JP2014086282A - 非水系蓄電デバイス用材料及びそれを用いた非水系蓄電デバイス - Google Patents
非水系蓄電デバイス用材料及びそれを用いた非水系蓄電デバイス Download PDFInfo
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- JP2014086282A JP2014086282A JP2012234611A JP2012234611A JP2014086282A JP 2014086282 A JP2014086282 A JP 2014086282A JP 2012234611 A JP2012234611 A JP 2012234611A JP 2012234611 A JP2012234611 A JP 2012234611A JP 2014086282 A JP2014086282 A JP 2014086282A
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- metal oxide
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- oxide sol
- power storage
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- GELKBWJHTRAYNV-UHFFFAOYSA-K lithium iron phosphate Chemical compound [Li+].[Fe+2].[O-]P([O-])([O-])=O GELKBWJHTRAYNV-UHFFFAOYSA-K 0.000 description 1
- VTHJTEIRLNZDEV-UHFFFAOYSA-L magnesium dihydroxide Chemical compound [OH-].[OH-].[Mg+2] VTHJTEIRLNZDEV-UHFFFAOYSA-L 0.000 description 1
- 239000000347 magnesium hydroxide Substances 0.000 description 1
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- 238000000465 moulding Methods 0.000 description 1
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- 125000004817 pentamethylene group Chemical group [H]C([H])([*:2])C([H])([H])C([H])([H])C([H])([H])C([H])([H])[*:1] 0.000 description 1
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- 238000010248 power generation Methods 0.000 description 1
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- SCPYDCQAZCOKTP-UHFFFAOYSA-N silanol Chemical compound [SiH3]O SCPYDCQAZCOKTP-UHFFFAOYSA-N 0.000 description 1
- 239000010703 silicon Substances 0.000 description 1
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- 238000012360 testing method Methods 0.000 description 1
- 229940073455 tetraethylammonium hydroxide Drugs 0.000 description 1
- LRGJRHZIDJQFCL-UHFFFAOYSA-M tetraethylazanium;hydroxide Chemical compound [OH-].CC[N+](CC)(CC)CC LRGJRHZIDJQFCL-UHFFFAOYSA-M 0.000 description 1
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- XOLBLPGZBRYERU-UHFFFAOYSA-N tin dioxide Chemical compound O=[Sn]=O XOLBLPGZBRYERU-UHFFFAOYSA-N 0.000 description 1
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- 229910052723 transition metal Inorganic materials 0.000 description 1
