JP2018080351A - Silver plated stainless steel and separator for use in fuel cell - Google Patents

Silver plated stainless steel and separator for use in fuel cell Download PDF

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JP2018080351A
JP2018080351A JP2016221486A JP2016221486A JP2018080351A JP 2018080351 A JP2018080351 A JP 2018080351A JP 2016221486 A JP2016221486 A JP 2016221486A JP 2016221486 A JP2016221486 A JP 2016221486A JP 2018080351 A JP2018080351 A JP 2018080351A
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stainless steel
silver
plating film
thickness
nickel
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JP6850987B2 (en
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秋草　順
Jun Akikusa
順 秋草
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Mitsubishi Materials Corp
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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
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    • Y02E60/50—Fuel cells

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Abstract

PROBLEM TO BE SOLVED: To provide silver plated stainless steel having an improved electroconductivity under a high temperature oxidative atmosphere, and a separator for use in a fuel cell.SOLUTION: The silver plated stainless steel composed of ferritic stainless steel base metal, a nickel plating film formed at least on a part of the ferritic stainless steel base metal, and a silver plating film formed to cover the nickel plating film, is characterized in that the thickness (dA) of the silver plating film is at least 1 μm and the ratio of the thickness (dN) of the nickel plating film relative to the thickness (dA) of the silver plating film (dN/dA) is from 0.5 to 1.5.SELECTED DRAWING: None

Description

本発明は、銀めっき被覆ステンレス鋼材及び燃料電池用セパレータに関し、詳細には下地ニッケルめっき膜の厚みが、銀めっき膜の厚みに対して所定の範囲内である銀めっき被覆ステンレス鋼材に関する。   The present invention relates to a silver plating coated stainless steel material and a fuel cell separator, and more particularly to a silver plating coated stainless steel material in which the thickness of a base nickel plating film is within a predetermined range with respect to the thickness of the silver plating film.

ステンレス鋼材は表面に酸化皮膜を有するため、耐食性、耐酸化性に優れる。しかし、酸化皮膜は半田付け性が極めて悪い。そこで、ステンレス鋼材を電気・電子部品として使用する際には、通常、銀めっきが施される。その際、銀めっき膜のステンレス鋼材への密着性を高めるために、下地としてニッケルめっきが施される。   Since the stainless steel material has an oxide film on the surface, it is excellent in corrosion resistance and oxidation resistance. However, the oxide film has extremely poor solderability. Therefore, when stainless steel is used as an electrical / electronic component, silver plating is usually applied. In that case, in order to improve the adhesiveness of the silver plating film to the stainless steel material, nickel plating is applied as a base.

ステンレス鋼材としてフェライト系ステンレス鋼を用い、該フェライト系ステンレス鋼にニッケルめっきを施した上に銀めっきを施すことにより、高温酸化雰囲気下で使用されても表面が酸化されることがなく、良好な導電性を示す銀めっき被覆フェライト系ステンレス鋼材が知られている（特許文献１）。   Ferritic stainless steel is used as a stainless steel material, and the surface of the ferritic stainless steel is nickel-plated and then silver-plated, so that the surface is not oxidized even when used in a high-temperature oxidizing atmosphere. A silver plating coated ferritic stainless steel material showing electrical conductivity is known (Patent Document 1).

特許第３９１８６１１号Japanese Patent No. 3918611

特許文献１記載の銀めっき被覆フェライト系ステンレス鋼材は、５００℃以上の温度の高温酸化雰囲気に曝された場合であっても良好な導電性等の特性を示すものの、さらなる導電性の向上が求められている。そこで、本発明は高温酸化雰囲気下での導電性をより向上することができる銀めっき被覆ステンレス鋼材及び燃料電池用セパレータを提供することを目的とする。   Although the silver plating coated ferritic stainless steel material described in Patent Document 1 exhibits good conductivity and the like even when exposed to a high-temperature oxidizing atmosphere at a temperature of 500 ° C. or higher, further improvement in conductivity is required. It has been. Therefore, an object of the present invention is to provide a silver-plated coated stainless steel material and a fuel cell separator that can further improve the conductivity in a high-temperature oxidizing atmosphere.

