CN108328585A - A kind of preparation method of boron nitride coated graphite alkene nanometer sheet - Google Patents
A kind of preparation method of boron nitride coated graphite alkene nanometer sheet Download PDFInfo
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- CN108328585A CN108328585A CN201810412566.3A CN201810412566A CN108328585A CN 108328585 A CN108328585 A CN 108328585A CN 201810412566 A CN201810412566 A CN 201810412566A CN 108328585 A CN108328585 A CN 108328585A
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- C01B21/00—Nitrogen; Compounds thereof
- C01B21/06—Binary compounds of nitrogen with metals, with silicon, or with boron, or with carbon, i.e. nitrides; Compounds of nitrogen with more than one metal, silicon or boron
- C01B21/064—Binary compounds of nitrogen with metals, with silicon, or with boron, or with carbon, i.e. nitrides; Compounds of nitrogen with more than one metal, silicon or boron with boron
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- C01P2002/80—Crystal-structural characteristics defined by measured data other than those specified in group C01P2002/70
- C01P2002/88—Crystal-structural characteristics defined by measured data other than those specified in group C01P2002/70 by thermal analysis data, e.g. TGA, DTA, DSC
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Abstract
The present invention is a kind of preparation method of boron nitride coated graphite alkene nanometer sheet.This method prepares boron nitride presoma using boric acid and melamine mixed liquor, under the addition of PVP K30, passes through presoma adhesion method so that boron nitride presoma graphene nano on piece be distributed more uniformly with extensively.In the present invention, the addition of surfactant is so that boron nitride presoma is more easy to be adhered to the surface of graphene nanometer sheet, and which greatly enhances the popularity of clad；With ammonia be sintering gas, can do reducibility gas again while nitrogen source is provided, so as to get product it is purer.
Description
Technical field
Technical solution of the present invention is related to a kind of preparation method of boron nitride coated graphite alkene nanometer sheet, by graphene nanometer sheet
Boric acid is put into the boron nitride precursor solution of melamine composition, after a series of processing, boron nitride coated graphite is made
Alkene nanosheet composite material, belongs to field of inorganic materials.
Background technology
Graphene (Graphene) be one kind by carbon atom with sp2Hydridization is in the Two-dimensional Carbon nanometer material of hexangle type honeycomb lattice
Material.Because it is with excellent electricity, optics and mechanical property, in material, the energy, biomedicine and drug delivery, micro-nano technology
Etc. have broad application prospects, it is considered to be one of revolutionary material of human future.But prepared by current industrial production
The cost of pure graphene is higher, complex process, and inexpensive substitute of the graphene nanometer sheet as pure graphene, has had both stone
The excellent electricity of black alkene, light and mechanical property, are widely used in field of industrial production.
Boron nitride (BN) is used as a kind of typical inorganic non-metallic material, has excellent thermal conductivity, corrosion resistance, electricity are absolutely
Edge, the advantages such as inoxidizability, chemical stability and thermal shock resistance are good, coefficient of thermal expansion is low are widely used in grinding material
The fields such as material, high temperature resistance material, high-temperature insulation material, heat enhancing additive, high-temperaure coating.Boron nitride is received with graphene
There is rice piece similar crystal structure, the high similarity of structure the two to be made easily to be combined matching and go to be nitrogenized
Boron coated graphite alkene nanosheet composite material.The synthesis of this composite material overcomes oxidizable under graphene nanometer sheet hot conditions
The shortcomings that, while improving graphene nanometer sheet antioxygenic property, and it is excellent with carbon material to combine boron nitride well
Heat conductivility has opened up extensive foreground and future for the extensive use under grapheme material high temperature.
