CN107188232A - A kind of petal-shaped tungsten sulfide nanosphere, preparation method and applications - Google Patents
A kind of petal-shaped tungsten sulfide nanosphere, preparation method and applications Download PDFInfo
- Publication number
- CN107188232A CN107188232A CN201710328302.5A CN201710328302A CN107188232A CN 107188232 A CN107188232 A CN 107188232A CN 201710328302 A CN201710328302 A CN 201710328302A CN 107188232 A CN107188232 A CN 107188232A
- Authority
- CN
- China
- Prior art keywords
- petal
- tungsten sulfide
- preparation
- shaped tungsten
- sulfide nanosphere
- Prior art date
- Legal status (The legal status is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the status listed.)
- Pending
Links
- ITRNXVSDJBHYNJ-UHFFFAOYSA-N tungsten disulfide Chemical compound S=[W]=S ITRNXVSDJBHYNJ-UHFFFAOYSA-N 0.000 title claims abstract description 45
- 239000002077 nanosphere Substances 0.000 title claims abstract description 31
- 238000002360 preparation method Methods 0.000 title claims abstract description 25
- UMGDCJDMYOKAJW-UHFFFAOYSA-N thiourea Chemical compound NC(N)=S UMGDCJDMYOKAJW-UHFFFAOYSA-N 0.000 claims abstract description 28
- UFHFLCQGNIYNRP-UHFFFAOYSA-N Hydrogen Chemical compound [H][H] UFHFLCQGNIYNRP-UHFFFAOYSA-N 0.000 claims abstract description 25
- 229910052739 hydrogen Inorganic materials 0.000 claims abstract description 25
- 239000001257 hydrogen Substances 0.000 claims abstract description 25
- 239000003054 catalyst Substances 0.000 claims abstract description 13
- 238000001027 hydrothermal synthesis Methods 0.000 claims abstract description 11
- 239000011259 mixed solution Substances 0.000 claims abstract description 11
- 230000015572 biosynthetic process Effects 0.000 claims abstract description 7
- 238000001035 drying Methods 0.000 claims abstract description 6
- 238000005119 centrifugation Methods 0.000 claims abstract description 5
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims abstract description 5
- 238000005406 washing Methods 0.000 claims abstract description 4
- 239000002244 precipitate Substances 0.000 claims description 6
- 238000004140 cleaning Methods 0.000 claims description 5
- 239000007788 liquid Substances 0.000 claims description 5
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 claims description 4
- 238000004108 freeze drying Methods 0.000 claims description 4
- 239000002002 slurry Substances 0.000 claims description 4
- 239000000243 solution Substances 0.000 claims description 3
- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical compound [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 claims description 2
- 239000006230 acetylene black Substances 0.000 claims description 2
- 239000011230 binding agent Substances 0.000 claims description 2
- 239000002904 solvent Substances 0.000 claims description 2
- 238000010790 dilution Methods 0.000 claims 1
- 239000012895 dilution Substances 0.000 claims 1
- 238000001556 precipitation Methods 0.000 claims 1
- 229910052721 tungsten Inorganic materials 0.000 abstract description 9
- 239000010937 tungsten Substances 0.000 abstract description 9
- WFKWXMTUELFFGS-UHFFFAOYSA-N tungsten Chemical compound [W] WFKWXMTUELFFGS-UHFFFAOYSA-N 0.000 abstract description 8
- 238000005516 engineering process Methods 0.000 abstract description 7
- 238000004073 vulcanization Methods 0.000 abstract description 7
- 238000006555 catalytic reaction Methods 0.000 abstract description 5
- 239000002994 raw material Substances 0.000 abstract description 5
- 230000000694 effects Effects 0.000 abstract description 4
- 238000003786 synthesis reaction Methods 0.000 abstract description 3
- NINIDFKCEFEMDL-UHFFFAOYSA-N Sulfur Chemical compound [S] NINIDFKCEFEMDL-UHFFFAOYSA-N 0.000 description 11
- 229910052717 sulfur Inorganic materials 0.000 description 8
- 239000011593 sulfur Substances 0.000 description 8
- 230000003197 catalytic effect Effects 0.000 description 6
- 238000000034 method Methods 0.000 description 6
- BASFCYQUMIYNBI-UHFFFAOYSA-N platinum Chemical compound [Pt] BASFCYQUMIYNBI-UHFFFAOYSA-N 0.000 description 6
- 239000000463 material Substances 0.000 description 5
- 238000011056 performance test Methods 0.000 description 5
