WO2023226515A1 - Mxene-based composite conductive paste, and preparation method therefor and use thereof - Google Patents
Mxene-based composite conductive paste, and preparation method therefor and use thereof Download PDFInfo
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- WO2023226515A1 WO2023226515A1 PCT/CN2023/079961 CN2023079961W WO2023226515A1 WO 2023226515 A1 WO2023226515 A1 WO 2023226515A1 CN 2023079961 W CN2023079961 W CN 2023079961W WO 2023226515 A1 WO2023226515 A1 WO 2023226515A1
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- WIPO (PCT)
- Prior art keywords
- mxene
- conductive
- based composite
- sodium
- composite conductive
- Prior art date
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- 239000002131 composite material Substances 0.000 title claims abstract description 59
- 238000002360 preparation method Methods 0.000 title claims abstract description 20
- 239000000463 material Substances 0.000 claims abstract description 19
- 239000002904 solvent Substances 0.000 claims abstract description 16
- 239000002482 conductive additive Substances 0.000 claims abstract description 15
- 239000011259 mixed solution Substances 0.000 claims abstract description 14
- 239000002994 raw material Substances 0.000 claims abstract description 7
- 238000002156 mixing Methods 0.000 claims abstract description 4
- 239000002002 slurry Substances 0.000 claims description 48
- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical compound [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 claims description 19
- 239000006185 dispersion Substances 0.000 claims description 16
- 239000000243 solution Substances 0.000 claims description 15
- 239000000843 powder Substances 0.000 claims description 12
- 239000002202 Polyethylene glycol Substances 0.000 claims description 9
- 229920001223 polyethylene glycol Polymers 0.000 claims description 9
- BQCADISMDOOEFD-UHFFFAOYSA-N Silver Chemical compound [Ag] BQCADISMDOOEFD-UHFFFAOYSA-N 0.000 claims description 8
- 239000000203 mixture Substances 0.000 claims description 8
- -1 polytetrafluoroethylene Polymers 0.000 claims description 8
- LYCAIKOWRPUZTN-UHFFFAOYSA-N Ethylene glycol Chemical compound OCCO LYCAIKOWRPUZTN-UHFFFAOYSA-N 0.000 claims description 7
- 239000002041 carbon nanotube Substances 0.000 claims description 7
- 229910021393 carbon nanotube Inorganic materials 0.000 claims description 7
- 239000010410 layer Substances 0.000 claims description 7
- 239000002135 nanosheet Substances 0.000 claims description 7
- 229910052709 silver Inorganic materials 0.000 claims description 7
- 239000004332 silver Substances 0.000 claims description 7
- 238000003756 stirring Methods 0.000 claims description 7
- 238000010146 3D printing Methods 0.000 claims description 6
- CSCPPACGZOOCGX-UHFFFAOYSA-N Acetone Chemical compound CC(C)=O CSCPPACGZOOCGX-UHFFFAOYSA-N 0.000 claims description 6
- WEVYAHXRMPXWCK-UHFFFAOYSA-N Acetonitrile Chemical compound CC#N WEVYAHXRMPXWCK-UHFFFAOYSA-N 0.000 claims description 6
- UHOVQNZJYSORNB-UHFFFAOYSA-N Benzene Chemical compound C1=CC=CC=C1 UHOVQNZJYSORNB-UHFFFAOYSA-N 0.000 claims description 6
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 claims description 6
- OKKJLVBELUTLKV-UHFFFAOYSA-N Methanol Chemical compound OC OKKJLVBELUTLKV-UHFFFAOYSA-N 0.000 claims description 6
- ZMXDDKWLCZADIW-UHFFFAOYSA-N N,N-Dimethylformamide Chemical compound CN(C)C=O ZMXDDKWLCZADIW-UHFFFAOYSA-N 0.000 claims description 6
- FKNQFGJONOIPTF-UHFFFAOYSA-N Sodium cation Chemical compound [Na+] FKNQFGJONOIPTF-UHFFFAOYSA-N 0.000 claims description 6
- YXFVVABEGXRONW-UHFFFAOYSA-N Toluene Chemical compound CC1=CC=CC=C1 YXFVVABEGXRONW-UHFFFAOYSA-N 0.000 claims description 6
- 229910021389 graphene Inorganic materials 0.000 claims description 6
- 238000007639 printing Methods 0.000 claims description 6
- SQGYOTSLMSWVJD-UHFFFAOYSA-N silver(1+) nitrate Chemical group [Ag+].[O-]N(=O)=O SQGYOTSLMSWVJD-UHFFFAOYSA-N 0.000 claims description 6
- 229910001415 sodium ion Inorganic materials 0.000 claims description 6
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims description 6
- RTZKZFJDLAIYFH-UHFFFAOYSA-N Diethyl ether Chemical compound CCOCC RTZKZFJDLAIYFH-UHFFFAOYSA-N 0.000 claims description 5
- HBBGRARXTFLTSG-UHFFFAOYSA-N Lithium ion Chemical compound [Li+] HBBGRARXTFLTSG-UHFFFAOYSA-N 0.000 claims description 5
- 229910001416 lithium ion Inorganic materials 0.000 claims description 5
- VNWKTOKETHGBQD-UHFFFAOYSA-N methane Chemical compound C VNWKTOKETHGBQD-UHFFFAOYSA-N 0.000 claims description 5
- IAZDPXIOMUYVGZ-UHFFFAOYSA-N Dimethylsulphoxide Chemical compound CS(C)=O IAZDPXIOMUYVGZ-UHFFFAOYSA-N 0.000 claims description 4
- ZHNUHDYFZUAESO-UHFFFAOYSA-N Formamide Chemical compound NC=O ZHNUHDYFZUAESO-UHFFFAOYSA-N 0.000 claims description 4
- SECXISVLQFMRJM-UHFFFAOYSA-N N-Methylpyrrolidone Chemical compound CN1CCCC1=O SECXISVLQFMRJM-UHFFFAOYSA-N 0.000 claims description 4
- 239000002033 PVDF binder Substances 0.000 claims description 4
- PPBRXRYQALVLMV-UHFFFAOYSA-N Styrene Chemical compound C=CC1=CC=CC=C1 PPBRXRYQALVLMV-UHFFFAOYSA-N 0.000 claims description 4
- 238000000498 ball milling Methods 0.000 claims description 4
- 239000003575 carbonaceous material Substances 0.000 claims description 4
- VYFYYTLLBUKUHU-UHFFFAOYSA-N dopamine Chemical compound NCCC1=CC=C(O)C(O)=C1 VYFYYTLLBUKUHU-UHFFFAOYSA-N 0.000 claims description 4
- 238000000034 method Methods 0.000 claims description 4
- BASFCYQUMIYNBI-UHFFFAOYSA-N platinum Chemical compound [Pt] BASFCYQUMIYNBI-UHFFFAOYSA-N 0.000 claims description 4
- 229920001343 polytetrafluoroethylene Polymers 0.000 claims description 4
- 239000004810 polytetrafluoroethylene Substances 0.000 claims description 4
- 229920002981 polyvinylidene fluoride Polymers 0.000 claims description 4
- 239000011734 sodium Substances 0.000 claims description 4
- 229910052708 sodium Inorganic materials 0.000 claims description 4
- VZGDMQKNWNREIO-UHFFFAOYSA-N tetrachloromethane Chemical compound ClC(Cl)(Cl)Cl VZGDMQKNWNREIO-UHFFFAOYSA-N 0.000 claims description 4
- 238000001238 wet grinding Methods 0.000 claims description 4
- 239000004372 Polyvinyl alcohol Substances 0.000 claims description 3
- DPXJVFZANSGRMM-UHFFFAOYSA-N acetic acid;2,3,4,5,6-pentahydroxyhexanal;sodium Chemical compound [Na].CC(O)=O.OCC(O)C(O)C(O)C(O)C=O DPXJVFZANSGRMM-UHFFFAOYSA-N 0.000 claims description 3
- 229910052799 carbon Inorganic materials 0.000 claims description 3
- 239000001768 carboxy methyl cellulose Substances 0.000 claims description 3
