CN105502365A - Method for preparing graphene by controlling thickness of primary carbon source - Google Patents
Method for preparing graphene by controlling thickness of primary carbon source Download PDFInfo
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- CN105502365A CN105502365A CN201511008374.9A CN201511008374A CN105502365A CN 105502365 A CN105502365 A CN 105502365A CN 201511008374 A CN201511008374 A CN 201511008374A CN 105502365 A CN105502365 A CN 105502365A
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Abstract
The invention discloses a method for preparing graphene by controlling thickness of a primary carbon source. In the method, by adopting graphene quantum dots as a growth template, the graphene quantum dots are dispersed into gelatinized starch; by means of high energy provided by high temperature and high pressure, carbon atoms obtained by decomposing a carbon organic material are arranged at an edge position of a graphite layer to grow out a larger graphene slice layer; moreover, by controlling a layer number of the primary graphene quantum dots, the graphene quantum dots of a corresponding layer number can be obtained is a controllable manner. The method is simple to operate, and is suitable for large-scale production and popularization.
Description
Technical field
The present invention relates to technical field of nanometer material preparation, particularly a kind of method preparing Graphene by controlling primary carbon source thickness.
Background technology
Graphene is the Two-dimensional Carbon atomic crystal in recent years found, is one of the study hotspot in current carbonaceous material and Condensed Matter Physics field.Graphene constructs the sp such as zero dimension soccerballene, one dimension carbon nanotube, said three-dimensional body phase graphite
2the basic structural unit of hydridization carbon.Although Graphene only has a carbon atom thickness, be also that oneself knows one the thinnest in material, but Graphene very rigid.In addition, carbon atom has four valence electrons, and each like this carbon atom can contribute the π-electron of a non-Cheng Jian, and these π-electrons become vertical direction can form π track with plane, π-electron then can move freely in crystal, gives the electroconductibility that Graphene is good.The characteristic of these excellences makes Graphene have very vast potential for future development.
As everyone knows, the number of plies meeting influence power, heat, the optical, electrical performance of Graphene, and the number of plies controlling Graphene is also just very most important.Section of China Patent Publication No. 103265021A China provides a kind of growth method of number of plies controllable grapheme, first prepare Ni/Cu system, and utilize ion implantation technique to introduce carbon source, by accurately controlling the dosage injecting carbon, successfully achieve the regulation and control to the Graphene number of plies.The graphene film that this invention obtains has that quality is good, large size and the controlled advantage of the number of plies, and is easy to transfer.In addition, ion implantation technique, annealing technology are all very ripe technique at current semicon industry, and the growth method of the number of plies controllable grapheme of this invention can promote the widespread use of Graphene in semi-conductor industry circle quickly.But the method is for the large application of ultracapacitor, energy-storage battery Graphene consumption, and the method cost is too high, is unfavorable for scale operation.
China Patent Publication No. 102492926A provides the preparation method of a kind of local monoatomic-layer graphene film, concrete steps are: the first step, being placed in by multi-layer graphene film on carrier table makes part to be processed unsettled, is then positioned in transmission electron microscope by carrier table; Second step, is elevated to 300-1300 DEG C by multi-layer graphene film temperature, utilizes current density to be greater than 1 × 10
2a/cm
2the multi-layer graphene film surface of convergence high-energy electron beam irradiation part to be processed, and continue 1-60 minute, the top layer carbon atom making the multi-layer graphene film of part to be processed, constantly by bombardment sputtering, is successively peeled off and is finally formed minority layer even individual layer and the Graphene of high crystalline.The thickness of Graphene and the area of single-layer graphene control by regulating the time of the beam diameter of electron beam, current density and electron beam irradiation.The method uses electron beam irradiation to peel off multilayer carbon atom, and obtain single-layer graphene, the method is a kind of operation of atomic level, and equipment is complicated, and technology difficulty is large.
China Patent Publication No. 104485310A provides a kind of method forming Graphene interconnection line, and it comprises the following steps: provide target substrate; Then in target substrate, form even and that thickness is controlled carbon source layer; Depositing metal Catalytic Layer on carbon source layer; Then under preset temp, adopt annealing process that the carbon source layer of deposit is converted into graphene layer; Remove metal catalytic layer subsequently; Finally adopt photoetching and etching technics to graphene layer patterning, to form Graphene interconnection line.A kind of method controlling carbon source layer thickness that this invention provides controls the thickness of Graphene, and method is simple.But the carbon source layer related in the program and layer metal deposition, whole process is equivalent to allow carbon atom resequence and obtains Graphene, cost intensive.
