KR20240049319A - Carbon nanotube dispersion, a conductive paste using the same, an electrode paste for a secondary battery, an electrode for a secondary battery, and a secondary battery - Google Patents
Carbon nanotube dispersion, a conductive paste using the same, an electrode paste for a secondary battery, an electrode for a secondary battery, and a secondary battery Download PDFInfo
- Publication number
- KR20240049319A KR20240049319A KR1020247008880A KR20247008880A KR20240049319A KR 20240049319 A KR20240049319 A KR 20240049319A KR 1020247008880 A KR1020247008880 A KR 1020247008880A KR 20247008880 A KR20247008880 A KR 20247008880A KR 20240049319 A KR20240049319 A KR 20240049319A
- Authority
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- South Korea
- Prior art keywords
- carbon nanotube
- secondary battery
- dispersion
- electrode
- secondary batteries
- Prior art date
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- 229910003002 lithium salt Inorganic materials 0.000 description 1
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- YYZUSRORWSJGET-UHFFFAOYSA-N octanoic acid ethyl ester Natural products CCCCCCCC(=O)OCC YYZUSRORWSJGET-UHFFFAOYSA-N 0.000 description 1
- 125000002347 octyl 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])[H] 0.000 description 1
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- UWJJYHHHVWZFEP-UHFFFAOYSA-N pentane-1,1-diol Chemical compound CCCCC(O)O UWJJYHHHVWZFEP-UHFFFAOYSA-N 0.000 description 1
- 125000001997 phenyl group Chemical group [H]C1=C([H])C([H])=C(*)C([H])=C1[H] 0.000 description 1
- WVDDGKGOMKODPV-ZQBYOMGUSA-N phenyl(114C)methanol Chemical compound O[14CH2]C1=CC=CC=C1 WVDDGKGOMKODPV-ZQBYOMGUSA-N 0.000 description 1
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- RKEWSXXUOLRFBX-UHFFFAOYSA-N pimavanserin Chemical compound C1=CC(OCC(C)C)=CC=C1CNC(=O)N(C1CCN(C)CC1)CC1=CC=C(F)C=C1 RKEWSXXUOLRFBX-UHFFFAOYSA-N 0.000 description 1
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- 239000002244 precipitate Substances 0.000 description 1
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- 125000004805 propylene group Chemical group [H]C([H])([H])C([H])([*:1])C([H])([H])[*:2] 0.000 description 1
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- 229920001027 sodium carboxymethylcellulose Polymers 0.000 description 1
- RPACBEVZENYWOL-XFULWGLBSA-M sodium;(2r)-2-[6-(4-chlorophenoxy)hexyl]oxirane-2-carboxylate Chemical compound [Na+].C=1C=C(Cl)C=CC=1OCCCCCC[C@]1(C(=O)[O-])CO1 RPACBEVZENYWOL-XFULWGLBSA-M 0.000 description 1
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- PZTAGFCBNDBBFZ-UHFFFAOYSA-N tert-butyl 2-(hydroxymethyl)piperidine-1-carboxylate Chemical compound CC(C)(C)OC(=O)N1CCCCC1CO PZTAGFCBNDBBFZ-UHFFFAOYSA-N 0.000 description 1
- FAGUFWYHJQFNRV-UHFFFAOYSA-N tetraethylenepentamine Chemical compound NCCNCCNCCNCCN FAGUFWYHJQFNRV-UHFFFAOYSA-N 0.000 description 1
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- YODZTKMDCQEPHD-UHFFFAOYSA-N thiodiglycol Chemical compound OCCSCCO YODZTKMDCQEPHD-UHFFFAOYSA-N 0.000 description 1
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Classifications
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- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01B—NON-METALLIC ELEMENTS; COMPOUNDS THEREOF; METALLOIDS OR COMPOUNDS THEREOF NOT COVERED BY SUBCLASS C01C
- C01B32/00—Carbon; Compounds thereof
- C01B32/15—Nano-sized carbon materials
- C01B32/158—Carbon nanotubes
- C01B32/168—After-treatment
- C01B32/174—Derivatisation; Solubilisation; Dispersion in solvents
-
- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01B—NON-METALLIC ELEMENTS; COMPOUNDS THEREOF; METALLOIDS OR COMPOUNDS THEREOF NOT COVERED BY SUBCLASS C01C
- C01B32/00—Carbon; Compounds thereof
- C01B32/15—Nano-sized carbon materials
- C01B32/158—Carbon nanotubes
-
- 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
- C09D201/00—Coating compositions based on unspecified macromolecular compounds
- C09D201/02—Coating compositions based on unspecified macromolecular compounds characterised by the presence of specified groups, e.g. terminal or pendant functional groups
-
- 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
- C09D5/00—Coating compositions, e.g. paints, varnishes or lacquers, characterised by their physical nature or the effects produced; Filling pastes
- C09D5/24—Electrically-conducting paints
-
- 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
- C09D7/00—Features of coating compositions, not provided for in group C09D5/00; Processes for incorporating ingredients in coating compositions
- C09D7/40—Additives
- C09D7/60—Additives non-macromolecular
- C09D7/61—Additives non-macromolecular inorganic
-
- 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
- H01B1/20—Conductive material dispersed in non-conductive organic material
- H01B1/24—Conductive material dispersed in non-conductive organic material the conductive material comprising carbon-silicon compounds, carbon or silicon
-
- 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
- H01M10/05—Accumulators with non-aqueous electrolyte
- H01M10/052—Li-accumulators
-
- 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
-
- 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
- H01M4/139—Processes of manufacture
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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
- H01M4/00—Electrodes
- H01M4/02—Electrodes composed of, or comprising, active material
- H01M4/62—Selection of inactive substances as ingredients for active masses, e.g. binders, fillers
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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
- H01M4/00—Electrodes
- H01M4/02—Electrodes composed of, or comprising, active material
- H01M4/62—Selection of inactive substances as ingredients for active masses, e.g. binders, fillers
- H01M4/624—Electric conductive fillers
- H01M4/625—Carbon or graphite
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- 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
Abstract
리튬 이온 전지 등의 이차 전지 등의 제조에 적합인 카본 나노 튜브 분산액, 도전 페이스트, 이차 전지용 전극 페이스트, 이차 전지용 전극, 이차 전지를 제공한다. 제1 개시의 카본 나노 튜브 분산액은, 카본 나노 튜브와, 수용성 고분자 재료와, 분산매를 적어도 포함하고, 카본 나노 튜브 농도 2 질량%로 조정한 분산액을, 50μm의 간극을 가지는 어플리케이터로 도포하여 제작한 건조 도막의 XYZ 표색계의 Y가, 6.0 이하인 것을 특징으로 하고, 또한, 제2 개시의 카본 나노 튜브 분산액에서는, 상기 카본 나노 튜브의 농도 2 질량%로 조정한 분산액을, 50μm의 간극을 가지는 어플리케이터로 도포하여 제작한 건조 도막의 L*a*b* 색공간의 a*와 b*가, 모두 마이너스인 것을 특징으로 한다.Provided are carbon nanotube dispersions, conductive pastes, electrode pastes for secondary batteries, electrodes for secondary batteries, and secondary batteries suitable for the production of secondary batteries such as lithium ion batteries. The carbon nanotube dispersion of the first disclosure is produced by applying a dispersion containing at least carbon nanotubes, a water-soluble polymer material, and a dispersion medium, and adjusting the carbon nanotube concentration to 2% by mass, using an applicator with a gap of 50 μm. It is characterized in that Y in the It is characterized in that both a * and b * of the L * a * b * color space of the dried coating film produced by application are negative.
Description
본 명세서는, 안정성과 도전 성능이 뛰어난 카본 나노 튜브 분산액, 이 분산액을 이용한 도전 페이스트, 리튬 이온 전지 등의 이차 전지의 제조에 적합하게 되는 이차 전지용 전극 페이스트, 이차 전지용 전극, 이차 전지에 관한 것이다.This specification relates to a carbon nanotube dispersion with excellent stability and conductive performance, a conductive paste using this dispersion, an electrode paste for secondary batteries suitable for the production of secondary batteries such as lithium ion batteries, electrodes for secondary batteries, and secondary batteries.
전기 자동차의 보급, 휴대 전화나 노트형 퍼스널 컴퓨터 등의 휴대 기기의 소형 경량화 및 고성능화에 수반하여, 높은 에너지 밀도를 가지는 이차 전지, 추가로, 그 이차 전지의 고용량화가 요구되고 있다. 이러한 배경 하에서 고에너지 밀도, 고전압이라고 하는 특징으로부터 비수계 전해액을 이용하는 리튬 이온 이차 전지가 많은 기기에 사용되게 되어 있다.With the spread of electric vehicles and the miniaturization, weight reduction, and higher performance of portable devices such as mobile phones and laptop-type personal computers, there is a demand for secondary batteries with high energy density and, in addition, higher capacity of the secondary batteries. Against this background, lithium-ion secondary batteries using non-aqueous electrolytes have come to be used in many devices due to their characteristics of high energy density and high voltage.
이들 리튬 이온 이차 전지에 이용되는 음극 재료나 양극 재료, 특히 양극 재료에 카본 나노 튜브 분산액 등을 이용하는 것에 의해, 양호한 도전 성능, 전극 저항을 저감할 수 있는 소량으로 효율적으로 도전 네트워크를 형성할 수 있는 것 등의 검토가 수행되고 있다.By using carbon nanotube dispersions, etc. for the negative and positive electrode materials used in these lithium ion secondary batteries, especially the positive electrode material, it is possible to efficiently form a conductive network in a small amount with good conductive performance and reduced electrode resistance. A review is being carried out.
예를 들면, 특허문헌 1에는, 수평균 분자량 1만 이상 15만 이하인 분산제 및 용매를 포함하고, 또한 카본 나노 튜브 100 중량부에 대해서 분산제를 250 중량부 이상 2000 중량부 이하의 비율로 포함하는 카본 나노 튜브 분산액으로서, 분산액의 pH가 8~12인 것을 특징으로 하는 카본 나노 튜브 분산액이 개시되고,For example, in Patent Document 1, carbon contains a dispersant and a solvent having a number average molecular weight of 10,000 to 150,000, and also contains a dispersant in a ratio of 250 to 2000 parts by weight based on 100 parts by weight of carbon nanotubes. As a nanotube dispersion, a carbon nanotube dispersion is disclosed, characterized in that the pH of the dispersion is 8 to 12,
특허문헌 2에는, 카본 나노 튜브의 분산액은, 분산매와, 평균 길이가 8μm 이상 10 mm 이하인 카본 나노 튜브와, 분자 내에 친수 구조부와 소수 구조부를 가지는 2종 이상의 계면활성제를 구비하는 것이 개시되고, Patent Document 2 discloses that a dispersion of carbon nanotubes includes a dispersion medium, carbon nanotubes with an average length of 8 μm or more and 10 mm or less, and two or more types of surfactants having a hydrophilic structure and a hydrophobic structure in the molecule,
특허문헌 3에는, 종래보다도 적은 분산제 사용량이어도 카본 나노 튜브의 고분산성을 유지하는 것이 가능한 카본 나노 튜브 분산액을 제공하기 위해서, 카본 나노 튜브 함유 조성물, 중량 평균 분자량 0.1만 이상 40만 이하의 분산제, 휘발성 염 및 수계 용매를 포함하는 카본 나노 튜브 분산액이 개시되고,Patent Document 3 discloses a composition containing carbon nanotubes, a dispersant with a weight average molecular weight of 0.10,000 to 400,000, and a volatile A carbon nanotube dispersion containing salt and an aqueous solvent is disclosed,
특허문헌 4에는, 유기 용매 중에서 뛰어난 분산성을 나타내는 것에 의해, 기재 상에 높은 도전성을 나타내는 카본 나노 튜브 분산액 및 그의 제조 방법을 제공하기 위해서, 카본 나노 튜브 함유 조성물, 특정 구조의 셀룰로오스 유도체, 및 유기 용매를 포함하는 카본 나노 튜브 분산액으로서, 상기 유기 용매는 비프로톤성 극성 용매 또는 테르펜류로부터 선택되는 1 종류 이상을 포함하는 것이고, 상기 카본 나노 튜브 분산액에 포함되는 카본 나노 튜브 함유 조성물의 농도가 1 질량% 이하이며, 당해 분산액을 1만 G에서 10분간 원심 처리를 한 후, 90vol%를 상청으로서 회수했을 때, 상청 부분의 카본 나노 튜브 분산액의 농도가, 원심 처리전의 카본 나노 튜브 분산액의 농도의 80% 이상인 카본 나노 튜브 분산액이 개시되고,In Patent Document 4, in order to provide a carbon nanotube dispersion liquid that exhibits excellent dispersibility in organic solvents and thus high conductivity on a substrate, and a method for producing the same, a carbon nanotube-containing composition, a cellulose derivative of a specific structure, and an organic A carbon nanotube dispersion containing a solvent, wherein the organic solvent contains at least one type selected from aprotic polar solvents or terpenes, and the concentration of the carbon nanotube-containing composition contained in the carbon nanotube dispersion is 1. % by mass or less, and when the dispersion is centrifuged at 10,000 G for 10 minutes and 90 vol% is recovered as the supernatant, the concentration of the carbon nanotube dispersion in the supernatant portion is the concentration of the carbon nanotube dispersion before centrifugation. A carbon nanotube dispersion of more than 80% is disclosed,
특허문헌 5에는, 카본 나노 튜브(CNT)를 포함하는 분산액으로서, CNT의 어스펙트비가 1,300 이상이며, 전단 속도 1,000/s에 있어서의 점도가 2.0 mPa·s 이상인 CNT를 포함하는 분산액, 또한, 이 CNT 100 질량부에 대해서, 겔 퍼미에이션 크로마토그래피로 측정한 중량 평균 분자량이 1만~40만인 분산제를 50~500 질량부 및 수계 용매를 포함하는 CTN를 포함하는 분산액, 추가로, 상기 분산제는 음이온성 분산제가 바람직하고, 그 중에서도, 카르복시메틸 셀룰로오스 또는 그의 염(Na 염, NH4 염 등)을 주성분으로 하는 것이 바람직한 CNT를 포함하는 분산액이 개시되고,Patent Document 5 discloses a dispersion containing carbon nanotubes (CNTs), wherein the aspect ratio of the CNTs is 1,300 or more and the viscosity at a shear rate of 1,000/s is 2.0 mPa·s or more. A dispersion containing 50 to 500 parts by mass of a dispersant with a weight average molecular weight of 10,000 to 400,000 as measured by gel permeation chromatography and CTN containing an aqueous solvent for 100 parts by mass of CNTs. Additionally, the dispersant is an anion. Disclosed is a dispersion containing CNTs in which a dispersant is preferred, and in particular, a dispersion containing carboxymethyl cellulose or a salt thereof (Na salt, NH 4 salt, etc.) as the main component is disclosed,
특허문헌 6에는, 카본 나노 튜브(A)와, 분산제(B)와, 물 및/또는 수용성 유기 용매를 포함하는 용매(C)를 포함하는 카본 나노 튜브 분산액으로서, 카본 나노 튜브(A)의 비표면적이 500~800 m2/g이며, 동적 광 산란법에 따라 측정한 누적 입경 D50이 200~1000 nm인 것을 특징으로 하는 카본 나노 튜브 분산액이 개시되어 있습니다.Patent Document 6 discloses a carbon nanotube dispersion containing carbon nanotubes (A), a dispersant (B), and a solvent (C) containing water and/or a water-soluble organic solvent, wherein the ratio of the carbon nanotubes (A) is A carbon nanotube dispersion is disclosed, which has a surface area of 500 to 800 m 2 /g and a cumulative particle diameter D50 of 200 to 1000 nm measured according to a dynamic light scattering method.
