CN106948165A - 一种自融合石墨烯纤维及其制备方法 - Google Patents
一种自融合石墨烯纤维及其制备方法 Download PDFInfo
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- CN106948165A CN106948165A CN201710294377.6A CN201710294377A CN106948165A CN 106948165 A CN106948165 A CN 106948165A CN 201710294377 A CN201710294377 A CN 201710294377A CN 106948165 A CN106948165 A CN 106948165A
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- 239000000835 fiber Substances 0.000 title claims abstract description 143
- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical compound [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 title claims abstract description 103
- 229910021389 graphene Inorganic materials 0.000 title claims abstract description 103
- 230000004927 fusion Effects 0.000 title claims abstract description 60
- 238000002360 preparation method Methods 0.000 title claims abstract description 10
- 239000002904 solvent Substances 0.000 claims abstract description 25
- 238000000034 method Methods 0.000 claims abstract description 16
- 238000001035 drying Methods 0.000 claims abstract description 7
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 claims description 37
- 239000007864 aqueous solution Substances 0.000 claims description 36
- MTHSVFCYNBDYFN-UHFFFAOYSA-N diethylene glycol Chemical compound OCCOCCO MTHSVFCYNBDYFN-UHFFFAOYSA-N 0.000 claims description 27
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- OKKJLVBELUTLKV-UHFFFAOYSA-N Methanol Chemical compound OC OKKJLVBELUTLKV-UHFFFAOYSA-N 0.000 claims description 18
- KWYUFKZDYYNOTN-UHFFFAOYSA-M Potassium hydroxide Chemical compound [OH-].[K+] KWYUFKZDYYNOTN-UHFFFAOYSA-M 0.000 claims description 18
- 239000000243 solution Substances 0.000 claims description 16
- XEKOWRVHYACXOJ-UHFFFAOYSA-N Ethyl acetate Chemical compound CCOC(C)=O XEKOWRVHYACXOJ-UHFFFAOYSA-N 0.000 claims description 15
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- WCUXLLCKKVVCTQ-UHFFFAOYSA-M Potassium chloride Chemical compound [Cl-].[K+] WCUXLLCKKVVCTQ-UHFFFAOYSA-M 0.000 claims description 8
- JUJWROOIHBZHMG-UHFFFAOYSA-N Pyridine Chemical compound C1=CC=NC=C1 JUJWROOIHBZHMG-UHFFFAOYSA-N 0.000 claims description 8
- FAPWRFPIFSIZLT-UHFFFAOYSA-M Sodium chloride Chemical compound [Na+].[Cl-] FAPWRFPIFSIZLT-UHFFFAOYSA-M 0.000 claims description 8
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- ZCCIPPOKBCJFDN-UHFFFAOYSA-N calcium nitrate Chemical compound [Ca+2].[O-][N+]([O-])=O.[O-][N+]([O-])=O ZCCIPPOKBCJFDN-UHFFFAOYSA-N 0.000 claims description 8
