CN101993064B - Method for preparing hydrophilic graphene - Google Patents

Method for preparing hydrophilic graphene Download PDF

Info

Publication number
CN101993064B
CN101993064B CN2010105235715A CN201010523571A CN101993064B CN 101993064 B CN101993064 B CN 101993064B CN 2010105235715 A CN2010105235715 A CN 2010105235715A CN 201010523571 A CN201010523571 A CN 201010523571A CN 101993064 B CN101993064 B CN 101993064B
Authority
CN
China
Prior art keywords
graphene
iron powder
graphite oxide
dispersion liquid
dispersion
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.)
Expired - Fee Related
Application number
CN2010105235715A
Other languages
Chinese (zh)
Other versions
CN101993064A (en
Inventor
沈小平
柏嵩
季振源
Current Assignee (The listed assignees may be inaccurate. Google has not performed a legal analysis and makes no representation or warranty as to the accuracy of the list.)
Jiangsu University
Original Assignee
Jiangsu University
Priority date (The priority date 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 date listed.)
Filing date
Publication date
Application filed by Jiangsu University filed Critical Jiangsu University
Priority to CN2010105235715A priority Critical patent/CN101993064B/en
Publication of CN101993064A publication Critical patent/CN101993064A/en
Application granted granted Critical
Publication of CN101993064B publication Critical patent/CN101993064B/en
Expired - Fee Related legal-status Critical Current
Anticipated expiration legal-status Critical

Links

Images

Abstract

The invention relates to a method for preparing hydrophilic graphene, belonging to the field of inorganic materials. The method comprises the following process flows of: oxidizing natural crystalline flake graphite used as a raw material to obtain graphite oxide by a Hummers method; then carrying out ultrasonic dispersion on the obtained graphite oxide in deionized water to ensure that the graphite oxide is peeled into a graphene oxide dispersion; regulating the pH value of the dispersion to 10-10.5; heating the dispersion to 100 DEG C; adding iron powder by a mass ratio of (0.5-2):1 of the iron powder to the graphite oxide; carrying out a refluxing reaction for 1-1.5h at 100 DEG C to obtain a graphene dispersion which can stably disperse in water; carrying out vacuum filtering on the dispersion through a microfiltration membrane; and finally, carrying out water washing and drying on an obtained solid product. The invention has the advantages of simple process, convenient operation, economy and environmental protection.

