CN111151275A - MoS2/Mo2C Complex, MoS2/Mo2C/CdS composite material and preparation method and application thereof - Google Patents
MoS2/Mo2C Complex, MoS2/Mo2C/CdS composite material and preparation method and application thereof Download PDFInfo
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- 229910052961 molybdenite Inorganic materials 0.000 title claims abstract description 111
- 229910052982 molybdenum disulfide Inorganic materials 0.000 title claims abstract description 111
- CWQXQMHSOZUFJS-UHFFFAOYSA-N molybdenum disulfide Chemical compound S=[Mo]=S CWQXQMHSOZUFJS-UHFFFAOYSA-N 0.000 title claims abstract description 93
- 229910003178 Mo2C Inorganic materials 0.000 title claims abstract description 45
- 239000002131 composite material Substances 0.000 title claims abstract description 43
- 238000002360 preparation method Methods 0.000 title claims abstract description 25
- 230000001699 photocatalysis Effects 0.000 claims abstract description 51
- NINIDFKCEFEMDL-UHFFFAOYSA-N Sulfur Chemical compound [S] NINIDFKCEFEMDL-UHFFFAOYSA-N 0.000 claims abstract description 38
- 229910052717 sulfur Inorganic materials 0.000 claims abstract description 35
- 239000011593 sulfur Substances 0.000 claims abstract description 35
- 150000001875 compounds Chemical class 0.000 claims abstract description 22
- 239000000463 material Substances 0.000 claims abstract description 19
- ZOKXTWBITQBERF-UHFFFAOYSA-N Molybdenum Chemical compound [Mo] ZOKXTWBITQBERF-UHFFFAOYSA-N 0.000 claims abstract description 18
- 238000000034 method Methods 0.000 claims abstract description 18
- 229910052750 molybdenum Inorganic materials 0.000 claims abstract description 18
- 239000011733 molybdenum Substances 0.000 claims abstract description 18
- 239000000203 mixture Substances 0.000 claims abstract description 16
- 229910017464 nitrogen compound Inorganic materials 0.000 claims abstract description 14
- 239000002243 precursor Substances 0.000 claims abstract description 12
- 238000002156 mixing Methods 0.000 claims abstract description 10
- 238000010000 carbonizing Methods 0.000 claims abstract description 6
- 230000002194 synthesizing effect Effects 0.000 claims abstract description 4
- 239000001257 hydrogen Substances 0.000 claims description 35
- 229910052739 hydrogen Inorganic materials 0.000 claims description 35
- UFHFLCQGNIYNRP-UHFFFAOYSA-N Hydrogen Chemical compound [H][H] UFHFLCQGNIYNRP-UHFFFAOYSA-N 0.000 claims description 34
- 239000011941 photocatalyst Substances 0.000 claims description 25
- UMGDCJDMYOKAJW-UHFFFAOYSA-N thiourea Chemical compound NC(N)=S UMGDCJDMYOKAJW-UHFFFAOYSA-N 0.000 claims description 21
- 238000004519 manufacturing process Methods 0.000 claims description 20
- 239000007789 gas Substances 0.000 claims description 18
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims description 18
- XSQUKJJJFZCRTK-UHFFFAOYSA-N Urea Natural products NC(N)=O XSQUKJJJFZCRTK-UHFFFAOYSA-N 0.000 claims description 16
- 229910052793 cadmium Inorganic materials 0.000 claims description 15
- BDOSMKKIYDKNTQ-UHFFFAOYSA-N cadmium atom Chemical compound [Cd] BDOSMKKIYDKNTQ-UHFFFAOYSA-N 0.000 claims description 15
- 229910001868 water Inorganic materials 0.000 claims description 15
- 238000001354 calcination Methods 0.000 claims description 13
- 239000000725 suspension Substances 0.000 claims description 13
- CKUAXEQHGKSLHN-UHFFFAOYSA-N [C].[N] Chemical compound [C].[N] CKUAXEQHGKSLHN-UHFFFAOYSA-N 0.000 claims description 11
- YUKQRDCYNOVPGJ-UHFFFAOYSA-N thioacetamide Chemical compound CC(N)=S YUKQRDCYNOVPGJ-UHFFFAOYSA-N 0.000 claims description 8
- DLFVBJFMPXGRIB-UHFFFAOYSA-N thioacetamide Natural products CC(N)=O DLFVBJFMPXGRIB-UHFFFAOYSA-N 0.000 claims description 8
- 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
- 229910001220 stainless steel Inorganic materials 0.000 claims description 5
- 239000010935 stainless steel Substances 0.000 claims description 5
- 238000003756 stirring Methods 0.000 claims description 5
- XUJNEKJLAYXESH-REOHCLBHSA-N L-Cysteine Chemical compound SC[C@H](N)C(O)=O XUJNEKJLAYXESH-REOHCLBHSA-N 0.000 claims description 4
- YKYOUMDCQGMQQO-UHFFFAOYSA-L cadmium dichloride Chemical compound Cl[Cd]Cl YKYOUMDCQGMQQO-UHFFFAOYSA-L 0.000 claims description 4
- QGBSISYHAICWAH-UHFFFAOYSA-N dicyandiamide Chemical compound NC(N)=NC#N QGBSISYHAICWAH-UHFFFAOYSA-N 0.000 claims description 4
- 238000001914 filtration Methods 0.000 claims description 4
- 238000010438 heat treatment Methods 0.000 claims description 4
- 238000001027 hydrothermal synthesis Methods 0.000 claims description 4
- 235000015393 sodium molybdate Nutrition 0.000 claims description 4
- 239000011684 sodium molybdate Substances 0.000 claims description 4
