CN102452650A - 一种低温化学法制备石墨烯的方法 - Google Patents
一种低温化学法制备石墨烯的方法 Download PDFInfo
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- CN102452650A CN102452650A CN2010105276791A CN201010527679A CN102452650A CN 102452650 A CN102452650 A CN 102452650A CN 2010105276791 A CN2010105276791 A CN 2010105276791A CN 201010527679 A CN201010527679 A CN 201010527679A CN 102452650 A CN102452650 A CN 102452650A
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- BEQZMQXCOWIHRY-UHFFFAOYSA-H dibismuth;trisulfate Chemical compound [Bi+3].[Bi+3].[O-]S([O-])(=O)=O.[O-]S([O-])(=O)=O.[O-]S([O-])(=O)=O BEQZMQXCOWIHRY-UHFFFAOYSA-H 0.000 description 1
- FLWXWKDFOLALOB-UHFFFAOYSA-H dysprosium(3+);trisulfate Chemical compound [Dy+3].[Dy+3].[O-]S([O-])(=O)=O.[O-]S([O-])(=O)=O.[O-]S([O-])(=O)=O FLWXWKDFOLALOB-UHFFFAOYSA-H 0.000 description 1
- 230000005611 electricity Effects 0.000 description 1
- 238000005265 energy consumption Methods 0.000 description 1
- 125000003700 epoxy group Chemical group 0.000 description 1
- YBYGDBANBWOYIF-UHFFFAOYSA-N erbium(3+);trinitrate Chemical compound [Er+3].[O-][N+]([O-])=O.[O-][N+]([O-])=O.[O-][N+]([O-])=O YBYGDBANBWOYIF-UHFFFAOYSA-N 0.000 description 1
- SYDXSHCNMKOQFW-UHFFFAOYSA-H erbium(3+);trisulfate Chemical compound [Er+3].[Er+3].[O-]S([O-])(=O)=O.[O-]S([O-])(=O)=O.[O-]S([O-])(=O)=O SYDXSHCNMKOQFW-UHFFFAOYSA-H 0.000 description 1
- HDGGAKOVUDZYES-UHFFFAOYSA-K erbium(iii) chloride Chemical compound Cl[Er](Cl)Cl HDGGAKOVUDZYES-UHFFFAOYSA-K 0.000 description 1
- GAGGCOKRLXYWIV-UHFFFAOYSA-N europium(3+);trinitrate Chemical compound [Eu+3].[O-][N+]([O-])=O.[O-][N+]([O-])=O.[O-][N+]([O-])=O GAGGCOKRLXYWIV-UHFFFAOYSA-N 0.000 description 1
- NNMXSTWQJRPBJZ-UHFFFAOYSA-K europium(iii) chloride Chemical compound Cl[Eu](Cl)Cl NNMXSTWQJRPBJZ-UHFFFAOYSA-K 0.000 description 1
- WLYAEQLCCOGBPV-UHFFFAOYSA-N europium;sulfuric acid Chemical compound [Eu].OS(O)(=O)=O WLYAEQLCCOGBPV-UHFFFAOYSA-N 0.000 description 1
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- 229960002089 ferrous chloride Drugs 0.000 description 1
- 235000003891 ferrous sulphate Nutrition 0.000 description 1
- 239000011790 ferrous sulphate Substances 0.000 description 1
- 230000005669 field effect Effects 0.000 description 1
- MEANOSLIBWSCIT-UHFFFAOYSA-K gadolinium trichloride Chemical compound Cl[Gd](Cl)Cl MEANOSLIBWSCIT-UHFFFAOYSA-K 0.000 description 1
