JP3864158B2 - Manufacturing method of fuel cell separator - Google Patents
Manufacturing method of fuel cell separator Download PDFInfo
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- JP3864158B2 JP3864158B2 JP2003417107A JP2003417107A JP3864158B2 JP 3864158 B2 JP3864158 B2 JP 3864158B2 JP 2003417107 A JP2003417107 A JP 2003417107A JP 2003417107 A JP2003417107 A JP 2003417107A JP 3864158 B2 JP3864158 B2 JP 3864158B2
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- 239000000446 fuel Substances 0.000 title claims description 68
- 238000004519 manufacturing process Methods 0.000 title claims description 35
- 229920001187 thermosetting polymer Polymers 0.000 claims description 34
- 239000011347 resin Substances 0.000 claims description 32
- 229920005989 resin Polymers 0.000 claims description 32
- 238000000465 moulding Methods 0.000 claims description 31
- 239000000463 material Substances 0.000 claims description 25
- 238000010438 heat treatment Methods 0.000 claims description 21
- 238000000034 method Methods 0.000 claims description 21
- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical compound [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 claims description 17
- 239000005011 phenolic resin Substances 0.000 claims description 9
- 238000003825 pressing Methods 0.000 claims description 6
- 229920000178 Acrylic resin Polymers 0.000 claims description 3
- 239000004925 Acrylic resin Substances 0.000 claims description 3
- 239000003822 epoxy resin Substances 0.000 claims description 3
- 239000007849 furan resin Substances 0.000 claims description 3
- 229920000647 polyepoxide Polymers 0.000 claims description 3
- 239000000203 mixture Substances 0.000 claims description 2
- 239000000155 melt Substances 0.000 claims 1
- 230000002950 deficient Effects 0.000 description 15
- 230000000052 comparative effect Effects 0.000 description 13
- UFHFLCQGNIYNRP-UHFFFAOYSA-N Hydrogen Chemical compound [H][H] UFHFLCQGNIYNRP-UHFFFAOYSA-N 0.000 description 11
- 229910052739 hydrogen Inorganic materials 0.000 description 11
- 239000001257 hydrogen Substances 0.000 description 11
- 238000000576 coating method Methods 0.000 description 8
- 239000011248 coating agent Substances 0.000 description 5
- 229910002804 graphite Inorganic materials 0.000 description 4
- 239000010439 graphite Substances 0.000 description 4
- 238000007731 hot pressing Methods 0.000 description 4
- 238000006243 chemical reaction Methods 0.000 description 3
- 238000000280 densification Methods 0.000 description 3
- 239000000843 powder Substances 0.000 description 3
- 239000007789 gas Substances 0.000 description 2
- 238000005259 measurement Methods 0.000 description 2
- 238000000691 measurement method Methods 0.000 description 2
- 238000002844 melting Methods 0.000 description 2
- 230000008018 melting Effects 0.000 description 2
- 239000002245 particle Substances 0.000 description 2
- ISWSIDIOOBJBQZ-UHFFFAOYSA-N Phenol Chemical compound OC1=CC=CC=C1 ISWSIDIOOBJBQZ-UHFFFAOYSA-N 0.000 description 1
- 230000005540 biological transmission Effects 0.000 description 1
- 230000006835 compression Effects 0.000 description 1
- 238000007906 compression Methods 0.000 description 1
- 230000007547 defect Effects 0.000 description 1
- 230000000694 effects Effects 0.000 description 1
- 150000002431 hydrogen Chemical class 0.000 description 1
- 230000014759 maintenance of location Effects 0.000 description 1
- 238000012986 modification Methods 0.000 description 1
- 230000004048 modification Effects 0.000 description 1
- 230000035699 permeability Effects 0.000 description 1
- 230000000704 physical effect Effects 0.000 description 1
- 238000005507 spraying Methods 0.000 description 1
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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
- Y02E60/30—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
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- Fuel Cell (AREA)
Description
本発明は、燃料電池に用いられる燃料電池用セパレータの製造方法に関する。 The present invention relates to a method for producing a fuel cell separator used in a fuel cell.
