JP5642442B2 - Method for producing porous body and porous body produced by the method - Google Patents
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本発明は、基材上に金属粉末よりなる多孔質体を製造する方法及びその方法で製造した多孔質体に関する。The present invention relates to a method for producing a porous body made of a metal powder on a substrate and a porous body produced by the method.
金属粉末により形成された多孔質体の製造方法として、金属粉末とバインダーを混合したものをプレス成形する方法や射出成形する方法が知られている。
プレス成形法や射出成形法は、金属粉末を型にあてはめて成形するため複雑な形状をした多孔質体の製造に適しているが、金属等の基材上に多孔質体を製造したり面積が広くて薄い多孔質体を製造する方法としては適していない。As a method for producing a porous body formed of metal powder, a method of press molding or injection molding of a mixture of metal powder and a binder is known.
The press molding method and injection molding method are suitable for manufacturing a porous body having a complicated shape because metal powder is applied to a mold, but the porous body can be manufactured on a base material such as metal. However, it is not suitable as a method for producing a wide and thin porous body.
一方、基材上に多孔質体を製造する方法のひとつとしてスクリーン印刷法があげられる。
スクリーン印刷法は、金属粉末にバインダー樹脂と有機溶剤を加えてペーストを製造し、これをスクリーン印刷機により基材上に塗布した後、昇温して脱バインダー処理を行って基材上に金属粉末から成る多孔質体を製造する方法であり、面積が広くて薄い多孔質体を製造することも可能となる（特許文献１、２参照）。On the other hand, a screen printing method is one of the methods for producing a porous body on a substrate.
In the screen printing method, a binder resin and an organic solvent are added to a metal powder to produce a paste, which is coated on a substrate with a screen printer, and then heated to perform a binder removal treatment to form a metal on the substrate. This is a method for producing a porous body made of powder, and it is also possible to produce a thin porous body having a large area (see Patent Documents 1 and 2).
しかしながら、ペーストを用いてスクリーン印刷法によって多孔質体を製造する場合、粒径が１００μｍを超える金属粉末の場合にはバインダー樹脂と有機溶剤を加えて混練してもスクリーン印刷に必要なペーストの流動性を確保することができず、滑らかな印刷を行うことが困難となるため、一般に金属粉末は粒径が１００μｍ以下の粉末に制限され、１００μｍ以上の粒径を有する金属粉末の多孔質体をスクリーン印刷法で製造することは従来困難であった。However, when a porous body is produced by screen printing using a paste, in the case of a metal powder having a particle size of more than 100 μm, the paste flow necessary for screen printing can be added even if a binder resin and an organic solvent are added and kneaded. In general, the metal powder is limited to a powder having a particle size of 100 μm or less, and a porous body of the metal powder having a particle size of 100 μm or more is difficult. It has been difficult to manufacture by the screen printing method.
また、粒径が１００μｍを超えるような粗粒の金属粉末を混練したペーストは、ペーストに含まれる金属粉末の粒径より大きな開口部の版を使用しても目詰まりを起こしやすく、一般的に使用されるポリエステル等の繊維製の紗を使用した場合には、紗が切れて版を損傷するという問題があった。In addition, a paste obtained by kneading coarse metal powder having a particle size exceeding 100 μm is likely to be clogged even if a plate having an opening larger than the particle size of the metal powder contained in the paste is used. In the case of using a fiber cocoon such as polyester used, there was a problem that the cocoon broke and the plate was damaged.
さらに、従来よりスクリーン印刷法に使われるペーストには有機溶剤が広く用いられてきたが、有機溶剤の使用は人体の安全性や環境面に問題があった。Furthermore, organic solvents have been widely used in pastes used in screen printing methods, but the use of organic solvents has been problematic in terms of human safety and the environment.
このようにスクリーン印刷法を用いて粒径１００μｍ以上の金属粉末により形成された多孔質体を基材上に効率よく製造する方法は未だ確立されていない。As described above, a method for efficiently producing a porous body formed of a metal powder having a particle size of 100 μm or more on a substrate using a screen printing method has not yet been established.
