JP5991894B2 - 電池電極又はセパレーター保護用セラミックスラリー - Google Patents
電池電極又はセパレーター保護用セラミックスラリー Download PDFInfo
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- JP5991894B2 JP5991894B2 JP2012212981A JP2012212981A JP5991894B2 JP 5991894 B2 JP5991894 B2 JP 5991894B2 JP 2012212981 A JP2012212981 A JP 2012212981A JP 2012212981 A JP2012212981 A JP 2012212981A JP 5991894 B2 JP5991894 B2 JP 5991894B2
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- NMOALOSNPWTWRH-UHFFFAOYSA-N tert-butyl 7,7-dimethyloctaneperoxoate Chemical compound CC(C)(C)CCCCCC(=O)OOC(C)(C)C NMOALOSNPWTWRH-UHFFFAOYSA-N 0.000 description 1
- 125000000999 tert-butyl group Chemical group [H]C([H])([H])C(*)(C([H])([H])[H])C([H])([H])[H] 0.000 description 1
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- 238000010998 test method Methods 0.000 description 1
- DZLFLBLQUQXARW-UHFFFAOYSA-N tetrabutylammonium Chemical compound CCCC[N+](CCCC)(CCCC)CCCC DZLFLBLQUQXARW-UHFFFAOYSA-N 0.000 description 1
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- 125000003396 thiol group Chemical group [H]S* 0.000 description 1
- KUAZQDVKQLNFPE-UHFFFAOYSA-N thiram Chemical compound CN(C)C(=S)SSC(=S)N(C)C KUAZQDVKQLNFPE-UHFFFAOYSA-N 0.000 description 1
- 229960002447 thiram Drugs 0.000 description 1
- 150000003606 tin compounds Chemical class 0.000 description 1
- XOLBLPGZBRYERU-UHFFFAOYSA-N tin dioxide Chemical compound O=[Sn]=O XOLBLPGZBRYERU-UHFFFAOYSA-N 0.000 description 1
- 229910001887 tin oxide Inorganic materials 0.000 description 1
- 229910052723 transition metal Inorganic materials 0.000 description 1
- 150000003624 transition metals Chemical class 0.000 description 1
- MZHULIWXRDLGRR-UHFFFAOYSA-N tridecyl 3-(3-oxo-3-tridecoxypropyl)sulfanylpropanoate Chemical compound CCCCCCCCCCCCCOC(=O)CCSCCC(=O)OCCCCCCCCCCCCC MZHULIWXRDLGRR-UHFFFAOYSA-N 0.000 description 1
- AVYKQOAMZCAHRG-UHFFFAOYSA-N triethoxy(3,3,4,4,5,5,6,6,7,7,8,8,8-tridecafluorooctyl)silane Chemical compound CCO[Si](OCC)(OCC)CCC(F)(F)C(F)(F)C(F)(F)C(F)(F)C(F)(F)C(F)(F)F AVYKQOAMZCAHRG-UHFFFAOYSA-N 0.000 description 1
- QQQSFSZALRVCSZ-UHFFFAOYSA-N triethoxysilane Chemical compound CCO[SiH](OCC)OCC QQQSFSZALRVCSZ-UHFFFAOYSA-N 0.000 description 1
- SEACXNRNJAXIBM-UHFFFAOYSA-N triethyl(methyl)azanium Chemical compound CC[N+](C)(CC)CC SEACXNRNJAXIBM-UHFFFAOYSA-N 0.000 description 1
- ZIBGPFATKBEMQZ-UHFFFAOYSA-N triethylene glycol Chemical compound OCCOCCOCCO ZIBGPFATKBEMQZ-UHFFFAOYSA-N 0.000 description 1
- JLGLQAWTXXGVEM-UHFFFAOYSA-N triethylene glycol monomethyl ether Chemical compound COCCOCCOCCO JLGLQAWTXXGVEM-UHFFFAOYSA-N 0.000 description 1
- ITMCEJHCFYSIIV-UHFFFAOYSA-M triflate Chemical compound [O-]S(=O)(=O)C(F)(F)F ITMCEJHCFYSIIV-UHFFFAOYSA-M 0.000 description 1
