TW201806221A - 電極用黏合劑組成物、電極用漿體、使用彼等之電極及電池 - Google Patents
電極用黏合劑組成物、電極用漿體、使用彼等之電極及電池 Download PDFInfo
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- TW201806221A TW201806221A TW106109352A TW106109352A TW201806221A TW 201806221 A TW201806221 A TW 201806221A TW 106109352 A TW106109352 A TW 106109352A TW 106109352 A TW106109352 A TW 106109352A TW 201806221 A TW201806221 A TW 201806221A
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- ULDDEWDFUNBUCM-UHFFFAOYSA-N pentyl prop-2-enoate Chemical compound CCCCCOC(=O)C=C ULDDEWDFUNBUCM-UHFFFAOYSA-N 0.000 description 1
- PNJWIWWMYCMZRO-UHFFFAOYSA-N pent‐4‐en‐2‐one Natural products CC(=O)CC=C PNJWIWWMYCMZRO-UHFFFAOYSA-N 0.000 description 1
- 150000002989 phenols Chemical class 0.000 description 1
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- 229920002312 polyamide-imide Polymers 0.000 description 1
- 229920000768 polyamine Polymers 0.000 description 1
- 229920000728 polyester Polymers 0.000 description 1
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- 239000003505 polymerization initiator Substances 0.000 description 1
- 230000000379 polymerizing effect Effects 0.000 description 1
- 229920000098 polyolefin Polymers 0.000 description 1
- 229920000069 polyphenylene sulfide Polymers 0.000 description 1
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- 229920001282 polysaccharide Polymers 0.000 description 1
- 239000005017 polysaccharide Substances 0.000 description 1
- 229920002451 polyvinyl alcohol Polymers 0.000 description 1
- 239000007774 positive electrode material Substances 0.000 description 1
- 229910001414 potassium ion Inorganic materials 0.000 description 1
- 238000001556 precipitation Methods 0.000 description 1
- NHARPDSAXCBDDR-UHFFFAOYSA-N propyl 2-methylprop-2-enoate Chemical compound CCCOC(=O)C(C)=C NHARPDSAXCBDDR-UHFFFAOYSA-N 0.000 description 1
- PNXMTCDJUBJHQJ-UHFFFAOYSA-N propyl prop-2-enoate Chemical compound CCCOC(=O)C=C PNXMTCDJUBJHQJ-UHFFFAOYSA-N 0.000 description 1
- LLHKCFNBLRBOGN-UHFFFAOYSA-N propylene glycol methyl ether acetate Chemical compound COCC(C)OC(C)=O LLHKCFNBLRBOGN-UHFFFAOYSA-N 0.000 description 1
- UBQKCCHYAOITMY-UHFFFAOYSA-N pyridin-2-ol Chemical compound OC1=CC=CC=N1 UBQKCCHYAOITMY-UHFFFAOYSA-N 0.000 description 1
- UMJSCPRVCHMLSP-UHFFFAOYSA-N pyridine Natural products COC1=CC=CN=C1 UMJSCPRVCHMLSP-UHFFFAOYSA-N 0.000 description 1
- 150000003222 pyridines Chemical class 0.000 description 1
- 239000011541 reaction mixture Substances 0.000 description 1
- 238000010992 reflux Methods 0.000 description 1
- 239000011342 resin composition Substances 0.000 description 1
- 238000007763 reverse roll coating Methods 0.000 description 1
- 150000003839 salts Chemical class 0.000 description 1
- 238000007650 screen-printing Methods 0.000 description 1
- 238000005204 segregation Methods 0.000 description 1
- 235000019983 sodium metaphosphate Nutrition 0.000 description 1
- 229910021384 soft carbon Inorganic materials 0.000 description 1
- 239000008107 starch Substances 0.000 description 1
- 235000019698 starch Nutrition 0.000 description 1
- 229920003048 styrene butadiene rubber Polymers 0.000 description 1
