CN112044451A - Pt3Co alloy modified atomic layer SnS2Preparation method and application of composite photocatalyst - Google Patents
Pt3Co alloy modified atomic layer SnS2Preparation method and application of composite photocatalyst Download PDFInfo
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- 239000002131 composite material Substances 0.000 title claims abstract description 33
- 238000000034 method Methods 0.000 title claims abstract description 11
- 229910045601 alloy Inorganic materials 0.000 title description 6
- 239000000956 alloy Substances 0.000 title description 6
- 239000000243 solution Substances 0.000 claims abstract description 43
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- 229910021641 deionized water Inorganic materials 0.000 claims abstract description 27
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Chemical compound O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims abstract description 27
- LYCAIKOWRPUZTN-UHFFFAOYSA-N Ethylene glycol Chemical compound OCCO LYCAIKOWRPUZTN-UHFFFAOYSA-N 0.000 claims abstract description 24
- XUJNEKJLAYXESH-REOHCLBHSA-N L-Cysteine Chemical compound SC[C@H](N)C(O)=O XUJNEKJLAYXESH-REOHCLBHSA-N 0.000 claims abstract description 18
- 238000002360 preparation method Methods 0.000 claims abstract description 16
- 239000011259 mixed solution Substances 0.000 claims abstract description 13
- 229910021627 Tin(IV) chloride Inorganic materials 0.000 claims abstract description 12
- HPGGPRDJHPYFRM-UHFFFAOYSA-J tin(iv) chloride Chemical compound Cl[Sn](Cl)(Cl)Cl HPGGPRDJHPYFRM-UHFFFAOYSA-J 0.000 claims abstract description 12
- 238000006243 chemical reaction Methods 0.000 claims abstract description 11
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- 239000004201 L-cysteine Substances 0.000 claims abstract description 9
- GVGUFUZHNYFZLC-UHFFFAOYSA-N dodecyl benzenesulfonate;sodium Chemical compound [Na].CCCCCCCCCCCCOS(=O)(=O)C1=CC=CC=C1 GVGUFUZHNYFZLC-UHFFFAOYSA-N 0.000 claims abstract description 9
- 229940080264 sodium dodecylbenzenesulfonate Drugs 0.000 claims abstract description 9
- 238000001035 drying Methods 0.000 claims abstract description 8
- 229910000531 Co alloy Inorganic materials 0.000 claims abstract description 7
- ALRFTTOJSPMYSY-UHFFFAOYSA-N tin disulfide Chemical compound S=[Sn]=S ALRFTTOJSPMYSY-UHFFFAOYSA-N 0.000 claims abstract description 7
- 238000001027 hydrothermal synthesis Methods 0.000 claims abstract description 5
- BASFCYQUMIYNBI-UHFFFAOYSA-N platinum Substances [Pt] BASFCYQUMIYNBI-UHFFFAOYSA-N 0.000 claims description 69
- 239000002243 precursor Substances 0.000 claims description 16
- 238000003756 stirring Methods 0.000 claims description 16
- CURLTUGMZLYLDI-UHFFFAOYSA-N Carbon dioxide Chemical compound O=C=O CURLTUGMZLYLDI-UHFFFAOYSA-N 0.000 claims description 14
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 claims description 12
- 238000005406 washing Methods 0.000 claims description 12
- 229910002092 carbon dioxide Inorganic materials 0.000 claims description 9
- GVPFVAHMJGGAJG-UHFFFAOYSA-L cobalt dichloride Chemical compound [Cl-].[Cl-].[Co+2] GVPFVAHMJGGAJG-UHFFFAOYSA-L 0.000 claims description 8
- CLSUSRZJUQMOHH-UHFFFAOYSA-L platinum dichloride Chemical compound Cl[Pt]Cl CLSUSRZJUQMOHH-UHFFFAOYSA-L 0.000 claims description 8
- 239000001569 carbon dioxide Substances 0.000 claims description 6
- 239000012279 sodium borohydride Substances 0.000 claims description 6
- 229910000033 sodium borohydride Inorganic materials 0.000 claims description 6
- 230000009467 reduction Effects 0.000 claims description 5
- 238000010335 hydrothermal treatment Methods 0.000 claims description 4
- 239000000203 mixture Substances 0.000 claims description 4
- WGCNASOHLSPBMP-UHFFFAOYSA-N hydroxyacetaldehyde Natural products OCC=O WGCNASOHLSPBMP-UHFFFAOYSA-N 0.000 claims description 3
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- 238000007865 diluting Methods 0.000 claims description 2
- 229910018979 CoPt Inorganic materials 0.000 claims 1
- KHMOASUYFVRATF-UHFFFAOYSA-J tin(4+);tetrachloride;pentahydrate Chemical compound O.O.O.O.O.Cl[Sn](Cl)(Cl)Cl KHMOASUYFVRATF-UHFFFAOYSA-J 0.000 claims 1
