CN111298786B - Micrometer hexagonal prism MoO 3-x Preparation method of photocatalytic material - Google Patents
Micrometer hexagonal prism MoO 3-x Preparation method of photocatalytic material Download PDFInfo
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- 239000000463 material Substances 0.000 title claims abstract description 25
- 230000001699 photocatalysis Effects 0.000 title claims abstract description 20
- 238000002360 preparation method Methods 0.000 title claims abstract description 8
- 238000000034 method Methods 0.000 claims abstract description 12
- WQZGKKKJIJFFOK-GASJEMHNSA-N Glucose Natural products OC[C@H]1OC(O)[C@H](O)[C@@H](O)[C@@H]1O WQZGKKKJIJFFOK-GASJEMHNSA-N 0.000 claims abstract description 10
- 239000008103 glucose Substances 0.000 claims abstract description 10
- 238000003756 stirring Methods 0.000 claims abstract description 10
- 238000001035 drying Methods 0.000 claims abstract description 5
- 238000005406 washing Methods 0.000 claims abstract description 5
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Chemical compound O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims description 14
- 239000008367 deionised water Substances 0.000 claims description 13
- 229910021641 deionized water Inorganic materials 0.000 claims description 13
- 239000002244 precipitate Substances 0.000 claims description 8
- 229920002538 Polyethylene Glycol 20000 Polymers 0.000 claims description 6
- 238000006243 chemical reaction Methods 0.000 claims description 4
- 239000000843 powder Substances 0.000 claims description 3
- 239000000725 suspension Substances 0.000 claims description 3
- 239000007788 liquid Substances 0.000 claims description 2
- 238000002156 mixing Methods 0.000 claims description 2
- QVGXLLKOCUKJST-UHFFFAOYSA-N atomic oxygen Chemical compound [O] QVGXLLKOCUKJST-UHFFFAOYSA-N 0.000 abstract description 10
- 239000001301 oxygen Substances 0.000 abstract description 10
- 229910052760 oxygen Inorganic materials 0.000 abstract description 10
- 239000000969 carrier Substances 0.000 abstract description 6
- 238000000926 separation method Methods 0.000 abstract description 6
- 238000005215 recombination Methods 0.000 abstract description 5
- 230000006798 recombination Effects 0.000 abstract description 5
- 239000003638 chemical reducing agent Substances 0.000 abstract description 4
- 238000007146 photocatalysis Methods 0.000 abstract description 4
- 230000008569 process Effects 0.000 abstract description 4
- 239000002994 raw material Substances 0.000 abstract description 3
- 230000009467 reduction Effects 0.000 abstract description 3
- 230000004044 response Effects 0.000 abstract description 3
- 230000002378 acidificating effect Effects 0.000 abstract description 2
- 238000011065 in-situ storage Methods 0.000 abstract description 2
- 230000004298 light response Effects 0.000 abstract description 2
- 239000007864 aqueous solution Substances 0.000 abstract 1
- 239000002131 composite material Substances 0.000 abstract 1
- 229910000476 molybdenum oxide Inorganic materials 0.000 description 33
- 239000011941 photocatalyst Substances 0.000 description 4
- 229910010413 TiO 2 Inorganic materials 0.000 description 3
- 239000003054 catalyst Substances 0.000 description 3
- 230000007613 environmental effect Effects 0.000 description 3
- 238000001228 spectrum Methods 0.000 description 3
- CIWBSHSKHKDKBQ-JLAZNSOCSA-N Ascorbic acid Chemical compound OC[C@H](O)[C@H]1OC(=O)C(O)=C1O CIWBSHSKHKDKBQ-JLAZNSOCSA-N 0.000 description 2
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 description 2
- KFZMGEQAYNKOFK-UHFFFAOYSA-N Isopropanol Chemical compound CC(C)O KFZMGEQAYNKOFK-UHFFFAOYSA-N 0.000 description 2
- 230000004075 alteration Effects 0.000 description 2
- 230000015556 catabolic process Effects 0.000 description 2
- 230000007547 defect Effects 0.000 description 2
- 238000006731 degradation reaction Methods 0.000 description 2
- 230000031700 light absorption Effects 0.000 description 2
- JKQOBWVOAYFWKG-UHFFFAOYSA-N molybdenum trioxide Chemical compound O=[Mo](=O)=O JKQOBWVOAYFWKG-UHFFFAOYSA-N 0.000 description 2
- 239000002957 persistent organic pollutant Substances 0.000 description 2
