CN108439394A - A method of preparing bortz powder-graphene composite material - Google Patents
A method of preparing bortz powder-graphene composite material Download PDFInfo
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- CN108439394A CN108439394A CN201810493126.5A CN201810493126A CN108439394A CN 108439394 A CN108439394 A CN 108439394A CN 201810493126 A CN201810493126 A CN 201810493126A CN 108439394 A CN108439394 A CN 108439394A
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- bortz powder
- powder
- composite material
- graphene
- bortz
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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
- C01B32/25—Diamond
- C01B32/28—After-treatment, e.g. purification, irradiation, separation or recovery
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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
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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 present invention provides a kind of method preparing bortz powder graphene composite material.Mainly comprise the following steps that：1. pre-processing bortz powder using Piranha washing lotion, powder surface impurity is removed, and to surface hydroxylation processing, it is multiple with deionized water centrifuge washing afterwards；2. the bortz powder ultrasonic disperse after washing adds appropriate graphene oxide water solution in deionized water；3. under magnetic agitation, certain density sodium borohydride aqueous solution is added dropwise in the dilute mixed liquor of bortz powder graphite oxide, continues stirring and be reduced completely to graphene oxide.4. bortz powder/graphene complex centrifuge washing is multiple；5. obtaining diamond graphene powder after freeze-drying.The technological process is simple to operation, and bortz powder is anticipated using Piranha washing lotion, can not only remove the impurity on bortz powder surface, but also carry out hydroxylating modification to bortz powder particle surface.
Description
Technical field
The present invention relates to the methods of bortz powder-graphene composite material, belong to materials chemistry preparing technical field.
Background technology
Diamond is a kind of simple substance being made of carbon, is one of allotrope of carbon.Diamond has excellent
Different mechanical property, the good capacity of heat transmission, chemical stability and negative electron compatibility etc..Diamond is heat conduction system in nature
The highest electrical isolation substance of number, therefore diamond causes extensive concern in performance application field.Diamond is typical
For valence crystal, the structure of ground state electron is 1s22s22p2, the 2s layer electronics of carbon atom with 2p layers in electronically form sp3Hydridization
Track, therefore each carbon atom carbon atom adjacent with surrounding, are formed the covalent bond of saturation with sp3 hybridized orbits, constitute positive four
The crystal structure of face body structure, diamond determines a series of its physicochemical properties with brilliances.
Graphene be one kind by carbon atom with sp2What hydridization was formed has cellular crystal structure two-dimension nano materials, solely
Special lattice structure makes it have the mechanical strength (1060GPa) of superelevation, electric conductivity (15000cm/ (Vs)) and thermal conductivity
(3000W/(m·K)).In addition graphene has a variety of excellent properties such as high temperature resistant, waterproof, alkali prevention salt corrosion.Therefore graphene
Scene effect transistor, high-frequency electron device, transparent conductive film, composite material, energy storage material, electrochemical sensor etc.
It has broad application prospects.
Bonded diamond and graphene excellent properties, obtained bortz powder/graphene composite material is in electronics and storage
The fields such as energy have broad application prospects.
Invention content
Technical problem：The object of the present invention is to provide a kind of methods preparing bortz powder-graphene composite material, utilize
Piranha washing lotion handles bortz powder, powder surface impurity is removed, and carry out hydroxylating processing to particle surface, with graphite oxide
After alkene mixing, sodium borohydride is recycled to be restored, after centrifuge washing drying, obtains bortz powder/graphene composite material.
Technical solution：The present invention handles bortz powder using Piranha washing lotion, after being mixed with graphene oxide, recycles boron
Sodium hydride is restored, and bortz powder/graphene composite material is obtained.Bortz powder is anticipated using Piranha washing lotion, no
The impurity on bortz powder surface can be only removed, and hydroxylating modification is carried out to bortz powder particle surface, makes itself and reduction
Graphene combination is more secured, stablizes.