- VWDWKYIASSYTQR-UHFFFAOYSA-N sodium nitrate Chemical compound [Na+].[O-][N+]([O-])=O VWDWKYIASSYTQR-UHFFFAOYSA-N 0.000 claims description 8
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- QTBSBXVTEAMEQO-UHFFFAOYSA-N Acetic acid Chemical compound CC(O)=O QTBSBXVTEAMEQO-UHFFFAOYSA-N 0.000 claims description 6
- IAZDPXIOMUYVGZ-UHFFFAOYSA-N Dimethylsulphoxide Chemical compound CS(C)=O IAZDPXIOMUYVGZ-UHFFFAOYSA-N 0.000 claims description 6
- KFZMGEQAYNKOFK-UHFFFAOYSA-N Isopropanol Chemical compound CC(C)O KFZMGEQAYNKOFK-UHFFFAOYSA-N 0.000 claims description 6
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- 150000001336 alkenes Chemical class 0.000 claims description 5
- 239000001110 calcium chloride Substances 0.000 claims description 5
- 229910001628 calcium chloride Inorganic materials 0.000 claims description 5
- CIWBSHSKHKDKBQ-JLAZNSOCSA-N Ascorbic acid Chemical compound OC[C@H](O)[C@H]1OC(=O)C(O)=C1O CIWBSHSKHKDKBQ-JLAZNSOCSA-N 0.000 claims description 4
- FERIUCNNQQJTOY-UHFFFAOYSA-N Butyric acid Chemical compound CCCC(O)=O FERIUCNNQQJTOY-UHFFFAOYSA-N 0.000 claims description 4
- PEDCQBHIVMGVHV-UHFFFAOYSA-N Glycerine Chemical compound OCC(O)CO PEDCQBHIVMGVHV-UHFFFAOYSA-N 0.000 claims description 4
- OFOBLEOULBTSOW-UHFFFAOYSA-N Malonic acid Chemical compound OC(=O)CC(O)=O OFOBLEOULBTSOW-UHFFFAOYSA-N 0.000 claims description 4
- FXHOOIRPVKKKFG-UHFFFAOYSA-N N,N-Dimethylacetamide Chemical compound CN(C)C(C)=O FXHOOIRPVKKKFG-UHFFFAOYSA-N 0.000 claims description 4
- MHABMANUFPZXEB-UHFFFAOYSA-N O-demethyl-aloesaponarin I Natural products O=C1C2=CC=CC(O)=C2C(=O)C2=C1C=C(O)C(C(O)=O)=C2C MHABMANUFPZXEB-UHFFFAOYSA-N 0.000 claims description 4
- PMZURENOXWZQFD-UHFFFAOYSA-L Sodium Sulfate Chemical compound [Na+].[Na+].[O-]S([O-])(=O)=O PMZURENOXWZQFD-UHFFFAOYSA-L 0.000 claims description 4
- 235000019270 ammonium chloride Nutrition 0.000 claims description 4
- 229940113088 dimethylacetamide Drugs 0.000 claims description 4
- XBDQKXXYIPTUBI-UHFFFAOYSA-N dimethylselenoniopropionate Natural products CCC(O)=O XBDQKXXYIPTUBI-UHFFFAOYSA-N 0.000 claims description 4
- BDAGIHXWWSANSR-UHFFFAOYSA-N methanoic acid Natural products OC=O BDAGIHXWWSANSR-UHFFFAOYSA-N 0.000 claims description 4
- 239000001103 potassium chloride Substances 0.000 claims description 4
- 235000011164 potassium chloride Nutrition 0.000 claims description 4
- UMJSCPRVCHMLSP-UHFFFAOYSA-N pyridine Natural products COC1=CC=CN=C1 UMJSCPRVCHMLSP-UHFFFAOYSA-N 0.000 claims description 4
- 239000011780 sodium chloride Substances 0.000 claims description 4
