CN105366663A - Method for doping synthesized sulfur with graphene - Google Patents
Method for doping synthesized sulfur with graphene Download PDFInfo
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- CN105366663A CN105366663A CN201410429208.5A CN201410429208A CN105366663A CN 105366663 A CN105366663 A CN 105366663A CN 201410429208 A CN201410429208 A CN 201410429208A CN 105366663 A CN105366663 A CN 105366663A
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- graphene
- sulfur doping
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- graphene oxide
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- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical compound [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 title claims abstract description 115
- 229910021389 graphene Inorganic materials 0.000 title claims abstract description 102
- NINIDFKCEFEMDL-UHFFFAOYSA-N Sulfur Chemical compound [S] NINIDFKCEFEMDL-UHFFFAOYSA-N 0.000 title claims abstract description 60
- 229910052717 sulfur Inorganic materials 0.000 title claims abstract description 45
- 239000011593 sulfur Substances 0.000 title claims abstract description 45
- 238000000034 method Methods 0.000 title claims abstract description 37
- RWSOTUBLDIXVET-UHFFFAOYSA-N Dihydrogen sulfide Chemical compound S RWSOTUBLDIXVET-UHFFFAOYSA-N 0.000 claims abstract description 21
- 239000007789 gas Substances 0.000 claims abstract description 21
- 229910000037 hydrogen sulfide Inorganic materials 0.000 claims abstract description 21
- 229910002804 graphite Inorganic materials 0.000 claims abstract description 12
- 239000010439 graphite Substances 0.000 claims abstract description 12
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims abstract description 7
- 238000001035 drying Methods 0.000 claims abstract description 3
- IJGRMHOSHXDMSA-UHFFFAOYSA-N Atomic nitrogen Chemical compound N#N IJGRMHOSHXDMSA-UHFFFAOYSA-N 0.000 claims description 14
- 230000003647 oxidation Effects 0.000 claims description 8
- 238000007254 oxidation reaction Methods 0.000 claims description 8
- 238000006243 chemical reaction Methods 0.000 claims description 7
- 229910052757 nitrogen Inorganic materials 0.000 claims description 7
- XKRFYHLGVUSROY-UHFFFAOYSA-N Argon Chemical compound [Ar] XKRFYHLGVUSROY-UHFFFAOYSA-N 0.000 claims description 4
- 230000035484 reaction time Effects 0.000 claims description 4
- 229910052786 argon Inorganic materials 0.000 claims description 2
- 239000001307 helium Substances 0.000 claims description 2
- 229910052734 helium Inorganic materials 0.000 claims description 2
- SWQJXJOGLNCZEY-UHFFFAOYSA-N helium atom Chemical compound [He] SWQJXJOGLNCZEY-UHFFFAOYSA-N 0.000 claims description 2
- 238000000859 sublimation Methods 0.000 claims description 2
- 230000008022 sublimation Effects 0.000 claims description 2
- 238000002360 preparation method Methods 0.000 abstract description 6
- 230000008014 freezing Effects 0.000 abstract 1
- 238000007710 freezing Methods 0.000 abstract 1
- 238000009776 industrial production Methods 0.000 abstract 1
- 239000011261 inert gas Substances 0.000 abstract 1
- 238000002441 X-ray diffraction Methods 0.000 description 13
- 239000005864 Sulphur Substances 0.000 description 12
- 238000001228 spectrum Methods 0.000 description 12
- 229910052799 carbon Inorganic materials 0.000 description 8
- 230000005540 biological transmission Effects 0.000 description 7
- 230000008569 process Effects 0.000 description 5
- 239000008367 deionised water Substances 0.000 description 4
- 229910021641 deionized water Inorganic materials 0.000 description 4
- 238000005516 engineering process Methods 0.000 description 4
- 239000000758 substrate Substances 0.000 description 4
- 150000001721 carbon Chemical group 0.000 description 3
- 238000004519 manufacturing process Methods 0.000 description 3
- 239000000463 material Substances 0.000 description 3
- VLKZOEOYAKHREP-UHFFFAOYSA-N n-Hexane Chemical compound CCCCCC VLKZOEOYAKHREP-UHFFFAOYSA-N 0.000 description 3
