CN110302811B - Bismuth oxychloride sheet material with radial cracks and preparation method and application thereof - Google Patents
Bismuth oxychloride sheet material with radial cracks and preparation method and application thereof Download PDFInfo
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- BWOROQSFKKODDR-UHFFFAOYSA-N oxobismuth;hydrochloride Chemical compound Cl.[Bi]=O BWOROQSFKKODDR-UHFFFAOYSA-N 0.000 title claims abstract description 102
- 229940073609 bismuth oxychloride Drugs 0.000 title claims abstract description 97
- 239000000463 material Substances 0.000 title claims abstract description 54
- 238000002360 preparation method Methods 0.000 title claims abstract description 11
- 238000006243 chemical reaction Methods 0.000 claims abstract description 14
- 238000000034 method Methods 0.000 claims abstract description 11
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims abstract description 11
- 238000001816 cooling Methods 0.000 claims abstract description 8
- 238000003756 stirring Methods 0.000 claims abstract description 7
- 238000005406 washing Methods 0.000 claims abstract description 7
- 239000003960 organic solvent Substances 0.000 claims abstract description 6
- 238000004108 freeze drying Methods 0.000 claims abstract description 3
- CSCPPACGZOOCGX-UHFFFAOYSA-N Acetone Chemical compound CC(C)=O CSCPPACGZOOCGX-UHFFFAOYSA-N 0.000 claims description 25
- LYCAIKOWRPUZTN-UHFFFAOYSA-N Ethylene glycol Chemical compound OCCO LYCAIKOWRPUZTN-UHFFFAOYSA-N 0.000 claims description 24
- 230000007797 corrosion Effects 0.000 claims description 24
- 238000005260 corrosion Methods 0.000 claims description 24
- 239000000203 mixture Substances 0.000 claims description 13
- 239000000047 product Substances 0.000 claims description 13
- PEDCQBHIVMGVHV-UHFFFAOYSA-N Glycerine Chemical compound OCC(O)CO PEDCQBHIVMGVHV-UHFFFAOYSA-N 0.000 claims description 12
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical group CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 claims description 11
- 239000001267 polyvinylpyrrolidone Substances 0.000 claims description 5
- 235000013855 polyvinylpyrrolidone Nutrition 0.000 claims description 5
- 229920000036 polyvinylpyrrolidone Polymers 0.000 claims description 5
- JHXKRIRFYBPWGE-UHFFFAOYSA-K bismuth chloride Chemical compound Cl[Bi](Cl)Cl JHXKRIRFYBPWGE-UHFFFAOYSA-K 0.000 claims description 4
- 239000002244 precipitate Substances 0.000 claims description 4
- 230000001699 photocatalysis Effects 0.000 abstract description 8
- 230000003197 catalytic effect Effects 0.000 abstract description 4
- 239000002086 nanomaterial Substances 0.000 abstract description 3
- 238000000926 separation method Methods 0.000 abstract description 2
- 238000009776 industrial production Methods 0.000 abstract 1
- 238000007146 photocatalysis Methods 0.000 abstract 1
- 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 description 7
- 229940043267 rhodamine b Drugs 0.000 description 7
- 239000002135 nanosheet Substances 0.000 description 5
- 239000003921 oil Substances 0.000 description 5
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- 238000006731 degradation reaction Methods 0.000 description 3
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- 238000005516 engineering process Methods 0.000 description 3
- WGCNASOHLSPBMP-UHFFFAOYSA-N hydroxyacetaldehyde Natural products OCC=O WGCNASOHLSPBMP-UHFFFAOYSA-N 0.000 description 3
- 239000002055 nanoplate Substances 0.000 description 3
- 239000000126 substance Substances 0.000 description 3
- 229910021607 Silver chloride Inorganic materials 0.000 description 2
- 230000002378 acidificating effect Effects 0.000 description 2
- 230000001276 controlling effect Effects 0.000 description 2
- 238000010586 diagram Methods 0.000 description 2
- 238000005530 etching Methods 0.000 description 2
- 238000003760 magnetic stirring Methods 0.000 description 2