- 239000004094 surface-active agent Substances 0.000 description 1
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- 150000003512 tertiary amines Chemical class 0.000 description 1
- 238000012360 testing method Methods 0.000 description 1
- 150000005621 tetraalkylammonium salts Chemical class 0.000 description 1
- ZUHZGEOKBKGPSW-UHFFFAOYSA-N tetraglyme Chemical compound COCCOCCOCCOCCOC ZUHZGEOKBKGPSW-UHFFFAOYSA-N 0.000 description 1
- UJJLJRQIPMGXEZ-UHFFFAOYSA-N tetrahydro-2-furoic acid Chemical compound OC(=O)C1CCCO1 UJJLJRQIPMGXEZ-UHFFFAOYSA-N 0.000 description 1
- 238000005979 thermal decomposition reaction Methods 0.000 description 1
- 150000003606 tin compounds Chemical class 0.000 description 1
- LDHQCZJRKDOVOX-UHFFFAOYSA-N trans-crotonic acid Natural products CC=CC(O)=O LDHQCZJRKDOVOX-UHFFFAOYSA-N 0.000 description 1
- ZFDIRQKJPRINOQ-UHFFFAOYSA-N transbutenic acid ethyl ester Natural products CCOC(=O)C=CC ZFDIRQKJPRINOQ-UHFFFAOYSA-N 0.000 description 1
- IMFACGCPASFAPR-UHFFFAOYSA-N tributylamine Chemical compound CCCCN(CCCC)CCCC IMFACGCPASFAPR-UHFFFAOYSA-N 0.000 description 1
- PAPBSGBWRJIAAV-UHFFFAOYSA-N ε-Caprolactone Chemical compound O=C1CCCCCO1 PAPBSGBWRJIAAV-UHFFFAOYSA-N 0.000 description 1
Classifications
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- C08K—Use of inorganic or non-macromolecular organic substances as compounding ingredients
- C08K3/00—Use of inorganic substances as compounding ingredients
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- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08K—Use of inorganic or non-macromolecular organic substances as compounding ingredients
- C08K5/00—Use of organic ingredients
- C08K5/04—Oxygen-containing compounds
- C08K5/05—Alcohols; Metal alcoholates
-
- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08L—COMPOSITIONS OF MACROMOLECULAR COMPOUNDS
- C08L1/00—Compositions of cellulose, modified cellulose or cellulose derivatives
- C08L1/02—Cellulose; Modified cellulose
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- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08L—COMPOSITIONS OF MACROMOLECULAR COMPOUNDS
- C08L25/00—Compositions of, homopolymers or copolymers of compounds having one or more unsaturated aliphatic radicals, each having only one carbon-to-carbon double bond, and at least one being terminated by an aromatic carbocyclic ring; Compositions of derivatives of such polymers
- C08L25/18—Homopolymers or copolymers of aromatic monomers containing elements other than carbon and hydrogen
-
- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08L—COMPOSITIONS OF MACROMOLECULAR COMPOUNDS
- C08L61/00—Compositions of condensation polymers of aldehydes or ketones; Compositions of derivatives of such polymers
- C08L61/04—Condensation polymers of aldehydes or ketones with phenols only
- C08L61/06—Condensation polymers of aldehydes or ketones with phenols only of aldehydes with phenols
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- H—ELECTRICITY
- H01—ELECTRIC ELEMENTS
- H01G—CAPACITORS; CAPACITORS, RECTIFIERS, DETECTORS, SWITCHING DEVICES, LIGHT-SENSITIVE OR TEMPERATURE-SENSITIVE DEVICES OF THE ELECTROLYTIC TYPE
