JP5695928B2 - 櫛型電極の製造方法 - Google Patents
櫛型電極の製造方法 Download PDFInfo
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- JP5695928B2 JP5695928B2 JP2011028228A JP2011028228A JP5695928B2 JP 5695928 B2 JP5695928 B2 JP 5695928B2 JP 2011028228 A JP2011028228 A JP 2011028228A JP 2011028228 A JP2011028228 A JP 2011028228A JP 5695928 B2 JP5695928 B2 JP 5695928B2
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- 238000007740 vapor deposition Methods 0.000 description 1
- 238000004804 winding Methods 0.000 description 1
- 150000003739 xylenols Chemical class 0.000 description 1
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Description
本発明は、以上のような状況に鑑みてなされたものであり、微細な形状である集電体の表面に、精度良く、多量の活物質を担持させることのできる櫛型電極の製造方法を提供することを目的とする。
(1)エポキシ基を有する化合物及びカチオン重合開始剤を含むカチオン重合系レジスト組成物
(2)ノボラック樹脂及び感光剤を含むノボラック系レジスト組成物
(3)酸解離性の脱離基を有し、当該脱離基が露光により光酸発生剤から発生する酸の作用で脱離することによりアルカリ可溶性が増大する樹脂、及び光酸発生剤を含む化学増幅系レジスト組成物
(4)エチレン性の不飽和結合を有するモノマー及び/又は樹脂、並びにラジカル重合開始剤を含み、エチレン性の不飽和結合を有するモノマーを含む場合には、当該モノマーの1分子中に含まれるエチレン性の不飽和結合が3個以下であるラジカル重合系レジスト組成物
櫛型電極1aと櫛型電極1bとの間には、空間又は両者を隔離するセパレータ(図示せず)が設けられ、両者が電気的に分離される。櫛型電極1a及び1bは、表面が不導体である基材4の表面に形成される。このような基材4としては、表面に酸化膜を有するシリコン基板が例示される。
集電体形成工程は、図2(a)から(f)で順次示される工程である。
この工程では、まず、基材4の表面に薄膜の導電層2が形成される(図2(a)〜(b))。基材4は、不導体又は少なくとも表面に不導体の層が形成された導体若しくは半導体であり、例えば、表面に酸化膜を有するシリコン基板が例示される。導電層2は、導体であり、好ましくは金属の薄膜である。基材4の表面に導電層2を形成させるには、PVD法又はCVD法のような蒸着法、スパッタ法、めっき法、金属箔接着法等、各種公知の方法を使用することができる。導電層2の厚さは、櫛型電極1a及び1bに要求される性能を考慮して適宜決定すればよい。
次に、レジスト塗布工程について説明する。レジスト塗布工程は、上記集電体形成工程の後に行われる工程であり、図2(g)で示される工程である。
この工程では、上記集電体形成工程で形成された集電体2a及び2bの部分を含む基材4の表面に、レジスト組成物を塗布してレジスト層6を形成させる。
次に、ガイド孔形成工程について説明する。ガイド孔形成工程は、上記レジスト塗布工程の後に行われる工程であり、図2(h)で示される工程である。なお、図2(h)では、図面の見易さを考慮して、ガイド孔7aの底部に存在する集電体2aを省略した。
