CN103255670A - Method for preparing graphene paper through utilizing electric field guidance - Google Patents
Method for preparing graphene paper through utilizing electric field guidance Download PDFInfo
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- CN103255670A CN103255670A CN2012100382562A CN201210038256A CN103255670A CN 103255670 A CN103255670 A CN 103255670A CN 2012100382562 A CN2012100382562 A CN 2012100382562A CN 201210038256 A CN201210038256 A CN 201210038256A CN 103255670 A CN103255670 A CN 103255670A
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Abstract
The invention provides a method for preparing graphene paper through utilizing electric field guidance. The method comprises the following steps: taking chloride intercalated graphite, adding deionized water, stirring to prepare an intercalated graphite suspension, peeling the intercalated graphite through utilizing supersonic waves to prepare a graphene-containing solution, dumping the intercalated graphite into a filter funnel, placing the filter funnel in a uniform electric field having an electric field intensity of 50-200V/m for the deposition of graphene in the graphene-containing solution, filtering after the basic deposition of graphene, and drying filter paper containing the obtained filter to prepare the graphene paper. The method has the advantages of simple equipment, easy and feasible operation, easy realization of the automatic and industrialized production, and ordered arrangement of graphene in the process; and the graphene paper prepared in the invention has the advantages of good mechanical properties, and realization of thickness control through the amount of the intercalated graphite, and has a higher conductivity than graphene paper prepared through a common oxidation reduction method.
Description
Technical field
The present invention relates to the synthetic field of new material, particularly relate to the method for utilizing electric field leading to prepare Graphene paper.
Background technology
Intercalated graphite just by extensively and profoundly its performance of research and application, possesses some particular performances again because it has kept the good performance of graphite after being found in 1841, can be used for fields such as conductor, superconductor, battery.
Graphene is a kind of two-dimentional carbon atom crystal that the strong K of the peace moral of Univ Manchester UK in 2004 sea nurse (Andre K.Geim) waits discovery, is the material with carbon element as thin as a wafer of single or multiple lift.Because its particular structure and photoelectric property make it become the research focus in fields such as material with carbon element, nanometer technology, Condensed Matter Physics and functional material, have attracted many scientific workers.Single-layer graphene has many advantageous properties, as 1. high strength, and the Young molar weight, (1,100GPa), fracture strength: (125GPa); 2. high heat conductance, (5,000W/mK); 3. high conductivity, carrier transport rate, (200,000cm
2/ V*s) etc.The Graphene paper made from Graphene is a lot of good performances also, the Graphene paper hardness of people such as Ali R.Ranjbartoreh preparation reaches the twice of carbon steel, thickness has only 3um, (the Ali R.Ranjbartoreh et al.JOURNAL OF APPLIED PHYSICS 109 of the 78MPa but tensile strength is only had an appointment, 014306,2011.), Xiaowei Yang etc. are preparation graphite oxide paper earlier, after reduction, become Graphene paper, the average elasticity modulus has only 76MPa, mechanical strength is on the low side (Xiaowei Yang.et al.Angew.Chem.Int.Ed.2011,50,7325-7328).
Summary of the invention
For addressing the above problem, the present invention aims to provide the method for utilizing electric field leading to prepare Graphene paper, can make the Graphene paper of satisfactory mechanical property by this method.
The method of utilizing electric field leading to prepare Graphene paper provided by the invention may further comprise the steps:
(1) gets the chloride intercalated graphite, add deionized water, stir and be made into the intercalated graphite turbid liquid that concentration is 5～10g/L down;
(2) the intercalated graphite turbid liquid is carried out ultrasonic wave and handle, make intercalated graphite peel off, make the solution that contains Graphene;
(3) solution that will contain Graphene is poured in the filter tunnel, and filter tunnel is placed electric-field intensity is the uniform electric field of 50～200V/m, and under the guiding of electric field force and charge interaction power, the Graphene that contains in the solution of Graphene deposits;
(4) treat that Graphene deposits substantially after, filter, the oven dry contain the filter paper of filtering thing, make Graphene paper.
