CN105776192A - Method for continuously preparing graphene nanoplatelets by means of grinding stripping - Google Patents
Method for continuously preparing graphene nanoplatelets by means of grinding stripping Download PDFInfo
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Abstract
The invention belongs to the technical field of graphene, and particularly relates to a method for continuously preparing graphene nanoplatelets by means of grinding stripping.The method comprises the steps that crystallized organic matter is uniformly dispersed in a graphite precursor through solvent dispersion, deformation force produced through repeated crystallization of the crystallized organic matter is utilized for enabling the graphite layer frame distance to be increased, and intercalated graphite is formed; the intercalated graphite is sent to a grinding stripping machine, the stripping and grinding effect of shear force formed in the mutual friction process of media and the graphite material is utilized, the intercalated graphite is stripped, and graphene nanoplatelets are formed; screening separation is conducted on stripped graphite through a vibrating screening machine, unstripped graphite is screened out to be stripped again, and the uniformly distributed graphene nanoplatelets are obtained.The number of layers of the prepared graphene nanoplatelets ranges from 10 to 100, the crystal structure is complete, the high-quality graphene nanoplatelets are produced in an efficient, low-cost and continuous mode under a high shear condition, the preparation process is green and environmentally friendly, and a significant market value is achieved.
Description
Technical field
The invention belongs to technical field of graphene, relate to a kind of method that mechanical stripping prepares Graphene, grind, particularly to a kind of utilization, the method preparing graphene microchip continuously of delaminating.
Background technology
Graphene is a kind of monolayer carbon atomic plane material separated from graphite material, is the two-dimensional material of the cellular hexaplanar structure formed with sp2 hydridization by carbon atom.Since two scientists of Univ Manchester UK in 2004 find Graphene with " adhesive tape " mechanical stripping, scientific circles and the focus of industrial quarters concern are just become.Graphene is at present the thinnest is also the hardest nano material; there is good electricity-optics performance, mechanical property, heat-conductive characteristic and high charge carrier mobility; the performance simultaneously also having numerous common materials such as stronger mechanical strength and pliability not possess, has potential application prospect at numerous areas such as the energy, electronic material, biomedicine and environmental conservation.
But, what expensive, the shortcoming such as productivity is low, poor ductility, preparation process are loaded down with trivial details of grapheme material was very big limits its application in actual industrial.Graphene microchip generally refers to the ultra-thin Graphene stratiform accumulation body that carbon-coating number is more than 10 layers, thickness is in 5-100 nanometer range.Graphene microchip maintains graphite original planar carbon hexatomic ring conjugation crystal structure, there is the shape ratio (diameter/thickness ratio) of super large, and there is nano thickness, therefore there is the mechanical strength of excellence, conduction, heat conductivility and good lubrication, high temperature resistant and anticorrosion properties etc..This makes graphene microchip form composite as additive with other Material cladding, it is possible not only to make the performance boosts such as the intensity of base material, hardness, corrosion-resistant, lubricity, heat conduction, and it can be made to have excellent conduction, antistatic property, thus obtaining the composite of excellent performance.
The preparation method of current graphene microchip includes ball-milling method, ultrasonic method, high-temperature expansion stripping method, oxidation-reduction method etc..Such as the China Patent Publication No. CN103601179A preparation method disclosing the controlled graphene microchip of size, with big particle diameter expansible graphite for raw material, highly expanded multiplying power expanded graphite is prepared under high temperature, with Organic substance for intercalation thing, in blended insertion expanded graphite lamella, prepare expanded graphite/Organic substance composite, adopt pulverizer to be ground into certain size size, high-temp combustion, expands and peels off the graphene microchip obtaining certain size.But adopting high-temperature expansion stripping to prepare Graphene, condition is harsh, the requirement of equipment is high, it is impossible to produce continuously, the large-scale production of restriction graphene microchip.
The preparation method that China Patent Publication No. CN103803533A discloses a kind of Graphene, expanded graphite and organic solvent mixing are carried out ultrasonic dissociating and obtain graphene microchip suspension, stand 0.2-5 hour, remove upper strata suspension, remove precipitate, dry in 80 degree of baking ovens after filtration and obtain graphene microchip.The method adopting ultrasonic stripping prepares graphene microchip; need not move through oxidation-reduction process; do not destroy the lattice structure of prepared Graphene; products obtained therefrom quality is high; but ultrasonic stripping method needs to use substantial amounts of organic solvent, contaminated environment, and the Graphene obtained is difficult to purifies and separates; ultrasonic time is long, is unfavorable for large-scale production.