- TVXXNOYZHKPKGW-UHFFFAOYSA-N sodium molybdate (anhydrous) Chemical compound [Na+].[Na+].[O-][Mo]([O-])(=O)=O TVXXNOYZHKPKGW-UHFFFAOYSA-N 0.000 claims description 4
- GWEVSGVZZGPLCZ-UHFFFAOYSA-N titanium dioxide Inorganic materials O=[Ti]=O GWEVSGVZZGPLCZ-UHFFFAOYSA-N 0.000 claims description 4
- XZMCDFZZKTWFGF-UHFFFAOYSA-N Cyanamide Chemical compound NC#N XZMCDFZZKTWFGF-UHFFFAOYSA-N 0.000 claims description 3
- 229920000877 Melamine resin Polymers 0.000 claims description 3
- 239000004202 carbamide Substances 0.000 claims description 3
- 238000001035 drying Methods 0.000 claims description 3
- JDSHMPZPIAZGSV-UHFFFAOYSA-N melamine Chemical compound NC1=NC(N)=NC(N)=N1 JDSHMPZPIAZGSV-UHFFFAOYSA-N 0.000 claims description 3
- 239000005864 Sulphur Substances 0.000 claims description 2
- APUPEJJSWDHEBO-UHFFFAOYSA-P ammonium molybdate Chemical compound [NH4+].[NH4+].[O-][Mo]([O-])(=O)=O APUPEJJSWDHEBO-UHFFFAOYSA-P 0.000 claims description 2
- 235000018660 ammonium molybdate Nutrition 0.000 claims description 2
- 239000011609 ammonium molybdate Substances 0.000 claims description 2
- 229940010552 ammonium molybdate Drugs 0.000 claims description 2
- LHQLJMJLROMYRN-UHFFFAOYSA-L cadmium acetate Chemical compound [Cd+2].CC([O-])=O.CC([O-])=O LHQLJMJLROMYRN-UHFFFAOYSA-L 0.000 claims description 2
- XIEPJMXMMWZAAV-UHFFFAOYSA-N cadmium nitrate Inorganic materials [Cd+2].[O-][N+]([O-])=O.[O-][N+]([O-])=O XIEPJMXMMWZAAV-UHFFFAOYSA-N 0.000 claims description 2
- 238000001816 cooling Methods 0.000 claims description 2
- NMHMNPHRMNGLLB-UHFFFAOYSA-N phloretic acid Chemical compound OC(=O)CCC1=CC=C(O)C=C1 NMHMNPHRMNGLLB-UHFFFAOYSA-N 0.000 claims description 2
- 238000000926 separation method Methods 0.000 abstract description 7
- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical compound [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 abstract description 5
- 229910052799 carbon Inorganic materials 0.000 abstract description 5
- 238000011068 loading method Methods 0.000 abstract description 5
- 238000007146 photocatalysis Methods 0.000 abstract description 4
- 150000002830 nitrogen compounds Chemical class 0.000 abstract description 3
- 229910052980 cadmium sulfide Inorganic materials 0.000 description 79
- 238000006243 chemical reaction Methods 0.000 description 8
- 229910000510 noble metal Inorganic materials 0.000 description 7
- 239000000243 solution Substances 0.000 description 7
- 239000007864 aqueous solution Substances 0.000 description 6
- 230000009286 beneficial effect Effects 0.000 description 6
- FIXLYHHVMHXSCP-UHFFFAOYSA-H azane;dihydroxy(dioxo)molybdenum;trioxomolybdenum;tetrahydrate Chemical compound N.N.N.N.N.N.O.O.O.O.O=[Mo](=O)=O.O=[Mo](=O)=O.O=[Mo](=O)=O.O=[Mo](=O)=O.O[Mo](O)(=O)=O.O[Mo](O)(=O)=O.O[Mo](O)(=O)=O FIXLYHHVMHXSCP-UHFFFAOYSA-H 0.000 description 5
- 238000003763 carbonization Methods 0.000 description 5
- -1 Transition Metal Sulfides Chemical class 0.000 description 4
- 239000012378 ammonium molybdate tetrahydrate Substances 0.000 description 4
- 239000003795 chemical substances by application Substances 0.000 description 4
- 238000000354 decomposition reaction Methods 0.000 description 4
- OISMQLUZKQIKII-UHFFFAOYSA-L dichlorocadmium;hydrate Chemical compound O.[Cl-].[Cl-].[Cd+2] OISMQLUZKQIKII-UHFFFAOYSA-L 0.000 description 4
- VYPSYNLAJGMNEJ-UHFFFAOYSA-N silicon dioxide Inorganic materials O=[Si]=O VYPSYNLAJGMNEJ-UHFFFAOYSA-N 0.000 description 4
- OKKJLVBELUTLKV-UHFFFAOYSA-N Methanol Chemical compound OC OKKJLVBELUTLKV-UHFFFAOYSA-N 0.000 description 3
- 239000003054 catalyst Substances 0.000 description 3
- 239000008367 deionised water Substances 0.000 description 3
- 229910021641 deionized water Inorganic materials 0.000 description 3
- 230000000694 effects Effects 0.000 description 3
- 239000002803 fossil fuel Substances 0.000 description 3
- 238000003760 magnetic stirring Methods 0.000 description 3
- 230000008569 process Effects 0.000 description 3
- 239000010453 quartz Substances 0.000 description 3
- 238000011160 research Methods 0.000 description 3
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 description 2
- OCDWFIWQOCOXKZ-UHFFFAOYSA-N cadmium(2+) dinitrate hydrate Chemical compound O.[Cd++].[O-][N+]([O-])=O.[O-][N+]([O-])=O OCDWFIWQOCOXKZ-UHFFFAOYSA-N 0.000 description 2
- HUKFCVYEXPZJJZ-UHFFFAOYSA-N cadmium;hydrate Chemical compound O.[Cd] HUKFCVYEXPZJJZ-UHFFFAOYSA-N 0.000 description 2
- 239000000969 carrier Substances 0.000 description 2
- 239000012159 carrier gas Substances 0.000 description 2
- 230000003197 catalytic effect Effects 0.000 description 2
- 238000011161 development Methods 0.000 description 2
- VDQVEACBQKUUSU-UHFFFAOYSA-M disodium;sulfanide Chemical compound [Na+].[Na+].[SH-] VDQVEACBQKUUSU-UHFFFAOYSA-M 0.000 description 2
- 238000004817 gas chromatography Methods 0.000 description 2