導電性を向上すべく本発明者らが種々検討したところ、下地ニッケルめっき膜の厚みを、銀めっき膜の厚みとほぼ同程度に厚くすることによって、耐高温酸化性が著しく向上することが見出された。即ち、本発明の銀めっき被覆ステンレス鋼材の第１の観点は、フェライト系ステンレス鋼母材、前記フェライト系ステンレス鋼母材の少なくとも一部上に施与されたニッケルめっき膜、及び前記ニッケルめっき膜を覆って施与された銀めっき膜、からなる銀めっき被覆ステンレス鋼材であって、前記銀めっき膜の厚み（ｄＡ）が１μｍ以上であり、前記銀めっき膜の厚み（ｄＡ）に対する前記ニッケルめっき膜の厚み（ｄＮ）の比（ｄＮ／ｄＡ）が０．５〜１．５であることを特徴とする。   As a result of various studies by the present inventors in order to improve the conductivity, it was found that the high temperature oxidation resistance is remarkably improved by increasing the thickness of the underlying nickel plating film to approximately the same as the thickness of the silver plating film. It was issued. That is, the first aspect of the silver-plated coated stainless steel material of the present invention is a ferritic stainless steel base material, a nickel plated film applied on at least a part of the ferritic stainless steel base material, and the nickel plated film A silver-plated coated stainless steel material coated with a silver-plated film, wherein the silver-plated film has a thickness (dA) of 1 μm or more, and the nickel-plated with respect to the thickness of the silver-plated film (dA) The film thickness (dN) ratio (dN / dA) is 0.5 to 1.5.

本発明の銀めっき被覆ステンレス鋼材の第２の観点は、第１の観点に基づく発明であって、前記ｄＡが５〜１０μｍであり、且つ、ｄＮ／ｄＡが０．８〜１．２であることを特徴とする。   The 2nd viewpoint of the silver plating coating stainless steel material of this invention is invention based on a 1st viewpoint, Comprising: Said dA is 5-10 micrometers, and dN / dA is 0.8-1.2. It is characterized by that.

本発明の第３の観点は、第１又は第２の観点に基づく銀めっき被覆ステンレス鋼材で構成された燃料電池用セパレータであることを特徴とする。   A third aspect of the present invention is a fuel cell separator composed of a silver-plated coated stainless steel material based on the first or second aspect.

本発明の第１の観点は、従来、銀めっき膜厚よりも薄いニッケルめっき膜厚を銀めっき膜厚とほぼ同程度に厚くし、それによって、高温酸化雰囲気下で長時間維持した後であっても比電気抵抗値の増加が少なく、優れた導電性を示すという効果を奏する。該銀めっき被覆ステンレス鋼材は、耐高温酸化性が要求される導電部材としての用途は勿論のこと、高温での金属光沢を利用した加熱炉部材としても有用である。   The first aspect of the present invention is that after a nickel plating film thickness that is thinner than the silver plating film thickness is increased to about the same as the silver plating film thickness, thereby maintaining it for a long time in a high-temperature oxidizing atmosphere. However, there is little increase in the specific electric resistance value, and there is an effect that excellent conductivity is exhibited. The silver-plated coated stainless steel material is useful not only as a conductive member that requires high-temperature oxidation resistance, but also as a heating furnace member utilizing metallic luster at a high temperature.

本発明の第２の観点は、ニッケルめっき膜厚を銀めっき膜厚と略同じにすることによって、高温酸化雰囲気下で長時間維持した後の比電気抵抗値の増加を大きく抑制するという効果を奏する。   The second aspect of the present invention has the effect of largely suppressing an increase in specific resistance value after maintaining for a long time in a high-temperature oxidizing atmosphere by making the nickel plating film thickness substantially the same as the silver plating film thickness. Play.

