CN105731440A - Method for achieving stripping preparation of graphene nanoplatelets by means of phase change material - Google Patents
Method for achieving stripping preparation of graphene nanoplatelets by means of phase change material Download PDFInfo
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Abstract
The invention provides a method for achieving stripping preparation of graphene nanoplatelets by means of a phase change material.The method comprises the steps that graphite serves as the raw materials, graphite powder is modified with boric acid, the phase change material is inserted into graphite layers in a molten state, the graphite layers are pulled and separated by means of microdefects formed due to the fact that volume shrinkage occurs when the phase change material is converted into the solid phase from the liquid phase, the graphite layers are mechanically sheared and stripped under the freezing condition, the phase change material is subjected to crystalline grain embrittlement under the freezing condition, the graphite layers are stripped instantly, and therefore the graphene nanoplatelets are obtained.The cost of the graphene nanoplatelets is greatly reduced, and the graphene nanoplatelets can be added and used in quantity in composite materials of rubber, plastics, coating, lubricating oil, sewage treatment and the like.The preparation method is easy to control and capable of achieving large-scale and stable production, auxiliary materials used in the production process are easy to clean and capable of being reused after being crystallized and separated, pollution-free preparation of the graphene nanoplatelets is achieved, and the method is beneficial for promoting large-scale application of graphene.
Description
Technical field
The present invention relates to grapheme material field, the preparation method being specifically related to graphene microchip, particularly relate to a kind of method utilizing phase change materials to peel off preparation graphene microchip.
Background technology
Graphene is the flaky substance referring exclusively to be made up of single carbon atom theoretically.At present, simplest method is by mechanical phonograph recorder separation, is directly cut down from bigger graphite crystal by graphene platelet.Surface expanded, that friction makes graphite can also be passed through and produce flocculus, the crystal of these flocculus shapes contains the Graphene of monolayer.But the thin slice that shortcoming is said method to be obtained is to filter out the graphene platelet of monolayer, and its size is wayward, it is impossible to reliably manufacture stable graphene film.
Advanced graphene preparation method mainly takes vapour deposition process, and after utilizing gaseous carbon source at high temperature to decompose, the catalytic growth on matrix surface prepares Graphene, and the method is the important method preparing high-quality and large area single-layer graphene.But its working condition is comparatively harsh, power consumption is big, and cost is high.And, directly adopt gaseous carbon sources largely to add the danger of production.
Domestic currently mainly to adopt graphite oxide reducing process be prepare the main method of Graphene, and the method is that graphite is carried out Strong oxdiative process, after obtaining graphite oxide, then it is carried out stripping prepares graphene oxide, eventually pass reduction treatment and obtain Graphene.Graphite oxide is warming up to 150～600 DEG C with certain heating rate by Chinese invention patent 200810151807.X under a high vacuum, maintains constant temperature 0.5～20H, obtains graphene oxide sheet.Due to the structure of meeting heavy damage graphene sheet layer in Strong oxdiative process, although through reduction treatment, the electron conjugated structure of graphene sheet layer obtains part and recovers, and the property indices of gained grapheme material still exists bigger gap with high-quality Graphene.In addition, the oxidizing process of graphite typically requires substantial amounts of highly acid oxidant such as concentrated sulphuric acid, concentrated nitric acid, potassium permanganate etc., and there is a need to high-temperature process in reduction process or use the chemical substance that hydrazine hydrate, sodium borohydride etc. are poisonous, and not only energy consumption is big, efficiency is low, and cost is high and contaminated environment.
Mechanical stripping method is a kind of simple method that can prepare high-quality graphene with low cost.In order to make graphite layers peeling-off, the stripping means that mechanical-physical stripping method is commonly used have conventional ball mill, stirring ball-milling, grinding etc..But by abrading-ball, graphite composite powder is ground, this method is big owing to local applies pressure, and powerful impulsive force can make Graphene produce fault of construction.Chinese invention patent application number 201280019582.7 discloses a kind of method preparing Graphene, grinds 4 hours acquisition Graphenes by grinding, ball milling, airflow milling etc. by ionic liquid.Promote the stripping of graphite by ionic liquid, but adopted the Graphene crystalline size grinding acquisition for a long time little, and graphene layer lattice can have been made to be affected by ionic liquid.