- H01G11/00—Hybrid capacitors, i.e. capacitors having different positive and negative electrodes; Electric double-layer [EDL] capacitors; Processes for the manufacture thereof or of parts thereof
- H01G11/22—Electrodes
- H01G11/30—Electrodes characterised by their material
- H01G11/32—Carbon-based
- H01G11/38—Carbon pastes or blends; Binders or additives therein
-
- H—ELECTRICITY
- H01—ELECTRIC ELEMENTS
- H01G—CAPACITORS; CAPACITORS, RECTIFIERS, DETECTORS, SWITCHING DEVICES, LIGHT-SENSITIVE OR TEMPERATURE-SENSITIVE DEVICES OF THE ELECTROLYTIC TYPE
- H01G11/00—Hybrid capacitors, i.e. capacitors having different positive and negative electrodes; Electric double-layer [EDL] capacitors; Processes for the manufacture thereof or of parts thereof
- H01G11/84—Processes for the manufacture of hybrid or EDL capacitors, or components thereof
- H01G11/86—Processes for the manufacture of hybrid or EDL capacitors, or components thereof specially adapted for electrodes
-
- H—ELECTRICITY
- H01—ELECTRIC ELEMENTS
- H01M—PROCESSES OR MEANS, e.g. BATTERIES, FOR THE DIRECT CONVERSION OF CHEMICAL ENERGY INTO ELECTRICAL ENERGY
- H01M4/00—Electrodes
- H01M4/02—Electrodes composed of, or comprising, active material
- H01M4/13—Electrodes for accumulators with non-aqueous electrolyte, e.g. for lithium-accumulators; Processes of manufacture thereof
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- H—ELECTRICITY
- H01—ELECTRIC ELEMENTS
- H01M—PROCESSES OR MEANS, e.g. BATTERIES, FOR THE DIRECT CONVERSION OF CHEMICAL ENERGY INTO ELECTRICAL ENERGY
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- H01M4/02—Electrodes composed of, or comprising, active material
- H01M4/13—Electrodes for accumulators with non-aqueous electrolyte, e.g. for lithium-accumulators; Processes of manufacture thereof
- H01M4/131—Electrodes based on mixed oxides or hydroxides, or on mixtures of oxides or hydroxides, e.g. LiCoOx
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- H—ELECTRICITY
- H01—ELECTRIC ELEMENTS
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- H01M4/02—Electrodes composed of, or comprising, active material
- H01M4/13—Electrodes for accumulators with non-aqueous electrolyte, e.g. for lithium-accumulators; Processes of manufacture thereof
- H01M4/134—Electrodes based on metals, Si or alloys
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- H—ELECTRICITY
- H01—ELECTRIC ELEMENTS
- H01M—PROCESSES OR MEANS, e.g. BATTERIES, FOR THE DIRECT CONVERSION OF CHEMICAL ENERGY INTO ELECTRICAL ENERGY
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- H01M4/02—Electrodes composed of, or comprising, active material
- H01M4/13—Electrodes for accumulators with non-aqueous electrolyte, e.g. for lithium-accumulators; Processes of manufacture thereof
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- H01M4/13—Electrodes for accumulators with non-aqueous electrolyte, e.g. for lithium-accumulators; Processes of manufacture thereof
- H01M4/139—Processes of manufacture
- H01M4/1391—Processes of manufacture of electrodes based on mixed oxides or hydroxides, or on mixtures of oxides or hydroxides, e.g. LiCoOx