- 238000009776 industrial production Methods 0.000 description 2
- JVTAAEKCZFNVCJ-UHFFFAOYSA-N lactic acid Chemical compound CC(O)C(O)=O JVTAAEKCZFNVCJ-UHFFFAOYSA-N 0.000 description 2
- 238000012986 modification Methods 0.000 description 2
- 230000004048 modification Effects 0.000 description 2
- 239000002135 nanosheet Substances 0.000 description 2
- 238000013032 photocatalytic reaction Methods 0.000 description 2
- 239000000843 powder Substances 0.000 description 2
- 238000004445 quantitative analysis Methods 0.000 description 2
- 239000011734 sodium Substances 0.000 description 2
- 229910052979 sodium sulfide Inorganic materials 0.000 description 2
- 229910052723 transition metal Inorganic materials 0.000 description 2
- 238000005406 washing Methods 0.000 description 2
- 235000008331 Pinus X rigitaeda Nutrition 0.000 description 1
- 235000011613 Pinus brutia Nutrition 0.000 description 1
- 241000018646 Pinus brutia Species 0.000 description 1
- 238000002441 X-ray diffraction Methods 0.000 description 1
- KJNYWDYNPPTGLP-UHFFFAOYSA-L cadmium(2+);diacetate;hydrate Chemical compound O.[Cd+2].CC([O-])=O.CC([O-])=O KJNYWDYNPPTGLP-UHFFFAOYSA-L 0.000 description 1
- 239000003153 chemical reaction reagent Substances 0.000 description 1
- 238000004140 cleaning Methods 0.000 description 1
- 239000003245 coal Substances 0.000 description 1
- 229910052681 coesite Inorganic materials 0.000 description 1
- 238000007796 conventional method Methods 0.000 description 1
- 229910052906 cristobalite Inorganic materials 0.000 description 1
- 239000013078 crystal Substances 0.000 description 1
- 238000005265 energy consumption Methods 0.000 description 1
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- 238000011156 evaluation Methods 0.000 description 1
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- 150000002431 hydrogen Chemical class 0.000 description 1
- 238000010335 hydrothermal treatment Methods 0.000 description 1
- 230000006872 improvement Effects 0.000 description 1
- 235000014655 lactic acid Nutrition 0.000 description 1
- 239000004310 lactic acid Substances 0.000 description 1
- 229910052751 metal Inorganic materials 0.000 description 1
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- 230000001603 reducing effect Effects 0.000 description 1
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- 238000001878 scanning electron micrograph Methods 0.000 description 1
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- 229910052682 stishovite Inorganic materials 0.000 description 1
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- 150000003624 transition metals Chemical class 0.000 description 1
- 229910052905 tridymite Inorganic materials 0.000 description 1
- 238000001132 ultrasonic dispersion Methods 0.000 description 1
- 238000001291 vacuum drying Methods 0.000 description 1
- 239000002699 waste material Substances 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
- B01J27/00—Catalysts comprising the elements or compounds of halogens, sulfur, selenium, tellurium, phosphorus or nitrogen; Catalysts comprising carbon compounds
- B01J27/20—Carbon compounds
- B01J27/22—Carbides
-
- 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
-
- 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
-
- 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
- Y02P—CLIMATE CHANGE MITIGATION TECHNOLOGIES IN THE PRODUCTION OR PROCESSING OF GOODS
- Y02P20/00—Technologies relating to chemical industry
- Y02P20/10—Process efficiency
- Y02P20/133—Renewable energy sources, e.g. sunlight
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- Chemical & Material Sciences (AREA)
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- Engineering & Computer Science (AREA)
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- Chemical Kinetics & Catalysis (AREA)
- Combustion & Propulsion (AREA)
- Inorganic Chemistry (AREA)
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Abstract
The invention relates to the technical field of photocatalytic materials, and provides a MoS2/Mo2C Complex, MoS2/Mo2A C/CdS composite material and a preparation method and application thereof. The MoS2/Mo2The preparation method of the C compound comprises the following steps: synthesizing MoS from molybdenum source and first sulfur source2(ii) a Mixing MoS2Mixing with carbon and nitrogen compound to obtain mixture, partially carbonizing precursor of the mixture to form MoS2/Mo2C complex. MoS prepared using this method2/Mo2The C compound has good carrier separation efficiency, abundant active sites and excellent photocatalytic performance. Mixing MoS2/Mo2MoS formed by loading C compound on CdS2/Mo2The C/CdS composite material can be applied to photocatalysis in large scale because of MoS2，Mo2Valence of C and CdSIs cheap and abundant.
