CN106362775B - A kind of high efficiency photocatalysis based on molybdenum sulfide prepares the nano material and preparation method of hydrogen - Google Patents
A kind of high efficiency photocatalysis based on molybdenum sulfide prepares the nano material and preparation method of hydrogen Download PDFInfo
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- 239000001257 hydrogen Substances 0.000 title claims abstract description 41
- 229910052739 hydrogen Inorganic materials 0.000 title claims abstract description 41
- CWQXQMHSOZUFJS-UHFFFAOYSA-N molybdenum disulfide Chemical compound S=[Mo]=S CWQXQMHSOZUFJS-UHFFFAOYSA-N 0.000 title claims abstract description 40
- UFHFLCQGNIYNRP-UHFFFAOYSA-N Hydrogen Chemical compound [H][H] UFHFLCQGNIYNRP-UHFFFAOYSA-N 0.000 title claims abstract description 32
- 230000001699 photocatalysis Effects 0.000 title claims abstract description 32
- 238000007146 photocatalysis Methods 0.000 title claims abstract description 32
- 239000002086 nanomaterial Substances 0.000 title claims abstract description 29
- 238000002360 preparation method Methods 0.000 title claims abstract description 16
- PCHJSUWPFVWCPO-UHFFFAOYSA-N gold Chemical compound [Au] PCHJSUWPFVWCPO-UHFFFAOYSA-N 0.000 claims abstract description 44
- 239000010931 gold Substances 0.000 claims abstract description 44
- 229910052737 gold Inorganic materials 0.000 claims abstract description 44
- 150000002431 hydrogen Chemical class 0.000 claims abstract description 9
- 239000002245 particle Substances 0.000 claims abstract description 8
- 238000000034 method Methods 0.000 claims abstract description 7
- 229920000642 polymer Polymers 0.000 claims abstract description 3
- 235000013339 cereals Nutrition 0.000 claims description 39
- 238000012360 testing method Methods 0.000 claims description 14
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Chemical compound O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims description 13
- 239000008367 deionised water Substances 0.000 claims description 12
- 229910021641 deionized water Inorganic materials 0.000 claims description 12
- 229910052724 xenon Inorganic materials 0.000 claims description 12
- FHNFHKCVQCLJFQ-UHFFFAOYSA-N xenon atom Chemical compound [Xe] FHNFHKCVQCLJFQ-UHFFFAOYSA-N 0.000 claims description 12
- 239000003643 water by type Substances 0.000 claims description 11
- NLJMYIDDQXHKNR-UHFFFAOYSA-K sodium citrate Chemical compound O.O.[Na+].[Na+].[Na+].[O-]C(=O)CC(O)(CC([O-])=O)C([O-])=O NLJMYIDDQXHKNR-UHFFFAOYSA-K 0.000 claims description 8
- 239000001509 sodium citrate Substances 0.000 claims description 8
- 239000007788 liquid Substances 0.000 claims description 7
- SJUCACGNNJFHLB-UHFFFAOYSA-N O=C1N[ClH](=O)NC2=C1NC(=O)N2 Chemical compound O=C1N[ClH](=O)NC2=C1NC(=O)N2 SJUCACGNNJFHLB-UHFFFAOYSA-N 0.000 claims description 6
- 238000006243 chemical reaction Methods 0.000 claims description 6
- XUJNEKJLAYXESH-UHFFFAOYSA-N cysteine Natural products SCC(N)C(O)=O XUJNEKJLAYXESH-UHFFFAOYSA-N 0.000 claims description 6
- 235000018417 cysteine Nutrition 0.000 claims description 6
- 239000011684 sodium molybdate Substances 0.000 claims description 6
- 235000015393 sodium molybdate Nutrition 0.000 claims description 6
- TVXXNOYZHKPKGW-UHFFFAOYSA-N sodium molybdate (anhydrous) Chemical compound [Na+].[Na+].[O-][Mo]([O-])(=O)=O TVXXNOYZHKPKGW-UHFFFAOYSA-N 0.000 claims description 6
- 238000002604 ultrasonography Methods 0.000 claims description 6
- 238000001027 hydrothermal synthesis Methods 0.000 claims description 5
- 229920000151 polyglycol Polymers 0.000 claims description 5
- 239000010695 polyglycol Substances 0.000 claims description 5
- 239000002243 precursor Substances 0.000 claims description 5
- 238000009835 boiling Methods 0.000 claims description 2
- 240000007594 Oryza sativa Species 0.000 claims 1
- 235000007164 Oryza sativa Nutrition 0.000 claims 1