Description

A kind of method for preparing hydrophilic graphene
Technical field
The invention belongs to the inorganic materials chemical field, relating to a kind of is the method that reductive agent prepares hydrophilic graphene with the iron powder.
Background technology
Graphene be 2004 found a kind of by sp 2The cellular two-dimentional carbonaceous novel material of periodicity that the carbon atom of hydridization forms with hexagonal array, it is considered to the basic structural unit of other dimension blackings such as soccerballene, carbon nanotube, graphite; Graphene shows the character of many excellences, and for example Graphene is the firmest in the world material (Young ' s modulus~1.0 TPa), and theoretical specific surface area is up to 2630 m 2/ g has high speed electronic mobility (~200000 cm under outstanding thermal conductivity (~5000 W/ (mK)) and the room temperature 2/ (Vs)), simultaneously, its particular structure makes it have special nature such as perfect quantum hall effect, unique quantum tunnel effect, ambipolar electric field effect.These excellent character have made Graphene become one of the most popular research topic in Materials science and condensed state physics field rapidly.
Preparation method of graphene mainly contains mechanically peel method, crystal epitaxy method, chemical reduction method etc. at present, and these methods respectively have its relative merits; Chemical reduction method is a kind of important preparation method; The main reductive agent reduction-oxidation graphite such as Hydrazine Hydrate 80, dimethylhydrazine, Peng Qinghuana that adopt; This method is suitable for the scale operation of Graphene, and still, reductive agents such as Hydrazine Hydrate 80, dimethylhydrazine not only price are higher; And having high toxicity, this has caused very big difficulty for the research and the application of Graphene.Present method adopt cheapness and the iron powder of environmental protection to be reductive agent prepare Graphene, avoided highly toxic materials such as use Hydrazine Hydrate 80, dimethylhydrazine, and can be in the aqueous solution uniform and stable dispersion of the Graphene of preparation.
Summary of the invention
The present invention has considered the problem that occurs in the prior art, and it is the method that reductive agent prepares hydrophilic graphene with the iron powder that purpose is to provide a kind of, adopts following technical scheme:
1) with the natural flake graphite is raw material, its oxidation obtained graphite oxide with the Hummers method;
2) with the graphite oxide ultra-sonic dispersion in water, form the graphene oxide dispersion liquid, the concentration of graphene oxide is 0.2~1.0 g/L;
3) using massfraction is pH value to 10~10.5 that 28% ammoniacal liquor is regulated dispersion liquid;
4) solution is heated to 100 ℃, adds iron powder, the mass ratio of iron powder and graphite oxide is in the scope of 0.5 ~ 2:1, at 100 ℃ of 1~1.5 h that reflux;
5) after the cooling, separate remaining iron powder, obtain black Graphene homodisperse liquid with magnet;
6) the Graphene dispersion liquid is through the millipore filtration vacuum filtration, and the solid product that obtains is with water washing three times, 60 ℃ of vacuum-dryings.
Principal feature of the present invention is: with iron powder cheap, environmental protection is reductive agent, obtains the Graphene dispersion liquid of stable dispersion in water fast, and technology of the present invention is simple, easy and simple to handle, cost is low.
Description of drawings
Fig. 1 is X-ray diffraction (XRD) spectrogram of the graphene film of the embodiment of the invention 1 preparation.Wherein X-coordinate is a diffraction angle (2 θ), unit for the degree ( 0); Ordinate zou is a diffraction intensity, and unit is cps;
Fig. 2 is transmission electron microscope (TEM) photo of the graphene film of the embodiment of the invention 1 preparation;
Fig. 3 is ESEM (SEM) photo of the graphene film of the embodiment of the invention 1 preparation.
Embodiment
Below in conjunction with accompanying drawing embodiments of the invention are done detailed explanation, but protection scope of the present invention is not limited to these embodiment.
Embodiment 1
Take by weighing the graphite oxide for preparing with the Hummers method and disperse in deionized water for ultrasonic, be configured to the dispersion liquid of 0.5 g/L concentration, the use massfraction is 28% ammoniacal liquor regulator solution pH=10; Solution is heated to 100 ℃, adds iron powder, the mass ratio of iron powder and graphite oxide is 2:1; React 1 h 100 ℃ of following stirring and refluxing, cooling separates remaining iron powder with magnet; Obtain finely dispersed Graphene dispersion liquid, place and do not have the deposition generation in one month; Graphene homodisperse liquid is through the millipore filtration vacuum filtration, and the solid product that obtains is with water washing three times, 60 ℃ of vacuum-dryings.
Gained Graphene dispersion liquid is stable black colloidal dispersion; Fig. 1 is the XRD figure of product, 2 θVery wide (a 002) diffraction peak has appearred in=24.8 places, and corresponding interlamellar spacing is about 0.36 nm, and (0.34 nm) is bigger than graphite, 2 θShow (100) diffraction peak that Graphene is weak about=44.6 °; Fig. 2 is the TEM figure of this product, can see large stretch of graphene film, and graphene film is totally smooth, and there is the fold as the silk part, and Fig. 3 is the SEM figure of this product.
Embodiment 2
Take by weighing the graphite oxide for preparing with the Hummers method and disperse in deionized water for ultrasonic, be configured to the dispersion liquid of 0.2 g/L concentration, the use massfraction is 28% ammoniacal liquor regulator solution pH=10; Solution is heated to 100 ℃, adds iron powder, the mass ratio of iron powder and graphite oxide is 2:1; React 1 h 100 ℃ of following stirring and refluxing, cooling separates remaining iron powder with magnet; Obtain finely dispersed Graphene dispersion liquid, place and do not have the deposition generation in one month; Graphene homodisperse liquid is through the millipore filtration vacuum filtration, and the solid product that obtains is with water washing three times, 60 ℃ of vacuum-dryings.
