CN103332688A - Method for synthesizing graphene with organic acid metal salt - Google Patents
Method for synthesizing graphene with organic acid metal salt Download PDFInfo
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- CN103332688A CN103332688A CN2013102965226A CN201310296522A CN103332688A CN 103332688 A CN103332688 A CN 103332688A CN 2013102965226 A CN2013102965226 A CN 2013102965226A CN 201310296522 A CN201310296522 A CN 201310296522A CN 103332688 A CN103332688 A CN 103332688A
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Abstract
The invention discloses a method for synthesizing graphene with organic acid metal salt. The method comprises the steps that a pipe furnace is pre-heated to 700-1300 DEG C, and protected by an inert atmosphere; the organic acid metal salt is placed in the pipe furnace protected by nitrogen, heated for 0.5-120min, and cooled to a room temperature; a solid product is obtained, washed, filtered and dried; and a graphene product is obtained. The method has the advantages of simplicity in operation, low cost and large-scale preparation under a formwork-free condition.
Description
Technical field
The invention belongs to a kind of method of synthesizing graphite alkene, be specifically related to a kind of method of metal salts of organic acids pyrolysis synthesizing graphite alkene.
Background technology
Graphene be discovered in recent years by individual layer sp
2The two-dimentional carbonaceous crystal that hydridization carbon constitutes has the specific surface area of excellent electroconductibility, mechanical property, superelevation and to good the passing through and the property transmitted etc. of guest molecule/ion, has potential using value at numerous areas.Along with going deep into of research, the demand that magnanimity obtains Graphene is strong day by day.Therefore, how to realize that scale preparation becomes one of restriction Graphene problem demanding prompt solution of further being studied and using.
At present, the method for having developed for preparing Graphene can be divided into two kinds of approach: " top-down " and " bottom-up " approach.Wherein the graphite oxide in " top-down " approach is peeled off method and is considered to the current effective ways that can obtain Graphene in a large number, but since the use havoc of strong oxidizer the conjugated structure of Graphene, cause the loss of its intrinsic electric property, need carry out follow-up reduction and handle to repair its electric property.[atom economy synthesizing graphite alkene/trimanganese tetroxide mixture is used for electric chemical super capacitor research, " nanoscale ",, the 5th volume, the 2999th page of (Highly Atom-Economic～Synthesis of Graphene/Mn in 2013
3O
4Hybrid Composites for Electrochemical Supercapacitors. Nanoscale, 2013, Vol.5,2999)].And preparation process is loaded down with trivial details, consumes lot of energy, and the use of simultaneously a large amount of strong oxidizers causes very big harm to environment.[chemical Vapor deposition process prepares the Graphene network structure of the internal communication of three-dimension flexible and conduction to chemical Vapor deposition process (CVD) in " bottom-up " approach, " nature material ", 2011, the 10th volume, the 424th page of (Three-dimensional Flexible and Conductive Interconnected Graphene Networks Grown by Chemical Vapour Deposition, Nat. Mater., 2011, Vol. 10,424)] can obtain high-quality minority layer even single-layer graphene, but requirement for experiment condition harshness, and need in aftertreatment, use strong acid etc. to remove template, not have advantage in magnanimity aspect synthetic.Therefore, desire breaks through the synthetic bottleneck of Graphene magnanimity, must research and develop new building-up process, under the situation of not using template, makes the directed spontaneous growth of carbon atom two dimension, and adopts the intrinsic technological method to suppress the accumulation of Graphene.Stride etc. are the pre-treatment of raw material process solution heat with ethanol and sodium, and incomplete combustion in air atmosphere obtains Graphene through supersound process then.[based on solvent thermal and the synthetic gram of ultrasonic procedure magnitude Graphene, " natural nanotechnology ", 2009, the Volume Four, the 30th page, (Gram-Scale Production of Graphene Based on Solvothermal Synthesis and Sonication, Nat. Nanotechnol, 2009, Vol. 4,30)].Christopher etc. then obtain sodium ethylate/ethanolic soln with sodium and excess ethyl alcohol reaction, obtain Graphene 900 ℃ of processing then.[utilize the synthetic minority layer graphene of approach mass-producing from bottom to top easily and graphene film; " materials chemistry magazine "; 2011; the 21st volume; the 3378th page; (Simple and Scalable Route for the ' Bottom-Up ' Synthesis of Few-Layer Graphene Platelets and Thin Films; J. Mater. Chem; 2011; Vol.21,3378)] though. these methods can obtain Graphene under the situation of not using template, need that all reactant is carried out pre-treatment and obtain intermediate; increase operating unit and preparation cost etc., aspect scale preparation, do not had advantage.
Summary of the invention
The purpose of this invention is to provide under a kind of no template situation, simple to operate, cost is low, has the method by the metal salts of organic acids synthesizing graphite alkene of scale preparation simultaneously.
Synthetic method of the present invention is raw material with the organic acid salt that contains metal, does not use template, need not raw material is carried out pre-treatment the one-step synthesis Graphene.The gained Graphene is three-dimensional net structure, when effectively suppressing the Graphene reunion, has kept its excellent performance.Simultaneously aspect scale preparation, has clear superiority.