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- H01M4/02—Electrodes composed of, or comprising, active material
- H01M4/13—Electrodes for accumulators with non-aqueous electrolyte, e.g. for lithium-accumulators; Processes of manufacture thereof
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- H01M4/1395—Processes of manufacture of electrodes based on metals, Si or alloys
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- H01M4/36—Selection of substances as active materials, active masses, active liquids
- H01M4/48—Selection of substances as active materials, active masses, active liquids of inorganic oxides or hydroxides
- H01M4/485—Selection of substances as active materials, active masses, active liquids of inorganic oxides or hydroxides of mixed oxides or hydroxides for inserting or intercalating light metals, e.g. LiTi2O4 or LiTi2OxFy
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- H01—ELECTRIC ELEMENTS
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- H01M4/02—Electrodes composed of, or comprising, active material
- H01M4/62—Selection of inactive substances as ingredients for active masses, e.g. binders, fillers
-
- 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
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- Chemical & Material Sciences (AREA)
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- Electric Double-Layer Capacitors Or The Like (AREA)
Abstract
本發明之目的在於提供一種作成電池時能夠獲得長期可靠性、即高容量保持率、以及初次充放電效率之電極用黏合劑組成物、電極用漿體、使用其之電極及電池。
本發明提供一種電極用黏合劑組成物,其含有(a)選自下述(a-1)~(a-3)中之至少1種的樹脂及(b)鹼性化合物,(a-1)聚羥基苯乙烯系樹脂;(a-2)側鏈具有選自羧基及磺酸基中之至少1種的聚苯乙烯系樹脂;(a-3)酚樹脂。
Description
本發明係關於黏合劑組成物,詳言之,本發明係關於電極用黏合劑組成物、電極用漿體、使用彼等之電極及電池。
近年來,隨著筆記型個人電腦或小型行動終端的爆發式普及,對可充電之小型、輕量、具高容量、高能量密度、高可靠性的二次電池的要求激增。
而且在汽車業界中,熱切期待藉由導入電動汽車(EV)或混合電力電動汽車(HEV)來降低二氧化碳排放量,亦積極進行開發掌握這些實用化的關鍵的馬達驅動用二次電池。
尤其是在電池當中被認為具有最高理論能量的鋰離子二次電池備受矚目,目前正急速進行開發。目前廣泛使用的鋰離子電池具有正極與負極經由隔離膜、電解質層進行連接、密封的構成,其中該正極係將鈷酸鋰等含鋰的複合氧化物等正極活性物質與包含聚偏二氟乙烯(PVDF)等二次電池電極用黏合劑(以下有時省略為
黏合劑)的二次電池電極用漿體(以下有時省略為漿體)塗布在鋁箔上所形成的正極,該負極係將碳系電極活性物質(以下有時省略為活性物質)等的可吸留釋放鋰離子的負極活性物質與包含PVDF或苯乙烯-丁二烯-橡膠(SBR)等黏合劑的漿體塗布在銅箔上所形成的負極。
二次電池電極用黏合劑組成物(以下有時省略為電極用黏合劑組成物)係將成為二次電池電極用黏合劑的物質溶解於有機溶媒而成者或是分散於有機溶媒或水而成者。將作為在此電極用黏合劑組成物中混合電極活性物質的混合物之二次電池電極用漿體利用例如刮刀塗布法、浸漬塗布法、逆輥塗法、直接輥塗法、刀塗法、旋轉塗布法等塗布在鋁或銅等的集電體上,以乾燥等方法去除溶媒,而使活性物質結合於集電體,並且使活性物質彼此結合來製造電極。將所製造的正/負極電極透過介隔例如多孔性聚丙烯製隔離膜來捲取,再經由其他步驟來製造電池。
電池的容量是根據活性物質的種類及量、電解液的種類及量等多種因素而決定,但電極用黏合劑組成物的性能亦為一個重要的因素。電極用黏合劑組成物能夠將足夠的量的活性物質結合於集電體,並且不會將活性物質彼此結合,無法得到初期容量大的電池,而且因為重複充放電,活性物質會從集電體脫落,電池的容量會下降。近年來,尤其是在負極中,為了負極的高容量化目的,已研究在活性物質中使用矽、鍺、錫或其合金等(例如參照專利文獻1)。
又,已提出為現有的電極用黏合劑組成物之將PVDF溶解於N-甲基吡咯啶酮等中的有機溶媒系黏合劑組成物、以及橡膠系高分子分散於水中之電極用黏合劑組成物(例如參照專利文獻2~5)。
此外,已報導藉由將聚醯亞胺系樹脂用於黏合劑,即便是充放電時的體積變化大的含矽負極,也能夠抑制長期循環試驗下的容量下降(例如參照專利文獻6~8)。
專利文獻1日本特開2009-199761號公報
專利文獻2日本特開平6-203833號公報
專利文獻3日本特開平5-62668號公報
專利文獻4日本特開平4-342966號公報
專利文獻5日本特開平8-124557號公報
專利文獻6日本特開2009-245773號公報
專利文獻7日本特開2010-062041號公報
專利文獻8日本特開2009-170384號公報
然而,在活性物質中使用矽、鍺、錫或其合金等的情況下,相對於以往所使用的碳系材料,每單位體積的鋰離子的吸留量大,一旦充分地進行充電時,就會有充分地進行放電時的活性物質自身的體積變化大的課題存在。
又,為現有的電極用黏合劑組成物之將PVDF溶解於N-甲基吡咯啶酮等中的有機溶媒系黏合劑組成物、以及橡膠系高分子分散於水中之電極用黏合劑組成物有著無法追隨活性物質的體積變化並且由於因重複充放電造成的結合力的劣化而無法長時間維持高容量的課題。
此外,聚醯亞胺系黏合劑組成物雖然具有高的循環性能,但卻有初次的充放電效率比PVDF或橡膠系高分子還要差的問題存在。