It practice, the preparation of single-layer graphene also rests in a small amount of preparation in grams at present, large-scale industrial production can be accomplished but without people.But meanwhile, the performance of Graphene excellence is badly in need of widely applying in fields such as composite, lubriation material, coating, sewage disposals, and prior art is difficult to meet this large-scale demand.Therefore the graphene microchip being unit with Graphene becomes Graphene by studying the optimum selection entered to application.Graphene microchip, it is multi-layer graphene structure, but the characteristic of Graphene, such as conduction, heat conduction, printing opacity, flexibility etc. are kept very well, can add to widely in existing various basic material as a kind of industrial raw materials, the performance of current material is improved.In order to obtain graphene microchip, Chinese invention patent application number 201310579504.9 discloses the graphene microchip preparation method that a kind of high-specific surface area, size are controlled, the method, with big particle diameter expansible graphite for raw material, prepares highly expanded multiplying power expanded graphite under high temperature；With Organic substance for intercalation thing, in blended insertion expanded graphite lamella, high-temp combustion under certain atmosphere, expand and peel off the graphene microchip obtaining certain size.But, in the thermal expansion process of graphite oxide, it is necessary to higher subnormal ambient realizes the successful expansion of graphite oxide, and its condition is harsher, the requirement of equipment is high, it is impossible to produce continuously, it is difficult to amplify, the development of restriction graphene microchip.
Graphene microchip is due to its good characteristic having, and its application is boundless, such as improves heat conduction and the heat dispersion of plastic cement, and plastic cement conducts electricity and antistatic modified, strengthens the intensity of plastic cement, and improves wear-resisting, greasy property and the corrosion resistance etc. of plastic cement.Owing to having nano thickness, easily and the uniform compound of other material such as polymeric material, and forming good compound interface, the high intensity of Graphene, lubrication, high temperature resistant and conductive characteristic can be taken in the middle of composite by graphene microchip, such that it is able to design, prepare high-performance composite materials.If Graphene plastics, Graphene rubber, Graphene conductive ink, Graphene coating, Graphene suction ripple hidden function plate, Graphene radiating element, Graphene functional coating etc. are all good application.It is desirable that realize when not damaging graphene layer crystal structure efficiently peeling off graphite to prepare graphene microchip, thus providing technical support for large-scale using mineral carbon alkene.
Summary of the invention
For the problems referred to above, the present invention proposes a kind of method utilizing phase change materials to peel off preparation graphene microchip.The method utilizes phase-change material to be changed into, by liquid phase, the microdefect that solid-phase generation volume contraction is formed, under freezing conditions mechanical shearing is peeled off and is obtained graphene microchip, the cost of graphene microchip is greatly reduced, makes graphene microchip can add use in a large number at composites such as rubber, plastics, coating, lubricating oil, sewage disposals.