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- 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
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- 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
- Y02E60/13—Energy storage using capacitors
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Abstract
【解決手段】下記式で表される官能基で金属酸化物ゾル1gあたり0.55〜5.5mmol修飾された修飾金属酸化物ゾルで表面処理されている非水系蓄電デバイス用材料。図1には交流内部抵抗の複素インピーダンスプロットを示す。低周波数側の円弧の大きさ(正極の電荷移動抵抗を含む)がセル1(未処理正極)で2.8Ω、セル2(処理正極1)で2.3Ω、セル3(処理正極2)で2.9Ωであり、セル2において、表面処理による正極の電荷移動抵抗低減効果が認められた。MOS(=O)2−R1−Si(CH3)n(−O−)3−n
【選択図】図1
Description
MOS(=O)2−R1−Si(CH3)n(−O−)3−n (1)
{式中Mは水素イオン、炭素数1〜4のアルキル基、金属イオン又はアンモニウム(NR2 4)基、R1は炭素数1〜10のアルキレン基(本アルキレン鎖中に、ウレタン結合又はウレア結合を含有していてもよい)であり、R2は同一或いは異なってもよい炭素数1〜5のアルキル基又は水素原子であり、nは0又は1を表す。}
〔2〕 さらに、下記式(2)で表されるケイ素系化合物を少なくとも1種含有する前記〔1〕に記載の修飾金属酸化物ゾルで表面処理されていることを特徴とする非水系蓄電デバイス材料。
X−(R3)m−Si(CH3)n(−Y)3−n (2)
{式中Xは、ビニル基、チオール基、アミノ基、塩素原子、アクリル基、メタクリル基、スチリル基、フェニル基、グリシドキシ基、3,4−エポキシシクロヘキシル基及びブロック化イソシアネート基からなる群から選ばれる官能基であり、R3は炭素数1〜5のアルキレン基であり、mは0又は1であり、Yは同一或いは異なってもよい炭素数1〜4のアルコキシ基又は水酸基、nは0又は1を表す。}
〔3〕 さらに、テトラアルコキシシラン及び/又はそのオリゴマーを含有する前記〔1〕又は前記〔2〕に記載の修飾金属酸化物ゾルで表面処理されていることを特徴とする非水系蓄電デバイス用材料。
〔4〕 前記金属酸化物ゾルがオルガノシリカゾルである前記〔1〕〜〔3〕のいずれかに記載の修飾金属酸化物ゾルで表面処理されていることを特徴とする非水系蓄電デバイス用材料。
〔5〕 前記金属酸化物ゾルで表面処理されている非水系蓄電デバイス用材料が、正極活物質、負極活物質、セパレータ、導電材のいずれか1種類以上であることを特徴とする前記〔1〕〜〔4〕のいずれかに記載の非水系蓄電デバイス用材料。
〔6〕 前記〔1〕〜〔5〕のいずれかに記載の非水系蓄電デバイス用材料を用いた非水系蓄電デバイス。
MOS(=O)2−R1−Si(CH3)n(−O−)3−n (1)
{式中Mは水素イオン、炭素数1〜4のアルキル基、金属イオン又はアンモニウム(NR2 4)基、R1は炭素数1〜10のアルキレン基(本アルキレン鎖中に、ウレタン結合又はウレア結合を含有していてもよい)であり、R2は同一或いは異なってもよい炭素数1〜5のアルキル基又は水素原子であり、nは0又は1を表す。}
これらのうち好ましくは、アルカリ金属イオンであり、特に好ましいのはリチウムイオン、ナトリウムイオンである。
HOSO2−CH2CH2CH2Si(−O−)3
LiOSO2−CH2CH2CH2Si(−O−)3
NaOSO2−CH2CH2CH2Si(−O−)3
KOSO2−CH2CH2CH2Si(−O−)3
NH4OSO2−CH2CH2CH2Si(−O−)3
N(CH3)4OSO2−CH2CH2CH2Si(−O−)3
NH(C2H5)3OSO2−CH2CH2CH2Si(−O−)3
AgOSO2−CH2CH2CH2Si(−O−)3
HOSO2−CH2CH2OCONHCH2CH2CH2Si(−O−)3
LiOSO2−CH2CH2OCONHCH2CH2CH2Si(−O−)3
NaOSO2−CH2CH2OCONHCH2CH2CH2Si(−O−)3
KOSO2−CH2CH2OCONHCH2CH2CH2Si(−O−)3
NH4OSO2−CH2CH2OCONHCH2CH2CH2Si(−O−)3
N(CH3)4OSO2−CH2CH2OCONHCH2CH2CH2Si(−O−)3
NH(C2H5)3OSO2−CH2CH2OCONHCH2CH2CH2Si(−O−)3
AgOSO2−CH2CH2OCONHCH2CH2CH2Si(−O−)3
HOSO2−CH2CH2NHCONHCH2CH2CH2Si(−O−)3
LiOSO2−CH2CH2NHCONHCH2CH2CH2Si(−O−)3
NaOSO2−CH2CH2NHCONHCH2CH2CH2Si(−O−)3
KOSO2−CH2CH2NHCONHCH2CH2CH2Si(−O−)3