- 239000000463 material Substances 0.000 abstract description 6
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- 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
- B01J27/043—Sulfides with iron group metals or platinum group metals
- B01J27/045—Platinum group metals
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- B01J35/00—Catalysts, in general, characterised by their form or physical properties
- B01J35/30—Catalysts, in general, characterised by their form or physical properties characterised by their physical properties
- B01J35/39—Photocatalytic properties
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Abstract
The invention belongs to the technical field of energy materials, and provides Pt3Co alloy modified atomic layer SnS2A composite photocatalyst and a preparation method and application thereof. The invention comprises the following steps: (1) pt3Preparation of Co (2) SnS2/Pt3Preparing a Co composite photocatalyst: taking a mixed solution of deionized water and ethylene glycol as a solvent, taking stannic chloride pentahydrate, L-cysteine and sodium dodecyl benzene sulfonate as raw materials, and adding a certain amount of Pt into the synthesized tin disulfide3Co gel solution is stirred, then poured into a vacuum reaction kettle for hydrothermal reaction, washed and put into a drying oven for drying after being naturally cooled to obtain SnS2/Pt3A Co composite photocatalyst; the method has the advantages of low cost, simple preparation, no resource waste and no secondary pollution, is a green, stable and efficient photoreduction technology, and aims to be used for photoreduction of CO2The problems of energy crisis and environment at present are solved.
Description
Technical Field
The invention relates to a Pt3Co alloy modified atomic layer SnS2A preparation method of a composite photocatalyst and application research thereof belong to the technical field of energy material preparation.
Background
With the rapid development of society, a great deal of fossil energy is consumed and simultaneously a great deal of greenhouse gas (the main product is CO)2And CH4Etc.), which raises a current set of energy crisis and environmental issues (e.g.: energy sources such as coal, petroleum and natural gas are gradually exhausted; sea level rise, glaciers melting, and global warming). How to solve the energy crisis and environmental problems is a major challenge facing the twenty-first century. Most researchers are motivated by photosynthesis to concentrate on studying how to treat CO2The conversion into carbon-containing value-added fuel, therefore, the photocatalytic reduction technology is currently considered to be an ideal method for realizing carbon cycle, and the development of a novel green, efficient and stable photocatalyst is urgently needed.
In recent years, researchers have achieved a series of results in the continuous search for emerging high-efficiency semiconductors. Such as TiO2、ZnO、g-C3N4、SnS2、CdS、CeVO4And BixOyClzAnd the like are widely applied to the fields of electric catalysis, lithium batteries, photocatalysis and the like.
Wherein, SnS2The crystal structure is layered, and the layered structure is composed of three closely connectedThe sandwich structure is characterized in that the upper layer and the lower layer are both sulfur atoms, and the middle sandwich layer is a tin atom. It is important to note here that in this layered crystal structure, the interaction between S and Sn within the S-Sn-S layer is due to covalent bonds, while the adjacent S-Sn-S layers are due to weak van der Waals forces. SnS2Unique crystal structure determining SnS2Has good performance in optics, electricity and gas sensitivity. In addition, SnS2The absorption wavelength threshold value is in a visible light range, and not only has good oxidation resistance and thermal stability, but also has good stability in an acidic solution and a neutral solution. Therefore, it is gradually considered as a potential photocatalyst with high quantum efficiency and is a hot point of research.
