CN113578353A - Preparation of polymolybdic acid-derived nickel metal sulfide and photocatalytic application thereof - Google Patents
Preparation of polymolybdic acid-derived nickel metal sulfide and photocatalytic application thereof Download PDFInfo
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- PXHVJJICTQNCMI-UHFFFAOYSA-N Nickel Chemical compound [Ni] PXHVJJICTQNCMI-UHFFFAOYSA-N 0.000 title claims abstract description 51
- 229910052759 nickel Inorganic materials 0.000 title claims abstract description 24
- 229910052976 metal sulfide Inorganic materials 0.000 title claims abstract description 23
- 239000002253 acid Substances 0.000 title claims abstract description 19
- 230000001699 photocatalysis Effects 0.000 title claims abstract description 19
- 238000002360 preparation method Methods 0.000 title claims abstract description 9
- UFHFLCQGNIYNRP-UHFFFAOYSA-N Hydrogen Chemical compound [H][H] UFHFLCQGNIYNRP-UHFFFAOYSA-N 0.000 claims abstract description 22
- 239000001257 hydrogen Substances 0.000 claims abstract description 22
- 229910052739 hydrogen Inorganic materials 0.000 claims abstract description 22
- 238000004519 manufacturing process Methods 0.000 claims abstract description 18
- 238000000034 method Methods 0.000 claims abstract description 8
- DDTIGTPWGISMKL-UHFFFAOYSA-N molybdenum nickel Chemical compound [Ni].[Mo] DDTIGTPWGISMKL-UHFFFAOYSA-N 0.000 claims abstract description 8
- UMGDCJDMYOKAJW-UHFFFAOYSA-N thiourea Chemical compound NC(N)=S UMGDCJDMYOKAJW-UHFFFAOYSA-N 0.000 claims abstract description 8
- 239000011941 photocatalyst Substances 0.000 claims abstract description 6
- XSQUKJJJFZCRTK-UHFFFAOYSA-N Urea Natural products NC(N)=O XSQUKJJJFZCRTK-UHFFFAOYSA-N 0.000 claims abstract description 4
- 238000001027 hydrothermal synthesis Methods 0.000 claims abstract description 4
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims description 20
- 239000008367 deionised water Substances 0.000 claims description 9
- 229910021641 deionized water Inorganic materials 0.000 claims description 9
- 238000006243 chemical reaction Methods 0.000 claims description 8
- QAOWNCQODCNURD-UHFFFAOYSA-N Sulfuric acid Chemical compound OS(O)(=O)=O QAOWNCQODCNURD-UHFFFAOYSA-N 0.000 claims description 6
- 229940101006 anhydrous sodium sulfite Drugs 0.000 claims description 6
- 238000009835 boiling Methods 0.000 claims description 6
- 238000001035 drying Methods 0.000 claims description 6
- 229910052961 molybdenite Inorganic materials 0.000 claims description 6
- 229910052982 molybdenum disulfide Inorganic materials 0.000 claims description 6
- 229910052979 sodium sulfide Inorganic materials 0.000 claims description 6
- GRVFOGOEDUUMBP-UHFFFAOYSA-N sodium sulfide (anhydrous) Chemical compound [Na+].[Na+].[S-2] GRVFOGOEDUUMBP-UHFFFAOYSA-N 0.000 claims description 6
- GEHJYWRUCIMESM-UHFFFAOYSA-L sodium sulfite Chemical compound [Na+].[Na+].[O-]S([O-])=O GEHJYWRUCIMESM-UHFFFAOYSA-L 0.000 claims description 6
- 238000005406 washing Methods 0.000 claims description 6
- 238000000354 decomposition reaction Methods 0.000 claims description 5
- 239000003795 chemical substances by application Substances 0.000 claims description 4
- APUPEJJSWDHEBO-UHFFFAOYSA-P ammonium molybdate Chemical compound [NH4+].[NH4+].[O-][Mo]([O-])(=O)=O APUPEJJSWDHEBO-UHFFFAOYSA-P 0.000 claims description 3
- 235000018660 ammonium molybdate Nutrition 0.000 claims description 3
- 239000011609 ammonium molybdate Substances 0.000 claims description 3
- 229940010552 ammonium molybdate Drugs 0.000 claims description 3