- FDWREHZXQUYJFJ-UHFFFAOYSA-M gold monochloride Chemical compound [Cl-].[Au+] FDWREHZXQUYJFJ-UHFFFAOYSA-M 0.000 claims 1
- 239000006193 liquid solution Substances 0.000 claims 1
- 239000002105 nanoparticle Substances 0.000 claims 1
- 235000009566 rice Nutrition 0.000 claims 1
- 238000010521 absorption reaction Methods 0.000 abstract description 6
- 239000003054 catalyst Substances 0.000 abstract description 6
- 230000003197 catalytic effect Effects 0.000 abstract description 6
- 150000001875 compounds Chemical class 0.000 abstract description 5
- 230000007547 defect Effects 0.000 abstract description 4
- 238000005516 engineering process Methods 0.000 abstract description 3
- 230000001808 coupling effect Effects 0.000 abstract description 2
- 239000000463 material Substances 0.000 description 8
- 230000000694 effects Effects 0.000 description 5
- 238000004519 manufacturing process Methods 0.000 description 5
- ZOKXTWBITQBERF-UHFFFAOYSA-N Molybdenum Chemical compound [Mo] ZOKXTWBITQBERF-UHFFFAOYSA-N 0.000 description 4
- 238000012512 characterization method Methods 0.000 description 4
- 238000010438 heat treatment Methods 0.000 description 4
- 239000002082 metal nanoparticle Substances 0.000 description 4
- 230000002186 photoactivation Effects 0.000 description 4
- LYCAIKOWRPUZTN-UHFFFAOYSA-N Ethylene glycol Chemical compound OCCO LYCAIKOWRPUZTN-UHFFFAOYSA-N 0.000 description 3
- 239000002131 composite material Substances 0.000 description 3
- 229910052750 molybdenum Inorganic materials 0.000 description 3
- 239000011733 molybdenum Substances 0.000 description 3
- 238000004073 vulcanization Methods 0.000 description 3
- 239000002202 Polyethylene glycol Substances 0.000 description 2
- GWEVSGVZZGPLCZ-UHFFFAOYSA-N Titan oxide Chemical compound O=[Ti]=O GWEVSGVZZGPLCZ-UHFFFAOYSA-N 0.000 description 2
- 229920001223 polyethylene glycol Polymers 0.000 description 2
- 238000011160 research Methods 0.000 description 2
- WUPHOULIZUERAE-UHFFFAOYSA-N 3-(oxolan-2-yl)propanoic acid Chemical compound OC(=O)CCC1CCCO1 WUPHOULIZUERAE-UHFFFAOYSA-N 0.000 description 1
- BRSVJNYNWNMJKC-UHFFFAOYSA-N [Cl].[Au] Chemical compound [Cl].[Au] BRSVJNYNWNMJKC-UHFFFAOYSA-N 0.000 description 1
- 239000002253 acid Substances 0.000 description 1
- 230000005540 biological transmission Effects 0.000 description 1
- 229910052980 cadmium sulfide Inorganic materials 0.000 description 1
- 239000011258 core-shell material Substances 0.000 description 1
- 230000005611 electricity Effects 0.000 description 1
- 230000002708 enhancing effect Effects 0.000 description 1
- 239000007789 gas Substances 0.000 description 1
- 230000031700 light absorption Effects 0.000 description 1
- 229910052751 metal Inorganic materials 0.000 description 1
- 239000002184 metal Substances 0.000 description 1
- 238000012827 research and development Methods 0.000 description 1
- 239000004408 titanium dioxide Substances 0.000 description 1
Classifications
-
- 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
- B01J27/051—Molybdenum
-
- B01J35/39—
-
- B01J35/393—
-
- B01J35/396—
-
- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01B—NON-METALLIC ELEMENTS; COMPOUNDS THEREOF; METALLOIDS OR COMPOUNDS THEREOF NOT COVERED BY SUBCLASS C01C
- C01B3/00—Hydrogen; Gaseous mixtures containing hydrogen; Separation of hydrogen from mixtures containing it; Purification of hydrogen
- C01B3/02—Production of hydrogen or of gaseous mixtures containing a substantial proportion of hydrogen
- C01B3/04—Production of hydrogen or of gaseous mixtures containing a substantial proportion of hydrogen by decomposition of inorganic compounds, e.g. ammonia
- C01B3/042—Decomposition of water
-
- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01B—NON-METALLIC ELEMENTS; COMPOUNDS THEREOF; METALLOIDS OR COMPOUNDS THEREOF NOT COVERED BY SUBCLASS C01C
- C01B2203/00—Integrated processes for the production of hydrogen or synthesis gas
