JP2007012292A - Graphite particle molding and its manufacturing method - Google Patents
Graphite particle molding and its manufacturing method Download PDFInfo
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- JP2007012292A JP2007012292A JP2005187840A JP2005187840A JP2007012292A JP 2007012292 A JP2007012292 A JP 2007012292A JP 2005187840 A JP2005187840 A JP 2005187840A JP 2005187840 A JP2005187840 A JP 2005187840A JP 2007012292 A JP2007012292 A JP 2007012292A
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- 239000002245 particle Substances 0.000 title claims abstract description 120
- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical compound [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 title claims abstract description 115
- 239000010439 graphite Substances 0.000 title claims abstract description 112
- 229910002804 graphite Inorganic materials 0.000 title claims abstract description 112
- 238000000465 moulding Methods 0.000 title claims abstract description 37
- 238000004519 manufacturing process Methods 0.000 title claims description 12
- 229920001187 thermosetting polymer Polymers 0.000 claims abstract description 46
- 239000011342 resin composition Substances 0.000 claims abstract description 32
- 239000011347 resin Substances 0.000 claims description 24
- 229920005989 resin Polymers 0.000 claims description 24
- RYGMFSIKBFXOCR-UHFFFAOYSA-N Copper Chemical compound [Cu] RYGMFSIKBFXOCR-UHFFFAOYSA-N 0.000 claims description 19
- 229910052802 copper Inorganic materials 0.000 claims description 19
- 239000010949 copper Substances 0.000 claims description 19
- 239000000446 fuel Substances 0.000 claims description 9
- 239000007772 electrode material Substances 0.000 claims description 5
- 238000003825 pressing Methods 0.000 abstract description 7
- 239000012778 molding material Substances 0.000 description 10
- 238000005260 corrosion Methods 0.000 description 9
- 230000007797 corrosion Effects 0.000 description 9
- 239000000463 material Substances 0.000 description 7
- 238000002844 melting Methods 0.000 description 5
- 230000008018 melting Effects 0.000 description 5
- 239000005011 phenolic resin Substances 0.000 description 5
- 230000000052 comparative effect Effects 0.000 description 4
- 230000014759 maintenance of location Effects 0.000 description 4
- 238000000034 method Methods 0.000 description 4
- XEEYBQQBJWHFJM-UHFFFAOYSA-N Iron Chemical compound [Fe] XEEYBQQBJWHFJM-UHFFFAOYSA-N 0.000 description 2
- PXHVJJICTQNCMI-UHFFFAOYSA-N Nickel Chemical compound [Ni] PXHVJJICTQNCMI-UHFFFAOYSA-N 0.000 description 2
- 206010040844 Skin exfoliation Diseases 0.000 description 2
- 229910052782 aluminium Inorganic materials 0.000 description 2
- XAGFODPZIPBFFR-UHFFFAOYSA-N aluminium Chemical compound [Al] XAGFODPZIPBFFR-UHFFFAOYSA-N 0.000 description 2
- 239000011230 binding agent Substances 0.000 description 2
- 230000000694 effects Effects 0.000 description 2
- 238000010438 heat treatment Methods 0.000 description 2
- 239000010410 layer Substances 0.000 description 2
- 229910052751 metal Inorganic materials 0.000 description 2
- 239000002184 metal Substances 0.000 description 2
- 239000007769 metal material Substances 0.000 description 2
- 239000004033 plastic Substances 0.000 description 2
- 230000003014 reinforcing effect Effects 0.000 description 2
- 239000000523 sample Substances 0.000 description 2
- 239000010935 stainless steel Substances 0.000 description 2
- 229910001220 stainless steel Inorganic materials 0.000 description 2
- 238000010998 test method Methods 0.000 description 2
- 229920000178 Acrylic resin Polymers 0.000 description 1
- 239000004925 Acrylic resin Substances 0.000 description 1
- 229920000049 Carbon (fiber) Polymers 0.000 description 1
- 229920000877 Melamine resin Polymers 0.000 description 1
- RTAQQCXQSZGOHL-UHFFFAOYSA-N Titanium Chemical compound [Ti] RTAQQCXQSZGOHL-UHFFFAOYSA-N 0.000 description 1
- 239000000956 alloy Substances 0.000 description 1
- 229910045601 alloy Inorganic materials 0.000 description 1
- QHIWVLPBUQWDMQ-UHFFFAOYSA-N butyl prop-2-enoate;methyl 2-methylprop-2-enoate;prop-2-enoic acid Chemical compound OC(=O)C=C.COC(=O)C(C)=C.CCCCOC(=O)C=C QHIWVLPBUQWDMQ-UHFFFAOYSA-N 0.000 description 1
- 239000004917 carbon fiber Substances 0.000 description 1
- 229910021393 carbon nanotube Inorganic materials 0.000 description 1
- 239000002041 carbon nanotube Substances 0.000 description 1
- 239000003822 epoxy resin Substances 0.000 description 1
- 239000012530 fluid Substances 0.000 description 1
- 239000007849 furan resin Substances 0.000 description 1
- PCHJSUWPFVWCPO-UHFFFAOYSA-N gold Chemical compound [Au] PCHJSUWPFVWCPO-UHFFFAOYSA-N 0.000 description 1
- 229910052737 gold Inorganic materials 0.000 description 1
- 239000010931 gold Substances 0.000 description 1
- LNEPOXFFQSENCJ-UHFFFAOYSA-N haloperidol Chemical compound C1CC(O)(C=2C=CC(Cl)=CC=2)CCN1CCCC(=O)C1=CC=C(F)C=C1 LNEPOXFFQSENCJ-UHFFFAOYSA-N 0.000 description 1
- 230000001771 impaired effect Effects 0.000 description 1
- 229910052742 iron Inorganic materials 0.000 description 1
- 239000000203 mixture Substances 0.000 description 1
- 229910052759 nickel Inorganic materials 0.000 description 1
- 230000001590 oxidative effect Effects 0.000 description 1
- 229920001568 phenolic resin Polymers 0.000 description 1
- 230000000704 physical effect Effects 0.000 description 1