- 230000003197 catalytic effect Effects 0.000 claims description 3
- 239000002131 composite material Substances 0.000 claims description 3
- 238000001816 cooling Methods 0.000 claims description 3
- LGQLOGILCSXPEA-UHFFFAOYSA-L nickel sulfate Chemical compound [Ni+2].[O-]S([O-])(=O)=O LGQLOGILCSXPEA-UHFFFAOYSA-L 0.000 claims description 3
- 229910000363 nickel(II) sulfate Inorganic materials 0.000 claims description 3
- USHAGKDGDHPEEY-UHFFFAOYSA-L potassium persulfate Chemical compound [K+].[K+].[O-]S(=O)(=O)OOS([O-])(=O)=O USHAGKDGDHPEEY-UHFFFAOYSA-L 0.000 claims description 3
- 239000000843 powder Substances 0.000 claims description 3
- 238000003756 stirring Methods 0.000 claims description 3
- 238000000967 suction filtration Methods 0.000 claims description 3
- 238000005303 weighing Methods 0.000 claims description 3
- 239000002994 raw material Substances 0.000 abstract description 3
- 238000005215 recombination Methods 0.000 abstract 1
- 230000006798 recombination Effects 0.000 abstract 1
- 238000013112 stability test Methods 0.000 abstract 1
- 229910052723 transition metal Inorganic materials 0.000 description 6
- 150000003624 transition metals Chemical class 0.000 description 6
- UCKMPCXJQFINFW-UHFFFAOYSA-N Sulphide Chemical compound [S-2] UCKMPCXJQFINFW-UHFFFAOYSA-N 0.000 description 4
- YGHCWPXPAHSSNA-UHFFFAOYSA-N nickel subsulfide Chemical compound [Ni].[Ni]=S.[Ni]=S YGHCWPXPAHSSNA-UHFFFAOYSA-N 0.000 description 4
- CWQXQMHSOZUFJS-UHFFFAOYSA-N molybdenum disulfide Chemical compound S=[Mo]=S CWQXQMHSOZUFJS-UHFFFAOYSA-N 0.000 description 3
- 239000003153 chemical reaction reagent Substances 0.000 description 2
- 229920001795 coordination polymer Polymers 0.000 description 2
- 239000013078 crystal Substances 0.000 description 2
- 229910052751 metal Inorganic materials 0.000 description 2
- 239000002184 metal Substances 0.000 description 2
- 239000002086 nanomaterial Substances 0.000 description 2
- 230000006911 nucleation Effects 0.000 description 2
- 238000010899 nucleation Methods 0.000 description 2
- 238000001907 polarising light microscopy Methods 0.000 description 2
- 229920006324 polyoxymethylene Polymers 0.000 description 2
- 229910052724 xenon Inorganic materials 0.000 description 2
- FHNFHKCVQCLJFQ-UHFFFAOYSA-N xenon atom Chemical compound [Xe] FHNFHKCVQCLJFQ-UHFFFAOYSA-N 0.000 description 2
- -1 Mo)VI Chemical class 0.000 description 1
- KEAYESYHFKHZAL-UHFFFAOYSA-N Sodium Chemical class [Na] KEAYESYHFKHZAL-UHFFFAOYSA-N 0.000 description 1
- 238000003917 TEM image Methods 0.000 description 1
- 238000005054 agglomeration Methods 0.000 description 1
- 230000002776 aggregation Effects 0.000 description 1
- 125000000129 anionic group Chemical group 0.000 description 1
- QVGXLLKOCUKJST-UHFFFAOYSA-N atomic oxygen Chemical compound [O] QVGXLLKOCUKJST-UHFFFAOYSA-N 0.000 description 1
- 230000015572 biosynthetic process Effects 0.000 description 1
- 239000003054 catalyst Substances 0.000 description 1
- 239000013256 coordination polymer Substances 0.000 description 1
- 238000005516 engineering process Methods 0.000 description 1
- 238000002474 experimental method Methods 0.000 description 1
- 238000005286 illumination Methods 0.000 description 1
- 229910052742 iron Inorganic materials 0.000 description 1
- 229910052748 manganese Inorganic materials 0.000 description 1
- 239000000463 material Substances 0.000 description 1
- 238000002156 mixing Methods 0.000 description 1
- 239000002057 nanoflower Substances 0.000 description 1
- 239000002135 nanosheet Substances 0.000 description 1