- 238000011161 development Methods 0.000 description 4
- 235000019441 ethanol Nutrition 0.000 description 4
- YNPNZTXNASCQKK-UHFFFAOYSA-N phenanthrene Chemical compound C1=CC=C2C3=CC=CC=C3C=CC2=C1 YNPNZTXNASCQKK-UHFFFAOYSA-N 0.000 description 4
- 239000005864 Sulphur Substances 0.000 description 3
- 239000003205 fragrance Substances 0.000 description 3
- 229910052697 platinum Inorganic materials 0.000 description 3
- XMVONEAAOPAGAO-UHFFFAOYSA-N sodium tungstate Chemical compound [Na+].[Na+].[O-][W]([O-])(=O)=O XMVONEAAOPAGAO-UHFFFAOYSA-N 0.000 description 3
- 238000012360 testing method Methods 0.000 description 3
- -1 transition metal chalcogenides Chemical class 0.000 description 3
- QAOWNCQODCNURD-UHFFFAOYSA-N Sulfuric acid Chemical compound OS(O)(=O)=O QAOWNCQODCNURD-UHFFFAOYSA-N 0.000 description 2
- 230000015556 catabolic process Effects 0.000 description 2
- 230000008859 change Effects 0.000 description 2
- 230000001276 controlling effect Effects 0.000 description 2
- 238000006731 degradation reaction Methods 0.000 description 2
- 230000007613 environmental effect Effects 0.000 description 2
- 238000004519 manufacturing process Methods 0.000 description 2
- 229910052751 metal Inorganic materials 0.000 description 2
- 239000002184 metal Substances 0.000 description 2
- VNWKTOKETHGBQD-UHFFFAOYSA-N methane Chemical compound C VNWKTOKETHGBQD-UHFFFAOYSA-N 0.000 description 2
- DGAQECJNVWCQMB-PUAWFVPOSA-M Ilexoside XXIX Chemical compound C[C@@H]1CC[C@@]2(CC[C@@]3(C(=CC[C@H]4[C@]3(CC[C@@H]5[C@@]4(CC[C@@H](C5(C)C)OS(=O)(=O)[O-])C)C)[C@@H]2[C@]1(C)O)C)C(=O)O[C@H]6[C@@H]([C@H]([C@@H]([C@H](O6)CO)O)O)O.[Na+] DGAQECJNVWCQMB-PUAWFVPOSA-M 0.000 description 1
- 229920000557 Nafion® Polymers 0.000 description 1
- 240000007594 Oryza sativa Species 0.000 description 1
- 235000007164 Oryza sativa Nutrition 0.000 description 1
- 229910021607 Silver chloride Inorganic materials 0.000 description 1
- 229910003090 WSe2 Inorganic materials 0.000 description 1
- 239000002253 acid Substances 0.000 description 1
- 230000004913 activation Effects 0.000 description 1
- 238000013019 agitation Methods 0.000 description 1
- HSFWRNGVRCDJHI-UHFFFAOYSA-N alpha-acetylene Natural products C#C HSFWRNGVRCDJHI-UHFFFAOYSA-N 0.000 description 1
- 230000033228 biological regulation Effects 0.000 description 1
- 150000001786 chalcogen compounds Chemical class 0.000 description 1
- 239000003245 coal Substances 0.000 description 1
- 238000002484 cyclic voltammetry Methods 0.000 description 1
- 230000007812 deficiency Effects 0.000 description 1
- 239000008367 deionised water Substances 0.000 description 1
- 229910021641 deionized water Inorganic materials 0.000 description 1
- 238000010586 diagram Methods 0.000 description 1
- 239000003792 electrolyte Substances 0.000 description 1
- 125000005909 ethyl alcohol group Chemical group 0.000 description 1
- 125000002534 ethynyl group Chemical group [H]C#C* 0.000 description 1
- 230000006872 improvement Effects 0.000 description 1
- 230000004048 modification Effects 0.000 description 1
- 238000012986 modification Methods 0.000 description 1
- 229910052961 molybdenite Inorganic materials 0.000 description 1
- CWQXQMHSOZUFJS-UHFFFAOYSA-N molybdenum disulfide Chemical compound S=[Mo]=S CWQXQMHSOZUFJS-UHFFFAOYSA-N 0.000 description 1
- 229910052982 molybdenum disulfide Inorganic materials 0.000 description 1
- 239000003345 natural gas Substances 0.000 description 1
- 229910000510 noble metal Inorganic materials 0.000 description 1
- 239000003921 oil Substances 0.000 description 1
- 238000005457 optimization Methods 0.000 description 1
- 239000010970 precious metal Substances 0.000 description 1
- 230000008569 process Effects 0.000 description 1
- 239000000047 product Substances 0.000 description 1
- 239000000376 reactant Substances 0.000 description 1
- 230000009467 reduction Effects 0.000 description 1
- 230000001172 regenerating effect Effects 0.000 description 1
- 230000001105 regulatory effect Effects 0.000 description 1
- 235000009566 rice Nutrition 0.000 description 1
- 238000009738 saturating Methods 0.000 description 1
- HKZLPVFGJNLROG-UHFFFAOYSA-M silver monochloride Chemical compound [Cl-].[Ag+] HKZLPVFGJNLROG-UHFFFAOYSA-M 0.000 description 1
