CN108862248A - A kind of quick macroblock quantization prepares graphene-metal oxide composite powder material method - Google Patents
A kind of quick macroblock quantization prepares graphene-metal oxide composite powder material method Download PDFInfo
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Abstract
The present invention provides a kind of quick macroblock quantization and prepares graphene-metal oxide composite powder material method, which is characterized in that the described method comprises the following steps：Under ultrasound and/or stirring, graphene oxide is dispersed in metal salt solution, after standing removal supernatant liquor, is dried to obtain the graphene oxide block materials of metal ion intercalation；The graphene oxide block materials of metal ion intercalation are heated at 400-600 DEG C, 20s-60min is reacted, obtains graphene-metal oxide composite powder material.The method of the present invention solves the reduction of graphene oxide and the oxidation of metal ion simultaneously; realize quick magnanimity prepares material; and it carries out the reduction of graphene oxide and the oxidation of metal ion preferably in air atmosphere; breach the prior art must just can guarantee under inert gas protection graphene oxide reduction the problem of, entire preparation process have it is easy to operate, at low cost, environmentally friendly, can be mass-produced.
Description
Technical field
The invention belongs to grapheme material preparation field, it is related to a kind of preparing graphene-metal oxide composite granule material
The method of material more particularly to a kind of quick macroblock quantization prepare graphene-metal oxide composite powder material method.
Background technique
Graphene is that a kind of carbon atom is connected with covalent bond in cellular single layer two-dimensional material, this monoatomic layer two
Tie up conductivity and thermal conductivity, big specific surface area and unique light that structure assigns the excellent mechanical characteristic of graphene, superelevation
Electrical characteristics.These excellent performances determine that graphene has a potential application in various fields, for example, electronics, information, the energy,
Composite material and biological medicine etc..However, simple graphene has a single function as active material, limit to a certain extent
Its practical application.Compared with graphene, metal oxide has unique characteristic of semiconductor, photoelectric conversion/response characteristic, more
Big specific capacity and higher catalytic activity etc..Graphene and metal oxide is compound by both realizations synergistic effect, pole
Big raising material property simultaneously expands its practical application area.
In terms of preparation, the production technology of graphene/metal oxide powder body material needs to take into account the preparation work of graphene
Skill and its combination process with oxide.The preparation method of graphene can be divided mainly into two classes at present：1) epitaxial growth method and change
Learn vapour deposition process；2) graphite particle is removed into graphene by the method for chemistry and/or physics, such as mechanical stripping method,
Electrochemical intercalation stripping method, oxidation-reduction method etc..Wherein, epitaxial growth method requirement condition is harsher, and graphene and substrate
Between there are it is stronger effect and be not easy to shift, it is difficult to realize large-scale production.Chemical vapour deposition technique mainly utilizes gaseous carbon source
Graphene is prepared in catalytic growth on the surface of the substrate after decomposing at high temperature.This method is to prepare high quality and large area list
The important method of layer graphene, but working condition is more harsh, and consume energy big, at high cost, complex process.Due to stone in graphite particle
The weak Van der Waals force interaction of black alkene piece interlayer, Geim seminar use adhesive tape to stick viscous pyrolytic graphite repeatedly earliest, then will
Obtained sample is transferred on silicon wafer, and single-layer graphene is prepared for the first time.But this method low yield, it is impossible to realize big rule
Mould preparation.In the recent period, three roller methods are invented using similar principle by Chen Guohua seminar, and glue is made in organic solvent in macromolecule dissolution
Graphite is removed layer by layer and graphene is made by glutinous agent by three-roller tool power and its grinding distribution effect.But the stone due to obtaining
Black alkene needs to utilize a large amount of solvents such as acetone, tetrahydrofuran, cyclohexanone etc. or high-temperature heating removal macromolecular adhesive, cost
High and pollution environment, limits it in the application of industrialization large-scale production.Oxidation-reduction method is that graphite particle initial oxidation is pre-
It handles and sufficiently removes in water, then graphene oxide is restored to obtain graphene.Since graphene oxide has been carried out
Tonne magnanimity production, and cheap, therefore, this method are considered as a kind of most possible realizing prepared by graphene industrialization
Important method.