有鑑於上述課題,本發明之目的在於提供不僅能夠在將矽、錫、鍺或其合金用於負極而製成電池時得到長期可靠性、也就是高容量保持率且初次充放電效率亦高的電極用黏合劑組成物、電極用漿體、使用其之電極及電池。
本發明為一種電極用黏合劑組成物,其含有(a)選自下述(a-1)~(a-3)中之至少1種的樹脂及(b)鹼性化合物,(a-1)聚羥基苯乙烯系樹脂;(a-2)側鏈具有選自羧基及磺酸基中之至少1種的聚苯乙烯系樹脂;(a-3)酚樹脂。
若根據本發明,能夠得到在作為電池時能得到長期可靠性、即高容量保持率且初次充放電效率高的
電極用黏合劑組成物、電極用漿體、使用其之電極,並且能夠具有高容量保持率、初次充放電效率的電池。
本發明為一種電極用黏合劑組成物,其含有(a)選自下述(a-1)~(a-3)中之至少1種的樹脂及(b)鹼性化合物,(a-1)聚羥基苯乙烯系樹脂;(a-2)側鏈具有選自羧基及磺酸基中之至少1種的聚苯乙烯系樹脂;(a-3)酚樹脂。
就本發明所使用的(a-1)聚羥基苯乙烯系樹脂而言,例如可列舉:以公知的方法將對羥基苯乙烯、間羥基苯乙烯、鄰羥基苯乙烯、對異丙烯基苯酚、間異丙烯基苯酚、鄰異丙烯基苯酚等之具有酚性羥基的芳香族乙烯化合物單獨或使用2種以上進行聚合所得到的聚合物、或前述芳香族乙烯化合物與其他乙烯基系化合物的共聚物。
又,本發明所使用的(a-1)聚羥基苯乙烯系樹脂可為將鍵結於芳香族環的氫原子的一部分以碳數1~20的烷基、氟烷基、烷氧基、酯基、氟原子或氯原子取代1~4個的結構等。
就本發明所使用的(a-2)側鏈具有選自羧基及磺酸基中之至少1種的聚苯乙烯系樹脂而言,例如可列舉:以公知的方法將對羧基苯乙烯、間羧基苯乙烯、鄰羧基苯乙烯、對磺化苯乙烯、間磺化苯乙烯、鄰磺化苯乙烯等之具有羧基或磺酸基的芳香族乙烯化合物單獨或使用2種以上進行聚合所得到的聚合物、或前述芳香族乙烯化合物與其他乙烯基系化合物的共聚物。
又,本發明所使用的(a-2)側鏈具有選自羧基及磺酸基中之至少1種的聚苯乙烯系樹脂,可為將鍵結於芳香族環的氫原子的一部分以碳數1~20的烷基、氟烷基、烷氧基、酯基、氟原子或氯原子取代1~4個的結構等。
本發明所使用的(a-2)側鏈具有選自羧基及磺酸基中之至少1種的聚苯乙烯系樹脂的較佳重量平均分子量較佳係以使用凝膠滲透層析術(GPC)測定之以聚苯乙烯換算為1,000~100,000,較佳為2,000~30,000的範圍。
就本發明所使用的(a-3)酚樹脂而言,有酚醛樹脂或可溶酚醛樹脂。此等係藉由使用公知的方法將各種苯酚類單獨或是該等的複數種的混合物以甲醛等醛類進行聚縮合而得到。
就構成酚醛樹脂及可溶酚醛樹脂的苯酚類而言,例如可列舉:苯酚、對甲酚、間甲酚、鄰甲酚、2,3-二甲基苯酚、2,4-二甲基苯酚、2,5-二甲基苯酚、2,6-二甲基苯酚、3,4-二甲基苯酚、3,5-二甲基苯酚、2,3,4-三
甲基苯酚、2,3,5-三甲基苯酚、3,4,5-三甲基苯酚、2,4,5-三甲基苯酚、亞甲基雙酚、亞甲基雙對甲酚、間苯二酚、鄰苯二酚、2-甲基間苯二酚、4-甲基間苯二酚、鄰氯苯酚、間氯苯酚、對氯苯酚、2,3-二氯苯酚、間甲氧基苯酚、對甲氧基苯酚、對丁氧基苯酚、鄰乙基苯酚、間乙基苯酚、對乙基苯酚、2,3-二乙基苯酚、2,5-二乙基苯酚、對異丙基苯酚、α-萘酚、β-萘酚等,此等係能夠單獨或作為複數種混合物來使用。
又,就醛類而言,除了甲醛,還可列舉:三聚甲醛、乙醛、苯甲醛、羥基苯甲醛、氯乙醛等,此等係能夠單獨或作為複數種混合物來使用。
又,本發明所使用的(a-3)酚樹脂可為將鍵結於芳香族環的氫原子的一部分以碳數1~20的烷基、氟烷基、烷氧基、酯基、氟原子或氯原子取代1~4個的結構等。
本發明所使用的(a-3)酚樹脂的較佳重量平均分子量係較佳以使用凝膠滲透層析術(GPC)測定之以聚苯乙烯換算為2,000~50,000,較佳為3,000~30,000的範圍。
從使電池充放電時的容量保持率提升的觀點來看,較佳的樹脂(a)為具有以下述通式(1)表示的結構的聚羥基苯乙烯系樹脂。
(通式(1)中,R1、R2係表示碳數1~5的有機基或鹵素,就較佳的碳數1~5的有機基而言,可列舉:烷基、烯基、炔基、氟烷基、烷氧基。R3係表示碳數1~20的1價的有機基,就較佳的碳數1~20的有機基而言,可列舉:烷基、烯基、炔基、或該等之中1個以上的氫經羥基、甲基丙烯醯氧基、丙烯醯氧基、環氧丙基醚基取代者。R4、R5、R6係表示氫原子、或碳數1~3的有機基,就較佳的碳數1~3的有機基而言,可列舉:烷基或氟烷基。a為0~4的整數,c為0~5的整數,b為1~5的整數,且a+b為1~5的整數。n1為10~10000的整數,n2、n3為0~10000的整數,且0.2≦n1/(n1+n2+n3)≦1。)
以通式(1)表示的樹脂係由n1個羥基苯乙烯系單體、n2個苯乙烯系單體、n3個其他乙烯基系化合物所構成。n1為10~10,000的整數,n2、n3為0~10,000的整數,且0.2≦n1/(n1+n2+n3)≦1。又,較佳為0.4≦n1/(n1+n2+n3)≦1,更佳為0.7≦n1/(n1+n2+n3)≦1,最佳為0.9≦n1/(n1+n2+n3)≦1。具有酚系羥基的羥基苯乙烯系單體的比例較大者具有黏合劑的結合力強、充放電時的容量保持率增加的優點,因而較佳。
較佳作為其他乙烯基系化合物的是共軛二烯系單體、烯性不飽和羧酸酯系單體、含環氧丙基的乙烯基單體、含磺酸基的乙烯基單體。
就較佳的其他乙烯基系化合物的具體例而言,可列舉:1,3-丁二烯、異戊二烯、2,3-二甲基-1,3-丁二烯、1,3-戊二烯、丙烯酸甲酯、丙烯酸乙酯、丙烯酸丙酯、丙烯酸丁酯、丙烯酸異丁酯、丙烯酸正戊酯、丙烯酸異戊酯、丙烯酸正己酯、丙烯酸-2-乙基己酯、丙烯酸正辛酯、丙烯酸-2-羥基乙酯、丙烯酸羥基丙酯、甲基丙烯酸丙酯、甲基丙烯酸丁酯、甲基丙烯酸異丁酯、甲基丙烯酸正戊酯、甲基丙烯酸異戊酯、甲基丙烯酸正己酯、甲基丙烯酸-2-乙基己酯、甲基丙烯酸正辛酯、甲基丙烯酸-2-羥基乙酯、甲基丙烯酸羥基丙酯、丙烯酸月桂酯、甲基丙烯酸月桂酯、丁烯酸甲酯、丁烯酸乙酯、異丁烯酸乙酯、甲基丙烯酸甲酯、甲基丙烯酸乙酯、丙烯酸、甲基丙烯酸、順丁烯二酸、反丁烯二酸、甲基順丁烯二酸、中康酸、戊烯二酸、伊康酸、四氫酞酸、丁烯酸、異丁烯酸、納迪克酸(nadic acid)、順丁烯二酸單辛酯、順丁烯二酸單丁酯、伊康酸單辛酯、苯乙烯、α-甲基苯乙烯、β-甲基苯乙烯、對三級丁基苯乙烯、氯苯乙烯等。
本發明所使用的聚羥基苯乙烯系樹脂的重量平均分子量以使用凝膠滲透層析術(GPC)測定的聚苯乙烯換算,較佳為3,000~60,000的範圍,更佳為3,000~25,000的範圍。
在本發明中,亦能夠併用(a-3)酚樹脂與(a-1)聚羥基苯乙烯系樹脂。從使電池充放電時的容量保持率提升的觀點來看,併用時的(a-1)聚羥基苯乙烯系樹脂的含有比率越多越佳。(a-3)酚樹脂與(a-1)聚羥基苯乙烯系樹脂的較佳含有比率以質量比計為50:50~0:100。
前述樹脂(a)可作為單體使用,或亦可以改善充放電特性或調節黏度等為目的而與其他樹脂摻混使用。
較佳作為其他樹脂者係可列舉:上述適用於共聚合的其他乙烯基系化合物的組合之樹脂,更具體來說,可列舉:聚丙烯酸、聚甲基丙烯酸、聚氧乙烯、聚(2-甲氧基乙氧基乙烯)、聚乙烯醇、聚乙烯磺酸、聚偏二氟乙烯、或直鏈澱粉、支鏈澱粉、澱粉、羧基甲基纖維素等多糖類等。
從使電池充放電時的容量保持率提升的觀點來看,作為其他樹脂之更佳者為以下述通式(3)表示的纖維素化合物。