- QLAFITOLRQQGTE-UHFFFAOYSA-H gadolinium(3+);trisulfate Chemical compound [Gd+3].[Gd+3].[O-]S([O-])(=O)=O.[O-]S([O-])(=O)=O.[O-]S([O-])(=O)=O QLAFITOLRQQGTE-UHFFFAOYSA-H 0.000 description 1
- MWFSXYMZCVAQCC-UHFFFAOYSA-N gadolinium(iii) nitrate Chemical compound [Gd+3].[O-][N+]([O-])=O.[O-][N+]([O-])=O.[O-][N+]([O-])=O MWFSXYMZCVAQCC-UHFFFAOYSA-N 0.000 description 1
- 239000007770 graphite material Substances 0.000 description 1
- 150000002431 hydrogen Chemical class 0.000 description 1
- RXPAJWPEYBDXOG-UHFFFAOYSA-N hydron;methyl 4-methoxypyridine-2-carboxylate;chloride Chemical compound Cl.COC(=O)C1=CC(OC)=CC=N1 RXPAJWPEYBDXOG-UHFFFAOYSA-N 0.000 description 1
- 229910017053 inorganic salt Inorganic materials 0.000 description 1
- NMCUIPGRVMDVDB-UHFFFAOYSA-L iron dichloride Chemical compound Cl[Fe]Cl NMCUIPGRVMDVDB-UHFFFAOYSA-L 0.000 description 1
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- RUTXIHLAWFEWGM-UHFFFAOYSA-H iron(3+) sulfate Chemical compound [Fe+3].[Fe+3].[O-]S([O-])(=O)=O.[O-]S([O-])(=O)=O.[O-]S([O-])(=O)=O RUTXIHLAWFEWGM-UHFFFAOYSA-H 0.000 description 1
- 229910000359 iron(II) sulfate Inorganic materials 0.000 description 1
- JEIPFZHSYJVQDO-UHFFFAOYSA-N iron(III) oxide Inorganic materials O=[Fe]O[Fe]=O JEIPFZHSYJVQDO-UHFFFAOYSA-N 0.000 description 1
- 229910000360 iron(III) sulfate Inorganic materials 0.000 description 1
- FYDKNKUEBJQCCN-UHFFFAOYSA-N lanthanum(3+);trinitrate Chemical compound [La+3].[O-][N+]([O-])=O.[O-][N+]([O-])=O.[O-][N+]([O-])=O FYDKNKUEBJQCCN-UHFFFAOYSA-N 0.000 description 1
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- 239000010410 layer Substances 0.000 description 1
- RLJMLMKIBZAXJO-UHFFFAOYSA-N lead nitrate Chemical compound [O-][N+](=O)O[Pb]O[N+]([O-])=O RLJMLMKIBZAXJO-UHFFFAOYSA-N 0.000 description 1
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- 239000011702 manganese sulphate Substances 0.000 description 1
- MIVBAHRSNUNMPP-UHFFFAOYSA-N manganese(2+);dinitrate Chemical compound [Mn+2].[O-][N+]([O-])=O.[O-][N+]([O-])=O MIVBAHRSNUNMPP-UHFFFAOYSA-N 0.000 description 1
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- 238000004377 microelectronic Methods 0.000 description 1
- 239000002086 nanomaterial Substances 0.000 description 1
- CFYGEIAZMVFFDE-UHFFFAOYSA-N neodymium(3+);trinitrate Chemical compound [Nd+3].[O-][N+]([O-])=O.[O-][N+]([O-])=O.[O-][N+]([O-])=O CFYGEIAZMVFFDE-UHFFFAOYSA-N 0.000 description 1
