CN115041198A - MoS 2 Preparation method and application of/CdS photocatalytic composite material - Google Patents
MoS 2 Preparation method and application of/CdS photocatalytic composite material Download PDFInfo
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- 238000004519 manufacturing process Methods 0.000 claims abstract description 24
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- TVXXNOYZHKPKGW-UHFFFAOYSA-N sodium molybdate (anhydrous) Chemical compound [Na+].[Na+].[O-][Mo]([O-])(=O)=O TVXXNOYZHKPKGW-UHFFFAOYSA-N 0.000 claims abstract description 6
- YUKQRDCYNOVPGJ-UHFFFAOYSA-N thioacetamide Chemical compound CC(N)=S YUKQRDCYNOVPGJ-UHFFFAOYSA-N 0.000 claims abstract description 6
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- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 claims description 12
- 238000005406 washing Methods 0.000 claims description 11
- QAOWNCQODCNURD-UHFFFAOYSA-N Sulfuric acid Chemical compound OS(O)(=O)=O QAOWNCQODCNURD-UHFFFAOYSA-N 0.000 claims description 10
- UMGDCJDMYOKAJW-UHFFFAOYSA-N thiourea Chemical compound NC(N)=S UMGDCJDMYOKAJW-UHFFFAOYSA-N 0.000 claims description 10
- 238000001035 drying Methods 0.000 claims description 8
- 238000003756 stirring Methods 0.000 claims description 8
- 239000008367 deionised water Substances 0.000 claims description 7
- 229910021641 deionized water Inorganic materials 0.000 claims description 7
- 238000006243 chemical reaction Methods 0.000 claims description 6
- XSQUKJJJFZCRTK-UHFFFAOYSA-N Urea Natural products NC(N)=O XSQUKJJJFZCRTK-UHFFFAOYSA-N 0.000 claims description 5
- XIEPJMXMMWZAAV-UHFFFAOYSA-N cadmium nitrate Inorganic materials [Cd+2].[O-][N+]([O-])=O.[O-][N+]([O-])=O XIEPJMXMMWZAAV-UHFFFAOYSA-N 0.000 claims description 5
- 239000011259 mixed solution Substances 0.000 claims description 5
- NMHMNPHRMNGLLB-UHFFFAOYSA-N phloretic acid Chemical compound OC(=O)CCC1=CC=C(O)C=C1 NMHMNPHRMNGLLB-UHFFFAOYSA-N 0.000 claims description 5
- 239000002244 precipitate Substances 0.000 claims description 5
- 239000013049 sediment Substances 0.000 claims description 4
- PIICEJLVQHRZGT-UHFFFAOYSA-N Ethylenediamine Chemical compound NCCN PIICEJLVQHRZGT-UHFFFAOYSA-N 0.000 claims description 3
- 238000000354 decomposition reaction Methods 0.000 claims description 3
- 238000002156 mixing Methods 0.000 claims description 3
- 239000000203 mixture Substances 0.000 claims description 3
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- 230000000694 effects Effects 0.000 abstract description 7
- 239000004065 semiconductor Substances 0.000 abstract description 6
- 238000007146 photocatalysis Methods 0.000 abstract description 5
- 239000011941 photocatalyst Substances 0.000 abstract description 3
- 238000001027 hydrothermal synthesis Methods 0.000 abstract description 2
- WUPHOULIZUERAE-UHFFFAOYSA-N 3-(oxolan-2-yl)propanoic acid Chemical compound OC(=O)CCC1CCCO1 WUPHOULIZUERAE-UHFFFAOYSA-N 0.000 description 47
- 229910052980 cadmium sulfide Inorganic materials 0.000 description 46
- 239000003054 catalyst Substances 0.000 description 4
- AFCARXCZXQIEQB-UHFFFAOYSA-N N-[3-oxo-3-(2,4,6,7-tetrahydrotriazolo[4,5-c]pyridin-5-yl)propyl]-2-[[3-(trifluoromethoxy)phenyl]methylamino]pyrimidine-5-carboxamide Chemical compound O=C(CCNC(=O)C=1C=NC(=NC=1)NCC1=CC(=CC=C1)OC(F)(F)F)N1CC2=C(CC1)NN=N2 AFCARXCZXQIEQB-UHFFFAOYSA-N 0.000 description 3
- 238000002441 X-ray diffraction Methods 0.000 description 3
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- 238000005119 centrifugation Methods 0.000 description 2
- 238000011161 development Methods 0.000 description 2
- 238000005516 engineering process Methods 0.000 description 2
- 239000007789 gas Substances 0.000 description 2
- JVTAAEKCZFNVCJ-UHFFFAOYSA-N lactic acid Chemical compound CC(O)C(O)=O JVTAAEKCZFNVCJ-UHFFFAOYSA-N 0.000 description 2
- 230000008569 process Effects 0.000 description 2
- 238000001878 scanning electron micrograph Methods 0.000 description 2
- 238000004626 scanning electron microscopy Methods 0.000 description 2
- 239000000243 solution Substances 0.000 description 2
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- RZVAJINKPMORJF-UHFFFAOYSA-N Acetaminophen Chemical compound CC(=O)NC1=CC=C(O)C=C1 RZVAJINKPMORJF-UHFFFAOYSA-N 0.000 description 1