At present, a two-dimensional/two-dimensional Z-shaped heterojunction is prepared by adopting a solvothermal method, and the two-dimensional/two-dimensional Z-shaped heterojunction shows good catalyst activity when used in an environment repairing process; in addition, the hydrothermal method is adopted to successfully prepare the alloy modified semiconductor composite material, and the alloy modified semiconductor composite material shows excellent energy storage performance in a super capacitor; however, the above composite materials also have problems such as a high recombination rate of photogenerated carriers and a low electron transport rate.
Thus, the present invention is directed to the construction of SnS2/Pt3The Co heterojunction realizes good photocatalytic reduction activity, the alloy modified semiconductor effectively promotes the separation of photo-generated electron hole pairs in the composite catalyst, expands the light absorption range of the material, enhances the photocatalytic activity of the material, and is applied to photocatalytic reduction of CO2Research in the field.
Disclosure of Invention
The invention adopts the technical means of solvothermal to successfully prepare SnS2/Pt3A Co composite photocatalyst; aims to solve the problems of high recombination rate of photon-generated carriers, narrow photoresponse range and the like.
The present invention achieves the above-described object by the following technical means.
SnS2/Pt3The preparation method of the Co composite photocatalyst comprises the following steps:
(1) preparation of Pt3Co precursor:
adding the platinum chloride solution and the cobalt chloride solution into a beaker in sequence, stirring, and then adding NaBH4Adding into the above mixed solution until the color of the solution changes from light yellow to black, standing the obtained solution at room temperature, washing with deionized water and ethanol for multiple times after standing to obtain Pt3A Co gel precursor; then diluting with deionized water to obtain Pt3The Co gel solution is reserved;
(2)SnS2/Pt3preparing a Co composite photocatalyst:
adding stannic chloride pentahydrate (SnCl)4·5H2O) is dissolved in the mixed solution of glycol and deionized water, then L-cysteine and sodium dodecyl benzene sulfonate are added, and the mixture is stirred uniformly to prepare tin disulfide; adding a certain amount of Pt3Co gel solution to form mixed solution, adding the mixed solution into a reaction kettle for hydrothermal reaction, naturally cooling to room temperature, washing, centrifuging and drying a product after the reaction to obtain SnS2/Pt3A Co composite photocatalyst.
In the step (1), the concentration of the platinum chloride solution is 1g/L, the concentration of the cobalt chloride solution is 1g/L, and NaBH is added4The concentration of the solution is 0.1M, the stirring time is 1h, the standing time is 3h, and Pt3The concentration of the Co gel solution was 2 mM.
In the step (2), the dosage ratio of the stannic chloride pentahydrate, the glycol, the deionized water, the L-cysteine and the sodium dodecyl benzene sulfonate is 0.0877 g: 15mL:15mL:0.2423 g: 0.5645 g.
In the step (2), the tin disulfide and Pt3Pt in Co gel solution3The mass ratio of Co is 1: (0.5 to 4).
In the step (2), the tin disulfide and Pt3Pt in Co gel solution3The mass ratio of Co is 1: 3.2.
in the step (2), the temperature of the hydrothermal treatment is 150-180 ℃; the hydrothermal treatment time was 10 h.
The SnS of the invention2/Pt3The Co is in the shape of a flake-particle structure and in the size of 2 to3nm。
Pt prepared by the invention3The application of the Co composite photocatalyst in reducing carbon dioxide.
In the technical scheme, the dosage of the deionized water can completely dissolve the soluble solid.
The invention has the beneficial effects that:
(1) the invention uses SnS2/Pt3The Co composite material has higher visible light response capability, and passes through Pt3Co is an electric conductor, the electron transmission is accelerated, the plasma resonance effect enables the SnS to have more hot electrons, and the SnS is improved to a greater extent2/Pt3Efficiency of Co photocatalytic reduction of carbon dioxide.
(2) Prepared SnS2Ultra-thin two-dimensional structure, Pt3Co is uniformly dispersed in SnS2In addition, more reaction sites are provided, so that more available electrons can participate in the photoreduction of carbon dioxide.
(3) The invention can prepare SnS through convenient hydrothermal method2/Pt3The Co composite photocatalyst takes the alloy as a bridge, so that the transmission of photon-generated carriers is accelerated, and the composite material is a high-efficiency and stable photocatalyst.