- 229920000647 polyepoxide Polymers 0.000 description 1
- 239000000843 powder Substances 0.000 description 1
- 230000002787 reinforcement Effects 0.000 description 1
- 230000000717 retained effect Effects 0.000 description 1
- 239000002344 surface layer Substances 0.000 description 1
- 239000010936 titanium Substances 0.000 description 1
- 229910052719 titanium Inorganic materials 0.000 description 1
- 229920006337 unsaturated polyester resin Polymers 0.000 description 1
Classifications
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- Y—GENERAL TAGGING OF NEW TECHNOLOGICAL DEVELOPMENTS; GENERAL TAGGING OF CROSS-SECTIONAL TECHNOLOGIES SPANNING OVER SEVERAL SECTIONS OF THE IPC; TECHNICAL SUBJECTS COVERED BY FORMER USPC CROSS-REFERENCE ART COLLECTIONS [XRACs] AND DIGESTS
- Y02—TECHNOLOGIES OR APPLICATIONS FOR MITIGATION OR ADAPTATION AGAINST CLIMATE CHANGE
- Y02E—REDUCTION OF GREENHOUSE GAS [GHG] EMISSIONS, RELATED TO ENERGY GENERATION, TRANSMISSION OR DISTRIBUTION
- Y02E60/00—Enabling technologies; Technologies with a potential or indirect contribution to GHG emissions mitigation
- Y02E60/10—Energy storage using batteries
-
- Y—GENERAL TAGGING OF NEW TECHNOLOGICAL DEVELOPMENTS; GENERAL TAGGING OF CROSS-SECTIONAL TECHNOLOGIES SPANNING OVER SEVERAL SECTIONS OF THE IPC; TECHNICAL SUBJECTS COVERED BY FORMER USPC CROSS-REFERENCE ART COLLECTIONS [XRACs] AND DIGESTS
- Y02—TECHNOLOGIES OR APPLICATIONS FOR MITIGATION OR ADAPTATION AGAINST CLIMATE CHANGE
- Y02E—REDUCTION OF GREENHOUSE GAS [GHG] EMISSIONS, RELATED TO ENERGY GENERATION, TRANSMISSION OR DISTRIBUTION
- Y02E60/00—Enabling technologies; Technologies with a potential or indirect contribution to GHG emissions mitigation
- Y02E60/30—Hydrogen technology
- Y02E60/50—Fuel cells
-
- Y—GENERAL TAGGING OF NEW TECHNOLOGICAL DEVELOPMENTS; GENERAL TAGGING OF CROSS-SECTIONAL TECHNOLOGIES SPANNING OVER SEVERAL SECTIONS OF THE IPC; TECHNICAL SUBJECTS COVERED BY FORMER USPC CROSS-REFERENCE ART COLLECTIONS [XRACs] AND DIGESTS
- Y02—TECHNOLOGIES OR APPLICATIONS FOR MITIGATION OR ADAPTATION AGAINST CLIMATE CHANGE
- Y02P—CLIMATE CHANGE MITIGATION TECHNOLOGIES IN THE PRODUCTION OR PROCESSING OF GOODS
- Y02P70/00—Climate change mitigation technologies in the production process for final industrial or consumer products
- Y02P70/50—Manufacturing or production processes characterised by the final manufactured product
Abstract
Description
本発明は、導電性の極めて良好な黒鉛粒子成形体及びその製造方法に関し、更に詳しくは、燃料電池用のセパレータなどに好適に用いることのできる黒鉛粒子成形体及びその製造方法に関する。 The present invention relates to a graphite particle molded body having extremely good electrical conductivity and a method for producing the same, and more particularly to a graphite particle molded body that can be suitably used for a separator for a fuel cell and the like and a method for producing the same.
黒鉛は、材質劣化が生じにくく、耐食性に優れた材料であり、また、電気抵抗が低く、良好な導電性を有する材料であることから、黒鉛粒子を熱硬化性樹脂等のバインダーで硬化成形した黒鉛粒子成形体は、例えば、燃料電池のセパレータなど、耐食性と導電性の要求される部位に利用されている。 Graphite is a material that is not easily deteriorated in material, has excellent corrosion resistance, and has low electrical resistance and good conductivity. Therefore, graphite particles are cured and molded with a binder such as a thermosetting resin. Graphite particle compacts are used, for example, in parts that require corrosion resistance and conductivity, such as fuel cell separators.
一方、銅、金、アルミニウム、ステンレスなどの金属材料は黒鉛に比べて導電性に優れた材料ではあるが、還元雰囲気化や酸化雰囲気化に曝されることで材質劣化が生じやすく、耐食性の劣る材料である。 On the other hand, metal materials such as copper, gold, aluminum, and stainless steel are excellent in conductivity as compared with graphite, but they are easily deteriorated by exposure to a reducing atmosphere or oxidizing atmosphere, resulting in poor corrosion resistance. Material.
そこで、黒鉛粒子成形体に、これら金属材料を埋設させて導電性を向上させるような試みがなされており、例えば、下記特許文献１には、複数の貫通穴を有した金属板を黒鉛粒子成形体に埋設させた燃料電池用セパレータについて開示されている。
黒鉛粒子成形体の導電性は、黒鉛粒子の密度が、緻密かつ均一であるほどより良好であるが、上記特許文献１の黒鉛粒子成形体では、金属板の表面はプレスされるが、金属板の貫通穴の内部はほとんどプレスされず、均一な密度にならないという問題点があった。そのため、成形材料を一旦バインダー（樹脂）の融点以上まで加熱し、成形材料に流動性を持たせてプレス成形をしていた。 The conductivity of the graphite particle compact is better as the density of the graphite particles is denser and uniform. In the graphite particle compact of Patent Document 1, the surface of the metal plate is pressed. The inside of the through hole was hardly pressed, and there was a problem that a uniform density was not achieved. For this reason, the molding material is once heated to the melting point of the binder (resin) or more, and the molding material is fluidized to perform press molding.
しかしながら、流動性を有する成形材料をプレス成形する際、加圧力を大きくすると、樹脂が浮き上がってしまい表層に樹脂層が形成され、導電性が損なわれやすいという問題点があることから、プレス成形時の加圧力は低く抑える必要があった。そのため、上記特許文献１では、成形材料を充分圧粉させることができず、得られる未硬化処理のプレス成形体は、強度、保形性共に劣るものとなりがちであったので、プレス成形体の硬化処理は、金型内で、プレスしながら行う必要があり、生産性が悪く、また、導電性の高い黒鉛粒子成形体が得られにくかった。 However, when press molding a fluid molding material, if the applied pressure is increased, the resin floats up and a resin layer is formed on the surface layer. It was necessary to keep the applied pressure low. Therefore, in Patent Document 1, the molding material cannot be sufficiently compacted, and the obtained uncured press-molded body tends to be inferior in strength and shape retention. The curing process needs to be performed while pressing in the mold, so that the productivity is poor and it is difficult to obtain a highly conductive graphite particle compact.