従来より、燃料電池を構成する一部材として燃料電池用セパレータがある。この燃料電池用セパレータは、左右両側面に複数個の溝部を備えて構成されており、その製造方法として、冷間プレス工程を備えた製造方法と、熱間プレス工程を備えた製造方法とが知られている。 Conventionally, there is a fuel cell separator as one member constituting a fuel cell. This fuel cell separator is configured to have a plurality of groove portions on both the left and right side surfaces. As a manufacturing method thereof, there are a manufacturing method including a cold pressing step and a manufacturing method including a hot pressing step. Are known.
前者の製造方法の概略を説明すると、まず、黒鉛粉末に熱硬化性樹脂が被覆されてなる熱硬化性樹脂被覆粉末黒鉛（以下、単に「燃料電池セパレータ用材料」という）を、プレス装置にセットされた常温の金型に充填し、１００ＭＰａ以上の高圧でプレス（冷間プレス）して、所定形状に成型し、その成型体を加熱して樹脂を硬化させる方法である。 The outline of the former production method will be explained. First, thermosetting resin-coated powder graphite (hereinafter simply referred to as “material for fuel cell separator”) obtained by coating graphite powder with thermosetting resin is set in a press device. This is a method in which the normal temperature mold is filled, pressed at a high pressure of 100 MPa or more (cold press), molded into a predetermined shape, and the molded body is heated to cure the resin.
次に後者の製造法の概略を説明すると、炭素粉末と熱硬化性樹脂を混合して、プレス装置にセットされた金型に投入し、それに圧縮力を作用させると同時に金型を加熱（熱間プレス）して、プレスとほぼ同時に樹脂を硬化させて製造する方法である（例えば特許文献１参照）。 Next, the outline of the latter manufacturing method will be explained. Carbon powder and a thermosetting resin are mixed, put into a mold set in a press apparatus, a compression force is applied to the mold, and the mold is heated (heated). This is a method in which the resin is cured almost simultaneously with the press (see, for example, Patent Document 1).
なお、上記した熱硬化性樹脂は、その物性として軟化溶解温度を有しており、この樹脂を加熱すると、まず軟化溶融が始まり、その後、硬化するものである。 The thermosetting resin described above has a softening and melting temperature as its physical properties. When this resin is heated, the softening and melting starts first and then hardens.
しかしながら、上記した製造方法には下記の問題点がある。
まず、前者の冷間プレス工程を備えた製造方法は、常温の金型を用い、１００ＭＰａ以上の高圧でもって加圧するとした、プレス圧力に依存したメカニズムであるため、熱硬化性樹脂の軟化が不十分となったり、一様な軟化状態とならず、緻密化が不完全となる場合が多い。
However, the above manufacturing method has the following problems.
First, the former manufacturing method including the cold pressing step uses a normal temperature mold and pressurizes with a high pressure of 100 MPa or more, and is a mechanism depending on the pressing pressure. Therefore, the thermosetting resin is softened. In many cases, it becomes insufficient or does not become a uniform softened state, and the densification is incomplete.
つまり、このような状態のまま樹脂を加熱して硬化させることで、不良品の発生頻度が極めて高くなり、歩留まりが低い、といった問題点を有している。 That is, there is a problem in that the resin is heated and cured in such a state so that the occurrence frequency of defective products becomes extremely high and the yield is low.
次に、後者の熱間プレス工程を備えた製造方法は、熱硬化性樹脂の熱硬化温度領域によるプレスであるために、キャビティ内の燃料電池セパレータ用材料は、すぐさま軟化溶解が始まり、その直後に硬化反応に転じる。 Next, since the latter manufacturing method including the hot pressing step is a pressing by a thermosetting temperature region of a thermosetting resin, the material for the fuel cell separator in the cavity immediately begins to soften and dissolve, and immediately thereafter. It turns into a curing reaction.
しかしながら、この一連の現象は、キャビティ内の燃料電池セパレータ用材料すべて同時に生じるのではなく、熱の伝わり方にムラがあるために時間差が生じている。その結果、黒鉛粒子間に熱硬化性樹脂が十分に行き渡る前に硬化したりして、緻密化が不完全となる場合がある。 However, this series of phenomena does not occur at the same time for all the fuel cell separator materials in the cavity, but causes a time difference due to unevenness in how heat is transmitted. As a result, the thermosetting resin may be hardened before it is sufficiently distributed between the graphite particles, resulting in incomplete densification.
