CN103880000A - Preparation method of ultralight graphene powder - Google Patents
Preparation method of ultralight graphene powder Download PDFInfo
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- CN103880000A CN103880000A CN201410081755.9A CN201410081755A CN103880000A CN 103880000 A CN103880000 A CN 103880000A CN 201410081755 A CN201410081755 A CN 201410081755A CN 103880000 A CN103880000 A CN 103880000A
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Abstract
The invention provides a preparation method of ultralight graphene powder. The method is mainly characterized by comprising the following steps: suspending graphene oxide powder obtained by adopting a known technology above the liquid level of a reductive solution in an enclosed reactor; heating the reductive solution to carry out a reduction reaction of the graphene oxide powder; and thermally treating the obtained reduced powder in vacuum or under atmosphere protection to obtain non-agglomerated ultralight graphene powder. The preparation method of ultralight graphene powder provided by the invention has the advantages of high efficiency, easiness in production expansion and operation, low cost, easiness in process control, and the like.
Description
Technical field
The preparation method who the invention discloses a kind of ultralight graphene powder, belongs to field of nano material preparation, particularly nano-graphene technical field of powdered material preparation.
Background technology
Graphene, because having unique two-dirnentional structure, is paid close attention in recent years greatly.Graphene shows the performance of many excellences, such as hardness is large, heat conductivity is high, electronic mobility is high, theoretical specific surface area is large etc.
The preparation of Graphene at present mainly contains following four kinds of methods: chemical Vapor deposition process (Obraztsov A N etal., Chemical vapour deposition:making graphene on a large scale. Nature Nanotechnology, 2009, 4:212), epitaxial growth method (Berger C et al. Electronic confinement and coherence in patterned epitaxial graphene. Science, 2006, 312:1191), micromechanics stripping method (Novoselov KS et al. electric field effect in atomically thin carbon films.Science, 2004, 306:666) and oxidation reduction process (Park S et al. Chemical methods for the production of graphenes. Nature Nanotechnology, 2009, 4:217).Wherein oxidation reduction process is suitable for the scale operation of Graphene.The step that oxidation reduction process is general is, uses intercalator, strong oxidizer to carry out intercalation, oxidation to graphite, then it reduced with reductive agents such as hydrazine hydrate, dimethylhydrazine, sodium borohydrides.The method of preparing graphene oxide mainly contains Brodie method, Staudenmaire method, Hummers method.Prepared graphene oxide has good dispersibility.But in follow-up Liquid reduction reaction process system, due to stronger Van der Waals force, make the spontaneous reunion of Graphene and pile up (Park S et al.Hydrazine-reduction of graphite-and graphene oxide.Carbon, 2011,49:3019), and because making it be not suitable for producing high-quality graphene; In addition, the efficiency of liquid-phase reduction is low.
Summary of the invention
The object of the invention is to overcome the deficiency of prior art; provide a kind of high and low cost of efficiency of Graphene, the graphene powder of preparation to produce without preparation method, the change of the ultralight graphene powder of reuniting, the inventive method is suitable for large-scale production graphene powder.
The preparation method of a kind of ultralight graphene powder of the present invention, comprises the following steps:
Step 1: place reducing solution in closed reactor bottom, by the unsettled graphene oxide powder reducing solution liquid level in closed reactor, graphene oxide powder does not directly contact with reducing solution;
Step 2: more than closed reactor is warming up to reducing solution vaporization temperature T?-? ℃, insulation, make reductive agent evaporation form steam and with graphene oxide powder generation reduction reaction, reduction reaction finishes, and obtains reduction state graphene powder;
Step 3: step 2 gained reduction state graphene powder is placed under vacuum or protective atmosphere, is heated to 500-800 ℃, heat-preserving deoxidizing, obtains ultralight graphene powder.
The preparation method of a kind of ultralight graphene powder of the present invention, graphene oxide powder adopts the one in Brodie method, Staudenmaire method, Hummers method to prepare described in step 1.
The preparation method of a kind of ultralight graphene powder of the present invention, the atmosphere described in step 1 in closed reactor can be that one or more gases in air, nitrogen, hydrogen or argon gas mix with arbitrary ratio.