本発明の第３の観点は、上記第１又は第２の観点の銀めっき被覆ステンレス鋼材で構成された燃料電池用セパレータであり、優れた耐熱性を示す。   The 3rd viewpoint of this invention is the separator for fuel cells comprised with the silver plating coating | coated stainless steel material of the said 1st or 2nd viewpoint, and shows the outstanding heat resistance.

本実施形態において、母材のフェライト系ステンレス鋼としては、フェライト系であれば任意の組成のステンレス鋼を用いることができる。例えば、ＳＵＳ４３０、ＳＵＳ４３０をベースに種々の元素が添加又は低下されたステンレス鋼、例えばＴｉを含むＳＵＨ４０９、Ａｌを含むＳＵＳ４０５、Ｓを含むＳＵＳ４３０Ｆ、Ｍｏを含むＳＵＳ４３４、Ｃが低減されたＳＵＳ４１０Ｌ、Ｃｒが低減されたＳＵＳ４２９等が挙げられる。これらのうち、精密加工性に優れ安価であることから、ＳＵＳ４３０が好ましい。   In the present embodiment, as the ferritic stainless steel of the base material, stainless steel having an arbitrary composition can be used as long as it is ferritic. For example, SUS430, stainless steel with various elements added or reduced based on SUS430, for example, SUH409 containing Ti, SUS405 containing Al, SUS430F containing S, SUS434 containing Mo, SUS410L with reduced C, Cr For example, reduced SUS429. Of these, SUS430 is preferable because it is excellent in precision workability and inexpensive.

ニッケルめっき膜は、フェライト系ステンレス鋼母材の少なくとも一部、例えば電気接点部位、に施与されている。ニッケルめっき膜は、電解めっき膜、無電解めっき膜のいずれであってよい。厚み制御がし易い点で、電解めっき膜であることが好ましい。   The nickel plating film is applied to at least a part of the ferritic stainless steel base material, for example, an electrical contact portion. The nickel plating film may be either an electrolytic plating film or an electroless plating film. In terms of easy thickness control, an electrolytic plating film is preferable.

銀めっき膜は、ニッケルめっき膜を覆って施与されている。銀めっき膜は、電解めっき膜、無電解めっき膜のいずれであってよく、好ましくは電解めっき膜である。銀めっき膜は、その厚み（ｄＡ）が少なくとも１μｍであり、好ましくは少なくとも５μｍである。ｄＡが１μｍ未満では、高温酸化性雰囲気中で十分な導電性を達成することが難しい。ｄＡの上限値については特に制限は無いが、コスト等の点で１０μｍ程度であるのが一般的である。但し、銀の融点（９６０℃）に近い程の高温環境下で使用する場合は、できるだけ厚くすることが好ましい。   The silver plating film is applied over the nickel plating film. The silver plating film may be either an electrolytic plating film or an electroless plating film, and is preferably an electrolytic plating film. The silver plating film has a thickness (dA) of at least 1 μm, preferably at least 5 μm. If dA is less than 1 μm, it is difficult to achieve sufficient conductivity in a high-temperature oxidizing atmosphere. Although there is no restriction | limiting in particular about the upper limit of dA, Generally it is about 10 micrometers in terms of cost etc. However, when used in a high temperature environment close to the melting point of silver (960 ° C.), it is preferable to make it as thick as possible.