- 229910052708 sodium Inorganic materials 0.000 description 1
- 239000011734 sodium Substances 0.000 description 1
- 230000006641 stabilisation Effects 0.000 description 1
- 238000011105 stabilization Methods 0.000 description 1
- 238000003860 storage Methods 0.000 description 1
- 229910052723 transition metal Inorganic materials 0.000 description 1
- 238000002604 ultrasonography Methods 0.000 description 1
- 239000002699 waste material Substances 0.000 description 1
- 239000003643 water by type Substances 0.000 description 1
Classifications
-
- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01G—COMPOUNDS CONTAINING METALS NOT COVERED BY SUBCLASSES C01D OR C01F
- C01G41/00—Compounds of tungsten
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01J—CHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
- B01J27/00—Catalysts comprising the elements or compounds of halogens, sulfur, selenium, tellurium, phosphorus or nitrogen; Catalysts comprising carbon compounds
- B01J27/02—Sulfur, selenium or tellurium; Compounds thereof
- B01J27/04—Sulfides
- B01J27/047—Sulfides with chromium, molybdenum, tungsten or polonium
-
- B01J35/33—
-
- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01P—INDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS
- C01P2004/00—Particle morphology
- C01P2004/01—Particle morphology depicted by an image
- C01P2004/03—Particle morphology depicted by an image obtained by SEM
-
- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01P—INDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS
- C01P2004/00—Particle morphology
- C01P2004/30—Particle morphology extending in three dimensions
- C01P2004/32—Spheres
Abstract
The present invention relates to a kind of three petal-shapeds tungsten sulfide nanosphere, preparation method and applications, it comprises the following steps：（a）By tungstates and thiocarbamide formation mixed solution soluble in water；The mass ratio of the tungstates and thiocarbamide is 4.2：1.3~5.3；（b）The mixed solution is placed in autoclave, hydro-thermal reaction is carried out in 220 ~ 250 DEG C, after centrifugation, washing, drying.Preparation technology is simple, and required equipment is conventional, and abundant raw material is cheap, realizes low cost synthesis petal-shaped tungsten sulfide nanometer electrical catalyst；The petal-shaped vulcanization tungsten catalyst of making has preferable electro-catalysis stability, after circulation 40000s, still keeps stable electrocatalytic hydrogen evolution activity.
Description
Technical field
The invention belongs to field of nanometer material technology, it is related to a kind of petal-shaped tungsten sulfide, and in particular to a kind of three petal-shapeds vulcanization
Tungsten nanosphere, preparation method and applications.
Background technology
With the progress and development of society, the development of energy field and resulting energy resource consumption and environmental problem,
Have become the global focus of attention.At present, the fossil energy increasingly depleted such as coal, oil, natural gas, becomes along with weather
Warm, increasingly serious the problems such as environmental degradation, people begin attempt to develop new clean energy resource.It is close as the energy being currently known
Highest, and clean, efficient regenerative resource are spent, hydrogen is the new energy for 21 century most having development potentiality, be expected to the general soon
To replace fossil energy widely to be used in the production and living of people.In recent decades, the technology such as hydrogen storage, production hydrogen is obtained
The development of leap, and in recent years, the technology that hydrogen is obtained by way of water-splitting has attracted the favor of numerous scholars, and
The precious metal materials such as platinum base are as efficient liberation of hydrogen catalyst but because its scarcity limits the condition of large-scale application.Cause
This, developing the overpotential during a kind of catalyst degradation electro-catalysis splitting water of Cheap highly effective turns into current extremely urgent
Task and challenge.
