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WO2011066811A1 - Procédés d'obtention d'un graphène flg et d'un film de graphène flg - Google Patents

Procédés d'obtention d'un graphène flg et d'un film de graphène flg Download PDF

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Publication number
WO2011066811A1
WO2011066811A1 PCT/CN2010/079477 CN2010079477W WO2011066811A1 WO 2011066811 A1 WO2011066811 A1 WO 2011066811A1 CN 2010079477 W CN2010079477 W CN 2010079477W WO 2011066811 A1 WO2011066811 A1 WO 2011066811A1
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Prior art keywords
graphite
anode
oligo
mpa
gas
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Ceased
Application number
PCT/CN2010/079477
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English (en)
Chinese (zh)
Inventor
陈永胜
吴英鹏
张龙
黄毅
Current Assignee (The listed assignees may be inaccurate. Google has not performed a legal analysis and makes no representation or warranty as to the accuracy of the list.)
Nankai University
Tianjin Pulan Nano Technology Co Ltd
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Nankai University
Tianjin Pulan Nano Technology Co Ltd
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Priority to CN201080062867.XA priority Critical patent/CN102781831B/zh
Publication of WO2011066811A1 publication Critical patent/WO2011066811A1/fr
Anticipated expiration legal-status Critical
Ceased legal-status Critical Current

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    • 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
    • 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
    • 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
    • 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
    • C01B32/194—After-treatment
    • 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
    • C01B2204/04—Specific amount of layers or specific thickness

