TWI450907B - 製造導電聚合物分散液的方法、由其形成之導電聚合物材料及利用該導電聚合物材料之固態電容 - Google Patents
製造導電聚合物分散液的方法、由其形成之導電聚合物材料及利用該導電聚合物材料之固態電容 Download PDFInfo
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- TWI450907B TWI450907B TW101122871A TW101122871A TWI450907B TW I450907 B TWI450907 B TW I450907B TW 101122871 A TW101122871 A TW 101122871A TW 101122871 A TW101122871 A TW 101122871A TW I450907 B TWI450907 B TW I450907B
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- Prior art keywords
- conductive polymer
- conductive
- polymerization
- present
- solid electrolytic
- Prior art date
Links
- 229920001940 conductive polymer Polymers 0.000 title claims description 49
- 238000000034 method Methods 0.000 title claims description 40
- 239000007787 solid Substances 0.000 title claims description 32
- 239000003990 capacitor Substances 0.000 title claims description 24
- 239000004815 dispersion polymer Substances 0.000 title claims description 17
- 239000002861 polymer material Substances 0.000 title claims description 16
- 239000000463 material Substances 0.000 title description 8
- 238000002360 preparation method Methods 0.000 title description 3
- 150000001875 compounds Chemical class 0.000 claims description 19
- 239000002904 solvent Substances 0.000 claims description 19
- 238000006116 polymerization reaction Methods 0.000 claims description 17
- 239000007800 oxidant agent Substances 0.000 claims description 14
- 229920000447 polyanionic polymer Polymers 0.000 claims description 12
- KAESVJOAVNADME-UHFFFAOYSA-N Pyrrole Chemical compound C=1C=CNC=1 KAESVJOAVNADME-UHFFFAOYSA-N 0.000 claims description 10
- PAYRUJLWNCNPSJ-UHFFFAOYSA-N Aniline Chemical compound NC1=CC=CC=C1 PAYRUJLWNCNPSJ-UHFFFAOYSA-N 0.000 claims description 6
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- VTLYFUHAOXGGBS-UHFFFAOYSA-N Fe3+ Chemical class [Fe+3] VTLYFUHAOXGGBS-UHFFFAOYSA-N 0.000 claims description 4
- 150000007524 organic acids Chemical class 0.000 claims description 3
- 230000000379 polymerizing effect Effects 0.000 claims description 3
- 229930192474 thiophene Natural products 0.000 claims description 3
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- 150000001879 copper Chemical class 0.000 claims description 2
- 235000005985 organic acids Nutrition 0.000 claims description 2
- JRKICGRDRMAZLK-UHFFFAOYSA-L persulfate group Chemical group S(=O)(=O)([O-])OOS(=O)(=O)[O-] JRKICGRDRMAZLK-UHFFFAOYSA-L 0.000 claims description 2
- 150000007522 mineralic acids Chemical class 0.000 claims 1
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- 230000000052 comparative effect Effects 0.000 description 7
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- HVOAFLJLVONUSZ-UHFFFAOYSA-N 2-ethylperoxythiophene Chemical compound CCOOC1=CC=CS1 HVOAFLJLVONUSZ-UHFFFAOYSA-N 0.000 description 6
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- CHQMHPLRPQMAMX-UHFFFAOYSA-L sodium persulfate Chemical compound [Na+].[Na+].[O-]S(=O)(=O)OOS([O-])(=O)=O CHQMHPLRPQMAMX-UHFFFAOYSA-L 0.000 description 6