(通式(3)中,R18係表示氫或CH2COOR19,複數個R18分別可為相同,亦可為不同。R19係表示氫、
鋰、鈉、或鉀,複數個R19分別可為相同,亦可為不同。
n7係表示10~100,000的整數。)
從使電池充放電時的容量保持率提升的觀點來看,其他樹脂的含量相對於樹脂(a)100質量份而言,較佳為5質量份以上,更佳為10質量份以上,再更佳為20質量份以上。又,從使電極的耐熱性提升的觀點來看,其他樹脂的含量相對於樹脂(a)100質量份而言,較佳為50質量份以下,更佳為40質量份以下,再更佳為30質量份以下。
本發明之黏合劑組成物包含(b)鹼性化合物,就(b)鹼性化合物而言,可列舉:3級胺、吡啶衍生物、四烷基銨鹽等有機含氮化合物、或含有鹼金屬、鹼土金屬的氫氧化化合物、碳酸氫化化合物、碳酸化合物等無機鹼化合物等。
就(b)鹼性化合物的較佳具體例而言,可列舉:三乙胺、三丁胺、乙醇胺、二乙醇胺、三乙醇胺、三異丙醇胺、吡啶、羥基吡啶、甲基吡啶、甲氧基吡啶、氫氧化鈉、氫氧化鉀、氫氧化鋰、氫氧化鈣、氫氧化鎂、碳酸鈉、碳酸鉀、碳酸鋰、碳酸鈣、碳酸氫鈉等。
從使電池充放電時的容量保持率提升的觀點來看,(b)鹼性化合物更佳為含有選自鹼金屬及鹼土金屬中之至少1種元素的鹼,最佳為含有鹼金屬的鹼。就(b)鹼性化合物的最佳具體例而言,可列舉:氫氧化鈉、氫氧化鉀、氫氧化鋰、碳酸鈉、碳酸鉀、碳酸鋰、碳酸氫鈉。
此等鹼性化合物與位於樹脂(a)側鏈的酚性羥基、羧基、磺酸基形成離子鍵,藉由將側鏈離子化,分子鏈的範圍會變大,或是透過離子性官能基帶來的接著性的效果等,作為用於電極的黏合劑的填料的結合性會提升。
(b)鹼性化合物的較佳添加量,相對於前述樹脂(a)的酚性羥基、羧基、磺酸基的總計100莫耳%而言,為5莫耳%以上,更佳為30莫耳%以上,再更佳為50莫耳%以上。藉由在此範圍內,而有電極用黏合劑的結合力增強、使電池充放電時的容量保持率提升的優點。又,(b)鹼性化合物的較佳添加量,相對於具有酚性羥基的樹脂的酚性羥基100莫耳%,為300莫耳%以下,更佳為200莫耳%以下,再更佳為100莫耳%以下,最佳為90莫耳%以下。藉由在此範圍內,而有能抑制鹼性化合物造成的電極的劣化、使電池充放電時的容量保持率提升的優點。
從使電池充放電時的容量保持率提升的觀點來看,本發明之黏合劑組成物係以含有熱交聯劑為佳。就熱交聯劑而言,較佳可使用環氧化合物、羥甲基化合物、甲氧基甲基化合物及二乙烯苯等。其中,為了維持黏合劑的強度,更佳為使用羥甲基、甲氧基甲基化合物。
就環氧化合物的較佳具體例而言,例如可列舉:雙酚A型環氧樹脂、雙酚F型環氧樹脂、丙二醇二環氧丙基醚、聚丙二醇二環氧丙基醚、聚甲基(環氧丙氧基丙基)矽氧烷等含環氧基的聚矽氧等,惟本發明不受限於此等。具體來說,可列舉:「EPICLON」(註冊商
標)850-S、EPICLON HP-4032、EPICLON HP-7200、EPICLON HP-820、EPICLON HP-4700、EPICLON EXA-4710、EPICLON HP-4770、EPICLON EXA-859CRP、EPICLON EXA-1514、EPICLON EXA-4880、EPICLON EXA-4850-150、EPICLON EXA-4850-1000、EPICLON EXA-4816、EPICLON EXA-4822(以上為商品名、DIC(股)製)、「RIKARESIN」(註冊商標)BEO-60E(以上為商品名、新日本理化(股)製)、EP-4003S、EP-4000S(以上為商品名、(股)ADEKA製)等。
又,就羥甲基化合物及甲氧基甲基化合物的較佳具體例而言,例如可列舉:DML-PC、DML-PEP、DML-OC、DML-OEP、DML-34X、DML-PTBP、DML-PCHP、DML-OCHP、DML-PFP、DML-PSBP、DML-POP、DML-MBOC、DML-MBPC、DML-MTrisPC、DML-BisOC-Z、DML-BisOCHP-Z、DML-BPC、DML-BisOC-P、DMOM-PC、DMOM-PTBP、DMOM-MBPC、TriML-P、TriML-35XL、TML-HQ、TML-BP、TML-pp-BPF、TML-BPE、TML-BPA、TML-BPAF、TML-BPAP、TMOM-BP、TMOM-BPE、TMOM-BPA、TMOM-BPAF、TMOM-BPAP、HML-TPPHBA、HML-TPHAP、HMOM-TPPHBA、HMOM-TPHAP(以上為商品名、本州化學工業(股)製)、或該等的鋰、鈉、鉀離子化物、「NIKALAC」(註冊商標)MX-290、NIKALAC MX-280、NIKALAC MX-270、NIKALAC MX-279、NIKALAC MW-100LM、NIKALAC MX-750LM(以上為商品名、(股)Sanwa Chemical製)。亦可含有2種以上的此等化合物。
在本發明之熱交聯劑中,尤其是以下述通式(2)表示的甲氧基甲基化合物由於具有水溶性,因此與包含樹脂(a)及鹼化合物(b)的組成物成分會很好地相溶,在製作電極時會相分離而不偏析,更加提高充放電時的容量保持率,因而其能夠最佳地使用。
(通式(2)中,R13、R14、R15分別可為相同,亦可為不同,係表示氫或1價的金屬陽離子。R16、R17分別可為相同,亦可為不同,係表示氫或碳數1~3的有機基。)
通式(2)中,R13、R14、R15係表示選自氫、1價的金屬陽離子中之至少1種元素,相對於R13、R14及R15的總計100莫耳%之10莫耳%以上為1價的金屬陽離子。較佳作為金屬陽離子者為鹼金屬,更佳為Na、Li、K。
從使電池充放電時的容量保持率提升的觀點來看,就金屬陽離子的導入量而言,相對於R13、R14及R15的總計100莫耳%,更佳為20莫耳%以上,再更佳為50莫耳%以上。
R16、R17係表示選自氫、碳數1~3的有機基中之至少1種。就較佳的碳數1~3的有機基而言,可列舉:烷基、烯基、炔基、氟烷基、烷氧基。
從使電池充放電時的容量保持率提升的觀點來看,熱交聯劑的含量相對於樹脂整體100質量份,較佳為0.1質量份以上,更佳為1質量份以上,再更佳為2質量份以上。又,從使電極的柔軟性提升的觀點來看,熱交聯劑的含量相對於樹脂整體100質量份,較佳為30質量份以下,更佳為20質量份以下,再更佳為10質量份以下。
再者,為了促進上述的環氧化合物、羥甲基化合物、甲氧基甲基化合物的交聯,亦可在本發明之黏合劑組成物中添加光酸產生劑或熱酸產生劑。
熱酸產生劑的熱分解起始溫度較佳為50℃~270℃,更佳為50℃~150℃。
就熱酸產生劑的具體例而言,可列舉鋶鹽、銨鹽、鏻鹽等鎓鹽等,但較佳為具有以下述通式(4)表示的結構的化合物。
通式(4)中,R20係表示選自碳數1~8的有機基及羥基中之至少1種。就較佳的碳數1~8的有機基而言,可列舉:碳數1~8的烷基、碳數1~4的酯基。R21、
R22係表示碳數1~16的有機基。R21、R22較佳係表示選自含有1個以上的碳數6~16的芳香環且芳香環的氫未經取代或是經碳數1~4的烷基、碳數1~4的氟烷基、羥基、鹵素、氰基、硝基、亞硝基取代的基、碳數1~10的烷基中之至少1種。R23係表示選自碳數1~8的烷基、碳數1~8的氟烷基中之至少1種。
就熱酸產生劑的特佳的例子而言,可列舉下述結構者等,但不限於此等。
