CN105000556A - Method for preparing graphene on large scale - Google Patents
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- CN105000556A CN105000556A CN201510546951.3A CN201510546951A CN105000556A CN 105000556 A CN105000556 A CN 105000556A CN 201510546951 A CN201510546951 A CN 201510546951A CN 105000556 A CN105000556 A CN 105000556A
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Abstract
The invention relates to a method for preparing graphene on a large scale, aims at solving the problems that a current method for preparing the graphene cannot realize mass production and is high in cost, and the aftertreatment process is complex and environmental pollution is more likely to happen. The method comprises the steps of uniformly mixing urea and magnesium powder according to the mass ratio of 1: (0.5 to 1), placing a mixture into inert gases, warming up to 700 to 1400 DEG C with the heating rate of 2 to 50 DEG C per minute, keeping for 1 to 20 hours, cooling to the room temperature, and then obtaining the graphene through acid pickling, ultrasound, suction filtration and drying. The method is simple in process, short in production cycle, simple in components of a reactant, low in price and cost, easy to produce on a large scale, can be used for preparing a new energy material which is used as an electrode material of lithium ion batteries, lithium-air batteries and supercapacitors as well as an oxidation-reduction catalyst of fuel cells.
Description
Technical field
The present invention relates to a kind of method that Graphene is prepared in mass-producing, belong to technical field of graphene preparation.
Background technology
Graphene be planar monolayer carbon atom combine closely formed bi-dimensional cellular lattice material, because the performances such as the chemical structure of its uniqueness, the specific surface area of super large and impayable electricity, mechanics, calorifics are with a wide range of applications in new energy materials, sensor, sorbing material, photocatalyst material, biomaterial and all kinds of field of compound material.The method preparing Graphene at present mainly contains: micromechanics stripping method, redox chemistry stripping method, solvent-thermal method, plane of crystal epitaxial growth method, surface of SiC greying method, chemical Vapor deposition process etc., but, existing method has cannot the shortcoming of scale operation, the most frequently used solvent-thermal method adopts natural graphite, potassium permanganate, the vitriol oil and concentrated nitric acid prepare Graphene, have cost high, aftertreatment technology is complicated and easily cause the problem of environmental pollution.Therefore, find and a kind of there is the study hotspot that technique is simple, cheap, graphene preparation method that is that easily realize the advantages such as industrialization scale operation becomes this field.
Summary of the invention
The object of the invention is in order to solve the existing method preparing Graphene cannot scale operation, cost high, aftertreatment technology is complicated and easily cause the problem of environmental pollution, provides a kind of mass-producing to prepare the method for Graphene.
The method of Graphene is prepared in a kind of mass-producing of the present invention, comprises the following steps:
One, by urea and magnesium powder according to mass ratio 1:(0.5 ~ 10) ratio mixing, obtain mixture A;
Two, mixture A is placed in rare gas element, is then warming up to 700 DEG C ~ 1400 DEG C with the temperature rise rate of 2 ~ 50 DEG C/min, keep 1 ~ 20h, after being cooled to room temperature, more namely obtain Graphene through overpickling, ultrasonic, suction filtration, oven dry.
Beneficial effect of the present invention is: raw material of the present invention is urea and magnesium powder; with low cost; and only use diluted acid during aftertreatment; technique is simple, easy to operate, environmental pollution is less; in addition present method with short production cycle, be easy to large-scale production; the Graphene of preparation is homogeneous, the number of plies is few, can be used for preparation as new energy materialses such as lithium ion battery, lithium-air battery and electrode material for super capacitor and fuel cell redox catalysts.
Accompanying drawing explanation
Fig. 1 is field emission scanning electron microscope (FESEM) picture of Graphene prepared by embodiment two;
Fig. 2 is the X-ray diffraction pattern (XRD) of Graphene prepared by embodiment two;
Fig. 3 is the Raman spectrogram of Graphene prepared by embodiment one, two, four, six and seven; Wherein a is Graphene prepared by embodiment one; B is Graphene prepared by embodiment two; C is Graphene prepared by embodiment four; D is Graphene prepared by embodiment six; E is Graphene prepared by embodiment seven;
Fig. 4 is the Raman spectrogram of Graphene prepared by embodiment eight ~ 11; Wherein a is Graphene prepared by embodiment eight; B is Graphene prepared by embodiment nine; C is Graphene prepared by embodiment ten; D is Graphene prepared by embodiment 11.
