CN109569572A - Preparation method of large-particle-size bismuth vanadate spheres - Google Patents
Preparation method of large-particle-size bismuth vanadate spheres Download PDFInfo
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- CN109569572A CN109569572A CN201811523447.1A CN201811523447A CN109569572A CN 109569572 A CN109569572 A CN 109569572A CN 201811523447 A CN201811523447 A CN 201811523447A CN 109569572 A CN109569572 A CN 109569572A
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- 238000002360 preparation method Methods 0.000 title claims abstract description 20
- 229910052797 bismuth Inorganic materials 0.000 title abstract description 10
- JCXGWMGPZLAOME-UHFFFAOYSA-N bismuth atom Chemical compound [Bi] JCXGWMGPZLAOME-UHFFFAOYSA-N 0.000 title abstract description 10
- LSGOVYNHVSXFFJ-UHFFFAOYSA-N vanadate(3-) Chemical compound [O-][V]([O-])([O-])=O LSGOVYNHVSXFFJ-UHFFFAOYSA-N 0.000 title abstract 7
- HEMHJVSKTPXQMS-UHFFFAOYSA-M Sodium hydroxide Chemical compound [OH-].[Na+] HEMHJVSKTPXQMS-UHFFFAOYSA-M 0.000 claims abstract description 66
- 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 abstract description 19
- UNTBPXHCXVWYOI-UHFFFAOYSA-O azanium;oxido(dioxo)vanadium Chemical compound [NH4+].[O-][V](=O)=O UNTBPXHCXVWYOI-UHFFFAOYSA-O 0.000 claims abstract description 17
- 239000000843 powder Substances 0.000 claims abstract description 15
- 238000001354 calcination Methods 0.000 claims abstract description 12
- BMYNFMYTOJXKLE-UHFFFAOYSA-N 3-azaniumyl-2-hydroxypropanoate Chemical compound NCC(O)C(O)=O BMYNFMYTOJXKLE-UHFFFAOYSA-N 0.000 claims abstract description 11
- 238000000227 grinding Methods 0.000 claims abstract description 8
- 239000007788 liquid Substances 0.000 claims description 44
- 239000000243 solution Substances 0.000 claims description 43
- KRKNYBCHXYNGOX-UHFFFAOYSA-N citric acid Chemical compound OC(=O)CC(O)(C(O)=O)CC(O)=O KRKNYBCHXYNGOX-UHFFFAOYSA-N 0.000 claims description 23
- GRYLNZFGIOXLOG-UHFFFAOYSA-N Nitric acid Chemical compound O[N+]([O-])=O GRYLNZFGIOXLOG-UHFFFAOYSA-N 0.000 claims description 7
- 239000011259 mixed solution Substances 0.000 claims description 7
- 229910017604 nitric acid Inorganic materials 0.000 claims description 7
- 238000001035 drying Methods 0.000 claims description 6
- 238000001914 filtration Methods 0.000 claims description 6
- 238000005406 washing Methods 0.000 claims description 6
- 229920002472 Starch Polymers 0.000 claims description 3
- 230000015572 biosynthetic process Effects 0.000 claims description 3
- 235000019698 starch Nutrition 0.000 claims description 3
- 239000008107 starch Substances 0.000 claims description 3
- KRKNYBCHXYNGOX-UHFFFAOYSA-K Citrate Chemical compound [O-]C(=O)CC(O)(CC([O-])=O)C([O-])=O KRKNYBCHXYNGOX-UHFFFAOYSA-K 0.000 claims 1
- 238000004090 dissolution Methods 0.000 claims 1
- 239000002904 solvent Substances 0.000 claims 1
- 239000003054 catalyst Substances 0.000 abstract description 3
- 238000004519 manufacturing process Methods 0.000 abstract description 3
- 238000011084 recovery Methods 0.000 abstract description 2
- 238000002156 mixing Methods 0.000 abstract 1
- 238000013032 photocatalytic reaction Methods 0.000 abstract 1
- 239000002244 precipitate Substances 0.000 abstract 1
- 239000002243 precursor Substances 0.000 abstract 1
- 235000015165 citric acid Nutrition 0.000 description 8
- 230000000052 comparative effect Effects 0.000 description 5
- 238000000034 method Methods 0.000 description 5
- OZKCXDPUSFUPRJ-UHFFFAOYSA-N oxobismuth;hydrobromide Chemical compound Br.[Bi]=O OZKCXDPUSFUPRJ-UHFFFAOYSA-N 0.000 description 5
- 238000003756 stirring Methods 0.000 description 5
- 238000001027 hydrothermal synthesis Methods 0.000 description 4
- 230000001699 photocatalysis Effects 0.000 description 4
- 230000003197 catalytic effect Effects 0.000 description 3
- 239000013049 sediment Substances 0.000 description 3
- 238000006243 chemical reaction Methods 0.000 description 2
- 239000000463 material Substances 0.000 description 2
- 235000012054 meals Nutrition 0.000 description 2
- 239000002245 particle Substances 0.000 description 2
- 239000002994 raw material Substances 0.000 description 2
- 238000001228 spectrum Methods 0.000 description 2
- GWEVSGVZZGPLCZ-UHFFFAOYSA-N titanium dioxide Inorganic materials O=[Ti]=O GWEVSGVZZGPLCZ-UHFFFAOYSA-N 0.000 description 2
- GPPXJZIENCGNKB-UHFFFAOYSA-N vanadium Chemical compound [V]#[V] GPPXJZIENCGNKB-UHFFFAOYSA-N 0.000 description 2