For the purpose for realizing above-mentioned, the technical solution of the method use of bortz powder/graphene composite material of the invention
Including：
Step 1 weighs bortz powder and is added in Piranha washing lotion, and ultrasonic disperse 20-50min, rear centrifuge washing is multiple,
Ultrasonic disperse is in 30-100mL deionized waters afterwards；
Appropriate graphene oxide water solution, ultrasonic disperse 10- are added into above-mentioned bortz powder dispersion liquid by step 2
60min；
During step 3 magnetic agitations, appropriate sodium borohydride aqueous solution is added dropwise, and continues magnetic agitation 1-3h.
After step 4 centrifuge washings are multiple, freeze-drying obtains bortz powder/graphene composite material
Wherein,
The Piranha washing lotion is the concentrated sulfuric acid and mixed solution of hydrogen peroxide, volume ratio 5:3-9:3.
The graphene oxide water solution is obtained by Hummers, a concentration of 6-12mg/mL, addition 2-8mL.
A concentration of 3.9M of the sodium borohydride aqueous solution.
Advantageous effect：Bortz powder is anticipated using Piranha washing lotion, can not only remove the miscellaneous of bortz powder surface
Matter, and hydroxylating modification is carried out to bortz powder particle surface, so that it is combined with reduced graphene more secured, stablizes.
By control graphene oxide addition, can obtain different quality than bortz powder/graphene composite wood
Material.The technical process is easy to operate, composite material is evenly distributed, and obtained bortz powder/graphene composite material is in electronics
It has broad application prospects with fields such as energy storage.
Description of the drawings
Fig. 1 is bortz powder-graphene composite material SEM figures.It is wrapped in gold while graphene uniform is can be found that from figure
Hard rock powder surface, combines closely with bortz powder.
Fig. 2 is bortz powder-graphene composite material Raman collection of illustrative plates.It can be found that the main spy of graphene three shakes from the figure
Peak, respectively D (1350cm-1), G (1680cm-1) and 2D (2680cm-1).Wherein the intensity at the peaks D is higher than G peak intensities, shows
There are more defects, such as fold for the graphene；And the intensity at the peaks 2D is far below the intensity at the peaks G, shows prepared graphite
The alkene number of plies is more.
Specific implementation mode
The present invention provides a kind of method preparing bortz powder/graphene composite material.First by 0.5-3g bortz powders
It is scattered in Piranha washing lotion, removes powder surface impurity, and hydroxylating processing is carried out to its surface, centrifuged using deionized water
Washing is multiple.Bortz powder ultrasonic disperse after washing adds a concentration of 10mg/L of 2-8mL in 30-100mL deionized waters
Graphene oxide water solution.The sodium borohydride solution that a concentration of 3.9M of 10-20mL are added is dilute mixed in bortz powder/graphite oxide
It closes in liquid, continues magnetic agitation to graphene oxide and be completely reduced.Bortz powder/graphene complex centrifuge washing is more
It is secondary.Finally freeze-drying obtains diamond/graphene composite material powder.Sample is observed using scanning electron microscope (SEM)
Pattern, Raman spectrum detect graphene structure.
Embodiment 1：
1g bortz powders are scattered in Piranha washing lotion, remove powder surface impurity, and hydroxylating is carried out to its surface
Processing utilizes deionized water centrifuge washing 3 times.Treated bortz powder ultrasonic disperse adds in 50mL deionized waters
The graphene oxide water solution of a concentration of 10mg/L of 5mL, ultrasonic disperse 30min.During magnetic agitation, it is dense that 15mL is added dropwise
The sodium borohydride solution for being 3.9M is spent in the dilute mixed liquor of bortz powder/graphite oxide, continues magnetic agitation 2h, until graphite oxide
Alkene is reduced completely.Bortz powder/graphene complex centrifuge washing is multiple.Finally freeze-drying obtains bortz powder/stone
Black alkene composite material powder.
