JP5400284B2 - 微細炭素繊維分散液の製造方法 - Google Patents
微細炭素繊維分散液の製造方法 Download PDFInfo
- Publication number
- JP5400284B2 JP5400284B2 JP2007225841A JP2007225841A JP5400284B2 JP 5400284 B2 JP5400284 B2 JP 5400284B2 JP 2007225841 A JP2007225841 A JP 2007225841A JP 2007225841 A JP2007225841 A JP 2007225841A JP 5400284 B2 JP5400284 B2 JP 5400284B2
- Authority
- JP
- Japan
- Prior art keywords
- fine carbon
- dispersion
- carbon fiber
- carbon fibers
- fine
- Prior art date
- Legal status (The legal status is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the status listed.)
- Active
Links
- 229920000049 Carbon (fiber) Polymers 0.000 title claims description 127
- 239000004917 carbon fiber Substances 0.000 title claims description 127
- 239000006185 dispersion Substances 0.000 title claims description 124
- VNWKTOKETHGBQD-UHFFFAOYSA-N methane Chemical compound C VNWKTOKETHGBQD-UHFFFAOYSA-N 0.000 title claims description 71
- 238000004519 manufacturing process Methods 0.000 title claims description 28
- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical compound [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 claims description 56
- 238000011282 treatment Methods 0.000 claims description 48
- 239000007864 aqueous solution Substances 0.000 claims description 21
- 238000003756 stirring Methods 0.000 claims description 21
- 229910052799 carbon Inorganic materials 0.000 claims description 20
- 239000000126 substance Substances 0.000 claims description 18
- 239000002245 particle Substances 0.000 claims description 15
- 239000007788 liquid Substances 0.000 claims description 12
- 239000002888 zwitterionic surfactant Substances 0.000 claims description 9
- 238000009826 distribution Methods 0.000 claims description 6
- 229920005862 polyol Polymers 0.000 claims description 5
- 150000003077 polyols Chemical class 0.000 claims description 5
- 239000002041 carbon nanotube Substances 0.000 description 36
- 229910021393 carbon nanotube Inorganic materials 0.000 description 28
- 238000000034 method Methods 0.000 description 27
- OGQYPPBGSLZBEG-UHFFFAOYSA-N dimethyl(dioctadecyl)azanium Chemical compound CCCCCCCCCCCCCCCCCC[N+](C)(C)CCCCCCCCCCCCCCCCCC OGQYPPBGSLZBEG-UHFFFAOYSA-N 0.000 description 23
- 239000011324 bead Substances 0.000 description 18
- 238000000576 coating method Methods 0.000 description 18
- -1 surfactants Chemical compound 0.000 description 17
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 description 16
- 239000002612 dispersion medium Substances 0.000 description 13
- PEDCQBHIVMGVHV-UHFFFAOYSA-N Glycerine Chemical compound OCC(O)CO PEDCQBHIVMGVHV-UHFFFAOYSA-N 0.000 description 12
- 238000010438 heat treatment Methods 0.000 description 12
- 230000008569 process Effects 0.000 description 12
- 239000004094 surface-active agent Substances 0.000 description 12
- 238000002156 mixing Methods 0.000 description 10
- 239000000203 mixture Substances 0.000 description 10
- 239000003054 catalyst Substances 0.000 description 9
- 239000000835 fiber Substances 0.000 description 9
- 239000000463 material Substances 0.000 description 8
- 239000000243 solution Substances 0.000 description 8
- 239000007789 gas Substances 0.000 description 7
- 229910021389 graphene Inorganic materials 0.000 description 7
- 229910052751 metal Inorganic materials 0.000 description 7
- 239000002184 metal Substances 0.000 description 7
- 239000002994 raw material Substances 0.000 description 7
- OKKJLVBELUTLKV-UHFFFAOYSA-N Methanol Chemical compound OC OKKJLVBELUTLKV-UHFFFAOYSA-N 0.000 description 6
- YXFVVABEGXRONW-UHFFFAOYSA-N Toluene Chemical compound CC1=CC=CC=C1 YXFVVABEGXRONW-UHFFFAOYSA-N 0.000 description 6