- 239000001301 oxygen Substances 0.000 description 1
- 229910052760 oxygen Inorganic materials 0.000 description 1
- 238000007146 photocatalysis Methods 0.000 description 1
- 238000006303 photolysis reaction Methods 0.000 description 1
- 230000015843 photosynthesis, light reaction Effects 0.000 description 1
- 239000002243 precursor Substances 0.000 description 1
- 238000001878 scanning electron micrograph Methods 0.000 description 1
- 238000000926 separation method Methods 0.000 description 1
- 239000011684 sodium molybdate Substances 0.000 description 1
- 235000015393 sodium molybdate Nutrition 0.000 description 1
- TVXXNOYZHKPKGW-UHFFFAOYSA-N sodium molybdate (anhydrous) Chemical compound [Na+].[Na+].[O-][Mo]([O-])(=O)=O TVXXNOYZHKPKGW-UHFFFAOYSA-N 0.000 description 1
- 238000001228 spectrum Methods 0.000 description 1
- WWNBZGLDODTKEM-UHFFFAOYSA-N sulfanylidenenickel Chemical compound [Ni]=S WWNBZGLDODTKEM-UHFFFAOYSA-N 0.000 description 1
- 230000002195 synergetic effect Effects 0.000 description 1
- 238000003786 synthesis reaction Methods 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
- B01J27/02—Sulfur, selenium or tellurium; Compounds thereof
- B01J27/04—Sulfides
- B01J27/047—Sulfides with chromium, molybdenum, tungsten or polonium
- B01J27/051—Molybdenum
- B01J27/0515—Molybdenum with iron group metals or platinum group metals
-
- 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
- B01J37/00—Processes, in general, for preparing catalysts; Processes, in general, for activation of catalysts
- B01J37/08—Heat treatment
- B01J37/10—Heat treatment in the presence of water, e.g. steam
-
- 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
-
- Y—GENERAL TAGGING OF NEW TECHNOLOGICAL DEVELOPMENTS; GENERAL TAGGING OF CROSS-SECTIONAL TECHNOLOGIES SPANNING OVER SEVERAL SECTIONS OF THE IPC; TECHNICAL SUBJECTS COVERED BY FORMER USPC CROSS-REFERENCE ART COLLECTIONS [XRACs] AND DIGESTS
- Y02—TECHNOLOGIES OR APPLICATIONS FOR MITIGATION OR ADAPTATION AGAINST CLIMATE CHANGE
- Y02E—REDUCTION OF GREENHOUSE GAS [GHG] EMISSIONS, RELATED TO ENERGY GENERATION, TRANSMISSION OR DISTRIBUTION
- Y02E60/00—Enabling technologies; Technologies with a potential or indirect contribution to GHG emissions mitigation
- Y02E60/30—Hydrogen technology
- Y02E60/36—Hydrogen production from non-carbon containing sources, e.g. by water electrolysis
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- Organic Chemistry (AREA)
- Engineering & Computer Science (AREA)
- Materials Engineering (AREA)
- Chemical Kinetics & Catalysis (AREA)
- Health & Medical Sciences (AREA)
- General Health & Medical Sciences (AREA)
- Combustion & Propulsion (AREA)
- Inorganic Chemistry (AREA)
- Physics & Mathematics (AREA)
- Thermal Sciences (AREA)
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Abstract
The invention relates to preparation of a polymolybdic acid-derived nickel metal sulfide and photocatalytic application thereof. The invention aims to solve the problems of the recombination of photogenerated holes and low hydrogen production efficiency of the existing photocatalyst. The adopted method comprises the following steps: the preparation method is characterized in that Waugh type nickel molybdenum nonapolyacid and thiourea are used as raw materials, a one-step hydrothermal synthesis method is adopted to prepare a nickel metal sulfide photocatalyst derived from polymolybdic acid, and the nickel metal sulfide photocatalyst is found to have high hydrogen production rate and good stability after photocatalytic hydrogen production and stability test.