- 229910002804 graphite Inorganic materials 0.000 claims description 3
- 239000010439 graphite Substances 0.000 claims description 3
- 229920003063 hydroxymethyl cellulose Polymers 0.000 claims description 3
- 229940031574 hydroxymethyl cellulose Drugs 0.000 claims description 3
- 229920002451 polyvinyl alcohol Polymers 0.000 claims description 3
- 229910001961 silver nitrate Inorganic materials 0.000 claims description 3
- 235000019812 sodium carboxymethyl cellulose Nutrition 0.000 claims description 3
- 229920001027 sodium carboxymethylcellulose Polymers 0.000 claims description 3
- ALSTYHKOOCGGFT-KTKRTIGZSA-N (9Z)-octadecen-1-ol Chemical compound CCCCCCCC\C=C/CCCCCCCCO ALSTYHKOOCGGFT-KTKRTIGZSA-N 0.000 claims description 2
- QGLWBTPVKHMVHM-KTKRTIGZSA-N (z)-octadec-9-en-1-amine Chemical compound CCCCCCCC\C=C/CCCCCCCCN QGLWBTPVKHMVHM-KTKRTIGZSA-N 0.000 claims description 2
- 239000002028 Biomass Substances 0.000 claims description 2
- LZZYPRNAOMGNLH-UHFFFAOYSA-M Cetrimonium bromide Chemical compound [Br-].CCCCCCCCCCCCCCCC[N+](C)(C)C LZZYPRNAOMGNLH-UHFFFAOYSA-M 0.000 claims description 2
- 229920001661 Chitosan Polymers 0.000 claims description 2
- RYGMFSIKBFXOCR-UHFFFAOYSA-N Copper Chemical compound [Cu] RYGMFSIKBFXOCR-UHFFFAOYSA-N 0.000 claims description 2
- XDTMQSROBMDMFD-UHFFFAOYSA-N Cyclohexane Chemical compound C1CCCCC1 XDTMQSROBMDMFD-UHFFFAOYSA-N 0.000 claims description 2
- 108010010803 Gelatin Proteins 0.000 claims description 2
- 229920002153 Hydroxypropyl cellulose Polymers 0.000 claims description 2
- DGAQECJNVWCQMB-PUAWFVPOSA-M Ilexoside XXIX Chemical compound C[C@@H]1CC[C@@]2(CC[C@@]3(C(=CC[C@H]4[C@]3(CC[C@@H]5[C@@]4(CC[C@@H](C5(C)C)OS(=O)(=O)[O-])C)C)[C@@H]2[C@]1(C)O)C)C(=O)O[C@H]6[C@@H]([C@H]([C@@H]([C@H](O6)CO)O)O)O.[Na+] DGAQECJNVWCQMB-PUAWFVPOSA-M 0.000 claims description 2
- FXHOOIRPVKKKFG-UHFFFAOYSA-N N,N-Dimethylacetamide Chemical compound CN(C)C(C)=O FXHOOIRPVKKKFG-UHFFFAOYSA-N 0.000 claims description 2
- DBMJMQXJHONAFJ-UHFFFAOYSA-M Sodium laurylsulphate Chemical compound [Na+].CCCCCCCCCCCCOS([O-])(=O)=O DBMJMQXJHONAFJ-UHFFFAOYSA-M 0.000 claims description 2
- 150000008051 alkyl sulfates Chemical group 0.000 claims description 2
- BTBJBAZGXNKLQC-UHFFFAOYSA-N ammonium lauryl sulfate Chemical compound [NH4+].CCCCCCCCCCCCOS([O-])(=O)=O BTBJBAZGXNKLQC-UHFFFAOYSA-N 0.000 claims description 2
- 229940063953 ammonium lauryl sulfate Drugs 0.000 claims description 2
- 239000007864 aqueous solution Substances 0.000 claims description 2
- 239000006229 carbon black Substances 0.000 claims description 2
- 229920003086 cellulose ether Polymers 0.000 claims description 2
- WOWHHFRSBJGXCM-UHFFFAOYSA-M cetyltrimethylammonium chloride Chemical compound [Cl-].CCCCCCCCCCCCCCCC[N+](C)(C)C WOWHHFRSBJGXCM-UHFFFAOYSA-M 0.000 claims description 2
- 229910052802 copper Inorganic materials 0.000 claims description 2
- 239000010949 copper Substances 0.000 claims description 2
- RZHBMYQXKIDANM-UHFFFAOYSA-N dioctyl butanedioate;sodium Chemical compound [Na].CCCCCCCCOC(=O)CCC(=O)OCCCCCCCC RZHBMYQXKIDANM-UHFFFAOYSA-N 0.000 claims description 2
- GVGUFUZHNYFZLC-UHFFFAOYSA-N dodecyl benzenesulfonate;sodium Chemical compound [Na].CCCCCCCCCCCCOS(=O)(=O)C1=CC=CC=C1 GVGUFUZHNYFZLC-UHFFFAOYSA-N 0.000 claims description 2
- TVACALAUIQMRDF-UHFFFAOYSA-N dodecyl dihydrogen phosphate Chemical compound CCCCCCCCCCCCOP(O)(O)=O TVACALAUIQMRDF-UHFFFAOYSA-N 0.000 claims description 2
- 229960003638 dopamine Drugs 0.000 claims description 2
- 229920000840 ethylene tetrafluoroethylene copolymer Polymers 0.000 claims description 2
- 229920000159 gelatin Polymers 0.000 claims description 2
- 239000008273 gelatin Substances 0.000 claims description 2
- 235000019322 gelatine Nutrition 0.000 claims description 2
- 235000011852 gelatine desserts Nutrition 0.000 claims description 2
- PCHJSUWPFVWCPO-UHFFFAOYSA-N gold Chemical compound [Au] PCHJSUWPFVWCPO-UHFFFAOYSA-N 0.000 claims description 2
- 229910052737 gold Inorganic materials 0.000 claims description 2
- 239000010931 gold Substances 0.000 claims description 2
- 239000001863 hydroxypropyl cellulose Substances 0.000 claims description 2
- 235000010977 hydroxypropyl cellulose Nutrition 0.000 claims description 2
- 229940094506 lauryl betaine Drugs 0.000 claims description 2
- DVEKCXOJTLDBFE-UHFFFAOYSA-N n-dodecyl-n,n-dimethylglycinate Chemical compound CCCCCCCCCCCC[N+](C)(C)CC([O-])=O DVEKCXOJTLDBFE-UHFFFAOYSA-N 0.000 claims description 2
- 229940055577 oleyl alcohol Drugs 0.000 claims description 2
- XMLQWXUVTXCDDL-UHFFFAOYSA-N oleyl alcohol Natural products CCCCCCC=CCCCCCCCCCCO XMLQWXUVTXCDDL-UHFFFAOYSA-N 0.000 claims description 2
- 229910052697 platinum Inorganic materials 0.000 claims description 2
- 229920000642 polymer Polymers 0.000 claims description 2
- 229940051841 polyoxyethylene ether Drugs 0.000 claims description 2
- 229920000056 polyoxyethylene ether Polymers 0.000 claims description 2
- 239000001267 polyvinylpyrrolidone Substances 0.000 claims description 2
- 229920000036 polyvinylpyrrolidone Polymers 0.000 claims description 2
- 235000013855 polyvinylpyrrolidone Nutrition 0.000 claims description 2
- CQLFBEKRDQMJLZ-UHFFFAOYSA-M silver acetate Chemical compound [Ag+].CC([O-])=O CQLFBEKRDQMJLZ-UHFFFAOYSA-M 0.000 claims description 2
- 229940071536 silver acetate Drugs 0.000 claims description 2
- XNGYKPINNDWGGF-UHFFFAOYSA-L silver oxalate Chemical compound [Ag+].[Ag+].[O-]C(=O)C([O-])=O XNGYKPINNDWGGF-UHFFFAOYSA-L 0.000 claims description 2
- JKOCEVIXVMBKJA-UHFFFAOYSA-M silver;butanoate Chemical compound [Ag+].CCCC([O-])=O JKOCEVIXVMBKJA-UHFFFAOYSA-M 0.000 claims description 2
- 239000002356 single layer Substances 0.000 claims description 2
- 229940080264 sodium dodecylbenzenesulfonate Drugs 0.000 claims description 2
- OABYVIYXWMZFFJ-ZUHYDKSRSA-M sodium glycocholate Chemical compound [Na+].C([C@H]1C[C@H]2O)[C@H](O)CC[C@]1(C)[C@@H]1[C@@H]2[C@@H]2CC[C@H]([C@@H](CCC(=O)NCC([O-])=O)C)[C@@]2(C)[C@@H](O)C1 OABYVIYXWMZFFJ-ZUHYDKSRSA-M 0.000 claims description 2
- 235000019333 sodium laurylsulphate Nutrition 0.000 claims description 2
- RYYKJJJTJZKILX-UHFFFAOYSA-M sodium octadecanoate Chemical compound [Na+].CCCCCCCCCCCCCCCCCC([O-])=O RYYKJJJTJZKILX-UHFFFAOYSA-M 0.000 claims description 2
- NWZBFJYXRGSRGD-UHFFFAOYSA-M sodium;octadecyl sulfate Chemical compound [Na+].CCCCCCCCCCCCCCCCCCOS([O-])(=O)=O NWZBFJYXRGSRGD-UHFFFAOYSA-M 0.000 claims description 2