Embodiment 3
Take by weighing the graphite oxide for preparing with the Hummers method and disperse in deionized water for ultrasonic, be configured to the dispersion liquid of 1.0 g/L concentration, the use massfraction is 28% ammoniacal liquor regulator solution pH=10; Solution is heated to 100 ℃, adds iron powder, the mass ratio of iron powder and graphite oxide is 2:1; React 1 h 100 ℃ of following stirring and refluxing, cooling separates remaining iron powder with magnet; Obtain finely dispersed Graphene dispersion liquid, place and do not have the deposition generation in one month; Graphene homodisperse liquid is through the millipore filtration vacuum filtration, and the solid product that obtains is with water washing three times, 60 ℃ of vacuum-dryings.
Embodiment 4
Take by weighing the graphite oxide for preparing with the Hummers method and disperse in deionized water for ultrasonic, be configured to the dispersion liquid of 0.5 g/L concentration, the use massfraction is 28% ammoniacal liquor regulator solution pH=10; Solution is heated to 100 ℃, adds iron powder, the mass ratio of iron powder and graphite oxide is at 1:2; React 1 h 100 ℃ of following stirring and refluxing, cooling separates remaining iron powder with magnet; Obtain finely dispersed Graphene dispersion liquid, place and do not have the deposition generation in one month; Graphene homodisperse liquid is through the millipore filtration vacuum filtration, and the solid product that obtains is with water washing three times, 60 ℃ of vacuum-dryings.
Embodiment 5
Take by weighing the graphite oxide for preparing with the Hummers method and disperse in deionized water for ultrasonic, be configured to the dispersion liquid of 0.2 g/L concentration, the use massfraction is 28% ammoniacal liquor regulator solution pH=10; Solution is heated to 100 ℃, adds iron powder, the mass ratio of iron powder and graphite oxide is at 1:2; React 1 h 100 ℃ of following stirring and refluxing, cooling separates remaining iron powder with magnet; Obtain finely dispersed Graphene dispersion liquid, place and do not have the deposition generation in one month; Graphene homodisperse liquid is through the millipore filtration vacuum filtration, and the solid product that obtains is with water washing three times, 60 ℃ of vacuum-dryings.
Embodiment 6
Take by weighing the graphite oxide for preparing with the Hummers method and disperse in deionized water for ultrasonic, be configured to the dispersion liquid of 1.0 g/L concentration, the use massfraction is 28% ammoniacal liquor regulator solution pH=10; Solution is heated to 100 ℃, adds iron powder, the mass ratio of iron powder and graphite oxide is at 1:2; React 1 h 100 ℃ of following stirring and refluxing, cooling separates remaining iron powder with magnet; Obtain finely dispersed Graphene dispersion liquid, place and do not have the deposition generation in one month; Graphene homodisperse liquid is through the millipore filtration vacuum filtration, and the solid product that obtains is with water washing three times, 60 ℃ of vacuum-dryings.
Embodiment 7
Take by weighing the graphite oxide for preparing with the Hummers method and disperse in deionized water for ultrasonic, be configured to the dispersion liquid of 0.5 g/L concentration, the use massfraction is 28% ammoniacal liquor regulator solution pH=10; Solution is heated to 100 ℃, adds iron powder, the mass ratio of iron powder and graphite oxide is at 1:1; React 1 h 100 ℃ of following stirring and refluxing, cooling separates remaining iron powder with magnet; Obtain finely dispersed Graphene dispersion liquid, place and do not have the deposition generation in one month; Graphene homodisperse liquid is through the millipore filtration vacuum filtration, and the solid product that obtains is with water washing three times, 60 ℃ of vacuum-dryings.
Embodiment 8
Take by weighing the graphite oxide for preparing with the Hummers method and disperse in deionized water for ultrasonic, be configured to the dispersion liquid of 0.2 g/L concentration, the use massfraction is 28% ammoniacal liquor regulator solution pH=10; Solution is heated to 100 ℃, adds iron powder, the mass ratio of iron powder and graphite oxide is 1:1; React 1 h 100 ℃ of following stirring and refluxing, cooling separates remaining iron powder with magnet; Obtain finely dispersed Graphene dispersion liquid, place and do not have the deposition generation in one month; Graphene homodisperse liquid is through the millipore filtration vacuum filtration, and the solid product that obtains is with water washing three times, 60 ℃ of vacuum-dryings.
Embodiment 9
Take by weighing the graphite oxide for preparing with the Hummers method and disperse in deionized water for ultrasonic, be configured to the dispersion liquid of 1.0 g/L concentration, the use massfraction is 28% ammoniacal liquor regulator solution pH=10; Solution is heated to 100 ℃, adds iron powder, the mass ratio of iron powder and graphite oxide is 1:1; React 1 h 100 ℃ of following stirring and refluxing, cooling separates remaining iron powder with magnet; Obtain finely dispersed Graphene dispersion liquid, place and do not have the deposition generation in one month; Graphene homodisperse liquid is through the millipore filtration vacuum filtration, and the solid product that obtains is with water washing three times, 60 ℃ of vacuum-dryings.
Embodiment 10
Take by weighing the graphite oxide for preparing with the Hummers method and disperse in deionized water for ultrasonic, be configured to the dispersion liquid of 0.5 g/L concentration, the use massfraction is 28% ammoniacal liquor regulator solution pH=10; Solution is heated to 100 ℃, adds iron powder, the mass ratio of iron powder and graphite oxide is 2:1; React 1.5 h 100 ℃ of following stirring and refluxing, cooling separates remaining iron powder with magnet; Obtain finely dispersed Graphene dispersion liquid, place and do not have the deposition generation in one month; Graphene homodisperse liquid is through the millipore filtration vacuum filtration, and the solid product that obtains is with water washing three times, 60 ℃ of vacuum-dryings.
