CN103628082A - Graphene preparation method - Google Patents
Graphene preparation method Download PDFInfo
- Publication number
- CN103628082A CN103628082A CN201210310387.1A CN201210310387A CN103628082A CN 103628082 A CN103628082 A CN 103628082A CN 201210310387 A CN201210310387 A CN 201210310387A CN 103628082 A CN103628082 A CN 103628082A
- Authority
- CN
- China
- Prior art keywords
- graphite
- graphene
- preparation
- intercalated graphite
- electrode
- Prior art date
- Legal status (The legal status is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the status listed.)
- Pending
Links
Images
Abstract
The invention relates to a graphene preparation method, which comprises the following six steps: 1, pressing graphite on a stainless steel current collector to obtain a working electrode of a three-electrode system, 2, preparing intercalation graphite by using the three-electrode system, 3, washing the intercalation graphite by using deionized water, 4, carrying out vacuum drying on the washed intercalation graphite to obtain dried intercalation graphite, 5, adding the dried intercalation graphite to low temperature liquefaction gas to soak, and taking out until the intercalation graphite is cooled, and 6, placing the cooled intercalation graphite in an oxygen-free environment to carry out heating stripping to obtain graphene. According to the present invention, the graphene preparation method has characteristics of simple operation and easy industrialization achievement, and the yield of the graphene prepared by using the graphene preparation method is high.
Description
Technical field
The present invention relates to the synthetic field of material, particularly a kind of preparation method of Graphene.
Background technology
Graphene is a kind of Two-dimensional Carbon atomic crystal of the discoveries such as the strong K sea nurse of the peace moral of Univ Manchester UK in 2004 (Andre K.Geim), and obtains the physics Nobel prize in 2010, again causes carbon material research boom.Because its unique structure and photoelectric property become the study hotspot in the fields such as carbon material, nanotechnology, Condensed Matter Physics and functional materials, many scientific workers have been attracted.Graphene has good conduction, heat conductivility and low thermal expansivity, can be used for electrode materials, matrix material etc.In current preparation method, there is graphite oxide reduction method, but the destruction that this method can cause graphene-structured; Also have by pyrolytic decomposition carbon source and prepare Graphene, but this method preparation efficiency is lower.
Summary of the invention
Given this, be necessary to provide the method for the higher Graphene of a kind of preparation efficiency.
A preparation method for Graphene, comprises the steps:
Step 1: graphite is suppressed on stainless steel collector, obtained the working electrode of three-electrode system;
Step 2: prepare intercalated graphite with described three-electrode system;
Step 3: by intercalated graphite described in washed with de-ionized water;
Step 4: the intercalated graphite after cleaning described in vacuum-drying, obtains dried intercalated graphite;
Step 5: described dried intercalated graphite is added and is dipped to the cooling rear taking-up of described intercalated graphite in liquefied gas at low temp;
Step 6: described cooled intercalated graphite is placed in to oxygen-free environment heating and peels off, obtain Graphene.
In an embodiment, in described three-electrode system, to electrode, be stereotype therein; Reference electrode is Hg/Hg
2sO
4; Electrolytic solution is pure intercalator.
In an embodiment, described graphite is natural flake graphite or synthetic graphite therein.
In an embodiment, described step 2 is by electrode, reference electrode and described working electrode are soaked in electrolytic solution jointly, in current density 5mA/cm therein
2~ 100mA/cm
21 hour ~ 20 hours preparation intercalated graphite of lower reaction.
In an embodiment, described electrolytic solution is at least one in formic acid, acetic acid, propionic acid, concentrated nitric acid, the vitriol oil and Nitromethane 99Min. therein.
In an embodiment, described vacuum drying step is that described intercalated graphite is positioned under vacuum condition therein, at 60 ℃ ~ 80 ℃, is dried 12 hours ~ 24 hours.
In an embodiment, in described step 5, it is 0.5 minute ~ 5 minutes that described dried intercalated graphite is added to the time of soaking in immersion in liquefied gas at low temp therein.