- RHVPCSSKNPYQDU-UHFFFAOYSA-H neodymium(3+);trisulfate;hydrate Chemical compound O.[Nd+3].[Nd+3].[O-]S([O-])(=O)=O.[O-]S([O-])(=O)=O.[O-]S([O-])(=O)=O RHVPCSSKNPYQDU-UHFFFAOYSA-H 0.000 description 1
- ATINCSYRHURBSP-UHFFFAOYSA-K neodymium(iii) chloride Chemical compound Cl[Nd](Cl)Cl ATINCSYRHURBSP-UHFFFAOYSA-K 0.000 description 1
- QMMRZOWCJAIUJA-UHFFFAOYSA-L nickel dichloride Chemical compound Cl[Ni]Cl QMMRZOWCJAIUJA-UHFFFAOYSA-L 0.000 description 1
- AMDUMQZTBRMNMG-UHFFFAOYSA-N nickel nitric acid Chemical compound [Ni].O[N+]([O-])=O AMDUMQZTBRMNMG-UHFFFAOYSA-N 0.000 description 1
- LGQLOGILCSXPEA-UHFFFAOYSA-L nickel sulfate Chemical compound [Ni+2].[O-]S([O-])(=O)=O LGQLOGILCSXPEA-UHFFFAOYSA-L 0.000 description 1
- 229910000363 nickel(II) sulfate Inorganic materials 0.000 description 1
- 239000007800 oxidant agent Substances 0.000 description 1
- PIBWKRNGBLPSSY-UHFFFAOYSA-L palladium(II) chloride Chemical compound Cl[Pd]Cl PIBWKRNGBLPSSY-UHFFFAOYSA-L 0.000 description 1
- GPNDARIEYHPYAY-UHFFFAOYSA-N palladium(ii) nitrate Chemical compound [Pd+2].[O-][N+]([O-])=O.[O-][N+]([O-])=O GPNDARIEYHPYAY-UHFFFAOYSA-N 0.000 description 1
- RPESBQCJGHJMTK-UHFFFAOYSA-I pentachlorovanadium Chemical compound [Cl-].[Cl-].[Cl-].[Cl-].[Cl-].[V+5] RPESBQCJGHJMTK-UHFFFAOYSA-I 0.000 description 1
- 230000000704 physical effect Effects 0.000 description 1
- YWECOPREQNXXBZ-UHFFFAOYSA-N praseodymium(3+);trinitrate Chemical compound [Pr+3].[O-][N+]([O-])=O.[O-][N+]([O-])=O.[O-][N+]([O-])=O YWECOPREQNXXBZ-UHFFFAOYSA-N 0.000 description 1
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- HWZAHTVZMSRSJE-UHFFFAOYSA-H praseodymium(iii) sulfate Chemical compound [Pr+3].[Pr+3].[O-]S([O-])(=O)=O.[O-]S([O-])(=O)=O.[O-]S([O-])(=O)=O HWZAHTVZMSRSJE-UHFFFAOYSA-H 0.000 description 1
- 230000001681 protective effect Effects 0.000 description 1
- 230000035484 reaction time Effects 0.000 description 1
- 230000009257 reactivity Effects 0.000 description 1
- 229910052707 ruthenium Inorganic materials 0.000 description 1
- YZDZYSPAJSPJQJ-UHFFFAOYSA-N samarium(3+);trinitrate Chemical compound [Sm+3].[O-][N+]([O-])=O.[O-][N+]([O-])=O.[O-][N+]([O-])=O YZDZYSPAJSPJQJ-UHFFFAOYSA-N 0.000 description 1