- 239000004317 sodium nitrate Substances 0.000 claims description 4
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- 239000001488 sodium phosphate Substances 0.000 claims description 4
- 229910000162 sodium phosphate Inorganic materials 0.000 claims description 4
- 238000007711 solidification Methods 0.000 claims description 4
- 230000008023 solidification Effects 0.000 claims description 4
- YLQBMQCUIZJEEH-UHFFFAOYSA-N tetrahydrofuran Natural products C=1C=COC=1 YLQBMQCUIZJEEH-UHFFFAOYSA-N 0.000 claims description 4
- RYFMWSXOAZQYPI-UHFFFAOYSA-K trisodium phosphate Chemical compound [Na+].[Na+].[Na+].[O-]P([O-])([O-])=O RYFMWSXOAZQYPI-UHFFFAOYSA-K 0.000 claims description 4
- NQPDZGIKBAWPEJ-UHFFFAOYSA-N valeric acid Chemical compound CCCCC(O)=O NQPDZGIKBAWPEJ-UHFFFAOYSA-N 0.000 claims description 4
- NWZSZGALRFJKBT-KNIFDHDWSA-N (2s)-2,6-diaminohexanoic acid;(2s)-2-hydroxybutanedioic acid Chemical compound OC(=O)[C@@H](O)CC(O)=O.NCCCC[C@H](N)C(O)=O NWZSZGALRFJKBT-KNIFDHDWSA-N 0.000 claims description 3
- RYHBNJHYFVUHQT-UHFFFAOYSA-N 1,4-Dioxane Chemical compound C1COCCO1 RYHBNJHYFVUHQT-UHFFFAOYSA-N 0.000 claims description 3
- SECXISVLQFMRJM-UHFFFAOYSA-N N-Methylpyrrolidone Chemical compound CN1CCCC1=O SECXISVLQFMRJM-UHFFFAOYSA-N 0.000 claims description 3
- IKDUDTNKRLTJSI-UHFFFAOYSA-N hydrazine monohydrate Substances O.NN IKDUDTNKRLTJSI-UHFFFAOYSA-N 0.000 claims description 3
- XMBWDFGMSWQBCA-UHFFFAOYSA-N hydrogen iodide Chemical compound I XMBWDFGMSWQBCA-UHFFFAOYSA-N 0.000 claims description 3
- 229940071870 hydroiodic acid Drugs 0.000 claims description 3
- SMZOUWXMTYCWNB-UHFFFAOYSA-N 2-(2-methoxy-5-methylphenyl)ethanamine Chemical compound COC1=CC=C(C)C=C1CCN SMZOUWXMTYCWNB-UHFFFAOYSA-N 0.000 claims description 2
- NIXOWILDQLNWCW-UHFFFAOYSA-N 2-Propenoic acid Natural products OC(=O)C=C NIXOWILDQLNWCW-UHFFFAOYSA-N 0.000 claims description 2
- OSWFIVFLDKOXQC-UHFFFAOYSA-N 4-(3-methoxyphenyl)aniline Chemical compound COC1=CC=CC(C=2C=CC(N)=CC=2)=C1 OSWFIVFLDKOXQC-UHFFFAOYSA-N 0.000 claims description 2
- KBIWNQVZKHSHTI-UHFFFAOYSA-N 4-n,4-n-dimethylbenzene-1,4-diamine;oxalic acid Chemical compound OC(=O)C(O)=O.CN(C)C1=CC=C(N)C=C1 KBIWNQVZKHSHTI-UHFFFAOYSA-N 0.000 claims description 2
- ZZZCUOFIHGPKAK-UHFFFAOYSA-N D-erythro-ascorbic acid Natural products OCC1OC(=O)C(O)=C1O ZZZCUOFIHGPKAK-UHFFFAOYSA-N 0.000 claims description 2
- MUBZPKHOEPUJKR-UHFFFAOYSA-N Oxalic acid Natural products OC(=O)C(O)=O MUBZPKHOEPUJKR-UHFFFAOYSA-N 0.000 claims description 2
- 229930003268 Vitamin C Natural products 0.000 claims description 2
