CN105585005A - A production device and a method for preparing graphene by adopting a mechanical stripping manner - Google Patents
A production device and a method for preparing graphene by adopting a mechanical stripping manner Download PDFInfo
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- CN105585005A CN105585005A CN201410570669.4A CN201410570669A CN105585005A CN 105585005 A CN105585005 A CN 105585005A CN 201410570669 A CN201410570669 A CN 201410570669A CN 105585005 A CN105585005 A CN 105585005A
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Abstract
The invention relates to a production device and a method for preparing graphene by adopting a mechanical stripping manner. The device and the method are characterized in that the method includes 1) a step of adding a graphite raw material purity of which is 98% or above and a particle size of which is 2 mum to 1 cm into a high-pressure water smashing device, starting a high pressure pump, regulating pressure, filtering a graphite scale mixed solution in a collecting tank and drying, 2) a step of adding the graphite scales after being filtered and dried, a dispersant and a solvent into a graphite expanding and heating device, and performing ultrasonic vibration to obtain uniformly dispersed suspension, 3) a step of feeding the heated suspension into a highly shearing device, and shearing, 4) a step of conveying graphene suspension to a centrifuge to obtain a filter cake, and 5) a step of washing the filter cake prepared in the step 4) with a proper amount of distilled water for three times, transferring the filter cake to a freeze dryer, and performing freeze drying for 3 h to obtain a graphene product.
Description
Technical field
The present invention relates to a kind of process units and preparation method of two-dimensional nano new material, be specifically related to a kind of process units and the preparation method of mechanical stripping legal system for Graphene that adopt.
Background technology
Graphene is mono-layer graphite in essence, also can think that Graphene is the CNT after launching. Graphene film (graphenesheets) provides many outstanding performances, and people are studying its purposes in nanoelectronics, nano-complex, battery, ultracapacitor, hydrogen storage and biologic applications. Use the major limitation of graphene film to be cannot produce in a large number it at present. Be similar to CNT and many other nano materials, synthetic and process in the process of a large amount of graphene films, crucial challenge is aggtegation. Unless separate completely each other, otherwise owing to existing Van der Waals to interact, the graphene film with high-specific surface area trended towards forming irreversible caking (agglomerates), even again piles up and forms graphite. Before this all for the work by the original large-scale production Graphene of chemical conversion or thermal expansion/also in, run into this problem. Prevent that aggtegation is for graphene film particular importance, this is because their most special performances are only relevant with independent sheet. By other molecules or polymer are attached on described graphene film, can reduce aggtegation. But, for majority application, do not wish to exist external stabilizing agent. Need new strategy to produce in a large number relatively pure graphene film, and make it keep each self-separation.
Comparatively cheap by the stacking graphite forming of flat graphene film, it can be obtained in a large number by natural origin and synthetic source. For generating graphene film, this common material with carbon element is the most easily to utilize and the most cheap source. Originally the machine cuts of graphite has caused the discovery of graphene film, and the current experimental research for most Graphenes. But the current production capacity of this method is low causes it to be not suitable for extensive use, is only applied in experiment.
A large amount of productions of high-quality graphene are the prerequisites that realizes Graphene extensive use, are also focuses of Graphene research always. Conventional graphene preparation method has four kinds at present: micromechanics stripping method, epitaxial growth method, chemical vapour deposition technique and graphite oxide reducing process. Micromechanics stripping method productive rate is too low, is only applicable to laboratory small-scale test; Epitaxial growth method is all had relatively high expectations for production equipment, condition, is not suitable for present stage production requirement; Chemical vapour deposition technique is difficult to obtain uniform single-layer graphene, and complex process; The reduced graphene that graphite oxide reducing process obtains often has too many defect, is fatal impact for the electrical properties of Graphene.
Summary of the invention
The object of the invention is to overcome above-mentioned deficiency, a kind of process units and the method for mechanical stripping legal system for Graphene that adopt is provided, can not destroy on the basis of graphite flake layer natural structure, obtain large area, do not have defective Graphene, the Graphene product making, by the adjusting of technological parameter, has ensured its good mode of appearance, and whole production process adopts physical method, environmental protection, technique is simple.