Step (1) is for to make the intercalated graphite turbid liquid by the chloride intercalated graphite.Described chloride intercalated graphite can adopt common molten-salt growth method or electrochemical process to make.Preferably, chloride is selected from a kind of or its any combination in iron chloride, nickel chloride, copper chloride, cobalt chloride, potassium chloride, lead chloride and the zinc chloride.
Step (2) is peeled off intercalated graphite for utilizing ultrasonic wave, makes the solution that contains Graphene.Still may exist the intercalated graphite that part is not peeled off in the described solution that contains Graphene.Preferably, ultrasonic time is 10～15 minutes.Described ultrasonic procedure can be used the ultrasonic cleaning instrument, and the power of described ultrasonic cleaning instrument is preferably 150～400w.
Step (3) is for utilizing electric field leading deposition Graphene.Major part is peeled off out the Graphene that produces from intercalated graphite and can be piled up in the mode of " building a wall " under the guiding of electric field force and charge interaction power, deposits.
Preferably, in the step (4), also comprise the inspection step to filtrate: with containing Ag
+Solution detect filtrate, as no chlorion, then will take off and contain the filter paper of filtering thing; Otherwise, filter liquor again.More preferably, being filtered into slowly the hot water that adds 80～90 ℃ in the filter tunnel again filters.Preferably, drying condition is: dried 12～18 hours under 60 ℃ of temperature.
The method of utilizing electric field leading to prepare Graphene paper provided by the invention, equipment is simple, and the operation simple and feasible easily is automated and suitability for industrialized production, and Graphene is arranged in order in its process.The Graphene paper that makes by preparation method of the present invention has good mechanical property, and thickness can be by the advantages such as amount control of intercalated graphite, compares the electric conductivity height with the Graphene paper of common oxidation-reduction method preparation.
Description of drawings
Fig. 1 is the embodiment of the invention one prepared Graphene paper SEM figure.
The specific embodiment
The following stated is preferred embodiment of the present invention; should be pointed out that for those skilled in the art, under the prerequisite that does not break away from the principle of the invention; can also make some improvements and modifications, these improvements and modifications also are considered as protection scope of the present invention.
The invention provides the method for utilizing electric field leading to prepare Graphene paper, may further comprise the steps:
(1) gets the chloride intercalated graphite, add deionized water, stir and be made into the intercalated graphite turbid liquid that concentration is 5～10g/L down;
(2) the intercalated graphite turbid liquid is carried out ultrasonic wave and handle, make intercalated graphite peel off, make the solution that contains Graphene;
(3) solution that will contain Graphene is poured in the filter tunnel, and filter tunnel is placed electric-field intensity is the uniform electric field of 50～200V/m, and under the guiding of electric field force and charge interaction power, the Graphene that contains in the solution of Graphene deposits;
(4) treat that Graphene deposits substantially after, filter, whole taking off contains the filter paper of filter thing subsequently, dries, and is Graphene paper.
Step (1) is for to make the intercalated graphite turbid liquid by the chloride intercalated graphite.Described chloride intercalated graphite can adopt common molten-salt growth method or electrochemical process to make.Chloride is selected from a kind of or its any combination in iron chloride, nickel chloride, copper chloride, cobalt chloride, potassium chloride, lead chloride and the zinc chloride.
Step (2) is peeled off intercalated graphite for utilizing ultrasonic wave, makes the solution that contains Graphene.Still may exist the intercalated graphite that part is not peeled off in the described solution that contains Graphene.Ultrasonic time is 10～15 minutes.Described ultrasonic procedure can be used the ultrasonic cleaning instrument, and the power of described ultrasonic cleaning instrument is preferably 150～400w.