- BDHFUVZGWQCTTF-UHFFFAOYSA-M sulfonate Chemical compound [O-]S(=O)=O BDHFUVZGWQCTTF-UHFFFAOYSA-M 0.000 claims description 2
- LCGLNKUTAGEVQW-UHFFFAOYSA-N Dimethyl ether Chemical compound COC LCGLNKUTAGEVQW-UHFFFAOYSA-N 0.000 claims 1
- 150000004996 alkyl benzenes Chemical class 0.000 claims 1
- UUAGAQFQZIEFAH-UHFFFAOYSA-N chlorotrifluoroethylene Chemical group FC(F)=C(F)Cl UUAGAQFQZIEFAH-UHFFFAOYSA-N 0.000 claims 1
- 229940124530 sulfonamide Drugs 0.000 claims 1
- XDRDMVYFQARLNH-UHFFFAOYSA-N tridecan-1-amine;hydrochloride Chemical compound Cl.CCCCCCCCCCCCCN XDRDMVYFQARLNH-UHFFFAOYSA-N 0.000 claims 1
- AQZSPJRLCJSOED-UHFFFAOYSA-M trimethyl(octyl)azanium;chloride Chemical compound [Cl-].CCCCCCCC[N+](C)(C)C AQZSPJRLCJSOED-UHFFFAOYSA-M 0.000 claims 1
- 238000003860 storage Methods 0.000 abstract description 3
- 238000013329 compounding Methods 0.000 abstract 1
- 239000007788 liquid Substances 0.000 description 5
- 239000004020 conductor Substances 0.000 description 4
- 239000008367 deionised water Substances 0.000 description 3
- 229910021641 deionized water Inorganic materials 0.000 description 3
- 230000005012 migration Effects 0.000 description 3
- 238000013508 migration Methods 0.000 description 3
- 238000012360 testing method Methods 0.000 description 3
- XNWFRZJHXBZDAG-UHFFFAOYSA-N 2-METHOXYETHANOL Chemical compound COCCO XNWFRZJHXBZDAG-UHFFFAOYSA-N 0.000 description 2
- 238000005054 agglomeration Methods 0.000 description 2
- 230000002776 aggregation Effects 0.000 description 2
- 230000009286 beneficial effect Effects 0.000 description 2
- 230000008901 benefit Effects 0.000 description 2
- 230000002427 irreversible effect Effects 0.000 description 2
- 229910052751 metal Inorganic materials 0.000 description 2
- 239000002184 metal Substances 0.000 description 2
- 229910052723 transition metal Inorganic materials 0.000 description 2
- 150000003624 transition metals Chemical class 0.000 description 2
- OSNIIMCBVLBNGS-UHFFFAOYSA-N 1-(1,3-benzodioxol-5-yl)-2-(dimethylamino)propan-1-one Chemical compound CN(C)C(C)C(=O)C1=CC=C2OCOC2=C1 OSNIIMCBVLBNGS-UHFFFAOYSA-N 0.000 description 1
- WHXSMMKQMYFTQS-UHFFFAOYSA-N Lithium Chemical compound [Li] WHXSMMKQMYFTQS-UHFFFAOYSA-N 0.000 description 1
- VBIIFPGSPJYLRR-UHFFFAOYSA-M Stearyltrimethylammonium chloride Chemical compound [Cl-].CCCCCCCCCCCCCCCCCC[N+](C)(C)C VBIIFPGSPJYLRR-UHFFFAOYSA-M 0.000 description 1
- 238000005411 Van der Waals force Methods 0.000 description 1
- 239000000654 additive Substances 0.000 description 1
- 125000005210 alkyl ammonium group Chemical group 0.000 description 1
- 229940077388 benzenesulfonate Drugs 0.000 description 1
- 230000015572 biosynthetic process Effects 0.000 description 1
- 230000008859 change Effects 0.000 description 1
- 239000006258 conductive agent Substances 0.000 description 1
- 230000032798 delamination Effects 0.000 description 1
- 238000001514 detection method Methods 0.000 description 1
- 238000010586 diagram Methods 0.000 description 1
- 239000007772 electrode material Substances 0.000 description 1
- 238000005516 engineering process Methods 0.000 description 1
- 239000000945 filler Substances 0.000 description 1
- 238000010438 heat treatment Methods 0.000 description 1
- 150000002500 ions Chemical class 0.000 description 1
- 238000011031 large-scale manufacturing process Methods 0.000 description 1
- 229910052744 lithium Inorganic materials 0.000 description 1
- 238000012986 modification Methods 0.000 description 1
- 230000004048 modification Effects 0.000 description 1
- SVBAPZTYWZGPKN-UHFFFAOYSA-N n-methyldodecan-1-amine;hydrochloride Chemical compound Cl.CCCCCCCCCCCCNC SVBAPZTYWZGPKN-UHFFFAOYSA-N 0.000 description 1
- 230000007935 neutral effect Effects 0.000 description 1
- 150000004767 nitrides Chemical class 0.000 description 1
- 238000011056 performance test Methods 0.000 description 1
- 229920002493 poly(chlorotrifluoroethylene) Polymers 0.000 description 1
- 239000005023 polychlorotrifluoroethylene (PCTFE) polymer Substances 0.000 description 1
- 235000019422 polyvinyl alcohol Nutrition 0.000 description 1
- 229920002620 polyvinyl fluoride Polymers 0.000 description 1
- 230000008569 process Effects 0.000 description 1
- 239000007787 solid Substances 0.000 description 1
- 238000013112 stability test Methods 0.000 description 1
- 238000013517 stratification Methods 0.000 description 1
- 239000000758 substrate Substances 0.000 description 1
- 238000003786 synthesis reaction Methods 0.000 description 1
Classifications
-
- 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
- H01B—CABLES; CONDUCTORS; INSULATORS; SELECTION OF MATERIALS FOR THEIR CONDUCTIVE, INSULATING OR DIELECTRIC PROPERTIES
- H01B13/00—Apparatus or processes specially adapted for manufacturing conductors or cables
Definitions
- the invention relates to the technical field of electrode materials and their preparation, and in particular to an MXene-based composite conductive slurry and its preparation method and application.
- Conductive slurry also known as conductive ink refers to a viscous liquid with electrical conductivity. It uses conductive materials dispersed in the slurry to build a conductive network to promote the migration of electrons.
- Conductive slurry is generally mainly composed of conductive materials, filled conductive additives, dispersion aids and solvents. Dispersion additives are used to evenly disperse the conductive material in the solvent to build a conductive network, and then filler conductive additives are added to fill the gaps in the conductive network and further improve the conductivity of the conductive slurry. Therefore, the conductivity, dispersion, stability and other properties of conductive paste directly affect its application in various fields.
- MXene As an emerging two-dimensional (2D) transition metal carbide/nitride, MXene has attracted widespread attention from researchers from various countries since 2011. In terms of structure, MXene is a two-dimensional material with a graphene-like structure composed of alternating carbon layers and transition metal layers. It has a large specific surface area and excellent metal conductivity. Compared with traditional conductive agents, such as conductive carbon black, carbon nanotubes, graphene, etc., MXene has higher conductivity and requires a relatively low dosage. More importantly, as a new type of conductive material, MXene has a three-dimensional conductive skeleton built by superimposing large layers of structure that can promote the rapid migration of electrons.