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- BHXBZLPMVFUQBQ-UHFFFAOYSA-K samarium(iii) chloride Chemical compound Cl[Sm](Cl)Cl BHXBZLPMVFUQBQ-UHFFFAOYSA-K 0.000 description 1
- 239000000523 sample Substances 0.000 description 1
- 235000010344 sodium nitrate Nutrition 0.000 description 1
- 239000004317 sodium nitrate Substances 0.000 description 1
- 238000000967 suction filtration Methods 0.000 description 1
- 150000003467 sulfuric acid derivatives Chemical class 0.000 description 1
- YJVUGDIORBKPLC-UHFFFAOYSA-N terbium(3+);trinitrate Chemical compound [Tb+3].[O-][N+]([O-])=O.[O-][N+]([O-])=O.[O-][N+]([O-])=O YJVUGDIORBKPLC-UHFFFAOYSA-N 0.000 description 1
- UFPWIQQSPQSOKM-UHFFFAOYSA-H terbium(3+);trisulfate Chemical compound [Tb+3].[Tb+3].[O-]S([O-])(=O)=O.[O-]S([O-])(=O)=O.[O-]S([O-])(=O)=O UFPWIQQSPQSOKM-UHFFFAOYSA-H 0.000 description 1
- GFISHBQNVWAVFU-UHFFFAOYSA-K terbium(iii) chloride Chemical compound Cl[Tb](Cl)Cl GFISHBQNVWAVFU-UHFFFAOYSA-K 0.000 description 1
- RBTVSNLYYIMMKS-UHFFFAOYSA-N tert-butyl 3-aminoazetidine-1-carboxylate;hydrochloride Chemical compound Cl.CC(C)(C)OC(=O)N1CC(N)C1 RBTVSNLYYIMMKS-UHFFFAOYSA-N 0.000 description 1
- LLZBVBSJCNUKLL-UHFFFAOYSA-N thulium(3+);trinitrate Chemical compound [Tm+3].[O-][N+]([O-])=O.[O-][N+]([O-])=O.[O-][N+]([O-])=O LLZBVBSJCNUKLL-UHFFFAOYSA-N 0.000 description 1
- NEEAOWXTIOQDFM-UHFFFAOYSA-H thulium(3+);trisulfate Chemical compound [Tm+3].[Tm+3].[O-]S([O-])(=O)=O.[O-]S([O-])(=O)=O.[O-]S([O-])(=O)=O NEEAOWXTIOQDFM-UHFFFAOYSA-H 0.000 description 1
- ILOTUXNTERMOJL-UHFFFAOYSA-K thulium(iii) chloride Chemical compound Cl[Tm](Cl)Cl ILOTUXNTERMOJL-UHFFFAOYSA-K 0.000 description 1
- FAKFSJNVVCGEEI-UHFFFAOYSA-J tin(4+);disulfate Chemical compound [Sn+4].[O-]S([O-])(=O)=O.[O-]S([O-])(=O)=O FAKFSJNVVCGEEI-UHFFFAOYSA-J 0.000 description 1
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- 231100000331 toxic Toxicity 0.000 description 1
- 230000002588 toxic effect Effects 0.000 description 1
- KAKNBYVEBALXNX-UHFFFAOYSA-K trichloropromethium Chemical compound [Cl-].[Cl-].[Cl-].[Pm+3] KAKNBYVEBALXNX-UHFFFAOYSA-K 0.000 description 1
- YQMWDQQWGKVOSQ-UHFFFAOYSA-N trinitrooxystannyl nitrate Chemical compound [Sn+4].[O-][N+]([O-])=O.[O-][N+]([O-])=O.[O-][N+]([O-])=O.[O-][N+]([O-])=O YQMWDQQWGKVOSQ-UHFFFAOYSA-N 0.000 description 1
- VLOPEOIIELCUML-UHFFFAOYSA-L vanadium(2+);sulfate Chemical compound [V+2].[O-]S([O-])(=O)=O VLOPEOIIELCUML-UHFFFAOYSA-L 0.000 description 1