- 238000005424 photoluminescence Methods 0.000 description 2
- 238000011160 research Methods 0.000 description 2
- 239000004065 semiconductor Substances 0.000 description 2
- 238000006467 substitution reaction Methods 0.000 description 2
- 238000003911 water pollution Methods 0.000 description 2
- QGZKDVFQNNGYKY-UHFFFAOYSA-O Ammonium Chemical compound [NH4+] QGZKDVFQNNGYKY-UHFFFAOYSA-O 0.000 description 1
- ZZZCUOFIHGPKAK-UHFFFAOYSA-N D-erythro-ascorbic acid Natural products OCC1OC(=O)C(O)=C1O ZZZCUOFIHGPKAK-UHFFFAOYSA-N 0.000 description 1
- UFHFLCQGNIYNRP-UHFFFAOYSA-N Hydrogen Chemical compound [H][H] UFHFLCQGNIYNRP-UHFFFAOYSA-N 0.000 description 1
- HBBGRARXTFLTSG-UHFFFAOYSA-N Lithium ion Chemical compound [Li+] HBBGRARXTFLTSG-UHFFFAOYSA-N 0.000 description 1
- 229910015711 MoOx Inorganic materials 0.000 description 1
- ZOKXTWBITQBERF-UHFFFAOYSA-N Molybdenum Chemical compound [Mo] ZOKXTWBITQBERF-UHFFFAOYSA-N 0.000 description 1
- 229930003268 Vitamin C Natural products 0.000 description 1
- 238000010521 absorption reaction Methods 0.000 description 1
- 238000000137 annealing Methods 0.000 description 1
- 239000012300 argon atmosphere Substances 0.000 description 1
- 230000003197 catalytic effect Effects 0.000 description 1
- 239000010406 cathode material Substances 0.000 description 1
- 150000001875 compounds Chemical class 0.000 description 1
- 230000002950 deficient Effects 0.000 description 1
- 230000000593 degrading effect Effects 0.000 description 1
- 238000011161 development Methods 0.000 description 1
- 239000000975 dye Substances 0.000 description 1
- 238000001941 electron spectroscopy Methods 0.000 description 1
- 238000005265 energy consumption Methods 0.000 description 1
- 238000004146 energy storage Methods 0.000 description 1
- 238000005516 engineering process Methods 0.000 description 1
- 238000003912 environmental pollution Methods 0.000 description 1
- 230000005284 excitation Effects 0.000 description 1
- 239000007789 gas Substances 0.000 description 1
- 239000001257 hydrogen Substances 0.000 description 1
- 229910052739 hydrogen Inorganic materials 0.000 description 1
- 229910001416 lithium ion Inorganic materials 0.000 description 1
- 238000004519 manufacturing process Methods 0.000 description 1
- 239000000203 mixture Substances 0.000 description 1
- 230000004048 modification Effects 0.000 description 1
- 238000012986 modification Methods 0.000 description 1
- 239000003607 modifier Substances 0.000 description 1
- 229910052750 molybdenum Inorganic materials 0.000 description 1
- 239000011733 molybdenum Substances 0.000 description 1
- 231100000956 nontoxicity Toxicity 0.000 description 1
- GEVPUGOOGXGPIO-UHFFFAOYSA-N oxalic acid;dihydrate Chemical compound O.O.OC(=O)C(O)=O GEVPUGOOGXGPIO-UHFFFAOYSA-N 0.000 description 1
- PQQKPALAQIIWST-UHFFFAOYSA-N oxomolybdenum Chemical compound [Mo]=O PQQKPALAQIIWST-UHFFFAOYSA-N 0.000 description 1
- 238000011056 performance test Methods 0.000 description 1
- 238000013032 photocatalytic reaction Methods 0.000 description 1
- 238000001556 precipitation Methods 0.000 description 1
- 239000002243 precursor Substances 0.000 description 1
- 230000035484 reaction time Effects 0.000 description 1
- 239000010865 sewage Substances 0.000 description 1
- 239000002904 solvent Substances 0.000 description 1
- 238000001179 sorption measurement Methods 0.000 description 1
- 230000003595 spectral effect Effects 0.000 description 1
- 238000004528 spin coating Methods 0.000 description 1
- 239000011232 storage material Substances 0.000 description 1
- 239000000126 substance Substances 0.000 description 1
- 238000012360 testing method Methods 0.000 description 1
- 229910052723 transition metal Inorganic materials 0.000 description 1
- 235000019154 vitamin C Nutrition 0.000 description 1
- 239000011718 vitamin C Substances 0.000 description 1
Classifications
-
- B01J35/39—
-
- 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
- B01J23/00—Catalysts comprising metals or metal oxides or hydroxides, not provided for in group B01J21/00
- B01J23/16—Catalysts comprising metals or metal oxides or hydroxides, not provided for in group B01J21/00 of arsenic, antimony, bismuth, vanadium, niobium, tantalum, polonium, chromium, molybdenum, tungsten, manganese, technetium or rhenium