- 239000003960 organic solvent Substances 0.000 description 5
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- NWUYHJFMYQTDRP-UHFFFAOYSA-N 1,2-bis(ethenyl)benzene;1-ethenyl-2-ethylbenzene;styrene Chemical compound C=CC1=CC=CC=C1.CCC1=CC=CC=C1C=C.C=CC1=CC=CC=C1C=C NWUYHJFMYQTDRP-UHFFFAOYSA-N 0.000 description 4
- IJGRMHOSHXDMSA-UHFFFAOYSA-N Atomic nitrogen Chemical compound N#N IJGRMHOSHXDMSA-UHFFFAOYSA-N 0.000 description 4
- 229910052782 aluminium Inorganic materials 0.000 description 4
- XAGFODPZIPBFFR-UHFFFAOYSA-N aluminium Chemical compound [Al] XAGFODPZIPBFFR-UHFFFAOYSA-N 0.000 description 4
- 239000003456 ion exchange resin Substances 0.000 description 4
- 229920003303 ion-exchange polymer Polymers 0.000 description 4
- 239000000203 mixture Substances 0.000 description 4
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- 238000003756 stirring Methods 0.000 description 4
- WEVYAHXRMPXWCK-UHFFFAOYSA-N Acetonitrile Chemical compound CC#N WEVYAHXRMPXWCK-UHFFFAOYSA-N 0.000 description 3
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- QVGXLLKOCUKJST-UHFFFAOYSA-N atomic oxygen Chemical compound [O] QVGXLLKOCUKJST-UHFFFAOYSA-N 0.000 description 3
- 238000005342 ion exchange Methods 0.000 description 3
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- GUVRBAGPIYLISA-UHFFFAOYSA-N tantalum atom Chemical compound [Ta] GUVRBAGPIYLISA-UHFFFAOYSA-N 0.000 description 3
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- 230000002378 acidificating effect Effects 0.000 description 2
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- 239000011261 inert gas Substances 0.000 description 2
- 229910000358 iron sulfate Inorganic materials 0.000 description 2
- BAUYGSIQEAFULO-UHFFFAOYSA-L iron(2+) sulfate (anhydrous) Chemical compound [Fe+2].[O-]S([O-])(=O)=O BAUYGSIQEAFULO-UHFFFAOYSA-L 0.000 description 2
- RUTXIHLAWFEWGM-UHFFFAOYSA-H iron(3+) sulfate Chemical compound [Fe+3].[Fe+3].[O-]S([O-])(=O)=O.[O-]S([O-])(=O)=O.[O-]S([O-])(=O)=O RUTXIHLAWFEWGM-UHFFFAOYSA-H 0.000 description 2
- 229910000360 iron(III) sulfate Inorganic materials 0.000 description 2
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- 239000000126 substance Substances 0.000 description 2
- 150000003577 thiophenes Chemical class 0.000 description 2
- RHUYHJGZWVXEHW-UHFFFAOYSA-N 1,1-Dimethyhydrazine Chemical compound CN(C)N RHUYHJGZWVXEHW-UHFFFAOYSA-N 0.000 description 1
- YMMGRPLNZPTZBS-UHFFFAOYSA-N 2,3-dihydrothieno[2,3-b][1,4]dioxine Chemical compound O1CCOC2=C1C=CS2 YMMGRPLNZPTZBS-UHFFFAOYSA-N 0.000 description 1
- GKWLILHTTGWKLQ-UHFFFAOYSA-N 2,3-dihydrothieno[3,4-b][1,4]dioxine Chemical compound O1CCOC2=CSC=C21 GKWLILHTTGWKLQ-UHFFFAOYSA-N 0.000 description 1
- NZCKWPBBYINXJT-UHFFFAOYSA-N 3,4-dihexyl-1h-pyrrole Chemical compound CCCCCCC1=CNC=C1CCCCCC NZCKWPBBYINXJT-UHFFFAOYSA-N 0.000 description 1
