CN110937593B - Nano-pore graphene and preparation method and application thereof - Google Patents
Nano-pore graphene and preparation method and application thereof Download PDFInfo
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- CN110937593B CN110937593B CN201811105139.7A CN201811105139A CN110937593B CN 110937593 B CN110937593 B CN 110937593B CN 201811105139 A CN201811105139 A CN 201811105139A CN 110937593 B CN110937593 B CN 110937593B
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- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical compound [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 title claims abstract description 70
- 229910021389 graphene Inorganic materials 0.000 title claims abstract description 69
- 239000011148 porous material Substances 0.000 title claims abstract description 32
- 238000002360 preparation method Methods 0.000 title claims abstract description 11
- 239000000178 monomer Substances 0.000 claims abstract description 16
- 239000000243 solution Substances 0.000 claims abstract description 15
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims abstract description 13
- 230000005669 field effect Effects 0.000 claims abstract description 10
- 239000002356 single layer Substances 0.000 claims abstract description 10
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- 239000000463 material Substances 0.000 claims abstract description 8
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- 230000000694 effects Effects 0.000 claims abstract description 5
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- 239000010410 layer Substances 0.000 claims abstract description 4
- YXFVVABEGXRONW-UHFFFAOYSA-N Toluene Chemical compound CC1=CC=CC=C1 YXFVVABEGXRONW-UHFFFAOYSA-N 0.000 claims description 22
- 238000000034 method Methods 0.000 claims description 21
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- XKRFYHLGVUSROY-UHFFFAOYSA-N Argon Chemical compound [Ar] XKRFYHLGVUSROY-UHFFFAOYSA-N 0.000 claims description 10
- RIOQSEWOXXDEQQ-UHFFFAOYSA-N triphenylphosphine Chemical compound C1=CC=CC=C1P(C=1C=CC=CC=1)C1=CC=CC=C1 RIOQSEWOXXDEQQ-UHFFFAOYSA-N 0.000 claims description 10
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- WLPUWLXVBWGYMZ-UHFFFAOYSA-N tricyclohexylphosphine Chemical compound C1CCCCC1P(C1CCCCC1)C1CCCCC1 WLPUWLXVBWGYMZ-UHFFFAOYSA-N 0.000 claims description 8
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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
-
- H—ELECTRICITY
- H01—ELECTRIC ELEMENTS
- H01L—SEMICONDUCTOR DEVICES NOT COVERED BY CLASS H10
- H01L29/00—Semiconductor devices adapted for rectifying, amplifying, oscillating or switching, or capacitors or resistors with at least one potential-jump barrier or surface barrier, e.g. PN junction depletion layer or carrier concentration layer; Details of semiconductor bodies or of electrodes thereof ; Multistep manufacturing processes therefor
- H01L29/02—Semiconductor bodies ; Multistep manufacturing processes therefor
- H01L29/12—Semiconductor bodies ; Multistep manufacturing processes therefor characterised by the materials of which they are formed
- H01L29/16—Semiconductor bodies ; Multistep manufacturing processes therefor characterised by the materials of which they are formed including, apart from doping materials or other impurities, only elements of Group IV of the Periodic System
- H01L29/1606—Graphene
-
- H—ELECTRICITY
- H01—ELECTRIC ELEMENTS
- H01L—SEMICONDUCTOR DEVICES NOT COVERED BY CLASS H10
- H01L31/00—Semiconductor devices sensitive to infrared radiation, light, electromagnetic radiation of shorter wavelength or corpuscular radiation and specially adapted either for the conversion of the energy of such radiation into electrical energy or for the control of electrical energy by such radiation; Processes or apparatus specially adapted for the manufacture or treatment thereof or of parts thereof; Details thereof
- H01L31/0248—Semiconductor devices sensitive to infrared radiation, light, electromagnetic radiation of shorter wavelength or corpuscular radiation and specially adapted either for the conversion of the energy of such radiation into electrical energy or for the control of electrical energy by such radiation; Processes or apparatus specially adapted for the manufacture or treatment thereof or of parts thereof; Details thereof characterised by their semiconductor bodies
- H01L31/0256—Semiconductor devices sensitive to infrared radiation, light, electromagnetic radiation of shorter wavelength or corpuscular radiation and specially adapted either for the conversion of the energy of such radiation into electrical energy or for the control of electrical energy by such radiation; Processes or apparatus specially adapted for the manufacture or treatment thereof or of parts thereof; Details thereof characterised by their semiconductor bodies characterised by the material
- H01L31/0264—Inorganic materials
- H01L31/028—Inorganic materials including, apart from doping material or other impurities, only elements of Group IV of the Periodic System
-
- 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
- C01B2204/02—Single layer graphene
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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
- C01B2204/04—Specific amount of layers or specific thickness
Abstract
The invention discloses a nano-pore graphene and a preparation method and application thereof, wherein the nano-pore graphene is of a single-layer structure or a multi-layer structure formed by periodically and closely stacking the single-layer structure, and the structural unit of the single-layer structure is as follows:
the preparation method of the nanopore graphene comprises the following steps: under the protection of inert gas, dissolving a monomer A, a monomer B and a catalyst in an organic solvent different from water to obtain an organic solution, dissolving alkali in water to generate an alkaline aqueous solution, placing the organic solution and the alkaline aqueous solution in the same container to form an interface, standing for 1-60 days at the temperature of more than 0 ℃ and less than 100 ℃, and obtaining the nanoporous graphene at the interface. The nanopore graphene is large in transverse dimension, high in order and high in field effect mobility. The preparation method has mild conditions and simple operation. The nano-pore graphene can be used as a channel material for preparing a field effect transistor and a photoelectric effect tube.