The content of the invention
A kind of preparation of petal-shaped tungsten sulfide nanosphere is provided the invention aims to overcome the deficiencies in the prior art
Method.
To reach above-mentioned purpose, the technical solution adopted by the present invention is：A kind of preparation side of petal-shaped tungsten sulfide nanosphere
Method, it comprises the following steps：
（a）By tungstates and thiocarbamide formation mixed solution soluble in water；The mass ratio of the tungstates and thiocarbamide is 4.2：1.3~
5.3；
（b）The mixed solution is placed in autoclave, hydro-thermal reaction is carried out in 220 ~ 250 DEG C, after centrifugation, washing, drying
.
Optimally, the step（b）In, room temperature is naturally cooled to after hydro-thermal reaction and takes out autoclave, upper strata of inclining is saturating
Prescribed liquid simultaneously takes out black precipitate.
Further, step（b）In, the time of the hydro-thermal reaction is 18 ~ 24 hours.
Optimally, step（b）In, alcohol progress eccentric cleaning is added into black precipitate.
Optimally, the step（b）In, dry mode is using freeze-drying.
A further object of the present invention is to provide a kind of for petal-shaped tungsten sulfide nanosphere made from the above method.
It is still another object of the present invention to provide a kind of above-mentioned petal-shaped tungsten sulfide nanosphere, it is used as liberation of hydrogen catalyst.
By controlling the content of sulphur in petal-shaped tungsten sulfide nanosphere to realize, the regulation to electrocatalytic hydrogen evolution performance can be realized.One
Determine in scope, the electrocatalytic hydrogen evolution performance of tungsten sulfide is improved with the increase of sulfur content.
Optimally, slurry is made in the binder solution that above-mentioned petal-shaped tungsten sulfide nanosphere and acetylene black, solvent dilute, then
It is spin-coated on drying on disk electrode and forms electrode film layer.
Because above-mentioned technical proposal is used, the present invention has following advantages compared with prior art：
（1）For this high problem of noble metal electro-catalysis price used at present, the present invention by the use of sodium tungstate and thiocarbamide as
Raw material, preparation technology is simple, and required equipment is conventional, and abundant raw material is cheap, realizes low cost synthesis petal-shaped tungsten sulfide
Nanometer electrical catalyst；
（2）The vulcanization of the high sulfur content prepared for current this not good problem of tungsten sulfide elctro-catalyst Hydrogen Evolution Performance, the present invention
Tungsten, greatly enhances pure tungsten sulfide electrocatalytic hydrogen evolution performance, in 10 mA/cm-2Current density under, its overpotential drop
Low 89 mV, tower phenanthrene youngster's slope of curve reduces 17 mV/dec；
（3）Regulate and control this problem for current tungsten sulfide elctro-catalyst Hydrogen Evolution Performance, the present invention is by simple adjustment tungsten sulfide
The content of sulphur, is successfully realized the improvement to pure tungsten sulfide electrocatalytic hydrogen evolution performance.Test obtained tungsten sulfide electrocatalytic hydrogen evolution
Performance is improved with the increase of sulfur content, reaches 10 mA/cm-2Current density required for overpotential gradually reduce, accordingly
The luxuriant and rich with fragrance youngster's slope of curve of tower be gradually reduced；
（4）For the problem of activity reduction, the present invention is made in the platinum base used at present and other catalysis material catalytic process
The petal-shaped vulcanization tungsten catalyst of work has preferable electro-catalysis stability, after circulation 40000s, still keeps stabilization
Electrocatalytic hydrogen evolution activity；
（5）Mentioned by the present invention by adjusting the content of sulphur in tungsten sulfide and then regulating and controlling the method for its electrocatalytic hydrogen evolution performance,
Can be generalized to improves the electro catalytic activity of other two-dimentional transition metal chalcogenides, such as MoS2, MoSe2, WSe2Deng enriching
Laminated metal chalcogen compound electrocatalysis characteristic optimization method.