したがって本発明の目的は、導電性に優れ、かつ、生産性の高い黒鉛粒子成形体及びその製造方法を提供することである。 Accordingly, an object of the present invention is to provide a graphite particle molded body having excellent conductivity and high productivity, and a method for producing the same.
上記目的を達成するため、本発明の第１は、導電性を有するメッシュを、黒鉛含有率６０〜９０質量％の熱硬化性樹脂組成物中に埋没するようにプレス成形し、硬化させて得られた成形体であることを特徴とする黒鉛粒子成形体を提供するものである。 In order to achieve the above object, the first of the present invention is obtained by press-molding and curing a conductive mesh so as to be embedded in a thermosetting resin composition having a graphite content of 60 to 90% by mass. It is an object of the present invention to provide a graphite particle molded body characterized by being a molded body.
上記第１の発明によれば、黒鉛粒子成形体に導電性を有するメッシュが埋設されているので、成形体の電気抵抗が低く、導電性が良好である。 According to the first aspect of the present invention, since the conductive mesh is embedded in the graphite particle molded body, the electrical resistance of the molded body is low and the electrical conductivity is good.
また、黒鉛含有率の下限を６０質量％としたことで、導電性を良好に保ち、また上限を９０質量％としたことで、強度を確保することができる。 In addition, when the lower limit of the graphite content is 60% by mass, the electrical conductivity is kept good, and when the upper limit is 90% by mass, the strength can be ensured.
また、この黒鉛粒子成形体は、成形材料をプレス成形し、このプレス成形体を硬化処理することで得られるが、プレス成形の際、特に上記熱硬化性樹脂組成物を融点以上まで加熱して流動性を持たせなくとも、比較的低温度であっても、プレスするだけで、メッシュの網目に黒鉛粒子がスムーズに充填され、緻密かつ均一な粒子密度を有するプレス成形体を得ることができる。 The graphite particle molded body is obtained by press-molding a molding material and curing the press-molded body. During the press molding, particularly, the thermosetting resin composition is heated to a melting point or higher. Even if it does not have fluidity, even at a relatively low temperature, a press-molded body having a dense and uniform particle density can be obtained by simply filling the mesh with a graphite particle simply by pressing. .
更に、プレス成形時の加圧力を増加させても、メッシュの網目に樹脂が回り込んで流動するため、樹脂が表面に浮き上がりにくくなり、導電性を損なうことなく、黒鉛粒子を充填して保形性の高いプレス成形体を得ることができる。このため、プレス成形体を金型から取り出してから硬化処理を行うこともでき、生産性に優れている。 Furthermore, even if the pressing force during press molding is increased, the resin flows around the mesh mesh and flows, so the resin is less likely to float on the surface, and the graphite particles are filled and retained without impairing conductivity. A highly press-formed body can be obtained. For this reason, after the press-molded body is taken out from the mold, the curing treatment can be performed, and the productivity is excellent.
本発明の第２は、前記第１の発明において、前記導電性を有するメッシュの厚さが、前記黒鉛粒子成形体の厚さの５〜３０％であることを特徴とする。 According to a second aspect of the present invention, in the first aspect, the thickness of the conductive mesh is 5 to 30% of the thickness of the graphite particle compact.
上記第２の発明によれば、導電性を有するメッシュが露出するのを防止して黒鉛粒子成形体の耐食性を損なうことなく導電性を向上させることができ、また、該メッシュと該熱硬化性樹脂組成物とを強固に密着させることができるので、導電性が極めて高い。 According to the second aspect of the invention, it is possible to improve the conductivity without impairing the corrosion resistance of the graphite particle compact by preventing the conductive mesh from being exposed, and the mesh and the thermosetting property. Since the resin composition can be firmly adhered, the conductivity is extremely high.
本発明の第３は、前記第１又は第２の発明において、前記導電性を有するメッシュが、前記熱硬化性樹脂組成物を構成する黒鉛粒子の平均粒径よりも大きい目開き寸法を有することを特徴とする。 According to a third aspect of the present invention, in the first or second aspect, the conductive mesh has an opening size larger than an average particle size of graphite particles constituting the thermosetting resin composition. It is characterized by.
上記第３の発明によれば、成形材料をプレスした時、メッシュの網目に黒鉛粒子がスムーズに流動して充填されるので、メッシュと黒鉛粒子とが良好に接触し、両者の境界面に生じる接触抵抗が少ないので、導電性を向上させることができる。 According to the third aspect of the invention, when the molding material is pressed, the graphite particles smoothly flow and fill the mesh mesh, so that the mesh and the graphite particles are in good contact with each other and are generated at the interface between them. Since there is little contact resistance, electroconductivity can be improved.
本発明の第４は、前記第１〜３のいずれか一つの発明において、前記導電性を有するメッシュが、銅で構成されていることを特徴とする。 According to a fourth aspect of the present invention, in any one of the first to third aspects, the conductive mesh is made of copper.
上記第４の発明によれば、銅はコスト、導電性の観点から、極めて良好な材料であることから、コストパフォーマンスに優れている。 According to the fourth aspect of the present invention, copper is an excellent material from the viewpoints of cost and conductivity, and therefore has excellent cost performance.
本発明の第５は、前記第１〜４のいずれか一つの発明において、燃料電池用セパレータ、電極端子、電池電極材から選ばれた一種として用いることを特徴とする。 A fifth aspect of the present invention is characterized in that, in any one of the first to fourth aspects, the invention is used as a kind selected from a separator for a fuel cell, an electrode terminal, and a battery electrode material.
上記第５の発明によれば、上記１〜４の発明の黒鉛粒子成形体は、従来の黒鉛粒子成形体よりも導電性に優れた黒鉛粒子成形体であることから、導電性と耐食性の要求される部材である燃料電池用セパレータ、電極端子、電池電極材として特に好適に用いることができる。 According to the fifth aspect, since the graphite particle compacts of the first to fourth aspects of the invention are graphite particle compacts that are more conductive than conventional graphite particle compacts, there is a need for conductivity and corrosion resistance. It can be particularly suitably used as a separator for fuel cells, electrode terminals, and battery electrode materials which are members to be used.