The object of the present invention is achieved like this: a kind of process units and the method for mechanical stripping legal system for Graphene that adopt, said method comprising the steps of:
Step 1, by purity more than 98%, particle diameter is that 1 μ m ~ 2cm graphite scale raw material is put in High-Pressure Water breaker, start high-pressure pump, regulate pressure 1.5atm, the High-Pressure Water spraying by giant clashes into graphite scale, then graphite scale mixed liquor is expelled in collecting tank, by the graphite scale mixed liquor filtering drying in collecting tank;
After step 2, filtering drying, graphite scale, dispersant and solvent are joined in graphite expansion heater, obtain homodisperse suspension by ultrasonic vibration, it is 80 ~ 150 DEG C that suspension is heated to temperature, duration 2 ~ 5h, wherein the mass concentration of graphite scale is 1% ~ 25%;
Step 3, heating suspension is later entered in high-shear device, add sodium acid carbonate and hydrochloric acid simultaneously, increasing clipper rotating speed is 2000-7500rpm/min, keeping reactor temperature is 80 DEG C ~ 150 DEG C, after 5 ~ 10h, stop reaction, by discharging opening, upper strata suspension is expelled in storage tank, leaves standstill 2 ~ 24h;
Step 4, the graphene suspension in storage tank is delivered in centrifuge, centrifuge speed is 1000-6000rpm/min, and 10min ~ 2h, gets supernatant liquor, and vacuum filtration obtains filter cake;
Step 5, the filter cake that step 4 is obtained wash 3 times with appropriate distilled water, and filter cake is transferred in freeze drier, and freeze drying 3h obtains Graphene product;
Described High-Pressure Water breaker comprises charging tank, giant, high-pressure pump and feeder, the bottom of described charging tank is connected with feeder, fix by support at described feeder, described giant is arranged in the connectivity part of charging tank and feeder, muzzle is positioned at charging tank inside, angle is 15 °, hydraulic pressure is 20kpa, described giant is connected with high-pressure pump, on the charging tank internal face of the muzzle opposite face of described giant, be provided with clipper, be provided with recoil water pipe in the bottom of described charging tank, described recoil water pipe is connected with water tank by recoil water pump, bottom at described charging tank is provided with agitator,
Described graphite expansion heater comprises heating furnace, above described heating furnace, be provided with charging aperture and thermometer, below is provided with discharging opening, below described heating furnace, arranged outside has chuck, on described chuck, be provided with heating agent import and heating agent outlet, heating agent adopts deep fat or steam, inside at described heating furnace is provided with paddle, described paddle is connected with the stirring motor at heating furnace top, in the internal side wall of described heating furnace, be evenly distributed with multiple Vltrasonic devices, act on graphite mixed liquor by Vltrasonic device and obtain homodisperse suspension;
Described high-shear device comprises reactor and motor, described motor is installed on the bottom of reactor, on the output of described motor, be connected with clipper, top at described reactor is provided with charging aperture, Pressure gauge and thermometer, on the internal face of described reactor, be provided with shearing groove, shear groove and be spiral escalation layout, middle and lower part at described reactor is provided with discharging opening, periphery at described reactor is provided with chuck, on described chuck, be provided with heating agent import and outlet, the discharging opening of described reactor is connected with the charging aperture of storage tank, the discharging opening of described storage tank is connected with the charging aperture of centrifuge, the discharging opening of described centrifuge is connected with the charging aperture of freeze drier, periphery at described clipper is nested with agitation blade, described agitation blade comprises holder and reach blade, described holder is nested and be fixed on the periphery of clipper, one end of described reach blade is connected with holder, incline direction is contrary with the direction of rotation of clipper, the other end of described reach blade is connected with end blade, described end blade and reach blade are vertical setting.
Described solvent comprises water, acetonitrile, n-butanol, ethanol, acetone, N, dinethylformamide, one or more mixtures in 1-METHYLPYRROLIDONE, dispersant comprises softex kw, lauryl sodium sulfate, neopelex, sodium taurocholate, polyvinyl alcohol, one or more in polyvinylpyrrolidone composite.
Described shearing groove is by tetrahedron or profile of tooth or both are in conjunction with forming.
The drift angle angle of the tetrahedron of described shearing groove or profile of tooth is 10 ° ~ 160 °, and length is 1cm-1000cm, and thickness is 0.5cm ~ 3cm.