つまり、この熱間プレス工程を備えた製造方法は、合理的な製造方法ではあるが、このような原因による不良品が発生する虞があり、必ずしも歩留まりが高いとはいえない。
また、不良品とまではいかなくても、緻密化が製品毎に多少異なるために、燃料電池の性能を決定づける一要因である燃料電池用セパレータのガス透過性や電気抵抗不良率にバラツキが生じ、個体差がでてしまう、といった問題点をも有している。
That is, the manufacturing method provided with this hot pressing process is a rational manufacturing method, but there is a risk that a defective product due to such a cause may occur, and the yield is not necessarily high.
Even if it is not a defective product, the densification differs slightly from product to product, resulting in variations in the gas permeability and electrical resistance failure rate of the fuel cell separator, which is one factor that determines the performance of the fuel cell. There are also problems such as individual differences.
そこで、本発明は、燃料電池セパレータの歩留まりを向上させ、性能差のない安定した燃料電池セパレータを製造することができる燃料電池セパレータの製造方法を提供することを目的とする。 Then, an object of this invention is to provide the manufacturing method of the fuel cell separator which can improve the yield of a fuel cell separator and can manufacture the stable fuel cell separator without a performance difference.
本発明は上記課題を解決すべく以下に掲げる構成とした。
請求項１記載の発明の要旨は、熱硬化性樹脂が被覆された黒鉛粉末を主成分とした燃料電池セパレータ用材料を用いた燃料電池セパレータの製造方法であって、前記燃料電池セパレータ用材料を、前記熱硬化性樹脂が軟化溶融するが硬化しない温度で無加圧で保持する加温処理工程と、前記加温処理工程の後で前記燃料電池セパレータ用材料を金型を用いて加圧成型する成型工程と、前記成型工程で成型された成型体を前記熱硬化性樹脂が硬化する温度で無加圧で保持する硬化工程とを備えることを特徴とした燃料電池セパレータの製造方法に存する。
請求項２記載の発明の要旨は、前記加温処理工程において、前記燃料電池セパレータ用材料が前記金型中に投入されていることを特徴とする請求項１に記載の燃料電池セパレータの製造方法に存する。
請求項３記載の発明の要旨は、前記加温処理工程における温度は、概ね４０〜８０℃の範囲であることを特徴とする請求項１または２に記載の燃料電池セパレータの製造方法に存する。
請求項４記載の発明の要旨は、前記成型工程での加圧力は、概ね１５ＭＰａ〜１００ＭＰａの範囲であることを特徴とする請求項１乃至３のいずれか１項に記載の燃料電池セパレータの製造方法に存する。
請求項５記載の発明の要旨は、前記硬化工程における温度は、８０℃〜２５０℃の範囲であることを特徴とする請求項１乃至４のいずれか１項に記載の燃料電池セパレータの製造方法に存する。
請求項６記載の発明の要旨は、前記熱硬化性樹脂は、フェノール樹脂、フラン樹脂、エポキシ樹脂、アクリル樹脂のいずれか、あるいはいずれかの混合物であることを特徴とする請求項１乃至５のいずれか１項に記載の燃料電池セパレータの製造方法に存する。
請求項７記載の発明の要旨は、請求項１乃至６のいずれか１項に記載の燃料電池セパレータの製造方法によって製造されたことを特徴とする燃料電池セパレータに存する。
The present invention is configured as follows to solve the above problems.
The gist of the invention described in
The gist of the invention described in
The gist of the invention described in claim 3 resides in the method for producing a fuel cell separator according to
The gist of the invention described in claim 4 is that the pressure applied in the molding step is generally in the range of 15 MPa to 100 MPa. The manufacture of the fuel cell separator according to any one of
The gist of the invention described in claim 5 is that the temperature in the curing step is in the range of 80 ° C to 250 ° C. The method for producing a fuel cell separator according to any one of
The gist of the invention described in claim 6 is that the thermosetting resin is any one of phenol resin, furan resin, epoxy resin, acrylic resin, or a mixture thereof. It exists in the manufacturing method of the fuel cell separator of any one.
The subject matter of the seventh aspect resides in a fuel cell separator manufactured by the method for manufacturing a fuel cell separator according to any one of the first to sixth aspects.