Description
Technical Field
The invention relates to the technical field of photocatalytic materials, in particular to a MoS2/Mo2C Complex, MoS2/Mo2A C/CdS composite material and a preparation method and application thereof.
Background
With the rapid growth of population and industrialization, the demand of people for energy is sharply increased. Limited storage of fossil fuels such as coal, oil and gas and the consumption thereofEnvironmental issues have created challenges to the sustainable development of our society. Solar-driven hydrogen production by water splitting is considered one of the most promising strategies to alleviate the global energy crisis, as solar energy and hydrogen with the highest energy density are clean, abundant and renewable. Basically, photocatalytic materials are required to be able to be applied in extreme environments, absorb visible light, and react with H2/H2O and OH/H2The energy bands of O are matched. Although many photocatalysts have been sought that can meet the above requirements, there are still significant challenges to developing ultra-efficient, low-cost, and stable photocatalysts. It has been demonstrated that loading a noble metal promoter can greatly enhance photocatalytic activity by attracting electrons to the promoter and leaving behind holes. However, noble metal supported photocatalysts are hampered by their high cost in practical photocatalytic water splitting applications.
Disclosure of Invention
The object of the present invention includes, for example, providing a MoS2/Mo2The C compound and the preparation method thereof have excellent HER performance and are beneficial to photocatalytic hydrogen evolution reaction.
The invention also aims to provide a composite photocatalytic material which has good carrier separation efficiency, abundant active sites and excellent photocatalytic performance.
The invention also provides a MoS2/Mo2The photocatalytic material prepared by the method has good carrier separation efficiency, abundant active sites and excellent photocatalytic performance.
The invention also aims to provide a composite photocatalytic material or MoS2/Mo2The C/CdS composite material is applied as a catalyst in photocatalytic hydrogen production.
The embodiment of the invention is realized by the following steps:
the embodiment of the invention provides a MoS2/Mo2A method of preparing a C complex, comprising: synthesizing MoS from molybdenum source and first sulfur source2(ii) a Mixing MoS2Mixing the mixture with carbon and nitrogen compounds to obtain a mixture,carbonizing a portion of a precursor of the mixture to form MoS2/Mo2C complex.
The embodiment of the invention provides a MoS2/Mo2C complex using the above MoS2/Mo2The C compound is prepared by the preparation method.
The embodiment of the invention provides a composite photocatalytic material, which comprises a photocatalyst and the MoS2/Mo2C Complex, MoS2/Mo2The C complex is supported on a photocatalyst.
The embodiment of the invention provides a MoS2/Mo2A method for preparing a C/CdS composite material, comprising: mixing the above MoS2/Mo2The C compound, the cadmium-containing hydrate and the second sulfur source are uniformly mixed, filtered and dried after hydrothermal reaction to form MoS2/Mo2C/CdS composite material.
The embodiment of the invention provides a composite photocatalytic material or MoS2/Mo2The C/CdS composite material is applied to photocatalytic hydrogen production or photoelectric devices.
The beneficial effects of the embodiment of the invention include:
the MoS provided by the invention2/Mo2The preparation method of the C compound has simple preparation process and easy operation, and is suitable for industrial production. MoS2/Mo2C has ultra-high HER activity, promoter MoS2/Mo2C can attract photo-generated electrons and leave holes, and is favorable for carrier separation and hydrogen generation2/Mo2C is formed on a photocatalyst and can further improve the catalytic performance, for example, supported on CdS, MoS2/Mo2The ratio of the C/CdS composite material to CdS to MoS2the/CdS was about 120 and 5 times higher. Obtained MoS2/Mo2The C/CdS can effectively replace the existing noble metal-loaded photocatalytic material. The MoS2/Mo2The C/CdS photocatalyst has higher photocatalytic performance than most CdS-based photocatalysts. It is even better than the Pt-containing photocatalystIs one of the most promising materials for industrial applications. Furthermore, MoS2/Mo2The price of C/CdS is not as high as 1/25 of the noble metal-based photocatalyst.
Drawings
In order to more clearly illustrate the technical solutions of the embodiments of the present invention, the drawings needed to be used in the embodiments will be briefly described below, it should be understood that the following drawings only illustrate some embodiments of the present invention and therefore should not be considered as limiting the scope, and for those skilled in the art, other related drawings can be obtained according to the drawings without inventive efforts.
FIG. 1 shows a MoS provided in example 1 of the present invention2、MoS2/Mo2C、CdS、MoS2CdS and MoS2/Mo2XRD pattern of C/CdS;
FIG. 2 shows MoS provided in example 1 of the present invention2/Mo2SEM image and EDX results for C/CdS;
FIG. 3 shows CdS, MoS provided in example 1 of the present invention2CdS and MoS2/Mo2Photocatalytic hydrogen evolution rate (a) of C/CdS; MoS2/Mo2And (b) researching hydrogen evolution repeatability of C/CdS.
Detailed Description
Embodiments of the present invention will be described in detail below with reference to examples, but it will be understood by those skilled in the art that the following examples are only illustrative of the present invention and should not be construed as limiting the scope of the present invention. The examples, in which specific conditions are not specified, were conducted under conventional conditions or conditions recommended by the manufacturer. The reagents or instruments used are not indicated by the manufacturer, and are all conventional products available commercially.
Following is a MoS according to an embodiment of the present invention2/Mo2C compound, composite photocatalytic material and MoS2/Mo2The C/CdS composite material, the preparation method and the application thereof and the method for preparing hydrogen by photocatalysis are specifically explained.
