CN102107870A - Method for quickly preparing reduced graphene by using microwaves - Google Patents
Method for quickly preparing reduced graphene by using microwaves Download PDFInfo
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- CN102107870A CN102107870A CN 201110072763 CN201110072763A CN102107870A CN 102107870 A CN102107870 A CN 102107870A CN 201110072763 CN201110072763 CN 201110072763 CN 201110072763 A CN201110072763 A CN 201110072763A CN 102107870 A CN102107870 A CN 102107870A
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- graphite
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- graphite oxide
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Abstract
The invention relates to a method for quickly preparing reduced graphene by using microwaves, which comprises the following steps: grinding graphite oxide into fine powder of which the particle size is 1-100 micrometers, and treating the graphite oxide with 100-2000W microwave radiation for 0.1-200 minutes in a vacuum degree of 0.01-10Pa or in a protective atmosphere, so that the graphite oxide quickly expands, thereby obtaining the reduced graphene. The invention has the advantages of simple preparation process and low preparation temperature, and is easy to operate.
Description
Technical field
The invention belongs to a kind of preparation method of grapheme material, relate in particular to a kind of preparation method of nanometer reduction grapheme material.
Background technology
Graphene (Graphene) is the two-dimentional carbon atom crystal of monatomic thickness, is the thinnest material that manually makes at present, it be considered to soccerballene, carbon nanotube and graphite basic structural unit (Geim, A.K. etc. nature material 6,183 (2007)).Graphene has excellent electroconductibility, thermal conductivity and mechanical property.In addition, tensile modulus of Graphene (1.01TPa) and ultimate strength (116GPa) are suitable with Single Walled Carbon Nanotube (SWCNT), its light weight is compared with carbon nanotube with the soccerballene of costliness, and Graphene has special electromagnetic property, for example, high electron mobility (σ under the room temperature
h＞15,000cm
2V
-1s
-1) (Geim, A.K. etc. nature material 6,183 (2007)), the electric conductivity (4e that can not disappear
2/ h), unusual quantum hall effect, little spin orbital interaction etc.; Graphene has high mechanical property, and be proved to be at present in the world the material of intensity maximum (tensile modulus E ≈ 1.01TPa and ultimate strength σ ≈ 130GPa) (Lee, C. etc. science 321,385 (2008).Rely on special two-dirnentional structure, high electricity/thermal conductivity, switching effect and low noise and other advantages, Graphene can be widely used in quantum devices such as single-molecule detection device, unicircuit, field-effect transistor.
Existing reduction graphene preparation method mainly is high temperature or low temperature rapid expansion method, and its main process is to be raw material with the graphite oxide, by being rapidly heated oxidized graphite flake layer is peeled off mutually under the vacuum state, obtains having the reduction Graphene of certain specific surface area.The silica tube that people such as Yang Quanhong (200810151807.X) will be equipped with graphite oxide puts into that environment stops a few hours more than 200 ℃, realizes being rapidly heated of sample, and obtaining specific surface area is 200～800m
2The graphene oxide of/g.But rate of heating is still slow, and it is also more to consume energy.But there is not microwave radiation to peel off the report of graphene oxide so far.
Summary of the invention
The objective of the invention is to overcome the shortcoming and defect in the prior art, a kind of quick method of Graphene of reducing for preparing is provided.
The present invention, the preparation method, it is characterized in that comprising following process:
It is 1～100 micron fine powder that graphite oxide is ground to form particle diameter; under vacuum tightness 0.01Pa～10Pa or atmosphere protection state, graphite oxide is carried out microwave radiation processing with 100W～2000W, 0.1～200min holds time; the graphite oxide volume expands rapidly, obtains reducing Graphene.
Described graphite oxide is synthetic by Hummers method, Brodie method, Staudenmaier method or electrochemical oxidation process, and used graphite raw material is blocky graphite, amorphous graphite (amorphous graphite), crystalline flake graphite, high crystalline graphite or synthetic graphite in building-up process.