그렇지만, 이들 특허문헌 1~6의 카본 나노 튜브 분산액 등에서는, 경시적으로 분산성이 저하하거나 하여, 안정성과 도전 성능을 고도로 양립하는 것이 어렵고, 높은 안정성과 도전 성능을 양립할 수 있는 카본 나노 튜브 분산액, 이것을 이용한 도전 페이스트, 이차 전지용 전극 페이스트 및 이차 전지용 전극, 이 전극을 이용한 리튬 이온 전지 등의 이차 전지가 갈망되고 있는 것이 현재 상태이다.However, in the carbon nanotube dispersions of Patent Documents 1 to 6, etc., the dispersibility deteriorates over time, making it difficult to achieve both high stability and conductive performance. Carbon nanotubes that can achieve both high stability and conductive performance are difficult to achieve. Currently, secondary batteries such as dispersions, conductive pastes using the same, electrode pastes for secondary batteries and electrodes for secondary batteries, and lithium ion batteries using these electrodes are desired.
본 개시는, 상기 종래의 과제 등에 대하여 해소하려고 하는 것이고, 높은 안정성과 도전 성능을 양립할 수 있는 카본 나노 튜브 분산액, 이것을 이용한 도전 페이스트, 이차 전지용 전극 페이스트 및 이차 전지용 전극, 이 전극을 이용한 리튬 이온 전지 등의 이차 전지를 제공하는 것을 목적으로 한다.The present disclosure is intended to solve the above conventional problems, including a carbon nanotube dispersion capable of achieving both high stability and conductive performance, a conductive paste using the same, an electrode paste for a secondary battery and an electrode for a secondary battery, and lithium ion using the electrode. The purpose is to provide secondary batteries such as batteries.
본 개시자들은, 상기 종래의 과제에 대하여 열심히 검토한 결과, 카본 나노 튜브와, 수용성 고분자 재료와, 분산매를 적어도 포함하고, 카본 나노 튜브를 농도 2 질량%로 조정한 분산액을, 50μm의 간극을 가지는 어플리케이터로 도포하여 제작한 건조 도막의 XYZ 표색계의 Y를, 소정치 이하로 하는 제1 개시에 의해, 또한, 카본 나노 튜브와, 수용성 고분자 재료와, 분산매를 적어도 포함하고, 카본 나노 튜브의 농도 2 질량%로 조정한 분산액을, 50μm의 간극을 가지는 어플리케이터로 도포하여 제작한 건조 도막의 L*a*b* 색공간의 a*와 b*를, 소정치로 하는 제2 개시에 의해, 상기 목적의 카본 나노 튜브 분산액, 이것을 이용한 도전 페이스트, 이차 전지용 전극 페이스트 및 이차 전지용 전극, 이 전극을 이용한 리튬 이온 전지 등의 이차 전지를 얻을 수 있는 것을 찾아내어, 본 개시를 완성하기에 이르렀던 것이다.As a result of diligent study of the above-described conventional problems, the present initiators have found that a dispersion containing at least carbon nanotubes, a water-soluble polymer material, and a dispersion medium, and adjusting the concentration of carbon nanotubes to 2% by mass, can be prepared with a gap of 50 μm. According to the first disclosure in which Y in the According to the second disclosure, a * and b * of the L * a * b * color space of the dry coating film produced by applying the dispersion adjusted to 2% by mass with an applicator having a gap of 50 μm are set to predetermined values. By discovering that secondary batteries such as the target carbon nanotube dispersion, a conductive paste using the same, an electrode paste for secondary batteries and electrodes for secondary batteries, and a lithium ion battery using this electrode can be obtained, the present disclosure has been completed.
즉, 제1 개시의 카본 나노 튜브 분산액은, 카본 나노 튜브와, 수용성 고분자 재료와, 분산매를 적어도 포함하고, 카본 나노 튜브를 농도 2 질량%로 조정한 분산액을, 50μm의 간극을 가지는 어플리케이터로 도포하여 제작한 건조 도막의 XYZ 표색계의 Y가, 6.0 이하인 것을 특징으로 하고, 제2 개시의 카본 나노 튜브 분산액은, 카본 나노 튜브와, 수용성 고분자 재료와, 분산매를 적어도 포함하고, 카본 나노 튜브의 농도 2 질량%로 조정한 분산액을, 50μm의 간극을 가지는 어플리케이터로 도포하여 제작한 건조 도막의 L*a*b* 색공간의 a*와 b*가, 모두 마이너스인 것을 특징으로 한다. That is, the carbon nanotube dispersion of the first disclosure includes at least carbon nanotubes, a water-soluble polymer material, and a dispersion medium, and the dispersion in which the concentration of carbon nanotubes is adjusted to 2% by mass is applied using an applicator with a gap of 50 μm. Characterized in that Y in the The dry film produced by applying the dispersion adjusted to 2% by mass with an applicator having a gap of 50 μm is characterized in that both a * and b * of the L * a * b * color space are negative.
상기 수용성 고분자 재료는, 비이온성 수용성 고분자와 음이온성 수용성 고분자로부터 선택되는 1 종류 이상의 고분자 재료인 것이 바람직하다. The water-soluble polymer material is preferably one or more types of polymer materials selected from nonionic water-soluble polymers and anionic water-soluble polymers.
본 개시에 있어서, 도전 페이스트는, 상기 각 구성의 카본 나노 튜브 분산액을 적어도 포함하는 것을 특징으로 하고, 또한, 이차 전지용 전극 페이스트는, 상기 각 구성의 카본 나노 튜브 분산액과, 이차 전지용 활물질을 적어도 포함하는 것을 특징으로 한다. In the present disclosure, the conductive paste is characterized in that it contains at least a carbon nanotube dispersion of each of the above-mentioned components, and the electrode paste for a secondary battery includes at least a carbon nanotube dispersion of each of the above-mentioned components and an active material for a secondary battery. It is characterized by:
본 개시의 이차 전지용 전극은, 상기 구성의 이차 전지용 전극 페이스트를 이용한 것을 특징으로 하고, 또한, 이차 전지는, 상기 구성의 이차 전지용 전극을 이용한 것을 특징으로 한다. The electrode for a secondary battery of the present disclosure is characterized by using the electrode paste for a secondary battery having the above-described structure, and the secondary battery is characterized by using the electrode for a secondary battery having the above-described structure.
덧붙여, 본 명세서에 있어서, 「본 개시」라고 말할 때는, 제1 개시 및 제2 개시를 포함하는 것을 말한다.In addition, in this specification, when referring to “this disclosure”, it means including the first disclosure and the second disclosure.
본 개시에 의하면, 높은 안정성과 도전 성능을 양립할 수 있는 카본 나노 튜브 분산액, 이것을 이용한 도전 페이스트, 이차 전지용 전극 페이스트 및 이차 전지용 전극, 이 전극을 이용한 리튬 이온 전지 등에 적합한 이차 전지를 제공할 수 있다.According to the present disclosure, a secondary battery suitable for a carbon nanotube dispersion capable of achieving both high stability and conductive performance, a conductive paste using the same, an electrode paste for a secondary battery and an electrode for a secondary battery, and a lithium ion battery using the electrode can be provided. .
본 개시의 목적 및 효과는, 특히 청구항에 있어서 지적되는 구성 요소 및 조합을 이용하는 것에 의해서 인식되고 또한 얻어지는 것이다. 상술의 일반적인 설명 및 후술의 상세한 설명의 양방은, 예시적 및 설명적인 것이며, 특허 청구의 범위에 기재되어 있는 본 개시를 제한하는 것은 아니다.The object and effect of the present disclosure are recognized and achieved by using the components and combinations particularly pointed out in the claims. Both the general description above and the detailed description below are illustrative and explanatory and do not limit the present disclosure as set forth in the claims.
이하에, 본 개시의 실시 형태를 자세하게 설명한다. 단, 본 개시의 기술적 범위는 하기에서 상술하는 실시 형태로 한정되지 않고, 특허 청구의 범위에 기재된 발명과 그의 균등물에 이르는 점에 유의하기 바란다. 또한, 본 개시는, 본 명세서에 개시되어 있는 내용과 당해 분야에 있어서의 기술 상식(설계 사항, 자명 사항을 포함한다)에 근거하여 실시할 수 있다. Below, embodiments of the present disclosure will be described in detail. However, please note that the technical scope of the present disclosure is not limited to the embodiments described in detail below, but extends to the invention described in the patent claims and equivalents thereof. In addition, the present disclosure can be implemented based on the content disclosed in this specification and common technical knowledge (including design matters and obvious matters) in the field.
<카본 나노 튜브 분산액><Carbon nanotube dispersion>
본 제1 개시의 카본 나노 튜브 분산액은, 카본 나노 튜브와, 수용성 고분자 재료와, 분산매를 적어도 포함하고, 카본 나노 튜브를 농도 2 질량%로 조정한 분산액을, 50μm의 간극을 가지는 어플리케이터로 도포하여 제작한 건조 도막의 XYZ 표색계의 Y가, 6.0 이하인 것을 특징으로 하는 것이고, 또한, 제2 개시의 카본 나노 튜브 분산액은, 카본 나노 튜브와, 수용성 고분자 재료와, 분산매를 적어도 포함하고, 카본 나노 튜브의 농도 2 질량%로 조정한 분산액을, 50μm의 간극을 가지는 어플리케이터로 도포하여 제작한 건조 도막의 L*a*b* 색공간의 a*와 b*가, 모두 마이너스인 것을 특징으로 하는 것이다.The carbon nanotube dispersion of the first disclosure includes at least carbon nanotubes, a water-soluble polymer material, and a dispersion medium, and the dispersion in which the concentration of the carbon nanotubes is adjusted to 2% by mass is applied using an applicator with a gap of 50 μm. The produced dried coating film is characterized in that Y in the A dispersion solution adjusted to a concentration of 2% by mass is applied with an applicator having a gap of 50 μm, and a * and b * of the L * a * b * color space of the dry film are both negative.
<카본 나노 튜브(CNT)><Carbon nanotubes (CNT)>
본 개시(제1 개시 및 제2 개시, 이하 동일)에 이용하는 카본 나노 튜브(CNT)로서는, 실질적으로 그라파이트의 1매면을 감아 통상(筒狀)으로 한 형상을 가지는 것이면 특별히 한정되지 않고, 그라파이트의 1매면을 1층으로 감은 단층 CNT, 2층 또는 3층 이상의 다층으로 감은 다층 CNT 모두 이용할 수 있다.The carbon nanotubes (CNTs) used in the present disclosure (first disclosure and second disclosure, hereinafter the same) are not particularly limited as long as they have a regular shape by substantially winding one surface of graphite, and include those of graphite. Both single-layer CNTs wound with one layer on each side and multi-layer CNTs wound with two or three or more layers can be used.
