材４はレジストシート６を製造材料としていることから，水素分離部材１の使用温度は，例えば１００〜１５０℃に限定される。
【００２１】
水素分離部材１は次のような方法で製造される。
【００２２】
（１）図９（ａ）に示すように，例えばＰＭＭＡよりなるレジストシート６の一面にＰｄよりなる水素分離膜２を，例えばスパッタリングにより形成する。
【００２３】
（２）図９（ｂ）に示すように，レジストシート６を被照射体とするＸ線リソグラフィを行うべく，そのレジストシート６の他面に図１０に示すＸ線マスク７を載せる。このＸ線マスク７は，複数の六角形細孔３に対応する六角形部分８をＸ線を透過させる材料，例えばＳｉＣ，Ｓｉ3 Ｎ4 ，ダイヤモンド等より構成され，また各六角形細孔３回りの周壁５に対応する部分９をＸ線を透過させない材料，例えばＡｕ，Ｔａ，Ｗ−Ｔｉ等より構成されている。Ｘ線マスク８の上方より，シンクロトロン放射（ＳＲ）光装置から直線性の良いＸ線，つまりＳＲ光Ｘ線を照射する。これによりレジストシート６のＸ線被照射部分，つまり各六角形細孔３に対応する部分は高分子の連鎖が切断されて分子量が減少し，一方，Ｘ線未照射分，つまり各六角形細孔３回りの周壁５に対応する部分は未変化である。
【００２４】
（３）図９（ｃ）に示すように，レジストシート６に現像液を付与すると，各六角形細孔３に対応する部分が溶解除去され，且つ各六角形細孔３回りの周壁５に対応する部分が残置された多孔質基材４が得られる。
【００２５】
例えば，ＰＴＦＥ，ＰＦＡ等よりなるレジストシート６を被照射体としてＸ線ドライエッチングを行い，これにより多孔質基材４を得ることもできる。即ち，図９（ｂ）工程において前記材料よりなるレジストシート６にＳＲ光Ｘ線を照射すると，各六角形細孔３に対応する部分が分解除去されるもので，したがって現像を行う必要がない。
【００２６】
このＸ線ドライエッチングは，第１実施例において，図４（ｂ），（ｅ）工程において適用可能である。
【００２７】
【発明の効果】
請求項１記載の発明によれば，金属を構成材料とする多孔質基材を備えた水素分離部材の製造工程数を少なくして製造能率を向上させると共に健全な水素分離膜を備えた水素分離部材を得ることが可能な製造方法を提供することができる。
【００２８】
請求項２記載の発明によれば，レジストシートを構成材料とする多孔質基材を有し，また健全な水素分離膜を備えた水素分離部材を能率良く得ることが可能な製造方法を提供することができる。
【図面の簡単な説明】
【図１】水素分離部材の一例の平面図である。
【図２】図１，３の２−２線断面図である。
【図３】図２の３矢視図である。
【図４】水素分離部材の一例の製造工程説明図である。
【図５】Ｘ線マスクの一例の平面図である。
【図６】水素分離部材の他例の平面図である。
【図７】図６，８の７−７線断面図である。
【図８】図７の８矢視図である。
【図９】水素分離部材の他例の製造工程説明図である。
【図１０】Ｘ線マスクの他例の平面図である。
【符号の説明】
１…………水素分離部材
２…………水素分離膜
３…………細孔
４…………多孔質基材
５…………周壁
６…………レジストシート
１０………細孔に対応する部分
１２………ネガティブモデル
１５………金属[0001]
TECHNICAL FIELD OF THE INVENTION
The present invention has a hydrogen separation member, in particular, a metal hydrogen separation membrane that selectively permeates hydrogen, and a porous substrate that supports the hydrogen separation membrane and has a plurality of pores that allow hydrogen to pass therethrough. The present invention relates to a method for manufacturing a hydrogen separation member.
[0002]
[Prior art]
The hydrogen separation member is used, for example, for extracting high-purity hydrogen from a mixed gas containing hydrogen. In this case, the thinner the hydrogen separation membrane, the higher the hydrogen permeation rate. Therefore, a thin film forming technique such as sputtering is employed in forming the membrane.