NH4OSO2−CH2CH2NHCONHCH2CH2CH2Si(−O−)3
N(CH3)4OSO2−CH2CH2NHCONHCH2CH2CH2Si(−O−)3
NH(C2H5)3OSO2−CH2CH2NHCONHCH2CH2CH2Si(−O−)3
AgOSO2−CH2CH2NHCONHCH2CH2CH2Si(−O−)
HOSO2−C6H4NHCONHCH2CH2CH2Si(−O−)3
LiOSO2−C6H4NHCONHCH2CH2CH2Si(−O−)3
NaOSO2−C6H4NHCONHCH2CH2CH2Si(−O−)3
KOSO2−C6H4NHCONHCH2CH2CH2Si(−O−)3
NH4OSO2−C6H4NHCONHCH2CH2CH2Si(−O−)3
N(CH3)4OSO2−C6H4NHCONHCH2CH2CH2Si(−O−)3
NH(C2H5)3OSO2−C6H4NHCONHCH2CH2CH2Si(−O−)3
AgOSO2−C6H4NHCONHCH2CH2CH2Si(−O−)3
LiOSO2−CH2CH2CH2SiCH3(−O−)2
NaOSO2−CH2CH2CH2SiCH3(−O−)2
KOSO2−CH2CH2CH2SiCH3(−O−)2
NH4OSO2−CH2CH2CH2SiCH3(−O−)2
NH(CH3)3OSO2−CH2CH2CH2SiCH3(−O−)2
NH(C2H5)3OSO2−CH2CH2CH2SiCH3(−O−)2
AgOSO2−CH2CH2CH2SiCH3(−O−)2
HOSO2−CH2CH2OCONHCH2CH2CH2SiCH3(−O−)2
LiOSO2−CH2CH2OCONHCH2CH2CH2SiCH3(−O−)2
NaOSO2−CH2CH2OCONHCH2CH2CH2SiCH3(−O−)2
KOSO2−CH2CH2OCONHCH2CH2CH2SiCH3(−O−)2
NH4OSO2−CH2CH2OCONHCH2CH2CH2SiCH3(−O−)2
NH(CH3)3OSO2−CH2CH2OCONHCH2CH2CH2SiCH3(−O−)2
NH(C2H5)3OSO2−CH2CH2OCONHCH2CH2CH2SiCH3(−O−)2
AgOSO2−CH2CH2OCONHCH2CH2CH2SiCH3(−O−)2
HOSO2−CH2CH2NHCONHCH2CH2CH2SiCH3(−O−)2
LiOSO2−CH2CH2NHCONHCH2CH2CH2SiCH3(−O−)2
NaOSO2−CH2CH2NHCONHCH2CH2CH2SiCH3(−O−)2
KOSO2−CH2CH2NHCONHCH2CH2CH2SiCH3(−O−)2
NH4OSO2−CH2CH2NHCONHCH2CH2CH2SiCH3(−O−)2
NH(CH3)3OSO2−CH2CH2NHCONHCH2CH2CH2SiCH3(−O−)2
NH(C2H5)3OSO2−CH2CH2NHCONHCH2CH2CH2SiCH3(−O−)2
AgOSO2−CH2CH2NHCONHCH2CH2CH2SiCH3(−O−)2
HOSO2−C6H4NHCONHCH2CH2CH2SiCH3(−O−)2
LiOSO2−C6H4NHCONHCH2CH2CH2SiCH3(−O−)2
NaOSO2−C6H4NHCONHCH2CH2CH2SiCH3(−O−)2
KOSO2−C6H4NHCONHCH2CH2CH2SiCH3(−O−)2
NH4OSO2−C6H4NHCONHCH2CH2CH2SiCH3(−O−)2
NH(CH3)3OSO2−C6H4NHCONHCH2CH2CH2SiCH3(−O−)2
NH(C2H5)3OSO2−C6H4NHCONHCH2CH2CH2SiCH3(−O−)2
AgOSO2−C6H4NHCONHCH2CH2CH2SiCH3(−O−)2
なお、オルガノゾルとは、有機溶媒にナノレベルの、表面改質をしたコロイダルシリカを安定的に分散させたコロイド溶液であり、アルコール、ケトン、エーテル、トルエンなどの各種有機溶媒に分散可能である。具体的には日産化学社製のオルガノシリカゾル(メタノールシリカゾル、IPA−ST、IPA−ST、IPA−ST−UP、IPA−ST−ZL、EG−ST、NPC−ST−30、DMAC−ST、MEK−ST、MIBK−ST、PMA−ST及びPGM−ST)や扶桑化学社製の高純度オルガノシリカゾル(PL−1−IPA、PL−2L−PGME及びPL−2L−MEK)などが挙げられる。これらは単独のみならず、複数で用いてもよい。
HS−R1−Si(CH3)n(−Y)3−n (SC1)
(Y−)3−n(CH3)Si−R1−S−S−R1−Si(CH3)n(−Y)3−n (SC2)
{式中R1は炭素数1〜10のアルキレン基(本アルキレン鎖中に、ウレタン結合又はウレア結合を含有していてもよい)であり、Yは同一或いは異なってもよい炭素数1〜4のアルコキシ基又は水酸基、nは0又は1を表す。}
CH3CH(HS)CH2Si(OC2H5)3
HSCH2CH2Si(OCH3)3
HSCH2CH2Si(OC2H5)3
HSCH2CH2OCONHCH2CH2CH2Si(OC2H5)3
HSCH2CH2NHCONHCH2CH2CH2Si(OC2H5)3
