CN106744872A - A kind of preparation method of the multi-layer graphene nanometer sheet of the boron hydride that adulterates - Google Patents
A kind of preparation method of the multi-layer graphene nanometer sheet of the boron hydride that adulterates Download PDFInfo
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- CN106744872A CN106744872A CN201611087679.8A CN201611087679A CN106744872A CN 106744872 A CN106744872 A CN 106744872A CN 201611087679 A CN201611087679 A CN 201611087679A CN 106744872 A CN106744872 A CN 106744872A
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- C01B3/00—Hydrogen; Gaseous mixtures containing hydrogen; Separation of hydrogen from mixtures containing it; Purification of hydrogen
- C01B3/0005—Reversible uptake of hydrogen by an appropriate medium, i.e. based on physical or chemical sorption phenomena or on reversible chemical reactions, e.g. for hydrogen storage purposes ; Reversible gettering of hydrogen; Reversible uptake of hydrogen by electrodes
- C01B3/001—Reversible uptake of hydrogen by an appropriate medium, i.e. based on physical or chemical sorption phenomena or on reversible chemical reactions, e.g. for hydrogen storage purposes ; Reversible gettering of hydrogen; Reversible uptake of hydrogen by electrodes characterised by the uptaking medium; Treatment thereof
- C01B3/0078—Composite solid storage mediums, i.e. coherent or loose mixtures of different solid constituents, chemically or structurally heterogeneous solid masses, coated solids or solids having a chemically modified surface region
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- C01P2002/01—Crystal-structural characteristics depicted by a TEM-image
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- C01P2004/03—Particle morphology depicted by an image obtained by SEM
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- Y02E—REDUCTION OF GREENHOUSE GAS [GHG] EMISSIONS, RELATED TO ENERGY GENERATION, TRANSMISSION OR DISTRIBUTION
- Y02E60/00—Enabling technologies; Technologies with a potential or indirect contribution to GHG emissions mitigation
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Abstract
The invention discloses a kind of preparation method of the multi-layer graphene nanometer sheet of the boron hydride that adulterates, belong to the synthesis technical field of grapheme material.The preparation method specifically includes following steps：A certain proportion of alkali halide, boron hydride and carbon material are chosen as initiation material, the pre- ball-milling treatment of difference；By alkali halide and boron hydride and carbon material mechanical mixture；Under mechanical force inducing action, there is chemical reaction generation alkali metal borohydride in above-mentioned alkali halide with boron hydride, while between inserting carbon material interlayer, graphene nanometer sheet is obtained so as to realize that solid-state is peeled off.Raw material sources of the present invention are extensively, inexpensive, preparation method be simple, environmentally friendly, prepared by easy scale, the graphene product of the doping boron hydride for obtaining has high capacitance and excellent chemical property, is had a wide range of applications in many new energy such as solar cell, aerospace material, photoelectric device, field emmision material, energy storage material, field of new.
Description
Technical field
The invention belongs to the synthesis technical field of grapheme material, and in particular to a kind of mechanical force drives in-situ preparation alkali gold
The method that category boron hydride insertion carbon material prepares multi-layer graphene nanometer sheet.
Background technology
2004, Univ Manchester UK Andre and Novoselov peeled off the mode of graphite using adhesive tape, first
To single-layer graphene.Since then, Graphene receives much concern and studies as a kind of new carbon, it be by carbon monoatomic layer or
The bi-dimensional cellular shape network structure that the several monoatomic layers of person are constituted, its basic structural unit is benzene hexatomic ring.Graphene has height
The excellent performance such as translucency and electric conductivity, high strength flexible and high-specific surface area, is expected in solar cell, Aero-Space
Many new energy such as material, photoelectric device, field emmision material, energy storage material, field of new are widely applied.But it is high
A large amount of preparation costs of the Graphene of quality are too high, constrain the large-scale application of the material.