本実施形態の銀めっき被覆ステンレス鋼材は、ニッケルめっき膜の厚み（ｄＮ）と銀めっき膜の厚み（ｄＡ）の比（ｄＮ／ｄＡ）が０．５〜１．５であることを特徴とする。該範囲内においては、銀めっき被覆ステンレス鋼材が高温（５００℃〜９６０℃）の酸化雰囲気に長時間（１００〜１０００時間）曝された後であっても、比電気抵抗値の初期比電気抵抗値に対する上昇率が１４％以下、好ましくは１２％以下である。好ましくはｄＮ／ｄＡが０．７〜１．３であり、より好ましくは０．８〜１．２である。   The silver-plated coated stainless steel material of this embodiment is characterized in that the ratio (dN / dA) of the thickness (dN) of the nickel plating film to the thickness (dA) of the silver plating film is 0.5 to 1.5. . Within this range, even after the silver-plated coated stainless steel material has been exposed to an oxidizing atmosphere at a high temperature (500 ° C. to 960 ° C.) for a long time (100 to 1000 hours), the initial specific electric resistance of the specific electric resistance value The rate of increase with respect to the value is 14% or less, preferably 12% or less. Preferably dN / dA is 0.7 to 1.3, more preferably 0.8 to 1.2.

より好ましくは、ｄＡが５〜１０μｍであり、且つ、ｄＮ／ｄＡが０．８〜１．２である。   More preferably, dA is 5 to 10 μm and dN / dA is 0.8 to 1.2.

本実施形態において、めっき膜の厚みの測定方法は特に限定されず、例えばＪＩＳ Ｈ ８５０１：１９９９に定められている電解式試験法、蛍光Ｘ線式試験法、走査電子顕微鏡試験方法に準じて行うことができる。本発明では、試験片の断面を切り出し、ＥＰＭＡ（電子線マイクロアナライザー）により測定した。   In the present embodiment, the method for measuring the thickness of the plating film is not particularly limited, and is performed according to, for example, an electrolytic test method, a fluorescent X-ray test method, and a scanning electron microscope test method defined in JIS H 8501: 1999. be able to. In the present invention, a cross section of the test piece was cut out and measured with an EPMA (electron beam microanalyzer).

本実施形態の銀めっき被覆ステンレス鋼材の用途としては、高温酸化雰囲気下における耐酸化性及び導電性が必要とされる用途、例えば、燃料電池のセパレータ又は電流取り出し端子、及び高温用導線等が挙げられる。また、銀めっき被覆ステンレス鋼材は、高温雰囲気下においても金属光沢を維持することから、高温雰囲気における輻射熱を利用する用途、例えば、加熱炉又は配管の内壁等にも使用できる。   Applications of the silver-plated coated stainless steel material of the present embodiment include applications that require oxidation resistance and conductivity in a high-temperature oxidizing atmosphere, such as fuel cell separators or current extraction terminals, and high-temperature conductors. It is done. Further, since the silver plating coated stainless steel material maintains the metallic luster even in a high temperature atmosphere, it can be used for applications utilizing radiant heat in a high temperature atmosphere, for example, the inner wall of a heating furnace or piping.

本実施形態の銀めっき被覆ステンレス鋼材は、定法に従い作ることができる。例えば、フェライト系ステンレス鋼母材に、脱脂、活性化等の前処理を施した後、ニッケルめっきを施す。ニッケルめっきは、上述のように電解めっき、例えばウッド浴、ワット浴、黒色ニッケルめっき浴、又はスルファミン酸浴で行うことが好ましい。次いで、ニッケルめっきされたフェライト系ステンレス鋼母材を水洗した後、シアン浴にて銀めっきを施し、水洗、乾燥を行う。めっき膜厚の制御は、めっき電流密度とめっき時間によって行うことができる。   The silver-plated coated stainless steel material of this embodiment can be made according to a regular method. For example, a pretreatment such as degreasing and activation is performed on a ferritic stainless steel base material, and then nickel plating is performed. The nickel plating is preferably performed by electrolytic plating as described above, for example, a wood bath, a watt bath, a black nickel plating bath, or a sulfamic acid bath. Next, the nickel-plated ferritic stainless steel base material is washed with water, then silver-plated in a cyan bath, washed with water and dried. The plating film thickness can be controlled by the plating current density and the plating time.