Brief description of the drawings
Fig. 1 is petal-shaped WS synthesized in the embodiment of the present invention 42- 4 scanning electron microscope diagram；
Fig. 2 is WS in the embodiment of the present invention 12- 1 HER catalytic performance test results；
The HER catalytic performance test results that Fig. 3 is WS2-2 in the embodiment of the present invention 2；
The HER catalytic performance test results that Fig. 4 is WS2-3 in the embodiment of the present invention 3；
The HER catalytic performance test results that Fig. 5 is WS2-4 in the embodiment of the present invention 4;
Fig. 6 is the luxuriant and rich with fragrance youngster's curve of tungsten sulfide electrocatalytic hydrogen evolution tower of four kinds of sulfur contents in 1-4 of the embodiment of the present invention；
Fig. 7 is the tungsten sulfide electrocatalytic hydrogen evolution stability of four kinds of sulfur contents in 1-4 of the embodiment of the present invention.
Embodiment
The preparation method of petal-shaped tungsten sulfide nanosphere of the present invention, it comprises the following steps：（a）Tungstates is molten with thiocarbamide
Yu Shuizhong formation mixed solutions；The mass ratio of the tungstates and thiocarbamide is 4.2：1.3~5.3；（b）The mixed solution is put
In autoclave, hydro-thermal reaction is carried out in 220 ~ 250 DEG C, after centrifugation, washing, drying.Made using sodium tungstate and thiocarbamide
For raw material, simply, required equipment is conventional by preparation technology, and abundant raw material is cheap, realizes low cost synthesis petal-shaped vulcanization
Tungsten nanometer electrical catalyst.
Step（b）In, room temperature is naturally cooled to after hydro-thermal reaction and takes out autoclave, upper transparent liquid of inclining simultaneously is taken out
Black precipitate；Alcohol is added into black precipitate and carries out eccentric cleaning；The time of the hydro-thermal reaction is 18 ~ 24 hours；Dry
Mode using freeze-drying.
The present invention is further described below in conjunction with accompanying drawing embodiment.
Embodiment 1
The present embodiment provides a kind of preparation method of petal-shaped tungsten sulfide nanosphere, and it comprises the following steps：
（a）4.2g sodium tungstates and 1.3g thiocarbamides are added in 50ml deionized waters, ultrasonic agitation forms mixed solution in 30 minutes；
（b）Mixed solution is transferred in autoclave, 220 DEG C are heated to, 24h is kept；Then room temperature is naturally cooled to take
Go out, upper transparent liquid is poured into waste liquid barrel, take out black precipitate material；Alcohol is added, then eccentric cleaning 3 times adds
Deionized water, eccentric cleaning 3 times；The product obtained after centrifugation is freezed by way of freeze-drying, obtained vulcanization
Tungsten nanosphere is named as WS2-1。
Embodiment 2
The present embodiment provides a kind of preparation method of petal-shaped tungsten sulfide nanosphere, its preparation process and the base in embodiment 1
This is consistent, unlike：The thiocarbamide of addition is 2.6g, and obtained tungsten sulfide nanosphere is named as WS2-2。
Embodiment 3
The present embodiment provides a kind of preparation method of petal-shaped tungsten sulfide nanosphere, its preparation process and the base in embodiment 1
This is consistent, unlike：The thiocarbamide of addition is 3.9g, and obtained tungsten sulfide nanosphere is named as WS2-3。
Embodiment 4
The present embodiment provides a kind of preparation method of petal-shaped tungsten sulfide nanosphere, its preparation process and the base in embodiment 1
This is consistent, unlike：The thiocarbamide of addition is 5.3g, and obtained tungsten sulfide nanosphere is named as WS2- 4, its pattern such as Fig. 1 institute
Show.
Embodiment 5
The present embodiment provides a kind of preparation method of petal-shaped tungsten sulfide nanosphere, its preparation process and the base in embodiment 1
This is consistent, unlike：The temperature of hydro-thermal reaction is 250 DEG C, and obtained tungsten sulfide nanosphere is named as WS2-5。
Embodiment 6
This example provides a kind of application of petal-shaped tungsten sulfide nanosphere, is specifically to vulcanize the petal-shaped obtained in embodiment 1 to 5
Tungsten nanosphere is prepared into tungsten sulfide catalyst electrode：Weigh 8 mg petal-shaped tungsten sulfides（WS2-1、WS2-2、WS2- 3 and WS2-4）、
2 mg acetylene blacks, are added in the mixed solution containing 350 μ L absolute ethyl alcohols and 95 μ L 5wt% Nafion, ultrasound 30 ~ 60 minutes,
Form mixed uniformly slurry.Take 7 μ L slurries to be coated in rotating disk electrode (r.d.e), dry 10 ~ 30 minutes, form uniform smooth
Electrode film layer, material load is 0.64 mg/cm-2。
The electrocatalytic hydrogen evolution performance test of tungsten sulfide in acid condition：Using the sulfuric acid of 0.5 mol/L as electrolyte, on
It is working electrode to state the vulcanization W film for being coated in disk electrode prepared by embodiment, and metal platinum filament is to electrode, saturation Ag/
AgCl is reference electrode, and rotating speed is 1600 rpms during test.Carry out before electrocatalysis characteristic test, first with 10 ~ 100 mV/s
Sweep speed carry out cyclic voltammetry scan 50 ~ 200 enclose, with cure activation tungsten catalyst.