本実施態様では、この工程において、上記レジスト塗布工程で形成されたレジスト層6に、櫛型形状である集電体2a及び2bと平面視で同一形状となる形状のガイド孔7a及び7bを形成させる。ガイド孔7a及び7bは、集電体2a及び2bの表面までレジスト層6を貫通する貫通孔として形成される。ガイド孔7a及び7bは、後に説明する活物質層形成工程において、正極又は負極活物質を堆積させるための鋳型として使用される。
次に、活物質層形成工程について説明する。活物質層形成工程は、上記ガイド孔形成工程の後に行われる工程であり、図2(i)で示される工程である。
この工程では、上記ガイド孔形成工程で形成されたガイド孔7a及び7bを鋳型として、集電体2aの表面に正極活物質層3aを、集電体2bの表面に負極活物質層3bをそれぞれ形成させる。これにより、櫛型電極1a及び1bが完成する。
クレゾール型ノボラック樹脂(m−クレゾール:p−クレゾール=6:4(質量比)、質量平均分子量20000)48質量部と、p−ヒドロキシスチレン及びスチレンの共重合体(ヒドロキシスチレン:スチレン=85:15(質量比)、質量平均分子量2500)12質量部と、アクリル酸1−エチルシクロヘキシル、ブチルアクリレート、アクリル酸及び2−メトキシエチルアクリレートの共重合体(組成比10:2:1:8(質量比)、質量平均分子量250000)40質量%と、光酸発生剤として、[2−(プロピルスルホニルオキシイミノ)−2,3−ジヒドロチオフェン−3−イリデン](o−トリル)アセトニトリル(IRGACURE PAG103(商品名)、チバスペシャリティケミカルズ社製)1質量部と、トリエタノールアミン0.1質量部とに対して、溶剤としてプロピレングリコールモノメチルエーテルアセテート(PGMEA)を固形分濃度が40質量%になるように添加してから、混合して溶解させ、実施例1のレジスト組成物とした。実施例1のレジスト組成物は、化学増幅系であり、ポジ型である。
クレゾール型ノボラック樹脂(m−クレゾール:p−クレゾール=6:4(質量比)、質量平均分子量30000)70質量部と、感光剤として1,4−ビス(4−ヒドロキシフェニルイソプロピリデニル)ベンゼンのナフトキノン−1,2−ジアジド−5−スルホン酸ジエステル15質量部と、可塑剤としてポリメチルビニルエーテル(質量平均分子量100000)15質量部とに対して、溶剤としてPGMEAを固形分濃度が40質量%になるように添加してから、混合して溶解させ、実施例2のレジスト組成物とした。実施例2のレジスト組成物は、ノボラック系であり、ポジ型である。
8官能ビスフェノールAノボラック型エポキシ樹脂(ジャパンエポキシレジン株式会社製、製品名jER157S70)100質量部と、カチオン重合開始剤として4−(2−クロロ−4−ベンゾイルフェニルチオ)フェニルビス(4−フルオロフェニル)スルホニウムヘキサフルオロアンチモネート(株式会社ADEKA製、SP−172)3質量部と、増感剤として1−ナフトール1質量部と、3−グリシドキシプロピルトリメトキシシラン5質量部とに対して、溶剤としてPGMEAを固形分濃度が70質量になるように添加してから、混合して溶解させ、実施例3のレジスト組成物とした。実施例3のレジスト組成物は、カチオン重合系であり、ネガ型である。
樹脂固形分に換算して100質量部のベンジルメタクリレート:メタクリル酸の質量比が80:20の共重合体(質量平均分子量80000、50質量%メチルエチルケトン溶液)と、二官能性モノマーとしてエトキシ化ビスフェノールAジメタクリレート(新中村化学工業株式会社製、製品名BPE500)と、ラジカル重合開始剤として2,4−ジエチルチオキサントン(日本化薬株式会社製、製品名DETX−S)3.5質量部と、を混合して溶解させ、実施例4のレジスト組成物とした。実施例4のレジスト組成物は、ラジカル重合系であり、ネガ型である。