以下、本発明を実施例により説明するが、本発明はこれらの実施例に限定されるものではない。
［実施例１〜９及び比較例１〜６］
ＳＵＳ４３０製の金属母材の表面に、表１〜３に示す厚みのニッケルめっき膜と銀めっき膜を形成した。
先ず、ＳＵＳ４３０から、幅２０×長さ４０×厚み２ｍｍの板状の試験片を切り出した。該金属母材の組成は以下のとおりである：
ＳＵＳ４３０：Ｃｒ１８ｗｔ％、Ｃ（炭素）０．１２ｗｔ％以下、Ｓi０．７５ｗｔ％以下、Ｍｎ１．０ｗｔ％以下、Ｐ（リン）０．０４ｗｔ％以下、Ｓ（硫黄）０．０３ｗｔ％以下、残Ｆｅおよび不可避不純物。 EXAMPLES Hereinafter, although an Example demonstrates this invention, this invention is not limited to these Examples.
[Examples 1 to 9 and Comparative Examples 1 to 6]
A nickel plating film and a silver plating film having thicknesses shown in Tables 1 to 3 were formed on the surface of a metal base material made of SUS430.
First, a plate-shaped test piece having a width of 20 × length of 40 × thickness of 2 mm was cut out from SUS430. The composition of the metal matrix is as follows:
SUS430: Cr 18 wt%, C (carbon) 0.12 wt% or less, Si 0.75 wt% or less, Mn 1.0 wt% or less, P (phosphorus) 0.04 wt% or less, S (sulfur) 0.03 wt% or less, residual Fe and Inevitable impurities.

試験片の全表面上に、表１〜３に示す厚みのニッケル（ｄＮ）めっき、次いで銀（ｄＡ）めっき膜を形成した。同じめっき条件で３試験片ずつめっきし、夫々について厚み及び初期比電気抵抗値を測定して平均を求めた。   A nickel (dN) plating having a thickness shown in Tables 1 to 3 and then a silver (dA) plating film was formed on the entire surface of the test piece. Three test pieces were plated under the same plating conditions, and the thickness and initial specific electric resistance value were measured for each to determine the average.

＜ニッケルめっきの条件＞
ニッケルめっきは、塩化ニッケルを２４０ｇ／L、及び塩酸を１２５ｍＬ／Lで含むウッド浴を用い、２５℃において、電流密度５Ａ／ｄｍ２の条件で実施した。その後、蒸留水で良く洗浄し、乾燥した。 <Nickel plating conditions>
Nickel plating was performed using a wood bath containing 240 g / L of nickel chloride and 125 mL / L of hydrochloric acid at 25 ° C. under a current density of 5 A / dm 2 . Thereafter, it was thoroughly washed with distilled water and dried.

＜銀めっきの条件＞
銀めっきは、シアン化銀カリウム２ｇ／Ｌ、及びシアン化ナトリウムを１００ｇ／Ｌで含む浴を用い、２５℃において、電流密度２Ａ／ｄｍ２の条件で実施した。その後、蒸留水で良く洗浄し、乾燥した。 <Conditions for silver plating>
Silver plating was performed using a bath containing 2 g / L of potassium silver cyanide and 100 g / L of sodium cyanide at 25 ° C. under a current density of 2 A / dm 2 . Thereafter, it was thoroughly washed with distilled water and dried.

＜めっき膜厚測定法＞
蛍光Ｘ線装置（日本電子社製）を用いてめっき表面の膜厚を測定した。 <Plating film thickness measurement method>
The film thickness of the plating surface was measured using a fluorescent X-ray apparatus (manufactured by JEOL Ltd.).

＜電気抵抗値の測定法＞
ミリオームメータ（ソーラートロン社製）を用いて、２枚の白金メッシュ（面積１ｃｍ２）に試験片を挟み、５ｋｇｆの荷重をかけて面積被抵抗値（ｍΩ・ｃｍ２）を測定した。
＜耐高温酸化性試験＞
得られた各試験片を、８００℃の空気雰囲気下において、１０００時間保持した後に比電気抵抗値を測定し、初期比電気抵抗値からの上昇率ΔＲ（％）を求めた。結果を表１〜３に示す。 <Measurement method of electrical resistance value>
A test piece was sandwiched between two platinum meshes (area: 1 cm 2 ) using a mirium meter (manufactured by Solartron), and an area resistance value (mΩ · cm 2 ) was measured by applying a load of 5 kgf.
<High temperature oxidation resistance test>
Each of the obtained test pieces was held in an air atmosphere at 800 ° C. for 1000 hours, and then the specific electric resistance value was measured to obtain the rate of increase ΔR (%) from the initial specific electric resistance value. The results are shown in Tables 1-3.