- QTTXPSXLMFARIT-UHFFFAOYSA-N 3,4-dimethoxy-1h-pyrrole Chemical compound COC1=CNC=C1OC QTTXPSXLMFARIT-UHFFFAOYSA-N 0.000 description 1
- CKGUYTNEYKYAQZ-UHFFFAOYSA-N 3-hexyl-1h-pyrrole Chemical compound CCCCCCC=1C=CNC=1 CKGUYTNEYKYAQZ-UHFFFAOYSA-N 0.000 description 1
- JEDHEMYZURJGRQ-UHFFFAOYSA-N 3-hexylthiophene Chemical compound CCCCCCC=1C=CSC=1 JEDHEMYZURJGRQ-UHFFFAOYSA-N 0.000 description 1
- OTODBDQJLMYYKQ-UHFFFAOYSA-N 3-methoxy-1h-pyrrole Chemical compound COC=1C=CNC=1 OTODBDQJLMYYKQ-UHFFFAOYSA-N 0.000 description 1
- RFSKGCVUDQRZSD-UHFFFAOYSA-N 3-methoxythiophene Chemical compound COC=1C=CSC=1 RFSKGCVUDQRZSD-UHFFFAOYSA-N 0.000 description 1
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- 229920002845 Poly(methacrylic acid) Polymers 0.000 description 1
- 229920000265 Polyparaphenylene Polymers 0.000 description 1
- ZLMJMSJWJFRBEC-UHFFFAOYSA-N Potassium Chemical compound [K] ZLMJMSJWJFRBEC-UHFFFAOYSA-N 0.000 description 1
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- 150000001298 alcohols Chemical class 0.000 description 1
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- 150000003863 ammonium salts Chemical class 0.000 description 1
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- 238000006056 electrooxidation reaction Methods 0.000 description 1
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- YFKNCTBAPAZLON-UHFFFAOYSA-N n,n-dimethyl-1h-indol-2-amine Chemical compound C1=CC=C2NC(N(C)C)=CC2=C1 YFKNCTBAPAZLON-UHFFFAOYSA-N 0.000 description 1
- 229910052758 niobium Inorganic materials 0.000 description 1
- 239000010955 niobium Substances 0.000 description 1
- GUCVJGMIXFAOAE-UHFFFAOYSA-N niobium atom Chemical compound [Nb] GUCVJGMIXFAOAE-UHFFFAOYSA-N 0.000 description 1
- 229910000484 niobium oxide Inorganic materials 0.000 description 1
- URLJKFSTXLNXLG-UHFFFAOYSA-N niobium(5+);oxygen(2-) Chemical compound [O-2].[O-2].[O-2].[O-2].[O-2].[Nb+5].[Nb+5] URLJKFSTXLNXLG-UHFFFAOYSA-N 0.000 description 1
- 239000012299 nitrogen atmosphere Substances 0.000 description 1
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- BPUBBGLMJRNUCC-UHFFFAOYSA-N oxygen(2-);tantalum(5+) Chemical compound [O-2].[O-2].[O-2].[O-2].[O-2].[Ta+5].[Ta+5] BPUBBGLMJRNUCC-UHFFFAOYSA-N 0.000 description 1
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- 229910052700 potassium Inorganic materials 0.000 description 1
- 239000011591 potassium Substances 0.000 description 1
- BDERNNFJNOPAEC-UHFFFAOYSA-N propan-1-ol Chemical compound CCCO BDERNNFJNOPAEC-UHFFFAOYSA-N 0.000 description 1
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- 229910052708 sodium Inorganic materials 0.000 description 1
- 239000011734 sodium Substances 0.000 description 1
- 230000003068 static effect Effects 0.000 description 1
- 229910001936 tantalum oxide Inorganic materials 0.000 description 1
- 239000010936 titanium Substances 0.000 description 1
- 229910052719 titanium Inorganic materials 0.000 description 1
