CN107416814A - A kind of method that graphene is prepared using solid phase assisted microwave synthesis - Google Patents
A kind of method that graphene is prepared using solid phase assisted microwave synthesis Download PDFInfo
- Publication number
- CN107416814A CN107416814A CN201710655878.2A CN201710655878A CN107416814A CN 107416814 A CN107416814 A CN 107416814A CN 201710655878 A CN201710655878 A CN 201710655878A CN 107416814 A CN107416814 A CN 107416814A
- Authority
- CN
- China
- Prior art keywords
- graphene
- solid phase
- prepared
- graphene oxide
- phase assisted
- Prior art date
- Legal status (The legal status is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the status listed.)
- Pending
Links
Classifications
-
- Y—GENERAL TAGGING OF NEW TECHNOLOGICAL DEVELOPMENTS; GENERAL TAGGING OF CROSS-SECTIONAL TECHNOLOGIES SPANNING OVER SEVERAL SECTIONS OF THE IPC; TECHNICAL SUBJECTS COVERED BY FORMER USPC CROSS-REFERENCE ART COLLECTIONS [XRACs] AND DIGESTS
- Y02—TECHNOLOGIES OR APPLICATIONS FOR MITIGATION OR ADAPTATION AGAINST CLIMATE CHANGE
- Y02P—CLIMATE CHANGE MITIGATION TECHNOLOGIES IN THE PRODUCTION OR PROCESSING OF GOODS
- Y02P20/00—Technologies relating to chemical industry
- Y02P20/10—Process efficiency
Landscapes
- Carbon And Carbon Compounds (AREA)
- Physical Or Chemical Processes And Apparatus (AREA)
Abstract
The invention discloses a kind of method that graphene is prepared using solid phase assisted microwave synthesis, by the first ultrasonic 10min 1h of the mixed liquor of graphite oxide and water, then 20 60min are centrifuged under conditions of 2000 3000rpm to the suspension of gained after ultrasound, supernatant liquor after centrifugation is graphene oxide colloid, is dried to obtain graphene oxide；The graphene oxide of above-mentioned gained and auxiliary absorbing material are put into industrial microwave oven reaction chamber simultaneously, under inert gas shielding, stop microwave after 15 90s are reacted under 300 2000W power condition, waits being cooled to room temperature and obtain graphene.Any chemical reagent harmful to human body and environment, safety and environmental protection need not be added in the course of reaction of the present invention；Its preparation technology is simple, and the reaction time is short, energy-efficient.
Description
Technical field
The invention belongs to materialogy field, is related to a kind of graphene, specifically a kind of to use solid phase assisted microwave synthesis system
The method of standby graphene.
Background technology
Graphene is one kind by sp2Hydridization carbon hexatomic ring composition two-dimensional and periodic honeycomb lattice structure it is new
Carbon nanomaterial, each C atoms are connected by very strong δ keys with 3 neighbouring C atoms in the lattice structure of ideal graphite alkene
Connect to form stable hexagonal structure；Each C atoms in hexatomic ring have the valence electron of a non-bonding, are hung down with plane
Straight direction forms the big pi bond of delocalization of conjugation, and the special lattice structure of graphene assigns its many unique performance.Its is special
Structure and excellent performance cause the extensive concern of material educational circles and community of physicists.Recent studies indicate that graphene has
There is the good spy of specific surface area, high mechanical strength, high electron mobility, thermal conduction characteristic and flexibility, the chemical stability of superelevation
Point, had broad application prospects in various fields such as material, electronics, chemistry, the energy, biological medicines.
People have carried out substantial amounts of research to the preparation method of graphene, property and application, but its preparation method
Development is still a bottleneck, although the various technologies for preparing grapheme material emerge in an endless stream, wherein also there is many methods to prepare
Go out graphene, but can not reach low cost, high quality, it is extensive simply required with technique, remain to be further improved and
Improve.How high-quality graphene is simultaneously prepared on a large scale, is become graphene industry with simple technique, minimum low cost
A technical barrier urgently to be resolved hurrily in development.