Description
Technical Field
The invention relates to the technical field of functional materials, in particular to a nanopore graphene and a preparation method and application thereof.
Background
Since the graphene is discovered in 2004, the graphene has attracted attention and is widely applied in the fields of electronics, energy storage, environmental management and the like. However, the material surface is filled with atomic and electron clouds, without additional pore structure, and without direct energy band gap, which results in the material not being used directly on top of the transistor.
In order to enable its use in transistors, it has been found that a direct energy band gap can be introduced into graphene by introducing a pore structure into the graphene. Based on this, various methods have been developed to modify it. The transformation method mainly comprises two methods: 1. drilling holes in the graphene directly, wherein the drilling method comprises an ultraviolet light etching method, an electron beam bombardment method, a local oxidation degradation method and the like; 2, polymerizing on the silver surface directly using hexaiodo-cyclohexa-m-benzene monomer. However, the first method has complex process conditions, the size of the prepared pores is generally from several nanometers to hundreds of nanometers, and the complete uniformity of the sizes of the pores cannot be ensured; the second method has harsh technological conditions, requires high temperature and high vacuum, and the obtained nano material has small transverse size of only a few nanometers to a dozen nanometers, is loaded on the metal surface, does not exist independently, and cannot be used as graphene in the true sense.
Therefore, how to establish a simple and mild method to prepare a large-scale and high-order nanoporous graphene material becomes an urgent problem to be solved, otherwise, the method is a night-time Tan for practical application.
Disclosure of Invention
In order to solve the problems in the prior art, the invention provides a nanopore graphene, a preparation method and an application thereof.
The preparation method has mild conditions and simple operation.
The nano-pore graphene can be used as a channel material for preparing a field effect transistor and a photoelectric effect tube.
The technical scheme adopted for realizing the above purpose of the invention is as follows:
a kind of nanometer hole graphene, the stated nanometer hole graphene is a single-layer structure, or the periodic close-packed multilayer structure that forms by the single-layer structure, the constitutional unit of the stated single-layer structure is:
wherein the dotted line is a chemical bond extending outward.
A preparation method of nanopore graphene comprises the following steps:
under the protection of inert gas, dissolving a monomer A, a monomer B and a catalyst in an organic solvent different from water to obtain an organic solution, dissolving alkali in water to generate an alkaline aqueous solution, placing the organic solution and the alkaline aqueous solution in the same container to form an interface, standing for 1-60 days at the temperature of more than 0 ℃ and less than 100 ℃, and obtaining the nano-pore graphene at the interface;
the structural general formula of the monomer A is as follows:
wherein X is
The dotted line represents a bond to a benzene ring;
the structural general formula of the monomer B is
the above reaction is shown below:
further, the catalyst is Pd (PPh)3)2Cl2、Pd(PPh3)4、Pd(PCy3)2Cl2、Pd(PCy3)4、 Pd(PBu3)2Cl2、Pd(PBu3)4、Pd(P(OMe)3)2Cl2、Pd(P(OMe)3)4、Pd(AsPh3)2Cl2、Pd(AsPh3)4、 Pd(dppe)Cl2、Pd(dppe)2、Pd(dppp)Cl2、、Pd(dppf)Cl2、Pd(OAc)2、PdCl2、Ni(dppf)Cl2、 Ni(dppe)Cl2、Ni(PPh3)2Cl2、Ni(PCy3)2Cl2、Ni(NEt3)2Cl2、Ni(bipy)Cl2、Ni(tppts)3、 Ni(COD)2/PPh3、Ni(COD)2/PCy3、NiCl2Or Ni (OAc)2。
Further, the organic solvent is alkane with 5-25 carbon atoms, toluene, ethylbenzene, xylene, trimethylbenzene, petroleum ether, chlorobenzene, dichlorobenzene, trichlorobenzene, dichloromethane, trichloromethane, dichloroethane, tetrachloroethane, trichloroethane, carbon tetrachloride, ethyl acetate or methyl acetate.