- B01J23/24—Chromium, molybdenum or tungsten
- B01J23/28—Molybdenum
-
- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01G—COMPOUNDS CONTAINING METALS NOT COVERED BY SUBCLASSES C01D OR C01F
- C01G39/00—Compounds of molybdenum
- C01G39/02—Oxides; Hydroxides
-
- 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
- C09—DYES; PAINTS; POLISHES; NATURAL RESINS; ADHESIVES; COMPOSITIONS NOT OTHERWISE PROVIDED FOR; APPLICATIONS OF MATERIALS NOT OTHERWISE PROVIDED FOR
- C09K—MATERIALS FOR MISCELLANEOUS APPLICATIONS, NOT PROVIDED FOR ELSEWHERE
- C09K11/00—Luminescent, e.g. electroluminescent, chemiluminescent materials
- C09K11/08—Luminescent, e.g. electroluminescent, chemiluminescent materials containing inorganic luminescent materials
- C09K11/67—Luminescent, e.g. electroluminescent, chemiluminescent materials containing inorganic luminescent materials containing refractory metals
- C09K11/68—Luminescent, e.g. electroluminescent, chemiluminescent materials containing inorganic luminescent materials containing refractory metals containing chromium, molybdenum or tungsten
- C09K11/681—Chalcogenides
-
- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01P—INDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS
- C01P2004/00—Particle morphology
- C01P2004/01—Particle morphology depicted by an image
- C01P2004/03—Particle morphology depicted by an image obtained by SEM
-
- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01P—INDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS
- C01P2004/00—Particle morphology
- C01P2004/30—Particle morphology extending in three dimensions
- C01P2004/40—Particle morphology extending in three dimensions prism-like
-
- 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
-
- 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
- C02F2101/308—Dyes; Colorants; Fluorescent agents
-
- 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
Abstract
Micrometer hexagonal prism MoO 3‑x A preparation method of a photocatalytic material belongs to the technical field of photocatalytic materials. The invention reduces MoO by glucose 3 MoO with oxygen-enriched vacancies on the surface is prepared 3‑x Photocatalytic material. In particular to a method for preparing a composite material by Na 2 MoO 4 ·2H 2 O reacts with HCl, glucose is taken as a reducing agent, stirring is carried out at normal temperature or low temperature, and finally, the MoO with oxygen-enriched vacancies on the surface is obtained through washing and drying 3‑x A micro hexagonal prism material. The invention is directed to MoO 3 The forbidden band width is wider, the response to visible light is weak, and MoO is realized in the photocatalysis process 3 The hole-electron pair recombination rate is high, and the separation efficiency of photo-generated carriers is low, and Na is adopted 2 MoO 4 ·2H 2 O is used as a raw material, glucose is used as a reducing agent, and MoO with oxygen-enriched vacancies on the surface is prepared by an in-situ reduction method in an acidic aqueous solution 3‑x The material narrows the forbidden bandwidth of the material, has wider visible light response range, promotes the separation efficiency of photon-generated carriers, and improves the photocatalysis performance of the material.
Description
Technical Field
The invention relates to a micron hexagonal prism MoO 3-x A preparation method of a photocatalytic material belongs to the technical field of photocatalytic materials, and particularly relates to a photocatalytic materialIs prepared by the preparation method of (1). The method is technically characterized by using Na 2 MoO 4 ·2H 2 O is used as a raw material, glucose reducer, and MoO with oxygen-enriched vacancies on the surface is prepared by adopting an in-situ reduction method under an acidic condition 3-x Photocatalytic material.
Background
With the continuous development of social economy, environmental pollution is a great concern, and meanwhile, people also put forward higher requirements on environmental quality, so that environmental protection and treatment problems are receiving more and more attention.