For solve the problems referred to above, the present invention by the following technical solutions:
A kind of method utilizing phase change materials to peel off preparation graphene microchip, it is characterized in that: with phase change materials for intercalator, intercalator is placed in graphite powder interlayer, phase change materials is utilized to be changed into, by liquid phase, the microdefect that solid-phase generation volume contraction is formed, being peeled off by mechanical shearing and obtain graphene microchip, concrete grammar is as follows:
(1) graphite powder is pressed quality 1:10-30 with absolute methanol or dehydrated alcohol, stirring 30-45min mix homogeneously at ambient temperature, add boric acid stirring to be completely dissolved to boric acid, close and place more than 24h, isolate absolute methanol or dehydrated alcohol, dry, obtain pretreating graphite powder, the addition of its mesoboric acid is the 3-5% of graphite powder quality；
(2) phase change materials is heated to being completely melt under 40-60 DEG C of condition, pretreating graphite powder step (1) obtained adds in the phase change materials being completely melt, 1-2h is disperseed with the rotating speed high-speed stirred of 200-800r/min, phase change materials is made to insert the interlayer of graphite, naturally cooling to room temperature, wherein pretreating graphite powder is 1:0.1-0.5 with the mass ratio of phase change materials；It is crystalloid solid phase when phase change materials is room temperature, is the phase-change material of liquid phase under 40-60 DEG C of condition；
(3) intercalated graphite that step (2) obtains is joined in mechanical shearing stripping off device, be held below under the cryogenic conditions of-15 DEG C by liquid nitrogen input, peel off to sheet thickness less than within the scope of 50nm, then discharging；
(4) material that step (3) obtains is carried out with deionized water, ethanol in cleaning machine, except maize without germ, phase change materials, dry, obtain graphene microchip.
Described phase-change material is crystalloid when solid phase, it is preferable that the one in positive certain herbaceous plants with big flowers acid, lauric acid, myristic acid.
Described phase-change material is hydrated salt.
Described hydrated salt is the one in Sodium acetate trihydrate, five water sodium thiosulfate, disodium hydrogen phosphate, sal glauberi, it is molten condition when 40-60 DEG C, very easily be combined with the layer part of graphite, and when room temperature, hydrated salt is owing to phase in version is to crystalline transformation, there is volume contraction, thus producing microdefect in graphite layers, embrittlement is easily there is when low temperature further as hydrated salt crystal, thus under the cryogenic conditions lower than-15 DEG C, graphite can be made to peel off by mechanical shearing stripping off device becomes graphene microchip.
Described mechanical shearing stripping off device is the medium grinder such as agitating ball mill, planetary ball mill of routine, vibrator, rotary-tube type ball mill, sand mill, or jet mill such as flat air flow crusher, circulation pipe air flow crasher, rotary ejection type jet mill, injecting type jet mill, target formula jet mill, fluidized bed airflow pulverizer, Counter-impact flow pulverizer, or high pressure grinding rolls.
The Van der Waals force of graphite powder interlayer makes graphite layers be difficult to peel off smoothly, and by can effectively reduce Van der Waals force at interlayer intercalation, but this intercalation remains and is difficult to separate graphite linings.Although existing organic or inorganic intercalator at present, but effect is unsatisfactory, is particularly difficult to volume production and prepares graphene microchip.The feature that the present invention highlights is to propose a kind of method utilizing phase change materials to peel off preparation graphene microchip, the method is with graphite for raw material, by utilizing boric acid that graphite powder is modifiied, phase-change material is made to insert graphite layers in the blown state, phase-change material is utilized to be changed into, by liquid phase, the microdefect that solid-phase generation volume contraction is formed, graphite layers is made to pull open, further, mechanical shearing is under freezing conditions utilized to peel off, phase-change material is crystalloid, enbrittling, under freezing conditions crystal grain embrittlement makes graphite linings moment peel off, thus obtaining graphene microchip.Further, the present invention adopts boric acid, phase-change material as preparing auxiliary agent, it is easy to clean and recycling after crystallization, it is achieved that pollution-free preparation graphene microchip.
A kind of method utilizing phase change materials to peel off preparation graphene microchip of the present invention; achieving large-scale production graphene microchip, the cost of graphene microchip is greatly reduced, graphene microchip has nano thickness; easily and the uniform compound of other material such as polymeric material, and form good compound interface；There is excellent conduction, lubrication, the characteristic such as corrosion-resistant, high temperature resistant.Use can be added in a large number in the composites such as rubber, plastics, coating, lubricating oil, sewage disposal.
