CN108428565B - Tungsten disulfide/graphene oxide composite material, preparation method and application - Google Patents
Tungsten disulfide/graphene oxide composite material, preparation method and application Download PDFInfo
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- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical compound [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 title claims abstract description 105
- 229910021389 graphene Inorganic materials 0.000 title claims abstract description 98
- ITRNXVSDJBHYNJ-UHFFFAOYSA-N tungsten disulfide Chemical compound S=[W]=S ITRNXVSDJBHYNJ-UHFFFAOYSA-N 0.000 title claims abstract description 97
- 239000002131 composite material Substances 0.000 title claims abstract description 59
- 238000002360 preparation method Methods 0.000 title claims abstract description 23
- 238000000034 method Methods 0.000 claims abstract description 18
- VWDWKYIASSYTQR-UHFFFAOYSA-N sodium nitrate Chemical compound [Na+].[O-][N+]([O-])=O VWDWKYIASSYTQR-UHFFFAOYSA-N 0.000 claims description 26
- 238000003756 stirring Methods 0.000 claims description 24
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Chemical compound O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims description 24
- 239000011541 reaction mixture Substances 0.000 claims description 22
- 239000006185 dispersion Substances 0.000 claims description 19
- MHAJPDPJQMAIIY-UHFFFAOYSA-N Hydrogen peroxide Chemical compound OO MHAJPDPJQMAIIY-UHFFFAOYSA-N 0.000 claims description 18
- 239000008367 deionised water Substances 0.000 claims description 13
- 229910021641 deionized water Inorganic materials 0.000 claims description 13
- 235000010344 sodium nitrate Nutrition 0.000 claims description 13
- 239000004317 sodium nitrate Substances 0.000 claims description 13
- 239000000843 powder Substances 0.000 claims description 12
- QAOWNCQODCNURD-UHFFFAOYSA-N sulfuric acid Substances OS(O)(=O)=O QAOWNCQODCNURD-UHFFFAOYSA-N 0.000 claims description 12
- 239000012286 potassium permanganate Substances 0.000 claims description 10
- 238000006243 chemical reaction Methods 0.000 claims description 7
- WFKWXMTUELFFGS-UHFFFAOYSA-N tungsten Chemical compound [W] WFKWXMTUELFFGS-UHFFFAOYSA-N 0.000 claims description 7
- 229910002804 graphite Inorganic materials 0.000 claims description 6
- 239000010439 graphite Substances 0.000 claims description 6
- -1 oxygen Graphite alkene Chemical class 0.000 claims description 5
- 238000000926 separation method Methods 0.000 claims description 5
- 239000008346 aqueous phase Substances 0.000 claims description 3
- 239000008240 homogeneous mixture Substances 0.000 claims description 3
- 229910052760 oxygen Inorganic materials 0.000 claims description 3
- 239000001301 oxygen Substances 0.000 claims description 3
- 239000000463 material Substances 0.000 abstract description 17
- 239000011229 interlayer Substances 0.000 abstract description 9
- 239000007772 electrode material Substances 0.000 abstract description 6
- 150000001875 compounds Chemical class 0.000 abstract description 5
- 230000002687 intercalation Effects 0.000 abstract description 4
- 238000009830 intercalation Methods 0.000 abstract description 4
- 241000446313 Lamella Species 0.000 abstract description 3
- 238000005411 Van der Waals force Methods 0.000 abstract description 3
- 230000000694 effects Effects 0.000 abstract description 3
- 230000005540 biological transmission Effects 0.000 description 9
- 239000010410 layer Substances 0.000 description 9
- 230000000052 comparative effect Effects 0.000 description 6
- 239000007788 liquid Substances 0.000 description 6
- 150000001336 alkenes Chemical class 0.000 description 5
- 239000000203 mixture Substances 0.000 description 5
- 229910052721 tungsten Inorganic materials 0.000 description 4
- 239000010937 tungsten Substances 0.000 description 4
- 238000002604 ultrasonography Methods 0.000 description 4
- 239000002356 single layer Substances 0.000 description 3
