TWI464939B - 鋰電池隔離膜 - Google Patents
鋰電池隔離膜 Download PDFInfo
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- TWI464939B TWI464939B TW100147276A TW100147276A TWI464939B TW I464939 B TWI464939 B TW I464939B TW 100147276 A TW100147276 A TW 100147276A TW 100147276 A TW100147276 A TW 100147276A TW I464939 B TWI464939 B TW I464939B
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- Prior art keywords
- pvdf
- polyvinylidene fluoride
- derivative
- layer
- lithium battery
- Prior art date
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- WHXSMMKQMYFTQS-UHFFFAOYSA-N Lithium Chemical compound [Li] WHXSMMKQMYFTQS-UHFFFAOYSA-N 0.000 title claims description 18
- 229910052744 lithium Inorganic materials 0.000 title claims description 18
- 239000002033 PVDF binder Substances 0.000 claims description 79
- 229920002981 polyvinylidene fluoride Polymers 0.000 claims description 79
- 229920000435 poly(dimethylsiloxane) Polymers 0.000 claims description 59
- 235000013870 dimethyl polysiloxane Nutrition 0.000 claims description 57
- 239000004205 dimethyl polysiloxane Substances 0.000 claims description 57
- -1 poly(dimethylsiloxane) Polymers 0.000 claims description 42
- 229920000139 polyethylene terephthalate Polymers 0.000 claims description 28
- 239000005020 polyethylene terephthalate Substances 0.000 claims description 28
- 229920000728 polyester Polymers 0.000 claims description 15
- 229920000642 polymer Polymers 0.000 claims description 14
- 150000002118 epoxides Chemical class 0.000 claims description 11
- 239000000463 material Substances 0.000 claims description 10
- 238000001029 thermal curing Methods 0.000 claims description 8
- 238000000576 coating method Methods 0.000 claims description 7
- 239000011248 coating agent Substances 0.000 claims description 6
- 229920001577 copolymer Polymers 0.000 claims description 5
- 229920005569 poly(vinylidene fluoride-co-hexafluoropropylene) Polymers 0.000 claims description 5
- 229920002215 polytrimethylene terephthalate Polymers 0.000 claims description 5
- 238000001723 curing Methods 0.000 claims description 4
- 239000004593 Epoxy Substances 0.000 claims description 3
- 230000008018 melting Effects 0.000 claims description 3
- 238000002844 melting Methods 0.000 claims description 3
- 229920000131 polyvinylidene Polymers 0.000 claims description 3
- LLLVZDVNHNWSDS-UHFFFAOYSA-N 4-methylidene-3,5-dioxabicyclo[5.2.2]undeca-1(9),7,10-triene-2,6-dione Chemical compound C1(C2=CC=C(C(=O)OC(=C)O1)C=C2)=O LLLVZDVNHNWSDS-UHFFFAOYSA-N 0.000 claims description 2
- 238000013007 heat curing Methods 0.000 claims description 2
- MZTRTOFFGGSUAN-UHFFFAOYSA-N CC1(C(OCCO1)O[Si](C)(C)C)C Chemical compound CC1(C(OCCO1)O[Si](C)(C)C)C MZTRTOFFGGSUAN-UHFFFAOYSA-N 0.000 claims 1
- CDCLSAPQCBVFHN-UHFFFAOYSA-N hydrazine;oxane Chemical compound NN.C1CCOCC1 CDCLSAPQCBVFHN-UHFFFAOYSA-N 0.000 claims 1
- 239000002131 composite material Substances 0.000 description 30
