CN106241790A - The complete intelligent preparation facilities of a kind of Graphene - Google Patents
The complete intelligent preparation facilities of a kind of Graphene Download PDFInfo
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- CN106241790A CN106241790A CN201610753756.2A CN201610753756A CN106241790A CN 106241790 A CN106241790 A CN 106241790A CN 201610753756 A CN201610753756 A CN 201610753756A CN 106241790 A CN106241790 A CN 106241790A
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- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01P—INDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS
- C01P2004/00—Particle morphology
- C01P2004/01—Particle morphology depicted by an image
- C01P2004/03—Particle morphology depicted by an image obtained by SEM
Abstract
The invention belongs to Graphene complete manufacture equipment technology field, be specifically related to the complete intelligent preparation facilities of a kind of Graphene, automatization's formula can produce high-quality graphene product;Its agent structure includes liquid inlet opening, powder body charging aperture, high speed shear device, ultrasonic oscillator, reactor, electronic scale, granularity monitor, good pressure distribution device, storage tank, liquid level sensor, peristaltic pump, exsiccator, console, switch valve, nozzle, check valve, pipeline, aerosol apparatus, hydraulic pump;The present invention compared with prior art, uses full-automatic intelligent to produce, and all materials fully-automatic production the most under sealed conditions decreases manual operation error, improves quality of graphene;Complete equipment only needs a people in console control, reduces cost of labor, and it is strong that automated production improves the conforming product rate feature of environmental protection, the Graphene zero defect obtained, good conductivity, and its apparatus structure is simple, simple operation, and applied environment is friendly.
Description
Technical field:
The invention belongs to Graphene complete manufacture equipment technology field, be specifically related to the complete intelligent preparation of a kind of Graphene
Device, automatization's formula can produce high-quality graphene product.
Background technology:
The two dimensional crystal of the hexagon cellular structure that Graphene is made up of with sp2 hybrid orbital monolayer carbon atom;This spy
Different structure also gives the many peculiar performances of Graphene, and such as Graphene is the thinnest material the highest with intensity;
The light transmittance of Graphene only has 2.3%, nearly transparent;Under room temperature, the electron mobility of Graphene is more than 15000cm2/ V s, and
Resistivity only about 10-8Ω m, for the material that resistivity is minimum;The heat conductivity of Graphene is up to 5300W/m K, compares Buddha's warrior attendant
Stone is taller.The at present conventional method preparing Graphene mainly includes following several: mechanical stripping method, oxidation-reduction method, outer
Epitaxial growth, chemical vapour deposition technique;Oxidation-reduction method refers to use strong oxidizer by graphite under conditions of concentrated sulphuric acid exists
Lamella aoxidizes, and interlamellar spacing increases, and obtains graphite oxide, and graphite oxide Surface oxygen-containing groups increases, and has stronger hydrophilic,
Water can obtain graphene oxide through ultrasonic, then obtain reduced graphene by reduction.Oxidation-reduction method produces Graphene
Process uses substantial amounts of concentrated sulphuric acid and heavy metallic salt, has a huge impact environment;After graphite is oxidized simultaneously, lattice is tied
Structure is by considerable damage, and original performance is lost significantly, and equipment can be caused corrosion by strong oxidizer and concentrated sulphuric acid, is greatly shortened
Service life of equipment, adds production cost.Although epitaxial growth method and chemical vapour deposition technique can obtain quality relatively
High Graphene, but large-scale production and high cost Graphene cannot be made cannot to realize large-scale application.Machinery stripping
From method be use cheap graphite be material, production process will not introduce concentrated sulphuric acid and strong oxidizer, directly use machinery
Shearing force breaks the Van der Waals force of graphite layers, peels off graphite;Graphene zero defect prepared by this mode, electric conductivity
Well, environmental protection is pollution-free;But production process is the most extensive at present, and manual intervention process is more, does not has complete intelligentized
Graphene manufacture is equipped, and this can produce considerable influence to the quality of Graphene.It is complete that present Mechanical Method prepares high-quality graphene
Intelligent equipment becomes market exigence, therefore seeks to design a kind of Graphene intelligent manufacturing equipment to reduce artificial behaviour
Make the error existed, it is achieved Graphene intellectuality produces, reduces cost, improves efficiency, environmental protection, there is good economic effect
Benefit and social benefit.
