CN101948107A - Method for preparing and purifying graphene by microwave radiation under vacuum - Google Patents
Method for preparing and purifying graphene by microwave radiation under vacuum Download PDFInfo
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- CN101948107A CN101948107A CN 201010281619 CN201010281619A CN101948107A CN 101948107 A CN101948107 A CN 101948107A CN 201010281619 CN201010281619 CN 201010281619 CN 201010281619 A CN201010281619 A CN 201010281619A CN 101948107 A CN101948107 A CN 101948107A
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Abstract
The invention discloses a method for preparing and purifying graphene by microwave radiation under vacuum. The method for preparing graphene is as follows: placing graphite oxide in a reactor, radiating the graphite oxide by microwaves under vacuum, and obtaining the graphene by heating and cleavage of the graphite oxide. The method for purifying graphene is as follows: placing graphene with low purity in a reactor, irradiating the graphite oxide by microwaves under vacuum, and obtaining the graphene with higher purity after impure graphene is subjected to heating and cleavage. The method is implemented under the vacuum condition, thus being favor to preventing the generated graphene from being oxidized by oxygen in the reactor, reducing the cleavage resistance of the graphite oxide, and ensuring the safety in the operation process, and the method also has the advantages of high production efficiency, low production cost, safe operation process, high product purity and the like, and can be used as one of the methods for preparing and purifying graphene massively.
Description
Technical field
The present invention relates to the method for preparation of microwave radiation under the vacuum and purifying Graphene, belong to the preparation and the purification technique of material.
Background technology
Graphene is a kind of two-dimentional carbon atom crystal of finding in 2004, is the carbon material as thin as a wafer of single or multiple lift.That day from finding, just become one of the research focus in fields such as carbon material, nanotechnology, Condensed Matter Physics and functional materials.
At present, the main preparation methods of Graphene has the chemical cleavage and the method for reducing of mechanical split the law, epitaxial crystal growth method, chemical Vapor deposition process, graphite oxide.Also have some other preparation method also to be developed successively, as gas phase plasma-grown technology, electrostatic deposition and high temperature and high pressure synthesis etc.Employing low-temperature negative-pressures such as Yang Quanhong chemistry cleavage method has realized the low-cost magnanimity preparation of Graphene, and negative pressure can guarantee that not only the required temperature of cleavage is lower, and can prevent that Graphene is oxidized.Utilize this method to obtain having the grapheme material of good nanostructure and energy storage character, thereby for the industrialization of Graphene and at energy storage Application for Field [the Wei Lv that lays a solid foundation, Dai-Ming Tang, Yan-Bing He et al.ACSNano, 2009,3 (11): 3730-3736. Yang Quan is red, Lv Wei, Sun Hui, high electrochemistry capacitance oxidization plumbago alkene and low temperature preparation method thereof and application, CN 200810151807.X].Microwave radiation also is used in the preparation process of Graphene, microwave irradiation in microwave radiation plasma enhanced chemical vapor deposition method, microwave radiation chemical Vapor deposition process, liquid phase microwave irradiation and the air atmosphere, these methods all have been used to synthesizing graphite alkene, and microwave irradiation has developed into a kind of important method for preparing Graphene.These two kinds of methods of microwave radiation plasma enhanced chemical vapor deposition method and microwave radiation chemical Vapor deposition process are to utilize the chemical vapour deposition Graphene of microwave-assisted, these two kinds of methods all need special equipment and operator to operate, equipment and production cost height, and complicated operation, yield poorly, be not easy to realize suitability for industrialized production.The liquid phase microwave irradiation is to utilize the graphite in the microwave radiation liquid phase medium to prepare Graphene, this method complicated operation, the Graphene of generation are assembled in drying process easily, and yield is less than 10%, owing in encloses container, operate, in preparation process, blast easily simultaneously.The method that also has the microwave radiation graphite oxide in air atmosphere, though this method productive rate height, but because Graphene can contact with airborne oxygen in the preparation process, again be oxidized easily, purity to Graphene is influential, for airtight container, emit a large amount of gas during the graphite oxide cleavage and also set off an explosion easily simultaneously.These problems are all restricting the industrialization development that microwave irradiation prepares Graphene.