The electrocatalytic hydrogen evolution performance of tungsten sulfide is improved with the increase of sulfur content.In order to obtain 10 mA/cm-2Electric current
Density, WS2-1、WS2-2、WS2-3、WS2Overpotential required for -4 is respectively 310,272,240 and 221 mV；On the other hand,
WS2-1、WS2-2、WS2-3、WS2The luxuriant and rich with fragrance youngster's slope of curve of -4 towers showed is respectively 64,52.3,50.8 and 47 mV/dec.I.e.
When the mass ratio of sodium tungstate in reactant and thiocarbamide is from 4.2：1.3 change to 4.2：When 5.3, resulting petal-shaped tungsten sulfide is received
Rice ball is in 10 mA/cm-2Current density when the liberation of hydrogen overpotential that needs be reduced to 221 mV by 310 mV, tower phenanthrene youngster's curve is oblique
Rate is that 64 mV/dec are reduced to 47 mV/dec, illustrates sulfur content highest WS2- 4 have highest electrocatalytic hydrogen evolution activity（I.e.
Electrocatalytic hydrogen evolution performance improves with the increase of sulfur content, as shown in Figures 2 to 6）.In addition, WS2-1、WS2-2、WS2-3、
WS2- 4 are all demonstrated by preferable electrocatalytic hydrogen evolution stability（As shown in Figure 7）.
The above embodiments merely illustrate the technical concept and features of the present invention, and its object is to allow person skilled in the art
Scholar can understand present disclosure and implement according to this, and it is not intended to limit the scope of the present invention, all according to the present invention
The equivalent change or modification that Spirit Essence is made, should all be included within the scope of the present invention.
Claims (8)
1. a kind of preparation method of petal-shaped tungsten sulfide nanosphere, it is characterised in that it comprises the following steps：
（a）By tungstates and thiocarbamide formation mixed solution soluble in water；The mass ratio of the tungstates and thiocarbamide is 4.2：1.3~
5.3；
（b）The mixed solution is placed in autoclave, hydro-thermal reaction is carried out in 220 ~ 250 DEG C, after centrifugation, washing, drying
.
2. the preparation method of petal-shaped tungsten sulfide nanosphere according to claim 1, it is characterised in that：The step（b）In,
Naturally cool to room temperature after hydro-thermal reaction to take out autoclave, upper transparent liquid of inclining simultaneously takes out black precipitate.
3. the preparation method of petal-shaped tungsten sulfide nanosphere according to claim 2, it is characterised in that：Step（b）In, it is described
The time of hydro-thermal reaction is 18 ~ 24 hours.
4. the preparation method of petal-shaped tungsten sulfide nanosphere according to claim 2, it is characterised in that：Step（b）In, to black
Alcohol, which is added, in color precipitation carries out eccentric cleaning.
5. the preparation method of petal-shaped tungsten sulfide nanosphere according to claim 1, it is characterised in that：The step（b）In,
Dry mode is using freeze-drying.
6. a kind of petal-shaped tungsten sulfide nanosphere, it is characterised in that：Its any described preparation method system in claim 1 to 5
.
7. the application of petal-shaped tungsten sulfide nanosphere described in a kind of claim 6, it is characterised in that：It is used as liberation of hydrogen catalyst.