- 229910052720 vanadium Inorganic materials 0.000 description 2
- 230000015556 catabolic process Effects 0.000 description 1
- 238000006555 catalytic reaction Methods 0.000 description 1
- 150000001875 compounds Chemical class 0.000 description 1
- 230000007812 deficiency Effects 0.000 description 1
- 238000006731 degradation reaction Methods 0.000 description 1
- 238000002474 experimental method Methods 0.000 description 1
- 239000008204 material by function Substances 0.000 description 1
- 231100000252 nontoxic Toxicity 0.000 description 1
- 230000003000 nontoxic effect Effects 0.000 description 1
- 238000004064 recycling Methods 0.000 description 1
- 239000004065 semiconductor Substances 0.000 description 1
- 230000009466 transformation Effects 0.000 description 1
- WQEVDHBJGNOKKO-UHFFFAOYSA-K vanadic acid Chemical compound O[V](O)(O)=O WQEVDHBJGNOKKO-UHFFFAOYSA-K 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
- B01J23/16—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
- B01J23/20—Vanadium, niobium or tantalum
- B01J23/22—Vanadium
-
- 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
- B01J35/00—Catalysts, in general, characterised by their form or physical properties
- B01J35/40—Catalysts, in general, characterised by their form or physical properties characterised by dimensions, e.g. grain size
-
- 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
- B01J35/50—Catalysts, in general, characterised by their form or physical properties characterised by their shape or configuration
-
- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01G—COMPOUNDS CONTAINING METALS NOT COVERED BY SUBCLASSES C01D OR C01F
- C01G31/00—Compounds of vanadium
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- Chemical & Material Sciences (AREA)
- Organic Chemistry (AREA)
- Engineering & Computer Science (AREA)
- Materials Engineering (AREA)
- Chemical Kinetics & Catalysis (AREA)
- Inorganic Chemistry (AREA)
- Catalysts (AREA)
- Inorganic Compounds Of Heavy Metals (AREA)
Abstract
The invention provides a preparation method of large-particle-size bismuth vanadate spheres, and relates to the field of novel catalysts. The preparation method comprises the following steps: respectively dissolving and mixing bismuth nitrate and ammonium metavanadate to obtain a bismuth vanadate precursor solution, calcining and grinding to form bismuth vanadate powder, and adding the obtained bismuth vanadate powder into concentrated hydrobromic acid. After the bismuth vanadate is dissolved, dropwise adding a sodium hydroxide solution to form a large-size bismuth vanadate sphere precipitate. The invention has the advantages of easy recovery after the photocatalytic reaction, simple preparation method, low production cost and the like.
Description
Technical field
The invention belongs to field of functional materials, are related to a kind of preparation method of big granularity pucherite ball.
Background technique
TiO2Since the features such as its stability is strong, oxidisability is strong, at low cost, resistance to photoetch is considered as being most suitable for for ring
The photochemical catalyst of border pollution control.But TiO2Still have it is some itself be difficult to the shortcomings that overcoming, if sun light utilization efficiency is low, be only capable of inhaling
It receives and accounts for the ultraviolet light of sunshine gross energy 4%, the deficiencies of in visible-range almost without photoresponse.And it is partly led in numerous
In body compound, pucherite is a kind of important semiconductor, has moderate band gap (2.4 eV), and there is good visible light to inhale
Receipts ability.Especially pucherite is non-toxic, ambient stable and good compatibility, cheap, and pucherite is easy preparation.Vanadic acid
These excellent performances of bismuth, make it show strong application potential in field of photocatalytic material.In recent years, granularity was in tens nanometer
Extensive preparation and research have been obtained to the pucherite in a few micrometers of ranges, has also shown higher photocatalytic activity.Such as
Zhao etc. (Cryst.Growth Des., 2017,17,2923-2928) uses hydrothermal process to synthesize scale as 1~2 μm
Pucherite.Zhang etc. (Phys. Chem. Chem. Phys., 2014,16,24519-24526) uses hydrothermal process system
For pucherite nanometer rods.Hereafter, people prepare nanoscale BiVO further through other a variety of methods4Visible light catalytic material.
