CN107175111B - A kind of support type Bi2MoO6/Cu(OH)2The preparation method of photochemical catalyst - Google Patents
A kind of support type Bi2MoO6/Cu(OH)2The preparation method of photochemical catalyst Download PDFInfo
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- CN107175111B CN107175111B CN201710319070.7A CN201710319070A CN107175111B CN 107175111 B CN107175111 B CN 107175111B CN 201710319070 A CN201710319070 A CN 201710319070A CN 107175111 B CN107175111 B CN 107175111B
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- 229910002900 Bi2MoO6 Inorganic materials 0.000 title claims abstract description 28
- 239000003054 catalyst Substances 0.000 title claims abstract description 21
- 238000002360 preparation method Methods 0.000 title claims abstract description 9
- JJLJMEJHUUYSSY-UHFFFAOYSA-L copper(II) hydroxide Inorganic materials [OH-].[OH-].[Cu+2] JJLJMEJHUUYSSY-UHFFFAOYSA-L 0.000 claims abstract description 17
- 239000011858 nanopowder Substances 0.000 claims abstract description 13
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims abstract description 10
- 230000003197 catalytic effect Effects 0.000 claims abstract description 7
- 239000011259 mixed solution Substances 0.000 claims description 22
- HEMHJVSKTPXQMS-UHFFFAOYSA-M Sodium hydroxide Chemical compound [OH-].[Na+] HEMHJVSKTPXQMS-UHFFFAOYSA-M 0.000 claims description 21
- 238000006243 chemical reaction Methods 0.000 claims description 18
- XTVVROIMIGLXTD-UHFFFAOYSA-N copper(II) nitrate Chemical compound [Cu+2].[O-][N+]([O-])=O.[O-][N+]([O-])=O XTVVROIMIGLXTD-UHFFFAOYSA-N 0.000 claims description 18
- RXPAJWPEYBDXOG-UHFFFAOYSA-N hydron;methyl 4-methoxypyridine-2-carboxylate;chloride Chemical compound Cl.COC(=O)C1=CC(OC)=CC=N1 RXPAJWPEYBDXOG-UHFFFAOYSA-N 0.000 claims description 14
- 239000000243 solution Substances 0.000 claims description 13
- 238000001027 hydrothermal synthesis Methods 0.000 claims description 12
- 239000011684 sodium molybdate Substances 0.000 claims description 12
- 235000015393 sodium molybdate Nutrition 0.000 claims description 12
- TVXXNOYZHKPKGW-UHFFFAOYSA-N sodium molybdate (anhydrous) Chemical compound [Na+].[Na+].[O-][Mo]([O-])(=O)=O TVXXNOYZHKPKGW-UHFFFAOYSA-N 0.000 claims description 12
- 238000003756 stirring Methods 0.000 claims description 8
- 238000013019 agitation Methods 0.000 claims description 5
- NASFKTWZWDYFER-UHFFFAOYSA-N sodium;hydrate Chemical compound O.[Na] NASFKTWZWDYFER-UHFFFAOYSA-N 0.000 claims description 5
- 239000008367 deionised water Substances 0.000 claims description 4
- 229910021641 deionized water Inorganic materials 0.000 claims description 4
- VLAPMBHFAWRUQP-UHFFFAOYSA-L molybdic acid Chemical compound O[Mo](O)(=O)=O VLAPMBHFAWRUQP-UHFFFAOYSA-L 0.000 claims description 2
- 239000001257 hydrogen Substances 0.000 abstract description 14
- 229910052739 hydrogen Inorganic materials 0.000 abstract description 14
- UFHFLCQGNIYNRP-UHFFFAOYSA-N Hydrogen Chemical compound [H][H] UFHFLCQGNIYNRP-UHFFFAOYSA-N 0.000 abstract description 13
- 239000003426 co-catalyst Substances 0.000 abstract description 4
- 239000000463 material Substances 0.000 abstract description 4
- 230000015572 biosynthetic process Effects 0.000 abstract description 3
- 150000001875 compounds Chemical class 0.000 abstract description 3
- 238000006303 photolysis reaction Methods 0.000 abstract description 3
- 230000015843 photosynthesis, light reaction Effects 0.000 abstract description 3
- 238000003786 synthesis reaction Methods 0.000 abstract description 3