Preparation method of the present invention is as follows:
(1) tube furnace is warmed up to 700-1300 ℃ in advance, and logical inert atmosphere protection;
(2) metal salts of organic acids is placed the tube furnace of using nitrogen protection, heating 0.5-120min, to be cooled to room temperature, obtain solid product.
(3) above-mentioned solid product washing, filtration, drying are obtained the Graphene product.
Described metal salts of organic acids comprises sodium acetate, Sodium Propionate, Sodium propanecarboxylate and Soduxin and potassium acetate, magnesium acetate, zinc acetate or venus crystals etc.
Described inert atmosphere is argon gas or nitrogen etc.
Described tube furnace is horizontal pipe furnace.
The present invention has following advantage:
(1) raw material such as used metal salts of organic acids is cheap and easy to get, need not pre-treatment, is conducive to reduce cost.
(2) the synthesis technique flow process is simple, and is easy and simple to handle, and influence factor is few, is convenient to control, favorable reproducibility.
(3) He Cheng Graphene can keep its pattern and not reunite.
(4) do not need additionally to introduce metal as substrate or template.
(5) be convenient to a large amount of synthesizing graphite alkenes of mass-producing.
Description of drawings
Fig. 1 is scanning electron microscope (SEM) photo of the synthetic Graphene of the embodiment of the invention 3 metal salts of organic acids pyrolysis.
Fig. 2 is Raman (Raman) spectrogram of the synthetic Graphene of the embodiment of the invention 3 metal salts of organic acids pyrolysis.
Fig. 3 is scanning electron microscope (SEM) photo of the synthetic Graphene of the embodiment of the invention 8 metal salts of organic acids pyrolysis.
Fig. 4 is Raman (Raman) spectrogram of the synthetic Graphene of the embodiment of the invention 8 metal salts of organic acids pyrolysis.
Fig. 5 is scanning electron microscope (SEM) photo of the synthetic Graphene of the embodiment of the invention 11 metal salts of organic acids pyrolysis.
Fig. 6 is Raman (Raman) spectrogram of the synthetic Graphene of the embodiment of the invention 11 metal salts of organic acids pyrolysis.
Embodiment
Embodiment 1
2g sodium acetate solid is positioned in the porcelain boat, is placed on the normal temperature district of the horizontal pipe furnace of nitrogen atmosphere protection.After treating that tube furnace is warmed up to 700 ℃, porcelain boat is pushed the flat-temperature zone, reaction 120min.After treating the product cooling, product is taken out, use deionized water wash, filter, drying is collected product.XPS analysis result shows that oxygen level is the 10%(atomic percent), scanning electron microscope show sample as a result is laminated structure, graphene-based lamellar spacing～4 nm.
Embodiment 2
2g sodium acetate solid is positioned in the porcelain boat, is placed on the normal temperature district of the horizontal pipe furnace of nitrogen atmosphere protection.After treating that tube furnace is warmed up to 1300 ℃, porcelain boat is pushed the flat-temperature zone, reaction 0.5min.After treating the product cooling, product is taken out, use deionized water wash, filter, drying is collected product.XPS analysis result shows that oxygen level is the 7%(atomic percent), scanning electron microscope show sample as a result is network structure, graphene-based lamellar spacing～2.2 nm
Embodiment 3
1.5g potassium acetate solid is positioned in the porcelain boat, is placed on the normal temperature district of the horizontal pipe furnace of argon atmospher protection.After treating that tube furnace is warmed up to 1000 ℃, porcelain boat is pushed the flat-temperature zone, reaction 2min.After treating the product cooling, product is taken out, use deionized water wash, filter, drying is collected product.XPS analysis result shows that oxygen level is the 7.0%(atomic percent), scanning electron microscope is the network-like structure of show sample as a result, graphene-based lamellar spacing～4.5 nm.
Embodiment 4
2g Sodium propanecarboxylate solid is positioned in the porcelain boat, is placed on the normal temperature district of the horizontal pipe furnace of argon atmospher protection.After treating that tube furnace is warmed up to 800 ℃, porcelain boat is pushed the flat-temperature zone, reaction 30min.After treating the product cooling, product is taken out, use deionized water wash, filter, drying is collected product.XPS analysis result shows that oxygen level is the 10%(atomic percent), scanning electron microscope show sample as a result is laminar structured, graphene-based lamellar spacing～5 nm.
Embodiment 5
2g Sodium Propionate solid is positioned in the porcelain boat, is placed on the normal temperature district of the horizontal pipe furnace of argon atmospher protection.After treating that tube furnace is warmed up to 800 ℃, porcelain boat is pushed the flat-temperature zone, reaction 100min.After treating the product cooling, product is taken out, use deionized water wash, filter, drying is collected product.XPS analysis result shows that oxygen level is the 9.5%(atomic percent), scanning electron microscope show sample as a result is laminar structured, graphene-based lamellar spacing～4.5 nm.