- 229910021382 natural graphite Inorganic materials 0.000 description 3
- 125000004429 atom Chemical group 0.000 description 2
- 230000015572 biosynthetic process Effects 0.000 description 2
- 239000003054 catalyst Substances 0.000 description 2
- 239000003795 chemical substances by application Substances 0.000 description 2
- 238000005229 chemical vapour deposition Methods 0.000 description 2
- 239000002184 metal Substances 0.000 description 2
- 229910021426 porous silicon Inorganic materials 0.000 description 2
- 239000000376 reactant Substances 0.000 description 2
- 238000006722 reduction reaction Methods 0.000 description 2
- 230000002829 reductive effect Effects 0.000 description 2
- 239000011232 storage material Substances 0.000 description 2
- 238000003786 synthesis reaction Methods 0.000 description 2
- 230000002194 synthesizing effect Effects 0.000 description 2
- ZOXJGFHDIHLPTG-UHFFFAOYSA-N Boron Chemical compound [B] ZOXJGFHDIHLPTG-UHFFFAOYSA-N 0.000 description 1
- UFHFLCQGNIYNRP-UHFFFAOYSA-N Hydrogen Chemical compound [H][H] UFHFLCQGNIYNRP-UHFFFAOYSA-N 0.000 description 1
- 238000010521 absorption reaction Methods 0.000 description 1
- 229910003481 amorphous carbon Inorganic materials 0.000 description 1
- 230000003321 amplification Effects 0.000 description 1
- QVGXLLKOCUKJST-UHFFFAOYSA-N atomic oxygen Chemical compound [O] QVGXLLKOCUKJST-UHFFFAOYSA-N 0.000 description 1
- 230000008901 benefit Effects 0.000 description 1
- 229910052796 boron Inorganic materials 0.000 description 1
- 239000006227 byproduct Substances 0.000 description 1
- 238000006555 catalytic reaction Methods 0.000 description 1
- 230000008859 change Effects 0.000 description 1
- 238000005336 cracking Methods 0.000 description 1
- 239000013078 crystal Substances 0.000 description 1
- 230000007547 defect Effects 0.000 description 1
- 238000009792 diffusion process Methods 0.000 description 1
- 239000006185 dispersion Substances 0.000 description 1
- 230000000694 effects Effects 0.000 description 1
- 239000007772 electrode material Substances 0.000 description 1
- 238000010894 electron beam technology Methods 0.000 description 1
- 238000004146 energy storage Methods 0.000 description 1
- 125000000524 functional group Chemical group 0.000 description 1
- 125000005842 heteroatom Chemical group 0.000 description 1
- 239000001257 hydrogen Substances 0.000 description 1
- 229910052739 hydrogen Inorganic materials 0.000 description 1
- 238000011031 large-scale manufacturing process Methods 0.000 description 1
- 239000011159 matrix material Substances 0.000 description 1
- 239000000203 mixture Substances 0.000 description 1
- 238000003199 nucleic acid amplification method Methods 0.000 description 1
- 150000002894 organic compounds Chemical class 0.000 description 1
- 239000001301 oxygen Substances 0.000 description 1
- 229910052760 oxygen Inorganic materials 0.000 description 1
- 239000002245 particle Substances 0.000 description 1
- 239000000843 powder Substances 0.000 description 1
- 230000009467 reduction Effects 0.000 description 1
- 239000004065 semiconductor Substances 0.000 description 1
- 239000000126 substance Substances 0.000 description 1
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- Carbon And Carbon Compounds (AREA)
Abstract
The invention relates to a method for doping synthesized sulfur with graphene. The problems that in the prior art, a sulfur-doped graphene preparation process is complex, high in cost and low in yield are mainly solved. Through the technical scheme of the method including the following steps of a, conducting ultrasonic stripping on graphite oxide in water to obtain a graphene oxide solution; b, freezing and drying the graphene oxide solution to obtain porous graphene oxide gel; c, making porous graphene oxide gel react with mixed gas of hydrogen sulfide and inert gas to obtain sulfur-doped graphene, the problems are well solved, and the method can be used for industrial production of sulfur-doped graphene.