Purified Graphene is a kind of simple substance of carbon, wherein except carbon, does not contain other elements.In preparation method of graphene, the chemical reduction or the cleavage that with the graphite oxide are raw material are a kind of methods of important magnanimity preparation, the Graphene of this method preparation can since cleavage or reduction not exclusively, its surface or edge still can contain oxy radical, carboxyl for example, epoxy group(ing) and hydroxyl etc.These oxy radicals cause defective on the two-dirnentional structure of Graphene, and these defectives all can impact character such as the electricity of Graphene and mechanics.Also there is not at present document or patent report solution about this major issue of purifying of Graphene.
Summary of the invention
The object of the present invention is to provide a kind of under vacuum the method for microwave radiation preparation and purifying Graphene.This method has the production efficiency height, and production cost is low, safe operation process, and the product purity advantages of higher can be used as one of method of magnanimity preparation and purifying Graphene.
The present invention is realized by following technical proposals, microwave radiation prepares the method for Graphene under a kind of vacuum, it is characterized in that comprising following process: graphite oxide is placed reactor, form under 0.01Pa～10kPa pressure, the employing frequency is 300MHz～300GHz, power is that the microwave of 50W～2000W carries out radiation 2s～600s to graphite oxide, and the graphite oxide cleavage of being heated obtains Graphene.
The method of microwave radiation purifying Graphene under a kind of vacuum, it is characterized in that comprising following process, oxygen element atomic ratio content is higher than 10% Graphene and places reactor, form under 0.01Pa～10kPa pressure, the employing frequency is 300MHz～300GHz, power is that the microwave of 50W～2000W carries out radiation 2s～600s to graphite oxide, and the impure Graphene cleavage of being heated obtains oxygen element atomic ratio content and is lower than 10% Graphene.
Present method is produced or the Graphene of purifying has following feature and advantage:
Utilize Graphene that vacuum condition helps preventing to generate by the dioxygen oxidation in the reactor, the condition of vacuum can reduce the dissociated resistance of graphite oxide simultaneously, the thickness of the Graphene of present method preparation is within 0.34nm～20nm, oxygen element atomic ratio content is lower than 10%, and specific surface area is at 400～2630m
2In/g the scope; For the Graphene of additive method preparation, also can utilize present method purifying simultaneously, utilize the Graphene oxygen element atomic ratio content of present method purifying to be lower than 10%, specific surface area is greater than 400m
2/ g, present method has proposed the purification process of Graphene under vacuum and the microwave radiation first, and is a kind of method for preparing high-quality Graphene; Volume expands rapidly and has caused potential safety hazard in the chemical cleavage process of graphite oxide, and present method keeps by utilizing vacuum pump constantly to take out the body that degass that the method for negative pressure has solved this problem in the reactor, is a kind of safe method; The elapsed time of present method is short, and the shortest needs 2s, and the production efficiency height is a kind of high-efficiency method; This method energy expenditure is little, and microwave irradiation power is little, and radiated time is short, and production cost is low, is a kind of low cost method; This method can be used for the suitability for industrialized production that magnanimity prepares Graphene, under vacuum condition, microwave radiation can make the raw material cleavage of being heated uniformly, and the vacuum microwave equipment and technology is comparative maturity, present method is a kind of magnanimity preparation, method of suitability for industrialized production of being easy to.
Embodiment
Embodiment 1
Sulfuric acid uniform mixing with 2g Graphite Powder 99 and 1g SODIUMNITRATE and 46mL mass concentration 98% stirs under the ice-water bath condition, slowly adds 6g potassium permanganate, and reaction 2h is transferred to it 35 ℃ of waters bath with thermostatic control then, reaction 30min.After dropwise adding the 92mL deionized water, temperature is risen to 98 ℃ continue reaction 3h, from water-bath, take out, further add the deionized water dilution, and handle the oxidizing substance in the reducing solution with 20mL mass concentration 30% superoxol.With the impurity in 5% the salt acid elution solvent soln, centrifuging is while hot also used the deionized water wash filter cake repeatedly, to washings pH value greater than 5,70 ℃ of vacuum-drying 48h, obtain graphite oxide.