- MXene conductive paste due to the large layer structure and high specific surface area of MXene, there are strong van der Waals forces between MXene sheets, causing irreversible stacking and agglomeration of MXene nanosheets, making it difficult to disperse evenly into the solvent, seriously affecting the It demonstrates the conductivity, dispersibility and other properties of MXene conductive paste.
- the exposed terminal metal atoms on the surface of the MXene sheet are easily oxidized, thereby losing the intrinsic properties of MXene. Therefore, how to develop a highly conductive, highly stable, and uniformly dispersed MXene conductive slurry has become an urgent technical problem that needs to be solved.
- the present invention provides an MXene-based composite conductive slurry and its preparation method and application to solve the problem of irreversible stacking and agglomeration of MXene nanosheets in the existing technology, which makes it difficult to evenly disperse into the solvent, thereby seriously affecting the MXene Technical issues related to the performance of conductive paste such as conductivity and dispersion.
- the present invention provides an MXene-based composite conductive slurry, which is compounded from the following raw materials in weight percentages: MXene conductive base material 0.01-50%, filled conductive additive 0-50%, dispersion aid 0.5 -10% and solvent 50-99.5%.
- the MXene conductive base material is MXene powder, MXene single-layer nanosheets, MXene multi-layer nanosheets, carbon nanotube@MXene composite materials, graphene@MXene composite materials, conductive One or more of carbon black@MXene composite materials, biomass carbon@MXene composite materials, and polymer @MXene composite materials.
- the filled conductive additive is one or more of carbon materials, nanometal powders, and organic silver, wherein the carbon material is conductive graphite, conductive carbon black, graphene or carbon nanotubes.
- the nanometal powder is silver nanometal, copper nanometal, gold nanometal or platinum nanometal powder;
- the organic silver is silver nitrate, silver acetate, silver oxalate or silver butyrate.
- the dispersion aids are sodium stearyl sulfate, sodium stearate, sodium dioctyl succinate sulfonate, sodium glycocholate, oleyl alcohol polyoxyethylene ether, alkyl Ammonium benzenesulfonate, sodium lauryl sulfate, ammonium lauryl sulfate, lauryl phosphate, sodium secondary alkyl sulfate, sodium alpha-alkenyl sulfonate, stearyltrimethylammonium chloride , cetyltrimethylammonium chloride, lauryl betaine, lauryl methyl ammonium chloride, polyvinyl alcohol, gelatin, hydroxymethylcellulose, hydroxypropylcellulose, cellulose ether , polyvinylidene fluoride, polyvinylpyrrolidone, polyethylene glycol or sodium carboxymethyl cellulose, carbon nanotube solution, chitosan aqueous solution,
- the solvent is water, methanol, ethanol, ethylene glycol, polyethylene glycol, diethyl ether, benzene, toluene, styrene, acetone, acetonitrile, formamide, dimethyl sulfoxide, One or more of carbon tetrachloride, N-methylpyrrolidone, N,N-dimethylformamide, N,N-dimethylacetamide, and cyclohexane.
- the invention also provides a preparation method of MXene-based composite conductive slurry, which includes the following steps:
- step 2) Add the MXene conductive base material and the filled conductive additive to the mixed solution prepared in step 1), and mix evenly to obtain an MXene-based composite conductive slurry.
- both steps 1) and 2) are mixed by stirring, ultrasonic, oscillating, wet grinding or ball milling, and the mixing time of step 2) is 0.1 to 24 hours.
- step 1) and step 2) in terms of weight percentage, the proportion of each raw material is: MXene conductive base material is 0.01-50%, filled conductive additive is 0-50%, dispersion aid The dosage is 0.5-10%, The solvent is 50-99.5%, and by changing the raw material ratio, the dispersion and stability of the MXene conductive-based material in the solvent can be achieved, as well as the conductivity of the product MXene-based composite conductive slurry can be controlled.
- the present invention also provides an application of MXene-based composite conductive slurry, which is used as a conductive additive in 3D printing, printing, touch screen films, displays, Transparent conductive films, sensors, flexible electronics, lithium-ion batteries, sodium-ion batteries or supercapacitors.
- the MXene-based composite conductive slurry of the present invention takes full advantage of the conductivity of MXene and further solves the problems of dispersion and storage stability of MXene. Moreover, compared with traditional conductive slurries, it has better performance in application The required amount is also relatively low, which is beneficial to saving materials, that is, reducing costs;
- the MXene-based composite conductive paste of the present invention can be widely used as a conductive additive in 3D printing, printing, touch screen films, displays, transparent conductive films, sensors, flexible electronic products, lithium-ion batteries, sodium-ion batteries, supercapacitors, etc.
- a stable conductive network can be built on the substrate to promote the rapid migration of electrons;
- the preparation method of the MXene-based composite conductive slurry of the present invention is simple and safe to operate, has mild conditions, is environmentally friendly, and can achieve large-scale production.
- Figure 1 is a diagram showing the stability test results of the MXene-based composite conductive slurries prepared in Examples 1 to 5 respectively.
- An MXene-based composite conductive slurry and a preparation method thereof includes the following steps:
- step (2) Add 10g of etched multi-layer MXene nanosheets and 1g of conductive carbon black to the mixed solution prepared in step (1), and treat it ultrasonically for 24 hours to obtain a water-based MXene-based composite conductive slurry.
- An MXene-based composite conductive slurry and a preparation method thereof includes the following steps:
- step (2) Add 200 mg of etched MXene powder and 500 mg of silver nanopowder to the mixed solution prepared in step (1), and perform wet grinding for 3 hours to obtain an MXene-based composite conductive slurry.
- An MXene-based composite conductive slurry and a preparation method thereof includes the following steps:
- step (2) Add 500 mg of MXene powder material and 200 mg of silver nitrate to the mixed solution prepared in step (1), and stir for 5 hours to obtain an MXene-based composite conductive slurry.
- An MXene-based composite conductive slurry and a preparation method thereof includes the following steps:
- step (2) Add 200 mg of MXene powder material and 500 mg of graphene into the mixed liquid prepared in step (1), and process it by ball milling for 14 hours to obtain an MXene-based composite conductive slurry.
- An MXene-based composite conductive slurry and a preparation method thereof includes the following steps:
- step (2) Add 100 mg of MXene powder material and 500 mg of conductive carbon black to the mixed liquid prepared in step (1), and stir for 20 hours to obtain an MXene-based composite conductive slurry.
- the MXene composite conductive slurry prepared in Examples 1 to 5 of the present invention has a neutral pH and exhibits excellent viscosity and solid content, which can fully satisfy the needs of 3D printing, printing, and touch screen films. , displays, transparent conductive films, sensors, flexible electronics, lithium-ion batteries, sodium-ion batteries and supercapacitors.
- the MXene-based composite conductive slurry prepared in Examples 1 to 5 was subjected to conductivity testing, and the results are shown in Table 2.
- the MXene composite conductive slurries prepared in Examples 1 to 5 of the present invention all exhibit excellent conductivity and can fully meet the needs of 3D printing, printing, touch screen films, displays, transparent conductive films, and sensors. , flexible electronic products, lithium-ion batteries, sodium-ion batteries and supercapacitors and other fields of demand for conductive paste.
- the MXene composite conductive slurry prepared in Examples 1 to 5 was subjected to a solid-liquid delamination test. As shown in Figure 1, it is an image obtained after one month of rest. It can be seen from observation that the MXene composite conductive slurry after one month of rest still remains Good dispersion and no solid-liquid stratification phenomenon occurred, indicating that it has good dispersion and good storage stability.
- Embodiments 1 to 5 are preferred examples of the synthesis of MXene-based composite conductive slurries of the present invention. It can be understood that each embodiment is the optimal ratio of the selected materials. In addition, from the perspective of conductivity performance, Embodiment 1 is the best, and all performances are stable and reliable. It is more suitable for 3D printing, printing, touch screen films, displays, transparent conductive films, sensors, flexible electronic products, lithium Applications in ion batteries, sodium-ion batteries and supercapacitors.