While generating high light catalytic activity, it there is catalyst recycling difficulty, thus appropriate increasing in catalytic process
The granularity for adding product is a kind of important means for increasing recovery efficiency, and by the way that little particle pucherite is spherical by agglomerating into
It does not lose the photocatalytic activity of pucherite while particle also, generation photo-generated carrier can be excited under visible light, and will be dirty
Contaminate object degradation.
Summary of the invention
The purpose of the present invention is to provide a kind of preparation method of big granularity pucherite ball, the present invention has light-catalyzed reaction
After be easily recycled, the advantages such as preparation method is easy, and production cost is low.
The present invention adopts the following technical scheme:
Step 1, a certain amount of bismuth nitrate is added in the mixed solution of nitric acid and citric acid, is stirred until homogeneous, form A liquid;
Step 2, a certain amount of ammonium metavanadate is added in sodium hydroxide solution, obtains B liquid;
Step 3, B liquid is added in A liquid, forms C liquid presoma, wherein the molar ratio of bismuth nitrate and ammonium metavanadate is 1:1;
Step 4, it is 6~7 with the pH value that NaOH solution adjusts C liquid presoma, obtains pucherite powder after dry, grinding, calcining;
Step 5, the pucherite powder that step 4 obtains is added in hydrobromic acid solution, obtains clear solution;
Step 6, NaOH solution is added in the clear solution that step 5 obtains, until the pH value of solution is 6~7, formation is sunk
Large-size pucherite ball can be obtained by filtering, washing and drying processing in starch.
Preferably, the concentration of bismuth nitrate is 0.1~2 mol/L in step 1, and the concentration of citric acid is 0.5~4 mol/L,
The molar ratio of bismuth nitrate and citric acid is 1:(2~5).
Preferably, the concentration of ammonium metavanadate is 0.1~2 mol/L in step 2.
Preferably, the concentration of NaOH solution is 2~6 mol/L in step 4, and calcination temperature is 400~600 DEG C, when calcining
Between be 3~5 hours.
Preferably, the concentration of hydrobromic acid is 10~12mol/L in step 5.
Preferably, the concentration of NaOH solution is 2~6 mol/L in step 6, and the pH value of solution is adjusted to 6~7.
The large-size pucherite ball, it is characterised in that pucherite is monocline phase structure, and the granularity of pucherite ball is 40
~90 μm, large-size pucherite ball is reunited by rodlike pucherite.
Compared with prior art, the invention has the following advantages:
The advantage that large-size pucherite ball prepared by the present invention is easily isolated in the photocatalytic process.Preparation process of the present invention has
The advantages that preparation method is easy, and production cost is low, easily operated.Above-mentioned improvement of the invention, has not only saved a large amount of energy,
And it unexpectedly realizes and prepares microscopic appearance rule pucherite by raw material of the random pucherite of pattern.The present invention breaks
Conventional produces the thinking of microscopic appearance rule pucherite with hydro-thermal method or solvent-thermal method, and substantially increases the conversion of reaction
Rate.Present invention saves a large amount of hydro-thermal reaction equipment, cost is significantly reduced.
Detailed description of the invention
Fig. 1 is the XRD diffracting spectrum of the large-size pucherite ball prepared in the embodiment of the present invention 1.
Fig. 2 is the SEM photograph of the large-size pucherite ball prepared in the embodiment of the present invention 1.
Fig. 3 is that the pucherite that the large-size pucherite ball prepared in the embodiment of the present invention 1 is obtained with embodiment 2 is urged by light
Yield after changing experiment.
Fig. 4 is the pucherite TEM photo prepared in the embodiment of the present invention 2.
Fig. 5 is pucherite/bismuth oxybromide XRD diffracting spectrum that comparative example 3 of the present invention obtains.
It can be seen that from the comparison of Fig. 1 and Fig. 5, it is monoclinic phase pucherite that embodiment 1, which obtains pucherite micron ball, and comparative example
3 obtain being pucherite/bismuth oxybromide.
It can be seen that from the comparison of Fig. 2 and Fig. 4, the spherical characteristics that embodiment 1 obtains pucherite micron ball are obvious, embodiment 2
Random feature is presented in gained pucherite pattern.