- 239000013638 trimer Substances 0.000 description 1
- 125000000391 vinyl group Chemical group [H]C([*])=C([H])[H] 0.000 description 1
- 229920002554 vinyl polymer Polymers 0.000 description 1
- 239000002699 waste material Substances 0.000 description 1
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Classifications
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01J—CHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
- B01J19/00—Chemical, physical or physico-chemical processes in general; Their relevant apparatus
- B01J19/08—Processes employing the direct application of electric or wave energy, or particle radiation; Apparatus therefor
- B01J19/12—Processes employing the direct application of electric or wave energy, or particle radiation; Apparatus therefor employing electromagnetic waves
- B01J19/122—Incoherent waves
- B01J19/126—Microwaves
-
- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08G—MACROMOLECULAR COMPOUNDS OBTAINED OTHERWISE THAN BY REACTIONS ONLY INVOLVING UNSATURATED CARBON-TO-CARBON BONDS
- C08G61/00—Macromolecular compounds obtained by reactions forming a carbon-to-carbon link in the main chain of the macromolecule
- C08G61/12—Macromolecular compounds containing atoms other than carbon in the main chain of the macromolecule
- C08G61/122—Macromolecular compounds containing atoms other than carbon in the main chain of the macromolecule derived from five- or six-membered heterocyclic compounds, other than imides
- C08G61/123—Macromolecular compounds containing atoms other than carbon in the main chain of the macromolecule derived from five- or six-membered heterocyclic compounds, other than imides derived from five-membered heterocyclic compounds
- C08G61/124—Macromolecular compounds containing atoms other than carbon in the main chain of the macromolecule derived from five- or six-membered heterocyclic compounds, other than imides derived from five-membered heterocyclic compounds with a five-membered ring containing one nitrogen atom in the ring
-
- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08G—MACROMOLECULAR COMPOUNDS OBTAINED OTHERWISE THAN BY REACTIONS ONLY INVOLVING UNSATURATED CARBON-TO-CARBON BONDS
- C08G61/00—Macromolecular compounds obtained by reactions forming a carbon-to-carbon link in the main chain of the macromolecule
- C08G61/12—Macromolecular compounds containing atoms other than carbon in the main chain of the macromolecule
- C08G61/122—Macromolecular compounds containing atoms other than carbon in the main chain of the macromolecule derived from five- or six-membered heterocyclic compounds, other than imides
- C08G61/123—Macromolecular compounds containing atoms other than carbon in the main chain of the macromolecule derived from five- or six-membered heterocyclic compounds, other than imides derived from five-membered heterocyclic compounds