- UQUAAQFOUDTPQJ-UHFFFAOYSA-N trihydroxy phosphite Chemical compound P(OO)(OO)OO UQUAAQFOUDTPQJ-UHFFFAOYSA-N 0.000 description 1
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- MTPVUVINMAGMJL-UHFFFAOYSA-N trimethyl(1,1,2,2,2-pentafluoroethyl)silane Chemical compound C[Si](C)(C)C(F)(F)C(F)(F)F MTPVUVINMAGMJL-UHFFFAOYSA-N 0.000 description 1
- AJURYMCOXVKKFB-UHFFFAOYSA-M trimethyl(3-prop-2-enoyloxypropyl)azanium;chloride Chemical compound [Cl-].C[N+](C)(C)CCCOC(=O)C=C AJURYMCOXVKKFB-UHFFFAOYSA-M 0.000 description 1
- USFMMZYROHDWPJ-UHFFFAOYSA-N trimethyl-[2-(2-methylprop-2-enoyloxy)ethyl]azanium Chemical compound CC(=C)C(=O)OCC[N+](C)(C)C USFMMZYROHDWPJ-UHFFFAOYSA-N 0.000 description 1
- JJWKIVJDHBBLHV-UHFFFAOYSA-N triphenyl(pyren-1-ylmethyl)phosphanium Chemical class C=1C=C(C2=C34)C=CC3=CC=CC4=CC=C2C=1C[P+](C=1C=CC=CC=1)(C=1C=CC=CC=1)C1=CC=CC=C1 JJWKIVJDHBBLHV-UHFFFAOYSA-N 0.000 description 1
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- 238000000108 ultra-filtration Methods 0.000 description 1
- 125000002948 undecyl group Chemical group [H]C([*])([H])C([H])([H])C([H])([H])C([H])([H])C([H])([H])C([H])([H])C([H])([H])C([H])([H])C([H])([H])C([H])([H])C([H])([H])[H] 0.000 description 1
- 238000009777 vacuum freeze-drying Methods 0.000 description 1
- NQPDZGIKBAWPEJ-UHFFFAOYSA-N valeric acid Chemical compound CCCCC(O)=O NQPDZGIKBAWPEJ-UHFFFAOYSA-N 0.000 description 1
- 239000004474 valine Substances 0.000 description 1
- 229910052720 vanadium Inorganic materials 0.000 description 1
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- 229910021489 α-quartz Inorganic materials 0.000 description 1
Classifications
-
- 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
Landscapes
- Cell Separators (AREA)
- Battery Electrode And Active Subsutance (AREA)
Description
本発明の(1)アミノ酸について説明する。アミノ酸は一分子中に、アミノ基−NHR1(式中、R1は、水素原子または有機基(例えば、C1〜C12アルキル基、C3〜C8シクロアルキル基又はC2〜C12アルケニル基であり、C1〜C12アルキル基は、アミノ基及びカルボキシル基が結合する炭素原子と一緒になって環を形成していてもよい。)である)とカルボキシル基−COOHの両方の官能基を持つ有機物を指す。本発明において、アミノ酸は、セラミックスラリーの製造におけるセラミック粒子の混和及び保存時、更に乾燥して保護多孔質膜を形成する際に凝集を防ぐ成分である。
本発明の(2)セラミック粒子について説明する。セラミック粒子は各種公知のセラミック粒子を用いることができる。例えば、アルミナ(例えば、コランダム)、シリカ、ジルコニア、ベリリア、酸化マグネシウム、チタニア、酸化鉄等の金属酸化物の粉末や、コロイダルシリカやチタニアゾル、アルミナゾル等のゾル、タルク、カオリナイト、スメクタイト等の粘土鉱物、炭化ケイ素、炭化チタン、等の炭化物、窒化ケイ素、窒化アルミニウム、窒化チタン等の窒化物、窒化ホウ素、ホウ化チタン、酸化ホウ素等のホウ化物、ムライト等の複合酸化物、水酸化リチウム、水酸化アルミニウム、水酸化マグネシウム、水酸化鉄、等の水酸化物、チタン酸バリウム、炭酸リチウム、炭酸カルシウム、炭酸マグネシウム、炭酸ストロンチウム、珪酸マグネシウム、珪酸リチウム、珪酸ナトリウム、珪酸カリウム、ガラス、セラミック粒子の多孔質体(例えば、シリカゲルや多孔質アルミナ、各種ゼオライト、珪藻土等)等が挙げられる。このようなセラミック粒子は、1種類、又は2種類以上を適宜組み合わせて使用することができる。セラミック粒子の大きさは、0.001〜100μmの範囲が好ましく、更に好ましくは0.005〜10μmの範囲である。
本発明の(3)結着剤について説明する。本発明の電池電極又はセパレーター保護用セラミックスラリーは、結着剤を含む。結着剤として、固体(例えば、粒子状)の結着剤又は液体の結着剤が挙げられる。結着剤は、溶媒に分散した状態、溶媒に溶解した状態、又は溶媒に分散した状態及び溶媒に溶解した状態であることもできる。