Further, the molar ratio of the monomer A to the monomer B was 1: 1.
Further, the alkali is Cs2CO3、K2CO3、Na2CO3、Li2CO3、CaCO3、MgCO3、CsOH、 CsHCO3、KHCO3、NaHCO3、LiHCO3、KOH、NaOH、LiOH、Ca(OH)2、Mg(OH)2Triethylamine, pyridine or piperidine.
Further, the inert gas is nitrogen, argon or carbon dioxide.
An application of nano-pore graphene in preparing a field effect transistor and a photoelectric effect tube as a channel material.
Compared with the prior art, the invention has the beneficial effects and advantages that:
1. the nano-pore graphene prepared by the method has the characteristics of large transverse dimension, high orderliness and high field effect mobility, and is suitable to be used as a channel material for preparing a field effect transistor and a photoelectric effect tube.
2. The nano-pore graphene prepared by the method does not need to depend on a substrate, and can independently and stably exist.
3. The method for preparing the nanopore graphene has the advantages of mild conditions, simple operation, wide sources of the used monomers, low price and direct purchase in the market.
Drawings
Fig. 1 is an optical microscope image of the nanoporous graphene prepared in example 1.
Fig. 2 is a scanning electron microscope image of the nanoporous graphene prepared in example 1.
Fig. 3 is an electron diffraction pattern of the nanoporous graphene obtained in example 1.
Fig. 4 is a high-resolution transmission electron microscope image of the nanoporous graphene obtained in example 1.
Fig. 5 is an a-B-C stacking diagram between layers of the nanoporous graphene obtained in example 1.
Detailed Description
The present invention will be described in detail with reference to specific examples.
Example 1
1mg of 1,3, 5-Triphenyl-Triboronate Tripinacol ester (CA No. 365564-05-2, FW:455.996), 1mg of 1,3, 5-triiodobenzene (CAS No. 626-44-8, FW:455.801) and 10mg of tetrakis (triphenylphosphine) palladium Pd (PPh) under the protection of argon3)4Dissolved in 20mL of toluene to give an organic solution, and 10mg of sodium carbonate was dissolved in 10mL of water to give an aqueous sodium carbonate solution. And (3) placing the organic solution and the sodium carbonate aqueous solution in the same container to form an interface, standing for 30 days at the temperature of 2 ℃, and obtaining the nanopore graphene at the interface.
The method comprises the steps of taking the nanopore graphene out of a silicon wafer with a prepared gold electrode, respectively cleaning the nanopore graphene for three times by using toluene, dichloromethane, water and ethanol, naturally drying the nanopore graphene in the air, directly loading the dried nanopore graphene on a glass sheet, observing the nanopore graphene by using an optical microscope, and obtaining an optical microscope image as shown in fig. 1, wherein the transverse dimension of the nanopore graphene is larger than 1 mm as can be seen from fig. 1.
The nanopore graphene is directly loaded on the micro-grid carbon net, scanning is carried out by using a scanning electron microscope, and the obtained scanning electron microscope image is shown in fig. 2, and as can be seen from fig. 2, the transverse dimension of the nanopore graphene is larger than 50 microns.
Fig. 3 shows an electron diffraction pattern of the nanoporous graphene obtained by electron diffraction analysis, and fig. 3 shows that the surface of the nanoporous graphene has high order.
Scanning the nano-pore graphene by using a high-resolution transmission electron microscope, wherein the obtained high-resolution transmission electron microscope image is as shown in fig. 4, the image can be shown in fig. 4, the single layer of the nano-pore graphene is composed of a plurality of structural units, and the structural units have the structural formula:
as shown in FIG. 5, the nanographene has a multilayer structure, and layers are obliquely stacked according to the mode of A-B-C.
Fishing out the nano-pore graphene by using a silicon wafer with a prepared gold electrode, respectively cleaning the nano-pore graphene by using methylbenzene, dichloromethane, water and ethanol for three times, naturally drying the nano-pore graphene in the air, and then drying the nano-pore graphene in vacuum at room temperature to obtain the nano-pore graphene with the field effect mobility of 8.2 multiplied by 10-3cm2/Vs。
Example 2
1mg of 1,3, 5-Triphenyl-Triboronate Tripinacol ester (CA No. 365564-05-2, FW:455.996), 1mg of 1,3, 5-triiodobenzene (CAS No. 626-44-8, FW:455.801) and 10mg of tetrakis (triphenylphosphine) palladium Pd (PPh) under the protection of argon3)4Dissolved in 20mL of chloroform to give an organic solution, and 10mg of sodium carbonate was dissolved in 10mL of water to give an aqueous sodium carbonate solution. And placing the organic solution and the sodium carbonate aqueous solution in the same container to form an interface, standing for 30 days at the temperature of 2 ℃, and obtaining the nanopore graphene at the interface.