- 239000007787 solid Substances 0.000 description 17
- 239000004745 nonwoven fabric Substances 0.000 description 16
- SECXISVLQFMRJM-UHFFFAOYSA-N N-Methylpyrrolidone Chemical compound CN1CCCC1=O SECXISVLQFMRJM-UHFFFAOYSA-N 0.000 description 12
- 239000007789 gas Substances 0.000 description 12
- 230000035699 permeability Effects 0.000 description 12
- VLKZOEOYAKHREP-UHFFFAOYSA-N n-Hexane Chemical compound CCCCCC VLKZOEOYAKHREP-UHFFFAOYSA-N 0.000 description 10
- ZWEHNKRNPOVVGH-UHFFFAOYSA-N 2-Butanone Chemical compound CCC(C)=O ZWEHNKRNPOVVGH-UHFFFAOYSA-N 0.000 description 9
- 238000003848 UV Light-Curing Methods 0.000 description 7
- 238000001035 drying Methods 0.000 description 6
- 238000002074 melt spinning Methods 0.000 description 6
- 238000007711 solidification Methods 0.000 description 6
- 230000008023 solidification Effects 0.000 description 6
- 238000005406 washing Methods 0.000 description 6
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 description 6
- XTDKZSUYCXHXJM-UHFFFAOYSA-N 2-methoxyoxane Chemical compound COC1CCCCO1 XTDKZSUYCXHXJM-UHFFFAOYSA-N 0.000 description 5
- 239000003054 catalyst Substances 0.000 description 5
- 238000004132 cross linking Methods 0.000 description 5
- BASFCYQUMIYNBI-UHFFFAOYSA-N platinum Chemical compound [Pt] BASFCYQUMIYNBI-UHFFFAOYSA-N 0.000 description 5
- 229920001843 polymethylhydrosiloxane Polymers 0.000 description 5
- 238000002360 preparation method Methods 0.000 description 5
- 239000003431 cross linking reagent Substances 0.000 description 4
- 239000002904 solvent Substances 0.000 description 4
- LYCAIKOWRPUZTN-UHFFFAOYSA-N Ethylene glycol Chemical compound OCCO LYCAIKOWRPUZTN-UHFFFAOYSA-N 0.000 description 2
- 230000004888 barrier function Effects 0.000 description 2
- 239000003792 electrolyte Substances 0.000 description 2
- 238000000034 method Methods 0.000 description 2
- OFXSXYCSPVKZPF-UHFFFAOYSA-N methoxyperoxymethane Chemical compound COOOC OFXSXYCSPVKZPF-UHFFFAOYSA-N 0.000 description 2
- VOQDCMULDZDDLP-UHFFFAOYSA-N 2-methoxy-2,3-dimethyloxane Chemical compound CC1C(OCCC1)(C)OC VOQDCMULDZDDLP-UHFFFAOYSA-N 0.000 description 1
- MMINFSMURORWKH-UHFFFAOYSA-N 3,6-dioxabicyclo[6.2.2]dodeca-1(10),8,11-triene-2,7-dione Chemical compound O=C1OCCOC(=O)C2=CC=C1C=C2 MMINFSMURORWKH-UHFFFAOYSA-N 0.000 description 1
- VEXZGXHMUGYJMC-UHFFFAOYSA-M Chloride anion Chemical compound [Cl-] VEXZGXHMUGYJMC-UHFFFAOYSA-M 0.000 description 1
- 239000004971 Cross linker Substances 0.000 description 1
- VGGSQFUCUMXWEO-UHFFFAOYSA-N Ethene Chemical compound C=C VGGSQFUCUMXWEO-UHFFFAOYSA-N 0.000 description 1
- 239000005977 Ethylene Substances 0.000 description 1
- 150000001335 aliphatic alkanes Chemical class 0.000 description 1
- 230000000052 comparative effect Effects 0.000 description 1
- 230000006835 compression Effects 0.000 description 1
- 238000007906 compression Methods 0.000 description 1
