CN115477548A - 一种自支撑三维多孔碳泡沫的制备方法 - Google Patents
一种自支撑三维多孔碳泡沫的制备方法 Download PDFInfo
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- CN115477548A CN115477548A CN202211063595.6A CN202211063595A CN115477548A CN 115477548 A CN115477548 A CN 115477548A CN 202211063595 A CN202211063595 A CN 202211063595A CN 115477548 A CN115477548 A CN 115477548A
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- porous carbon
- ammonium
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- VNWKTOKETHGBQD-UHFFFAOYSA-N methane Chemical compound C VNWKTOKETHGBQD-UHFFFAOYSA-N 0.000 title claims abstract description 33
- 238000002360 preparation method Methods 0.000 title claims abstract description 14
- 238000005245 sintering Methods 0.000 claims abstract description 43
- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical compound [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 claims abstract description 37
- 229910052799 carbon Inorganic materials 0.000 claims abstract description 27
- 238000000034 method Methods 0.000 claims abstract description 27
- 238000007731 hot pressing Methods 0.000 claims abstract description 24
- 238000006243 chemical reaction Methods 0.000 claims abstract description 16
- 150000003839 salts Chemical class 0.000 claims abstract description 10
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Chemical compound O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims description 21
- 239000011259 mixed solution Substances 0.000 claims description 19
- 239000003575 carbonaceous material Substances 0.000 claims description 18
- KRKNYBCHXYNGOX-UHFFFAOYSA-N citric acid Chemical compound OC(=O)CC(O)(C(O)=O)CC(O)=O KRKNYBCHXYNGOX-UHFFFAOYSA-N 0.000 claims description 15
- 235000002639 sodium chloride Nutrition 0.000 claims description 15
- FAPWRFPIFSIZLT-UHFFFAOYSA-M Sodium chloride Chemical compound [Na+].[Cl-] FAPWRFPIFSIZLT-UHFFFAOYSA-M 0.000 claims description 14
- 239000008367 deionised water Substances 0.000 claims description 14
- 229910021641 deionized water Inorganic materials 0.000 claims description 14
- 229910017053 inorganic salt Inorganic materials 0.000 claims description 14
- WCUXLLCKKVVCTQ-UHFFFAOYSA-M Potassium chloride Chemical compound [Cl-].[K+] WCUXLLCKKVVCTQ-UHFFFAOYSA-M 0.000 claims description 13
- IJGRMHOSHXDMSA-UHFFFAOYSA-N Atomic nitrogen Chemical compound N#N IJGRMHOSHXDMSA-UHFFFAOYSA-N 0.000 claims description 12
- 239000000243 solution Substances 0.000 claims description 12
- XSQUKJJJFZCRTK-UHFFFAOYSA-N Urea Chemical compound NC(N)=O XSQUKJJJFZCRTK-UHFFFAOYSA-N 0.000 claims description 11
- 238000001035 drying Methods 0.000 claims description 11
- 239000000843 powder Substances 0.000 claims description 11
- 230000008569 process Effects 0.000 claims description 10
- UMGDCJDMYOKAJW-UHFFFAOYSA-N thiourea Chemical compound NC(N)=S UMGDCJDMYOKAJW-UHFFFAOYSA-N 0.000 claims description 10
- MUBZPKHOEPUJKR-UHFFFAOYSA-N Oxalic acid Chemical compound OC(=O)C(O)=O MUBZPKHOEPUJKR-UHFFFAOYSA-N 0.000 claims description 9
- 238000005520 cutting process Methods 0.000 claims description 9
- 238000004146 energy storage Methods 0.000 claims description 8
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 claims description 7
- PMZURENOXWZQFD-UHFFFAOYSA-L Sodium Sulfate Chemical compound [Na+].[Na+].[O-]S([O-])(=O)=O PMZURENOXWZQFD-UHFFFAOYSA-L 0.000 claims description 7
- 239000010439 graphite Substances 0.000 claims description 7
- 229910002804 graphite Inorganic materials 0.000 claims description 7