- STZCRXQWRGQSJD-GEEYTBSJSA-M methyl orange Chemical group [Na+].C1=CC(N(C)C)=CC=C1\N=N\C1=CC=C(S([O-])(=O)=O)C=C1 STZCRXQWRGQSJD-GEEYTBSJSA-M 0.000 description 2
- 229940012189 methyl orange Drugs 0.000 description 2
- 239000011259 mixed solution Substances 0.000 description 2
- 230000007935 neutral effect Effects 0.000 description 2
- 239000000843 powder Substances 0.000 description 2
- 230000001105 regulatory effect Effects 0.000 description 2
- 239000004065 semiconductor Substances 0.000 description 2
- HKZLPVFGJNLROG-UHFFFAOYSA-M silver monochloride Chemical compound [Cl-].[Ag+] HKZLPVFGJNLROG-UHFFFAOYSA-M 0.000 description 2
- 239000000725 suspension Substances 0.000 description 2
- 229920000557 Nafion® Polymers 0.000 description 1
- XUIMIQQOPSSXEZ-UHFFFAOYSA-N Silicon Chemical compound [Si] XUIMIQQOPSSXEZ-UHFFFAOYSA-N 0.000 description 1
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- RKTYLMNFRDHKIL-UHFFFAOYSA-N copper;5,10,15,20-tetraphenylporphyrin-22,24-diide Chemical compound [Cu+2].C1=CC(C(=C2C=CC([N-]2)=C(C=2C=CC=CC=2)C=2C=CC(N=2)=C(C=2C=CC=CC=2)C2=CC=C3[N-]2)C=2C=CC=CC=2)=NC1=C3C1=CC=CC=C1 RKTYLMNFRDHKIL-UHFFFAOYSA-N 0.000 description 1
- 239000002537 cosmetic Substances 0.000 description 1
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- 239000003792 electrolyte Substances 0.000 description 1
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- 230000008014 freezing Effects 0.000 description 1
- 238000005286 illumination Methods 0.000 description 1
- 229910000734 martensite Inorganic materials 0.000 description 1
- 238000005259 measurement Methods 0.000 description 1
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- 239000002057 nanoflower Substances 0.000 description 1
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- 238000013033 photocatalytic degradation reaction Methods 0.000 description 1
- 238000001782 photodegradation Methods 0.000 description 1
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- FHNFHKCVQCLJFQ-UHFFFAOYSA-N xenon atom Chemical compound [Xe] FHNFHKCVQCLJFQ-UHFFFAOYSA-N 0.000 description 1
Images
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
- B01J27/06—Halogens; Compounds thereof
-
- B01J35/33—
-
- B01J35/39—
Abstract
The invention provides a preparation method of a bismuth oxychloride sheet material with radial cracks on the surface, belonging to the field of inorganic nano materials. The preparation method comprises the following steps: dispersing the prepared bismuth oxychloride flaky material into water or an organic solvent in an open system, stirring in an oil bath at 25-200 ℃, naturally cooling after the reaction is finished, carrying out centrifugal separation, washing and freeze drying to obtain the bismuth oxychloride flaky material with radial cracks, wherein the cracks are uniform. The method has the advantages of simple operation, low cost and good repeatability, is suitable for industrial production, and shows excellent catalytic activity in the aspect of photocatalysis.
Description
Technical Field
The invention belongs to the field of inorganic nano materials, and particularly relates to a bismuth oxychloride sheet material with radial cracks, a preparation method and application of the material in the aspect of photoelectrocatalysis.
Background
Bismuth oxychloride (BiOCl) is a high-grade environment-friendly, non-toxic, low-cost, easy to prepare and stable-structure material, and can be widely used in the fields of cosmetics, photoelectric catalysts and the like. Since bismuth oxychloride has a tetragonal martensitic layered structure, it is characterized by [ Bi ]2O2]2+Layer sandwiching bis [ Cl ]2]2-The layer, resulting in the generation of an Internal Electric Field (IEF), can promote the separation of photo-excited electron-hole pairs, thereby having excellent photocatalytic activity in the field of degrading contaminants. Therefore, bismuth oxychloride materials are in the favor of researchers.
