CN104465127A - Method for rapid preparation of grapheme/silver sulfide quantum dot nanocomposite and product - Google Patents
Method for rapid preparation of grapheme/silver sulfide quantum dot nanocomposite and product Download PDFInfo
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- 229910052946 acanthite Inorganic materials 0.000 title claims abstract description 47
- 229940056910 silver sulfide Drugs 0.000 title claims abstract description 47
- XUARKZBEFFVFRG-UHFFFAOYSA-N silver sulfide Chemical compound [S-2].[Ag+].[Ag+] XUARKZBEFFVFRG-UHFFFAOYSA-N 0.000 title claims abstract description 45
- 239000002096 quantum dot Substances 0.000 title claims abstract description 40
- 239000002114 nanocomposite Substances 0.000 title claims abstract description 31
- 238000000034 method Methods 0.000 title claims abstract description 22
- 238000002360 preparation method Methods 0.000 title claims abstract description 12
- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical compound [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 claims abstract description 78
- 229910021389 graphene Inorganic materials 0.000 claims abstract description 76
- CSCPPACGZOOCGX-UHFFFAOYSA-N Acetone Chemical compound CC(C)=O CSCPPACGZOOCGX-UHFFFAOYSA-N 0.000 claims abstract description 14
- IAZDPXIOMUYVGZ-UHFFFAOYSA-N Dimethylsulphoxide Chemical compound CS(C)=O IAZDPXIOMUYVGZ-UHFFFAOYSA-N 0.000 claims abstract description 13
- SQGYOTSLMSWVJD-UHFFFAOYSA-N silver(1+) nitrate Chemical compound [Ag+].[O-]N(=O)=O SQGYOTSLMSWVJD-UHFFFAOYSA-N 0.000 claims abstract description 11
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 claims abstract description 10
- 239000002356 single layer Substances 0.000 claims abstract description 10
- 238000001291 vacuum drying Methods 0.000 claims abstract description 3
- 239000000463 material Substances 0.000 claims description 36
- 238000005119 centrifugation Methods 0.000 claims description 16
- 239000002131 composite material Substances 0.000 claims description 15
- 239000000047 product Substances 0.000 claims description 11
- 229960001760 dimethyl sulfoxide Drugs 0.000 claims description 7
- 239000000376 reactant Substances 0.000 claims description 6
- 229910001961 silver nitrate Inorganic materials 0.000 claims description 4
- 239000012153 distilled water Substances 0.000 claims description 2
- 239000003960 organic solvent Substances 0.000 claims description 2
- 238000004506 ultrasonic cleaning Methods 0.000 claims description 2
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Chemical compound O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims description 2
- 239000006228 supernatant Substances 0.000 claims 1
- 238000006243 chemical reaction Methods 0.000 abstract description 6
- 238000004519 manufacturing process Methods 0.000 abstract description 5
- 230000008901 benefit Effects 0.000 abstract description 3
- 235000019441 ethanol Nutrition 0.000 abstract 1
- 238000000926 separation method Methods 0.000 abstract 1
- 239000002105 nanoparticle Substances 0.000 description 6
- BQCADISMDOOEFD-UHFFFAOYSA-N Silver Chemical compound [Ag] BQCADISMDOOEFD-UHFFFAOYSA-N 0.000 description 5
- 230000002194 synthesizing effect Effects 0.000 description 5
- 101710134784 Agnoprotein Proteins 0.000 description 4
- 239000006227 byproduct Substances 0.000 description 4
- 150000001875 compounds Chemical class 0.000 description 4
- 238000002474 experimental method Methods 0.000 description 4
- 238000011010 flushing procedure Methods 0.000 description 4
- 229910002804 graphite Inorganic materials 0.000 description 4
- 239000010439 graphite Substances 0.000 description 4
- 238000005457 optimization Methods 0.000 description 4
- 229910052709 silver Inorganic materials 0.000 description 4
- 229910001220 stainless steel Inorganic materials 0.000 description 4
- 239000010935 stainless steel Substances 0.000 description 4
- 238000003756 stirring Methods 0.000 description 4
- LYCAIKOWRPUZTN-UHFFFAOYSA-N Ethylene glycol Chemical compound OCCO LYCAIKOWRPUZTN-UHFFFAOYSA-N 0.000 description 3
