CN102225759A - Low-temperature preparation method of hydroxy-functionalized graphene - Google Patents
Low-temperature preparation method of hydroxy-functionalized graphene Download PDFInfo
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- CN102225759A CN102225759A CN 201110093909 CN201110093909A CN102225759A CN 102225759 A CN102225759 A CN 102225759A CN 201110093909 CN201110093909 CN 201110093909 CN 201110093909 A CN201110093909 A CN 201110093909A CN 102225759 A CN102225759 A CN 102225759A
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- temperature preparation
- ball milling
- hydroxyl functional
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- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical compound [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 title claims abstract description 44
- 238000002360 preparation method Methods 0.000 title claims abstract description 19
- 229910021389 graphene Inorganic materials 0.000 title claims description 33
- KWYUFKZDYYNOTN-UHFFFAOYSA-M Potassium hydroxide Chemical compound [OH-].[K+] KWYUFKZDYYNOTN-UHFFFAOYSA-M 0.000 claims abstract description 27
- 238000000498 ball milling Methods 0.000 claims abstract description 23
- 125000002887 hydroxy group Chemical group [H]O* 0.000 claims abstract description 15
- 239000008367 deionised water Substances 0.000 claims abstract description 9
- 229910021641 deionized water Inorganic materials 0.000 claims abstract description 9
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Chemical compound O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims abstract description 9
- 230000007935 neutral effect Effects 0.000 claims abstract description 4
- 239000007787 solid Substances 0.000 claims abstract description 4
- VYPSYNLAJGMNEJ-UHFFFAOYSA-N Silicium dioxide Chemical compound O=[Si]=O VYPSYNLAJGMNEJ-UHFFFAOYSA-N 0.000 claims description 12
- 229910052799 carbon Inorganic materials 0.000 abstract description 3
- 239000002086 nanomaterial Substances 0.000 abstract description 2
- 238000003801 milling Methods 0.000 abstract 1
- 238000000034 method Methods 0.000 description 5
- XEEYBQQBJWHFJM-UHFFFAOYSA-N Iron Chemical compound [Fe] XEEYBQQBJWHFJM-UHFFFAOYSA-N 0.000 description 4
- -1 hydroxyl Graphene Chemical compound 0.000 description 4
- 230000033444 hydroxylation Effects 0.000 description 3
- 238000005805 hydroxylation reaction Methods 0.000 description 3
- 230000003197 catalytic effect Effects 0.000 description 2
- 238000005229 chemical vapour deposition Methods 0.000 description 2
- 238000002425 crystallisation Methods 0.000 description 2
- 230000008025 crystallization Effects 0.000 description 2
- 239000006185 dispersion Substances 0.000 description 2
- 238000005516 engineering process Methods 0.000 description 2
- 229910052739 hydrogen Inorganic materials 0.000 description 2
- 239000001257 hydrogen Substances 0.000 description 2
- 229910052742 iron Inorganic materials 0.000 description 2
- 239000007788 liquid Substances 0.000 description 2
- 239000000463 material Substances 0.000 description 2
- 238000001556 precipitation Methods 0.000 description 2
- 239000002994 raw material Substances 0.000 description 2
- XMWRBQBLMFGWIX-UHFFFAOYSA-N C60 fullerene Chemical compound C12=C3C(C4=C56)=C7C8=C5C5=C9C%10=C6C6=C4C1=C1C4=C6C6=C%10C%10=C9C9=C%11C5=C8C5=C8C7=C3C3=C7C2=C1C1=C2C4=C6C4=C%10C6=C9C9=C%11C5=C5C8=C3C3=C7C1=C1C2=C4C6=C2C9=C5C3=C12 XMWRBQBLMFGWIX-UHFFFAOYSA-N 0.000 description 1
- 239000004215 Carbon black (E152) Substances 0.000 description 1
- UFHFLCQGNIYNRP-UHFFFAOYSA-N Hydrogen Chemical compound [H][H] UFHFLCQGNIYNRP-UHFFFAOYSA-N 0.000 description 1
- 238000002441 X-ray diffraction Methods 0.000 description 1
- 125000004429 atom Chemical group 0.000 description 1
- 230000009286 beneficial effect Effects 0.000 description 1
- 230000005540 biological transmission Effects 0.000 description 1
- 239000002041 carbon nanotube Substances 0.000 description 1
- 229910021393 carbon nanotube Inorganic materials 0.000 description 1
- 230000006378 damage Effects 0.000 description 1
- 238000000502 dialysis Methods 0.000 description 1
- 239000002270 dispersing agent Substances 0.000 description 1
- 230000002349 favourable effect Effects 0.000 description 1
- 125000000524 functional group Chemical group 0.000 description 1
- 229910002804 graphite Inorganic materials 0.000 description 1
- 239000010439 graphite Substances 0.000 description 1
- 239000007770 graphite material Substances 0.000 description 1
- 229930195733 hydrocarbon Natural products 0.000 description 1
- 150000002430 hydrocarbons Chemical class 0.000 description 1
- 125000004435 hydrogen atom Chemical class [H]* 0.000 description 1
- 125000004356 hydroxy functional group Chemical group O* 0.000 description 1
- 239000010410 layer Substances 0.000 description 1
- 239000012528 membrane Substances 0.000 description 1
- 239000000203 mixture Substances 0.000 description 1
- 229910021421 monocrystalline silicon Inorganic materials 0.000 description 1