(4) The invention realizes the purpose of using SnS2/Pt3The Co nano composite material is used as a photocatalyst, under the excitation condition of visible light, the photo-generated electrons realize a special catalysis or conversion process through the interface interaction effect with carbon dioxide gas molecules, so that the purpose of converting the carbon dioxide gas into the organic fuel is realized, the method does not cause resource waste and secondary pollution, is simple and convenient to operate, and is a green, environment-friendly and efficient pollution treatment technology.
Drawings
In FIG. 1, a is SnS prepared in example 12B is the SnS prepared in example 12/Pt3XRD pattern of Co, c is SnS prepared in example 22/Pt3XRD pattern of Co, d is SnS prepared in example 32/Pt3XRD pattern of Co, e is SnS prepared in example 42/Pt3XRD pattern of Co.
In FIG. 2, a is SnS prepared in example 12B is the SnS prepared in example 12/Pt3DRS map of Co, c is SnS prepared in example 22/Pt3DRS map of Co, d is SnS prepared in example 32/Pt3DRS map of Co, e is SnS prepared in example 42/Pt3DRS map of Co.
FIG. 3 shows SnS prepared in example 32/Pt3TEM image of Co composite photocatalyst.
Detailed Description
The invention is further described with reference to the drawings and the detailed description.
Photocatalytic activity evaluation of the photocatalyst prepared in the present invention: under visible light conditions, 0.02g of catalyst and 100ml of deionized water solution were added to the photoreactor, and CO was introduced at a large flow rate2Injecting CO at a certain pressure after the gas in the kettle is exhausted2A gas. The custom xenon lamp was turned on under magnetic stirring and samples were analyzed at 1h intervals. Finally, CO is obtained through calculation2Gas reduction CO yield.
Example 1:
(1)Pt3preparation of Co gel precursor:
adding 1g/L platinum chloride solution and 1g/L cobalt chloride solution into a beaker in sequence, stirring for 1h, and then adding NaBH4(0.1M) adding into the above mixed solution until the color of the solution changes from light yellow to black, standing the obtained solution at room temperature (3h), washing with deionized water and ethanol for multiple times to obtain Pt3A Co gel precursor;
(2)SnS2/Pt3preparing a Co composite photocatalyst:
0.0877g SnCl was weighed out4·5H2Placing O (stannic chloride pentahydrate) into a glass beaker, adding 10mL of deionized water and 20mL of ethylene glycol to completely dissolve the O (stannic chloride pentahydrate), magnetically stirring, adding 0.2423g of L-cysteine and 0.5645g of sodium dodecyl benzene sulfonate to generate white precipitate, and continuously stirring for 0.5 h; 1ml of Pt3Adding Co (2mM) precursor into the mixture, mixing the mixture uniformly, and then adding the mixtureThe resulting suspension was poured into a 50ml reactor and heated at 160 ℃ for 10 hours. Washing, centrifuging and drying to obtain SnS2/Pt3A Co composite photocatalyst;
(3) taking 0.02g of catalyst and 100ml of deionized water from the sample in the step (2), adding the catalyst and the deionized water into a photoreactor, and introducing CO at a large flow rate2Injecting CO at a certain pressure after the gas in the kettle is exhausted2A gas. The custom xenon lamp was turned on under magnetic stirring and samples were analyzed at 1h intervals. After 5h of irradiation, CO was calculated2The gas reduced CO yield was 24.5. mu. mol/g.