The preparation method that China Patent Publication No. CN104709900A discloses nano-graphene sheet, graphite material is carried out intercalation oxidation with intercalator and oxidant and forms graphite oxide, graphite oxide is made to peel off as nano-graphite chip architecture by high-temperature heating, it is suspended in liquid, impose the mechanical shear stress more than 5000psi, the lateral dimension of reduction nano-graphite chip architecture and thickness, form nano-graphene sheet suspension, drying and isolate nano-graphene sheet, heat reduction obtains graphene film.Adopting redox method to prepare graphene film, can destroy the structure of Graphene, affect its performance, and need in production process to use substantial amounts of chemical reagent, energy consumption is big and contaminated environment.
In sum, the preparation method of current graphene microchip is limited to each side factors such as production cost and properties of product, still without industrial applications.Therefore in the urgent need to developing the graphene microchip production method of a kind of high efficiency, low cost, high product performance.
Summary of the invention
The present invention is directed to the demand of current burgeoning graphene microchip, it is proposed to a kind of utilization grinds the method preparing graphene microchip continuously of delaminating.The deformation power that the repeated crystallization utilizing crystallization organic produces makes graphite linings frame distance increase, form intercalated graphite, intercalated graphite is sent into and grinds machine for cutting charge into pieces, utilize the stripping mill effect of the shearing force that medium formed with graphite material phase mutual friction, make intercalated graphite peel off and form graphene microchip, by vibrating screen classifier, the graphite peeled off is carried out screening sorting, unstripped graphite is filtered out and re-starts stripping, obtain the graphene microchip being evenly distributed.The graphene microchip number of plies prepared by the inventive method is 10 ~ 100 layers, crystal structure is complete, and product quality is high, it is achieved that continuous prodution high-quality graphene microplate under high shear mechanical condition, can be used for anticorrosive paint, improve the pliability of coating, wearability and rustless property.
For achieving the above object, the present invention adopts the following technical scheme that
A kind of utilization grinds the method that Graphene is prepared in machine for cutting charge into pieces stripping, it is characterized in that increasing the interlamellar spacing of graphite by the organic crystallization that repeats, utilizing the shearing force that grinding delaminates is formed to peel off graphite and obtain the graphene microchip that the number of plies is 10 ~ 100 layers, concrete grammar is as follows:
(1) it is that 2 ~ 3:1 mixing is as material with carbon element in mass ratio using expanded graphite and organic polymer, sending into screw extruder and carry out extruding carbonization, pass into reducibility gas, arranging carburizing temperature is 300 ~ 500 DEG C, make organic polymer carbonization, be mixed to form Graphene presoma with expanded graphite；
(2) it is 1:1 ~ 10 in mass ratio by the Graphene presoma in step (1) and ethanol water, stirs 15 ~ 30min mixing at ambient temperature, add surfactant and continue stirring 10 ~ 20min, make graphite presoma be dispersed in ethanol water；
(3) add and the crystallization organic matter that graphite presoma mass ratio is 0.1 ~ 0.15:1, stirring mixing makes in the layer structure that crystallization organic matter is dispersed in graphite presoma, it is heated to 40 ~ 80 DEG C, solvent evaporative crystallization is organic to be precipitated out with crystal form, continuously adds ethanol water, makes crystallization organic matter again dissolve, reheat and precipitate out, so repeating 2 ~ 3 times, graphite layers is gradually increased along with organic solid-liquid transformation, obtains intercalated graphite；
(4) intercalated graphite that step (3) obtained adds grinds in machine for cutting charge into pieces, and arranging mixing speed is 500 ~ 1000rpm, utilizes the stripping mill effect of the shearing force that medium formed with graphite material phase mutual friction, makes intercalated graphite stripping formation graphene microchip；By vibrating screen classifier, the graphite peeled off is carried out screening sorting, unstripped graphite is filtered out and re-starts stripping, obtain the graphene microchip head product being evenly distributed；
(5) collect the graphene microchip head product collected in step (4) to clean 2 ~ 3 times with water, ethanol, acetone respectively, carry out dissolution, cleaning, filtration, dry obtain the graphene microchip that the number of plies is 10 ~ 100 layers.