Embodiment
Technical solution of the present invention is not limited to following cited embodiment, also comprises the arbitrary combination between each embodiment.
Embodiment one: the method for Graphene is prepared in a kind of mass-producing of present embodiment, comprises the following steps:
One, by urea and magnesium powder according to mass ratio 1:(0.5 ~ 10) ratio mixing, obtain mixture A;
Two, mixture A is placed in rare gas element, is then warming up to 700 DEG C ~ 1400 DEG C with the temperature rise rate of 2 ~ 50 DEG C/min, keep 1 ~ 20h, after being cooled to room temperature, more namely obtain Graphene through overpickling, ultrasonic, suction filtration, oven dry.
The beneficial effect of present embodiment is: raw material of the present invention is urea and magnesium powder; with low cost; and only use diluted acid during aftertreatment; technique is simple, easy to operate, less to environment dirt; in addition present method with short production cycle, be easy to large-scale production; the Graphene of preparation is homogeneous, the number of plies is few, can be used for preparation as new energy materialses such as lithium ion battery, lithium-air battery and electrode material for super capacitor and fuel cell redox catalysts.
Embodiment two: present embodiment and embodiment one unlike: the urea described in step one and magnesium powder mix according to the ratio of mass ratio 1:1.Other is identical with embodiment one.
Embodiment three: present embodiment and embodiment one or two unlike: the urea described in step one and magnesium powder mix according to the ratio of mass ratio 1:2.Other is identical with embodiment one or two.
Embodiment four: present embodiment and one of embodiment one to three unlike: the urea described in step one and magnesium powder mix according to the ratio of mass ratio 1:3.Other is identical with one of embodiment one to three.
Embodiment five: present embodiment and one of embodiment one to four unlike: the urea described in step one and magnesium powder mix according to the ratio of mass ratio 1:5.Other is identical with one of embodiment one to four.
Embodiment six: one of present embodiment and embodiment one to five unlike: the hold-time described in step 2 is 2h.Other is identical with one of embodiment one to five.
Embodiment seven: one of present embodiment and embodiment one to six unlike: be warming up to 800 DEG C with the temperature rise rate of 5 DEG C/min described in step 2.Other is identical with one of embodiment one to six.
Embodiment eight: one of present embodiment and embodiment one to seven unlike: be warming up to 900 DEG C with the temperature rise rate of 5 DEG C/min described in step 2.Other is identical with one of embodiment one to seven.
Embodiment nine: one of present embodiment and embodiment one to eight unlike: be warming up to 1000 DEG C with the temperature rise rate of 5 DEG C/min described in step 2.Other is identical with one of embodiment one to eight.
Embodiment ten: one of present embodiment and embodiment one to nine unlike: be warming up to 1100 DEG C with the temperature rise rate of 5 DEG C/min described in step 2.Other is identical with one of embodiment one to nine.
Embodiment 11: one of present embodiment and embodiment one to ten unlike: be warming up to 1200 DEG C with the temperature rise rate of 5 DEG C/min described in step 2.Other is identical with one of embodiment one to ten.
Embodiment 12: one of present embodiment and embodiment one to ten one are one or more in nitrogen, argon gas and helium mixed gass of being mixed by any ratio unlike: the rare gas element described in step 2.Other is identical with one of embodiment one to ten one.
Embodiment 13: one of present embodiment and embodiment one to ten two are one or more in hydrochloric acid, sulfuric acid, nitric acid and phosphoric acid mixtures of being mixed by any ratio unlike: the acid that in step 2, pickling is used, and the concentration of pickling acid used is 1mol/L.Other is identical with one of embodiment one to ten two.