또한, 카본 나노 튜브의 형태로서는, 예를 들면, 그라파이트 위스커, 필라멘트 카본, 그라파이트 파이버, 극세 탄소 튜브, 카본 튜브, 카본 피브릴, 카본 마이크로 튜브 및 카본 나노 섬유를 들 수 있지만, 이들로 한정되지 않고, 이들 각 단독 또는 2종 이상을 조합(이하, 간단하게 「적어도 1종」이라고 한다)이어도 된다. In addition, examples of the forms of carbon nanotubes include, but are not limited to, graphite whiskers, filament carbon, graphite fibers, ultrafine carbon tubes, carbon tubes, carbon fibrils, carbon microtubes, and carbon nanofibers. , each of these may be used alone or in combination of two or more types (hereinafter simply referred to as “at least one type”).
또한, 카본 나노 튜브의 평균 외경은, 분산액의 점도, 도전성, 안정성의 점으로부터, 1 nm 이상 90 nm 이하인 것이 바람직하고, 3 nm 이상 30 nm 이하인 것이 보다 바람직하고, 3 nm 이상 15 nm 이하인 것이 더욱 바람직하다.In addition, the average outer diameter of the carbon nanotubes is preferably 1 nm or more and 90 nm or less, more preferably 3 nm or more and 30 nm or less, and even more preferably 3 nm or more and 15 nm or less from the viewpoint of viscosity, conductivity, and stability of the dispersion. desirable.
본 개시에 있어서, 카본 나노 튜브의 평균 외경이란, 투과형 전자 현미경의 10만배 이상의 배율의 화상을 이용하여 측정한 충분한 n수의 외형의 산술 평균값을 말한다.In the present disclosure, the average outer diameter of a carbon nanotube refers to the arithmetic mean value of a sufficient n number of external shapes measured using an image of a transmission electron microscope at a magnification of 100,000 times or more.
또한, 본 개시에 이용하는 카본 나노 튜브의 순도는, 90~100 질량%가 바람직하고, 특히 95~100 질량%가 바람직하다. 덧붙여, 카본 나노 튜브의 순도는, JIS K 1469나 JIS K 6218에 준거하여 측정한 회분을 불순물로 하고, 그 불순물 양에 근거하여 산출된다.Additionally, the purity of the carbon nanotubes used in the present disclosure is preferably 90 to 100% by mass, and particularly 95 to 100% by mass. In addition, the purity of carbon nanotubes is calculated based on the amount of impurities, using the ash content measured in accordance with JIS K 1469 or JIS K 6218 as an impurity.
구체적으로 이용할 수 있는 카본 나노 튜브(CNT)로서는, 예를 들면, Cnano사 제의 FloTube9000(평균 외경 11 nm), 호도가야 카가쿠사 제의 MWNT-7(평균 외경 70 nm), 쇼와 덴코사 제의 VGCF-S(평균 외경 80 nm), VGCF-X(평균 외경 15 nm) 등의 적어도 1종을 이용할 수 있다. Carbon nanotubes (CNTs) that can be specifically used include, for example, FloTube9000 (average outer diameter 11 nm) manufactured by Cnano, MWNT-7 (average outer diameter 70 nm) manufactured by Hodogaya Chemical Company, and Showa Denko. At least one type such as VGCF-S (average outer diameter 80 nm) and VGCF-X (average outer diameter 15 nm) can be used.
이들 카본 나노 튜브(CNT)의 함유량은, 용도에 따라서, 적합한 함유량을 설정할 수 있고, 특별히 한정되는 것은 아니다.The content of these carbon nanotubes (CNTs) can be set to an appropriate content depending on the application, and is not particularly limited.
예를 들면, 도전 페이스트, 이차 전지용 전극 페이스트, 이차 전지용 전극 등에 이용하는 경우는, 높은 안정성과 도전 성능을 양립하는 점, 분산액 제조시의 점도의 점으로부터, 그의 함유량은, 분산액 전량에 대해서, 0.1~15.0 질량%로 하는 것이 바람직하고, 더욱 바람직하게는 0.1~10.0 질량%, 보다 바람직하게는 0.5~8.0 질량%, 1.0~6.0 질량%, 특히 2.0~5.0 질량%로 하는 것이 바람직하다.For example, when using it for electrically conductive paste, electrode paste for secondary batteries, electrodes for secondary batteries, etc., its content is 0.1 to 0.1 based on the total amount of the dispersion, from the viewpoint of both high stability and conductive performance and the viscosity during preparation of the dispersion. It is preferably 15.0 mass%, more preferably 0.1 to 10.0 mass%, more preferably 0.5 to 8.0 mass%, 1.0 to 6.0 mass%, especially 2.0 to 5.0 mass%.
이 카본 나노 튜브(CNT)의 함유량을 0.1 질량% 이상으로 하는 것에 의해, 충분한 도전성을 확보할 수 있게 되어, 한편, 15.0 질량% 이하로 하는 것에 의해, 분산액의 안정성과 양호한 도전성을 확보할 수 있는 것이 된다.By setting the carbon nanotube (CNT) content to 0.1 mass% or more, sufficient conductivity can be secured, while by setting it to 15.0 mass% or less, the stability of the dispersion and good conductivity can be secured. It becomes a thing.
<수용성 고분자 재료><Water-soluble polymer material>
본 개시에 이용하는 수용성 고분자 재료는, 물에 가용인 것, 또는, 이용하는 분산매(물 이외의 용매)에 용해하는 것이면 특별히 한정되지 않고 이용할 수 있다.The water-soluble polymer material used in the present disclosure is not particularly limited and can be used as long as it is soluble in water or soluble in the dispersion medium (solvent other than water) used.
물에 가용인 고분자 재료로서는, 예를 들면, 단백질이나 전분 등의 천연 고분자 재료의 외, 폴리아크릴산, 폴리아크릴 아미드, 폴리옥시에틸렌 옥시드, 폴리비닐 피롤리돈, 폴리비닐 알코올, 폴리비닐 아미드, 폴리아민 등의 합성 고분자 재료 등을 들 수 있다. 이들 수용성 고분자 재료는, 카본 나노 튜브(CNT)의 분산제나 결착제로서 기능하는 것이다.Water-soluble polymer materials include, for example, natural polymer materials such as proteins and starch, polyacrylic acid, polyacryl amide, polyoxyethylene oxide, polyvinyl pyrrolidone, polyvinyl alcohol, polyvinyl amide, and synthetic polymer materials such as polyamine. These water-soluble polymer materials function as dispersants and binders for carbon nanotubes (CNTs).
또한, 상기 물 이외의 용매에 용해하는 수용성 고분자 재료로서는, 완전하게 용해하는 경우 뿐만 아니라, 일부가 용해하는 상태이어도 된다. 이들 수용성의 고분자를 이용하는 것에 의해, 카본 나노 튜브(CNT)가 가지는 도전성을 해치지 않고 안정하게 분산하는 것이 가능해진다.In addition, the water-soluble polymer material that dissolves in solvents other than water may be partially dissolved as well as completely dissolved. By using these water-soluble polymers, it becomes possible to stably disperse carbon nanotubes (CNTs) without impairing their conductivity.
수용성 고분자 재료로서는, 특히, 비이온성 수용성 고분자와 음이온성 수용성 고분자로부터 선택되는 적어도 1 종류 이상의 것을 이용하는 것이 바람직하고, 카본 나노 튜브(CNT)가 가지는 도전성을 해치지 않고 안정하게 분산하는 것에 특히 적합한 것이 된다.As a water-soluble polymer material, it is particularly preferable to use at least one type selected from nonionic water-soluble polymers and anionic water-soluble polymers, and it is particularly suitable for stably dispersing carbon nanotubes (CNTs) without impairing the conductivity of carbon nanotubes (CNTs). .
이용할 수 있는 비이온성 수용성 고분자로서는, 예를 들면, 폴리옥시에틸렌 알킬 에테르, 폴리옥시알킬렌 유도체, 폴리옥시에틸렌 페닐 에테르, 소르비탄 지방산 에스테르, 폴리옥시에틸렌 소르비탄 지방산 에스테르 및 알킬 아릴 에테르, 글리세롤 보레이트 지방산 에스테르 및 폴리옥시에틸렌 글리세롤 지방산 에스테르, 크산탄 검, 웨란 검, 석시노글리칸, 폴리비닐 알코올(PVAL 또는 PVOH), 폴리비닐 피롤리돈, 폴리비닐 아세탈 등의 적어도 1종을 들 수 있다.Nonionic water-soluble polymers that can be used include, for example, polyoxyethylene alkyl ethers, polyoxyalkylene derivatives, polyoxyethylene phenyl ethers, sorbitan fatty acid esters, polyoxyethylene sorbitan fatty acid esters and alkyl aryl ethers, and glycerol borate. and at least one type such as fatty acid ester, polyoxyethylene glycerol fatty acid ester, xanthan gum, welan gum, succinoglycan, polyvinyl alcohol (PVAL or PVOH), polyvinyl pyrrolidone, and polyvinyl acetal.
이용할 수 있는 음이온성 수용성 고분자로서는, 예를 들면, 지방산 및 그의 염, 폴리설폰산 및 그의 염, 폴리카르복시산 및 그의 염, 알킬 황산 에스테르 및 그의 염, 알킬 아릴 설폰산 및 그의 염, 알킬 나프타렌 설폰산 및 그의 염, 디알킬설폰산 및 그의 염, 디알킬 설포석신산 및 그의 염, 알킬 인산 및 그의 염, 폴리옥시에틸렌 알킬 에테르 황산 및 그의 염, 폴리옥시에틸렌 알킬 아릴 에테르 황산 및 그의 염, 나프탈렌 설폰산 포르말린 축합물 및 그의 염, 폴리옥시에틸렌 알킬 인산 설폰산 및 그의 염, 스틸렌 아크릴 수지 등의 아크릴계 고분자, 카르복시메틸 셀룰로오스 또는 그의 나트륨(Na) 염 등의 셀룰로오스계 고분자 등의 적어도 1종을 들 수 있다.Anionic water-soluble polymers that can be used include, for example, fatty acids and their salts, polysulfonic acids and their salts, polycarboxylic acids and their salts, alkyl sulfuric acid esters and their salts, alkyl aryl sulfonic acids and their salts, and alkyl naphthalene sulfonates. Fonic acid and its salts, dialkyl sulfonic acid and its salts, dialkyl sulfosuccinic acid and its salts, alkyl phosphoric acid and its salts, polyoxyethylene alkyl ether sulfuric acid and its salts, polyoxyethylene alkyl aryl ether sulfuric acid and its salts, naphthalene Sulfonic acid formalin condensate and its salts, polyoxyethylene alkyl phosphoric acid sulfonic acid and its salts, acrylic polymers such as styrene acrylic resin, and cellulose polymers such as carboxymethyl cellulose or its sodium (Na) salt. You can.
바람직하게는, 도전성을 저해하지 않는 점으로부터, 이용하는 비이온성 수용성 고분자로서는, 폴리비닐 피롤리돈의 사용이 바람직하고, 또한, 음이온성 수용성 고분자에서는, 아크릴계 고분자, 셀룰로오스계 고분자의 사용이 바람직하다.Preferably, the nonionic water-soluble polymer used is polyvinyl pyrrolidone because it does not impair conductivity, and the anionic water-soluble polymer is preferably an acrylic polymer or a cellulose polymer.
이들 수용성 고분자 재료의 (합계) 함유량은, 용도에 따라서, 적합한 함유량을 설정할 수 있고, 특별히 한정되는 것은 아니다.The (total) content of these water-soluble polymer materials can be set to an appropriate content depending on the application, and is not particularly limited.
예를 들면, 도전 페이스트, 이차 전지용 전극 페이스트, 이차 전지용 전극 등에 이용하는 경우는, 높은 안정성과 도전 성능을 양립하기 위해서, 그의 함유량은, 분산액 전량에 대해서, 0.005~20 질량%로 하는 것이 바람직하고, 특히 바람직하게는, 0.025~16 질량%로 하는 것이 바람직하다.For example, when using for conductive paste, electrode paste for secondary batteries, electrodes for secondary batteries, etc., in order to achieve both high stability and conductive performance, its content is preferably 0.005 to 20% by mass based on the total amount of the dispersion, Particularly preferably, it is preferably set to 0.025 to 16 mass%.
이들 고분자 재료의 함유량을 0.005 질량% 이상으로 하는 것에 의해, 카본 나노 튜브(CNT)의 분산 안정성이 양호해지고, 한편, 20 질량% 이하로 하는 것에 의해, 분산액의 안정성과 양호한 도전성을 확보할 수 있는 것이 된다.By setting the content of these polymer materials to 0.005 mass% or more, the dispersion stability of carbon nanotubes (CNTs) becomes good, while by setting it to 20 mass% or less, the stability of the dispersion and good conductivity can be ensured. It becomes a thing.