3,4−エポキシシクロヘキシルメチルメタクリレート:スチレン:3−トリメトキシシリルプロピルメタクリレート=60:35:5(質量比)の共重合体(質量平均分子量45000)40質量部と、ラジカル重合開始剤(チバスペシャリティケミカルズ社製、製品名CGI−242)2質量部と、3−メタクリロキキシプロピルトリメトキシシラン10質量部と、6官能モノマーとしてジペンタエリスリトールヘキサアクリレート(製品名:DPHA、ダイセルサイテック社製)50質量部と、重合禁止剤として1,5−ジヒドロキシナフタレンを0.8質量部とに対して、溶剤としてPGMEAを固形分濃度が50質量%になるように添加してから、混合して溶解させ、比較例1のレジスト組成物とした。比較例1のレジスト組成物は、ラジカル重合系であり、ネガ型である。
[試験例1]
5インチのシリコンウェーハの表面にスパッタ法によって厚さ500nmの銅の層を形成させた。その後、形成させた銅の層の表面に実施例1のレジスト組成物を塗布し、レジスト組成物に含まれていた溶剤を蒸発させ、厚さ20μmのレジスト層を形成させた。このレジスト層にマスクを通して、紫外線(ghi混合線、300mJ/cm2)を照射し、次いでアルカリ現像液で現像し、純水で洗浄した。これを試験例1の試験片とした。
5インチのシリコンウェーハの表面にスパッタ法によって厚さ500nmの銅の層を形成させた。その後、形成させた銅の層の表面に実施例2のレジスト組成物を塗布し、レジスト組成物に含まれていた溶剤を蒸発させ、厚さ20μmのレジスト層を形成させた。このレジスト層にマスクを通して、紫外線(ghi混合線、3000mJ/cm2)を照射し、次いでアルカリ現像液で現像し、純水で洗浄した。これを試験例2の試験片とした。
5インチのシリコンウェーハの表面にスパッタ法によって厚さ500nmの銅の層を形成させた。その後、形成させた銅の層の表面に実施例2のレジスト組成物を塗布し、レジスト組成物に含まれていた溶剤を蒸発させ、厚さ20μmのレジスト層を形成させた。このレジスト層にマスクを通して、紫外線(ghi混合線、3000mJ/cm2)を照射し、次いでアルカリ現像液で現像し、純水で洗浄した。その後、得られた樹脂パターンにアフターキュアとして、紫外線(ghi混合線)を10分間照射した。これを試験例3の試験片とした。
5インチのシリコンウェーハの表面にスパッタ法によって厚さ500nmの銅の層を形成させた。その後、形成させた銅の層の表面に実施例3のレジスト組成物を塗布し、レジスト組成物に含まれていた溶剤を蒸発させ、厚さ20μmのレジスト層を形成させた。このレジスト層にマスクを通して、紫外線(ghi混合線、300mJ/cm2)を照射し、次いでアルカリ現像液で現像し、純水で洗浄した。これを試験例4の試験片とした。
5インチのシリコンウェーハの表面にスパッタ法によって厚さ500nmの銅の層を形成させた。その後、形成させた銅の層の表面に実施例4のレジスト組成物を塗布し、レジスト組成物に含まれていた溶剤を蒸発させ、厚さ20μmのレジスト層を形成させた。このレジスト層にマスクを通して、紫外線(ghi混合線、300mJ/cm2)を照射し、次いでアルカリ現像液で現像し、純水で洗浄した。これを試験例5の試験片とした。
5インチのシリコンウェーハの表面にスパッタ法によって厚さ500nmの銅の層を形成させた。その後、形成させた銅の層の表面に比較例1のレジスト組成物を塗布し、レジスト組成物に含まれていた溶剤を蒸発させ、厚さ20μmのレジスト層を形成させた。このレジスト層にマスクを通して、紫外線(ghi混合線、300mJ/cm2)を照射し、次いでアルカリ現像液で現像し、純水で洗浄した。これを比較試験例1の試験片とした。
試験例1〜5及び比較試験例1の試験片のそれぞれについて、形成された樹脂パターンを顕微鏡で観察し、残渣の有無を調べた。そして、観察の結果、残渣の無いものをパターニング性良好(○)とし、残渣の存在するものをパターニング性不良(×)として評価した。その結果を表1に示す。