Summary of the invention:
It is an object of the invention to the shortcoming overcoming prior art to exist, seek to design the complete intelligent system of a kind of Graphene
Standby device, makes graphite powder fully shear stripping by arranging high speed shear device, ultrasonic oscillator and good pressure distribution device, is formed
Graphene powder.
To achieve these goals, the agent structure of the complete intelligent preparation facilities of Graphene that the present invention relates to includes liquid
Body charging aperture, powder body charging aperture, high speed shear device, ultrasonic oscillator, reactor, electronic scale, granularity monitor, good pressure distribution
Device, storage tank, liquid level sensor, peristaltic pump, exsiccator, console, switch valve, nozzle, check valve, pipeline, aerosol apparatus, hydraulic pressure
Pump;Console is independently arranged at outside complete intelligent other all parts of preparation facilities of Graphene and other all parts electrical information
Connect, in order to control detect the working condition of other all parts and control the opening and closing of other all parts;Liquid enters
Material mouth and powder body charging aperture are separately positioned on the upper end of reactor, and electronic scale is arranged on the bottom of reactor, in order to by reactor
Gross weight Real-time Feedback pass through liquid feedstock respectively to console, liquid material and the graphite composite powder material of preparing Graphene
Mouth and powder body charging aperture enter reactor under the control of console;High speed shear device is arranged on the upper and lower two ends of reactor, in order to
Liquid material and graphite powder material to entering in reactor carry out high speed shear;Reactor is internally provided with the shake of multiple ultrasound wave
Swing device, in order to material is carried out ultrasonic wave concussion stripping;It is internal so that on-line monitoring material that granularity Detection device is arranged on reactor
Granularity variable condition;Good pressure distribution device is arranged on the outside of reactor, is connected with reactor by switch valve and pipeline, in order to
The material processed through reactor is carried out good pressure distribution;The bottom of good pressure distribution device is provided with hydraulic pump, in order to material
Pressurizeing, the internal left and right sides of hydraulic pump is symmetrically arranged with two check valves, in order to shunt the material after pressurization;High
The top of pressure disperser has been arranged oppositely two nozzles, a diameter of 10 μm-1mm of nozzle, in order to real to two strands of materials of pressurization
Now ejection at a high speed;Storage tank is connected with high speed disperser by pipeline, in order to the material that storage processed through high speed disperser,
The upper and lower of storage tank is respectively arranged with liquid level sensor, and liquid level sensor is connected with high speed disperser electrical information, in order to
Control the opening and closing of high speed disperser;Exsiccator is connected with storage tank by switch valve, peristaltic pump and pipeline, in order to entering
The material entered carries out heated drying of spraying;Peristaltic pump is arranged in the pipeline that storage tank stretches out, in order to controls material and at the uniform velocity enters dry
In dry device;Aerosol apparatus is arranged on the top of exsiccator and is connected with pipeline, in order to spray the material entered.
The agent structure of the console that the present invention relates to includes that centre console switch, a key produce touch screen, display screen, warning
Lamp, operation button and scram button;Between console with other each parts, electrical information is connected, to control and to protect whole Graphene
The operation of complete intelligent preparation facilities and safety;Display screen is arranged on the top of console, to show the shape of each component working
State information;It is provided with a key on console halfpace and produces touch screen, in order to use touch control type operation to control institute in display screen
The operation of display unit;Multiple alarm lamp and operation button, each alarm lamp and operation it is correspondingly arranged on console halfpace
The corresponding parts of button, in the work of operation this button corresponding component of button control, whether alarm lamp shows its corresponding component
Fault;Scram button is arranged on the side of operation button, in order to when component malfunction, whole Graphene out of service is complete
The operation of intelligent preparation facilities;Centre console switch is arranged on the side of console, to switch console.
