CN113952964B - Preparation method and application of 2D/3D structured molybdenum disulfide/indium oxide nanocomposite - Google Patents
Preparation method and application of 2D/3D structured molybdenum disulfide/indium oxide nanocomposite Download PDFInfo
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- 239000002114 nanocomposite Substances 0.000 title claims abstract description 48
- 238000002360 preparation method Methods 0.000 title claims abstract description 14
- 229910003437 indium oxide Inorganic materials 0.000 title claims abstract description 11
- PJXISJQVUVHSOJ-UHFFFAOYSA-N indium(iii) oxide Chemical compound [O-2].[O-2].[O-2].[In+3].[In+3] PJXISJQVUVHSOJ-UHFFFAOYSA-N 0.000 title claims abstract description 11
- CWQXQMHSOZUFJS-UHFFFAOYSA-N molybdenum disulfide Chemical compound S=[Mo]=S CWQXQMHSOZUFJS-UHFFFAOYSA-N 0.000 title claims abstract description 11
- 229910052982 molybdenum disulfide Inorganic materials 0.000 title claims abstract description 11
- 239000000463 material Substances 0.000 claims abstract description 46
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims abstract description 46
- 230000001699 photocatalysis Effects 0.000 claims abstract description 28
- XSQUKJJJFZCRTK-UHFFFAOYSA-N Urea Chemical compound NC(N)=O XSQUKJJJFZCRTK-UHFFFAOYSA-N 0.000 claims abstract description 26
- 239000004202 carbamide Substances 0.000 claims abstract description 26
- VBXWCGWXDOBUQZ-UHFFFAOYSA-K diacetyloxyindiganyl acetate Chemical compound [In+3].CC([O-])=O.CC([O-])=O.CC([O-])=O VBXWCGWXDOBUQZ-UHFFFAOYSA-K 0.000 claims abstract description 26
- UFHFLCQGNIYNRP-UHFFFAOYSA-N Hydrogen Chemical compound [H][H] UFHFLCQGNIYNRP-UHFFFAOYSA-N 0.000 claims abstract description 24
- 229910052739 hydrogen Inorganic materials 0.000 claims abstract description 24
- 239000001257 hydrogen Substances 0.000 claims abstract description 24
- 238000006243 chemical reaction Methods 0.000 claims abstract description 23
- 238000001027 hydrothermal synthesis Methods 0.000 claims abstract description 21
- 238000004519 manufacturing process Methods 0.000 claims abstract description 20
- 238000000034 method Methods 0.000 claims abstract description 15
- PYWVYCXTNDRMGF-UHFFFAOYSA-N rhodamine B Chemical compound [Cl-].C=12C=CC(=[N+](CC)CC)C=C2OC2=CC(N(CC)CC)=CC=C2C=1C1=CC=CC=C1C(O)=O PYWVYCXTNDRMGF-UHFFFAOYSA-N 0.000 claims abstract description 13
- 229940043267 rhodamine b Drugs 0.000 claims abstract description 13
- 235000015393 sodium molybdate Nutrition 0.000 claims abstract description 11
- 239000011684 sodium molybdate Substances 0.000 claims abstract description 11
- TVXXNOYZHKPKGW-UHFFFAOYSA-N sodium molybdate (anhydrous) Chemical compound [Na+].[Na+].[O-][Mo]([O-])(=O)=O TVXXNOYZHKPKGW-UHFFFAOYSA-N 0.000 claims abstract description 11
- YUKQRDCYNOVPGJ-UHFFFAOYSA-N thioacetamide Chemical compound CC(N)=S YUKQRDCYNOVPGJ-UHFFFAOYSA-N 0.000 claims abstract description 11
- DLFVBJFMPXGRIB-UHFFFAOYSA-N thioacetamide Natural products CC(N)=O DLFVBJFMPXGRIB-UHFFFAOYSA-N 0.000 claims abstract description 11
- 239000012153 distilled water Substances 0.000 claims description 33
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 claims description 28
- 238000010438 heat treatment Methods 0.000 claims description 19
- 238000001035 drying Methods 0.000 claims description 14
- 239000011259 mixed solution Substances 0.000 claims description 14
- 239000002243 precursor Substances 0.000 claims description 14
- 239000000243 solution Substances 0.000 claims description 14
- 239000000725 suspension Substances 0.000 claims description 14
- 238000005406 washing Methods 0.000 claims description 14
- 238000001816 cooling Methods 0.000 claims description 12
- 238000003756 stirring Methods 0.000 claims description 8
- 239000003054 catalyst Substances 0.000 claims description 7
- 230000001105 regulatory effect Effects 0.000 claims description 7
- 238000006731 degradation reaction Methods 0.000 claims description 4
- -1 polytetrafluoroethylene Polymers 0.000 claims description 2
- 229920001343 polytetrafluoroethylene Polymers 0.000 claims description 2
- 239000004810 polytetrafluoroethylene Substances 0.000 claims description 2
- 230000000630 rising effect Effects 0.000 claims description 2
- 238000005303 weighing Methods 0.000 claims description 2
- 239000002135 nanosheet Substances 0.000 abstract description 8
- 238000013033 photocatalytic degradation reaction Methods 0.000 abstract description 7
- 239000002994 raw material Substances 0.000 abstract description 5