<분산매><Dispersion medium>
본 개시에 이용하는 분산매는, 비이온성 수용성 고분자와 음이온성 수용성 고분자 등의 수용성 고분자 재료를 일부에서도 용해시킬 수 있는 것이면, 물(정제수, 증류수, 순수, 초순수 등), 유기 용매 등 특별히 한정되지 않고 이용하는 것이 가능하다.The dispersion medium used in the present disclosure is not particularly limited and can be used as long as it can partially dissolve water-soluble polymer materials such as nonionic water-soluble polymers and anionic water-soluble polymers, such as water (purified water, distilled water, pure water, ultrapure water, etc.), organic solvents, etc. It is possible.
분산매로서는, 단독으로 이용하는 것뿐만 아니라, 2 종류 이상을 혼합하여 이용하는 것도 가능하고, 물과 유기 용매의 조합이어도, 혼합 가능한 범위에서 적절히 조정하여 이용하는 것이 가능하다.As a dispersion medium, it is possible not only to use it alone, but also to mix two or more types, and even if it is a combination of water and an organic solvent, it is possible to use it by adjusting it appropriately within the mixing range.
유기 용매로서는, 예를 들면, 방향족류, 알코올류, 다가 알코올류, 글리콜 에테르류, 에스테르류 등을 이용할 수 있다. 이들 용매는, 단독으로 이용해도 되고, 또는 조합하여 이용해도 된다.As the organic solvent, for example, aromatics, alcohols, polyhydric alcohols, glycol ethers, esters, etc. can be used. These solvents may be used individually or may be used in combination.
방향족류로서는, 예를 들면, 벤질 알코올, 에틸렌글리콜 모노메틸 에테르, 에틸렌글리콜 모노에틸 에테르, 에틸렌글리콜 모노부틸 에테르, 에틸렌글리콜 모노페닐 에테르, 에틸렌글리콜 모노벤질 에테르, 프로필렌글리콜 모노페닐 에테르, 디에틸렌글리콜 모노메틸 에테르, 디에틸렌글리콜 모노에틸 에테르, 디에틸렌글리콜 모노부틸 에테르, 디에틸렌글리콜 모노페닐 에테르, 프로필렌글리콜 모노메틸 에테르, 프로필렌글리콜 모노에틸 에테르, 프로필렌글리콜 모노부틸 에테르, 에틸렌글리콜 모노메틸 에테르 아세테이트, 트리에틸렌글리콜 모노메틸 에테르, 트리에틸렌글리콜 모노에틸 에테르, 트리에틸렌글리콜 모노부틸 에테르, 에틸렌글리콜 모노페닐 에테르, 프로필렌글리콜 모노페닐 에테르, 알킬 설폰산 페닐 에스테르, 프탈산 부틸, 프탈산 에틸 헥실, 프탈산 트리데실, 트리멜리트산 에틸 헥실, 디에틸렌글리콜 디벤조에이트, 디프로필렌글리콜 디벤조에이트 등을 이용할 수 있다.Examples of aromatics include benzyl alcohol, ethylene glycol monomethyl ether, ethylene glycol monoethyl ether, ethylene glycol monobutyl ether, ethylene glycol monophenyl ether, ethylene glycol monobenzyl ether, propylene glycol monophenyl ether, and diethylene glycol. Monomethyl ether, Diethylene glycol monoethyl ether, Diethylene glycol monobutyl ether, Diethylene glycol monophenyl ether, Propylene glycol monomethyl ether, Propylene glycol monoethyl ether, Propylene glycol monobutyl ether, Ethylene glycol monomethyl ether acetate, Triethylene glycol monomethyl ether, triethylene glycol monoethyl ether, triethylene glycol monobutyl ether, ethylene glycol monophenyl ether, propylene glycol monophenyl ether, alkyl sulfonic acid phenyl ester, butyl phthalate, ethyl hexyl phthalate, tridecyl phthalate, Ethyl hexyl trimellitate, diethylene glycol dibenzoate, dipropylene glycol dibenzoate, etc. can be used.
알코올류로서는, 예를 들면, 에탄올, n-프로판올, 이소프로판올, n-부탄올, 이소부탄올, tert-부틸 알코올, 1-펜탄올, 이소아밀 알코올, sec-아밀 알코올, 3-펜탄올, tert-아밀 알코올, n-헥산올, 메틸 아밀 알코올, 2-에틸 부탄올, n-헵탄올, 2-헵탄올, 3-헵탄올, n-옥탄올, 2-옥탄올, 2-에틸헥산올, 3,5,5-트리메틸헥산올, 노난올, n-데칸올, 운데칸올, n-데칸올, 트리메틸 노닐 알코올, 테트라데칸올, 헵타데칸올, 시클로헥산올, 2-메틸시클로헥산올 등을 이용할 수 있다.Alcohols include, for example, ethanol, n-propanol, isopropanol, n-butanol, isobutanol, tert-butyl alcohol, 1-pentanol, isoamyl alcohol, sec-amyl alcohol, 3-pentanol, and tert-amyl. Alcohol, n-hexanol, methyl amyl alcohol, 2-ethyl butanol, n-heptanol, 2-heptanol, 3-heptanol, n-octanol, 2-octanol, 2-ethylhexanol, 3,5 , 5-trimethylhexanol, nonanol, n-decanol, undecanol, n-decanol, trimethyl nonyl alcohol, tetradecanol, heptadecanol, cyclohexanol, 2-methylcyclohexanol, etc. .
다가 알코올류로서는, 예를 들면, 에틸렌글리콜, 디에틸렌글리콜, 트리에틸렌글리콜, 폴리에틸렌글리콜, 프로필렌글리콜, 디프로필렌글리콜, 폴리프로필렌글리콜, 부틸렌글리콜, 헥산디올, 펜탄디올, 글리세린, 헥산트리올, 티오 디글리콜, 3-메틸-1,3-부탄디올, 트리에틸렌글리콜, 디프로필렌글리콜, 1,3-프로판디올, 1,3-부탄디올, 1,5-펜탄디올, 헥실렌글리콜, 옥틸렌글리콜 등을 이용할 수 있다.Polyhydric alcohols include, for example, ethylene glycol, diethylene glycol, triethylene glycol, polyethylene glycol, propylene glycol, dipropylene glycol, polypropylene glycol, butylene glycol, hexanediol, pentanediol, glycerin, hexanetriol, Thiodiglycol, 3-methyl-1,3-butanediol, triethylene glycol, dipropylene glycol, 1,3-propanediol, 1,3-butanediol, 1,5-pentanediol, hexylene glycol, octylene glycol, etc. can be used.
글리콜 에테르류로서는, 예를 들면, 메틸 이소프로필 에테르, 에틸 에테르, 에틸 프로필 에테르, 에틸 부틸 에테르, 이소프로필 에테르, 부틸 에테르, 헥실 에테르, 2-에틸 헥실 에테르, 에틸렌글리콜 모노헥실 에테르, 에틸렌글리콜 모노-2-에틸 부틸 에테르, 에틸렌글리콜 모노메틸 에테르, 에틸렌글리콜 모노에틸 에테르, 에틸렌글리콜 모노부틸 에테르, 디에틸렌글리콜 모노메틸 에테르, 디에틸렌글리콜 모노에틸 에테르, 디에틸렌글리콜 모노부틸 에테르, 트리에틸렌글리콜 모노부틸 에테르, 테트라에틸렌글리콜 모노부틸 에테르, 3-메틸-3-메톡시-1-부탄올, 3-메톡시-1-부탄올, 프로필렌글리콜 모노메틸 에테르, 프로필렌글리콜 모노에틸 에테르, 프로필렌글리콜 모노프로필 에테르, 프로필렌글리콜 모노부틸 에테르, 프로필렌글리콜 터셔리-부틸 에테르, 디프로필렌글리콜 모노메틸 에테르, 디프로필렌글리콜 모노에틸 에테르, 디프로필렌글리콜 모노프로필 에테르, 디프로필렌글리콜 모노부틸 에테르, 트리프로필렌글리콜 모노메틸 에테르, 트리프로필렌글리콜 모노부틸 에테르, 테트라프로필렌글리콜 모노부틸 에테르 등을 이용할 수 있다.Examples of glycol ethers include methyl isopropyl ether, ethyl ether, ethyl propyl ether, ethyl butyl ether, isopropyl ether, butyl ether, hexyl ether, 2-ethylhexyl ether, ethylene glycol monohexyl ether, and ethylene glycol mono. -2-ethyl butyl ether, ethylene glycol monomethyl ether, ethylene glycol monoethyl ether, ethylene glycol monobutyl ether, diethylene glycol monomethyl ether, diethylene glycol monoethyl ether, diethylene glycol monobutyl ether, triethylene glycol mono Butyl ether, tetraethylene glycol monobutyl ether, 3-methyl-3-methoxy-1-butanol, 3-methoxy-1-butanol, propylene glycol monomethyl ether, propylene glycol monoethyl ether, propylene glycol monopropyl ether, Propylene glycol monobutyl ether, propylene glycol tertiary-butyl ether, dipropylene glycol monomethyl ether, dipropylene glycol monoethyl ether, dipropylene glycol monopropyl ether, dipropylene glycol monobutyl ether, tripropylene glycol monomethyl ether, tripropylene glycol monomethyl ether Propylene glycol monobutyl ether, tetrapropylene glycol monobutyl ether, etc. can be used.
에스테르류로서는, 예를 들면, 프로필렌글리콜 메틸 에테르 아세테이트, 프로필렌글리콜 디아세테이트, 3-메틸-3-메톡시 부틸 아세테이트, 프로필렌글리콜 에틸 에테르 아세테이트, 에틸렌글리콜 에틸 에테르 아세테이트, 포름산 부틸, 포름산 이소부틸, 포름산 이소아밀, 아세트산 프로필, 아세트산 부틸, 아세트산 이소프로필, 아세트산 이소부틸, 아세트산 이소아밀, 프로피온산 메틸, 프로피온산 에틸, 프로피온산 프로필, 프로피온산 이소부틸, 프로피온산 이소아밀, 부틸산 메틸, 부틸산 에틸, 부틸산 프로필, 이소부틸산 메틸, 이소부틸산 에틸, 이소부틸산 프로필, 발레르산 메틸, 발레르산 에틸, 발레르산 프로필, 이소발레르산 메틸, 이소발레르산 에틸, 이소발레르산 프로필, 트리메틸 아세트산 메틸, 트리메틸 아세트산 에틸, 트리메틸 아세트산 프로필, 카프로산 메틸, 카프로산 에틸, 카프로산 프로필, 카프릴산 메틸, 카프릴산 에틸, 카프릴산 프로필, 라우린산 메틸, 라우린산 에틸, 올레인산 메틸, 올레인산 에틸, 카프릴산 트리글리세라이드, 구연산 트리부틸 아세테이트, 옥시스테아린산 옥틸, 프로필렌글리콜 모노리시놀레이트, 2-히드록시이소부틸산 메틸, 3-메톡시 부틸 아세테이트 등을 이용할 수 있다.As esters, for example, propylene glycol methyl ether acetate, propylene glycol diacetate, 3-methyl-3-methoxy butyl acetate, propylene glycol ethyl ether acetate, ethylene glycol ethyl ether acetate, butyl formate, isobutyl formate, and formic acid. Isoamyl, propyl acetate, butyl acetate, isopropyl acetate, isobutyl acetate, isoamyl acetate, methyl propionate, ethyl propionate, propyl propionate, isobutyl propionate, isoamyl propionate, methyl butyrate, ethyl butyrate, propyl butyrate, Methyl isobutyrate, ethyl isobutyrate, propyl isobutyrate, methyl valerate, ethyl valerate, propyl valerate, methyl isovalerate, ethyl isovalerate, propyl isovalerate, methyl trimethyl acetate, ethyl trimethyl acetate, Trimethyl propyl acetate, methyl caproate, ethyl caproate, propyl caproate, methyl caprylate, ethyl caprylate, propyl caprylate, methyl laurate, ethyl laurate, methyl oleate, ethyl oleate, caprylic acid Triglyceride, tributyl acetate citrate, octyl oxystearate, propylene glycol monoricinoleate, methyl 2-hydroxyisobutyrate, 3-methoxy butyl acetate, etc. can be used.