本発明の第６は、導電性を有するメッシュを、熱硬化性樹脂と黒鉛粒子とを含有する熱硬化性樹脂組成物中に埋没させ、６０〜１００℃、５００〜２０００ｋｇｆ／ｃｍ２の条件でプレス成形し、その後、該プレス成形体を熱硬化処理することを特徴とする黒鉛粒子成形体の製造方法を提供するものである。 6th of this invention embeds the mesh which has electroconductivity in the thermosetting resin composition containing a thermosetting resin and graphite particle | grains, and the conditions of 60-100 degreeC and 500-2000 kgf / cm < 2 >. The present invention provides a method for producing a graphite particle molded body, which is subjected to press molding, and then subjected to thermosetting treatment.
上記第６の発明によれば、プレス成形時において、導電性を有するメッシュと、熱硬化性樹脂と黒鉛粒子とを含有する熱硬化性樹脂組成物とを、例えば、熱硬化性樹脂の融点以上まで加熱して流動性を持たせなくとも、プレスによりメッシュの線材の間隙に黒鉛粒子がスムーズに入り込み、均一で緻密な粒子密度を有する黒鉛粒子成形体を得ることができ、成形を熱硬化性樹脂の融点以下の６０〜１００℃で行うことができる。また、熱硬化性樹脂の粘度が高い状態でプレス成形できるので、成形圧力を５００〜２０００ｋｇｆ／ｃｍ２としても、プレス成形体の表面に樹脂が浮き上がるといった虞れがなく、得られる黒鉛粒子成形体は、極めて高い導電性を有する。 According to the sixth invention, at the time of press molding, the conductive mesh and the thermosetting resin composition containing the thermosetting resin and the graphite particles are, for example, not less than the melting point of the thermosetting resin. Even if it is not heated to give fluidity, the graphite particles smoothly enter into the gaps between the mesh wires by pressing, and a graphite particle compact with a uniform and dense particle density can be obtained. It can carry out at 60-100 degreeC below melting | fusing point of resin. In addition, since the thermosetting resin can be press-molded with a high viscosity, there is no fear that the resin will float on the surface of the press-molded body even when the molding pressure is 500 to 2000 kgf / cm 2 , and the resulting graphite particle molded body is obtained. Has very high electrical conductivity.
そして、導電性を有するメッシュと、熱硬化性樹脂と黒鉛粒子とを含有する熱硬化性樹脂組成物とを、６０〜１００℃、５００〜２０００ｋｇｆ／ｃｍ２の成形条件でプレス成形して得られるプレス成形体は、緻密でかつ均一な粒子密度を有し、また、未硬化の状態であっても保形性の高いものであるため、プレス成形体の硬化処理を金型から取り出して行うことができ、生産性も優れている。 And it is obtained by press-molding a conductive mesh and a thermosetting resin composition containing a thermosetting resin and graphite particles under molding conditions of 60 to 100 ° C. and 500 to 2000 kgf / cm 2. The press-molded body has a dense and uniform particle density, and has high shape retention even in an uncured state. Therefore, the press-molded body should be taken out of the mold. And productivity is excellent.
本発明の第７は、前記第６の発明において、前記熱硬化性樹脂組成物をシート状成形体とし、該シート状成形体で、前記導電性を有するメッシュを挟み込んでプレス成形することを特徴とする。 According to a seventh aspect of the present invention, in the sixth aspect, the thermosetting resin composition is formed into a sheet-like molded body, and the sheet-shaped molded body is press-molded with the mesh having the conductivity interposed therebetween. And
上記第７の発明によれば、得られる黒鉛粒子成形体における導電性を有するメッシュを埋設させる位置を特定でき、例えば、黒鉛成形体を所望の形状に加工したり、貫通穴などを設ける場合において、導電性を有するメッシュが露出するといったことを防止できる。 According to the seventh invention, the position where the conductive mesh in the obtained graphite particle molded body is embedded can be specified. For example, when processing the graphite molded body into a desired shape or providing a through hole or the like, It is possible to prevent the conductive mesh from being exposed.
本発明の第８は、前記第６又は７の発明において、前記導電性を有するメッシュとして、前記黒鉛粒子成形体の厚さの５〜３０％となるものを用いることを特徴とする。 An eighth aspect of the present invention is characterized in that, in the sixth or seventh aspect of the invention, the conductive mesh is 5-30% of the thickness of the graphite particle compact.
上記第８の発明によれば、導電性を有するメッシュが露出するのを防止して黒鉛粒子成形体の耐食性を損なうことなく導電性を向上でき、また、該メッシュと該熱硬化性樹脂組成物とを強固に接着させることができるので導電性の高い黒鉛粒子成形体を製造することができる。 According to the eighth aspect of the present invention, the conductive mesh can be prevented from being exposed and the conductivity can be improved without impairing the corrosion resistance of the graphite particle molded body, and the mesh and the thermosetting resin composition can be improved. Can be firmly bonded to each other, so that a highly conductive graphite particle molded body can be produced.
本発明の第９は、前記第６〜８のいずれか一つの発明において、前記導電性を有するメッシュとして、前記熱硬化性樹脂組成物に含まれる黒鉛粒子の粒径よりも大きい目開き寸法を有するものを用いることを特徴とする。 In a ninth aspect of the present invention, according to any one of the sixth to eighth aspects, an opening size larger than the particle size of the graphite particles contained in the thermosetting resin composition is used as the conductive mesh. It is characterized by using what has.
上記第９の発明によれば、メッシュの網目を介して黒鉛粒子粉を接触させることができるので、異質な材料が接触する境界面に生じる接触抵抗を低減でき、より導電性の高い黒鉛粒子成形体を製造することができる。 According to the ninth aspect of the invention, since the graphite particle powder can be contacted through the mesh network, it is possible to reduce the contact resistance generated at the interface where the foreign material contacts, and to form graphite particles with higher conductivity. The body can be manufactured.
本発明の第１０は、前記第６〜９のいずれか一つの発明において、前記導電性を有するメッシュとして、銅で構成されたものを用いることを特徴とする。 A tenth aspect of the present invention is characterized in that, in any one of the sixth to ninth aspects, a mesh made of copper is used as the conductive mesh.