- VHUUQVKOLVNVRT-UHFFFAOYSA-N Ammonium hydroxide Chemical compound [NH4+].[OH-] VHUUQVKOLVNVRT-UHFFFAOYSA-N 0.000 description 2
- 241000209094 Oryza Species 0.000 description 2
- 235000007164 Oryza sativa Nutrition 0.000 description 2
- 238000005054 agglomeration Methods 0.000 description 2
- 230000002776 aggregation Effects 0.000 description 2
- 239000000908 ammonium hydroxide Substances 0.000 description 2
- 230000015572 biosynthetic process Effects 0.000 description 2
- 230000007812 deficiency Effects 0.000 description 2
- 125000000524 functional group Chemical group 0.000 description 2
- 230000003647 oxidation Effects 0.000 description 2
- 238000007254 oxidation reaction Methods 0.000 description 2
- 238000006722 reduction reaction Methods 0.000 description 2
- 235000009566 rice Nutrition 0.000 description 2
- 239000004575 stone Substances 0.000 description 2
- 239000002023 wood Substances 0.000 description 2
- BWGNESOTFCXPMA-UHFFFAOYSA-N Dihydrogen disulfide Chemical compound SS BWGNESOTFCXPMA-UHFFFAOYSA-N 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
- 239000003990 capacitor Substances 0.000 description 1
- 229910052799 carbon Inorganic materials 0.000 description 1
- 230000008859 change Effects 0.000 description 1
- 238000009833 condensation Methods 0.000 description 1
- 230000005494 condensation Effects 0.000 description 1
- 239000013078 crystal Substances 0.000 description 1
- 239000000428 dust Substances 0.000 description 1
- 238000000635 electron micrograph Methods 0.000 description 1
- 238000002156 mixing Methods 0.000 description 1
- 238000012986 modification Methods 0.000 description 1
- 230000004048 modification Effects 0.000 description 1
- 230000008569 process Effects 0.000 description 1
- 230000009467 reduction Effects 0.000 description 1
- 238000011946 reduction process Methods 0.000 description 1
- 238000009738 saturating Methods 0.000 description 1
- 239000013049 sediment Substances 0.000 description 1
- 239000000126 substance Substances 0.000 description 1
- 238000006467 substitution reaction Methods 0.000 description 1
- 239000006228 supernatant Substances 0.000 description 1
- 239000013589 supplement Substances 0.000 description 1
- 238000004627 transmission electron microscopy Methods 0.000 description 1
Classifications
-
- H—ELECTRICITY
- H01—ELECTRIC ELEMENTS
- H01G—CAPACITORS; CAPACITORS, RECTIFIERS, DETECTORS, SWITCHING DEVICES OR LIGHT-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
-
- H—ELECTRICITY
- H01—ELECTRIC ELEMENTS
- H01G—CAPACITORS; CAPACITORS, RECTIFIERS, DETECTORS, SWITCHING DEVICES OR LIGHT-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
-
- H—ELECTRICITY
- H01—ELECTRIC ELEMENTS
- H01G—CAPACITORS; CAPACITORS, RECTIFIERS, DETECTORS, SWITCHING DEVICES OR LIGHT-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
-
- H—ELECTRICITY
- H01—ELECTRIC ELEMENTS
- H01G—CAPACITORS; CAPACITORS, RECTIFIERS, DETECTORS, SWITCHING DEVICES OR LIGHT-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
-
- 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
Abstract
The invention discloses a kind of tungsten disulfide/graphene oxide composite materials, including tungsten disulfide nano slices and graphene oxide, and the tungsten disulfide nano slices are interspersed between the lamella of graphene oxide.Preferably, the tungsten disulfide nano slices intert mutually compound with graphene oxide.The invention also discloses the method for preparing the tungsten disulfide/graphene oxide composite material and the purposes of the tungsten disulfide/graphene oxide composite material, for example, prepare electrode material, the purposes in supercapacitor.The present invention van der waals force different from both two-dimensional material interlayers of graphene oxide using tungsten disulfide nano slices, it is allowed to mutual intercalation, to reduce respective reuniting effect, and then its dispersibility can be increased, it can be as the preparation devices such as supercapacitor or battery, the especially excellent material of the electrode of such devices.