또한, 에탄올 아민, 디에탄올 아민, 트리에탄올 아민, N-메틸 디에탄올 아민, N-에틸 디에탄올 아민, 모르폴린, N-에틸모르폴린, 에틸렌 디아민, 디에틸렌 디아민, 트리에틸렌 테트라민, 테트라에틸렌 펜타민, 폴리에틸렌 이민, 펜타메틸 디에틸렌 트리아민, 테트라메틸 프로필렌 디아민 등의 아민계, N-메틸-2-피롤리돈(NMP), N-에틸-2-피롤리돈(NEP), N,N-디메틸 포름아미드, N,N-디메틸아세토아미드, N,N-디에틸아세토아미드, N-메틸 카프로락탐 등의 아미드계, 시클로헥실 피롤리돈, 2-옥사졸리돈, 1,3-디메틸-2-이미다졸리딘온, γ-부티로락톤 등의 복소환계, 디메틸 설폭시드 등의 설폭시드계, 헥사메틸포스포로 트리아미드, 설포란 등의 설폰계, 우레아, 아세토니트릴 등의 적어도 1종을 사용할 수 있다.In addition, ethanol amine, diethanol amine, triethanol amine, N-methyl diethanol amine, N-ethyl diethanol amine, morpholine, N-ethylmorpholine, ethylene diamine, diethylene diamine, triethylene tetramine, tetraethylene pentaamine. Amines such as amine, polyethylene imine, pentamethyl diethylene triamine, and tetramethyl propylene diamine, N-methyl-2-pyrrolidone (NMP), N-ethyl-2-pyrrolidone (NEP), N, N -Amides such as dimethyl formamide, N,N-dimethylacetoamide, N,N-diethylacetoamide, and N-methyl caprolactam, cyclohexyl pyrrolidone, 2-oxazolidone, 1,3-dimethyl- Heterocyclic systems such as 2-imidazolidinone and γ-butyrolactone, sulfoxide systems such as dimethyl sulfoxide, sulfone systems such as hexamethylphosphorotriamide and sulfolane, and at least one type such as urea and acetonitrile. can be used.
본 개시의 카본 나노 튜브 분산액에는, 그 용도에 따른 첨가제를 더해도 된다. 예를 들면, 증점제로서 카르복시메틸 셀룰로오스 나트륨, 침강 방지제, 습윤제, 유화제, 새깅 방지제, 소포제, 레벨링제, 가소제, 방곰팡이·방조제, 항균제 등을 들 수 있다.Additives depending on the intended use may be added to the carbon nanotube dispersion of the present disclosure. For example, thickeners include sodium carboxymethyl cellulose, anti-settling agents, wetting agents, emulsifiers, anti-sagging agents, anti-foaming agents, leveling agents, plasticizers, anti-mold and algae agents, and anti-bacterial agents.
제1 개시의 카본 나노 튜브 분산액은, 상술의 카본 나노 튜브와, 수용성 고분자 재료와, 분산매를 적어도 포함하고, 카본 나노 튜브를 농도 2 질량%로 조정한 분산액을, 50μm의 간극을 가지는 어플리케이터로 도포하여 제작한 건조 도막의 XYZ 표색계의 Y가, 6.0 이하가 되는 것을 특징으로 하는 것이고, 또한, 제2 개시의 카본 나노 튜브 분산액은, 상술의 카본 나노 튜브와, 수용성 고분자 재료와, 분산매를 적어도 포함하고, 카본 나노 튜브의 농도 2 질량%로 조정한 분산액을, 50μm의 간극을 가지는 어플리케이터로 도포하여 제작한 건조 도막의 L*a*b* 색공간의 a*와 b*가, 모두 마이너스인 것을 특징으로 하는 것이다.The carbon nanotube dispersion of the first disclosure contains at least the carbon nanotubes described above, a water-soluble polymer material, and a dispersion medium, and the dispersion is adjusted to a concentration of 2% by mass of the carbon nanotubes, and is applied using an applicator with a gap of 50 μm. The Y in the Then, a dispersion solution adjusted to a concentration of 2% by mass of carbon nanotubes was applied with an applicator having a gap of 50 μm, and a * and b * of the L * a * b * color space of the dried film were both negative. It is a feature.
제1 개시에 있어서의 상기 배합 특성의 카본 나노 튜브 분산액에 있어서, 이 건조 도막과 XYZ 표색계에 있어서의 X, Y, Z와의 상관 관계에 대하여 수많은 시험 평가를 수행했는데, 상기 카본 나노 튜브 분산액의 건조 도막의 XYZ 표색계의, 특히 Y가 소정치 이하가 되는 것이 그의 도전성과 안정성의 양립에 있어서 최고도가 되는 것이 판명되었다.Regarding the carbon nanotube dispersion liquid with the above-mentioned mixing characteristics in the first disclosure, numerous tests and evaluations were conducted on the correlation between this dried coating film and X, Y, and Z in the XYZ color system. The drying of the carbon nanotube dispersion liquid It was found that in the XYZ colorimetric system of the coating film, especially when Y is below a predetermined value, it is the best in terms of both conductivity and stability.
이 제1 개시에서는, 이 도전성과 안정성과의 양립에 있어서 최고도가 되는 카본 나노 튜브 분산액은, 건조 도막의 XYZ 표색계의 Y가, 6.0 이하가 되는 것이고, 바람직하게는, 0 이상, 5.0 이하, 보다 바람직하게는 0 이상, 4. 5 이하, 특히 바람직하게는 0 이상, 4.0 이하가 되는 것이 바람직하다.In this first disclosure, the carbon nanotube dispersion that achieves the highest level of coexistence of conductivity and stability is one in which Y in the XYZ colorimetric system of the dry coating film is 6.0 or less, preferably 0 or more and 5.0 or less. More preferably, it is 0 or more and 4.5 or less, and particularly preferably 0 or more and 4.0 or less.
이 제1 개시에 있어서의 카본 나노 튜브 분산액에 있어서의 건조 도막의 XYZ 표색계의 Y가, 6.0 초과가 되는 분산액에서는, 도전성이 악화되어 버리기 때문에, 바람직하지 않다.In the carbon nanotube dispersion in this first disclosure, the Y in the XYZ color system of the dried coating film exceeds 6.0, which is not preferable because the conductivity deteriorates.
또한, 제1 개시에 있어서, 상기 「카본 나노 튜브를 농도 2 질량%로 조정한 분산액을, 50μm의 간극을 가지는 어플리케이터로 도포하여 제작한 건조 도막」으로 규정한 것은, 동일한 조건에서 색상을 평가하는 이유에 의한 것이다.In addition, in the first disclosure, the definition as "a dry coating film produced by applying a dispersion of carbon nanotubes adjusted to a concentration of 2% by mass with an applicator with a gap of 50 μm" means evaluating color under the same conditions. It is for a reason.
본 제1 개시(후술하는 실시예를 포함한다)에 있어서, 상기 건조 도막의 XYZ 표색계에 의한 측정은, 분광 측색계에 근거하는 것이고, 예를 들면, SC-T(P)(스가 시험기사 제)를 이용하여 측정할 수 있다. In this first disclosure (including the examples described later), the measurement of the dried coating film using the ) can be used to measure.
또한, 제2 개시에 있어서의 상기 배합 특성의 카본 나노 튜브 분산액에 있어서, 상기 제1 개시와 다른 시점으로부터 도전성과 안정성의 양립을 검토했는데, 이 건조 도막과 L*a*b* 색공간의 a*와 b*의 상관 관계에 대하여 수많은 시험 평가를 수행했는데, 상기 카본 나노 튜브 분산액의 건조 도막의 L*a*b* 색공간의 특히 a*와 b*가, 소정값으로 되는 것이 그 도전성과 안정성의 양립에 있어서 최고도로 되는 것이 판명되었다.In addition, in the carbon nanotube dispersion liquid with the above-mentioned mixing characteristics in the second disclosure, coexistence of conductivity and stability was examined from a different viewpoint than the first disclosure, and the dry coating film and a in the L * a * b * color space were examined. Numerous tests and evaluations were conducted on the correlation between * and b * , and it was found that, in particular, a * and b * of the L * a * b * color space of the dried coating film of the carbon nanotube dispersion liquid were set to a predetermined value to determine the conductivity and It was found to be the best in terms of both stability and stability.
여기서, 제2 개시에서는, 이 도전성과 안정성과의 양립에 있어서 최고도로 되는 카본 나노 튜브 분산액은, 카본 나노 튜브의 농도 2 질량%로 조정한 용액을, 50μm의 간극을 가지는 어플리케이터로 도포하여 제작한 건조 도막의 L*a*b* 색공간의 a*와 b*가, 모두 마이너스인 것이 필요하다고 하는 것을 알 수 있었다.Here, in the second disclosure, the carbon nanotube dispersion that has the highest level of coexistence of conductivity and stability is produced by applying a solution with a carbon nanotube concentration adjusted to 2% by mass using an applicator with a gap of 50 μm. It was found that both a * and b * of the L * a * b * color space of the dry film were required to be negative.
바람직하게는, a*와 b*가, 모두 마이너스로서, a*의 절대값의 최대값을 A, b*의 절대값의 최대값을 B로 했을 때에, 0.1 A 이상 1.0 A 이하, 및/또는, 0.1 B 이상 1.0 B 이하를 만족시키는 것이 바람직하고, 특히 바람직하게는, 상기 A가 0.5 A 이상 1.0 A 이하, 및, 상기 B가 0.5 B 이상 1.0 B 이하로 되는 것이 바람직하다.Preferably, a * and b * are both negative, and when the maximum absolute value of a * is set to A and the maximum absolute value of b * is set to B, it is 0.1 A or more and 1.0 A or less, and/or , it is preferable to satisfy 0.1 B or more and 1.0 B or less, and especially preferably, the A is 0.5 A or more and 1.0 A or less, and the B is 0.5 B or more and 1.0 B or less.
이 카본 나노 튜브 분산액에 있어서의 건조 도막의 L*a*b* 색공간의 a*와 b*가 적어도 1개가 플러스이거나 하는 분산액에서는, 도전성이 악화하기 때문에, 바람직하지 않다.In this carbon nanotube dispersion, in which at least one a * and b * of the L * a * b * color space of the dried coating film is positive, the conductivity deteriorates, so it is not preferable.
또한, 제2 개시에 있어서, 상기 「카본 나노 튜브를 농도 2 질량%로 조정한 분산액을, 50μm의 간극을 가지는 어플리케이터로 도포하여 제작한 건조 도막」으로 규정한 것은, 상기 제1 개시와 같이, 동일한 조건에서 색상을 평가하는 이유에 의한 것이다.In addition, in the second disclosure, the definition of "a dry coating film produced by applying a dispersion of carbon nanotubes adjusted to a concentration of 2 mass% using an applicator with a gap of 50 μm" is as in the first disclosure, This is because colors are evaluated under the same conditions.
본 제2 개시(후술하는 실시예를 포함한다)에 있어서, 상기 건조 도막의 XYZ 표색계에 의한 측정은, 분광 측색계에 근거하는 것이고, 예를 들면, SC-T(P)(스가 시험기사 제)를 이용하여 측정할 수 있다.In the present second disclosure (including the examples described later), the measurement of the dried coating film using the ) can be used to measure.
본 개시에 있어서, 상기 각 특성의 카본 나노 튜브 분산액을 얻음에는, 상기 배합 특성의 각 성분을 하기에 나타내는 바와 같은 분산 장치에 의해 적합한 조건에서 분산하여 조제할 수 있다.In the present disclosure, in order to obtain a carbon nanotube dispersion having each of the above-mentioned properties, each component of the above-mentioned properties can be prepared by dispersing each component under suitable conditions using a dispersing device as shown below.
예를 들면, 분산 장치로서는, 안료 분산 등에 통상 이용되고 있는 분산기를 사용할 수 있고, 예를 들면, 디스퍼, 호모 믹서, 자전 공전 믹서, 헨셸 믹서, 플레니터리 믹서 등의 믹서류, (고압) 호모지나이저, 페인트 컨디셔너, 콜로이드 밀류, 비즈 밀, 콘 밀, 볼 밀, 샌드 밀, 아트라이터, 펄 밀, 코볼 밀 등의 미디어형 분산기, 습식 제트 밀, 박막 선회형 고속 믹서 등의 미디아 레스 분산기, 그 외 롤 밀 등을 들 수 있지만, 이들로 한정되는 것은 아니다.For example, as the dispersion device, dispersers commonly used for pigment dispersion, etc. can be used, for example, mixers such as dispers, homomixers, rotation mixers, Henschel mixers, and planetary mixers, (high pressure) Media-type dispersers such as homogenizers, paint conditioners, colloid mills, bead mills, cone mills, ball mills, sand mills, artwriters, pearl mills, cobol mills, and media-less dispersers such as wet jet mills and thin-film swirling high-speed mixers. , other roll mills, etc., but are not limited to these.
바람직한 분산 장치로서는, 안정성이나 분산 효율의 점으로부터, 박막 선회형 고속 믹서나 비즈 밀 등이 바람직하다.As a preferable dispersion device, a thin film swirling high-speed mixer, a bead mill, etc. are preferable from the viewpoint of stability and dispersion efficiency.
또한, 본 개시의 카본 나노 튜브 분산액의 점도(25℃)는, 안정성의 점, 핸들링의 점으로부터, 콘 플레이트 점도계, 로터 회전 속도 10 rpm(전단 속도 38.3s-1)에서, 1~10000 mPa·s인 것이 바람직하고, 1~5000 mPa·s인 것이 보다 바람직하다.In addition, the viscosity (25°C) of the carbon nanotube dispersion of the present disclosure is 1 to 10000 mPa·1, from the viewpoint of stability and handling, at a cone plate viscometer and a rotor rotation speed of 10 rpm (shear rate 38.3 s -1 ). It is preferable that it is s, and it is more preferable that it is 1-5000 mPa·s.