HSC6H4NHCONHCH2CH2CH2Si(OC2H5)3
(OC2H5)3SiCH2CH2CH2−S−S−CH2CH2CH2Si(OC2H5)3
熱処理温度は50℃〜250℃であり、好ましくは100℃〜200℃である。
3−(トリメトキシシリル)プロパン−1−チオール(チッソ製)1.0部(5.1モル部)をエタノール36部に溶解させた後、オルガノシリカゾル(日産化学製、30%イソプロパノール溶液)6.0部、水6.5部を加え24時間加熱還流した。冷却後過酸化水素水(三徳化学製、30%水溶液)3.5部(30.8モル部)を加え24時間加熱還流した。反応終了後室温まで冷却後、水酸化リチウム1水和物0.214部(5.1モル部)を少量の水に溶かして加え中和後、水を加えて全体の量を50部にすることにより、本発明の化合物、LiOSO2−CH2CH2CH2Si(−O−)3基で修飾されたイソプロパノールシリカゾルを含むエタノール溶液を得た。
正極活物質としてLiCoO2(平均粒径:10μm)を用いた。上記合成例で得たエタノール溶液を、エタノールで20倍に希釈した溶液50部にLiCoO210部を加え5分間超音波照射した。吸引ろ過後、乳鉢ですりつぶした後、150℃で2時間熱処理することにより本発明の修飾金属酸化物ゾルで表面処理した正極活物質を得た。正極活物質に対し、修飾金属酸化物ゾルの重量は0.2%であった(処理正極活物質1)。
未処理正極活物質(LiCoO2)、処理正極活物質1、処理正極活物質2を用い、正極を試作した。まず、前記3種類の活物質91重量部に導電材であるアセチレンブラックを4重量部、乾式混合した。バインダーであるPTFEを5重量部、加え混練し、更に、アセトンを加え、2軸ロールを用い混練混合し、圧延ロールを用いて厚さ80μmの正極シートを得た。この正極シートを所定の電極面積(14mm×20mm)に打ち抜き、導電性接着剤で厚さ20μmのアルミニウム箔に貼り付け、170℃で10時間真空乾燥することにより、3種類の正極(未処理正極、処理正極1、処理正極2)を得た。前記、Al箔上の電極層の密度はいずれも3.2g/cm3であった。
Claims (6)
- 下記式(1)で表される官能基で金属酸化物ゾル1gあたり0.55〜5.5mmol修飾された修飾金属酸化物ゾルで表面処理されていることを特徴とする非水系蓄電デバイス用材料。
MOS(=O)2−R1−Si(CH3)n(−O−)3−n (1)
{式中Mは水素イオン、炭素数1〜4のアルキル基、金属イオン又はアンモニウム(NR2 4)基、R1は炭素数1〜10のアルキレン基(本アルキレン鎖中に、ウレタン結合又はウレア結合を含有していてもよい)であり、R2は同一或いは異なってもよい炭素数1〜5のアルキル基又は水素原子であり、nは0又は1を表す。} - さらに、下記式(2)で表されるケイ素系化合物を少なくとも1種含有する請求項1に記載の修飾金属酸化物ゾルで表面処理されていることを特徴とする非水系蓄電デバイス材料。
X−(R3)m−Si(CH3)n(−Y)3−n (2)
{式中Xは、ビニル基、チオール基、アミノ基、塩素原子、アクリル基、メタクリル基、スチリル基、フェニル基、グリシドキシ基、3,4−エポキシシクロヘキシル基及びブロック化イソシアネート基からなる群から選ばれる官能基であり、R3は炭素数1〜5のアルキレン基であり、mは0又は1であり、Yは同一或いは異なってもよい炭素数1〜4のアルコキシ基又は水酸基、nは0又は1を表す。} - さらに、テトラアルコキシシラン及び/又はそのオリゴマーを含有する請求項1又は2に記載の修飾金属酸化物ゾルで表面処理されていることを特徴とする非水系蓄電デバイス用材料。
- 前記金属酸化物ゾルがオルガノシリカゾルである請求項1〜3のいずれかに記載の修飾金属酸化物ゾルで表面処理されていることを特徴とする非水系蓄電デバイス用材料。
- 前記金属酸化物ゾルで表面処理されている非水系蓄電デバイス用材料が、正極活物質、負極活物質、セパレータ、導電材のいずれか1種類以上であることを特徴とする請求項1〜4のいずれかに記載の非水系蓄電デバイス用材料。
- 請求項1〜5のいずれかに記載の非水系蓄電デバイス用材料を用いた非水系蓄電デバイス。
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JP2015222666A (ja) * | 2014-05-23 | 2015-12-10 | 株式会社Kri | 非水系蓄電デバイス用表面処理材料 |
WO2016046868A1 (ja) * | 2014-09-22 | 2016-03-31 | 株式会社日立製作所 | リチウムイオン二次電池用正極活物質、正極材料及びリチウムイオン二次電池 |
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JP2007280832A (ja) * | 2006-04-10 | 2007-10-25 | Matsushita Electric Ind Co Ltd | 二次電池用正極板の製造方法と二次電池用正極板およびこれを用いた非水系二次電池 |
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