- 238000002791 soaking Methods 0.000 claims description 7
- 239000011780 sodium chloride Substances 0.000 claims description 7
- 229910052938 sodium sulfate Inorganic materials 0.000 claims description 7
- 235000011152 sodium sulphate Nutrition 0.000 claims description 7
- ATRRKUHOCOJYRX-UHFFFAOYSA-N Ammonium bicarbonate Chemical compound [NH4+].OC([O-])=O ATRRKUHOCOJYRX-UHFFFAOYSA-N 0.000 claims description 6
- OAICVXFJPJFONN-UHFFFAOYSA-N Phosphorus Chemical compound [P] OAICVXFJPJFONN-UHFFFAOYSA-N 0.000 claims description 6
- BUGBHKTXTAQXES-UHFFFAOYSA-N Selenium Chemical compound [Se] BUGBHKTXTAQXES-UHFFFAOYSA-N 0.000 claims description 6
- CDBYLPFSWZWCQE-UHFFFAOYSA-L Sodium Carbonate Chemical compound [Na+].[Na+].[O-]C([O-])=O CDBYLPFSWZWCQE-UHFFFAOYSA-L 0.000 claims description 6
- 239000004115 Sodium Silicate Substances 0.000 claims description 6
- NINIDFKCEFEMDL-UHFFFAOYSA-N Sulfur Chemical compound [S] NINIDFKCEFEMDL-UHFFFAOYSA-N 0.000 claims description 6
- 239000001099 ammonium carbonate Substances 0.000 claims description 6
- 125000004429 atom Chemical group 0.000 claims description 6
- 125000004432 carbon atom Chemical group C* 0.000 claims description 6
- 229910052757 nitrogen Inorganic materials 0.000 claims description 6
- 229910052698 phosphorus Inorganic materials 0.000 claims description 6
- 239000011574 phosphorus Substances 0.000 claims description 6
- BWHMMNNQKKPAPP-UHFFFAOYSA-L potassium carbonate Chemical compound [K+].[K+].[O-]C([O-])=O BWHMMNNQKKPAPP-UHFFFAOYSA-L 0.000 claims description 6
- 239000001103 potassium chloride Substances 0.000 claims description 6
- 235000011164 potassium chloride Nutrition 0.000 claims description 6
- 229910052711 selenium Inorganic materials 0.000 claims description 6
- 239000011669 selenium Substances 0.000 claims description 6
- JPJALAQPGMAKDF-UHFFFAOYSA-N selenium dioxide Chemical compound O=[Se]=O JPJALAQPGMAKDF-UHFFFAOYSA-N 0.000 claims description 6
- NTHWMYGWWRZVTN-UHFFFAOYSA-N sodium silicate Chemical compound [Na+].[Na+].[O-][Si]([O-])=O NTHWMYGWWRZVTN-UHFFFAOYSA-N 0.000 claims description 6
- 229910052911 sodium silicate Inorganic materials 0.000 claims description 6
- 229910052979 sodium sulfide Inorganic materials 0.000 claims description 6
- GRVFOGOEDUUMBP-UHFFFAOYSA-N sodium sulfide (anhydrous) Chemical compound [Na+].[Na+].[S-2] GRVFOGOEDUUMBP-UHFFFAOYSA-N 0.000 claims description 6
- 229910052717 sulfur Inorganic materials 0.000 claims description 6
- 239000011593 sulfur Substances 0.000 claims description 6
- YWYZEGXAUVWDED-UHFFFAOYSA-N triammonium citrate Chemical compound [NH4+].[NH4+].[NH4+].[O-]C(=O)CC(O)(CC([O-])=O)C([O-])=O YWYZEGXAUVWDED-UHFFFAOYSA-N 0.000 claims description 6
- WQZGKKKJIJFFOK-GASJEMHNSA-N Glucose Natural products OC[C@H]1OC(O)[C@H](O)[C@@H](O)[C@@H]1O WQZGKKKJIJFFOK-GASJEMHNSA-N 0.000 claims description 5
- UYJXRRSPUVSSMN-UHFFFAOYSA-P ammonium sulfide Chemical compound [NH4+].[NH4+].[S-2] UYJXRRSPUVSSMN-UHFFFAOYSA-P 0.000 claims description 5
- 238000004108 freeze drying Methods 0.000 claims description 5
- 239000008103 glucose Substances 0.000 claims description 5
- 239000005720 sucrose Substances 0.000 claims description 5
- 229930006000 Sucrose Natural products 0.000 claims description 4
- CZMRCDWAGMRECN-UGDNZRGBSA-N Sucrose Chemical compound O[C@H]1[C@H](O)[C@@H](CO)O[C@@]1(CO)O[C@@H]1[C@H](O)[C@@H](O)[C@H](O)[C@@H](CO)O1 CZMRCDWAGMRECN-UGDNZRGBSA-N 0.000 claims description 4