이와 같이 구성되는 본 개시의 카본 나노 튜브 분산액은, 높은 안정성과 도전 성능을 양립할 수 있는 것이 된다. 이 카본 나노 튜브 분산액은, 종래에 없는 뛰어난 성능을 가지므로, 도전 페이스트, 이차 전지용 전극 페이스트 및 이차 전지용 전극, 이 전극을 이용한 리튬 이온 전지 등에 적합한 이차 전지 등에 이용할 수 있는 것이 된다.The carbon nanotube dispersion of the present disclosure configured in this way is capable of achieving both high stability and conductive performance. Since this carbon nanotube dispersion has superior performance that is unprecedented in the past, it can be used in secondary batteries suitable for conductive pastes, electrode pastes for secondary batteries, electrodes for secondary batteries, and lithium ion batteries using this electrode.
<도전 페이스트><Challenge paste>
본 개시의 도전 페이스트는, 상기 제1 개시 또는 제2 개시의 카본 나노 튜브 분산액을 적어도 포함하는 것을 특징으로 하는 것이고, 도전성 수지 제품, 도전성 접착제, 프린트 배선 용도 등에 이용할 수 있다.The conductive paste of the present disclosure is characterized by containing at least the carbon nanotube dispersion of the first or second disclosure, and can be used for conductive resin products, conductive adhesives, printed wiring applications, etc.
이 도전 페이스트로서는, 상술의 높은 안정성과 도전 성능을 양립할 수 있는 상기 제1 개시 또는 제2 개시의 카본 나노 튜브 분산액에, 적어도 수지 성분을 첨가하여 구성할 수 있다. 수지 성분으로서는, 예를 들면, 열경화성 수지, 자외선 경화성 수지 등을 사용할 수 있다.This electrically conductive paste can be formed by adding at least a resin component to the carbon nanotube dispersion liquid of the first or second disclosure, which is capable of achieving both the above-described high stability and conductive performance. As the resin component, for example, thermosetting resin, ultraviolet curing resin, etc. can be used.
<이차 전지용 전극 페이스트, 이차 전지용 전극><Electrode paste for secondary batteries, electrodes for secondary batteries>
본 개시의 이차 전지용 전극 페이스트는, 상기 제1 개시 또는 제2 개시의 카본 나노 튜브 분산액과, 이차 전지용 활물질을 적어도 포함하는 것을 특징으로 하는 것이고, 본 개시의 이차 전지용 전극은, 상기 구성의 이차 전지용 전극 페이스트를 이용하는 것을 특징으로 하는 것이다.The electrode paste for a secondary battery of the present disclosure is characterized in that it contains at least the carbon nanotube dispersion of the first or second disclosure and an active material for a secondary battery, and the electrode for a secondary battery of the present disclosure has the above-mentioned structure for use in a secondary battery. It is characterized by using electrode paste.
상기 제1 개시 또는 제2 개시의 카본 나노 튜브 분산액은, 그대로, 또는, 희석, 또는, 농축하여 이용할 수 있다.The carbon nanotube dispersion of the first or second disclosure can be used as is, diluted, or concentrated.
이차 전지용 전극 페이스트, 이차 전지용 전극에 함유되는 카본 나노 튜브는, 전극 특성이나 셀화된 후의 전지 용량이나 충방전 특성 등에 의해 적절히 조정되고, 최적인 함유량으로 여겨지는 것이지만, 1~15 질량부가 되도록 함유되는 것이 바람직하다.The carbon nanotubes contained in the electrode paste for secondary batteries and the electrodes for secondary batteries are appropriately adjusted depending on the electrode characteristics, battery capacity after cellization, charge/discharge characteristics, etc., and are considered to be the optimal content, but are contained so as to be 1 to 15 parts by mass. It is desirable.
상기 이차 전지용 전극 페이스트에 이용하는 활물질로서는, 양극 활성 물질, 또는 음극 활성 물질의 어느 것에도 사용할 수 있다.As the active material used in the electrode paste for secondary batteries, either a positive electrode active material or a negative electrode active material can be used.
이차 전지용 양극 활물질로서는, 리튬 이온 전지의 양극에 사용 가능한 통상의 양극 활물질(리튬 이온을 가역적으로 출입시키는 활물질)이면, 특별히 한정되지 않고 이용할 수 있다.As a positive electrode active material for a secondary battery, any normal positive electrode active material (an active material that reversibly takes lithium ions in and out) that can be used in the positive electrode of a lithium ion battery can be used without particular limitation.
예를 들면, 리튬-니켈 복합 산화물, 리튬-코발트 복합 산화물, 리튬-망간 복합 산화물, 리튬-니켈-망간 복합 산화물, 리튬-니켈-코발트 복합 산화물, 리튬-니켈-알루미늄 복합 산화물, 리튬-니켈-코발트-알루미늄 복합 산화물, 리튬-니켈-망간-코발트 복합 산화물, 리튬-니켈-망간-알루미늄 복합 산화물, 리튬-니켈-코발트-망간-알루미늄 복합 산화물 등의 리튬과 천이 금속과의 복합 산화물, TiS2, FeS, MoS2 등의 천이 금속 황화물, MnO, V2O5, V6O13, TiO2 등의 천이 금속 산화물, 올리빈형 리튬 인산화물 등을 들 수 있다. 올리빈형 리튬 인산화물은, 예를 들면, Mn, Cr, Co, Cu, Ni, V, Mo, Ti, Zn, Al, Ga, Mg, B, Nb, 및 Fe로 이루어지는 군 중 적어도 1종의 원소와, 리튬과, 인과, 산소를 포함하고 있다. 이들 화합물은 그 특성을 향상시키기 위해서 일부의 원소를 부분적으로 다른 원소로 치환한 것이어도 된다.For example, lithium-nickel composite oxide, lithium-cobalt composite oxide, lithium-manganese composite oxide, lithium-nickel-manganese composite oxide, lithium-nickel-cobalt composite oxide, lithium-nickel-aluminum composite oxide, lithium-nickel- Complex oxides of lithium and transition metal, such as cobalt-aluminum complex oxide, lithium-nickel-manganese-cobalt complex oxide, lithium-nickel-manganese-aluminum complex oxide, lithium-nickel-cobalt-manganese-aluminum complex oxide, TiS 2 , transition metal sulfides such as FeS and MoS 2 , transition metal oxides such as MnO, V 2 O 5 , V 6 O 13 , and TiO 2 , and olivine-type lithium phosphate. Olivine-type lithium phosphate is, for example, at least one element from the group consisting of Mn, Cr, Co, Cu, Ni, V, Mo, Ti, Zn, Al, Ga, Mg, B, Nb, and Fe. It contains lithium, phosphorus, and oxygen. These compounds may have some elements partially replaced with other elements in order to improve their properties.
바람직한 이차 전지용 양극 활물질로서는, 리튬-니켈 복합 산화물이며, 더욱 바람직하게는, 상기 리튬-니켈 복합 산화물이, 식: LiNiXM1YM2ZO2(M1 및 M2는, Al, B, 알칼리 금속, 알칼리토류 금속, 천이 금속의 원소의 중 적어도 1종 이상의 금속 원소, 0.8≤X≤1.0, 0≤Y≤0.2, 0≤Z≤0.2)로 나타내는 리튬-니켈 복합 산화물이 바람직하다. A preferred positive electrode active material for secondary batteries is lithium-nickel composite oxide , and more preferably , the lithium-nickel composite oxide has the formula: LiNi A lithium-nickel composite oxide containing at least one metal element selected from alkaline earth metals and transition metal elements, 0.8≤X≤1.0, 0≤Y≤0.2, 0≤Z≤0.2) is preferable.
이들 이차 전지용 양극의 활물질은, 1종만을 단독으로 이용해도 되고, 2종 이상을 조합하여 이용해도 된다.These active materials of the positive electrode for secondary batteries may be used individually, or may be used in combination of two or more types.
이차 전지용 음극으로서는, 리튬 이온 전지의 음극에 사용 가능한 통상의 음극 활물질이면, 특별히 한정되지 않고 이용할 수 있다.As a negative electrode for a secondary battery, any normal negative electrode active material that can be used for the negative electrode of a lithium ion battery can be used without particular limitation.
이차 전지용 음극 활물질로서는, 리튬 이온 전지의 음극에 사용 가능한 통상의 음극 활물질이면, 특별히 한정되지 않고 이용할 수 있다.As a negative electrode active material for a secondary battery, any normal negative electrode active material that can be used for the negative electrode of a lithium ion battery can be used without particular limitation.
이용할 수 있는 이차 전지용 음극 활물질로서는, 예를 들면, 리튬 금속, 리튬 합금, 주석 화합물 등의 무기 화합물, 리튬 이온을 흡장 방출 가능한 탄소질 재료, 복수의 원소를 포함하는 복합 산화물, 도전성 폴리머 등을 들 수 있다. 탄소질 재료는, 예를 들면, 코크스류, 유리상 탄소류, 그라파이트류, 난(難)흑연화성 탄소류, 열분해 탄소류, 탄소 섬유 등을 들 수 있다. 이 중, 인조 흑연, 천연 흑연 등의 그라파이트류가, 금속 리튬에 가까운 작동 전위를 가져, 높은 작동 전압에서의 충방전이 가능하고 지지염으로서 리튬염을 사용했을 경우에 자기 방전을 억제하고, 또한 충전시에 있어서의 불가역 용량을 줄일 수 있기 때문에, 바람직하다. 복합 산화물로서는, 예를 들면, 리튬 티탄 복합 산화물이나 리튬 바나듐 복합 산화물 등을 들 수 있다. 이차 전지용 음극 활물질로서는, 이 중, 금속 산화물 재료나 탄소질 재료가 안전성의 면에서 보아 바람직하다.Examples of negative electrode active materials for secondary batteries that can be used include inorganic compounds such as lithium metal, lithium alloy, and tin compounds, carbonaceous materials capable of inserting and releasing lithium ions, complex oxides containing multiple elements, and conductive polymers. You can. Carbonaceous materials include, for example, coke, glassy carbon, graphite, non-graphitizable carbon, pyrolytic carbon, and carbon fiber. Among these, graphites such as artificial graphite and natural graphite have an operating potential close to that of metallic lithium, enable charging and discharging at high operating voltages, and suppress self-discharge when lithium salts are used as supporting salts. This is preferable because the irreversible capacity during charging can be reduced. Examples of the complex oxide include lithium titanium complex oxide and lithium vanadium complex oxide. As a negative electrode active material for secondary batteries, metal oxide materials and carbonaceous materials are preferable from the viewpoint of safety.
또한, 이차 전지용 전극 페이스트에는, 상기 제1 개시 또는 제2 개시의 카본 나노 튜브 분산액과, 이차 전지용의 양극 또는 음극의 활물질과, 추가로 결착재(바인더)를 포함하는 것이 바람직하다.In addition, the electrode paste for secondary batteries preferably contains the carbon nanotube dispersion liquid of the first or second disclosure, an active material for the positive or negative electrode for secondary batteries, and further a binder.
이용할 수 있는 결착재(바인더)로서는, 예를 들면, 폴리이미드계 수지, 폴리플루오르화 비닐리덴(PVdF), 폴리테트라플루오로에틸렌, 4플루오르화 에틸렌·6플루오르화 프로필렌·플루오르화 비닐리덴계 공중합체, 6플루오르화 프로필렌·플루오르화 비닐리덴계 공중합체, 4플루오르화 에틸렌·퍼플루오로비닐 에테르계 공중합체 등의 불소 수지, 폴리에틸렌, 폴리프로필렌 등의 폴리올레핀 수지, 폴리비닐 피롤리돈, 폴리비닐 알코올, 스티렌 부타디엔 고무(SBR), 아크릴계 수지 등을 들 수 있다. 이들 결착재는 2종 이상을 혼합하여 이용해도 된다.As binders (binder) that can be used, for example, polyimide resin, polyvinylidene fluoride (PVdF), polytetrafluoroethylene, ethylene tetrafluoride, propylene hexafluoride, and vinylidene fluoride. Polymers, fluororesins such as hexafluorinated propylene/vinylidene fluoride copolymers, tetrafluorinated ethylene/perfluorovinyl ether copolymers, polyolefin resins such as polyethylene and polypropylene, polyvinyl pyrrolidone, and polyvinyl. Alcohol, styrene butadiene rubber (SBR), acrylic resin, etc. can be mentioned. Two or more types of these binders may be mixed and used.
이들 결착재의 양은, 집전박에 대한 밀착성, 셀화된 후의 전지 용량이나 충방전 특성의 점으로부터, 바람직하게는, 이차 전지용 전극 페이스트 전량에 대해서, 0.2~3.0 질량부, 보다 바람직하게는, 0.5~2.5 질량부 첨가하는 것이 바람직하다.The amount of these binders is preferably 0.2 to 3.0 parts by mass, more preferably 0.5 to 2.5 parts by mass, based on the total amount of electrode paste for secondary batteries, from the viewpoint of adhesion to the current collector foil, battery capacity and charge/discharge characteristics after cellization. It is preferable to add it in parts by mass.