本発明によれば、成型体を成型する成型工程において、熱硬化性樹脂が軟化溶融した状態の燃料電池セパレータ用材料を用いることで、樹脂硬化反応が起こることなく、黒鉛粉末間に熱硬化性樹脂を十分に行き渡らせることができる。さらに、硬化工程において成型体を硬化させることで、製品毎に性能のバラツキのない均質の燃料電池セパレータを製造することができる。したがって、製品の歩留まりを向上することができる。 According to the present invention, in the molding process of molding a molded body, by using a material for a fuel cell separator in which a thermosetting resin is softened and melted, a thermosetting property is not generated between graphite powders without causing a resin curing reaction. The resin can be fully distributed. Furthermore, by curing the molded body in the curing step, it is possible to produce a homogeneous fuel cell separator that does not vary in performance from product to product. Therefore, the product yield can be improved.
特に、熱硬化温度での一段成型（冷間プレス、熱間プレス）に比べて、樹脂不均一による電気抵抗不良率、水素透過不良率が半分以下となり、製品の歩留まりが極めて向上することができる。
また、熱硬化性樹脂が軟化しているため、短時間（極端に言えば一瞬）で所要の形状に成型することができる。
In particular, compared to single-stage molding (cold press, hot press) at the thermosetting temperature, the electrical resistance failure rate and the hydrogen permeation failure rate due to resin non-uniformity are less than half, and the product yield can be greatly improved. .
Further, since the thermosetting resin is softened, it can be molded into a required shape in a short time (in short, in an instant).
また、成型工程の処理前に、加温装置で金型を予熱し、軟化溶融した燃料電池セパレータ用材料を用いることで、成型工程に要する時間を大幅に短縮できる。とくに金型を複数個予め用意しておくことで、極めて効率的に成型工程を行うことができる。
さらに、金型にヒータを内装させた場合、燃料電池セパレータ用材料をそのまま充填することができ、利便性を向上することができる。
燃料電池セパレータ用材料の加温温度や加圧力を限定したことで、上記の効果が最も顕著に得ることができる。
In addition, the time required for the molding process can be greatly shortened by using the fuel cell separator material that has been preheated and softened and melted with a heating device before the molding process. In particular, by preparing a plurality of molds in advance, the molding process can be performed very efficiently.
Further, when the heater is built in the mold, the fuel cell separator material can be filled as it is, and the convenience can be improved.
By limiting the heating temperature and pressure of the fuel cell separator material, the above-mentioned effects can be obtained most remarkably.
次に、本発明の実施の形態を添付図面を用いて説明をする。
まず、燃料電池セパレータ用材料ａについて説明すると、この燃料電池セパレータ用材料ａは黒鉛粉末を熱硬化性樹脂で被覆されてなる。
Next, embodiments of the present invention will be described with reference to the accompanying drawings.
First, the fuel cell separator material a will be described. The fuel cell separator material a is obtained by coating graphite powder with a thermosetting resin.
この上記した熱硬化性樹脂は、フェノール樹脂、フラン樹脂、エポキシ樹脂、アクリル樹脂、あるいはこれらの混合系などの熱硬化性樹脂等、いずれでも良い。また、被覆方法としては、一般的に用いられる溶液被覆、スプレー被覆、反応被覆、溶融被覆などいずれを用いても良いものである。ただし反応被覆は単一の樹脂系に用いる場合が多い。 This thermosetting resin may be any of a thermosetting resin such as a phenol resin, a furan resin, an epoxy resin, an acrylic resin, or a mixed system thereof. As a coating method, any of commonly used solution coating, spray coating, reaction coating, melt coating and the like may be used. However, reactive coatings are often used for single resin systems.
次に、以上のように構成された燃料電池セパレータ用材料ａを用いた燃料電池セパレータＡの製造方法を、順を追って説明する。
（１）第１の加温処理工程
複数個の上下一対の金型１と、その金型１の下型内（キャビティ内）に所定量の燃料電池セパレータ用材料ａを投入する。そして、この複数個の金型１を工業用オーブンまたはコンベアなどの搬送手段を有した炉等の加温装置２にセットし、概ね４０〜８０℃範囲内程度に収まるような温度に加温して予熱する（図１（ａ）参照）。
Next, a manufacturing method of the fuel cell separator A using the fuel cell separator material a configured as described above will be described in order.