Description
Technical field
The present invention relates to a kind of method of synthesizing sulfur doping Graphene.
Background technology
Graphene is with sp by carbon atom
2the two dimensional crystal material of hybridized orbital composition hexagonal network structure, there is very excellent performance, as high electronic mobility, good thermal conductivity, light transmission and good stability, can be applicable to the fields such as semiconductor material, matrix material, battery electrode material, hydrogen storage material, field emmision material and hypersensor.Doping is the effective way changing Graphene electronic structure and chemical property.The lattice that hetero atom is graphene-doped, not only effectively can introduce band gap, and can increase the defect of Graphene and the reactive behavior of local, thus produces many new functions.Research finds that nitrogen, boron or phosphoric also effectively can change its performance by graphene-doped lattice, and relatively less to the research of other element doping.
Element sulphur is a kind of potential doped element theoretically, but sulphur atom differs more with carbon atom radius, and electronegativity is close with carbon atom, therefore element sulphur be not easy graphene-doped lattice.Patent CN201110095599.8 discloses a kind of preparation method of sulfur-doped graphene films, its respectively with sulphur powder and hexane for sulphur source and carbon source, chemical Vapor deposition process is adopted to grow sulfur-doped graphene films on the metallic substrate, but the method needs complicated metal catalyst pretreatment technology, yield poorly, cost is high, is difficult to scale operation.M ü llen etc. reports a kind of method (AdvancedFunctionalMaterials preparing sulfur doping Graphene and nitrogen-doped graphene on porous silicon plate; 2012; 22; 3634-3640.); it adopts hydrogen sulfide to do reductive agent and doping sulphur source; the element sulphur doping of Graphene is realized while high temperature reduction graphene oxide; but the method need use porous silicon plate to support dispersion graphene oxide; increase technical process and production cost; limits throughput, is unfavorable for large-scale production.
Summary of the invention
Technical problem to be solved by this invention is that prior art exists sulfur doping Graphene complicated process of preparation, cost is high, the problem yielded poorly, and provides a kind of method of synthesis sulfur doping Graphene newly.The method can be used for preparation of industrialization sulfur doping Graphene, has the advantage that technique is simple, cost is low, be easy to industry amplification.
For solving the problems of the technologies described above, the technical solution used in the present invention is as follows: a kind of method of synthesizing sulfur doping Graphene, comprises the following steps:
A) by graphite oxide ultrasonic stripping in water, graphene oxide solution is obtained;
B) by described graphene oxide solution lyophilize, porous oxidation Graphene gel is obtained;
C) by the mixed gas reaction of described porous oxidation Graphene gel and hydrogen sulfide and rare gas element, described sulfur doping Graphene is obtained.
In technique scheme, preferably, step a) ultrasonic splitting time be 0.5 ~ 2 hour.
In technique scheme, preferably, the concentration of described graphene oxide solution is 0.1 ~ 7 mg/ml.More preferably, the concentration of described graphene oxide solution is 0.5 ~ 5 mg/ml.
In technique scheme, preferably, step b) lyophilize temperature is-10 ~-50 DEG C, sublimation drying is 12 ~ 48 hours.
In technique scheme, preferably, in the mixed gas of described hydrogen sulfide and rare gas element, the volume percent of hydrogen sulfide is 5 ~ 30%
In technique scheme, preferably, described rare gas element is at least one in nitrogen, argon gas or helium.