The bismuth oxychloride has various shapes, such as nanoflower, nanometer, nanotube, nanosheet and the like. Of all the morphologies of bismuth oxychloride, the sheet-like BiOCl structure is easier to synthesize because BiOCl has a specific layered crystal structure. So far, the size and thickness of a sheet-like BiOCl structure can be regulated by various methods, and the obtained BiOCl crystal exhibits excellent catalytic activity.
Zhanghongjie et al synthesized a three-dimensional layered structure composed of a plurality of two-dimensional (2D) nanosheets, and the obtained three-dimensional layered structure with a larger specific surface area and more photocatalytic active sites effectively promoted the photocatalytic decomposition of Methyl Orange (MO). Wujuanjuan et al regulated the reaction temperature to obtain BiOCl nanoplates of different sizes and different {001} face exposure ratios, and found that BiOCl nanoplates with more {001} face exposure ratios reduced the photocatalytic degradation efficiency of rhodamine B (RhB) compared to nanoplates in other articles. Zhang concisely et al found that BiOCl nanosheets with appropriate {001} plane exposure ratios can enhance photodegradation of rhodamine B by adjusting the pH of the reaction to obtain BiOCl nanosheets with different {001} plane exposure ratios. In addition to controlling the thickness and size of the BiOCl sheet, defects in the sheet surface can also, in principle, affect the final catalytic performance. However, there have been no reports in the prior art of controlling the surface morphology of BiOCl sheets, possibly due to the difficulty in utilizing such complex structures.
Therefore, in order to further improve the photoelectrocatalysis activity of the bismuth oxychloride, the surface of the bismuth oxychloride is corroded to form radial cracks by adopting a wet chemical corrosion method, the method mainly utilizes air to corrode the surface of the bismuth oxychloride sheet, and the radial cracks can further improve the photoelectrocatalysis activity of the bismuth oxychloride, so that the material of the bismuth oxychloride can be widely applied in the field of catalysis.
Disclosure of Invention
The technical problem solved by the invention is as follows: the invention provides a bismuth oxychloride sheet catalytic material with radial cracks, and provides a method for synthesizing the bismuth oxychloride sheet material with radial cracks by adopting a wet chemical corrosion technology for the first time.
In order to solve the technical problems, the technical scheme adopted by the invention is as follows: a bismuth oxychloride sheet material having radial cracks etched on the surface thereof is provided.
The preparation method of the bismuth oxychloride sheet material with radial cracks comprises the following steps:
i, keeping a closed reaction system, and preparing a BiOCl sheet material before corrosion;
and II, dispersing the bismuth oxychloride sheet material prepared in the step I into water or an organic solvent in an open system, stirring in an oil bath at the temperature of 25-200 ℃, reacting for 1 minute to 200 hours, cooling, purifying the product, and freeze-drying.
Preferably, the step i maintains a closed reaction system, and the specific steps for preparing the BiOCl sheet material before corrosion are as follows: keeping a closed reaction system, dissolving bismuth chloride and polyvinylpyrrolidone in ethylene glycol, adjusting the pH value to 3 by adopting HCl, finally carrying out oil bath on the mixture at 165 ℃, stirring for more than 17 hours to generate white precipitate, cooling to room temperature, and washing the product with a mixture of acetone and water for three times to obtain the BiOCl flaky material before corrosion. In the step II, the organic solvent is ethanol, glycol, acetone and glycerol. The product was purified by washing the product three times with a mixture of acetone and water.
The second preparation method of the bismuth oxychloride sheet material with radial cracks comprises the following steps: maintaining an open reaction system, dispersing the bismuth oxychloride sheet material prepared by dissolving bismuth chloride and polyvinylpyrrolidone into ethylene glycol, adjusting the pH value to be acidic or neutral by adopting HCl, finally carrying out oil bath at the temperature of 105 ℃ and 195 ℃ on the mixture, stirring for more than 17 hours to generate white precipitate, cooling to room temperature, and washing the product by using a mixture of acetone and water to obtain the bismuth oxychloride sheet material with radial cracks.