(1) First Heating Process Step A predetermined amount of the fuel cell separator material a is put into a plurality of upper and lower pairs of
なお、燃料電池セパレータ用材料ａは必ずしも金型１に投入し、金型１と一緒に加温する必要性はなく、金型１と燃料電池セパレータ用材料ａ（所望の容器に入れて）とを分別し、それぞれを加温しても良い。
The fuel cell separator material a does not necessarily need to be put into the
キャビティ内の燃料電池セパレータ用材料ａは、加温が進むにつれて軟化溶融し始め、流動性を有する所謂ゲル化して、黒鉛粉末間に熱硬化性樹脂が十分に行き渡るようになる。
なお、この第１の加温処理工程に替えて、金型１にヒータを内装させ（図示せず）、該ヒータによって金型１を加温して、上記した熱硬化性樹脂を軟化溶融可能な温度に加温してもよい（第２の加温処理工程）。
The fuel cell separator material a in the cavity begins to soften and melt as the heating proceeds, so-called gelling having fluidity, and the thermosetting resin is sufficiently distributed between the graphite powders.
In place of the first heating process, a heater is installed in the mold 1 (not shown), and the
（２）成型工程
第１の加温処理工程が終了したら、金型１をプレス装置３にセットして、概ね２０ＭＰａ〜８０ＭＰａの加圧力でもって加圧成型する（図１（ｂ）参照）。なお、プレス装置が過大になるという点で圧力の上限として１００ＭＰａ未満であることが望ましく、また、製品の強度などの機械的性質及び電気的な性質を満足するために、圧力の下限は、概ね１５ＭＰａは必要である。
(2) Molding process When the first heating process is completed, the
（３）硬化工程
加圧成型が終了したら、プレス装置３から金型１を取り外し、その状態のまま、一般的な熱硬化性樹脂が硬化開始する約８０℃〜２５０℃未満に予熱された専用炉４（または上記の加温装置２を共用しても良い）に順次搬入し、熱硬化させる（図１（ｃ）参照）。
所定時間経過後、熱硬化が完了した形成された燃料電池セパレータＡを、金型１から脱型して一連の処理が終了する（図１（ｄ）参照）。
(3) Curing process After press molding is completed, the
After a predetermined time has elapsed, the formed fuel cell separator A that has undergone thermosetting is removed from the
この硬化処理は、金型１ごと処理しているが、加圧成型が終了した成型体を金型１から脱型し、その成型体を専用炉４または上記の加温装置２に搬入し、熱硬化させても良い。なお、金型１から脱型した硬化処理前の成型体は、極端な外力を与えれば変形するものの、すでに保形性を有しているために、脱型してもは型くずれすることはない。
This curing process is performed for each
特に、第２の加温処理工程を採用した場合、金型１をプレス装置３に取り付けたままにして、加圧成型が終了した成型体を金型１から脱型する方法が生産性が向上することから好適である。
In particular, when the second heating process is employed, productivity is improved by removing the molded body after the pressure molding is completed from the
次に、上記した製造方法を、実施例及び比較例を挙げて、本発明を更に具合的に説明する。
まず、各実施例及び各比較例において共通する燃料電池セパレータ用材料ａの構成を説明すると、平均粒子径が５〜５０μm程度の球状または鱗状の黒鉛粉末１００重量部に対し、２０重量部のフェノール樹脂を溶液被覆法によって被覆したものを用いた。このフェノール樹脂の熱硬化開始温度は８０℃程度である。
Next, the present invention will be described more specifically with reference to the above-described production methods, with Examples and Comparative Examples.
First, the structure of the fuel cell separator material “a” common in each example and each comparative example will be described. 20 parts by weight of phenol with respect to 100 parts by weight of spherical or scaly graphite powder having an average particle diameter of about 5 to 50 μm. What coated resin by the solution coating method was used. The thermosetting start temperature of this phenol resin is about 80 ° C.
そして、上記した第１の加温処理工程、成型工程、硬化工程を経て燃料電池セパレータＡを製造するが、このとき、成型温度（金型１と燃料電池セパレータ用材料ａの温度）と、成型圧力（プレス圧）と、黒鉛粉末の形状とを適宜を替えてサンプルとしての燃料電池セパレータＡを製造し、それぞれサンプル数１００において、電気抵抗の不良発生率（電気抵抗不良率：電気抵抗の不合格ラインを、２０ｍΩｃｍ以上とする）と、水素透過の不良率（水素透過不良率：１０−１１ｍｏｌ／ｍ２ｓＰａ以上とする）を算出した。
The fuel cell separator A is manufactured through the first heating process, the molding process, and the curing process described above. At this time, the molding temperature (the temperature of the
なお、この電気抵抗の計測方法は、燃料電池用セパレータを、長さ２００ｍｍ、断面が１ｍｍ四方の供試体に加工し、該供試体を用いて４端子法にて測定を行った。
また、水素透過の計測方法は、ＪＩＳ Ｋ７１２６のＡ法（差圧法）に準じて行い、試料調湿：２３℃、５０％ＲＨ＊４８Ｈｒ以上、測定温度：２３℃、使用ガス種：水素ガス、の条件下で行った。
In this measurement method of electric resistance, a fuel cell separator was processed into a specimen having a length of 200 mm and a cross section of 1 mm square, and measurement was performed by the four-terminal method using the specimen.