Current recombination process is coprecipitated using hydro-thermal or dipping usually using graphene oxide and metal precursor as raw material
The methods of shallow lake obtains graphene oxide/metal precursor compound, then obtains graphite by modes such as electronation or heat treatments
Alkene/metal oxide hybrid material, processing step is complicated, and time-consuming.Wherein, chemical reduction procedure uses hydrazine hydrate, hydroboration
The toxic chemical substance such as sodium, not only low efficiency but also pollution environment, endanger the health of staff.In contrast, it heat-treats
Method is environmentally protective can be made high-quality graphene, but usually there is treatment temperature height, processing currently based on the method for thermal reduction
The problems such as time is long, energy consumption is high, at high cost.
CN102757041A discloses a kind of graphene/metal oxide raw powder's production technology.By graphite oxidation at oxygen
Graphite alkene, and after being stripped out in parent, it is dissolved in solvent with metallic compound, graphite is produced in reduction under overcritical effect
Alkene/metal-oxide powder.The technique asepsis environment-protecting, but process conditions require harshness to be unfavorable for implementing.
CN106957053A discloses a kind of method that iron powder is the quick macroscopic preparation of graphene of reducing agent.Using Hummer
Method prepares graphite oxide, is diluted with water, and ultrasonic vibration obtains graphene oxide acid solution, and iron powder reducing is added under Elevated Temperature Conditions, stands
Graphene powder is filtered to obtain in cooling, but longer the time required to the technique, is not suitable for quickly preparing.
CN106299310A discloses a kind of method of efficiently preparation graphene/metal oxide composite material, passes through γ
X ray irradiation x, the graphite oxide single step reaction of induced adsorption metal ion obtains graphene/metal oxide composite material, synchronous
Realize the reduction of graphene oxide and the oxidation of metal ion.But this method needs gamma Rays, is not appropriate for quickly making
Standby a large amount of graphene/metal oxide composite materials.
Therefore, the dimensionally stable of simple and easy, at low cost one kind, high yield, pollution-free, easy popularization and oxide is developed
The graphene of Load Balanced and the new method of Graphene/metal oxide hybrid material are to graphene and graphene-based composite material
Industrial application be of great significance.
Summary of the invention
In view of the deficiencies of the prior art, to prepare graphene-metal oxide compound the purpose of the present invention is to provide a kind of
The method of powder body material is especially to provide a kind of quick macroblock quantization and prepares graphene-metal oxide composite powder material side
Method.
In order to achieve that object of the invention, the present invention uses following technical scheme：
On the one hand, the present invention, which provides, a kind of prepares graphene-metal oxide composite powder material method, the method
Include the following steps：
(1) under ultrasound and/or stirring, graphene oxide is dispersed in metal salt solution, stands removal supernatant liquor
Afterwards, the graphene oxide block materials of metal ion intercalation are dried to obtain；
(2) the graphene oxide block materials for the metal ion intercalation that step (1) obtains are heated at 400-600 DEG C,
20s-60min is reacted, graphene-metal oxide composite powder material is obtained.
In the present invention, by the way that graphene oxide to be dispersed in metal salt solution, then heating can at high temperature
Complete the preparation of graphene-metal oxide composite powder material, in this process, the reduction of graphene oxide and metal oxygen
The oxidation reaction of change carries out simultaneously.Quickly graphene oxide composite material is rapidly heated under high temperature, causes to contain on graphene oxide
Oxygen groups are quickly removed at high temperature, and do not influence the integrally-built integrality of graphene, can guarantee graphene oxide
Reduction, improves the electric conductivity of graphene；The metal ion being attached on graphene oxide in this process quickly aoxidizes, in oxygen
While becoming vapor and carbon dioxide on graphite alkene under oxygen-containing group high temperature, enriched so that graphene composite material generates
Pore structure, increase its specific surface area, optimize the fit structure of metal oxide and graphene, so that graphene composite wood
Material performance is optimized.
Preferably, the frequency of the ultrasound be 50-1000W, such as 50W, 60W, 70W, 80W, 100W, 120W, 150W,
180W, 200W, 250W, 280W, 300W, 350W, 400W, 450W, 500W, 600W, 700W, 800W, 900W or 1000W.
Preferably, the rate of the stirring be 20-1000rpm, such as 20rpm, 50rpm, 80rpm, 100rpm,
150rpm, 200rpm, 400rpm, 600rpm, 800rpm, 900rpm or 1000rpm.
Preferably, it is described ultrasound and/or stirring time be 1-60min, such as 1min, 5min, 8min, 10min,
13min, 15min, 18min, 20min, 25min, 30min, 40min, 45min, 50min or 60min.