In an embodiment, it is characterized in that therein, described liquefied gas at low temp is liquid nitrogen, liquid argon or liquid hydrogen.
In an embodiment, described heating stripping conditions is therein: 800 ℃ ~ 1100 ℃ of temperature, 30 seconds ~ 120 seconds time.
The preparation method of above-mentioned Graphene adopts three-electrode system electrolytic preparation intercalated graphite, then intercalated graphite is soaked in liquefied gas at low temp after refrigeration, then heating is just peeled off and can be accessed Graphene, and the reaction times is short, thereby make preparation efficiency high, and Graphene has kept higher specific conductivity; And the preparation method preparation technology of above-mentioned Graphene is simply easy to realize industrialization.
Accompanying drawing explanation
Fig. 1 is preparation method's schema of the Graphene of an embodiment;
Fig. 2 is the scanning electron microscope (SEM) photograph (SEM) of the Graphene of embodiment 1 preparation.
Embodiment
Below mainly in conjunction with the drawings and the specific embodiments the preparation method of Graphene is described in further detail.
As shown in Figure 1, the preparation method of the Graphene of an embodiment, comprises the steps:
Step S110: graphite is suppressed on stainless steel collector, obtained the working electrode of three-electrode system.
Graphite and binding agent are positioned on collector, then with mould, are pressed into the working electrode of three-electrode system.Collector preferably adopts stainless steel collector.
Graphite can, for the conventional graphite in this area, be preferably natural flake graphite or synthetic graphite.
Preferably, three-electrode system to electrode, be stereotype, reference electrode is Hg/Hg
2sO
4.
Step S120: prepare intercalated graphite with three-electrode system.
Adopt three-electrode system to prepare intercalated graphite.Preparation method will be for being jointly soaked in electrolytic solution electrode, reference electrode and working electrode, in current density 5mA/cm
2~ 100mA/cm
2in room temperature reaction, after 1 hour ~ 20 hours, filter and obtain intercalated graphite.
Wherein, electrolytic solution is at least one in formic acid, acetic acid, propionic acid, concentrated nitric acid, the vitriol oil and Nitromethane 99Min..
Wherein, concentrated nitric acid is that mass percentage concentration is 68% nitric acid; The vitriol oil is that mass percentage concentration is 98% sulfuric acid.
This several electrolytic solution also plays the effect of intercalator simultaneously, and under electric field action, electrolytic solution forms potential difference at working electrode surface, constantly overcomes graphite layers reactive force under the driving of potential difference, is inserted into graphite layers, obtains intercalated graphite.
Adopt electrolytic process to prepare intercalated graphite, preparation efficiency is high.
Step S130: use washed with de-ionized water intercalated graphite.
The intercalated graphite preparing with deionized water cleaning step S120, to avoid that impurity is introduced to subsequent step.
Step S140: the intercalated graphite after vacuum-drying is cleaned, obtains dried intercalated graphite.
Dried intercalated graphite is placed under vacuum condition, at 60 ℃ ~ 80 ℃, is dried 12 hours ~ 24 hours.
Step S150: dried intercalated graphite is added and is dipped to the cooling rear taking-up of intercalated graphite in liquefied gas at low temp.
Wherein, liquefied gas at low temp is liquid nitrogen, liquid argon or liquid hydrogen.
Preferably, the time that dried intercalated graphite is soaked in liquefied gas at low temp is 0.5 minute ~ 5 minutes, so that intercalated graphite is fully cooling.
Step S160: cooled intercalated graphite is placed in to oxygen-free environment heating and peels off, obtain Graphene.
Wherein, oxygen-free environment refers to the environment of nitrogen, argon gas or helium.
The condition that heating is peeled off is 800 ℃ ~ 1100 ℃ of temperature, 30 seconds ~ 120 seconds time.
At oxygen-free environment and 800 ℃ ~ 1100 ℃, heat and peel off, avoid the structure of Graphene to be damaged, so that the Graphene preparing has higher specific conductivity.