8. the application of petal-shaped tungsten sulfide nanosphere according to claim 7, it is characterised in that：By it and acetylene black, solvent
The binder solution of dilution is made slurry, then is spin-coated on drying on disk electrode and forms electrode film layer.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201710328302.5A CN107188232A (en) | 2017-05-11 | 2017-05-11 | A kind of petal-shaped tungsten sulfide nanosphere, preparation method and applications |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201710328302.5A CN107188232A (en) | 2017-05-11 | 2017-05-11 | A kind of petal-shaped tungsten sulfide nanosphere, preparation method and applications |
Publications (1)
| Publication Number | Publication Date |
|---|---|
| CN107188232A true CN107188232A (en) | 2017-09-22 |
Family
ID=59873262
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| CN201710328302.5A Pending CN107188232A (en) | 2017-05-11 | 2017-05-11 | A kind of petal-shaped tungsten sulfide nanosphere, preparation method and applications |
Country Status (1)
| Country | Link |
|---|---|
| CN (1) | CN107188232A (en) |
Cited By (7)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN107907557A (en) * | 2017-11-21 | 2018-04-13 | 苏州大学 | A kind of WS2S atom deposits Pt the verification method of selection in nanometer sheet |
| CN108899496A (en) * | 2018-06-20 | 2018-11-27 | 电子科技大学 | Graphene adulterates WS2Preparation method and the application in lithium/sodium-ion battery |
| CN109264784A (en) * | 2018-10-30 | 2019-01-25 | 陕西科技大学 | A kind of preparation method of the flower-shaped tungsten disulfide electrode material of three-dimensional self assembly |
| CN110683581A (en) * | 2018-07-04 | 2020-01-14 | 湖北大学 | Self-assembly thousand-layer-shaped WS2Method for preparing nano structure |
| CN112316956A (en) * | 2020-11-16 | 2021-02-05 | 青岛科技大学 | WS (WS)2Preparation method and application of/FeS nanosphere hybrid catalyst |
| CN113999495A (en) * | 2021-11-16 | 2022-02-01 | 嘉兴学院 | Carbon fiber/epoxy composite material with integrated structure and function and preparation method thereof |
| CN114835163A (en) * | 2022-05-24 | 2022-08-02 | 南京邮电大学 | Novel tungsten sulfide photo-thermal material for water quality purification and preparation and application thereof |
Citations (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN103818963A (en) * | 2014-02-21 | 2014-05-28 | 福州大学 | One-step hydrothermal method for synthesizing nanoflake tungsten sulfide |
-
2017
- 2017-05-11 CN CN201710328302.5A patent/CN107188232A/en active Pending
Patent Citations (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN103818963A (en) * | 2014-02-21 | 2014-05-28 | 福州大学 | One-step hydrothermal method for synthesizing nanoflake tungsten sulfide |
Non-Patent Citations (4)
| Title |
|---|
| M. THRIPURANTHAKA等: "Temperature dependent Raman spectroscopy of chemically derived few layer MoS2and WS2nanosheets", 《APPLIED PHYSICS LETTERS》 * |
| QIN LIU等: "Stable metallic 1T-WS2ultrathin nanosheets as a promising agent for near-infrared photothermal ablation cancer therapy", 《NANO RESEARCH》 * |
| 张向华: "超薄MS2（M=Mo,W）纳米片的制备与性能研究", 《中国博士学位论文全文数据库 工程科技Ⅰ辑 》 * |
| 谢俊峰: "二维晶体的功能导向性设计及其电化学性能研究", 《中国博士学位论文全文数据库 工程科技Ⅰ辑》 * |
Cited By (12)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN107907557A (en) * | 2017-11-21 | 2018-04-13 | 苏州大学 | A kind of WS2S atom deposits Pt the verification method of selection in nanometer sheet |
| CN107907557B (en) * | 2017-11-21 | 2020-04-28 | 苏州大学 | WS (WS)2Verification method for Pt deposition selection by S atoms in nanosheets |
| CN108899496A (en) * | 2018-06-20 | 2018-11-27 | 电子科技大学 | Graphene adulterates WS2Preparation method and the application in lithium/sodium-ion battery |
| CN108899496B (en) * | 2018-06-20 | 2021-11-02 | 电子科技大学 | Graphene doped WS2Preparation method and application in lithium/sodium ion battery |
| CN110683581A (en) * | 2018-07-04 | 2020-01-14 | 湖北大学 | Self-assembly thousand-layer-shaped WS2Method for preparing nano structure |
| CN109264784A (en) * | 2018-10-30 | 2019-01-25 | 陕西科技大学 | A kind of preparation method of the flower-shaped tungsten disulfide electrode material of three-dimensional self assembly |
| CN112316956A (en) * | 2020-11-16 | 2021-02-05 | 青岛科技大学 | WS (WS)2Preparation method and application of/FeS nanosphere hybrid catalyst |
| CN112316956B (en) * | 2020-11-16 | 2022-09-06 | 青岛科技大学 | WS (WS) 2 Preparation method and application of FeS nanosphere hybrid catalyst |