It is high to there is cost in present existing scheme, complex process, the shortcoming that operation easier is large.Therefore, also do not have at present a kind of cost low, eco-friendly, control Graphene expeditiously.
Summary of the invention
In order to solve deficiency and the defect of aforesaid method, the present invention develops a kind of method preparing Graphene by controlling primary carbon source thickness.Because the monolayer carbon atom of graphene quantum dot does not have dangling bonds in layer, the dangling bonds of carbon atom are all at mono-layer graphite edge.Therefore, when high-energy carbon atom is in mono-layer graphite surface diffusion, can stops at edge, help graphene quantum dot marginal growth, obtain larger Graphene.So, by controlling the number of plies of graphene quantum dot, the thickness of last Graphene just can be controlled.Described method adopts graphene quantum dot as growth templates, graphene quantum dot is dispersed in pasted starch, by the high-energy that High Temperature High Pressure provides, the carbon atom arrangement that decomposition carbon element organic materials obtains, to graphite linings marginal position, grows larger graphene sheet layer.Described method is simple to operate, by controlling the number of plies of starting graphite alkene quantum dot, and the graphene quantum dot of the corresponding number of plies of controlled acquisition.
The invention provides a kind of method preparing Graphene by controlling primary carbon source thickness, it is characterized in that, said method comprising the steps of:
A. carbon element organic materials is pressed mass ratio 5-10:1 with few layer graphite quantum to mix, add stirrer, stir, mix with deionized water, obtain mixing solutions, keep whipped state;
B. in the solution of step a acquisition, add pre-gelatinized starch, the weight of pre-gelatinized starch is 2-5 times of deionized water, adds catalyzer, stirs, obtain carbon element gelatinized mixture;
C. under protection of inert gas, the carbon element gelatinized mixture that step b obtains is added high-temperature high-pressure reaction kettle, and temperature in the kettle is 500-800 DEG C, and pressure is 20-50MPa, process 1-3h, and obtain solid product, this solid product is the pre-powder process of Graphene;
D. pre-for Graphene powder process is put into dimethyl formamide liquid, ultrasonic separation 30-60 minute, centrifugal, get supernatant liquid, obtain Graphene.
Wherein, described few layer graphite quantum dot is 1-10 carbon atomic layer thickness, the graphite flake of sheet footpath within 100nm.
Optionally, a kind of method preparing Graphene by controlling primary carbon source thickness according to claim 1, it is characterized in that, described carbon element organic materials is starch based, Mierocrystalline cellulose, xylogen and decolorizing carbon.
Optionally, a kind of method preparing Graphene by controlling primary carbon source thickness according to claim 1, it is characterized in that, described stirrer stirring velocity is 500-1500r/min.
Optionally, a kind of method preparing Graphene by controlling primary carbon source thickness according to claim 1, it is characterized in that, described rare gas element is nitrogen, carbonic acid gas, argon gas, helium.
Optionally, a kind of method preparing Graphene by controlling primary carbon source thickness according to claim 1, it is characterized in that, the part by weight of the pre-powder process of described Graphene and dimethyl formamide liquid is 1-3:10.
Above-mentioned one or more technical scheme in the embodiment of the present application, at least has one or more technique effects following:
1, this kind of method adopts graphene quantum dot as growth templates, graphene quantum dot is dispersed in pasted starch, by the high-energy that High Temperature High Pressure provides, the carbon atom arrangement that decomposition carbon element organic materials obtains, to graphite linings marginal position, grows larger Graphene synusia.Moreover, by controlling the number of plies of starting graphite alkene quantum dot, the graphene quantum dot of the corresponding number of plies of controlled acquisition.
2, the equipment of this kind of method employing is that conventional nano prepares industrial equipments, and simple to operate, quality product is controlled, with low cost, is applicable to scale operation and popularizes.
3, this kind of method adopts carbon element organic materials as carbon source, draws materials extensively, is conducive to reducing production cost, is applicable to industrial production.
Embodiment
By embodiment, the present invention is described in further detail, but this should be interpreted as scope of the present invention is only limitted to following example.When not departing from aforesaid method thought of the present invention, the various replacement made according to ordinary skill knowledge and customary means or change, all should be within the scope of the present invention.