- 238000000926 separation method Methods 0.000 abstract description 5
- 230000005012 migration Effects 0.000 abstract description 4
- 238000013508 migration Methods 0.000 abstract description 4
- 238000004134 energy conservation Methods 0.000 abstract description 3
- 238000001354 calcination Methods 0.000 abstract description 2
- 230000003197 catalytic effect Effects 0.000 abstract description 2
- 238000005265 energy consumption Methods 0.000 abstract description 2
- 230000007613 environmental effect Effects 0.000 abstract description 2
- 231100000252 nontoxic Toxicity 0.000 abstract description 2
- 230000003000 nontoxic effect Effects 0.000 abstract description 2
- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical compound [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 description 7
- 238000002441 X-ray diffraction Methods 0.000 description 7
- 229910052799 carbon Inorganic materials 0.000 description 6
- 238000000354 decomposition reaction Methods 0.000 description 6
- 238000010586 diagram Methods 0.000 description 5
- 230000000694 effects Effects 0.000 description 4
- OKKJLVBELUTLKV-UHFFFAOYSA-N Methanol Chemical compound OC OKKJLVBELUTLKV-UHFFFAOYSA-N 0.000 description 3
- 238000003917 TEM image Methods 0.000 description 3
- 239000003795 chemical substances by application Substances 0.000 description 3
- 230000018109 developmental process Effects 0.000 description 3
- CURLTUGMZLYLDI-UHFFFAOYSA-N Carbon dioxide Chemical compound O=C=O CURLTUGMZLYLDI-UHFFFAOYSA-N 0.000 description 2
- 239000002131 composite material Substances 0.000 description 2
- JVTAAEKCZFNVCJ-UHFFFAOYSA-N lactic acid Chemical compound CC(O)C(O)=O JVTAAEKCZFNVCJ-UHFFFAOYSA-N 0.000 description 2
- 239000002064 nanoplatelet Substances 0.000 description 2
- 229910000510 noble metal Inorganic materials 0.000 description 2
- 238000013032 photocatalytic reaction Methods 0.000 description 2
- 230000009467 reduction Effects 0.000 description 2
- 230000004044 response Effects 0.000 description 2
- 238000001132 ultrasonic dispersion Methods 0.000 description 2
- 239000003403 water pollutant Substances 0.000 description 2
- 239000004809 Teflon Substances 0.000 description 1
- 229920006362 Teflon® Polymers 0.000 description 1
- 229910010413 TiO 2 Inorganic materials 0.000 description 1
- GSEJCLTVZPLZKY-UHFFFAOYSA-N Triethanolamine Chemical compound OCCN(CCO)CCO GSEJCLTVZPLZKY-UHFFFAOYSA-N 0.000 description 1
- 238000013019 agitation Methods 0.000 description 1
- 230000009286 beneficial effect Effects 0.000 description 1
- 230000005540 biological transmission Effects 0.000 description 1
- 230000033558 biomineral tissue development Effects 0.000 description 1
- 230000015572 biosynthetic process Effects 0.000 description 1
- 239000001569 carbon dioxide Substances 0.000 description 1
- 229910002092 carbon dioxide Inorganic materials 0.000 description 1
- 230000015556 catabolic process Effects 0.000 description 1
- 238000003421 catalytic decomposition reaction Methods 0.000 description 1
- 150000001875 compounds Chemical class 0.000 description 1
- 238000010276 construction Methods 0.000 description 1
- 238000005516 engineering process Methods 0.000 description 1
- 239000003344 environmental pollutant Substances 0.000 description 1
- 238000003912 environmental pollution Methods 0.000 description 1
- 229910021389 graphene Inorganic materials 0.000 description 1
- 230000036541 health Effects 0.000 description 1
- 239000004310 lactic acid Substances 0.000 description 1
- 235000014655 lactic acid Nutrition 0.000 description 1
- 230000031700 light absorption Effects 0.000 description 1
- 238000011068 loading method Methods 0.000 description 1
- 239000002086 nanomaterial Substances 0.000 description 1
- 231100000956 nontoxicity Toxicity 0.000 description 1
- 239000002957 persistent organic pollutant Substances 0.000 description 1
- 238000007146 photocatalysis Methods 0.000 description 1
- 231100000719 pollutant Toxicity 0.000 description 1
- 230000008569 process Effects 0.000 description 1
- 238000001878 scanning electron micrograph Methods 0.000 description 1
- 238000004626 scanning electron microscopy Methods 0.000 description 1
- 239000004065 semiconductor Substances 0.000 description 1
- 239000000126 substance Substances 0.000 description 1
- 238000003786 synthesis reaction Methods 0.000 description 1
- 229910052723 transition metal Inorganic materials 0.000 description 1
- 150000003624 transition metals Chemical class 0.000 description 1