Generally acknowledge that the main method for preparing graphene has mechanical stripping method, chemical vapour deposition technique, solid-phase epitaxial growth at present
Method, oxidation-reduction method.In these techniques, oxidation-reduction method is the method for being easiest to realize large-scale production graphene,
Oxidation-reduction method mainly includes oxidation, the stripping of graphite oxide and three processes of reduction of graphene oxide of graphite.But by
Substantial amounts of oxygen-containing functional group such as carboxyl, hydroxyl, epoxy radicals are introduced in the oxidizing process in graphite so that prepared by final peel off
Graphene contain a large amount of oxygen-containing functional groups；To recover the intrinsic property of graphene, electronation, high temperature thermal reduction etc. need to be used
Post-process to remove the oxy radical of surface of graphene oxide.Electronation is often hydrazine hydrate, ethylenediamine, to benzene two with reducing agent
Phenol etc., although reduction effect is pretty good, complex process and reagent has toxicity can increase burden to environment and the mankind；Tradition
Even if reduction can not be reduced thoroughly at high temperature for heating, existence time is long and consumes energy the shortcomings that big.
Microwave heating method has quick heating, can improve the advantages of reaction speed as a kind of new mode of heating, by
Researcher attempts the reduction research for graphene oxide.At present, achieved using Microwave Solid heating redox graphene
Breakthrough, Chhowalla research teams are reduced using the pre-heat treatment combination pulse microwave（Household microwave oven 1000W power,
The microwave pulse of 1-2 seconds）Method（High-quality graphene via microwave reduction of
solution-exfoliated graphene oxide, Science, 2016, 353(6306):1413.）, the stone of preparation
Black alkene oxy radical removal amount is high, surface defect quantity is few.Pre-add heat treatment can make graphene oxide reducing degree improve from
And strengthening its absorbing property, moment high fever caused by strong suction ripple can make graphene oxide that depth deoxidation occur and promote carbon atom
Restructuring reduce defect.But this process also needs the participation of long period traditional heating mode to carry out in advance graphene oxide
Reduction.In addition, simple Microwave Solid heating technique, there is also certain challenge for the large-scale production to material.
The thinking of solid phase assisted microwave synthesis method redox graphene brings opportunity for the solution of above mentioned problem.Solid phase auxiliary is micro-
Wave heating is by the use of absorbing material as indirect thermal source to other non-absorbing materials（Or the non-material for inhaling ripple during normal temperature）Heated,
The advantages of combining traditional heating and microwave heating, is a kind of collaboration mode of heating, and its heating process is roughly divided into absorbing material
Preheating, heat transfer, the internal heat transfer of non-absorbing material between absorbing material and non-absorbing material（Or Wave heating itself is inhaled with passing
Heat）.Solid phase assisted microwave synthesis heating can avoid to form too high thermograde, preferably resistance to heating inside and outside material simultaneously
Only heat is lost, and material itself can be made to reach higher temperature, so as to effectively shorten the heat time, saves the energy.
Chinese patent CN201710218841.3 be " a kind of microwave radiation technology high-quality redox graphene of triggering mode
Preparation method ", during redox graphene have the time is short, energy consumption is low, free of contamination advantage, shortcoming has graphene
Directly contact and be not readily separated with triggering agent, and easily cause graphene pollution；The process of graphene oxide film is complicated；Reaction
During graphene oxide directly graphene oxide can be caused to be wasted with air contact.Graphene and auxiliary in the present invention
Separation problem is not present in absorbing material, and graphene oxide can be arbitrary form also without thin layer is made, and protect atmosphere not
It can cause to waste, auxiliary absorbing material can also reuse, and technique is simple in addition, saves resource and to human body and environment without danger
Evil.
The content of the invention
For above-mentioned technical problem of the prior art, graphite is prepared using solid phase assisted microwave synthesis the invention provides one kind
The method of alkene, the described this method for preparing graphene using solid phase assisted microwave synthesis will solve graphite oxide of the prior art
Alkene reducing process is complicated, pollutes environment, consume energy big technical problem.
The invention provides a kind of method that graphene is prepared using solid phase assisted microwave synthesis, comprise the following steps：
1) by the first ultrasonic 10min-1h of the mixed liquor of graphite oxide and water, then to the suspension of gained after ultrasound in 2000-
20-60min is centrifuged under conditions of 3000rpm, the supernatant liquor after centrifugation is graphene oxide colloid, and stone must be aoxidized by being dried
Black alkene；
2) by step 1）The graphene oxide and auxiliary absorbing material of gained are put into industrial microwave oven reaction chamber simultaneously, in inertia
Under gas shield, microwave is closed after reacting 15-90s under 300-2000W power condition, waits being cooled to room temperature and obtain graphite
Alkene.