- 241000282414 Homo sapiens Species 0.000 description 1
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- 229920006362 Teflon® Polymers 0.000 description 1
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- 239000007864 aqueous solution Substances 0.000 description 1
- QVGXLLKOCUKJST-UHFFFAOYSA-N atomic oxygen Chemical compound [O] QVGXLLKOCUKJST-UHFFFAOYSA-N 0.000 description 1
- 230000005587 bubbling Effects 0.000 description 1
- 239000000969 carrier Substances 0.000 description 1
- 239000012159 carrier gas Substances 0.000 description 1
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- 238000004817 gas chromatography Methods 0.000 description 1
- 125000004435 hydrogen atom Chemical group [H]* 0.000 description 1
- 238000005286 illumination Methods 0.000 description 1
- 235000014655 lactic acid Nutrition 0.000 description 1
- 239000004310 lactic acid Substances 0.000 description 1
- 230000004298 light response Effects 0.000 description 1
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- 238000012986 modification Methods 0.000 description 1
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- 229910052757 nitrogen Inorganic materials 0.000 description 1
- 239000001301 oxygen Substances 0.000 description 1
- 229910052760 oxygen Inorganic materials 0.000 description 1
- 239000002245 particle Substances 0.000 description 1
- 238000013033 photocatalytic degradation reaction Methods 0.000 description 1
- 229910052697 platinum Inorganic materials 0.000 description 1
- 231100000719 pollutant Toxicity 0.000 description 1
- -1 polytetrafluoroethylene Polymers 0.000 description 1
- 229920001343 polytetrafluoroethylene Polymers 0.000 description 1
- 239000004810 polytetrafluoroethylene Substances 0.000 description 1
- 239000005297 pyrex Substances 0.000 description 1
- 239000002994 raw material Substances 0.000 description 1
- URGAHOPLAPQHLN-UHFFFAOYSA-N sodium aluminosilicate Chemical compound [Na+].[Al+3].[O-][Si]([O-])=O.[O-][Si]([O-])=O URGAHOPLAPQHLN-UHFFFAOYSA-N 0.000 description 1
- 238000006467 substitution reaction Methods 0.000 description 1
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- 229910052724 xenon Inorganic materials 0.000 description 1
- FHNFHKCVQCLJFQ-UHFFFAOYSA-N xenon atom Chemical compound [Xe] FHNFHKCVQCLJFQ-UHFFFAOYSA-N 0.000 description 1
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- 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
- 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
-
- 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
-
- 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
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- Chemical & Material Sciences (AREA)
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- Engineering & Computer Science (AREA)
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- Chemical Kinetics & Catalysis (AREA)
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Abstract
The invention discloses a MoS 2 A preparation method and application of a/CdS photocatalytic composite material belong to the field of photocatalysis. The preparation method of the composite material comprises the following steps: sodium molybdate, thioacetamide and CdS powder are fully mixed in water for hydrothermal reaction to obtain MoS 2 The CdS photocatalytic composite material. The mol ratio of Mo to Cd in the composite material is preferably 5-20%, and when the mol ratio of Mo to Cd is 10%, the photocatalytic hydrogen production activity is optimal, and the hydrogen production rate is 621.3 mu mol/h. The MoS provided by the invention 2 the/CdS photocatalytic composite material has excellent visible light photocatalytic hydrogen production performance, which proves that the two-dimensional layered material MoS 2 Can be used as a cocatalyst to obviously improve the photocatalytic hydrogen production activity of CdS, and provides a method and an idea for developing high-activity semiconductor composite photocatalysts in the future.
Description
Technical Field
The invention relates to the field of photocatalysis, in particular to MoS 2 Preparation method and application of/CdS photocatalytic composite material.