Step (3) is for utilizing electric field leading deposition Graphene.Major part is peeled off out the Graphene that produces from intercalated graphite and can be piled up in the mode of " building a wall " under the guiding of electric field force and charge interaction power, deposits.After treating that Graphene deposits substantially, filter for the first time.Can remove the intercalated graphite of not peeling off in the filter process.
Preferably, in the step (4), also comprise the inspection step to filtrate: with containing Ag
+Solution detect filtrate, as no chlorion, then will take off and contain the filter paper of filtering thing; Otherwise, filter liquor again; The described Ag that contains
+The preferred AgNO of solution
3Solution.More preferably, being filtered into slowly the hot water that adds 80～90 ℃ in the filter tunnel again filters.Drying condition is: dried 12～18 hours under 60 ℃ of temperature.
The method of utilizing electric field leading to prepare Graphene paper provided by the invention, equipment is simple, and the operation simple and feasible easily is automated and suitability for industrialized production, and Graphene is arranged in order in its process.The Graphene paper that makes by preparation method of the present invention has good mechanical property, and thickness can be by the advantages such as amount control of intercalated graphite, compares the electric conductivity height with the Graphene paper of common oxidation-reduction method preparation.
Embodiment one
Utilize electric field leading to prepare the method for Graphene paper, may further comprise the steps:
(1) gets 10g iron chloride intercalated graphite and join in the beaker, add the 1L deionized water then, stir and be made into the intercalated graphite turbid liquid that concentration is 10g/L down;
(2) the intercalated graphite turbid liquid is carried out ultrasonic wave and handle, used the ultrasonic cleaning instrument ultrasonic 10 minutes, the power of ultrasonic cleaning instrument is preferably 150w, makes intercalated graphite peel off, and makes the solution that contains Graphene;
(3) solution that will contain Graphene is poured in the filter tunnel, and filter tunnel is placed electric-field intensity is the uniform electric field of 200V/m, and under the guiding of electric field force and charge interaction power, the Graphene that contains in the solution of Graphene deposits;
(4) treat that Graphene deposits substantially after, directly filter, finish direct filtration after, slowly the hot water of 90 ℃ of addings filters again in the filter tunnel, to using AgNO
3After detection filtrate does not have chlorion, again the filter paper integral body of filtering thing containing in the filter tunnel is taken off, dried 18 hours down at 60 ℃, make Graphene paper.
Fig. 1 is the embodiment of the invention one prepared Graphene paper SEM figure.As can be seen from Figure 1, the Graphene paper that makes is stepped construction, and the similar mode with " building a wall " of this structure is piled up.
Through the thin film mechanical performance tester test of U.S. CE TR company, the tensile strength test data of the Graphene paper that present embodiment makes is 623MPa.
Embodiment two
Utilize electric field leading to prepare the method for Graphene paper, may further comprise the steps:
(1) gets 5g cobalt chloride intercalated graphite and join in the beaker, add the 1L deionized water then, stir and be made into the intercalated graphite turbid liquid that concentration is 5g/L down;
(2) the intercalated graphite turbid liquid is carried out ultrasonic wave and handle, used the ultrasonic cleaning instrument ultrasonic 15 minutes, the power of ultrasonic cleaning instrument is preferably 400w, makes intercalated graphite peel off, and makes the solution that contains Graphene;
(3) solution that will contain Graphene is poured in the filter tunnel, and filter tunnel is placed electric-field intensity is the uniform electric field of 50V/m, and under the guiding of electric field force and charge interaction power, the Graphene that contains in the solution of Graphene deposits;
(4) treat that Graphene deposits substantially after, directly filter, finish direct filtration after, slowly the hot water of 80 ℃ of addings filters again in the filter tunnel, to using AgNO
3After detection filtrate does not have chlorion, again the filter paper integral body of filtering thing containing in the filter tunnel is taken off, dried 12 hours down at 60 ℃, make Graphene paper.