Definitions

  • the present application relates to carbon materials and methods for their preparation, and in particular to a process for the preparation of graphene containing different layers and solutions and films thereof.
  • Carbon has many forms of existence, including common graphite, diamond, amorphous carbon, and carbon 60 found in recent years, carbon nanotubes, and graphene. Although these materials are composed of carbon, the structure and properties vary greatly. Among them, graphene is a single-layer graphite or a multi-layer graphite material composed of a single piece of graphite. Graphene materials have many excellent properties, such as extremely high electrical conductivity and mechanical properties. Therefore, the film obtained from the graphene material has a wide application prospect. However, there is currently no good large-scale preparation method. Therefore, there is an urgent need for a large-scale preparation method that is feasible from both research and industrial applications. Overview
  • An aspect of the present application provides a method of preparing an oligo-pigment graphite, the method comprising:
  • Another aspect of the present application provides a method of producing an oligolithic graphite film, the method comprising: mixing an oligolithic graphite solid obtained in the foregoing method with a solvent to prepare a solution, coating the solution, and forming a film Heat in an inert gas.
  • Fig. 1 is an electron transmission micrograph of an oligo-ply graphite synthesized by an arc method in a mixed gas atmosphere of H 2 and He.
  • Fig. 3 is an atomic force micrograph of an oligo-ply graphite synthesized by an arc method in a mixed gas atmosphere of CO 2 (30% partial pressure) and He.
  • Figure 4 is an XRD pattern of oligo-ply graphite.
  • Figure 5 is a thermograviogram of oligo-ply graphite.
  • Fig. 6 is an electron transmission micrograph of an oligo-ply graphite synthesized by an arc method in a mixed gas atmosphere of C0 2 (25% partial pressure) and He.
  • Fig. 7 is a high-resolution electron transmission micrograph of the oligo-ply graphite synthesized by the arc method in a mixed gas atmosphere of C0 2 (25% partial pressure) and He.
  • Fig. 8 is a high-resolution electron transmission micrograph of an oligo-ply graphite synthesized by an arc method in a mixed gas atmosphere of C0 2 (25% partial pressure) and He.
  • Fig. 9 is an atomic force micrograph of an oligo-ply graphite synthesized by an arc method in a mixed gas atmosphere of CO 2 (40% partial pressure) and He.
  • Fig. 10 is a high-resolution electron transmission micrograph of an oligographite synthesized by an arc method in a mixed gas atmosphere of CO 2 (40% partial pressure) and He.
  • Figure 11 is a graph showing the conductivity of a film made of an oligo graphite solution.
  • oligolayer graphite (FG) as used in the present invention means that its molecular constituent unit is
  • single-layer graphite refers to a two-dimensional planar molecular skeleton consisting of a single layer of carbon atoms with a single-chip area between 10 nm 2 and 1000 ⁇ m 2 and a single-sheet thickness between about 0.34 nm and 2 nm.
  • the carbon atoms of the edge portion of the layer in "oligolayer graphite” and “single layer graphite” may be bonded to different organic functional groups such as a hydroxyl group, an amino group, a carboxyl group, an epoxy group or the like depending on the specific preparation method and preparation conditions.
  • An aspect of the present application provides a method of preparing an oligo-pigment graphite, the method comprising:
  • Exemplary inert gases that can be used in the present application include N 2 , He, Ne, Ar, Kr, and Xe.
  • the inert gas is He or Ar or a mixture thereof.
  • Exemplary gases that are reactive with carbon in the present application include, but are not limited to, ammonia, hydrogen, carbon dioxide, air, oxygen, and the like.
  • the volume ratio of the inert gas to the gas which is reactive with carbon in the mixed gas is from 9:95 to 95:5. In certain embodiments of the present application, the volume of the inert gas and the gas reactive with carbon in the mixed gas is from 80:20 to 20:80. In certain embodiments of the present application, the volume of the inert gas and the gas reactive with carbon in the mixed gas is from 75:25 to 25:75.
  • the total pressure of the mixed gas is from 0.02 MPa to 0.4 MPa. In certain embodiments, the total pressure of the mixed gas is from 0.05 MPa to 0.3 MPa. In some embodiments, the total pressure of the mixed gas is from 0.07 MPa to 0.2 MPa.
  • both electrodes are electrodes of carbon material. In some embodiments, both electrodes are electrodes of graphite.
  • the arc discharge process may employ an alternating arc discharge or a direct current arc discharge, and the discharge voltage is 10-200 V, and the current is 10-250A. In certain embodiments, in the method of preparing oligo-pigmented graphite, the arc discharge process may employ an alternating arc discharge or a direct current arc discharge with a discharge voltage of 10-80 V and a current of 50-200 A.
  • the arc discharge process employs a DC arc discharge with a discharge voltage of 15-50 V and a current of 80-180 A. In some embodiments, the arc discharge process employs a direct current arc discharge with a discharge voltage of 15-40 V and a current of 100-150 A.
  • the current during discharge is controlled by the power supply and the voltage between the two electrodes is adjusted by adjusting the distance between the two electrodes.
  • the anode is a consumable electrode.
  • the discharge between the cathode and the anode is exhausted to the anode.
  • a method of making oligo-pigment graphite comprising:
  • Two carbon electrodes are provided as a cathode and an anode, wherein the larger diameter is the cathode and the smaller diameter is the anode;
  • the cathode has a diameter of from 3 mm to 10 cm. In some embodiments, the cathode has a diameter of 1 cm. In certain embodiments, the anode has a diameter of from 2 mm to 8 cm. In certain embodiments, the anode has a diameter of 5 mm.
  • the mixed gas is comprised of an inert gas and a gas that is reactive toward carbon.