- C01B2203/10—Catalysts for performing the hydrogen forming reactions
- C01B2203/1041—Composition of the catalyst
-
- 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
- Y02E60/30—Hydrogen technology
- Y02E60/36—Hydrogen production from non-carbon containing sources, e.g. by water electrolysis
Abstract
The present invention relates to nano materials and preparation method that a kind of high efficiency photocatalysis based on molybdenum sulfide prepares hydrogen, in the nano material of molybdenum sulfide, add gold nano grain, not only widen the absorption region of visible light, photo-generated carrier can also be made to be transferred to gold nano grain simultaneously, further solve the easily compound defect of the photo-generated carrier of molybdenum sulfide.On the other hand, gold nano grain is at polymer state, and the quantity of gold nano grain is 26, and that between gold nano grain and particle is specially 5 7nm.So it is short it is specific make to generate strong coupling effect between particle and particle, from there is the absorption for further improving light.Meanwhile preparation process is the method for using a step hydro-thermal, eliminates complicated preparation process, and greatly reduce cost.Since it prepares as photocatalysis the catalyst of hydrogen, catalytic effect is notable, can be pushed further into the technology extensive use that photocatalysis prepares hydrogen.
Description
Technical field
The invention belongs to catalytic field, be related to a kind of high efficiency photocatalysis based on molybdenum sulfide prepare hydrogen nano material and
Preparation method.
Background technology
In order to solve the energy crisis encountered at present, photocatalysis prepares this field of hydrogen and has also obtained extensive concern
And research.From initial titanium dioxide, cadmium sulfide to the two-dimensional material studied extensively at present, photocatalysis prepares the nanometer material of hydrogen
Material has obtained significant progress.But the catalytic efficiency of catalyst still cannot be improved effectively.Presently, in light
In the preparation of catalyst, efficient catalyst is still the emphasis of research and development.(X.Xie,K.Kretschmer,G.Wang,
Nanoscale 2015,7,13278.Y.Yan,B.Xia,Z.Xu,X.Wang,ACS Catal.2014,4,1693.)。
In recent years, due to the hydrogen evolution activity site of high activity, molybdenum sulfide receives extensively as good catalyzing manufacturing of hydrogen material
General research.(N.Kumar,and J.M.Seminario,J.Phys.Chem.C 2015,119,29157.J.Benson,M.Li,
S.Wang, P.Wang, P.Papakonstantinou, ACS Appl.Mater.Inter.2015,7,14113.) but due to
The absorption region of its visible light is relatively narrow, while the defect that photo-generated carrier is easily compound, and molybdenum sulfide does not have as catalyzing manufacturing of hydrogen material
It is used widely.(Q.Liu,X.Li,Q.He,A.Khalil,D.Liu,T.Xiang,X.Wu,L.Song,Small 2015,
11,5556.)。
To solve the above-mentioned problems, metal nanoparticle is introduced into molybdenum sulfide and metal nano is made by researchers
Grain/vulcanization molybdenum composite material.Utilize the plasma effect and metal nanoparticle of metal nanoparticle and the activity of molybdenum sulfide
The absorption region of contact surface, the composite material not only visible light is wider, but also photo-generated carrier is easily separated, improves catalyzing manufacturing of hydrogen
Efficiency.However, the plasma enhancing catalytic efficiency of the compound is still very low.(Z.B.Zhuang,W.C.Sheng,Y.S.Yan,
Adv.Mater.2014,26,3950.)。
Invention content
Technical problems to be solved
In order to avoid the shortcomings of the prior art, the present invention proposes that a kind of high efficiency photocatalysis based on molybdenum sulfide prepares hydrogen
The nano material and preparation method of gas.