- 239000007772 electrode material Substances 0.000 description 3
- 229910052737 gold Inorganic materials 0.000 description 3
- 239000010931 gold Substances 0.000 description 3
- 229910000510 noble metal Inorganic materials 0.000 description 3
- BASFCYQUMIYNBI-UHFFFAOYSA-N platinum Substances [Pt] BASFCYQUMIYNBI-UHFFFAOYSA-N 0.000 description 3
- 239000004332 silver Substances 0.000 description 3
- RTZKZFJDLAIYFH-UHFFFAOYSA-N Diethyl ether Chemical compound CCOCC RTZKZFJDLAIYFH-UHFFFAOYSA-N 0.000 description 2
- UHYPYGJEEGLRJD-UHFFFAOYSA-N cadmium(2+);selenium(2-) Chemical compound [Se-2].[Cd+2] UHYPYGJEEGLRJD-UHFFFAOYSA-N 0.000 description 2
- 239000003638 chemical reducing agent Substances 0.000 description 2
- 238000010586 diagram Methods 0.000 description 2
- 238000002189 fluorescence spectrum Methods 0.000 description 2
- PCHJSUWPFVWCPO-UHFFFAOYSA-N gold Chemical compound [Au] PCHJSUWPFVWCPO-UHFFFAOYSA-N 0.000 description 2
- -1 graphite alkene Chemical class 0.000 description 2
- 239000010410 layer Substances 0.000 description 2
- 239000002905 metal composite material Substances 0.000 description 2
- 239000002086 nanomaterial Substances 0.000 description 2
- 230000003287 optical effect Effects 0.000 description 2
- 229910052697 platinum Inorganic materials 0.000 description 2
- 230000008569 process Effects 0.000 description 2
- 238000011160 research Methods 0.000 description 2
- 239000002904 solvent Substances 0.000 description 2
- 239000000126 substance Substances 0.000 description 2
- 229910052717 sulfur Inorganic materials 0.000 description 2
- 239000011593 sulfur Substances 0.000 description 2
- 239000004593 Epoxy Substances 0.000 description 1
- 238000001069 Raman spectroscopy Methods 0.000 description 1
- 229910006404 SnO 2 Inorganic materials 0.000 description 1
- 229910010413 TiO 2 Inorganic materials 0.000 description 1
- 238000004833 X-ray photoelectron spectroscopy Methods 0.000 description 1
- 238000009825 accumulation Methods 0.000 description 1
- 239000002253 acid Substances 0.000 description 1
- 150000001336 alkenes Chemical class 0.000 description 1
- 229940037003 alum Drugs 0.000 description 1
- 230000015572 biosynthetic process Effects 0.000 description 1
- 238000006555 catalytic reaction Methods 0.000 description 1
- 239000013066 combination product Substances 0.000 description 1
- 229940127555 combination product Drugs 0.000 description 1
- 239000002322 conducting polymer Substances 0.000 description 1
- 229920001940 conductive polymer Polymers 0.000 description 1
- 230000007547 defect Effects 0.000 description 1
- 125000000118 dimethyl group Chemical group [H]C([H])([H])* 0.000 description 1
- 230000000694 effects Effects 0.000 description 1
- 239000002082 metal nanoparticle Substances 0.000 description 1
- 238000012986 modification Methods 0.000 description 1
- 230000004048 modification Effects 0.000 description 1
- 230000001473 noxious effect Effects 0.000 description 1
- 230000005693 optoelectronics Effects 0.000 description 1
- 230000003647 oxidation Effects 0.000 description 1
- 238000007254 oxidation reaction Methods 0.000 description 1
- 229910052763 palladium Inorganic materials 0.000 description 1
- KDLHZDBZIXYQEI-UHFFFAOYSA-N palladium Substances [Pd] KDLHZDBZIXYQEI-UHFFFAOYSA-N 0.000 description 1
- 239000002245 particle Substances 0.000 description 1
- 229920000642 polymer Polymers 0.000 description 1
- 239000011148 porous material Substances 0.000 description 1
- 239000010970 precious metal Substances 0.000 description 1
- 238000013139 quantization Methods 0.000 description 1
- 238000012827 research and development Methods 0.000 description 1
- 230000004044 response Effects 0.000 description 1
- 150000003839 salts Chemical class 0.000 description 1
- 239000010944 silver (metal) Substances 0.000 description 1
- 238000006884 silylation reaction Methods 0.000 description 1
- 239000002594 sorbent Substances 0.000 description 1
- 238000012360 testing method Methods 0.000 description 1
- 229910000314 transition metal oxide Inorganic materials 0.000 description 1
Classifications