In a first aspect, embodiments of the present invention provide a MoS2/Mo2C compositeA method of making the compound, comprising the steps of:
s101, synthesizing MoS from a molybdenum source and a first sulfur source2。
Specifically, the molybdenum source and the first sulfur source are stirred in water for 50-70min, then the solution is transferred into a 50mL stainless steel autoclave and kept at 200 ℃ for 20-30h, and then the solution is filtered, washed by deionized water and dried in vacuum to obtain MoS2(ii) a Preferably, the molybdenum source comprises at least one of ammonium molybdate and sodium molybdate; preferably, the first sulphur source comprises one or more of thiourea, thioacetamide and cysteine.
Wherein the molar weight ratio of the molybdenum source to the first sulfur source is nMo:nS1: 2-6. In other embodiments, the molybdenum source and the first sulfur source may be used in a ratio (molar ratio) ranging from, for example, any one of 1:2, 1:3, 1:4, 1:5, or 1:6, or any two of them. If the ratio of the amount of the molybdenum source to the first sulfur source is less than 1:2, e.g., 1:1, MoS cannot be synthesized sufficiently2There will be a portion of the sulfur-poor MoS2-x(ii) a If the ratio of the amount of molybdenum source to the amount of the first sulfur source is greater than 1:6, e.g., 1:7, MoS can be synthesized2But results in excessive waste of the sulfur source.
S102, MoS2Mixing with carbon and nitrogen compound to obtain mixture, and partially carbonizing precursor of the mixture to form MoS2/Mo2C complex;
specifically, Ar-H is firstly used2Removing air in the calcining equipment by using gas; preferably, Ar-H2The flow rate of the gas is 10-100 sccm, and in other embodiments, Ar-H2The flow rate of the gas is any one of 10, 20, 30, 40, 50, 60, 70, 80, 90, 100sccm or a range of values between any two; preferably, the calcination apparatus is a tube furnace. Preferably, Ar-H2H in gas2In an amount of 5-10% of the total gas, and in other embodiments, Ar-H2H in gas2Is present in an amount of 5%, 6%, 7%, 8%, 9%, 10% of the total gas, or a range between any two. H2Can promote the reduction of the + 4-valent Mo into the + 2-valent Mo (Mo)2Mo in C) and then carbonized into Mo 2C. WhilePure Ar gas has no reducing effect.
Then calcining the precursor of the mixture in a calcining device with air removed at 400-500 ℃ for 1-4 hours, heating to 800-1050 ℃ at a heating rate of 8-12 ℃/min, calcining for 1-5 hours, and naturally cooling to room temperature to form MoS2/Mo2C complex; preferably, the MoS is such that, when mixed to give a mixture2The mass ratio of the carbon-nitrogen compound to the carbon-nitrogen compound is 1:1 to 20 (for example, any one or a range between 1:1, 1:5, 1:10, 1:15, and 1: 20); preferably, the carbon nitrogen compound comprises one or more of urea, melamine, dicyandiamide and cyanamide. The carbonized MoS is researched and invented by the inventor2/Mo2The C complex has better metallic properties to facilitate the separation of photogenerated carriers.
The choice of a stepwise temperature increase is currently sufficient carbonization. 400-500 ℃ is the temperature at which the carbon-nitrogen compound forms a relatively stable network carbon source, and the further temperature rise is the carbonization process. If the temperature is raised directly to the target temperature, too high a temperature may result in too rapid volatilization of the carbon source and insufficient carbonization. The precursor MoS can be maintained as much as possible at a specific temperature rise rate2The morphology of (2).
In other embodiments of the present invention, the calcination is performed at 400-500 ℃ for 1-4 hours, for example, at a value in the range of 400, 410, 420, 430, 440, 450, 460, 470, 480, 490, 500 or any value in the range of any two in the range of 1, 2, 3, 4 h. The temperature increase rate from 400-500 ℃ to 800-1050 ℃ may be, for example, any one or any range between 8, 9, 10, 11, 12 ℃/min. The calcination is carried out at 800-1050 ℃ for 1-5 hours, for example, the calcination may be carried out at a range value of 800, 850, 900, 950, 1000, 1050 ℃ or any two of them for 1, 2, 3, 4, 5 hours or any two of them.
In a second aspect, the present embodiment further provides a MoS2/Mo2A C/CdS composite material and a preparation method thereof.
Specifically, the MoS is prepared2/Mo2The C complex is loaded in CdS to form MoS2/Mo2C/CdS composite material.
Specifically, the cadmium-containing hydrate and MoS2/Mo2The C compound and the second sulfur source are mixed uniformly, then are filtered and dried after hydrothermal reaction, and MoS is formed2/Mo2A C/CdS composite material; wherein the cadmium hydrate and MoS are contained2/Mo2The mass ratio of the C compound to the second sulfur source is 1: 0.01-0.02: 1.1-1.2; preferably 1: 0.013: 1.15. the research of the inventor finds that when the cadmium hydrate and the MoS are contained2/Mo2If the C complex and the second sulfur source exceed this range, the photocatalytic performance of the material is deteriorated.
Preferably, the method controls the cadmium-containing hydrate and MoS2/Mo2The addition sequence of the C complex and the second sulfur source can improve the loading capacity and the loading uniformity. Specifically, cadmium-containing hydrate is dissolved in water, and MoS is added2/Mo2And C, stirring the compound to form a suspension, placing the suspension at room temperature after the suspension is formed, adding a second sulfur source into the suspension, stirring for 0.5-5h, and transferring the suspension into a stainless steel autoclave to react for 6-24 h at 150-200 ℃. Followed by filtration, deionized water washing and vacuum drying to form MoS2/Mo2C/CdS composite material.