Embodiment 11
Take by weighing the graphite oxide for preparing with the Hummers method and disperse in deionized water for ultrasonic, be configured to the dispersion liquid of 0.2 g/L concentration, the use massfraction is 28% ammoniacal liquor regulator solution pH=10; Solution is heated to 100 ℃, adds iron powder, the mass ratio of iron powder and graphite oxide is 2:1; React 1.5 h 100 ℃ of following stirring and refluxing, cooling separates remaining iron powder with magnet; Obtain finely dispersed Graphene dispersion liquid, place and do not have the deposition generation in one month; Graphene homodisperse liquid is through the millipore filtration vacuum filtration, and the solid product that obtains is with water washing three times, 60 ℃ of vacuum-dryings.
Embodiment 12
Take by weighing the graphite oxide for preparing with the Hummers method and disperse in deionized water for ultrasonic, be configured to the dispersion liquid of 1.0 g/L concentration, the use massfraction is 28% ammoniacal liquor regulator solution pH=10; Solution is heated to 100 ℃, adds iron powder, the mass ratio of iron powder and graphite oxide is 2:1; React 1.5 h 100 ℃ of following stirring and refluxing, cooling separates remaining iron powder with magnet; Obtain finely dispersed Graphene dispersion liquid, place and do not have the deposition generation in one month; Graphene homodisperse liquid is through the millipore filtration vacuum filtration, and the solid product that obtains is with water washing three times, 60 ℃ of vacuum-dryings.
Embodiment 13
Take by weighing the graphite oxide for preparing with the Hummers method and disperse in deionized water for ultrasonic, be configured to the dispersion liquid of 0.5 g/L concentration, the use massfraction is 28% ammoniacal liquor regulator solution pH=10; Solution is heated to 100 ℃, adds iron powder, the mass ratio of iron powder and graphite oxide is 1:2; React 1.5 h 100 ℃ of following stirring and refluxing, cooling separates remaining iron powder with magnet; Obtain finely dispersed Graphene dispersion liquid, place and do not have the deposition generation in one month; Graphene homodisperse liquid is through the millipore filtration vacuum filtration, and the solid product that obtains is with water washing three times, 60 ℃ of vacuum-dryings.
Embodiment 14
Take by weighing the graphite oxide for preparing with the Hummers method and disperse in deionized water for ultrasonic, be configured to the dispersion liquid of 0.2 g/L concentration, the use massfraction is 28% ammoniacal liquor regulator solution pH=10; Solution is heated to 100 ℃, adds iron powder, the mass ratio of iron powder and graphite oxide is 1:2; React 1.5 h 100 ℃ of following stirring and refluxing, cooling separates remaining iron powder with magnet; Obtain finely dispersed Graphene dispersion liquid, place and do not have the deposition generation in one month; Graphene homodisperse liquid is through the millipore filtration vacuum filtration, and the solid product that obtains is with water washing three times, 60 ℃ of vacuum-dryings.
Embodiment 15
Take by weighing the graphite oxide for preparing with the Hummers method and disperse in deionized water for ultrasonic, be configured to the dispersion liquid of 1.0 g/L concentration, the use massfraction is 28% ammoniacal liquor regulator solution pH=10; Solution is heated to 100 ℃, adds iron powder, the mass ratio of iron powder and graphite oxide is 1:2; React 1.5 h 100 ℃ of following stirring and refluxing, cooling separates remaining iron powder with magnet; Obtain finely dispersed Graphene dispersion liquid, place and do not have the deposition generation in one month; Graphene homodisperse liquid is through the millipore filtration vacuum filtration, and the solid product that obtains is with water washing three times, 60 ℃ of vacuum-dryings.
Embodiment 16
Take by weighing the graphite oxide for preparing with the Hummers method and disperse in deionized water for ultrasonic, be configured to the dispersion liquid of 0.5 g/L concentration, the use massfraction is 28% ammoniacal liquor regulator solution pH=10; Solution is heated to 100 ℃, adds iron powder, the mass ratio of iron powder and graphite oxide is 1:1; React 1.5 h 100 ℃ of following stirring and refluxing, cooling separates remaining iron powder with magnet; Obtain finely dispersed Graphene dispersion liquid, place and do not have the deposition generation in one month; Graphene homodisperse liquid is through the millipore filtration vacuum filtration, and the solid product that obtains is with water washing three times, 60 ℃ of vacuum-dryings.
Embodiment 17
Take by weighing the graphite oxide for preparing with the Hummers method and disperse in deionized water for ultrasonic, be configured to the dispersion liquid of 0.2 g/L concentration, the use massfraction is 28% ammoniacal liquor regulator solution pH=10; Solution is heated to 100 ℃, adds iron powder, the mass ratio of iron powder and graphite oxide is 1:1; React 1.5 h 100 ℃ of following stirring and refluxing, cooling separates remaining iron powder with magnet; Obtain finely dispersed Graphene dispersion liquid, place and do not have the deposition generation in one month; Graphene homodisperse liquid is through the millipore filtration vacuum filtration, and the solid product that obtains is with water washing three times, 60 ℃ of vacuum-dryings.
Embodiment 18
Take by weighing the graphite oxide for preparing with the Hummers method and disperse in deionized water for ultrasonic, be configured to the dispersion liquid of 1.0 g/L concentration, the use massfraction is 28% ammoniacal liquor regulator solution pH=10; Solution is heated to 100 ℃, adds iron powder, the mass ratio of iron powder and graphite oxide is 1:1; React 1.5 h 100 ℃ of following stirring and refluxing, cooling separates remaining iron powder with magnet; Obtain finely dispersed Graphene dispersion liquid, place and do not have the deposition generation in one month; Graphene homodisperse liquid is through the millipore filtration vacuum filtration, and the solid product that obtains is with water washing three times, 60 ℃ of vacuum-dryings.