Described organic polymer is any one in polyvinyl alcohol, Polyethylene Glycol, polylactic acid, polyacrylic acid.
Described crystallization organic matter is any one in arginine, theanine, glutamine.
Described surfactant is any one in tetramethyl ammonium hydrogen carbonate, dodecyl tetramethyl guanidine carbonate, cetyl trimethylammonium bromide, cetyl benzenesulfonic acid sodium.
The described ethanol water described in step (2) is the solution that ethanol is prepared for 1:1 ~ 2 by volume with water.
The described agitator grinding machine for cutting charge into pieces is multi-layer discs, disk is carved with at least 4 equally distributed circulation ports, disk border is uniformly distributed 4 lead angles, when agitator drives graphite material to rotate, because of differential relation, medium forms the stripping mill effect based on shearing force with graphite material phase mutual friction, it is achieved effectively dissociating of lamellar graphite, makes graphite peel off and forms the graphene microchip being evenly distributed；Connect vibrating screen classifier immediately below described grinding machine for cutting charge into pieces, the graphite not being completely exfoliated is sorted, classification, repeatedly delaminate to not up to the graphene film required.
A kind of utilization of the present invention grinds the method preparing graphene microchip continuously of delaminating, graphite is formed Graphene presoma with organic polymer by screw rod shearing carbonization, by solvent dispersion, crystallization organic matter is dispersed in Graphene presoma, made the organic matter being interspersed in graphite layers precipitate out with crystal form by heating crystalline, repeatedly dissolve heating crystalline, by the force attenuation graphite layers power that organic repeated deformation produces, make graphite layers distance increase, be beneficial to the stripping of graphite.Form intercalated graphite, intercalated graphite is sent into and grinds machine for cutting charge into pieces, utilize the stripping mill effect of the shearing force that medium formed with graphite material phase mutual friction, make intercalated graphite peel off and form graphene microchip, by vibrating screen classifier, the graphite peeled off is carried out screening to sort, unstripped graphite is filtered out and re-starts stripping, obtain the graphene microchip being evenly distributed.The present invention utilizes the graphene microchip grinding preparation continuously of delaminating, and the number of plies is evenly distributed, and yield is high, cost is low, it is suitable for anticorrosive paint, makes the pliability of coating, wearability, corrosion-resistant, rustless property etc. promote, promote graphene microchip large-scale application in anticorrosive paint.Main performance advantage such as table 1 of graphene microchip prepared by the present invention.
| Index name | Radial dimension | Thickness | Yield | Cost |
| Index performance | 5~10μm | 10 ~ 100 layers | 150~250kg/h | 0.2 ~ 0.6 yuan/g |
The present invention is a kind of utilizes the method grinding preparation preparation graphene microchip of delaminating continuously, and compared with prior art prominent feature and beneficial effect are in that:
1, increase graphite layers from, it is thus achieved that intercalated graphite by the repeated crystallization that crystallization is organic, utilize the efficient stripping of graphite.
2, carry out intercalated graphite shearing and peel off by grinding the shear action produced of delaminating, it is to avoid the damage of graphene layer structure；Utilize vibrosieve that unstripped graphite is carried out screening and separating, again peel off, improve the charge stripping efficiency of graphite.
3, invention preparation method put into little, cost is low, non-environmental-pollution, can prepare graphene microchip fast and efficiently, is advantageously implemented the continuous large-scale production of high-quality graphene microplate.
Detailed description of the invention
Below in conjunction with detailed description of the invention, the present invention is explained in detail, is not restricted to the present invention.When without departing from said method thought of the present invention, the various replacements made according to ordinary skill knowledge and customary means or improvement, should be included within protection scope of the present invention.