本發明之黏合劑組成物亦可進一步視需要地含有相對於樹脂的總量100質量份為0.1~10質量份的界面活性劑或胺基丙基三甲氧基矽烷、三甲氧基乙烯基矽烷、三甲氧基環氧丙氧基矽烷等矽烷偶合劑、三系化合物、啡啉系化合物、三唑系化合物等。藉由含有此等,能夠更加提高與活性物質或金屬箔的接著性。
本發明之電極用黏合劑組成物有時亦可作為溶液使用。黏合劑溶液的濃度與黏度的範圍較佳為濃度1~50質量%且黏度1mPa‧秒~1000Pa‧秒的範圍,更佳為濃度5~30質量%且黏度100mPa‧秒~100Pa‧秒。
就黏合劑溶液所使用的溶媒而言,可列舉:水、NMP、DMAC、DMF、DMSO、GBL、丙二醇二甲基醚、乳酸乙酯、環己酮、四氫呋喃、丙二醇單甲基醚乙酸酯、各種醇類、甲基乙基酮、甲基異丁基酮等。
從安全性的觀點來看,係以溶媒的80%以上為水為佳。
本發明之電極用黏合劑組成物亦能夠與本發明之電極用黏合劑組成物作為含有填料的電極用漿體來使用。
就用於二次電池或電雙層電容器時的較佳填料而言,可列舉:含有碳、矽、錫、鍺、鈦、鐵、鈷、鎳、錳、銅、銀、鋅、銦、鉍、銻或鉻等原子的化合物。較佳為含有碳、錳、鈷、鎳、鐵、矽、鈦、錫、及鍺之中至少1種的原子的化合物,更佳為含有矽、氧化矽及鈦酸鋰之中至少1種的化合物。
若將這些化合物作為填料使用,填料就能夠發揮作為活性物質的作用。因此,藉由在本發明之樹脂中添加填料作成漿體,而能夠作為二次電池或電雙層電容器的電極用漿體來使用。
又,就正極用填料的例子而言,可列舉:磷酸鐵鋰、鈷酸鋰、鎳酸鋰、錳酸鋰、活性碳、碳奈米管等。
又,就負極用填料的例子而言,可列舉:鈦酸鋰、硬碳(hard carbon)、軟碳(soft carbon)、活性碳、碳奈米管、包含矽、錫、鍺原子的化合物等。尤其是將含有矽、錫、鍺原子的化合物作為填料使用的蓄電池在充電時活性物質的體積膨脹大,因此將本發明之經離子化的芳香族樹脂作為黏合劑使用會使活性物質的劣化減少,甚至是使充放電時的容量劣化減少,故而較佳。
就含有矽原子(矽)的化合物而言,例如可列舉:(1)矽微粒子、(2)錫、鎳、銅、鐵、鈷、錳、鋅、銦、銀、鈦、鍺、鉍、銻或鉻與矽的合金(3)硼、氮、氧或碳與矽的化合物、或是此等進一步具有列在(2)中的金屬的化合物等。就矽的合金或是化合物的一例而言,可列舉:SiB4、SiB6、Mg2Si、Ni2Si、TiSi2、MoSi2、CoSi2、NiSi2、CaSi2、CrSi2、Cu5Si、FeSi2、MnSi2、NbSi2、TaSi2、VSi2、WSi2、ZnSi2、SiC、Si3N4、Si2N2O、SiOv(0<v≦2)或LiSiO等。
就含有錫原子的化合物而言,例如可列舉:(1)矽、鎳、銅、鐵、鈷、錳、鋅、銦、銀、鈦、鍺、鉍、銻或鉻與錫的合金、(2)氧或碳與錫的化合物、或此等更具有(1)所例示的金屬者等。就錫的合金或是化合物的一例而言,可列舉:SnOw(0<w≦2)、SnSiO3、LiSnO或Mg2Sn等。
就含有鍺原子的化合物而言,可列舉:矽或錫與鍺的合金等。
填料的粒度分布中之中位直徑(d50)較佳為0.01~20μm的範圍內。又,填料的表面亦可施加使用矽烷偶合劑等的處理。
此處,中位直徑係能夠使用堀場製作所製雷射繞射/散射式粒度分布測定裝置LA-920來測定。測定前,將適量的試料添加至偏磷酸鈉水溶液中,花費10分鐘以超音波洗淨機使其分散後進行測定。藉此,在粉體凝集而成的試料中解除凝集,並且抑制粒徑大的粉體的沉澱等,而能夠測定正確的粒度分布。
從能夠進一步提升接著性這樣的觀點來看,本發明之電極用漿體中除了溶媒以外的電極用黏合劑組成物的含量相對於填料100質量份而言,較佳為1質量份以上,更佳為3質量份以上,再更佳為5質量份以上。又,為了減少電阻而增加填料的填充量,電極用黏合劑組成物的含量相對於填料100質量份而言,較佳為20質量份以下,更佳為15質量份以下,再更佳為12質量份以下。
為了使二次電池用電極或電容器用電極的電阻降低,本發明之負極用糊劑亦可含有石墨、超導碳黑(KetjenBlack)、碳奈米管、乙炔黑等導電性粒子。此等的含量係以相對於負極活性物質100質量份為0.1質量份以上20質量份以下為佳。
本發明之電極用黏合劑組成物及電極用漿體係能夠藉由將(a)樹脂、(b)鹼性化合物、視需要而添加的溶媒及其他添加劑混合或混鍊而得到。混合的情況係可
列舉:在玻璃製的燒瓶或不鏽鋼製的容器等中裝入各成分並透過機械攪拌器等將其攪拌溶解的方法、以超音波溶解的方法、以行星式攪拌消泡裝置進行攪拌溶解的方法等。又,混鍊的情況係可列舉:使用行星攪拌機、三輥磨機、球磨機、均質機等的方法。關於混合及混鍊的條件,並沒有特殊的限定。
又,為了去除異物,可將混合、混鍊後的電極用黏合劑組成物或電極用漿體以0.01μm~100μm的孔徑的過濾器過濾。過濾器的材質有聚丙烯(PP)、聚乙烯(PE)、耐綸(NY)、聚四氟乙烯(PTFE)等,但較佳為聚乙烯或耐綸。又,在樹脂組成物中含有填料或有機顏料的情況下,較佳為使用具有比這些粒徑還大的孔徑的過濾器。
能夠藉由將本發明之電極用黏合劑組成物或電極用漿體塗布在基材的單面或雙面上並使其乾燥來製作積層體。
基材係可使用導電性基材或具有導電性配線的絕緣基材。
較佳作為導電性基材的有銅、鋁、不鏽鋼、鎳、金、銀或該等的合金、碳等,但不限於此等。尤其是以銅、鋁、不鏽鋼、鎳以及含有該等的合金為更佳。
就具有導電性配線的絕緣基材而言,可列舉:使用前述導電性基材所使用的金屬或含有該等的合金的配線形成於聚醯亞胺、聚醯胺醯亞胺、聚醯胺、聚酯、丙烯酸樹脂、環氧樹脂、酚樹脂、聚矽氧樹脂基材上而成者,但不限於此等。
接著,針對本發明之積層體之製造方法舉例說明。
首先在基材上以1~500μm的厚度塗布本發明之電極用漿體。就基材而言,在將積層體用於鋰離子電池負極(以下有時省略為負極)的情況下通常會使用銅箔,在永用於鋰離子電池正極(以下有時省略為正極)或電雙層電容器正負極的情況下,可列舉:鋁箔、鎳箔、鈦箔、銅箔等,通常使用鋁箔。塗布能夠使用網版印刷、輥塗布、狹縫塗布等方法。
塗布電極用漿體後,為了去除溶媒,在100℃~250℃下加熱處理10分鐘~24小時。為了抑制水分的混入,較佳為在氮氣等不活性氣體中或真空中進行加熱。
接著針對使用本發明之正極及負極的鋰離子電池、電雙層電容器進行說明。
藉由將對本發明之正極與負極透過隔離膜積層複數個而成者,與電解液一起置入金屬殼體等的外裝材進行密封,能夠得到二次電池或電雙層電容器。
就隔離膜的例子而言,可列舉:聚乙烯、聚丙烯等聚烯烴、或纖維素、聚苯硫醚、聚芳醯胺、聚醯亞胺等的微多孔膜或不織布等。
為了提高耐熱性,可在隔離膜的表面塗布陶瓷等。
電解液中使用的溶媒用作參與電池的電化學反應的離子能夠移動的介質。就較佳的溶媒而言,可列舉:碳酸酯系、酯系、醚系、酮系、醇系、非質子性溶
媒。就前述碳酸酯系溶媒而言,可列舉:碳酸二甲酯(DMC)、碳酸二乙酯(DEC)、碳酸二丙酯(DPC)、碳酸甲基丙酯(MPC)、碳酸乙基丙酯(EPC)、碳酸甲基乙基酯(MEC)、碳酸乙基甲酯(EMC)、碳酸伸乙酯(EC)、碳酸伸丙酯(PC)、碳酸伸丁酯(BC)等。就前述酯系溶媒而言,可列舉:乙酸甲酯、乙酸乙酯、乙酸正丙酯、甲基丙酸鹽、乙基丙酸鹽、γ-丁內酯、癸內酯、戊內酯、甲羥戊酸內酯(mevalonolactone)、己內酯等。就前述醚系溶媒而言,可列舉:二丁基醚、四甘醇二甲醚、二甘醇二甲醚、二甲氧基乙烷、2-甲基四氫呋喃、四氫呋喃等。就前述酮系溶媒而言,可列舉:環己酮等。就前述醇系溶媒而言,可列舉:乙基醇、異丙基醇等。就前述非質子性溶媒而言,可列舉:腈類、二甲基甲醯胺等醯胺類、1,3-二氧戊環等二氧戊環類、環丁碸類等。可使用2種以上的此等溶媒,能夠根據目標的電池的性能而適當地選擇含量比。例如,在前述碳酸酯系溶媒的情況下,較佳為以1:1~1:9的體積比將環狀碳酸酯與鏈狀碳酸酯組合使用,能夠提升電解液的性能。