Description
Technical field
Present invention relates particularly to a kind of tungsten disulfide/graphene oxide composite material, preparation method invention and applications, belong to
In materials science field.
Background technique
Graphene and tungsten disulfide belong to the two-dimensional material of honeycomb six-membered ring structure, and interlayer is van der waals force
In conjunction with, multilayer is tended to both under native state reunites together, the thicker flat crystal of formation.By Hummer ' s method oxygen
The graphene (r-GO) of change, interlayer are strutted by various functional groups, to removing thicker sheet for relatively thin single layer/few layer
Graphene oxide obtains biggish specific surface area, so as to be applied to the electrode material of supercapacitor.
But before making electrode material, the step of graphene oxide is also needed by restoring, removes interlayer functional group.?
The atomic layer being lifted off of in this step is often reunited together again, loses the advantage of its specific surface area, and then is made
The performance for the electrode material prepared is unable to get biggish promotion.
Summary of the invention
The main purpose of the present invention is to provide a kind of tungsten disulfide/graphene oxide composite material, preparation method with
Using to overcome deficiency in the prior art.
For realization aforementioned invention purpose, the technical solution adopted by the present invention includes:
The embodiment of the invention provides a kind of tungsten disulfide/graphene oxide composite materials comprising Wolfram disulfide nano
Piece and graphene oxide, and the tungsten disulfide nano slices are interspersed between the lamella of graphene oxide.
Further, the tungsten disulfide nano slices intert mutually compound with graphene oxide.
Further, the tungsten disulfide and graphene oxide are amorphous state, and diffraction pattern is without bright and sharp diffraction spot.
The embodiment of the invention also provides a kind of preparation methods of tungsten disulfide/graphene oxide composite material comprising:
Graphene oxide is prepared using Hummer ' s method；
Under conditions of temperature is 0 DEG C, the homogeneous mixture of tungsten disulfide powder and sodium nitrate is mixed instead with the concentrated sulfuric acid
It answers, potassium permanganate is added later, and the reaction was continued, the first reaction mixture is obtained,
Thereafter, at room temperature successively into the first reaction mixture be added deionized water, the reaction was continued for hydrogen peroxide, formed
Second reaction mixture；
Separation obtains the uniform dispersion of tungsten disulfide nano slices from the second reaction mixture；
The tungsten disulfide nano slices are mixed in aqueous phase system with the graphene oxide, form the curing
Tungsten/graphene oxide composite material.
The embodiment of the invention also provides tungsten disulfide/graphene oxide composite woods by aforementioned any method preparation
Material, the tungsten disulfide/graphene oxide composite material include interspersed compound tungsten disulfide nano slices and graphite oxide mutually
Alkene.
The embodiment of the invention also provides the purposes of the tungsten disulfide/graphene oxide composite material, such as are preparing
Purposes in electrode material, supercapacitor, battery etc..
Compared with the prior art, the present invention makes two kind two by the way that tungsten disulfide nano slices are compound with graphene oxide composite material
The structure that mutual intercalation is formed between dimension material, is conducive to avoid the reunion in further reduction reaction between graphene atomic layer,
Its dispersion degree and specific surface area are improved, so as to greatly improve its chemical property as electrode of super capacitor, and then also
Be conducive to improve the performance of specific capacitance of supercapacitor etc..
Detailed description of the invention
Fig. 1 is a kind of transmission electron microscope photograph of tungsten disulfide/graphene oxide composite material in the embodiment of the present invention 1
Piece.
Fig. 2 is a kind of transmission electron microscope photograph of tungsten disulfide/graphene oxide composite material in the embodiment of the present invention 1
Piece.
Fig. 3 is a kind of transmission electron microscope photograph of tungsten disulfide/graphene oxide composite material in the embodiment of the present invention 1
Piece.
Fig. 4 is a kind of transmission electron microscope photograph of tungsten disulfide/graphene oxide composite material in the embodiment of the present invention 2
Piece.