- 238000006555 catalytic reaction Methods 0.000 abstract description 2
- 239000002800 charge carrier Substances 0.000 abstract description 2
- 239000010949 copper Substances 0.000 description 6
- BASFCYQUMIYNBI-UHFFFAOYSA-N platinum Chemical compound [Pt] BASFCYQUMIYNBI-UHFFFAOYSA-N 0.000 description 6
- 238000004519 manufacturing process Methods 0.000 description 5
- 230000001699 photocatalysis Effects 0.000 description 5
- 239000002803 fossil fuel Substances 0.000 description 4
- BDJYZEWQEALFKK-UHFFFAOYSA-N bismuth;hydrate Chemical compound O.[Bi] BDJYZEWQEALFKK-UHFFFAOYSA-N 0.000 description 3
- 239000003795 chemical substances by application Substances 0.000 description 3
- 230000000694 effects Effects 0.000 description 3
- 238000005516 engineering process Methods 0.000 description 3
- 229910052751 metal Inorganic materials 0.000 description 3
- 239000002184 metal Substances 0.000 description 3
- 238000000034 method Methods 0.000 description 3
- 238000007146 photocatalysis Methods 0.000 description 3
- 229910052697 platinum Inorganic materials 0.000 description 3
- VNWKTOKETHGBQD-UHFFFAOYSA-N methane Chemical compound C VNWKTOKETHGBQD-UHFFFAOYSA-N 0.000 description 2
- 239000002245 particle Substances 0.000 description 2
- 239000004065 semiconductor Substances 0.000 description 2
- GSEJCLTVZPLZKY-UHFFFAOYSA-N Triethanolamine Chemical compound OCCN(CCO)CCO GSEJCLTVZPLZKY-UHFFFAOYSA-N 0.000 description 1
- 230000009286 beneficial effect Effects 0.000 description 1
- 239000003245 coal Substances 0.000 description 1
- 230000002508 compound effect Effects 0.000 description 1
- 238000001816 cooling Methods 0.000 description 1
- 238000000354 decomposition reaction Methods 0.000 description 1
- 238000010586 diagram Methods 0.000 description 1
- 238000001035 drying Methods 0.000 description 1
- 230000005611 electricity Effects 0.000 description 1
- 230000002708 enhancing effect Effects 0.000 description 1
- 238000003912 environmental pollution Methods 0.000 description 1
- 239000007789 gas Substances 0.000 description 1
- 150000002431 hydrogen Chemical class 0.000 description 1
- 238000005286 illumination Methods 0.000 description 1
- 238000002156 mixing Methods 0.000 description 1
- 239000003345 natural gas Substances 0.000 description 1
- 239000003208 petroleum Substances 0.000 description 1
- 239000011941 photocatalyst Substances 0.000 description 1
- 239000000843 powder Substances 0.000 description 1
- 238000005406 washing Methods 0.000 description 1
- 229910052724 xenon Inorganic materials 0.000 description 1
- FHNFHKCVQCLJFQ-UHFFFAOYSA-N xenon atom Chemical compound [Xe] FHNFHKCVQCLJFQ-UHFFFAOYSA-N 0.000 description 1
Classifications
-
- 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
- B01J23/70—Catalysts comprising metals or metal oxides or hydroxides, not provided for in group B01J21/00 of the iron group metals or copper
- B01J23/76—Catalysts comprising metals or metal oxides or hydroxides, not provided for in group B01J21/00 of the iron group metals or copper combined with metals, oxides or hydroxides provided for in groups B01J23/02 - B01J23/36
- B01J23/84—Catalysts comprising metals or metal oxides or hydroxides, not provided for in group B01J21/00 of the iron group metals or copper combined with metals, oxides or hydroxides provided for in groups B01J23/02 - B01J23/36 with arsenic, antimony, bismuth, vanadium, niobium, tantalum, polonium, chromium, molybdenum, tungsten, manganese, technetium or rhenium
- B01J23/85—Chromium, molybdenum or tungsten