The preparation method of a kind of ultralight graphene powder of the present invention, in step 1, in described reducing solution, solute is selected from least one in hydrazine, sodium borohydride, vitamins C, and solvent is selected from water and/or organic solvent; Described organic solvent is selected from least one in methyl alcohol, ethanol, acetone, dimethyl formamide, poly(vinylidene fluoride).
The preparation method of a kind of ultralight graphene powder of the present invention, the mass percentage concentration of described reducing solution is 40～80%.
The preparation method of a kind of ultralight graphene powder of the present invention, the volume of described reducing solution and the quality of graphene oxide are by the proportional arrangement of 10～200ml/g.
The preparation method of a kind of ultralight graphene powder of the present invention, in step 2, the mark that reduction reaction finishes is that products therefrom color all changes black into.
The preparation method of a kind of ultralight graphene powder of the present invention, in step 3, the vacuum tightness of described vacuum is 10
-5pa～10
-2pa; Described protective atmosphere refers to the one in nitrogen, hydrogen or argon gas.
The preparation method of a kind of ultralight graphene powder of the present invention, in step 3, the heating and thermal insulation time is 0.5-5h.
Advantage of the present invention and positively effect:
(1) the present invention is by the unsettled graphene oxide powder reducing solution liquid level in closed reactor, then by controlling the temperature of closed reactor, guarantee form and the graphene oxide powder generation reduction reaction of reductive agent with gaseous state, prepare reduction state graphene product, thereby avoided the defect that traditional liquid phase method easily occurs that Graphene product is reunited;
(2) reduction state graphene product is heat-treated, can remove wherein unnecessary oxygen, improve carbon, oxygen ratio in Graphene, prepare efficiently, fast ultralight graphene powder;
(3) the present invention easily realizes the volume production of Graphene.
Accompanying drawing explanation
Fig. 1 is the scanning electron microscope (SEM) photograph of the prepared graphene powder of comparative example 1.
Fig. 2 is the prepared graphene powder photo figure of embodiment 1.
Fig. 3 is the scanning electron microscope (SEM) photograph of the prepared graphene powder of embodiment 1.
Can find out from accompanying drawing 3, prepared graphene powder is fluffy, there is no agglomeration, and graphene film is transparent, without obviously curling, and the radial dimension of lamella is about 50 microns, and atomic force microscope result shows that the thickness of gained Graphene is 3-5 nanometer.
Embodiment
Describe below by specific embodiment, further set forth substantive distinguishing features of the present invention, but the present invention is not so limited.
Comparative example 1: 100mg graphene oxide powder is scattered in 500ml deionized water, add 5ml ammoniacal liquor, 1ml hydrazine hydrate, reaction is placed in to 90 ℃ of water-baths and reacts after 3h, solution is cooled to room temperature, suction filtration, washing, dry after, obtain Liquid preparation methods graphene powder.
Accompanying drawing 1 is the scanning electron microscope picture of gained graphene powder, can find out, has obvious reunion, caking phenomenon between gained Graphene.
Embodiment 1:
On the hydrazine hydrate solution liquid level that is 80% by the unsettled 100mg graphene oxide powder 1ml concentration in the closed reactor that is filled with nitrogen, guarantee that powder and hydrazine solution are contactless; Again by closed reactor feeding temperature-raising to 100 ℃, and after maintaining 3h, power-off makes reactor cooling, then takes out powder product; Gained powder is placed in to vacuum electric furnace, rises to 500 ℃ of insulation 2h, vacuum tightness is 10
-5pa, obtains without the ultralight graphene powder of reuniting.
Accompanying drawing 2 and accompanying drawing 3 are respectively digital photograph and the scanning electron microscope picture of the graphene powder of preparation.Can find out, prepared graphene powder is fluffy, there is no agglomeration, and graphene film is transparent, without obviously curling, and the radial dimension of lamella is about 50 microns, and atomic force microscope result shows that the thickness of gained Graphene is 3-5 nanometer.
Embodiment 2:
By on the unsettled 100mg graphene oxide powder reducing solution liquid level in the closed reactor that is filled with argon gas, guarantee that powder and reducing solution are contactless, this reducing solution is that 40% hydrazine hydrate and 1ml dehydrated alcohol mix by 2ml concentration; Again by closed reactor feeding temperature-raising to 120 ℃, and maintain 2h, power-off, makes reactor cooling, then takes out product, and the electric furnace that gained powder is placed in to argon gas atmosphere protection rises to 600 ℃ of insulation 0.5h, obtains without the ultralight graphene powder of reuniting.