- MCMNRKCIXSYSNV-UHFFFAOYSA-N Zirconium dioxide Chemical compound O=[Zr]=O MCMNRKCIXSYSNV-UHFFFAOYSA-N 0.000 description 6
- 230000002776 aggregation Effects 0.000 description 6
- 230000015572 biosynthetic process Effects 0.000 description 6
- 238000006243 chemical reaction Methods 0.000 description 6
- 238000010008 shearing Methods 0.000 description 6
- 238000005979 thermal decomposition reaction Methods 0.000 description 6
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 description 5
- 229920003171 Poly (ethylene oxide) Polymers 0.000 description 5
- 238000004220 aggregation Methods 0.000 description 5
- 239000003575 carbonaceous material Substances 0.000 description 5
- 230000003197 catalytic effect Effects 0.000 description 5
- 239000011248 coating agent Substances 0.000 description 5
- 239000008367 deionised water Substances 0.000 description 5
- 229910021641 deionized water Inorganic materials 0.000 description 5
- 229930195733 hydrocarbon Natural products 0.000 description 5
- 150000002430 hydrocarbons Chemical class 0.000 description 5
- 239000011159 matrix material Substances 0.000 description 5
- 239000000047 product Substances 0.000 description 5
- 239000011347 resin Substances 0.000 description 5
- 229920005989 resin Polymers 0.000 description 5
- 230000009471 action Effects 0.000 description 4
- 150000001722 carbon compounds Chemical class 0.000 description 4
- 238000000354 decomposition reaction Methods 0.000 description 4
- 125000000524 functional group Chemical group 0.000 description 4
- 239000000693 micelle Substances 0.000 description 4
- 150000002894 organic compounds Chemical class 0.000 description 4
- UHOVQNZJYSORNB-UHFFFAOYSA-N Benzene Chemical compound C1=CC=CC=C1 UHOVQNZJYSORNB-UHFFFAOYSA-N 0.000 description 3
- XEKOWRVHYACXOJ-UHFFFAOYSA-N Ethyl acetate Chemical compound CCOC(C)=O XEKOWRVHYACXOJ-UHFFFAOYSA-N 0.000 description 3
- LYCAIKOWRPUZTN-UHFFFAOYSA-N Ethylene glycol Chemical compound OCCO LYCAIKOWRPUZTN-UHFFFAOYSA-N 0.000 description 3
- DNIAPMSPPWPWGF-UHFFFAOYSA-N Propylene glycol Chemical compound CC(O)CO DNIAPMSPPWPWGF-UHFFFAOYSA-N 0.000 description 3
- 150000005215 alkyl ethers Chemical class 0.000 description 3
- 239000002717 carbon nanostructure Substances 0.000 description 3
- 125000003178 carboxy group Chemical group [H]OC(*)=O 0.000 description 3
- 239000002270 dispersing agent Substances 0.000 description 3
- 238000011049 filling Methods 0.000 description 3
- 150000002500 ions Chemical class 0.000 description 3
- 239000011164 primary particle Substances 0.000 description 3
- 239000011269 tar Substances 0.000 description 3
- SVTBMSDMJJWYQN-UHFFFAOYSA-N 2-methylpentane-2,4-diol Chemical compound CC(O)CC(C)(C)O SVTBMSDMJJWYQN-UHFFFAOYSA-N 0.000 description 2
- DIROHOMJLWMERM-UHFFFAOYSA-N 3-[dimethyl(octadecyl)azaniumyl]propane-1-sulfonate Chemical compound CCCCCCCCCCCCCCCCCC[N+](C)(C)CCCS([O-])(=O)=O DIROHOMJLWMERM-UHFFFAOYSA-N 0.000 description 2
- XKRFYHLGVUSROY-UHFFFAOYSA-N Argon Chemical compound [Ar] XKRFYHLGVUSROY-UHFFFAOYSA-N 0.000 description 2
- 239000004215 Carbon black (E152) Substances 0.000 description 2
- UGFAIRIUMAVXCW-UHFFFAOYSA-N Carbon monoxide Chemical compound [O+]#[C-] UGFAIRIUMAVXCW-UHFFFAOYSA-N 0.000 description 2
- RTZKZFJDLAIYFH-UHFFFAOYSA-N Diethyl ether Natural products CCOCC RTZKZFJDLAIYFH-UHFFFAOYSA-N 0.000 description 2
- XEEYBQQBJWHFJM-UHFFFAOYSA-N Iron Chemical compound [Fe] XEEYBQQBJWHFJM-UHFFFAOYSA-N 0.000 description 2
- CTQNGGLPUBDAKN-UHFFFAOYSA-N O-Xylene Chemical compound CC1=CC=CC=C1C CTQNGGLPUBDAKN-UHFFFAOYSA-N 0.000 description 2
- 229910019142 PO4 Inorganic materials 0.000 description 2
- 238000001069 Raman spectroscopy Methods 0.000 description 2