Further, step 1）Described in graphene oxide product be membranaceous, powdery or freeze-drying into bulk.
Further, any one or two or more group of the described inert gas in nitrogen, argon gas, helium
Close.
Further, described graphene oxide and auxiliary absorbing material are not directly contacted with.
Further, described auxiliary absorbing material be selected from bulky silicon carbide, block graphite, carborundum powder, graphite powder or
Any one in person's carbon dust.
Further, if auxiliary absorbing material is powder body material, graphene oxide is positioned over first quartz glass
In container, the first described quartz container is positioned in second quartz container, the first described quartz glass
There is annular space between container and the second quartz container, first quartz container and the second quartz container it
Between be provided with auxiliary absorbing material.
Further, if auxiliary absorbing material is bulk material, graphene oxide is positioned over a quartz container
In, the periphery of described quartz container is provided with auxiliary absorbing material.
Solid phase and obtained graphene oxide are put into industrial microwave oven by the present invention simultaneously, are made using solid phase absorbing material
Graphene oxide is heated for indirect thermal source, under inert gas shielding, the reduction of graphene oxide is successfully realized, obtains
Obtain graphene.The advantages of being heated present invention incorporates traditional heating and microwave, mode of heating reduction-oxidation graphite is cooperateed with one kind
Alkene.Solid phase assisted microwave synthesis heating can avoid to form too high thermograde, preferably prevent to being heated inside and outside material simultaneously
Scattering and disappearing for heat, can make material itself reach higher temperature, so as to effectively shorten the heat time, save the energy, simplify
Technique.
The present invention compares with prior art, and its technological progress is significant.First using absorbing material solid phase as indirect
Thermal source heats to graphene oxide, combines the advantages of traditional heating and microwave heat, is successfully realized graphene oxide
Reduction；Secondly relative to traditional chemical reduction method, this method need not add any chemical reagents, nontoxic, safety
Environmental protection；Finally relative to traditional thermal reduction method, the method is simple to operate, and the reaction time is short, energy-efficient.Reduce rear oxidation graphite
The interlamellar spacing of alkene film is obviously reduced, and has the characteristics of reducing degree is higher.Its preparation technology is simple, is easy to industrial metaplasia
Production.
Brief description of the drawings
Fig. 1 is auxiliary wave absorbing agent material when be powder, the microwave placement schematic diagram of graphene oxide.
Fig. 2 is auxiliary wave absorbing agent material when being block, and the microwave of graphene oxide places schematic diagram.
Embodiment
Embodiment 1
Using the mixed liquor for improving Hummers methods and preparing graphite oxide and water, comprise the following steps that：
Measure the 96mL concentrated sulfuric acids to be placed in drying receptacle, add 2g sodium nitrate thereto, after stirring dissolves sodium nitrate, add
2g crystalline flake graphites, after crystalline flake graphite is uniformly dispersed, 12g potassium permanganate is slowly added to, reacts 1.45h, whole process uses ice
Bath makes system be maintained at 0-3 DEG C, and then temperature rises to 35 DEG C of reaction 2h, and 80mL deionizations are then slowly added into reaction system
Water, temperature rise to 95 DEG C of reaction 30min, are slowly added into 200mL deionized waters again afterwards, then add 10mL H2O2, continue
10min, the reaction solution centrifugation of gained are reacted, gained precipitation is washed with the HCl/water solution that 1000mL mass percent concentrations are 5%,
With metal ion of going out, then it is washed with deionized until the pH of efflux is neutrality, obtains the mixing of graphite oxide and water
Liquid.
Embodiment 2
A kind of method that solid phase assisted microwave synthesis redox graphene prepares graphene, specifically comprises the following steps：
（1）, by the mixed liquor of graphite oxide and water to 1L, ultrasonic 45min under 80W, 40KHz, to the suspension of gained after ultrasound
2000rpm centrifugation 60min are controlled, takes supernatant to be ground in vacuum drying chamber after 80 DEG C of dry 24h, obtains graphene oxide powder
Body；
Described graphite oxide and the mixed liquor of water are prepared using improved Hummers methods；
（2）, 150g silicon carbide powders 5 are filled in the annular space between the first quartz glass 1 and the second quartz glass 3,
And by 200mg steps（1）Graphene oxide 2 is made to be put into the first quartz glass 1（As shown in Figure 1）, it is micro- to place into industry
Being vacuumized in ripple stove makes absolute pressure in burner hearth be less than 0.1MPa, is vacuumized again after logical argon gas to normal pressure, repeats this process three times.