Compared with prior art, the present invention has following beneficial effect:
1, the present invention holds on to Graphene and peels off in preparation process, most important shear action, logical excessive speeds, shear the modes such as arranging of groove, give full play to shearing between material and material under high rotating speed with " collision " of groove, having realized the success of Graphene peels off, in addition, because the method that adopts physics to peel off is produced Graphene, prime cost is graphite, labour cost, charges for water and electricity and administration fee, graphite raw material is cheap, and by further optimum management, production cost has high advantage.
2, the Graphene quality that the present invention adopts mechanical stripping method to make is good, and graphite, by the mutual shear action of self, can be removed surperficial micro powder granule. Through follow-up centrifugation, the dry Graphene distribution homogeneous making, edge is rounded.
3, the present invention does not use strong acid and strong base or other noxious materials, and production process environmental protection is pollution-free. The successful preparation of New Two Dimensional material Graphene can produce huge economic and social benefit, and environment is not existed to any destruction.
4, the Graphene that the present invention produces provides important raw material for composite, photoelectric field field, due to surface smoothing, and yardstick homogeneous, neat in edge, is applied in " the four large characteristics " of the performance Graphene that the field such as Material cladding can be maximum. Preserved preferably the lamellar structure of Graphene, in use procedure, interfacial interaction is strong, can bring into play maximum material mechanical performance.
Brief description of the drawings
Fig. 1 is the structural representation of mesohigh current breaker of the present invention.
Fig. 2 is the structural representation of graphite expansion heater in the present invention.
Fig. 3 is the structural representation of high-shear device in the present invention.
Fig. 4 is the structural representation of clipper in high-shear device of the present invention.
Wherein:
Charging tank 1
Giant 2
High-pressure pump 3
Feeder 4
Support 5
Clipper 6
Recoil water pipe 7
Recoil water pump 8
Water tank 9
Agitator 10
Heating furnace 101
Charging aperture 102
Thermometer 103
Discharging opening 104
Chuck 105
Hot coal import 106
Heating agent outlet 107
Paddle 108
Stirring motor 109
Vltrasonic device 110
Reactor 201
Motor 202
Clipper 203
Agitation blade 2031
Holder 2032
Reach blade 2033
End blade 2034
Charging aperture 204
Pressure gauge 205
Thermometer 206
Shear groove 207
Discharging opening 208
Storage tank 209
Centrifuge 2010
Freeze drier 2011.
Detailed description of the invention
Referring to Fig. 1-Fig. 4, the present invention relates to a kind of process units and the method for mechanical stripping legal system for Graphene that adopt:
Embodiment mono-,
Step 1, referring to Fig. 1, by purity more than 98%, particle diameter is that the graphite scale raw material of 100 μ m is put in High-Pressure Water breaker, start high-pressure pump, regulate pressure 20kpa, the High-Pressure Water spraying by giant clashes into graphite scale, destroy the Van der Waals force of its interlayer, graphite scale is peeled off, then graphite scale mixed liquor is expelled in collecting tank, by the graphite scale mixed liquor filtering drying in collecting tank;
Step 2, referring to Fig. 2, after drying after filtration, 50kg graphite scale and 1kg sodium taurocholate dispersant are joined in graphite expansion heater, adding 350kg distilled water, the ultrasonic vibration 2h that is 50w by frequency, obtain homodisperse suspension, then in chuck, pass into deep fat or steam, making to be heated to temperature is 80 DEG C, duration is 5h, opens stirring motor in heating process, makes suspension obtain homogeneous heating by paddle, because temperature rising graphite scale Van der Waals force between layers reduces, be convenient to shearing below;
Step 3, referring to Fig. 3, heating suspension is later entered in high-shear device, add saleratus 2kg and hydrochloric acid 3.5kg simultaneously, sodium carbonate and hydrochloric acid enter into the interlayer reaction of graphite scale, the carbon dioxide producing backs down the layer of graphite scale and layer, increasing clipper rotating speed is 5000rpm/min, due to higher rotating speed, shearing between material self and the interaction of shearing groove with inwall, graphite is successively peeled off, keep steady temperature, rotating speed, after 5h, stop reaction, by discharging opening, upper strata suspension is expelled in storage tank, leave standstill 24h,
Step 4, the graphene suspension in storage tank is delivered in centrifuge, centrifuge speed is 1000-6000rpm/min, centrifugal action 10min, and by centrifugal, the graphite not being stripped from multi-layer graphene has been deposited in bottom, gets supernatant liquor, vacuum filtration;
Step 5, filter cake that step 4 is obtained are with appropriate absolute ethanol washing 3 times, and filter cake is transferred in freeze drier, and freeze drying 3h obtains Graphene product.