By following verification experimental verification beneficial effect of the present invention:
Embodiment one: the method for Graphene is prepared in the present embodiment mass-producing, comprises the following steps:
One, urea and magnesium powder are mixed according to the ratio of mass ratio 1:1, obtain mixture A;
Two, mixture A is placed in rare gas element, is then warming up to 700 DEG C with the temperature rise rate of 5 DEG C/min, keep 2h, after being cooled to room temperature, more namely obtain Graphene through overpickling, ultrasonic, suction filtration, oven dry.
The present embodiment employing concentration is that the sulfuric acid of 1mol/L carries out pickling.
Embodiment two: the method for Graphene is prepared in the present embodiment mass-producing, comprises the following steps:
One, urea and magnesium powder are mixed according to the ratio of mass ratio 1:1, obtain mixture A;
Two, mixture A is placed in rare gas element, is then warming up to 800 DEG C with the temperature rise rate of 5 DEG C/min, keep 2h, after being cooled to room temperature, more namely obtain Graphene through overpickling, ultrasonic, suction filtration, oven dry.
The present embodiment employing concentration is that the sulfuric acid of 1mol/L carries out pickling.
In the present embodiment, as shown in Figure 1, in the present embodiment, obtained sample has sheet structure to the FESEM figure of obtained product as can be seen from Figure 1.
In the present embodiment, the X-ray diffraction pattern figure of obtained product as shown in Figure 2, a very sharp-pointed diffraction peak appears at [002] diffraction surfaces that 26.2 ° correspond to graphite as seen from Figure 2, and this shows that in the present embodiment, obtained sample is the graphite-structure having a kind of high-sequential.
Embodiment three: the method for Graphene is prepared in the present embodiment mass-producing, comprises the following steps:
One, urea and magnesium powder are mixed according to the ratio of mass ratio 1:1, obtain mixture A;
Two, mixture A is placed in rare gas element, is then warming up to 900 DEG C with the temperature rise rate of 5 DEG C/min, keep 2h, after being cooled to room temperature, more namely obtain Graphene through overpickling, ultrasonic, suction filtration, oven dry.
The present embodiment employing concentration is that the sulfuric acid of 1mol/L carries out pickling.
Embodiment four: the method for Graphene is prepared in the present embodiment mass-producing, comprises the following steps:
One, urea and magnesium powder are mixed according to the ratio of mass ratio 1:1, obtain mixture A;
Two, mixture A is placed in rare gas element, is then warming up to 1000 DEG C with the temperature rise rate of 5 DEG C/min, keep 2h, after being cooled to room temperature, more namely obtain Graphene through overpickling, ultrasonic, suction filtration, oven dry.
The present embodiment employing concentration is that the sulfuric acid of 1mol/L carries out pickling.
Embodiment five: the method for Graphene is prepared in the present embodiment mass-producing, comprises the following steps:
One, urea and magnesium powder are mixed according to the ratio of mass ratio 1:1, obtain mixture A;
Two, mixture A is placed in rare gas element, is then warming up to 1100 DEG C with the temperature rise rate of 5 DEG C/min, keep 2h, after being cooled to room temperature, more namely obtain Graphene through overpickling, ultrasonic, suction filtration, oven dry.
The present embodiment employing concentration is that the sulfuric acid of 1mol/L carries out pickling.
Embodiment six: the method for Graphene is prepared in the present embodiment mass-producing, comprises the following steps:
One, urea and magnesium powder are mixed according to the ratio of mass ratio 1:1, obtain mixture A;
Two, mixture A is placed in rare gas element, is then warming up to 1200 DEG C with the temperature rise rate of 5 DEG C/min, keep 2h, after being cooled to room temperature, more namely obtain Graphene through overpickling, ultrasonic, suction filtration, oven dry.
The present embodiment employing concentration is that the sulfuric acid of 1mol/L carries out pickling.