The bismuth oxychloride sheet material with radial cracks can be widely applied to the aspect of photoelectrocatalysis.
The invention has the beneficial effects that: compared with the prior art, the bismuth oxychloride with radial cracks can further improve the photoelectrocatalysis activity of the bismuth oxychloride, so that the bismuth oxychloride can be widely applied to the field of catalysis. In addition, the sheet material of bismuth oxychloride with radial cracks can be applied to the field of semiconductor photoelectrocatalysis, and is improved compared with the sheet material of non-corroded bismuth oxychloride.
In addition, radial cracks are corroded on the surface of the bismuth oxychloride by adopting a wet chemical corrosion technology, the method mainly utilizes the air to participate in the wet chemical process to corrode the surface of the bismuth oxychloride sheet, and the yield is high and can reach more than 96%. The method has the advantages of simple preparation conditions, simplicity, easy obtaining and high repeatability. In addition, the bismuth oxychloride sheet material with radial cracks can be applied to the field of semiconductor photoelectrocatalysis, and is improved in the aspect of photoelectrocatalysis compared with the non-corroded bismuth oxychloride sheet material.
Drawings
FIG. 1 is a diagram showing the appearance of BiOCl sheet materials of different forms under a field emission scanning electron microscope; (a) BiOCl sheet material before corrosion prepared under closed system reaction; (b) BiOCl sheet material before corrosion prepared under open system reaction condition; (c, d) corroded bismuth oxychloride with radial cracks prepared under the reaction condition of an open system;
FIG. 2 is an XRD pattern of three different bismuth oxychloride sheets;
FIG. 3 (a) is an i-t curve of bismuth oxychloride before and after corrosion, and (B) is a degradation diagram of bismuth oxychloride to rhodamine B before and after corrosion.
Detailed Description
The invention will be further described with reference to the accompanying drawings.
EXAMPLE 1 preparation of BiOCl sheet Material with radial cracks
The first step is as follows: while maintaining the closed reaction system, 9.7 g of bismuth chloride (BiCl)3) And 7.7 g of polyvinylpyrrolidone (PVP) was dissolved in 7 m L of Ethylene Glycol (EG), then HCl was added to the above mixture to adjust the pH to be acidic to neutral, optimally pH =3, and finally the mixture was subjected to oil bath at 105 ℃ and 195 ℃ for more than 17 hours under magnetic stirring to generate white precipitates, finally, after naturally cooling to room temperature, the product was washed three times with a mixture of acetone and water to obtain a BiOCl sheet material before etching, 2. mu. L of bismuth oxychloride solution was dropped on the already washed silicon wafer, naturally dried, and then the morphology of the BiOCl sheet material was characterized under an acceleration voltage of 3 kV using a JEO L JSM-7600F field emission scanning electron microscope (FE-SEM), and it was found that the bismuth oxychloride material had a square morphology, particularly, sharp at the four corners, as shown in FIG. 1 (a).
The second step is that: under the condition of an open system, dispersing 4 mg of the bismuth oxychloride sheet material prepared in the first step into 2 ml of water or an organic solvent solution with similar compatibility properties such as ethanol, glycol, acetone and glycerol (glycerol), preferably glycol, stirring the bismuth oxychloride sheet material in an oil bath at 25-200 ℃, wherein the reaction time can be corroded within 1 minute to 200 hours, (note: the corrosion time depends on the concentration of the bismuth oxychloride and the corrosion temperature, the bismuth oxychloride sheet material can be corroded into particles finally), naturally cooling the bismuth oxychloride sheet material, washing the product with a mixture of acetone and water for three times, freezing and drying the product overnight, and by the same FE-SEM characterization technology, the BiOCl sheet material with clear radial cracks can be obtained, and the bismuth oxychloride material with a smooth surface before being corroded has uniform and fine radial cracks, the morphology of BiOCl at 3 minutes of etching is shown in FIG. 1 (c, d).