- 238000005336 cracking Methods 0.000 description 1
- 125000004956 cyclohexylene group Chemical group 0.000 description 1
- 238000004880 explosion Methods 0.000 description 1
- WGCNASOHLSPBMP-UHFFFAOYSA-N hydroxyacetaldehyde Natural products OCC=O WGCNASOHLSPBMP-UHFFFAOYSA-N 0.000 description 1
- 238000013021 overheating Methods 0.000 description 1
- KKEYFWRCBNTPAC-UHFFFAOYSA-L terephthalate(2-) Chemical compound [O-]C(=O)C1=CC=C(C([O-])=O)C=C1 KKEYFWRCBNTPAC-UHFFFAOYSA-L 0.000 description 1
Classifications
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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
- H01M10/00—Secondary cells; Manufacture thereof
- H01M10/42—Methods or arrangements for servicing or maintenance of secondary cells or secondary half-cells
- H01M10/4235—Safety or regulating additives or arrangements in electrodes, separators or electrolyte
-
- C—CHEMISTRY; METALLURGY
- C09—DYES; PAINTS; POLISHES; NATURAL RESINS; ADHESIVES; COMPOSITIONS NOT OTHERWISE PROVIDED FOR; APPLICATIONS OF MATERIALS NOT OTHERWISE PROVIDED FOR
- C09D—COATING COMPOSITIONS, e.g. PAINTS, VARNISHES OR LACQUERS; FILLING PASTES; CHEMICAL PAINT OR INK REMOVERS; INKS; CORRECTING FLUIDS; WOODSTAINS; PASTES OR SOLIDS FOR COLOURING OR PRINTING; USE OF MATERIALS THEREFOR
- C09D1/00—Coating compositions, e.g. paints, varnishes or lacquers, based on inorganic substances
-
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- D06—TREATMENT OF TEXTILES OR THE LIKE; LAUNDERING; FLEXIBLE MATERIALS NOT OTHERWISE PROVIDED FOR
- D06N—WALL, FLOOR, OR LIKE COVERING MATERIALS, e.g. LINOLEUM, OILCLOTH, ARTIFICIAL LEATHER, ROOFING FELT, CONSISTING OF A FIBROUS WEB COATED WITH A LAYER OF MACROMOLECULAR MATERIAL; FLEXIBLE SHEET MATERIAL NOT OTHERWISE PROVIDED FOR
- D06N3/00—Artificial leather, oilcloth or other material obtained by covering fibrous webs with macromolecular material, e.g. resins, rubber or derivatives thereof
- D06N3/0002—Artificial leather, oilcloth or other material obtained by covering fibrous webs with macromolecular material, e.g. resins, rubber or derivatives thereof characterised by the substrate
- D06N3/0011—Artificial leather, oilcloth or other material obtained by covering fibrous webs with macromolecular material, e.g. resins, rubber or derivatives thereof characterised by the substrate using non-woven fabrics
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- D06N3/00—Artificial leather, oilcloth or other material obtained by covering fibrous webs with macromolecular material, e.g. resins, rubber or derivatives thereof
- D06N3/0002—Artificial leather, oilcloth or other material obtained by covering fibrous webs with macromolecular material, e.g. resins, rubber or derivatives thereof characterised by the substrate
- D06N3/0015—Artificial leather, oilcloth or other material obtained by covering fibrous webs with macromolecular material, e.g. resins, rubber or derivatives thereof characterised by the substrate using fibres of specified chemical or physical nature, e.g. natural silk