- HIVLDXAAFGCOFU-UHFFFAOYSA-N ammonium hydrosulfide Chemical compound [NH4+].[SH-] HIVLDXAAFGCOFU-UHFFFAOYSA-N 0.000 claims description 4
- 238000001816 cooling Methods 0.000 claims description 4
- 239000011812 mixed powder Substances 0.000 claims description 4
- 239000007787 solid Substances 0.000 claims description 4
- 238000001694 spray drying Methods 0.000 claims description 4
- 239000000126 substance Substances 0.000 claims description 4
- BJEPYKJPYRNKOW-REOHCLBHSA-N (S)-malic acid Chemical compound OC(=O)[C@@H](O)CC(O)=O BJEPYKJPYRNKOW-REOHCLBHSA-N 0.000 claims description 3
- OWEGMIWEEQEYGQ-UHFFFAOYSA-N 100676-05-9 Natural products OC1C(O)C(O)C(CO)OC1OCC1C(O)C(O)C(O)C(OC2C(OC(O)C(O)C2O)CO)O1 OWEGMIWEEQEYGQ-UHFFFAOYSA-N 0.000 claims description 3
- GUBGYTABKSRVRQ-XLOQQCSPSA-N Alpha-Lactose Chemical compound O[C@@H]1[C@@H](O)[C@@H](O)[C@@H](CO)O[C@H]1O[C@@H]1[C@@H](CO)O[C@H](O)[C@H](O)[C@H]1O GUBGYTABKSRVRQ-XLOQQCSPSA-N 0.000 claims description 3
- USFZMSVCRYTOJT-UHFFFAOYSA-N Ammonium acetate Chemical compound N.CC(O)=O USFZMSVCRYTOJT-UHFFFAOYSA-N 0.000 claims description 3
- 239000005695 Ammonium acetate Substances 0.000 claims description 3
- 229910000013 Ammonium bicarbonate Inorganic materials 0.000 claims description 3
- FEWJPZIEWOKRBE-JCYAYHJZSA-N Dextrotartaric acid Chemical compound OC(=O)[C@H](O)[C@@H](O)C(O)=O FEWJPZIEWOKRBE-JCYAYHJZSA-N 0.000 claims description 3
- 229930091371 Fructose Natural products 0.000 claims description 3
- 239000005715 Fructose Substances 0.000 claims description 3
- RFSUNEUAIZKAJO-ARQDHWQXSA-N Fructose Chemical compound OC[C@H]1O[C@](O)(CO)[C@@H](O)[C@@H]1O RFSUNEUAIZKAJO-ARQDHWQXSA-N 0.000 claims description 3
- 108010010803 Gelatin Proteins 0.000 claims description 3
- GUBGYTABKSRVRQ-QKKXKWKRSA-N Lactose Natural products OC[C@H]1O[C@@H](O[C@H]2[C@H](O)[C@@H](O)C(O)O[C@@H]2CO)[C@H](O)[C@@H](O)[C@H]1O GUBGYTABKSRVRQ-QKKXKWKRSA-N 0.000 claims description 3
- GUBGYTABKSRVRQ-PICCSMPSSA-N Maltose Natural products O[C@@H]1[C@@H](O)[C@H](O)[C@@H](CO)O[C@@H]1O[C@@H]1[C@@H](CO)OC(O)[C@H](O)[C@H]1O GUBGYTABKSRVRQ-PICCSMPSSA-N 0.000 claims description 3
- 229910019142 PO4 Inorganic materials 0.000 claims description 3
- 239000004111 Potassium silicate Substances 0.000 claims description 3
- FEWJPZIEWOKRBE-UHFFFAOYSA-N Tartaric acid Natural products [H+].[H+].[O-]C(=O)C(O)C(O)C([O-])=O FEWJPZIEWOKRBE-UHFFFAOYSA-N 0.000 claims description 3
- BJEPYKJPYRNKOW-UHFFFAOYSA-N alpha-hydroxysuccinic acid Natural products OC(=O)C(O)CC(O)=O BJEPYKJPYRNKOW-UHFFFAOYSA-N 0.000 claims description 3
- 229940043376 ammonium acetate Drugs 0.000 claims description 3
- 235000019257 ammonium acetate Nutrition 0.000 claims description 3
- 235000012538 ammonium bicarbonate Nutrition 0.000 claims description 3
- BIGPRXCJEDHCLP-UHFFFAOYSA-N ammonium bisulfate Chemical compound [NH4+].OS([O-])(=O)=O BIGPRXCJEDHCLP-UHFFFAOYSA-N 0.000 claims description 3
- 235000012501 ammonium carbonate Nutrition 0.000 claims description 3
- VBIXEXWLHSRNKB-UHFFFAOYSA-N ammonium oxalate Chemical compound [NH4+].[NH4+].[O-]C(=O)C([O-])=O VBIXEXWLHSRNKB-UHFFFAOYSA-N 0.000 claims description 3
- BFNBIHQBYMNNAN-UHFFFAOYSA-N ammonium sulfate Chemical compound N.N.OS(O)(=O)=O BFNBIHQBYMNNAN-UHFFFAOYSA-N 0.000 claims description 3
- 229910052921 ammonium sulfate Inorganic materials 0.000 claims description 3
- 235000011130 ammonium sulphate Nutrition 0.000 claims description 3