- KUBYTSCYMRPPAG-UHFFFAOYSA-N ytterbium(3+);trinitrate Chemical compound [Yb+3].[O-][N+]([O-])=O.[O-][N+]([O-])=O.[O-][N+]([O-])=O KUBYTSCYMRPPAG-UHFFFAOYSA-N 0.000 description 1
- KVCOOBXEBNBTGL-UHFFFAOYSA-H ytterbium(3+);trisulfate Chemical compound [Yb+3].[Yb+3].[O-]S([O-])(=O)=O.[O-]S([O-])(=O)=O.[O-]S([O-])(=O)=O KVCOOBXEBNBTGL-UHFFFAOYSA-H 0.000 description 1
- CKLHRQNQYIJFFX-UHFFFAOYSA-K ytterbium(III) chloride Chemical compound [Cl-].[Cl-].[Cl-].[Yb+3] CKLHRQNQYIJFFX-UHFFFAOYSA-K 0.000 description 1
- 235000005074 zinc chloride Nutrition 0.000 description 1
- 239000011592 zinc chloride Substances 0.000 description 1
- 229960001939 zinc chloride Drugs 0.000 description 1
- NWONKYPBYAMBJT-UHFFFAOYSA-L zinc sulfate Chemical compound [Zn+2].[O-]S([O-])(=O)=O NWONKYPBYAMBJT-UHFFFAOYSA-L 0.000 description 1
- 229910000368 zinc sulfate Inorganic materials 0.000 description 1
- 229960001763 zinc sulfate Drugs 0.000 description 1
- DUNKXUFBGCUVQW-UHFFFAOYSA-J zirconium tetrachloride Chemical compound Cl[Zr](Cl)(Cl)Cl DUNKXUFBGCUVQW-UHFFFAOYSA-J 0.000 description 1
- ZXAUZSQITFJWPS-UHFFFAOYSA-J zirconium(4+);disulfate Chemical compound [Zr+4].[O-]S([O-])(=O)=O.[O-]S([O-])(=O)=O ZXAUZSQITFJWPS-UHFFFAOYSA-J 0.000 description 1
Classifications
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- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01B—NON-METALLIC ELEMENTS; COMPOUNDS THEREOF; METALLOIDS OR COMPOUNDS THEREOF NOT COVERED BY SUBCLASS C01C
- C01B32/00—Carbon; Compounds thereof
- C01B32/15—Nano-sized carbon materials
- C01B32/182—Graphene
- C01B32/198—Graphene oxide
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01J—CHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
- B01J21/00—Catalysts comprising the elements, oxides, or hydroxides of magnesium, boron, aluminium, carbon, silicon, titanium, zirconium, or hafnium
- B01J21/02—Boron or aluminium; Oxides or hydroxides thereof
- B01J21/04—Alumina
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01J—CHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
- B01J27/00—Catalysts comprising the elements or compounds of halogens, sulfur, selenium, tellurium, phosphorus or nitrogen; Catalysts comprising carbon compounds
- B01J27/06—Halogens; Compounds thereof
- B01J27/08—Halides
- B01J27/10—Chlorides