- C08G61/126—Macromolecular compounds containing atoms other than carbon in the main chain of the macromolecule derived from five- or six-membered heterocyclic compounds, other than imides derived from five-membered heterocyclic compounds with a five-membered ring containing one sulfur atom in the ring
-
- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08L—COMPOSITIONS OF MACROMOLECULAR COMPOUNDS
- C08L65/00—Compositions of macromolecular compounds obtained by reactions forming a carbon-to-carbon link in the main chain; Compositions of derivatives of such polymers
-
- H—ELECTRICITY
- H01—ELECTRIC ELEMENTS
- H01B—CABLES; CONDUCTORS; INSULATORS; SELECTION OF MATERIALS FOR THEIR CONDUCTIVE, INSULATING OR DIELECTRIC PROPERTIES
- H01B1/00—Conductors or conductive bodies characterised by the conductive materials; Selection of materials as conductors
- H01B1/06—Conductors or conductive bodies characterised by the conductive materials; Selection of materials as conductors mainly consisting of other non-metallic substances
- H01B1/12—Conductors or conductive bodies characterised by the conductive materials; Selection of materials as conductors mainly consisting of other non-metallic substances organic substances
- H01B1/122—Ionic conductors
-
- H—ELECTRICITY
- H01—ELECTRIC ELEMENTS
- H01G—CAPACITORS; CAPACITORS, RECTIFIERS, DETECTORS, SWITCHING DEVICES, LIGHT-SENSITIVE OR TEMPERATURE-SENSITIVE DEVICES OF THE ELECTROLYTIC TYPE
- H01G9/00—Electrolytic capacitors, rectifiers, detectors, switching devices, light-sensitive or temperature-sensitive devices; Processes of their manufacture
- H01G9/0029—Processes of manufacture
- H01G9/0036—Formation of the solid electrolyte layer
-
- H—ELECTRICITY
- H01—ELECTRIC ELEMENTS
- H01G—CAPACITORS; CAPACITORS, RECTIFIERS, DETECTORS, SWITCHING DEVICES, LIGHT-SENSITIVE OR TEMPERATURE-SENSITIVE DEVICES OF THE ELECTROLYTIC TYPE
- H01G9/00—Electrolytic capacitors, rectifiers, detectors, switching devices, light-sensitive or temperature-sensitive devices; Processes of their manufacture
- H01G9/004—Details
- H01G9/022—Electrolytes; Absorbents
- H01G9/025—Solid electrolytes
-
- H—ELECTRICITY
- H01—ELECTRIC ELEMENTS
- H01G—CAPACITORS; CAPACITORS, RECTIFIERS, DETECTORS, SWITCHING DEVICES, LIGHT-SENSITIVE OR TEMPERATURE-SENSITIVE DEVICES OF THE ELECTROLYTIC TYPE
- H01G9/00—Electrolytic capacitors, rectifiers, detectors, switching devices, light-sensitive or temperature-sensitive devices; Processes of their manufacture
- H01G9/004—Details
- H01G9/022—Electrolytes; Absorbents
- H01G9/025—Solid electrolytes
- H01G9/028—Organic semiconducting electrolytes, e.g. TCNQ
-
- H—ELECTRICITY
- H01—ELECTRIC ELEMENTS
- H01G—CAPACITORS; CAPACITORS, RECTIFIERS, DETECTORS, SWITCHING DEVICES, LIGHT-SENSITIVE OR TEMPERATURE-SENSITIVE DEVICES OF THE ELECTROLYTIC TYPE
- H01G9/00—Electrolytic capacitors, rectifiers, detectors, switching devices, light-sensitive or temperature-sensitive devices; Processes of their manufacture
- H01G9/004—Details
- H01G9/022—Electrolytes; Absorbents
