JP6203931B2 - 電気化学素子 - Google Patents
電気化学素子 Download PDFInfo
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- JP6203931B2 JP6203931B2 JP2016238675A JP2016238675A JP6203931B2 JP 6203931 B2 JP6203931 B2 JP 6203931B2 JP 2016238675 A JP2016238675 A JP 2016238675A JP 2016238675 A JP2016238675 A JP 2016238675A JP 6203931 B2 JP6203931 B2 JP 6203931B2
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- Prior art keywords
- hydrogen
- metal layer
- alloy
- hydrogen discharge
- separator
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Images
Classifications
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Description
前記水素排出膜は、金属層を含み、
前記セパレータは、パルプを含み、石英管燃焼ガス吸収イオンクロマトグラフィ法による全硫黄成分の含有量が400ppm以下であることを特徴とする電気化学素子、に関する。
すなわち硫黄成分は、硫化水素、メチルメルカプタン、硫化メチル、二硫化メチルなどの形態や、セルロース等と直接的に結合した有機硫黄化合物として存在している。セパレータに残留しているこれらの硫黄成分は、チップや原麻等の原料から樹脂(リグニン)を除去してパルプを作製する際の薬剤や、それら薬剤と原料が反応した結果生じたものである。チップや原麻からパルプを作製する方法(蒸解方法)は複数知られており、クラフト法やサルファイト法、ソーダ法などが良く用いられている。前記方法においては、蒸解工程、過酸化水素や酵素などによる脱リグニン工程、及びパルプ中の異物や残留成分を除去するため精選・洗浄工程が行われるが、これらの工程をより厳密に行うことで、セパレータ中の硫黄成分の含有量を低減することができる。
これらのパルプや繊維は、漂白処理されていても良く、また、溶解パルプのように精製されたものや、マーセル化パルプであっても良い。
木材パルプとしては、トウヒ、モミ、マツ、ツガなどの針葉樹、ブナ、ナラ、カバ、ユーカリなどの広葉樹が利用できる。非木材パルプとしては、マニラ麻、サイザル麻、バナナ、パイナップルなどの葉脈繊維、コウゾ、三椏、ガンピ、ジュート、ケナフ、大麻、フラックスなどのジンピ繊維、エスパルト、竹、バガス、稲ワラ、麦ワラ、アシなどの禾本科植物繊維、綿、リンター、カポックなどの種毛繊維、椰子などの果実繊維、その他の植物としてイグサやサバイ草など種々の植物が利用できる。再生セルロース繊維としては、溶剤紡糸再生セルロース繊維が好適に使用できる。これらは単独で使用しても良く、複数種選択して使用しても良い。
無漂白ソーダパルプ、無漂白溶解クラフトパルプ、無漂白溶解サルファイトパルプ、無漂白溶解ソーダパルプ、TCF漂白クラフトパルプ、TCF漂白サルファイトパルプ、TCF漂白ソーダパルプ、TCF漂白溶解クラフトパルプ、TCF漂白溶解サルファイトパルプ、TCF漂白溶解ソーダパルプである。そして、これらのパルプにマーセル化処理が施されていてもよい。
〔圧延法によるPd−Au合金層(Au含有量30mol%)の作製〕
インゴット中のAu含有量が30mol%となるようにPd及びAu原料をそれぞれ秤量し、水冷銅坩堝を備えたアーク溶解炉に投入し、大気圧のArガス雰囲気中でアーク溶解した。得られたボタンインゴットをロール径100mmの2段圧延機を用いて厚さ5mmになるまで冷間圧延して板材を得た。その後、ガラス管の中に圧延した板材を入れ、ガラス管の両端を封止した。ガラス管内部を室温で5×10−4Paまで減圧し、その後700℃まで昇温して24時間放置し、その後室温まで冷却した。この熱処理により、合金中のPd及びAuの偏析を解消した。次に、ロール径100mmの2段圧延機を用いて板材を厚さ100μmになるまで冷間圧延し、さらにロール径20mmの2段圧延機を用いて板材を厚さ20μmになるまで冷間圧延した。その後、ガラス管の中に圧延した板材を入れ、ガラス管の両端を封止した。ガラス管内部を室温で5×10−4Paまで減圧し、その後500℃まで昇温して1時間放置し、その後室温まで冷却した。この熱処理により、圧延によって生じたPd−Au合金内部のひずみを除去し、厚さ20μm、Au含有量30mol%のPd−Au合金層からなる水素排出膜を作製した。
製造例1で作製した水素排出膜、及び全硫黄成分の含有量が34ppmであるクラフト紙をセパレータとして使用してアルミ電解コンデンサを作製した。