- NINIDFKCEFEMDL-UHFFFAOYSA-N Sulfur Chemical compound [S] NINIDFKCEFEMDL-UHFFFAOYSA-N 0.000 description 2
- WYURNTSHIVDZCO-UHFFFAOYSA-N Tetrahydrofuran Chemical compound C1CCOC1 WYURNTSHIVDZCO-UHFFFAOYSA-N 0.000 description 2
- YTPLMLYBLZKORZ-UHFFFAOYSA-N Thiophene Chemical compound C=1C=CSC=1 YTPLMLYBLZKORZ-UHFFFAOYSA-N 0.000 description 2
- 238000005054 agglomeration Methods 0.000 description 2
- 150000001298 alcohols Chemical class 0.000 description 2
- 239000002280 amphoteric surfactant Substances 0.000 description 2
- 239000003945 anionic surfactant Substances 0.000 description 2
- 150000001721 carbon Chemical class 0.000 description 2
- 229910002091 carbon monoxide Inorganic materials 0.000 description 2
- 239000003093 cationic surfactant Substances 0.000 description 2
- 238000004040 coloring Methods 0.000 description 2
- 230000006378 damage Effects 0.000 description 2
- 230000007547 defect Effects 0.000 description 2
- 235000014113 dietary fatty acids Nutrition 0.000 description 2
- BHATUINFZWUDIX-UHFFFAOYSA-O dimethyl-(3-sulfopropyl)-tetradecylazanium Chemical compound CCCCCCCCCCCCCC[N+](C)(C)CCCS(O)(=O)=O BHATUINFZWUDIX-UHFFFAOYSA-O 0.000 description 2
- 239000012153 distilled water Substances 0.000 description 2
- 150000002148 esters Chemical class 0.000 description 2
- 238000001704 evaporation Methods 0.000 description 2
- 230000008020 evaporation Effects 0.000 description 2
- 229930195729 fatty acid Natural products 0.000 description 2
- 239000000194 fatty acid Substances 0.000 description 2
- 239000011521 glass Substances 0.000 description 2
- 239000008187 granular material Substances 0.000 description 2
- 229910002804 graphite Inorganic materials 0.000 description 2
- 239000010439 graphite Substances 0.000 description 2
- 230000036571 hydration Effects 0.000 description 2
- 238000006703 hydration reaction Methods 0.000 description 2
- 125000001165 hydrophobic group Chemical group 0.000 description 2
- 239000002116 nanohorn Substances 0.000 description 2
- 239000002736 nonionic surfactant Substances 0.000 description 2
- 235000021317 phosphate Nutrition 0.000 description 2
- 230000000704 physical effect Effects 0.000 description 2
- 229920000642 polymer Polymers 0.000 description 2
- 239000000843 powder Substances 0.000 description 2
- 238000012545 processing Methods 0.000 description 2
- 238000011160 research Methods 0.000 description 2
- 239000002109 single walled nanotube Substances 0.000 description 2
- 239000003381 stabilizer Substances 0.000 description 2
- 230000003068 static effect Effects 0.000 description 2
- 239000000758 substrate Substances 0.000 description 2
- 229910052717 sulfur Inorganic materials 0.000 description 2
- 239000011593 sulfur Substances 0.000 description 2
- 150000003464 sulfur compounds Chemical class 0.000 description 2
- 229910052723 transition metal Inorganic materials 0.000 description 2
- 150000003623 transition metal compounds Chemical class 0.000 description 2
- 150000003624 transition metals Chemical class 0.000 description 2
- 239000008096 xylene Substances 0.000 description 2
- PUPZLCDOIYMWBV-UHFFFAOYSA-N (+/-)-1,3-Butanediol Chemical compound CC(O)CCO PUPZLCDOIYMWBV-UHFFFAOYSA-N 0.000 description 1
- 229940043375 1,5-pentanediol Drugs 0.000 description 1
- IIZPXYDJLKNOIY-JXPKJXOSSA-N 1-palmitoyl-2-arachidonoyl-sn-glycero-3-phosphocholine Chemical compound CCCCCCCCCCCCCCCC(=O)OC[C@H](COP([O-])(=O)OCC[N+](C)(C)C)OC(=O)CCC\C=C/C\C=C/C\C=C/C\C=C/CCCCC IIZPXYDJLKNOIY-JXPKJXOSSA-N 0.000 description 1
- UMCMPZBLKLEWAF-BCTGSCMUSA-N 3-[(3-cholamidopropyl)dimethylammonio]propane-1-sulfonate Chemical compound 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)NCCC[N+](C)(C)CCCS([O-])(=O)=O)C)[C@@]2(C)[C@@H](O)C1 UMCMPZBLKLEWAF-BCTGSCMUSA-N 0.000 description 1