In addition, in the first step of the preparation method of the BiOCl sheet material with radial cracks, a closed system is changed into an open system, so that the bismuth oxychloride sheet nano material with radial cracks can be directly obtained, the shape representation is carried out through the field emission scanning electron microscope, four corners of the bismuth oxychloride obtained in the open system are relatively round, and the four corners of the bismuth oxychloride not obtained in the closed system are sharp, as shown in FIG. 1 (b), and the same radial cracks can also be obtained by corroding the bismuth oxychloride sheet with round corners;
example 2 determination of the Properties of BiOCl sheet Material with radial cracks
The bismuth oxychloride sheet prepared in example 1 and the BiOCl sheet having radial cracks were each freeze-dried to obtain white powders, and the three powders were subjected to X-ray diffraction (XRD) characterization, and it was found that each of the bismuth oxychloride sheets corresponds to a bismuth oxychloride PDF card (JCPDS number 06-0249) and has no hetero-peak, and thus, the structure of the bismuth oxychloride before and after corrosion did not change and the purity was high, as shown in fig. 2 (note: X-ray diffraction (XRD) characterization on Smart L ab (rigaku) with Cu Ka1 (k = 0.154178 nm) as a light source for 4min-1Is obtained to determineThe phase structure and purity of the crystals are considered. )
Example 3 application of BiOCl sheet Material before and after Corrosion in photo (electro) catalysis
And (3) photoelectrocatalysis test: a typical procedure for preparing a photoelectrode is as follows: a mass (2 mg) of the above prepared BiOCl flakes was dispersed in a volume (100 microliters) of ethanol and a volume (12 microliters) of 5% Nafion solution was added to the above solution. The prepared mixed solution (20 μ l) was then uniformly coated on an ITO electrode (d =1 cm) and naturally dried. The photocurrent was measured on a Chenhua CHI 660E electrochemical workstation with a standard three-electrode system, using a Pt electrode as counter electrode, an Ag/AgCl (3.5M) electrode as reference electrode and an ITO electrode as working electrode. Na (Na)2SO4(0.5M) and KBrO3(0.1 mmol) was used as an electrolyte. The i-t curve was measured at 0V (vs. 3M Ag/AgCl) under 300W xenon illumination.
Photocatalytic test of BiOCl sheet material prepared as described above (5 mg) was mixed with 10 m L20 mg/L rhB aqueous solution (20 mg. L)-1) The suspension mixture is then irradiated with a solar simulator (P L S-SXE300, Perfect L light) under magnetic stirring every 5 or 10 minutes, a small amount of suspension is taken out and centrifuged before spectroscopic measurement every 5 or 10 minutes, an amount of RhB mixed solution is taken, fluorescence of the sample is excited with a 532 nm laser (L CX-532S, Oxxius), and the spectrum of the solution is analyzed with a spectrometer (iHR 550, Horiba) equipped with a cooled Charge Coupled Device (CCD) camera (Syncerity, JHY), spectrophotometrically with a photoluminescence (P L) excited at 532 nm (L CX-532S, Oxxius).
As shown in fig. 3 (a), when the photocurrent curves of the bismuth oxychloride before and after the corrosion were analyzed, the bismuth oxychloride had a photocurrent response, and the current ratio of the bismuth oxychloride with radial cracks on the surface after the corrosion was high, increasing the photocurrent by about eight times, so that the bismuth oxychloride with radial cracks after the corrosion had significantly improved the photocatalytic efficiency.
As shown in fig. 3 (B), when the photocatalytic data analysis of bismuth oxychloride before and after corrosion is performed, the degradation rate of the non-corroded bismuth oxychloride nanosheet to rhodamine B is 72%, and the degradation rate of the bismuth oxychloride with radial cracks on the surface after corrosion to rhodamine B is 92%, it can be found that the photocatalytic efficiency of the bismuth oxychloride sheet material with radial cracks on the surface is obviously improved.
The foregoing shows and describes the general principles and broad features of the present invention and advantages thereof. It will be understood by those skilled in the art that the present invention is not limited to the embodiments described above, which are described in the specification and illustrated only to illustrate the principle of the present invention, but that various changes and modifications may be made therein without departing from the spirit and scope of the present invention, which fall within the scope of the invention as claimed. The scope of the invention is defined by the appended claims and equivalents thereof.