Embodiment bis-,
Step 1, by purity more than 98%, particle diameter is that the graphite scale raw material of 150 μ m is put in High-Pressure Water breaker, start high-pressure pump, regulate pressure 20kpa, the High-Pressure Water spraying by giant clashes into graphite scale, destroys the Van der Waals force of its interlayer, and graphite scale is peeled off, then graphite scale mixed liquor is expelled in collecting tank, by the graphite scale mixed liquor filtering drying in collecting tank;
Step 2, after filtration dry after, 20kg graphite scale and 1kg polyvinyl alcohol dispersant are joined in graphite expansion heater, add again in 400kgN-methyl pyrrolidone, the ultrasonic vibration 3h that is 50w by frequency, obtain homodisperse suspension, then in chuck, pass into deep fat or steam, making to be heated to temperature is 100 DEG C, duration is 2h, in heating process, open stirring motor, make suspension obtain homogeneous heating by paddle, because temperature rising graphite scale Van der Waals force between layers reduces, be convenient to shearing below;
Step 3, heating suspension is later entered in high-shear device, add saleratus 2kg and hydrochloric acid 3.5kg simultaneously, sodium carbonate and hydrochloric acid enter into the interlayer reaction of graphite scale, the carbon dioxide producing backs down the layer of graphite scale and layer, increasing clipper rotating speed is 3500rpm/min, due to higher rotating speed, the shearing between material self and the interaction of shearing groove with inwall, successively peeled off graphite. Keep steady temperature, rotating speed, after 8h, stop reaction, by discharging opening, upper strata suspension is expelled in storage tank, leave standstill 15h;
Step 4, the graphene suspension in storage tank is delivered in centrifuge, centrifuge speed is 2000-5000rpm/min, centrifugal action 1h, and by centrifugal, the graphite not being stripped from multi-layer graphene has been deposited in bottom, gets supernatant liquor, vacuum filtration;
Step 5, filter cake that step 4 is obtained are with appropriate absolute ethanol washing 3 times, and filter cake is transferred in freeze drier, and freeze drying 3h obtains Graphene product.
Embodiment tri-,
Step 1, by purity more than 98%, particle diameter is that the graphite scale raw material of 250 μ m is put in High-Pressure Water breaker, start high-pressure pump, regulate pressure 1.5atm, the High-Pressure Water spraying by giant clashes into graphite scale, destroys the Van der Waals force of its interlayer, and graphite scale is peeled off, then graphite scale mixed liquor is expelled in collecting tank, by the graphite scale mixed liquor filtering drying in collecting tank;
Step 2, through filter dry after, 30kg graphite scale and 1kg lauryl sodium sulfate dispersant are joined in graphite expansion heater, add again in 500kgN-methyl pyrrolidone, the ultrasonic vibration 3h that is 60w by frequency, obtain homodisperse suspension, then in chuck, pass into deep fat or steam, making to be heated to temperature is 120 DEG C, duration is 3h, in heating process, open stirring motor, make suspension obtain homogeneous heating by paddle, because temperature rising graphite scale Van der Waals force between layers reduces, be convenient to shearing below;
Step 3, heating suspension is later entered in high-shear device, add saleratus 2kg and hydrochloric acid 3.5kg simultaneously, sodium acid carbonate and hydrochloric acid enter into the interlayer reaction of graphite scale, the carbon dioxide producing backs down the layer of graphite scale and layer, increasing clipper rotating speed is 7500rpm/min, due to higher rotating speed, the shearing between material self and the interaction of shearing groove with inwall, successively peeled off graphite. Keep steady temperature, rotating speed, after 7h, stop reaction, by discharging opening, upper strata suspension is expelled in storage tank, leave standstill 12h;
Step 4, the graphene suspension in storage tank is delivered in centrifuge, centrifuge speed is 1000-6000rpm/min, centrifugal action 2h, by centrifugal, the graphite not being stripped from multi-layer graphene is deposited in bottom, gets supernatant liquor, vacuum filtration, the filter cake obtaining;
Step 5, filter cake that step 4 is obtained are with appropriate absolute ethanol washing 3 times, and filter cake is transferred in freeze drier, and freeze drying 3h obtains Graphene product.