Boron nitride coated graphite alkene technology of preparing has corresponding research report, such as：Shi gang et al. utilize CVD
(chemical vapour deposition technique) is prepared for the boron nitride in nanometer super capacitor device-Graphene electrodes monolayer material.(G.Shi,
Y.Hanlumyuang,Z.Liu,Y.J.Gong,Boron Nitride-Graphene Nanocapacitor and the
Origins of Anomalous Size-Dependent Increase of Capacitance,Nano Lett.14
(2014)1739-1744.)；Gao guanhui et al. are by the interaction between Van der Waals force using the method for liquid phase stripping
Prepare the boron nitride-graphene solid manually stacked.(G.Gao,W.Gao,E.Cannuccia,J.Taha,L.Balicas,
Artificially stacked atomic layers:towards new van derWaals solids,Nano
Lett.10(2013)1-21.)；Sun guoxun etc. are carrier using sodium borohydride-ammonium sulfate solution, in stainless steel high pressure
It is heat-treated in kettle system, has then synthesized boron nitride coating on functionalized redox graphene.(G.X.Sun,
J.Q.Bi,W.L.Wang,J.D.Zhang,One-pot synthesis ofreduced graphene oxide@boron
nitride nanosheet hybrids with enhanced oxidation-resistant properties,
Appl.Surf.Sci.8(2017)207.).However, above method is to the more demanding of equipment, operating method is complex, at
This is higher, and coated state and the uniformity coefficient of boron nitride are difficult to control, and are unfavorable for industrialized production.Thus, this patent provides
A kind of ease of Use method goes to prepare boron nitride coated graphite alkene nanosheet composite material, i.e., graphene nanometer sheet is added to boron
Acid in the mixed solution of melamine, form boron nitride coated graphite alkene nanometer sheet presoma, by presoma after drying and grinding
Powder high temperature sintering under ammonia atmosphere obtains boron nitride coated graphite alkene nanosheet composite material.The synthesis of the material not only makes
The antioxygenic property of graphene at high temperature greatly improves, and combines graphene nanometer sheet and the excellent thermal conductivity of boron nitride
Can, this greatly extends the application under graphene nanometer sheet hot conditions.
Invention content
The purpose of the present invention is to provide a kind of of low cost, easy to operate, property for deficiency present in current techniques
The preparation method of the excellent boron nitride coated graphite alkene nanosheet composite material of energy.The present invention is mixed using boric acid with melamine
Liquid prepares boron nitride presoma, under the addition of PVP K30, passes through presoma adhesion method so that before boron nitride
Drive body graphene nano on piece be distributed more uniformly with extensively.The addition of surfactant makes boron nitride presoma be more easy to
It is adhered to the surface of graphene nanometer sheet, which greatly enhances the popularity of clad.It is sintering gas with ammonia, nitrogen is being provided
Reducibility gas can be done while source again, so as to get product it is purer.
The technical solution adopted by the present invention is：
A kind of preparation method of boron nitride coated graphite alkene nanometer sheet, includes the following steps：
(1) melamine and boric acid are dissolved in absolute ethyl alcohol, stir, adds graphene nanometer sheet powder and surface
Activating agent, 1.5~2.5h of ultrasound are stirred, filtering；
Wherein, 0.309~4.944g of boric acid, 0.315~5.04g of melamine are added in every 20~40ml absolute ethyl alcohols,
1.5~2.0g of 0.03~0.24g of graphene nanometer sheet and surfactant；The surfactant is polyvinylpyrrolidone
K30；
(2) filtrate in step (1) is dried in drying box；Wherein drying box uses vacuum drying chamber；
Wherein, drying temperature is 40~65 DEG C, and drying time is 8~12h；
(3) 1.5 are sintered at ammonia atmosphere, 900~1200 DEG C after taking the desciccate mechanical lapping obtained in step (2)
Boron nitride coated graphite alkene nanometer sheet composite powder material is made in~3.5h.
The molar ratio of boric acid and melamine is 1 in the step (1):3~5:1.
The present invention substantive distinguishing features be：
(1) the present invention can reduce surface energy by the addition of surfactant PVP K30 using it
And strong cementation so that boron nitride presoma is more easy to be adhered to the surface of graphene nanometer sheet；
(2) the presoma adhesion method that is used is easier than traditional powder mixing process so that boron nitride presoma
Graphene nano on piece distribution it is extensive with it is uniform.
(3) use of ammonia gas is more important in sintering processes, and the use of ammonia not only can make product purer,
And nitrogen source can be served as with extra acid reaction.
(4) ultrasonic time of matters is more important in step 1, and ultrasonic time is too short, and material mixes uneven, presoma
It is not easy to adhere to, overlong time, the structure of graphene nanometer sheet be destroyed more serious.
The beneficial effects of the invention are as follows：
(1) it by the present invention in that with boric acid-melamine precursor process, is easier than traditional powder mixing process
So that boron nitride presoma graphene nano on piece be distributed it is extensive with it is uniform.
(2) present invention using polyvinylpyrrolidone k30 be used as surfactant, using its can reduce surface energy and by force
Strong cementation so that boron nitride presoma is more easy to be adhered to the surface of graphene nanometer sheet, and utilization rate is high, shown in Fig. 2
The boron nitride coating of cladding sample is evenly distributed, and cladding is in extensive range, works well.
(3) present invention significantly improves the oxidation resistance temperature of original graphite alkene nanometer sheet, can be seen in conjunction with Fig. 4 and Fig. 5
The oxidation resistance temperature for going out to coat sample improves 260 DEG C than the oxidation resistance temperature of original graphite alkene nanometer sheet.