本発明は、このような従来の多孔質体の製造方法の難点を解消するためになされたものであり、経済性や品質の安定性に優れ、環境負荷が少なく多量生産に適した金属粉末の多孔質体の製造方法を提供することと、このような方法を用いて製造した多孔質体を提供することを目的としている。The present invention has been made in order to eliminate the disadvantages of the conventional method for producing a porous body, and is a metal powder that is excellent in economic efficiency and quality stability, has a low environmental burden and is suitable for mass production. It aims at providing the manufacturing method of a porous body, and providing the porous body manufactured using such a method.
本発明に係る多孔質体の製造方法は、
基材上に金属粉末よりなる多孔質体を製造する方法であって、
水溶性のバインダー樹脂を水に溶かした水溶液（以下、水性バインダーと呼ぶ）を基材上にスクリーン印刷により塗布した後、該水性バインダー上に金属粉末を散布し、その後乾燥して散布した金属粉末からなる多孔質体を形成することを特徴としている。また、水性バインダーのスクリーン印刷工程及び金属粉末の散布工程を繰り返すことにより多層化することを特徴としている。また、得られた金属粉末の多孔質体を金属粉末の焼結可能な温度環境下で加熱処理し、金属粉末を焼結させることを特徴としている。
The method for producing a porous body according to the present invention includes:
A method for producing a porous body made of a metal powder on a substrate,
An aqueous solution in which a water-soluble binder resin is dissolved in water (hereinafter referred to as an aqueous binder) is applied on a substrate by screen printing, and then a metal powder is sprayed on the aqueous binder, and then dried and sprayed. It is characterized by forming a porous body made of In addition, it is characterized in that it is multilayered by repeating the screen printing process of the aqueous binder and the spraying process of the metal powder. In addition, the porous body of the obtained metal powder is heat-treated in a temperature environment where the metal powder can be sintered to sinter the metal powder.
本発明によれば、従来のように金属粉末とバインダー樹脂と有機溶剤を混練したペーストをスクリーン印刷工程で使わず、金属粉末を別の工程で扱うため、粒径１００μｍ以上の大きな金属粉末を使用することが出来る。本発明における金属粉末は、金属単体からなる純金属粉末でも、合金粉末でも、それらの混合粉末でも良い。According to the present invention, since a paste obtained by kneading a metal powder, a binder resin and an organic solvent is not used in the screen printing process as in the prior art, and the metal powder is handled in a separate process, a large metal powder having a particle size of 100 μm or more is used. I can do it. The metal powder in the present invention may be a pure metal powder made of a single metal, an alloy powder, or a mixed powder thereof.
本発明においては、予め金属粉末とバインダー樹脂と有機溶剤を混練してペーストを作成する必要がないため製造工程を簡略化することができる。In the present invention, it is not necessary to previously knead the metal powder, the binder resin, and the organic solvent to create a paste, so that the manufacturing process can be simplified.
また、金属粉末が含まれたペーストでは、乾燥したペーストの再利用が困難なためペーストを使用する場合には金属粉末の材料歩留まりを高くすることが困難であったが、本発明においては、水性バインダーの塗布後に別工程で金属粉末を散布させるため、金属粉末の回収や再利用も容易に行うことができ、高い材料歩留まりを達成することができる。In addition, in the paste containing the metal powder, it is difficult to recycle the dried paste, so it is difficult to increase the material yield of the metal powder when using the paste. Since the metal powder is sprayed in a separate process after the binder is applied, the metal powder can be easily recovered and reused, and a high material yield can be achieved.
また、本発明においてはスクリーン印刷工程において金属粉末を使用しないため、目詰まりが起こりにくくメンテナンスが容易となる。また、水性バインダーを使用するため、版の洗浄が容易となる。In the present invention, since metal powder is not used in the screen printing process, clogging hardly occurs and maintenance is easy. Further, since an aqueous binder is used, the plate can be easily cleaned.
本発明において使用する水性バインダーは、水を主成分とする溶媒と熱分解時に残渣が残りにくい水溶性のアクリル系樹脂あるいはセルロース系樹脂で構成されるものが望ましく、界面活性剤や防腐剤を添加しても良い。また、水性バインダーの粘度は、スクリーン印刷に適するように５０〜３００ｄＰａ・ｓが望ましい。
有機溶媒を含まない水性バインダーを使用することにより安全性に優れ環境負荷の少ない方法で多孔質体を製造することができる。The water-based binder used in the present invention is preferably composed of a water-based solvent and a water-soluble acrylic resin or cellulose resin that hardly retains residues during thermal decomposition, and a surfactant or preservative is added. You may do it. The viscosity of the aqueous binder is preferably 50 to 300 dPa · s so as to be suitable for screen printing.