Claims (5)
1. adopt process units and the method for mechanical stripping legal system for Graphene, it is characterized in that said method comprising the steps of:
Step 1, by purity more than 98%, particle diameter is that the graphite raw material of 2 μ m ~ 1cm is put in High-Pressure Water breaker, start high-pressure pump, the High-Pressure Water spraying by giant clashes into graphite scale, then graphite scale mixed liquor is expelled in collecting tank, by the graphite scale mixed liquor filtering drying in collecting tank;
After step 2, filtering drying, graphite scale, dispersant and solvent are joined in graphite expansion heater, obtain homodisperse suspension by ultrasonic vibration, it is 80 ~ 150 DEG C that suspension is heated to temperature, duration 2 ~ 5h, wherein the mass concentration of graphite scale is 1% ~ 25%;
Step 3, heating suspension is later entered in high-shear device, add saleratus and hydrochloric acid simultaneously, increasing clipper rotating speed is 7500rpm/min, keeping reactor temperature is 80 DEG C ~ 150 DEG C, after 5 ~ 10h, stop reaction, by discharging opening, upper strata suspension is expelled in storage tank, leaves standstill 12 ~ 24h;
Step 4, the graphene suspension in storage tank is delivered in centrifuge, centrifuge speed is 1000-6000rpm/min, and 10min ~ 2h, gets supernatant liquor, and vacuum filtration obtains filter cake;
Step 5, the filter cake that step 4 is obtained wash 3 times with appropriate distilled water, and filter cake is transferred in freeze drier, and freeze drying 3h obtains Graphene product;
Described device comprises charging tank (1), giant (2), high-pressure pump (3) and feeder (4), the bottom of described charging tank (1) is connected with feeder (4), fixing by support (5) at described feeder (4), described giant (2) is arranged in the connectivity part of charging tank (1) and feeder (4), muzzle is positioned at charging tank (1) inside, described giant (2) is connected with high-pressure pump (3), on charging tank (1) internal face of the muzzle opposite face of described giant (2), be provided with clipper (6), be provided with recoil water pipe (7) in the bottom of described charging tank (1), described recoil water pipe (7) is connected with water tank (9) by recoil water pump (8), be provided with agitator (10) in the bottom of described charging tank (1),
Described graphite expansion heater comprises heating furnace (101), be provided with charging aperture (102) and thermometer (103) in described heating furnace (101) top, below is provided with discharging opening (104), there is chuck (105) in the below arranged outside of described heating furnace (101), on described chuck (105), be provided with heating agent import (106) and heating agent outlet (107), be provided with paddle (108) in the inside of described heating furnace (101), described paddle (108) is connected with the stirring motor (109) at heating furnace (101) top, in the internal side wall of described heating furnace (101), be evenly distributed with multiple Vltrasonic devices (110),
Described high-shear device comprises reactor (201) and motor (202), described motor (202) is installed on the bottom of reactor (201), on the output of described motor (202), be connected with clipper (203), be provided with charging aperture (204) at the top of described reactor (201), Pressure gauge (205) and thermometer (206), on the internal face of described reactor (201), be provided with and shear groove (207), described shearing groove (207) is spiral escalation and arranges, be provided with discharging opening (208) in the middle and lower part of described reactor (201), the discharging opening of described reactor (201) is connected with the charging aperture of storage tank (209), the discharging opening of described storage tank (209) is connected with the charging aperture of centrifuge (210), the discharging opening of described centrifuge (210) is connected with the charging aperture of freeze drier (211).
2. a kind of process units and the method for mechanical stripping legal system for Graphene that adopt according to claim 1, it is characterized in that solvent comprises water, benzinum, N, one or more mixtures of dinethylformamide, 1-METHYLPYRROLIDONE, acetone, ether, ethyl acetate, toluene, dispersant comprises softex kw, lauryl sodium sulfate, neopelex, sodium taurocholate, polyvinyl alcohol, one or more in polyvinylpyrrolidone composite.
3. a kind of process units and the method for mechanical stripping legal system for Graphene that adopt according to claim 1, it is characterized in that being nested with agitation blade (2031) in the periphery of described clipper (203), described agitation blade (2031) comprises holder (2032) and reach blade (2033), described holder (2032) is nested and be fixed on the periphery of clipper (203), one end of described reach blade (2033) is connected with holder (2032), incline direction is contrary with the direction of rotation of clipper (203), the other end of described reach blade (2033) is connected with end blade (2034), described end blade (2034) is vertical setting with reach blade (2033).