Claims (6)
1. A bismuth oxychloride sheet material, wherein radial cracks are corroded on the surface of the bismuth oxychloride sheet material.
2. A preparation method for preparing the bismuth oxychloride sheet material of claim 1, which comprises the following steps:
i, keeping a closed reaction system, and preparing a BiOCl sheet material before corrosion;
and II, dispersing the bismuth oxychloride sheet material prepared in the step I into water or an organic solvent in an open system, stirring in an oil bath at the temperature of 25-200 ℃, reacting for 1 minute to 200 hours, cooling, wherein the corrosion time depends on the concentration of the bismuth oxychloride and the corrosion temperature, and after a product is corroded into a sheet with radial cracks on the surface, purifying the product, and freeze-drying.
3. A method for preparing bismuth oxychloride sheet material according to claim 2, wherein the step i is performed by maintaining a closed reaction system, and the specific steps for preparing the BiOCl sheet material before corrosion are as follows: keeping a closed reaction system, dissolving bismuth chloride and polyvinylpyrrolidone in ethylene glycol, adjusting the pH value to 3 by adopting HCl, finally carrying out oil bath on the mixture at 165 ℃, stirring for more than 17 hours to generate white precipitate, cooling to room temperature, and washing the product by using a mixture of acetone and water to obtain the BiOCl flaky material before corrosion.
4. The method for preparing bismuth oxychloride sheet material according to claim 2, wherein in the step ii, the organic solvent is ethanol, ethylene glycol, acetone or glycerol.
5. A method for preparing bismuth oxychloride sheet material according to claim 2, wherein in the step ii, the product is purified by washing the product three times with a mixture of acetone and water.
6. Use of bismuth oxychloride platelets of claim 1 in photoelectrocatalysis.
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|---|---|---|---|---|
| CN104069876A (en) * | 2014-06-24 | 2014-10-01 | 华中师范大学 | Ag-BiOCl compound photocatalyst prepared by depositing nanometer silver on [001] crystal face of BiOCl nanometer sheet and method |
| CN108502926A (en) * | 2018-05-15 | 2018-09-07 | 安徽师范大学 | BiOCl nano-rings and its synthetic method |
| CN108579770A (en) * | 2018-05-15 | 2018-09-28 | 安徽师范大学 | A method of carrying out degradation of contaminant using BiOCl nano-rings |
| CN109759095A (en) * | 2019-01-21 | 2019-05-17 | 陕西科技大学 | A kind of BiOBr hollow fibre, preparation method and its application as photochemical catalyst in light degradation dyestuff |
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| Publication number | Priority date | Publication date | Assignee | Title |
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| US9399576B2 (en) * | 2014-01-14 | 2016-07-26 | King Fahd University Of Petroleum And Minerals | 450 nm visible light-induced photosensitized degradation of rhodamine B molecules over BiOBr in aqueous solution |
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|---|---|---|---|---|
| CN104069876A (en) * | 2014-06-24 | 2014-10-01 | 华中师范大学 | Ag-BiOCl compound photocatalyst prepared by depositing nanometer silver on [001] crystal face of BiOCl nanometer sheet and method |
| CN108502926A (en) * | 2018-05-15 | 2018-09-07 | 安徽师范大学 | BiOCl nano-rings and its synthetic method |
| CN108579770A (en) * | 2018-05-15 | 2018-09-28 | 安徽师范大学 | A method of carrying out degradation of contaminant using BiOCl nano-rings |
| CN109759095A (en) * | 2019-01-21 | 2019-05-17 | 陕西科技大学 | A kind of BiOBr hollow fibre, preparation method and its application as photochemical catalyst in light degradation dyestuff |
Non-Patent Citations (2)
| Title |
|---|
| Shape Evolution of Layer-Structured Bismuth Oxychloride Nanostructures via Low-Temperature Chemical Vapor Transport;Hailin Peng et al.;《Chem. Mater.》;20081219;第21卷(第2期);第248-252页 * |
| Understanding size-dependent properties of BiOCl nanosheets and exploring more catalysis;Benxia Li et al.;《Journal of Colloid and Interface Science》;20170620;第505卷;第654-660页 * |
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