Scanning electron microscope and atomic force microscope test result show: prepared graphene powder is fluffy, there is no agglomeration, graphene film is transparent, nothing is obviously curling, the radial dimension of lamella is about 50 microns, and atomic force microscope result shows that the thickness of gained Graphene is 3-5 nanometer.
Embodiment 3:
By on the liquid level of the unsettled reducing solution in the closed reactor that is filled with air of 100mg graphene oxide powder, guarantee that powder and solution are contactless, this reducing solution is that 10ml concentration is 40% sodium borohydride solution; Again by closed reactor feeding temperature-raising to 120 ℃, and maintain 5h, power-off, makes reactor cooling, then takes out product, and gained powder is placed in to electric furnace, rises to 500 ℃ of insulation 0.5h, and vacuum tightness is 10
-3pa, obtains without the ultralight graphene powder of reuniting.
Scanning electron microscope and atomic force microscope test result show: prepared graphene powder is fluffy, there is no agglomeration, graphene film is transparent, nothing is obviously curling, the radial dimension of lamella is about 80 microns, and atomic force microscope result shows that the thickness of gained Graphene is 3-5 nanometer.
Embodiment 4:
By on the liquid level of the unsettled reducing solution in the closed reactor that is filled with air of 100mg graphene oxide powder, guarantee that powder and solution are contactless, this reducing solution is the vitamin c solution of 20ml concentration 80%; Again by closed reactor feeding temperature-raising to 100 ℃, and maintain 4h, power-off, makes reactor cooling, then takes out product, and gained powder is placed in to electric furnace, under nitrogen atmosphere protection, rises to 800 ℃ of insulation 1h, obtains without the ultralight graphene powder of reuniting.
Scanning electron microscope and atomic force microscope test result show: prepared graphene powder is fluffy, there is no agglomeration, graphene film is transparent, nothing is obviously curling, the radial dimension of lamella is about 60 microns, and atomic force microscope result shows that the thickness of gained Graphene is 1-5 nanometer.
Embodiment 5:
By on the unsettled 100mg graphene oxide powder reductibility liquid level in the closed reactor that is filled with air, guarantee that powder and solution are contactless, this reducing solution is mixed by the hydrazine hydrate solution of 1ml concentration 40%, the vitamin c solution of 1ml concentration 80% and the sodium borohydride solution that 1ml concentration is 40%; Again by closed reactor feeding temperature-raising to 120 ℃, and maintain 3h, power-off, makes reactor cooling, then takes out product, and gained powder is placed in to electric furnace, rises to 700 ℃ of insulation 0.5h, and vacuum tightness is 10
-2pa, obtains without the ultralight graphene powder of reuniting.
Scanning electron microscope and atomic force microscope test result show: prepared graphene powder is fluffy, there is no agglomeration, graphene film is transparent, nothing is obviously curling, the radial dimension of lamella is about 100 microns, and atomic force microscope result shows that the thickness of gained Graphene is 3-5 nanometer.
Embodiment 6:
By on the unsettled 100mg graphene oxide powder reductibility liquid level in the closed reactor that is filled with air, guarantee that powder and solution are contactless, the hydrazine hydrate solution of this reducing solution 1ml concentration 40%, vitamin c solution and the 1ml methanol solution of 1ml concentration 40% mix; Again by closed reactor feeding temperature-raising to 100 ℃, and maintain 8h, power-off, makes reactor cooling, then takes out product, and gained powder is placed in to electric furnace, under nitrogen atmosphere protection, rises to 700 ℃ of insulation 1.5h, obtains without the ultralight graphene powder of reuniting.
Scanning electron microscope and atomic force microscope test result show: prepared graphene powder is fluffy, there is no agglomeration, graphene film is transparent, nothing is obviously curling, the radial dimension of lamella is about 80 microns, and atomic force microscope result shows that the thickness of gained Graphene is 3-6 nanometer.