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- H—ELECTRICITY
- H01—ELECTRIC ELEMENTS
- H01G—CAPACITORS; CAPACITORS, RECTIFIERS, DETECTORS, SWITCHING DEVICES, LIGHT-SENSITIVE OR TEMPERATURE-SENSITIVE DEVICES OF THE ELECTROLYTIC TYPE
- H01G11/00—Hybrid capacitors, i.e. capacitors having different positive and negative electrodes; Electric double-layer [EDL] capacitors; Processes for the manufacture thereof or of parts thereof
- H01G11/22—Electrodes
- H01G11/30—Electrodes characterised by their material
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- H—ELECTRICITY
- H01—ELECTRIC ELEMENTS
- H01G—CAPACITORS; CAPACITORS, RECTIFIERS, DETECTORS, SWITCHING DEVICES, LIGHT-SENSITIVE OR TEMPERATURE-SENSITIVE DEVICES OF THE ELECTROLYTIC TYPE
- H01G11/00—Hybrid capacitors, i.e. capacitors having different positive and negative electrodes; Electric double-layer [EDL] capacitors; Processes for the manufacture thereof or of parts thereof
- H01G11/22—Electrodes
- H01G11/24—Electrodes characterised by structural features of the materials making up or comprised in the electrodes, e.g. form, surface area or porosity; characterised by the structural features of powders or particles used therefor
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- H—ELECTRICITY
- H01—ELECTRIC ELEMENTS
- H01G—CAPACITORS; CAPACITORS, RECTIFIERS, DETECTORS, SWITCHING DEVICES, LIGHT-SENSITIVE OR TEMPERATURE-SENSITIVE DEVICES OF THE ELECTROLYTIC TYPE
- H01G11/00—Hybrid capacitors, i.e. capacitors having different positive and negative electrodes; Electric double-layer [EDL] capacitors; Processes for the manufacture thereof or of parts thereof
- H01G11/22—Electrodes
- H01G11/30—Electrodes characterised by their material
- H01G11/32—Carbon-based
- H01G11/36—Nanostructures, e.g. nanofibres, nanotubes or fullerenes
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- H—ELECTRICITY
- H01—ELECTRIC ELEMENTS
- H01G—CAPACITORS; CAPACITORS, RECTIFIERS, DETECTORS, SWITCHING DEVICES, LIGHT-SENSITIVE OR TEMPERATURE-SENSITIVE DEVICES OF THE ELECTROLYTIC TYPE
- H01G11/00—Hybrid capacitors, i.e. capacitors having different positive and negative electrodes; Electric double-layer [EDL] capacitors; Processes for the manufacture thereof or of parts thereof
- H01G11/84—Processes for the manufacture of hybrid or EDL capacitors, or components thereof
- H01G11/86—Processes for the manufacture of hybrid or EDL capacitors, or components thereof specially adapted for electrodes
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- Y—GENERAL TAGGING OF NEW TECHNOLOGICAL DEVELOPMENTS; GENERAL TAGGING OF CROSS-SECTIONAL TECHNOLOGIES SPANNING OVER SEVERAL SECTIONS OF THE IPC; TECHNICAL SUBJECTS COVERED BY FORMER USPC CROSS-REFERENCE ART COLLECTIONS [XRACs] AND DIGESTS
- Y02—TECHNOLOGIES OR APPLICATIONS FOR MITIGATION OR ADAPTATION AGAINST CLIMATE CHANGE
- Y02E—REDUCTION OF GREENHOUSE GAS [GHG] EMISSIONS, RELATED TO ENERGY GENERATION, TRANSMISSION OR DISTRIBUTION
- Y02E60/00—Enabling technologies; Technologies with a potential or indirect contribution to GHG emissions mitigation
- Y02E60/13—Energy storage using capacitors
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Abstract
The invention relates to a method for rapid preparation of a grapheme/silver sulfide quantum dot nanocomposite. The method includes the steps that graphene oxide and AgNO3 are scattered in a dimethyl sulfoxide solution, and the solution is stirred and then transferred into a high pressure reactor for a reaction at the temperature of 150 DEG C to 200 DEG C for 10-15 hours; a product generated from the reaction is rinsed with acetone many times and is cleaned through ethyl alcohol in an ultrasonic vibration mode, and the grapheme/silver sulfide quantum dot nanocomposite is obtained through centrifugal separation and vacuum drying, is of a good and stable single-layer structure and has the photoelectronic property. The method has the advantages that the preparation process is simple and power consumption is low, and both productivity and product performance are greatly promoted in production preparation.