[0003]
However, since there are multiple pore openings on the surface of the porous substrate on which the hydrogen separation membrane is formed, the hydrogen separation membrane partially sinks into the pore openings during membrane formation, and the membrane is thin. There have been such problems that the depressed portion is torn and pinholes are generated, and the depressed portion becomes thick and the permselectivity to hydrogen becomes insufficient.
[0004]
Therefore, the following method has been developed to solve the above problem. That is, (1) an electrolytic plating process is performed on one surface of a metal plate to form a hydrogen separation film, (2) a photoresist layer is formed on the surface of the hydrogen separation film, and (3) photolithography is applied to the photoresist layer. To obtain a negative model of the porous substrate in which the portions corresponding to the plurality of pores are left and the portions corresponding to the peripheral walls of the pores are removed. (4) Electroplating the negative model, Filling the portion corresponding to the peripheral wall of the pores with metal, (5) removing the portion corresponding to the pores of the negative model to obtain a porous body made of metal, (6) separating the metal plate from the hydrogen separation membrane That is, such a means is adopted. In this case, it is possible to replace the photolithography with the X-ray lithography (for example, see Patent Document 1).
[0005]
[Patent Document 1]
JP-A-11-104472, [0010], FIG.
[0006]
[Problems to be solved by the invention]
However, in the above-mentioned conventional method, since the hydrogen separation membrane and the porous substrate are formed by electrolytic plating using a metal plate as an electrode, the metal plate must be finally separated from the hydrogen separation membrane. The formation of a photoresist layer is also an essential step when performing photolithography, and there is a problem that the number of steps for manufacturing a hydrogen separating member is large and the manufacturing efficiency is poor. In addition, there is a possibility that the thin hydrogen separation membrane may be damaged during the operation of separating the metal plate.
[0007]
[Means for Solving the Problems]
SUMMARY OF THE INVENTION It is an object of the present invention to provide a manufacturing method capable of improving the manufacturing efficiency by reducing the number of manufacturing steps of a hydrogen separation member and obtaining a hydrogen separation member having a sound hydrogen separation membrane.
[0008]
According to the present invention, in order to achieve the above object, according to the present invention, there is provided a metal hydrogen separation membrane that selectively permeates hydrogen, a porous base material that supports the hydrogen separation membrane and has a plurality of pores through which hydrogen passes. In producing a hydrogen separation member having: a step of forming the hydrogen separation film on one surface of a resist sheet, and performing one of X-ray lithography and X-ray dry etching using the resist sheet as an irradiation target; Obtaining a negative model of the porous substrate, in which portions corresponding to the plurality of pores are left and portions corresponding to peripheral walls around the respective pores are removed; A step of filling the recess corresponding to the surrounding peripheral wall with a metal by electroforming, and a step of removing the portion corresponding to each pore of the negative model to obtain the porous substrate made of the metal. Method of manufacturing a hydrogen separation member.
[0009]
According to the above method, a hydrogen separation member can be obtained in four steps, and the number of manufacturing steps is smaller than that in the conventional method of six steps, so that the manufacturing efficiency can be improved. On the other hand, work related to the hydrogen separation membrane involves masking performed prior to electroforming and connection of lead wires for use as electrodes, so it is easy to avoid damage to the hydrogen separation membrane due to this work. It is.
[0010]
Further, according to the present invention, a hydrogen separation member having a metal hydrogen separation membrane that selectively permeates hydrogen and a porous base material that supports the hydrogen separation membrane and has a plurality of pores that allow hydrogen to pass therethrough. Forming a hydrogen separation membrane on one surface of a resist sheet for obtaining the porous substrate; and performing one of X-ray lithography and X-ray dry etching using the resist sheet as an object to be irradiated. And forming the plurality of pores to obtain the porous substrate, and a method for producing a hydrogen separation member using the method.
[0011]
The operating temperature of the hydrogen separating member thus obtained is limited to, for example, 100 to 150 ° C. because the porous base material is made of a resist sheet. Also in this case, the number of manufacturing steps is as small as two steps, so that the manufacturing efficiency can be improved.
[0012]
When comparing X-ray lithography and X-ray dry etching, in the case of X-ray dry etching, development is not required, so that it is more efficient than X-ray lithography.