By the graphene microchip test that preparation method of the present invention is obtained, its thickness is within the scope of 15-50nm, in Graphene stratiform accumulation body.By the graphene microchip operating specification according to Nano filling, the mass fraction with 3% is filled and is scattered in ABS resin, and the electrical conductivity of its composite reaches 2.6 × 10-4S/cm。
A kind of utilization of the present invention turns material mutually and becomes the method peeling off preparation graphene microchip, and compared with prior art, its prominent feature and excellent effect are in that:
1, utilize boric acid that graphite powder is modifiied, phase-change material is made to insert graphite layers in the blown state, utilize phase change materials to be changed into, by liquid phase, the microdefect that solid-phase generation volume contraction is formed, make graphite layers pull open, make graphite become the graphene microchip piled up by Graphene unit.
2, under freezing conditions mechanical shearing is peeled off, and phase change materials under freezing conditions crystal grain embrittlement makes graphite linings moment peel off, thus obtaining graphene microchip.
3, preparation method of the present invention is easily controllable; scale steady production can be realized; the auxiliary material that production process uses easily cleans and recycling after crystallization, it is achieved that pollution-free preparation graphene microchip, Productive statistics is little, cost is low, have significant market using value.
Detailed description of the invention
Below by way of detailed description of the invention, the present invention is described in further detail, but this should not being interpreted as, the scope of the present invention is only limitted to Examples below.When without departing from said method thought of the present invention, the various replacements made according to ordinary skill knowledge and customary means or change, should be included in the scope of the present invention.
Embodiment 1
A kind of method utilizing phase change materials to peel off preparation graphene microchip, concrete grammar is as follows:
(1) graphite powder is pressed quality 1:30 with dehydrated alcohol, at ambient temperature stirring 45min mix homogeneously, add boric acid stirring and be completely dissolved to boric acid, close and place more than 24h, isolate dehydrated alcohol, dry, obtaining pretreating graphite powder, the addition of its mesoboric acid is the 4% of graphite powder quality；
(2) Sodium acetate trihydrate is heated to being completely melt under 40 DEG C of conditions, pretreating graphite powder step (1) obtained adds the Sodium acetate trihydrate being completely melt, 2h is disperseed with the rotating speed high-speed stirred of 500r/min, Sodium acetate trihydrate is made to insert the interlayer of graphite, naturally cooling to room temperature, wherein pretreating graphite powder is 1:0.4 with the mass ratio of Sodium acetate trihydrate；
(3) intercalated graphite that step (2) obtains is joined in agitating ball mill stripping off device, be held below under the cryogenic conditions of-15 DEG C by liquid nitrogen input, peel off to sheet thickness less than within the scope of 50nm, then discharging；
(4) material that step (3) obtains is carried out with deionized water in cleaning machine, except maize without germ, Sodium acetate trihydrate, dry, obtain graphene microchip.
Embodiment 2
A kind of method utilizing phase change materials to peel off preparation graphene microchip, concrete grammar is as follows:
(1) graphite powder is pressed quality 1:10 with absolute methanol, at ambient temperature stirring 30min mix homogeneously, add boric acid stirring and be completely dissolved to boric acid, close and place more than 24h, isolate absolute methanol, dry, obtaining pretreating graphite powder, the addition of its mesoboric acid is the 5% of graphite powder quality；
(2) sal glauberi is heated to being completely melt under 60 DEG C of conditions, pretreating graphite powder step (1) obtained adds the sal glauberi being completely melt, 2h is disperseed with the rotating speed high-speed stirred of 200r/min, sal glauberi is made to insert the interlayer of graphite, naturally cooling to room temperature, wherein pretreating graphite powder is 1:0.5 with the mass ratio of sal glauberi；
(3) intercalated graphite that step (2) obtains is joined circulation pipe air flow crasher and shears in stripping off device, be held below by liquid nitrogen input under the cryogenic conditions of-15 DEG C, peel off to sheet thickness less than 50nm scope, then discharging；
(4) material that step (3) obtains is carried out with deionized water in cleaning machine, except maize without germ, sal glauberi, dry, obtain graphene microchip.