Description
Technical field
The invention belongs to field of polymer composite material, relate to Graphene/silver sulfide quantum dot nano composite material, preparation method.
Background technology
Graphene, after being successfully separated from 2004 by Geim with Novoselov of graceful Chester university of Britain and being characterized, the performance due to its excellence becomes star's material that scientists is paid close attention to.Graphene is the layer structure material of individual layer and multilayer, there is Large ratio surface sum pore volume, its abundant surface group not only becomes good sorbent material, also makes it for being compounded to form the backing material of sandwich as with nano material.
For obtaining the material with high photoelectric properties, various material just in the middle of research and development like a raging fire, particularly graphene nano particle composite material.Graphene nano particle composite has the special performance in photoelectric field application. and the nano particle that can form compound with Graphene has a lot, as metal nanoparticles loaded (Pt, Au, Pd, Ag), oxide nano-particles (Cu
2o, TiO
2, SnO
2) and quantum dot etc.
Silver strip is immersed successively in the graphene oxide solution of silylation and noble metal (gold or silver) colloidal sol, the silver strip/graphene oxide/noble metal composite of sandwich-like can be obtained.Be that graphene oxide and precious metal salt (gold or platinum) can reduce by reducing agent simultaneously with ethylene glycol, one step obtains graphene-supported noble metal composite. and these compounds have good optical property, and the Raman signal of Graphene (or graphene oxide) can be made obviously to be strengthened.
Jiang Lin (Donghua University's Master's thesis in 2013: the preparation of Graphene and composite material, sign and chemical property) etc. once utilized solvent structure method, successful synthesizing graphite alkene related compound material, comprised Ni (OH)
2/ CoO/ rGO, Ni (OH)
2/ rGO and CO
9s
8/ rGO composite nano materials.By unitary electrode material (as transition metal oxide, the conducting polymer) compound of Graphene and ultracapacitor, obviously can promote its ratio capacitance and improve its capacitance characteristic (electric capacity multiplying power, cyclical stability etc.) under high current density.(the Geng X M such as nearest Geng, Niu L, Xing Z Y, et al. Aqueous-processable noncovalent graphene and quantum dotscomposites for transparent and flexible optoelectronic films, Adv. Mater. 2010,22:638-642) by two-step method prepared CdSe quantum dot modify Graphene.Although the optical Response of the CdSe graphene nanocomposite material that this method obtains is improved, lacking strong evidence proves that the black alkene of oxidation is completely reduced, because also there is obvious epoxy ether key in X X-ray photoelectron spectroscopy X display Graphene.Although the research of its quantum dot load Graphene achieves some results, but still can not meet practical needs.
Presently, with the preparation method of graphene nano particle composite material, it is in cost of manufacture, and on process cycle and institute's product yield, one or more aspects have defect.The present invention: a kind of in dimethyl sulphoxide solution directly by the one-step method for synthesizing of graphene oxide synthesizing graphite alkene-silver sulfide, solve the poor and problem of instability of the product property directly brought by simple and easy single step reaction synthesizing graphite alkene-silver sulfide by graphene oxide.This method is one-step method for synthesizing, and except having the advantage of simple and easy and low power consuming, in solution, the high stability of single-layer graphene oxide also ensure that the formation of single-layer graphene film in whole combination product.The product of gained has better structure and photoelectron performance thus.
Summary of the invention
The object of this research is that solution load quantization point graphene nano particle composite preparation technology is loaded down with trivial details, and the problem that product qualities is inferior, provides a kind of method preparing Graphene/silver sulfide quantum dot nano composite material fast.The method has the advantage of the simple and easy and low power consuming of manufacture craft, no matter is productive rate, or properties of product are all improved significantly in manufacture; Prepared graphene-sulfur argentum nano composite material has good structure and photoelectric properties, and application prospect is extensive, can be used as the potential electrode material preparing ultracapacitor.