固体の結着剤としては、各種公知の固体の結着剤を用いることが出来る。固体の結着剤として、熱可塑性の有機物の粒子、有機物の結晶、及び熱融着時に架橋する有機物の粒子が挙げられる。固体の結着剤の平均粒子径は特に限定されず、0.01〜500μmとすることができる。
有機物の結晶としては、ヒドラジド結晶、酸無水物結晶、アミン結晶、イミダゾール結晶、及びトリアジン結晶やこれらの混晶が例示できる。有機物の結晶の融点は、40℃以上であるのが好ましく、50〜300℃であるのがより好ましい。
熱融着時に架橋する有機物の粒子は、各種公知の潜在性硬化型の固形樹脂の粒子である。潜在性硬化型の固形樹脂として、エポキシ樹脂、エポキシ樹脂とオキシラン化合物との混合物、(メタ)アクリル酸エステル、及び活性水素基を有するプレポリマーが挙げられる。よって、熱融着時に架橋する有機物の粒子として、固形のエポキシ樹脂に潜在性の熱開始剤を配合した粒子;固形のエポキシ樹脂とオキシラン化合物との混合物に潜在性の熱開始剤を配合した粒子;固形の(メタ)アクリル酸エステルと、硬化剤又は開始剤とを含む系である粒子;並びに、活性水素基を有するプレポリマーと架橋剤との組み合わせである粒子;が挙げられる。本発明において、(メタ)アクリル酸エステルとは、アクリル酸エステル及びメタクリル酸エステルを示す。
トリアリルスルホニウムヘキサフルオロアンチモネートなどのスルホニウム塩;
トリフェニルピレニルメチルホスホニウム塩などのホスホニウム塩;
(η6−ベンゼン)(η5−シクロペンタジエニル)鉄(II)ヘキサフルオロアンチモネート;
o−ニトロベンジルシリルエーテルとアルミニウムアセチルアセトナートとの組み合わせ;
シルセスキオキサンとアルミニウムアセチルアセトナートとの組み合わせ;
等が例示できる。
本発明の結着剤として液状の結着剤を使用することが出来る。
液状のプレポリマーと開始剤との混合物として、光ラジカル開始剤又は熱ラジカル発生剤と、(メタ)アクリル基、アリル基、ビニル基、マレイミド基などを有する化合物との組み合わせ;光カチオン開始剤又は熱カチオン開始剤と、エポキシ基、オキセタン環等のオキシラン環、ビニルエーテル、環状アセタールなどを有する化合物との組み合わせ;並びに、光アニオン開始剤と、エポキシ基を有する化合物及び/又はシアノアクリレート基を有する化合物との組合せ;を例示できる。なお、(メタ)アクリル基は、アクリル基及びメタクリル基を含む。
固形の高分子物質を溶媒に溶かした液状の結着剤として、前述の高分子粒子を溶媒に溶かしたもの及び溶媒に懸濁したものが例示できる。溶媒としては、固形高分子を溶かすことが出来る溶媒から適宜選択することが出来、2以上を混合して用いることもできる。
ゾルゲル反応によって固形の無機物となる液状の結着剤としては、トリエトキシシラン、トリメトキシシラン、アルミニウムイソプロポキシド、チタンテトライソプロポキシド、チタンテトラノルマルブトキシド、チタンブトキシドダイマー、チタンテトラー2ーエチルヘキソキシド、チタンジイソプロポキシビス(アセチルアセトネート)、チタンテトラアセチルアセトネート、チタンジオクチロキシビス(オクチレングリコレート)、チタンジイソプロポキシビス(エチルアセトアセテート)、チタンジイソプロポキシビス(トリエタノールアミネート)、乳酸チタン、ポリヒドロキシチタンステアレート、ジルコニウムテトラノルマルプロポキシド、ジルコニウムテトラノルマルブトキシド、ジルコウニウムテトラアセチルアセトネート、ジルコニウムトリブトキシモノアセチルアセトネート、ジルコニウムモノブトキシアセチルアセトネートビス(エチルアセトアセテート)、ジルコニウムジブトキシビス(エチルアセトアセテート)、ジルコニウムテトラアセチルアセトネート、ジルコニウムトリブトキシモノステアレート、などを例示する事が出来る。また、これらはゾルゲル反応用の触媒を添加する事ができる。ゾルゲル反応用の触媒として、無機成分を加水分解し重縮合させる反応のための触媒であれば特に限定されない。このような触媒として、塩酸のような酸;水酸化ナトリウムのようなアルカリ;アミン;あるいはジブチルスズジアセテ−ト、ジブチルスズジオクテ−ト、ジブチルスズジラウレート、ジブチルスズジマレート、ジオクチルスズジラウレート、ジオクチルスズジマレート、オクチル酸スズ等の有機スズ化合物;イソプロピルトリイソステアロイルチタネート、イソプロピルトリス(ジオクチルパイロホスフェート)チタネート、ビス(ジオクチルパイロホスフェート)オキシアセテートチタネート、テトラアルキルチタネート等の有機チタネート化合物;テトラブチルジルコネート、テトラキス(アセチルアセトナート)ジルコニウム、テトライソブチルジルコネート、ブトキシトリス(アセチルアセトナート)ジルコニウム、ナフテン酸ジルコニウム等の有機ジルコニウム化合物;トリス(エチルアセトアセテート)アルミニウム、トリス(アセチルアセトナート)アルミニウム等の有機アルミニウム化合物;ナフテン酸亜鉛、ナフテン酸コバルト、オクチル酸コバルト等の有機金属触媒等を挙げることができる。これらの中でも、市販品としてジブチルスズ化合物(三共有機化学(株)製SCAT−24)を具体的に挙げることができる。これらの化合物は、1種類、又は2種類以上を組み合わせて使用することができる。
ゾルゲル反応によって固形の無機物となる液状の結着剤の他に、固形の無機物が得られる液状の結着剤として、水ガラスを例示できる。具体的には、JIS規格表K1408の1号水ガラス、2号水ガラス、3号水ガラスや、メタ珪酸ナトリウム1種、メタ珪酸ナトリウム2種、1号珪酸カリ、2号珪酸カリ、及び珪酸リチウム等を用いる事が出来る。
本発明の(4)溶媒について説明する。本発明の電池電極又はセパレーター保護用セラミックスラリーは、安定剤として添加するアミノ酸を溶かし、蒸散に伴う空隙を発生させまた流動性を調整するために溶媒を有する。溶媒の蒸散は、加熱乾燥、真空乾燥、凍結乾燥、又はこれらの組み合わせにより行うことができる。また、電池に使用する電解液溶媒を事前に添加しておき、電解質の含浸をアシストさせることも出来る。
本発明の電池電極又はセパレーター保護用セラミックスラリーは、更に、その他の粒子として、有機フィラー、炭素系フィラーからなる群より選択される1以上の粒子を含む事ができる。