Described atmosphere is nitrogen or argon gas.
The present invention utilizes microwave irradiation to add hot preparation reduction-oxidation graphite.This reduction Graphene thickness is 0.3～20nm, and specific surface area is 300～1500m
2/ g.
The present invention has following advantage: preparation process is simpler, and preparation temperature is low, and easy handling, and energy expenditure is lower, and made reduction Graphene specific surface area can reach 300～1500m
2/ g, reduction Graphene thickness is 0.3～20nm.This material has good electrochemical energy.Its preparation process is simple, and application prospect is extensive.
Description of drawings
Fig. 1 is the high resolution transmission electron microscopy photo of the embodiment of the invention 1 reduction Graphene.
Embodiment
The present invention is described in detail below in conjunction with drawings and Examples:
Embodiment 1 is a raw material with the crystalline flake graphite, adopts the Hummers legal system to be equipped with graphite oxide.In ice bath, the vitriol oil of 10g Graphite Powder 99 and 5g SODIUMNITRATE and 230mL is mixed, slowly add 30gKMnO in the stirring
4It is transferred to 35 ℃ of water-bath 30min.Progressively add the 460mL deionized water, temperature rises to 98 ℃ and continues reaction 40min, and mixture becomes glassy yellow by brown.Further thin up, and with the H of massfraction 30%
2O
2Solution-treated, the unreacted permanganic acid that neutralizes, centrifuging and repetitive scrubbing filter cake then with its vacuum-drying, promptly obtain graphite oxide.
It is 1～80 micron fine powder that the graphite oxide of making is ground to form particle diameter, and the graphite oxide after pulverizing is packed in the microwave radiation device, begins to vacuumize, and vacuum tightness is 10Pa, the beginning carry out microwave radiation heating.Microwave power 800W, the 1min that holds time obtains reducing Graphene.Utilize the specific surface area of nitrogen adsorption assay gained reduction Graphene, adsorption temp is liquid nitrogen temperature (77K), and the specific surface area that records is 450m
2/ g.This reduction graphene film thickness is 0.3～15nm
Embodiment 2 is a raw material with high crystalline graphite, adopts the Hummers legal system to be equipped with graphite oxide.In ice bath, the vitriol oil of 1g Graphite Powder 99 and 0.5g SODIUMNITRATE and 23mL is mixed, slowly add 3g KMnO in the stirring
4It is transferred to 35 ℃ of water-bath 30min.Progressively add the 46mL deionized water, temperature rises to 98 ℃ and continues reaction 40min, and mixture becomes glassy yellow by brown.Further thin up, and with the H of massfraction 30%
2O
2Solution-treated, the unreacted permanganic acid that neutralizes, centrifuging and repetitive scrubbing filter cake then with its vacuum-drying, promptly obtain graphite oxide.
It is 1～60 micron fine powder that the graphite oxide of making is ground to form particle diameter, the graphite oxide after pulverizing is packed in the microwave radiation device, and under the nitrogen atmosphere state, the beginning carry out microwave radiation heating.Electric power 300W, the 2min that holds time obtains reducing Graphene.Utilize the specific surface area of nitrogen adsorption assay gained reduction Graphene, adsorption temp is liquid nitrogen temperature (77K), and the specific surface area that records is 380m
2/ g.This reduction graphene film thickness is 0.3～18nm
Embodiment 3 is that raw material is a raw material with the crystalline flake graphite, adopts the Hummers legal system to be equipped with graphite oxide.In ice bath, the vitriol oil of 20g Graphite Powder 99 and 10g SODIUMNITRATE and 460mL is mixed, slowly add 60g KMnO in the stirring
4It is transferred to 35 ℃ of water-bath 30min.Progressively add the 920mL deionized water, temperature rises to 98 ℃ and continues reaction 40min, and mixture becomes glassy yellow by brown.Further thin up, and with the H of massfraction 30%
2O
2Solution-treated, the unreacted permanganic acid that neutralizes, centrifuging and repetitive scrubbing filter cake then with its vacuum-drying, promptly obtain graphite oxide.