- GUQQBLRVXOUDTN-XOHPMCGNSA-N 3-[dimethyl-[3-[[(4r)-4-[(3r,5s,7r,8r,9s,10s,12s,13r,14s,17r)-3,7,12-trihydroxy-10,13-dimethyl-2,3,4,5,6,7,8,9,11,12,14,15,16,17-tetradecahydro-1h-cyclopenta[a]phenanthren-17-yl]pentanoyl]amino]propyl]azaniumyl]-2-hydroxypropane-1-sulfonate Chemical compound 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)NCCC[N+](C)(C)CC(O)CS([O-])(=O)=O)C)[C@@]2(C)[C@@H](O)C1 GUQQBLRVXOUDTN-XOHPMCGNSA-N 0.000 description 1
- XPFCZYUVICHKDS-UHFFFAOYSA-N 3-methylbutane-1,3-diol Chemical compound CC(C)(O)CCO XPFCZYUVICHKDS-UHFFFAOYSA-N 0.000 description 1
- QTBSBXVTEAMEQO-UHFFFAOYSA-M Acetate Chemical compound CC([O-])=O QTBSBXVTEAMEQO-UHFFFAOYSA-M 0.000 description 1
- 241000234282 Allium Species 0.000 description 1
- 235000002732 Allium cepa var. cepa Nutrition 0.000 description 1
- XMWRBQBLMFGWIX-UHFFFAOYSA-N C60 fullerene Chemical class C12=C3C(C4=C56)=C7C8=C5C5=C9C%10=C6C6=C4C1=C1C4=C6C6=C%10C%10=C9C9=C%11C5=C8C5=C8C7=C3C3=C7C2=C1C1=C2C4=C6C4=C%10C6=C9C9=C%11C5=C5C8=C3C3=C7C1=C1C2=C4C6=C2C9=C5C3=C12 XMWRBQBLMFGWIX-UHFFFAOYSA-N 0.000 description 1
- 229910000669 Chrome steel Inorganic materials 0.000 description 1
- SNPLKNRPJHDVJA-ZETCQYMHSA-N D-panthenol Chemical compound OCC(C)(C)[C@@H](O)C(=O)NCCCO SNPLKNRPJHDVJA-ZETCQYMHSA-N 0.000 description 1
- MBMLMWLHJBBADN-UHFFFAOYSA-N Ferrous sulfide Chemical compound [Fe]=S MBMLMWLHJBBADN-UHFFFAOYSA-N 0.000 description 1
- UFHFLCQGNIYNRP-UHFFFAOYSA-N Hydrogen Chemical compound [H][H] UFHFLCQGNIYNRP-UHFFFAOYSA-N 0.000 description 1
- ZOKXTWBITQBERF-UHFFFAOYSA-N Molybdenum Chemical compound [Mo] ZOKXTWBITQBERF-UHFFFAOYSA-N 0.000 description 1
- 239000002202 Polyethylene glycol Substances 0.000 description 1
- XBDQKXXYIPTUBI-UHFFFAOYSA-M Propionate Chemical compound CCC([O-])=O XBDQKXXYIPTUBI-UHFFFAOYSA-M 0.000 description 1
- 229910000831 Steel Inorganic materials 0.000 description 1
- ULUAUXLGCMPNKK-UHFFFAOYSA-N Sulfobutanedioic acid Chemical compound OC(=O)CC(C(O)=O)S(O)(=O)=O ULUAUXLGCMPNKK-UHFFFAOYSA-N 0.000 description 1
- 238000005411 Van der Waals force Methods 0.000 description 1
- KXKVLQRXCPHEJC-UHFFFAOYSA-N acetic acid trimethyl ester Natural products COC(C)=O KXKVLQRXCPHEJC-UHFFFAOYSA-N 0.000 description 1
- 239000002253 acid Substances 0.000 description 1
- 150000007513 acids Chemical class 0.000 description 1
- 239000013543 active substance Substances 0.000 description 1
- 238000013019 agitation Methods 0.000 description 1
- 125000000217 alkyl group Chemical group 0.000 description 1
- 125000005037 alkyl phenyl group Chemical group 0.000 description 1
- 150000008051 alkyl sulfates Chemical class 0.000 description 1
- 150000008052 alkyl sulfonates Chemical class 0.000 description 1
- PNEYBMLMFCGWSK-UHFFFAOYSA-N aluminium oxide Inorganic materials [O-2].[O-2].[O-2].[Al+3].[Al+3] PNEYBMLMFCGWSK-UHFFFAOYSA-N 0.000 description 1
- 229910052786 argon Inorganic materials 0.000 description 1
- 230000008901 benefit Effects 0.000 description 1
- WGQKYBSKWIADBV-UHFFFAOYSA-N benzylamine Chemical class NCC1=CC=CC=C1 WGQKYBSKWIADBV-UHFFFAOYSA-N 0.000 description 1
- 239000006229 carbon black Substances 0.000 description 1
- 239000002238 carbon nanotube film Substances 0.000 description 1
- 239000000919 ceramic Substances 0.000 description 1
- 230000008859 change Effects 0.000 description 1
- 238000005229 chemical vapour deposition Methods 0.000 description 1
- 229910017052 cobalt Inorganic materials 0.000 description 1
- 239000010941 cobalt Substances 0.000 description 1
- GUTLYIVDDKVIGB-UHFFFAOYSA-N cobalt atom Chemical compound [Co] GUTLYIVDDKVIGB-UHFFFAOYSA-N 0.000 description 1
- 230000000052 comparative effect Effects 0.000 description 1