Embodiment 7:
By on the unsettled 100mg graphene oxide powder reductibility liquid level in the closed reactor that is filled with air, guarantee that powder and solution are contactless, the hydrazine hydrate solution of this reducing solution 1ml concentration 40%, sodium borohydride solution and the 2ml acetone soln of 1ml concentration 40% mix; Again by closed reactor feeding temperature-raising to 100 ℃, and maintain 3h, power-off, makes reactor cooling, then takes out product, and gained powder is placed in to electric furnace, under argon gas atmosphere protection, rises to 800 ℃ of insulation 0.5h, obtains without the ultralight graphene powder of reuniting.
Scanning electron microscope and atomic force microscope test result show: prepared graphene powder is fluffy, there is no agglomeration, graphene film is transparent, nothing is obviously curling, the radial dimension of lamella is about 70 microns, and atomic force microscope result shows that the thickness of gained Graphene is 3-5 nanometer.
Embodiment 8:
By on the unsettled 100mg graphene oxide powder reductibility liquid level in the closed reactor that is filled with air, guarantee that powder and solution are contactless, the vitamin c solution of this reducing solution 1ml concentration 40%, sodium borohydride solution and the 8ml dimethyl formamide of 1ml concentration 40% mix; Again by closed reactor feeding temperature-raising to 100 ℃, and maintain 5h, power-off, makes reactor cooling, then takes out product, and gained powder is placed in to electric furnace, under argon gas atmosphere protection, rises to 700 ℃ of insulation 1h, obtains without the ultralight graphene powder of reuniting.
Scanning electron microscope and atomic force microscope test result show: prepared graphene powder is fluffy, there is no agglomeration, graphene film is transparent, nothing is obviously curling, the radial dimension of lamella is about 110 microns, and atomic force microscope result shows that the thickness of gained Graphene is 1-5 nanometer.
Embodiment 9:
By on the unsettled 100mg graphene oxide powder reductibility liquid level in the closed reactor that is filled with nitrogen, guarantee that powder and solution are contactless, the hydrazine hydrate solution of this reducing solution 1ml concentration 40%, the vitamin c solution of 1ml concentration 40% and 1ml poly(vinylidene fluoride) solution mix; Again by closed reactor feeding temperature-raising to 100 ℃, and maintain 5h, power-off, makes reactor cooling, then takes out product, and gained powder is placed in to electric furnace, under nitrogen atmosphere protection, rises to 600 ℃ of insulation 2h, obtains without the ultralight graphene powder of reuniting.
Scanning electron microscope and atomic force microscope test result show: prepared graphene powder is fluffy, there is no agglomeration, graphene film is transparent, nothing is obviously curling, the radial dimension of lamella is about 80 microns, and atomic force microscope result shows that the thickness of gained Graphene is 1-5 nanometer.
Embodiment 10:
By on the unsettled 100mg graphene oxide powder reductibility liquid level in the closed reactor that is filled with argon gas, guarantee that powder and solution are contactless, this reducing solution is mixed by hydrazine hydrate solution, the vitamin c solution of 2ml concentration 40%, the sodium borohydride solution of 2ml concentration 40%, 2ml poly(vinylidene fluoride), 2ml dimethyl formamide, 2ml acetone soln, the 2ml ethanolic soln of 2ml concentration 40%; Again by closed reactor feeding temperature-raising to 100 ℃, and maintain 5h, power-off, makes reactor cooling, then takes out product, and gained powder is placed in to electric furnace, under argon gas atmosphere protection, rises to 500 ℃ of insulation 1.5h, obtains without the ultralight graphene powder of reuniting.
Scanning electron microscope and atomic force microscope test result show: prepared graphene powder is fluffy, there is no agglomeration, graphene film is transparent, nothing is obviously curling, the radial dimension of lamella is about 100 microns, and atomic force microscope result shows that the thickness of gained Graphene is 3-5 nanometer.
Claims (9)
1. a preparation method for ultralight graphene powder, comprises the following steps:
Step 1: place reducing solution in closed reactor bottom, by the unsettled graphene oxide powder reducing solution liquid level in closed reactor, graphene oxide powder does not directly contact with reducing solution;
Step 2: more than closed reactor is warming up to reducing solution vaporization temperature T, insulation, make reductive agent evaporation form steam and with graphene oxide powder generation reduction reaction, reduction reaction finishes, and obtains reduction state graphene powder;
Step 3: step 2 gained reduction state graphene powder is placed under vacuum or protective atmosphere, is heated to 500-800 ℃, heat-preserving deoxidizing, obtains ultralight graphene powder.