Example 2:
(1)Pt3preparation of Co gel precursor:
adding 1g/L platinum chloride solution and 1g/L cobalt chloride solution into a beaker in sequence, stirring for 1h, and then adding NaBH4(0.1M) adding into the above mixed solution until the color of the solution changes from light yellow to black, standing the obtained solution at room temperature (3h), washing with deionized water and ethanol for multiple times to obtain Pt3A Co gel precursor;
(2)SnS2/Pt3preparing a Co composite photocatalyst:
0.0877g SnCl was weighed out4·5H2Placing O (stannic chloride pentahydrate) into a glass beaker, adding 10mL of deionized water and 20mL of ethylene glycol to completely dissolve the O (stannic chloride pentahydrate), magnetically stirring, adding 0.2423g of L-cysteine and 0.5645g of sodium dodecyl benzene sulfonate to generate white precipitate, and continuously stirring for 0.5 h; 3ml of Pt3Co (2mM) precursor was added thereto and mixed well, and the resulting suspension was poured into a 50ml reaction vessel and heated at 160 ℃ for 10 hours. Washing, centrifuging and drying to obtain SnS2/Pt3A Co composite photocatalyst;
(3) taking 0.02g of catalyst and 100ml of deionized water from the sample in the step (2), adding the catalyst and the deionized water into a photoreactor, and introducing CO at a large flow rate2Injecting CO at a certain pressure after the gas in the kettle is exhausted2A gas. The custom xenon lamp was turned on under magnetic stirring and samples were analyzed at 1h intervals. After 5h of irradiation, the CO2 gas reduced CO to 40.4. mu. mol/g was calculated.
Example 3:
(1)Pt3preparation of Co gel precursor:
adding 1g/L platinum chloride solution and 1g/L cobalt chloride solution into a beaker in sequence, stirring for 1h, and then adding NaBH4(0.1M) adding into the above mixed solution until the color of the solution changes from light yellow to black, standing the obtained solution at room temperature (3h), washing with deionized water and ethanol for multiple times to obtain Pt3A Co gel precursor;
(2)SnS2/Pt3preparing a Co composite photocatalyst:
0.0877g SnCl was weighed out4·5H2Placing O (stannic chloride pentahydrate) into a glass beaker, adding 10mL of deionized water and 20mL of ethylene glycol to completely dissolve the O (stannic chloride pentahydrate), magnetically stirring, adding 0.2423g of L-cysteine and 0.5645g of sodium dodecyl benzene sulfonate to generate white precipitate, and continuously stirring for 0.5 h; mixing 5ml of Pt3Co (2mM) precursor was added thereto and mixed well, and the resulting suspension was poured into a 50ml reaction vessel and heated at 160 ℃ for 10 hours. Washing, centrifuging and drying to obtain SnS2/Pt3A Co composite photocatalyst;
(3) taking 0.02g of catalyst and 100ml of deionized water from the sample in the step (2), adding the catalyst and the deionized water into a photoreactor, and introducing CO at a large flow rate2Injecting CO at a certain pressure after the gas in the kettle is exhausted2A gas. The custom xenon lamp was turned on under magnetic stirring and samples were analyzed at 1h intervals. After 5h of irradiation, CO was calculated2The gas reduced CO was 92.3. mu. mol/g.
Example 4:
(1)Pt3preparation of Co gel precursor:
adding 1g/L platinum chloride solution and 1g/L cobalt chloride solution into a beaker in sequence, stirring for 1h, and then adding NaBH4(0.1M) adding into the above mixed solution until the color of the solution changes from light yellow to black, standing the obtained solution at room temperature (3h), washing with deionized water and ethanol for multiple times to obtain Pt3A Co gel precursor;
(2)SnS2/Pt3preparing a Co composite photocatalyst:
0.0877g SnCl was weighed out4·5H2Placing O (stannic chloride pentahydrate) into a glass beaker, adding 10mL of deionized water and 20mL of ethylene glycol to completely dissolve the O (stannic chloride pentahydrate), magnetically stirring, adding 0.2423g of L-cysteine and 0.5645g of sodium dodecyl benzene sulfonate to generate white precipitate, and continuously stirring for 0.5 h; mixing 7ml of Pt3Co (2mM) precursor was added thereto and mixed well, and the resulting suspension was poured into a 50ml reaction vessel and heated at 160 ℃ for 10 hours. Washing, centrifuging and drying to obtain SnS2/Pt3A Co composite photocatalyst;
(3) taking 0.02g of catalyst and 100ml of deionized water from the sample in the step (2), adding the catalyst and the deionized water into a photoreactor, and introducing CO at a large flow rate2Injecting CO at a certain pressure after the gas in the kettle is exhausted2A gas. The custom xenon lamp was turned on under magnetic stirring and samples were analyzed at 1h intervals. After 5h of irradiation, CO was calculated2The gas reduced CO was 52.6. mu. mol/g.