Intercalated graphite is soaked in liquefied gas at low temp be placed in again 800 ℃ ~ 1100 ℃ after refrigeration but and be incubated 30 seconds ~ 120 seconds, form the larger temperature difference, be conducive to intercalated graphite thermo-cracking and peel off formation Graphene, improve preparation efficiency.
The preparation method of above-mentioned Graphene, adopts three-electrode system electrolytic preparation intercalated graphite, then intercalated graphite is soaked in liquefied gas at low temp to refrigeration, then heating is just peeled off and can be accessed Graphene, reaction times is short, thereby makes preparation efficiency high, and Graphene has kept higher specific conductivity; And the preparation method preparation technology of above-mentioned Graphene is simply easy to realize industrialization.
In addition, Graphene prepared by the preparation method of above-mentioned Graphene has higher specific conductivity, and intercalated graphite is in being prepared into the process of Graphene, without using other chemical reagent to realize green non-pollution preparation.Preparation method's raw material sources of above-mentioned Graphene are wide, and cost is low.
Be below specific embodiment part:
Embodiment 1
Being prepared as follows of the Graphene of the present embodiment:
(1) preparation of intercalated graphite: adopt stainless steel substrates as collector, about 2g natural flake graphite is pressed and is placed on collector, obtain working electrode with mould compacting, it is 75 * 40 * 7mm that graphite is pressed into specification
3graphite flake, using stereotype as to electrode, Hg/Hg
2sO
4as reference electrode, formic acid, as electrolytic solution, is put into electrolyzer by three electrodes, and is fully immersed in electrolytic solution; Under room temperature, in current density, be 5mA/cm
2react 20 hours, filter electrolyzer, obtain filter residue, by filter residue washed with de-ionized water, through vacuum drying oven in 60 ℃ be dried 24 hours after, obtain intercalated graphite.
(2) get dried intercalated graphite and install to a small vessels, put in the container that liquid nitrogen is housed, soak 5 minutes; make intercalated graphite cooling rear taking-up completely, being put into temperature is 1100 ℃, in the retort furnace of nitrogen protection; keep taking out afterwards for 30 seconds, obtain the graphene powder of the present embodiment.
Fig. 2 represents is the scanning electron microscope (SEM) photograph (SEM) of the Graphene prepared of the present embodiment.From Fig. 2, can learn, the thickness of Graphene prepared by the present embodiment is about 0.5 nanometer ~ 3.5 nanometer, and graphene sheet layer is more concentrated, peels off respond well.
Through the test of four point probe resistance meter, obtain the specific conductivity of the present embodiment Graphene, refer to table 1.
Embodiment 2
Being prepared as follows of the Graphene of the present embodiment:
(1) preparation of intercalated graphite: adopt stainless steel substrates as collector, about 2g synthetic graphite is pressed and is placed on collector, obtain working electrode with mould compacting, it is 75 * 40 * 7mm that graphite is pressed into specification
3graphite flake, using stereotype as to electrode, Hg/Hg
2sO
4as reference electrode, acetic acid, as electrolytic solution, is put into electrolyzer by three electrodes, and is fully immersed in electrolytic solution; Under room temperature, in current density, be 20mA/cm
2react 1 hour, filter electrolyzer, obtain filter residue, by filter residue washed with de-ionized water, through vacuum drying oven in 70 ℃ be dried 20 hours after, obtain intercalated graphite.
(2) get dried intercalated graphite and install to a small vessels, put in the container that liquid hydrogen is housed, soak 3 minutes; make intercalated graphite cooling rear taking-up completely, being put into temperature is 800 ℃, in the retort furnace of helium protection; keep taking out afterwards for 50 seconds, obtain the graphene powder of the present embodiment.
Through the test of four point probe resistance meter, obtain the specific conductivity of the present embodiment Graphene, refer to table 1.