- H01G9/025—Solid electrolytes
- H01G9/032—Inorganic semiconducting electrolytes, e.g. MnO2
-
- H—ELECTRICITY
- H01—ELECTRIC ELEMENTS
- H01G—CAPACITORS; CAPACITORS, RECTIFIERS, DETECTORS, SWITCHING DEVICES, LIGHT-SENSITIVE OR TEMPERATURE-SENSITIVE DEVICES OF THE ELECTROLYTIC TYPE
- H01G9/00—Electrolytic capacitors, rectifiers, detectors, switching devices, light-sensitive or temperature-sensitive devices; Processes of their manufacture
- H01G9/15—Solid electrolytic capacitors
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- Chemical & Material Sciences (AREA)
- Chemical Kinetics & Catalysis (AREA)
- Engineering & Computer Science (AREA)
- Electrochemistry (AREA)
- Power Engineering (AREA)
- Organic Chemistry (AREA)
- Health & Medical Sciences (AREA)
- Microelectronics & Electronic Packaging (AREA)
- Medicinal Chemistry (AREA)
- Polymers & Plastics (AREA)
- Physics & Mathematics (AREA)
- Electromagnetism (AREA)
- General Health & Medical Sciences (AREA)
- Toxicology (AREA)
- Manufacturing & Machinery (AREA)
- Spectroscopy & Molecular Physics (AREA)
- Inorganic Chemistry (AREA)
- Polyoxymethylene Polymers And Polymers With Carbon-To-Carbon Bonds (AREA)
- Compositions Of Macromolecular Compounds (AREA)
Description
本發明係關於一種製備導電聚合物分散液的方法、由該方法所形成的導電聚合物材料及利用該導電聚合物材料之固態電容。
近年來,由於導電聚合物在電性的提升及加工性的改良,其經濟效益逐漸獲得重視。已知的π-共軛的導電聚合物包括聚吡咯類(polypyrroles)、聚噻吩類(polythiophenes)、聚苯胺類(polyanilines)、聚伸苯基類(polyphenylenes)、聚乙炔類(polyacetylenes)及聚(對伸苯基-伸乙烯基類)及其衍生物等。導電聚合物層在工業上有許多用途,例如電容中的對電極、固態電解質及作為抗靜電/靜電耗散之塗膜等。
導電聚合物經由單體(例如視需要經取代之噻吩類、苯胺類及吡咯類及彼等之寡聚物及其衍生物)之化學氧化或電化學氧化方法而製備,其中因製程較簡單且較便宜,化學氧化方式之聚合作用係最為普及。例如US 5,035,926揭示一種氧化聚合3,4-伸乙基二氧基噻吩(3,4-ethylenedioxythiophene,EDOT或EDT)以製備聚(3,4-伸乙基二氧基噻吩)之方法,所產生之聚噻吩具有高的導電係數。
然而,上述聚(3,4-伸乙基二氧基噻吩)在加工處理上並不容易,因此為改善其加工性,US 5,300,575揭露利用衍生自聚對苯乙烯磺酸之聚陰離子(polyanion),以使上述導電聚合物可具有較高的聚合速率且可在液態中穩定地形成,其在一般大氣濕度下亦可保有抗靜電性質(參US 5,300,575第1欄第60至68行)。然
而,此方式的缺點為其聚合反應時間長達24小時。
US 2011/0049433提出一種改良之製備水性或非水性導電聚合物分散液之方法,其係利用超音波來縮短反應時間及降低分散液之黏度。此方式雖可藉由超音波縮短其反應時間,然而其反應仍需添加硫酸鐵作為觸媒以催化氧化劑之反應。而額外添加之觸媒在後續去離子製程所產生之離子交換樹脂廢棄物,會對環境帶來不良影響。
US 2011/0122546及US 2011/0233450皆提到一種製備導電聚合物之改良方法,其可產生具高導電性之導電高分子及具低等效串聯電阻(equivalent series resistance,ESR)之固態電容。該等方法雖未提及使用硫酸鐵作為觸媒以催化氧化劑之反應,惟其仍需至少50小時的反應時間。
鑑於上述,產業上仍迄尋求一種更經濟及對環境友善之製備導電聚合物的方法,且所產生之導電聚合物材料亦具有高導電性。
本發明之一目的即在於提供一種製備導電聚合物分散液的方法,能解決至少一上述問題。特定言之,本發明之一目的即為提供一種反應時間較短、對環境較友善之製備導電聚合物分散液的方法,由該分散液所製得之導電聚合物材料具有低表面阻抗(即高導電性)。根據本發明,該製備導電聚合物分散液的方法包括:於一溶劑中加入導電化合物、聚陰離子及氧化劑;及利用微波聚合該導電化合物。
本發明另一目的在於提供一種導電聚合物材料,其係藉由自
上述製備的導電聚合物分散液中移除溶劑所形成。
本發明再另一目的在於提供一種包含固態電解層之固態電容,該固態電解層包含前述之導電聚合物材料。
本發明再另一目的係提供一種製備固態電容的方法,其包括:於陽極上形成介電層;及於該介電層上施用前述導電聚合物分散液或將該介電層含浸於前述導電聚合物分散液中,以於該介電層上形成包含前述導電聚合物材料之固態電解層。
本發明之製備導電聚合物分散液的方法,其反應時間較目前使用的方法為短。此外,因本發明方法不需利用觸媒,其後續不需利用例如離子交換樹脂等機制回收觸媒,其對環境較友善。且本發明方法可獲得具有降低之表面阻抗的導電聚合物材料。
本發明之製備導電聚合物分散液之方法包括:於一溶劑中加入導電化合物、聚陰離子及氧化劑;及利用微波聚合該導電化合物。
本發明所使用之導電化合物一般係指可產生導電聚合物之單體及其衍生物、寡聚物及其衍生物或上述任何之組合。
可用於本發明中的單體為相關技術領域中所已知,舉例言之,可選自由吡咯(pyrrole)、噻吩(thiophene)、苯胺(aniline)及其混合物所組成之群組。