FIG. 1 is an XRD pattern of the photocatalyst showing clearly SnS2All diffraction peaks matched well with the standard card, indicating successful preparation of the desired material.
FIG. 2 is a DRS plot of a photocatalyst showing, with clarity, alloy-modified SnS2The photocatalyst widens the light absorption range. SnS2At Pt3The absorption range of light under the modification effect of the Co alloy is 385-720 nm, which shows that Pt3The Co alloy can broaden the light absorption range of the semiconductor.
FIG. 3 shows SnS2/Pt3TEM image of Co composite photocatalyst, from which SnS can be seen2/Pt3The morphology of Co is a sheet-particle structure, and the size of Co is 2-3 nm.
The present invention is not limited to the above-described embodiments, and any obvious improvements, substitutions or modifications can be made by those skilled in the art without departing from the spirit of the present invention.
Claims (8)
1.Pt3Co alloy modified atomic layer SnS2The preparation method of the composite photocatalyst is characterized in that,
(1) preparation of Pt3Co precursor:
adding the platinum chloride solution and the cobalt chloride solution into a beaker in sequence, stirring, and then adding NaBH4Adding into the above mixed solution until the color of the solution changes from light yellow to black, standing the obtained solution at room temperature, washing with deionized water and ethanol for multiple times after standing to obtain Pt3A Co gel precursor; then diluting with deionized water to obtain Pt3The Co gel solution is reserved;
(2)SnS2/Pt3preparing a Co composite photocatalyst:
adding stannic chloride pentahydrate (SnCl)4·5H2O) is dissolved in the mixed solution of glycol and deionized water, then L-cysteine and sodium dodecyl benzene sulfonate are added, and the mixture is stirred uniformly to prepare tin disulfide; adding a certain amount of Pt3Co gel solution to form mixed solution, adding the mixed solution into a reaction kettle for hydrothermal reaction, naturally cooling to room temperature, washing, centrifuging and drying a product after the reaction to obtain SnS2/Pt3A Co composite photocatalyst.
2. The method according to claim 1, wherein in the step (1), the concentration of the platinum chloride solution is 1g/L, the concentration of the cobalt chloride solution is 1g/L, and NaBH is added4The concentration of the solution is 0.1M, the stirring time is 1h, the standing time is 3h, and Pt3The concentration of the Co gel solution was 2 mM.
3. The method according to claim 1, wherein in the step (2), the tin chloride pentahydrate, the ethylene glycol, the deionized water, the L-cysteine and the sodium dodecylbenzenesulfonate are used in a ratio of 0.0877 g: 15mL:15mL:0.2423 g: 0.5645 g.
4. The method of claim 1, wherein in step (2), the tin disulfide is reacted with Pt3CoPt in gel solution3The mass ratio of Co is 1: (0.5 to 4).
5. The method according to claim 4, wherein in the step (2), the tin disulfide is reacted with Pt3Pt in Co gel solution3The mass ratio of Co is 1: 3.2.
6. the preparation method as claimed in claim 1, wherein the temperature of the hydrothermal treatment in step (2) is 150-180 ℃; the hydrothermal treatment time was 10 h.
7. Pt3Co alloy modified atomic layer SnS2The composite photocatalyst is characterized by being prepared by the preparation method of any one of claims 1 to 6, having a sheet-added particle structure and a size of 2 to 3 nm.
8. Subjecting the Pt of claim 7 to3Co alloy modified atomic layer SnS2Use of a composite photocatalyst for the reduction of carbon dioxide.
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| CN104923263A (en) * | 2015-05-20 | 2015-09-23 | 湖北大学 | Composite photocatalytic water splitting catalyst and preparation method thereof |
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| CN104923263A (en) * | 2015-05-20 | 2015-09-23 | 湖北大学 | Composite photocatalytic water splitting catalyst and preparation method thereof |
| CN110252346A (en) * | 2019-05-29 | 2019-09-20 | 江苏大学 | A kind of MoS2/SnS2The preparation method and purposes of/r-GO composite photo-catalyst |
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