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- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01B—NON-METALLIC ELEMENTS; COMPOUNDS THEREOF; METALLOIDS OR COMPOUNDS THEREOF NOT COVERED BY SUBCLASS C01C
- C01B32/00—Carbon; Compounds thereof
- C01B32/15—Nano-sized carbon materials
- C01B32/182—Graphene
- C01B32/184—Preparation
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- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01B—NON-METALLIC ELEMENTS; COMPOUNDS THEREOF; METALLOIDS OR COMPOUNDS THEREOF NOT COVERED BY SUBCLASS C01C
- C01B2204/00—Structure or properties of graphene
- C01B2204/20—Graphene characterized by its properties
- C01B2204/22—Electronic properties
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- Chemical & Material Sciences (AREA)
- Organic Chemistry (AREA)
- Engineering & Computer Science (AREA)
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- Chemical Kinetics & Catalysis (AREA)
- Nanotechnology (AREA)
- Inorganic Chemistry (AREA)
- Carbon And Carbon Compounds (AREA)
- Catalysts (AREA)
Abstract
本发明公开了属于石墨烯的化学合成技术领域的一种低温化学法制备石墨烯的方法，该方法以化学氧化制备的石墨烯氧化物为原料，包括将石墨烯氧化物还原成石墨烯的还原反应步骤，所述还原反应步骤以硼氢化钠为还原剂，通过催化剂的辅助，在80℃～150℃的温度下实现对石墨烯氧化物的还原，将石墨烯氧化物上面的含氧官能团(环氧、羟基、羧基及羰基)去除，较彻底恢复石墨烯的导电性，制得石墨烯。本发明的方法为一种适合于大规模工业化生产的低温化学法制备石墨烯的方法。该方法具有还原温度低，反应温和可控，还原更彻底，对环境友好，适合工业化生产等优点。
Description
技术领域
本发明属于石墨烯的化学合成技术领域，特别涉及一种低温化学法制备石墨烯的方法，具体为具有单个碳原子厚度的石墨纳米材料的低温催化还原制备方法。用该方法制备的石墨烯可广泛用于微电子器件、传感器及新能源材料等领域。
背景技术
石墨烯是英国科学家在2004年发现的具有一个碳原子厚度的片状石墨材料。由于石墨烯的长程π共轭键的作用，使其在电学、力学、热学具有十分优异的性能，将是一种用途十分广泛的新材料，是目前的一个研究热点。
目前石墨烯的制备方法主要有机械剥离法、化学气相沉积法、外延生长法、化学氧化还原法。机械剥离法是最早用来制备石墨烯的方法，它是把石墨片放在两个平面之间，然后两个平面相互摩擦，可以制备出结构非常接近原石墨层结构的石墨烯片并广泛用于其基本物理性质(电导率、热导率、弹性模量、硬度等)的研究。但机械剥离法由于剥离方法的局限性，其不适合大规模工业化制备石墨烯。化学气相沉积法是在单晶或多晶Ni、Cu、Ru等基板上沉积出石墨烯。化学气相沉积法虽然可以大规模制备石墨烯，但由于其所用设备和基板材料均较昂贵，这会大大提高其大规模工业化生产的成本。外延生长法是利用单晶SiC、Ru等单晶体的某一个晶面作为生长面，在超高真空条件下生长石墨烯。外延生长法由于使用单晶SiC作为基板且需要超高真空的苛刻条件，因此此法较难实现大规模工业化生产，即使生产，其成本也会很高。化学氧化还原法制备石墨烯分两步：第一步是制备石墨烯氧化物。具体步骤是首先用浓硫酸、高锰酸钾、双氧水、过氧化苯甲酰(BPO)等强氧化剂将石墨氧化成石墨氧化物。石墨氧化物是在石墨单层上引入环氧、羟基、羰基及羧基等含氧官能团后，石墨单层层间距扩大的氧化石墨。将此石墨氧化物超声分散或加热膨胀即可获得石墨烯氧化物。第二步是还原石墨烯氧化物，即将石墨烯氧化物表面上的含氧官能团去除。常用的还原方法有高温还原法、还原剂还原法及二者的复合还原。化学氧化还原法工艺简单，不需要精密而昂贵的设备，是一种适合大规模工业化生产的方法。