The present invention uses the complete intelligent preparation technology of Graphene to specifically include material filling, graphite lift-off processing, high pressure
Dispersion processes and four steps of spray drying:
(1), material filling: controlled the liquid material of weight needed for liquid inlet opening adds in reactor by console,
The liquid material weight added is carried out feedback control by the electronic scale arranged bottom reactor;Liquid material filling after, then by
Control platform controls powder body charging aperture and adds the graphite composite powder material of required weight, the graphite composite powder weight of material of addition in reactor
Feedback control is carried out by the electronic scale arranged bottom reactor;
(2), graphite lift-off processing: after material filling, console control high speed shear device and open, material is existed
High speed shear stripping is carried out under 100-5000rpm rotating speed;After high speed shear device runs 5 minutes, open ultrasonic oscillator, simultaneously
Graphite powder material under fluid conditions is peeled off until granularity monitor monitors under 0.2-5KW power ultrasonic shakes
When granularity is 10-50 μm, closing high-speed clipper and ultrasonic oscillator, obtain graphite and peel off material;
(3), good pressure distribution process: while closing high-speed clipper and ultrasonic oscillator open good pressure distribution device and
Switch valve, peels off material by the graphite prepared by step (2) in a kettle. and sends in good pressure distribution device, be then turned on hydraulic pressure
Graphite is peeled off material and is forced into applying 10-300MPa and flows to nozzle by check valve by pump, and graphite is peeled off material and passed through
Nozzle forms two strands and clashes to high pressure liquid stream ejection at a high speed so that graphite is peeled off material refinement and formed graphene dispersion
Liquid;
(4), it is spray-dried: the graphene dispersing solution making step (3) be formed enters in storage tank, and the liquid level in storage tank passes
When the graphene dispersing solution that sensor monitoring is injected is to predetermined water level, good pressure distribution device cuts out;It is then turned on exsiccator and peristaltic pump,
Graphene dispersing solution sprays in exsiccator after passing through aerosol apparatus with the speed of 1-3000ml/min under the promotion of peristaltic pump,
Being dried at a temperature of 80-200 DEG C and form graphene powder, recovery gets product.
The present invention compared with prior art, uses full-automatic intelligent to produce, and all materials are the most complete
Automatically produce, decrease manual operation error, improve quality of graphene;Complete equipment only needs a people in console control, fall
Low cost of labor, automated production improves conforming product rate;Mechanical Method prepare Graphene do not use substantial amounts of sulphuric acid and
The strong oxidizing property heavy metallic salts such as potassium permanganate, therefore equipment will not cause corrosion to connect and reduce production cost, and the feature of environmental protection is strong,
The Graphene zero defect arrived, good conductivity;Its Graphene production technology principle is reliable, reasonable in design, and apparatus structure is simple, operation
Convenient, applied environment is friendly.
Accompanying drawing illustrates:
Fig. 1 is the agent structure principle schematic of the complete intelligent preparation facilities of the Graphene that the present invention relates to.
Fig. 2 is the console agent structure principle schematic that the present invention relates to.
Fig. 3 is the FB(flow block) of the complete intelligent preparation technology of the Graphene that the present invention relates to.
Fig. 4 is the electron scanning micrograph of the Graphene that the present invention produces.
Specific embodiment:
Below by embodiment and combine accompanying drawing the present invention will be further described.
Embodiment 1:
The agent structure of the complete intelligent preparation facilities of Graphene that the present embodiment relates to includes liquid inlet opening 1, powder body
Charging aperture 2, high speed shear device 3, ultrasonic oscillator 4, reactor 5, electronic scale 6, granularity monitor 7, good pressure distribution device 8, storage
Batch can 9, liquid level sensor 10, peristaltic pump 11, exsiccator 12, console 13, switch valve 14, nozzle 15, check valve 16, pipeline
17, aerosol apparatus 18, hydraulic pump 19;Console 13 is independently arranged at outside complete intelligent other all parts of preparation facilities of Graphene
It is connected with other all parts electrical information, in order to control detect the working condition of other all parts and control other all parts
Opening and closing;Liquid inlet opening 1 and powder body charging aperture 2 are separately positioned on the upper end of reactor 5, and electronic scale 6 is arranged on instead
Answer the bottom of still 5, in order to by the gross weight Real-time Feedback of reactor 5 to console 13, prepare Graphene liquid material and
Graphite composite powder material enters reactor 5 by liquid inlet opening 1 and powder body charging aperture 2 respectively under the control of console 13;High
Speed clipper 3 is arranged on reactor about 5 two ends, in order to liquid material and graphite powder material to entering in reactor 5 are carried out
High speed shear;Reactor 5 is internally provided with multiple ultrasonic wave concussion device 4, in order to material is carried out ultrasonic wave concussion stripping;Granularity