製造例1で作製した水素排出膜、及び全硫黄成分の含有量が69ppmであるクラフト紙をセパレータとして使用してアルミ電解コンデンサを作製した。
製造例1で作製した水素排出膜、及び全硫黄成分の含有量が57ppmであるクラフト紙をセパレータとして使用してアルミ電解コンデンサを作製した。
製造例1で作製した水素排出膜、及び全硫黄成分の含有量が110ppmであるクラフト紙をセパレータとして使用してアルミ電解コンデンサを作製した。
製造例1で作製した水素排出膜、及び全硫黄成分の含有量が250ppmであるクラフト紙をセパレータとして使用してアルミ電解コンデンサを作製した。
製造例1で作製した水素排出膜、及び全硫黄成分の含有量が380ppmであるクラフト紙をセパレータとして使用してアルミ電解コンデンサを作製した。
製造例1で作製した水素排出膜、及び全硫黄成分の含有量が480ppmであるクラフト紙をセパレータとして使用してアルミ電解コンデンサを作製した。
製造例1で作製した水素排出膜、及び全硫黄成分の含有量が570ppmであるクラフト紙をセパレータとして使用してアルミ電解コンデンサを作製した。
(石英管燃焼法イオンクロマトグラフィによる全硫黄成分の含有量の測定)
「JIS K0127 『イオンクロマトグラフィー通則』」に従って測定した。なお、試料は「同JIS K0127 6.3.5 有機化合物の燃焼前処理」に記載された、石英管燃焼法よる前処理を行い、発生ガスを吸収液に吸収させて測定に使用した。分析装置は、以下を使用した。
(1)自動試料燃焼装置
装置:三菱化学アナリテック社製「AQF−2100H」
温度:Inlet 1000℃,Outlet 1100℃
ガス流量:O2 400mL/min,Ar/O2200mL/min,Ar(送水ユニット:目盛2) 100mL/min
(2)イオンクロマトグラフ(アニオン)
装置:Thermo Fisher Scientific社製「DX−320」
分離カラム:Dionex IonPac AS15 (4mm×250mm)
ガードカラム:Dionex IonPac AG15 (4mm×50mm)
除去システム:Dionex AERS-500(リサイクルモード)
検出器:電気伝導度検出器
溶離液:KOH水溶液
溶離液流量:1.2mL/min
試料注入量:250μL
製造例1で作製した水素排出膜をスウェージロック社製のVCRコネクターに取り付け、片側にSUSチューブを取り付け、密封された空間(63.5ml)を作製した。チューブ内を真空ポンプで減圧後、水素ガスの圧力が0.15MPaになるように調整し、105℃の環境下での圧力変化をモニターした。圧力変化により水素排出膜を透過した水素モル数(体積)がわかるため、これを1日当たりの透過量に換算して水素透過量を算出した。例えば、2時間で圧力が0.15MPaから0.05MPaに変化した場合(変化量0.10MPa)、水素排出膜を透過した水素体積は63.5mlになる。よって、1日当たりの水素透過量は63.5×24/2=762ml/dayとなる。水素排出膜の水素透過量は、10ml/day以上であることが好ましく、100ml/day以上であることがより好ましい。
密閉されたSUS缶内に、実施例及び比較例で用いたセパレータ50gにエチレングリコールを含浸した試料をそれぞれ入れ、製造例1で作製した水素排出膜(15mm×15mm)をSUS缶の蓋から吊り下げた。105℃で12時間熱処理を行い、試料から発生したガスを水素排出膜の表面に曝露させた。その後、前記と同様の方法で水素透過性の評価を行った。
実施例及び比較例で作製したアルミ電解コンデンサに、雰囲気温度105℃で400Vの電圧印加を500時間行った。その後、アルミ電解コンデンサのアルミケースの変形を目視で確認した。
〇:アルミケースの形状変化なし
×:アルミケースの膨れあり
2:金属層
3:接着剤
4:支持体
5:治具
6:コンデンサ素子
7:陽極箔
8:陰極箔
9:電解紙(セパレータ)
10:リード線
11:封口体
12:ケース
Claims (5)
- 水素排出膜を備えており、かつセパレータを介して陽極と陰極が積層された積層体を有する電気化学素子であって、
前記水素排出膜は、金属層を含み、
前記金属層は、Pd合金を含む合金層であり、
前記セパレータは、パルプを含み、石英管燃焼ガス吸収イオンクロマトグラフィ法による全硫黄成分の含有量が400ppm以下であることを特徴とする電気化学素子。 - 前記Pd合金は、第11族元素を20〜65mol%含む請求項1記載の電気化学素子。
- 前記第11族元素は、Au、Ag、及びCuからなる群より選択される少なくとも1種である請求項2記載の電気化学素子。
- 前記水素排出膜は、金属層の片面又は両面に支持体を有する請求項1〜3のいずれかに記載の電気化学素子。
- 前記電気化学素子が、アルミ電解コンデンサ又はリチウムイオン電池である請求項1〜4のいずれかに記載の電気化学素子。
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