Get the graphite oxide 2g that the step makes, be positioned in the reactor.Utilize vacuum pump to vacuumize, when vacuum tightness reaches 2Pa, stop to vacuumize, feeding argon gas to air pressure is 0.1MPa, repeats to vacuumize logical argon gas twice again, utilizes vacuum pump to be evacuated to vacuum tightness at last and is 2Pa.With the power microwave frequency is 2450MHz, and power is 800W, microwave radiation 300s.After reaction finishes, after temperature is reduced to room temperature in the cooling question response device.Collect the Graphene sample, adopt XPS and sample is tested test result than nitrogen surface-area tester: the atomic ratio content of oxygen element is about 7% in the Graphene, and specific surface area is about 510m
2/ g.
Embodiment 2
The process of present embodiment is identical with embodiment 1 with condition, and just the power with microwave is adjusted to 1500W, and radiated time is adjusted to 100s, still can obtain the Graphene sample.Adopt XPS and sample is tested test result than nitrogen surface-area tester: the atomic ratio content of oxygen element is about 7% in the Graphene, and specific surface area is about 500m
2/ g.
Embodiment 3
Press the preparation method of embodiment 1, just the power with microwave is adjusted to 2000W, and radiated time is adjusted to 2s, and other reaction conditions is constant, can obtain the Graphene sample.
Embodiment 4
Press the preparation method of embodiment 1, just the frequency with microwave is adjusted to 2000MHz, and other reaction conditions is constant, can obtain the Graphene sample.
Embodiment 5
Press the preparation method of embodiment 1, just the frequency with microwave is adjusted to 3000MHz, and other reaction conditions is constant, can obtain the Graphene sample.
Embodiment 6
Press the preparation method of embodiment 1, just the quality with graphite oxide changes 50g into, and other reaction conditions is constant, still can obtain the Graphene sample.
Embodiment 7
Method by embodiment 1 prepares graphite oxide, vacuumize after packing into dried graphite oxide in the sample hose, when vacuum tightness reaches 10kPa, begin heating, 20 ℃/min of temperature rise rate is warming up to 200 ℃, keep 2h, obtain the Graphene head product, learn that by test the atomic ratio content of its oxygen element is about 20%, specific surface area is about 200m
2/ g.The Graphene that will obtain according to above-mentioned steps is positioned in the reaction vessel, utilizes vacuum pump to vacuumize, when vacuum tightness reaches 2Pa, stop to vacuumize, feeding argon gas to air pressure is 0.1MPa, repeat to vacuumize logical argon gas twice again, utilize vacuum pump to be evacuated to vacuum tightness at last and be 2Pa.Regulating the power microwave frequency is 2450MHz, and power is 100W, and radiated time is 800s, the beginning microwave radiation.Reaction is opened cooling water valve after finishing, and after temperature is reduced to room temperature in the question response device, stops water flowing.Obtain the Graphene sample of purifying, adopt XPS and than nitrogen surface-area tester sample is tested, the atomic ratio content of its oxygen element of test shows is about 8%, and specific surface area is about 450m
2/ g.
Embodiment 8
Press the method for embodiment 7, just the power with microwave is adjusted to 2000W, and radiated time is adjusted to 2s, and other reaction conditions is constant, can obtain the Graphene sample of purifying.
Embodiment 9
Press the method for embodiment 7, just the frequency with microwave is adjusted to 2000MHz, and other reaction conditions is constant, can obtain the Graphene sample of purifying.
Embodiment 10
Press the method for embodiment 7, just the quality of the low Graphene of purity is changed into 75g, other reaction conditions is constant, still can obtain the Graphene sample of purifying.