Background
With the rapid development of industry and the massive combustion of fossil fuels, the problems of environmental pollution and energy shortage faced by human beings are increasingly highlighted. In recent years, photocatalytic technology is considered as one of effective approaches to solve environmental and energy problems. In order to realize the practical application of the technology, how to improve the light energy utilization rate, the catalytic activity and the stability of the photocatalyst is a key and difficult point of research. Therefore, there is an urgent need for the research of novel photocatalytic materials having development potential.
Cadmium sulfide (CdS) is a semiconductor photocatalytic material which is of great interest, and can be used for photocatalytic degradation of pollutants and decomposition of hydrogen in water due to good visible light response capability and proper energy band position. However, since the photogenerated carriers of CdS are easily recombined, the hydrogen production cannot be achieved by using CdS alone. The introduction of noble metals, such as Pt, as promoters in semiconductors is an effective way to improve the photocatalytic hydrogen production efficiency. However, the high cost and rarity of noble metals limit their practical application. In recent years, the two-dimensional layered material has remarkable advantages in the field of photocatalysis, and the layered material modified on the semiconductor photocatalysis material has the functions of fast transferring and separating photogenerated electrons and holes, which is beneficial to improving the photocatalysis hydrogen production effect of the material. MoS 2 As a typical two-dimensional layered material, the material has a special layered structure and semiconductor properties, and is simple in preparation method and wide in raw material source. Thus, the invention is based on CdS and uses MoS 2 The catalyst is used as a catalyst promoter to improve the photocatalytic hydrogen production performance of CdS.
Disclosure of Invention
The invention aims to provide a MoS 2 A preparation method and application of a CdS photocatalytic composite material. The MoS 2 The CdS photocatalytic composite material is synthesized by a secondary hydrothermal method, has the characteristics of simple preparation method, low cost, short preparation time and high operability, and has higher photocatalytic hydrogen production performance.
The purpose of the invention is realized by the following technical scheme:
MoS 2 The preparation method of the/CdS photocatalytic composite material comprises the following steps: sodium molybdate, thioacetamide and CdS powder were added to water and stirred well. The mixed solution reacts for 20 to 24 hours at the temperature of between 160 and 200 ℃, the mixed solution is cooled and then centrifuged to obtain sediment, and the sediment is washed and dried to obtain MoS 2 The CdS photocatalytic composite material.
The CdS is preferably prepared by a process comprising the steps of:
(1) cadmium nitrate and thiourea were dissolved in ethylenediamine. In this step, the molar ratio of cadmium nitrate to thiourea is preferably 8.5-11: 28-32.
(2) Reacting the mixture obtained in the step (1) at the temperature of 150 ℃ and 180 ℃ for 40-50h, centrifuging and collecting precipitates after the reaction, and washing for several times. In the step, the washing is preferably performed by alternately washing with ethanol and deionized water for 5-7 times.
(3) And (3) mixing and stirring the product obtained in the step (2) with sulfuric acid, and then centrifugally drying to obtain CdS powder. In the step, the concentration of the sulfuric acid is preferably 0.01-0.02mol/L, the stirring time is preferably 2-3h, and the drying condition is preferably kept at 50-70 ℃ for 10-14 h.
The molar ratio of sodium molybdate to thioacetamide is preferably 1-3: 4-6. The washing is preferably performed 2-3 times by alternately washing with ethanol and deionized water. The drying condition is preferably kept at 50-70 ℃ for 10-14 h.
The MoS 2 The mol percentage of Mo and Cd in the/CdS photocatalytic composite material is preferably 5-20%; more preferably, MoS 2 The mol percentage of Mo and Cd in the/CdS photocatalytic composite material is 10%.
MoS 2 the/CdS photocatalytic composite material is obtained by the preparation method.
The above MoS 2 Application of the CdS photocatalytic composite material in photocatalytic water decomposition hydrogen production.
Compared with the prior art, the invention has the following advantages and beneficial effects:
(1) the invention selects the MoS with the two-dimensional layered structure 2 The catalyst promoter modified CdS significantly improves the photocatalytic hydrogen production capability of CdS, can replace noble metal as a high-efficiency catalyst promoter for photocatalytic research and application, and provides a method and an idea for developing a high-activity semiconductor composite photocatalyst in the future.
(2) The preparation method is simple, low in cost, short in preparation time and high in operability.
Drawings
FIG. 1 is a MoS prepared in example 1 2 XRD pattern of/CdS composite material.
FIG. 2 is a MoS prepared in example 1 2 SEM image of/CdS composite material.
FIG. 3 is the MoS prepared in example 1 2 a/CdS composite material photocatalytic hydrogen production diagram.