- B01J23/88—Molybdenum
- B01J23/887—Molybdenum containing in addition other metals, oxides or hydroxides provided for in groups B01J23/02 - B01J23/36
- B01J23/8876—Arsenic, antimony or bismuth
-
- 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
-
- 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
- B01J37/34—Irradiation by, or application of, electric, magnetic or wave energy, e.g. ultrasonic waves ; Ionic sputtering; Flame or plasma spraying; Particle radiation
- B01J37/341—Irradiation by, or application of, electric, magnetic or wave energy, e.g. ultrasonic waves ; Ionic sputtering; Flame or plasma spraying; Particle radiation making use of electric or magnetic fields, wave energy or particle radiation
- B01J37/344—Irradiation by, or application of, electric, magnetic or wave energy, e.g. ultrasonic waves ; Ionic sputtering; Flame or plasma spraying; Particle radiation making use of electric or magnetic fields, wave energy or particle radiation of electromagnetic wave energy
- B01J37/346—Irradiation by, or application of, electric, magnetic or wave energy, e.g. ultrasonic waves ; Ionic sputtering; Flame or plasma spraying; Particle radiation making use of electric or magnetic fields, wave energy or particle radiation of electromagnetic wave energy of microwave energy
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- Chemical & Material Sciences (AREA)
- Engineering & Computer Science (AREA)
- Chemical Kinetics & Catalysis (AREA)
- Organic Chemistry (AREA)
- Physics & Mathematics (AREA)
- Materials Engineering (AREA)
- Health & Medical Sciences (AREA)
- Toxicology (AREA)
- Plasma & Fusion (AREA)
- Optics & Photonics (AREA)
- Electromagnetism (AREA)
- Thermal Sciences (AREA)
- Catalysts (AREA)
Abstract
The invention discloses a kind of support type Bi2MoO6/Cu(OH)2The preparation method of photochemical catalyst belongs to the synthesis technical field of inorganic environment-friendly catalysis material.Technical solution of the present invention main points are as follows: by cheap Cu (OH)2Load to Bi2MoO6The surface of nano-powder, Cu (OH)2Promote electric charge carrier from Bi as co-catalyst2MoO6Move to Cu (OH)2On, it is suppressed that electrons and holes it is compound, to improve Bi2MoO6The catalytic activity of photolysis water hydrogen has huge potential prospects for commercial application.
Description
Technical field
The invention belongs to the synthesis technical fields of inorganic environment-friendly catalysis material, and in particular to a kind of support type Bi2MoO6/
Cu(OH)2The preparation method of photochemical catalyst.
Background technique
For example coal, petroleum, natural gas are as a kind of non-renewable energy resources for fossil fuel, in the hair of human lives and world economy
It is all played a crucial role in exhibition process.However, but having ignored resource while the mankind are exploited wantonly using fossil fuel
The increasingly problem of energy crisis of reduction, the burning of fossil fuel also bring serious environmental pollution to global range.Therefore, it sends out
Opening up clean reproducible energy becomes the project that whole world researchers pay attention to.Hydrogen as energy source is because its is efficient, environmental-friendly and can follow
The features such as ring utilizes will be possible to replace the status of fossil fuel in future.Hydrogen is prepared using semiconductor material photochemical catalyzing
Gas is considered as the hydrogen producing technology of great prospect.