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Abstract
An MXene-based composite conductive paste, and a preparation method therefor and the use thereof. The MXene-based composite conductive paste is prepared by compounding the following raw materials, in percentages by weight: 0.01-50% of an MXene conductive base material, 0-50% of a filling conductive additive, 0.5-10% of a dispersing auxiliary, and 50-99.5% of a solvent. The preparation method comprises: 1) adding a dispersing auxiliary into a solvent, and mixing same until uniform to obtain a mixed solution; and 2) adding an MXene conductive base material and a filling conductive additive to the mixed solution prepared in step 1), and mixing same until uniform to obtain an MXene-based composite conductive paste. The MXene-based composite conductive paste of the present invention has the characteristics of better conductivity, good dispersity, relatively good storage stability, etc.; moreover, compared with a traditional conductive paste, the amount thereof required during use is also relatively low, such that the saving of materials is facilitated, that is, the cost is reduced.
Description
交叉引用cross reference
本申请要求于2022年5月23日提交的中国申请202210563559.X的优先权，其全部内容通过引用并入本文。This application claims priority from Chinese application 202210563559.X filed on May 23, 2022, the entire content of which is incorporated herein by reference.
本发明涉及电极材料及其制备技术领域，具体涉及一种MXene基复合导电浆料及其制备方法和应用。The invention relates to the technical field of electrode materials and their preparation, and in particular to an MXene-based composite conductive slurry and its preparation method and application.
导电浆料(又称导电油墨)是指一种具有导电能力的粘稠液体，其是借助分散于浆料中的导电材料来构建导电网络来促进电子的迁移。导电浆料一般主要是由导电材料、填充导电添加剂、分散助剂和溶剂组成。采用分散助剂将导电材料均匀分散在溶剂中以构建导电网络，然后加入填充导电添加剂来弥补导电网络的空隙位置，进一步提升导电浆料的导电性。因此，导电浆料的电导率、分散性和稳定性等属性直接影响了其在各大领域的应用。Conductive slurry (also known as conductive ink) refers to a viscous liquid with electrical conductivity. It uses conductive materials dispersed in the slurry to build a conductive network to promote the migration of electrons. Conductive slurry is generally mainly composed of conductive materials, filled conductive additives, dispersion aids and solvents. Dispersion additives are used to evenly disperse the conductive material in the solvent to build a conductive network, and then filler conductive additives are added to fill the gaps in the conductive network and further improve the conductivity of the conductive slurry. Therefore, the conductivity, dispersion, stability and other properties of conductive paste directly affect its application in various fields.
MXene作为一种新兴的二维(2D)过渡金属碳化物/氮化物，自2011年以来便受到了各国研究者的广泛关注。在结构方面，MXene是由碳层和过渡金属层交替组成的类石墨烯结构的二维材料，具有较大的比表面积和优异的金属导电性。相比于传统的导电剂，比如，导电炭黑、碳纳米管、石墨烯等，MXene具有更高的导电率，所需用量也相对较低。更重要的是，MXene作为一种新型的导电材料，其大片层结构相互叠加构建的三维导电骨架能够促进电子的快速迁移。As an emerging two-dimensional (2D) transition metal carbide/nitride, MXene has attracted widespread attention from researchers from various countries since 2011. In terms of structure, MXene is a two-dimensional material with a graphene-like structure composed of alternating carbon layers and transition metal layers. It has a large specific surface area and excellent metal conductivity. Compared with traditional conductive agents, such as conductive carbon black, carbon nanotubes, graphene, etc., MXene has higher conductivity and requires a relatively low dosage. More importantly, as a new type of conductive material, MXene has a three-dimensional conductive skeleton built by superimposing large layers of structure that can promote the rapid migration of electrons.
然而，由于MXene的大片层结构和高比表面积，MXene片层与片层之间存在较强的范德华作用力，使得MXene纳米片发生不可逆的堆叠和团聚，难以均匀的分散到溶剂中，严重影响了MXene导电浆料的导电性、分散性等性能的发挥。此外，MXene片层表面暴露的末端金属原子极易被氧化，从而丧失MXene的本征属性。因此，如何开发一种高导电、高稳定、均匀分散的MXene导电浆料已成为当前亟待解决的技术难题。However, due to the large layer structure and high specific surface area of MXene, there are strong van der Waals forces between MXene sheets, causing irreversible stacking and agglomeration of MXene nanosheets, making it difficult to disperse evenly into the solvent, seriously affecting the It demonstrates the conductivity, dispersibility and other properties of MXene conductive paste. In addition, the exposed terminal metal atoms on the surface of the MXene sheet are easily oxidized, thereby losing the intrinsic properties of MXene. Therefore, how to develop a highly conductive, highly stable, and uniformly dispersed MXene conductive slurry has become an urgent technical problem that needs to be solved.
发明内容Contents of the invention
基于此，本发明提供了一种MXene基复合导电浆料及其制备方法和应用，以解决现有技术的MXene纳米片发生不可逆的堆叠和团聚，难以均匀的分散到溶剂中，从而严重影响MXene导电浆料的导电性、分散性等性能发挥的技术问题。
Based on this, the present invention provides an MXene-based composite conductive slurry and its preparation method and application to solve the problem of irreversible stacking and agglomeration of MXene nanosheets in the existing technology, which makes it difficult to evenly disperse into the solvent, thereby seriously affecting the MXene Technical issues related to the performance of conductive paste such as conductivity and dispersion.
为实现上述目的，本发明提供了一种MXene基复合导电浆料，其由以下重量百分比的原料复配制成：MXene导电基材料0.01-50％、填充导电添加剂0-50％、分散助剂0.5-10％和溶剂50-99.5％。In order to achieve the above purpose, the present invention provides an MXene-based composite conductive slurry, which is compounded from the following raw materials in weight percentages: MXene conductive base material 0.01-50%, filled conductive additive 0-50%, dispersion aid 0.5 -10% and solvent 50-99.5%.
作为本发明的进一步优选技术方案，所述MXene导电基材料为MXene粉体、MXene单片层纳米片、MXene多片层纳米片、碳纳米管@MXene复合材料、石墨烯@MXene复合材料、导电炭黑@MXene复合材料、生物质碳@MXene复合材料、高分子聚合物@MXene复合材料中的一种或多种。As a further preferred technical solution of the present invention, the MXene conductive base material is MXene powder, MXene single-layer nanosheets, MXene multi-layer nanosheets, carbon nanotube@MXene composite materials, graphene@MXene composite materials, conductive One or more of carbon black@MXene composite materials, biomass carbon@MXene composite materials, and polymer @MXene composite materials.
作为本发明的进一步优选技术方案，所述填充导电添加剂为碳材料、纳米金属粉、有机银中的一种或多种，其中，碳材料为导电石墨、导电炭黑、石墨烯或碳纳米管；所述纳米金属粉为银纳米金属、铜纳米金属、金纳米金属或铂纳米金属粉；有机银为硝酸银、醋酸银、草酸银或丁酸银。As a further preferred technical solution of the present invention, the filled conductive additive is one or more of carbon materials, nanometal powders, and organic silver, wherein the carbon material is conductive graphite, conductive carbon black, graphene or carbon nanotubes. ; The nanometal powder is silver nanometal, copper nanometal, gold nanometal or platinum nanometal powder; the organic silver is silver nitrate, silver acetate, silver oxalate or silver butyrate.
作为本发明的进一步优选技术方案，所述分散助剂为十八烷基硫酸钠、硬脂酸钠、二辛基琥珀酸磺酸钠、甘胆酸钠、油醇聚氧乙烯醚、烷基苯磺酸胺、十二烷基硫酸钠、十二烷基硫酸铵、十二烷基磷酸酯、仲烷基硫酸钠、α-烯基磺酸钠、十八烷基三甲基氯化铵、十六烷基三甲基氯化铵、十二烷基甜菜碱、十二烷基甲基氯化铵、聚乙烯醇、明胶、羟甲基纤维素、羟丙基纤维素、纤维素醚、聚偏氟乙烯、聚乙烯吡咯烷酮、聚乙二醇或羧甲基纤维素钠、碳纳米管溶液、壳聚糖水溶液、多巴胺溶液、油胺、聚乙二醇单甲醚、十六烷基三甲基溴化铵、十二烷基苯磺酸钠、聚偏氟乙烯、四氟乙烯-乙烯共聚物、聚四氟乙烯、聚全氟乙丙烯、聚三氟氯乙烯或聚氟乙烯中的一种或多种。As a further preferred technical solution of the present invention, the dispersion aids are sodium stearyl sulfate, sodium stearate, sodium dioctyl succinate sulfonate, sodium glycocholate, oleyl alcohol polyoxyethylene ether, alkyl Ammonium benzenesulfonate, sodium lauryl sulfate, ammonium lauryl sulfate, lauryl phosphate, sodium secondary alkyl sulfate, sodium alpha-alkenyl sulfonate, stearyltrimethylammonium chloride , cetyltrimethylammonium chloride, lauryl betaine, lauryl methyl ammonium chloride, polyvinyl alcohol, gelatin, hydroxymethylcellulose, hydroxypropylcellulose, cellulose ether , polyvinylidene fluoride, polyvinylpyrrolidone, polyethylene glycol or sodium carboxymethyl cellulose, carbon nanotube solution, chitosan aqueous solution, dopamine solution, oleylamine, polyethylene glycol monomethyl ether, cetyl Trimethylammonium bromide, sodium dodecyl benzene sulfonate, polyvinylidene fluoride, tetrafluoroethylene-ethylene copolymer, polytetrafluoroethylene, polyperfluoroethylene-propylene, polychlorotrifluoroethylene or polyvinyl fluoride of one or more.