Description
Technical Field
The invention relates to a polymolybdic acid-derived nickel metal sulfide nano material.
Background
The solar energy is a focus of great attention on photolysis water hydrogen production, and the photocatalytic hydrogen production is a technology capable of converting solar energy into clean and renewable hydrogen energy. Compared with single metal sulfide, the bimetal sulfide shows obvious advantages in the process of photocatalytic hydrogen production by virtue of unique bimetal synergistic effect.
The Polyacids (POMs) are used as a molecular platform capable of providing a plurality of transition metal sources at the same time, and the problem that the growth process is difficult to control due to inconsistent nucleation rates of all components caused by the introduction of the transition metals is well solved. In particular, in one aspect, the polyoxometallate, as a polynuclear inorganic metal anionic oxygen cluster, can provide multiple sources of early transition metals (particularly Mo)VI、WVIAnd VV). Another one isIn one aspect, the organometallic polymer has a diverse, tunable structure that facilitates the introduction of a second transition metal (particularly Co, Ni, Fe, Mn, etc.). Thus, the polyacid-based metal-organic coordination polymers as precursors provide opportunities for the synthesis of highly dispersed bimetallic sulfide materials.
Disclosure of Invention
Based on the background, the invention aims to provide a preparation method and a photocatalytic application of a nickel metal sulfide derived from polymolybdic acid, wherein the preparation method is simple and convenient and has low cost. The prepared nano material has high hydrogen production rate and good stability.
The purpose of the invention is realized as follows:
a method of preparing a polymolybdic acid-derivatized nickel metal sulfide, comprising the steps of:
(1) 0.47g of nickel sulfate was weighed out and dissolved in 5mL of boiling water to give a solution a, 4.94g of ammonium molybdate was weighed out next and dissolved in 20mL of deionized water to give a solution B, the pH was adjusted to 4.1 with 1mol/L of sulfuric acid solution, the solution B was heated to boiling and the solution B was added to the solution a while hot, at which time 0.75g of potassium persulfate was added in addition. And (3) after the solution is cooled to room temperature, carrying out suction filtration and washing to obtain gray powder, namely the nickel-molybdenum nonapolyacid, and drying in a 60 ℃ oven for later use.
(2) Weighing 0.0369g of nickel-molybdenum nonapolyacid and 0.06g of thiourea, dispersing in 10ml of deionized water, stirring for 2-3 hours on a magnetic stirrer, placing in a hydrothermal reaction kettle under the reaction conditions of 200 ℃ and 24 hours, and naturally cooling to room temperature after the reaction is finished.
(3) Repeatedly washing the obtained composite material with deionized water, and drying in a 60 ℃ oven to obtain Ni3S2-MoS2And forming flower-like clusters.
The application of the nickel metal sulfide derived from polymolybdic acid is mainly in the aspect of hydrogen production by photocatalytic water.