Detailed description of the preferred embodiments
The following examples are intended to further illustrate the present invention and should not be construed as limiting the present invention, and any other changes, modifications, substitutions, combinations and simplifications which do not depart from the spirit and principle of the present invention should be construed as equivalents thereof, and shall be included within the scope of the present invention. Unless otherwise specified, the technical means used in the examples are conventional means well known to those skilled in the art.
Example 1:
(1) CdS Material preparation
10.4mmol of cadmium nitrate and 31.2mmol of thiourea were dissolved in 50mL of ethylenediamine and stirred until completely dissolved. The resulting mixture was reacted in a 100mL teflon lined reactor at 160 ℃ for 48h, centrifuged after reaction (6000r, 8min) and the precipitate was collected, followed by 5-7 washes with ethanol alternating with deionized water. And (4) mixing the product obtained after centrifugation (6000r for 8min) with 0.02mol/L sulfuric acid and stirring for 2h, and drying the obtained solution at 60 ℃ for 12h after centrifugation (6000r for 8min) to obtain CdS powder.
(2)MoS 2 Preparation of/CdS composite material
0.2mmol sodium molybdate and 0.8mmol thioacetamide were dissolved in 60mL deionized water, followed by the addition of the prepared CdS powder and stirring well. The ratio of Mo to Cd in the composite material is adjusted by changing the addition of CdS, wherein Mo: the percentage of Cd (mole ratio) is 5%, 7.5%, 10%, 12.5%, 15%, 17.5%, 20%, named R5, R7.5, R10, R12.5, R15, R17.5, R20 respectively. Reacting the obtained mixed solution in a 100mL polytetrafluoroethylene reaction kettle at 180 ℃ for 24h, cooling the reaction kettle to room temperature, centrifuging (6000r, 8min) to obtain precipitate, alternately washing the precipitate with ethanol and deionized water for 2-3 times, and drying in a 60 ℃ oven to obtain MoS 2 a/CdS composite material.
(3)MoS 2 Photocatalytic hydrogen production activity experiment of/CdS composite material
The photocatalytic hydrogen production experimental device is manufactured by using a 100mL pyrex glass flat-bottomed flask with good airtightness, and a magnetic stirrer is arranged at the bottom of the photocatalytic hydrogen production experimental device. A350W xenon lamp was equipped with an ultraviolet filter (. lamda. ≦ 420nm) as a visible light source and placed 15cm from the photocatalytic reaction apparatus. The light spot focused on the glass flask was measured byA visible light radiometer (Model: FZ-A, China) in the wavelength range of 420-1000nm to have an illumination intensity of about 70mW cm -2 . 50mg of the MoS prepared above was weighed 2 the/CdS composite material is dispersed in 80mL of aqueous solution containing 10 vol% of lactic acid, and before the photocatalytic reaction, a one-way air outlet with a valve is reserved in the photocatalytic hydrogen production reactor, and nitrogen is introduced for bubbling for 30min to remove air in a bottle and dissolved oxygen in the solution. Turning on a light source to irradiate from one side of a light sending glass container filled with reaction suspension liquid in the photocatalytic reactor, and continuously stirring by magnetic force in the whole photocatalytic reaction process to ensure MoS 2 Suspension of CdS sample particles 0.4mL of gas was sampled every 1 hour and tested by gas chromatography (GC-14C, TCD, N) 2 A carrier gas, which is a gas that is,
molecular sieves, Shimadzu, Japan).
Structural characterization and performance testing:
(1) XRD analysis
To the MoS obtained at different load ratios 2 XRD analysis of the/CdS photocatalytic composite material is carried out, as shown in figure 1. All diffraction peaks for all samples correspond to pure hexagonal phase CdS, consistent with standard card (JCPDS card No. 41-1049). Peak intensity of each diffraction peak following MoS 2 An increase in the ratio and a decrease in the ratio indicate MoS 2 Crystallinity of CdS with MoS 2 The ratio is increased and decreased.
(2) SEM analysis
To the MoS obtained at different load ratios 2 SEM analysis of the/CdS photocatalytic composite material is shown in FIG. 2. FIGS. 2-A, B, C are MoS, respectively 2 、CdS、MoS 2 SEM image of/CdS. FIG. 2-A shows pure MoS 2 The sample presents flower-shaped nanospheres, is in a folded and clustered state, and is uniform in size and uniform in dispersion. FIG. 2-B shows CdS in rod-like structure and in pure hexagonal crystal form. FIG. 2-C shows the load ratio Mo: MoS with Cd of 10% 2 Morphology of CdS samples, MoS 2 Spread and wrapped on a cadmium sulfide rod, the two are fully connected and MoS 2 The agglomeration between the nanosheets was reduced, indicating MoS 2 The successful load of.