Embodiment 3
Being prepared as follows of the Graphene of the present embodiment:
(1) preparation of intercalated graphite: adopt stainless steel substrates as collector, about 2g natural flake graphite is positioned on collector, obtain working electrode with mould compacting, it is 75 * 40 * 7mm that graphite is pressed into specification
3graphite flake, using stereotype as to electrode, Hg/Hg
2sO
4as reference electrode, propionic acid, as electrolytic solution, is put into electrolyzer by three electrodes, and is fully immersed in electrolytic solution; Under room temperature, in current density, be 50mA/cm
2react 2 hours, filter electrolyzer, obtain filter residue, by filter residue washed with de-ionized water, through vacuum drying oven in 80 ℃ be dried 12 hours after, obtain intercalated graphite.
(2) get dried intercalated graphite and install to a small vessels, put in the container that liquid hydrogen is housed, soak 1 minute; make intercalated graphite cooling rear taking-up completely, being put into temperature is 1000 ℃, in the retort furnace of argon shield; keep taking out afterwards for 100 seconds, obtain the graphene powder of the present embodiment.
Through the test of four point probe resistance meter, obtain the specific conductivity of the present embodiment Graphene, refer to table 1.
Embodiment 4
Being prepared as follows of the Graphene of the present embodiment:
(1) preparation of intercalated graphite: adopt stainless steel substrates as collector, about 2g synthetic graphite is positioned on collector, obtain working electrode with mould compacting, it is 75 * 40 * 7mm that graphite is pressed into specification
3graphite flake, using stereotype as to electrode, Hg/Hg
2sO
4as reference electrode, concentrated nitric acid (mass percentage concentration is 68%), as electrolytic solution, is put into electrolyzer by three electrodes, and is fully immersed in electrolytic solution; Under room temperature, in current density, be 100mA/cm
2react 5 hours, filter electrolyzer, obtain filter residue, by filter residue washed with de-ionized water, through vacuum drying oven in 75 ℃ be dried 15 hours after, obtain intercalated graphite.
(2) get dried intercalated graphite and install to a small vessels, put in the container that liquid argon is housed, soak 0.5 minute; make intercalated graphite cooling rear taking-up completely, being put into temperature is 1050 ℃, in the retort furnace of nitrogen protection; keep taking out afterwards for 120 seconds, obtain the graphene powder of the present embodiment.
Through the test of four point probe resistance meter, obtain the specific conductivity of the present embodiment Graphene, refer to table 1.
Embodiment 5
Being prepared as follows of the Graphene of the present embodiment:
(1) preparation of intercalated graphite: adopt stainless steel substrates as collector, about 2g natural flake graphite is positioned on collector, obtain working electrode with mould compacting, it is 75 * 40 * 7mm that graphite is pressed into specification
3graphite flake, using stereotype as to electrode, Hg/Hg
2sO
4as reference electrode, the vitriol oil (mass percentage concentration is 98%), as electrolytic solution, is put into electrolyzer by three electrodes, and is fully immersed in electrolytic solution; Under room temperature, in current density, be 80mA/cm
2react 10 hours, filter electrolyzer, obtain filter residue, by filter residue washed with de-ionized water, through vacuum drying oven in 65 ℃ be dried 18 hours after, obtain intercalated graphite.
(2) get dried intercalated graphite and install to a small vessels, put in the container that liquid nitrogen is housed, soak 1 minute; make intercalated graphite cooling rear taking-up completely, being put into temperature is 900 ℃, in the retort furnace of argon shield; keep taking out afterwards for 90 seconds, obtain the graphene powder of the present embodiment.
Through the test of four point probe resistance meter, obtain the specific conductivity of the present embodiment Graphene, refer to table 1.
Embodiment 6
Being prepared as follows of the Graphene of the present embodiment:
(1) preparation of intercalated graphite: adopt stainless steel substrates as collector, about 2g synthetic graphite is positioned on collector, obtain working electrode with mould compacting, it is 75 * 40 * 7mm that graphite is pressed into specification
3graphite flake, using stereotype as to electrode, Hg/Hg
2sO
4as reference electrode, Nitromethane 99Min., as electrolytic solution, is put into electrolyzer by three electrodes, and is fully immersed in electrolytic solution; Under room temperature, in current density, be 40mA/cm
2react 15 hours, filter electrolyzer, obtain filter residue, by filter residue washed with de-ionized water, through vacuum drying oven in 60 ℃ be dried 20 hours after, obtain intercalated graphite.