Embodiment 1
(1) expanded graphite and polyvinyl alcohol are mixed as material with carbon element for 3:1 in mass ratio, sending into screw extruder and carry out extruding carbonization, pass into reducibility gas, arranging carburizing temperature is 500 DEG C, make polyvinyl alcohol carbonization, be mixed to form Graphene presoma with expanded graphite；
(2) it is 1:10 in mass ratio by the Graphene presoma in step (1) and ethanol water, stirs 15 ~ 30min mixing at ambient temperature, add tetramethyl ammonium hydrogen carbonate and continue stirring 10 ~ 20min, make graphite presoma be dispersed in ethanol water；
(3) adding with graphite presoma mass ratio is the arginine of 0.1:1, stirring mixing makes in the layer structure that crystallization organic matter is dispersed in graphite presoma, it is heated to 40 ~ 80 DEG C, solvent evaporative crystallization is organic to be precipitated out with crystal form, continuously adds ethanol water, makes crystallization organic matter again dissolve, reheat and precipitate out, so repeating 2 ~ 3 times, graphite layers is gradually increased along with organic solid-liquid transformation, obtains intercalated graphite；
(4) intercalated graphite that step (3) obtained adds grinds in machine for cutting charge into pieces, and arranging mixing speed is 500 ~ 1000rpm, utilizes the stripping mill effect of the shearing force that medium formed with graphite material phase mutual friction, makes intercalated graphite stripping formation graphene microchip；By vibrating screen classifier, the graphite peeled off is carried out screening sorting, unstripped graphite is filtered out and re-starts stripping, obtain the graphene microchip head product being evenly distributed；
(5) collect the graphene microchip head product collected in step (4) to clean 2 ~ 3 times with water, ethanol, acetone respectively, carry out dissolution, cleaning, filtration, dry obtain the graphene microchip that the number of plies is 10 ~ 100 layers.
Embodiment 2
(1) expanded graphite and Polyethylene Glycol are mixed as material with carbon element for 2:1 in mass ratio, sending into screw extruder and carry out extruding carbonization, pass into reducibility gas, arranging carburizing temperature is 300 DEG C, make organic polymer carbonization, be mixed to form Graphene presoma with expanded graphite；
(2) it is 1:8 in mass ratio by the Graphene presoma in step (1) and ethanol water, stir 15 ~ 30min mixing at ambient temperature, add dodecyl tetramethyl guanidine carbonate and continue stirring 10 ~ 20min, make graphite presoma be dispersed in ethanol water；
(3) adding with graphite presoma mass ratio is the theanine of 0.15:1, stirring mixing makes in the layer structure that crystallization organic matter is dispersed in graphite presoma, it is heated to 40 ~ 80 DEG C, solvent evaporative crystallization is organic to be precipitated out with crystal form, continuously adds ethanol water, makes crystallization organic matter again dissolve, reheat and precipitate out, so repeating 2 ~ 3 times, graphite layers is gradually increased along with organic solid-liquid transformation, obtains intercalated graphite；
(4) intercalated graphite that step (3) obtained adds grinds in machine for cutting charge into pieces, and arranging mixing speed is 500 ~ 1000rpm, utilizes the stripping mill effect of the shearing force that medium formed with graphite material phase mutual friction, makes intercalated graphite stripping formation graphene microchip；By vibrating screen classifier, the graphite peeled off is carried out screening sorting, unstripped graphite is filtered out and re-starts stripping, obtain the graphene microchip head product being evenly distributed；
(5) collect the graphene microchip head product collected in step (4) to clean 2 ~ 3 times with water, ethanol, acetone respectively, carry out dissolution, cleaning, filtration, dry obtain the graphene microchip that the number of plies is 10 ~ 100 layers.
Embodiment 3
(1) expanded graphite and polylactic acid are mixed as material with carbon element for 2:1 in mass ratio, sending into screw extruder and carry out extruding carbonization, pass into reducibility gas, arranging carburizing temperature is 500 DEG C, make organic polymer carbonization, be mixed to form Graphene presoma with expanded graphite；
(2) it is 1:5 in mass ratio by the Graphene presoma in step (1) and ethanol water, stir 15 ~ 30min mixing at ambient temperature, add cetyl trimethylammonium bromide and continue stirring 10 ~ 20min, make graphite presoma be dispersed in ethanol water；
(3) adding with graphite presoma mass ratio is the glutamine of 0.12:1, stirring mixing makes in the layer structure that crystallization organic matter is dispersed in graphite presoma, it is heated to 40 ~ 80 DEG C, solvent evaporative crystallization is organic to be precipitated out with crystal form, continuously adds ethanol water, makes crystallization organic matter again dissolve, reheat and precipitate out, so repeating 2 ~ 3 times, graphite layers is gradually increased along with organic solid-liquid transformation, obtains intercalated graphite；
(4) intercalated graphite that step (3) obtained adds grinds in machine for cutting charge into pieces, and arranging mixing speed is 500 ~ 1000rpm, utilizes the stripping mill effect of the shearing force that medium formed with graphite material phase mutual friction, makes intercalated graphite stripping formation graphene microchip；By vibrating screen classifier, the graphite peeled off is carried out screening sorting, unstripped graphite is filtered out and re-starts stripping, obtain the graphene microchip head product being evenly distributed；
(5) collect the graphene microchip head product collected in step (4) to clean 2 ~ 3 times with water, ethanol, acetone respectively, carry out dissolution, cleaning, filtration, dry obtain the graphene microchip that the number of plies is 10 ~ 100 layers.