Embodiment 2：
0.5g bortz powders are scattered in Piranha washing lotion, remove powder surface impurity, and hydroxyl is carried out to its surface
Change is handled, and utilizes deionized water centrifuge washing 3 times.Treated bortz powder ultrasonic disperse adds in 40mL deionized waters
Add the graphene oxide water solution of a concentration of 10mg/L of 3mL, ultrasonic disperse 20min.During magnetic agitation, 10mL is added dropwise
The sodium borohydride solution of a concentration of 3.9M continues magnetic agitation 1h in the dilute mixed liquor of bortz powder/graphite oxide, until oxidation stone
Black alkene is reduced completely.Bortz powder/graphene complex centrifuge washing is multiple.Finally freeze-drying obtain bortz powder/
Graphene composite material powder.
Embodiment 3：
2.5g bortz powders are scattered in Piranha washing lotion, remove powder surface impurity, and hydroxyl is carried out to its surface
Change is handled, and utilizes deionized water centrifuge washing 3 times.Treated bortz powder ultrasonic disperse adds in 60mL deionized waters
Add the graphene oxide water solution of a concentration of 10mg/L of 3mL, ultrasonic disperse 50min.During magnetic agitation, 10mL is added dropwise
The sodium borohydride solution of a concentration of 3.9M continues magnetic agitation 1h in the dilute mixed liquor of bortz powder/graphite oxide, until oxidation stone
Black alkene is reduced completely.Bortz powder/graphene complex centrifuge washing is multiple.Finally freeze-drying obtain bortz powder/
Graphene composite material powder.
Claims (6)
1. a kind of method preparing bortz powder-graphene composite material, it is characterised in that this method includes：
Step 1 weighs bortz powder and is added in Piranha washing lotion, and ultrasonic disperse, centrifuge washing is multiple, and rear ultrasonic disperse is in going
In ionized water, bortz powder dispersion liquid is made；
Graphene oxide water solution is added into above-mentioned bortz powder dispersion liquid in step 2, and bortz powder-is made in ultrasonic disperse
Graphene oxide dispersion；
It is water-soluble that sodium borohydride is added dropwise by during above-mentioned bortz powder-graphene oxide dispersion magnetic agitation in step 3
Liquid, and continue magnetic agitation 1-3h；
Step 4 by step 3 treated dispersion liquid centrifuge washing it is multiple after, freeze-drying obtains bortz powder-graphene
Composite material.
2. the preparation method of bortz powder-graphene composite material as described in claim 1, which is characterized in that in step 1
The Piranha washing lotion is the concentrated sulfuric acid and mixed solution of hydrogen peroxide, volume ratio 5:3-9:3.
3. the preparation method of bortz powder-graphene composite material as described in claim 1, which is characterized in that in step 2
The graphene oxide water solution is obtained by Hummers, a concentration of 6-12mg/mL, addition 2-8mL.
4. the preparation method of bortz powder-graphene composite material as described in claim 1, which is characterized in that in step 3
A concentration of 1-4M of the sodium borohydride aqueous solution.
5. the preparation method of bortz powder-graphene composite material as described in claim 1, which is characterized in that in step 1,
The time of the ultrasonic disperse is 20-50min.
6. the preparation method of bortz powder-graphene composite material as described in claim 1, which is characterized in that in step 2,
The time of the ultrasonic disperse is 10-60min.
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| EP2504278A2 (en) * | 2009-11-25 | 2012-10-03 | Massachusetts Institute of Technology | Systems and methods for enhancing growth of carbon-based nanostructures |
| CN104870365A (en) * | 2012-10-12 | 2015-08-26 | 国立研究开发法人科学技术振兴机构 | Nano-diamond particle and method for producing same, and fluorescent molecular probe and method for analyzing structure of protein |
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| CN107032347A (en) * | 2016-02-03 | 2017-08-11 | 现代自动车株式会社 | Graphene oxide Nano diamond compound, its manufacture method and the nano-fluid including it |
| CN106237984A (en) * | 2016-07-29 | 2016-12-21 | 燕山大学 | A kind of method that graphene oxide and chemical modification thereof are prepared in diadust surface |
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