The application method comprises the following steps: sodium sulfide and anhydrous sodium sulfite are used as sacrificial agents, a system for producing hydrogen by photocatalytic water decomposition is used as a catalytic system with the highest hydrogen production, and the average hydrogen production efficiency is 2770 mu mol g-1·h-1Therefore, the polymolybdic acid-derived nickel metal sulfide is a high-efficiency photocatalyst for photocatalytic water decomposition.
Compared with the prior art, the invention has the following characteristics:
the invention adopts Polyacid (POMs) as a molecular platform which can provide a plurality of transition metal sources at the same time, and well solves the problem that the growth process is difficult to control due to the inconsistent nucleation rate of each component caused by the introduction of the transition metal. The technical bottlenecks of uneven mixing of reaction raw materials, mutual separation, asynchronous reaction, inconsistent product morphology, easy agglomeration and the like in the traditional technical line for preparing the bimetallic sulfide by using simple sodium molybdate and metal salt as main raw materials are broken through, so that the highly dispersed and uniformly distributed bimetallic sulfide is directionally prepared. The average hydrogen production efficiency is 2770 mu mol g by using a 500W xenon lamp as a light source and sodium sulfide and anhydrous sodium sulfite as sacrificial agents-1·h-1。
Detailed Description
The present invention will be described in detail below with reference to the accompanying drawings and examples.
Example 1, a polymolybdic acid-derivatized nickel metal sulfide, comprising the following preparative steps:
(1) 0.47g of nickel sulfate was weighed out and dissolved in 5mL of boiling water to give a solution a, 4.94g of ammonium molybdate was weighed out next and dissolved in 20mL of deionized water to give a solution B, the pH was adjusted to 4.1 with 1mol/L of sulfuric acid solution, the solution B was heated to boiling and the solution B was added to the solution a while hot, at which time 0.75g of potassium persulfate was added in addition. And (3) after the solution is cooled to room temperature, carrying out suction filtration and washing to obtain gray powder, namely the nickel-molybdenum nonapolyacid, and drying in a 60 ℃ oven for later use.
(2) Weighing 0.0369g of nickel-molybdenum nonapolyacid and 0.06g of thiourea, dispersing in 10ml of deionized water, stirring for 2-3 hours on a magnetic stirrer, placing in a hydrothermal reaction kettle under the reaction conditions of 200 ℃ and 24 hours, and naturally cooling to room temperature after the reaction is finished.
(3) Repeatedly washing the obtained composite material with deionized water, and drying in a 60 deg.C oven to obtain the final productTo Ni3S2-MoS2And forming flower-like clusters.
The invention is further described with reference to the following drawings and examples:
drawings
FIG. 1 shows a polymolybdic acid-derived nickel metal sulfide and MoS2(JCPDS,No.37-1492)、Ni3S2(JCPDS, No.44-1418) XRD spectrum. Nickel metal sulfide and MoS derived from polymolybdic acid2(JCPDS,No. 37-1492)、Ni3S2(JCPDS, No.44-1418) has good matching properties, and specifically, diffraction peaks appearing at 14.1 °, 39.4 ° and 58.6 ° are assigned to MoS2(JCPDS, No.37-1492) with (002) and (003) planes and (110) plane. The positions of diffraction peaks appearing at 44.3 °, 37.7 ° and 31.1 ° at the same time are assigned to Ni3S2(JCPDS, No.44-1418) with (202), (003) and (110) crystal planes.
FIG. 2 is a scanning electron micrograph, MoS, of a polymolybdic acid-derived nickel metal sulfide2And Ni3S2The nano-sheet structure of (2) is crossed to form a nano-flower cluster.
FIG. 3 is a transmission electron micrograph of a polymolybdic acid-derived nickel metal sulfide showing lattice spacings of 0.35nm and 0.61nm, respectively, corresponding to Ni3S2(003) plane of (C) and MoS2(002) crystal face of (a).