- WQZGKKKJIJFFOK-VFUOTHLCSA-N beta-D-glucose Chemical compound OC[C@H]1O[C@@H](O)[C@H](O)[C@@H](O)[C@@H]1O WQZGKKKJIJFFOK-VFUOTHLCSA-N 0.000 claims description 3
- GUBGYTABKSRVRQ-QUYVBRFLSA-N beta-maltose Chemical compound OC[C@H]1O[C@H](O[C@H]2[C@H](O)[C@@H](O)[C@H](O)O[C@@H]2CO)[C@H](O)[C@@H](O)[C@@H]1O GUBGYTABKSRVRQ-QUYVBRFLSA-N 0.000 claims description 3
- 239000004202 carbamide Substances 0.000 claims description 3
- 235000013877 carbamide Nutrition 0.000 claims description 3
- 239000003795 chemical substances by application Substances 0.000 claims description 3
- 238000011049 filling Methods 0.000 claims description 3
- 239000008273 gelatin Substances 0.000 claims description 3
- 229920000159 gelatin Polymers 0.000 claims description 3
- 235000019322 gelatine Nutrition 0.000 claims description 3
- 235000011852 gelatine desserts Nutrition 0.000 claims description 3
- 238000010438 heat treatment Methods 0.000 claims description 3
- 239000008101 lactose Substances 0.000 claims description 3
- 239000001630 malic acid Substances 0.000 claims description 3
- 235000011090 malic acid Nutrition 0.000 claims description 3
- 239000005416 organic matter Substances 0.000 claims description 3
- 235000006408 oxalic acid Nutrition 0.000 claims description 3
- 239000010452 phosphate Substances 0.000 claims description 3
- NBIIXXVUZAFLBC-UHFFFAOYSA-K phosphate Chemical compound [O-]P([O-])([O-])=O NBIIXXVUZAFLBC-UHFFFAOYSA-K 0.000 claims description 3
- ACVYVLVWPXVTIT-UHFFFAOYSA-M phosphinate Chemical compound [O-][PH2]=O ACVYVLVWPXVTIT-UHFFFAOYSA-M 0.000 claims description 3
- 229910000027 potassium carbonate Inorganic materials 0.000 claims description 3
- 235000011181 potassium carbonates Nutrition 0.000 claims description 3
- NNHHDJVEYQHLHG-UHFFFAOYSA-N potassium silicate Chemical compound [K+].[K+].[O-][Si]([O-])=O NNHHDJVEYQHLHG-UHFFFAOYSA-N 0.000 claims description 3
- 229910052913 potassium silicate Inorganic materials 0.000 claims description 3
- 235000019353 potassium silicate Nutrition 0.000 claims description 3
- OTYBMLCTZGSZBG-UHFFFAOYSA-L potassium sulfate Chemical compound [K+].[K+].[O-]S([O-])(=O)=O OTYBMLCTZGSZBG-UHFFFAOYSA-L 0.000 claims description 3
- 229910052939 potassium sulfate Inorganic materials 0.000 claims description 3
- DPLVEEXVKBWGHE-UHFFFAOYSA-N potassium sulfide Chemical compound [S-2].[K+].[K+] DPLVEEXVKBWGHE-UHFFFAOYSA-N 0.000 claims description 3
- 235000011151 potassium sulphates Nutrition 0.000 claims description 3
- 229910000029 sodium carbonate Inorganic materials 0.000 claims description 3
- 235000017550 sodium carbonate Nutrition 0.000 claims description 3
- RBRLCUAPGJEAOP-UHFFFAOYSA-M sodium selanide Chemical compound [Na+].[SeH-] RBRLCUAPGJEAOP-UHFFFAOYSA-M 0.000 claims description 3
- 235000019794 sodium silicate Nutrition 0.000 claims description 3
- AKHNMLFCWUSKQB-UHFFFAOYSA-L sodium thiosulfate Chemical compound [Na+].[Na+].[O-]S([O-])(=O)=S AKHNMLFCWUSKQB-UHFFFAOYSA-L 0.000 claims description 3
- 235000019345 sodium thiosulphate Nutrition 0.000 claims description 3
- 239000011975 tartaric acid Substances 0.000 claims description 3
- 235000002906 tartaric acid Nutrition 0.000 claims description 3
- NJRXVEJTAYWCQJ-UHFFFAOYSA-N thiomalic acid Chemical compound OC(=O)CC(S)C(O)=O NJRXVEJTAYWCQJ-UHFFFAOYSA-N 0.000 claims description 3
- 230000001105 regulatory effect Effects 0.000 abstract description 7
- 238000003860 storage Methods 0.000 abstract description 5
- 239000007772 electrode material Substances 0.000 abstract description 3