(4) present invention takes full advantage of the stability under the conditions of boron nitride high-temperature, obtained boron nitride coated graphite alkene
Nanosheet composite material not only overcomes disadvantage oxidizable in air under graphene nanometer sheet high temperature, in combination with boron nitride
Excellent heat conductivility, to greatly expand the application of graphene nanometer sheet at high temperature.
(5) the method for the present invention instrument equipment is simple, easy to operate, of low cost, the stable structure and performance of product
It is excellent, be conducive to produce on a large scale.
Description of the drawings
The present invention will be further described with reference to the accompanying drawings and examples.
Fig. 1 is X-ray diffraction (XRD) figure of the boron nitride coated graphite alkene nanometer sheet of the embodiment of the present invention 2, wherein figure
1a is the XRD diagram of original graphite alkene nanometer sheet, and Fig. 1 b are the XRD diagram for coating sample；
Fig. 2 is transmission electron microscope (TEM) photo of the boron nitride coated graphite alkene nanometer sheet of the embodiment of the present invention 3, wherein figure
2a is certain part cladding sample image under transmission electron microscope, and Fig. 2 b are that this sample segment high power transmits enlarged drawing.
Fig. 3 is infrared (FTIR) image of the boron nitride coated graphite alkene nanometer sheet of the embodiment of the present invention 3；Wherein, Fig. 3 a
Scheme for the FTIR of original graphite alkene nanometer sheet, Fig. 3 b are the FTIR figures for coating sample；
Fig. 4 is hot weight-differential heat (TG-DTA) picture of the raw graphite alkene nanometer sheet used in the present invention.
Fig. 5 is hot weight-differential heat (TG-DTA) picture of the boron nitride coated graphite alkene nanometer sheet of the embodiment of the present invention 8.
Specific implementation mode
Embodiment 1
(1) in molar ratio 1:3,0.824g boric acid (0.0133 mole), 5.04g melamines (0.04 mole) are weighed,
(this substance is well known materials, density range 0.2-0.4g/cc, relative gravity ranging from 2.0- to 0.03g graphene nanometer sheets
2.25g/), it pours into successively in 20ml absolute ethyl alcohols, stirs 0.5h, 1.5g polyvinylpyrrolidone k30 are then added, room temperature is stirred
1h is mixed, then ultrasound 2h, stirring 10h are filtered again；
(2) filtrate is put into vacuum drying chamber at 60 DEG C dry 12h, it is dry obtains boron nitride coated graphite alkene nanometer sheet
Dry sample presoma；
(3) composite granule that presoma obtained after mechanical lapping is put into porcelain boat, (the 100ml/ under ammonia atmosphere
Min), 1100 DEG C of high-temperature calcinations of tube furnace, soaking time 2h are utilized, you can it is compound to obtain boron nitride coated graphite alkene nanometer sheet
Material.
Embodiment 2
(1) in molar ratio 1:1, weigh 1.236g boric acid (0.02 mole), 2.52g melamines (0.02 mole), 0.06g
Graphene nanometer sheet is poured into successively in 40ml absolute ethyl alcohols, stirs 0.5h, 1.8g polyvinylpyrrolidone k30, room is then added
Temperature stirring 1h, then ultrasound 1.5h, stirring 10h are filtered again.
(2) filtrate is put into vacuum drying chamber at 60 DEG C dry 12h, it is dry obtains boron nitride coated graphite alkene nanometer sheet
Dry sample presoma；
(3) composite granule that presoma obtained after mechanical lapping is put into porcelain boat, under ammonia atmosphere, utilizes pipe
The 1050 DEG C of high-temperature calcinations of formula stove, soaking time 3h, you can obtain boron nitride coated graphite alkene nanosheet composite material.
Fig. 1 is respectively the XRD curves of graphene nanometer sheet, boron nitride coated graphite alkene nanosheet composite material, by graphite
The XRD curves of alkene nanometer sheet obtain there is apparent characteristic peak at 2 θ=26.55 ° and 54.65 °, correspond respectively to (002) and
(004) crystal face has apparent feature for boron nitride coated graphite alkene nanosheet composite material 2 θ=26.45 ° and 54.60 °
Peak corresponds respectively to (002) and (004) crystal face, and composite material also has obviously in 2 θ=41.65 °, 43.99 °, 77.37 °
Characteristic peak, these peaks correspond respectively to (100), (101), (110) crystal face of boron nitride.By comparing XRD curves it is found that can
To illustrate that there is the presence of boron nitride clad on graphene nanometer sheet surface.