(3) Photocatalytic hydrogen production analysis
To the MoS obtained at different load ratios 2 The hydrogen production rate of the/CdS photocatalytic composite material under visible light is measured, and the result is shown in figure 3. The results show CdS and MoS 2 Has no obvious hydrogen production effect under the independent action. And MoS 2 the/CdS composite material shows extremely strong photocatalytic hydrogen production performance. Random MoS 2 Increased proportion of (5% -20%), MoS 2 The photocatalytic hydrogen production performance of the/CdS composite material is increased and then reduced, and MoS is obtained under the condition that the load proportion is 10 percent 2 The fastest hydrogen production rate of/CdS is 621.3 mu mol/h.
Claims (10)
1. MoS 2 The preparation method of the/CdS photocatalytic composite material is characterized by comprising the following steps of: the method comprises the following steps: adding sodium molybdate, thioacetamide and CdS powder into water, and fully stirring; the mixed solution reacts for 20 to 24 hours at the temperature of between 160 and 200 ℃, the mixed solution is cooled and then centrifuged to obtain sediment, and the sediment is washed and dried to obtain MoS 2 The CdS photocatalytic composite material.
2. The MoS of claim 1, wherein 2 The preparation method of the/CdS photocatalytic composite material is characterized by comprising the following steps of: the CdS is prepared by a method comprising the following steps of:
(1) dissolving cadmium nitrate and thiourea in ethylenediamine;
(2) reacting the mixture obtained in the step (1) at the temperature of 150 ℃ and 180 ℃ for 40-50h, centrifuging and collecting precipitates after the reaction, and washing for a plurality of times;
(3) and (3) mixing and stirring the product obtained in the step (2) with sulfuric acid, and then centrifugally drying to obtain CdS powder.
3. MoS according to claim 2 2 The preparation method of the/CdS photocatalytic composite material is characterized by comprising the following steps of: in the step (1), the molar ratio of the cadmium nitrate to the thiourea is 8.5-11: 28-32.
4. MoS according to claim 2 2 The preparation method of the/CdS photocatalytic composite material is characterized by comprising the following steps of: in the step (2), the washing is alternately washing by using ethanol and deionized water, and the washing times are 5-7 times.
5. MoS according to claim 2 2 The preparation method of the/CdS photocatalytic composite material is characterized by comprising the following steps of: in the step (2), the concentration of the sulfuric acid is 0.01-0.02mol/L, the stirring time is 2-3h, and the drying condition is that the temperature is kept at 50-70 ℃ for 10-14 h.
6. The MoS of claim 1 2 The preparation method of the/CdS photocatalytic composite material is characterized by comprising the following steps of: the molar ratio of the sodium molybdate to the thioacetamide is 1-3: 4-6.
7. The MoS of claim 1 2 The preparation method of the/CdS photocatalytic composite material is characterized by comprising the following steps of: the washing is to use ethanol and deionized water to wash for 2 to 3 times alternately; the drying condition is to keep 10-14h at 50-70 ℃.
8. The MoS of claim 1 2 The preparation method of the/CdS photocatalytic composite material is characterized by comprising the following steps of: the MoS 2 The mol ratio of Mo to Cd in the/CdS photocatalytic composite material is 5-20%.
9. MoS 2 the/CdS photocatalytic composite material is characterized in that: obtained by the production method according to any one of claims 1 to 8.
10. The method of claim 9MoS of (1) 2 Application of the CdS photocatalytic composite material in photocatalytic water decomposition hydrogen production.
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Citations (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN105664977A (en) * | 2016-02-03 | 2016-06-15 | 中国科学院化学研究所 | Molybdenum disulfide-cadmium sulfide nanometer composite material and preparing method and application thereof |
| CN105688945A (en) * | 2016-03-22 | 2016-06-22 | 福州大学 | Composite photo-catalyst with molybdenum disulfide (MoS2) nanosheet/cadmium sulfide (CdS) nanowire core-shell structure |
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| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN105664977A (en) * | 2016-02-03 | 2016-06-15 | 中国科学院化学研究所 | Molybdenum disulfide-cadmium sulfide nanometer composite material and preparing method and application thereof |
| CN105688945A (en) * | 2016-03-22 | 2016-06-22 | 福州大学 | Composite photo-catalyst with molybdenum disulfide (MoS2) nanosheet/cadmium sulfide (CdS) nanowire core-shell structure |
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