- 239000002245 particle Substances 0.000 abstract description 3
- 238000003756 stirring Methods 0.000 description 5
- 238000004140 cleaning Methods 0.000 description 4
- 239000002131 composite material Substances 0.000 description 4
- 238000005303 weighing Methods 0.000 description 4
- 239000011230 binding agent Substances 0.000 description 3
- 238000009792 diffusion process Methods 0.000 description 3
- 230000000694 effects Effects 0.000 description 3
- 239000003792 electrolyte Substances 0.000 description 3
- 238000001953 recrystallisation Methods 0.000 description 3
- CURLTUGMZLYLDI-UHFFFAOYSA-N Carbon dioxide Chemical compound O=C=O CURLTUGMZLYLDI-UHFFFAOYSA-N 0.000 description 2
- FKNQFGJONOIPTF-UHFFFAOYSA-N Sodium cation Chemical compound [Na+] FKNQFGJONOIPTF-UHFFFAOYSA-N 0.000 description 2
- 239000011149 active material Substances 0.000 description 2
- 239000002482 conductive additive Substances 0.000 description 2
- 238000003487 electrochemical reaction Methods 0.000 description 2
- 238000007710 freezing Methods 0.000 description 2
- 230000008014 freezing Effects 0.000 description 2
- -1 glucose-ammonium sulfide Chemical compound 0.000 description 2
- 238000011065 in-situ storage Methods 0.000 description 2
- 150000002500 ions Chemical class 0.000 description 2
- 230000004048 modification Effects 0.000 description 2
- 238000012986 modification Methods 0.000 description 2
- 239000002135 nanosheet Substances 0.000 description 2
- 238000001878 scanning electron micrograph Methods 0.000 description 2
- 229910001415 sodium ion Inorganic materials 0.000 description 2
- CSCBOLSODHVJSE-UHFFFAOYSA-N C(CC(O)(C(=O)O)CC(=O)O)(=O)O.NC(=S)N Chemical compound C(CC(O)(C(=O)O)CC(=O)O)(=O)O.NC(=S)N CSCBOLSODHVJSE-UHFFFAOYSA-N 0.000 description 1
- 241000282414 Homo sapiens Species 0.000 description 1
- 238000003917 TEM image Methods 0.000 description 1
- 239000013543 active substance Substances 0.000 description 1
- 229910001413 alkali metal ion Inorganic materials 0.000 description 1
- 230000004075 alteration Effects 0.000 description 1
- 230000009286 beneficial effect Effects 0.000 description 1
- 230000005540 biological transmission Effects 0.000 description 1
- 239000003990 capacitor Substances 0.000 description 1
- 239000001569 carbon dioxide Substances 0.000 description 1
- 229910002092 carbon dioxide Inorganic materials 0.000 description 1
- 239000012876 carrier material Substances 0.000 description 1
- 230000008859 change Effects 0.000 description 1
- 239000011248 coating agent Substances 0.000 description 1
- 238000000576 coating method Methods 0.000 description 1
- 239000006258 conductive agent Substances 0.000 description 1
- 230000001351 cycling effect Effects 0.000 description 1
- 230000007547 defect Effects 0.000 description 1
- 238000005516 engineering process Methods 0.000 description 1
- 230000007613 environmental effect Effects 0.000 description 1
- 229910052739 hydrogen Inorganic materials 0.000 description 1
- 239000001257 hydrogen Substances 0.000 description 1
- 238000011068 loading method Methods 0.000 description 1
- 238000004519 manufacturing process Methods 0.000 description 1
- 239000000463 material Substances 0.000 description 1
- 239000011159 matrix material Substances 0.000 description 1
- 238000002156 mixing Methods 0.000 description 1
- 238000006386 neutralization reaction Methods 0.000 description 1
- 239000011148 porous material Substances 0.000 description 1
- 238000006467 substitution reaction Methods 0.000 description 1