Fig. 5 a is a kind of transmission electron microscope of tungsten disulfide/graphene oxide composite material in the embodiment of the present invention 2
Photo.
Fig. 5 b is a kind of electronic diffraction photo of tungsten disulfide/graphene oxide composite material in the embodiment of the present invention 2.
Fig. 6 is a kind of transmission electron microscope photo of graphene oxide composite material in comparative example 1 of the present invention.
Fig. 7 is a kind of transmission electron microscope photo of graphene oxide composite material in comparative example 1 of the present invention.
Fig. 8 is a kind of transmission electron microscope photo of graphene oxide composite material in comparative example 1 of the present invention.
Fig. 9 is a kind of X-ray diffractogram of tungsten disulfide/graphene oxide composite material in the embodiment of the present invention 1.
Specific embodiment
In view of deficiency in the prior art, inventor is studied for a long period of time and is largely practiced, and is able to propose of the invention
Technical solution.The technical solution, its implementation process and principle etc. will be further explained as follows.
A kind of tungsten disulfide/graphene oxide composite material that the one aspect of the embodiment of the present invention provides includes curing
Tungsten nanometer sheet and graphene oxide, and the tungsten disulfide nano slices are interspersed between the lamella of graphene oxide.
Wherein, by the way that tungsten disulfide nano slices are interspersed between graphene oxide layer, the composition two to be formed can be made
Tungsten sulfide/graphene oxide composite material is reunited less, and then can also avoid graphite in the reduction process of this kind of composite material
The reunion of alkene atom interlayer, improves its dispersion performance and specific surface area.
Further, the tungsten disulfide nano slices intert mutually compound with graphene oxide.Utilize this two kinds two-dimentional materials
Different van der waals force etc. between the bed of material can reduce by two kinds of respective reuniting effects of two-dimensional material.
Further, the tungsten disulfide and graphene oxide are amorphous state, and diffraction pattern is without bright and sharp diffraction spot.
The other side of the embodiment of the present invention, which additionally provides, a kind of prepares the tungsten disulfide/graphene oxide composite wood
The method of material comprising:
Graphene oxide is prepared using Hummer ' s method；
Under conditions of temperature is 0 DEG C, the homogeneous mixture of tungsten disulfide powder and sodium nitrate is mixed instead with the concentrated sulfuric acid
It answers, potassium permanganate is added later, and the reaction was continued, the first reaction mixture is obtained,
Thereafter, at room temperature successively into the first reaction mixture be added deionized water, the reaction was continued for hydrogen peroxide, formed
Second reaction mixture；
Separation obtains the uniform dispersion of tungsten disulfide nano slices from the second reaction mixture；
The tungsten disulfide nano slices are mixed in aqueous phase system with the graphene oxide, form the curing
Tungsten/graphene oxide composite material.
In some embodiments, the preparation method includes:
Tungsten disulfide is uniformly mixed with sodium nitrate, is persistently stirred under condition of ice bath, and be slowly added into the concentrated sulfuric acid, after
Continuous stirring 20min or more, is slowly added to potassium permanganate later, is further continued for stirring 15min or more, forms the first reaction mixture；
It is continuously stirred at room temperature the first reaction mixture 12h or more, is slowly added dropwise later into deionized water, is further continued for stirring
30min or more is mixed, is slowly added to hydrogen peroxide thereafter, and continues to stir 2h or more, forms the second reaction mixture；
Separation obtains the uniform dispersion of tungsten disulfide nano slices from the second reaction mixture；
Uniform point of graphene oxide prepared by the uniform dispersion of the tungsten disulfide nano slices and Hummer ' s method
Dispersion liquid mixing, ultrasonic 2h or more obtain tungsten disulfide/graphene oxide composite material.
Further, the mass ratio of the tungsten disulfide and sodium nitrate is preferably 1.5:0.17.
Further, the amount ratio of the tungsten disulfide powder and the concentrated sulfuric acid is preferably 1.5g:11.5mL.
Further, the mass ratio of the potassium permanganate and the tungsten disulfide powder is preferably 1:1.
Further, the deionized water and the volume ratio of the concentrated sulfuric acid are preferably 50:11.5.