Preferably, the metal salt be iron chloride, nickel chloride, cobalt chloride, manganese chloride, molybdenum chloride, copper chloride, ferric nitrate,
Appointing in nickel nitrate, cobalt nitrate, nitric acid molybdenum, copper nitrate, ferric acetate, nickel acetate, cobalt acetate, manganese acetate, acetic acid molybdenum or copper acetate
It anticipates a kind of or at least two combinations.
Preferably, the concentration of the metal salt solution is 0.05mol L-1-5mol L-1, such as 0.05mol L-1、
0.08mol L-1、0.1mol L-1、0.3mol L-1、0.5mol L-1、0.8mol L-1、1mol L-1、2mol L-1、3mol L-1、4mol L-1Or 5mol L-1。
Preferably, the mass ratio of the graphene oxide and metal salt is 1:0.1-1:10, such as 1:0.1,1:0.3,1:
0.5,1:0.8,1:1,1:1.2,1:1.5,1:2,1:3,1:4,1:5,1:6,1:7,1:8,1:9 or 1:10.
In the present invention, step (1) described drying preferably spontaneously dries.Obtained after the drying of step (1) metal from
The graphene oxide block materials of sub- intercalation, metal ion, which is attached on the lamella of graphene, forms metal ion, generates stone
The intercalation configuration of black alkene lamella and metal ion.
In the present invention, the graphene oxide block materials obtained step (1) in step (2) add at 400-600 DEG C
Heat, such as heating temperature are 400 DEG C, 420 DEG C, 450 DEG C, 480 DEG C, 500 DEG C, 520 DEG C, 550 DEG C, 580 DEG C or 600 DEG C.Reaction
Time can for 20s, 25s, 30s, 40s, 45s, 50s, 1min, 5min, 10min, 15min, 20min, 25min, 30min,
35min, 40min, 45min, 50min, 55min or 60min.
The present invention needs to select the treatment temperature of suitable graphene oxide block materials, if temperature is too low, such as
It is 300 DEG C, even lower, then oxygen-containing group on graphene oxide can be made to be difficult the removal for having higher degree, influence graphite oxide
The reduction effect of alkene, and but also metal oxide is not easy to be formed, and then influence the structure and property of graphene composite material
The performance of energy.If temperature is excessively high, not only oxygen-containing group is destroyed on graphene oxide, but also graphene itself and composite wood
Material overall structure can wreck, and the structure and performance that also will affect composite material play.
Preparation method of the present invention can quickly macroscopic preparation of graphene-metal oxide composite powder material, preferably
Heating temperature is 500-600 DEG C, reaction time 20-40s.
Preferably, step (2) reaction carries out in inert gas shielding or air, preferably carries out in air.This
Invention can be completed not needing under inert gas shielding, complete the reduction of graphene oxide and the oxidation of metal ion, break through
The problem of must just can guarantee the reduction of graphene oxide under inert gas protection in the prior art.
As the preferred technical solution of the present invention, the quick macroblock quantization prepares graphene and graphene-metal oxide
The method of composite powder material specifically includes following steps：
(1) under ultrasound and/or stirring, it is 0.05mol L that graphene oxide, which is dispersed in concentration,-1-5mol L-1Metal
In salting liquid, so that the mass ratio of graphene oxide and metal salt is 1:0.1-1:10, it is naturally dry after standing removal supernatant liquor
The dry graphene oxide block materials for obtaining metal ion intercalation；
(2) the graphene oxide block materials for the metal ion intercalation that step (1) obtains are heated at 400-600 DEG C,
20s-60min is reacted, the reaction carries out in air, obtains graphene-metal oxide composite powder material.
Compared with existing synthetic method, preparation method of the present invention is not related to organic solvent, and gained powder body material is not required to
Post-processing can be used directly.And entire preparation process have it is easy to operate, at low cost, environmentally friendly, can quickly produce on a large scale
The advantages that.
On the other hand, the graphene-metal oxide being prepared the present invention provides preparation method as described above is compound
Powder body material.
Preferably, the average-size of metal oxide is less than in the graphene-metal oxide composite powder material
100nm, such as can be 90nm, 85nm, 80nm, 70nm, 60nm, 50nm, 40nm, 30nm, 20nm, 10nm, 5nm etc..
The graphene that the present invention is prepared-metal oxide composite powder material has abundant pore structure, by this
Invention preparation method optimizes the configuration structure of graphene and metal oxide, so that graphene-metal oxide composite granule
The electrochemistry and catalytic performance of material are improved.