Embodiment 3
A kind of method utilizing phase change materials to peel off preparation graphene microchip, concrete grammar is as follows:
(1) graphite powder is pressed quality 1:15 with dehydrated alcohol, at ambient temperature stirring 45min mix homogeneously, add boric acid stirring and be completely dissolved to boric acid, close and place more than 24h, isolate dehydrated alcohol, dry, obtaining pretreating graphite powder, the addition of its mesoboric acid is the 3% of graphite powder quality；
(2) five water sodium thiosulfate are heated to being completely melt under 50 DEG C of conditions, pretreating graphite powder step (1) obtained adds in the five water sodium thiosulfate being completely melt, 1h is disperseed with the rotating speed high-speed stirred of 800r/min, five water sodium thiosulfate are made to insert the interlayer of graphite, naturally cooling to room temperature, wherein the mass ratio of pretreating graphite powder and five water sodium thiosulfate is 1:0.3；
(3) intercalated graphite that step (2) obtains is joined in target formula jet mill mechanical shearing stripping off device, be held below under the cryogenic conditions of-15 DEG C by liquid nitrogen input, peel off to sheet thickness less than within the scope of 50nm, then discharging；
(4) material that step (3) obtains is carried out with deionized water in cleaning machine, except maize without germ, five water sodium thiosulfate, dry, obtain graphene microchip.
Embodiment 4
A kind of method utilizing phase change materials to peel off preparation graphene microchip, concrete grammar is as follows:
(1) graphite powder is pressed quality 1:30 with absolute methanol, at ambient temperature stirring 30min mix homogeneously, add boric acid stirring and be completely dissolved to boric acid, close and place more than 24h, isolate absolute methanol, dry, obtaining pretreating graphite powder, the addition of its mesoboric acid is the 3% of graphite powder quality；
(2) disodium hydrogen phosphate is heated to being completely melt under 60 DEG C of conditions, pretreating graphite powder step (1) obtained adds in the disodium hydrogen phosphate being completely melt, 1.5h is disperseed with the rotating speed high-speed stirred of 400r/min, disodium hydrogen phosphate is made to insert the interlayer of graphite, naturally cooling to room temperature, wherein pretreating graphite powder is 1:0.1 with the mass ratio of disodium hydrogen phosphate；
(3) intercalated graphite that step (2) obtains is joined in high pressure grinding rolls mechanical shearing stripping off device, be held below under the cryogenic conditions of-15 DEG C by liquid nitrogen input, peel off to sheet thickness less than within the scope of 50nm, then discharging；
(4) material that step (3) obtains is carried out with deionized water in cleaning machine, except maize without germ, disodium hydrogen phosphate, dry, obtain graphene microchip.
Embodiment 5
A kind of method utilizing phase change materials to peel off preparation graphene microchip, concrete grammar is as follows:
(1) graphite powder is pressed quality 1:30 with absolute methanol, at ambient temperature stirring 30min mix homogeneously, add boric acid stirring and be completely dissolved to boric acid, close and place more than 24h, isolate absolute methanol, dry, obtaining pretreating graphite powder, the addition of its mesoboric acid is the 3% of graphite powder quality；
(2) myristic acid is heated to being completely melt under 60 DEG C of conditions, pretreating graphite powder step (1) obtained adds in the myristic acid being completely melt, 1.5h is disperseed with the rotating speed high-speed stirred of 400r/min, myristic acid is made to insert the interlayer of graphite, naturally cooling to room temperature, wherein pretreating graphite powder is 1:0.1 with the mass ratio of myristic acid；
(3) intercalated graphite that step (2) obtains is joined in rotary ejection type jet mill mechanical shearing stripping off device, be held below under the cryogenic conditions of-15 DEG C by liquid nitrogen input, peel off to sheet thickness less than within the scope of 50nm, then discharging；
(4) material that step (3) obtains is carried out with deionized water, ethanol in cleaning machine, except maize without germ, myristic acid, dry, obtain graphene microchip.