- 238000004627 transmission electron microscopy Methods 0.000 description 1
- 239000002351 wastewater Substances 0.000 description 1
Classifications
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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
-
- B01J35/39—
-
- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01B—NON-METALLIC ELEMENTS; COMPOUNDS THEREOF; METALLOIDS OR COMPOUNDS THEREOF NOT COVERED BY SUBCLASS C01C
- C01B3/00—Hydrogen; Gaseous mixtures containing hydrogen; Separation of hydrogen from mixtures containing it; Purification of hydrogen
- C01B3/02—Production of hydrogen or of gaseous mixtures containing a substantial proportion of hydrogen
- C01B3/04—Production of hydrogen or of gaseous mixtures containing a substantial proportion of hydrogen by decomposition of inorganic compounds, e.g. ammonia
- C01B3/042—Decomposition of water
-
- C—CHEMISTRY; METALLURGY
- C02—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
- C02F—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
- C02F1/00—Treatment of water, waste water, or sewage
- C02F1/30—Treatment of water, waste water, or sewage by irradiation
-
- C—CHEMISTRY; METALLURGY
- C02—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
- C02F—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
- C02F2101/00—Nature of the contaminant
- C02F2101/30—Organic compounds
- C02F2101/34—Organic compounds containing oxygen
-
- C—CHEMISTRY; METALLURGY
- C02—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
- C02F—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
- C02F2101/00—Nature of the contaminant
- C02F2101/30—Organic compounds
- C02F2101/36—Organic compounds containing halogen
-
- C—CHEMISTRY; METALLURGY
- C02—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
- C02F—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
- C02F2101/00—Nature of the contaminant
- C02F2101/30—Organic compounds
- C02F2101/38—Organic compounds containing nitrogen
-
- C—CHEMISTRY; METALLURGY
- C02—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
- C02F—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
- C02F2305/00—Use of specific compounds during water treatment
- C02F2305/10—Photocatalysts
-
- Y—GENERAL TAGGING OF NEW TECHNOLOGICAL DEVELOPMENTS; GENERAL TAGGING OF CROSS-SECTIONAL TECHNOLOGIES SPANNING OVER SEVERAL SECTIONS OF THE IPC; TECHNICAL SUBJECTS COVERED BY FORMER USPC CROSS-REFERENCE ART COLLECTIONS [XRACs] AND DIGESTS
- Y02—TECHNOLOGIES OR APPLICATIONS FOR MITIGATION OR ADAPTATION AGAINST CLIMATE CHANGE
- Y02E—REDUCTION OF GREENHOUSE GAS [GHG] EMISSIONS, RELATED TO ENERGY GENERATION, TRANSMISSION OR DISTRIBUTION
- Y02E60/00—Enabling technologies; Technologies with a potential or indirect contribution to GHG emissions mitigation
- Y02E60/30—Hydrogen technology
- Y02E60/36—Hydrogen production from non-carbon containing sources, e.g. by water electrolysis
Abstract
The invention relates to a preparation method and application of a 2D/3D structured molybdenum disulfide/indium oxide nanocomposite, which uses indium acetate, urea, thioacetamide and sodium molybdate as raw materials to prepare In with a 3D structure by a hydrothermal-calcining method 2 O 3 Nanocubes, and then MoS with 2D structure by simple hydrothermal method 2 Nanosheets loaded to In 2 O 3 2D/3D structure MoS with low cost and high catalytic activity is synthesized on the surface of nanocube 2 /In 2 O 3 A nanocomposite. By In 2 O 3 Characteristics of material energy band structure and MoS 2 The material can accelerate the photo-generated electron-hole separation/migration rate, and the constructed MoS 2 /In 2 O 3 The nanocomposite can be used for high-efficiency photocatalytic water splitting to prepare hydrogen and coupled photocatalytic degradation rhodamine B reaction. The raw materials of the invention have the advantages of low price, simple preparation and the like, reduce energy consumption and reaction cost, are convenient for mass production, are nontoxic and harmless, and meet the requirements of energy conservation, environmental protection and sustainable development.
Description
Technical Field
The invention belongs to the technical field of nano material synthesis, and utilizes a simple hydrothermal method to synthesize molybdenum disulfide (MoS) with a 2D/3D structure 2 ) Indium oxide (In) 2 O 3 ) Nanocomposite materialThe material can be used for high-efficiency photocatalytic decomposition of water to prepare hydrogen and coupled photocatalytic degradation of rhodamine B.