2. the preparation method of a kind of ultralight graphene powder according to claim 1, is characterized in that: described in step 1, graphene oxide powder adopts the one in Brodie method, Staudenmaire method, Hummers method to prepare.
3. the preparation method of a kind of ultralight graphene powder according to claim 1 and 2, is characterized in that: in step 1, in described reducing solution, solute is selected from least one in hydrazine, sodium borohydride, vitamins C, and solvent is selected from water and/or organic solvent.
4. the preparation method of a kind of ultralight graphene powder according to claim 3, is characterized in that: described organic solvent is selected from least one in methyl alcohol, ethanol, acetone, dimethyl formamide, poly(vinylidene fluoride).
5. the preparation method of a kind of ultralight graphene powder according to claim 4, is characterized in that: the mass percentage concentration of described reducing solution is 40～80%.
6. the preparation method of a kind of ultralight graphene powder according to claim 5, is characterized in that: the volume of described reducing solution and the quality of graphene oxide are by the proportional arrangement of 10～200ml/g.
7. the preparation method of a kind of ultralight graphene powder according to claim 6, is characterized in that: in step 2, the mark that reduction reaction finishes is that products therefrom color all changes black into.
8. the preparation method of a kind of ultralight graphene powder according to claim 7, is characterized in that: in step 3, the vacuum tightness of described vacuum is 10
-5pa～10
-2pa; Described protective atmosphere refers to the one in nitrogen, hydrogen or argon gas.
9. the preparation method of a kind of ultralight graphene powder according to claim 8, is characterized in that: in step 3, the heating and thermal insulation time is 0.5-5h.
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| CN104409569A (en) * | 2014-11-20 | 2015-03-11 | 齐鲁工业大学 | Environment-friendly preparation method of graphene-sliver composite material with three-dimensional network structure |
| CN105776199A (en) * | 2016-05-20 | 2016-07-20 | 东南大学 | Method for reducing graphene oxide |
| CN106698399A (en) * | 2016-12-16 | 2017-05-24 | 北京鼎臣超导科技有限公司 | Graphene and preparation method thereof |
| CN107827097A (en) * | 2017-11-22 | 2018-03-23 | 四川大学 | A kind of graphene synthetic method without external energy input |
| CN111244451A (en) * | 2020-01-15 | 2020-06-05 | 中国科学院苏州纳米技术与纳米仿生研究所 | Magnesium ion battery negative electrode material, magnesium ion battery and preparation method thereof |
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Cited By (9)
| Publication number | Priority date | Publication date | Assignee | Title |
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| CN104409569A (en) * | 2014-11-20 | 2015-03-11 | 齐鲁工业大学 | Environment-friendly preparation method of graphene-sliver composite material with three-dimensional network structure |
| CN104409569B (en) * | 2014-11-20 | 2016-12-07 | 齐鲁工业大学 | The environment-friendly preparation method thereof of three-dimensional net structure Graphene-silver composite material |
| CN105776199A (en) * | 2016-05-20 | 2016-07-20 | 东南大学 | Method for reducing graphene oxide |
| CN106698399A (en) * | 2016-12-16 | 2017-05-24 | 北京鼎臣超导科技有限公司 | Graphene and preparation method thereof |
| CN106698399B (en) * | 2016-12-16 | 2019-01-04 | 北京鼎臣超导科技有限公司 | A kind of graphene and preparation method thereof |
| CN107827097A (en) * | 2017-11-22 | 2018-03-23 | 四川大学 | A kind of graphene synthetic method without external energy input |
| CN111244451A (en) * | 2020-01-15 | 2020-06-05 | 中国科学院苏州纳米技术与纳米仿生研究所 | Magnesium ion battery negative electrode material, magnesium ion battery and preparation method thereof |
| CN111244451B (en) * | 2020-01-15 | 2022-05-10 | 中国科学院苏州纳米技术与纳米仿生研究所 | Magnesium ion battery negative electrode material, magnesium ion battery and preparation method thereof |
| CN112945997A (en) * | 2021-02-01 | 2021-06-11 | 天津艾克凯胜石墨烯科技有限公司 | Sample preparation method for aqueous graphene slurry before scanning electron microscope |
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Application publication date: 20140625 |