Embodiment 6
A kind of method utilizing phase change materials to peel off preparation graphene microchip, concrete grammar is as follows:
(1) graphite powder is pressed quality 1:10 with absolute methanol, at ambient temperature stirring 30min mix homogeneously, add boric acid stirring and be completely dissolved to boric acid, close and place more than 24h, isolate absolute methanol, dry, obtaining pretreating graphite powder, the addition of its mesoboric acid is the 5% of graphite powder quality；
(2) lauric acid is heated to being completely melt under 60 DEG C of conditions, pretreating graphite powder step (1) obtained adds the lauric acid being completely melt, 2h is disperseed with the rotating speed high-speed stirred of 200r/min, lauric acid is made to insert the interlayer of graphite, naturally cooling to room temperature, wherein pretreating graphite powder and lauric mass ratio are 1:0.5；
(3) intercalated graphite that step (2) obtains is joined circulation pipe air flow crasher and shears in stripping off device, be held below by liquid nitrogen input under the cryogenic conditions of-15 DEG C, peel off to sheet thickness less than 50nm scope, then discharging；
(4) material that step (3) obtains is carried out with deionized water, ethanol in cleaning machine, except maize without germ, lauric acid, dry, obtain graphene microchip.
Claims (7)
1. one kind utilizes the method that phase change materials peels off preparation graphene microchip, it is characterized in that: with phase change materials for intercalator, intercalator is placed in graphite powder interlayer, phase change materials is utilized to be changed into, by liquid phase, the microdefect that solid-phase generation volume contraction is formed, being peeled off by mechanical shearing and obtain graphene microchip, concrete grammar is as follows:
(1) graphite powder is pressed quality 1:10-30 with absolute methanol or dehydrated alcohol, stirring 30-45min mix homogeneously at ambient temperature, add boric acid stirring to be completely dissolved to boric acid, close and place more than 24h, isolate absolute methanol or dehydrated alcohol, dry, obtain pretreating graphite powder, the addition of its mesoboric acid is the 3-5% of graphite powder quality；
(2) phase change materials is heated to being completely melt under 40-60 DEG C of condition, pretreating graphite powder step (1) obtained adds in the phase change materials being completely melt, 1-2h is disperseed with the rotating speed high-speed stirred of 200-800r/min, phase change materials is made to insert the interlayer of graphite, naturally cooling to room temperature, wherein pretreating graphite powder is 1:0.1-0.5 with the mass ratio of phase change materials；It is crystalloid solid phase when phase change materials is room temperature, is the phase-change material of liquid phase under 40-60 DEG C of condition；
(3) intercalated graphite that step (2) obtains is joined in mechanical shearing stripping off device, be held below under the cryogenic conditions of-15 DEG C by liquid nitrogen input, peel off to sheet thickness less than within the scope of 50nm, then discharging；
(4) material that step (3) obtains is carried out with deionized water, ethanol in cleaning machine, except maize without germ, phase change materials, dry, obtain graphene microchip.
2. according to claim 1 a kind of utilize phase change materials peel off preparation graphene microchip method, it is characterised in that: described phase-change material is the one in the acid of positive certain herbaceous plants with big flowers, lauric acid, myristic acid.
3. according to claim 1 a kind of utilize phase change materials peel off preparation graphene microchip method, it is characterised in that: described phase-change material is hydrated salt.
4. according to claim 3 a kind of utilize phase change materials peel off preparation graphene microchip method, it is characterised in that: described hydrated salt is the one in Sodium acetate trihydrate, five water sodium thiosulfate, disodium hydrogen phosphate, sal glauberi.
5. according to claim 1 a kind of utilize phase change materials peel off preparation graphene microchip method, it is characterised in that: described mechanical shearing stripping off device is agitating ball mill, planetary ball mill, vibrator, rotary-tube type ball mill or sand mill.