Specific embodiment:
The present invention is described further with currently preferred specific embodiment with reference to the accompanying drawing, raw material is that analysis is pure.
Embodiment 1:
Step 1, the bismuth nitrate of 50mmol is added in the mixed solution of 1 mol/L nitric acid and 2 mol/L citric acids, stirring is extremely
Uniformly, A liquid is formed;
Step 2, the ammonium metavanadate of 50mmol is added in 1 mol/L sodium hydroxide solution, obtains B liquid;
Step 3, B liquid is added in A liquid, forms C liquid presoma, wherein the molar ratio of bismuth nitrate and ammonium metavanadate is 1:1;
Step 4, it is 6~7 with the pH value that the NaOH solution of 1 mol/L adjusts C liquid presoma, obtains vanadium after dry, grinding, calcining
Sour bismuth meal end;
Step 5, the pucherite powder that step 4 obtains is added in 10 mol/L hydrobromic acid solutions, obtains clear solution;
Step 6, NaOH solution is added in the clear solution that step 5 obtains, until the pH value of solution is 6~7, formation is sunk
Large-size pucherite ball can be obtained by filtering, washing and drying processing in starch.
Embodiment 2:
Step 1, the bismuth nitrate of 50mmol is added in the mixed solution of 1 mol/L nitric acid and 2 mol/L citric acids, stirring is extremely
Uniformly, A liquid is formed;
Step 2, the ammonium metavanadate of 50mmol is added in 1 mol/L sodium hydroxide solution, obtains B liquid;
Step 3, B liquid is added in A liquid, forms C liquid presoma, wherein the molar ratio of bismuth nitrate and ammonium metavanadate is 1:1;
Step 4, it is 6~7 with the pH value that the NaOH solution of 1 mol/L adjusts C liquid presoma, obtains vanadium after dry, grinding, calcining
Sour bismuth meal end.
Comparative example 1
Step 1, the bismuth nitrate of 50mmol is added in the mixed solution of 1 mol/L nitric acid and 2 mol/L citric acids, stirring is extremely
Uniformly, A liquid is formed;
Step 2, the ammonium metavanadate of 50mmol is added in 1 mol/L sodium hydroxide solution, obtains B liquid;
Step 3, B liquid is added in A liquid, forms C liquid presoma, wherein the molar ratio of bismuth nitrate and ammonium metavanadate is 1:1;
It step 4, is 6~7 with the pH value that the NaOH solution of 1 mol/L adjusts C liquid presoma, dry, grinding, 450 DEG C of calcinings 4 are small
When after obtain pucherite powder;
Step 5, the pucherite powder that step 4 obtains is added in 4 mol/L hydrobromic acid solutions, clear solution cannot be obtained,
Sediment obtains pucherite/bismuth oxybromide by filtering, washing and drying processing.
Comparative example 2
Step 1, the bismuth nitrate of 50mmol is added in the mixed solution of 1 mol/L nitric acid and 2 mol/L citric acids, stirring is extremely
Uniformly, A liquid is formed;
Step 2, the ammonium metavanadate of 50mmol is added in 1 mol/L sodium hydroxide solution, obtains B liquid;
Step 3, B liquid is added in A liquid, forms C liquid presoma, wherein the molar ratio of bismuth nitrate and ammonium metavanadate is 1:1;
It step 4, is 6~7 with the pH value that the NaOH solution of 1 mol/L adjusts C liquid presoma, dry, grinding, 450 DEG C of calcinings 4 are small
When after obtain pucherite powder;
Step 5, the pucherite powder that step 4 obtains is added in 1 mol/L hydrobromic acid solution, clear solution cannot be obtained,
Sediment obtains pucherite/bismuth oxybromide by filtering, washing and drying processing.
Comparative example 3
Step 1, the bismuth nitrate of 50mmol is added in the mixed solution of 1 mol/L nitric acid and 2 mol/L citric acids, stirring is extremely
Uniformly, A liquid is formed;
Step 2, the ammonium metavanadate of 50mmol is added in 1 mol/L sodium hydroxide solution, obtains B liquid;
Step 3, B liquid is added in A liquid, forms C liquid presoma, wherein the molar ratio of bismuth nitrate and ammonium metavanadate is 1:1;
It step 4, is 6~7 with the pH value that the NaOH solution of 1 mol/L adjusts C liquid presoma, dry, grinding, 450 DEG C of calcinings 4 are small
When after obtain pucherite powder;
Step 5, the pucherite powder that step 4 obtains is added in 0.1 mol/L hydrobromic acid solution, cannot be obtained transparent molten
Liquid, sediment obtain pucherite/bismuth oxybromide by filtering, washing and drying processing.