Through the thin film mechanical performance tester test of U.S. CE TR company, the tensile strength test data of the Graphene paper that present embodiment makes is 474MPa.
Embodiment three
Utilize electric field leading to prepare the method for Graphene paper, may further comprise the steps:
(1) gets 6g potassium chloride intercalated graphite and join in the beaker, add the 1L deionized water then, stir and be made into the intercalated graphite turbid liquid that concentration is 6g/L down;
(2) the intercalated graphite turbid liquid is carried out ultrasonic wave and handle, used the ultrasonic cleaning instrument ultrasonic 12 minutes, the power of ultrasonic cleaning instrument is preferably 200w, makes intercalated graphite peel off, and makes the solution that contains Graphene;
(3) solution that will contain Graphene is poured in the filter tunnel, and filter tunnel is placed electric-field intensity is the uniform electric field of 100V/m, and under the guiding of electric field force and charge interaction power, the Graphene that contains in the solution of Graphene deposits;
(4) treat that Graphene deposits substantially after, directly filter, finish direct filtration after, slowly the hot water of 83 ℃ of addings filters again in the filter tunnel, to using AgNO
3After detection filtrate does not have chlorion, again the filter paper integral body of filtering thing containing in the filter tunnel is taken off, dried 15 hours down at 60 ℃, make Graphene paper.
Through the thin film mechanical performance tester test of U.S. CE TR company, the tensile strength test data of the Graphene paper that present embodiment makes is 536MPa.
Embodiment four
Utilize electric field leading to prepare the method for Graphene paper, may further comprise the steps:
(1) gets 8g nickel chloride intercalated graphite and join in the beaker, add the 1L deionized water then, stir and be made into the intercalated graphite turbid liquid that concentration is 8g/L down;
(2) the intercalated graphite turbid liquid is carried out ultrasonic wave and handle, used the ultrasonic cleaning instrument ultrasonic 14 minutes, the power of ultrasonic cleaning instrument is preferably 250w, makes intercalated graphite peel off, and makes the solution that contains Graphene;
(3) solution that will contain Graphene is poured in the filter tunnel, and filter tunnel is placed electric-field intensity is the uniform electric field of 120V/m, and under the guiding of electric field force and charge interaction power, the Graphene that contains in the solution of Graphene deposits;
(4) treat that Graphene deposits substantially after, directly filter, finish direct filtration after, slowly the hot water of 85 ℃ of addings filters again in the filter tunnel, to using AgNO
3After detection filtrate does not have chlorion, again the filter paper integral body of filtering thing containing in the filter tunnel is taken off, dried 14 hours down at 60 ℃, make Graphene paper.
Through the thin film mechanical performance tester test of U.S. CE TR company, the tensile strength test data of the Graphene paper that present embodiment makes is 487MPa.
Claims (7)
1. utilize electric field leading to prepare the method for Graphene paper, it is characterized in that, may further comprise the steps:
(1) gets the chloride intercalated graphite, add deionized water, stir and be made into the intercalated graphite turbid liquid that concentration is 5～10g/L down;
(2) described intercalated graphite turbid liquid is carried out ultrasonic wave and handle, make described intercalated graphite peel off, make the solution that contains Graphene;
(3) the described solution that contains Graphene is poured in the filter tunnel, and described filter tunnel is placed electric-field intensity is the uniform electric field of 50～200V/m, under the guiding of electric field force and charge interaction power, the Graphene in the described solution that contains Graphene deposits;
(4) treat that described Graphene deposits substantially after, filter, the oven dry contain the filter paper of filtering thing, make Graphene paper.
2. the method for claim 1 is characterized in that, in the step (1), described chloride is selected from a kind of or its any combination in iron chloride, nickel chloride, copper chloride, cobalt chloride, potassium chloride, lead chloride and the zinc chloride.
3. the method for claim 1 is characterized in that, in the step (2), described ultrasonic time is 10～15 minutes.