Embodiment one
The present embodiment preparation process is as follows:
Get carbon element organic materials wheat starch 500g to press quality 100g with few layer graphite quantum and mix, few layer graphite quantum dot is 1 carbon atomic layer thickness, and sheet footpath is the graphite flake of 20nm.Said mixture is added stirrer, and arranging stirrer stirring velocity is 500r/min, stirs, and adds 1L deionized water, obtains mixing solutions, keeps whipped state.In above-mentioned solution, add 2kg pre-gelatinized starch, add catalyzer, stir, obtain carbon element gelatinized mixture.Under inert nitrogen gas protection, carbon element gelatinized mixture is added high-temperature high-pressure reaction kettle, controlling temperature in the kettle is 500 DEG C, and pressure is 20MPa, and process 1h, obtain solid product, this solid product is the pre-powder process of Graphene.Get the pre-powder process of 1kg Graphene and 3kg dimethyl formamide liquid, dimethyl formamide liquid is put in pre-for Graphene powder process, ultrasonic separation 30 minutes, centrifugal, get supernatant liquid, obtain Graphene.
After tested, the Graphene that embodiment one prepares is of a size of 2.09 μm (selected area sizes), and thickness is 0.53nm, and productive rate is 1.5%.
Embodiment two
Get carbon element organic materials wheat starch 500g to press quality 100g with few layer graphite quantum and mix, few layer graphite quantum dot is 3 carbon atomic layer thickness, and sheet footpath is the graphite flake of 20nm.Said mixture is added stirrer, and arranging stirrer stirring velocity is 500r/min, stirs, and adds 1L deionized water, obtains mixing solutions, keeps whipped state.In above-mentioned solution, add 2kg pre-gelatinized starch, add catalyzer, stir, obtain carbon element gelatinized mixture.Under inert nitrogen gas protection, carbon element gelatinized mixture is added high-temperature high-pressure reaction kettle, controlling temperature in the kettle is 500 DEG C, and pressure is 20MPa, and process 1h, obtain solid product, this solid product is the pre-powder process of Graphene.Get the pre-powder process of 1kg Graphene and 3kg dimethyl formamide liquid, dimethyl formamide liquid is put in pre-for Graphene powder process, ultrasonic separation 30 minutes, centrifugal, get supernatant liquid, obtain Graphene.
The Graphene prepared is of a size of 3.23 μm (selected area sizes), and thickness is 1.02nm, and productive rate is 1.7%.
Embodiment three
Get carbon element organic materials wheat starch 500g to press quality 100g with few layer graphite quantum and mix, few layer graphite quantum dot is 6 carbon atomic layer thickness, and sheet footpath is the graphite flake of 20nm.Said mixture is added stirrer, and arranging stirrer stirring velocity is 500r/min, stirs, and adds 1L deionized water, obtains mixing solutions, keeps whipped state.In above-mentioned solution, add 2kg pre-gelatinized starch, add catalyzer, stir, obtain carbon element gelatinized mixture.Under inert nitrogen gas protection, carbon element gelatinized mixture is added high-temperature high-pressure reaction kettle, controlling temperature in the kettle is 500 DEG C, and pressure is 20MPa, and process 1h, obtain solid product, this solid product is the pre-powder process of Graphene.Get the pre-powder process of 1kg Graphene and 3kg dimethyl formamide liquid, dimethyl formamide liquid is put in pre-for Graphene powder process, ultrasonic separation 30 minutes, centrifugal, get supernatant liquid, obtain Graphene.
After tested, the Graphene that embodiment three prepares is of a size of 2.09 μm (selected area sizes), and thickness is 2.17nm, and productive rate is 1.5%.
Embodiment four
Get carbon element organic materials xylogen 500g to press quality 100g with few layer graphite quantum and mix, few layer graphite quantum dot is 6 carbon atomic layer thickness, and sheet footpath is the graphite flake of 20nm.Said mixture is added stirrer, and arranging stirrer stirring velocity is 1000r/min, stirs, and adds 1L deionized water, obtains mixing solutions, keeps whipped state.In above-mentioned solution, add 2kg pre-gelatinized starch, add catalyzer, stir, obtain carbon element gelatinized mixture.Under inert nitrogen gas protection, carbon element gelatinized mixture is added high-temperature high-pressure reaction kettle, controlling temperature in the kettle is 700 DEG C, and pressure is 50MPa, and process 1h, obtain solid product, this solid product is the pre-powder process of Graphene.Get the pre-powder process of 1kg Graphene and 5kg dimethyl formamide liquid, dimethyl formamide liquid is put in pre-for Graphene powder process, ultrasonic separation 30 minutes, centrifugal, get supernatant liquid, obtain Graphene.
After tested, the Graphene that embodiment four prepares is of a size of 4.01 μm (selected area sizes), and thickness is 1.97nm, and productive rate is 1.2%.