化学还原法中的高温还原法是将石墨烯氧化物在有保护气体(氩气)和还原气体(氢气)的混合气氛中加热到1000℃左右，利用高温及氢气将石墨烯氧化物上的含氧官能团去除，从而制得石墨烯。高温还原法虽然还原效果很好，但高温耗能大，设备复杂，还原基板需要耐高温，这样大大限制了它的使用范围。还原剂还原法是一种可以实现石墨烯氧化物低温还原的有效方法。常用的还原剂有硼氢化钠(NaBH4)、肼(N2H4)及其衍生物、氢化钠(NaH)等。国内外许多研究者用此方法制备石墨烯。新加坡南阳理工大学的陈鹏用肼作为还原剂，在80℃还原石墨烯氧化物24小时，然后再将其在含有20％氢气的氩气气氛中，在400℃、800℃及1000℃进一步还原，得到石墨烯。最后用制备出的石墨烯制作了场效应晶体管，测试发现只用N2H4还原的石墨烯制备出的晶体管的空穴迁移率比1000℃还原的石墨烯制备出的低约两个数量级。这说明肼的还原效果不是太好。美国莱斯大学的M.Ajayan用NaBH4在80℃还原石墨烯氧化物1小时，测得其电导率只有82.3S m-1，与多晶石墨的电导率105S m-1相去甚远。美国堪萨斯州立大学的Vikas Berry用NaH在甲醇溶液中还原石墨烯氧化物，反应很剧烈很快(不到1分钟)并有大量氢气产生，制得的石墨烯的导电率在4500～10625S m-1。综合这些研究可以发现，石墨烯氧化物还原这一步是化学氧化还原法制备石墨烯的关键，而现有的还原剂还原法均存在还原不彻底的问题。另外，有机还原剂肼及其衍生物毒性很大，不是一种环境友好的还原剂。而氢化钠等反应活性又太高，致使还原反应过于剧烈而不易控制。对于实现石墨烯的大规模制备，需要一种温和可控且对环境友好的可在较低温度实现石墨烯氧化物还原的方法。
发明内容
本发明的目的是提供一种低温化学还原制备石墨烯的方法，该方法以化学氧化制备的石墨烯氧化物为原料，包括将石墨烯氧化物还原成石墨烯的还原反应步骤，所述还原反应以硼氢化钠为还原剂，通过催化剂的辅助，在80℃～150℃的温度下将石墨烯氧化物还原成石墨烯。其中，还原反应的温度优选140℃。
进一步的，上述还原反应步骤中，硼氢化钠与石墨烯氧化物的质量比可以为1∶0.12，所述催化剂与石墨烯氧化物的质量比可以为7∶12。
上述还原反应步骤中，还原反应的时间(加热的时间)范围可以是0.25～3小时，最好是3小时。
进一步的，本发明还给出了上述还原反应步骤中优选的催化剂，所用催化剂可以为以下物质中的一种或多种：铝、镍、铁(包括二价铁和三价铁)、铜、锌、锆、钴(包括二价钴和三价钴)、钯、铋、铅、锡、锰、钒、铬、锂或者稀土的氯化物、硝酸盐或者硫酸盐。上述物质不含结晶水或者含有结晶水。
所述的稀土包括镧、铈、镨、钕、钷、钐、铕、钆、铽、镝、鈥、铒、铥、镱或者镥中的一种或几种。
具体为：所用催化剂可以为以下物质中的一种或多种：氯化铝、氯化镍、氯化铁、氯化亚铁、氯化铜、氯化亚铜、氯化锌、氯化锆、氯化钴、氯化亚钴、氯化钯、氯化铋、氯化锡、氯化铅、氯化锰、氯化钒、氯化铬、氯化铝、氯化锂、硝酸铝、硝酸镍、硝酸铁、硝酸亚铁、硝酸铜、硝酸亚铜、硝酸锌、硝酸锆、硝酸钴、硝酸亚钴、硝酸钯、硝酸铋、硝酸铅、硝酸锡、硝酸锰、硝酸钒、硝酸铬、硝酸锂、硫酸铝、硫酸镍、硫酸铁、硫酸亚铁、硫酸铜、硫酸亚铜、硫酸锌、硫酸锆、硫酸钴、硫酸亚钴、硫酸钯、硫酸铋、硫酸铅、硫酸锡、硫酸锰、硫酸钒、硫酸铬、硫酸锂、稀土氯化物(氯化镧、氯化铈、氯化镨、氯化钕、氯化钷、氯化钐、氯化铕、氯化钆、氯化铽、氯化镝、氯化鈥、氯化铒、氯化铥、氯化镱、氯化镥)、稀土硝酸盐(硝酸镧、硝酸铈、硝酸镨、硝酸钕、硝酸钷、硝酸钐、硝酸铕、硝酸钆、硝酸铽、硝酸镝、硝酸鈥、硝酸铒、硝酸铥、硝酸镱、硝酸镥)、稀土硫酸盐(硫酸镧、硫酸铈、硫酸镨、硫酸钕、硫酸钷、硫酸钐、硫酸铕、硫酸钆、硫酸铽、硫酸镝、硫酸鈥、硫酸铒、硫酸铥、硫酸镱、硫酸镥)，上述物质不含结晶水或者含有结晶水。
该方法具体工艺过程如下：
(1)首先以化学氧化制备的石墨烯氧化物溶解在溶剂中，超声使其在溶剂中均匀分散；
(2)将还原剂硼氢化钠溶解在溶剂中，超声使其完全溶解；
(3)将催化剂溶解在溶剂中，超声使其完全溶解；
(4)将步骤(1)制备的含有石墨烯氧化物的溶剂、步骤(2)制备的含有硼氢化钠的溶剂以及步骤(3)制备的含有催化剂的溶剂混合均匀，得到混合溶液；
(5)在搅拌条件下加热步骤(4)制备的混合溶液，使石墨烯氧化物还原成石墨烯。
在上述步骤(1)、步骤(2)和步骤(3)中，所用的溶剂可以为水，N-甲基吡咯烷酮(NMP)，N-乙基吡咯烷酮(NEP)，N，N-二甲基甲酰胺(DMF)，异丙醇，丙酮，甲醇，乙烯二醇，二甲基乙酰胺(DMA)，二甲亚砜(DMSO)，氯仿，二苄醚，乙醇中的一种或多种。
上述还原反应步骤中，所用搅拌方式可以是磁力搅拌或者机械搅拌；加热的方式可以是水浴加热、油浴加热、微波加热或者超声加热。
本发明的方法以化学氧化制备的石墨烯氧化物为原料，以硼氢化钠为还原剂，通过加入适量的催化剂，辅助硼氢化钠将石墨烯氧化物上面的含氧官能团(环氧、羟基、羧基及羰基)去除，较彻底恢复石墨烯的导电性。
本发明的有益效果为：本发明采用的是以对环境友好的无机盐硼氢化钠为还原剂，通过催化剂的辅助在较低的温度下实现对石墨烯氧化物的还原，从而制得石墨烯。总体上来说，本发明的优点是还原方法简单，还原温度低，耗能小，拓宽了化学氧化还原法制备石墨烯的应用范围，成本低廉，对环境友好。
本发明的方法为一种适合于大规模工业化生产的低温化学法制备石墨烯的方法。该方法具有还原温度低，反应温和可控，还原更彻底，对环境友好，适合工业化生产等优点，采用本方法制备的石墨烯的电导率可达50～820S/m。
具体实施方式
以下结合实例进一步阐明本发明的特点，但不局限于实例。
实例中所用石墨烯氧化物的制备方法：将3g石墨粉，3g硝酸钠和138ml浓硫酸冰浴混匀；然后缓慢加入18g高锰酸钾，磁力搅拌混匀后在35℃水浴中加热1h；接着加入240ml去离子水并在90℃加热0.5h，加热结束后加入600ml去离子水和18ml双氧水。