또한, 이차 전지용 전극 페이스트에는, 각종 용매를 사용해도 된다. 용매로서는, 예를 들면, 물(정제수, 이온 교환수, 증류수, 초순수 등), 방향족계 용매, 알코올류, 다가 알코올류, 에테르계 용매, 글리콜 에테르계 용매, 에스테르계 용매, 아민계 용매, 아미드계 용매, 복소환계 용매, 설폭시드계 용매, 설폰계 용매 등을 들 수 있다. 이들 용매는, 각 단독 또는 2종 이상을 혼합하여 이용해도 된다.Additionally, various solvents may be used for the electrode paste for secondary batteries. Examples of solvents include water (purified water, ion-exchanged water, distilled water, ultrapure water, etc.), aromatic solvents, alcohols, polyhydric alcohols, ether solvents, glycol ether solvents, ester solvents, amine solvents, and amides. Examples include solvents, heterocyclic solvents, sulfoxide solvents, and sulfone solvents. These solvents may be used individually or in combination of two or more.
이들 용매의 양은, 전극용 분산체를 도공할 때에, 적절한 점성으로 끝내는 필요성의 점으로부터, 바람직하게는, 이차 전지용 전극 페이스트 전량에 대해서, 0.5~80 질량부, 보다 바람직하게는, 1~70 질량부 첨가하는 것이 바람직하다.The amount of these solvents is preferably 0.5 to 80 parts by mass, more preferably 1 to 70 parts by mass, based on the entire amount of electrode paste for secondary batteries, from the viewpoint of the need to achieve an appropriate viscosity when coating the dispersion for electrodes. It is desirable to add additional
또한, 상기 카본 나노 튜브 분산액, 활물질, 결착재 외에, 본 개시의 효과를 해치지 않는 범위에서, 레벨링제, 고체 전해질재 등을 적절히 배합할 수 있다.Additionally, in addition to the carbon nanotube dispersion liquid, active material, and binder, a leveling agent, a solid electrolyte material, etc. can be appropriately mixed within a range that does not impair the effect of the present disclosure.
이와 같이 구성되는 이차 전지용 전극 페이스트는, 상기 제1 개시 또는 제2 개시의 카본 나노 튜브 분산액과, 이차 전지용의 양극 또는 음극의 활물질과, 결착재(바인더), 용매 등을, 예를 들면, 2축형의 혼련기 등을 이용하는 것에 의해 조제할 수 있다.The electrode paste for secondary batteries configured in this way includes the carbon nanotube dispersion of the first or second disclosure, an active material for the positive or negative electrode for secondary batteries, a binder, a solvent, etc., for example, 2 It can be prepared by using a shaft-type kneader or the like.
얻어진 이차 전지용 전극 페이스트를 리튬 이온 이차 전지의 도전성 부재인 집전체 상에 도포하고 건조하는 것에 의해 소정의 리튬 이온 이차 전지용 양극, 음극을 얻을 수 있게 되고, 본 개시에서는, 장기간의 반복 충방전에 견딜 수 있는 전지 성능을 실현하는 이차 전지용 전극 페이스트, 이차 전지용 전극을 얻을 수 있게 된다.By applying the obtained secondary battery electrode paste onto a current collector, which is a conductive member of a lithium ion secondary battery, and drying it, a given positive electrode and a negative electrode for a lithium ion secondary battery can be obtained. In the present disclosure, the electrode paste can withstand repeated charging and discharging over a long period of time. It is possible to obtain electrode paste for secondary batteries and electrodes for secondary batteries that realize acceptable battery performance.
상기 전극에 사용하는 집전체의 재질이나 형상은 특별히 한정되지 않고, 각종 이차 전지에 있던 것을 적절히 선택할 수 있다. 예를 들면, 집전체의 재질로서는, 알루미늄, 구리, 니켈, 티탄, 또는 스텐레스 등의 금속이나 합금을 들 수 있다. 또한, 형상으로서는, 일반적으로는 평판상의 박이 이용되지만, 표면을 조면화한 것이나, 구멍 뚫린 박상(箔狀)의 것, 및 메쉬상의 집전체도 사용할 수 있다.The material or shape of the current collector used in the electrode is not particularly limited, and those found in various secondary batteries can be appropriately selected. For example, the material of the current collector includes metals or alloys such as aluminum, copper, nickel, titanium, or stainless steel. Additionally, as a shape, a flat foil is generally used, but a foil-shaped foil with a roughened surface, a perforated foil, and a mesh-shaped current collector can also be used.
집전체 상에 전극 페이스트를 도공하는 방법으로서는, 특히 제한은 없고 공지의 방법을 이용할 수 있다. 구체적으로는, 다이 코팅법, 딥 코팅법, 롤 코팅법, 닥터 코팅법, 나이프 코팅법, 스프레이 코팅법, 그라비아 코팅법, 스크린 인쇄법 또는 정전 도장법 등을 들 수가 있고, 건조 방법으로서는 방치 건조, 송풍 건조기, 온풍 건조기, 적외선 가열기, 원적외선 가열기 등을 사용할 수 있지만, 특별히 이들로 한정되는 것은 아니다.There is no particular limitation as a method for coating the electrode paste on the current collector, and a known method can be used. Specifically, die coating method, dip coating method, roll coating method, doctor coating method, knife coating method, spray coating method, gravure coating method, screen printing method, or electrostatic coating method can be used. Drying methods include standing drying, A blow dryer, a warm air dryer, an infrared heater, a far infrared heater, etc. can be used, but are not particularly limited to these.
또한, 도포 후에 평판 프레스나 캘린더 롤 등에 의한 압연 처리를 수행해도 된다. 전극재층의 두께는, 일반적으로는 1μm 이상, 500μm 이하이며, 바람직하게는 10μm 이상, 300μm 이하이다.Additionally, after application, rolling treatment using a flat press, calendar roll, etc. may be performed. The thickness of the electrode material layer is generally 1 μm or more and 500 μm or less, and is preferably 10 μm or more and 300 μm or less.
<이차 전지, 리튬 이온 이차 전지><Secondary battery, lithium ion secondary battery>
본 개시의 이차 전지는, 상기 이차 전지용 전극을 이용한 것을 특징으로 하는 것이고, 바람직하게는, 양극과, 음극과, 전해질을 구비하여 이루어지는 리튬 이온 이차 전지의 양극, 음극에 상기 이차 전지용 전극을 이용한 것이 바람직하다. 이하에 있어서, 리튬 이온 이차 전지에 이용했을 경우에 대하여 설명한다.The secondary battery of the present disclosure is characterized by using the above secondary battery electrode. Preferably, the above secondary battery electrode is used for the positive and negative electrodes of a lithium ion secondary battery comprising a positive electrode, a negative electrode, and an electrolyte. desirable. Below, the case of use in a lithium ion secondary battery will be explained.
양극으로서는, 상기 집전체 상에 양극 활물질을 포함하는 상술의 전극용 페이스트를 도공 건조하여 전극을 제작한 것을 사용할 수 있다.As the positive electrode, an electrode produced by coating and drying the above-described electrode paste containing the positive electrode active material on the current collector can be used.
음극으로서는, 집전체 상에 음극 활물질을 포함하는 전극용 페이스트를 도공 건조하여 전극을 제작한 것을 사용할 수 있다.As the negative electrode, an electrode produced by coating and drying an electrode paste containing a negative electrode active material on a current collector can be used.
전해질로서는, 이온이 이동 가능한 종래 공지의 여러가지 것을 사용할 수 있다. 예를 들면, LiBF4, LiClO4, LiPF6, LiAsF6, LiSbF6, LiCF3SO3, Li(CF3SO2)2N, LiC4F9SO3, Li(CF3SO2)3C, LiI, LiBr, LiCl, LiAlCl, LiHF2, LiSCN, 또는 LiBPh4(다만, Ph는 페닐기이다) 등 리튬염을 포함하는 것을 들 수 있지만, 이들로 한정되지 않는다. 전해질은 비수계의 용매에 용해하여, 전해액으로서 사용하는 것이 바람직하다.As the electrolyte, various conventionally known electrolytes capable of moving ions can be used. For example, LiBF 4 , LiClO 4 , LiPF 6 , LiAsF 6 , LiSbF 6 , LiCF 3 SO 3 , Li(CF 3 SO 2 ) 2 N, LiC 4 F 9 SO 3 , Li(CF 3 SO 2 ) 3 C , LiI, LiBr, LiCl, LiAlCl, LiHF 2 , LiSCN, or LiBPh 4 (however, Ph is a phenyl group), but are not limited to these. The electrolyte is preferably dissolved in a non-aqueous solvent and used as an electrolyte solution.
비수계의 용매로서는, 특별히 한정은 되지 않지만, 예를 들면, 에틸렌 카보네이트, 프로필렌 카보네이트, 부틸렌 카보네이트, 디메틸 카보네이트, 에틸 메틸 카보네이트, 및 디에틸 카보네이트 등의 카보네이트류; γ-부티로락톤, γ-발레로락톤, 및 γ-옥타노익 락톤 등의 락톤류; 테트라히드로퓨란, 2-메틸 테트라히드로퓨란, 1,3-디옥소란, 4-메틸-1,3-디옥소란, 1,2-메톡시 에탄, 1,2-에톡시 에탄, 및 1,2-디부톡시 에탄 등의 글라임류; 메틸포르메이트, 메틸아세테이트, 및 메틸프로피오네이트 등의 에스테르류; 디메틸 설폭시드, 및 설포란 등의 설폭시드류; 및, 아세토니트릴 등의 니트릴류 등을 들 수 있다. 이들 용매는, 각각 단독으로 사용해도 되지만, 2종 이상을 혼합하여 사용해도 된다.Non-aqueous solvents are not particularly limited and include, for example, carbonates such as ethylene carbonate, propylene carbonate, butylene carbonate, dimethyl carbonate, ethyl methyl carbonate, and diethyl carbonate; Lactones such as γ-butyrolactone, γ-valerolactone, and γ-octanoic lactone; Tetrahydrofuran, 2-methyl tetrahydrofuran, 1,3-dioxolane, 4-methyl-1,3-dioxolane, 1,2-methoxy ethane, 1,2-ethoxy ethane, and 1, glymes such as 2-dibutoxy ethane; esters such as methyl formate, methyl acetate, and methyl propionate; Sulfoxides such as dimethyl sulfoxide and sulfolane; and nitriles such as acetonitrile. These solvents may be used individually, or two or more types may be mixed and used.
본 개시에 있어서, 리튬 이온 이차 전지에는, 세퍼레이터를 포함하는 것이 바람직하다. 세퍼레이터로서는, 예를 들면, 폴리에틸렌 부직포, 폴리프로필렌 부직포, 폴리아미드 부직포 및 이들에 친수성 처리를 가한 것을 들 수 있지만, 특별히 이들로 한정되는 것은 아니다.In the present disclosure, it is preferable that the lithium ion secondary battery includes a separator. Examples of the separator include polyethylene nonwoven fabric, polypropylene nonwoven fabric, polyamide nonwoven fabric, and those that have been subjected to hydrophilic treatment, but are not particularly limited to these.
리튬 이온 이차 전지의 구조는 특별히 한정되지 않지만, 통상, 양극 및 음극과, 필요에 따라서 설치되는 세퍼레이터로부터 구성되고, 페이퍼형, 원통형, 버튼형, 적층형 등, 사용하는 목적에 따른 여러 가지의 형상으로 할 수 있다.The structure of a lithium ion secondary battery is not particularly limited, but is usually composed of a positive electrode, a negative electrode, and a separator installed as needed, and can be of various shapes depending on the purpose of use, such as paper type, cylindrical type, button type, and stacked type. You can.
이와 같이 구성되는 본 개시의 이차 전지로 이루어지는 리튬 이온 이차 전지 등은, 장기간의 반복 충방전에 견딜 수 있는 전지 성능을 실현하는 이차 전지를 얻을 수 있게 된다.A lithium ion secondary battery made of the secondary battery of the present disclosure configured in this way can obtain a secondary battery that realizes battery performance that can withstand repeated charging and discharging over a long period of time.
[실시예][Example]
이하에 본 개시를 실시예에 의해 설명하지만, 본 개시는 이들 실시예로 한정되는 것은 아니다.The present disclosure will be described below by way of examples, but the present disclosure is not limited to these examples.
[제1 개시: 실시예 1~11, 비교예 1~2: 카본 나노 튜브 분산액의 조제][First disclosure: Examples 1 to 11, Comparative examples 1 to 2: Preparation of carbon nanotube dispersion]
하기 표 1에 나타내는 배합 조성 [카본 나노 튜브, 분산제(고분자 재료), 분산매의 각 량]으로, 하기 분산 장치, 분산 조건으로 분산하여 카본 나노 튜브 분산액을 조제했다.A carbon nanotube dispersion was prepared using the mixing composition shown in Table 1 below (each amount of carbon nanotubes, dispersant (polymer material), and dispersion medium) and dispersing using the following dispersing device and dispersing conditions.