Claims (3)

1. method for preparing hydrophilic graphene is characterized in that:, specifically may further comprise the steps as reductive agent with iron powder:
1) with the natural flake graphite is raw material, its oxidation obtained graphite oxide with the Hummers method;
2) graphite oxide is disperseed in deionized water for ultrasonic, form the graphene oxide dispersion liquid, the concentration of graphene oxide does
0.2~1.0?g/L;
3) regulate pH value to 10 ~ 10.5 of graphene oxide dispersion liquid with ammoniacal liquor;
4) the graphene oxide dispersion liquid is heated to 100 ℃, adds iron powder, the mass ratio of iron powder and graphite oxide is in the scope of 0.5~2:1, at 100 ℃ of 1 ~ 1.5 h that reflux;
5) after the cooling, separate remaining iron powder, obtain black Graphene homodisperse liquid with magnet;
6) with Graphene homodisperse liquid through the millipore filtration vacuum filtration, and the solid product that obtains washed and dry.
2. a kind of according to claim 1 method for preparing hydrophilic graphene is characterized in that: what the Graphene of preparation was stable is dispersed in the water, forms stable colloidal dispersion.
3. a kind of according to claim 1 method for preparing hydrophilic graphene is characterized in that: the massfraction of ammoniacal liquor is 28%.
CN2010105235715A 2010-10-29 2010-10-29 Method for preparing hydrophilic graphene Expired - Fee Related CN101993064B (en)