For achieving the above object, the technical solution used in the present invention is: a kind of method preparing Graphene/silver sulfide quantum dot nano composite material fast, comprises the following steps:
(1) by graphene oxide and silver nitrate in mass ratio 1:1-2 be distributed in dimethyl sulphoxide solution, obtained solution A; Graphene oxide is peeled off through ultrasonic by native graphite alkene, and centrifugation obtains;
(2) solution A is transferred in autoclave, at 150-200 DEG C of temperature, react 10-15 h;
(3) solution step (2) obtained carries out ultrasonic cleaning with two in acetone, ethanol and distilled water kind successively;
(4) by the product centrifugation that step (3) obtains, vacuumize obtains Graphene/silver sulfide quantum dot nano composite material.
As optimization, in step (1), ultrasonic supersonic frequency when peeling off is 20-60 kHz, and the time is 20-40 min; Centrifugation rate during centrifugation is 2000-4000 rpm, and the time is 5-30 min; With the centrifugation of 3000-6000 rpm speed in step (4), during vacuumize, temperature is 40-80 DEG C, and the time is 6-24 h.
As optimization, in step (1), described graphene oxide and the mass ratio of silver nitrate are 1:1.1-1.2.
As optimization, solution A is transferred in autoclave in step (2), reacts, the reactant liquor then will obtained at 170-190 DEG C of temperature, after being cooled to room temperature, then adding organic solvent and washs.
As optimization, in step (4), product centrifugation speed is 5000-6000 rpm; Vacuumize temperature is 50-80 DEG C, adopts vacuum drying oven dry.
A kind of Graphene/silver sulfide quantum dot nano composite material obtained as the preparation method as described in arbitrary in claim 1-5.
Described Graphene/silver sulfide quantum dot nano composite material has well stable single layer structure.
The present invention adopts solvent-thermal method one step to prepare, dimethyl alum not only makes solvent but also serve as reducing agent, under high-temperature high-voltage reaction condition, silver sulfide quantum dot is disconnected from each other and be dispersed on graphene film both sides well, its particle diameter is about 10 nm, effectively prevent the accumulation of graphene film, make prepared composite material have well stable single layer structure, and most of region of graphene film is obtained for the modification of silver sulfide nano-quantum point.Prepared graphene-sulfur argentum nano composite material has stable structure and good photoelectric properties, and application prospect is extensive, can be used as the potential electrode material preparing ultracapacitor.
The present invention is an one-step preparation method, and simple and fast consumes energy low, does not need strong acid, highly basic or noxious substance catalysis, and reaction condition is gentle, and energy-conserving and environment-protective, are applicable to suitability for industrialized production.
Below in conjunction with the drawings and specific embodiments, the present invention is described in further detail.
Accompanying drawing explanation
Fig. 1 is the scanning electron microscope (SEM) photograph that the present invention prepares the Graphene/silver sulfide quantum dot nano composite material of gained.
Fig. 2 is the X-ray diffractogram that the present invention prepares the Graphene/silver sulfide quantum dot nano composite material of gained.
Fig. 3 is the infrared spectrogram of graphene oxide and Graphene/silver sulfide quantum dot nano composite material.
Fig. 4 is Graphene and Graphene/silver sulfide quantum dot nano composite material fluorescence Spectra comparison diagram.
Embodiment
Embodiment 1:
By graphene oxide (40 mg) and AgNO
3(67.5 mg) is distributed in dimethyl sulfoxide solution (50 mL).After vigorous stirring, solution is transferred in polytetrafluoroethyllining lining stainless steel autoclave reacts 12h at 180 DEG C of temperature.By the intensive flushing of solution acetone obtained, then in ultrasonic cleaner, clean the silver sulfide quantum dot removing unreacted reactant and be not attached on graphene film with alcohol.By product with 4000 r pm centrifugations, then dry in vacuum desiccator.The prepared composite material of experiment has well stable single layer structure, and stability is better, and load silver sulfide quantum point grain diameter is approximately 10 nm.The infrared spectrogram of the graphene oxide and Graphene/silver sulfide quantum dot nano composite material of preparing gained is shown in Fig. 1.Graphene as can be observed from Figure/silver sulfide quantum dot nano composite material obviously weakens at the stretching vibration absworption peak of 3422 cm-1 place O-H, illustrates that the oxy radical of this invention Graphene greatly reduces, and graphene oxide is successfully reduced after reaction.The scanning electron microscope (SEM) photograph preparing the Graphene/silver sulfide quantum dot nano composite material of gained is shown in Fig. 2.Can find out from figure (a) and successfully prepare Graphene/silver sulfide quantum dot nano composite material.Silver sulfide quantum dot can be observed comparatively to be evenly distributed on Graphene from figure (b).Can observe from figure (c), the silver sulfide quantum point grain diameter of preparation is approximately 10 nm.Result shows: successfully obtained Graphene/silver sulfide quantum dot nano composite material target product.