Further, the temperature for the deionized water being added in the first reaction mixture of Xiang Suoshu is preferably 60 DEG C.
Further, the mass ratio of the carbon dust and tungsten disulfide powder that are used to prepare the graphene oxide is preferably 1:6,
Tungsten disulfide nano slices and graphene oxide in the compound of formation can be so set more fully to be intercalation into other side's
Interlayer.
In some more specifically case study on implementation of the invention, a kind of to prepare the tungsten disulfide/graphene oxide multiple
The method of condensation material may include steps of:
(1) about 1.5g tungsten disulfide is uniformly mixed with about 0.17g sodium nitrate powder, is persistently stirred under condition of ice bath,
Slowly the about 11.5mL concentrated sulfuric acid is added in the mixture of tungsten disulfide and sodium nitrate；
(2) maintain ice bath, stirring condition described in step (1), after about 20min, be slowly added to about 1.5g potassium permanganate,
Continue to stir 15min；
(3) ice bath is removed, after continuing stir about 12h under room temperature (about 25 DEG C), the deionized water of 50mL is slowly added dropwise
(temperature is preferably 60 DEG C or so) after continuing stir about 30min, is slowly added to the hydrogen peroxide that about 1.6mL concentration is 30%, continues
Stir 2h；
(4) step (3) resulting materials are repeatedly centrifuged and are washed, and with the oxidation stone that uses similar step to prepare
Black alkene material (i.e. the graphene oxide composite material of Hummer ' s method preparation) is blended, and ultrasonic 2h or more is to get tungsten disulfide/oxidation stone
Black alkene composite material.
In abovementioned steps (4), the time that blend can also be carried out to ultrasound is appropriately extended, and supernatant is removed, and
Deionized water is rejoined in sediment continues ultrasound.
The other side of the embodiment of the present invention additionally provides a kind of tungsten disulfide/graphite oxide prepared by preceding method
Alkene composite material, the tungsten disulfide/graphene oxide composite material include mutually interspersed compound tungsten disulfide nano slices with
Graphene oxide.
In previously described embodiments of the present invention, the tungsten disulfide atomic layer intercalation peeled away by using Hummer ' s method into
Enter graphene oxide interlayer, it, can be to avoid in composite material especially with the graphene oxide interlayer of Hummer ' s method preparation
Graphene oxide reunite again in reduction step later.
The other side of the embodiment of the present invention additionally provides the tungsten disulfide/graphene oxide composite material in system
Purposes in standby electrode material.
The other side of the embodiment of the present invention additionally provides the tungsten disulfide/graphene oxide composite material in system
Purposes in the elements such as standby supercapacitor or battery, equipment.
Below in conjunction with several examples and drawings, further description of the technical solution of the present invention.
Embodiment 1: a kind of tungsten disulfide/graphene oxide composite material is present embodiments provided, wherein tungsten disulfide is received
Rice piece is interspersed in graphene oxide atom interlayer.
Tungsten disulfide/graphene oxide composite material preparation method includes:
1, the preparation of tungsten disulfide nano slices
(1) 1.5g tungsten disulfide is uniformly mixed with 0.17g sodium nitrate powder, is persistently stirred under condition of ice bath, slowly
Ground the 11.5mL concentrated sulfuric acid is added in the mixture of tungsten disulfide and sodium nitrate；
(2) it maintains ice bath, stirring condition described in step (1) to be slowly added to 1.5g potassium permanganate after twenty minutes, continues
Stir 15min；
(3) ice bath is removed, after persistently stirring 12h under room temperature (about 25 DEG C), the deionized water of 50mL is slowly added dropwise (about
60 DEG C), continue after stirring 30min, is slowly added to the hydrogen peroxide that 1.6mL concentration is 30%, continues stirring 2 hours；
(4) step (3) resulting materials are repeatedly centrifuged and are washed, the dispersion liquid of tungsten disulfide nano slices is made.