めっき液(EEJA社製、Microfab Au100)を用意し、試験例1〜5及び比較試験例1の試験片のそれぞれについて、用意しためっき液に60℃で30分間浸漬した。その後、試験片の表面の樹脂パターンを顕微鏡で観察し、めっき液への浸漬による樹脂パターンのクラックの発生の有無を調べた。評価は、クラックの発生の無いものをめっき液耐性良好(○)とし、クラックの発生の有るものをめっき液耐性不良(×)とした。その結果を表1に示す。
評価溶剤として、純水、メタノール、エタノール、イソプロピルアルコール(IPA)、プロピレングリコール(PG)、ジブチルエーテル(DBE)、アセトニトリル、トルエン及びm−キシレンを用意した。これらの評価溶剤のそれぞれを使用して、以下の方法で溶剤耐性評価を行った。なお、試験例5及び比較試験例1については、先のめっき液耐性試験が良好でなかったため、溶剤耐性試験を行わなかった。
1)試験例1〜4のそれぞれについて、室温にて、形成させた樹脂パターンの表面に評価溶剤をスポイトで1〜2滴滴下した。
2)純水及びプロピレングリコール以外の溶剤は、滴下後、自然乾燥にて溶剤を除去した。プロピレングリコールは、滴下してから5分後に純水で洗浄し、窒素ブローにより風乾した。純水は、滴下してから5分後に窒素ブローにより風乾した。
3)溶剤を除去した後の樹脂パターンの表面を金属顕微鏡にて観察し、樹脂パターンの膜べりが観察されないものを溶剤耐性良好(○)とし、樹脂パターンの膜べりが観察されたものを溶剤耐性不良(×)とした。その結果を表1に示す。
試験例3及び4でめっき液耐性及び溶剤耐性が良好だったので、これらの試験例で使用した実施例2又は3のレジスト組成物を使用して櫛型電極を作製した。なお、この櫛型電極は、上述した本発明の櫛型電極の製造方法の第一実施態様によるものとした。
まず、5インチのシリコンウェーハの表面にスパッタ法によりチタン及び金の膜をそれぞれ50及び100nm順次形成させた。次に、形成させた金の膜の表面にレジスト組成物(東京応化工業株式会社製、製品名TFR−940PM)をスピンコート法(1580rpm、25秒間)により塗布し、120℃で60秒間プリベークした。次いで、櫛型形状における歯の本数100対(片方の櫛型電極に含まれる歯の本数が100本)、パターン太さ20μm、スペースギャップ10nmである一対の櫛型形状が対向して形成されたマスクを使用して、レジスト組成物を選択露光(ghi混合線、露光量600mJ/cm2、ハードコンタクト)し、アルカリ現像液で現像し、得られた樹脂パターンを130℃で180秒間ポストベークした。次いで、パターンの形成されたシリコンウェーハを、KI/I2水溶液(水:KI:I2=40:4:1(質量比))に浸漬して、上記で形成させた金の膜のうち表面が露出した部分をエッチングし、イオン交換水で洗浄し、さらに、フッ化水素水溶液(0.2質量%)に浸漬して、金の膜が除去されて露出したチタンの膜をエッチングし、イオン交換水で洗浄した。その後、シリコンウェーハをアセトンに浸漬して、樹脂パターンを剥離することによって、シリコンウェーハの表面に1対の櫛型形状の集電体を形成した。このようなシリコンウェーハを2枚作製した。
櫛型の集電体が形成されたシリコンウェーハのうちの1枚を使用して、実施例2のレジスト組成物によるガイド孔を作製した。まず、集電体の形成されたシリコンウェーハの表面に、実施例2のレジスト組成物をスピンコート法により塗布し、30μmのレジスト層を形成させ、120℃にて6分間プリベークした。そして、形成された櫛型の集電体と平面視で同一形状となるポジマスクを使用して、櫛型の集電体の上部に位置するレジスト層に露光(ghi混合線、3000mJ/cm2、ハードコンタクト)した。次いで、アルカリ現像液で現像し、アフターキュアとして形成されたパターンに紫外線(ghi混合線)を10分間照射した。これにより、シリコンウェーハの表面に、1対の櫛型形状のガイド孔を形成させた。なお、ガイド孔の底部には、櫛型形状の集電体が露出していた。