Priority Applications (1)

Application Number Priority Date Filing Date Title
CN2010105235715A CN101993064B (en) 2010-10-29 2010-10-29 Method for preparing hydrophilic graphene

Applications Claiming Priority (1)

Application Number Priority Date Filing Date Title
CN2010105235715A CN101993064B (en) 2010-10-29 2010-10-29 Method for preparing hydrophilic graphene

Publications (2)

Publication Number Publication Date
CN101993064A CN101993064A (en) 2011-03-30
CN101993064B true CN101993064B (en) 2012-11-07

Family

ID=43783902

Family Applications (1)

Application Number Title Priority Date Filing Date
CN2010105235715A Expired - Fee Related CN101993064B (en) 2010-10-29 2010-10-29 Method for preparing hydrophilic graphene

Country Status (1)

Country Link
CN (1) CN101993064B (en)

Cited By (1)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN103030170A (en) * 2013-01-16 2013-04-10 哈尔滨工业大学 Preparation method for cuprous oxide/reduced graphene oxide composite functional material

Families Citing this family (13)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN102219210B (en) * 2011-04-11 2012-12-05 复旦大学 Chemical method for preparing graphene
CN102259850A (en) * 2011-06-20 2011-11-30 江苏大学 Method for oxidizing graphene
CN102332573B (en) * 2011-06-24 2014-04-09 福州大学 One-dimensional core-shell structure material for lithium ion battery, and preparation method of one-dimensional core-shell structure material
CN102431997B (en) * 2011-09-07 2013-05-08 南京师范大学 Graphene oxide with antibacterial and anticoagulant functions and preparation method thereof
CN103578771A (en) * 2012-07-18 2014-02-12 海洋王照明科技股份有限公司 Graphene thin film and preparation method and application thereof
CN104769755B (en) * 2012-09-29 2018-02-06 华东理工大学 For manufacturing the method and composition of metal oxide graphene complex
CN103072976B (en) * 2012-12-28 2015-01-14 同济大学 Transfer method of graphene or oxidized graphene thin film
US10002720B2 (en) 2013-03-05 2018-06-19 East China University Of Science And Technology Preparation of metal oxide-graphene composite films
CN103240007A (en) * 2013-05-13 2013-08-14 嵇天浩 Method for preparing graphene-oxide-filled microfiltration composite material
CN103871753B (en) * 2014-02-26 2016-09-14 江苏昊华精细化工有限公司 The preparation method of hydrophilic graphene thin film
CN106145097B (en) * 2016-06-13 2018-07-27 南京工业大学 A kind of preparation method for the redox graphene that hydrophilic and hydrophobic is controllable
CN106957053A (en) * 2017-04-13 2017-07-18 山东玉皇新能源科技有限公司 A kind of iron powder is the method for the quick macroscopic preparation of graphene of reducing agent
CN110844964B (en) * 2018-12-07 2020-11-10 中国环境科学研究院 Application of green modified carbon nano material in adsorption of organic pollutants in water