Background
Global energy crisis and environmental pollution are two major problems facing the world today. At present, the photocatalysis technology has the advantages of energy conservation, cleanness, no pollution and the like, and is widely concerned in solving the problems of energy and environment. Generally, in the hydrogen production process by photocatalytic decomposition of water, sacrificial agents such as methanol, triethanolamine, lactic acid and the like are required to be added to accelerate the consumption of photo-generated holes, so that photo-generated electrons are efficiently involved in the hydrogen production reaction. However, these non-renewable sacrificial agents are important chemical raw materials, and the use of them as sacrificial agents for photocatalytic hydrogen production reactions does not meet the requirements of sustainable development. On the other hand, organic dye wastewater represented by rhodamine B poses serious harm to the ecosystem and human health. Therefore, if the photocatalytic hydrogen production and the photocatalytic degradation of rhodamine B can be performed in one photocatalytic system, the problems of energy and environment caused by social development are likely to be solved.
Indium oxide (In) 2 O 3 ) The material is a typical n-type semiconductor material, has a band gap energy of about 2.8eV, and has the advantages of excellent photochemical stability, proper light absorption, no toxicity, no harm and the like, so that the material is widely applied to reactions such as photocatalytic water splitting for hydrogen production, photocatalytic degradation of organic pollutants, photocatalytic carbon dioxide reduction and the like. However, due to its photo-generated electron-hole separation, slow migration rate, single In 2 O 3 Materials generally exhibit low photocatalytic activity in photocatalytic reactions. Molybdenum disulfide (MoS) 2 ) Is a transition metal dihalide compound similar to a graphene two-dimensional structure, and is greatly concerned in photocatalytic reaction as a cocatalyst capable of replacing noble metal. For example: moS (MoS) 2 With TiO 2 The composite material can be constructed to remarkably improve the photocatalytic hydrogen production performance; moS (MoS) 2 With Cu 2 The O-constructed composite material can obviously accelerate the photocatalytic degradation of dye. However, moS of the current 2D/3D structure 2 /In 2 O 3 Nanocomposite construction and application thereof in photocatalytic hydrogen production by photocatalytic decomposition of water and coupled photocatalytic degradationThe related study of Jie Luodan Ming B has not been reported yet.
Disclosure of Invention
The object of the present invention is to provide MoS with 2D/3D structure 2 /In 2 O 3 Method for preparing nanocomposite and MoS with 2D/3D structure 2 /In 2 O 3 The nanocomposite is used for preparing hydrogen by photocatalytic decomposition of water and coupled with photocatalytic degradation of rhodamine B. The MoS 2 /In 2 O 3 The nano composite material has high catalytic activity, and achieves the purpose of removing water pollutants while preparing hydrogen.
The technical proposal of the invention
2D/3D structure MoS 2 /In 2 O 3 A method of preparing a nanocomposite comprising the steps of:
step 1: a certain amount of indium acetate and urea are weighed and respectively placed in 15mL and 20mL of distilled water, after stirring at room temperature to enable the indium acetate and the urea to be completely dissolved, the urea solution is dropwise added into the indium acetate solution by a suction pipe to form uniform mixed solution.
The molar ratio of the indium acetate to the urea is 1:12.8.
Step 2: transferring the mixed solution into an autoclave with a polytetrafluoroethylene lining with a certain volume, heating at a certain temperature for a certain time, performing hydrothermal reaction, after the autoclave is cooled to room temperature, centrifugally collecting white products, washing with distilled water and ethanol for 3 times respectively, and drying in an oven at 80 ℃ to obtain a precursor.
The volume of the autoclave is 50mL; the hydrothermal reaction temperature is 130 ℃ and the time is 12 hours.
Step 3: placing the precursor In a muffle furnace at room temperature, regulating a certain heating rate to perform heating reaction, and cooling the muffle furnace to room temperature after the reaction is finished to obtain In with a 3D structure 2 O 3 Nanocubes.
The heating rate is 2 ℃/min; the heating reaction temperature was 600℃for 2 hours.
Step 4: weighing a certain amount of In 2 O 3 Dispersing with ultrasonic wave in distilled water, adding a solutionAnd (3) quantitatively stirring sodium molybdate and thioacetamide by ultrasonic until the materials are completely dispersed to form uniform suspension.
The In is 2 O 3 The mass is 300mg; the molar ratio of sodium molybdate to thioacetamide is 1:5.
Step 5: transferring the suspension completely into a polytetrafluoroethylene-lined autoclave with a certain volume, heating at a certain temperature for a certain time, performing hydrothermal reaction, cooling the reacted autoclave to room temperature, centrifuging to collect samples, washing with distilled water and ethanol for 3 times respectively, drying in an oven at 80 ℃ to obtain MoS with a 2D/3D structure 2 /In 2 O 3 A nanocomposite.
The volume of the autoclave is 50mL; the hydrothermal reaction temperature is 210 ℃ and the time is 24 hours.