本発明の電池電極又はセパレーター保護用セラミックスラリーは、コアシェル型の発泡剤を含むことができる。このような発泡剤として、EXPANCEL(日本フィライト株式会社製)などを用いることが出来る。シェルは有機物であるから、電解液に対する長期信頼性が乏しい。そのため、このコアシェル型発泡剤を更に無機物で被覆したものを用いることもできる。このような無機物として、アルミナ、シリカ、ジルコニア、ベリリア、酸化マグネシウム、チタニア、及び酸化鉄等の金属酸化物;コロイダルシリカやチタニアゾル、アルミナゾル等のゾル;シリカゲル、及び活性アルミナ等のゲル;ムライト等の複合酸化物;水酸化アルミニウム、水酸化マグネシウム、水酸化鉄等の水酸化物:並びに、チタン酸バリウムを例示することが出来る。これらの無機物は、ゾルゲル反応や加熱によりセラミック粒子表面に被覆させることが出来る。また、無機物の被覆の前に、表面をクロメート処理やプラズマ処理、PVAやカルボキシメチルセルロース、澱粉などの水溶性高分子及びこれらに前述のポリカルボン酸を加えてエステル架橋させた配合物で表面処理することで密着性を上げることもできる。
本発明の電池電極又はセパレーター保護用セラミックスラリーは、上記コアシェル型発泡剤を、セラミック粒子及び結着剤の合計100重量部に対して、1〜99重量部含むのが好ましく、10〜98重量部含むのがより好ましく、20〜97重量部含むのがさらに好ましい。
本発明の電池電極又はセパレーター保護用セラミックスラリーは、各種イオン源となる塩を配合することができる。これによって、イオン伝導性を向上させる事が出来る。使用する電池の電解質を加えることも出来る。リチウムイオン電池の場合は、電解質として、水酸化リチウム、珪酸リチウム、六フッ化リン酸リチウム、四フッ化ホウ酸リチウム、過塩素酸リチウム、リチウムビス(トリフルオロメタンスルホニル)イミド、リチウムビス(ペンタフルオロエタンスルホニル)イミド、及びトリフルオロメタンスルホン酸リチウム等を例示でき、ナトリウムイオン電池の場合は、水酸化ナトリウム、及び過塩素酸ナトリウム等を例示できる。カルシウムイオン電池の場合は、電解質として、水酸化カルシウム、及び過塩素酸カルシウム等を例示できる。マグネシウムイオン電池の場合は、電解質として、過塩素酸マグネシウム等を例示できる。電気二重層キャパシタの場合は、電解質として、四フッ化ホウ酸テトラエチルアンモニウム、トリエチルメチルアンモニウムビス(トリフルオロメタンスルホニル)イミド、及びテトラエチルアンモニウムビス(トリフルオロメタンスルホニル)イミド等を例示できる。
本発明の電池電極又はセパレーター保護用セラミックスラリーは、イオン性を有する液体を含むことができる。イオン性を有する液体は、前記塩が溶媒に溶解した溶液又はイオン性液体であり得る。塩が溶媒に溶解した溶液として、六フッ化リン酸リチウム、又はホウフッ化テトラエチルアンモニウム等の塩が、ジメチルカーボネート等の溶媒に溶解した溶液が例示できる。
本発明の電池電極又はセパレーター保護用セラミックスラリーは、さらに、カップリング剤を含むことができる。カップリング剤は、好ましいものを含め、先に例示したカップリング剤が例示できる。カップリング剤の含有量は、セラミック粒子100重量部に対して、0.001〜10重量部含むのが好ましく、0.01〜5重量部含むのがより好ましい。
本発明の電池電極又はセパレーター保護用セラミックスラリーは、安定剤を選択して含むことができる。このような安定剤としては、具体的には2,6−ジ−tert−ブチル−フェノール、2,4−ジ−tert−ブチル−フェノール、2,6−ジ−tert−ブチル−4−エチル−フェノール、2,4−ビス−(n−オクチルチオ)−6−(4−ヒドロキシ−3,5−ジ−tert−ブチル−アニリノ)−1,3,5−トリアジン等によって例示されるフェノール系酸化防止剤;アルキルジフェニルアミン、N,N’−ジフェニル−p−フェニレンジアミン、6−エトキシ−2,2,4−トリメチル−1,2−ジヒドロキノリン、N−フェニル−N’−イソプロピル−p−フェニレンジアミン等によって例示される芳香族アミン系酸化防止剤;ジラウリル−3,3’−チオジプロピオネート、ジトリデシル−3,3’−チオジプロピオネート、ビス[2−メチル−4−{3−n−アルキルチオプロピオニルオキシ}−5−tert−ブチル−フェニル]スルフィド、2−メルカプト−5−メチル−ベンゾイミダゾール等によって例示されるサルファイド系ヒドロペルオキシド分解剤;トリス(イソデシル)ホスファイト、フェニルジイソオクチルホスファイト、ジフェニルイソオクチルホスファイト、ジ(ノニルフェニル)ペンタエリトリトールジホスファイト、3,5−ジ−tert−ブチル−4−ヒドロキシ−ベンジルホスファートジエチルエステル、ナトリウムビス(4−tert−ブチルフェニル)ホスファート等によって例示されるリン系ヒドロペルオキシド分解剤;フェニルサリチラート、4−tert−オクチルフェニルサリチラート等によって例示されるサリチレート系光安定剤;2,4−ジヒドロキシベンゾフェノン、2−ヒドロキシ−4−メトキシベンゾフェノン−5−スルホン酸等によって例示されるベンゾフェノン系光安定剤;2−(2’−ヒドロキシ−5’−メチルフェニル)ベンゾトリアゾール、2,2’−メチレンビス[4−(1,1,3,3−テトラメチルブチル)−6−(2N−ベンゾトリアゾール−2−イル)フェノール]等によって例示されるベンゾトリアゾール系光安定剤;フェニル−4−ピペリジニルカルボナート、セバシン酸ビス−[2,2,6,6−テトラメチル−4−ピペリジニル]等によって例示されるヒンダードアミン系光安定剤;[2,2’−チオ−ビス(4−t−オクチルフェノラート)]−2−エチルヘキシルアミン−ニッケル−(II)によって例示されるNi系光安定剤;シアノアクリレート系光安定剤;シュウ酸アニリド系光安定剤;フラーレン、水添フラーレン、水酸化フラーレン等のフラーレン系光安定剤等を挙げることができる。これらの安定剤は、1種類、又は2種類以上を組み合わせて使用することができる。
本発明の電池電極又はセパレーター保護用セラミックスラリーは、さらに、防腐剤を含むことができ、これにより、該スラリーの保存安定性を調節できる。