Figure 2018080351
Figure 2018080351

Figure 2018080351
Figure 2018080351

Figure 2018080351
Figure 2018080351

上表に示す通り、ｄＮ／ｄＡが本発明の範囲であるものは、比電気抵抗値の上昇率ΔＲ（％）が少なく、導電性に優れていた。特に、実施例５及び８については、ΔＲ（％）が４％以下という極めて優れた導電性を示した。

As shown in the above table, those having dN / dA within the range of the present invention had a small increase rate ΔR (%) in specific electric resistance value and were excellent in conductivity. In particular, Examples 5 and 8 exhibited extremely excellent conductivity with ΔR (%) of 4% or less.

Claims (3)

フェライト系ステンレス鋼母材、
前記フェライト系ステンレス鋼母材の少なくとも一部上に施与されたニッケルめっき膜、及び
前記ニッケルめっき膜を覆って施与された銀めっき膜、
からなる銀めっき被覆ステンレス鋼材であって、
前記銀めっき膜の厚み（ｄＡ）が１μｍ以上であり、
前記銀めっき膜の厚み（ｄＡ）に対する前記ニッケルめっき膜の厚み（ｄＮ）の比（ｄＮ／ｄＡ）が０．５〜１．５であることを特徴とする銀めっき被覆ステンレス鋼材。 Ferritic stainless steel base material,
A nickel plating film applied on at least a part of the ferritic stainless steel base material; and a silver plating film applied over the nickel plating film;
A silver-plated coated stainless steel material comprising:
The silver plating film has a thickness (dA) of 1 μm or more,
A ratio of the thickness (dN) of the nickel plating film to the thickness (dA) of the silver plating film (dN / dA) is 0.5 to 1.5. 前記ｄＡが５〜１０μｍであり、且つ、ｄＮ／ｄＡが０．８〜１．２であることを特徴とする請求項１記載の銀めっき被覆ステンレス鋼材。   2. The silver-plated coated stainless steel material according to claim 1, wherein the dA is 5 to 10 μm and the dN / dA is 0.8 to 1.2. 請求項１又は２記載の銀めっき被覆ステンレス鋼材で構成されたことを特徴とする燃料電池用セパレータ。


A fuel cell separator comprising the silver-plated coated stainless steel material according to claim 1 or 2.


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Citations (4)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
JPS6123789A (en) * 1984-07-09 1986-02-01 Furukawa Electric Co Ltd:The Method for plating stainless steel with noble metal
JP2002216807A (en) * 2000-11-16 2002-08-02 Mitsubishi Materials Corp Air electrode collector for solid electrolyte type fuel cell
JP2003328156A (en) * 2002-05-09 2003-11-19 Mitsubishi Materials Corp High temperature heat-resistant member
JP2011216277A (en) * 2010-03-31 2011-10-27 Mitsubishi Materials Corp Solid oxide fuel cell

Patent Citations (4)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
JPS6123789A (en) * 1984-07-09 1986-02-01 Furukawa Electric Co Ltd:The Method for plating stainless steel with noble metal
JP2002216807A (en) * 2000-11-16 2002-08-02 Mitsubishi Materials Corp Air electrode collector for solid electrolyte type fuel cell
JP2003328156A (en) * 2002-05-09 2003-11-19 Mitsubishi Materials Corp High temperature heat-resistant member
JP2011216277A (en) * 2010-03-31 2011-10-27 Mitsubishi Materials Corp Solid oxide fuel cell

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