Embodiment 3
(1) in molar ratio 2:1, weigh 2.472g boric acid (0.04 mole), 2.52g melamines (0.02 mole), 0.12g
Graphene nanometer sheet is poured into successively in 40ml absolute ethyl alcohols, stirs 0.5h, 2.0g polyvinylpyrrolidone k30, room is then added
Temperature stirring 1h, then ultrasound 2h, stirring 10h are filtered again；
(2) filtrate is put into vacuum drying chamber at 50 DEG C dry 12h, it is dry obtains boron nitride coated graphite alkene nanometer sheet
Dry sample presoma；
(3) composite granule that presoma obtained after mechanical lapping is put into porcelain boat, under ammonia atmosphere, utilizes pipe
The 1200 DEG C of high-temperature calcinations of formula stove, soaking time 1.5h, you can obtain boron nitride coated graphite alkene nanosheet composite material.
Fig. 2 is the TEM pictures of boron nitride coated graphite alkene nanometer sheet, and as can be seen from Fig., graphene nanometer sheet surface has
Apparent boron nitride clad exists, and the thickness of clad is relatively uniform, and measurement can obtain clad interplanar distance and be
0.334nm corresponds to h-BN (002) crystal face.
Fig. 3 is the FTIR pictures of boron nitride coated graphite alkene nanometer sheet, as can be seen from Fig., graphene nanometer sheet and nitridation
Boron coated graphite alkene nanosheet composite material is all in 3448cm-1、1630cm-1And 2340cm-1There is typical characteristic absorption peak, and
Boron nitride coated graphite alkene nanosheet composite material is also in 1386cm-1、1121cm-1And 805cm-1There is absorption peak, corresponds respectively to
The vibrations of B-N, C-O and B-N-B, it may be said that bright graphene nano on piece has the presence of boron nitride clad.
Embodiment 4
(1) in molar ratio 3:1, weigh 3.708g boric acid (0.06 mole), 2.52g melamines (0.02 mole), 0.12g
Graphene nanometer sheet is poured into successively in 30ml absolute ethyl alcohols, stirs 0.5h, 1.8g polyvinylpyrrolidone k30, room is then added
Temperature stirring 1h, then ultrasound 2h, stirring 10h are filtered again；
(2) filtrate is put into vacuum drying chamber at 60 DEG C dry 12h, it is dry obtains boron nitride coated graphite alkene nanometer sheet
Dry sample presoma；
(3) composite granule that presoma obtained after mechanical lapping is put into porcelain boat, under ammonia atmosphere, utilizes pipe
The 900 DEG C of high-temperature calcinations of formula stove, soaking time 3.5h, you can obtain boron nitride coated graphite alkene nanosheet composite material.
Embodiment 5
(1) in molar ratio 3:1, weigh 3.708 boric acid (0.06 mole), 2.52g melamines (0.02 mole), 0.24g
Graphene nanometer sheet is poured into successively in 30ml absolute ethyl alcohols, stirs 0.5h, 1.8g polyvinylpyrrolidone k30, room is then added
Temperature stirring 1h, then ultrasound 2h, stirring 10h are filtered again；
(2) filtrate is put into vacuum drying chamber at 60 DEG C dry 12h, it is dry obtains boron nitride coated graphite alkene nanometer sheet
Dry sample presoma；
(3) composite granule that presoma obtained after mechanical lapping is put into porcelain boat, under ammonia atmosphere, utilizes pipe
The 1200 DEG C of high-temperature calcinations of formula stove, soaking time 3.5h, you can obtain boron nitride coated graphite alkene nanosheet composite material.
Embodiment 6
(1) in molar ratio 3:1, weigh 3.708 boric acid (0.06 mole), 2.52g melamines (0.02 mole), 0.12g
Graphene nanometer sheet is poured into successively in 30ml absolute ethyl alcohols, stirs 0.5h, 1.8g polyvinylpyrrolidone k30, room is then added
Temperature stirring 1h, then ultrasound 2h, stirring 10h are filtered again；
(2) filtrate is put into vacuum drying chamber at 60 DEG C dry 12h, it is dry obtains boron nitride coated graphite alkene nanometer sheet
Dry sample presoma；
(3) composite granule that presoma obtained after mechanical lapping is put into porcelain boat, under ammonia atmosphere, utilizes pipe
The 1200 DEG C of high-temperature calcinations of formula stove, soaking time 1.5h, you can obtain boron nitride coated graphite alkene nanosheet composite material.