By using an aqueous binder that does not contain an organic solvent, a porous body can be produced by a method that is excellent in safety and has a low environmental impact.
本発明において金属粉末を散布させる方法としては、吹き付ける方法や重力落下させる方法があげられる。これらの方法により、スクリーン印刷により塗布された水性バインダー上に、効率良く且つ確実に金属粉末を付着させることができる。また、散布時に基材に付着しなかった余分な粉末は回収し、再び散布させる工程に再利用することができる。In the present invention, the method of spraying the metal powder includes a spraying method and a gravity dropping method. By these methods, the metal powder can be efficiently and reliably attached onto the aqueous binder applied by screen printing. Moreover, the excess powder which did not adhere to the base material at the time of dispersion | distribution can be collect | recovered, and it can be reused for the process to disperse again.
本発明においては、スクリーン印刷による水性バインダーの塗布工程と水性バインダー上への金属粉末の散布工程の後、乾燥処理を行って水性バインダーを乾燥させて金属粉末を基材に固着させ、引き続いて基材に固着した金属粉末の上にスクリーン印刷による水性バインダーの塗布と水性バインダー上への金属粉末の散布を行って二層化した多孔質体を製造することが可能である。更に、水性バインダーの塗布工程と水性バインダー上への金属粉末の散布工程を繰り返すことによって多層化することも可能である。In the present invention, after the step of applying the aqueous binder by screen printing and the step of spraying the metal powder onto the aqueous binder, a drying treatment is performed to dry the aqueous binder to fix the metal powder to the substrate. It is possible to produce a two-layered porous body by applying an aqueous binder by screen printing onto a metal powder fixed to the material and spraying the metal powder onto the aqueous binder. Furthermore, it is also possible to make multilayer by repeating the application | coating process of an aqueous binder, and the dispersion | distribution process of the metal powder on an aqueous binder.
本発明において水性バインダーを乾燥させる方法としては、自然乾燥があげられる。また、温風を吹付けるなどして強制乾燥を行っても良い。In the present invention, the method for drying the aqueous binder includes natural drying. Further, forced drying may be performed by blowing warm air or the like.
本発明においては、スクリーン印刷による水性バインダーの塗布工程と水性バインダー上への金属粉末の散布工程によって得られた多孔質状の金属粉末を、焼結形成が可能な温度環境下で加熱することにより基材上に焼結された金属粉末多孔質体を製造することができる。この際、焼結工程の前に水性バインダーを構成するバインダー樹脂を分解させるために脱バインダー工程を行うのが望ましい。In the present invention, the porous metal powder obtained by the application process of the aqueous binder by screen printing and the dispersion process of the metal powder on the aqueous binder is heated in a temperature environment in which sintering can be formed. A metal powder porous body sintered on a substrate can be produced. At this time, it is desirable to perform a debinding step in order to decompose the binder resin constituting the aqueous binder before the sintering step.
本発明によれば、金属粉末とバインダーを混合したペーストを予め製造する必要がなく、また安定性に優れ、環境負荷が少なく多量生産に適した金属粉末の多孔質体を製造することができ、工業上非常に有益である。したがって、金属多孔質体の有するフィルタ機能や担持機能を利用し、排気ガス用や水処理用のフィルタ部材や、燃料電池等の各種部材を実用化する上で有用な技術となる。According to the present invention, it is not necessary to manufacture a paste in which a metal powder and a binder are mixed in advance, and it is possible to manufacture a porous body of metal powder that is excellent in stability and has a low environmental burden and is suitable for mass production. It is very useful industrially. Therefore, it becomes a useful technique for putting various members such as exhaust gas and water treatment filter members and fuel cells into practical use by utilizing the filter function and supporting function of the metal porous body.
以下、本発明を実施例により具体的に説明する。Hereinafter, the present invention will be specifically described by way of examples.