At present, the preparation method of Graphene is summed up, and has micromechanics stripping method, chemical vapour deposition technique (CVD), reduction
Graphite oxide method etc..Micromechanics stripping method is the method for preparing Graphene earliest, is using the bonding force of adhesive tape, by taking off repeatedly
Tear a Graphene to be separated from directional thermal decomposition graphite, (K.S.Noveselov, et al.Science, 306,666 (2004)), most
Adhesive tape is removed so as to obtain the Graphene of individual layer or few layer with acetone equal solvent afterwards.The method can prepare high-quality graphene,
But time and effort consuming cannot large-scale application.Chemical vapour deposition technique is, by the use of carbon compounds such as methane as carbon source, to pass through
It grows Graphene (Jessica Campos-Delgado, et al.Nano Letters, 8,9 in matrix surface pyrolytic
(2008)).The method can prepare larger-size grapheme material, but the too high and prepared Graphene of preparation cost
The uncontrollable number of plies, and then limit the application of this method.Reduction-oxidation graphite method is largely to prepare the main flow side of Graphene at present
Method.The method first prepares graphite oxide first with graphite powder as raw material using methods such as Hummers, is then obtained by stripping
Graphene oxide, Graphene (Vincent C, et al.Nat Nanotech, 4,25 are obtained finally by redox graphene
(2008)).Oxidation-reduction method prepares the most easy method of Graphene with its technique simple and easy to apply as laboratory, but oxygen
The shortcoming for changing reducing process is that a large amount of preparation easily brings waste liquor contamination to there is fault of construction with the Graphene for preparing.Such as five yuan
There is oxide group in the topological defects such as ring, heptatomic ring, this can cause Graphene electrical property loss of energy, make the application of Graphene
It is restricted.
To solve the problems, such as above-mentioned preparation method, it is as follows to there are Patents in the country.China Patent No.：
20111028370.5, patent name：A kind of method for preparing high-quality graphene.The method is one kind with halogen or metal halogen
Compound is raw material for the graphite intercalation compound of intercalator, is expanded using oxalic acid or hydrogenperoxide steam generator, then ultrasound stripping
From preparing Graphene.The method can only realize prepared by the Graphene of single batch hectogram level.China Patent No.：
200910084879.1, patent name：The preparation method of Graphene.The method is by CNT and oxidant in ionic liquid
Middle reaction prepares Graphene.But the method easily introduces fault of construction in Graphene causes electric property relatively low.It can be seen that, at present
The technical costs for preparing Graphene is high, complex process is not met by industrial requirement.
The content of the invention
Pass through mechanical ball mill with carbon material using in-situ preparation alkali metal borohydride present invention aim at one kind is provided
The method for preparing multi-layer graphene nanometer sheet, to easily single batch prepare substantial amounts of Graphene and receive using after the present invention
Rice piece.
A kind of method for preparing multi-layer graphene nanometer sheet that the present invention is provided, specifically includes following steps：
(1) alkali halide MX, boron hydride and each one kind of carbon material are taken, and is pre-processed respectively；
(2) alkali halide and boron hydride and carbon material are pre-mixed；
The alkali halide is 1 with boron hydride mol ratio:1, the carbon material addition is mixture gross mass
5~20%；
(3) mixture as obtained by the method for mechanical ball mill acts on step (2), alkali halide MX and hydroboration
There is chemical reaction generation alkali metal borohydride MBH in thing4, while in inserting carbon material interlayer, so as to obtain a nanometer hydroboration
Multi-layer graphene nanometer sheet of the thing uniform load on graphite flake layer.
Further, the alkali halide MX is the first main group alkali metal halide, wherein M=Li, Na, K,
Ru；X=F, Cl, Br, I.
Further, the boron hydride is LiBH4、NaBH4、KBH4、Ca(BH4)2With Mg (BH4)2In any one.
Further, the carbon material include artificial/natural graphite powder, expanded graphite, onion carbon, multi-walled carbon nano-tubes with
And any one in stratiform carbide.
Further, the pretreatment of the step (1) is：Alkali halide needs ball milling into nano-sized powders；Boron
Hydride needs ball milling powdered；Carbon material needs to carry out ball milling to reach micron-scale.
Further, the parameter of step (3) mechanical ball mill is set to：Ratio of grinding media to material 30：1, rotational speed of ball-mill is 400rpm,
Ball-milling Time is 5~10h.
It is related to alkali halide MX in the step (3) with boron hydride reaction in-situ preparation alkali metal borohydride
Process.The energy of course of reaction derives from the energy that outside mechanical ball mill is produced.Related reaction equation is：MX+NBH4→
MBH4+NX
Inventor thinks to make alkali halide MX that displacement reaction occur with boron hydride by high-energy mechanical ball milling
In-situ preparation MBH4, raw material are cubic crystal and dispersed are presented before reaction, the product after high-energy mechanical ball milling reacts
Smooth and continuity surface is presented, the change of microscopic appearance may certify that the carrying out of this displacement reaction.