- D06N3/0036—Polyester fibres
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- D06—TREATMENT OF TEXTILES OR THE LIKE; LAUNDERING; FLEXIBLE MATERIALS NOT OTHERWISE PROVIDED FOR
- D06N—WALL, FLOOR, OR LIKE COVERING MATERIALS, e.g. LINOLEUM, OILCLOTH, ARTIFICIAL LEATHER, ROOFING FELT, CONSISTING OF A FIBROUS WEB COATED WITH A LAYER OF MACROMOLECULAR MATERIAL; FLEXIBLE SHEET MATERIAL NOT OTHERWISE PROVIDED FOR
- D06N3/00—Artificial leather, oilcloth or other material obtained by covering fibrous webs with macromolecular material, e.g. resins, rubber or derivatives thereof
- D06N3/0043—Artificial leather, oilcloth or other material obtained by covering fibrous webs with macromolecular material, e.g. resins, rubber or derivatives thereof characterised by their foraminous structure; Characteristics of the foamed layer or of cellular layers
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- D06—TREATMENT OF TEXTILES OR THE LIKE; LAUNDERING; FLEXIBLE MATERIALS NOT OTHERWISE PROVIDED FOR
- D06N—WALL, FLOOR, OR LIKE COVERING MATERIALS, e.g. LINOLEUM, OILCLOTH, ARTIFICIAL LEATHER, ROOFING FELT, CONSISTING OF A FIBROUS WEB COATED WITH A LAYER OF MACROMOLECULAR MATERIAL; FLEXIBLE SHEET MATERIAL NOT OTHERWISE PROVIDED FOR
- D06N3/00—Artificial leather, oilcloth or other material obtained by covering fibrous webs with macromolecular material, e.g. resins, rubber or derivatives thereof
- D06N3/04—Artificial leather, oilcloth or other material obtained by covering fibrous webs with macromolecular material, e.g. resins, rubber or derivatives thereof with macromolecular compounds obtained by reactions only involving carbon-to-carbon unsaturated bonds
- D06N3/047—Artificial leather, oilcloth or other material obtained by covering fibrous webs with macromolecular material, e.g. resins, rubber or derivatives thereof with macromolecular compounds obtained by reactions only involving carbon-to-carbon unsaturated bonds with fluoropolymers
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- D06—TREATMENT OF TEXTILES OR THE LIKE; LAUNDERING; FLEXIBLE MATERIALS NOT OTHERWISE PROVIDED FOR
- D06N—WALL, FLOOR, OR LIKE COVERING MATERIALS, e.g. LINOLEUM, OILCLOTH, ARTIFICIAL LEATHER, ROOFING FELT, CONSISTING OF A FIBROUS WEB COATED WITH A LAYER OF MACROMOLECULAR MATERIAL; FLEXIBLE SHEET MATERIAL NOT OTHERWISE PROVIDED FOR
- D06N3/00—Artificial leather, oilcloth or other material obtained by covering fibrous webs with macromolecular material, e.g. resins, rubber or derivatives thereof
- D06N3/12—Artificial leather, oilcloth or other material obtained by covering fibrous webs with macromolecular material, e.g. resins, rubber or derivatives thereof with macromolecular compounds obtained otherwise than by reactions only involving carbon-to-carbon unsaturated bonds, e.g. gelatine proteins