4. the method for claim 1 is characterized in that, in the step (2), described ultrasonic procedure is used the ultrasonic cleaning instrument, and the power of described ultrasonic cleaning instrument is preferably 150～400w.
5. the method for claim 1 is characterized in that, in the step (4), also comprises the inspection step to filtrate: detect filtrate with the solution that contains Ag+, as no chlorion, then will take off and contain the filter paper of filtering thing; Otherwise, filter liquor again.
6. method as claimed in claim 5 is characterized in that, in the step (4), the described hot water that adds 80～90 ℃ in the filter tunnel that is filtered into again slowly filters.
7. the method for claim 1 is characterized in that, in the step (4), described drying condition is: dried 12～18 hours under 60 ℃ of temperature.
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Cited By (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN103482621A (en) * | 2013-09-11 | 2014-01-01 | 黄镇东 | Oxidized or deoxidated graphene-based macro material and preparing method thereof |
| CN104261387A (en) * | 2014-09-16 | 2015-01-07 | 中山大学 | Method for large-area preparation of graphene based carbon paper and graphene based carbon paper prepared thereby |
| CN104291327A (en) * | 2014-09-24 | 2015-01-21 | 北京化工大学常州先进材料研究院 | Method for preparing graphene by peeling graphite in electrochemical manner by using molten salt |
| CN115571873A (en) * | 2019-05-30 | 2023-01-06 | 常州第六元素材料科技股份有限公司 | Impurity removal method for reducing graphene oxide film by using hydrogen halide |
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| CN102021633A (en) * | 2009-09-09 | 2011-04-20 | 中国科学院金属研究所 | Preparation method of graphene thin film field emission material |
| CN102066245A (en) * | 2007-10-19 | 2011-05-18 | 卧龙岗大学 | Process for the preparation of graphene |
| CN102321994A (en) * | 2011-06-13 | 2012-01-18 | 哈尔滨工业大学 | The nanometer Preparation Method made of paper that contains Graphene |
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Patent Citations (4)
| Publication number | Priority date | Publication date | Assignee | Title |
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| CN102066245A (en) * | 2007-10-19 | 2011-05-18 | 卧龙岗大学 | Process for the preparation of graphene |
| CN101513998A (en) * | 2009-02-11 | 2009-08-26 | 中国科学院山西煤炭化学研究所 | Method for preparing ordered graphene oxide films |
| CN102021633A (en) * | 2009-09-09 | 2011-04-20 | 中国科学院金属研究所 | Preparation method of graphene thin film field emission material |
| CN102321994A (en) * | 2011-06-13 | 2012-01-18 | 哈尔滨工业大学 | The nanometer Preparation Method made of paper that contains Graphene |
Cited By (6)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN103482621A (en) * | 2013-09-11 | 2014-01-01 | 黄镇东 | Oxidized or deoxidated graphene-based macro material and preparing method thereof |
| CN103482621B (en) * | 2013-09-11 | 2016-01-20 | 黄镇东 | Oxidation or reduced graphene base macroscopic material and preparation method thereof |
| CN104261387A (en) * | 2014-09-16 | 2015-01-07 | 中山大学 | Method for large-area preparation of graphene based carbon paper and graphene based carbon paper prepared thereby |
| CN104261387B (en) * | 2014-09-16 | 2016-06-01 | 中山大学 | A kind of big area prepares the method for Graphene carbon paper and the Graphene carbon paper of preparation thereof |
| CN104291327A (en) * | 2014-09-24 | 2015-01-21 | 北京化工大学常州先进材料研究院 | Method for preparing graphene by peeling graphite in electrochemical manner by using molten salt |
| CN115571873A (en) * | 2019-05-30 | 2023-01-06 | 常州第六元素材料科技股份有限公司 | Impurity removal method for reducing graphene oxide film by using hydrogen halide |
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Application publication date: 20130821 |