Bi2MoO6Since its relatively narrow forbidden bandwidth, good thermal stability and photocatalysis performance are to by people
Extensive concern, conduction band potential ratio EH2/H+It is more negative, meet the condition that photochemical catalyzing prepares hydrogen, is a kind of very potential
Photocatalysis hydrogen production material.But pure Bi2MoO6During photochemical catalyzing there are light induced electron and hole be easy it is compound,
The low disadvantage of quantum efficiency limits its application industrially.In order to improve Bi2MoO6Quantum efficiency and photolysis water hydrogen
Efficiency, be usually supported on Bi for metal platinum as co-catalyst2MoO6Surface, so that the compound effect of light induced electron be effectively reduced
Rate, and then improve Bi2MoO6The efficiency of photolysis water hydrogen.However, promoter metal platinum is expensive, thus limit its
Application in industry.The present invention is by cheap Cu (OH)2Load to Bi2MoO6Surface, Cu (OH)2Promote electricity as co-catalyst
Charge carrier is from Bi2MoO6Move to Cu (OH)2On, it is suppressed that electrons and holes it is compound, to improve Bi2MoO6Photocatalytic water system
The catalytic activity of hydrogen has huge potential prospects for commercial application.
Summary of the invention
The technical problem to be solved by the present invention is to provide support type Bi that is a kind of easy to operate and being easily achieved2MoO6/Cu
(OH)2The preparation method of photochemical catalyst, support type Bi made from this method2MoO6/Cu(OH)2The visible light utilization efficiency of photochemical catalyst
Height, photo-quantum efficiency are high and photocatalytic hydrogen production activity is good.
The present invention adopts the following technical scheme that solve above-mentioned technical problem, a kind of support type Bi2MoO6/Cu(OH)2Light is urged
The preparation method of agent, it is characterised in that specific steps are as follows:
(1) by five nitric hydrate bismuths and two molybdic acid hydrate sodium, 2:1 is dissolved in deionized water in molar ratio under agitation
The mixed solution of bismuth nitrate and sodium molybdate is formed, is turned after the mixed solution of bismuth nitrate and sodium molybdate is stirred 2h at room temperature
It moves in hydrothermal reaction kettle, then hydrothermal reaction kettle is put into microwave dissolver in 120 DEG C of microwave reaction 5-30min, to anti-
It cooled down after answering, wash, be dried to obtain Bi2MoO6Nano-powder;
(2) copper nitrate solution is prepared, sodium hydroxide is added into copper nitrate solution under stirring and step (1) obtains
Bi2MoO6Nano-powder obtains mixed solution, and wherein the molar ratio of sodium hydroxide and copper nitrate is 1:0.5, Bi2MoO6Nanometer
The molar ratio of powder and copper nitrate is 1:0.005-0.015;
(3) reaction 6h is stirred at room temperature in the mixed solution that step (2) obtains, filters, is dried to obtain after reaction
Support type Bi with high catalytic activity2MoO6/Cu(OH)2Photochemical catalyst.
Further preferably, the molar concentration of bismuth nitrate is 0.01- in the mixed solution of the bismuth nitrate and sodium molybdate
0.05mol/L。
Further preferably, the molar concentration of copper nitrate is 0.001-0.006mol/L in the copper nitrate solution.
Compared with the prior art, the invention has the following beneficial effects:
1, the support type Bi that band structure matches is prepared using suitable synthesis technology2MoO6/Cu(OH)2Photocatalysis
Agent can make photo-generated carrier be injected into another kind by a kind of energy level of semiconductive particles using the energy level difference between two kinds of semiconductors
On the energy level of semiconductive particles, to improve the separative efficiency of photogenerated charge, and then the hydrogen manufacturing of loaded photocatalyst is improved
Energy;
2, fast and the features such as solution is heated evenly according to the microwave-hydrothermal method rate of heat addition, it is prepared using microwave-hydrothermal method
The high activity Bi that crystallite size is small and reunion degree is low2MoO6Nano-powder effectively increases support type Bi2MoO6/Cu(OH)2Light
The activity of catalyst;
3, using cheap Cu (OH)2Co-catalyst replaces expensive metal platinum, to effectively reduce support type
Bi2MoO6/Cu(OH)2The production cost of photochemical catalyst promotes its prospects for commercial application.