Moreover, the measurement method of hydrogen permeation is performed according to A method (differential pressure method) of JIS K7126, sample humidity control: 23 ° C., 50% RH * 48Hr or more, measurement temperature: 23 ° C., gas type used: hydrogen gas, It carried out on condition of this.
実施例１は、黒鉛粉末の形状を球状とし、成型温度を、フェノール樹脂の熱硬化開始温度８０℃以下である６５℃にし、成型圧力を２０ＭＰａとした。その結果、電気抵抗不良率は０．３％、水素透過不良率は０．５％であり、実施例１にかかる条件下によって製造された燃料電池用セパレータは、不良品の発生率が極めて低いことが確認された。 In Example 1, the shape of the graphite powder was spherical, the molding temperature was 65 ° C., which is 80 ° C. or less, the thermosetting temperature of the phenol resin, and the molding pressure was 20 MPa. As a result, the defective rate of electrical resistance is 0.3%, the defective rate of hydrogen permeation is 0.5%, and the fuel cell separator manufactured under the conditions according to Example 1 has a very low incidence of defective products. It was confirmed.
実施例２は、黒鉛粉末の形状を球状とし、成型温度を、フェノール樹脂の熱硬化開始温度８０℃以下である７０℃にし、成型圧力を３０ＭＰａとした。その結果、電気抵抗不良率は０．４％、水素透過不良率は０．４％であり、実施例２にかかる条件下によって製造された燃料電池用セパレータは、不良品の発生率が極めて低いことが確認された。 In Example 2, the shape of the graphite powder was spherical, the molding temperature was set to 70 ° C., which is 80 ° C. or less, the thermosetting temperature of the phenol resin, and the molding pressure was set to 30 MPa. As a result, the failure rate of electrical resistance is 0.4% and the failure rate of hydrogen permeation is 0.4%. The fuel cell separator manufactured under the conditions according to Example 2 has a very low incidence of defective products. It was confirmed.
実施例３は、黒鉛粉末の形状を鱗状とし、成型温度を、フェノール樹脂の熱硬化開始温度８０℃以下である６５℃にし、成型圧力を２０ＭＰａとした。その結果、電気抵抗不良率は０．８％、水素透過不良率は０．７％であり、実施例３にかかる条件下によって製造された燃料電池用セパレータは、不良品の発生率が極めて低いことが確認された。 In Example 3, the shape of the graphite powder was scale-like, the molding temperature was 65 ° C., which is 80 ° C. or less of the thermosetting temperature of the phenol resin, and the molding pressure was 20 MPa. As a result, the electrical resistance failure rate is 0.8% and the hydrogen permeation failure rate is 0.7%, and the fuel cell separator manufactured under the conditions according to Example 3 has a very low incidence of defective products. It was confirmed.
次に、本願発明の条件下から外れたものを比較例として説明する。
［比較例１］
比較例１は、黒鉛粉末の形状を球状とし、成型温度を、フェノール樹脂の熱硬化開始温度８０℃を下方に大きく外れた２５℃にし、成型圧力を２０ＭＰａとした。その結果、電気抵抗不良率は８％、水素透過不良率は１１％であり、比較例１にかかる条件下によって製造された燃料電池用セパレータは、不良品の発生率が極めて高いことが確認された。
Next, what deviated from the conditions of the present invention will be described as a comparative example.
[Comparative Example 1]
In Comparative Example 1, the shape of the graphite powder was spherical, the molding temperature was set to 25 ° C., which was far below the thermosetting start temperature of phenol resin, and the molding pressure was set to 20 MPa. As a result, the failure rate of electrical resistance was 8% and the failure rate of hydrogen permeation was 11%. It was confirmed that the fuel cell separator manufactured under the conditions according to Comparative Example 1 had a very high incidence of defective products. It was.