In technique scheme, preferably, step c) temperature of reaction is 500 ~ 1000 DEG C, the reaction times is 5 minutes ~ 3 hours.More preferably, temperature of reaction is 550 ~ 900 DEG C, and the reaction times is 10 minutes ~ 2 hours.
In technique scheme, preferably, in hydrogen sulfide and graphene oxide solution, the weight ratio of graphene oxide is 1 ~ 50.
In the present invention, take graphene oxide as presoma, obtain homodisperse graphene oxide solution by ultrasonic stripping, after lyophilize, obtain the graphene oxide gel of holey; When the mixed gas pyroreaction with hydrogen sulfide and rare gas element, hydrogen sulfide is diffused into surface of graphene oxide by porous network structure, with oxygen-containing functional group generation reduction reaction and the doping reaction of surface of graphene oxide, while redox graphene, achieve the element sulphur doping of Graphene.
Compared with prior art, the present invention obtains the graphene oxide of holey by lyophilize process graphene oxide solution, this vesicular structure is conducive to the diffusion of reactant gases, avoid in conventional art as increasing the contact area of graphene oxide and reactant gases and the mode that adopts substrate to support, simplify preparation technology, reduce the cost using substrate, improve treatment capacity; The present invention prepares sulfur doping Graphene by redox graphene, and avoid the metal catalyst substrate processing step of complexity during chemical Vapor deposition process production Graphene, technique is simpler, and cost is cheaper, and treatment capacity is larger; The present invention adopts hydrogen sulfide to do reductive agent and sulphur source, and the by products such as the amorphous carbon produced when avoiding cracking sulfur-containing organic compound, make the sulfur doping Graphene of preparation purer; In the present invention the treatment capacity of sulfur doping Graphene large, be easy to mass-producing and amplify, can be applicable in the suitability for industrialized production of sulfur doping Graphene, meet the fields such as absorption, catalysis and energy storage material to the throughput requirements of sulfur doping Graphene, achieve good technique effect.
Accompanying drawing explanation
Fig. 1 is X-ray diffraction spectrum (XRD) figure of natural graphite, graphite oxide and sulfur doping Graphene in the present invention's [embodiment 1].Wherein, A is natural graphite, and B is graphite oxide, and C is sulfur doping Graphene.
Fig. 2 is scanning electronic microscope (SEM) figure of sulfur doping Graphene prepared by the present invention's [embodiment 1].
Fig. 3 is transmission electron microscope (TEM) figure of sulfur doping Graphene prepared by the present invention's [embodiment 1].
Fig. 4 is x-ray photoelectron power spectrum (XPS) figure of S2p in the sulfur doping Graphene prepared of the present invention's [embodiment 1].
Fig. 1 is X-ray diffraction spectrum (XRD) figure of natural graphite, graphite oxide and sulfur doping Graphene.Sulfur doping Graphene is in 2 θ=26.6 belonging to graphite
0place, and 2 θ=10.8 of graphite oxide
0place, all without obvious XRD diffraction peak, has Graphene X ray diffracting characteristic.
Fig. 2 is scanning electronic microscope (SEM) figure of sulfur doping Graphene.Transparent spun silk shape graphene sheet layer is mutually stacking, forms the Graphene particle of bulk multi-hole.
Fig. 3 is transmission electron microscope (TEM) figure of sulfur doping Graphene, a few near-transparent of graphene film under electron beam irradiation, the gauffer that surface presentation is intrinsic.
Fig. 4 is x-ray photoelectron power spectrum (XPS) figure of S2p in sulfur doping Graphene, and wherein peak, 163.9eV place corresponds to C-S-C2p
3/2key, peak, 165.1eV place corresponds to C-S-C2p
1/2key, peak, 168.5eV place corresponds to C-SO
x-C key, show part sulphur atom alternate c atoms enter in Graphene lattice.
Below by embodiment, the invention will be further elaborated.