On the other hand, it is dynamic in preparation that the present invention provides graphene as described above-metal oxide composite powder materials
Application in power battery, supercapacitor, energy-storage battery, electronic material, communication material, catalysis material or biological medicine material.
Compared with the existing technology, the invention has the advantages that：
The present invention is using graphene oxide and metal salt as raw material, the quick magnanimity preparation by the way of a step high-temperature heat treatment
Graphene-metal oxide composite powder material is obtained, while solving the reduction of graphene oxide and the oxygen of metal ion
Change, realizes the material for preparing of quick magnanimity, and its reduction and gold for carrying out graphene oxide preferably in air atmosphere
The oxidation for belonging to ion, breaches asking for the reduction that must just can guarantee graphene oxide under inert gas protection in the prior art
Topic, entire preparation process have it is easy to operate, at low cost, environmentally friendly, can be mass-produced, the graphene composite material being prepared
Pore structure abundant is generated, its specific surface area is increased, optimizes the fit structure of metal oxide and graphene, so that graphite
Alkene composite property is optimized, and power battery, supercapacitor, energy-storage battery, electronics, communication, letter can be widely used in
Breath, catalysis and biological medicine etc. field.
Detailed description of the invention
Fig. 1 is graphene-iron chloride composite powder material scanning electron microscope (SEM) photograph that embodiment 1 is prepared, and scale is
10μm。
Fig. 2 is graphene-iron chloride composite powder material scanning electron microscope (SEM) photograph that embodiment 1 is prepared, and scale is
500nm。
Fig. 3 is graphene-iron chloride composite powder material transmission electron microscope picture that embodiment 1 is prepared, and scale is
500nm。
Fig. 4 is graphene-iron chloride composite powder material XPS figure that embodiment 1 is prepared.
Specific embodiment
The technical scheme of the invention is further explained by means of specific implementation.Those skilled in the art should be bright
, the described embodiments are merely helpful in understanding the present invention, should not be regarded as a specific limitation of the invention.
Embodiment 1
In the present embodiment, graphene-metal-oxide powder material is prepared by following preparation method, specifically include as
Lower step：
(1) graphene oxide 100mg, iron chloride 10mg are weighed, the two mass ratio is 1:0.1, stone will be aoxidized under ultrasound
It is 0.05mol L that black alkene, which is scattered in concentration,-1Ferric chloride in aqueous solution in, ultrasonic frequency be 60W, ultrasonic disperse 20min, to equal
It after even dispersion, staticly settles, removes last time clear liquid, then spontaneously dry at room temperature and obtain the oxidation of metal ion intercalation
Graphene block materials；
(2) the graphene oxide block materials for the metal ion intercalation that step (1) obtains are placed in tube furnace, air atmosphere
Lower 500 DEG C of heat treatment 25s is enclosed, graphene-iron chloride composite powder material is obtained.
Using scanning electron microscope (JEOL, JSM-6700F, Japan, Japan Electronics) to the graphene-iron chloride being prepared
Composite powder material is characterized, as a result as depicted in figs. 1 and 2, from figure 1 it appears that in the composite granule of preparation, oxygen
Compound particle is uniformly distributed in powder body material.Figure is further amplified for Fig. 1's in Fig. 2, further verifies the equal of oxide particle
It is even to inlay, while can see composite powder material with pore structure abundant.
Using transmission electron microscope (JEOL, JSM-6700F, Japan, Japan Electronics) to the graphene-iron chloride being prepared
Composite powder material is characterized, as a result as shown in figure 3, it can be seen from the figure that oxidate nano project is uniformly distributed in stone
Black alkene sheet surfaces, particle size are less than 100nm.
X-ray photoelectron spectroscopy (PE company of U.S. PHI-5400 type) is compound to the graphene-iron chloride being prepared
Powder body material is characterized, as a result as shown in figure 4, it can be seen from the figure that in XPS photoelectron spectroscopy be located at 711.2eV and
Two peaks of 724.7eV can belong to di-iron trioxide well.
Embodiment 2
In the present embodiment, graphene-metal-oxide powder material is prepared by following preparation method, specifically include as
Lower step：
(1) graphene oxide 100mg, metal salt 100mg are weighed, the two mass ratio is 1:1, by oxygen under ultrasound and stirring
It is 0.5mol L that graphite alkene, which is scattered in concentration,-1Aqueous metal salt in, ultrasonic frequency be 80W, ultrasonic disperse 10min,
Stirring rate is 100rpm, after evenly dispersed, is staticly settled, and removes last time clear liquid, then spontaneously dries at room temperature
Obtain the graphene oxide block materials of metal ion intercalation；
(2) the graphene oxide block materials for the metal ion intercalation that step (1) obtains are placed in tube furnace, air atmosphere
Lower 600 DEG C of heat treatment 20s is enclosed, graphene-metal oxide composite powder material is obtained.