- 238000013329 compounding Methods 0.000 description 1
- 150000001875 compounds Chemical class 0.000 description 1
- 238000011109 contamination Methods 0.000 description 1
- 238000007796 conventional method Methods 0.000 description 1
- 239000013078 crystal Substances 0.000 description 1
- QBHFVMDLPTZDOI-UHFFFAOYSA-N dodecylphosphocholine Chemical compound CCCCCCCCCCCCOP([O-])(=O)OCC[N+](C)(C)C QBHFVMDLPTZDOI-UHFFFAOYSA-N 0.000 description 1
- 150000002170 ethers Chemical class 0.000 description 1
- 238000002474 experimental method Methods 0.000 description 1
- 150000004665 fatty acids Chemical class 0.000 description 1
- KTWOOEGAPBSYNW-UHFFFAOYSA-N ferrocene Chemical compound [Fe+2].C=1C=C[CH-]C=1.C=1C=C[CH-]C=1 KTWOOEGAPBSYNW-UHFFFAOYSA-N 0.000 description 1
- 239000002657 fibrous material Substances 0.000 description 1
- 239000010419 fine particle Substances 0.000 description 1
- 238000005187 foaming Methods 0.000 description 1
- 229910003472 fullerene Inorganic materials 0.000 description 1
- 238000002309 gasification Methods 0.000 description 1
- 229960005150 glycerol Drugs 0.000 description 1
- 230000005484 gravity Effects 0.000 description 1
- 239000001307 helium Substances 0.000 description 1
- 229910052734 helium Inorganic materials 0.000 description 1
- SWQJXJOGLNCZEY-UHFFFAOYSA-N helium atom Chemical compound [He] SWQJXJOGLNCZEY-UHFFFAOYSA-N 0.000 description 1
- 229940051250 hexylene glycol Drugs 0.000 description 1
- 239000001257 hydrogen Substances 0.000 description 1
- 229910052739 hydrogen Inorganic materials 0.000 description 1
- 230000006872 improvement Effects 0.000 description 1
- 239000012535 impurity Substances 0.000 description 1
- 238000010348 incorporation Methods 0.000 description 1
- 239000008235 industrial water Substances 0.000 description 1
- 239000011261 inert gas Substances 0.000 description 1
- 239000013067 intermediate product Substances 0.000 description 1
- 239000002563 ionic surfactant Substances 0.000 description 1
- 229910052742 iron Inorganic materials 0.000 description 1
- 239000000787 lecithin Substances 0.000 description 1
- 229940067606 lecithin Drugs 0.000 description 1
- 235000010445 lecithin Nutrition 0.000 description 1
- 239000002609 medium Substances 0.000 description 1
- 150000002739 metals Chemical class 0.000 description 1
- PQLXHQMOHUQAKB-UHFFFAOYSA-N miltefosine Chemical compound CCCCCCCCCCCCCCCCOP([O-])(=O)OCC[N+](C)(C)C PQLXHQMOHUQAKB-UHFFFAOYSA-N 0.000 description 1
- 229910052750 molybdenum Inorganic materials 0.000 description 1
- 239000011733 molybdenum Substances 0.000 description 1
- 239000002048 multi walled nanotube Substances 0.000 description 1
- 239000002088 nanocapsule Substances 0.000 description 1
- 229910021392 nanocarbon Inorganic materials 0.000 description 1
- 239000002071 nanotube Substances 0.000 description 1
- 230000007935 neutral effect Effects 0.000 description 1
- MDNHUELOANFCGT-UHFFFAOYSA-N octyl 2-(trimethylazaniumyl)ethyl phosphate Chemical compound CCCCCCCCOP([O-])(=O)OCC[N+](C)(C)C MDNHUELOANFCGT-UHFFFAOYSA-N 0.000 description 1
- 239000003960 organic solvent Substances 0.000 description 1
- 229940101267 panthenol Drugs 0.000 description 1
- 239000011619 pantothenol Substances 0.000 description 1
- 235000020957 pantothenol Nutrition 0.000 description 1
- WCVRQHFDJLLWFE-UHFFFAOYSA-N pentane-1,2-diol Chemical compound CCCC(O)CO WCVRQHFDJLLWFE-UHFFFAOYSA-N 0.000 description 1
- 230000002093 peripheral effect Effects 0.000 description 1
- 239000005011 phenolic resin Substances 0.000 description 1
- 229920001223 polyethylene glycol Polymers 0.000 description 1
- 229920001184 polypeptide Polymers 0.000 description 1
- 229920001451 polypropylene glycol Polymers 0.000 description 1