Embodiment seven: the method for Graphene is prepared in the present embodiment mass-producing, comprises the following steps:
One, urea and magnesium powder are mixed according to the ratio of mass ratio 1:1, obtain mixture A;
Two, mixture A is placed in rare gas element, is then warming up to 1400 DEG C with the temperature rise rate of 5 DEG C/min, keep 2h, after being cooled to room temperature, more namely obtain Graphene through overpickling, ultrasonic, suction filtration, oven dry.
The present embodiment employing concentration is that the sulfuric acid of 1mol/L carries out pickling.
As shown in Figure 3, a is Graphene prepared by embodiment one to the Raman spectrogram of Graphene prepared by embodiment one, two, four, six and seven; B is Graphene prepared by embodiment two; C is Graphene prepared by embodiment four; D is Graphene prepared by embodiment six; E is Graphene prepared by embodiment seven; As can be seen from the figure D peak, G peak and 2D peak, illustrate that embodiment one, two, four, six and seventy percent merit prepares Graphene, and pass through the ratio at 2D peak and G peak, can find out that the obtained Graphene number of plies is less.
Embodiment eight: the method for Graphene is prepared in the present embodiment mass-producing, comprises the following steps:
One, urea and magnesium powder are mixed according to the ratio of mass ratio 1:2, obtain mixture A;
Two, mixture A is placed in rare gas element, is then warming up to 800 DEG C with the temperature rise rate of 5 DEG C/min, keep 2h, after being cooled to room temperature, more namely obtain Graphene through overpickling, ultrasonic, suction filtration, oven dry.
The present embodiment employing concentration is that the hydrochloric acid of 1mol/L carries out pickling.
Fig. 3 a is the Raman spectrum of obtained product in the present embodiment, as can be seen from the figure D peak, G peak and 2D peak, illustrates that in the present embodiment, obtained sample is Graphene.
Embodiment nine: the method for Graphene is prepared in the present embodiment mass-producing, comprises the following steps:
One, urea and magnesium powder are mixed according to the ratio of mass ratio 1:3, obtain mixture A;
Two, mixture A is placed in rare gas element, is then warming up to 800 DEG C with the temperature rise rate of 5 DEG C/min, keep 2h, after being cooled to room temperature, more namely obtain Graphene through overpickling, ultrasonic, suction filtration, oven dry.
The present embodiment employing concentration is that the hydrochloric acid of 1mol/L carries out pickling.
Embodiment ten: the method for Graphene is prepared in the present embodiment mass-producing, comprises the following steps:
One, urea and magnesium powder are mixed according to the ratio of mass ratio 1:4, obtain mixture A;
Two, mixture A is placed in rare gas element, is then warming up to 800 DEG C with the temperature rise rate of 5 DEG C/min, keep 2h, after being cooled to room temperature, more namely obtain Graphene through overpickling, ultrasonic, suction filtration, oven dry.
The present embodiment employing concentration is that the hydrochloric acid of 1mol/L carries out pickling.
Fig. 3 c is the Raman spectrum of obtained product in the present embodiment, as can be seen from the figure D peak, G peak and 2D peak, illustrates that in the present embodiment, obtained sample is Graphene.
Embodiment 11: the method for Graphene is prepared in the present embodiment mass-producing, comprises the following steps:
One, urea and magnesium powder are mixed according to the ratio of mass ratio 1:5, obtain mixture A;
Two, mixture A is placed in rare gas element, is then warming up to 800 DEG C with the temperature rise rate of 5 DEG C/min, keep 2h, after being cooled to room temperature, more namely obtain Graphene through overpickling, ultrasonic, suction filtration, oven dry.
The present embodiment employing concentration is that the hydrochloric acid of 1mol/L carries out pickling.
As shown in Figure 4, a is Graphene prepared by embodiment eight to the Raman spectrogram of Graphene prepared by embodiment eight ~ 11; B is Graphene prepared by embodiment nine; C is Graphene prepared by embodiment ten; D is Graphene prepared by embodiment 11; As can be seen from the figure D peak, G peak and 2D peak, illustrate that embodiment eight ~ 11 successfully prepares Graphene, and pass through the ratio at 2D peak and G peak, can find out that the obtained Graphene number of plies is less.