Detailed description of the invention
Fig. 1 is support type Bi prepared by the embodiment of the present invention 1 under the irradiation of 300W xenon lamp2MoO6/Cu(OH)2Photochemical catalyst
With pure Bi2MoO6The photocatalytic hydrogen production by water decomposition efficiency column diagram (operating condition: the amount of catalyst: 0.05g of photochemical catalyst;It sacrifices
The amount of agent triethanolamine: 10mL).It can be seen from the figure that under the irradiation of simulated visible light, after illumination 6h, support type
Bi2MoO6/Cu(OH)2The hydrogen generation efficiency of photochemical catalyst is apparently higher than pure Bi2MoO6The hydrogen generation efficiency of photochemical catalyst is shown obvious
The photocatalytic activity of enhancing.
Specific embodiment
Above content of the invention is described in further details by the following examples, but this should not be interpreted as to this
The range for inventing above-mentioned theme is only limitted to embodiment below, and all technologies realized based on above content of the present invention belong to this hair
Bright range.
Embodiment 1
(1) five nitric hydrate bismuth of 0.01mol and bis- molybdic acid hydrate sodium of 0.005mol are dissolved in 1000mL under agitation
The mixed solution that bismuth nitrate and sodium molybdate are formed in deionized water, at room temperature by the mixed solution of bismuth nitrate and sodium molybdate
It is transferred to hydrothermal reaction kettle after stirring 2h, then hydrothermal reaction kettle is put into microwave dissolver in 120 DEG C of microwave reaction 5min,
To cool down, wash after reaction, be dried to obtain Bi2MoO6Nano-powder;
(2) the copper nitrate solution 25mL for preparing 0.001mol/L, is added under stirring into copper nitrate solution
The Bi that 0.05mmol sodium hydroxide and 5mmol step (1) obtain2MoO6Nano-powder obtains mixed solution;
(3) reaction 6h is stirred at room temperature in the mixed solution that step (2) obtains, filters, is dried to obtain after reaction
Support type Bi with high catalytic activity2MoO6/Cu(OH)2Photochemical catalyst.
Embodiment 2
(1) five nitric hydrate bismuth of 0.02mol and bis- molybdic acid hydrate sodium of 0.01mol are dissolved in 1000mL under agitation
The mixed solution that bismuth nitrate and sodium molybdate are formed in ionized water, at room temperature stirs the mixed solution of bismuth nitrate and sodium molybdate
It is transferred to hydrothermal reaction kettle after mixing 2h, then hydrothermal reaction kettle is put into microwave dissolver in 120 DEG C of microwave reaction 10min,
To cool down, wash after reaction, be dried to obtain Bi2MoO6Nano-powder;
(2) the copper nitrate solution 75mL for preparing 0.002mol/L, is added under stirring into copper nitrate solution
The Bi that 0.3mmol sodium hydroxide and 10mmol step (1) obtain2MoO6Nano-powder obtains mixed solution;
(3) reaction 6h is stirred at room temperature in the mixed solution that step (2) obtains, filters, is dried to obtain after reaction
Support type Bi with high catalytic activity2MoO6/Cu(OH)2Photochemical catalyst.
Embodiment 3
(1) five nitric hydrate bismuth of 0.05mol and bis- molybdic acid hydrate sodium of 0.025mol are dissolved in 1000mL under agitation
The mixed solution that bismuth nitrate and sodium molybdate are formed in deionized water, at room temperature by the mixed solution of bismuth nitrate and sodium molybdate
It is transferred to hydrothermal reaction kettle after stirring 2h, then hydrothermal reaction kettle is put into microwave dissolver in 120 DEG C of microwave reactions
Bi can be obtained to cooling after reaction, washing, drying in 30min2MoO6Nano-powder;
(2) the copper nitrate solution 50mL for preparing 0.006mol/L, is added under stirring into copper nitrate solution
The Bi that 0.6mmol sodium hydroxide and 30mmol step (1) obtain2MoO6Nano-powder obtains mixed solution;
(3) reaction 6h is stirred at room temperature in the mixed solution that step (2) obtains, filters, is dried to obtain after reaction
Support type Bi with high catalytic activity2MoO6/Cu(OH)2Photochemical catalyst.