[0013]
BEST MODE FOR CARRYING OUT THE INVENTION
[First embodiment]
1 to 3, a hydrogen separation member 1 has a metal hydrogen separation membrane 2 that selectively permeates hydrogen and a plurality of hexagonal pores 3 that support the hydrogen separation membrane 2 and allow hydrogen to pass therethrough. And a porous substrate 4 having a honeycomb structure. The hydrogen separation membrane 2 is made of Pd or a Pd alloy such as a Pd-Ag alloy, and has a thickness of 0.1 to 2.0 μm, for example, 0.2 μm. The porous substrate 4 is made of a metal such as Ni or Cu, and has a thickness of 25 to 200 μm, for example, 100 μm. The length a between the opposing corners of the hexagonal pores 3 is, for example, 5 μm, and the thickness b between adjacent hexagonal pores 3 on the peripheral wall 5 around the pores 3 is, for example, 3 μm. In forming the hydrogen separation membrane 2, PVD, for example, sputtering, ion plating, ion beam evaporation, or the like is adopted, but plating, plasma CVD, or the like can also be applied.
[0014]
The hydrogen separating member 1 is manufactured by the following method.
[0015]
(1) As shown in FIG. 4A, a hydrogen separation film 2 made of Pd is formed on one surface of a resist sheet 6 made of, for example, PMMA by, for example, sputtering.
[0016]
(2) As shown in FIG. 4B, an X-ray mask 7 shown in FIG. 5 is placed on the other surface of the resist sheet 6 in order to perform X-ray lithography using the resist sheet 6 as an irradiation target. This X-ray mask 7 is made of a material that does not transmit X-rays, such as Au, Ta, W-Ti, etc., in hexagonal portions 8 corresponding to the plurality of hexagonal pores 3. The portion 9 corresponding to the peripheral wall 5 is made of a material that transmits X-rays, for example, SiC, Si 3 N 4 , diamond or the like. From above the X-ray mask 7, a synchrotron radiation (SR) light device irradiates X-rays with good straightness, that is, SR light X-rays. Thereby, the X-ray irradiated portion of the resist sheet 6, that is, the portion corresponding to the peripheral wall 5 around each hexagonal pore 3 is broken in the chain of the polymer, and the molecular weight is reduced. The portion corresponding to each hexagonal pore 3 is unchanged.
[0017]
(3) As shown in FIG. 4 (c), when the developing solution is applied to the resist sheet 6, the portions 10 corresponding to the respective hexagonal pores 3 are left, and the peripheral wall 5 around each hexagonal pore 3 is formed. A concave portion 11 obtained by dissolving and removing a corresponding portion, that is, a negative model 12 of the porous substrate 4 is obtained.
[0018]
As shown in FIG. 4 (d), the hydrogen separation membrane 2 is covered with an electrically insulating mask 13, and the surrounding surface of the negative model 12 is surrounded by an electrically insulating mold 14. A recess 15 corresponding to the peripheral wall 5 around each hexagonal pore 3 is filled with a metal 15, for example, Ni by electroforming.
[0019]
(5) As shown in FIG. 4E, the portion 10, the mask 13, and the mold 14 corresponding to each hexagonal pore 3 of the negative model 12 are removed to obtain the porous substrate 4 made of the metal 15. . In removing the portion 10, dissolution with a solvent, application of a developing solution after SR light X-ray irradiation, and the like are performed.
[0020]
[Second embodiment]
The hydrogen separation member 1 shown in FIGS. 6 to 8 has a metal hydrogen separation membrane 2 made of Pd or the like as described above, and a porous substrate 4 having the same form as described above. However, since the porous substrate 4 uses the resist sheet 6 as a manufacturing material, the operating temperature of the hydrogen separation member 1 is limited to, for example, 100 to 150 ° C.
[0021]
The hydrogen separating member 1 is manufactured by the following method.
[0022]
(1) As shown in FIG. 9A, a hydrogen separation film 2 made of Pd is formed on one surface of a resist sheet 6 made of, for example, PMMA by, for example, sputtering.