上記第１０の発明によれば、コスト、導電性の観点から銅は優れた材料であり、また、熱硬化性樹脂組成物との接着性が良好であることから、導電性の高い黒鉛粒子成形体を低コストで製造することができる。 According to the tenth aspect of the present invention, copper is an excellent material from the viewpoint of cost and conductivity, and has good adhesion to the thermosetting resin composition. The body can be manufactured at low cost.
本発明の黒鉛粒子成形体は、導電性が極めて良好であり、また、強度も高く、耐食性・導電性を要求する部材に特に好適に利用できる。 The graphite particle molded body of the present invention has extremely good conductivity, high strength, and can be particularly suitably used for a member that requires corrosion resistance and conductivity.
また、この黒鉛粒子成形体を製造するにあたって、成形材料をプレスして黒鉛粒子の圧粉されたプレス成形体とするが、その際、成形材料に均一に圧力がかかりやすく、メッシュの線材の外周に沿って黒鉛粒子が入り込むので、特に成形材料を樹脂の融点以上まで加熱して流動性を持たせなくとも、均一かつ緻密な粒子密度を有するプレス成形体を得ることができる。そのため、プレス成形時の加圧力を大きくすることができ、また、これにより、黒鉛粒子が充分圧粉され、保形性の高いプレス成形体を得ることができるので、硬化処理をプレス成形した金型などから取り出して行うことができ、生産性にも優れている。 Further, in producing this graphite particle molded body, the molding material is pressed into a pressed molded body in which graphite particles are compacted. At this time, the molding material is easily subjected to uniform pressure, and the outer periphery of the mesh wire rod Since the graphite particles enter along, the press-molded body having a uniform and dense particle density can be obtained even without heating the molding material to the melting point of the resin or more to impart fluidity. Therefore, it is possible to increase the pressurizing force at the time of press molding, and this makes it possible to obtain a press-molded body with sufficiently compacted graphite particles and high shape retention. It can be taken out from the mold and is excellent in productivity.
本発明の黒鉛粉成形体は、導電性を有するメッシュと、それを包含する黒鉛含有率６０〜９０質量％の熱硬化性樹脂組成物とで構成されている。 The graphite powder molded body of the present invention is composed of a conductive mesh and a thermosetting resin composition including the graphite content rate of 60 to 90% by mass.
導電性を有するメッシュとしては、固有抵抗率が黒鉛よりも低く、５ｍΩ・ｃｍ以下である材料で構成されているものであれば特に限定はなく、例えば、銅、ステンレス、アルミニウム、鉄、チタン、ニッケル又はそれらの合金などが挙げられ、なかでも、コストと導電性のバランスの観点から銅であることが好ましい。 The conductive mesh is not particularly limited as long as it is made of a material having a specific resistivity lower than that of graphite and 5 mΩ · cm or less. For example, copper, stainless steel, aluminum, iron, titanium, Nickel or an alloy thereof may be used, and among these, copper is preferable from the viewpoint of balance between cost and conductivity.
メッシュの構造としては、平織り状、綾織り、平畳織り、綾畳織りなどが挙げられる。 Examples of the mesh structure include plain weave, twill, flat tatami and twill.
また、メッシュを構成する線材の平均線径（直径）としては、０．０２５〜２．０ｍｍであるものが好ましく、より好ましくは０．１〜０．２ｍｍである。線径が０．０２５ｍｍ未満であると、単位面積当りの質量を同じにしようとすると、目開きが小さくなり、プレス時にメッシュの網目に黒鉛粒子がスムーズに充填されず、メッシュと黒鉛粒子とが良好に接触できないことがあり、それにより両者の境界面に生じる接触抵抗が大きくなり、導電性が損なわれる虞れがある。また、２．０ｍｍより大きいと、単位面積当りの質量を同じにしようとすると、目開きが大きくなりすぎて、黒鉛粒子同士の接触が多くなり、導電性の著しい向上が認められないことがある。 Moreover, as an average wire diameter (diameter) of the wire which comprises a mesh, what is 0.025-2.0 mm is preferable, More preferably, it is 0.1-0.2 mm. If the wire diameter is less than 0.025 mm, when trying to make the mass per unit area the same, the mesh opening becomes small, and the mesh particles are not filled smoothly into the mesh mesh during pressing. There may be cases where the contact cannot be made satisfactorily, thereby increasing the contact resistance generated at the boundary surface between the two, which may impair the conductivity. On the other hand, if it is larger than 2.0 mm, when trying to make the mass per unit area the same, the opening becomes too large, the contact between graphite particles increases, and the conductivity may not be significantly improved. .
また、メッシュを構成する線材の断面形状としては、特に限定しないが、熱硬化性樹脂組成物が回り込みやすくするため丸線が好ましい。 In addition, the cross-sectional shape of the wire constituting the mesh is not particularly limited, but a round wire is preferable in order for the thermosetting resin composition to easily wrap around.
メッシュの厚さとしては、得られる黒鉛粉成形体の厚さの５〜３０％であることが好ましく、より好ましくは１０〜２０％である。メッシュの厚さが、得られる黒鉛成形体の厚さの５％未満であると、導電性の上昇効果がほとんど得られず、また、メッシュによる補強強化もほとんど得られず、更にはメッシュと熱硬化性樹脂組成物との界面で剥離してしまう虞れがあり、一方、３０％より厚いと、メッシュが露出して、得られる黒鉛粒子成形体の耐食性が劣ったり、また、メッシュと熱硬化性樹脂組成物との界面で剥離してしまう虞れがある。 The thickness of the mesh is preferably 5 to 30%, more preferably 10 to 20% of the thickness of the obtained graphite powder molded body. When the thickness of the mesh is less than 5% of the thickness of the obtained graphite molded body, the effect of increasing the conductivity is hardly obtained, and the reinforcing reinforcement by the mesh is hardly obtained. There is a risk of peeling at the interface with the curable resin composition. On the other hand, if it is thicker than 30%, the mesh is exposed, and the resulting graphite particle molded body has poor corrosion resistance, and the mesh and the thermoset are cured. There is a possibility of peeling at the interface with the conductive resin composition.
