CN110357078A - A kind of graphene microballoon and preparation method thereof - Google Patents
A kind of graphene microballoon and preparation method thereof Download PDFInfo
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- CN110357078A CN110357078A CN201910750134.8A CN201910750134A CN110357078A CN 110357078 A CN110357078 A CN 110357078A CN 201910750134 A CN201910750134 A CN 201910750134A CN 110357078 A CN110357078 A CN 110357078A
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- graphene
- microballoon
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- graphene oxide
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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
Abstract
The invention discloses a kind of graphene microballoons and preparation method thereof, wherein, the preparation method is using graphene oxide and template as raw material, slurry is formed by the way that appropriate solvent is added, composite material is obtained using spray drying, and ultra-high temperature heat treatment, redox graphene and the template that melts away are carried out to the composite material under vacuum, obtain the graphene microballoon of size tunable.Graphene method for preparing microsphere provided by the invention is simple to operation, and can prepare that size is controllable, non-bloating graphene microballoon.
Description
Technical field
The present invention relates to field of preparation of graphene, and in particular to a kind of graphene microballoon and preparation method thereof.
Background technique
Graphene is a kind of new material of individual layer laminated structure being made of carbon atom, it has superelevation mobility, low electricity
The features such as resistance rate, high-ratio surface, high thermal conductivity coefficient and high mechanical strength, is widely used in biology, chemistry, physics and material
Equal fields.
Most of graphene involved in the prior art is all two-dimension plane structure, so that the relevant nature of graphene is all
It is confined in two-dimensional surface.For example, graphene planes thermal coefficient is 5300W/m*K, however thermal coefficient is low in vertical direction
In 40W/mK, this has seriously affected its practical application.
Therefore, three-dimensional grapheme microballoon research is increasingly taken seriously, and how to prepare that size is controllable, non-bloating three-dimensional stone
Black alkene microballoon is still a technological difficulties.
Summary of the invention
Place in view of above-mentioned deficiencies of the prior art, the purpose of the present invention is to provide a kind of graphene microballoon and its preparations
Method, it is intended to solve the problems, such as that the prior art is difficult to prepare that size is controllable, non-bloating graphene microballoon.
A kind of preparation method of graphene microballoon, wherein comprising steps of
In a solvent by graphene oxide dispersion, graphene oxide dispersion is made；
The graphene oxide dispersion is mixed with template, composite material is made；
Under vacuum conditions, the composite material is heat-treated, graphene microballoon is made.
The preparation method of the graphene microballoon, wherein it is described to mix the graphene oxide dispersion with template,
Be made composite material the step of include:
Template is added into the graphene oxide dispersion, mixing makes graphene oxide be adsorbed on the template table
Graphene oxide-template slurry is made in face；
Spray drying treatment is carried out to the graphene oxide-template slurry, the composite material is made.
The preparation method of the graphene microballoon, wherein in the graphene oxide-template slurry, graphene oxide
Mass ratio with template is 1-5:50-500.
The preparation method of the graphene microballoon, wherein the temperature of the spray drying treatment is 100-300 DEG C.
The preparation method of the graphene microballoon, wherein the solvent is selected from deionized water, methanol, ethyl alcohol, acetone and different
One of propyl alcohol is a variety of.
The preparation method of the graphene microballoon, wherein the template be selected from silicon dioxide microsphere, silicon nitride microballoon,
One of aluminum oxide micro-sphere or copper oxide microballoon.
The preparation method of the graphene microballoon, wherein under conditions of vacuum degree is lower than 10Pa, to the composite material
2000-3000 DEG C of heat treatment is carried out, graphene microballoon is made.
The preparation method of the graphene microballoon, wherein the diameter of the graphene microballoon is 1-10um.
A kind of graphene microballoon, wherein be made using the preparation method of graphene microballoon of the present invention.
The utility model has the advantages that being with graphene oxide and template the present invention provides a kind of preparation method of graphene microballoon
Raw material forms slurry by the way that appropriate solvent is added, obtains composite material using spray drying, and under vacuum to the composite wood
Material carries out ultra-high temperature heat treatment, redox graphene and the template that melts away, and obtains the graphene microballoon of size tunable.This hair
The graphene method for preparing microsphere of bright offer is simple to operation, and can prepare that size is controllable, non-bloating graphene microballoon.
Detailed description of the invention
Fig. 1 is a kind of flow chart of the preparation method preferred embodiment of graphene microballoon of the present invention.
Specific embodiment
The present invention provides a kind of graphene microballoon and preparation method thereof, to make the purpose of the present invention, technical solution and effect
Clearer, clear, the present invention is described in more detail as follows in conjunction with drawings and embodiments.It should be appreciated that this place is retouched
It states that specific examples are only used to explain the present invention, is not intended to limit the present invention.
Referring to Fig. 1, Fig. 1 is a kind of process of the preparation method preferred embodiment of graphene microballoon provided by the invention
Figure, wherein as shown, comprising steps of
S100, graphene oxide is dispersed in a solvent, graphene oxide dispersion to be made；
S200, the graphene oxide dispersion is mixed with template, composite material is made；
S300, under vacuum conditions, is heat-treated the composite material, and graphene microballoon is made.