It is internal so that the granularity variable condition of on-line monitoring material that detector 7 is arranged on reactor 5;Good pressure distribution device 8 is arranged on reaction
The outside of still 5, is connected with reactor by switch valve 14 and pipeline 17, in order to carry out the material processed through reactor 5
Good pressure distribution;The bottom of good pressure distribution device 8 is provided with hydraulic pump 19, in order to pressurize material, about hydraulic pump 19 inside
Lateral symmetry is provided with two check valves 16, in order to shunt the material after pressurization;The top of good pressure distribution device 8 is to setting
It is equipped with two nozzles 15, a diameter of 10 μm-1mm of nozzle 15, in order to two strands of materials of pressurization are realized ejection at a high speed;Storage tank
9 are connected with high speed disperser 8 by pipeline 17, in order to store the material processed through high speed disperser 8, storage tank 9 upper
Portion and bottom are respectively arranged with liquid level sensor 10, and liquid level sensor 10 is connected with high speed disperser 8 electrical information, in order to control height
The opening and closing of speed disperser 8;Exsiccator 12 is connected with storage tank 9 by switch valve 14, peristaltic pump 11 and pipeline 17, in order to
The material entered is carried out heated drying of spraying;Peristaltic pump 11 is arranged in the pipeline 17 that storage tank 9 stretches out, in order to control material even
Speed enters in exsiccator 12;Aerosol apparatus 18 is arranged on the top of exsiccator 12 and is connected with pipeline 17, in order to enter the material entered
Row spraying.
The agent structure of the console 13 that the present embodiment relates to include centre console switch 131, key produce touch screen 132,
Display screen 133, alarm lamp 134, operation button 135 and scram button 136;Between console 13 and other each parts, electrical information is even
Connect, to control and to protect operation and the safety of the complete intelligent preparation facilities of whole Graphene;Display screen 133 is arranged on console
The top of 13, to show the status information of each component working;It is provided with a key on console 13 halfpace and produces touch screen
132, in order to use touch control type operation to control the operation of shown parts in display screen 133;Correspondence on console 13 halfpace
Multiple alarm lamp 134 and operation button 135, each alarm lamp 134 and the corresponding parts of operation button 135 are set, in operation
Button 135 controls the work of this button corresponding component, and alarm lamp 134 shows its corresponding component whether fault;Scram button 136 sets
Put the side at operation button 135, in order to the complete intelligent preparation dress of whole Graphene out of service when component malfunction
The operation put;Centre console switch 131 is arranged on the side of console 13, to switch console 13.
The present embodiment relates to the complete intelligent preparation technology of Graphene and includes that material filling, graphite lift-off processing, high pressure divide
Dissipate and process and be spray-dried four steps:
(1), material filling: controlled liquid inlet opening 1 by console 13 and add the liquids of required weight in reactor 5
Material, the liquid material weight of addition is carried out feedback control by the electronic scale 6 arranged bottom reactor 5;After liquid material filling, then
Controlled powder body charging aperture 2 by console 13 in reactor 5, add the graphite composite powder material of required weight, the graphite composite powder of addition
Weight of material is carried out feedback control by the electronic scale 6 arranged bottom reactor 5;
(2), graphite lift-off processing: after material filling, console 13 control high speed shear device 3 and open, to material
High speed shear stripping is carried out under 100-5000rpm rotating speed;After high speed shear device 3 runs 5 minutes, open ultrasonic oscillator 4,
Graphite powder material under fluid conditions is peeled off until granularity monitor 7 under 0.2-5KW power ultrasonic shakes simultaneously
Monitor granularity when being 10-50 μm, closing high-speed clipper 3 and ultrasonic oscillator 7, obtain graphite and peel off material;
(3), good pressure distribution processes: open good pressure distribution device while closing high-speed clipper 3 and ultrasonic oscillator 7
8 and switch valve 14, the graphite prepared by step (2) in reactor 5 is peeled off material and sends in good pressure distribution device 8, then
Open hydraulic pump 19 graphite stripping material is forced into applying 10-300MPa and flows to nozzle 15, stone by check valve 16
Ink stripping material forms two strands by nozzle 15 and clashes to high pressure liquid stream ejection at a high speed so that graphite is peeled off material and refined
Form graphene dispersing solution;
(4), it is spray-dried: the graphene dispersing solution making step (3) be formed enters in storage tank 9, the liquid level in storage tank 9
When the graphene dispersing solution that sensor 10 monitoring is injected is to predetermined water level, good pressure distribution device 8 cuts out;It is then turned on exsiccator 12 He
Peristaltic pump 11, graphene dispersing solution sprays into after passing through aerosol apparatus 18 with the speed of 1-3000ml/min under the promotion of peristaltic pump 11
In exsiccator 12, being dried and form graphene powder at a temperature of 80-200 DEG C, recovery gets product.