Embodiment 4
(1) expanded graphite and polyacrylic acid are mixed as material with carbon element for 3:1 in mass ratio, sending into screw extruder and carry out extruding carbonization, pass into reducibility gas, arranging carburizing temperature is 400 DEG C, make organic polymer carbonization, be mixed to form Graphene presoma with expanded graphite；
(2) it is 1:5 in mass ratio by the Graphene presoma in step (1) and ethanol water, stirs 15 ~ 30min mixing at ambient temperature, add cetyl benzenesulfonic acid sodium and continue stirring 10 ~ 20min, make graphite presoma be dispersed in ethanol water；
(3) adding with graphite presoma mass ratio is the glutamine of 0.1:1, stirring mixing makes in the layer structure that crystallization organic matter is dispersed in graphite presoma, it is heated to 40 ~ 80 DEG C, solvent evaporative crystallization is organic to be precipitated out with crystal form, continuously adds ethanol water, makes crystallization organic matter again dissolve, reheat and precipitate out, so repeating 2 ~ 3 times, graphite layers is gradually increased along with organic solid-liquid transformation, obtains intercalated graphite；
(4) intercalated graphite that step (3) obtained adds grinds in machine for cutting charge into pieces, and arranging mixing speed is 500 ~ 1000rpm, utilizes the stripping mill effect of the shearing force that medium formed with graphite material phase mutual friction, makes intercalated graphite stripping formation graphene microchip；By vibrating screen classifier, the graphite peeled off is carried out screening sorting, unstripped graphite is filtered out and re-starts stripping, obtain the graphene microchip head product being evenly distributed；
(5) collect the graphene microchip head product collected in step (4) to clean 2 ~ 3 times with water, ethanol, acetone respectively, carry out dissolution, cleaning, filtration, dry obtain the graphene microchip that the number of plies is 10 ~ 100 layers.
Claims (7)
1. one kind utilizes the method grinding preparation graphene microchip of delaminating continuously, it is characterized in that increasing the interlamellar spacing of graphite by the organic crystallization that repeats, utilizing the shearing force that grinding delaminates is formed to peel off graphite and obtain the graphene microchip that the number of plies is 10 ~ 100 layers, concrete grammar is as follows:
(1) it is that 2 ~ 3:1 mixing is as material with carbon element in mass ratio using expanded graphite and organic polymer, sending into screw extruder and carry out extruding carbonization, pass into reducibility gas, arranging carburizing temperature is 300 ~ 500 DEG C, make organic polymer carbonization, be mixed to form Graphene presoma with expanded graphite；
(2) it is 1:1 ~ 10 in mass ratio by the Graphene presoma in step (1) and ethanol water, stirs 15 ~ 30min mixing at ambient temperature, add surfactant and continue stirring 10 ~ 20min, make graphite presoma be dispersed in ethanol water；
(3) add and the crystallization organic matter that graphite presoma mass ratio is 0.1 ~ 0.15:1, stirring mixing makes in the layer structure that crystallization organic matter is dispersed in graphite presoma, it is heated to 40 ~ 80 DEG C, solvent evaporative crystallization is organic to be precipitated out with crystal form, continuously adds ethanol water, makes crystallization organic matter again dissolve, reheat and precipitate out, so repeating 2 ~ 3 times, graphite layers is gradually increased along with organic solid-liquid transformation, obtains intercalated graphite；
(4) intercalated graphite that step (3) obtained adds grinds in machine for cutting charge into pieces, and arranging mixing speed is 500 ~ 1000rpm, utilizes the stripping mill effect of the shearing force that medium formed with graphite material phase mutual friction, makes intercalated graphite stripping formation graphene microchip；By vibrating screen classifier, the graphite peeled off is carried out screening sorting, unstripped graphite is filtered out and re-starts stripping, obtain the graphene microchip head product being evenly distributed；
(5) collect the graphene microchip head product collected in step (4) to clean 2 ~ 3 times with water, ethanol, acetone respectively, carry out dissolution, cleaning, filtration, dry obtain the graphene microchip that the number of plies is 10 ~ 100 layers；
The described agitator grinding machine for cutting charge into pieces is multi-layer discs, disk is carved with equally distributed circulation port, disk border is uniformly distributed 4 lead angles, when agitator drives graphite material to rotate, because of differential relation, medium forms the stripping mill effect based on shearing force with graphite material phase mutual friction, it is achieved effectively dissociating of lamellar graphite, makes graphite peel off and forms the graphene microchip being evenly distributed；
Connect vibrating screen classifier immediately below described grinding machine for cutting charge into pieces, the graphite not being completely exfoliated is sorted, classification, repeatedly delaminate to not up to the graphene film required.