The present embodiment forms slurry using graphene oxide and template as raw material, by the way that appropriate solvent is added, to the slurry
Material carries out spray drying treatment and obtains composite material, and carries out ultra-high temperature heat treatment to the composite material under vacuum, also
Former graphene oxide and the template that melts away obtain size tunable and non-bloating three-dimensional grapheme microballoon.
The present embodiment makes graphene oxide table by the heat treatment under vacuum conditions to composite material progress ultra-high temperature
The group in face removes, and repairs the conjugated structure on its surface, the graphene microballoon restored.
In some embodiments, described to mix the graphene oxide dispersion with template, composite material is made
The step of include: that template is added into the graphene oxide dispersion, mixing so that graphene oxide is adsorbed on the template
Graphene oxide-template slurry is made in agent surface；Spray drying treatment is carried out to the graphene oxide-template slurry,
The composite material is made.
In the present embodiment, the template primarily serves supporting role, and the graphene oxide and template are in solvent
During middle mixing, the graphene oxide is attached to the template surface by physical absorption, and passes through self assembly shape
At micro-sphere structure.
It in some embodiments, can be with Effective Regulation most by adjusting the quality proportioning of graphene oxide and template
The size of graphene microballoon made from end.In some preferred embodiments, the graphene oxide-template slurry
In, the mass ratio of graphene oxide and template is 1-5:50-500, and in the proportional region, the graphene oxide can fill
Divide and be adsorbed on template surface, forms the composite material of micro-sphere structure.
In some embodiments, the solvent is selected from one of deionized water, methanol, ethyl alcohol, acetone and isopropanol
Or it is a variety of, but not limited to this.
In some embodiments, the template is selected from silicon dioxide microsphere, silicon nitride microballoon, aluminum oxide micro-sphere or oxygen
Change one of copper microballoon, but not limited to this.
In some embodiments, the temperature of the spray drying treatment is 100-300 DEG C, within this temperature range, institute
The solvent stated in graphene oxide-template slurry can be effectively removed, and obtain the composite material of micro-sphere structure.
In some embodiments, under conditions of vacuum degree is lower than 10Pa, 2000-3000 is carried out to the composite material
DEG C heat treatment, be made graphene microballoon.In the present embodiment, oxidation stone can be quickly removed in the vacuum environment lower than 10Pa
The gas generated in black alkene reduction process, while reducing fusing point；On the other hand, 2000-3000 DEG C of heat treatment can melt away mould
Plate agent effectively repairs the conjugated structure of surface of graphene oxide, obtains more perfect graphene-structured, and enhance graphene film
Between interact, to inhibit graphene microsphere expansion.
In some embodiments, a kind of graphene microballoon is also provided, using the preparation method of graphene microballoon of the present invention
It is made.In some embodiments, the diameter of the graphene microballoon is 1-10um.The graphene microballoon prepared through the invention
Excellent thermal coefficient is all had in the horizontal direction and the vertical direction.
Explanation is further explained to a kind of preparation method of graphene microballoon of the present invention below by specific embodiment:
Embodiment 1
The graphene oxide water solution 100ml of 5mg/ml is prepared, silicon dioxide microsphere 20g is added thereto, stirs to get
Dispersion liquid.The dispersion liquid is spray-dried, 260 DEG C of inlet temperature, 120 DEG C of outlet temperature spray drying obtain graphene oxide
With the compound of silica.
The compound is placed in vacuum degree 1Pa environment, be warming up to 2500 DEG C and maintains 30min, obtains graphene microballoon.
The graphene microsphere diameter is about 5um.Graphene microballoon punching press is formed a film, measuring its horizontal thermal conductivity factor is
1800W/mK, vertical thermal conductivity 1100W/mK.
Embodiment 2
The graphene oxide ethanol solution 100ml of 5mg/ml is prepared, silicon dioxide microsphere 15g is added thereto, stirs
To dispersion liquid.The dispersion liquid is spray-dried, 250 DEG C of inlet temperature, 100 DEG C of outlet temperature spray drying obtain graphite oxide
The compound of alkene and silica.
The compound is placed in vacuum degree 1Pa environment, be warming up to 2800 DEG C and maintains 30min, obtains graphene microballoon.
The graphene microsphere diameter is about 4um.Graphene microballoon punching press is formed a film, measuring its horizontal thermal conductivity factor is
1900W/mK, vertical thermal conductivity 1200W/mK.
Embodiment 3
The graphene oxide ethanol solution 100ml of 10mg/ml is prepared, silicon dioxide microsphere 50g is added thereto, stirs
To dispersion liquid.The dispersion liquid is spray-dried, 300 DEG C of inlet temperature, 100 DEG C of outlet temperature spray drying obtain graphite oxide
The compound of alkene and silica.