Technical solution
A kind of high efficiency photocatalysis based on molybdenum sulfide prepares the nano material of hydrogen, it is characterised in that gold nano grain is at more
The quantity of multimeric state, gold nano grain is 2-6, and the distance between gold nano grain and particle are 5-7nm;The molar ratio of element
Value Wei Mu ︰ Liu ︰ gold is 1.0 ︰, 1.9 ︰ 1.2.
A method of preparing the nano material that the high efficiency photocatalysis based on molybdenum sulfide prepares hydrogen, it is characterised in that
Steps are as follows:
The preparation of step 1, gold nano grain:The deionized water of the chlorauric acid solution of 200 μ l and 100ml is mixed and heated to
The sodium citrate solution of 700 μ l is added dropwise after boiling, is heated to 100 DEG C and 10-15min is kept to obtain gold nano grain;The chlorine gold
A concentration of 50-100mg/ml of acid solution;The sodium citrate solution is 1-5wt%;
The preparation of step 2, molybdenum sulfide precursor solution:The cysteine of 0.5-1.0g is dissolved in 100ml deionized waters,
Obtain solution A;The sodium molybdate of 0.5-1.0g is dissolved in the deionized water of 100ml, solution B is obtained;Solution A and solution B are pressed
Volume ratio 2:1 mixing ultrasound 2-4h obtains molybdenum sulfide precursor solution;
Step 3:The gold nano grain solution of 40-80ml is mixed with the polyglycol solution of 10-30ml, later with vulcanization
Molybdenum precursor solution is mixed, and the hydro-thermal reaction of 10-24h is carried out at 200 DEG C;After reaction, by solution dry to get
To the nano material of gold nano grain and molybdenum sulfide nucleocapsid;A concentration of 1%-3% of the polyglycol solution.
A kind of method that the high efficiency photocatalysis based on molybdenum sulfide prepares the nano material of hydrogen described in test, feature exist
In:The nano material of the gold nano grain and molybdenum sulfide nucleocapsid of 0.1g, is dispersed in 100ml deionized waters;It is urged using light
Change equipment and carries out the test that photocatalysis prepares hydrogen;The test condition that photocatalysis prepares hydrogen is:Light source is xenon lamp, electricity consumption flow control
Xenon source intensity processed, electric current 15A.
Advantageous effect
A kind of high efficiency photocatalysis based on molybdenum sulfide proposed by the present invention prepares the nano material and preparation method of hydrogen,
In the nano material of molybdenum sulfide, gold nano grain is added, not only widens the absorption region of visible light, while photoproduction can also be made
Carrier transport further solves the easily compound defect of the photo-generated carrier of molybdenum sulfide to gold nano grain.On the other hand, Jenner
Rice grain is at polymer state, and the quantity of gold nano grain is 2-6, and that between gold nano grain and particle is specially 5-7nm.Such as
This it is short it is specific make to generate strong coupling effect between particle and particle, from there is the absorption for further improving light.Meanwhile
Preparation process is the method for using a step hydro-thermal, eliminates complicated preparation process, and greatly reduce cost.Due to its work
The catalyst of hydrogen is prepared for photocatalysis, catalytic effect is notable, can be pushed further into photocatalysis prepare hydrogen technology it is wide
General application.