  • the method is carried out in an electric furnace.
  • the oligo-pigment graphite obtained by the method may contain graphene sheets of different layers.
  • Another aspect of the present application provides a method of preparing an oligolithic graphite film, the method comprising: directly applying the oligo-pigment graphite solid to a film, or mixing with a solvent to prepare a solution, coating the solution, and The formed film is heated in an inert gas to controllably remove functional groups on the graphene sheets and repair defects to restore the intrinsic conductivity of the graphene to obtain a highly conductive film.
  • a graphene conductive film can be obtained by reducing with a reducing agent, including a gas reducing agent.
  • the solvent used in the preparation of the oligo graphite solution may be any volatile solvent, and exemplary solvents include, but are not limited to: water; hydrazine, hydrazine-dimethylformamide (DMF), hydrazine, hydrazine-dimethyl ethene Amides such as amides; alcohols such as ethanol, methanol, isopropanol; dimethyl sulfoxide (DMSO); Chlorinated solvents such as chlorobenzene, dichlorobenzene, and dichloromethane; esters such as ethyl acetate, methyl acetate, and dimethyl phthalate (DMP).
  • exemplary solvents include, but are not limited to: water; hydrazine, hydrazine-dimethylformamide (DMF), hydrazine, hydrazine-dimethyl ethene Amides such as amides; alcohols such as ethanol, methanol, isopropanol;
  • a coating film method well known in the art may be employed, including but not limited to spin coating, spray coating, dipping, and the like.
  • an oligo-graphite film of the present application may optionally include adding a dispersing agent, a thickener, etc. to the solution prepared by mixing the above oligo-pigment graphite solution or the above-mentioned oligo-pigment graphite solid and a solvent before performing the coating film.
  • a dispersing agent e.g., sodium bicarbonate
  • a thickener e.g., sodium bicarbonate
  • a step of reducing the conductivity of the film by using a reducing agent after the coating film may be optionally included.
  • the reducing vapor is hydrazine hydrate vapor.
  • a pure carbon rod was used as the anode.
  • a mixture of H 2 and He (pressure ratio 1:1) was introduced into the electric arc furnace to a pressure of 0.07 MPa in the furnace. Set the output current to 100 A.
  • the voltage was maintained at about 30 V by adjusting the distance between the cathode and the anode, and the pressure in the furnace was maintained at about 0.07 MPa.
  • the anode is consumed and the reaction is completed.
  • the product collected in the electric arc furnace is oligo graphite.
  • a pure carbon rod was used as the anode.
  • a mixture of H 2 and He is introduced into the electric arc furnace (pressure ratio)
  • the pressure in the furnace is 0.07 MPa. Set the output current to 150 A. After the discharge started, the voltage was maintained at about 37 V by adjusting the distance between the cathode and the anode, and the pressure in the furnace was maintained at about 0.07 MPa. The anode is consumed and the reaction is completed. The product collected in the electric arc furnace is oligo graphite.
  • Fig. 1 is an electron transmission micrograph of an oligo-ply graphite synthesized by an arc method in a mixed gas atmosphere of H 2 and He.
  • the product is in the form of an oligo-graphite structure, and some of the sheet-like structures are bent to form wrinkles, and a layered structure can be seen.
  • Example 3
  • a pure carbon rod was used as the anode.
  • a mixture of C0 2 and He (C0 2 5% partial pressure) was introduced into the electric arc furnace to a pressure of 0.07 MPa in the furnace. Set the output current to 150 A.
  • the voltage was maintained at about 32 V by adjusting the distance between the cathode and the anode, and the pressure in the furnace was maintained at about 0.07 MPa.
  • the anode is consumed and the reaction is completed.
  • the product collected in the electric arc furnace is oligo graphite.
  • a pure carbon rod was used as the anode.
  • a mixture of C0 2 and He (C0 2 accounted for 30% partial pressure) was introduced into the electric arc furnace to a pressure of 0.07 MPa in the furnace. Set the output current to 150 A. After the discharge started, the voltage was maintained at about 22 V by adjusting the distance between the cathode and the anode, and the pressure in the furnace was maintained at about 0.07 MPa. The anode is consumed and the reaction is completed. The product collected in the electric arc furnace is oligo graphite.
  • a pure carbon rod was used as the anode.
  • a mixture of C0 2 and He (C0 2 accounted for 30% partial pressure) was introduced into the electric arc furnace to a pressure of 0.07 MPa in the furnace. Set the output current to 200 A. After the discharge started, the voltage was maintained at about 20 V by adjusting the distance between the cathode and the anode, and the pressure in the furnace was maintained at about 0.07 MPa. The anode is consumed and the reaction is completed. The product collected in the electric arc furnace is oligo graphite.
  • a pure carbon rod was used as the anode.
  • a mixture of C0 2 and He (C0 2 accounted for 30% partial pressure) was introduced into the electric arc furnace to a pressure of 0.17 MPa in the furnace. Set the output current to 150 A.
  • the voltage was maintained at about 20 V by adjusting the distance between the cathode and the anode, and the pressure in the furnace was maintained at about 0.17 MPa.
  • the anode is consumed and the reaction is completed.
  • the product collected in the electric arc furnace is oligo graphite.
  • FIG. 2 is a Raman spectrum of an oligo-ply graphite synthesized by an arc method in a mixed gas atmosphere of CO 2 (30% partial pressure) and He. From the half-width and peak shape of its 2D peak, it can be estimated that the product is mainly 4 layers of oligo-pigment graphite.
  • Figure 3 is an atomic force micrograph of the oligo-ply graphite synthesized by arc method in a mixed gas atmosphere of CO 2 (30% partial pressure) and He. As can be seen from the figure, the partial thickness of the product graphite sheet is about 2.62 nm, indicating that the product is Oligomerized graphite sheet structure.