- 230000004083 survival effect Effects 0.000 description 1
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- C04B38/00—Porous mortars, concrete, artificial stone or ceramic ware; Preparation thereof
- C04B38/04—Porous mortars, concrete, artificial stone or ceramic ware; Preparation thereof by dissolving-out added substances
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- C04B35/00—Shaped ceramic products characterised by their composition; Ceramics compositions; Processing powders of inorganic compounds preparatory to the manufacturing of ceramic products
- C04B35/515—Shaped ceramic products characterised by their composition; Ceramics compositions; Processing powders of inorganic compounds preparatory to the manufacturing of ceramic products based on non-oxide ceramics
- C04B35/52—Shaped ceramic products characterised by their composition; Ceramics compositions; Processing powders of inorganic compounds preparatory to the manufacturing of ceramic products based on non-oxide ceramics based on carbon, e.g. graphite
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- C04B35/00—Shaped ceramic products characterised by their composition; Ceramics compositions; Processing powders of inorganic compounds preparatory to the manufacturing of ceramic products
- C04B35/622—Forming processes; Processing powders of inorganic compounds preparatory to the manufacturing of ceramic products
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- C—CHEMISTRY; METALLURGY
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- C04B35/00—Shaped ceramic products characterised by their composition; Ceramics compositions; Processing powders of inorganic compounds preparatory to the manufacturing of ceramic products
- C04B35/622—Forming processes; Processing powders of inorganic compounds preparatory to the manufacturing of ceramic products
- C04B35/64—Burning or sintering processes
- C04B35/645—Pressure sintering
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- H—ELECTRICITY
- H01—ELECTRIC ELEMENTS
- H01G—CAPACITORS; CAPACITORS, RECTIFIERS, DETECTORS, SWITCHING DEVICES, LIGHT-SENSITIVE OR TEMPERATURE-SENSITIVE DEVICES OF THE ELECTROLYTIC TYPE
- H01G11/00—Hybrid capacitors, i.e. capacitors having different positive and negative electrodes; Electric double-layer [EDL] capacitors; Processes for the manufacture thereof or of parts thereof
- H01G11/22—Electrodes
- H01G11/30—Electrodes characterised by their material
- H01G11/32—Carbon-based
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- H—ELECTRICITY
- H01—ELECTRIC ELEMENTS
- H01G—CAPACITORS; CAPACITORS, RECTIFIERS, DETECTORS, SWITCHING DEVICES, LIGHT-SENSITIVE OR TEMPERATURE-SENSITIVE DEVICES OF THE ELECTROLYTIC TYPE
- H01G11/00—Hybrid capacitors, i.e. capacitors having different positive and negative electrodes; Electric double-layer [EDL] capacitors; Processes for the manufacture thereof or of parts thereof
- H01G11/22—Electrodes
- H01G11/30—Electrodes characterised by their material
- H01G11/32—Carbon-based
- H01G11/36—Nanostructures, e.g. nanofibres, nanotubes or fullerenes
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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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- C04B2235/00—Aspects relating to ceramic starting mixtures or sintered ceramic products
- C04B2235/65—Aspects relating to heat treatments of ceramic bodies such as green ceramics or pre-sintered ceramics, e.g. burning, sintering or melting processes