The argon gas of stream is first passed through before unlatching microwave in reaction chamber, to remove the oxygen remained in reaction chamber.Under 2000W, 15s is reacted
Afterwards, microwave is closed, room temperature is cooled to, obtains graphene.
Determined through x-ray photoelectron energy spectrum diagram, graphene oxide C/O atomic ratios are 2.5 before reduction, are risen to after carrying out reduction
20.1。
Embodiment 3
A kind of method that solid phase assisted microwave synthesis redox graphene prepares graphene, specifically comprises the following steps：
（1）, by the mixed liquor of graphite oxide and water to 0.5L, ultrasonic 45min under 80W, 40KHz, the suspension to gained after ultrasound
Hydraulic control 2500rpm centrifuges 30min, takes supernatant to be collected in air dry oven after 60 DEG C of dry 24h, obtains graphene oxide
Fragment；
Described graphite oxide and the mixed liquor of water are prepared using improved Hummers methods；
（2）, 80g powdered graphites 5 are filled in the annular space between the first quartz glass 1 and the second quartz glass 3, and will
100mg steps (1) are made graphene oxide 2 and are put into the first quartz glass 1（As shown in Figure 1）, place into industrial microwave oven
In vacuumize and absolute pressure in burner hearth is less than 0.1MPa, vacuumized again after logical argon gas to normal pressure, repeat this process three times.Open
The nitrogen of stream is first passed through before microwave in reaction chamber, to remove the oxygen remained in reaction chamber.Under 300W, after reacting 90s, close
Microwave, room temperature is cooled to, obtains graphene.
Determined through x-ray photoelectron energy spectrum diagram, graphene oxide C/O atomic ratios are 2.5 before reduction, are risen to after carrying out reduction
15.8。
Embodiment 4
A kind of method that solid phase assisted microwave synthesis redox graphene prepares graphene, specifically comprises the following steps：
（1）, by the mixed liquor of graphite oxide and water to 1L, ultrasonic 45min under 80W, 40KHz, to the suspension of gained after ultrasound
3000rpm centrifugation 20min are controlled, takes supernatant to be collected after being freeze-dried, obtains block graphene oxide；
Described graphite oxide and the mixed liquor of water are prepared using improved Hummers methods；
（2）And 500mg graphene oxides 2 are put into small (band stomata 4) quartz glass 1 with cover and are put into furnace chamber, it is carbonized
Silicon bulk 5 is dispersed in the outside of quartz glass 1（As shown in Figure 2）, placing into industrial microwave oven to vacuumize makes in burner hearth absolutely
0.1MPa is less than to pressure, is vacuumized again after logical argon gas to normal pressure, repeats this process three times.First lead in reaction chamber before unlatching microwave
The argon gas to become a mandarin, to remove the oxygen remained in reaction chamber.Under 1500W, after reacting 60s, microwave is closed, is cooled to room temperature,
Obtain graphene.
Determined through x-ray photoelectron energy spectrum diagram, graphene oxide C/O atomic ratios are 2.5 before reduction, are risen to after carrying out reduction
20.3。
In summary, a kind of solid phase assisted microwave synthesis redox graphene of the invention is prepared obtained by the method for graphene
Redox graphene, its preparation technology is simple, is easy to industrialized production, has in heat dissipation from microelectronic devices field potential real
Border application value.
Described above is only the citing of embodiments of the present invention, it is noted that for the ordinary skill of the art
For personnel, without departing from the technical principles of the invention, some improvement can also be made, these improvement also should be regarded as this
The protection domain of invention.
Claims (7)
- A kind of 1. method that graphene is prepared using solid phase assisted microwave synthesis, it is characterised in that comprise the following steps：1）By the first ultrasonic 10min-1h of the mixed liquor of graphite oxide and water, then to the suspension of gained after ultrasound in 2000- 20-60min is centrifuged under conditions of 3000rpm, the supernatant liquor after centrifugation is graphene oxide colloid, and stone must be aoxidized by being dried Black alkene；2）By step 1）The graphene oxide and auxiliary absorbing material of gained are put into industrial microwave oven reaction chamber simultaneously, in inertia Under gas shield, microwave is closed after reacting 15-90s under 300-2000W power condition, waits being cooled to room temperature and obtain graphite Alkene.