ＳＵＳ３０４製の板より作製した１００ｍｍ×２００ｍｍ×０．５ｍｍの基板、１００μｍ〜２００μｍの粒径を有する粉末を重量比で９３％含むＳＵＳ３０４粉末、及び水溶性のバインダー樹脂（セルロース系樹脂）を水に溶かした水性バインダーを用意した。また、ポリエステル製の紗（メッシュ数１００、線径５５μｍ、オープニング１９９μｍ）を使用し、５０ｍｍ×１００ｍｍのパターンが描かれたスクリーン印刷用の版を用意した。
まず基板上に、スクリーン印刷機を用いて水性バインダーをおよそ７０μｍの厚さ塗布した後、バインダーが乾燥する前にバインダー上に振動式フィーダー装置でＳＵＳ３０４粉末を散布した。次に、室温で１時間乾燥後、基板上のＳＵＳ３０４粉末の付着状況を観察した結果、粉末は基板上に均一に付着固定されていた。
引き続いて、粉末散布した基板を１２７３Ｋで１２００ｓｅｃ加熱し、ＳＵＳ３０４粉末の焼結処理を行った。焼結処理後のＳＵＳ３０４粉末を観察し、良好な多孔質体が基板上に形成されていることを確認した。次に、多孔質体の厚さを１０か所で測定した結果、平均厚さは３１８μｍであった。また、基板上に作製された多孔質体の質量を測定した結果、５．４ｇであった。A 100 mm × 200 mm × 0.5 mm substrate prepared from a SUS304 plate, SUS304 powder containing 93% by weight of a powder having a particle size of 100 μm to 200 μm, and a water-soluble binder resin (cellulosic resin) in water A dissolved aqueous binder was prepared. Further, a screen printing plate on which a pattern of 50 mm × 100 mm was drawn was prepared using a polyester basket (number of meshes 100, wire diameter 55 μm, opening 199 μm).
First, an aqueous binder was applied to a thickness of about 70 μm on a substrate using a screen printing machine, and then SUS304 powder was spread on the binder with a vibratory feeder device before the binder was dried. Next, after drying at room temperature for 1 hour, the state of adhesion of the SUS304 powder on the substrate was observed, and as a result, the powder was uniformly adhered and fixed on the substrate.
Subsequently, the powder-spreaded substrate was heated at 1273K for 1200 seconds to perform a SUS304 powder sintering process. The sintered SUS304 powder was observed, and it was confirmed that a good porous body was formed on the substrate. Next, as a result of measuring the thickness of the porous body at 10 locations, the average thickness was 318 μm. Moreover, it was 5.4 g as a result of measuring the mass of the porous body produced on the board | substrate.
実施例１と同じＳＵＳ３０４基板、水性バインダー及びスクリーン印刷用の版を用意した。また、３００μｍ〜５００μｍの粒径を有する粉末を重量比で８８％含むＳＵＳ３１６粉末を用意した。
実施例１と同様に基板上に水性バインダーを塗布した後、ＳＵＳ３１６粉末を散布し、乾燥後基板上のＳＵＳ３１６粉末の付着状況を観察した結果、粉末は基板上に均一に付着固定されていた。
引き続いて、粉末散布した基板を１２７３Ｋで１２００ｓｅｃ加熱し、ＳＵＳ３１６粉末の焼結処理を行った。焼結処理後のＳＵＳ３１６粉末を観察し、良好な多孔質体が基板上に形成されていることを確認した。次に、多孔質体の厚さを１０か所で測定した結果、平均厚さは５１０μｍであった。また、基板上に作製された多孔質体の質量を測定した結果、７．２ｇであった。The same SUS304 substrate, aqueous binder, and screen printing plate as in Example 1 were prepared. In addition, SUS316 powder containing 88% by weight of powder having a particle size of 300 μm to 500 μm was prepared.
In the same manner as in Example 1, after applying an aqueous binder on the substrate, SUS316 powder was dispersed, and after drying, the state of adhesion of the SUS316 powder on the substrate was observed. As a result, the powder was uniformly adhered and fixed on the substrate.
Subsequently, the powder-spreaded substrate was heated at 1273 K for 1200 seconds to perform a SUS316 powder sintering process. The sintered SUS316 powder was observed and it was confirmed that a good porous body was formed on the substrate. Next, as a result of measuring the thickness of the porous body at 10 locations, the average thickness was 510 μm. Moreover, it was 7.2g as a result of measuring the mass of the porous body produced on the board | substrate.