It is 20～60 microns fine powder that the graphite oxide of making is ground to form particle diameter, the graphite oxide after pulverizing is packed in the microwave radiation device, and under the carbon dioxide atmosphere state, the beginning carry out microwave radiation heating.Electric power 2000W, the 10min that holds time obtains reducing Graphene.Utilize the specific surface area of nitrogen adsorption assay gained reduction Graphene, adsorption temp is liquid nitrogen temperature (77K), and the specific surface area that records is 545m
2/ g, this reduction graphene film thickness is 0.3～15nm
Embodiment 4 is a raw material with the blocky graphite, adopts the Hummers legal system to be equipped with graphite oxide.In ice bath, the vitriol oil of 5g Graphite Powder 99 and 2.5g SODIUMNITRATE and 125mL is mixed, slowly add 15gKMnO in the stirring
4It is transferred to 35 ℃ of water-bath 30min.Progressively add the 230mL deionized water, temperature rises to 98 ℃ and continues reaction 40min, and mixture becomes glassy yellow by brown.Further thin up, and with the H of massfraction 30%
2O
2Solution-treated, the unreacted permanganic acid that neutralizes, centrifuging and the vacuum-drying of repetitive scrubbing filter cake promptly obtain graphite oxide.
It is 50～80 microns fine powder that the graphite oxide of making is ground to form particle diameter, and the graphite oxide after pulverizing is packed in the microwave radiation device, begins to vacuumize, and vacuum tightness is 5Pa, the beginning carry out microwave radiation heating.Microwave power 1300W, the 5min that holds time obtains reducing Graphene.Utilize the specific surface area of nitrogen adsorption assay gained reduction Graphene, adsorption temp is liquid nitrogen temperature (77K), and the specific surface area that records is 985m
2/ g.This reduction graphene film thickness is 0.3～10nm
Embodiment 5 is a raw material with the amorphous graphite, adopts the Hummers legal system to be equipped with graphite oxide.In ice bath, the vitriol oil of 10g Graphite Powder 99 and 5g SODIUMNITRATE and 230mL is mixed, slowly add 30gKMnO in the stirring
4It is transferred to 35 ℃ of water-bath 30min.Progressively add the 460mL deionized water, temperature rises to 98 ℃ and continues reaction 40min, and mixture becomes glassy yellow by brown.Further thin up, and with the H of massfraction 30%
2O
2Solution-treated, the unreacted permanganic acid that neutralizes, centrifuging and repetitive scrubbing filter cake then with its vacuum-drying, promptly obtain graphite oxide.
It is 60～100 microns fine powder that the graphite oxide of making is ground to form particle diameter, and the graphite oxide after pulverizing is packed in the microwave radiation device, begins to vacuumize, and vacuum tightness is 3Pa, the beginning carry out microwave radiation heating.Electric power 1500W, the 20min that holds time obtains reducing Graphene.Utilize the specific surface area of nitrogen adsorption assay gained reduction Graphene, adsorption temp is liquid nitrogen temperature (77K), and the specific surface area that records is 1125m
2/ g.This reduction graphene film thickness is 0.3～0.8nm
Embodiment 6 is a raw material with the amorphous graphite, adopts the Staudenmaier legal system to be equipped with graphite oxide.It is 1～30 micron fine powder that the graphite oxide of making is ground to form particle diameter, and the graphite oxide after pulverizing is packed in the microwave radiation device, begins to vacuumize, and vacuum tightness is 1Pa, the beginning carry out microwave radiation heating.Electric power 1400W, the 60min that holds time obtains reducing Graphene.Utilize the specific surface area of nitrogen adsorption assay gained reduction Graphene, adsorption temp is liquid nitrogen temperature (77K), and the specific surface area that records is 1200m
2/ g.This reduction graphene film thickness is 0.3～0.7nm
Embodiment 7 is a raw material with the amorphous graphite, adopts the Brodie legal system to be equipped with graphite oxide.It is 1～50 micron fine powder that the graphite oxide of making is ground to form particle diameter, and the graphite oxide after pulverizing is packed in the microwave radiation device, begins to vacuumize, and vacuum tightness is 0.1Pa, the beginning carry out microwave radiation heating.Electric power 1800W, the 60min that holds time obtains reducing Graphene.Utilize the specific surface area of nitrogen adsorption assay gained reduction Graphene, adsorption temp is liquid nitrogen temperature (77K), and the specific surface area that records is 1200m
2/ g.This reduction graphene film thickness is 0.3～0.7nm.