作为本发明的进一步优选技术方案，所述溶剂为水、甲醇、乙醇、乙二醇、聚乙二醇、乙醚、苯、甲苯、苯乙烯、丙酮、乙腈、甲酰胺、二甲基亚砜、四氯化碳、N-甲基吡咯烷酮、N,N-二甲基甲酰胺、N,N-二甲基乙酰胺、环己烷中的一种或多种。As a further preferred technical solution of the present invention, the solvent is water, methanol, ethanol, ethylene glycol, polyethylene glycol, diethyl ether, benzene, toluene, styrene, acetone, acetonitrile, formamide, dimethyl sulfoxide, One or more of carbon tetrachloride, N-methylpyrrolidone, N,N-dimethylformamide, N,N-dimethylacetamide, and cyclohexane.
根据本发明的另一方面，本发明提还供了一种MXene基复合导电浆料的制备方法，包括以下步骤：According to another aspect of the invention, the invention also provides a preparation method of MXene-based composite conductive slurry, which includes the following steps:
1)将分散助剂添加到溶剂中，混合均匀，得到混合液；1) Add the dispersing aid to the solvent and mix evenly to obtain a mixed solution;
2)将MXene导电基材料和填充导电添加剂加入到步骤1)制备得到的混合液中，混合均匀，得到MXene基复合导电浆料。2) Add the MXene conductive base material and the filled conductive additive to the mixed solution prepared in step 1), and mix evenly to obtain an MXene-based composite conductive slurry.
作为本发明的进一步优选技术方案，步骤1)和步骤2)均采用搅拌、超声、振荡、湿磨或球磨的方式进行混合处理，步骤2)进行混合处理的时间为0.1～24h。As a further preferred technical solution of the present invention, both steps 1) and 2) are mixed by stirring, ultrasonic, oscillating, wet grinding or ball milling, and the mixing time of step 2) is 0.1 to 24 hours.
作为本发明的进一步优选技术方案，步骤1)和步骤2)中，按重量百分比计，各原料配比为：MXene导电基材料为0.01-50％、填充导电添加剂为0-50％、分散助剂为0.5-10％、
溶剂为50-99.5％，且通过改变原料配比，可实现对MXene导电基材料在溶剂中的分散性和稳定性，以及对产物MXene基复合导电浆料的电导率进行调控。As a further preferred technical solution of the present invention, in step 1) and step 2), in terms of weight percentage, the proportion of each raw material is: MXene conductive base material is 0.01-50%, filled conductive additive is 0-50%, dispersion aid The dosage is 0.5-10%, The solvent is 50-99.5%, and by changing the raw material ratio, the dispersion and stability of the MXene conductive-based material in the solvent can be achieved, as well as the conductivity of the product MXene-based composite conductive slurry can be controlled.
根据本发明的又一方面，本发明还提还供了一种MXene基复合导电浆料的应用，所述MXene基复合导电浆料作为导电添加剂应用于3D打印、印刷、触屏膜、显示器、透明导电膜、传感器、柔性电子产品、锂离子电池、钠离子电池或超级电容器。According to another aspect of the present invention, the present invention also provides an application of MXene-based composite conductive slurry, which is used as a conductive additive in 3D printing, printing, touch screen films, displays, Transparent conductive films, sensors, flexible electronics, lithium-ion batteries, sodium-ion batteries or supercapacitors.
本发明的MXene基复合导电浆料及其制备方法和应用，采用上述技术方案，可以达到如下有益效果：The MXene-based composite conductive slurry of the present invention and its preparation method and application can achieve the following beneficial effects by adopting the above technical solution:
1)本发明的MXene基复合导电浆料充分发挥了MXene导电性的优势，并进一步解决了MXene的分散性和储存稳定性的难题，而且，与传统的导电浆料相比，其在应用中所需用量也相对较低，从而有利于节省材料，即减少成本；1) The MXene-based composite conductive slurry of the present invention takes full advantage of the conductivity of MXene and further solves the problems of dispersion and storage stability of MXene. Moreover, compared with traditional conductive slurries, it has better performance in application The required amount is also relatively low, which is beneficial to saving materials, that is, reducing costs;
2)本发明的MXene基复合导电浆料可以作为导电添加剂广泛应用于3D打印、印刷、触屏膜、显示器、透明导电膜、传感器、柔性电子产品、锂离子电池、钠离子电池和超级电容器等领域中，可以在基体上构建稳固的导电网络，促进电子的快速迁移；2) The MXene-based composite conductive paste of the present invention can be widely used as a conductive additive in 3D printing, printing, touch screen films, displays, transparent conductive films, sensors, flexible electronic products, lithium-ion batteries, sodium-ion batteries, supercapacitors, etc. In the field, a stable conductive network can be built on the substrate to promote the rapid migration of electrons;
3)本发明的MXene基复合导电浆料的制备方法操作简便安全、条件温和、环境友好，可实现大规模生产。3) The preparation method of the MXene-based composite conductive slurry of the present invention is simple and safe to operate, has mild conditions, is environmentally friendly, and can achieve large-scale production.
下面结合附图和具体实施方式对本发明作进一步详细的说明。The present invention will be described in further detail below with reference to the accompanying drawings and specific embodiments.
图1为实施例一至五分别制备得到的MXene基复合导电浆料的稳定性测试结果图。Figure 1 is a diagram showing the stability test results of the MXene-based composite conductive slurries prepared in Examples 1 to 5 respectively.
本发明目的实现、功能特点及优点将结合实施例，参照附图做进一步说明。The realization of the purpose, functional features and advantages of the present invention will be further described with reference to the embodiments and the accompanying drawings.
下面将结合附图以及具体实施方式，对本发明做进一步描述。较佳实施例中所引用的如“上”、“下”、“左”、“右”、“中间”及“一”等用语，仅为便于叙述的明了，而非用以限定本发明可实施的范围，其相对关系的改变或调整，在无实质变更技术内容下，当亦视为本发明可实施的范畴。The present invention will be further described below in conjunction with the accompanying drawings and specific embodiments. Terms such as "upper", "lower", "left", "right", "middle" and "one" cited in the preferred embodiments are only used to facilitate the description and are not used to limit the scope of the present invention. Changes or adjustments in the scope of implementation and relative relationships shall also be regarded as the scope within which the present invention can be implemented, provided there is no substantial change in the technical content.
实施例一Embodiment 1
一种MXene基复合导电浆料及其制备方法，其制备方法包括以下步骤：An MXene-based composite conductive slurry and a preparation method thereof. The preparation method includes the following steps:
(1)在室温条件下，将100g羟甲基纤维素添加到500mL的去离子水中，以超声方式混合均匀，得到混合液；(1) At room temperature, add 100g of hydroxymethylcellulose to 500mL of deionized water, and mix evenly with ultrasonic to obtain a mixed solution;
(2)将10g刻蚀后的多层MXene纳米片和1g导电炭黑加入到步骤(1)制备得到的混合液中，采用超声方式进行处理24h，即得到水系的MXene基复合导电浆料。
(2) Add 10g of etched multi-layer MXene nanosheets and 1g of conductive carbon black to the mixed solution prepared in step (1), and treat it ultrasonically for 24 hours to obtain a water-based MXene-based composite conductive slurry.