- 235000011054 acetic acid Nutrition 0.000 claims description 2
- 150000001298 alcohols Chemical class 0.000 claims description 2
- 235000011114 ammonium hydroxide Nutrition 0.000 claims description 2
- 239000003638 chemical reducing agent Substances 0.000 claims description 2
- DQYBDCGIPTYXML-UHFFFAOYSA-N ethoxyethane;hydrate Chemical compound O.CCOCC DQYBDCGIPTYXML-UHFFFAOYSA-N 0.000 claims description 2
- 235000019253 formic acid Nutrition 0.000 claims description 2
- 235000011187 glycerol Nutrition 0.000 claims description 2
- 150000007524 organic acids Chemical class 0.000 claims description 2
- 235000005985 organic acids Nutrition 0.000 claims description 2
- 235000019260 propionic acid Nutrition 0.000 claims description 2
- IUVKMZGDUIUOCP-BTNSXGMBSA-N quinbolone Chemical compound O([C@H]1CC[C@H]2[C@H]3[C@@H]([C@]4(C=CC(=O)C=C4CC3)C)CC[C@@]21C)C1=CCCC1 IUVKMZGDUIUOCP-BTNSXGMBSA-N 0.000 claims description 2
- 239000012279 sodium borohydride Substances 0.000 claims description 2
- 229910000033 sodium borohydride Inorganic materials 0.000 claims description 2
- 229910052938 sodium sulfate Inorganic materials 0.000 claims description 2
- 235000011152 sodium sulphate Nutrition 0.000 claims description 2
- 239000004575 stone Substances 0.000 claims description 2
- 238000001291 vacuum drying Methods 0.000 claims description 2
- 229940005605 valeric acid Drugs 0.000 claims description 2
- 235000019154 vitamin C Nutrition 0.000 claims description 2
- 239000011718 vitamin C Substances 0.000 claims description 2
- BDERNNFJNOPAEC-UHFFFAOYSA-N propan-1-ol Chemical compound CCCO BDERNNFJNOPAEC-UHFFFAOYSA-N 0.000 claims 2
- 239000002253 acid Substances 0.000 claims 1
- 230000008569 process Effects 0.000 abstract description 3
- 239000011230 binding agent Substances 0.000 abstract description 2
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- 239000004744 fabric Substances 0.000 abstract 1
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- 208000012886 Vertigo Diseases 0.000 description 6
- 239000003795 chemical substances by application Substances 0.000 description 4
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- 238000007500 overflow downdraw method Methods 0.000 description 3
- 239000006185 dispersion Substances 0.000 description 2
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- 230000004048 modification Effects 0.000 description 2
- 238000012986 modification Methods 0.000 description 2
- OXHNLMTVIGZXSG-UHFFFAOYSA-N 1-Methylpyrrole Chemical class CN1C=CC=C1 OXHNLMTVIGZXSG-UHFFFAOYSA-N 0.000 description 1