The beneficial effects of the invention are that
1. The invention utilizes MoS with 2D lamellar structure 2 The nanosheet material can effectively accelerate the photo-generated electron-hole separation/migration rate, replace the traditional noble metal Pt-based cocatalyst, and successfully construct the low-cost and high-catalytic-activity 2D/3D structure MoS 2 /In 2 O 3 A nanocomposite.
2. The invention utilizes In 2 O 3 The material has the characteristics of energy band structure (electrons generated by a conduction band can reduce water to produce hydrogen and holes generated by a valence band can oxidize pollutants), and the photocatalytic water decomposition hydrogen production reaction and the photocatalytic rhodamine B degradation reaction are cooperatively coupled, so that the purpose of removing water pollutants while preparing hydrogen is achieved.
3. The raw materials of the invention have the advantages of low price, simple preparation and the like, reduce energy consumption and reaction cost, are convenient for mass production, are nontoxic and harmless, and meet the requirements of energy conservation, environmental protection and sustainable development.
Drawings
The accompanying drawings, which are incorporated in and constitute a part of this specification, illustrate embodiments consistent with the invention and together with the description, serve to explain the principles of the invention.
FIG. 1A is a block diagram of the present invention according to example 1In 2 O 3 X-ray diffraction pattern (XRD) of nanocubes.
FIG. 1B is a MoS prepared in example 2 of the present invention 2 XRD pattern of nanoplatelets.
FIG. 1C shows MoS prepared in examples 3-6 of the present invention 2 /In 2 O 3 XRD pattern of nanocomposite.
FIG. 2A shows In prepared In example 1 of the present invention 2 O 3 Scanning Electron Microscope (SEM) images of nanocubes.
FIG. 2B is a MoS prepared in example 2 of the present invention 2 Transmission Electron Microscope (TEM) images of the nanoplatelets.
FIGS. 2C and 2D are graphs showing 10% MoS prepared in example 5 of the present invention 2 /In 2 O 3 TEM image of nanocomposite.
FIG. 3A shows In prepared In example 1 and example 5 of the present invention 2 O 3 Nanocubes and 10% mos 2 /In 2 O 3 Photoelectric diagram of nanocomposite.
FIG. 3B shows the In prepared In example 1 and example 5 of the present invention 2 O 3 Nanocubes and 10% mos 2 /In 2 O 3 Electrochemical impedance diagram of nanocomposite.
FIG. 4A shows the In prepared In example 1 and examples 3 to 6 of the present invention 2 O 3 Nanocubes and MoS 2 /In 2 O 3 A photo-catalytic decomposition water hydrogen production rate histogram of the nanocomposite.
FIG. 4B shows the In prepared In example 1 and examples 3-6 of the present invention 2 O 3 Nanocubes and MoS 2 /In 2 O 3 Overall organic carbon removal histogram of the photocatalytic degradation rhodamine B of the nanocomposite.
Specific embodiments of the present invention have been shown by way of the above drawings and will be described in more detail below. The drawings and the written description are not intended to limit the scope of the inventive concepts in any way, but rather to illustrate the inventive concepts to those skilled in the art by reference to the specific embodiments.
Detailed Description
The invention aims to provide a MoS with a 2D/3D structure 2 /In 2 O 3 The preparation method of the nanocomposite material uses the synthesized nanocomposite material as a catalyst for high-efficiency photocatalytic hydrogen production by water decomposition and coupled photocatalytic rhodamine B degradation reaction. The method uses indium acetate, urea, thioacetamide and sodium molybdate as raw materials, and prepares In with 3D structure by a hydrothermal-calcining method 2 O 3 Nanocubes, and then MoS with 2D structure by simple hydrothermal method 2 Nanosheets loaded to In 2 O 3 Nanometer cube surface, moS for constructing 2D/3D structure 2 /In 2 O 3 A nanocomposite.
The present invention will be described in detail with reference to the following examples, so that those skilled in the art can better understand the present invention, but the present invention is not limited to the following examples.
Example 1: preparation of In 2 O 3 Nanocubes
Step 1: 1.0948g of indium acetate and 2.8829g of urea are respectively weighed and placed in 15mL of distilled water and 20mL of distilled water, and after the indium acetate and the 2.8829g of urea are stirred at room temperature for 15min to be completely dissolved, the urea solution is dropwise added into the indium acetate solution by a suction pipe to form a uniform mixed solution.
Step 2: transferring the mixed solution into a 50mL polytetrafluoroethylene-lined autoclave, performing hydrothermal reaction for 12h at 130 ℃, after the autoclave is cooled to room temperature, centrifugally collecting a white product, washing with distilled water and ethanol for 3 times respectively, and drying in an oven at 80 ℃ to obtain a precursor.
Step 3: placing the precursor In a muffle furnace at room temperature, regulating the heating rate to be 2 ℃/min, heating at 600 ℃ for reaction for 2 hours, and cooling the muffle furnace to room temperature after the reaction is finished to obtain In with a 3D structure 2 O 3 Nanocubes.