Embodiment above describes basic principles and main features of the invention and advantage, the technical staff of the industry should
Understand, the present invention is not limited to the above embodiments, and the above embodiments and description only describe originals of the invention
Reason, under the range for not departing from the principle of the invention, various changes and improvements may be made to the invention, these changes and improvements are each fallen within
In the scope of protection of the invention.
Claims (3)
1. a kind of support type Bi2MoO6/Cu(OH)2The preparation method of photochemical catalyst, it is characterised in that specific steps are as follows:
(1) by five nitric hydrate bismuths and two molybdic acid hydrate sodium, 2:1 is dissolved in deionized water and being formed in molar ratio under agitation
The mixed solution of bismuth nitrate and sodium molybdate is transferred to after the mixed solution of bismuth nitrate and sodium molybdate is stirred 2h at room temperature
In hydrothermal reaction kettle, then hydrothermal reaction kettle is put into microwave dissolver in 120 DEG C of microwave reaction 5-30min, wait react knot
It cooled down after beam, wash, be dried to obtain Bi2MoO6Nano-powder;
(2) copper nitrate solution is prepared, is added what sodium hydroxide and step (1) obtained into copper nitrate solution under stirring
Bi2MoO6Nano-powder obtains mixed solution, and wherein the molar ratio of sodium hydroxide and copper nitrate is 1:0.5, Bi2MoO6Nano powder
The molar ratio of body and copper nitrate is 1:0.005-0.015;
(3) reaction 6h is stirred at room temperature in the mixed solution that step (2) obtains, filters after reaction, is dried to obtain and has
The support type Bi of high catalytic activity2MoO6/Cu(OH)2Photochemical catalyst.
2. support type Bi according to claim 12MoO6/Cu(OH)2The preparation method of photochemical catalyst, it is characterised in that: institute
The molar concentration for stating bismuth nitrate in the mixed solution of bismuth nitrate and sodium molybdate is 0.01-0.05mol/L.
3. support type Bi according to claim 12MoO6/Cu(OH)2The preparation method of photochemical catalyst, it is characterised in that: institute
The molar concentration for stating copper nitrate in copper nitrate solution is 0.001-0.006mol/L.
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Citations (2)
Publication number | Priority date | Publication date | Assignee | Title |
---|---|---|---|---|
CN103418381A (en) * | 2013-08-26 | 2013-12-04 | 天津师范大学 | High-performance Ag2O/Bi2WO6 compound light catalyst and preparing method thereof |
CN105772018A (en) * | 2016-04-18 | 2016-07-20 | 河南师范大学 | Bi2WO6-BiFeO3 compound photocatalyst and preparing method thereof |
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2017
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Patent Citations (2)
Publication number | Priority date | Publication date | Assignee | Title |
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CN103418381A (en) * | 2013-08-26 | 2013-12-04 | 天津师范大学 | High-performance Ag2O/Bi2WO6 compound light catalyst and preparing method thereof |
CN105772018A (en) * | 2016-04-18 | 2016-07-20 | 河南师范大学 | Bi2WO6-BiFeO3 compound photocatalyst and preparing method thereof |
Non-Patent Citations (1)
Title |
---|
A one-pot method for the preparation of grapheme-Bi2MoO6 hybrid photocatalysts that are responsive to visible-light and have excellent photocatalytic activity in the degradation of organic pollutants;Peifang Wang等;《CARBON》;20120710;第50卷;第5256-5264页 * |
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