(2) get dried intercalated graphite and install to a small vessels, put in the container that liquid argon is housed, soak 2 minutes; make intercalated graphite cooling rear taking-up completely, being put into temperature is 950 ℃, in the retort furnace of helium protection; keep taking out afterwards for 60 seconds, obtain the graphene powder of the present embodiment.
Through the test of four point probe resistance meter, obtain the specific conductivity of the present embodiment Graphene, refer to table 1.
Embodiment 7
Being prepared as follows of the Graphene of the present embodiment:
(1) preparation of intercalated graphite: adopt stainless steel substrates as collector, about 2g natural flake graphite is positioned on collector, obtain working electrode with mould compacting, it is 75 * 40 * 7mm that graphite is pressed into specification
3graphite flake, using stereotype as to electrode, Hg/Hg
2sO
4as reference electrode, the mixed solution of acetic acid and Nitromethane 99Min. is as electrolytic solution, and wherein, the volume ratio of acetic acid and Nitromethane 99Min. is 1:1, three electrodes is put into electrolyzer, and be fully immersed in electrolytic solution; Under room temperature, in current density, be 10mA/cm
2react 6 hours, filter electrolyzer, obtain filter residue, by washed with de-ionized water filter residue for, through vacuum drying oven in 80 ℃ be dried 12 hours after, obtain intercalated graphite.
(2) get dried intercalated graphite and install to a small vessels, put in the container that liquid hydrogen is housed, soak 4 minutes; make intercalated graphite cooling rear taking-up completely, being put into temperature is 1000 ℃, in the retort furnace of nitrogen protection; keep taking out afterwards for 30 seconds, obtain the graphene powder of the present embodiment.
Through the test of four point probe resistance meter, obtain the specific conductivity of the present embodiment Graphene, refer to table 1.
Embodiment 8
Being prepared as follows of the Graphene of the present embodiment:
(1) preparation of intercalated graphite: adopt stainless steel substrates as collector, about 2g synthetic graphite is positioned on collector, obtain working electrode with mould compacting, it is 75 * 40 * 7mm that graphite is pressed into specification
3graphite flake, using stereotype as to electrode, Hg/Hg
2sO
4as reference electrode, the mixed solution of formic acid and the vitriol oil (mass percentage concentration of sulfuric acid is 98%) is as electrolytic solution, and wherein, the volume ratio of formic acid and sulfuric acid is 4:1, three electrodes is put into electrolyzer, and be fully immersed in electrolytic solution; Under room temperature, in current density, be 30mA/cm
2react 8 hours, filter electrolyzer, obtain filter residue, by filter residue washed with de-ionized water, through vacuum drying oven in 70 ℃ be dried 15 hours after, obtain intercalated graphite.
(2) get dried intercalated graphite and install to a small vessels, put in the container that liquid argon is housed, soak 5 minutes; make intercalated graphite cooling rear taking-up completely, being put into temperature is 1100 ℃, in the retort furnace of helium protection; keep taking out afterwards for 80 seconds, obtain the graphene powder of the present embodiment.
Through the test of four point probe resistance meter, obtain the specific conductivity of the present embodiment Graphene, refer to table 1.
Embodiment 9
Being prepared as follows of the Graphene of the present embodiment:
(1) preparation of intercalated graphite: adopt stainless steel substrates as collector, about 2g natural flake graphite is positioned on collector, obtain working electrode with mould compacting, it is 75 * 40 * 7mm that graphite is pressed into specification
3graphite flake, using stereotype as to electrode, Hg/Hg
2sO
4as reference electrode, the mixed solution of propionic acid and concentrated nitric acid (mass percentage concentration of nitric acid is 68%) is as electrolytic solution, and wherein, the volume ratio of propionic acid and concentrated nitric acid is that 1:2 puts into electrolyzer by three electrodes, and is fully immersed in electrolytic solution; Under room temperature, in current density, be 5mA/cm
2react 15 hours, filter electrolyzer, obtain filter residue, by filter residue washed with de-ionized water, through vacuum drying oven in 80 ℃ be dried 20 hours after, obtain intercalated graphite.