Embodiment 3
In the present embodiment, graphene-metal-oxide powder material is prepared by following preparation method, specifically include as
Lower step：
(1) graphene oxide 100mg, metal salt 1g are weighed, the two mass ratio is 1:10, by graphene oxide under ultrasound
Being scattered in concentration is 3mol L-1Aqueous metal salt in, ultrasonic frequency be 100W, ultrasonic disperse 10min, to evenly dispersed
Afterwards, it staticly settles, removes last time clear liquid, then spontaneously dry at room temperature and obtain the graphene oxide of metal ion intercalation
Block materials；
(2) the graphene oxide block materials for the metal ion intercalation that step (1) obtains are placed in tube furnace, air atmosphere
Lower 550 DEG C of heat treatment 30s is enclosed, graphene-metal oxide composite powder material is obtained.
Embodiment 4
In the present embodiment, graphene-metal-oxide powder material is prepared by following preparation method, specifically include as
Lower step：
(1) graphene oxide 100mg, metal salt 500mg are weighed, the two mass ratio is 1:5, by graphite oxide under ultrasound
It is 2mol L that alkene, which is scattered in concentration,-1Aqueous metal salt in, ultrasonic frequency be 100W, ultrasonic disperse 5min, to uniformly divide
It after dissipating, staticly settles, removes last time clear liquid, then spontaneously dry at room temperature and obtain the graphite oxide of metal ion intercalation
Alkene block materials；
(2) the graphene oxide block materials for the metal ion intercalation that step (1) obtains are placed in tube furnace, air atmosphere
Lower 600 DEG C of heat treatment 25s is enclosed, graphene-metal oxide composite powder material is obtained.
Embodiment 5
In the present embodiment, graphene-metal-oxide powder material is prepared by following preparation method, specifically include as
Lower step：
(1) graphene oxide 100mg, metal salt 200mg are weighed, the two mass ratio is 1:2, by graphite oxide under ultrasound
It is 5mol L that alkene, which is scattered in concentration,-1Aqueous metal salt in, ultrasonic frequency be 80W, ultrasonic disperse 15min, to uniformly divide
It after dissipating, staticly settles, removes last time clear liquid, then spontaneously dry at room temperature and obtain the graphite oxide of metal ion intercalation
Alkene block materials；
(2) the graphene oxide block materials for the metal ion intercalation that step (1) obtains are placed in tube furnace, air atmosphere
Lower 600 DEG C of heat treatment 40s is enclosed, graphene-metal oxide composite powder material is obtained.
Embodiment 6
In the present embodiment, graphene-metal-oxide powder material is prepared by following preparation method, specifically include as
Lower step：
(1) graphene oxide 100mg, metal salt 100mg are weighed, the two mass ratio is 1:1, by graphite oxide under ultrasound
It is 1mol L that alkene, which is scattered in concentration,-1Aqueous metal salt in, ultrasonic frequency be 50W, ultrasonic disperse 10min, to uniformly divide
It after dissipating, staticly settles, removes last time clear liquid, then spontaneously dry at room temperature and obtain the graphite oxide of metal ion intercalation
Alkene block materials；
(2) the graphene oxide block materials for the metal ion intercalation that step (1) obtains are placed in tube furnace, indifferent gas
500 DEG C of heat treatment 30s under conditions of body protection, obtain graphene-metal oxide composite powder material.
Embodiment 7
In the present embodiment, graphene-metal-oxide powder material is prepared by following preparation method, specifically include as
Lower step：
(1) graphene oxide 100mg, metal salt 1g are weighed, the two mass ratio is 1:10, by graphene oxide under ultrasound
Being scattered in concentration is 5mol L-1Aqueous metal salt in, ultrasonic frequency be 60W, ultrasonic disperse 15min, to evenly dispersed
Afterwards, it staticly settles, removes last time clear liquid, then spontaneously dry at room temperature and obtain the graphene oxide of metal ion intercalation
Block materials；
(2) the graphene oxide block materials for the metal ion intercalation that step (1) obtains are placed in tube furnace, indifferent gas
600 DEG C of heat treatment 20s under conditions of body protection, obtain graphene-metal oxide composite powder material.