［比較例２］
比較例２は、従来の熱間プレス工程による製法であり、黒鉛粉末の形状を球状とし、成型温度を、フェノール樹脂の熱硬化開始温度８０℃を上方に大きく外れた１５０℃にし、成型圧力を２０ＭＰａとした。その結果、電気抵抗不良率は１３％、水素透過不良率は０．５％であり、比較例２にかかる条件下によって製造された燃料電池用セパレータは、電気抵抗不良率のみ不良品の発生率が１割を越え、不良品の発生率が極めて高いことが確認された。
[Comparative Example 2]
Comparative Example 2 is a manufacturing method using a conventional hot pressing process, in which the shape of the graphite powder is made spherical, the molding temperature is set to 150 ° C., which is far from the thermosetting start temperature 80 ° C. of the phenol resin, and the molding pressure is set to The pressure was 20 MPa. As a result, the electrical resistance failure rate is 13% and the hydrogen permeation failure rate is 0.5%, and the fuel cell separator manufactured under the conditions according to Comparative Example 2 has only an electrical resistance failure rate and the occurrence rate of defective products. Over 10%, and it was confirmed that the incidence of defective products was extremely high.
［比較例３］
比較例３は、黒鉛粉末の形状を球状とし、成型温度を、フェノール樹脂の熱硬化開始温度８０℃以下である６５℃にし、成型圧力を５ＭＰａとした。その結果、電気抵抗不良率は１５％、水素透過不良率は１３％であり、比較例３にかかる条件下によって製造された燃料電池用セパレータは、電気抵抗不良率、水素透過不良率とも不良品の発生率が１割を越え、不良品の発生率が極めて高いことが確認された。
[Comparative Example 3]
In Comparative Example 3, the shape of the graphite powder was spherical, the molding temperature was 65 ° C., which is 80 ° C. or less, and the molding pressure was 5 MPa. As a result, the electrical resistance failure rate is 15% and the hydrogen permeation failure rate is 13%. The fuel cell separator manufactured under the conditions according to Comparative Example 3 is a defective product in both the electrical resistance failure rate and the hydrogen transmission failure rate. It was confirmed that the rate of occurrence of defects exceeded 10% and the rate of defective products was extremely high.
以上、これら実施例１〜３及び比較例１〜３をまとめると、表１のようになる。 The above Examples 1 to 3 and Comparative Examples 1 to 3 are summarized as shown in Table 1.
以上、本実施の形態及び本実施例にかかる燃料電池セパレータの製造方法と、その製造方法を用いて製造された燃料電池セパレータの不良品発生率を説明したが、上述した実施の形態及び実施例は、本発明の好適な実施の形態の一例を示すものであり、本発明はそれに限定されるものではなく、その要旨を逸脱しない範囲内において、種々変形実施が可能である。 As described above, the manufacturing method of the fuel cell separator according to the present embodiment and the example and the defective product occurrence rate of the fuel cell separator manufactured by using the manufacturing method have been described. These show an example of a preferred embodiment of the present invention, and the present invention is not limited thereto, and various modifications can be made without departing from the scope of the invention.
ａ 燃料電池セパレータ用材料
Ａ 燃料電池セパレータ
１ 金型
２ 加温装置
３ プレス装置
４ 専用炉
a Fuel cell separator material A
Claims (7)
前記燃料電池セパレータ用材料を、前記熱硬化性樹脂が軟化溶融するが硬化しない温度で無加圧で保持する加温処理工程と、
前記加温処理工程の後で前記燃料電池セパレータ用材料を金型を用いて加圧成型する成型工程と、
前記成型工程で成型された成型体を前記熱硬化性樹脂が硬化する温度で無加圧で保持する硬化工程と、
を備えることを特徴とした燃料電池セパレータの製造方法。 A method of manufacturing a fuel cell separator using a fuel cell separator material mainly composed of graphite powder coated with a thermosetting resin,
A heating treatment step of holding the fuel cell separator material without pressure at a temperature at which the thermosetting resin softens and melts but does not cure;
A molding step of pressure-molding the fuel cell separator material using a mold after the heating treatment step;
A curing step of holding the molded body molded in the molding step without pressure at a temperature at which the thermosetting resin is cured;
A method for producing a fuel cell separator, comprising:
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