- 229920000642 polymer Polymers 0.000 description 1
- 239000002356 single layer Substances 0.000 description 1
- 229910001220 stainless steel Inorganic materials 0.000 description 1
- 239000010935 stainless steel Substances 0.000 description 1
- 239000000126 substance Substances 0.000 description 1
- 238000001291 vacuum drying Methods 0.000 description 1
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Abstract
The invention relates to a novel and simple low-temperature preparation method of hydroxy-functionalized grapheme, belonging to the field of novel carbon nanomaterials. The preparation method provided by the invention comprises the following steps of: adding graphite powder and potassium hydroxide solid to a ball milling tank, then adding milling balls to the ball milling tank, placing the ball milling tank in a ball mill, continuously ball-milling under air blast and room temperature conditions at a speed of 200-400 r/min for 10-16 hours, transferring the ball-mill product to a sample bottle by deionized water, and then removing unreacted potassium hydroxide by deionized water until the solution was neutral. By using the preparation method provided by the invention, hydroxy-functionalized grapheme can be prepared at room temperature, and the hydroxy-functionalized grapheme has a lamellar structure, contains a large number of hydroxyl groups on the surface, well remained internal structure and a high crystallinity.
Description
Technical field
The present invention relates to a kind of low temperature preparation method of novel easy hydroxyl functional Graphene, belong to novel carbon nanomaterial field.
Background technology
Graphene is a kind of two-dimentional atomic structure of carbon of finding in recent years, and thickness in monolayer only is the graphite material of an atom thick, and has become one of at present the most popular research field.Graphene still is the basic structural unit of zero dimension soccerballene, one dimension carbon nanotube and three-dimensional graphite, thereby has the character of many uniquenesses.As big specific surface area, excellent electronic conduction character, excellent mechanical property and extra light quality.These unique character make it have huge application potential in biotechnology and life science, and it still makes nano electron device---the best materials of RF transistors.In addition, the derivative of its functionalization---graphene oxide also is a kind of important function material.
Existing preparation method of graphene mainly is a chemical Vapor deposition process.The main process of chemical Vapor deposition process is to be raw material with the hydrocarbon polymer, is serving as on the metallic membrane of catalyzer, and high-temperature catalytic decomposes raw material, in the presence of hydrogen, thereby obtains a layer graphene on its surface.But it needs higher temperature, and it is dangerous big and foreign matter content is more and limited its application that high temperature feeds hydrogen down.
Summary of the invention
Need high-temperature catalytic to cause dangerous bigger technical problem for solving existing graphene preparation method existence, the invention provides a kind of low temperature preparation method of hydroxyl functional Graphene.
For solving the problems of the technologies described above, the present invention adopts following technical scheme:
A kind of low temperature preparation method of hydroxyl functional Graphene, it is characterized in that: Graphite Powder 99 and potassium hydroxide solid are joined among the ball milling tank body, add at the ball milling tank body then and carry out spin, again ball grinder is put into ball mill, under air blast and normal temperature condition, after the continuous ball milling 10-16 of 200-400 rev/min speed hour, the ball milling product is transferred in the sample bottle with deionized water, and then with deionized water unreacted potassium hydroxide is removed, be neutral until solution.
The weight ratio of Graphite Powder 99 and oxyhydroxide is preferably 1:15 ~ 1:20, preferably 1:20.
The order number of the Graphite Powder 99 among the present invention is-100.
Spin is preferably selected agate ball for use among the present invention.Because potassium hydroxide is alkaline high, corrodibility is very strong, and other spheroids (as stainless steel iron ball or iron content mixture spheroid) easily are corroded.Agate ball then can not be corroded
The diameter of above-mentioned agate ball is 3mm.
Above-mentioned agate ball add-on accounts for 1/5th of agate jar volume.
The invention has the beneficial effects as follows: adopt aforesaid method, can obtain the hydroxyl Graphene at normal temperatures, this hydroxyl Graphene is laminated structure, and great amount of hydroxy group functional group is contained on its surface, and the internal structure of Graphene remains intact, and crystallization degree is higher.