(2) get dried intercalated graphite and install to a small vessels, put in the container that liquid nitrogen is housed, soak 3 minutes; make intercalated graphite cooling rear taking-up completely, being put into temperature is 900 ℃, in the retort furnace of nitrogen protection; keep taking out afterwards for 120 seconds, obtain the graphene powder of the present embodiment.
Through the test of four point probe resistance meter, obtain the specific conductivity of the present embodiment Graphene, refer to table 1.
Embodiment 10
Being prepared as follows of the Graphene of the present embodiment:
(1) preparation of intercalated graphite: adopt stainless steel substrates as collector, about 2g synthetic graphite is positioned on collector, obtain working electrode with mould compacting, it is 75 * 40 * 7mm that graphite is pressed into specification
3graphite flake, using stereotype as to electrode, Hg/Hg
2sO
4as reference electrode, acetic acid solution, as electrolytic solution, is put into electrolyzer by three electrodes, and is fully immersed in electrolytic solution; Under room temperature, in current density, be 100mA/cm
2react 2 hours, filter electrolyzer, obtain filter residue, by filter residue washed with de-ionized water, through vacuum drying oven in 60 ℃ be dried 18 hours after, obtain intercalated graphite.
(2) get dried intercalated graphite and install to a small vessels, put in the container that liquid argon is housed, soak 2 minutes; make intercalated graphite cooling rear taking-up completely, being put into temperature is 800 ℃, in the retort furnace of argon shield; keep taking out afterwards for 100 seconds, obtain the graphene powder of the present embodiment.
Through the test of four point probe resistance meter, obtain the specific conductivity of the present embodiment Graphene, refer to table 1.
Embodiment 11
Being prepared as follows of the Graphene of the present embodiment:
(1) preparation of intercalated graphite: adopt stainless steel substrates as collector, about 2g synthetic graphite is positioned on collector, obtain working electrode with mould compacting, it is 75 * 40 * 7mm that graphite is pressed into specification
3graphite flake, using stereotype as to electrode, Hg/Hg
2sO
4as reference electrode, Nitromethane 99Min., as electrolytic solution, is put into electrolyzer by three electrodes, and is fully immersed in electrolytic solution; Under room temperature, in current density, be 50mA/cm
2react 1 hour, filter electrolyzer, obtain filter residue, by filter residue washed with de-ionized water, through vacuum drying oven in 80 ℃ be dried 20 hours after, obtain intercalated graphite.
(2) get dried intercalated graphite and install to a small vessels, put in the container that liquid hydrogen is housed, soak 0.5 minute; make intercalated graphite cooling rear taking-up completely, being put into temperature is 1000 ℃, in the retort furnace of nitrogen protection; keep taking out afterwards for 60 seconds, obtain the graphene powder of the present embodiment.
Through the test of four point probe resistance meter, obtain the specific conductivity of the present embodiment Graphene, refer to table 1.
What table 1 represented is productive rate and the specific conductivity of the Graphene of embodiment 1 ~ embodiment 11 preparations.
Table 1
From table 1, can learn, the specific conductivity of the Graphene of embodiment 1 ~ embodiment 11 preparations is 1.4 * 10
4s/m ~ 7.1 * 10
4between S/m,, the specific conductivity of Graphene prepared by traditional oxidation reduction process is only 10
3s/m magnitude, specific conductivity improves greatly.
The above embodiment has only expressed several embodiment of the present invention, and it describes comparatively concrete and detailed, but can not therefore be interpreted as the restriction to the scope of the claims of the present invention.It should be pointed out that for the person of ordinary skill of the art, without departing from the inventive concept of the premise, can also make some distortion and improvement, these all belong to protection scope of the present invention.Therefore, the protection domain of patent of the present invention should be as the criterion with claims.