Preferably, the cadmium-containing hydrate comprises one or more of cadmium nitrate, cadmium chloride and cadmium acetate; the second sulfur source comprises one or more of thiourea, thioacetamide and cysteine.
In a second aspect, embodiments of the present invention provide a MoS2/Mo2C/CdS composite material obtained by MoS2/Mo2The C/CdS composite material is prepared by the preparation method. The crystalline phase and structure of the sample were characterized by Rigaku smartlab X-ray diffractometer (XRD). Scanning Electron Microscopy (SEM) and Energy Dispersive Spectrometer (EDS) were tested by Zeiss Sigma.
In a third aspect, the embodiment of the present invention provides an MoS as described above2/Mo2C/CdS composite materialThe catalyst is applied to photocatalytic hydrogen production. The above MoS2/Mo2The C/CdS composite material can be used as a high-efficiency photocatalyst for water decomposition hydrogen production driven by solar energy, has ultrahigh photocatalytic activity, and has the speed of 32mmol/h/g, which is about 120 times of CdS.
In a fourth aspect, the embodiment of the present invention provides an MoS as described above2/Mo2Method for preparing hydrogen by C/CdS composite material photocatalysis, MoS2/Mo2The C/CdS composite material is used as a catalyst to catalyze the water solution containing the sacrificial agent so as to prepare hydrogen. In this example, the aqueous solution containing the sacrificial agent includes Na2SO3And Na2S, methanol aqueous solution, ethanol aqueous solution or lactic acid aqueous solution. Wherein, MoS2/Mo2The photocatalytic hydrogen production performance of the C/CdS composite material can be improved by adding the C/CdS composite material into an aqueous solution containing a sacrificial agent and introducing N2Air was removed and evaluated at room temperature against a quartz reactor system. The reaction system was sonicated to uniformly disperse the photocatalyst, then N was used before irradiation2Air was removed and the reaction was carried out under magnetic stirring. Quantitative analysis of the gaseous product by Agilent gas chromatography (N)2As carrier gas and the detector as TCD thermal conductivity detector). Wherein the ultrasonic dispersion time of the reaction system is 10-30 minutes. General formula (N)2The time for removing the air is 10-60 minutes. The amount of the gas product is 0.1-1 mL. MoS2/Mo2Before the photocatalytic hydrogen production performance of C/CdS is repeated, N is introduced every time2The previous gas was removed and then the photocatalytic reaction was performed under magnetic stirring.
The inventor's experiments and theoretical researches show that two-dimensional (2D) Transition Metal Sulfides (TMDs) having a sandwich structure, in which a transition metal layer is located between two layers of elemental sulfur, have HER catalytic activity. For example, MoS2And WS2Have been used as promoters to enhance photocatalytic hydrogen evolution performance. However, these TMDs are active at their metal edges and inert at their basal faces, which limits their role in photocatalytic performance. In this embodiment, the MoS is obtained by2Partially carbonised to form MoS2/Mo2C, overcoming MoS2And exhibit a relatively pure MoS2Higher HER Performance, MoS2/Mo2The C/CdS compound shows ultrahigh photocatalytic activity in the hydrogen production process, and the rate is 32mmol/h/g and is about 120 times of that of CdS.
In addition, it is noted that in the present embodiment, MoS2/Mo2The C compound can also be loaded on the surface of other photocatalysts including but not limited to CdS, g-C3N4And TiO2One or more of (a).
Wherein, MoS2/Mo2The specific method for loading the C complex into CdS is described in the text, and MoS can be loaded by the conventional method by the person skilled in the art2/Mo2The C compound is loaded on other photocatalysts (for example: g-C)3N4And/or TiO2) Thereby obtaining the composite photocatalytic material with excellent HER performance. The composite photocatalytic material can also be used for photocatalytic hydrogen production or photoelectric devices.
A MoS of the present invention is described below with reference to the following examples2/Mo2The C/CdS composite material, the preparation method and the application thereof, and the method for preparing hydrogen by photocatalysis are further explained.
Example 1
The embodiment provides a MoS2/Mo2The preparation method of the C/CdS composite material comprises the following steps:
S1、MoS2preparation of
Preparation of MoS by hydrothermal method2First, 1.24g of ammonium molybdate tetrahydrate (NH)4)6Mo7O24·4H2O) and 2.66g of thiourea (CH)4N2S) was added to 30mL Deionized (DI) water and stirred for 60 minutes. The solution was then transferred to a 50mL stainless steel autoclave and held at 200 ℃ for 24 hours. Filtering the obtained product, washing the product with deionized water and drying the product in vacuum to obtain MoS2。
S2、MoS2/Mo2C preparation
Firstly, the prepared MoS2(125mg) with 1g of dimerCyanamide powder (C)2H4N4) Mixing, placing in a tube furnace with Ar-H2The gas removed air (30 sccm). Then calcining the precursor of the mixture at 450 ℃ for 2 hours, raising the temperature to 950 ℃ at a temperature raising rate of 10 ℃/min and partially carbonizing the precursor for 2 hours to form MoS2/Mo2C complex, Ar-H in the course of the reaction2The flow rate of the gas was 50 sccm.