Embodiment 12: the method for Graphene is prepared in the present embodiment mass-producing, comprises the following steps:
One, urea and magnesium powder are mixed according to the ratio of mass ratio 1:0.5, obtain mixture A;
Two, mixture A is placed in rare gas element, is then warming up to 800 DEG C with the temperature rise rate of 5 DEG C/min, keep 2h, after being cooled to room temperature, more namely obtain Graphene through overpickling, ultrasonic, suction filtration, oven dry.
The present embodiment employing concentration is that the phosphoric acid of 1mol/L carries out pickling.
Above-described specific descriptions; be only preferred embodiment of the present invention, the protection domain be not intended to limit the present invention, within the spirit and principles in the present invention all; any amendment of making, equivalent replacement, improvement etc., all should be included within protection scope of the present invention.
Claims (10)
1. a method for Graphene is prepared in mass-producing, it is characterized in that the method comprises the following steps:
One, by urea and magnesium powder according to mass ratio 1:(0.5 ~ 10) ratio mixing, obtain mixture A;
Two, mixture A is placed in rare gas element, is then warming up to 700 DEG C ~ 1400 DEG C with the temperature rise rate of 2 ~ 50 DEG C/min, keep 1 ~ 20h, after being cooled to room temperature, more namely obtain Graphene through overpickling, ultrasonic, suction filtration, oven dry.
2. the method for Graphene is prepared in a kind of mass-producing according to claim 1, it is characterized in that urea described in step one and magnesium powder mix according to the ratio of mass ratio 1:1.
3. the method for Graphene is prepared in a kind of mass-producing according to claim 1, it is characterized in that urea described in step one and magnesium powder mix according to the ratio of mass ratio 1:2.
4. the method for Graphene is prepared in a kind of mass-producing according to claim 1, it is characterized in that urea described in step one and magnesium powder mix according to the ratio of mass ratio 1:3.
5. the method for Graphene is prepared in a kind of mass-producing according to claim 1, it is characterized in that urea described in step one and magnesium powder mix according to the ratio of mass ratio 1:5.
6. the method for Graphene is prepared in a kind of mass-producing according to claim 1, it is characterized in that the hold-time described in step 2 is 2h.
7. the method for Graphene is prepared in a kind of mass-producing according to claim 1, it is characterized in that being warming up to 800 DEG C with the temperature rise rate of 5 DEG C/min described in step 2.
8. the method for Graphene is prepared in a kind of mass-producing according to claim 1, it is characterized in that being warming up to 900 DEG C with the temperature rise rate of 5 DEG C/min described in step 2.
9. the method for Graphene is prepared in a kind of mass-producing according to claim 1, and the rare gas element that it is characterized in that described in step 2 is one or more in nitrogen, argon gas and helium mixed gass of being mixed by any ratio.
10. the method for Graphene is prepared in a kind of mass-producing according to claim 1; it is characterized in that acid that in step 2, pickling is used is one or more in hydrochloric acid, sulfuric acid, nitric acid and phosphoric acid mixtures of being mixed by any ratio, the concentration of pickling acid used is 1mol/L.
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Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
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| CN108862244A (en) * | 2017-05-11 | 2018-11-23 | 天津理工大学 | The magnanimity preparation method of nitrogen-doped graphene |
| CN113061406A (en) * | 2021-05-07 | 2021-07-02 | 哈尔滨凯美斯科技有限公司 | Nano-oriented heat-conducting adhesive film for electronic component packaging and preparation method thereof |
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| Publication number | Priority date | Publication date | Assignee | Title |
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| CN108862244A (en) * | 2017-05-11 | 2018-11-23 | 天津理工大学 | The magnanimity preparation method of nitrogen-doped graphene |
| CN113061406A (en) * | 2021-05-07 | 2021-07-02 | 哈尔滨凯美斯科技有限公司 | Nano-oriented heat-conducting adhesive film for electronic component packaging and preparation method thereof |
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