レジスト組成物として実施例3のレジスト組成物を使用したこと以外は、上記実施例2のレジスト組成物の場合と同様に、シリコンウェーハの表面に、1対の櫛型形状のガイド孔を作製した。
上記実施例2又は3のレジスト組成物によるガイド孔が形成されたシリコンウェーハのそれぞれについて、一対の櫛型集電体における一方の集電体表面に電気泳動法による正極活物質層を堆積させた後、他方の集電体表面にめっき法による負極活物質層を形成させた。
電気泳動法による正極活物質層の堆積を、LiCoO2粒子を10g/Lの濃度で分散させ、かつ導電助剤としてカーボンブラック(ケッチェンブラック)を0.6g/L、結着剤としてポリフッ化ビニリデンを0.4g/L、ヨウ素を0.2g/Lの濃度で含むアセトンにシリコンウェーハを浸漬し、櫛型形状の集電体の一方とそれに対向する集電体との間に電圧を印加し行った。集電体間の電場強度が100V/cmとなる電圧を1秒間印加する操作を5回繰り返すことによって行った。次いで、めっき法による負極活物質層の形成を、SnCl2・2H2Oを0.175M、NiCl2・6H2Oを0.075M、グリシンを0.125M、K4P2O7を0.50M含む水溶液に28%のアンモニア水を1vol%添加したメッキ浴を用いて電解めっきにより行った。
2 導電層
2a、2b 集電体
3a、3b 活物質層
4 基材
6 レジスト層
7a、7b ガイド孔
Claims (2)
- 正極及び負極がそれぞれ櫛型形状として形成され、前記正極及び負極が櫛型形状の歯の部分で互い違いに組み合うように対向配置され、正極及び負極が活物質層である二次電池用櫛型電極の製造方法であって、
基材の表面に導電層を形成させ、当該導電層を少なくとも一対の櫛型形状にパターニングして集電体を形成させる集電体形成工程と、
集電体形成工程で形成された集電体部分を含む前記基材の表面に、レジスト組成物を塗布してレジスト層を形成させるレジスト塗布工程と、
前記レジスト層の表面にマスクを通して光を照射し、アルカリ現像液で現像することにより、前記レジスト層のうち前記集電体の上部に位置する部分を除去して、前記集電体の上方に、正極又は負極を形成させるためのガイド孔を形成させるガイド孔形成工程と、
前記ガイド孔を鋳型として、電気泳動法又はめっき法により、前記集電体の表面に活物質層を形成させる活物質層形成工程を有し、
前記レジスト組成物が、下記(1)〜(3)のレジスト組成物のいずれかであり、前記レジスト組成物が下記(1)の場合には、前記活物質層形成工程は電気泳動法又はめっき法により行われ、前記レジスト組成物が下記(2)又は(3)の場合には、前記活物質層形成工程はめっき法により行われることを特徴とする二次電池用櫛型電極の製造方法。
(1)4〜12官能性の多官能エポキシ樹脂及びカチオン重合開始剤を含むカチオン重合系レジスト組成物
(2)フェノール、クレゾール又はキシレノールとホルムアルデヒドとを酸性触媒の存在下に縮合させたノボラック樹脂及び感光剤を含むノボラック系レジスト組成物
(3)カルボキシル基の一部が保護基により保護されたポリアクリル酸及び水酸基の一部が保護基により保護されたポリヒドロキシスチレンからなる群から選択される、酸解離性の脱離基を有し、当該脱離基が露光により光酸発生剤から発生する酸の作用で脱離することによりアルカリ可溶性が増大する樹脂、及び光酸発生剤を含む化学増幅系レジスト組成物。 - 前記レジスト組成物が、上記(1)である請求項1記載の櫛型電極の形成方法。
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