Claims (3)
1. the complete intelligent preparation facilities of Graphene, it is characterised in that its agent structure includes liquid inlet opening, powder body
Charging aperture, high speed shear device, ultrasonic oscillator, reactor, electronic scale, granularity monitor, good pressure distribution device, storage tank, liquid
Level sensor, peristaltic pump, exsiccator, console, switch valve, nozzle, check valve, pipeline, aerosol apparatus, hydraulic pump;Console is only
Vertical being arranged on outside complete intelligent other all parts of preparation facilities of Graphene is connected with other all parts electrical information, in order to control
System detects the working condition of other all parts and controls the opening and closing of other all parts;Liquid inlet opening and powder body enter
Material mouth is separately positioned on the upper end of reactor, and electronic scale is arranged on the bottom of reactor, in order to by real-time for the gross weight of reactor
Feeding back to console, liquid material and the graphite composite powder material of preparing Graphene are fed by liquid inlet opening and powder body respectively
Mouth enters reactor under the control of console;High speed shear device is arranged on the upper and lower two ends of reactor, in order to entering reactor
In liquid material and graphite powder material carry out high speed shear;Reactor is internally provided with multiple ultrasonic wave concussion device, in order to right
Material carries out ultrasonic wave concussion stripping;Granularity Detection device is arranged on reactor inside so that the granularity of on-line monitoring material changes shape
State;Good pressure distribution device is arranged on the outside of reactor, is connected with reactor by switch valve and pipeline, in order to through reactor
The material processed carries out good pressure distribution;The bottom of good pressure distribution device is provided with hydraulic pump, in order to pressurize material, hydraulic pressure
The internal left and right sides of pump is symmetrically arranged with two check valves, in order to shunt the material after pressurization;Good pressure distribution device upper
Portion has been arranged oppositely two nozzles, a diameter of 10 μm-1mm of nozzle, in order to two strands of materials of pressurization are realized ejection at a high speed;Storage
Batch can is connected with high speed disperser by pipeline, in order to the material that storage processed through high speed disperser, the top of storage tank
Being respectively arranged with liquid level sensor with bottom, liquid level sensor is connected with high speed disperser electrical information, in order to control high speed dispersion
The opening and closing of device;Exsiccator is connected with storage tank by switch valve, peristaltic pump and pipeline, in order to carry out the material entered
Spraying heated drying;Peristaltic pump is arranged in the pipeline that storage tank stretches out, in order to controls material and at the uniform velocity enters in exsiccator;Aerosol apparatus
The top being arranged on exsiccator is connected with pipeline, in order to spray the material entered.
The complete intelligent preparation facilities of Graphene the most according to claim 1, it is characterised in that the main body of described console
Structure includes that centre console switch, a key produce touch screen, display screen, alarm lamp, operation button and scram button;Console and its
Between his each parts, electrical information connects, to control and to protect operation and the safety of the complete intelligent preparation facilities of whole Graphene;
Display screen is arranged on the top of console, to show the status information of each component working;It is provided with one on console halfpace
Key produces touch screen, in order to use touch control type operation to control the operation of shown parts in display screen;On console halfpace
It is correspondingly arranged multiple alarm lamp and operation button, each alarm lamp and the operation corresponding parts of button, in operation button control
The work of this button corresponding component, alarm lamp shows its corresponding component whether fault;Scram button is arranged on the one of operation button
Side, in order to the operation of the complete intelligent preparation facilities of whole Graphene out of service when component malfunction;Centre console switch
It is arranged on the side of console, to switch console.