Compared with catalyst material hydrogen manufacturing, gold nano grain provided by the invention/molybdenum sulfide core-shell structured nanomaterials are not
Only there is stronger light absorption, and customer service photo-generated carrier easily compound defect.On the other hand, which has more
High plasma enhances catalytic efficiency.The hydrogen-producing speed of the material is to be currently known one of maximum material of hydrogen-producing speed, is reached
2510.7 every gram of micromoles.
Description of the drawings
Fig. 1 is the transmission electron microscope picture of metal nanoparticle/vulcanization molybdenum composite material.Wherein 0.5 μm is size scale
Fig. 2 is the X-ray energy spectrometer interpretation of result figure of the nano material of gold nano grain and molybdenum sulfide nucleocapsid
Specific implementation mode
In conjunction with embodiment, attached drawing, the invention will be further described:
Embodiment one:
The deionized water mixing for taking the chlorauric acid solution (50mg/ml) and 100ml of 200 μ l, is heated to boil, then be added dropwise
The sodium citrate solution (1wt%) of 700 μ l, heating 10min obtain gold nano grain solution.The cysteine of 0.5g is taken to be dissolved in
In 100ml deionized waters, solution A is obtained.It takes the sodium molybdate of 0.5-1.0g to be dissolved in the deionized water of 100ml, obtains solution B.
Solution A and solution B by volume 2:1 mixing ultrasound 2-4h.40-80ml gold nano grain solution is added to 10ml, 1% it is poly-
It in ethylene glycol solution, is mixed later with the ultrasonic mixing liquid of above-mentioned A and B, the hydro-thermal that 10h is then carried out at 200 DEG C is anti-
It answers.After reaction, solution is dried for 24 hours down for 110 degree in an oven, you can obtains gold nano grain/molybdenum sulfide nucleocapsid
Nano material.
Characterization:The nano material for taking gold nano grain/molybdenum sulfide nucleocapsid of 0.1g, is dispersed in 100ml deionized waters
In.Photoactivation equipment carries out the test that photocatalysis prepares hydrogen.The test condition that photocatalysis prepares hydrogen is:Light source is xenon
Lamp, with current control xenon source intensity, electric current 15A.Maximum hydrogen output is 2500.7 every gram of micromoles.
Embodiment two:
The deionized water mixing for taking the chlorauric acid solution (70mg/ml) and 100ml of 200 μ l, is heated to boil, then be added dropwise
The sodium citrate solution (2wt%) of 700 μ l, heating 15min obtain gold nano grain solution.The cysteine of 0.7g is taken to be dissolved in
In 100ml deionized waters, solution A is obtained.It takes the sodium molybdate of 0.7g to be dissolved in the deionized water of 100ml, obtains solution B.Solution A
With solution B by volume 2:1 mixing ultrasound 2-4h.50ml gold nano grain solution is added to 20ml, 2% polyethylene glycol is molten
It in liquid, is mixed later with the ultrasonic mixing liquid of above-mentioned A and B, the hydro-thermal reaction of 16h is then carried out at 200 DEG C.Reaction knot
Shu Hou, solution dry down 36h for 110 degree in an oven, you can obtain the nano material of gold nano grain/molybdenum sulfide nucleocapsid.
Characterization:The nano material for taking gold nano grain/molybdenum sulfide nucleocapsid of 0.1g, is dispersed in 100ml deionized waters
In.Photoactivation equipment carries out the test that photocatalysis prepares hydrogen.The test condition that photocatalysis prepares hydrogen is:Light source is xenon
Lamp, with current control xenon source intensity, electric current 15A.Maximum hydrogen output is 2510.7 every gram of micromoles.