- D06N3/128—Artificial leather, oilcloth or other material obtained by covering fibrous webs with macromolecular material, e.g. resins, rubber or derivatives thereof with macromolecular compounds obtained otherwise than by reactions only involving carbon-to-carbon unsaturated bonds, e.g. gelatine proteins with silicon polymers
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- D—TEXTILES; PAPER
- D06—TREATMENT OF TEXTILES OR THE LIKE; LAUNDERING; FLEXIBLE MATERIALS NOT OTHERWISE PROVIDED FOR
- D06N—WALL, FLOOR, OR LIKE COVERING MATERIALS, e.g. LINOLEUM, OILCLOTH, ARTIFICIAL LEATHER, ROOFING FELT, CONSISTING OF A FIBROUS WEB COATED WITH A LAYER OF MACROMOLECULAR MATERIAL; FLEXIBLE SHEET MATERIAL NOT OTHERWISE PROVIDED FOR
- D06N3/00—Artificial leather, oilcloth or other material obtained by covering fibrous webs with macromolecular material, e.g. resins, rubber or derivatives thereof
- D06N3/18—Artificial leather, oilcloth or other material obtained by covering fibrous webs with macromolecular material, e.g. resins, rubber or derivatives thereof with two layers of different macromolecular materials
- D06N3/183—Artificial leather, oilcloth or other material obtained by covering fibrous webs with macromolecular material, e.g. resins, rubber or derivatives thereof with two layers of different macromolecular materials the layers are one next to the other
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- H01M—PROCESSES OR MEANS, e.g. BATTERIES, FOR THE DIRECT CONVERSION OF CHEMICAL ENERGY INTO ELECTRICAL ENERGY
- H01M50/00—Constructional details or processes of manufacture of the non-active parts of electrochemical cells other than fuel cells, e.g. hybrid cells
- H01M50/40—Separators; Membranes; Diaphragms; Spacing elements inside cells
- H01M50/409—Separators, membranes or diaphragms characterised by the material
- H01M50/411—Organic material
- H01M50/414—Synthetic resins, e.g. thermoplastics or thermosetting resins
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- H01M—PROCESSES OR MEANS, e.g. BATTERIES, FOR THE DIRECT CONVERSION OF CHEMICAL ENERGY INTO ELECTRICAL ENERGY
- H01M50/00—Constructional details or processes of manufacture of the non-active parts of electrochemical cells other than fuel cells, e.g. hybrid cells
- H01M50/40—Separators; Membranes; Diaphragms; Spacing elements inside cells
- H01M50/409—Separators, membranes or diaphragms characterised by the material
- H01M50/411—Organic material
- H01M50/414—Synthetic resins, e.g. thermoplastics or thermosetting resins
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- H01M50/00—Constructional details or processes of manufacture of the non-active parts of electrochemical cells other than fuel cells, e.g. hybrid cells
- H01M50/40—Separators; Membranes; Diaphragms; Spacing elements inside cells
- H01M50/409—Separators, membranes or diaphragms characterised by the material