- 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 description 1
- 241000446313 Lamella Species 0.000 description 1
- KDYFGRWQOYBRFD-UHFFFAOYSA-N Succinic acid Natural products OC(=O)CCC(O)=O KDYFGRWQOYBRFD-UHFFFAOYSA-N 0.000 description 1
- 239000000853 adhesive Substances 0.000 description 1
- QVGXLLKOCUKJST-UHFFFAOYSA-N atomic oxygen Chemical compound [O] QVGXLLKOCUKJST-UHFFFAOYSA-N 0.000 description 1
- 230000008901 benefit Effects 0.000 description 1
- KDYFGRWQOYBRFD-NUQCWPJISA-N butanedioic acid Chemical compound O[14C](=O)CC[14C](O)=O KDYFGRWQOYBRFD-NUQCWPJISA-N 0.000 description 1
- 229910052799 carbon Inorganic materials 0.000 description 1
- 235000009508 confectionery Nutrition 0.000 description 1
- 230000007547 defect Effects 0.000 description 1
- 238000010586 diagram Methods 0.000 description 1
- 235000019441 ethanol Nutrition 0.000 description 1
- 229910002804 graphite Inorganic materials 0.000 description 1
- 239000010439 graphite Substances 0.000 description 1
- 150000002576 ketones Chemical class 0.000 description 1
- 238000005259 measurement Methods 0.000 description 1
- 238000001000 micrograph Methods 0.000 description 1
- 229910052760 oxygen Inorganic materials 0.000 description 1
- 239000001301 oxygen Substances 0.000 description 1
- HNJBEVLQSNELDL-UHFFFAOYSA-N pyrrolidin-2-one Chemical compound O=C1CCCN1 HNJBEVLQSNELDL-UHFFFAOYSA-N 0.000 description 1
- 239000011734 sodium Substances 0.000 description 1
- 229910052708 sodium Inorganic materials 0.000 description 1
- 239000000126 substance Substances 0.000 description 1
- 230000008961 swelling Effects 0.000 description 1
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- D06M11/00—Treating fibres, threads, yarns, fabrics or fibrous goods made from such materials, with inorganic substances or complexes thereof; Such treatment combined with mechanical treatment, e.g. mercerising
- D06M11/01—Treating fibres, threads, yarns, fabrics or fibrous goods made from such materials, with inorganic substances or complexes thereof; Such treatment combined with mechanical treatment, e.g. mercerising with hydrogen, water or heavy water; with hydrides of metals or complexes thereof; with boranes, diboranes, silanes, disilanes, phosphines, diphosphines, stibines, distibines, arsines, or diarsines or complexes thereof