- 102000004196 processed proteins & peptides Human genes 0.000 description 1
- 108090000765 processed proteins & peptides Proteins 0.000 description 1
- 230000002035 prolonged effect Effects 0.000 description 1
- BDERNNFJNOPAEC-UHFFFAOYSA-N propan-1-ol Chemical compound CCCO BDERNNFJNOPAEC-UHFFFAOYSA-N 0.000 description 1
- KCXFHTAICRTXLI-UHFFFAOYSA-N propane-1-sulfonic acid Chemical compound CCCS(O)(=O)=O KCXFHTAICRTXLI-UHFFFAOYSA-N 0.000 description 1
- 238000010298 pulverizing process Methods 0.000 description 1
- 238000000197 pyrolysis Methods 0.000 description 1
- 238000001953 recrystallisation Methods 0.000 description 1
- 150000003839 salts Chemical class 0.000 description 1
- 239000004576 sand Substances 0.000 description 1
- 239000011163 secondary particle Substances 0.000 description 1
- 238000004904 shortening Methods 0.000 description 1
- 239000002904 solvent Substances 0.000 description 1
- 238000004611 spectroscopical analysis Methods 0.000 description 1
- 238000004528 spin coating Methods 0.000 description 1
- 239000010959 steel Substances 0.000 description 1
- 150000005846 sugar alcohols Polymers 0.000 description 1
- BDHFUVZGWQCTTF-UHFFFAOYSA-M sulfonate Chemical compound [O-]S(=O)=O BDHFUVZGWQCTTF-UHFFFAOYSA-M 0.000 description 1
- 238000003786 synthesis reaction Methods 0.000 description 1
- 230000002194 synthesizing effect Effects 0.000 description 1
- 150000005621 tetraalkylammonium salts Chemical class 0.000 description 1
- BETUMLXGYDBOLV-UHFFFAOYSA-N tetradecyl 2-(trimethylazaniumyl)ethyl phosphate Chemical compound CCCCCCCCCCCCCCOP([O-])(=O)OCC[N+](C)(C)C BETUMLXGYDBOLV-UHFFFAOYSA-N 0.000 description 1
- YLQBMQCUIZJEEH-UHFFFAOYSA-N tetrahydrofuran Natural products C=1C=COC=1 YLQBMQCUIZJEEH-UHFFFAOYSA-N 0.000 description 1
- 238000004227 thermal cracking Methods 0.000 description 1
- 229930192474 thiophene Natural products 0.000 description 1
- 239000011882 ultra-fine particle Substances 0.000 description 1
- 230000008016 vaporization Effects 0.000 description 1
- 229910052724 xenon Inorganic materials 0.000 description 1
- FHNFHKCVQCLJFQ-UHFFFAOYSA-N xenon atom Chemical compound [Xe] FHNFHKCVQCLJFQ-UHFFFAOYSA-N 0.000 description 1
Classifications
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B82—NANOTECHNOLOGY
- B82Y—SPECIFIC USES OR APPLICATIONS OF NANOSTRUCTURES; MEASUREMENT OR ANALYSIS OF NANOSTRUCTURES; MANUFACTURE OR TREATMENT OF NANOSTRUCTURES
- B82Y30/00—Nanotechnology for materials or surface science, e.g. nanocomposites
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B82—NANOTECHNOLOGY
- B82Y—SPECIFIC USES OR APPLICATIONS OF NANOSTRUCTURES; MEASUREMENT OR ANALYSIS OF NANOSTRUCTURES; MANUFACTURE OR TREATMENT OF NANOSTRUCTURES
- B82Y40/00—Manufacture or treatment of nanostructures
-
- 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
- C01B2202/00—Structure or properties of carbon nanotubes
- C01B2202/20—Nanotubes characterized by their properties
- C01B2202/28—Solid content in solvents
Description
(微細炭素繊維)
本発明の微細炭素繊維分散液の製造方法において、分散対象となる微細炭素繊維としては、特に限定されるものではないが、主として、炭素の六員環配列構造を有する構造体であって、この構造体の三次元のディメンションのうち少なくとも1つの寸法がナノメートルの領域にある、たとえば、数〜数100nm程度のオーダーを有する、ものが代表的なものである。
上記したような微細炭素繊維を分散させるために、後述するような両親媒性物質を含有する水溶液中を調製する上で使用する水としては、市水、工業用水、脱イオン水、蒸留水等を用いることができるが、分散液のpH値を安定に所定範囲とする上で、脱イオン水、蒸留水を用いることが望ましく、さらに経済的見地から脱イオン水を用いることが可能である。
本発明において用いられる両親媒性物質としては、特に限定されるものではなく、陰イオン界面活性剤、陽イオン界面活性剤、両性イオン界面活性剤、非イオン性界面活性剤等の公知の各種の界面活性剤、さらに、分子中に親水基(ないしは親水団)および疎水基(ないし疎水団)を有するその他の各種化合物を使用することが可能である。
本発明においては、上記したような微細炭素繊維の凝集体を、両親媒性物質を含有する水溶液に撹拌等によりせん断力を加えながら分散させるものであるが、この際の撹拌方法としては、特に限定されるものではなく、従来、公知の各種の方法を単独であるいは複数組み合わせて、採択することが可能である。例えば、自動式ないし手動式のシェイカー、マグネティックスターラー、超音波振動子、その他、パドルおよびブレード等の各種攪拌子を備えた攪拌機、ビーズミル等のメディアミル、スタティックミキサー等の静止型撹拌機等を用いることが挙げられるが、このうち特に、メディアミルを用いて分散処理を行うことが望ましい。メディアミルは、微細炭素繊維凝集体に対し、均一かつ良好にせん断力を加えることができ、微細炭素繊維凝集体の解砕および分散化を効率よく行えるためである。