Claims (5)
1. a method of utilizing microwave to prepare fast to reduce Graphene is characterized in that comprising the steps:
It is 1～100 micron fine powder that graphite oxide is ground to form particle diameter; under vacuum tightness 0.01Pa～10Pa or atmosphere protection state, graphite oxide is carried out microwave radiation processing with 100W～2000W, 0.1～200min holds time; the graphite oxide volume expands rapidly, obtains reducing Graphene.
2. a kind of method of utilizing microwave to prepare fast to reduce Graphene as claimed in claim 1 is characterized in that described graphite oxide is synthetic by Hummers method, Brodie method, Staudenmaier method or electrochemical oxidation process.
3. a kind of method of utilizing microwave to prepare fast to reduce Graphene as claimed in claim 2, it is characterized in that described in Hummers method, Brodie method, Staudenmaier method or electrochemical oxidation process building-up process used graphite raw material be blocky graphite, amorphous graphite, crystalline flake graphite, high crystalline graphite or synthetic graphite.
4. a kind of method of utilizing microwave to prepare fast to reduce Graphene as claimed in claim 1 is characterized in that described atmosphere is nitrogen or argon gas.
5. a kind of method of utilizing microwave to prepare fast to reduce Graphene as claimed in claim 1, the thickness that it is characterized in that described reduction Graphene is 0.3～20nm, specific surface area is 300～1500m
2/ g.
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| CN102502611A (en) * | 2011-11-15 | 2012-06-20 | 东南大学 | Method for rapidly preparing graphene in large quantities by utilizing graphite oxides |
| CN102557020A (en) * | 2011-12-31 | 2012-07-11 | 上海大学 | Simple method for preparing high-quality graphene with stable solution |
| CN102583328A (en) * | 2012-01-12 | 2012-07-18 | 常州第六元素材料科技股份有限公司 | Technique for preparing graphene oxide through microwave expansion |
| CN102603014A (en) * | 2011-10-08 | 2012-07-25 | 北京中科微纳物联网技术股份有限公司 | Environment-friendly and efficient method for preparing iron sesquioxide/graphene composite material |
| 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 |
| CN102976315A (en) * | 2012-12-10 | 2013-03-20 | 西北工业大学 | Microwave-assisted method for preparing graphene through reduction of sodium citrate |
| CN103359715A (en) * | 2012-03-31 | 2013-10-23 | 海洋王照明科技股份有限公司 | Preparation method of graphite oxide |
| CN103833013A (en) * | 2012-11-23 | 2014-06-04 | 海洋王照明科技股份有限公司 | Graphene and preparation method thereof |
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| CN109231190A (en) * | 2018-11-02 | 2019-01-18 | 重庆大学 | Prepare redox graphene method and its redox graphene obtained |
| CN109292761A (en) * | 2018-12-07 | 2019-02-01 | 四川聚创石墨烯科技有限公司 | A kind of method of smooth microwave reduction graphene oxide |
| CN109292761B (en) * | 2018-12-07 | 2021-05-04 | 四川聚创石墨烯科技有限公司 | Method for reducing graphene oxide by optical microwave |
| CN110342501A (en) * | 2019-08-28 | 2019-10-18 | 徐州宇帆机电科技有限公司 | A kind of method that pulsed high energy microwave quickly restores preparation high quality reduced graphene |
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Application publication date: 20110629 |