Organic dyes are important factors causing water pollution, and in recent years, a method for catalytically degrading organic pollutants in water by using a photocatalyst becomes an important means in the field of water pollution treatment. Compared with the traditional sewage treatment such as adsorption and precipitation, the photocatalysis method has the advantages of simple process, low energy consumption and the like, and can lead most of organic matters which are difficult to degrade at normal temperature and normal pressure to be oxidized and decomposed into CO 2 And H 2 O。
At present, more researches are carried out, and the photocatalyst with more mature technology is nano TiO 2 The photocatalyst has the advantages of high catalytic activity, good thermal stability, low price, no toxicity and the like. But due to TiO 2 The forbidden bandwidth of (2) is narrow (3.2 eV), the spectral absorption threshold is 387nm, and only the ultraviolet light part of the solar spectrum can be utilized. In addition, tiO 2 The electron-hole recombination rate generated by excitation is high, so that the light quantum efficiency is low, and the application range of the self-inherent defect is greatly limited. To solve this problem, researchers have desired to find other new semiconductor catalysts to replace or modify TiO 2 。
Molybdenum is a typical transition metal element, has rich chemical valence and numerous compounds, and therefore, has application in various fields such as catalysts, battery materials, superconducting materials, energy storage materials and the like. Wherein MoO 3 Is an N-type semiconductor material with a unique channel structure, and has gained wide attention in the fields of organic pollutant degradation, hydrogen production, solar cells, gas sensors and the like in recent years. Despite MoO 3 Has good application prospect as a photocatalyst,it still has some limitations, mainly MoO 3 The forbidden band width of (2) is wider, the response to visible light is lacking, and in addition, moO in the photocatalysis process 3 The hole-electron pair recombination rate is high, and the separation efficiency of the photogenerated carriers is low.
Research shows that the introduction of oxygen vacancy can promote the separation process of photon-generated carriers and expand MoO 3 And improves the photocatalytic performance of the light absorption range of the light-emitting diode. "Over 100-nm-Thick MoOx Films with Superior Hole Collection and Transport Properties for Organic Solar Cells" (Advanced Energy Materials,2018,8 (25)) published by Bei Yang et al, preparing a solution by using ammonium paramolybdate as a precursor and vitamin C as a reducing agent, spin-coating to form a film, and performing high-temperature annealing treatment to obtain MoO rich in oxygen vacancies 3-x A film. Experimental results show that the light absorption capacity of the film is greatly improved. Li Chunxiao et al published "high-performance lithium ion battery cathode material MoO 3-x Is carried out by molybdenum trioxide (MoO) 3 ) With oxalic acid dihydrate (H) 2 C 2 O 4 ·2H 2 O) is used as a main raw material, deionized water is used for preparing a solution, and isopropanol (C) 3 H 8 O) is used as a solvent, and is reacted for 12 hours at 120 ℃, and then is kept at 120 ℃ for 2 hours under argon atmosphere, so as to prepare the flower-shaped molybdenum oxide (MoO) with an oxygen defect structure 3-x ). But is reported at present in MoO 3 The process of introducing oxygen vacancies is complex.
Disclosure of Invention
The invention aims to solve the MoO 3 The forbidden bandwidth is wider, the response to visible light is lacking, the hole-electron pair recombination rate is high, and the separation efficiency of the photon-generated carriers is low.
The technical proposal adopted for realizing the purpose of the invention is to prepare a micron hexagonal prism MoO 3-x A photocatalytic material characterized by comprising the steps of:
1) Na is mixed with 2 MoO 4 ·2H 2 O is dissolved in deionized water;
the Na is 2 MoO 4 ·2H 2 The mol volume ratio (mol: L) of O to deionized water is 1:4-25;
2) Adding PEG-20000 into the solution in the step 1), and stirring until the solution is clear;
the PEG-20000 and Na 2 MoO 4 ·2H 2 The mass ratio (g: g) of O is 1:3-20;
3) Slowly dripping concentrated HCl into the solution obtained in the step 2), stirring for 30min, and uniformly mixing;
the volume ratio (L:L) of the concentrated HCl to the deionized water is as follows: 8-25;
4) Adding 0.2-1 g glucose into the solution in the step 3), and uniformly dispersing;
the glucose and Na 2 MoO 4 ·2H 2 The mass ratio (g: g) of O is 1:1-10;
5) Stirring the suspension liquid obtained in the step 4) at 25-80 ℃ for reaction for 1-12 h;
6) Washing the solution in the step 5) with deionized water, centrifuging to obtain a precipitate, and drying the precipitate at 60 ℃ for 10-20 h to obtain blue or deep blue MoO 3-x And (3) powder.
Compared with the prior art, the invention has the remarkable advantages that:
(1) The invention takes common glucose as a modifier and adopts a one-step reduction method to successfully prepare the surface oxygen-enriched vacancy MoO 3-x And a micron hexagonal prism.
(2) MoO prepared by the invention 3-x The material has wider visible light response range, high separation efficiency of photo-generated carriers, good photocatalytic activity and high degradation efficiency on organic matters.
(3) The preparation method is simple, can react at normal temperature or low temperature, and has short reaction time, economy and environmental protection.