本発明の電池電極又はセパレーター保護用セラミックスラリーは、ぬれ性や消泡性を調節する目的で、さらに、界面活性剤を含むことができる。また、本発明の電池電極又はセパレーター保護用セラミックスラリーは、さらにイオン伝導性を向上する目的で、イオン性の界面活性剤を含むことができる。
本発明の電池電極又はセパレーター保護用セラミックスラリーは、上記成分を混合し撹拌することによって作製できる。撹拌は、プロペラ式ミキサー、プラネタリーミキサー、ハイブリッドミキサー、ニーダー、乳化用ホモジナイザー、及び超音波ホモジナイザー等の撹拌装置を用いて行うことができる。また、必要に応じて加熱又は冷却しながら撹拌することもできる。更に、ビーズミルやロールミルを用いてセラミック粒子を粉砕し粒子径を揃えたり小さくしたりすることもできる。
本発明の電池電極又はセパレーター表面保護方法は、電池電極又はセパレーター表面に、上記の電池電極又はセパレーター保護用セラミックスラリーの層を少なくとも1層以上形成し、前記溶媒を蒸散させることで空隙を有する保護用セラミック複合多孔質膜を形成する工程を含む。本発明の電池電極又はセパレーター保護用セラミック複合多孔質膜によって、電池電極又はセパレーターの表面は保護される。
本発明は、前記電池電極又はセパレーター表面保護方法において、本発明の電池電極又はセパレーター保護用セラミックスラリーを用いて得られる保護用セラミック複合多孔質膜にも関する。すなわち、本発明の電池電極又はセパレーター保護用セラミックスラリーを用いて得られる保護用セラミック複合多孔質膜の製造方法は、結着剤が溶媒に溶解した状態である場合、電池電極又はセパレーター表面に、前記電池電極又はセパレーター保護用セラミックスラリーのコート層を少なくとも1層以上形成する工程、及び溶媒を蒸散させる工程を含む。また、結着剤が溶媒に溶解しない固体の場合は、電池電極又はセパレーター表面に、前記電池電極又はセパレーター保護用セラミックスラリーのコート層を少なくとも1層以上形成する工程、溶媒を蒸散させる工程、及び前記溶媒を蒸散させる温度条件で固体の結着剤が熱融着しない場合は前記固体の結着剤を加熱融着する工程を含む。
本発明の電池電極又はセパレーター保護用セラミック複合多孔質膜の製造方法において、電池電極やセパレーターに対する保護用セラミック複合多孔質膜スラリーのコート層の形成は、グラビアコーターやスリットダイコーター、スプレーコーター、ディッピングなどを利用することが出来る。コート層の厚さは0.01〜100μmの範囲が好ましく、電気特性及び密着性の観点から0.05〜50μmの範囲が更に好ましい。本発明において、コート層の乾燥厚み、つまり保護用セラミック複合多孔質膜の厚みが、0.01〜100μmの範囲が好ましく、0.05〜50μmの範囲が更に好ましい。保護用セラミック複合多孔質膜の厚みがあまり薄いと電子電導に対する絶縁性が悪くなり、ショートの危険性が増す。保護用セラミック複合多孔質膜の厚みが厚すぎると抵抗が厚みに比例して上がるためイオン伝導に対する抵抗が高くなり、電池の充放電特性が低下する。
溶媒は、加熱したり真空にしたりすることで蒸散させることが出来、加熱法としては熱風炉や赤外線ヒーター、ヒートロールなどを用いることができ、真空乾燥はチャンバー内に保護用セラミック複合多孔質膜スラリーの塗膜をいれ真空にすることで乾燥できる。また、昇華性がある溶媒を用いる場合、凍結乾燥させることで溶媒を蒸散させることも出来る。加熱法における加熱温度及び加熱時間は、溶媒が蒸散する温度及び時間であれば特に限定されず、例えば80〜120℃で、0.1時間〜2時間とすることができる。溶媒を蒸散させることにより、本発明の電池電極又はセパレーター保護用セラミックスラリーの溶媒を除いた成分が、電池電極又はセパレーターと密着し、結着剤がホットメルト粒子の場合は熱融着することで本発明の保護用セラミック複合多孔質膜が形成される。
本発明の電池電極又はセパレーター保護用セラミック複合多孔質膜の製造方法において、結着剤を粒子状で使用する場合、結着剤同士を熱融着させて固化させることができる。その場合、粒子が完全に溶融する温度で熱融着させて固化させることも出来るし、有機物粒子の表面だけが熱溶解して溶着し相互に密着した状態で冷却することで粒子同士が点で密着し隙間が開いた状態で固化させることも出来る。前者の熱融着固化によれば、連続相になっている部分が多く、イオン伝導性や機械的強度及び耐熱性が高い。後者の熱融着固化によれば、連続相になっている部分が少ない分、融着した有機物粒子を通じたイオン伝導性や機械的強度及び耐熱性には劣るが、粒子間の空隙に電解液が含浸することでイオン伝導性を向上させることが出来る。また、後者はランダムに隙間が開いた構造になるため、デントライトが発生した場合、その直線的な成長を妨げることでショートを防ぐ効果を高めることも出来る。ホットメルトの際の加熱融着方法は、熱風やホットプレート、オーブン、赤外線、超音波融着など各種公知の方法を用いることが出来、加熱時にプレスすることで保護剤層の密度を高めることも出来る。また、冷却は自然冷却の他、冷却ガス、放熱板への押し付けなど各種公知の方法を用いることが出来る。また、結着剤が溶融する温度まで加熱する場合は、結着剤が溶融する温度で、0.1〜1000秒加熱することができる。
本発明の電池電極又はセパレーター保護用セラミック複合多孔質膜の製造方法では、磁場及び/又は電場を用いて配合材料を配向させた状態で固化することができる。これにより、イオン伝導性や機械的強度及び耐熱性に異方性がある保護用セラミック複合多孔質膜を形成できる。前述の高分子材料の場合、延伸することで磁化率及び/又は誘電率に異方性を与えることが出来るので、磁場及び/又は電場で配向させることが出来る。また、セルロース等の異方性がある繊維を用いることもできる。このような高分子を延伸して作製したファイバーや繊維を粉砕して粒子にし、長軸方向を電極面に垂直に立つように配向させることでイオン伝導性を向上させることが出来る。有機物結晶に付いては、結晶磁気及び/又は誘電率異方性があるものは磁場及び/又は電場で配向出来、前述の通りの効果を発揮させることが出来る。磁場及び/又は電場は静磁場及び/又は電場でも回転磁場及び/又は電場のような時間変動磁場及び/又は電場でも良く、磁場と電場は同時に印加しても良い。