2, the preparation of graphene oxide can be prepared using hummers method, be specifically comprised the following steps:
(1) 1.5g graphite powder is uniformly mixed with 0.17g sodium nitrate powder, is persistently stirred under condition of ice bath, slowly
The 11.5mL concentrated sulfuric acid is added in tungsten disulfide and sodium nitrate mixture；
(2) it maintains ice bath, stirring condition described in step (1) to be slowly added to 1.5g potassium permanganate after twenty minutes, continues
Stirring 15 minutes；
(3) ice bath is removed, after persistently stirring 12 hours under room temperature (about 25 DEG C), the deionized water of 50mL is slowly added dropwise
(about 60 DEG C) after continuing stirring 30 minutes, are slowly added to the hydrogen peroxide that 1.6mL concentration is 30%, continue stirring 2 hours；
(4) step (3) resulting materials are repeatedly centrifuged and are washed, the dispersion liquid of graphene oxide is made.
3, tungsten disulfide nano slices dispersion liquid is mixed with graphene oxide dispersion, ultrasound 2 hours to get curing
Tungsten/graphene oxide composite material.
Embodiment 2: a kind of tungsten disulfide/graphene oxide composite material is present embodiments provided, wherein tungsten disulfide is received
Rice piece is interspersed between graphene atomic layer.
Tungsten disulfide/graphene oxide composite material preparation method includes:
Step (1)~step (4): it is identical with step (1)~step (4) in embodiment 1, obtain tungsten disulfide/oxygen
Graphite alkene composite material；
Step (5): ammonium hydroxide is added dropwise in Xiang Qianshu tungsten disulfide/graphene oxide composite material dispersion liquid and persistently stirs
It mixes, pH value is made to become greater to 10 from 7, continue ultrasound 2h or so later.
Comparative example 1: preparing graphene oxide composite material by the way of same as Example 1, the backward graphene oxide
Ammonium hydroxide is added dropwise in the dispersion liquid of material, until pH value is adjusted to 10, is further continued for ultrasonic 2h.
Tungsten disulfide/the graphene oxide composite material and comparative example 1 finally obtained to previous embodiment 1, embodiment 2
In finally obtain graphene oxide composite material obtained and tested.As follows will make an explanation to test result explanation.
Please referring to Fig. 1, Fig. 2 and Fig. 3 is finally the obtained tungsten disulfide/graphene oxide composite wood of the embodiment of the present invention 1
The transmission electron microscope photo of material, it can be seen that tungsten disulfide nano slices in the tungsten disulfide/graphene oxide composite material,
The dispersion effect of graphene oxide is preferable, while wherein there is the more accordion atomic layer for being separated into few layer/single layer.
Please referring to Fig. 4 and Fig. 5 a, by the embodiment of the present invention 2 finally to obtain tungsten disulfide/graphene oxide composite material saturating
Penetrate electron micrograph, it can be seen that the more flaky texture quilt of fold in tungsten disulfide/graphene oxide composite material
It is reduced to the less flaky texture of fold, and agglomeration has obtained good control.
The electronics that Fig. 5 b is final the obtained tungsten disulfide/graphene oxide composite material of the embodiment of the present invention 2 is please referred to spread out
Penetrate photo, it can be seen that wherein without bright and sharp diffraction spot, illustrate that sample is amorphous state, and the lattice of diffraction ring and graphene oxide
Constant matches.
Please refer to the transmission electron microscopy that Fig. 6, Fig. 7 and Fig. 8 are final the obtained graphene oxide composite materials of comparative example 1 of the present invention
Mirror photo, it is seen that its agglomeration is serious, wherein few layer/single layer structure of fine dispersion is substantially not present.
The X-ray that Fig. 9 is final the obtained tungsten disulfide/graphene oxide composite material of the embodiment of the present invention 1 is please referred to spread out
Penetrate figure, it is seen that tungsten disulfide coexists with graphene oxide in the sample.
Technical solution of the present invention is described in detail in embodiment described above, it should be understood that the above is only
For specific embodiments of the present invention, it is not intended to restrict the invention, all any modifications made in spirit of the invention,
Supplement or similar fashion substitution etc., should all be included in the protection scope of the present invention.