분산 장치: 횡형 비즈 밀 Dispersing device: horizontal bead mill
분산 조건: Φ0.5 mm 지르코니아 비즈 Dispersion conditions: Φ0.5 mm zirconia beads
얻어진 카본 나노 튜브 분산액의 카본 나노 튜브 농도를, 분산매로서 이용한 정제수 또는 NMP를 이용하여 2 질량%로 조정하고, 그 농도 조정한 분산액을, 50μm의 간극을 가지는 어플리케이터(YD-2형/요시미트 세이키사 제)로 PET 필름 상에 도포하고, 온도 80℃에서 건조하여 제작한 건조 도막의 XYZ 표색계의 각 값을 하기 표 1에 기재하면서, 하기 방법으로, 안정성과 도전성에 대해서, 하기 평가 기준에 의하여 평가했다. 이들 평가 결과를 하기 표 1에 나타내다.The carbon nanotube concentration of the obtained carbon nanotube dispersion was adjusted to 2% by mass using purified water or NMP as a dispersion medium, and the concentration-adjusted dispersion was applied to an applicator (YD-2 type/Yoshimit Sei) with a gap of 50 μm. Each value of the evaluated. The results of these evaluations are shown in Table 1 below.
[제2 개시: 실시예 12~22, 비교예 3~6: 카본 나노 튜브 분산액의 조제][Second disclosure: Examples 12 to 22, Comparative Examples 3 to 6: Preparation of carbon nanotube dispersion]
하기 표 2에 나타내는 배합 조성 [카본 나노 튜브, 분산제(고분자 재료), 분산매의 각 량]으로, 하기 분산 장치, 분산 조건으로 분산하여 카본 나노 튜브 분산액을 조제했다. A carbon nanotube dispersion was prepared using the mixing composition shown in Table 2 below (each amount of carbon nanotubes, dispersant (polymer material), and dispersion medium) and dispersing using the following dispersing device and dispersing conditions.
분산 장치: 횡형 비즈 밀 Dispersing device: horizontal bead mill
분산 조건: Φ0.5 mm 지르코니아 비즈 Dispersion conditions: Φ0.5 mm zirconia beads
얻어진 카본 나노 튜브 분산액의 카본 나노 튜브 농도를, 분산매로서 이용한 정제수 또는 NMP를 이용하여 2 질량%로 조정하고, 그 농도 조정한 분산액을, 50μm의 간극을 가지는 어플리케이터(YD-2형/요시미트 세이키사 제)로 PET 필름 상에 도포하고, 온도 80℃에서 건조하여 제작한 건조 도막의 L*a*b* 색공간의 a*와 b*의 각 값을 하기 표 2에 기재하면서, 하기 방법으로, 안정성과 도전성에 대해서, 하기 평가 기준에 의하여 평가했다. 이들 평가 결과를 하기 표 2에 나타내다.The carbon nanotube concentration of the obtained carbon nanotube dispersion was adjusted to 2% by mass using purified water or NMP as a dispersion medium, and the concentration-adjusted dispersion was applied to an applicator (YD-2 type/Yoshimit Sei) with a gap of 50 μm. The values of a * and b * in the L * a * b * color space of the dry coating film produced by applying it on a PET film and drying at a temperature of 80 ° C. are listed in Table 2 below, and were prepared by the following method. , stability and conductivity were evaluated according to the following evaluation criteria. The results of these evaluations are shown in Table 2 below.
(건조 도막의 XYZ 표색계 또는 L*a*b* 색공간의 각 값의 측정 방법) (Method of measuring each value of the XYZ colorimetric system or L * a * b * color space of the dried film)
측정 장치: 분광 측색계(SC-T(P), 스가 시켄키사 제) Measuring device: Spectrophotometer (SC-T(P), manufactured by Suga Shikenki Co., Ltd.)
광학 조건: 확산 조명 8° 수광 d8방식(정반사를 제외하다) Optical conditions: Diffuse illumination 8° light receiving d8 method (excluding regular reflection)
광원: 12V 50W 할로겐 램프Light source: 12V 50W halogen lamp
측색 조건: D65 광, 2°시야 Colorimetry conditions: D65 light, 2° field of view
측정 영역: 5φ(3개소 측정의 평균)Measurement area: 5ϕ (average of 3 measurements)
(분산액 점도의 측정 방법) (Method for measuring dispersion viscosity)
콘 플레이트형 점도계(토키 산교사 제, 1°34´R24 콘)를 이용하여 25℃에서 10 rpm(전단 속도 38.3s-1)의 조건에 의해, 점도를 측정했다.The viscosity was measured at 25°C and 10 rpm (shear rate 38.3 s -1 ) using a cone plate type viscometer (1°34'R24 cone, manufactured by Toki Sangyo Co., Ltd.).
(안정성의 평가 방법)(Stability evaluation method)
(1) 경시 점도의 변화율, (2) 경시에서의 액의 외관, (3) 경시 후의 액을 막으로 했을 때의 상태를 각각 평가하고, 그들의 결과[(1)~(3)]로부터 하기 평가 기준으로 안정성을 종합 평가했다.(1) The rate of change in viscosity over time, (2) the appearance of the liquid over time, and (3) the state of the liquid as a film after time elapsed were evaluated respectively, and the following evaluations were made based on the results [(1) to (3)]. Based on the standard, stability was comprehensively evaluated.
(1) 경시 점도의 변화율의 평가 방법 (1) Method for evaluating the rate of change in viscosity over time
완성한 분산액을, 25℃ 환경 하에서 1주간 두었을 때의 상기 점도 측정 방법에 의하여 구한 점도값의 변화로부터, 변화율(1주일 후/초기)을 구하고, 하기 평가 기준으로 경시 점도 변화율을 평가했다.The rate of change (after 1 week/initial) was determined from the change in viscosity value obtained by the viscosity measurement method above when the completed dispersion was placed in an environment at 25°C for 1 week, and the rate of change in viscosity over time was evaluated using the following evaluation criteria.
평가 기준:Evaluation standard:
A: 변화율이 200% 미만 A: Rate of change is less than 200%
B: 변화율이 200% 이상 500% 미만 B: Rate of change greater than 200% but less than 500%
C: 변화율이 500% 이상 C: Rate of change greater than 500%
(2) 경시에서의 액의 외관(2) Appearance of liquid over time
상기 (1)의 25℃ 환경 하에 1주간 두었을 때의 분산액의 외관을 하기 평가 기준으로 관능 평가했다.The appearance of the dispersion liquid (1) when placed in an environment at 25°C for one week was sensory evaluated using the following evaluation criteria.
평가 기준: Evaluation standard:
A: 분리도 농도 차이도 없고 균일 A: No separation or concentration difference, uniform
B: 분리나 농도 차이를 조금 볼 수 있지만, 간단하게 재교반에 의한 균일화가 가능 B: Separation and concentration differences can be seen slightly, but homogenization can be easily achieved by re-stirring.
C: 카본 나노 튜브가 침강하여, 재교반에 의한 균일화를 할 수 없다 C: Carbon nanotubes precipitate and cannot be homogenized by re-stirring.
(3) 경시 후의 액을 막으로 했을 때의 상태(3) The state of the liquid after aging as a film
완성한 분산액을, PET 필름(루미러 #100-T60, 도레이사)의 편면에 간극이 50μm인 어플리케이터로 도포한 후, 온도 80℃에서 건조하고, 얻어진 막의 상태를 하기 평가 기준으로 관능 평가했다.The completed dispersion was applied to one side of a PET film (Lumiror #100-T60, Toray Co., Ltd.) with an applicator with a gap of 50 μm, then dried at a temperature of 80°C, and the state of the obtained film was sensory evaluated using the following evaluation criteria.
A: 균일하고 평활한 도막을 얻을 수 있다 A: A uniform and smooth coating film can be obtained.
B: 응집립(粒)이 몇 개 보이거나, 혹은 약간 면내에 농도 차이가 있다 B: A few aggregated grains are visible, or there is a slight difference in concentration within the plane.
C: 표면이 까칠까칠해져 있거나, 혹은 균일하게 도포할 수 없다 C: The surface is rough or cannot be applied evenly.
안정성의 평가 기준: Evaluation criteria for stability:
◎: 상기 (1)~(3)의 평가 결과의 3항목이 모두 A평가 ◎: All three items in the evaluation results (1) to (3) above were rated A.
○: 상기 (1)~(3)의 평가 결과 중 2항목에서 A평가, 또한 C평가가 없다. ○: Among the evaluation results (1) to (3) above, 2 items received an A rating, and there was no C rating.
△: 상기 (1)~(3)의 평가 결과 중 A평가가 0~1항목, 또한 C평가가 없다 △: Among the evaluation results of (1) to (3) above, A evaluation is 0 to 1 item, and there is no C evaluation.
Х: 상기 (1)~(3)의 평가 결과 중 C평가가 1항목 이상 Х: Among the evaluation results in (1) to (3) above, at least one item received a C rating.
(도전성의 평가 방법) (Method for evaluating challenge)
완성한 분산액을, PET 필름(루미러 #100-T60, 도레이사)의 편면에 간극이 50μm인 어플리케이터로 도포한 후, 온도 80℃에서 건조하고, 얻어진 막의 저항값을 측정했다. 저항값은 시트 저항으로서, 탐침 간격 10 mm의 4탐침 프로브와 밀리 오옴 하이 테스터 3227(히오키 덴키사 제)로 이루어지는 장치를 이용하여 측정하고, 하기 평가 기준으로 도전성을 평가했다.The completed dispersion was applied to one side of a PET film (Lumiror #100-T60, Toray Co., Ltd.) with an applicator with a gap of 50 μm, dried at a temperature of 80°C, and the resistance value of the resulting film was measured. The resistance value was measured as sheet resistance using an apparatus consisting of a four-probe probe with a probe spacing of 10 mm and a milliohm Hi-Tester 3227 (manufactured by Hioki Denki Co., Ltd.), and conductivity was evaluated using the following evaluation criteria.
평가 기준: Evaluation standard:
◎: 시트 저항이 250Ω/□ 미만 ◎: Sheet resistance is less than 250Ω/□
○: 시트 저항이 250Ω/□ 이상 400Ω/□ 미만 ○: Sheet resistance is more than 250Ω/□ and less than 400Ω/□
△: 시트 저항이 400Ω/□ 이상 800Ω/□ 미만 △: Sheet resistance is more than 400Ω/□ and less than 800Ω/□
Х: 시트 저항이 800Ω/□ 이상 Х: Sheet resistance is 800Ω/□ or more
상기 표 1의 평가 결과 등으로부터 분명한 바와 같이, 제1 개시의 범위 내인 실시예 1~11의 카본 나노 튜브 분산액은, 안정성과 도전성이 고도로 양립하고, 아울러 뛰어난 것이 되었다. 이것에 비하여, 비교예 1~2의 카본 나노 튜브 분산액은, 상기 특성을 만족할 수 없었다.As is clear from the evaluation results in Table 1 above, the carbon nanotube dispersions of Examples 1 to 11, which fall within the scope of the first disclosure, have both high stability and conductivity, and are also excellent. In contrast, the carbon nanotube dispersions of Comparative Examples 1 and 2 could not satisfy the above characteristics.
상기 표 2의 평가 결과 등으로부터 분명한 바와 같이, 제2 개시의 범위 내인 실시예 12~22의 카본 나노 튜브 분산액은, 안정성과 도전성이 고도로 양립하고, 아울러 뛰어난 것이 되었다. 이것에 비하여, 비교예 3~6의 카본 나노 튜브 분산액은, 상기 특성을 만족할 수 없었다.As is clear from the evaluation results in Table 2 above, the carbon nanotube dispersions of Examples 12 to 22, which are within the scope of the second disclosure, have both high stability and conductivity, and are also excellent. In contrast, the carbon nanotube dispersions of Comparative Examples 3 to 6 could not satisfy the above characteristics.
카본 나노 튜브 분산액은, 안정성과 도전 성능이 뛰어나, 연료 전지, 각종 전극, 전자파 쉴드재, 도전성 수지, 전계 방출 디스플레이용 부재 등의 재료로서 유용하고, 특히 리튬 이온 이차 전지 등의 전극의 제조에 적합한 전극 페이스트, 전극의 제조에 이용할 수 있고, 장기간의 반복 충방전에 견딜 수 있는 뛰어난 전지 성능을 실현할 수 있다.Carbon nanotube dispersions have excellent stability and electrical conductivity, and are useful as materials for fuel cells, various electrodes, electromagnetic wave shielding materials, conductive resins, and members for field emission displays, and are particularly suitable for the production of electrodes such as lithium ion secondary batteries. It can be used in the production of electrode paste and electrodes, and excellent battery performance that can withstand repeated charging and discharging over a long period of time can be realized.
Claims (7)
상기 수용성 고분자 재료가, 비이온성 수용성 고분자와 음이온성 수용성 고분자로부터 선택되는 1 종류 이상의 고분자 재료인 것을 특징으로 하는, 카본 나노 튜브 분산액.In claim 1 or claim 2,
A carbon nanotube dispersion, characterized in that the water-soluble polymer material is at least one type of polymer material selected from nonionic water-soluble polymers and anionic water-soluble polymers.
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