本文中所述之「寡聚物」具有本發明所屬技術領域中之一般意義,例如指由有限之前述單體所組成之化合物。舉例而言,指可產生導電聚合物之單體之二聚物、三聚物、四聚物或五聚
物等。
本文中所述之「單體之衍生物」具有本發明所屬技術領域中所知之一般意義,例如,指經取代之前述單體。
本文中所述之「寡聚物之衍生物」具有本發明所屬技術領域中所知之一般意義,例如,指經取代之前述寡聚物。
舉例而言,「吡咯」及「吡咯之衍生物」皆指經聚合後,會產生具有類似吡咯結構之導電聚合物的單體。
可用於本發明之吡咯衍生物,例如包括,但不限於:3-烷基吡咯,如3-己基吡咯;3,4-二烷基吡咯,如3,4-二己基吡咯;3-烷氧基吡咯,如3-甲氧基吡咯;及3,4-二烷氧基吡咯,如3,4-二甲氧基吡咯。
可用於本發明之噻吩衍生物,例如包括但不限於:3,4-伸乙基二氧基噻吩及其衍生物;3-烷基噻吩,如3-己基噻吩;及3-烷氧基噻吩,如3-甲氧基噻吩。
可用於本發明之苯胺衍生物,例如包括但不限於:2-烷基苯胺,如2-甲基苯胺;及2-烷氧基苯胺,如2-甲氧基苯胺。
根據本發明之具體實施例,所使用之導電化合物係3,4-伸乙基二氧基噻吩或其衍生物,例如包括,但不限於:3,4-(1-烷基)伸乙基二氧基噻吩,如3,4-(1-己基)伸乙基二氧基噻吩。
本發明方法所使用導電化合物之量並未特別限制。然而,若為了得到具有可接受之導電性的導電性聚合物,該導電化合物在溶劑中之量為約0.1重量%至約20重量%,較佳為約0,1重量%至約5重量%。
可用於本發明之聚陰離子為相關技術領域中所已知者,例如
可為,聚羧酸(如聚丙烯酸、聚甲基丙烯酸或聚順丁烯二酸)、聚磺酸(如聚對苯乙烯磺酸、聚酯磺酸及聚(2-丙烯醯胺-2-甲基丙磺酸))或其鹽類。聚磺酸之鹽類例如包含,但不限於,聚磺酸之鋰鹽、鈉鹽、鉀鹽及銨鹽。較佳之聚陰離子為聚對苯乙烯磺酸。
可提供該聚陰離子之聚羧酸或聚磺酸較佳具有1,000至2,000,000,更佳具有2,000至500,000之分子量。舉例而言,聚對苯乙烯磺酸及聚丙烯酸之製備方法例如已揭露於Houben Weyl,Methoden der organischen Chemie[Methods of Organic Chemistry],vol.E 20 Makromolekulare Stoffe (Macromolecular Substances),part 2,(1987),p.1141 ff.)。
本發明所使用之聚陰離子之量並未特別限制。然而,若為了得到具有可接受導電性的導電性聚合物,該聚陰離子在溶劑中之用量為約1重量%至約20重量%,較佳為約1重量%至約5重量%。
可用於本發明之氧化劑為相關技術領域中所已知者,其包括但不限於:鐵(III)鹽類,如FeCl3
及Fe(ClO4
)3
;有機酸之鐵(III)鹽類;過氧化氫;過氧硫酸鹽類;過硫酸鹽類;過硼酸鹽類;及銅鹽,如四氟硼酸銅。較佳為有機酸之鐵鹽類或過氧硫酸鹽類,特較佳者過氧二硫酸鈉。上述氧化劑可單獨使用或合併使用。
本發明所使用之氧化劑之量並未特別限制。然而,若為了在溫和的氧化環境下,得到具有高導電性之導電性聚合物材料,該氧化劑在溶劑中之用量為約0.1重量%至約15重量%,較佳為
約0.5重量%至約5重量%。
可用於本發明中之溶劑較佳選自可與該導電化合物達到可接受的相容效果之溶劑。該溶劑可為水(較佳為去離子水)、有機溶劑或混合水之有機溶劑。有機溶劑包括:醇類,如甲醇、乙醇及丙醇;芳香烴類,如苯、甲苯及二甲苯;脂肪烴類,如己烷;及非質子極性溶劑,如N,N-二甲基甲醯胺、二甲基亞碸、乙腈及丙酮。上述有機溶劑可單獨使用或合併使用。溶劑較佳包含水、醇類有機溶劑及非質子極性溶劑中之至少一者,其較佳之選擇包括水、乙醇、二甲基亞碸、乙醇與水的混合物及二甲基亞碸與水的混合物。
如上所述,本發明方法係以微波方式進行導電化合物的聚合反應。舉例而言,可將含有導電化合物、聚陰離子及氧化劑之溶液置於微波反應器中,並施予150W至1000W功率、較佳為200W至950W功率、更佳為300W至900W之功率之能量。
根據本發明之一具體實施例,係使用介於2.0GHZ至3.0GHZ之間之微波頻率。
本發明方法係在惰性環境下進行。舉例而言,在氧化劑加入溶液前,該溶液先藉由通入惰性氣體至少5分鐘,較佳20分鐘,以除去氧及/或水氣,產生惰性環境。本文中所指惰性環境,係指溶液中溶氧度低於3ppm。合適之惰性氣體為相關領域中所熟知者,例如氬氣、氦氣或氮氣。
本發明方法之聚合反應是在約0℃至約35℃之溫度下進行;較佳係在約6℃至約29℃之溫度下進行;更佳係在約9℃至約26℃之溫度下進行。
本發明方法之聚合時間係介於約6至約23小時之間,較佳介於約5至約21小時之間,更佳介於約3至6小時之間。
本發明可進一步使用導電性加強劑(conductivity enhancer),以增強本發明之導電聚合物分散液之導電性。適用的導電性加強劑可為本發明所屬技術領域中所已知者,例如二甲基亞碸。
本發明之分散液經製備後,該分散液可進一步以鹼性及酸性離子交換樹脂(例如鹼性及酸性離子交換樹脂)處理以移除鹽類。
本發明另提供一種自上述導電聚合物分散液移除溶劑後所形成之導電聚合物材料。其中係可利用乾燥方法以自導電聚合物分散液移除溶劑。該用於乾燥之溫度未有特別限制,只要在該溫度具有移除溶劑之可能性即可。然而,該溫度之上限較佳係小於300℃,以避免因熱產生材料之劣化。乾燥時間係可隨乾燥溫度調整,但只要其不會損害到導電聚合物之導電性,其並不受特別限制。
本發明之導電聚合物材料可利用作為固態電容之固態電解層。該導電聚合物材料具有高導電性,因此可得到具有低等效串聯電阻(equivalent series resistance,ESR)之固態電容。
以下將藉由圖1說明根據本發明之一實施例之固態電解層及固態電容之製造方法。
如圖1所示,本發明之固態電容1,其包含:陽極3;介電層5,其形成於該陽極3上;陰極7;及固態電解層(圖未顯示),其位於該介電層5與該陰極7之間,其中該固態電解層係包含上述之導電聚合物材料。導線9a與9b係作為陰極7及陽極3與外部線路連接之端子。
上述固態電容,可為鋁固態電容、鉭固態電容或鈮固態電容,利用已知之材料,藉由已知之技術製成。舉例言之,固態電容主體部份可由一個經過蝕刻的導電金屬箔作為陽極箔,陽極箔表面並經過陽極氧化處理,該陽極箔且引出導線而為陽極,一個金屬箔作為陰極箔所製成,該陰極箔並引出導線而成為陰極;由氧化物或其類似物所構成之介電層係形成於陽極箔上之表面上,並介於陽極箔與陰極箔之間,上述陽極箔、陰極箔可由鋁、鉭、鈮、鋁氧化物、鉭氧化物、鈮氧化物、鋁表面鍍鈦或鋁表面鍍碳所組成。
本發明之導電聚合物分散液可在電容器中進行聚合反應或者在電容器外進行聚合反應以形成固態電解層之導電聚合物。若在電容器外進行聚合反應,上述陽極箔、陰極箔,可以塗佈或含浸(immerse)於本發明之進行聚合反應後之導電聚合物分散液,經除去溶劑後(例如利用乾燥),於介電層與陰極箔之間形成固態電解層。其中除去溶劑之方法如先前所述。