就電解液中使用的電解質的例子而言,可列舉:六氟磷酸鋰、氟硼酸鋰、過氯酸鋰等鋰鹽、四氟硼酸四乙銨、四氟硼酸三乙基甲基銨等銨鹽等。
為了更詳細地說明本發明,於下面列舉實施例,但本發明並不受限於這些實施例。還有,使用下面的方法進行實施例中的電極用黏合劑組成物的評價。
(1)負極的製作
將下述合成例3所得到的負極活性物質80質量份、固體成分濃度20重量%的電極用黏合劑組成物75質量份與作為助導劑的乙炔黑5質量份溶解於適量的溶劑(與製作電極用黏合劑組成物時使用者為相同者)中進行攪拌後,得到漿體狀的糊劑。使用刮刀將所得到的糊劑塗布在電解銅箔上,在110℃下乾燥30分鐘,製成電極。接著,將該電極的塗布部沖切成直徑16mm的圓形,進行150℃、24小時的真空乾燥,製作負極。
不過,僅在電極用黏合劑組成物使用聚醯亞胺前驅物溶液(組成物15)的情況下,於110℃下乾燥30分鐘後,在沖切成圓形前追加於350℃下施加熱處理1小時的步驟。
(2)電極特性評價
使用本發明之電極用黏合劑組成物,以下面的方法評價作為電池的長期可靠性。
為了測定充放電特性,使用HS Cell(寶泉(股)製),鋰離子電池的組裝是在氮氣環境下進行。在單電池(cell)內依序疊上將製作的負極沖切成直徑16mm的圓形者、將成為隔離膜的多孔膜(寶泉(股)製)沖切成直徑24mm者、作為正極之將在鋁箔上鍛燒鈷酸鋰製的活性物質而成者(寶泉(股)製)沖切成直徑16mm者,注入MIRET1(三井化學(股)製)1mL作為電解液後進行封裝,得到鋰離子電池。
將如上所述地製作的鋰離子電池,以6mA的恆定電流充電直到電池電壓達到4.2V,接著在4.2V的恆定電壓下充電直到從充電開始達到總計2小時30分鐘為止。之後,停止充電30分鐘,以6mA的恆定電流放電直到電池電壓達到2.7V,進行第1次循環的充放電。又,之後以同樣的條件重複充放電19次,針對總計20次循環,測定各循環的充電容量及放電容量。
根據下式,計算容量保持率。
容量保持率(%)=(第20次循環的放電容量/第1次循環的放電容量)×100
又,根據下式,計算初次充放電效率。
初次充放電效率(%)=(第1次循環的放電容量/第1次循環的充電容量)×100
合成例1:酚樹脂(NV-01)的合成
在乾燥氮氣氣流下,於燒瓶中置入間甲酚57g(0.6莫耳)、對甲酚38g(0.4莫耳)、37質量%甲醛水溶液75.5g(甲醛0.93莫耳)、草酸二水合物0.63g(0.005莫耳)、甲基異丁基酮264g後,將燒瓶浸在油浴中,一邊使反應液回流,一邊進行聚縮合反應4小時。之後,花費3小時將油浴的溫度升溫後,將燒瓶內的壓力減壓至30~50mmHg以去除揮發性物質,將已溶解的樹脂冷卻至室溫,得到苯酚酚醛清漆樹脂(NV-01)的聚合物固體85g。
合成例2:聚羥基苯乙烯(PHS-01)的合成
在1公升的燒瓶中裝入作為溶媒的四氫呋喃550ml、作為聚合起始劑的正丁基鋰4×10-4莫耳後,在該混合溶液中於-78℃下添加以50ml的四氫呋喃稀釋的對乙烯基苯氧基二甲基苯基甲基二甲基矽烷(p-vinylphenoxy dimethyl phenyl carbinyl dimethylsilane)25g並聚合1小時後,溶液呈現紅色。確認達到所想要的聚合度後,在反應溶液中添加甲醇結束聚合反應。將該反應混合物注入至甲醇中使聚合物沉澱,將沉澱的聚合物洗淨及乾燥,得到聚(對乙烯基苯氧基二甲基苯基甲基二甲基矽烷)。
接著,將所得到的聚(對乙烯基苯氧基二甲基苯基甲基二甲基矽烷)12g溶解於250ml的丙酮中,加入少量的鹽酸,在60℃下進行攪拌6小時後,將該混合溶液注入至乙基醚中,使聚合物沉澱,將沉澱的聚合物洗淨及乾燥,得到8g的聚羥基苯乙烯(PHS-01)的聚合物,其重量平均分子量為23,000。
合成例3:負極活性物質的合成
將粒徑約10μm的天然石墨50g(富士黑鉛(股)製、CBF1)與奈米矽粉末60g(Aldrich公司製)與碳黑10g(三菱化學(股)製、3050)混合,在球磨機中以旋轉數600rpm使其良好地分散12小時,之後在80℃下真空乾燥12小時,得到Si-C系的負極活性物質。
合成例4:聚醯亞胺前驅物溶液(PI-01)的合成
在1公升的燒瓶中加入N-甲基-2-吡咯啶酮123.3g,使對苯二胺8.1g、4,4’-二胺基二苯基醚5.0g溶解。在其中加入3,3’,4,4’-聯苯基四羧酸二酐28g,在60℃下進行攪拌6小時後,冷卻至室溫得到固體成分濃度25重量%的聚醯亞胺前驅物溶液(PI-01)。
組成物1~15
根據表1所示的摻合比,製作固體成分濃度20重量%的電極用黏合劑組成物。
對於組成物1~15,將容量保持率與初次充放電效率的評價結果示於表2。
還有,在表1中,PVDF係表示Kishida Chemical製聚偏二氟乙烯,CMC係表示Daicel製羧基甲基纖維素#2200,DMOM-PTBP、HMOM-W、熱酸產生劑N係表示下述結構。
Claims (18)
- 一種電極用黏合劑組成物,其含有(a)選自下述(a-1)~(a-3)中之至少1種的樹脂及(b)鹼性化合物,(a-1)聚羥基苯乙烯系樹脂;(a-2)側鏈具有選自羧基及磺酸基中之至少1種的聚苯乙烯系樹脂;(a-3)酚樹脂。
- 如請求項1之電極用黏合劑組成物,該(a)樹脂包含具有以下述通式(1)表示的結構之聚羥基苯乙烯系樹脂,
- 如請求項1或2之電極用黏合劑組成物,其相對於該(a)樹脂中之酚性羥基、羧基、磺酸基的總計100莫耳%而言,含有5~100莫耳%的該(b)鹼性化合物。
- 如請求項1至3中任一項之電極用黏合劑組成物,其中該(b)鹼性化合物包含選自包含鹼金屬及鹼土金屬之群組中之至少1種元素。
- 如請求項1至4中任一項之電極用黏合劑組成物,其進一步包含熱交聯劑。
- 如請求項5之電極用黏合劑組成物,其中該熱交聯劑包含具有以下述通式(2)表示的結構之化合物,
- 如請求項1至6中任一項之電極用黏合劑組成物,其進一步含有具有以下述通式(3)表示的結構之纖維素化合物,
- 如請求項1至7中任一項之電極用黏合劑組成物,其進一步含有溶媒。
- 如請求項8之電極用黏合劑組成物,其中該溶媒的80重量%以上為水。
- 一種漿體,其含有如請求項1至9中任一項之電極用黏合劑組成物與填料。
- 如請求項10之漿體,其中該填料包含具有選自包含碳、錳、鈷、鎳、鐵、矽、鈦、錫及鍺之群組中之至少1種的化合物。
- 如請求項10或11之漿體,其中該填料包含選自包含矽、氧化矽及鈦酸鋰之群組中之至少1種。
- 一種積層體,其係在導電性基材或具有導電性配線的絕緣基材的至少一面上具有由如請求項10至12中任一項之漿體製膜而成的層之積層體。
- 一種積層體之製造方法,其包含:將如請求項10至12中任一項之漿體塗布在導電性基材或具有導電性配線的絕緣基材的至少一面上形成塗布膜之步驟,以及將該塗布膜乾燥之步驟。
- 一種二次電池用電極,其具有如請求項13之積層體。
- 一種電雙層電容器用電極,其具有如請求項13之積層體。
- 一種二次電池,其具有如請求項15之二次電池用電極。
- 一種電雙層電容器,其具有如請求項16之電雙層電容器用電極。
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