Embodiment 7
(1) in molar ratio 4:1, weigh 4.944g boric acid (0.08 mole), 2.52g melamines (0.02 mole), 0.12g
Graphene nanometer sheet is poured into successively in 40ml absolute ethyl alcohols, stirs 0.5h, 1.8g polyvinylpyrrolidone k30, room is then added
Temperature stirring 1h, then ultrasound 2h, stirring 10h are filtered again；
(2) filtrate is put into vacuum drying chamber at 60 DEG C dry 12h, it is dry obtains boron nitride coated graphite alkene nanometer sheet
Dry sample presoma；
(3) composite granule that presoma obtained after mechanical lapping is put into porcelain boat, under ammonia atmosphere, utilizes pipe
The 1200 DEG C of high-temperature calcinations of formula stove, soaking time 2h, you can obtain boron nitride coated graphite alkene nanosheet composite material.
Embodiment 8
(1) in molar ratio 5:1, weigh that 0.7725g boric acid (0.0125 mole), (0.0025 rubs 0.315g melamines
You), 0.12g graphene nanometer sheets are poured into successively in 40ml absolute ethyl alcohols, stir 0.5h, 1.8g polyvinyl pyrroles are then added
1h is stirred at room temperature in alkanone k30, and then ultrasound 2h, stirring 10h are filtered again；
(2) filtrate is put into vacuum drying chamber at 60 DEG C dry 12h, it is dry obtains boron nitride coated graphite alkene nanometer sheet
Dry sample presoma；
(3) composite granule that presoma obtained after mechanical lapping is put into porcelain boat, under ammonia atmosphere, utilizes pipe
The 1000 DEG C of high-temperature calcinations of formula stove, soaking time 2h, you can obtain boron nitride coated graphite alkene nanosheet composite material.
Fig. 4 is the TG-DTA curves of graphene nanometer sheet, by the hot weight-differential heat curve of graphene nanometer sheet it is found that original
The beginning oxidizing temperature of graphene nanometer sheet is at 560 DEG C or so.
Fig. 5 is the TG-DTA curves of boron nitride coated graphite alkene nanosheet composite material, is received by boron nitride coated graphite alkene
The curve of rice piece composite material can show that the beginning oxidizing temperature of cladding sample is 820 DEG C, the oxidizing temperature of this and boron nitride
Unanimously, that is, after coating the oxidizing temperature of sample improves 260 DEG C compared with original graphite alkene nanometer sheet, it was demonstrated that boron nitride coated graphite
The successful preparation of alkene nanosheet composite material.
Unaccomplished matter of the present invention is known technology.
Claims (2)
1. a kind of preparation method of boron nitride coated graphite alkene nanometer sheet, it is characterized in that this approach includes the following steps：
(1) melamine and boric acid are dissolved in absolute ethyl alcohol, are stirred, added graphene nanometer sheet powder and surface is lived
Property agent, 1.5 ~ 2.5h of ultrasound, stir, filtering；
Wherein, 0.309 ~ 4.944g of boric acid, 0.315 ~ 5.04g of melamine are added in every 20 ~ 40ml absolute ethyl alcohols, graphene is received
Rice 0.03 ~ 0.24g of piece and 1.5 ~ 2.0g of surfactant；The surfactant is PVP K30；
(2) filtrate in step (1) is dried in drying box；Wherein drying box uses vacuum drying chamber；
Wherein, drying temperature is 40 ~ 65 DEG C, and drying time is 8 ~ 12h；
(3) take after the desciccate mechanical lapping obtained in step (2) at ammonia atmosphere, 900 ~ 1200 DEG C sintering 1.5 ~
Boron nitride coated graphite alkene nanometer sheet composite powder material is made in 3.5h.
2. a kind of preparation method of boron nitride coated graphite alkene nanometer sheet as described in claim 1, it is characterized in that the step
Suddenly（1）The molar ratio of middle boric acid and melamine is 1:3~5:1.
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| CN110510604A (en) * | 2019-09-09 | 2019-11-29 | 吉林大学 | A kind of graphene/boron nitride stratiform heterojunction structure and preparation method thereof |
| CN110510604B (en) * | 2019-09-09 | 2022-11-18 | 吉林大学 | Graphene/boron nitride layered heterostructure and preparation method thereof |
| CN111747386A (en) * | 2020-06-28 | 2020-10-09 | 武汉工程大学 | Morphology-controllable boron nitride nanostructure-graphene composite material and preparation method thereof |
| CN111747386B (en) * | 2020-06-28 | 2021-10-12 | 武汉工程大学 | Morphology-controllable boron nitride nanostructure-graphene composite material and preparation method thereof |
| CN115260995A (en) * | 2022-07-22 | 2022-11-01 | 中国地质大学（武汉） | Double-network heat-conducting porous aerogel energy storage material and preparation method and application thereof |
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