若在電容器內進行聚合反應,則可將上述陽極箔、陰極箔,先含浸(immerse)於包含導電化合物、聚陰離子及氧化劑之溶液中,再以微波方式使導電化合物聚合,並經除去溶劑後(例如利用乾燥),於介電層與陰極箔之間形成固態電解層。
或者,可將上述陽極箔、陰極箔,先含浸(immerse)於包含導電化合物之第一溶液中,再含浸於包含聚陰離子及氧化劑之第二溶液中,再以微波方式使導電化合物聚合,並經除去溶劑後(例如利用乾燥),於介電層與陰極箔之間形成固態電解層。
電容元件在內部形成固態電解層後,便可利用已知技術及材
料,形成固態電容。例如,該電容元件可裝於具有底部之盒體,而留有讓導線9a及9b露出之開口之密封元件可置於盒體頂部,密封後便可形成固態電容。
連接於陰極箔及陽極箔之導線數量並無特別限制,只要確認陰極箔及陽極箔皆有導線連接即可。陰極箔及陽極箔之數量亦無特別限制,舉例而言,陰極箔可與陽極箔一樣多,或者較多。
茲以下列具體實施態樣以進一步例示說明本發明。
將221.45克之去離子水裝入500毫升具夾套的玻璃容器中,其後,將8.75克之聚對苯乙烯磺酸(30wt%,平均分子量Mw=75,000克/莫耳)水溶液加入。溶液在攪拌過程中通氮以除氧,於氮氣環境下將1.065克之3,4-伸乙基二氧基噻吩(EDOT)加入。將22.475克之過氧二硫酸鈉(11wt%)加入後,置入微波反應器內,以500W功率、2.45GHZ之參數反應,並且持續攪拌至反應完成(以薄膜色層分析試片確認反應完全),共需時5小時,期間溶液經由恆溫控制器將循環水注入玻璃容器夾套中以控制反應溫度維持於25℃,得到一分散液。
反應完成後所得之分散液藉由添加25克之Lewatit MP 62(鹼性離子交換物質,Lanxess AG)及25克之Lewatit S 100(酸性離子交換物質,Lanxess AG)連同藉由磁性攪拌器之攪拌歷時2小時後脫鹽後,通過濾布過濾出離子交換物質。取9.5克脫鹽後之溶液、9.5克異丙醇(IPA)與1克之二甲亞碸(調整流平性及增加導電度)充分混合。取一片清潔之PET膜置於線棒塗佈機上,及2
毫升之上述之混合物,利用5號線棒均勻塗佈於該PET膜上。其後,於130℃之熱風烘箱乾燥歷時3分鐘完成。以表面阻抗儀(Mitsubishi MCP-T610)以10V電壓,量測其表面阻抗值。
反應流程與條件如實例1,惟微波反應器之參數改為800W功率、2.45GHZ。反應完全共需時4小時。
反應流程與條件如實例1,惟微波反應器之參數改為200W功率、2.45GHZ。反應完全共需時21小時。
反應流程與條件如實例1,惟不利用微波反應器,而係持續攪拌至反應完全。反應完全共需時24小時。
反應流程與條件如實例1,惟係利用150W功率、43KHZ之超音波而非微波反應器,及其反應溫度係維持在24℃。反應完全共需時13小時。
反應流程與條件如比較例2,惟於以超音波加速反應前,添加0.054克硫酸鐵作為觸媒以期縮短反應時間。反應完全共需時6小時。
反應流程與條件如比較例1,惟添加過氧二硫酸鈉水溶液時,同時添加0.054克硫酸鐵作為觸媒以期縮短反應時間。反應完全共需時22小時。
經上述過程製得之各實例與比較例之比較如以下各表。
由表1可知,不添加觸媒的情況下,利用微波不僅可大幅縮短反應時間,且也可大幅下降表面阻抗(即表面導電度提升)。
由表2可知,於攪拌或超音波反應環境中添加觸媒有助於加速反應,但其功效相較於微波反應(不添加觸媒)仍顯不夠,且表面阻抗仍較高。
由表3可知,於200W低功率的微波反應環境下仍有助於降低表面阻抗,但其縮短反應時間效果不如500 W或800 W功率者。
由以上結果可知,利用微波可縮短導電化合物之聚合時間,且降低所產生之導電聚合物之表面阻抗;此外,因本發明方法不需觸媒幫助聚合,後續並不需回收觸媒之機制,其對環境較友善。本發明可廣泛應用於需電容器之產業,例如LED燈驅動電源、電子節能燈和整流器、車用電子設備、電腦主板、變頻器、網路通訊、醫療設備電源、UPS等高端領域。
1‧‧‧固態電容
3‧‧‧陽極
5‧‧‧介電層
7‧‧‧陰極
9a‧‧‧導線
9b‧‧‧導線
圖1顯示根據本發明之一實施例之固態電容。
1‧‧‧固態電容
3‧‧‧陽極
5‧‧‧介電層
7‧‧‧陰極
9a‧‧‧導線
9b‧‧‧導線
Claims (10)
- 一種製備導電聚合物分散液之方法,其包括:加入導電化合物、聚陰離子及氧化劑於一溶劑中;及利用微波聚合該導電化合物。
- 如請求項1之方法,其中係以150W至1000W之微波能量進行該聚合反應。
- 如請求項2之方法,其中係以200W至950W之微波能量進行該聚合反應。
- 如請求項3之方法,其中係以300W至900W之微波能量進行該聚合反應。
- 如請求項1之方法,其中該微波之頻率為係介於2.0GHZ至3.0GHZ之間。
- 如請求項1之方法,其中該聚合反應係在惰性環境下進行。
- 如請求項1之方法,其中該導電化合物係選自由吡咯、噻吩及苯胺及其衍生物及寡聚物所組成之群組。
- 如請求項1之方法,其中該氧化劑係選自由鐵(III)鹽類、有機酸之鐵(III)鹽類、過氧硫酸鹽類、過硫酸鹽類、過硼酸鹽類、銅鹽及含有機基團之無機酸所組成之群組。
- 一種導電聚合物材料,其係將根據請求項1之方法所製備之導電聚合物分散液去除溶劑而得。
- 一種固態電容,其包含:陽極; 介電層,形成於該陽極上;陰極;及固態電解層,其位於該介電層與該陰極之間,其中該固態電解層包含請求項9之導電聚合物材料。
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US13/718,410 US20130342967A1 (en) | 2012-06-26 | 2012-12-18 | Method for preparing conductive polymer dispersion, conductive polymer material made therefrom and solid electrolytic capacitor using the material |
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JP7220791B2 (ja) | 2018-12-11 | 2023-02-10 | キョーセラ・エイブイエックス・コンポーネンツ・コーポレーション | 固有導電性ポリマーを含む固体電解キャパシタ |
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KR20220113704A (ko) | 2019-12-10 | 2022-08-16 | 교세라 에이브이엑스 컴포넌츠 코포레이션 | 안정성이 증가된 탄탈 커패시터 |
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