メッシュの目開き寸法としては、使用する黒鉛粒子の粒径よりも大きいことが好ましく、より好ましくは１５０〜２５０μｍである。メッシュの目開き寸法が使用する黒鉛粒子の粒径よりも大きいものであれば、成形材料をプレスした時、メッシュの網目に黒鉛粒子がスムーズに流動して充填されるので、メッシュと黒鉛粒子とが良好に接触し、両者の境界面に生じる接触抵抗が少なくなるので、導電性を向上させることができる。 The mesh opening size is preferably larger than the particle size of the graphite particles used, and more preferably 150 to 250 μm. If the mesh opening size is larger than the particle size of the graphite particles used, when the molding material is pressed, the graphite particles smoothly flow and fill the mesh mesh. Can be satisfactorily brought into contact with each other and the contact resistance generated at the interface between the two is reduced, so that the conductivity can be improved.
熱硬化性樹脂組成物としては、黒鉛粒子の含有量が６０〜９０質量％で、熱硬化性樹脂の含有量が１０〜４０質量％である組成物を用いる。黒鉛粒子の含有量は、８０〜９０質量％であることが好ましい。また、熱硬化性樹脂の含有量は、１０〜２０質量％であることが好ましい。黒鉛粒子の含有量が６０質量％未満であると、導電性の不充分な黒鉛粒子成形体となりがちであり、一方、９０質量％を越えると、強度的に脆くなりやすく、耐久性や保形性に劣る黒鉛粒子成形体となりがちである。 As the thermosetting resin composition, a composition having a graphite particle content of 60 to 90% by mass and a thermosetting resin content of 10 to 40% by mass is used. The content of the graphite particles is preferably 80 to 90% by mass. Moreover, it is preferable that content of a thermosetting resin is 10-20 mass%. If the content of the graphite particles is less than 60% by mass, the graphite particles tend to be inadequately conductive. It tends to be a graphite particle molded body having inferior properties.
黒鉛粒子としては、平均粒径５〜１００μｍであるものが好ましく、より好ましくは１０〜６０μｍである。平均粒子径が５μｍ未満であると、黒鉛粒子成形体の導電性が劣りがちであり、１００μｍよりも大きいと、黒鉛粒子成形体の強度が劣りがちであり、また、黒鉛粒子成形体の厚みを薄くすることが困難である。 The graphite particles are preferably those having an average particle size of 5 to 100 μm, more preferably 10 to 60 μm. When the average particle diameter is less than 5 μm, the conductivity of the graphite particle molded body tends to be inferior. When it is larger than 100 μm, the strength of the graphite particle molded body tends to be inferior, and the thickness of the graphite particle molded body is reduced. It is difficult to make it thinner.
熱硬化性樹脂としては、フェノール樹脂、メラミン樹脂、不飽和ポリエステル樹脂、エポキシ樹脂、フラン樹脂、アクリル樹脂、あるいはこれらの混合系などのものが挙げられ、なかでも黒鉛粒子との濡れ性に優れているという理由からフェノール樹脂が好ましい。 Examples of thermosetting resins include phenolic resins, melamine resins, unsaturated polyester resins, epoxy resins, furan resins, acrylic resins, and mixed systems thereof, and in particular, excellent wettability with graphite particles. Phenol resin is preferred because it is.
また、熱硬化性樹脂組成物には、黒鉛粒子と熱硬化性樹脂のほかに、更に必要に応じてカーボンナノチューブやカーボン繊維などを含有させてもよい。これらの含有量は合計して５質量％以下とすることが好ましい。 In addition to the graphite particles and the thermosetting resin, the thermosetting resin composition may further contain carbon nanotubes, carbon fibers, and the like as necessary. The total content of these is preferably 5% by mass or less.
次に、本発明の黒鉛粒子成形体の製造方法について説明する。
図１（ａ）、（ｂ）に示すように、まず、所望の形状を有するプレス金型１の下金型１ａに、熱硬化性樹脂と黒鉛粒子とを含有する熱硬化性樹脂組成物２を充填し、導電性を有するメッシュ３を、該熱硬化性樹脂組成物２中に埋没させて、上金型１ｂによりプレス成形（以下「本プレス」と記す）する。
Next, the manufacturing method of the graphite particle molded object of this invention is demonstrated.
As shown in FIGS. 1A and 1B, first, a thermosetting resin composition 2 containing a thermosetting resin and graphite particles in a lower die 1a of a press die 1 having a desired shape. The conductive mesh 3 is embedded in the thermosetting resin composition 2 and press-molded (hereinafter referred to as “main press”) with the upper mold 1b.
本発明では、熱硬化性樹脂組成物２として、あらかじめ仮プレスしてシート状成形体としたものを用い、シート状成形体で導電性を有するメッシュを挟み込むようにして本プレスすることが好ましい。また、シート状成形体としては、熱硬化性樹脂組成物を、６０〜１００℃で、２００〜２０００ｋｇｆ／ｃｍ２で仮プレスしたものを用いることが好ましい。 In the present invention, it is preferable that the thermosetting resin composition 2 is pre-pressed into a sheet-like molded body in advance, and this press is performed by sandwiching a conductive mesh between the sheet-like molded body. Moreover, as a sheet-like molded object, it is preferable to use what pre-pressed the thermosetting resin composition at 60-100 degreeC at 200-2000 kgf / cm < 2 >.
熱硬化性樹脂組成物２として仮プレスされたシート状成形体を用いることで、導電性を有するメッシュが所望の位置に配置された黒鉛粒子成形体を得ることができるので、例えば、黒鉛粒子成形体に穴などを設ける必要がある場合などにおいて、該メッシュが露出するといった問題を回避できる。 By using a preliminarily pressed sheet-like molded body as the thermosetting resin composition 2, a graphite particle molded body in which a conductive mesh is disposed at a desired position can be obtained. When it is necessary to provide a hole or the like in the body, the problem that the mesh is exposed can be avoided.
本プレスは、成形温度６０〜１００℃、成形圧力５００〜２０００ｋｇｆ／ｃｍ２の条件で行う。成形温度としては６０〜８０℃であることが好ましい。また、成形圧力としては１０００〜２０００ｋｇｆ／ｃｍ２であることが好ましい。 This press is performed under conditions of a molding temperature of 60 to 100 ° C. and a molding pressure of 500 to 2000 kgf / cm 2 . The molding temperature is preferably 60 to 80 ° C. The molding pressure is preferably 1000 to 2000 kgf / cm 2 .