Drawings
FIG. 1 (a) MoO prepared in example 1 3-x FIG. 1 (b) is an electron microscope (SEM) image of the material, and FIG. 2 shows MoO prepared in example 2 3 Electron Microscope (SEM) images of the material.
FIGS. 2 (a) and (b) are X-ray electron spectroscopy (XPS) spectra of the materials prepared in example 1 and example 2, respectively.
FIG. 3 is a Photoluminescence (PL) spectrum of the material prepared by examples 1 and 2.
FIG. 4 is a graph showing the photocatalytic performance test of the materials prepared in examples 1 and 2.
Detailed Description
The present invention will be further described with reference to the following examples and drawings, but it should not be construed that the scope of the subject matter of the present invention is limited to the following examples and drawings. Various substitutions and alterations are made according to the ordinary skill and familiar means of the art without departing from the technical spirit of the invention, and all such substitutions and alterations are intended to be included in the scope of the invention.
Example 1:
1) 1.2g of Na 2 MoO 4 ·2H 2 O is dissolved in 50ml deionized water;
2) Adding 0.1g of PEG-20000 into the solution in the step 1), and stirring until the solution is clear;
3) Slowly dripping 3.5ml of concentrated HCl into the solution in the step 2), and stirring for 30min;
4) Adding 0.5g glucose into the solution in the step 3), and uniformly dispersing;
5) Stirring the suspension in the step 4) at 60 ℃ for reaction for 4 hours;
6) Washing the solution obtained in the step 5) with deionized water, centrifuging to obtain precipitate, and drying the precipitate at 60 ℃ for 12h to obtain blue or deep blue MoO 3-x And (3) powder.
Example 2:
1) 1 to 2g of Na 2 MoO 4 ·2H 2 O was dissolved in 50ml deionized water.
2) 0.1g PEG-20000 was added to the solution in step 1) and stirred until the solution was clear.
3) 3.5ml of concentrated HCl is taken and slowly dripped into the solution in the step 2), and the mixture is stirred for 30min.
4) Washing the precipitate with deionized water and ethanol, centrifuging, and drying the precipitate at 60deg.C for 12 hr to obtain MoO 3 Micrometer columns.
SEM (FIG. 1) XPS (FIG. 2) test shows that MoO prepared according to the present invention 3 The micron rod presents regular hexagonal prism shape and has smooth surface; after modification treatment, moO 3 Surface portionMo of (c) is reduced from +6 to +5 to make MoO 3-x Part of the surface of the sample is defective, and many oxygen vacancies are formed. At the same time MoO 3-x The recombination ability of the photogenerated electron-hole pairs is effectively suppressed (fig. 3). Thus MoO 3-x In the photocatalytic reaction of the catalyst, more photo-generated electron-hole pairs can participate in the reaction, and the photocatalytic performance is more excellent (fig. 4).
Claims (2)
1. Micrometer hexagonal prism MoO 3-x The preparation method of the photocatalytic material is characterized by comprising the following steps: the method comprises the following steps:
1) Na is mixed with 2 MoO 4 ·2H 2 O is dissolved in deionized water;
the Na is 2 MoO 4 ·2H 2 The mol volume ratio (mol: L) of O to deionized water is 1:4-25;
2) Adding PEG-20000 into the solution in the step 1), and stirring until the solution is clear;
the PEG-20000 and Na 2 MoO 4 ·2H 2 The mass ratio (g: g) of O is 1:3-20;
3) Slowly dripping concentrated HCl into the solution obtained in the step 2), stirring for 30min, and uniformly mixing;
the volume ratio (L:L) of the concentrated HCl to the deionized water is as follows: 8-25;
4) Adding 0.2-1 g glucose into the solution in the step 3), and uniformly dispersing;
the glucose and Na 2 MoO 4 ·2H 2 The mass ratio (g: g) of O is 1:1-10;
5) Stirring the suspension liquid obtained in the step 4) at 25-80 ℃ for reaction for 1-12 h;
6) Washing the solution in the step 5) with deionized water, centrifuging to obtain a precipitate, and drying the precipitate at 60 ℃ for 10-20 h to obtain blue or deep blue MoO 3-x And (3) powder.
2. A micrometer hexagonal prism MoO according to claim 1 3-x The preparation method of the photocatalytic material is characterized in that the prepared MoO 3-x Is a micron hexagonal prism.
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CN105664921A (en) * | 2016-03-09 | 2016-06-15 | 陕西科技大学 | Preparation method of high-performance nano W0.4Mo0.6O3 photocatalyst |
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Title |
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硝酸辅助的六方相MoO_3的制备及其光催化性质;宋继梅;梅雪峰;王红;高菲;赵绍娟;胡海琴;;中国钼业(05);全文 * |
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