4. a kind of process units and the method for mechanical stripping legal system for Graphene that adopt according to claim 1, is characterized in that described shearing groove (207) by tetrahedron or profile of tooth or both are in conjunction with forming.
5. a kind of process units and the method for mechanical stripping legal system for Graphene that adopt according to claim 1, it is characterized in that the tetrahedron of described shearing groove (207) or the drift angle angle of profile of tooth are 10 ° ~ 160 °, length is 1cm-1000cm, and thickness is 0.5cm ~ 3cm.
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| CN106365160A (en) * | 2016-10-21 | 2017-02-01 | 杭州国彪超声设备有限公司 | Graphite oxide ultrasonic-stripping device |
| CN106542526A (en) * | 2016-11-08 | 2017-03-29 | 成都新柯力化工科技有限公司 | A kind of utilization fluid accelerates the apparatus and method that Graphene slurry is peeled off in stirring |
| CN106957054A (en) * | 2017-05-05 | 2017-07-18 | 安徽大学 | A kind of method that sodium alginate up-stripping prepares graphene under high shear dispersion |
| CN107098355A (en) * | 2017-05-08 | 2017-08-29 | 塔里木大学 | A kind of quick stripping means of expanded vermiculite |
| CN107986264A (en) * | 2017-11-28 | 2018-05-04 | 深圳市中科智诚科技有限公司 | A kind of safe ultrasonic wave graphene based on Internet of Things peels off preparation facilities |
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| CN111285361A (en) * | 2020-04-14 | 2020-06-16 | 中北大学 | High-efficiency liquid-phase mechanical preparation method of low-defect and high-dispersion graphene |
| CN113145283A (en) * | 2021-02-23 | 2021-07-23 | 邯郸钢铁集团有限责任公司 | Laboratory equipment and method for preparing graphene by using tar residues |
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| CN106365160A (en) * | 2016-10-21 | 2017-02-01 | 杭州国彪超声设备有限公司 | Graphite oxide ultrasonic-stripping device |
| CN106542526A (en) * | 2016-11-08 | 2017-03-29 | 成都新柯力化工科技有限公司 | A kind of utilization fluid accelerates the apparatus and method that Graphene slurry is peeled off in stirring |
| CN106542526B (en) * | 2016-11-08 | 2018-08-24 | 成都新柯力化工科技有限公司 | A kind of device and method accelerating stirring stripping graphene slurry using fluid |
| CN106957054A (en) * | 2017-05-05 | 2017-07-18 | 安徽大学 | A kind of method that sodium alginate up-stripping prepares graphene under high shear dispersion |
| CN107098355A (en) * | 2017-05-08 | 2017-08-29 | 塔里木大学 | A kind of quick stripping means of expanded vermiculite |
| CN107986264A (en) * | 2017-11-28 | 2018-05-04 | 深圳市中科智诚科技有限公司 | A kind of safe ultrasonic wave graphene based on Internet of Things peels off preparation facilities |
| CN107986264B (en) * | 2017-11-28 | 2020-06-30 | 瑞安市任奇科技有限公司 | Safe ultrasonic graphene stripping preparation device based on Internet of things |
| CN110042284A (en) * | 2019-05-08 | 2019-07-23 | 东南大学 | A kind of preparation method of high-strength aluminum alloy |
| CN111285361A (en) * | 2020-04-14 | 2020-06-16 | 中北大学 | High-efficiency liquid-phase mechanical preparation method of low-defect and high-dispersion graphene |
| CN113555229A (en) * | 2020-04-26 | 2021-10-26 | 中天超容科技有限公司 | Graphene paper current collector, preparation method and supercapacitor |
| CN113555229B (en) * | 2020-04-26 | 2023-04-21 | 中天超容科技有限公司 | Graphene paper current collector, preparation method and supercapacitor |
| CN113145283A (en) * | 2021-02-23 | 2021-07-23 | 邯郸钢铁集团有限责任公司 | Laboratory equipment and method for preparing graphene by using tar residues |
| CN115289828A (en) * | 2022-08-10 | 2022-11-04 | 福建壹工软包装科技有限公司 | Graphene composite particle preparation device and application method thereof |
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Application publication date: 20160518 |