MX and LiBH4There is the ultra-fine size alkali metal borohydride MBH of displacement reaction generation4Nanocrystal.And due to changing
The carrying out of displacement reaction is learned, MBH is induced4Nano dot enters and is uniformly dispersed between graphite flake layer, expanded graphite meterial
Lamella generates graphene nanometer sheet.
Compared with prior art, the present invention has following technique effect：
1st, the preparation method raw material sources are extensively, inexpensive, preparation method be simple, environmentally friendly, prepared by easy scale；It is a kind of
Preparation method with promotional value, being capable of achieving multi-layer graphene nanometer sheet produce in batches, for energy storage.
2nd, the graphene product of the doping boron hydride obtained by the inventive method has high capacitance and excellent electrification
Performance is learned, in many new energy such as solar cell, aerospace material, photoelectric device, field emmision material, energy storage material, newly
Material Field has a wide range of applications.
Brief description of the drawings
Fig. 1 is the electron microscopic picture of the graphene nanometer sheet prepared by the embodiment of the present invention 1；
Wherein：The nanometer sheet of (a) superposition state；The nanometer sheet of (b) cleavage state completely；(c) nanometer sheet front elevation；(d) nanometer
Piece indulges face figure, and (a, b are SEM pictures；C, d are TEM pictures).
Fig. 2 is the KBH of the graphene nanometer sheet load prepared by the embodiment of the present invention 14With the KBH for being not added with graphite4It is de-
Hydrogen curve comparison figure.
Fig. 3 is the electron microscopic picture after the complete cleavage of graphene nanometer sheet prepared by the embodiment of the present invention 2；
Wherein：(a, b) SEM pictures；(c) TEM front elevations；D () TEM indulges face figure.
Fig. 4 is SEM picture of the graphene nanometer sheet prepared by the embodiment of the present invention 3 in different phase；
Wherein：(a) starting stage；B () inserts Cleaving Process；Nanoscale twins after (c, d) cleavage.
Specific embodiment
The present invention is described in more detail below by reference to embodiment, but protection scope of the present invention is not received
It is limited to these embodiments.
Embodiment 1 --- potassium borohydride inserts preparing graphite alkene nanometer sheet
Potassium chloride, lithium borohydride, graphite powder are carried out into pre- ball milling, concrete technology is as follows：Ratio of grinding media to material 40:1, rotating speed
200rpm, Ball-milling Time 10h.Potassium chloride/lithium borohydride is according to mol ratio 1：1 mixing, is subsequently adding the graphite powder of gross mass 5%
It is well mixed.It is 30 that ball milling parameter sets ratio of grinding media to material:1, rotational speed of ball-mill is 400rpm, and Ball-milling Time is 5h.As shown in figure 1, logical
This method is crossed, 5~7 layers of graphene nanometer sheet can be obtained, while potassium borohydride (its typical spacing of lattice d=0.301nm) adheres to
At graphene nanometer sheet (its typical spacing of lattice d=0.335nm).With pure KBH4Compare, prepared graphene nanometer sheet is born
The KBH of load4With more excellent hydrogen storage property, as shown in Figure 2.
Embodiment 2 --- sodium borohydride inserts preparing graphite alkene nanometer sheet
Sodium chloride, lithium borohydride, graphite powder are carried out into pre- ball milling, concrete technology is as follows：Ratio of grinding media to material 40:1, rotating speed
200rpm, Ball-milling Time 10h.Sodium chloride/lithium borohydride is according to mol ratio 1：1 mixing, is subsequently adding the graphite powder of gross mass 5%
It is well mixed.It is 30 that ball milling parameter sets ratio of grinding media to material：1, rotational speed of ball-mill is 400rpm, using batch (-type) rotating ball milling method,
Ball milling 30min interval 1min, Ball-milling Time is 10h altogether.As shown in figure 3, forming the graphene nano lamella with accordion, allusion quotation
Type example has 5~7 layers.