Embodiment three:
The deionized water mixing for taking the chlorauric acid solution (80mg/ml) and 100ml of 200 μ l, is heated to boil, then be added dropwise
The sodium citrate solution (3wt%) of 700 μ l, heating 10min obtain gold nano grain solution.The cysteine of 0.8g is taken to be dissolved in
In 100ml deionized waters, solution A is obtained.It takes the sodium molybdate of 0.8g to be dissolved in the deionized water of 100ml, obtains solution B.Solution A
With solution B by volume 2:1 mixing ultrasound 2-4h.60ml gold nano grain solution is added to 30ml, 3%, polyethylene glycol is molten
It in liquid, is mixed later with the ultrasonic mixing liquid of above-mentioned A and B, the hydro-thermal reaction of 18h is then carried out at 200 DEG C.Reaction knot
Shu Hou, solution dry down 48h for 110 degree in an oven, you can obtain the nano material of gold nano grain/molybdenum sulfide nucleocapsid.
Characterization:The nano material for taking gold nano grain/molybdenum sulfide nucleocapsid of 0.1g, is dispersed in 100ml deionized waters
In.Photoactivation equipment carries out the test that photocatalysis prepares hydrogen.The test condition that photocatalysis prepares hydrogen is:Light source is xenon
Lamp, with current control xenon source intensity, electric current 15A.Maximum hydrogen output is 2503.7 every gram of micromoles.
Example IV:
The deionized water mixing for taking the chlorauric acid solution (80mg/ml) and 100ml of 200 μ l, is heated to boil, then be added dropwise
The sodium citrate solution (5wt%) of 700 μ l, heating 10min obtain gold nano grain solution.The cysteine of 1.0g is taken to be dissolved in
In 100ml deionized waters, solution A is obtained.It takes the sodium molybdate of 1.0g to be dissolved in the deionized water of 100ml, obtains solution B.Solution A
With solution B by volume 2:1 mixing ultrasound 4h.60ml gold nano grain solution is added to 30ml, 3% polyglycol solution
In, it is mixed later with the ultrasonic mixing liquid of above-mentioned A and B, hydro-thermal reaction for 24 hours is then carried out at 200 DEG C.Reaction terminates
Afterwards, solution dries down 48h for 110 degree in an oven, you can obtains the nano material of gold nano grain/molybdenum sulfide nucleocapsid.
Characterization:The nano material for taking gold nano grain/molybdenum sulfide nucleocapsid of 0.1g, is dispersed in 100ml deionized waters
In.Photoactivation equipment carries out the test that photocatalysis prepares hydrogen.The test condition that photocatalysis prepares hydrogen is:Light source is xenon
Lamp, with current control xenon source intensity, electric current 15A.2503.7 every gram of micromole of maximum production hydrogen rate.
Claims (3)
1. a kind of high efficiency photocatalysis based on molybdenum sulfide prepares the nano material of hydrogen, it is characterised in that:The nano material is
Gold nano grain and molybdenum sulfide nucleocapsid, for gold nano grain at polymer state, the quantity of gold nano grain is 2-6, Jenner
The distance between rice grain and particle are 5-7nm;The molar ratio Wei Mu ︰ Liu ︰ gold of element is 1.0 ︰, 1.9 ︰ 1.2.