Embodiment
[embodiment 1]
The ultrasonic stripping in 100 ml deionized water of 300 milligrams of graphite oxides is prepared 3 mg/ml graphene oxide solution for 1.5 hours, at-40 DEG C, lyophilize obtains porous oxidation Graphene gel in 24 hours, the volume percent passing into hydrogen sulfide is the hydrogen sulfide of 20% and the mixed gas of nitrogen, react 30 minutes at 900 DEG C, be cooled to room temperature, i.e. obtained sulfur doping Graphene, wherein the atomic percentage conc of sulphur is 1.65%.
Obtained sulfur doping Graphene X-ray diffraction spectrum (XRD) figure, scanning electronic microscope (SEM) figure, transmission electron microscope (TEM) figure, and x-ray photoelectron power spectrum (XPS) figure is shown in accompanying drawing, show sulphur atom alternate c atoms enter in Graphene lattice.
[embodiment 2]
The ultrasonic stripping in 100 ml deionized water of 50 milligrams of graphite oxides is prepared 0.5 mg/ml graphene oxide solution for 1 hour, at-40 DEG C, lyophilize obtains porous oxidation Graphene gel in 48 hours, the volume percent passing into hydrogen sulfide is the hydrogen sulfide of 5% and the mixed gas of nitrogen, react 2 hours at 550 DEG C, be cooled to room temperature, i.e. obtained sulfur doping Graphene, wherein the atomic percentage conc of sulphur is 2.37%.
Obtained sulfur doping Graphene X-ray diffraction spectrum (XRD) figure, scanning electronic microscope (SEM) figure, transmission electron microscope (TEM) figure, and x-ray photoelectron power spectrum (XPS) figure is similar to [embodiment 1].
[embodiment 3]
The ultrasonic stripping in 100 ml deionized water of 500 milligrams of graphite oxides is prepared 5 mg/ml graphene oxide solution for 2 hours, at-20 DEG C, lyophilize obtains porous oxidation Graphene gel in 12 hours, the volume percent passing into hydrogen sulfide is the hydrogen sulfide of 30% and the mixed gas of nitrogen, react 1 hour at 900 DEG C, be cooled to room temperature, i.e. obtained sulfur doping Graphene, wherein the atomic percentage conc of sulphur is 1.53%.
Obtained sulfur doping Graphene X-ray diffraction spectrum (XRD) figure, scanning electronic microscope (SEM) figure, transmission electron microscope (TEM) figure, and x-ray photoelectron power spectrum (XPS) figure is similar to [embodiment 1].
[embodiment 4]
The ultrasonic stripping in 100 ml deionized water of 200 milligrams of graphite oxides is prepared 2 mg/ml graphene oxide solution for 1.5 hours, at-30 DEG C, lyophilize obtains porous oxidation Graphene gel in 36 hours, the volume percent passing into hydrogen sulfide is the hydrogen sulfide of 10% and the mixed gas of nitrogen, react 1.5 hours at 800 DEG C, be cooled to room temperature, i.e. obtained sulfur doping Graphene, wherein the atomic percentage conc of sulphur is 1.73%.
Obtained sulfur doping Graphene X-ray diffraction spectrum (XRD) figure, scanning electronic microscope (SEM) figure, transmission electron microscope (TEM) figure, and x-ray photoelectron power spectrum (XPS) figure is similar to [embodiment 1].
Claims (10)
1. synthesize a method for sulfur doping Graphene, comprise the following steps:
A) by graphite oxide ultrasonic stripping in water, graphene oxide solution is obtained;
B) by described graphene oxide solution lyophilize, porous oxidation Graphene gel is obtained;
C) by the mixed gas reaction of described porous oxidation Graphene gel and hydrogen sulfide and rare gas element, described sulfur doping Graphene is obtained.
2. synthesize the method for sulfur doping Graphene according to claim 1, it is characterized in that step a) ultrasonic splitting time be 0.5 ~ 2 hour.