Embodiment 3 --- potassium borohydride insertion onion carbon prepares graphene nanometer sheet
Potassium chloride, lithium borohydride, onion carbon are carried out into pre- ball milling, concrete technology is as follows：Ratio of grinding media to material 40:1, rotating speed
200rpm, Ball-milling Time 10h.Potassium chloride/lithium borohydride is according to mol ratio 1：1 mixing, is subsequently adding the onion that gross mass is 5%
Carbon is well mixed.It is 30 that ball milling parameter sets ratio of grinding media to material:1, rotational speed of ball-mill is 400rpm, and Ball-milling Time is 5h.As shown in figure 4,
In reactant substrate, the Nano graphite lamella of fold sample is presented.
Claims (6)
1. it is a kind of adulterate boron hydride multi-layer graphene nanometer sheet preparation method, it is characterised in that comprise the following steps that：
(1) alkali halide MX, boron hydride and each one kind of carbon material are taken, and is pre-processed respectively；
(2) alkali halide and boron hydride and carbon material are pre-mixed；
The alkali halide is 1 with boron hydride mol ratio:1, the carbon material addition for mixture gross mass 5~
20%；
(3) mixture as obtained by the method for mechanical ball mill acts on step (2), alkali halide MX sends out with boron hydride
Biochemical reaction generation alkali metal borohydride MBH4, while in inserting carbon material interlayer, it is equal so as to obtain nanometer boron hydride
The even multi-layer graphene nanometer sheet being supported on graphite flake layer.
2. a kind of preparation method of the multi-layer graphene nanometer sheet of boron hydride that adulterates as claimed in claim 1, its feature exists
In, the alkali halide MX is the first main group alkali metal halide, wherein：M=Li, Na, K, Ru；X=F, Cl, Br,
I。
3. a kind of preparation method of the multi-layer graphene nanometer sheet of boron hydride that adulterates as claimed in claim 1, its feature exists
In the boron hydride is LiBH4、NaBH4、KBH4、Ca(BH4)2With Mg (BH4)2In any one.
4. a kind of preparation method of the multi-layer graphene nanometer sheet of boron hydride that adulterates as claimed in claim 1, its feature exists
In the carbon material is included in artificial/natural graphite powder, expanded graphite, onion carbon, multi-walled carbon nano-tubes and stratiform carbide
Any one.
5. a kind of preparation method of the multi-layer graphene nanometer sheet of boron hydride that adulterates as claimed in claim 1, its feature exists
In the pretreatment of the step (1) is：Alkali halide needs ball milling into nano-sized powders；Boron hydride needs ball milling
It is powdered；Carbon material needs to carry out ball milling to reach micron-scale.
6. a kind of preparation method of the multi-layer graphene nanometer sheet of boron hydride that adulterates as claimed in claim 1, its feature exists
In the parameter of step (3) mechanical ball mill is set to：Ratio of grinding media to material 30：1, rotational speed of ball-mill is 400rpm, Ball-milling Time is 5~
10h。
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Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
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| CN108163842A (en) * | 2018-01-23 | 2018-06-15 | 内蒙古农业大学 | A kind of preparation method and application of graphene nano pipe |
| CN111268642A (en) * | 2020-01-16 | 2020-06-12 | 长沙理工大学 | Sodium borohydride/nitrogen-doped graphene hydrogen storage composite material and preparation method thereof |
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| CN102219187A (en) * | 2010-04-15 | 2011-10-19 | 中国科学院大连化学物理研究所 | Preparation method for calcium borohydride hydrogen-storage material |
| CN102718183A (en) * | 2012-07-13 | 2012-10-10 | 常州大学 | High-hydrogen-storage-capacity lithium borohydride/graphene (LiBH4/RGO) composite hydrogen storage material and preparation method thereof |
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| CN102219187A (en) * | 2010-04-15 | 2011-10-19 | 中国科学院大连化学物理研究所 | Preparation method for calcium borohydride hydrogen-storage material |
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Cited By (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN108163842A (en) * | 2018-01-23 | 2018-06-15 | 内蒙古农业大学 | A kind of preparation method and application of graphene nano pipe |
| CN111268642A (en) * | 2020-01-16 | 2020-06-12 | 长沙理工大学 | Sodium borohydride/nitrogen-doped graphene hydrogen storage composite material and preparation method thereof |
| CN111268642B (en) * | 2020-01-16 | 2022-12-06 | 长沙理工大学 | Sodium borohydride/nitrogen-doped graphene hydrogen storage composite material and preparation method thereof |
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Application publication date: 20170531 |