本発明は、上記電池電極又はセパレーター保護用セラミック複合多孔質膜で保護されたか、上記電池電極又はセパレーター保護用セラミック複合多孔質膜の製造方法により製造した保護用セラミック複合多孔質膜を有する電池電極及び/又はセパレーターに関する。
本発明の電池電極又はセパレーター保護用セラミック複合多孔質膜で保護された電池電極又はセパレーターは、本発明のスラリーを電池電極又はセパレーターにコートして、次いで溶媒を蒸散させることで製造できる。電池電極としては、公知の各種電池や電気二重層型キャパシタの正極及び/又は負極を例示でき、これらの少なくとも一面に電池電極又はセパレーター保護用セラミックスラリーを塗布又は含浸することができる。セパレーターとしては、ポリプロピレンやポリエチレン製の多孔質材料やセルロース製やポリプロピレン、ポリエチレン、ポリエステル製の不織布などを例示でき、これらの両面又は片面に塗布したり少なくとも一部を含浸させたり出来る。本発明の電池電極又はセパレーター保護用セラミックスラリーは、対向するセパレーターや電極に密着させた状態で用いることができ、溶媒が蒸散しないうちにセパレーターと電極とを密着させてから乾燥させたり電池組み立て後にホットプレスを行ったりすることでこれら部材を密着させることも出来る。
本発明は、本発明の電池電極又はセパレーター保護用セラミックスラリーで保護された電池電極及び/又はセパレーターを含む電池に関する。電池の製造は、公知の方法によって行うことができる。また、電池は電解液を保護用セラミック複合多孔質膜に含浸させてイオン伝導性を付与したり保護用セラミック複合多孔質膜自体にイオン伝導性を持たせ固体電解質膜として電池に組み込みこんだりすることも出来る。
セラミックスラリー中のイオン性不純物の量は以下の方法で測定し、算出した。
(測定試料作製)
自動乳鉢(日陶科学株式会社製;ANM−200、アルミナ乳鉢)にセラミックスラリーに使う配合比率のうち溶媒以外の成分の合計量が1gになる量でのセラミック粒子を入れ、2時間すりつぶした後、その他の原料を加え更に2時間すりつぶした。その後、イオン交換水を99g入れ更に2時間すりつぶした。攪拌後、蒸散した分の水を追加しPTFE製の200ml耐圧容器に入れ120℃で24時間加圧加熱した。蒸散した水を追加したのち10,000Gで1時間遠心分離し、50nmのマイクロポアフィルターでフィルタリングしながら、上澄みをデカンテーションで50g分取した。
(導電率測定)
測定は、上澄みをイオン交換水で100倍に希釈したものをイオンクロマトグラフィー(日本ダイオネクス社製;ICS−500、AS11HCカラム;アニオン、CS11HClアニオン)で測定し、カチオンとアニオンのトータル量を計算し、イオン性成分の量をppmで算出した。なお、本実施例で検出されたのは、トータルイオン成分中の5%程度がCl−で5%程度が有機酸(酢酸、プロピオン酸等)、70%程度がNa+イオン、20%程度がK+イオン、であった。これは高分子合成の際の添加剤であったりセラミック粒子の製造過程で混入したりしたものである。
[試験例2]
セラミックスラリー中に含まれるアミノ酸の添加量を以下の方法で測定した。
(測定試料作製と測定)
イオン交換水、セラミック粒子、及びアミノ酸のみを含み、その他の材料を配合する直前の分散液50gを200mlのアルミナ製るつぼに入れ、120℃×24時間加熱した後重量を測定し乾燥重量を求め、更に1200℃×24時間加熱し残った灰分との重量差をアミノ酸添加量として算出した。
[試験例3]
セラミックスラリーの安定性を以下の方法で測定した。
(測定試料作製)
50mlのガラス製スクリュー管瓶に各種セラミックスラリーを30gいれ60℃で1ヶ月静置し、その後セラミックスラリーを30mg/Lの濃度になるように水に分散させたものを100ml作製し、バッチセルに入れて、次いで装置組みつけの攪拌子で10分間攪拌した。
(粒子径及び粒度分布の測定)
堀場製作所株式会社製;レーザー回折/散乱式粒度分布測定装置Partica LA−950V2を用いて平均粒子径を測定した。
[試験例4]
後述する実施例及び比較例で製造したリチウムイオン二次電池について、下記の特性を測定した。
(初期容量測定)
初期容量を出すために0.015mAの定電流で電圧が4.15Vになるまで充電し、次いで4.2Vまで0.01mAの定電流で電圧が4.2Vになるまで充電し、ついで4.2Vの定電圧で2時間充電した。その後、0.01mAの定電流で電圧が3.5Vになるまで放電した。これを3回繰り返し、3回目の放電容量を初期容量とした。
(初期内部抵抗)
初期容量を測定したセルを4.2Vの電位にし、その電位をセンターに±15mVの電圧変化で1kHzのインピーダンスを測定した。
(レート特性)
初期容量から放電レートを求めて、放電レート別の放電容量を測定した。充電は毎回10時間かけて定電流で4.2Vまで電圧を上げた後、4.2V定電圧で2時間充電した。その後、10時間かけて定電流で3.5Vになるまで放電し、このときの放電容量を0.1Cの放電容量とした。次に同様に充電した後0.1Cで求めた放電容量から1時間で放電が完了する電流値で放電しそのときの放電容量を求め1Cのときの放電容量とした。同様に、3C、10C、30Cのときの放電用量を求め、0.1Cの時の放電容量を100%としたときの容量維持率を算出した。
(サイクル寿命)
1Cで4.2Vまで充電し、4.2Vの定電圧で2時間充電したあと1Cで3.5Vまで放電する充電及び放電試験を実施した。このとき、放電容量が最初の1回目の放電に対して何%になるかを計算し、容量が80%を下回ったときの充電及び放電回数を寿命とした。
(耐熱絶縁性試験)
1Cで4.2Vまで充電し、4.2Vの定電圧で2時間充電し満充電にした状態で、25℃から260℃まで1時間に10℃ずつ昇温させ、その後およそ25℃まで1時間に20℃ずつ冷却する試験を実施し、耐久試験後の抵抗を前記「(初期内部抵抗)」の測定法で確認した。評価基準は以下の通りであった。
1kHzのインピーダンスが
◎;10MΩ以上
○:100〜10MΩ
△:1〜100kΩ
×:1kΩ未満
(耐熱外観確認(耐熱剥離試験))
試験法は、前述の耐熱絶縁試験と同じで、試験後の電池を分解して内部の様子を確認した。評価基準は以下の通りであった。
◎:正極と負極のダイレクトタッチは無く絶縁状態が保たれており電池電極保護層は電極及び/又はセパレーターに密着していた