[0023]
(2) As shown in FIG. 9B, an X-ray mask 7 shown in FIG. 10 is placed on the other surface of the resist sheet 6 in order to perform X-ray lithography using the resist sheet 6 as an irradiation target. The X-ray mask 7 is made of a material that transmits X-rays through hexagonal portions 8 corresponding to the plurality of hexagonal pores 3, for example, SiC, Si 3 N 4 , diamond, or the like. The portion 9 corresponding to the surrounding peripheral wall 5 is made of a material that does not transmit X-rays, for example, Au, Ta, W-Ti or the like. From above the X-ray mask 8, X-rays with good linearity, that is, SR light X-rays, are emitted from a synchrotron radiation (SR) light device. As a result, the portion of the resist sheet 6 which is exposed to X-rays, that is, the portion corresponding to each hexagonal pore 3, is broken in the chain of the polymer and the molecular weight is reduced. The portion corresponding to the peripheral wall 5 around the hole 3 is unchanged.
[0024]
(3) As shown in FIG. 9 (c), when a developing solution is applied to the resist sheet 6, a portion corresponding to each hexagonal pore 3 is dissolved and removed, and the peripheral wall 5 around each hexagonal pore 3 is removed. A porous substrate 4 having a corresponding portion left is obtained.
[0025]
For example, the porous substrate 4 can be obtained by performing X-ray dry etching using a resist sheet 6 made of PTFE, PFA or the like as an irradiation target. That is, when the resist sheet 6 made of the above material is irradiated with the SR light X-rays in the step of FIG. 9B, the portions corresponding to the respective hexagonal pores 3 are decomposed and removed, so that there is no need to perform development .
[0026]
This X-ray dry etching is applicable in the steps of FIGS. 4B and 4E in the first embodiment.
[0027]
【The invention's effect】
According to the first aspect of the present invention, the number of steps for manufacturing a hydrogen separation member having a porous base material made of metal is reduced, thereby improving the production efficiency and hydrogen separation with a sound hydrogen separation membrane. A manufacturing method capable of obtaining a member can be provided.
[0028]
According to the second aspect of the present invention, there is provided a manufacturing method capable of efficiently obtaining a hydrogen separation member having a porous base material using a resist sheet as a constituent material and having a sound hydrogen separation membrane. be able to.
[Brief description of the drawings]
FIG. 1 is a plan view of an example of a hydrogen separation member.
FIG. 2 is a sectional view taken along line 2-2 of FIGS.
FIG. 3 is a view as viewed in the direction of arrow 3 in FIG. 2;
FIG. 4 is a diagram illustrating a manufacturing process of an example of a hydrogen separation member.
FIG. 5 is a plan view of an example of an X-ray mask.
FIG. 6 is a plan view of another example of the hydrogen separation member.
FIG. 7 is a sectional view taken along line 7-7 of FIGS.
8 is a view taken in the direction of the arrow 8 in FIG. 7;
FIG. 9 is an explanatory view of a manufacturing process of another example of the hydrogen separation member.
FIG. 10 is a plan view of another example of the X-ray mask.
[Explanation of symbols]
1 ... Hydrogen separation member 2 ... Hydrogen separation membrane 3 ... Pores 4 ... Porous base material 5 ... Peripheral wall 6 ... Resist sheet 10 ... Narrow Portion corresponding to hole 12 Negative model 15 Metal

Claims (2)