Embodiment five
Get carbon element organic materials xylogen 500g to press quality 100g with few layer graphite quantum and mix, few layer graphite quantum dot is 6 carbon atomic layer thickness, and sheet footpath is the graphite flake of 20nm.Said mixture is added stirrer, and arranging stirrer stirring velocity is 1500r/min, stirs, and adds 1L deionized water, obtains mixing solutions, keeps whipped state.In above-mentioned solution, add 5kg pre-gelatinized starch, add catalyzer, stir, obtain carbon element gelatinized mixture.Under inert nitrogen gas protection, carbon element gelatinized mixture is added high-temperature high-pressure reaction kettle, controlling temperature in the kettle is 700 DEG C, and pressure is 50MPa, and process 3h, obtain solid product, this solid product is the pre-powder process of Graphene.Get the pre-powder process of 1kg Graphene and 5kg dimethyl formamide liquid, dimethyl formamide liquid is put in pre-for Graphene powder process, ultrasonic separation 30 minutes, centrifugal, get supernatant liquid, obtain Graphene.
After tested, the Graphene that embodiment five prepares is of a size of 1.59 μm (selected area sizes), and thickness is 2.21nm, and productive rate is 1.3%.
Although describe the preferred embodiments of the present invention, those skilled in the art once obtain the basic creative concept of cicada, then can make other change and amendment to these embodiments.So claims are intended to be interpreted as comprising preferred embodiment and falling into all changes and the amendment of the scope of the invention.
Obviously, those skilled in the art can carry out various change and modification to the present invention and not depart from the spirit and scope of the present invention.Like this, if these amendments of the present invention and modification belong within the scope of the claims in the present invention and equivalent technologies thereof, then the present invention is also intended to comprise these change and modification.
Claims (5)
1. preparing a method for Graphene by controlling primary carbon source thickness, it is characterized in that, said method comprising the steps of:
A. carbon element organic materials is pressed mass ratio 5-10:1 with few layer graphite quantum to mix, add stirrer, stir, mix with deionized water, obtain mixing solutions, keep whipped state;
B. in the solution of step a acquisition, add pre-gelatinized starch, the weight of pre-gelatinized starch is 2-5 times of deionized water, adds catalyzer, stirs, obtain carbon element gelatinized mixture;
C. under protection of inert gas, the carbon element gelatinized mixture that step b obtains is added high-temperature high-pressure reaction kettle, and temperature in the kettle is 500-800 DEG C, and pressure is 20-50MPa, process 1-3h, and obtain solid product, this solid product is the pre-powder process of Graphene;
D. pre-for Graphene powder process is put into dimethyl formamide liquid, ultrasonic separation 30-60 minute, centrifugal, get supernatant liquid, obtain Graphene;
Wherein, described few layer graphite quantum dot is 1-10 carbon atomic layer thickness, the graphite flake of sheet footpath within 100nm.
2. a kind of method preparing Graphene by controlling primary carbon source thickness according to claim 1, it is characterized in that, described carbon element organic materials is starch based, Mierocrystalline cellulose, xylogen and decolorizing carbon.
3. a kind of method preparing Graphene by controlling primary carbon source thickness according to claim 1, it is characterized in that, described stirrer stirring velocity is 500-1500r/min.
4. a kind of method preparing Graphene by controlling primary carbon source thickness according to claim 1, it is characterized in that, described rare gas element is nitrogen, carbonic acid gas, argon gas, helium.
5. a kind of method preparing Graphene by controlling primary carbon source thickness according to claim 1, it is characterized in that, the part by weight of the pre-powder process of described Graphene and dimethyl formamide liquid is 1-3:10.
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| Publication number | Priority date | Publication date | Assignee | Title |
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| CN106365152A (en) * | 2016-08-31 | 2017-02-01 | 南通绿业中试技术研究院有限公司 | Preparation method of graphene nanosheet |
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| CN104528696A (en) * | 2014-12-16 | 2015-04-22 | 中国科学院宁波材料技术与工程研究所 | Preparation method for graphene and graphene |
| CN105060288A (en) * | 2015-09-21 | 2015-11-18 | 中南大学 | Method for preparing graphene from biomass waste |
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| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN104016341A (en) * | 2014-07-01 | 2014-09-03 | 济南圣泉集团股份有限公司 | Preparation method of porous graphene |
| CN104528696A (en) * | 2014-12-16 | 2015-04-22 | 中国科学院宁波材料技术与工程研究所 | Preparation method for graphene and graphene |
| CN105060288A (en) * | 2015-09-21 | 2015-11-18 | 中南大学 | Method for preparing graphene from biomass waste |
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| Publication number | Priority date | Publication date | Assignee | Title |
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| CN106365152A (en) * | 2016-08-31 | 2017-02-01 | 南通绿业中试技术研究院有限公司 | Preparation method of graphene nanosheet |
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Application publication date: 20160420 |