- H01M50/449—Separators, membranes or diaphragms characterised by the material having a layered structure
- H01M50/454—Separators, membranes or diaphragms characterised by the material having a layered structure comprising a non-fibrous layer and a fibrous layer superimposed on one another
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- H01M50/40—Separators; Membranes; Diaphragms; Spacing elements inside cells
- H01M50/409—Separators, membranes or diaphragms characterised by the material
- H01M50/449—Separators, membranes or diaphragms characterised by the material having a layered structure
- H01M50/457—Separators, membranes or diaphragms characterised by the material having a layered structure comprising three or more layers
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- H01—ELECTRIC ELEMENTS
- H01M—PROCESSES OR MEANS, e.g. BATTERIES, FOR THE DIRECT CONVERSION OF CHEMICAL ENERGY INTO ELECTRICAL ENERGY
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Description
本發明係有關於一種鋰電池隔離膜，特別是有關於一種具有高耐熱鋰電池隔離膜。
二次鋰電池因其具有高能量密度等優點，已是電動車主要能量來源之一。隨著電動車動力需求提高，動力電池能量密度提高，電池功率輸出需求與尺寸也隨之增大，致在高功率電池運作時會產生更大量的熱。由於電解液為非水性且易燃的溶劑，因此，電池內部零件安全性的提升具有絕對必要性，若無法有效率地將熱能排除，將造成電池溫度上升。
如何防止電池因過熱而導致溶劑起火爆炸之發生，安全保證即成為重要課題之一。因此，設計一鋰電池隔離膜，使其具有控制電流，避免電解液直接接觸以及高耐熱之特性，並且具有良好之機械性質以及熱穩定性，不因電極膨脹產生破裂，或是受到壓縮而降低電池功率，以及不因耐熱性不佳破裂造成電池短路等，已是各方努力研究追求的目標。
本發明之一實施例，提供一種鋰電池隔離膜，包括：一聚酯不織布支撐材；一聚偏二氟乙烯(polyvinylidene fluoride,PVDF)或其衍生物層，形成於該聚酯不織布支撐材上；以及一紫外光固化(UV-curing)或熱固化(thermal-curing)高分子層，形成於該聚偏二氟乙烯(PVDF)或其衍生物層上。
該聚酯不織布支撐材包括聚對苯二甲酸乙二酯(poly(ethylene terephthalate),PET)、聚對苯二甲酸丙二酯(poly(propylene terephthalate),PPT)、聚對苯二甲酸環己二甲酯(poly(cyclohexylene dimethylene terephthalate),PCT)或上述之組合。
該聚偏二氟乙烯(PVDF)或其衍生物層包括聚偏二氟乙烯(PVDF)、聚偏二氟乙烯-六氟丙烯(PVDF-HFP)共聚物、聚偏二氟乙烯-三氟氯乙烯(PVDF-CTFE)共聚物或其衍生物或組合。該聚偏二氟乙烯(PVDF)或其衍生物層之熔點介於160~175℃。該聚偏二氟乙烯(PVDF)或其衍生物層之塗佈量(coating weight)介於35.6~89g/m2
。
該紫外光固化或熱固化高分子層包括聚二甲基矽氧烷(poly(dimethylsiloxane),PDMS)或環氧化物。該聚二甲基矽氧烷(PDMS)係由末端具有二甲基乙烯基(dimethylvinyl)、二甲基己烯基(dimethylhexenyl)或三甲基矽氧烷基(trimethylsiloxy)之二甲基矽氧烷或其組合所製備。該聚二甲基矽氧烷(PDMS)為交聯型聚二甲基矽氧烷。該紫外光固化或熱固化高分子層之塗佈量(coating weight)介於19.4~36.4g/m2
。
本發明所製備之複合隔離膜包含：(1)多孔性聚酯不織布、(2)聚偏二氟乙烯(PVDF)或其衍生物以及(3)例如聚二甲基矽氧烷(PDMS)或環氧化物(epoxy)的紫外光固化(UV-curing)或熱固化(thermal-curing)高分子等三種材料，其中例如聚二甲基矽氧烷(PDMS)或環氧化物(epoxy)的紫外光固化(UV-curing)或熱固化(thermal-curing)高分子之功能為調整整體複合隔離膜之氣體穿透度，而聚偏二氟乙烯(PVDF)或其衍生物則主要扮演具有耐熱功能的隔離層角色，另多孔性聚酯不織布則作為高溫下具備尺寸安定性的支撐層。本發明由上述三種材料所製備而成的複合隔離膜可有效提升鋰電池使用之安全性。
為讓本發明之上述目的、特徵及優點能更明顯易懂，下文特舉一較佳實施例，作詳細說明如下：
本發明之一實施例，提供一種鋰電池隔離膜。鋰電池隔離膜包括一聚酯不織布支撐材、一聚偏二氟乙烯(polyvinylidene fluoride,PVDF)或其衍生物層以及一紫外光固化(UV-curing)或熱固化(thermal-curing)高分子層。聚偏二氟乙烯(PVDF)或其衍生物層形成於聚酯不織布支撐材上。紫外光固化或熱固化高分子層形成於聚偏二氟乙烯(PVDF)或其衍生物層上。
上述聚酯不織布支撐材可包括聚對苯二甲酸乙二酯(poly(ethylene terephthalate),PET)、聚對苯二甲酸丙二酯(poly(propylene terephthalate),PPT)、聚對苯二甲酸環己二甲酯(poly(cyclohexylene dimethylene terephthalate),PCT)或其組合，例如聚對苯二甲酸乙二酸環己二甲酯(poly(cyclohexylene dimethylene terephthalate) acid,PCTA)或聚對苯二甲酸乙二醇環己二甲酯(poly(cyclohexylene dimethylene terephthalate) glycol,PCTG)。