6. according to claim 1 a kind of utilize phase change materials peel off preparation graphene microchip method, it is characterised in that: described mechanical shearing stripping off device is flat air flow crusher, circulation pipe air flow crasher, rotary ejection type jet mill, injecting type jet mill, target formula jet mill, fluidized bed airflow pulverizer or Counter-impact flow pulverizer.
7. according to claim 1 a kind of utilize phase change materials peel off preparation graphene microchip method, it is characterised in that: described mechanical shearing stripping off device is high pressure grinding rolls.
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Cited By (6)
| Publication number | Priority date | Publication date | Assignee | Title |
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| CN106542524A (en) * | 2016-10-21 | 2017-03-29 | 成都新柯力化工科技有限公司 | A kind of graphene dispersion body and preparation method thereof |
| CN106928906A (en) * | 2017-05-02 | 2017-07-07 | 吉林建筑大学 | A kind of stannic oxide/graphene nano inorganic phase-changing material and preparation method thereof |
| CN107098338A (en) * | 2017-06-08 | 2017-08-29 | 乌兰察布市大盛石墨新材料股份有限公司 | A kind of grapheme material and preparation method thereof, the saggar for preparing graphene |
| TWI668187B (en) * | 2016-10-07 | 2019-08-11 | 林逸樵 | Device for rapidly producing graphene and method thereof |
| CN111559743A (en) * | 2020-05-25 | 2020-08-21 | 西安稀有金属材料研究院有限公司 | Preparation method and application of graphene powder |
| CN113816371A (en) * | 2021-09-25 | 2021-12-21 | 凯盛石墨碳材料有限公司 | Method for preparing expandable graphite by freeze-drying |
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| CN102786045A (en) * | 2012-07-27 | 2012-11-21 | 中国航空工业集团公司北京航空材料研究院 | Method for preparing oxidized graphene |
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| CN102786045A (en) * | 2012-07-27 | 2012-11-21 | 中国航空工业集团公司北京航空材料研究院 | Method for preparing oxidized graphene |
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| Publication number | Priority date | Publication date | Assignee | Title |
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| TWI668187B (en) * | 2016-10-07 | 2019-08-11 | 林逸樵 | Device for rapidly producing graphene and method thereof |
| CN106542524A (en) * | 2016-10-21 | 2017-03-29 | 成都新柯力化工科技有限公司 | A kind of graphene dispersion body and preparation method thereof |
| CN106542524B (en) * | 2016-10-21 | 2019-03-08 | 成都新柯力化工科技有限公司 | A kind of graphene dispersion body and preparation method thereof |
| CN106928906A (en) * | 2017-05-02 | 2017-07-07 | 吉林建筑大学 | A kind of stannic oxide/graphene nano inorganic phase-changing material and preparation method thereof |
| CN106928906B (en) * | 2017-05-02 | 2019-08-02 | 吉林建筑大学 | A kind of stannic oxide/graphene nano inorganic phase-changing material and preparation method thereof |
| CN107098338A (en) * | 2017-06-08 | 2017-08-29 | 乌兰察布市大盛石墨新材料股份有限公司 | A kind of grapheme material and preparation method thereof, the saggar for preparing graphene |
| CN107098338B (en) * | 2017-06-08 | 2023-07-18 | 乌兰察布市大盛石墨新材料股份有限公司 | Graphene material, preparation method thereof and sagger for preparing graphene |
| CN111559743A (en) * | 2020-05-25 | 2020-08-21 | 西安稀有金属材料研究院有限公司 | Preparation method and application of graphene powder |
| CN113816371A (en) * | 2021-09-25 | 2021-12-21 | 凯盛石墨碳材料有限公司 | Method for preparing expandable graphite by freeze-drying |
| CN113816371B (en) * | 2021-09-25 | 2023-09-08 | 凯盛石墨碳材料有限公司 | Method for preparing expandable graphite through freeze-drying |
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