3. synthesize the method for sulfur doping Graphene according to claim 1, it is characterized in that the concentration of described graphene oxide solution is 0.1 ~ 7 mg/ml.
4. synthesize the method for sulfur doping Graphene according to claim 3, it is characterized in that the concentration of described graphene oxide solution is 0.5 ~ 5 mg/ml.
5. synthesize the method for sulfur doping Graphene according to claim 1, it is characterized in that step b) lyophilize temperature is-10 ~-50 DEG C, sublimation drying is 12 ~ 48 hours.
6. synthesize the method for sulfur doping Graphene according to claim 1, it is characterized in that the volume percent of hydrogen sulfide in the mixed gas of described hydrogen sulfide and rare gas element is 5 ~ 30%.
7. synthesize the method for sulfur doping Graphene according to claim 1, it is characterized in that described rare gas element is at least one in nitrogen, argon gas or helium.
8. synthesize the method for sulfur doping Graphene according to claim 1, it is characterized in that step c) temperature of reaction is 500 ~ 1000 DEG C, the reaction times is 5 minutes ~ 3 hours.
9. synthesize the method for sulfur doping Graphene according to claim 8, it is characterized in that step c) temperature of reaction is 550 ~ 900 DEG C, the reaction times is 10 minutes ~ 2 hours.
10. synthesize the method for sulfur doping Graphene according to claim 1, it is characterized in that the weight ratio of graphene oxide in hydrogen sulfide and graphene oxide solution is 1 ~ 50.
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Cited By (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN108039464A (en) * | 2017-11-30 | 2018-05-15 | 暨南大学 | A kind of self-supporting sodium ions to potassium ions battery material and preparation method and application |
| CN108046240A (en) * | 2017-12-13 | 2018-05-18 | 南京红太阳新能源有限公司 | A kind of preparation method of the graphene composite material of nitrogen thiation |
| CN108545714A (en) * | 2018-05-13 | 2018-09-18 | 程桂平 | A kind of preparation method of sulfur-bearing nitrogen-doped carbon |
Citations (3)
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|---|---|---|---|---|
| CN102191476A (en) * | 2011-04-11 | 2011-09-21 | 兰州大学 | Method for preparing sulfur-doped graphene films |
| CN102583340A (en) * | 2012-01-20 | 2012-07-18 | 中国科学院上海硅酸盐研究所 | High-conductivity graphene material with low-temperature gas-phase reduction and preparation method thereof |
| CN103387226A (en) * | 2013-07-05 | 2013-11-13 | 清华大学深圳研究生院 | Preparation method for graphene |
-
2014
- 2014-08-27 CN CN201410429208.5A patent/CN105366663A/en active Pending
Patent Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN102191476A (en) * | 2011-04-11 | 2011-09-21 | 兰州大学 | Method for preparing sulfur-doped graphene films |
| CN102583340A (en) * | 2012-01-20 | 2012-07-18 | 中国科学院上海硅酸盐研究所 | High-conductivity graphene material with low-temperature gas-phase reduction and preparation method thereof |
| CN103387226A (en) * | 2013-07-05 | 2013-11-13 | 清华大学深圳研究生院 | Preparation method for graphene |
Non-Patent Citations (1)
| Title |
|---|
| HWEE LING POH,ET AL.: "Sulfur-Doped Graphene via Thermal Exfoliation of Graphite Oxide in H2S, SO2, or CS2 Gas", 《ACS NANO》 * |
Cited By (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN108039464A (en) * | 2017-11-30 | 2018-05-15 | 暨南大学 | A kind of self-supporting sodium ions to potassium ions battery material and preparation method and application |
| CN108046240A (en) * | 2017-12-13 | 2018-05-18 | 南京红太阳新能源有限公司 | A kind of preparation method of the graphene composite material of nitrogen thiation |
| CN108545714A (en) * | 2018-05-13 | 2018-09-18 | 程桂平 | A kind of preparation method of sulfur-bearing nitrogen-doped carbon |
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Application publication date: 20160302 |