上述聚偏二氟乙烯(PVDF)或其衍生物層為多孔性，其可包括聚偏二氟乙烯(PVDF)、聚偏二氟乙烯-六氟丙烯(PVDF-HFP)共聚物、聚偏二氟乙烯-三氟氯乙烯(PVDF-CTFE)共聚物或其衍生物或組合，熔點介於160~175℃，塗佈量(coating weight)介於35.6~89g/m2
。
上述紫外光固化或熱固化高分子層可包括聚二甲基矽氧烷(poly(dimethylsiloxane),PDMS)或環氧化物，其塗佈量(coating weight)介於19.4~36.4g/m2
。上述聚二甲基矽氧烷(PDMS)可由末端具有二甲基乙烯基(dimethylvinyl)、二甲基己烯基(dimethylhexenyl)或三甲基矽氧烷基(trimethylsiloxy)之二甲基矽氧烷或其組合所製備。上述聚二甲基矽氧烷(PDMS)可為交聯型聚二甲基矽氧烷。
本發明之一實施例，提供一種鋰電池隔離膜之製備方法。在一實施例中，所製備的隔離膜為”三層”複合隔離膜(A/B/C)。A層為多孔性聚酯不織布，例如聚對苯二甲酸乙二酯(PET)、聚對苯二甲酸丙二酯(PPT)、聚對苯二甲酸環己二甲酯(PCT)或其組合，膜厚約30~40μm。B層為聚偏二氟乙烯(PVDF)或其衍生物，例如聚偏二氟乙烯(PVDF)、聚偏二氟乙烯-六氟丙烯(PVDF-HFP)共聚物、聚偏二氟乙烯-三氟氯乙烯(PVDF-CTFE)共聚物或其衍生物或組合。C層為紫外光固化(UV-curing)或熱固化(thermal-curing)高分子，例如聚二甲基矽氧烷(PDMS)或環氧化物。A層是以熔融噴絲或是濕式抄紙(wet-laid)製備而成。再將聚偏二氟乙烯(PVDF)或其衍生物溶解於例如N-甲基吡咯酮(N-methyl pyrrolidone,NMP)的溶劑中形成固含量介於10~25wt%之溶液。再將此溶液以濕式塗佈法塗佈在A層上，經水之凝固、清洗及乾燥後，製備得B層。隨後，將聚二甲基矽氧烷(PDMS)或環氧化物溶解(稀釋)於例如正己烷(n-hexane)或丁酮(MEK)的溶劑中配製成固含量介於40~75wt%之聚二甲基矽氧烷(PDMS)或環氧化物溶液。
之後，分別加入相對於聚二甲基矽氧烷(PDMS)固含量之5wt%，例如甲基氫矽氧烷(methyl hydrogen siloxane)之交聯劑與相對於聚二甲基矽氧烷(PDMS)或環氧化物固含量之5wt%，例如鉑金屬錯合物的催化劑於上述聚二甲基矽氧烷(PDMS)溶液，或是將環氧化物溶液稀釋於丁酮中，待攪拌均勻後，將聚二甲基矽氧烷(PDMS)或環氧化物溶液塗佈於聚偏二氟乙烯(PVDF)或其衍生物層/聚酯不織布上。經100~120℃交聯反應後，即形成本發明複合隔離膜。
本發明所製備之複合隔離膜包含：(1)多孔性聚酯不織布、(2)聚偏二氟乙烯(PVDF)或其衍生物以及(3)例如聚二甲基矽氧烷(PDMS)或環氧化物(epoxy)的紫外光固化(UV-curing)或熱固化(thermal-curing)高分子等三種材料，其中例如聚二甲基矽氧烷(PDMS)或環氧化物(epoxy)的紫外光固化(UV-curing)或熱固化(thermal-curing)高分子之功能為調整整體複合隔離膜之氣體穿透度，而聚偏二氟乙烯(PVDF)或其衍生物則主要扮演具有耐熱功能的隔離層角色，另多孔性聚酯不織布則作為高溫製程下具備尺寸安定性的支撐層。本發明由上述三種材料所製備而成的複合隔離膜可有效提升鋰電池使用之安全性。
【實施例1】
本發明隔離膜之製備(1)
本實施例所製備的隔離膜為三層複合隔離膜(A/B/C)。A層為多孔性聚對苯二甲酸乙二酯(PET)不織布，膜厚約30~40μm，B層為聚偏二氟乙烯(PVDF)，C層為聚二甲基矽氧烷(PDMS)。A層是以熔融噴絲壓製而製成。再將聚偏二氟乙烯(PVDF)溶解於N-甲基吡咯酮(N-methyl pyrrolidone,NMP)中形成固含量14wt%之溶液。再將此溶液塗佈在A層上，經水之凝固、清洗及乾燥後，製備得B層。隨後，將聚二甲基矽氧烷(PDMS)溶解(稀釋)於正己烷(n-hexane)中配製成固含量40wt%之溶液。隨即分別加入5wt%甲基氫矽氧烷(methyl hydrogen siloxane)(交聯劑)與5wt%鉑金屬錯合物(催化劑)，上述含量以聚二甲基矽氧烷(PDMS)固含量為基準。待攪拌均勻後，將聚二甲基矽氧烷(PDMS)溶液塗佈於聚偏二氟乙烯(PVDF)/聚對苯二甲酸乙二酯(PET)不織布上。經120℃交聯反應後，即形成本實施例複合隔離膜。本實施例複合隔離膜的氣體穿透度(Gurley值)約為6.3sec/10cc，抗張強度為305kgf/cm2
。此複合隔離膜經過200℃、烘烤20分鐘後仍能保有隔離膜之完整性，如第1圖所示，此時，其氣體穿透度(Gurley值)約為3.1sec/10cc。
【實施例2】
本發明隔離膜之製備(2)
本實施例所製備的隔離膜為三層複合隔離膜(A/B/C)。A層為多孔性聚對苯二甲酸乙二酯(PET)不織布，膜厚約30~40μm，B層為聚偏二氟乙烯(PVDF)，C層為聚二甲基矽氧烷(PDMS)。A層是以熔融噴絲壓製而製成。再將聚偏二氟乙烯(PVDF)溶解於N-甲基吡咯酮(N-methyl pyrrolidone,NMP)中形成固含量14wt%之溶液。再將此溶液塗佈在A層上，經水之凝固、清洗及乾燥後，製備得B層。隨後，將聚二甲基矽氧烷(PDMS)溶解(稀釋)於正己烷(n-hexane)中配製成固含量50wt%之溶液。隨即分別加入5wt%甲基氫矽氧烷(methyl hydrogen siloxane)(交聯劑)與5wt%鉑金屬錯合物(催化劑)，上述含量以聚二甲基矽氧烷(PDMS)固含量為基準。待攪拌均勻後，將聚二甲基矽氧烷(PDMS)溶液塗佈於聚偏二氟乙烯(PVDF)/聚對苯二甲酸乙二酯(PET)不織布上。經120℃交聯反應後，即形成本實施例複合隔離膜。本實施例複合隔離膜的氣體穿透度(Gurley值)約為21.2sec/10cc，抗張強度為325 kgf/cm2
。此複合隔離膜經過200℃、烘烤20分鐘後仍能保有隔離膜之完整性，此時，其氣體穿透度(Gurley值)約為10.6 sec/10cc。
【實施例3】
本發明隔離膜之製備(3)
本實施例所製備的隔離膜為三層複合隔離膜(A/B/C)。A層為多孔性聚對苯二甲酸乙二酯(PET)不織布，膜厚約30~40μm，B層為聚偏二氟乙烯(PVDF)，C層為聚二甲基矽氧烷(PDMS)。A層是以熔融噴絲壓製而製成。再將聚偏二氟乙烯(PVDF)溶解於N-甲基吡咯酮(N-methyl pyrrolidone,NMP)中形成固含量14wt%之溶液。再將此溶液塗佈在A層上，經水之凝固、清洗及乾燥後，製備得B層。隨後，將聚二甲基矽氧烷(PDMS)溶解(稀釋)於正己烷(n-hexane)中配製成固含量60wt%之溶液。隨即分別加入5wt%甲基氫矽氧烷(methyl hydrogen siloxane)(交聯劑)與5wt%鉑金屬錯合物(催化劑)，上述含量以聚二甲基矽氧烷(PDMS)固含量為基準。待攪拌均勻後，將聚二甲基矽氧烷(PDMS)溶液塗佈於聚偏二氟乙烯(PVDF)/聚對苯二甲酸乙二酯(PET)不織布上。經120℃交聯反應後，即形成本實施例複合隔離膜。本實施例複合隔離膜的氣體穿透度(Gurley值)約為79.3sec/10cc，抗張強度為350kgf/cm2