- C04B2235/656—Aspects relating to heat treatments of ceramic bodies such as green ceramics or pre-sintered ceramics, e.g. burning, sintering or melting processes characterised by specific heating conditions during heat treatment
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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
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- Organic Chemistry (AREA)
- Microelectronics & Electronic Packaging (AREA)
- Inorganic Chemistry (AREA)
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Abstract
本发明属于电化学能源转换与存储电极材料的技术领域,具体涉及一种自支撑三维多孔碳泡沫的制备方法,采用水溶性无机盐作为模板,通过一步热压烧结法制备出一种尺寸可调、易裁切的自支撑三维多孔碳泡沫。本发明所使用的盐模板成本较低,使用不同种类的盐作为模板,可调控模板的粒径大小并最终对三维多孔碳的孔径进行可控调节,另外,水溶性盐模板通过水洗就能去除,可回收再利用。本发明所采用的热压烧结法可以在高温烧结的同时对样品施加压力,在压力、高温和模板的三重作用下,碳源碳化并相互连接,形成具有良好力学性能的自支撑三维多孔碳结构。
Description
技术领域
本发明属于电化学能源转换与存储电极材料的技术领域,具体涉及一种自支撑三维多孔碳泡沫的制备方法。
背景技术
由于经济的发展和人口的增加,二氧化碳的过度排放导致地球气候和环境急剧变化,能源危机与环境问题严重威胁人类的生存和发展,因此,迫切需要实现碳中和的发展模式。为了实现这一目标,电化学能源转换和存储技术起着重要的作用。碳材料因比表面积大、电导率高、稳定性好等优点,无论是直接作为电极活性材料,还是作为其他电化学活性材料的载体材料,在双电层电容、碱金属离子电池负极,以及电催化等领域具有重要的应用前景。
在众多碳材料结构中,自支撑三维分级多孔碳泡沫具有连续的导电网络、连通的孔网络结构和良好的机械性能,可以在材料和电极尺度同时促进电解液的扩散、暴露活性位点、加快电子的传输和缓冲工作中的体积变化,被当作理想的电化学转换和储能器件的电极或骨架。碳材料的本征活性还能通过元素掺杂方式进行进一步的调控。
现有粉末电极中,集流体、粘结剂以及导电剂等非化学活性物质的引入,混料、涂膜、干燥等耗时。
发明内容
本发明的目的在于:针对现有技术的不足,提供一种自支撑三维多孔碳泡沫的制备方法,能够制备自支撑三维多孔碳泡沫,有助于降低生产成本。
为了实现上述目的,本发明采用如下技术方案:
一种自支撑三维多孔碳泡沫的制备方法,包括:
步骤一、将作为碳源的水溶性固体有机物和作为模板的水溶性无机盐溶于去离子水中,按照混水溶液中碳原子与盐的摩尔比为1:1-8配制成总浓度为0.5-5mol/L的混合溶液;
步骤二、对混合溶液进行再结晶,得到碳源均匀包覆无机盐的混合粉末;
步骤三、将预设量粉末装填于热压烧结石墨模具中,将模具放入热压烧结炉内,在真空条件下,600-1000℃热压烧结1-3h,烧结过程中,对样品施加10-40MPa的压力,反应结束后,冷却到室温,得到块体;
步骤四、用酒精清除块体中的脱模剂,再用去离子水反复浸泡去除其中的水溶性无机盐模板,烘干后得到自支撑三维多孔碳泡沫;
步骤五、将自支撑三维多孔碳泡沫切割成所需大小的尺寸,用作电化学转换与储能电极。
优选的,所述步骤一中,还包括:
在溶液中加入预设量可溶性氮源、磷源、硫源、或硒源对碳材料形成掺杂的物质,从而在热压烧结过程中形成异质原子掺杂,按照混水溶液中掺杂原子与碳原子的摩尔比为1:10-15配置溶液。
优选的,所述步骤二中,所述碳源为柠檬酸、柠檬酸铵、葡糖糖、蔗糖、乳糖、果糖、明胶、麦芽糖、苹果酸、酒石酸、草酸、草酸铵、乙酸铵中的一种或多种。
优选的,所述步骤一中,作为模板的水溶性无机盐为氯化钠、氯化钾、硫酸钠、硫酸钾、硅酸钠、硅酸钾、碳酸钠、碳酸钾中的一种或多种。
优选的,所述氮源为尿素、碳酸氢铵、碳酸铵、硫酸铵、硫酸氢铵中的一种或多种;所述磷源为水溶性磷酸二氢盐、水溶性次亚磷酸盐中的一种或多种;所述硫源为硫化钠、硫化钾、硫脲、硫代硫酸钠、硫代苹果酸、硫化铵、硫化氢铵中的一种或多种;所述硒源为硒氢化钠、二氧化硒中的一种或多种。
优选的,所述步骤二中,对混合溶液进行再结晶,包括加热干燥、冷冻干燥、喷雾干燥中的一种。
本发明的有益效果在于,本发明采用水溶性无机盐作为模板,通过一步热压烧结法制备出一种尺寸可调、易裁切的自支撑三维多孔碳泡沫。本发明所使用的盐模板成本较低,使用不同种类的盐作为模板或者采用不同的再结晶方法,可轻松调控模板的粒径大小并最终对三维多孔碳的孔径进行可控调节,另外,水溶性盐模板通过水洗就能去除,易回收再利用。本发明所采用的热压烧结法可以在高温烧结的同时对样品施加压力,在压力、高温和模板的三重作用下,碳源碳化并相互连接,一步形成具有良好力学性能的自支撑三维多孔碳结构。本发明制备的自支撑三维多孔碳泡沫可裁切,并直接用作电化学能源转换与存储电极或骨架,具有良好的电化学反应动力学,自支撑三维多孔碳材料作为电极使用时由于内部碳纳米片相互连接而形成三维导电网络,提高电极的导电性;自支撑三维多孔碳作为电极时省去了集流体、粘结剂以及导电添加剂,降低了电化学体系的成本;原位形成的自支撑结构具有的良好力学性能以及分级多孔结构,促进了离子和电解液扩散并增强了电极结构的稳定性。
附图说明
下面将参考附图来描述本发明示例性实施方式的特征、优点和技术效果。
图1为本发明的实施例1制备的自支撑三维多孔碳的示意图。
图2为本发明的实施例1制备的自支撑三维多孔碳的SEM图之一。
图3为本发明的实施例1制备的自支撑三维多孔碳的SEM图之二。
图4为本发明的实施例1制备的自支撑三维多孔碳的TEM图。
图5为本发明的实施例1制备的自支撑三维多孔碳作为钠离子电池负极的循环性能图。
图6为本发明的实施例1制备的自支撑三维多孔碳作为钠离子电池负极的倍率性能图。
具体实施方式
如在说明书及权利要求当中使用了某些词汇来指称特定组件。本领域技术人员应可理解,硬件制造商可能会用不同名词来称呼同一个组件。本说明书及权利要求并不以名称的差异来作为区分组件的方式,而是以组件在功能上的差异来作为区分的准则。如在通篇说明书及权利要求当中所提及的“包含”为一开放式用语,故应解释成“包含但不限定于”。“大致”是指在可接受的误差范围内,本领域技术人员能够在一定误差范围内解决技术问题,基本达到技术效果。
此外,术语“第一”、“第二”等仅用于描述目的,而不能理解为指示或暗示相对重要性。
在发明中,除非另有明确的规定和限定,术语“安装”、“相连”、“连接”、“固定”等术语应做广义理解,例如,可以是固定连接,也可以是可拆卸连接,或一体地连接;可以是机械连接,也可以是电连接;可以是直接相连,也可以通过中间媒介间接相连,可以是两个元件内部的连通。对于本领域的普通技术人员而言,可以根据具体情况理解上述术语在本发明中的具体含义。
以下结合附图1~6对本发明作进一步详细说明,但不作为对本发明的限定。
自支撑三维多孔碳泡沫的制备方法,包括:
步骤一、将作为碳源的水溶性固体有机物和作为模板的水溶性无机盐溶于去离子水中,按照混水溶液中碳原子与盐的摩尔比为1:1-8配制成总浓度为0.5-5mol/L的混合溶液;
步骤二、对混合溶液进行再结晶,得到碳源均匀包覆无机盐的混合粉末;
步骤三、将预设量粉末装填于热压烧结石墨模具中,将模具放入热压烧结炉内,在真空条件下,600-1000℃热压烧结1-3h,烧结过程中,对样品施加10-40MPa的压力,反应结束后,冷却到室温,得到块体;