  • Example 7
  • a pure carbon rod was used as the anode.
  • a mixture of C0 2 and He (C0 2 accounted for 30% partial pressure) was introduced into the electric arc furnace to a pressure of 0.10 MPa in the furnace. Set the output current to 150 A. After the start of the discharge, the voltage was maintained at about 20 V by adjusting the distance between the cathode and the anode, and the pressure in the furnace was maintained at about 0.10 MPa. The anode is consumed and the reaction is completed.
  • the flocculent product collected in the electric arc furnace is oligo graphite.
  • a pure carbon rod was used as the anode.
  • a mixture of C0 2 and He (C 2 2 is divided by 25%) is introduced into the electric arc furnace to a pressure of 0.20 MPa in the furnace. Set the output current to 150 A. After the discharge started, the voltage was maintained at about 20 V by adjusting the distance between the cathode and the anode, and the pressure in the furnace was maintained at about 0.20 MPa. The anode is consumed and the reaction is completed.
  • the product collected in the electric arc furnace is oligo graphite.
  • Figure 4 is an XRD pattern of the obtained oligo-ply graphite. It can be seen from the figure that the two peaks indicate that the distance between the product sheets is 3.4 nm and 4.2 nm, respectively, and the peak at 3.4 nm is sharper, indicating that there is a relatively complete ordinary graphite sheet structure in the product, and 4.2 nm The peak is wider, indicating that the product has a layer spacing larger than that of the ordinary graphite sheet, and is in an amorphous state, which conforms to the structure of the oligo graphite.
  • Figure 5 is a thermograviogram of the obtained oligo-ply graphite. As can be seen from the figure, the product has little thermal weight loss throughout the temperature zone, indicating that the product contains less functional groups, much smaller than the single layer graphite and oligo-pigment graphite produced by the conventional solution method.
  • Fig. 6 is an electron transmission micrograph of an oligo-ply graphite synthesized by an arc method in a mixed gas atmosphere of C0 2 (25% partial pressure) and He. It can be seen from the figure that the product is a flaky structure of oligo-pigmented graphite, and part of the graphite sheet layer forms wrinkles.
  • Fig. 7 is a high-resolution electron transmission micrograph of the oligo-ply graphite synthesized by the arc method in a mixed gas atmosphere of C0 2 (25% partial pressure) and He. It can be seen from the figure that the product is a flaky structure of oligo-ply graphite, and the edge indicated by the arrow is a three-layer graphite sheet structure.
  • Fig. 8 is a high-resolution electron transmission micrograph of an oligo-ply graphite synthesized by an arc method in a mixed gas atmosphere of C0 2 (25% partial pressure) and He. The flaky graphene formed can be seen from the electron micrograph, and the number of layers of the graphene sheet pleats indicated by the arrows is two, four, and five layers, respectively.
  • Example 9
  • a pure carbon rod was used as the anode.
  • a mixture of C0 2 and He (C 2 2 is divided by 25%) is introduced into the electric arc furnace to a pressure of 0.17 MPa in the furnace. Set the output current to 150 A.
  • the voltage was maintained at about 20 V by adjusting the distance between the cathode and the anode, and the pressure in the furnace was maintained at about 0.17 MPa.
  • the anode is consumed and the reaction is completed.
  • the flocculent product collected in the electric arc furnace is oligo graphite.
  • a pure carbon rod was used as the anode.
  • a mixture of C0 2 and He (C0 2 accounted for 40% partial pressure) was introduced into the electric arc furnace to a pressure of 0.17 MPa in the furnace. Set the output current to 150 A. After the discharge started, the voltage was maintained at about 20 V by adjusting the distance between the cathode and the anode, and the pressure in the furnace was maintained at about 0.17 MPa. The anode is consumed and the reaction is completed.
  • the product collected in the electric arc furnace is oligo graphite.
  • Fig. 9 is an atomic force micrograph of an oligo-ply graphite synthesized by an arc method in a mixed gas atmosphere of CO 2 (40% partial pressure) and He.
  • the partial thickness of the product graphite sheet was 2.80 nm, indicating that the product was an oligo-graphite sheet structure.
  • Fig. 10 is a high-resolution electron transmission micrograph of an oligo-ply graphite synthesized by an arc method in a mixed gas atmosphere of CO 2 (40% partial pressure) and He. It can be seen from the figure that the product is a flaky structure of oligo-pigment graphite, and the edge indicated by the arrow is a six-layer graphite sheet structure.
  • Example 11
  • the pure carbon rod is machined and used as an anode.
  • a mixture of C0 2 and Ar is introduced (( 0 2 is 33% partial pressure) to a furnace pressure of 0.17 MPa.
  • the output current is set to 150 A.
  • the voltage is maintained by adjusting the distance between the cathode and the anode.
  • the pressure in the furnace was maintained at about 0.17 MPa.
  • the anode was consumed and the reaction was completed.
  • the product in the collection arc furnace was oligo graphite.
  • the pure carbon rod is machined and used as an anode.
  • a mixture of air and He air 50% partial pressure
  • the voltage was maintained at about 30 V by adjusting the distance between the cathode and the anode, and the pressure in the furnace was maintained at 0.17-0.20 MPa.
  • the anode is consumed and the reaction is completed.
  • the product in the collection arc furnace is oligo graphite. Oligo-layer graphite solution preparation
  • the oligo graphite solution prepared in Example 13 or 14 was obtained by spin coating on a cleaned quartz sheet, and dried by heating to obtain an oligo graphite conductive film.
  • Figure 11 is a graph showing the conductivity of a film made of an oligo graphite solution. Conductivity is ⁇ 10 3