実施例１と同じＳＵＳ３０４基板、ＳＵＳ３０４粉末、水性バインダー及びスクリーン印刷用の版を用意した。
実施例１と同様に基板上に水性バインダーを塗布した後、ＳＵＳ３０４粉末を散布し、室温で乾燥させた。次に、基板上に形成されたＳＵＳ３０４粉末層の上にスクリーン印刷機を用いて水性バインダーを塗布し、その後バインダーが乾燥する前にバインダー上に振動式フィーダー装置でＳＵＳ３０４粉末を散布した後、乾燥させた。引き続いて、同様に基板上に形成されたＳＵＳ３０４粉末層の上に水性バインダーを塗布した後、ＳＵＳ３０４粉末を散布した。
基板上のＳＵＳ３０４粉末の付着状況を観察した結果、粉末は基板上に均一に付着固定されていた。図１は、その時の外観状況を２００倍率の顕微鏡により観察したものである。
引き続いて、粉末散布した基板を１２７３Ｋで１２００ｓｅｃ加熱し、ＳＵＳ３０４粉末の焼結処理を行った。焼結処理後のＳＵＳ３０４粉末を観察し、良好な多孔質体が基板上に形成されていることを確認した。次に、多孔質体の厚さを１０か所で測定した結果、平均厚さは６７２μｍであった。また、基板上に作製された多孔質体の質量を測定した結果、１５．６ｇであった。The same SUS304 substrate, SUS304 powder, aqueous binder and screen printing plate as in Example 1 were prepared.
After applying an aqueous binder on the substrate in the same manner as in Example 1, SUS304 powder was dispersed and dried at room temperature. Next, an aqueous binder is applied on the SUS304 powder layer formed on the substrate using a screen printer, and then the SUS304 powder is sprayed on the binder with a vibratory feeder device before the binder is dried, and then dried. I let you. Subsequently, an aqueous binder was applied on the SUS304 powder layer similarly formed on the substrate, and then SUS304 powder was dispersed.
As a result of observing the adhesion state of the SUS304 powder on the substrate, the powder was uniformly adhered and fixed on the substrate. FIG. 1 is an observation of the appearance at that time with a microscope at 200 magnifications.
Subsequently, the powder-spreaded substrate was heated at 1273K for 1200 seconds to perform a SUS304 powder sintering process. The sintered SUS304 powder was observed, and it was confirmed that a good porous body was formed on the substrate. Next, as a result of measuring the thickness of the porous body at 10 locations, the average thickness was 672 μm. Moreover, as a result of measuring the mass of the porous body produced on the board | substrate, it was 15.6g.
実施例１と同じＳＵＳ３０４基板及びＳＵＳ３０４粉末を用意した。また、スクリーン印刷用の版として、ポリエステル製の紗（メッシュ数６０、線径７０μｍ、オープニング３５３μｍ）を使用し、５０ｍｍ×１００ｍｍのパターンが描かれた版を用意した。
次にバインダー樹脂（エチルセルロース）をテルピネオールに溶かし、ＳＵＳ３０４粉末と混練して粘度３１０ｄＰａ・ｓのペーストを作製した。
基板上に、スクリーン印刷機を用いてペーストの塗布を行ったが、スクリーンのメッシュが目詰まりを起こした。また、メッシュが損傷して基板上に良好なペーストの塗布をすることができなかった。The same SUS304 substrate and SUS304 powder as in Example 1 were prepared. Further, as a plate for screen printing, a plate with a 50 mm × 100 mm pattern was prepared using a polyester basket (mesh number 60, wire diameter 70 μm, opening 353 μm).
Next, binder resin (ethyl cellulose) was dissolved in terpineol and kneaded with SUS304 powder to prepare a paste having a viscosity of 310 dPa · s.
The paste was applied onto the substrate using a screen printer, but the screen mesh was clogged. In addition, the mesh was damaged and it was not possible to apply a good paste on the substrate.
Claims (4)
水溶性のバインダー樹脂を水に溶かした水溶液を基材上にスクリーン印刷により塗布した後、該水溶液上に金属粉末を散布し、その後乾燥して散布した金属粉末からなる多孔質体を形成することを特徴とする多孔質体の製造方法。 A method for producing a porous body made of a metal powder on a substrate,
An aqueous solution in which a water-soluble binder resin is dissolved in water is applied on a substrate by screen printing, then a metal powder is sprayed on the aqueous solution, and then dried to form a porous body made of the dispersed metal powder. A method for producing a porous body characterized by the above.
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| CN110831714B (en) * | 2017-07-06 | 2022-11-18 | 株式会社Lg化学 | Method for producing metal foam |
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