Claims (10)
1. a kind of preparation method of tungsten disulfide/graphene oxide composite material, characterized by comprising:
Graphene oxide is prepared using hummers method；
Under conditions of temperature is 0 DEG C, by the homogeneous mixture of tungsten disulfide powder and sodium nitrate and concentrated sulfuric acid hybrid reaction, it
Potassium permanganate is added afterwards, and the reaction was continued, obtains the first reaction mixture；
Thereafter, at room temperature successively into the first reaction mixture be added deionized water, the reaction was continued for hydrogen peroxide, formed second
Reaction mixture；
Separation obtains the uniform dispersion of tungsten disulfide nano slices from the second reaction mixture；
The tungsten disulfide nano slices are mixed in aqueous phase system with the graphene oxide, form the tungsten disulfide/oxygen
Graphite alkene composite material.
2. preparation method according to claim 1, characterized by comprising:
Tungsten disulfide is uniformly mixed with sodium nitrate, is persistently stirred under condition of ice bath, and be slowly added into the concentrated sulfuric acid, continues to stir
20min or more is mixed, is slowly added to potassium permanganate later, stirring 15min or more is further continued for, forms the first reaction mixture；
It is continuously stirred at room temperature the first reaction mixture 12h or more, is slowly added dropwise later into deionized water, is further continued for stirring
30min or more is slowly added to thereafter hydrogen peroxide, and continues to stir 2h or more, forms the second reaction mixture；
Separation obtains the uniform dispersion of tungsten disulfide nano slices from the second reaction mixture；
The uniform dispersion for the graphene oxide that the uniform dispersion of the tungsten disulfide nano slices is prepared with hummers method is mixed
It closes, ultrasonic 2h or more, obtains tungsten disulfide/graphene oxide composite material.
3. preparation method according to claim 1 or 2, it is characterised in that: the mass ratio of the tungsten disulfide and sodium nitrate
For 1.5:0.17.
4. preparation method according to claim 1 or 2, it is characterised in that: the use of the tungsten disulfide powder and the concentrated sulfuric acid
Amount is than being 1.5g:11.5mL.
5. preparation method according to claim 1 or 2, it is characterised in that: the potassium permanganate and the curing tungsten powder
The mass ratio of body is 1:1.
6. preparation method according to claim 1 or 2, it is characterised in that: the hydrogen peroxide and the curing tungsten powder
The amount ratio of body is 1.6mL:1.5g.
7. preparation method according to claim 1 or 2, it is characterised in that: the body of the deionized water and the concentrated sulfuric acid
Product is than being 50:11.5.
8. preparation method according to claim 1 or 2, it is characterised in that: be added in the first reaction mixture of Xiang Suoshu
The temperature of the deionized water is 60 DEG C.
9. preparation method according to claim 1 or 2, it is characterised in that: be used to prepare the graphite of the graphene oxide
The mass ratio of powder and tungsten disulfide powder is 1:6.
10. tungsten disulfide/the graphene oxide composite material prepared by any one of claim 1-9 the method, described two
Tungsten sulfide/graphene oxide composite material includes interspersed compound tungsten disulfide nano slices and graphene oxide mutually, wherein two
Tungsten sulfide and graphene oxide are amorphous state and diffraction pattern without bright and sharp diffraction spot.
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| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201710076173 | 2017-02-13 | ||
| CN2017100761735 | 2017-02-13 |
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| Publication Number | Publication Date |
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| CN108428565A CN108428565A (en) | 2018-08-21 |
| CN108428565B true CN108428565B (en) | 2019-09-27 |
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| CN109181638A (en) * | 2018-09-05 | 2019-01-11 | 南京理工大学 | A kind of tungsten disulfide-redox graphene three-dimensional self-assembled structures absorbing material |
| CN109326787B (en) * | 2018-10-30 | 2021-08-10 | 陕西科技大学 | Preparation method of tungsten disulfide/GO composite electrode material |
| CN111799458B (en) * | 2020-07-31 | 2022-02-11 | 陕西科技大学 | Tin elemental composite tungsten disulfide/reduced graphene oxide composite electrode material and preparation method and application thereof |
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