○:正極と負極のダイレクトタッチは無く絶縁状態が保たれているが電池電極保護層は一部浮きが見られるが剥離はしていない
△:脱離が進行し、正負極の一部がむき出しになっている
×:正負極がタッチしショートしている状態
[試験例3]
後述する実施例及び比較例で製造した多孔質膜について、下記の特性を測定した。
(空隙率)
直径50mm、深さ20mmのアルミパンに、溶媒と結着剤とセラミック粒子とアミノ酸から成る電池電極又はセパレーター保護用セラミックスラリーを3g入れ、60℃×3時間乾燥させ皮膜を作製した。これを10mm角で切り取り、重量を測定した後、厚みをマイクロゲージで100点、幅と高さを20点測定し体積を求め、実測した重量と体積からかさ密度を求めた(かさ密度=重量/体積)。配合した材料の比重と組成比から真密度を計算で求め、見掛けの密度と真密度から空隙率を算出した(空隙率%=(1−かさ密度/真密度)×100)。
実施例1では、セパレーター保護用セラミックスラリーを正極にコートして、溶媒を蒸散させることにより得られる保護用セラミック複合多孔質膜を有する正極を用いてリチウムイオン二次電池を製造する方法を説明する。
(セラミックスラリー1の作製)
100Lポリプロピレン製タンクにイオン交換水50Lとアスパラギン酸1.3kgを加え1時間攪拌。そこへ、α−石英粒子(株式会社龍森製;A−1)50kgを加え、12時間攪拌して分散液を作製した。これを冷却しながらベッセル容積20Lのビーズミル(0.5mmジルコニアビーズ80%充填、周速10m/s)を用いて1週間循環粉砕して微粉砕スラリーを作製した。微粉砕スラリーを目開き5μmのナイロンメッシュでフィルタリングし、更に2Tの電磁石で磁性異物を取り除き、工程で抜けたイオン交換水を加えて水を48.7%、アスパラギン酸を1.3%、α−石英を50.0%含む分散液98.0kgを作製した。
前記スラリー50kgに更にエチレン・酢酸ビニル共重合エマルジョン(株式会社クラレ製;パンフレックスOM−4000NT)を1.5kg加え6時間攪拌して、電池電極又はセパレーター保護用セラミックスラリー(セラミックスラリー1)を得た。
冷却ジャケット付きの10Lプラネタリーミキサーに、PVdF(ポリフッ化ビニリデン)の15%NMP(N−メチルピロリドン)溶液(株式会社クレハ製;クレハKFポリマー#1120)530部、コバルト酸リチウム(略称=LCO)(日本化学工業株式会社製;セルシードC−5H)1140部、アセチレンブラック(電気化学工業株式会社製;デンカブラックHS−100)120部、NMP5400部を加え液温が30℃を超えないように冷却しながら均一になるまで攪拌した。これを、圧延アルミ集電体(日本製箔株式会社製;幅300mm、厚さ20μm)に幅180mm、厚さ200μmで塗工し、130℃温風炉で30秒乾燥させた。これを線圧530kgf/cmでロールプレスした。プレス後の正極活物質層の厚みは22μmであった。
冷却ジャケットつきの10Lプラネタリーミキサーに、PVdFの15%NMP溶液(株式会社クレハ製;クレハKFポリマー#9130)520部、グラファイト(日本黒鉛株式会社製;GR−15)1180部、NMP4100部を加え液温が30℃を超えないように冷却しながら均一になるまで攪拌した。これを、圧延銅箔集電体(日本製箔株式会社製;幅300mm、厚さ20μm)に幅180mm、厚さ200μmで塗工し、100℃温風炉で2分間乾燥させた。これを線圧360kgf/cmでロールプレスした。プレス後の負極活物質層の厚みは28μmであった。
前記正極に前記セラミックスラリー1を乾燥厚みが2μmになるようにグラビアコーターを用いて塗工し、60℃×120秒温風炉で加熱し、電池電極又はセパレーター保護用セラミック複合多孔質膜の厚みが2μmである、保護用セラミック複合多孔質膜を有する正極を製造した。
負極及び保護用セラミック複合多孔質膜を有する正極を、短辺に10mmの幅で両端に活物質層が塗工されていない領域が含まれるように40mm×50mmでカットし、金属がむき出しになっている部分に正極はアルミのタブを、負極にニッケルのタブを抵抗溶接で接合した。セパレーター(セルガード株式会社製;#2400)を幅45mm、長さ120mmにカットし、3つに折り返してその間に正極及び負極が対向するように挟み込み、これを幅50mm長さ100mmのアルミラミネートセルを二つ折りにしたもので挟み、タブが当たる部分にシーラントを挟み込んだ上でシーラント部分とそれに直交する辺を熱ラミネートして袋状にした。これを100℃の真空オーブンに24時間入れて真空乾燥させ、次いでドライブローブボックス中で6フッ化リン酸リチウム/EC:DEC=1:1 1M電解液(キシダ化学株式会社製;LBG−96533)を注入し、真空含浸した後、余った電解液を扱き出し、真空シーラーで接合密封して、リチウムイオン二次電池を製造した。
[実施例2]
実施例2では、セパレーター保護用セラミックスラリーをセパレーターにコートして、溶媒を蒸散させることにより得られる保護用セラミック複合多孔質膜を有するセパレーターを用いてリチウムイオン二次電池を製造する方法を説明する。
100Lポリプロピレン製タンクにイオン交換水50Lとアスパラギン酸1kgを加え1時間攪拌した。そこへ、コランダム(昭和電工株式会社製;A−50−F)100kgを加え、12時間攪拌して67%分散液を作製した。これを冷却しながらベッセル容積20Lのビーズミル(0.3mmジルコニアビーズ80%充填、周速10m/s)を用いて1週間循環粉砕して微粉砕スラリーを作製した。前記微粉砕スラリーを目開き5μmのナイロンメッシュでフィルタリングし、100Lポリプロピレン製タンク内に溜めて2日間静置した後、容積の1/5の上澄み層をポンプで除去した後、残り3/5を中間層としてポンプで分取して100Lのポリプロピレン製タンクに溜め、容器の底に残った1/5を沈降層として除去した。分取した3/5に付いては抜けたイオン交換水を加えて67%にした後、50Lのポリプロピレン製のタンクに溜め更に2日間静置した後、同様に上澄み層と沈降層とを除去した。この中間層を分取する操作をポリプロピレン製のタンクの容量を20Lに変えて後3回繰り返した後、最終的に分取した中間層から更に2Tの電磁石で磁性異物を取り除き、工程で抜けたイオン交換水を加えて水を34.6%、アスパラギン酸を0.40%、コランダムを65.0%含む分散液130.0kgを作製した。