2. a kind of utilization according to claim 1 grinds the method preparing graphene microchip continuously of delaminating, it is characterised in that described organic polymer is any one in polyvinyl alcohol, Polyethylene Glycol, polylactic acid, polyacrylic acid.
3. a kind of utilization according to claim 1 grinds the method preparing graphene microchip continuously of delaminating, it is characterised in that the ethanol water described in step (2) is ethanol is the solution of 1:1 ~ 2 preparation by volume with water.
4. a kind of utilization according to claim 1 grinds the method preparing graphene microchip continuously of delaminating, it is characterised in that described surfactant is any one in tetramethyl ammonium hydrogen carbonate, dodecyl tetramethyl guanidine carbonate, cetyl trimethylammonium bromide, cetyl benzenesulfonic acid sodium.
5. a kind of utilization according to claim 1 grinds the method preparing graphene microchip continuously of delaminating, it is characterised in that described crystallization organic matter is any one in arginine, theanine, glutamine.
6. a kind of utilization according to claim 1 grinds the method preparing graphene microchip continuously of delaminating, it is characterised in that be carved with at least 4 equally distributed circulation ports on the described disk grinding machine for cutting charge into pieces.
7. a kind of utilization according to claim 1 grinds the method preparing graphene microchip continuously of delaminating, it is characterised in that described graphene microchip is used for anticorrosive paint.
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| CN106566302A (en) * | 2016-10-20 | 2017-04-19 | 成都新柯力化工科技有限公司 | Graphene composite dispersion liquid for anticorrosion coating and preparation method thereof |
| CN106744876A (en) * | 2016-12-21 | 2017-05-31 | 成都新柯力化工科技有限公司 | A kind of method that utilization multi-level cone type kneading machine prepares grapheme material |
| CN106908463A (en) * | 2017-03-09 | 2017-06-30 | 成都新柯力化工科技有限公司 | A kind of method of utilization surface sweeping Electronic Speculum detection graphene microchip layer distribution |
| CN107892294A (en) * | 2017-12-31 | 2018-04-10 | 周思齐 | The method and apparatus that high purity graphite rod produces graphene |
| CN113675391A (en) * | 2021-08-05 | 2021-11-19 | 常熟理工学院 | Heterogeneous layered composite material for lithium ion battery cathode and preparation method thereof |
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| CN115231559A (en) * | 2022-08-24 | 2022-10-25 | 常熟世名化工科技有限公司 | Graphene, preparation method thereof and graphene water-based dispersion |
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| CN106566302A (en) * | 2016-10-20 | 2017-04-19 | 成都新柯力化工科技有限公司 | Graphene composite dispersion liquid for anticorrosion coating and preparation method thereof |
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| CN106744876A (en) * | 2016-12-21 | 2017-05-31 | 成都新柯力化工科技有限公司 | A kind of method that utilization multi-level cone type kneading machine prepares grapheme material |
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| CN107892294A (en) * | 2017-12-31 | 2018-04-10 | 周思齐 | The method and apparatus that high purity graphite rod produces graphene |
| CN113675391A (en) * | 2021-08-05 | 2021-11-19 | 常熟理工学院 | Heterogeneous layered composite material for lithium ion battery cathode and preparation method thereof |
| 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 |
| CN115231559A (en) * | 2022-08-24 | 2022-10-25 | 常熟世名化工科技有限公司 | Graphene, preparation method thereof and graphene water-based dispersion |
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