Citations (4)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
US20090068740A1 (en) * 2004-07-30 2009-03-12 The Brigham And Women's Hospital, Inc. Amorphous cell delivery vehicle treated with physical/physicochemical stimuli
WO2009143405A2 (en) * 2008-05-22 2009-11-26 The University Of North Carolina At Chapel Hill Synthesis of graphene sheets and nanoparticle composites comprising same
CN101691204A (en) * 2009-08-13 2010-04-07 苏州纳米技术与纳米仿生研究所 Stable nano graphene oxide under physiological condition and preparation method thereof
CN101844762A (en) * 2010-05-28 2010-09-29 江苏大学 Method for preparing hydrophilic graphene

Patent Citations (4)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
US20090068740A1 (en) * 2004-07-30 2009-03-12 The Brigham And Women's Hospital, Inc. Amorphous cell delivery vehicle treated with physical/physicochemical stimuli
WO2009143405A2 (en) * 2008-05-22 2009-11-26 The University Of North Carolina At Chapel Hill Synthesis of graphene sheets and nanoparticle composites comprising same
CN101691204A (en) * 2009-08-13 2010-04-07 苏州纳米技术与纳米仿生研究所 Stable nano graphene oxide under physiological condition and preparation method thereof
CN101844762A (en) * 2010-05-28 2010-09-29 江苏大学 Method for preparing hydrophilic graphene

Non-Patent Citations (1)

* Cited by examiner, † Cited by third party
Title
马文石等.石墨烯的制备与表征.《高校化学工程学报》.2010,第24卷(第4期),第719-722页. *

Cited By (1)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN103030170A (en) * 2013-01-16 2013-04-10 哈尔滨工业大学 Preparation method for cuprous oxide/reduced graphene oxide composite functional material

Also Published As

Publication number Publication date
CN101993064A (en) 2011-03-30

Similar Documents

Publication Publication Date Title
CN101993064B (en) Method for preparing hydrophilic graphene
CN106449169B (en) A kind of preparation method of graphene-based composite material
CN103950923B (en) A kind of novel method preparing high-quality Graphene
CN105271217B (en) A kind of preparation method of the three-dimensional grapheme of N doping
CN105932252B (en) A kind of sulphur selenizing molybdenum/carbon nano tube compound material and its preparation and application
CN102659099B (en) Preparation method of anisotropic graphene foam
CN102694171B (en) Hydrothermal preparation method for composite material of single-layer WS2 and graphene
CN101602504B (en) Preparation method of graphene based on ascorbic acid
CN104556018B (en) A kind of preparation method of high-quality graphene conductive film
CN102689896B (en) Method for preparing nitrogen doping functionalized oxide graphene simultaneously performing reduction
CN105126876B (en) A kind of flower-shaped carbon load MoS2Composite of nano particle and preparation method thereof
WO2015184816A1 (en) Nitrogen-doped graphene sheet and method for preparation and use thereof
CN108565434B (en) Preparation method of tungsten disulfide/nitrogen and sulfur co-doped graphene compound
CN103787288B (en) A kind of preparation method of boron nitride alkene nanometer sheet
CN105322147B (en) A kind of tungsten disulfide/carbon nano-fiber/graphene composite material and preparation method thereof
CN101844762B (en) Method for preparing hydrophilic graphene
CN103626167B (en) A kind of preparation method of Graphene
CN105280900A (en) Tungsten disulfide/graphene nanobelt composite material and preparation method thereof
CN104174422A (en) High nitrogen doped graphene and fullerene-like molybdenum selenide hollow-ball nanocomposite and preparation method thereof
CN106587019A (en) Preparation method for lignin-based biological carbon/graphene composite nanometer material
CN103408003B (en) Method for preparing graphene
CN104150469A (en) Method capable of preparing few-layer graphene powder in batches
CN102502610A (en) Simple method for preparing a large amount of graphene
CN102694172B (en) Preparation method of composite nano material of single-layer WS2 and graphene
CN104998630A (en) Titanium dioxide/graphene nanocomposite, and normal-temperature preparation method and application thereof

Legal Events

Date Code Title Description
C06 Publication
PB01 Publication
C10 Entry into substantive examination
SE01 Entry into force of request for substantive examination
C14 Grant of patent or utility model
GR01 Patent grant
CF01 Termination of patent right due to non-payment of annual fee

Granted publication date: 20121107

Termination date: 20151029

EXPY Termination of patent right or utility model