2. a kind of method for preparing the high efficiency photocatalysis based on molybdenum sulfide described in claim 1 and preparing the nano material of hydrogen,
It is characterized in that steps are as follows:
The preparation of step 1, gold nano grain:The deionized water of the chlorauric acid solution of 200 μ l and 100ml is mixed and heated to boiling
The sodium citrate solution of 700 μ l is added dropwise afterwards, is heated to 100 DEG C and 10-15min is kept to obtain gold nano grain;The gold chloride is molten
A concentration of 50-100mg/ml of liquid;The sodium citrate solution is 1-5wt%;
The preparation of step 2, molybdenum sulfide precursor solution:The cysteine of 0.5-1.0g is dissolved in 100ml deionized waters, is obtained
Solution A;The sodium molybdate of 0.5-1.0g is dissolved in the deionized water of 100ml, solution B is obtained;Solution A and solution B are pressed into volume
Than 2:1 mixing ultrasound 2-4h obtains molybdenum sulfide precursor solution;
Step 3:The gold nano grain solution of 40-80ml is mixed with the polyglycol solution of 10-30ml, later with before molybdenum sulfide
It drives liquid solution to be mixed, the hydro-thermal reaction of 10-24h is carried out at 200 DEG C;After reaction, solution is dried to get to gold
The nano material of nano particle and molybdenum sulfide nucleocapsid;A concentration of 1%-3% of the polyglycol solution.
3. a kind of testing the high efficiency photocatalysis nano material system based on molybdenum sulfide obtained using preparation method described in claim 2
The method of standby hydrogen, it is characterised in that:The high efficiency photocatalysis nano material based on molybdenum sulfide of 0.1g, be dispersed in 100ml go from
In sub- water;The test that photocatalysis prepares hydrogen is carried out using photocatalysis equipment;The test condition that photocatalysis prepares hydrogen is:Light source
For xenon lamp, with current control xenon source intensity, electric current 15A.
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CN107598182B (en) * | 2017-07-24 | 2019-05-10 | 西北工业大学 | Gold nano grain-molybdenum disulfide-gold hypersensitive SERS base material and preparation method |
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Citations (4)
Publication number | Priority date | Publication date | Assignee | Title |
---|---|---|---|---|
US8597397B2 (en) * | 2005-01-14 | 2013-12-03 | Cabot Corporation | Production of metal nanoparticles |
CN104681815A (en) * | 2015-02-11 | 2015-06-03 | 深圳新宙邦科技股份有限公司 | Spherical molybdenum disulfide composite material and preparation method and application thereof |
CN104722316A (en) * | 2015-03-26 | 2015-06-24 | 电子科技大学 | Molybdenum disulfide composite nano-gold photocatalyst and preparation method thereof |
CN105366726A (en) * | 2015-12-16 | 2016-03-02 | 中国科学院理化技术研究所 | Preparation method of hollow spherical molybdenum disulfide of laminated shell layer structure |
-
2016
- 2016-08-10 CN CN201610653761.6A patent/CN106362775B/en active Active
Patent Citations (4)
Publication number | Priority date | Publication date | Assignee | Title |
---|---|---|---|---|
US8597397B2 (en) * | 2005-01-14 | 2013-12-03 | Cabot Corporation | Production of metal nanoparticles |
CN104681815A (en) * | 2015-02-11 | 2015-06-03 | 深圳新宙邦科技股份有限公司 | Spherical molybdenum disulfide composite material and preparation method and application thereof |
CN104722316A (en) * | 2015-03-26 | 2015-06-24 | 电子科技大学 | Molybdenum disulfide composite nano-gold photocatalyst and preparation method thereof |
CN105366726A (en) * | 2015-12-16 | 2016-03-02 | 中国科学院理化技术研究所 | Preparation method of hollow spherical molybdenum disulfide of laminated shell layer structure |
Non-Patent Citations (3)
Title |
---|
Au Nanoparticle-Modifi ed MoS 2 Nanosheet-Based Photoelectrochemical Cells for Water Splitting;Zongyou Yin et al.;《small》;20140307;第10卷(第17期);3537-3543 * |
Identification of Active Edge Sites for Electrochemical H2 Evolution from MoS2 Nanocatalysts;Thomas F. Jaramillo et al.;《SCIENCE》;20070706;第317卷;100-102 * |
Synthesis of Au-MoS2 Nanocomposites: Thermal and Friction-Induced Changes to the Structure;Thomas W Scharf et al.;《ACS Appl. Mater. Interfaces》;20131105;第5卷(第22期);11762–11767 * |
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