- D06M11/05—Treating fibres, threads, yarns, fabrics or fibrous goods made from such materials, with inorganic substances or complexes thereof; Such treatment combined with mechanical treatment, e.g. mercerising with hydrogen, water or heavy water; with hydrides of metals or complexes thereof; with boranes, diboranes, silanes, disilanes, phosphines, diphosphines, stibines, distibines, arsines, or diarsines or complexes thereof with water, e.g. steam; with heavy water
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- D—TEXTILES; PAPER
- D01—NATURAL OR MAN-MADE THREADS OR FIBRES; SPINNING
- D01D—MECHANICAL METHODS OR APPARATUS IN THE MANUFACTURE OF ARTIFICIAL FILAMENTS, THREADS, FIBRES, BRISTLES OR RIBBONS
- D01D5/00—Formation of filaments, threads, or the like
- D01D5/06—Wet spinning methods
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- D01—NATURAL OR MAN-MADE THREADS OR FIBRES; SPINNING
- D01D—MECHANICAL METHODS OR APPARATUS IN THE MANUFACTURE OF ARTIFICIAL FILAMENTS, THREADS, FIBRES, BRISTLES OR RIBBONS
- D01D10/00—Physical treatment of artificial filaments or the like during manufacture, i.e. during a continuous production process before the filaments have been collected
- D01D10/06—Washing or drying
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- D01D5/00—Formation of filaments, threads, or the like
- D01D5/04—Dry spinning methods
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- D01F—CHEMICAL FEATURES IN THE MANUFACTURE OF ARTIFICIAL FILAMENTS, THREADS, FIBRES, BRISTLES OR RIBBONS; APPARATUS SPECIALLY ADAPTED FOR THE MANUFACTURE OF CARBON FILAMENTS
- D01F9/00—Artificial filaments or the like of other substances; Manufacture thereof; Apparatus specially adapted for the manufacture of carbon filaments
- D01F9/08—Artificial filaments or the like of other substances; Manufacture thereof; Apparatus specially adapted for the manufacture of carbon filaments of inorganic material
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- D06M11/07—Treating fibres, threads, yarns, fabrics or fibrous goods made from such materials, with inorganic substances or complexes thereof; Such treatment combined with mechanical treatment, e.g. mercerising with halogens; with halogen acids or salts thereof; with oxides or oxyacids of halogens or salts thereof
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Abstract
本发明公开了一种自融合石墨烯纤维及其制备方法。将干燥的氧化石墨烯纤维浸入溶剂中,溶胀后提出搭接在一起,待其干燥后氧化石墨烯纤维实现了相互融合粘结,进一步还原即可得到自融合石墨烯纤维。自融合的整个过程可在1分钟之内快速完成,不须添加额外的粘结剂,操作简单、省时、环保,粘结强度高,能保持石墨烯纤维本身优异的机械强度、电导率等性能,对进一步制备出具有优异性能的石墨烯纤维二维织物或三维网络块体材料有极大的研究及应用价值。
Description
技术领域
本发明涉及石墨烯纤维,尤其涉及一种自融合石墨烯纤维及其制备方法。
背景技术