Claims (9)
1. a preparation method for Graphene, is characterized in that, comprises the steps:
Step 1: graphite is suppressed on stainless steel collector, obtained the working electrode of three-electrode system;
Step 2: prepare intercalated graphite with described three-electrode system;
Step 3: by intercalated graphite described in washed with de-ionized water;
Step 4: the intercalated graphite after cleaning described in vacuum-drying, obtains dried intercalated graphite;
Step 5: described dried intercalated graphite is added and is dipped to the cooling rear taking-up of described intercalated graphite in liquefied gas at low temp;
Step 6: described cooled intercalated graphite is placed in to oxygen-free environment heating and peels off, obtain Graphene.
2. the preparation method of Graphene according to claim 1, is characterized in that, in described three-electrode system, to electrode, is stereotype; Reference electrode is Hg/Hg
2sO
4; Electrolytic solution is pure intercalator.
3. the preparation method of Graphene according to claim 1 and 2, is characterized in that, described graphite is natural flake graphite or synthetic graphite.
4. the preparation method of Graphene according to claim 1, is characterized in that, described step 2 is by electrode, reference electrode and described working electrode are soaked in electrolytic solution jointly, in current density 5mA/cm
2~ 100mA/cm
21 hour ~ 20 hours preparation intercalated graphite of lower reaction.
5. the preparation method of Graphene according to claim 4, is characterized in that, described electrolytic solution is at least one in formic acid, acetic acid, propionic acid, concentrated nitric acid, the vitriol oil and Nitromethane 99Min..
6. the preparation method of Graphene according to claim 1, is characterized in that, described vacuum drying step is that described intercalated graphite is positioned under vacuum condition, at 60 ℃ ~ 80 ℃, is dried 12 hours ~ 24 hours.
7. the preparation method of Graphene according to claim 1, is characterized in that, in described step 5, it is 0.5 minute ~ 5 minutes that described dried intercalated graphite is added to the time of soaking in immersion in liquefied gas at low temp.
8. according to the preparation method of the Graphene described in claim 1 or 7, it is characterized in that, described liquefied gas at low temp is liquid nitrogen, liquid argon or liquid hydrogen.
9. the preparation method of Graphene according to claim 1, is characterized in that, described heating stripping conditions is: 800 ℃ ~ 1100 ℃ of temperature, 30 seconds ~ 120 seconds time.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201210310387.1A CN103628082A (en) | 2012-08-28 | 2012-08-28 | Graphene preparation method |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201210310387.1A CN103628082A (en) | 2012-08-28 | 2012-08-28 | Graphene preparation method |
Publications (1)
| Publication Number | Publication Date |
|---|---|
| CN103628082A true CN103628082A (en) | 2014-03-12 |
Family
ID=50209523
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| CN201210310387.1A Pending CN103628082A (en) | 2012-08-28 | 2012-08-28 | Graphene preparation method |
Country Status (1)
| Country | Link |
|---|---|
| CN (1) | CN103628082A (en) |
Cited By (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN104894594A (en) * | 2015-05-26 | 2015-09-09 | 广东烛光新能源科技有限公司 | Graphene preparation method |
| CN105088261A (en) * | 2014-05-14 | 2015-11-25 | 国能纳米科技有限公司 | Preparation method of graphene |
| CN106435632A (en) * | 2016-09-20 | 2017-02-22 | 南昌大学 | Preparation method for boron-doped graphene |
| CN115074752A (en) * | 2022-06-28 | 2022-09-20 | 北京科技大学 | Laminated electrode for improving molten salt electrolysis graphitization efficiency, preparation and application |
Citations (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US4102960A (en) * | 1976-12-15 | 1978-07-25 | Stackpole Carbon Company | Process for making high strength flexible graphite foil |
| CN1224693A (en) * | 1998-01-24 | 1999-08-04 | 北京华锐新材料技术发展有限公司 | Chemical graft process to prepare expansive graphite |