上記したような分散処理を施すことによって得られる本発明に係る微細炭素分散液においては、微細炭素繊維が十分に分散され、分散媒中で単繊維状で安定して分散されている。このため、当該微細炭素繊維分散液を、導電性被膜、帯電防止被膜、電磁波制御性被膜、高硬度ないし耐摩耗性被膜、着色被膜等の各種機能性被膜の形成、あるいは、マトリックス材となる各種物質へ微細炭素繊維の配合に適用した場合、微細炭素繊維が均一かつ単分散化された製品を得ることができ、微細炭素繊維が本来有する優れた、導電性、制電性、着色性、物理的強度、化学的安定性等の特性を最大限に発揮した、高機能、高性能の製品を製造することが可能となる。
実施例1
まず、両性界面活性剤3−(N,N’−ジメチルステアリルアンモニオ)プロパンスルフォネート4.0gに対し脱イオン水960ml、グリセロール40mlの割合で添加して、界面活性剤溶液(pH 6.08)を調製した。
実施例1において、CNT20gに対し、界面活性剤溶液500mlを配合して、ボール入り胴体(ボール直径150mm)内に入れ、ある程度手によりかき混ぜた後、上記ボール入り胴体を回転架台(アサヒ理化研究所 As ONE)に乗せ1時間撹拌し、ペーストゾル状とした後、このペーストゾルに残りの界面活性剤溶液500mlを添加し、ビーズミルにて分散処理した以外は実施例1と同様にしてCNT分散液を調製した。分散液のpHは、予備混合処理および分散処理の期間を通じて、pH6.0〜6.5の範囲に維持されており、予備混合処理を行ったことで、ビーズミルでの分散処理操作がより円滑に進行した。
界面活性剤溶液として、両性界面活性剤3−(N,N’−ジメチルステアリルアンモニオ)プロパンスルフォネート4.0gに対し脱イオン水1000ml割合で添加して調製したもの(グリセロール添加なし)を用いた以外は、実施例1と同様にしてCNT分散液を調製した。
実施例3において、ボールミルによる撹拌時間をより長時間化させる以外は、実施例1と同様にしてCNT分散液の調製を試みた。その結果、撹拌時間7時間前までは、pH値が5.5〜6.5の範囲内に維持され、CNTが分散液内において分散される傾向にあったが、撹拌時間が7時間を越えるあたりでpH値の大きな変動が生じ、CNTの凝集が発生し、良好な分散状態を保持できなくなった。
Claims (6)
- 微細炭素繊維の凝集体を、両性イオン性界面活性剤を含有する水溶液に分散させた微細炭素繊維分散液の製造方法であって、微細炭素繊維を分散させる分散工程において、分散液のpHを5.5〜6.5に保持することを特徴とする微細炭素分散液の製造方法。
- 前記分散工程において、メディアミルを用いることを特徴とする請求項1に記載の微細炭素繊維分散液の製造方法。
- 前記メディアミルを用いて分散処理を行うに先立ち、回転撹拌により予備混合を行うことを特徴とする請求項1または2に記載の微細炭素繊維分散液の製造方法。
- 両親媒性物質を含有する水溶液がさらに水溶性ポリオール類を含有するものであることを特徴とする請求項1〜3のいずれか1つに記載の微細炭素繊維分散液の製造方法。
- 微細炭素繊維の凝集体を、両性イオン性界面活性剤を含有する水溶液に分散させた微細炭素繊維分散液であって、微細炭素繊維を分散させる分散工程において、分散液のpHを5.5〜6.5に保持することで得られることを特徴とする両性イオン性界面活性剤を含むpH5.5〜6.5の水溶液中に分散されている微細炭素分散液。
- 分散液中の微細炭素が、粒度分布において90%が0.2μm以内に入るものであることを特徴とする請求項5に記載の微細炭素繊維分散液。
Priority Applications (2)
Application Number | Priority Date | Filing Date | Title |
---|---|---|---|
JP2007225841A JP5400284B2 (ja) | 2007-08-31 | 2007-08-31 | 微細炭素繊維分散液の製造方法 |
PCT/JP2008/065558 WO2009028672A1 (ja) | 2007-08-31 | 2008-08-29 | 微細炭素繊維分散液の製造方法 |
Applications Claiming Priority (1)
Application Number | Priority Date | Filing Date | Title |
---|---|---|---|
JP2007225841A JP5400284B2 (ja) | 2007-08-31 | 2007-08-31 | 微細炭素繊維分散液の製造方法 |
Publications (2)
Publication Number | Publication Date |
---|---|
JP2009057241A JP2009057241A (ja) | 2009-03-19 |
JP5400284B2 true JP5400284B2 (ja) | 2014-01-29 |
Family
ID=40387382
Family Applications (1)
Application Number | Title | Priority Date | Filing Date |
---|---|---|---|
JP2007225841A Active JP5400284B2 (ja) | 2007-08-31 | 2007-08-31 | 微細炭素繊維分散液の製造方法 |
Country Status (2)
Country | Link |
---|---|
JP (1) | JP5400284B2 (ja) |
WO (1) | WO2009028672A1 (ja) |
Families Citing this family (1)
Publication number | Priority date | Publication date | Assignee | Title |
---|---|---|---|---|
JP6652049B2 (ja) * | 2014-05-30 | 2020-02-19 | 日本ゼオン株式会社 | カーボンナノチューブ分散液の製造方法およびカーボンナノチューブ分散液、複合材料用組成物の製造方法および複合材料の製造方法、並びに、複合材料および複合材料成形体 |
Family Cites Families (3)
Publication number | Priority date | Publication date | Assignee | Title |
---|---|---|---|---|
JP3991602B2 (ja) * | 2001-03-02 | 2007-10-17 | 富士ゼロックス株式会社 | カーボンナノチューブ構造体の製造方法、配線部材の製造方法および配線部材 |
JP2005035810A (ja) * | 2003-07-15 | 2005-02-10 | Mikuni Color Ltd | 0次元又は1次元炭素構造体の分散液 |
JP4528324B2 (ja) * | 2007-01-11 | 2010-08-18 | 本田技研工業株式会社 | 熱輸送流体およびその製造方法 |
-
2007
- 2007-08-31 JP JP2007225841A patent/JP5400284B2/ja active Active
-
2008
- 2008-08-29 WO PCT/JP2008/065558 patent/WO2009028672A1/ja active Application Filing
Also Published As
Publication number | Publication date |
---|---|
WO2009028672A1 (ja) | 2009-03-05 |
JP2009057241A (ja) | 2009-03-19 |
Similar Documents
Publication | Publication Date | Title |
---|---|---|
US20210178470A1 (en) | 3d printers and feedstocks for 3d printers | |