石墨烯是一类具有单原子层厚度的碳的同素异形体,具有低密度、极高的力学强度、热导率和电导率,自2004年Geim等人报道以来(Science,2004,306:666-669)引起了广泛关注。石墨烯纤维是由石墨烯片层集成的一维宏观组装体,由于石墨烯本身的优异性能而具有质轻、高的热导率和电导率等性能。目前得到较粗石墨烯纤维的方法一般是利用大直径的纺丝头进行纺丝(Accounts of chemical research,2014,47(4):1267-1276)或将较细的石墨烯纤维集成为丝束(Acta Astronautica,2013,82(2):221-224)。大直径的纺丝头纺丝时由于工艺的缺陷,往往导致石墨烯纤维内外结构差异较大,不易得到具有优良性能的石墨烯纤维。较细的石墨烯纤维集成为丝束时,由于丝束中纤维之间的相互作用较弱,石墨烯纤维本身的优异性在丝束中无法充分体现。
本发明利用墨烯纤维在溶剂中的溶胀作用实现纤维间的快速融合粘结,得到直径增大的自融合石墨烯纤维。相比于融合前的石墨烯纤维,自融合后的石墨烯纤维直径较大,能保持融合前石墨烯纤维本身优异的导电性等功能性。由于制备过程中多根石墨烯纤维并排搭接、融合,因此自融合后的石墨烯纤维表面具有轴向沟槽,导致大的比表面积,有利于对纤维进一步功能化改性,提高改性剂的负载量。且此自融合方法不须添加额外的粘结剂,操作简单、省时、环保,粘结强度高。
发明内容
现有的较粗的石墨烯基纤维制备方法一般是利用大直径的纺丝头进行纺丝或将较细的石墨烯纤维集成为丝束。大直径的纺丝头纺丝时往往导致石墨烯纤维内外结构差异较大,不易得到具有优良性能的石墨烯纤维。较细的石墨烯纤维集成为丝束时,由于丝束中纤维间的相互作用较弱而使纤维本身的优异性无法充分体现。针对该问题,本发明提供一种具有较大直径的自融合石墨烯纤维及其制备方法。
本发明的目的是通过以下技术方案实现的:一种自融合石墨烯纤维,其特征在于,所述自融合石墨烯纤维直径≥1μm,由多根石墨烯纤维融合而成,石墨烯片沿轴向定向排列,片层间距≤1nm,密度≥0.8g/cm3。纤维表面具有轴向沟槽。
进一步地,所述自融合石墨烯纤维直径≥100μm。
进一步地,所述自融合石墨烯纤维直径≥1000μm。
一种自融合石墨烯纤维的制备方法,包括以下步骤:
(1)将氧化石墨烯纤维真空干燥。
(2)将干燥后的纤维在溶剂中浸泡,使纤维被充分浸润溶胀。
(3)将2根或2根以上纤维同时从溶剂中提出,在溶剂-空气界面处,纤维由于受到溶剂的表面张力作用而自发融合。
(4)将自融合的石墨烯纤维干燥后,进行还原,得到高性能的自融合石墨烯纤维。
进一步地,所述步骤(1)中的氧化石墨烯纤维通过干法或湿法纺丝制备得到。其中纺丝液的溶剂为水、N,N-二甲基甲酰胺、N,N-二甲基乙酰胺、四氢呋喃、二甲亚砜、N-甲基吡咯烷酮、乙二醇、二甘醇、吡啶、乙酸乙酯、二氧六环、丁酮、异丙醇等。湿法纺丝的凝固液为氢氧化钠的甲醇溶液、氢氧化钠的乙醇溶液、氢氧化钾的甲醇溶液、氢氧化钾的乙醇溶液、氢氧化钠的水溶液、硫酸钠的水溶液、氯化钠的水溶液、氯化钙的水溶液、硝酸钠的水溶液、硝酸钙的水溶液、磷酸钠的水溶液、氯化钾的水溶液、氯化铵的水溶液、氨水、水乙醚、乙醇、乙酸乙酯、丙酮或这些溶液的混合液。
进一步地,所述真空干燥的温度为室温~100℃,时间为1~10h。
进一步地,步骤(2)中所述的溶剂为:水、甲醇、乙醇、异丙醇、乙二醇、丙三醇、二甘醇等醇类、甲酸、醋酸、丙酸、丁酸、戊酸、乙二酸、丙二酸、丁二酸、丙烯酸等有机酸、丙酮、丁酮、N,N-二甲基甲酰胺、N,N-二甲基乙酰胺、四氢呋喃、二甲亚砜、N-甲基吡咯烷酮、吡啶、二氧六环、氯化钠的水溶液、氯化钙的水溶液、硝酸钠的水溶液、硝酸钙的水溶液、磷酸钠的水溶液、氯化钾的水溶液、氯化铵的水溶液、氢氧化钾的水溶液、氢氧化钠的水溶液或这些溶液的混合液。
进一步地,在溶剂中的浸泡时间≥0.1s。
进一步地,还原方法为使用氢碘酸、水合肼、维他命C、硼氢化钠等化学还原剂进行还原或100~3000℃热还原。
本发明与现有技术相比,具有的优势如下:
(1)利用氧化石墨烯纤维自身的溶胀实现相互融合粘结,方法简单省时,采用的溶剂环保、广泛易得。该融合方法具有很大的应用价值。
(2)利用此制备方法可以任意增大石墨烯纤维的直径,且石墨烯纤维本身的优异性能得以保持。石墨烯纤维自融合后直径增大,内外结构差别几乎不存在,能保持融合前石墨烯纤维优良的力学性能及导电导热等功能性。
(3)自融合后的石墨烯纤维表面具有轴向沟槽,导致大的比表面积,有利于对纤维进行进一步的功能化改性,提高改性剂的负载量。
(4)粘结强度高。石墨烯纤维自融合后在拉伸过程中不滑脱,重新浸泡在溶剂中不散开。
附图说明
图1、图2分别是10根石墨烯纤维自融合后截面和侧面的扫描电子显微镜照片。图1表明自融合石墨烯纤维的内外结构较为均一,图2表明石墨烯纤维间实现了良好的自融合。
图3为纤维在溶剂表面处融合示意图。
具体实施方式
本发明公开了一种自融合石墨烯纤维及其制备方法。利用石墨烯纤维在溶胀状态下自身的相互融合作用实现纤维的融合,得到直径增大的自融合石墨烯纤维。相比于其他方法得到的较粗的纤维,该融合方法得到的较粗纤维内外结构、片层间距较均一,且保持了融合前石墨烯纤维优异的力学性能及导电导热等功能性。
为实现石墨烯纤维的融合,本发明将溶液湿纺得到的氧化石墨烯纤维重新分散在溶剂中,使纤维被浸润溶胀,从而使纤维中的石墨烯片层具有微弱的自由度,能够在搭接后实现接触处片层的重新排列和相互融合,纤维间依靠强的π-π相互作用而粘合,最终得到的自粘结石墨烯纤维保持了粘结前石墨烯纤维的导电导热等性能,解决了粗纤维内外结构差异较大或相互作用较弱导致的纤维性能较差等技术问题,具有很大的实际应用价值。
本发明所述的纤维提出方法,可以为:用镊子夹住多根纤维的一端,将多根纤维一起提出,如图3所示。
下面通过实施例对本发明进行具体描述,本实施例只用于对本发明做进一步的说明,不能理解为对本发明保护范围的限制,本领域的技术人员根据上述发明的内容做出一些非本质的改变和调整,均属于本发明的保护范围。
实施例1:
(1)使用湿法纺丝制备氧化石墨烯纤维。其中氧化石墨烯纤维的分散液为N,N-二甲基甲酰胺,凝固液为乙酸乙酯。
(2)将氧化石墨烯纤维在室温下真空干燥3h。