。此複合隔離膜經過200℃、烘烤20分鐘後仍能保有隔離膜之完整性，此時，其氣體穿透度(Gurley值)約為46.5sec/10cc。
【實施例4】
本發明隔離膜之製備(4)
本實施例所製備的隔離膜為三層複合隔離膜(A/B/C)。A層為多孔性聚對苯二甲酸乙二酯(PET)不織布，膜厚約30~40μm，B層為聚偏二氟乙烯(PVDF)，C層為聚二甲基矽氧烷(PDMS)。A層是以熔融噴絲壓製而製成。再將聚偏二氟乙烯(PVDF)溶解於N-甲基吡咯酮(N-methyl pyrrolidone,NMP)中形成固含量14wt%之溶液。再將此溶液塗佈在A層上，經水之凝固、清洗及乾燥後，製備得B層。隨後，將聚二甲基矽氧烷(PDMS)溶解(稀釋)於正己烷(n-hexane)中配製成固含量75wt%之溶液。隨即分別加入5wt%甲基氫矽氧烷(methyl hydrogen siloxane)(交聯劑)與5wt%鉑金屬錯合物(催化劑)，上述含量以聚二甲基矽氧烷(PDMS)固含量為基準。待攪拌均勻後，將聚二甲基矽氧烷(PDMS)溶液塗佈於聚偏二氟乙烯(PVDF)/聚對苯二甲酸乙二酯(PET)不織布上。經120℃交聯反應後，即形成本實施例複合隔離膜。本實施例複合隔離膜的氣體穿透度(Gurley值)約為185.2sec/10cc，抗張強度為411kgf/cm2
。此複合隔離膜經過200℃、烘烤20分鐘後仍能保有隔離膜之完整性，此時，其氣體穿透度(Gurley值)約為32sec/10cc。
【比較實施例1】
習知隔離膜之製備
本實施例所製備的隔離膜為二層複合隔離膜(A/B)。A層為多孔性聚對苯二甲酸乙二酯(PET)不織布，膜厚約30~40μm，B層為聚偏二氟乙烯(PVDF)。A層是以熔融噴絲壓製而製成。再將聚偏二氟乙烯(PVDF)溶解於N-甲基吡咯酮(N-methyl pyrrolidone,NMP)中形成固含量14wt%之溶液。再將此溶液塗佈在A層上，經水之凝固、清洗及乾燥後，製備得B層，即形成本實施例複合隔離膜。本實施例複合隔離膜的氣體穿透度(Gurley值)約為1.5sec/10cc，抗張強度為290kgf/cm2
。此複合隔離膜經過200℃、烘烤20分鐘後複合隔離膜的氣體穿透度(Gurley值)小於1sec/10cc而無法量測，不適用於電池隔離膜。
雖然本發明已以較佳實施例揭露如上，然其並非用以限定本發明，任何熟習此項技藝者，在不脫離本發明之精神和範圍內，當可作更動與潤飾，因此本發明之保護範圍當視後附之申請專利範圍所界定者為準。
第1圖係根據本發明之一實施例，經200℃、烘烤20分鐘後，本發明複合隔離膜之態樣。
Claims (7)
- 一種鋰電池隔離膜，包括：一聚酯不織布支撐材；一聚偏二氟乙烯(polyvinylidene fluoride,PVDF)或其衍生物層，形成於該聚酯不織布支撐材上；以及一紫外光固化(UV-curing)或熱固化(thermal-curing)高分子層，形成於該聚偏二氟乙烯(PVDF)或其衍生物層上，其中該紫外光固化或熱固化高分子層包括聚二甲基矽氧烷(poly(dimethylsiloxane),PDMS)或環氧化物(Epoxy)，且該紫外光固化或熱固化高分子層之塗佈量(coating weight)介於19.4~36.4g/m2 。
- 如申請專利範圍第1項所述之鋰電池隔離膜，其中該聚酯不織布支撐材包括聚對苯二甲酸乙二酯(poly(ethylene terephthalate),PET)、聚對苯二甲酸丙二酯(poly(propylene terephthalate),PPT)、聚對苯二甲酸環己二甲酯(poly(cyclohexylene dimethylene terephthalate),PCT)或其組合。
- 如申請專利範圍第1項所述之鋰電池隔離膜，其中該聚偏二氟乙烯(PVDF)或其衍生物層包括聚偏二氟乙烯(PVDF)、聚偏二氟乙烯-六氟丙烯(PVDF-HFP)共聚物、聚偏二氟乙烯-三氟氯乙烯(PVDF-CTFE)共聚物或其衍生物或組合。
- 如申請專利範圍第1項所述之鋰電池隔離膜，其中該聚偏二氟乙烯(PVDF)或其衍生物層之熔點介於160~175℃。
- 如申請專利範圍第1項所述之鋰電池隔離膜，其中該聚二甲基矽氧烷(PDMS)係由末端具有二甲基乙烯基(dimethylvinyl)、二甲基己烯基(dimethylhexenyl)或三甲基矽氧烷基(trimethylsiloxy)之二甲基矽氧烷或其組合所製備。
- 如申請專利範圍第1項所述之鋰電池隔離膜，其中該聚二甲基矽氧烷(PDMS)為交聯型聚二甲基矽氧烷。
- 如申請專利範圍第1項所述之鋰電池隔離膜，其中該聚偏二氟乙烯(PVDF)或其衍生物層之塗佈量(coating weight)介於35.6~89g/m2 。
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| KR101709697B1 (ko) | 2014-12-30 | 2017-02-23 | 삼성에스디아이 주식회사 | 리튬 이차 전지용 세퍼레이터 및 이를 포함하는 리튬 이차 전지 |
| KR101551757B1 (ko) * | 2014-12-30 | 2015-09-10 | 삼성에스디아이 주식회사 | 다공성 내열층 조성물, 다공성 내열층을 포함하는 분리막, 상기 분리막을 이용한 전기 화학 전지, 및 상기 분리막의 제조 방법 |
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Also Published As
| Publication number | Publication date |
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| CN103171208B (zh) | 2016-02-24 |
| TW201327984A (zh) | 2013-07-01 |
| US9257725B2 (en) | 2016-02-09 |
| US20130157107A1 (en) | 2013-06-20 |
| CN103171208A (zh) | 2013-06-26 |
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