实施例二Embodiment 2
一种MXene基复合导电浆料及其制备方法，其制备方法包括以下步骤：An MXene-based composite conductive slurry and a preparation method thereof. The preparation method includes the following steps:
(1)在室温条件下，将1g的聚乙二醇添加到19mL的去离子水中，以湿磨方式混合处理直至聚乙二醇完全溶解，得到混合液；(1) At room temperature, add 1 g of polyethylene glycol to 19 mL of deionized water, and mix with wet grinding until the polyethylene glycol is completely dissolved to obtain a mixed solution;
(2)将200mg刻蚀后的MXene粉体和500mg银纳米粉末加入到步骤(1)制备得到的混合液中，采用湿磨方式进行处理3h，得到MXene基复合导电浆料。(2) Add 200 mg of etched MXene powder and 500 mg of silver nanopowder to the mixed solution prepared in step (1), and perform wet grinding for 3 hours to obtain an MXene-based composite conductive slurry.
实施例三Embodiment 3
一种MXene基复合导电浆料及其制备方法，其制备方法包括以下步骤：An MXene-based composite conductive slurry and a preparation method thereof. The preparation method includes the following steps:
(1)在室温条件下，将由1g的聚乙烯醇溶液和0.5g羧甲基纤维素钠溶液的组成的复合分散助剂添加到2L的去离子水中，以搅拌方式混合均匀，得到混合液；(1) At room temperature, add a composite dispersion aid consisting of 1g of polyvinyl alcohol solution and 0.5g of sodium carboxymethylcellulose solution to 2L of deionized water, and mix evenly with stirring to obtain a mixed solution;
(2)将500mg MXene粉体材料和200mg硝酸银加入到步骤(1)制备得到的混合液中，采用搅拌的方式进行处理5h，得到MXene基复合导电浆料。(2) Add 500 mg of MXene powder material and 200 mg of silver nitrate to the mixed solution prepared in step (1), and stir for 5 hours to obtain an MXene-based composite conductive slurry.
实施例四Embodiment 4
一种MXene基复合导电浆料及其制备方法，其制备方法包括以下步骤：An MXene-based composite conductive slurry and a preparation method thereof. The preparation method includes the following steps:
(1)在室温条件下，将2g聚乙二醇单甲醚分散助剂添加到200mLN-甲基吡咯烷酮溶液中，以球磨的方式混合均匀，得到混合液。(1) At room temperature, add 2 g of polyethylene glycol monomethyl ether dispersion aid to 200 mL of N-methylpyrrolidone solution, and mix evenly by ball milling to obtain a mixed solution.
(2)将200mg的MXene粉体材料和500mg的石墨烯加入到步骤(1)制备得到的混合液中，采用球磨的方式进行处理14h，得到有MXene基复合导电浆料。(2) Add 200 mg of MXene powder material and 500 mg of graphene into the mixed liquid prepared in step (1), and process it by ball milling for 14 hours to obtain an MXene-based composite conductive slurry.
实施例五Embodiment 5
一种MXene基复合导电浆料及其制备方法，其制备方法包括以下步骤：An MXene-based composite conductive slurry and a preparation method thereof. The preparation method includes the following steps:
(1)在室温条件下，将1g聚四氟乙烯添加到19g的N-甲基吡咯烷酮溶液中，在50℃加热条件及搅拌下，搅拌1小时直至聚四氟乙烯完全溶解，得到混合液；(1) At room temperature, add 1g of polytetrafluoroethylene to 19g of N-methylpyrrolidone solution, stir for 1 hour under heating conditions and stirring at 50°C until the polytetrafluoroethylene is completely dissolved, and obtain a mixed solution;
(2)将100mg的MXene粉体材料和500mg的导电炭黑加入到步骤(1)制备得到的混合液中，采用搅拌的方式进行处理20h得到MXene基复合导电浆料。(2) Add 100 mg of MXene powder material and 500 mg of conductive carbon black to the mixed liquid prepared in step (1), and stir for 20 hours to obtain an MXene-based composite conductive slurry.
将实施例1至5制备得到的MXene基复合导电浆料进行性能检测，检测结果如下表1所示。The performance of the MXene-based composite conductive slurry prepared in Examples 1 to 5 was tested, and the test results are shown in Table 1 below.
表1.实施例一到五制备的MXene复合导电浆料的性能检测结果
Table 1. Performance test results of MXene composite conductive slurries prepared in Examples 1 to 5
Table 1. Performance test results of MXene composite conductive slurries prepared in Examples 1 to 5
从表1中可以看出，本发明中实施例一到五所制备的MXene复合导电浆料的PH为中性，以及呈现出优异的粘度和固含量，完全可以满足3D打印、印刷、触屏膜、显示器、透明导电膜、传感器、柔性电子产品、锂离子电池、钠离子电池和超级电容器等领域中对导电浆料的需求。As can be seen from Table 1, the MXene composite conductive slurry prepared in Examples 1 to 5 of the present invention has a neutral pH and exhibits excellent viscosity and solid content, which can fully satisfy the needs of 3D printing, printing, and touch screen films. , displays, transparent conductive films, sensors, flexible electronics, lithium-ion batteries, sodium-ion batteries and supercapacitors.
将实施例1至5制备得到的MXene基复合导电浆料进行电导率测试，结果如表2所示。The MXene-based composite conductive slurry prepared in Examples 1 to 5 was subjected to conductivity testing, and the results are shown in Table 2.
表2.实施例一到五制备的MXene复合导电浆料的电导率检测结果
Table 2. Conductivity detection results of the MXene composite conductive slurry prepared in Examples 1 to 5
Table 2. Conductivity detection results of the MXene composite conductive slurry prepared in Examples 1 to 5
从表2中可以看出，本发明中实施例一到五所制备的MXene复合导电浆料均表现出优异的导电性，完全可以满足3D打印、印刷、触屏膜、显示器、透明导电膜、传感器、柔性电子产品、锂离子电池、钠离子电池和超级电容器等领域中对导电浆料的需求。As can be seen from Table 2, the MXene composite conductive slurries prepared in Examples 1 to 5 of the present invention all exhibit excellent conductivity and can fully meet the needs of 3D printing, printing, touch screen films, displays, transparent conductive films, and sensors. , flexible electronic products, lithium-ion batteries, sodium-ion batteries and supercapacitors and other fields of demand for conductive paste.
将实施例一至五制备得到的MXene复合导电浆料进行固液分层测试，如图1所示，为静止一个月之后获取的图像，通过观察可知，静止一个月之后的MXene复合导电浆依然保持良好的分散性，均没有出现固液分层现象，表明其具有良好的分散性和较好的储存稳定性。The MXene composite conductive slurry prepared in Examples 1 to 5 was subjected to a solid-liquid delamination test. As shown in Figure 1, it is an image obtained after one month of rest. It can be seen from observation that the MXene composite conductive slurry after one month of rest still remains Good dispersion and no solid-liquid stratification phenomenon occurred, indicating that it has good dispersion and good storage stability.
上述实施例一至五为本发明合成MXene基复合导电浆料的较佳实例，可以理解为，各实施例中均为所选取材料的最佳配比。此外，从电导率性能上来看，实施例一为最佳，且各项性能均稳定、可靠，更适合在3D打印、印刷、触屏膜、显示器、透明导电膜、传感器、柔性电子产品、锂离子电池、钠离子电池和超级电容器等领域中的应用。The above-mentioned Embodiments 1 to 5 are preferred examples of the synthesis of MXene-based composite conductive slurries of the present invention. It can be understood that each embodiment is the optimal ratio of the selected materials. In addition, from the perspective of conductivity performance, Embodiment 1 is the best, and all performances are stable and reliable. It is more suitable for 3D printing, printing, touch screen films, displays, transparent conductive films, sensors, flexible electronic products, lithium Applications in ion batteries, sodium-ion batteries and supercapacitors.
虽然以上描述了本发明的具体实施方式，但是本领域熟练技术人员应当理解，这些仅是举例说明，可以对本实施方式做出多种变更或修改，而不背离本发明的原理和实质，本发明的保护范围仅由所附权利要求书限定。
Although the specific embodiments of the present invention have been described above, those skilled in the art should understand that these are only examples, and various changes or modifications can be made to the embodiments without departing from the principles and essence of the present invention. The scope of protection is limited only by the appended claims.