Comparative Examples 1
Get the graphite oxide 2g that produces according to the method for embodiment 1, be positioned in the reactor.In the air atmosphere normal pressure, regulating the power microwave frequency is 2450MHz, and power is 800W, and radiated time is 300s, the beginning microwave radiation.Reaction is opened cooling water valve after finishing, and after temperature is reduced to room temperature in the question response device, stops water flowing.Collect the Graphene sample.Adopt XPS and than nitrogen surface-area tester sample is tested, the oxygen element atomic ratio content of the Graphene that obtains is about 15%, and specific surface area is about 220m
2/ g adopts the quality of the Graphene that present method produces higher by contrast as can be known.
Comparative Examples 2
Get the graphite oxide 2g that produces according to the method for embodiment 1, be positioned in the reactor.Utilize vacuum pump to vacuumize, when vacuum tightness reaches 2Pa, stop to vacuumize, feeding argon gas to air pressure is 0.1MPa, repeats to vacuumize logical argon gas twice again, and feeding argon gas to air pressure at last is 0.1MPa.Regulating the power microwave frequency is 2450MHz, and power is 800W, and radiated time is 300s, the beginning microwave radiation.Reaction is opened cooling water valve after finishing, and after temperature is reduced to room temperature in the question response device, stops water flowing.Collect the Graphene sample.Adopt XPS and than nitrogen surface-area tester sample is tested, the atomic ratio content of its oxygen element of test shows is about 11%, and specific surface area is about 270m
2/ g.Adopt the quality of the Graphene that present method produces higher as can be known by contrast.
Claims (2)
1. microwave radiation prepares the method for Graphene under the vacuum, it is characterized in that comprising following process: graphite oxide is placed reactor, form under 0.01Pa～10kPa pressure, the employing frequency is 300MHz～300GHz, power is that the microwave of 50W～2000W carries out radiation 2s～600s to graphite oxide, and the graphite oxide cleavage of being heated obtains Graphene.
2. the method for microwave radiation purifying Graphene under the vacuum, it is characterized in that comprising following process, oxygen element atomic ratio content is higher than 10% Graphene and places reactor, form under 0.01Pa～10kPa pressure, the employing frequency is 300MHz～300GHz, power is that the microwave of 50W～2000W carries out radiation 2s～600s to graphite oxide, and the impure Graphene cleavage of being heated obtains oxygen element atomic ratio content and is lower than 10% Graphene.
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| CN102107870A (en) * | 2011-03-23 | 2011-06-29 | 中国科学院山西煤炭化学研究所 | Method for quickly preparing reduced graphene by using microwaves |
| CN102139873A (en) * | 2011-02-17 | 2011-08-03 | 无锡第六元素高科技发展有限公司 | Method for preparing graphene material by microwave irradiation in vacuum or inert gas environment |
| CN102180439A (en) * | 2011-03-31 | 2011-09-14 | 华中科技大学 | Carbon microtructure with graphene integrated on surface and preparation method thereof |
| CN102180462A (en) * | 2011-02-17 | 2011-09-14 | 无锡第六元素高科技发展有限公司 | Method for preparing modified graphene material in controlled atmosphere environment by microwave irradiation |
| CN102502611A (en) * | 2011-11-15 | 2012-06-20 | 东南大学 | Method for rapidly preparing graphene in large quantities by utilizing graphite oxides |
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| CN102602925A (en) * | 2012-04-13 | 2012-07-25 | 常州第六元素材料科技股份有限公司 | Method for preparing graphene by virtue of high-pressure reduction |
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| CN106629697A (en) * | 2016-12-27 | 2017-05-10 | 东南大学 | Preparation method of graphene particle composite material |
| CN106629680A (en) * | 2016-12-27 | 2017-05-10 | 东南大学 | Preparation method of graphene metal composite material |
| CN107381565A (en) * | 2016-05-17 | 2017-11-24 | 湖南国盛石墨科技有限公司 | A kind of purification treating method of micro crystal graphite |
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Application publication date: 20110119 |