成形温度が６０℃未満であると、粒子密度を緻密化させることができず、導電性の高い黒鉛粒子成形体が得られない虞れがあり、１００℃よりも高いと、熱硬化性樹脂が流動性を持ち始めてしまうので、プレス成形により樹脂が表面に浮き上がりやすくなってしまい、黒鉛粒子成形体の導電性を損ないやすい。また、成形圧力が５００ｋｇｆ／ｃｍ２未満であると、粒子密度を緻密化させることができず、導電性の高い黒鉛粒子成形体が得られない虞れがあり、また、２０００ｋｇｆ／ｃｍ２よりも大きくしても、さほど黒鉛粒子成形体の粒子密度は向上せず、そればかりか、表面に樹脂層を形成してしまう虞れがあるので導電性が損なわれやすい。 If the molding temperature is less than 60 ° C, the particle density cannot be densified, and a highly conductive graphite particle molded body may not be obtained. If the molding temperature is higher than 100 ° C, the thermosetting resin Since it starts to have fluidity, the resin tends to float on the surface by press molding, and the conductivity of the graphite particle molded body tends to be impaired. Further, if the molding pressure is less than 500 kgf / cm 2 , the particle density cannot be densified, and a highly conductive graphite particle molded body may not be obtained, and more than 2000 kgf / cm 2. Even if it is increased, the particle density of the graphite particle molded body is not improved so much, and there is a possibility that a resin layer may be formed on the surface.
次いで、この所望の形状にプレス成形されたプレス成形体４を、図１（ｃ）に示すように硬化処理して黒鉛粒子成形体とする。 Next, the press-molded body 4 press-molded into the desired shape is cured as shown in FIG. 1C to obtain a graphite particle molded body.
このプレス成形体４は、黒鉛粒子がしっかりと圧粉されているので、未硬化状態であっても保形性に優れたものである。そのため、硬化処理を金型内でプレスしながら行わなくとも、緻密で均一な粒子密度を有し、所望の形状を有した黒鉛粒子成形体を得ることができるので、例えば、未硬化処理のプレス成形体４を金型１から取り出し、加熱炉などに投入して硬化処理してもよい。 Since this press-molded body 4 is firmly compacted with graphite particles, it has excellent shape retention even in an uncured state. Therefore, it is possible to obtain a graphite particle compact having a dense and uniform particle density and having a desired shape without pressing the curing process in a mold. The molded body 4 may be taken out from the mold 1 and placed in a heating furnace or the like to be cured.
硬化処理条件としては、使用する熱硬化性樹脂の種類により異なり、特に限定はしないが、例えば、フェノール樹脂を用いた場合は、１５０〜１７０℃で、０．５〜１時間とすることが好ましい。 Curing treatment conditions vary depending on the type of thermosetting resin used, and are not particularly limited. For example, when a phenol resin is used, it is preferably 150 to 170 ° C. and 0.5 to 1 hour. .
こうして得られた黒鉛粒子形体は、ＪＩＳ−Ｋ−７１９４の導電性プラスチックの４探針法による抵抗試験方法に準拠した黒鉛粒子成形体の固有抵抗率が５ｍΩ・ｃｍ以下で、従来の黒鉛粒子成形体よりも導電性に優れ、更には、メッシュによる補強効果により、機械強度も優れたものであり、例えば、燃料電池用セパレータ、燃料電池用セパレータ、電極端子、電池電極材などのような特に耐食性と導電性の要求される部材として好適に用いることができる。 The graphite particle shape thus obtained has a specific resistivity of 5 mΩ · cm or less according to a resistance test method based on a four-probe method of conductive plastic of JIS-K-7194. It has better electrical conductivity than the body, and also has excellent mechanical strength due to the reinforcing effect of the mesh. For example, it is particularly resistant to corrosion such as fuel cell separators, fuel cell separators, electrode terminals, battery electrode materials, etc. And can be suitably used as a member requiring electrical conductivity.
以下実施例を用いて本発明の効果を説明する。 The effects of the present invention will be described below using examples.
（実施例１）
平均粒子径１７μｍの黒鉛８６質量％、フェノール樹脂１４質量％からなる熱硬化性樹脂組成物を、１０００ｋｇｆ／ｃｍ２、６０℃の成形条件で仮プレスしてシート状成形体とした。次いで、このシート状成形体上に、銅メッシュ（目開き０．２８０ｍｍ、厚さ０．２８ｍｍ）を設置し、更に同様のシート状成形体を銅メッシュ上に配置した。次いで、この積層体を１０００ｋｇｆ／ｃｍ２、６０℃の成形条件でプレス成形（本プレス）して、厚さ１．１８ｍｍのプレス成形体を得た。そして、このプレス成形体を１６０℃で６０分間硬化処理して実施例１の黒鉛粒子成形体を得た。
Example 1
A thermosetting resin composition comprising 86% by mass of graphite having an average particle diameter of 17 μm and 14% by mass of phenol resin was temporarily pressed under molding conditions of 1000 kgf / cm 2 and 60 ° C. to obtain a sheet-like molded body. Next, a copper mesh (aperture 0.280 mm, thickness 0.28 mm) was placed on the sheet-like molded body, and a similar sheet-like molded body was further placed on the copper mesh. Next, this laminate was press-molded (main press) under molding conditions of 1000 kgf / cm 2 and 60 ° C. to obtain a press-molded body having a thickness of 1.18 mm. The press-molded body was cured at 160 ° C. for 60 minutes to obtain a graphite particle molded body of Example 1.
（実施例２）
実施例１のシート状成形体を用いた。次いで、シート状成形体上に、銅メッシュ（目開き０．２８０、厚さ０．２８ｍｍ）を設置し、同様のシート状成形体を銅メッシュ上に配置して、１０００ｋｇｆ／ｃｍ２、６０℃の成形条件でプレス成形（本プレス）して、厚さ２．３０ｍｍのプレス成形体を得た。そして、このプレス成形体を１６０℃で６０分間硬化処理して実施例２の黒鉛粒子成形体を得た。
(Example 2)
The sheet-like molded body of Example 1 was used. Next, a copper mesh (aperture 0.280, thickness 0.28 mm) is placed on the sheet-like molded body, and a similar sheet-like molded body is placed on the copper mesh, 1000 kgf / cm 2 , 60 ° C. A press-molded body having a thickness of 2.30 mm was obtained by press molding (main press) under the molding conditions described above. Then, this press-molded body was cured at 160 ° C. for 60 minutes to obtain a graphite particle molded body of Example 2.