Description of drawings
The infrared spectrogram of the hydroxylation Graphene that Fig. 1 makes for the embodiment of the invention.
Fig. 2 schemes for the SEM of the hydroxylation Graphene that example of the present invention makes.
The XRD figure of the hydroxylation Graphene that Fig. 3 makes for example of the present invention.
The figure as a result that Fig. 4 investigates for rotational speed of ball-mill of the present invention.
The figure as a result that Fig. 5 investigated for the ball milling time.
Embodiment
With the 10mg specification is-100 purpose flaky graphite powder and 200mg potassium hydroxide solid, joins among the agate jar body of 250ml, and adding exsiccant diameter is that the agate ball of 3mm carries out ball milling, and add-on accounts for 1/5th of agate jar volume.Then ball grinder is put into ball mill, under air blast and normal temperature condition, after the continuous ball milling 10-16 of 200-400 rev/min speed hour, the ball milling product is transferred in the sample bottle of 20ml with the 10ml deionized water.Then it is packed into and change deionized water repeatedly in the dialysis tubing unreacted potassium hydroxide is removed, be neutral until solution.Obtain the hydroxyl Graphene of favorable dispersity.
Dispersant liquid drop on smooth monocrystalline silicon piece, is put into vacuum drying oven, and vacuum tightness is 0.1Pa, dried overnight.Obtain the chemical structure on Graphene surface after measuring by Fourier infrared spectrograph; It is laminated structure to utilize transmission electron microscope observation, and X-ray diffraction analysis finds that the grafting of hydroxyl does not change the internal structure of Graphene, and degree of crystallinity is good.
As can be seen from Figure 1, with to add 150mgKOH(be that the weight ratio of Graphite Powder 99 and oxyhydroxide is 1:15) compare, the weight ratio that adds 200mgKOH(and be Graphite Powder 99 and oxyhydroxide is 1:20) behind the ball milling, hydroxyl peak obviously strengthens (near the 3400cm-1), illustrates that the Graphene surface contains more hydroxy functional group.
By among Fig. 2 as can be seen, obtained flaky Graphene by above preparation method.
We can learn from Fig. 3, and the Graphene internal crystallization degree that adopts above preparation method to obtain good (peak is thin and sharp) illustrates that the hydroxyl Graphene that adopts present method to prepare is less to the destruction of its internal structure.
As can be seen from Figure 4, when rotating speed is 200r/min, obtain the product maximum (charateristic avsorption band of Graphene is positioned at about 260nm approximately) of Graphene.
Fig. 5. be that ball milling 4h, 8h, 16h after product have just been transferred to the deployment conditions in the deionized water from left to right successively among a figure, we can find that precipitation appears rapidly in ball milling 4h after product, and ball milling 8h and 16h then present more uniform dispersion liquid.Fig. 5. b figure is with spend the night deployment conditions after leaving standstill of above-mentioned three's solution, and finding spends the night leaves standstill the also appearance precipitation of back ball milling 8h, but ball milling 16h still present good dispersion state, thereby confirm that the best ball milling time is 10-16h.
Claims (7)
1. the low temperature preparation method of a hydroxyl functional Graphene, it is characterized in that: Graphite Powder 99 and potassium hydroxide solid are joined among the ball milling tank body, add at the ball milling tank body then and carry out spin, again ball grinder is put into ball mill, under air blast and normal temperature condition, after the continuous ball milling 10-16 of 200-400 rev/min speed hour, the ball milling product is transferred in the sample bottle with deionized water, and then with deionized water unreacted potassium hydroxide is removed, be neutral until solution.
2. the low temperature preparation method of hydroxyl functional Graphene as claimed in claim 1 is characterized in that: the weight ratio of Graphite Powder 99 and oxyhydroxide is 1:15 ~ 1:20.
3. the low temperature preparation method of hydroxyl functional Graphene as claimed in claim 2 is characterized in that: the weight ratio of Graphite Powder 99 and oxyhydroxide is 1:20.
4. the low temperature preparation method of hydroxyl functional Graphene as claimed in claim 1 is characterized in that: the order number of described Graphite Powder 99 is-100.
5. the low temperature preparation method of hydroxyl functional Graphene as claimed in claim 1 is characterized in that: described spin is an agate ball.
6. the low temperature preparation method of hydroxyl functional Graphene as claimed in claim 4 is characterized in that: the diameter of described agate ball is 3mm.
7. the low temperature preparation method of hydroxyl functional Graphene as claimed in claim 5 is characterized in that: the agate ball add-on accounts for 1/5th of agate jar volume.
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