Example 2: preparation of MoS 2 Nanosheets
Step 1: 0.3088g of sodium molybdate and 0.5635g of thioacetamide are weighed and placed in 35mL of distilled water, and the sodium molybdate and the thioacetamide are completely dispersed by ultrasonic stirring for 30min at room temperature to form a uniform suspension.
Step 2: transferring the suspension into 50mL polytetrafluoroethylene-lined autoclave, performing hydrothermal reaction at 210 ℃ for 24 hours, centrifuging to collect black products after the autoclave is cooled to room temperature, washing with distilled water and ethanol for 3 times respectively, and drying in an oven at 80 ℃ to obtain MoS with a 2D structure 2 A nano-sheet.
Example 3: preparation of 5% MoS 2 /In 2 O 3 Nanocomposite material
Step 1: 1.0948g of indium acetate and 2.8829g of urea are respectively weighed and placed in 15mL of distilled water and 20mL of distilled water, and after the indium acetate and the 2.8829g of urea are stirred at room temperature for 15min to be completely dissolved, the urea solution is dropwise added into the indium acetate solution by a suction pipe to form a uniform mixed solution.
Step 2: transferring the mixed solution into a 50mL polytetrafluoroethylene-lined autoclave, performing hydrothermal reaction for 12h at 130 ℃, after the autoclave is cooled to room temperature, centrifugally collecting a white product, washing with distilled water and ethanol for 3 times respectively, and drying in an oven at 80 ℃ to obtain a precursor.
Step 3: placing the precursor In a muffle furnace at room temperature, regulating the heating rate to be 2 ℃/min, heating at 600 ℃ for reaction for 2 hours, and cooling the muffle furnace to room temperature after the reaction is finished to obtain In with a 3D structure 2 O 3 Nanocubes.
Step 4: 300mg of In was weighed 2 O 3 Ultrasonic dispersing in 35mL distilled water, adding 0.0193g sodium molybdate and 0.0352g thioacetamide, ultrasonic stirring until the materials are completely dispersed, forming a uniform suspension.
Step 5: transferring the suspension completely into 50mL polytetrafluoroethylene-lined autoclave, performing hydrothermal reaction at 210 ℃ for 24 hours, cooling the autoclave to room temperature, centrifugally collecting the product, washing with distilled water and ethanol for 3 times respectively, and drying in an oven at 80 ℃ to obtain 5% MoS 2 /In 2 O 3 A nanocomposite.
Example 4: preparation of 7.5% MoS 2 /In 2 O 3 Nanocomposite material
Step 1: 1.0948g of indium acetate and 2.8829g of urea are respectively weighed and placed in 15mL of distilled water and 20mL of distilled water, and after the indium acetate and the 2.8829g of urea are stirred at room temperature for 15min to be completely dissolved, the urea solution is dropwise added into the indium acetate solution by a suction pipe to form a uniform mixed solution.
Step 2: transferring the mixed solution into a 50mL polytetrafluoroethylene-lined autoclave, performing hydrothermal reaction for 12h at 130 ℃, after the autoclave is cooled to room temperature, centrifugally collecting a white product, washing with distilled water and ethanol for 3 times respectively, and drying in an oven at 80 ℃ to obtain a precursor.
Step 3: placing the precursor In a muffle furnace at room temperature, regulating the heating rate to be 2 ℃/min, heating at 600 ℃ for reaction for 2 hours, and cooling the muffle furnace to room temperature after the reaction is finished to obtain In with a 3D structure 2 O 3 Nanocubes.
Step 4: 300mg of In was weighed 2 O 3 Ultrasonic dispersing in 35mL distilled water, adding 0.0289g sodium molybdate and 0.0528g thioacetamide, ultrasonic stirring until the materials are completely dispersed, and forming uniform suspension.
Step 5: transferring the suspension completely into 50mL polytetrafluoroethylene-lined autoclave, performing hydrothermal reaction at 210 ℃ for 24 hours, cooling the autoclave to room temperature, centrifugally collecting the product, washing with distilled water and ethanol for 3 times respectively, and drying in an oven at 80 ℃ to obtain 7.5% MoS 2 /In 2 O 3 A nanocomposite.
Example 5: preparation of 10% MoS 2 /In 2 O 3 Nanocomposite material
Step 1: 1.0948g of indium acetate and 2.8829g of urea are respectively weighed and placed in 15mL of distilled water and 20mL of distilled water, and after the indium acetate and the 2.8829g of urea are stirred at room temperature for 15min to be completely dissolved, the urea solution is dropwise added into the indium acetate solution by a suction pipe to form a uniform mixed solution.
Step 2: transferring the mixed solution into a 50mL polytetrafluoroethylene-lined autoclave, performing hydrothermal reaction for 12h at 130 ℃, after the autoclave is cooled to room temperature, centrifugally collecting a white product, washing with distilled water and ethanol for 3 times respectively, and drying in an oven at 80 ℃ to obtain a precursor.