Embodiment 2:
By graphene oxide (40 mg) and AgNO
3(67.5 mg) is distributed in dimethyl sulfoxide solution (50 mL).After vigorous stirring, solution is transferred in polytetrafluoroethyllining lining stainless steel autoclave reacts 15 h at 180 DEG C of temperature.By the intensive flushing of solution acetone obtained, then in ultrasonic cleaner, clean the silver sulfide quantum dot removing unreacted reactant and be not attached on graphene film with alcohol.By product with 4000 r pm centrifugations, then dry in vacuum desiccator.The prepared composite material of experiment has well stable single layer structure, and stability is better, and load silver sulfide quantum point grain diameter is approximately 12 nm.
Embodiment 3:
By graphene oxide (40 mg) and AgNO
3(67.5 mg) is distributed in dimethyl sulfoxide solution (50 mL).After vigorous stirring, solution is transferred in polytetrafluoroethyllining lining stainless steel autoclave answers 10 h at 160 DEG C of temperature.By the intensive flushing of solution acetone obtained, then in ultrasonic cleaner, clean the silver sulfide quantum dot removing unreacted reactant and be not attached on graphene film with alcohol.By product with 4000 rpm centrifugations, then dry in vacuum desiccator.The prepared composite material of experiment has well stable single layer structure, and stability is better, and load silver sulfide quantum point grain diameter is approximately 8 nm.Graphene and the Graphene/silver sulfide quantum dot nano composite material fluorescence Spectra comparison diagram of preparing gained are shown in Fig. 3.From figure, curve (b) can learn that simple grapheme material there is no obvious fluorescent effect, when silver sulfide nano-quantum point successfully loads to graphenic surface, fluorescence property as curve (a) composite material is obviously strengthened, this with test as expected that ideal material premium properties is consistent.
Embodiment 4:
By graphene oxide (30 mg) and AgNO
3(60.8 mg) is distributed in dimethyl sulfoxide solution (50 mL).After vigorous stirring, solution is transferred in polytetrafluoroethyllining lining stainless steel autoclave reacts 10h at 180 DEG C of temperature.By the intensive flushing of solution acetone obtained, then in ultrasonic cleaner, clean the silver sulfide quantum dot removing unreacted reactant and be not attached on graphene film with alcohol.By product with 4000 rpm centrifugations, then dry in vacuum desiccator.The prepared composite material of experiment has well stable single layer structure, and stability is better, and load silver sulfide quantum point grain diameter is approximately 9 nm.The X-ray diffractogram preparing the Graphene/silver sulfide quantum dot nano composite material of gained is shown in Fig. 4.Appear at 2 θ=26.0o (100) as can be observed from Figure, 28.8o (101), 30.6o (102), 34.0o (103), 38.2o (105), 44.6o (110), eight diffraction maximums of 5 3.2o (114), 58.4o (116), are the characteristic diffraction peak of monoclinic system silver sulfide, on graphene composite material prepared by explanation, successful load has silver sulfide quantum dot, and the average grain diameter being obtained silver sulfide quantum dot by Scherrer formulae discovery is 9.7 nm.
Above-described embodiment is implemented under premised on technical solution of the present invention, given detailed embodiment and process, is to further illustrate of the present invention, instead of limits the scope of the invention.