Embodiment 8
In the present embodiment, graphene-metal-oxide powder material is prepared by following preparation method, specifically include as
Lower step：
(1) graphene oxide 100mg, metal salt 100mg are weighed, the two mass ratio is 1:1, by graphite oxide under ultrasound
It is 2mol L that alkene, which is scattered in concentration,-1Aqueous metal salt in, ultrasonic frequency be 80W, ultrasonic disperse 10min, to uniformly divide
It after dissipating, staticly settles, removes last time clear liquid, then spontaneously dry at room temperature and obtain the graphite oxide of metal ion intercalation
Alkene block materials；
(2) the graphene oxide block materials for the metal ion intercalation that step (1) obtains are placed in tube furnace, indifferent gas
400 DEG C of heat treatment 30min under conditions of body protection, obtain graphene-metal oxide composite powder material.
The present invention illustrates the process method of the present invention through the above embodiments, but the invention is not limited to above-mentioned techniques
Step is done not mean that the present invention must rely on the above process steps to be carried out.Person of ordinary skill in the field should
It is illustrated, any improvement in the present invention, the addition of equivalence replacement and auxiliary element to raw material selected by the present invention, concrete mode
Selection etc., all of which fall within the scope of protection and disclosure of the present invention.
Claims (10)
1. a kind of prepare graphene-metal oxide composite powder material method, which is characterized in that the method includes following
Step：
(1) under ultrasound and/or stirring, graphene oxide is dispersed in metal salt solution, after standing removal supernatant liquor, is done
The dry graphene oxide block materials for obtaining metal ion intercalation；
(2) the graphene oxide block materials for the metal ion intercalation that step (1) obtains are heated at 400-600 DEG C, is reacted
20s-60min obtains graphene-metal oxide composite powder material.
2. preparation method according to claim 1, which is characterized in that the frequency of the ultrasound is 50-1000W；
Preferably, the rate of the stirring is 20-1000rpm；
Preferably, the time of the ultrasound and/or stirring is 1-60min.
3. preparation method according to claim 1 or 2, which is characterized in that the metal salt is iron chloride, nickel chloride, chlorine
Change cobalt, manganese chloride, molybdenum chloride, copper chloride, ferric nitrate, nickel nitrate, cobalt nitrate, nitric acid molybdenum, copper nitrate, ferric acetate, nickel acetate, vinegar
In sour cobalt, manganese acetate, acetic acid molybdenum or copper acetate any one or at least two combination.
4. preparation method according to any one of claim 1-3, which is characterized in that the concentration of the metal salt solution is
0.05mol L-1-5mol L-1。
5. preparation method described in any one of -4 according to claim 1, which is characterized in that the graphene oxide and metal salt
Mass ratio be 1:0.1-1:10.
6. preparation method according to any one of claims 1-5, which is characterized in that step (1) drying is nature
It is dry.
7. preparation method according to claim 1 to 6, which is characterized in that the temperature of step (2) described heating
It is 500-600 DEG C, reaction time 20-40s；
Preferably, step (2) reaction carries out in inert gas shielding or air, preferably carries out in air.
8. preparation method described in any one of -7 according to claim 1, which is characterized in that the preparation method includes following step
Suddenly：
(1) under ultrasound and/or stirring, it is 0.05mol L that graphene oxide, which is dispersed in concentration,-1-5mol L-1Metal salt solution
In, so that the mass ratio of graphene oxide and metal salt is 1:0.1-1:10, after standing removal supernatant liquor, natural drying is obtained
The graphene oxide block materials of metal ion intercalation；
(2) the graphene oxide block materials for the metal ion intercalation that step (1) obtains are heated at 400-600 DEG C, is reacted
20s-60min, the reaction carry out in air, obtain graphene-metal oxide composite powder material.
9. the graphene that preparation method according to claim 1 to 8 is prepared-metal oxide composite powder
Body material；
Preferably, the average-size of metal oxide is less than 100nm in the graphene-metal oxide composite powder material.
10. graphene according to claim 9-metal oxide composite powder material is preparing power battery, super electricity
Application in container, energy-storage battery, electronic material, communication material, catalysis material or biological medicine material.
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| CN113980654A (en) * | 2021-11-18 | 2022-01-28 | 湘潭大学 | Graphene alloy composite phase change material and preparation method and application thereof |
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