Step 3: placing the precursor in a muffle furnace at room temperatureHeating and reacting for 2 hours at 600 ℃ with the temperature rising rate regulated and controlled to be 2 ℃/min, and obtaining In with a 3D structure after the reaction is finished and the muffle furnace is cooled to room temperature 2 O 3 Nanocubes.
Step 4: 300mg of In was weighed 2 O 3 Ultrasonic dispersion in 35mL distilled water followed by addition of 0.0386g sodium molybdate and 0.0704g thioacetamide, followed by ultrasonic agitation until the material is completely dispersed, to form a uniform suspension.
Step 5: transferring the suspension completely into 50mL polytetrafluoroethylene-lined autoclave, performing hydrothermal reaction at 210 ℃ for 24 hours, cooling the autoclave to room temperature, centrifugally collecting the product, washing with distilled water and ethanol for 3 times respectively, and drying in an oven at 80 ℃ to obtain 10% MoS 2 /In 2 O 3 A nanocomposite.
Example 6: preparation of 12.5% MoS 2 /In 2 O 3 Nanocomposite material
Step 1: 1.0948g of indium acetate and 2.8829g of urea are respectively weighed and placed in 15mL of distilled water and 20mL of distilled water, and after the indium acetate and the 2.8829g of urea are stirred at room temperature for 15min to be completely dissolved, the urea solution is dropwise added into the indium acetate solution by a suction pipe to form a uniform mixed solution.
Step 2: transferring the mixed solution into a 50mL polytetrafluoroethylene-lined autoclave, performing hydrothermal reaction for 12h at 130 ℃, after the autoclave is cooled to room temperature, centrifugally collecting a white product, washing with distilled water and ethanol for 3 times respectively, and drying in an oven at 80 ℃ to obtain a precursor.
Step 3: placing the precursor In a muffle furnace at room temperature, regulating the heating rate to be 2 ℃/min, heating at 600 ℃ for reaction for 2 hours, and cooling the muffle furnace to room temperature after the reaction is finished to obtain In with a 3D structure 2 O 3 Nanocubes.
Step 4: 300mg of In was weighed 2 O 3 Ultrasonic dispersion in 35mL distilled water, then adding 0.0483g sodium molybdate and 0.0880g thioacetamide, ultrasonic stirring until the materials are completely dispersed, forming uniform suspension.
Step 5: the suspension was transferred completely to a 50mL teflon lined autoclaveIn the method, hydrothermal reaction is carried out for 24 hours at 210 ℃, after the autoclave is cooled to room temperature, products are centrifugally collected, distilled water and ethanol are respectively used for washing for 3 times, and drying is carried out in an oven at 80 ℃ to obtain 12.5 percent MoS 2 /In 2 O 3 A nanocomposite.
The crystalline phase structure of the catalyst in the present invention is determined by X-ray diffraction (XRD). The XRD patterns of fig. 1A, 1B and 1C can be seen: in (In) 2 O 3 Nanocubes and MoS 2 The characteristic diffraction peaks of the nano-sheet material are consistent with the standard cards JCPDS No.71-2194 and JCPDS No.37-1492, which show that the pure phase In 2 O 3 And MoS 2 Have been successfully prepared; and at MoS 2 /In 2 O 3 In nanocomposite material, due to MoS 2 The loading content was relatively low and all nanocomposites exhibited In 2 O 3 Is not observed by the characteristic XRD diffraction peaks of (2) 2 Is a characteristic peak of (2).
The surface morphology and microstructure of the catalyst in the present invention are determined by Scanning Electron Microscopy (SEM) and Transmission Electron Microscopy (TEM). The SEM image of fig. 2A can be seen: pure phase In prepared 2 O 3 The material has an obvious 3D cube structure; the TEM image of fig. 2B can be seen: pure phase MoS prepared 2 The material has an obvious 2D nano-sheet structure; the TEM images of fig. 2C and 2D can be seen: moS at a mass ratio of 10% 2 Loaded In 2 O 3 After the surface, 10% MoS was prepared 2 /In 2 O 3 Nanocomposite materials still exhibit phase-purity In 2 O 3 MoS of a two-dimensional layered structure is uniformly distributed on the surface of the nano-cube structure 2 A nano-sheet. This result indicates MoS of unique 2D/3D structure 2 /In 2 O 3 Nanocomposite materials have been successfully synthesized.
The photo-generated electron-hole separation/transport rate of the catalyst in the present invention is determined by the photocurrent response and electrochemical impedance. The photocurrent response diagram of fig. 3A can be seen: with pure phase In 2 O 3 Compared with the material, 10% MoS of the material is prepared 2 /In 2 O 3 Nanocomposite has significant improvementsIs a photocurrent density of (a); the electrochemical impedance diagram of fig. 3B can be seen: with pure phase In 2 O 3 Compared with the material, 10% MoS of the material is prepared 2 /In 2 O 3 Nanocomposite materials have significantly reduced impedance semicircle. This result indicates MoS 2 Can greatly improve In as a cocatalyst 2 O 3 Photo-generated electron-hole separation/migration rate of the material.