- A kind of 2. method that graphene is prepared using solid phase assisted microwave synthesis as claimed in claim 1, it is characterised in that：Step 1） Described in graphene oxide product be membranaceous, powdery or freeze-drying into bulk.
- A kind of 3. method that graphene is prepared using solid phase assisted microwave synthesis as claimed in claim 1, it is characterised in that：Described Any one or two or more combination of the inert gas in nitrogen, argon gas, helium.
- A kind of 4. method that graphene is prepared using solid phase assisted microwave synthesis as claimed in claim 1, it is characterised in that：Described Graphene oxide and auxiliary absorbing material are not directly contacted with.
- A kind of 5. method that graphene is prepared using solid phase assisted microwave synthesis as claimed in claim 1, it is characterised in that：Described Aid in any one of absorbing material in bulky silicon carbide, block graphite, carborundum powder, graphite powder or carbon dust.
- A kind of 6. method that graphene is prepared using solid phase assisted microwave synthesis as claimed in claim 1, it is characterised in that：If auxiliary Absorbing material is powdery, and graphene oxide product is positioned in first quartz container, the described first quartzy glass Glass container is positioned in second quartz container, the first described quartz container and the second quartz container it Between there is annular space, annular space between first quartz container and the second quartz container filling powdery auxiliary inhales ripple Material.
- A kind of 7. method that graphene is prepared using solid phase assisted microwave synthesis as claimed in claim 1, it is characterised in that：If auxiliary Wave absorbing agent material is block, and graphene oxide product is positioned in a quartz container, is held in described quartz glass Place auxiliary absorbing material in the periphery of device.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201710655878.2A CN107416814A (en) | 2017-08-03 | 2017-08-03 | A kind of method that graphene is prepared using solid phase assisted microwave synthesis |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201710655878.2A CN107416814A (en) | 2017-08-03 | 2017-08-03 | A kind of method that graphene is prepared using solid phase assisted microwave synthesis |
Publications (1)
| Publication Number | Publication Date |
|---|---|
| CN107416814A true CN107416814A (en) | 2017-12-01 |
Family
ID=60437349
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| CN201710655878.2A Pending CN107416814A (en) | 2017-08-03 | 2017-08-03 | A kind of method that graphene is prepared using solid phase assisted microwave synthesis |
Country Status (1)
| Country | Link |
|---|---|
| CN (1) | CN107416814A (en) |
Cited By (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN109019578A (en) * | 2018-10-16 | 2018-12-18 | 上海应用技术大学 | A kind of method of microwave reduction graphene oxide |
| CN112320796A (en) * | 2020-10-30 | 2021-02-05 | 浙江锂宸新材料科技有限公司 | Preparation method for simply increasing graphite layer spacing |
| CN116161652A (en) * | 2023-04-23 | 2023-05-26 | 湖南金阳烯碳新材料股份有限公司 | Energy-saving recyclable graphene purification processing method |
| CN116239106A (en) * | 2023-02-16 | 2023-06-09 | 广东轻工职业技术学院 | Method for preparing high-heat-conductivity reduced graphene oxide aerogel by microwave assistance |
Citations (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN102730678A (en) * | 2012-07-23 | 2012-10-17 | 贵州新碳高科有限责任公司 | Device and method for preparing graphene powder |
| CN103342358A (en) * | 2013-07-19 | 2013-10-09 | 东南大学 | Method for quickly preparing large amount of layer number controllable high-quality graphene |
| CN103787316A (en) * | 2013-12-31 | 2014-05-14 | 深圳粤网节能技术服务有限公司 | Oxidized graphene based on mixed acid system and preparation method of graphene |
| CN104591177A (en) * | 2015-02-03 | 2015-05-06 | 辽宁工程技术大学 | Method for preparing self-supporting three-dimensional porous graphene composite microsphere |
| CN104671238A (en) * | 2015-02-06 | 2015-06-03 | 中国科学院山西煤炭化学研究所 | Method for quickly preparing high-performance graphene |
-
2017
- 2017-08-03 CN CN201710655878.2A patent/CN107416814A/en active Pending
Patent Citations (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN102730678A (en) * | 2012-07-23 | 2012-10-17 | 贵州新碳高科有限责任公司 | Device and method for preparing graphene powder |