Embodiment 6
2g venus crystals solid is positioned in the porcelain boat, is placed on the normal temperature district of the horizontal pipe furnace of argon atmospher protection.After treating that tube furnace is warmed up to 1150 ℃, porcelain boat is pushed the flat-temperature zone, reaction 5min.After treating the product cooling, product is taken out, use deionized water wash, filter, drying is collected product.XPS analysis result shows that oxygen level is the 6.5%(atomic percent), scanning electron microscope is the network-like structure of show sample as a result, graphene-based lamellar spacing～4.0 nm.
Embodiment 7
2g Soduxin solid is positioned in the porcelain boat, is placed on the normal temperature district of the horizontal pipe furnace of argon atmospher protection.After treating that tube furnace is warmed up to 700 ℃, porcelain boat is pushed the flat-temperature zone, reaction 50min.After treating the product cooling, product is taken out, use deionized water wash, filter, drying is collected product.XPS analysis result shows that oxygen level is the 8.5%(atomic percent), scanning electron microscope show sample as a result is laminar structured, graphene-based lamellar spacing～3.5 nm.
Embodiment 8
2g zinc acetate solid is positioned in the porcelain boat, is placed on the normal temperature district of the horizontal pipe furnace of argon atmospher protection.After treating that tube furnace is warmed up to 900 ℃, porcelain boat is pushed the flat-temperature zone, reaction 2min.After treating the product cooling, product is taken out, use deionized water wash, filter, drying is collected product.XPS analysis result shows that oxygen level is the 8.8%(atomic percent), scanning electron microscope is the network-like structure of show sample as a result, graphene-based lamellar spacing～5.5 nm.
Embodiment 9
2g venus crystals solid is positioned in the porcelain boat, is placed on the normal temperature district of the horizontal pipe furnace of argon atmospher protection.After treating that tube furnace is warmed up to 1100 ℃, porcelain boat is pushed the flat-temperature zone, reaction 2min.After treating the product cooling, product is taken out, use deionized water wash, filter, drying is collected product.XPS analysis result shows that oxygen level is the 8.5%(atomic percent), scanning electron microscope is the network-like structure of show sample as a result, graphene-based lamellar spacing～5.5 nm.
Embodiment 10
2g Sodium Propionate solid is positioned in the porcelain boat, is placed on the normal temperature district of the horizontal pipe furnace of argon atmospher protection.After treating that tube furnace is warmed up to 1200 ℃, porcelain boat is pushed the flat-temperature zone, reaction 1.5min.After treating the product cooling, product is taken out, use deionized water wash, filter, drying is collected product.XPS analysis result shows that oxygen level is the 6.5%(atomic percent), scanning electron microscope is the network-like structure of show sample as a result, graphene-based lamellar spacing～3.0 nm.
Embodiment 11
2g Soduxin solid is positioned in the porcelain boat, is placed on the normal temperature district of the horizontal pipe furnace of argon atmospher protection.After treating that tube furnace is warmed up to 1000 ℃, porcelain boat is pushed the flat-temperature zone, reaction 2.5min.After treating the product cooling, product is taken out, use deionized water wash, filter, drying is collected product.XPS analysis result shows that oxygen level is the 7.5%(atomic percent), scanning electron microscope is the network-like structure of show sample as a result, graphene-based lamellar spacing～4.8nm.
Embodiment 12
2g magnesium acetate solid is positioned in the porcelain boat, is placed on the normal temperature district of the horizontal pipe furnace of argon atmospher protection.After treating that tube furnace is warmed up to 1050 ℃, porcelain boat is pushed the flat-temperature zone, reaction 1min.After treating the product cooling, product is taken out, use deionized water wash, filter, drying is collected product.XPS analysis result shows that oxygen level is the 8.5%(atomic percent), scanning electron microscope is the network-like structure of show sample as a result, graphene-based lamellar spacing～3.5 nm.
Claims (4)
1. the method by the metal salts of organic acids synthesizing graphite alkene is characterized in that comprising the steps:
Tube furnace is warmed up to 700-1300 ℃ in advance, and logical inert atmosphere protection;
(2) metal salts of organic acids is placed the tube furnace of using nitrogen protection, heating 0.5-120min, to be cooled to room temperature, obtain solid product;
(3) above-mentioned solid product washing, filtration, drying are obtained the Graphene product.
2. a kind of method by the metal salts of organic acids synthesizing graphite alkene as claimed in claim 1 is characterized in that described metal salts of organic acids is sodium acetate, Sodium Propionate, Sodium propanecarboxylate, Soduxin, potassium acetate, magnesium acetate, zinc acetate or venus crystals.
3. a kind of method by the metal salts of organic acids synthesizing graphite alkene as claimed in claim 1 is characterized in that described inert atmosphere is argon gas or nitrogen.
4. a kind of method by the metal salts of organic acids synthesizing graphite alkene as claimed in claim 1 is characterized in that described tube furnace is horizontal pipe furnace.
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| CN103601178A (en) * | 2013-11-19 | 2014-02-26 | 中国科学院山西煤炭化学研究所 | Method for synthesizing graphene from solid organic acid |
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| C06 | Publication | ||
| PB01 | Publication | ||
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