3. one kind uses the method that device as claimed in claim 1 prepares Graphene, it is characterised in that its preparation technology specifically wraps
Include material filling, graphite lift-off processing, good pressure distribution process and are spray-dried four steps:
(1), material filling: controlled liquid inlet opening by console and add the liquid material of required weight in reactor, add
Liquid material weight by bottom reactor arrange electronic scale carry out feedback control;After liquid material filling, then by console
Controlling powder body charging aperture and add the graphite composite powder material of required weight in reactor, the graphite composite powder weight of material of addition is by instead
The electronic scale answering bottom portion to arrange carries out feedback control;
(2), graphite lift-off processing: after material filling, console control high speed shear device and open, to material at 100-
High speed shear stripping is carried out under 5000rpm rotating speed;After high speed shear device runs 5 minutes, open ultrasonic oscillator, simultaneously to liquid
Graphite powder material under concrete conditions in the establishment of a specific crime carries out peeling off until granularity monitor monitors granularity under 0.2-5KW power ultrasonic shakes
During for 10-50 μm, closing high-speed clipper and ultrasonic oscillator, obtain graphite and peel off material;
(3), good pressure distribution processes: open good pressure distribution device and switch while closing high-speed clipper and ultrasonic oscillator
Valve, peels off material by the graphite prepared by step (2) in a kettle. and sends in good pressure distribution device, be then turned on hydraulic pump pair
Graphite is peeled off material and is carried out being forced into applying 10-300MPa and flowing to nozzle by check valve, and graphite is peeled off material and passed through nozzle
Form two strands to clash to high pressure liquid stream ejection at a high speed so that graphite is peeled off material refinement and formed graphene dispersing solution;
(4), it is spray-dried: the graphene dispersing solution making step (3) be formed enters in storage tank, the liquid level sensor in storage tank
When the graphene dispersing solution that monitoring is injected is to predetermined water level, good pressure distribution device cuts out;It is then turned on exsiccator and peristaltic pump, graphite
Alkene dispersion liquid sprays in exsiccator, at 80-200 after passing through aerosol apparatus with the speed of 1-3000ml/min under the promotion of peristaltic pump
Being dried at a temperature of DEG C and form graphene powder, recovery gets product.
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CN106622086A (en) * | 2017-01-03 | 2017-05-10 | 青岛华高墨烯科技股份有限公司 | Piston cover type high-pressure reactor |
CN106629695A (en) * | 2017-01-03 | 2017-05-10 | 青岛华高墨烯科技股份有限公司 | Preparation device of graphene composite dispersion liquid |
CN110064329A (en) * | 2019-04-08 | 2019-07-30 | 宁波锋成纳米科技有限公司 | A kind of ultrasonic disperse device and method |
CN112607728A (en) * | 2020-11-20 | 2021-04-06 | 中国科学院深圳先进技术研究院 | Automatic device for preparing graphene composite material by ultrasonic-assisted supercritical fluid |
CN112859676A (en) * | 2021-01-05 | 2021-05-28 | 杭州精浩机械有限公司 | Material treatment controlgear based on ultrasonic wave |
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CN105819438A (en) * | 2016-05-06 | 2016-08-03 | 成都新柯力化工科技有限公司 | Method for preparing nanometer graphene materials in large scale mode through hydraulic shearing |
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CN106622086A (en) * | 2017-01-03 | 2017-05-10 | 青岛华高墨烯科技股份有限公司 | Piston cover type high-pressure reactor |
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CN110064329B (en) * | 2019-04-08 | 2021-11-05 | 宁波锋成纳米科技有限公司 | Ultrasonic dispersion equipment and method |
CN112607728A (en) * | 2020-11-20 | 2021-04-06 | 中国科学院深圳先进技术研究院 | Automatic device for preparing graphene composite material by ultrasonic-assisted supercritical fluid |
CN112859676A (en) * | 2021-01-05 | 2021-05-28 | 杭州精浩机械有限公司 | Material treatment controlgear based on ultrasonic wave |
CN112859676B (en) * | 2021-01-05 | 2023-12-26 | 杭州精浩机械有限公司 | Material processing control equipment based on ultrasonic wave |
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