前記分散液3kgに水1kgを加え、更にポリオキシエチレン(明成化学工業株式会社製;アルコックスE−30)0.1kg加え6時間攪拌して溶解させ、次いでドデシルベンゼンスルホン酸リチウムの55%水溶液0.005kgを加え更に2時間攪拌し、最後に工程で抜けたイオン交換水を加え、水49.7%、アスパラギン酸0.30%、コランダム47.5%、ポリオキシエチレン2.4%、ドデシルベンゼンスルホン酸リチウム0.10%の電池電極又はセパレーター保護用セラミックスラリー(セラミックスラリー2)を4.1kg得た。
実施例1の方法で製造した。
実施例1の方法で製造した。
セパレーター(セルガード株式会社製;#2400)に厚みが片面1μm、両面合わせて2μmになるように前記セラミックスラリー2をグラビアコーターを用いて塗工し、60℃×120秒温風炉で加熱し、電池電極又はセパレーター保護用セラミック複合多孔質膜の乾燥厚みが2μmである、保護用セラミック複合多孔質膜を有するセパレーターを製造した。
実施例1の方法で製造した。
[実施例3]
実施例3では、セパレーター保護用セラミックスラリーをセパレーターにコートして、溶媒を蒸散させることにより得られる保護用セラミック複合多孔質膜を有するセパレーターを用いてリチウムイオン二次電池を製造する方法を説明する。
100Lポリプロピレン製タンクにイオン交換水50Lとコランダム(昭和電工株式会社製;A−50−F)100kgを加え、12時間攪拌して67%分散液を作製した。これを冷却しながらベッセル容積20Lのビーズミル(0.3mmジルコニアビーズ80%充填、周速10m/s)を用いて1週間循環粉砕して分散液を作製した。そこに、イオン交換性樹脂(三菱化学株式会社製;ダイヤイオンSK−1BHとSA−10AOHの1:2混合物)50kgを入れ12時間攪拌しイオン交換を実施した。前記イオン交換性樹脂を含む分散液を目開き5μmのナイロンメッシュでフィルタリングし、コランダムを68%含む分散液140kgを作製した。これを、100Lポリプロピレン製タンク内に入れ、アスパラギン酸を0.952kg加えて12時間攪拌した。それを、2日間静置した後、容積の1/5の上澄み層をポンプで除去した後、残り3/5を中間層としてポンプで分取して100Lのポリプロピレン製タンクに溜め、容器の底に残った1/5を沈降層として除去した。分取した3/5に付いては抜けたイオン交換水を加えて67%にした後、50Lのポリプロピレン製のタンクに溜め更に2日間静置した後、同様に上澄み層と沈降層とを除去した。この中間層を分取する操作をポリプロピレン製のタンクの容量を20Lに変えて後3回繰り返した後、最終的に分取した中間層から更に2Tの電磁石で磁性異物を取り除き、工程で抜けたイオン交換水を加えて水を34.6%、アスパラギン酸を0.40%、コランダムを65.0%含む分散液130.0kgを作製した。
前記分散液3kgに水1kgを加え、更にポリオキシエチレン(明成化学工業株式会社製;アルコックスE−30)0.1kg加え6時間攪拌して溶解させ、次いでドデシルベンゼンスルホン酸リチウムの55%水溶液0.005kgを加え更に2時間攪拌し、最後に工程で抜けた分の水を加え、水49.7%、アスパラギン酸0.30%、コランダム47.5%、ポリオキシエチレン2.4%、ドデシルベンゼンスルホン酸リチウム0.1%の電池電極又はセパレーター保護用セラミックスラリー(セラミックスラリー3)を4.1kg得た。
実施例1の方法で製造した。
実施例1の方法で製造した。
実施例3の方法で製造した。
実施例1の方法で製造した。
[比較例1]
電池電極又はセパレーター保護用セラミック複合多孔質膜を有さない電極及びセパレーターを用いたこと以外は実施例1と同じ方法で、リチウムイオン二次電池を製造した。
アスパラギン酸を添加しなかったこと以外は実施例1と同じ方法で、リチウムイオン二次電池を製造した。
[比較例3]
アスパラギン酸を添加しなかったこと以外は実施例2と同じ方法で、リチウムイオン二次電池を製造した。
1 電池電極又はセパレーター保護用セラミック複合多孔質膜
2 活物質層
3 集電体
4 セパレーター
Claims (4)
- α−アミノ酸、セラミック粒子、結着剤及び溶媒を含む、電池電極又はセパレーター保護用セラミックスラリー。
- α−アミノ酸以外のイオン性成分の量が1000ppm以下であることを特徴とする請求項1記載の電池電極又はセパレーター保護用セラミックスラリー。
- 請求項1又は2記載の電池電極又はセパレーター保護用セラミックスラリーを用いて得られる保護用セラミック複合多孔質膜を有する、電池電極又はセパレーター。
- 請求項3記載の電池電極又はセパレーターを有する電池。
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JP2008016313A (ja) * | 2006-07-06 | 2008-01-24 | Matsushita Electric Ind Co Ltd | 二次電池用部材の製造方法および製造装置 |
JP5181632B2 (ja) * | 2007-11-15 | 2013-04-10 | Jsr株式会社 | 電池電極用バインダー組成物、電池電極用バインダー組成物の製造方法、電池電極用ペースト、電池電極、及び電池電極の製造方法 |
JP2010102868A (ja) * | 2008-10-22 | 2010-05-06 | Toyota Motor Corp | リチウム二次電池 |
JP2010244818A (ja) * | 2009-04-06 | 2010-10-28 | Hitachi Maxell Ltd | 非水二次電池 |
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CN109390532A (zh) * | 2017-08-07 | 2019-02-26 | 上海凯矜新材料科技有限公司 | 锂电池基膜涂布用浆料及其制备方法 |
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