采用抽滤的方法将还原得到的石墨烯制备成石墨烯膜，然后用台阶仪测石墨烯膜的膜厚，四探针法测其电导率。
实施例1
将120mg石墨烯氧化物(GO)分散在200ml N，N-二甲基甲酰胺(DMF)中，1g硼氢化钠溶解在25ml DMF中，0.07g无水氯化铝溶解在25ml DMF中。然后将三种溶液混合，在磁力搅拌下在140℃还原3h。
测试结果为：石墨烯膜的电导率为820S/m。
在不同催化剂催化条件下，改变还原温度和还原时间，其它条件不变的前提下，得到的其它石墨烯的电导率如下表所示：
对比例1
将120mg石墨烯氧化物(GO)分散在200ml N，N-二甲基甲酰胺(DMF)中，1g硼氢化钠溶解在25ml DMF中。然后将两种溶液混合，在磁力搅拌下在140℃还原3h。
测试结果为：石墨烯膜的电导率为130S/m。
通过对比实施例1与对比例1的石墨烯膜的电导率，可知催化剂采用无水AlCl3将石墨烯膜的电导率提高了6倍多，采用无水AlCl3辅助硼氢化钠催化还原石墨烯氧化物，能得到效果较好的石墨烯。
Claims (10)
1.一种低温化学法制备石墨烯的方法，该方法以化学氧化制备的石墨烯氧化物为原料，包括将石墨烯氧化物还原成石墨烯的还原反应步骤，其特征在于：所述还原反应以硼氢化钠为还原剂，通过催化剂的辅助，在80℃～150℃的温度下将石墨烯氧化物还原成石墨烯。
2.根据权利要求1所述的低温化学法制备石墨烯的方法，其特征在于：所述还原反应的温度为140℃。
3.根据权利要求1所述的低温化学法制备石墨烯的方法，其特征在于：所述还原反应步骤中，硼氢化钠与石墨烯氧化物的质量比是1∶0.12。
4.根据权利要求1所述的低温化学法制备石墨烯的方法，其特征在于：所述催化剂与石墨烯氧化物的质量比是7∶12。
5.根据权利要求1所述的低温化学法制备石墨烯的方法，其特征在于：所述还原反应步骤中，还原反应的时间是0.25～3小时。
6.根据权利要求1所述的低温化学法制备石墨烯的方法，其特征在于：所述催化剂为以下物质中的一种或多种：铝、镍、铁、铜、锌、锆、钴、钯、铋、铅、锡、锰、钒、铬、锂或者稀土的氯化物、硝酸盐或者硫酸盐，上述物质不含结晶水或者含有结晶水。
7.根据权利要求1所述的低温化学法制备石墨烯的方法，其特征在于：所述的稀土包括镧、铈、镨、钕、钷、钐、铕、钆、铽、镝、鈥、铒、铥、镱或者镥中的一种或几种。
8.根据权利要求1所述的低温化学法制备石墨烯的方法，其特征在于：该方法具体工艺过程如下：
(1)首先以化学氧化制备的石墨烯氧化物溶解在溶剂中，超声使其在溶剂中均匀分散；
(2)将还原剂硼氢化钠溶解在溶剂中，超声使其完全溶解；
(3)将催化剂溶解在溶剂中，超声使其完全溶解；
(4)将步骤(1)制备的含有石墨烯氧化物的溶剂、步骤(2)制备的含有硼氢化钠的溶剂以及步骤(3)制备的含有催化剂的溶剂混合均匀，得到混合溶液；
(5)在搅拌条件下加热步骤(4)制备的混合溶液，使石墨烯氧化物还原成石墨烯。
9.根据权利要求8所述的低温化学法制备石墨烯的方法，其特征在于：在所述步骤(1)、步骤(2)和步骤(3)中，所用的溶剂为水，N-甲基吡咯烷酮(NMP)，N-乙基吡咯烷酮(NEP)，N，N-二甲基甲酰胺(DMF)，异丙醇，丙酮，甲醇，乙烯二醇，二甲基乙酰胺(DMA)，二甲亚砜(DMSO)，氯仿，二苄醚，乙醇中的一种或多种。
10.根据权利要求8所述的低温化学法制备石墨烯的方法，其特征在于：所用搅拌方式是磁力搅拌或者机械搅拌；所述加热的方式是水浴加热、油浴加热、微波加热或者超声加热。
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| CN103011147A (zh) * | 2012-12-27 | 2013-04-03 | 中南大学 | 一种热还原制备石墨烯的方法 |
| CN103241734A (zh) * | 2013-05-17 | 2013-08-14 | 上海理工大学 | 一种氧化石墨烯的还原方法 |
| CN103241734B (zh) * | 2013-05-17 | 2014-11-26 | 上海理工大学 | 一种氧化石墨烯的还原方法 |
| CN103964425A (zh) * | 2014-05-15 | 2014-08-06 | 河南大学 | 一种超声辐射快速制备石墨烯的方法 |
| CN105129779A (zh) * | 2015-07-30 | 2015-12-09 | 复旦大学 | 一种超级电容器电极用高性能还原石墨烯的制备方法 |
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| CN112010298A (zh) * | 2020-08-14 | 2020-12-01 | 兰州大学 | 一种快速高效宏量制备大片径氧化石墨烯的方法 |
| CN112195038A (zh) * | 2020-11-03 | 2021-01-08 | 四川润和催化新材料股份有限公司 | 一种原油处理剂及其制备方法 |
| CN114276850A (zh) * | 2021-12-24 | 2022-04-05 | 安徽工业大学 | 一种氟掺杂石墨烯负载Pb复合材料及其制备方法和应用 |
| CN114276850B (zh) * | 2021-12-24 | 2023-02-07 | 安徽工业大学 | 一种氟掺杂石墨烯负载Pb复合材料及其制备方法和应用 |
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