Above said content is only the basic explanation under present inventive concept, by reading description of the invention to the present invention
Any equivalent transformation that technical solution is taken should all belong to this hair as long as it does not depart from the spirit and scope of the technical scheme of the present invention
Bright protection scope.
Claims (7)
1. a kind of preparation method of big granularity pucherite ball, it is characterised in that pucherite is monocline phase structure, the grain of pucherite ball
Degree is 40~90 μm, and large-size pucherite ball is reunited by rodlike pucherite, specifically includes following preparation step:
Step 1, a certain amount of bismuth nitrate is added in the mixed solution of nitric acid and citric acid, is stirred until homogeneous, form A liquid;
Step 2, a certain amount of ammonium metavanadate is added in sodium hydroxide solution, obtains B liquid;
Step 3, B liquid is added in A liquid, forms C liquid, wherein the molar ratio of bismuth nitrate and ammonium metavanadate is 1:1;
Step 4, it is 6~7 with the pH value that NaOH solution adjusts C liquid presoma, obtains pucherite powder after dry, grinding, calcining;
Step 5, the pucherite powder that step 4 obtains is added in hydrobromic acid solution, pucherite powder is completely molten by hydrobromic acid
Solution obtains clear solution;
Step 6, NaOH solution is added in the clear solution that step 5 obtains, until the pH value of solution is 6~7, formation is sunk
Large-size pucherite ball can be obtained by filtering, washing and drying processing in starch.
2. a kind of preparation method of big granularity pucherite ball according to claim 1, it is characterised in that: described in step 1
The concentration of bismuth nitrate is 0.1~2 mol/L, and the concentration of citric acid is 0.5~4 mol/L, the molar ratio of bismuth nitrate and citric acid
For 1:(2~5).
3. a kind of preparation method of big granularity pucherite ball according to claim 1, it is characterised in that: described in step 2
The concentration of ammonium metavanadate is 0.1~2 mol/L.
4. a kind of preparation method of big granularity pucherite ball according to claim 1, it is characterised in that: described in step 3
Buffer of the citrate ion as solution in C liquid.
5. a kind of preparation method of big granularity pucherite ball according to claim 1, it is characterised in that: described in step 4
The concentration of NaOH solution is 2~6 mol/L, and calcination temperature is 400~600 DEG C, and calcination time is 3~5 hours.
6. a kind of preparation method of big granularity pucherite ball according to claim 1, it is characterised in that: described in step 5
The concentration of hydrobromic acid is 10~12mol/L, the solvent using hydrobromic acid as dissolution pucherite powder.
7. a kind of preparation method of big granularity pucherite ball according to claim 1, it is characterised in that: described in step 6
Large-size pucherite ball is reunited by rodlike pucherite, and the concentration of NaOH solution is 2~6 mol/L, and the pH value of solution is adjusted
To 6~7.
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US4115141A (en) * | 1976-06-22 | 1978-09-19 | E. I. Du Pont De Nemours And Company | Process for the preparation of pigmentary bright primrose yellow bismuth vanadate |
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CN108246279A (en) * | 2018-04-02 | 2018-07-06 | 哈尔滨理工大学 | A kind of pucherite/bismuth oxide and preparation method |
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2018
- 2018-12-13 CN CN201811523447.1A patent/CN109569572B/en not_active Expired - Fee Related
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US4115141A (en) * | 1976-06-22 | 1978-09-19 | E. I. Du Pont De Nemours And Company | Process for the preparation of pigmentary bright primrose yellow bismuth vanadate |
CN103495410A (en) * | 2013-09-05 | 2014-01-08 | 沈阳理工大学 | Preparation method for layered BiVO4 photocatalyst with rice straw as template |
CN107442103A (en) * | 2017-08-25 | 2017-12-08 | 东北师范大学 | The preparation method of pucherite/titanium dioxide composite film |
CN108246279A (en) * | 2018-04-02 | 2018-07-06 | 哈尔滨理工大学 | A kind of pucherite/bismuth oxide and preparation method |
CN108622934A (en) * | 2018-05-22 | 2018-10-09 | 天津城建大学 | A kind of self assembly micro nano structure BiVO4The simple preparation method of microballoon |
Non-Patent Citations (4)
Title |
---|
JUNQI LI ET AL.: "BiVO4 hollow spheres with hierarchical microstructures and enhanced photocatalytic performance under visible‐light illumination", 《PHYSICA STATUS SOLIDI A》 * |
LIANWEI SHAN ET AL.: "Enhanced photocatalytic activity with a heterojunction between BiVO4 and BiOI", 《JOURNAL OF ALLOYS AND COMPOUNDS》 * |
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