（実施例３）
実施例１のシート状成形体を用いた。次いで、シート状成形体上に、銅メッシュ（目開き０．１５４、厚さ０．２０ｍｍ）を設置し、同様のシート状成形体を銅メッシュ上に配置して、１０００ｋｇｆ／ｃｍ２、６０℃の成形条件でプレス成形（本プレス）して、厚さ２．０９ｍｍのプレス成形体を得た。そして、このプレス成形体を１６０℃で６０分間硬化処理して実施例３の黒鉛粒子成形体を得た。
(Example 3)
The sheet-like molded body of Example 1 was used. Next, a copper mesh (aperture 0.154, thickness 0.20 mm) was placed on the sheet-like molded body, and a similar sheet-like molded body was placed on the copper mesh, 1000 kgf / cm 2 , 60 ° C. A press-molded body having a thickness of 2.09 mm was obtained. And this press-molded body was cured at 160 ° C. for 60 minutes to obtain a graphite particle molded body of Example 3.
（実施例４）
実施例１のシート状成形体を用いた。次いで、シート状成形体上に、銅メッシュ（目開き０．１５４、厚さ０．２０ｍｍ）を設置し、同様のシート状成形体を銅メッシュ上に配置して、５００ｋｇｆ／ｃｍ２、６０℃の成形条件でプレス成形（本プレス）して、厚さ２．４４ｍｍのプレス成形体を得た。そして、このプレス成形体を１６０℃で６０分間硬化処理して実施例４の黒鉛粒子成形体を得た。
Example 4
The sheet-like molded body of Example 1 was used. Next, a copper mesh (aperture 0.154, thickness 0.20 mm) is placed on the sheet-like molded body, and a similar sheet-like molded body is placed on the copper mesh, 500 kgf / cm 2 , 60 ° C. A press-molded body having a thickness of 2.44 mm was obtained by press molding (main press) under the molding conditions. The press-molded body was cured at 160 ° C. for 60 minutes to obtain a graphite particle molded body of Example 4.
（実施例５）
実施例１のシート状成形体を用いた。次いで、シート状成形体上に、銅メッシュ（目開き０．２８０、厚さ０．２８ｍｍ）を設置し、同様のシート状成形体を銅メッシュ上に配置して、１０００ｋｇｆ／ｃｍ２、６０℃の成形条件でプレス成形（本プレス）して、厚さ５．６１ｍｍのプレス成形体を得た。そして、このプレス成形体を１６０℃で６０分間硬化処理して実施例５の黒鉛粒子成形体を得た。
(Example 5)
The sheet-like molded body of Example 1 was used. Next, a copper mesh (aperture 0.280, thickness 0.28 mm) is placed on the sheet-like molded body, and a similar sheet-like molded body is placed on the copper mesh, 1000 kgf / cm 2 , 60 ° C. A press-molded body having a thickness of 5.61 mm was obtained by press molding (main press) under the molding conditions described above. Then, this press-molded body was cured at 160 ° C. for 60 minutes to obtain a graphite particle molded body of Example 5.
（比較例１）
平均粒子径１７μｍの黒鉛８６質量％、フェノール樹脂１４質量％からなる熱硬化性樹脂組成物を、１０００ｋｇｆ／ｃｍ２、６０℃の成形条件でプレス成形（本プレス）して、厚さ１．９０ｍｍのプレス成形体を得た。そして、このプレス成形体を１６０℃で６０分間硬化処理して比較例１の黒鉛粒子成形体を得た。
(Comparative Example 1)
A thermosetting resin composition composed of 86% by mass of graphite having an average particle size of 17 μm and 14% by mass of phenol resin was press-molded (main press) under molding conditions of 1000 kgf / cm 2 and 60 ° C., and the thickness was 1.90 mm. The press-molded body was obtained. The press-molded body was cured at 160 ° C. for 60 minutes to obtain a graphite particle molded body of Comparative Example 1.
〔物性試験〕
上記実施例１〜５及び比較例１の黒鉛粒子成形体について、ＪＩＳ−Ｋ−７１９４の導電性プラスチックの４探針法による抵抗試験方法に準拠して、それぞれの黒鉛粒子成形体の固有抵抗率（ｍΩ・ｃｍ）を測定した。結果を表１に記す。
[Physical property test]
About the graphite particle molded bodies of Examples 1 to 5 and Comparative Example 1 above, the specific resistivity of each graphite particle molded body in accordance with the resistance test method based on the 4-probe method of conductive plastic of JIS-K-7194 (MΩ · cm) was measured. The results are shown in Table 1.
上記結果より、導電性を有するメッシュを埋設した実施例1〜５の黒鉛粒子成形体は、導電性を有するメッシュを埋設していない比較例１の黒鉛粒子成形体よりも固有抵抗率が低く、導電性の極めて良好なものであった。 From the above results, the graphite particle molded bodies of Examples 1 to 5 embedded with conductive mesh have lower specific resistivity than the graphite particle molded body of Comparative Example 1 without embedded conductive mesh, The conductivity was very good.
本発明の黒鉛粒子成形体は、例えば燃料電池のセパレータや電極材料として用いることができる。 The graphite particle compact of the present invention can be used, for example, as a fuel cell separator or electrode material.
１：プレス金型
２：熱硬化性樹脂組成物
３：メッシュ
４：プレス成形体
1: Press mold 2: Thermosetting resin composition 3: Mesh 4: Press-molded body
Claims (10)
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| JP2005187840A JP2007012292A (en) | 2005-06-28 | 2005-06-28 | Graphite particle molding and its manufacturing method |
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| JP2005187840A JP2007012292A (en) | 2005-06-28 | 2005-06-28 | Graphite particle molding and its manufacturing method |
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Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| WO2008133333A1 (en) * | 2007-04-25 | 2008-11-06 | Jfe Chemical Corporation | Carbonaceous sheet and fuel cell separator using the same |
| JP2013516505A (en) * | 2009-12-31 | 2013-05-13 | エスゲーエル カーボン ソシエタス ヨーロピア | Graphite-containing plate and method for producing graphite-containing plate |
-
2005
- 2005-06-28 JP JP2005187840A patent/JP2007012292A/en active Pending
Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| WO2008133333A1 (en) * | 2007-04-25 | 2008-11-06 | Jfe Chemical Corporation | Carbonaceous sheet and fuel cell separator using the same |
| JP2013516505A (en) * | 2009-12-31 | 2013-05-13 | エスゲーエル カーボン ソシエタス ヨーロピア | Graphite-containing plate and method for producing graphite-containing plate |
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