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  • Materials Engineering (AREA)
  • Physics & Mathematics (AREA)
  • Inorganic Chemistry (AREA)
  • Condensed Matter Physics & Semiconductors (AREA)
  • General Physics & Mathematics (AREA)
  • Crystallography & Structural Chemistry (AREA)
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Abstract

On prévoit un procédé d'obtention d'un graphène FLG consistant à : (1) fournir deux électrodes de carbone tenant lieu de cathode et anode et (2) appliquer une tension entre les deux électrodes sous une atmosphère de gaz mixte contenant un gaz inerte et un gaz réagissant au carbone. On prévoit encore un procédé d'obtention d'un film de graphène FLG consistant à : (1) enrober avec le solide de graphène FLG ou mélanger le solide de graphène FLG avec un solvant pour obtenir une dispersion, puis enrober avec la dispersion et (2) chauffer et réduire le film obtenu sous une atmosphène de gaz inerte ou de gaz réducteur.
PCT/CN2010/079477 2009-12-04 2010-12-06 Procédés d'obtention d'un graphène flg et d'un film de graphène flg Ceased WO2011066811A1 (fr)

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Cited By (1)

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CN103311441A (zh) * 2012-03-09 2013-09-18 北京大学 一种石墨烯悬浊液分散系及其在薄膜太阳能电池中的应用

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WO2009129194A2 (fr) * 2008-04-14 2009-10-22 Massachusetts Institute Of Technology Graphène à un plan et à nombre limité de plans de grande surface sur des substrats arbitraires

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CN1796334A (zh) * 2004-12-27 2006-07-05 陈瑾惠 碳/碳复合材料及其制造方法

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WO2009129194A2 (fr) * 2008-04-14 2009-10-22 Massachusetts Institute Of Technology Graphène à un plan et à nombre limité de plans de grande surface sur des substrats arbitraires
CN101474898A (zh) * 2009-01-16 2009-07-08 南开大学 基于石墨烯的导电碳膜及制备方法和应用

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SUBRAHMANYAM, K. S. ET AL.: "Simple Method of Preparing Graphene Flakes by an Arc-Discharge Method", J. PHYS. CHEM. C, vol. 113, no. 11, 20 February 2009 (2009-02-20), pages 4257 - 4259 *
WU, ZHONGSHUAI ET AL.: "Synthesis of Graphene Sheets with High Electrical Conductivity and Good Thermal Stability by Hydrogen Arc Discharge Exfoliation", ACS NANO, vol. 3, no. 2, 3 February 2009 (2009-02-03), pages 411 - 417, XP055203869, DOI: doi:10.1021/nn900020u *

Cited By (1)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN103311441A (zh) * 2012-03-09 2013-09-18 北京大学 一种石墨烯悬浊液分散系及其在薄膜太阳能电池中的应用

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