FIG. 4 is a graph showing the hydrogen production rate for 6 hours for a polymolybdic acid-derived nickel metal sulfide and nickel molybdenum nonapolyacid prepared with sodium sulfide and anhydrous sodium sulfite as sacrificial reagents. In the experiment, by comparing the influence of various sacrificial agents on the system, sodium sulfide and anhydrous sodium sulfite are finally selected as the sacrificial agents, the system for decomposing water by photocatalysis to produce hydrogen is the catalytic system with the highest hydrogen production, and the average hydrogen production efficiency is 2770 mu mol g-1·h-1Therefore, the polymolybdic acid-derived nickel metal sulfide is a high-efficiency photocatalyst for photocatalytic water decomposition.
FIG. 5 is a graph showing the 30 hour stability of one of the polymolybdic acid-derivatized nickel metal sulfides prepared with sodium sulfide and anhydrous sodium sulfite as sacrificial reagents. The 5-cycle test was performed for 30h under illumination with a 500W xenon lamp as the light source. The photocatalytic activity is not lost after 30 hours of circulation, which shows that the nickel sulfide has very good circulation stability, and the prepared polymolybdic acid-derived nickel metal sulfide can be used as a very stable catalyst for photocatalytic hydrogen production.
Claims (3)
1. The preparation method of the polymolybdic acid-derived nickel metal sulfide and the photocatalytic application thereof comprises the following steps:
(1) 0.47g of nickel sulfate was weighed out and dissolved in 5mL of boiling water to give a solution a, 4.94g of ammonium molybdate was weighed out next and dissolved in 20mL of deionized water to give a solution B, the pH was adjusted to 4.1 with 1mol/L of sulfuric acid solution, the solution B was heated to boiling and the solution B was added to the solution a while hot, at which time 0.75g of potassium persulfate was added in addition. And (3) after the solution is cooled to room temperature, carrying out suction filtration and washing to obtain gray powder, namely the nickel-molybdenum nonapolyacid, and drying in a 60 ℃ oven for later use.
(2) Weighing 0.0369g of nickel-molybdenum nonapolyacid and 0.06g of thiourea, dispersing in 10ml of deionized water, stirring for 2-3 hours on a magnetic stirrer, placing in a hydrothermal reaction kettle under the reaction conditions of 200 ℃ and 24 hours, and naturally cooling to room temperature after the reaction is finished.
(3) Repeatedly washing the obtained composite material with deionized water, and drying in a 60 ℃ oven to obtain Ni3S2-MoS2And forming flower-like clusters.
2. The preparation method and the photocatalytic application of the polymolybdic acid-derived nickel metal sulfide of claim 1, wherein the preparation method and the application of the polymolybdic acid-derived nickel metal sulfide are used for photocatalytic hydrogen production.
3. The use according to claim 2, characterized in that the method of application is as follows: sodium sulfide and anhydrous sodium sulfite are used as sacrificial agents, a system for producing hydrogen by photocatalytic water decomposition is used as a catalytic system with the highest hydrogen production, and the average hydrogen production efficiency is 2770 mu mol g-1·h-1Therefore, the polymolybdic acid-derived nickel metal sulfide is a high-efficiency photocatalyst for photocatalytic water decomposition.
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Cited By (3)
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CN114950491A (en) * | 2022-03-09 | 2022-08-30 | 哈尔滨理工大学 | Preparation of nickel-molybdenum-cadmium trimetal nano material constructed by polyacid and photocatalytic application of nickel-molybdenum-cadmium trimetal nano material |
CN115159452A (en) * | 2022-08-19 | 2022-10-11 | 上海大学 | Bimetal sulfide composite magnesium-based hydrogen storage material and preparation method thereof |
CN115254160A (en) * | 2022-03-31 | 2022-11-01 | 北华大学 | Biochar-based supported polyacid catalyst and application thereof |
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Cited By (3)
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CN115159452A (en) * | 2022-08-19 | 2022-10-11 | 上海大学 | Bimetal sulfide composite magnesium-based hydrogen storage material and preparation method thereof |
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