| CN103342358A (en) * | 2013-07-19 | 2013-10-09 | 东南大学 | Method for quickly preparing large amount of layer number controllable high-quality graphene |
| CN103787316A (en) * | 2013-12-31 | 2014-05-14 | 深圳粤网节能技术服务有限公司 | Oxidized graphene based on mixed acid system and preparation method of graphene |
| CN104591177A (en) * | 2015-02-03 | 2015-05-06 | 辽宁工程技术大学 | Method for preparing self-supporting three-dimensional porous graphene composite microsphere |
| CN104671238A (en) * | 2015-02-06 | 2015-06-03 | 中国科学院山西煤炭化学研究所 | Method for quickly preparing high-performance graphene |
Non-Patent Citations (2)
| Title |
|---|
| WUFENG CHEN ET AL.: "Preparation of graphene by the rapid and mild thermal reduction of graphene oxide induced by microwaves", 《CARBON》 * |
| 姜洪舟等: "《无机非金属材料热工设备》", 28 February 2015, 武汉：武汉理工大学出版社 * |
Cited By (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN109019578A (en) * | 2018-10-16 | 2018-12-18 | 上海应用技术大学 | A kind of method of microwave reduction graphene oxide |
| CN112320796A (en) * | 2020-10-30 | 2021-02-05 | 浙江锂宸新材料科技有限公司 | Preparation method for simply increasing graphite layer spacing |
| CN116239106A (en) * | 2023-02-16 | 2023-06-09 | 广东轻工职业技术学院 | Method for preparing high-heat-conductivity reduced graphene oxide aerogel by microwave assistance |
| CN116161652A (en) * | 2023-04-23 | 2023-05-26 | 湖南金阳烯碳新材料股份有限公司 | Energy-saving recyclable graphene purification processing method |
Similar Documents
| Publication | Publication Date | Title |
|---|---|---|
| CN107416814A (en) | A kind of method that graphene is prepared using solid phase assisted microwave synthesis | |
| CN104030275B (en) | A kind of preparation method of redox graphene heat conduction thin film | |
| CN104826582B (en) | A kind of preparation method of graphene meso-porous titanium dioxide silica aerogel | |
| CN101913600B (en) | Method for preparing graphene/semiconductor quantum dot composite material | |
| CN106542509A (en) | A kind of efficient method for preparing class Graphene carbonitride | |
| CN107827102A (en) | A kind of method for preparing graphene | |
| CN104591551A (en) | Preparation method of graphene-coated glass fiber composite material | |
| CN109019578A (en) | A kind of method of microwave reduction graphene oxide | |
| CN106832961B (en) | The preparation method of graphene thermal conductive silicon rubber mat | |
| CN102502611A (en) | Method for rapidly preparing graphene in large quantities by utilizing graphite oxides | |
| WO2016011905A1 (en) | Silver-doped graphene composite paper and preparation method therefor | |
| WO2012109969A1 (en) | Method for producing graphene material by microwave irradiation in a vacuum or inert-gas environment | |
| CN103359709A (en) | Preparation method of nitrogen-doped graphene | |
| CN104386676A (en) | Preparation method of graphene | |
| CN102807845A (en) | Preparation method for high heat conduction and radiation material by intercalating metal particles between layers of thin-layer graphene | |
| CN103811721B (en) | A kind of preparation method of lithium battery cathode plate | |
| CN107986267A (en) | The method and its heating furnace that a kind of redox graphene powder upgrading is modified | |
| TWI546254B (en) | Method of surface modifying graphene | |
| WO2012109968A1 (en) | Method for preparing modified graphene material by microwave irradiation in controlled atmosphere | |
| KR101470927B1 (en) | Method of Copper Oxide-Zinc Oxide/reduced graphene oxide composite | |
| CN104003372A (en) | Graphene material and preparation method thereof | |
| CN108996496A (en) | A method of preparing graphene/graphene mixed film | |
| CN104689798A (en) | Method for preparing composite mesoporous material | |
| CN106673634A (en) | Quantum magnetic sheet material | |
| CN103803534B (en) | A kind of preparation method of Graphene silicon nano power powder composite material |
Legal Events
| Date | Code | Title | Description |
|---|---|---|---|
| PB01 | Publication | ||
| PB01 | Publication | ||
| SE01 | Entry into force of request for substantive examination | ||
| WD01 | Invention patent application deemed withdrawn after publication |
Application publication date: 20171201 |
|
| WD01 | Invention patent application deemed withdrawn after publication |