Claims (7)
1. prepare a method for Graphene/silver sulfide quantum dot nano composite material fast, it is characterized in that, comprise the following steps:
(1) by graphene oxide and silver nitrate in mass ratio 1:1-2 be distributed in dimethyl sulphoxide solution, obtained solution A; Graphene oxide is peeled off through ultrasonic by general graphene oxide, and centrifugation obtains;
(2) solution A is transferred in autoclave, at 150-200 DEG C of temperature, react 10-15 h;
(3) solution step (2) obtained carries out ultrasonic cleaning with two in acetone, ethanol and distilled water kind successively;
(4) by the product centrifugation that step (3) obtains, vacuumize obtains Graphene/silver sulfide quantum dot nano composite material.
2. prepare as claimed in claim 1 the method for Graphene/silver sulfide quantum dot nano composite material fast, it is characterized in that, in step (1), ultrasonic supersonic frequency when peeling off is 20-60 kHz, and the time is 20-40 min, gets the supernatant liquor after ultrasonic peeling off; Centrifugation rate during centrifugation is 2000-4000 rpm, and the time is 5-30 min; With the centrifugation of 3000-6000 rpm speed in step (4), during vacuumize, temperature is 40-80 DEG C, and the time is 6-24 h.
3. prepare the method for Graphene/silver sulfide quantum dot nano composite material as claimed in claim 1 fast, it is characterized in that, in step (1), described graphene oxide and the mass ratio of silver nitrate are 1:1.1-1.2.
4. prepare the method for Graphene/silver sulfide quantum dot nano composite material as claimed in claim 1 fast, it is characterized in that, in step (2), solution A is transferred in autoclave, react at 170-190 DEG C of temperature, then the reactant liquor will obtained, after being cooled to room temperature, then adding organic solvent and wash.
5. prepare the method for Graphene/silver sulfide quantum dot nano composite material as claimed in claim 2 fast, it is characterized in that, in step (4), product centrifugation speed is 5000-6000 r pm; Vacuumize temperature is 50-80 DEG C, adopts vacuum drying oven dry.
6. Graphene/silver sulfide quantum dot nano the composite material obtained as the preparation method as described in arbitrary in claim 1-5.
7. Graphene/silver sulfide quantum dot nano composite material as claimed in claim 6, it is characterized in that, it has well stable single layer structure.
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Cited By (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN108516539A (en) * | 2018-07-12 | 2018-09-11 | 清华大学 | A kind of preparation method of graphene hydrogel and its application in the treatment of waste water |
| CN108622924A (en) * | 2018-06-27 | 2018-10-09 | 清华大学 | Silver sulfide quantum dot-graphene aerogel composite material and preparation method |
| CN108816247A (en) * | 2018-06-27 | 2018-11-16 | 清华大学 | Utilize silver sulfide quantum dot-graphene hydrogel light degradation organic dyestuff method |
| CN112795108A (en) * | 2021-02-09 | 2021-05-14 | 上海光研化学技术有限公司 | Quantum dot diffusion plate |
| CN113368876A (en) * | 2021-06-29 | 2021-09-10 | 江苏大学 | Carbon dot-assisted Zn-AgIn5S8/Co9S8Preparation method of quantum dots and application of quantum dots in photohydrolysis hydrogen production |
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| CN103232058A (en) * | 2013-05-16 | 2013-08-07 | 东华大学 | Method for preparing copper sulphide/graphene nano-composite material |
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| CN108622924A (en) * | 2018-06-27 | 2018-10-09 | 清华大学 | Silver sulfide quantum dot-graphene aerogel composite material and preparation method |
| CN108816247A (en) * | 2018-06-27 | 2018-11-16 | 清华大学 | Utilize silver sulfide quantum dot-graphene hydrogel light degradation organic dyestuff method |
| CN108622924B (en) * | 2018-06-27 | 2019-10-18 | 清华大学 | Silver sulfide quantum dot-graphene aerogel composite material and preparation method |
| CN108816247B (en) * | 2018-06-27 | 2020-01-07 | 清华大学 | Method for photodegradation of organic dye by using silver sulfide quantum dot-graphene hydrogel |
| CN108516539A (en) * | 2018-07-12 | 2018-09-11 | 清华大学 | A kind of preparation method of graphene hydrogel and its application in the treatment of waste water |
| CN108516539B (en) * | 2018-07-12 | 2019-07-12 | 清华大学 | A kind of preparation method of graphene hydrogel and its application in the treatment of waste water |
| CN112795108A (en) * | 2021-02-09 | 2021-05-14 | 上海光研化学技术有限公司 | Quantum dot diffusion plate |
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