水素を選択的に透過させる金属製水素分離膜（２）と，その水素分離膜（２）を支持し，且つ水素を通過させる複数の細孔（３）を持つ多孔質基材（４）とを有する水素分離部材（１）を製造するに当り，レジストシート（６）の一面に前記水素分離膜（２）を形成する工程と，前記レジストシート（６）を被照射体とする，Ｘ線リソグラフィおよびＸ線ドライエッチングの一方を行って，複数の前記細孔（３）に対応する部分（１０）を残置され，且つ各細孔（３）回りの周壁（５）に対応する部分を除去された，前記多孔質基材（４）のネガティブモデル（１２）を得る工程と，前記ネガティブモデル（１２）の，各細孔（３）回りの周壁（５）に対応する凹部（１１）に電鋳によって金属（１５）を充填する工程と，前記ネガティブモデル（１２）の各細孔（３）に対応する部分（１０）を除去して前記金属（１５）よりなる前記多孔質基材（４）を得る工程，とを用いることを特徴とする水素分離部材の製造方法。A metal hydrogen separation membrane (2) for selectively permeating hydrogen, and a porous substrate (4) supporting the hydrogen separation membrane (2) and having a plurality of pores (3) for passing hydrogen. Forming a hydrogen separation film (2) on one surface of a resist sheet (6) when manufacturing a hydrogen separation member (1) having: By performing one of lithography and X-ray dry etching, portions (10) corresponding to the plurality of pores (3) are left, and portions corresponding to the peripheral wall (5) around each of the pores (3) are removed. Obtaining the negative model (12) of the porous substrate (4), and forming the negative model (12) in the concave portion (11) corresponding to the peripheral wall (5) around each pore (3) in the negative model (12). Filling a metal (15) by electroforming; Removing the portion (10) corresponding to each pore (3) of the metal (12) to obtain the porous substrate (4) made of the metal (15). A method for manufacturing a separation member. 水素を選択的に透過させる金属製水素分離膜（３）と，その水素分離膜（２）を支持し，且つ水素を通過させる複数の細孔（３）を持つ多孔質基材（４）とを有する水素分離部材（１）を製造するに当り，前記多孔質基材（４）を得るためのレジストシート（６）の一面に前記水素分離膜（２）を形成する工程と，前記レジストシート（６）を被照射体とする，Ｘ線リソグラフィおよびＸ線ドライエッチングの一方を行って前記複数の前記細孔（３）を形成することにより前記多孔質基材（４）を得る工程と，を用いることを特徴とする水素分離部材の製造方法。A metal hydrogen separation membrane (3) for selectively permeating hydrogen, and a porous substrate (4) supporting the hydrogen separation membrane (2) and having a plurality of pores (3) for passing hydrogen. Forming a hydrogen separation membrane (2) on one surface of a resist sheet (6) for obtaining the porous substrate (4) in manufacturing the hydrogen separation member (1) having (6) using the object to be irradiated, performing one of X-ray lithography and X-ray dry etching to form the plurality of pores (3), thereby obtaining the porous substrate (4); A method for producing a hydrogen separation member, characterized by using:
JP2002361643A 2002-12-13 2002-12-13 Method for producing hydrogen separation member Expired - Fee Related JP3845372B2 (en)

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JP2006068699A (en) * 2004-09-06 2006-03-16 New Industry Research Organization Filter, microreactor and manufacturing method for the same, structure constituted of juxtaposed microreactors, and analyzer
JP2008068231A (en) * 2006-09-15 2008-03-27 Kitami Institute Of Technology Hydrogen-permeable membrane and its manufacturing method
JP2008289970A (en) * 2007-05-23 2008-12-04 Sumitomo Metal Mining Co Ltd Hydrogen permeable membrane and its manufacturing method
WO2012063953A1 (en) * 2010-11-11 2012-05-18 東京エレクトロン株式会社 Method for producing filtration filter
WO2013147540A1 (en) * 2012-03-30 2013-10-03 한국전기연구원 Composite separating film formed from metal supporting layer and metal oxide film, using concavo-convex patterned metal, and production method therefor
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* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
JP2006068699A (en) * 2004-09-06 2006-03-16 New Industry Research Organization Filter, microreactor and manufacturing method for the same, structure constituted of juxtaposed microreactors, and analyzer
JP2008068231A (en) * 2006-09-15 2008-03-27 Kitami Institute Of Technology Hydrogen-permeable membrane and its manufacturing method
JP2008289970A (en) * 2007-05-23 2008-12-04 Sumitomo Metal Mining Co Ltd Hydrogen permeable membrane and its manufacturing method
WO2012063953A1 (en) * 2010-11-11 2012-05-18 東京エレクトロン株式会社 Method for producing filtration filter
JP2012101196A (en) * 2010-11-11 2012-05-31 Tokyo Electron Ltd Method for manufacturing filter for filtration
WO2013147540A1 (en) * 2012-03-30 2013-10-03 한국전기연구원 Composite separating film formed from metal supporting layer and metal oxide film, using concavo-convex patterned metal, and production method therefor
KR101379498B1 (en) * 2012-03-30 2014-04-01 한국전기연구원 composite membranes consisted of metallic supporter and metal oxide membrane using metals patterned as prominent planes and depressed planes and their fabrication method
WO2014098038A1 (en) * 2012-12-17 2014-06-26 日東電工株式会社 Hydrogen-releasing film
JPWO2014098038A1 (en) * 2012-12-17 2017-01-12 日東電工株式会社 Hydrogen discharge membrane

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