(3)将步骤(2)得到的纤维在水中浸泡1min,使纤维被充分浸润溶胀。
(4)将10000左右根纤维(计量法)同时从溶剂中提出,在溶剂-空气界面处,10000根左右纤维由于受到溶剂的表面张力作用而自发融合。
(5)将自融合的氧化石墨烯纤维干燥后,使用水合肼还原。
经过以上步骤,多根石墨烯纤维完全融合,形成整体结构。纤维表面具有明显的轴向沟槽,可用于表面负载。融合前石墨烯纤维直径为20μm,力学强度为203MPa;多根石墨烯纤维融合后直径为1120μm,石墨烯片层间距为0.5~0.8nm,结构均一,电导率为285S/m,力学强度为476MPa。
实施例2:
(1)使用湿法纺丝制备氧化石墨烯纤维。其中氧化石墨烯纤维的分散液为水,凝固液为氯化钙的水溶液。
(2)将氧化石墨烯纤维在60℃下真空干燥1h。
(3)将步骤(2)得到的纤维在水中浸泡0.1s,使纤维被充分浸润溶胀。
(4)将100根纤维同时从溶剂中提出,在溶剂-空气界面处,100根纤维由于受到溶剂的表面张力作用而自发融合。
(5)将自融合的氧化石墨烯纤维干燥后,使用氢碘酸还原。
经过以上步骤,100根石墨烯纤维完全融合,形成整体结构。纤维表面具有明显的轴向沟槽,可用于表面负载。融合前石墨烯纤维直径为12μm,力学强度为280MPa;100根石墨烯纤维融合后直径为176μm,石墨烯片层间距为0.7~1nm,结构均一,电导率为1.4×104S/m,力学强度为292MPa。
实施例3:
(1)使用干法纺丝制备氧化石墨烯纤维。
(2)将氧化石墨烯纤维在100℃下真空干燥10h。
(3)将步骤(2)得到的纤维在水和乙醇的混合液(水与乙醇的体积比=3)中浸泡2h,使纤维被充分浸润溶胀。
(4)将4根纤维同时从溶剂中提出,在溶剂-空气界面处,4根纤维由于受到溶剂的表面张力作用而自发融合。
(5)将自融合的氧化石墨烯纤维干燥后,使用硼氢化钠还原。
经过以上步骤,4根石墨烯纤维完全融合,形成整体结构。纤维表面具有明显的轴向沟槽,可用于表面负载。融合前石墨烯纤维直径为18μm,力学强度为242MPa;4根石墨烯纤维融合后直径为32μm,石墨烯片层间距为0.5~0.7nm,结构均一,电导率为448S/m,力学强度为353MPa。
实施例4:
步骤(1)~(2)与实施例3相同。
(3)将步骤(2)得到的纤维在水和乙醇的混合液(水与乙醇的体积比=1)中浸泡2h,使纤维被充分浸润溶胀。
(4)将8根纤维同时从溶剂中提出,在溶剂-空气界面处,8根纤维由于受到溶剂的表面张力作用而自发融合。
(5)将自融合的氧化石墨烯纤维干燥后,进行200℃热还原。
经过以上步骤,8根石墨烯纤维完全融合,形成整体结构。纤维表面具有明显的轴向沟槽,可用于表面负载。融合前石墨烯纤维直径为18μm,力学强度为242MPa;8根石墨烯纤维融合后直径为36μm,石墨烯片层间距为0.6~0.8nm,结构均一,电导率为103S/m,力学强度为326MPa。
实施例5:
步骤(1)~(4)与实施例1相同。
(5)将自融合的氧化石墨烯纤维干燥后,进行3000℃热还原。
经过以上步骤,多根石墨烯纤维完全融合,形成整体结构。纤维表面具有明显的轴向沟槽,可用于表面负载。融合前石墨烯纤维直径为20μm,力学强度为203MPa;多根石墨烯纤维融合后直径为923μm,石墨烯片层间距为0.8~1nm,结构均一,电导率为1.9×105S/m,力学强度为289MPa。
Claims (9)
1.一种自融合石墨烯纤维,其特征在于,所述自融合石墨烯纤维直径≥1μm,由多根石墨烯纤维融合而成,石墨烯片沿轴向定向排列,片层间距≤1nm,密度≥0.8g/cm3。纤维表面具有轴向沟槽。
2.根据权利要求1所述的自融合石墨烯纤维,其特征在于,所述自融合石墨烯纤维直径≥100μm。
3.根据权利要求1所述的自融合石墨烯纤维,其特征在于,所述自融合石墨烯纤维直径≥1000μm。
4.一种自融合石墨烯纤维的制备方法,其特征在于,包括以下步骤:
(1)将氧化石墨烯纤维真空干燥。
(2)将干燥后的纤维在溶剂中浸泡,使纤维被充分浸润溶胀。
(3)将2根或2根以上纤维同时从溶剂中提出,在溶剂-空气界面处,纤维由于受到溶剂的表面张力作用而自发融合。
(4)将自融合的纤维干燥后,进行还原,得到自融合石墨烯纤维。
5.根据权利要求4所述的方法,其特征在于,所述步骤(1)中的氧化石墨烯纤维通过干法或湿法纺丝制备得到。其中纺丝液的溶剂为水、N,N-二甲基甲酰胺、N,N-二甲基乙酰胺、四氢呋喃、二甲亚砜、N-甲基吡咯烷酮、乙二醇、二甘醇、吡啶、乙酸乙酯、二氧六环、丁酮、异丙醇等。湿法纺丝的凝固液为氢氧化钠的甲醇溶液、氢氧化钠的乙醇溶液、氢氧化钾的甲醇溶液、氢氧化钾的乙醇溶液、氢氧化钠的水溶液、硫酸钠的水溶液、氯化钠的水溶液、氯化钙的水溶液、硝酸钠的水溶液、硝酸钙的水溶液、磷酸钠的水溶液、氯化钾的水溶液、氯化铵的水溶液、氨水、水乙醚、乙醇、乙酸乙酯、丙酮或这些溶液的混合液。
6.根据权利要求4所述的方法,其特征在于,所述步骤(1)中真空干燥的温度为室温~100℃,时间为1~10h。
7.根据权利要求4所述的方法,其特征在于,步骤(2)中所述的溶剂为:水、甲醇、乙醇、异丙醇、乙二醇、丙三醇、二甘醇等醇类、甲酸、醋酸、丙酸、丁酸、戊酸、乙二酸、丙二酸、丁二酸、丙烯酸等有机酸、丙酮、丁酮、N,N-二甲基甲酰胺、N,N-二甲基乙酰胺、四氢呋喃、二甲亚砜、N-甲基吡咯烷酮、吡啶、二氧六环、氯化钠的水溶液、氯化钙的水溶液、硝酸钠的水溶液、硝酸钙的水溶液、磷酸钠的水溶液、氯化钾的水溶液、氯化铵的水溶液、氢氧化钾的水溶液、氢氧化钠的水溶液或这些溶液的混合液。
8.根据权利要求4所述的方法,其特征在于,在溶剂中的浸泡时间≥0.1s。
9.根据权利要求4所述的方法,其特征在于,还原方法为使用氢碘酸、水合肼、维他命C、硼氢化钠等化学还原剂进行还原或100~3000℃热还原。
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