| CN113999495A (en) * | 2021-11-16 | 2022-02-01 | 嘉兴学院 | Carbon fiber/epoxy composite material with integrated structure and function and preparation method thereof |
| CN113999495B (en) * | 2021-11-16 | 2023-07-07 | 嘉兴学院 | Structural-function-integrated carbon fiber/epoxy composite material and preparation method thereof |
| CN114835163A (en) * | 2022-05-24 | 2022-08-02 | 南京邮电大学 | Novel tungsten sulfide photo-thermal material for water quality purification and preparation and application thereof |
| CN114835163B (en) * | 2022-05-24 | 2023-07-21 | 南京邮电大学 | Novel tungsten sulfide photo-thermal material for water purification and preparation and application thereof |
Similar Documents
| Publication | Publication Date | Title |
|---|---|---|
| CN107188232A (en) | A kind of petal-shaped tungsten sulfide nanosphere, preparation method and applications | |
| Chen et al. | Recent advances in the utilization of copper sulfide compounds for electrochemical CO2 reduction | |
| CN108796551B (en) | Sea urchin-shaped cobalt sulfide catalyst loaded on foamed nickel, preparation method thereof and application of catalyst as electrolyzed water oxygen evolution catalyst | |
| CN109659143A (en) | A kind of nickel hydroxide/three nickel of curing/foam nickel composite and the preparation method and application thereof | |
| CN106532040B (en) | A kind of H-MoS2/ NG nanocomposite and preparation method and application | |
| CN108147472A (en) | A kind of preparation method of hollow cobalt sulfide microspherical catalyst | |
| CN108441884A (en) | Compound Electrocatalytic Activity for Hydrogen Evolution Reaction agent of molybdenum disulfide/carbon and preparation method thereof | |
| CN109621981B (en) | Metal oxide-sulfide composite oxygen evolution electrocatalyst and preparation method and application thereof | |
| CN107326384A (en) | Composite of eight nine cobalts of vulcanization and titanium dioxide and its preparation method and application | |
| CN109954503A (en) | A kind of nickelous selenide and ternary selenizing ferronickel composite electrocatalyst and preparation method and application | |
| CN106622301B (en) | A kind of MoS of hierarchical structure2Difunctional VPO catalysts of nanosphere and its preparation method and application | |
| CN109355673B (en) | Au-Ag/Ag2S heterojunction nano hydrogen evolution catalyst and preparation method thereof | |
| CN112958116B (en) | Bi2O2.33-CdS composite photocatalyst and preparation process thereof | |
| CN106563471A (en) | Core-shell CoS2@NG nanometer composite material, and preparation and application thereof | |
| CN108493297B (en) | Preparation method of three-dimensional hollow selenium nickel sulfide nano-frame catalyst | |
| CN110474050A (en) | A kind of doping type carbon/manganese sulfide composite material and preparation method thereof | |
| CN111974415A (en) | Copper sulfide/brass mesh electrode material with nanosheet array structure and preparation method and application thereof | |
| CN110586127B (en) | Preparation method and application of platinum-cobalt bimetallic hollow nanospheres | |
| CN106299395B (en) | A kind of NiO/rGO composite material having efficient electric catalytic oxidation-reduction performance | |
| CN106129414B (en) | A kind of high specific capacity secondary ion battery metal organic cathode material and preparation method thereof | |
| CN108273524B (en) | Carbon composite material modified by chalcogenide and transition metal and preparation method and application thereof | |
| Guo et al. | Direct Z-scheme high-entropy metal phosphides/ZnIn2S4 heterojunction for efficient photocatalytic hydrogen evolution | |
| CN108404938A (en) | A kind of electrocatalytic hydrogen evolution MoS2Nano flower sphere catalyst and preparation method thereof | |
| CN108823602A (en) | A kind of vulcanization ruthenium particulate composite, preparation method and the usage | |
| CN107293759A (en) | A kind of preparation method of fuel cell oxygen reduction electrocatalyst |
Legal Events
| Date | Code | Title | Description |
|---|---|---|---|
| PB01 | Publication | ||
| PB01 | Publication | ||
| SE01 | Entry into force of request for substantive examination | ||
| SE01 | Entry into force of request for substantive examination | ||
| RJ01 | Rejection of invention patent application after publication |
Application publication date: 20170922 |
|
| RJ01 | Rejection of invention patent application after publication |