The compound is placed in vacuum degree 1Pa environment, be warming up to 3000 DEG C and maintains 30min, obtains graphene microballoon.
The graphene microsphere diameter is about 6um.Graphene microballoon punching press is formed a film, measuring its horizontal thermal conductivity factor is
2300W/mK, vertical thermal conductivity 1500W/mK.
Embodiment 4
The graphene oxide ethanol solution 100ml of 20mg/ml is prepared, silicon dioxide microsphere 100g, stirring are added thereto
Obtain dispersion liquid.The dispersion liquid is spray-dried, 250 DEG C of inlet temperature, 120 DEG C of outlet temperature spray drying obtain oxidation stone
The compound of black alkene and silica.
The compound is placed in vacuum degree 5Pa environment, be warming up to 3000 DEG C and maintains 20min, obtains graphene microballoon.
The graphene microsphere diameter is about 8um.Graphene microballoon punching press is formed a film, measuring its horizontal thermal conductivity factor is
2400W/mK, vertical thermal conductivity 1600W/mK.
Embodiment 5
The graphene oxide ethanol solution 100ml of 50mg/ml is prepared, silicon dioxide microsphere 300g, stirring are added thereto
Obtain dispersion liquid.The dispersion liquid is spray-dried, 280 DEG C of inlet temperature, 110 DEG C of outlet temperature spray drying obtain oxidation stone
The compound of black alkene and silica.
The compound is placed in vacuum degree 7Pa environment, be warming up to 2500 DEG C and maintains 40min, obtains graphene microballoon.
The graphene microsphere diameter is about 7um.Graphene microballoon punching press is formed a film, measuring its horizontal thermal conductivity factor is
2500W/mK, vertical thermal conductivity 1500W/mK.
In conclusion being with graphene oxide and template the present invention provides a kind of preparation method of graphene microballoon
Raw material forms slurry by the way that appropriate solvent is added, obtains composite material using spray drying, and under vacuum to the composite wood
Material carries out ultra-high temperature heat treatment, redox graphene and the template that melts away, and obtains the graphene microballoon of size tunable.This hair
The graphene method for preparing microsphere of bright offer is simple to operation, and can prepare that size is controllable, non-bloating graphene microballoon.
It, can according to the technique and scheme of the present invention and this hair it is understood that for those of ordinary skills
Bright design is subject to equivalent substitution or change, and all these changes or replacement all should belong to the guarantor of appended claims of the invention
Protect range.
Claims (9)
1. a kind of preparation method of graphene microballoon, which is characterized in that comprising steps of
In a solvent by graphene oxide dispersion, graphene oxide dispersion is made；
The graphene oxide dispersion is mixed with template, composite material is made；
Under vacuum conditions, the composite material is heat-treated, graphene microballoon is made.
2. the preparation method of graphene microballoon according to claim 1, which is characterized in that described by the graphene oxide point
Dispersion liquid is mixed with template, be made composite material the step of include:
Template is added into the graphene oxide dispersion, mixing makes graphene oxide be adsorbed on the template surface,
Graphene oxide-template slurry is made；
Spray drying treatment is carried out to the graphene oxide-template slurry, the composite material is made.
3. the preparation method of graphene microballoon according to claim 2, which is characterized in that the graphene oxide-template
In slurry, the mass ratio of graphene oxide and template is 1-5:50-500.
4. the preparation method of graphene microballoon according to claim 2, which is characterized in that the temperature of the spray drying treatment
It is 100-300 DEG C.
5. the preparation method of graphene microballoon according to claim 1, which is characterized in that the solvent be selected from deionized water,
One of methanol, ethyl alcohol, acetone and isopropanol are a variety of.
6. the preparation method of graphene microballoon according to claim 1, which is characterized in that the template is selected from silica
One of microballoon, silicon nitride microballoon, aluminum oxide micro-sphere or copper oxide microballoon.
7. the preparation method of graphene microballoon according to claim 1, which is characterized in that be lower than the condition of 10Pa in vacuum degree
Under, 2000-3000 DEG C of heat treatment is carried out to the composite material, and graphene microballoon is made.
8. the preparation method of graphene microballoon according to claim 1, which is characterized in that the diameter of the graphene microballoon is
1-10um。
9. a kind of graphene microballoon, which is characterized in that be made using any one preparation method of claim 1-8.
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Citations (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN105217622A (en) * | 2015-11-13 | 2016-01-06 | 武汉大学 | A kind of preparation method of controlled three-dimensional grapheme microballoon |
| CN106966383A (en) * | 2017-04-28 | 2017-07-21 | 杭州高烯科技有限公司 | A kind of spitball shape graphene microballoon and preparation method thereof |
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Patent Citations (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN105217622A (en) * | 2015-11-13 | 2016-01-06 | 武汉大学 | A kind of preparation method of controlled three-dimensional grapheme microballoon |
| CN106966383A (en) * | 2017-04-28 | 2017-07-21 | 杭州高烯科技有限公司 | A kind of spitball shape graphene microballoon and preparation method thereof |
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Application publication date: 20191022 |