| CN101460393A (en) * | 2006-06-08 | 2009-06-17 | 戴雷克塔普拉斯专利及科技有限公司 | Production of nano-structures |
| CN102431998A (en) * | 2011-09-20 | 2012-05-02 | 深圳市长宜景鑫投资有限公司 | Method for preparing high-quality graphene in large scale by intercalation stripping of graphite by chemical method |
-
2012
- 2012-08-28 CN CN201210310387.1A patent/CN103628082A/en active Pending
Patent Citations (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US4102960A (en) * | 1976-12-15 | 1978-07-25 | Stackpole Carbon Company | Process for making high strength flexible graphite foil |
| CN1224693A (en) * | 1998-01-24 | 1999-08-04 | 北京华锐新材料技术发展有限公司 | Chemical graft process to prepare expansive graphite |
| CN101460393A (en) * | 2006-06-08 | 2009-06-17 | 戴雷克塔普拉斯专利及科技有限公司 | Production of nano-structures |
| CN102431998A (en) * | 2011-09-20 | 2012-05-02 | 深圳市长宜景鑫投资有限公司 | Method for preparing high-quality graphene in large scale by intercalation stripping of graphite by chemical method |
Non-Patent Citations (1)
| Title |
|---|
| G.M.MORALES等: ""High-quality few layer graphene produced by electrochemical intercalation and microwave-assisted expansion of graphite"", 《CARBON》 * |
Cited By (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN105088261A (en) * | 2014-05-14 | 2015-11-25 | 国能纳米科技有限公司 | Preparation method of graphene |
| CN104894594A (en) * | 2015-05-26 | 2015-09-09 | 广东烛光新能源科技有限公司 | Graphene preparation method |
| CN106435632A (en) * | 2016-09-20 | 2017-02-22 | 南昌大学 | Preparation method for boron-doped graphene |
| CN115074752A (en) * | 2022-06-28 | 2022-09-20 | 北京科技大学 | Laminated electrode for improving molten salt electrolysis graphitization efficiency, preparation and application |
| CN115074752B (en) * | 2022-06-28 | 2024-03-01 | 北京科技大学 | Laminated electrode for improving graphitization efficiency of molten salt electrolysis, preparation and application |
Similar Documents
| Publication | Publication Date | Title |
|---|---|---|
| EP3266743B1 (en) | Method for preparing biomass graphene by using cellulose as raw material | |
| CN102464313B (en) | Preparation method of graphene | |
| CN102942177B (en) | Method for preparing graphene sheet | |
| CN105060288B (en) | A kind of method that Graphene is prepared for raw material with biomass waste material | |
| CN102786045B (en) | Method for preparing oxidized graphene | |
| CN104773730A (en) | Method for preparing graphene | |
| CN103626163A (en) | Graphene preparation method | |
| CN103183334A (en) | Preparation method of size controllable grapheme | |
| CN104071777B (en) | A kind of preparation method of Graphene | |
| CN103626166A (en) | Graphene preparation method | |
| CN104118867A (en) | Preparation method of graphite oxide | |
| CN102583338A (en) | High-quality graphene powder and preparation method thereof | |
| CN103991860A (en) | Nitrogen-doped graphene and preparation method thereof | |
| CN102757035B (en) | Preparation method of graphene | |
| CN104817075A (en) | Preparation method of highly-dispersed graphene oxide nanobelt liquid | |
| CN103569992A (en) | Preparation method of carbon nanotube | |
| CN103628082A (en) | Graphene preparation method | |
| CN104386676A (en) | Preparation method of graphene | |
| CN102464312A (en) | Preparation method of graphene | |
| CN107934947B (en) | Graphene preparation method based on efficient surfactant | |
| CN103387223A (en) | Preparation method of graphite | |
| CN111717911A (en) | Preparation method of graphene film | |
| CN103626164A (en) | Graphene preparation method | |
| CN103359713A (en) | Preparation method of graphene | |
| CN103626165A (en) | Graphene preparation method |
Legal Events
| Date | Code | Title | Description |
|---|---|---|---|
| PB01 | Publication | ||
| PB01 | Publication | ||
| EXSB | Decision made by sipo to initiate substantive examination | ||
| SE01 | Entry into force of request for substantive examination | ||
| WD01 | Invention patent application deemed withdrawn after publication |
Application publication date: 20140312 |
|
| WD01 | Invention patent application deemed withdrawn after publication |