Claims (9)
- 一种MXene基复合导电浆料，其特征在于，由以下重量百分比的原料复配制成：MXene导电基材料0.01-50％、填充导电添加剂0-50％、分散助剂0.5-10％和溶剂50-99.5％。An MXene-based composite conductive slurry, characterized in that it is made of the following raw materials in weight percentage: 0.01-50% of MXene conductive base material, 0-50% of filled conductive additives, 0.5-10% of dispersion aids and 50% of solvent -99.5%.
- 根据权利要求1所述的MXene基复合导电浆料，其特征在于，所述MXene导电基材料为MXene粉体、MXene单片层纳米片、MXene多片层纳米片、碳纳米管@MXene复合材料、石墨烯@MXene复合材料、导电炭黑@MXene复合材料、生物质碳@MXene复合材料、高分子聚合物@MXene复合材料中的一种或多种。The MXene-based composite conductive slurry according to claim 1, wherein the MXene conductive base material is MXene powder, MXene single-layer nanosheet, MXene multi-layer nanosheet, carbon nanotube@MXene composite material , one or more of graphene@MXene composite materials, conductive carbon black@MXene composite materials, biomass carbon@MXene composite materials, and polymer @MXene composite materials.
- 根据权利要求1所述的MXene基复合导电浆料，其特征在于，所述填充导电添加剂为碳材料、纳米金属粉、有机银中的一种或多种，其中，碳材料为导电石墨、导电炭黑、石墨烯或碳纳米管；所述纳米金属粉为银纳米金属、铜纳米金属、金纳米金属或铂纳米金属粉；有机银为硝酸银、醋酸银、草酸银或丁酸银。The MXene-based composite conductive slurry according to claim 1, wherein the filled conductive additive is one or more of carbon materials, nanometal powders, and organic silver, wherein the carbon materials are conductive graphite, conductive graphite, and conductive silver. Carbon black, graphene or carbon nanotubes; the nanometal powder is silver nanometal, copper nanometal, gold nanometal or platinum nanometal powder; the organic silver is silver nitrate, silver acetate, silver oxalate or silver butyrate.
- 根据权利要求1所述的MXene基复合导电浆料，其特征在于，所述分散助剂为十八烷基硫酸钠、硬脂酸钠、二辛基琥珀酸磺酸钠、甘胆酸钠、油醇聚氧乙烯醚、烷基苯磺酸胺、十二烷基硫酸钠、十二烷基硫酸铵、十二烷基磷酸酯、仲烷基硫酸钠、α-烯基磺酸钠、十八烷基三甲基氯化铵、十六烷基三甲基氯化铵、十二烷基甜菜碱、十二烷基甲基氯化铵、聚乙烯醇、明胶、羟甲基纤维素、羟丙基纤维素、纤维素醚、聚偏氟乙烯、聚乙烯吡咯烷酮、聚乙二醇或羧甲基纤维素钠、碳纳米管溶液、壳聚糖水溶液、多巴胺溶液、油胺、聚乙二醇单甲醚、十六烷基三甲基溴化铵、十二烷基苯磺酸钠、聚偏氟乙烯、四氟乙烯-乙烯共聚物、聚四氟乙烯、聚全氟乙丙烯、聚三氟氯乙烯或聚氟乙烯中的一种或多种。The MXene-based composite conductive slurry according to claim 1, wherein the dispersion aid is sodium stearyl sulfate, sodium stearate, sodium dioctyl succinate sulfonate, sodium glycocholate, Oleyl alcohol polyoxyethylene ether, alkyl benzene sulfonamide, sodium lauryl sulfate, ammonium lauryl sulfate, lauryl phosphate, sodium secondary alkyl sulfate, sodium α-alkenyl sulfonate, ten Octyltrimethylammonium chloride, cetyltrimethylammonium chloride, lauryl betaine, laurylmethylammonium chloride, polyvinyl alcohol, gelatin, hydroxymethylcellulose, Hydroxypropylcellulose, cellulose ether, polyvinylidene fluoride, polyvinylpyrrolidone, polyethylene glycol or sodium carboxymethylcellulose, carbon nanotube solution, chitosan aqueous solution, dopamine solution, oleylamine, polyethylene glycol Alcohol monomethyl ether, cetyl trimethyl ammonium bromide, sodium dodecyl benzene sulfonate, polyvinylidene fluoride, tetrafluoroethylene-ethylene copolymer, polytetrafluoroethylene, polyperfluoroethylene-propylene, poly One or more of chlorotrifluoroethylene or polyfluoroethylene.
- 根据权利要求1所述的MXene基复合导电浆料，其特征在于，所述溶剂为水、甲醇、乙醇、乙二醇、聚乙二醇、乙醚、苯、甲苯、苯乙烯、丙酮、乙腈、甲酰胺、二甲基亚砜、四氯化碳、N-甲基吡咯烷酮、N,N-二甲基甲酰胺、N,N-二甲基乙酰胺、环己烷中的一种或多种。The MXene-based composite conductive slurry according to claim 1, wherein the solvent is water, methanol, ethanol, ethylene glycol, polyethylene glycol, ether, benzene, toluene, styrene, acetone, acetonitrile, One or more of formamide, dimethyl sulfoxide, carbon tetrachloride, N-methylpyrrolidone, N,N-dimethylformamide, N,N-dimethylacetamide, and cyclohexane .
- 一种权利要求1-5任一项所述的MXene基复合导电浆料的制备方法，其特征在于，包括以下步骤：A method for preparing the MXene-based composite conductive slurry according to any one of claims 1 to 5, characterized in that it includes the following steps:1)将分散助剂添加到溶剂中，混合均匀，得到混合液；1) Add the dispersing aid to the solvent and mix evenly to obtain a mixed solution;2)将MXene导电基材料和填充导电添加剂加入到步骤1)制备得到的混合液中，混合均匀，得到MXene基复合导电浆料。2) Add the MXene conductive base material and the filled conductive additive to the mixed solution prepared in step 1), and mix evenly to obtain an MXene-based composite conductive slurry.
- 根据权利要求6所述的MXene基复合导电浆料的制备方法，其特征在于，步骤1)和步骤2)均采用搅拌、超声、振荡、湿磨或球磨的方式进行混合处理，步骤2)进行混合处理的时间为0.1～24h。The method for preparing MXene-based composite conductive slurry according to claim 6, wherein step 1) and step 2) are mixed by stirring, ultrasonic, oscillating, wet grinding or ball milling, and step 2) is performed The time of mixing treatment is 0.1~24h.
- 根据权利要求6所述的MXene基复合导电浆料的制备方法，其特征在于，步骤1)和 步骤2)中，按重量百分比计，各原料配比为：MXene导电基材料为0.01-50％、填充导电添加剂为0-50％、分散助剂为0.5-10％、溶剂为50-99.5％，且通过改变原料配比，可实现对MXene导电基材料在溶剂中的分散性和稳定性，以及对产物MXene基复合导电浆料的电导率进行调控。The preparation method of MXene-based composite conductive slurry according to claim 6, characterized in that step 1) and In step 2), in terms of weight percentage, the proportion of each raw material is: MXene conductive base material is 0.01-50%, filled conductive additive is 0-50%, dispersing aid is 0.5-10%, and solvent is 50-99.5% , and by changing the raw material ratio, the dispersion and stability of the MXene conductive-based material in the solvent can be achieved, as well as the conductivity of the product MXene-based composite conductive slurry can be controlled.
- 一种权利要求1-5任一项所述的MXene基复合导电浆料的应用，其特征在于，所述MXene基复合导电浆料作为导电添加剂应用于3D打印、印刷、触屏膜、显示器、透明导电膜、传感器、柔性电子产品、锂离子电池、钠离子电池或超级电容器。 An application of the MXene-based composite conductive slurry according to any one of claims 1 to 5, characterized in that the MXene-based composite conductive slurry is used as a conductive additive in 3D printing, printing, touch screen films, displays, Transparent conductive films, sensors, flexible electronics, lithium-ion batteries, sodium-ion batteries or supercapacitors.
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| CN112992402A (en) * | 2021-04-16 | 2021-06-18 | 西安宏星电子浆料科技股份有限公司 | Silver and two-dimensional MXene mixed system conductor slurry for chip resistor and preparation method thereof |
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| CN113881286A (en) * | 2020-07-02 | 2022-01-04 | 中国科学院大连化学物理研究所 | Water-based MXene ink-jet printing conductive ink and preparation method and application thereof |
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