The photocatalytic performance of the catalyst is determined by photocatalytic hydrogen production by photocatalytic water splitting and photocatalytic rhodamine B reduction. The hydrogen production rate histogram of fig. 4A can be seen: pure phase In 2 O 3 The material shows very low photocatalytic hydrogen production activity, and the prepared MoS 2 /In 2 O 3 The nano composite material can obviously improve the photocatalytic hydrogen production activity. Wherein, 10% MoS 2 /In 2 O 3 The nanocomposite material shows the highest hydrogen production activity (15.5 mu mol/g/h) compared with pure-phase In 2 O 3 The material was 77.5 times higher. The rhodamine B total organic carbon removal histogram of fig. 4B can be seen: pure phase In 2 O 3 The material has the lowest total organic carbon removal rate, and the synthesized MoS 2 /In 2 O 3 The removal rate of the total organic carbon of the nano composite material is greatly improved. Wherein, 10% MoS 2 /In 2 O 3 The nanocomposite had the highest total organic carbon removal (63.1%) with approximately pure phase In 2 O 3 12 times the material. Further, as can be seen from fig. 4A and 4B, the hydrogen production rate of the catalyst is directly proportional to both the total organic carbon removal rate of rhodamine B. This result indicates the MoS produced 2 /In 2 O 3 The nano composite material can obviously accelerate the degradation and mineralization process of rhodamine B molecules while obviously improving the hydrogen production reaction by photocatalytic water splitting.
Claims (6)
1. A preparation method of a 2D/3D structured molybdenum disulfide/indium oxide nanocomposite is characterized by comprising the following steps: the method comprises the following steps:
step 1: weighing a certain amount of indium acetate and urea, respectively placing the indium acetate and the urea in 15mL and 20mL distilled water, stirring at room temperature to completely dissolve the indium acetate and the urea, and dropwise dripping the urea solution into the indium acetate solution by using a suction pipe to form a uniform mixed solution;
step 2: transferring the mixed solution into an autoclave with a polytetrafluoroethylene lining with a certain volume, heating at a certain temperature for a certain time, performing hydrothermal reaction, cooling the autoclave to room temperature, centrifuging to collect white product, washing with distilled water and ethanol for 3 times respectively, and standing at 80 deg.f o Drying in a baking oven to obtain a precursor;
step 3: placing the precursor In a muffle furnace at room temperature, regulating a certain heating rate to perform heating reaction, and cooling the muffle furnace to room temperature after the reaction is finished to obtain In with a 3D structure 2 O 3 A nanocube;
step 4: weigh 300mg In 2 O 3 Ultrasonically dispersing in distilled water with a certain volume, then adding 0.0386g sodium molybdate and 0.0704g thioacetamide, and forming uniform suspension after ultrasonic stirring until the materials are completely dispersed;
step 5: transferring the suspension completely into a polytetrafluoroethylene-lined autoclave with a certain volume, heating at a certain temperature for a certain time, performing hydrothermal reaction, cooling the autoclave to room temperature, centrifuging to collect sample, washing with distilled water and ethanol for 3 times, respectively, and collecting sample at 80 o Drying in a C oven to finally obtain the MoS with the 2D/3D structure 2 /In 2 O 3 A nanocomposite.
2. The method for preparing the 2D/3D structured molybdenum disulfide/indium oxide nanocomposite material according to claim 1, wherein the method comprises the following steps: the molar ratio of the indium acetate to the urea in the step 1 is 1:12.8.
3. The method for preparing the 2D/3D structured molybdenum disulfide/indium oxide nanocomposite material according to claim 1, wherein the method comprises the following steps: the autoclave volume of step 2 was 50mL; the hydrothermal reaction temperature was 130℃and the time was 12h.
4. According to the weightsThe method for preparing the 2D/3D structured molybdenum disulfide/indium oxide nanocomposite material as claimed in claim 1, which is characterized in that: the temperature rising rate in the step 3 is 2 o C/min; the heating reaction temperature was 600 o C. Time was 2h.
5. The method for preparing the 2D/3D structured molybdenum disulfide/indium oxide nanocomposite material according to claim 1, wherein the method comprises the following steps: the autoclave volume of step 5 was 50mL; the hydrothermal reaction temperature is 210 o C. The time was 24h.
6. The 2D/3D structured molybdenum disulfide/indium oxide nanocomposite prepared by the preparation method of any one of claims 1-5 is used as a catalyst for high-efficiency photocatalytic water splitting hydrogen production coupled rhodamine B degradation reaction.
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