步骤四、用酒精清除块体中的脱模剂,再用去离子水反复浸泡去除其中的水溶性无机盐模板,烘干后得到自支撑三维多孔碳泡沫;
步骤五、将自支撑三维多孔碳泡沫切割成所需大小的尺寸,直接用作电化学转换与储能的自支撑电极或者用作骨架进一步负载活性材料。
需要说明的是:采用水溶性无机盐作为模板,通过一步热压烧结法制备出一种尺寸可调、易裁切的自支撑三维多孔碳泡沫。本发明所使用的盐模板成本较低,使用不同种类的盐作为模板或者采用不同的再结晶方法,可轻松调控模板的粒径大小并最终对三维多孔碳的孔径进行可控调节,另外,水溶性盐模板通过水洗就能去除,易回收再利用。本发明所采用的热压烧结法可以在高温烧结的同时对样品施加压力,在压力、高温和模板的三重作用下,碳源碳化并相互连接,一步形成具有良好力学性能的自支撑三维多孔碳结构。本发明制备的自支撑三维多孔碳泡沫可裁切,并直接用作电化学能源转换与存储电极或骨架,具有良好的电化学反应动力学,自支撑三维多孔碳材料作为电极使用时由于内部碳纳米片相互连接而形成三维导电网络,提高电极的导电性;自支撑三维多孔碳作为电极时省去了集流体、粘结剂以及导电添加剂,降低了电化学体系的成本;原位形成的自支撑结构具有的良好力学性能以及分级多孔结构,促进了离子和电解液扩散并增强了电极结构的稳定性。
在根据本发明的自支撑三维多孔碳泡沫的制备方法中,步骤一中,还包括:
为了进一步对碳基体进行修饰改性,在制备过程中,在溶液中加入预设量可溶性氮源、磷源、硫源、或硒源对碳材料形成掺杂的物质,从而在热压烧结过程中形成异质原子掺杂,按照混水溶液中掺杂原子与碳原子的摩尔比为1:10-15配置溶液。
在根据本发明的自支撑三维多孔碳泡沫的制备方法中,步骤二中,碳源为柠檬酸、柠檬酸铵、葡糖糖、蔗糖、乳糖、果糖、明胶、麦芽糖、苹果酸、酒石酸、草酸、草酸铵、乙酸铵等水溶性固体有机物中的一种或多种。
在根据本发明的自支撑三维多孔碳泡沫的制备方法中,步骤一中,作为模板的水溶性无机盐为氯化钠、氯化钾、硫酸钠、硫酸钾、硅酸钠、硅酸钾、碳酸钠、碳酸钾等可溶性无机盐中的一种或多种。
在根据本发明的自支撑三维多孔碳泡沫的制备方法中,氮源为尿素、碳酸氢铵、碳酸铵、硫酸铵、硫酸氢铵中的一种或多种;磷源为水溶性磷酸二氢盐、水溶性次亚磷酸盐中的一种或多种;硫源为硫化钠、硫化钾、硫脲、硫代硫酸钠、硫代苹果酸、硫化铵、硫化氢铵中的一种或多种;硒源为硒氢化钠、二氧化硒中的一种或多种。
在根据本发明的自支撑三维多孔碳泡沫的制备方法中,步骤二中,对混合溶液进行再结晶,包括加热干燥、冷冻干燥、喷雾干燥中的一种。
实施例1
1)称取柠檬酸0.7g、硫脲0.16g、氯化钠7.1g溶于60mL去离子水中,充分搅拌至完全溶解后,得到混合溶液A;
2)将混合溶液置于冰箱中冷冻24h后转移至冻干机内,在-50℃下冷冻干燥,得到柠檬酸-硫脲复合薄膜均匀包覆于氯化钠表面的复合粉末B;
3)取预设量粉末B置于直径为20mm的热压烧结石墨模具中,将模具放入热压烧结炉内,于真空条件下,650℃热压烧结1h,烧结过程中,压力为30MPa,经热压烧结冷却后得到块体C;
4)将块体C用酒精清洗后,用去离子水反复浸泡去除其中的氯化钠盐模板,烘干后得到自支撑三维多孔碳材料D;
5)将自支撑三维多孔碳材料D切割为合适大小的尺寸,用作电化学转换与储能电极。
实施例2
1)称取柠檬酸铵4.054g、硫化钠0.65g、氯化钾59.6g溶于300mL去离子水中,充分搅拌至完全溶解后,得到混合溶液A;
2)将混合溶液通过喷雾干燥后,得到柠檬酸铵均匀包覆的硫化钠与氯化钾混合粉末B;
3)取预设量粉末B置于直径为20mm的热压烧结石墨模具中,将模具放入热压烧结炉内,于真空条件下,650℃热压烧结2h,烧结过程中,压力为20MPa,经热压烧结后得到块体C;
4)将块体C用酒精清洗后,用去离子水反复浸泡去除其中的氯化钾盐模板,烘干后得到自支撑三维多孔碳材料D;
5)将自支撑三维多孔碳材料D切割为合适大小的尺寸,用作电化学转换与储能电极。
实施例3
1)称取葡萄糖4.054g、硫化铵0.925g、硫酸钠134.228g溶于350mL去离子水中,充分搅拌至完全溶解后,得到混合溶液A;
2)将混合溶液置于冰箱中冷冻24h后转移至冻干机内,在-50℃下冷冻干燥得到葡萄糖-硫化铵均匀包覆于硫酸钠表面的复合粉末B;
3)取预设量粉末B于直径为10mm的热压烧结石墨模具中,将模具放入热压烧结炉内,于真空条件下,700℃热压烧结1h,烧结过程中,压力为30MPa,经热压烧结后得到块体C;
4)将块体C用酒精清洗后,用去离子水反复浸泡去除其中的硫酸钠盐模板,烘干后得到自支撑三维多孔碳材料D;
5)将自支撑三维多孔碳材料D切割为合适大小的尺寸,用作电化学转换与储能电极。
实施例4
1)称取蔗糖2.583g、硫化氢铵0.3085g、硅酸钠107.036g溶于300mL去离子水中,充分搅拌至完全溶解后,得到混合溶液A;
2)将混合溶液加热搅拌直至水分完全蒸发后,得到硫化氢铵-蔗糖均匀包覆于硅酸钠表面的复合粉末B;
3)取预设量粉末B于直径为10mm的热压烧结石墨模具中,将模具放入热压烧结炉内,于真空条件下,600℃热压烧结2h,烧结过程中,压力为40MPa,经热压烧结后得到块体C;
4)将块体C用酒精清洗后,用去离子水反复浸泡去除其中的硅酸钠盐模板,烘干后得到自支撑三维多孔碳材料D;
5)将自支撑三维多孔碳材料D裁切为合适大小的尺寸,用作电化学转换与储能电极。
根据上述说明书的揭示和教导,本发明所属领域的技术人员还能够对上述实施方式进行变更和修改。因此,本发明并不局限于上述的具体实施方式,凡是本领域技术人员在本发明的基础上所作出的任何显而易见的改进、替换或变型均属于本发明的保护范围。此外,尽管本说明书中使用了一些特定的术语,但这些术语只是为了方便说明,并不对本发明构成任何限制。
Claims (6)
1.一种自支撑三维多孔碳泡沫的制备方法,其特征在于,包括:
步骤一、将作为碳源的水溶性固体有机物和作为模板的水溶性无机盐溶于去离子水中,按照混水溶液中碳原子与盐的摩尔比为1:1-8配制成总浓度为0.5-5mol/L的混合溶液;
步骤二、对混合溶液进行再结晶,得到碳源均匀包覆无机盐的混合粉末;
步骤三、将预设量粉末装填于热压烧结石墨模具中,将模具放入热压烧结炉内,在真空条件下,600-1000℃热压烧结1-3h,烧结过程中,对样品施加10-40MPa的压力,反应结束后,冷却到室温,得到块体;
步骤四、用酒精清除块体中的脱模剂,再用去离子水反复浸泡去除其中的水溶性无机盐模板,烘干后得到自支撑三维多孔碳泡沫;
步骤五、将自支撑三维多孔碳泡沫切割成所需大小的尺寸,用作电化学转换与储能电极。
2.如权利要求1所述的一种自支撑三维多孔碳泡沫的制备方法,其特征在于,所述步骤一中,还包括:
在溶液中加入预设量可溶性氮源、磷源、硫源、或硒源对碳材料形成掺杂的物质,从而在热压烧结过程中形成异质原子掺杂,按照混水溶液中掺杂原子与碳原子的摩尔比为1:10-15配置溶液。
3.如权利要求2所述的一种自支撑三维多孔碳泡沫的制备方法,其特征在于:所述步骤二中,所述碳源为柠檬酸、柠檬酸铵、葡糖糖、蔗糖、乳糖、果糖、明胶、麦芽糖、苹果酸、酒石酸、草酸、草酸铵、乙酸铵中的一种或多种。
4.如权利要求1所述的一种自支撑三维多孔碳泡沫的制备方法,其特征在于:所述步骤一中,作为模板的水溶性无机盐为氯化钠、氯化钾、硫酸钠、硫酸钾、硅酸钠、硅酸钾、碳酸钠、碳酸钾中的一种或多种。
5.如权利要求2所述的一种自支撑三维多孔碳泡沫的制备方法,其特征在于:所述氮源为尿素、碳酸氢铵、碳酸铵、硫酸铵、硫酸氢铵中的一种或多种;所述磷源为水溶性磷酸二氢盐、水溶性次亚磷酸盐中的一种或多种;所述硫源为硫化钠、硫化钾、硫脲、硫代硫酸钠、硫代苹果酸、硫化铵、硫化氢铵中的一种或多种;所述硒源为硒氢化钠、二氧化硒中的一种或多种。
6.如权利要求1所述的一种自支撑三维多孔碳泡沫的制备方法,其特征在于:所述步骤二中,对混合溶液进行再结晶,包括加热干燥、冷冻干燥、喷雾干燥中的一种。
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