S3、MoS2/Mo2C/CdS preparation
0.73g of cadmium chloride hydrate (CdCl) are initially introduced2·2.5H2O) was dissolved in 30mL Deionized (DI) water. Then 9.2mgMoS2/Mo2C is added to the above solution. After stirring for 60 minutes, 0.84g of thiourea was added to the suspension and stirring was continued for 60 minutes. Then, the above solution was transferred to a 50mL stainless steel autoclave and maintained at 180 ℃ for 12 hours. The resulting product was filtered, DI washed and vacuum dried to yield MoS2/Mo2C/CdS。
Example 2
Examples 2-5 are essentially the same as example 1, except that: in example 1, the molybdenum source was ammonium molybdate tetrahydrate, the first sulfur source was thiourea, the carbon nitride compound was dicyandiamide powder, the cadmium-containing hydrate was cadmium chloride hydrate, and the second sulfur source was thiourea;
in example 2, the molybdenum source was sodium molybdate, the first sulfur source was thioacetamide, the carbon nitrogen compound was urea, the cadmium-containing hydrate was cadmium nitrate hydrate, and the second sulfur source was thioacetamide;
in example 3, the molybdenum source was ammonium molybdate tetrahydrate, the first sulfur source was thioacetamide, the carbon nitrogen compound was melamine, the cadmium-containing hydrate was cadmium acetate hydrate, and the second sulfur source was thioacetamide;
in example 4, the molybdenum source was sodium molybdate, the first sulfur source was thiourea, the carbon nitrogen compound was cyanamide, the cadmium-containing hydrate was cadmium nitrate hydrate, and the second sulfur source was thiourea;
in example 5, the molybdenum source was ammonium molybdate tetrahydrate, the first sulfur source was cysteine, the carbon nitride compound was dicyandiamide, the cadmium-containing hydrate was cadmium chloride hydrate, and the second sulfur source was cysteine.
Example 6
MoS as provided in example 12/Mo2The photocatalytic hydrogen production performance of the C/CdS composite material is as follows:
MoS2/Mo2photocatalytic Hydrogen production Performance of C/CdS by adding 50mg of photocatalyst to 85mL of aqueous solution containing sacrificial agent (0.35M Na)2SO3And 0.25M Na2S) and evaluated at room temperature against a quartz reactor system. The reaction system was sonicated for 15 minutes to uniformly disperse the photocatalyst, and then N was passed through for 15 minutes before light was applied2Air was removed and the reaction was carried out under magnetic stirring. At a specific time, the gaseous product (ca. 0.4mL) was taken for quantitative analysis (N) by Agilent gas chromatography (GC7890B)2As carrier gas and the detector as TCD thermal conductivity detector).
MoS was studied by XRD2，MoS2/Mo2C，CdS，MoS2CdS and MoS2/Mo2The crystal structure of the C/CdS sample is shown in FIG. 1. For MoS2/Mo2XRD profile of C (FIG. 1a), except MoS2In addition to the main peak of (A), many small MoS's also appear1.58Indicating vacancies of S. These S vacancies favor carbonization to form Mo2C. Due to Mo2Low C content, only a small Mo2The C diffraction peak was revealed. When MoS2And MoS2/Mo2Both C and CdS showed a characteristic peak of CdS (fig. 1 b). Despite MoS2And Mo2C has no obvious diffraction peak due to low content, but MoS2/Mo2SEM picture and EDS results of C/CdS clearly show MoS2And Mo2The presence of C (fig. 2). As shown in fig. 2, MoS2/Mo2CdS with C/CdS in pine tree shape and MoS in nano sheet shape2/Mo2C (fig. 2a and b). And the EDS results further confirm CdS and MoS2/Mo2The presence of C (fig. 2C). Furthermore, we have found MoS2/Mo2C still maintains the nanosheet structure without collapsing, which facilitates the photocatalytic reaction.
CdS、MoS2CdS and MoS2/Mo2The photocatalytic hydrogen production performance of C/CdS is evaluated in a quartz container under the irradiation of visible light. As shown in FIG. 3a, pure CdS showed slow photocatalytic hydrogen evolution activity (0.27mmol/h/g) when loaded with MoS2The photocatalytic activity of CdS is obviously improved. Surprisingly, MoS2/Mo2The C is loaded on CdS, so that the photocatalytic performance of the CdS is further improved compared with that of CdS and MoS2the/CdS was about 120 and 5 times higher. MoS2/Mo2The photocatalytic performance of C/CdS is also better than that of MXene-loaded CdS, which is recently reported. This phenomenon is attributed to MoS with ultra-high HER activity2/Mo2The presence of C. Due to the cocatalyst MoS2/Mo2C can attract photo-generated electrons and leave holes, facilitating carrier separation and hydrogen generation. In practical applications, the evaluation of the stability of the photocatalyst is also important. Research shows that MoS2/Mo2After 4 cycles (20 hours, FIG. 3b) of C/CdS, there was no significant decrease in photocatalytic activity, indicating its high stability and potential for practical use.
The invention obtains high-performance MoS through simple carbonization and hydrothermal treatment in several steps2/Mo2C/CdS photocatalytic Material, in one aspect Mo2C-grafted MoS2Has better metallicity and is beneficial to the separation of photogenerated carriers, and MoS2/Mo2The excellent HER performance of C is beneficial to the photocatalytic hydrogen evolution reaction.
Compared with the prior art, the invention provides a novel high-activity MoS2/Mo2The C/CdS composite material has simple preparation process and easy operation, and is suitable for industrial production. MoS prepared by the method of the invention2/Mo2The C/CdS can effectively replace the existing noble metal-loaded photocatalytic material. MoS provided in the present example2/Mo2C/CdS is used as a high-efficiency photocatalyst for solar-driven hydrogen production by water decomposition, wherein MoS2/Mo2C is a cocatalyst. MoS2/Mo2The C/CdS compound shows ultrahigh photocatalytic activity in the hydrogen production process, and the rate is 32mmol/h/g and is about 120 times of that of CdS. We expect MoS2/Mo2The C/CdS is rich and cheap and does not contain noble metal photocatalyst and can be applied to actual photocatalytic water decomposition for hydrogen production.