Fishing out the nano-pore graphene by using a silicon wafer with a prepared gold electrode, respectively cleaning the nano-pore graphene by using toluene, dichloromethane, water and ethanol for three times, naturally airing the nano-pore graphene, and then carrying out room temperature treatmentVacuum drying, and measuring the field effect mobility of the nano-pore graphene to be 9.1 multiplied by 10-3cm2/Vs。
Example 3
1mg of 1,3, 5-Triphenyl-Triboronate Tripinacol ester (CA No. 365564-05-2, FW:455.996), 1.5mg of 1,3, 5-Tribromobenzene (CAS No. 626-44-8, FW:455.801) and 10mg of palladium bis (triphenylphosphine) dichloride Pd (PPh3)2Cl under the protection of argon2Dissolved in 20mL of toluene to give an organic solution, and 10mg of sodium hydroxide was added to 10mL of water to give an aqueous sodium hydroxide solution. And placing the organic solution and the sodium hydroxide aqueous solution in the same container to form an interface, standing for 30 days at 10 ℃, and obtaining the nanopore graphene at the interface.
Fishing out the nano-pore graphene by using a silicon wafer with a prepared gold electrode, respectively cleaning the nano-pore graphene by using methylbenzene, dichloromethane, water and ethanol for three times, naturally drying the nano-pore graphene in the air, and then drying the nano-pore graphene in vacuum at room temperature to obtain the nano-pore graphene with the field effect mobility of 1.5 multiplied by 10-2cm2/Vs。
Claims (7)
1. A preparation method of nanopore graphene is characterized by comprising the following steps:
under the protection of inert gas, dissolving a monomer A, a monomer B and a catalyst in an organic solvent which is not soluble with water to obtain an organic solution, dissolving alkali in water to generate an alkaline aqueous solution, placing the organic solution and the alkaline aqueous solution in the same container to form an interface, standing for 1-60 days at the temperature of more than 0 ℃ and less than 100 ℃, and obtaining the nano-pore graphene at the interface;
the structural general formula of the monomer A is as follows:
wherein X is
、
、
Or
The dotted line represents a bond to a benzene ring;
the structural general formula of the monomer B is
the nano-pore graphene is of a single-layer structure or a multi-layer structure formed by periodically and closely stacking the single-layer structure, and the structural units of the single-layer structure are as follows:
wherein the dotted lines are the connecting bonds between the structural units.
2. The method for preparing nanoporous graphene according to claim 1, wherein: the catalyst is Pd (PPh)3)2Cl2、Pd(PPh3)4、Pd(PCy3)2Cl2、Pd(PCy3)4、Pd(PBu3)2Cl2、Pd(PBu3)4、Pd(AsPh3)2Cl2、Pd(AsPh3)4、Pd(dppe)Cl2、Pd(dppe)2、Pd(dppp)Cl2、Pd(dppf)Cl2、Pd(OAc)2、PdCl2、Ni(dppf)Cl2、Ni(dppe)Cl2、Ni(PPh3)2Cl2、Ni(PCy3)2Cl2、Ni(NEt3)2Cl2、Ni(bipy)Cl2、Ni(tppts)、Ni(COD)2/PPh3、Ni(COD)2/PCy3、NiCl2Or Ni (OAc)2。
3. The method for preparing nanoporous graphene according to claim 1, wherein: the organic solvent is alkane with 5-25 carbon atoms, toluene, ethylbenzene, xylene, trimethylbenzene, petroleum ether, chlorobenzene, dichlorobenzene, trichlorobenzene, dichloromethane, trichloromethane, dichloroethane, tetrachloroethane, trichloroethane, carbon tetrachloride, ethyl acetate or methyl acetate.
4. The method for preparing nanoporous graphene according to claim 1, wherein: the molar ratio of the monomer A to the monomer B was 1: 1.
5. The method for preparing nanoporous graphene according to claim 1, wherein: the alkali is Cs2CO3、K2CO3、Na2CO3、Li2CO3、CaCO3、MgCO3、CsOH、CsHCO3、KHCO3、NaHCO3、LiHCO3、KOH、NaOH、LiOH、Ca(OH)2、Mg(OH)2Triethylamine, pyridine or piperidine.
6. The method for preparing nanoporous graphene according to claim 1, wherein: the inert gas is nitrogen or argon.
7. Application of the nano-porous graphene prepared by the method in claim 1 in preparation of field effect transistors and photoelectric effect tubes as channel materials.
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