JP5301793B2 (ja) | 再分散用微細炭素繊維集合塊およびその製造方法 | |
Zhou et al. | Effective control of nanodefects in multiwalled carbon nanotubes by acid treatment | |
JP5634543B2 (ja) | 超低嵩密度のバンドル部分を有する高伝導性カーボンナノチューブ及びその製造方法 | |
JP5871395B2 (ja) | 除去可能添加物を含む、溶剤性カーボンナノチューブインクおよび水性カーボンナノチューブインク | |
Guo et al. | Synthesis of novel Sb2O3 and Sb2O5 nanorods | |
WO2006117924A1 (ja) | 透明導電膜および透明導電膜用コーティング組成物 | |
EP2351704A1 (en) | Aqueous dispersion of carbon microfibers, process for producing the aqueous dispersion, and article produced using same | |
US20100308279A1 (en) | Conductive Silicone and Methods for Preparing Same | |
US20150340117A1 (en) | Method for producing conductive film | |
WO2010008046A1 (ja) | 炭素繊維の集合体、その製造方法及びそれらを含有する複合材料 | |
Yu et al. | Coating MWNTs with Cu2O of different morphology by a polyol process | |
WO2010002004A1 (ja) | 炭素繊維及び複合材料 | |
Nam et al. | Green, fast, and scalable production of reduced graphene oxide via Taylor vortex flow | |
US20100197832A1 (en) | Isolated nanotubes and polymer nanocomposites | |
JP5400284B2 (ja) | 微細炭素繊維分散液の製造方法 | |
JP5110059B2 (ja) | 微細な炭素繊維および微細な炭素短繊維 | |
He et al. | Fabrication of carbon nanotube-reinforced 6061Al alloy matrix composites by an in situ synthesis method combined with hot extrusion technique | |
JP2006183227A (ja) | 炭素繊維構造体 | |
Alcázar et al. | Production and characterization of carbon nanotubes by methane decomposition over Ni–Fe/Al2O3 catalyst and its application as nanofillers in polypropylene matrix | |
Seo et al. | Templated, carbothermal reduction synthesis of mesoporous silicon carbide from carbon nanotube–mesoporous silica core–shell composite | |
Kang et al. | In situ synthesis of carbon onion/nanotube reinforcements in copper powders | |
He et al. | Fabrication of carbon nanomaterials by chemical vapor deposition | |
Hwang et al. | Synthesis of sea urchin-like carbon nanotubes on nano-diamond powder | |
JP2018030770A (ja) | ナノ炭素材料の分散方法、ナノ炭素材料の分散液及びナノ炭素材料複合体 |
Legal Events
Date | Code | Title | Description |
---|---|---|---|
A621 | Written request for application examination |
Free format text: JAPANESE INTERMEDIATE CODE: A621 Effective date: 20100430 |
|
A131 | Notification of reasons for refusal |
Free format text: JAPANESE INTERMEDIATE CODE: A131 Effective date: 20121002 |
|
A521 | Request for written amendment filed |
Free format text: JAPANESE INTERMEDIATE CODE: A523 Effective date: 20121203 |
|
TRDD | Decision of grant or rejection written | ||
A01 | Written decision to grant a patent or to grant a registration (utility model) |
Free format text: JAPANESE INTERMEDIATE CODE: A01 Effective date: 20131001 |
|
A61 | First payment of annual fees (during grant procedure) |
Free format text: JAPANESE INTERMEDIATE CODE: A61 Effective date: 20131025 |
|
R150 | Certificate of patent or registration of utility model |
Ref document number: 5400284 Country of ref document: JP Free format text: JAPANESE INTERMEDIATE CODE: R150 Free format text: JAPANESE INTERMEDIATE CODE: R150 |
|
R250 | Receipt of annual fees |
Free format text: JAPANESE INTERMEDIATE CODE: R250 |
|
R250 | Receipt of annual fees |
Free format text: JAPANESE INTERMEDIATE CODE: R250 |
|
R250 | Receipt of annual fees |
Free format text: JAPANESE INTERMEDIATE CODE: R250 |
|
R250 | Receipt of annual fees |
Free format text: JAPANESE INTERMEDIATE CODE: R250 |
|
R250 | Receipt of annual fees |
Free format text: JAPANESE INTERMEDIATE CODE: R250 |
|
R250 | Receipt of annual fees |
Free format text: JAPANESE INTERMEDIATE CODE: R250 |
|
R250 | Receipt of annual fees |
Free format text: JAPANESE INTERMEDIATE CODE: R250 |
|
R250 | Receipt of annual fees |
Free format text: JAPANESE INTERMEDIATE CODE: R250 |