Hydrogen is considered an ideal substitute for fossil fuels and there are a number of processes in the industry for producing hydrogen, such as electrolytic water, petroleum cracking and water gas processes. However, current methods of producing hydrogen still come at the expense of energy consumption, such as electrical energy and fossil fuels. The emerging solar-driven water decomposition hydrogen production method is the most environment-friendly hydrogen production method because the solar energy is environment-friendly and abundant and the product (H) is2And O2) And (4) cleaning. Therefore, the industrialization of photocatalytic hydrogen production has huge market, which is not only beneficial to the social development of people, but also beneficial to the environmental protection. MoS provided by the embodiment of the invention2/Mo2The C/CdS photocatalyst has higher photocatalytic performance than most CdS-based photocatalysts. It is even superior to Pt-containing photocatalysts and would be one of the most promising materials for industrial applications. Furthermore, MoS2/Mo2The price of C/CdS is not as high as 1/25 of the noble metal-based photocatalyst.
The above is only a preferred embodiment of the present invention, and is not intended to limit the present invention, and various modifications and changes will occur to those skilled in the art. Any modification, equivalent replacement, or improvement made within the spirit and principle of the present invention should be included in the protection scope of the present invention.
Claims (10)
1. MoS2/Mo2A method for preparing a C complex, comprising:
synthesizing MoS from molybdenum source and first sulfur source2(ii) a The MoS is treated2Mixing with a carbon-nitrogen compound to obtain a mixture, partially carbonizing a precursor of said mixture to form MoS2/Mo2C complex.
2. The MoS of claim 12/Mo2The method for preparing the C complex is characterized in that the MoS is synthesized2The method comprises the following steps: placing the molybdenum source and the first sulfur source in waterStirring for 50-70min, maintaining at 200 deg.C for 20-30h, filtering, and drying to obtain MoS2；
Preferably, the molar weight ratio of the molybdenum source to the first sulfur source is nMo:nS＝1:2-6；
Preferably, the molybdenum source comprises at least one of ammonium molybdate and sodium molybdate;
preferably, the first sulphur source comprises one or more of thiourea, thioacetamide and cysteine.
3. The MoS of claim 12/Mo2A method of preparing a C-composite, wherein the precursor of the carbonized part of the mixture comprises: calcining the precursor of the mixture at 400-500 ℃ for 1-4 hours, then heating to 800-1050 ℃ at a heating rate of 8-12 ℃/min, calcining for 1-5 hours, and naturally cooling to room temperature to form the MoS2/Mo2C complex;
preferably, the MoS is such that, when the mixture is mixed, the MoS is2The mass ratio of the carbon-nitrogen compound to the carbon-nitrogen compound is 1: 1-20;
preferably, the carbon nitrogen compound comprises one or more of urea, melamine, dicyandiamide and cyanamide.
4. The MoS of claim 12/Mo2The preparation method of the C compound is characterized by further comprising the step of using Ar-H to prepare a precursor of the mixture before carbonizing the precursor2Removing air in the calcining equipment by using gas;
preferably, said Ar-H2The flow rate of the gas is 10-100 sccm;
preferably, the calcination apparatus is a tube furnace;
preferably, said Ar-H2H in gas2The content of (A) is 5-10% of the total gas.
5. MoS2/Mo2C complex, characterized in that it is prepared by using a compound according to any one of claims 1 to 4The MoS2/Mo2The C compound is prepared by the preparation method.
6. A composite photocatalytic material comprising a photocatalyst and the MoS of claim 52/Mo2C complex, said MoS2/Mo2C compound is loaded on the photocatalyst;
preferably, the photocatalyst comprises CdS, g-C3N4And TiO2One or more of (a).
7. MoS2/Mo2The preparation method of the C/CdS composite material is characterized by comprising the following steps of: the MoS of claim 52/Mo2Uniformly mixing the C compound, the cadmium-containing hydrate and the second sulfur source, filtering and drying after hydrothermal reaction to form the MoS2/Mo2A C/CdS composite material;
preferably, the cadmium-containing hydrate and the MoS2/Mo2The mass ratio of the C compound to the second sulfur source is 1: 0.01-0.02: 1.1-1.2; preferably 1: 0.013: 1.15;
preferably, the cadmium-containing hydrate comprises one or more of cadmium nitrate, cadmium chloride and cadmium acetate;
preferably, the second sulfur source comprises one or more of thiourea, thioacetamide and cysteine.
8. The MoS of claim 72/Mo2The preparation method of the C/CdS composite material is characterized in that the cadmium-containing hydrate and the MoS are mixed2/Mo2The C complex and the second sulfur source comprise: dissolving the cadmium-containing hydrate in water, and adding the MoS2/Mo2C, stirring to form a suspension, and then adding the second sulfur source to the suspension.
9. The MoS of claim 82/Mo2C/CdS composite materialThe preparation method is characterized in that after the suspension is formed, the suspension is placed at room temperature, then the second sulfur source is added into the suspension, the suspension is stirred for 0.5 to 5 hours, and then the suspension is transferred into a stainless steel autoclave to react for 6 to 24 hours at the temperature of 150 to 200 ℃.
10. A composite photocatalytic material as set forth in claim 6 or a MoS as set forth in claim 72/Mo2MoS prepared by preparation method of C/CdS composite material2/Mo2The C/CdS composite material is applied to photocatalytic hydrogen production or photoelectric devices.
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