CN104588045A - Ultra-thin BiOCl nano-sheet, preparation method and application thereof - Google Patents
Ultra-thin BiOCl nano-sheet, preparation method and application thereof Download PDFInfo
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- CN104588045A CN104588045A CN201510019624.2A CN201510019624A CN104588045A CN 104588045 A CN104588045 A CN 104588045A CN 201510019624 A CN201510019624 A CN 201510019624A CN 104588045 A CN104588045 A CN 104588045A
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Abstract
The invention relates to an ultra-thin BiOCl nano-sheet, a preparation method and application of the nano-sheet. The preparation method comprises the following steps: (1) respectively dissolving Bi(NO3)3.5H2O and Na2C3O4 in water; (2) adding a Na2C2O4 solution to a Bi(NO3)3 solution and stirring; (3) reacting an obtained mixed solution; (4) cooling; (5) drying; (6) calcining; (7) dissolving Bi2O3 in an HCl solution; (8) reacting an obtained mixed solution; (9) cooling; and (10) drying to obtain an ultra-thin BiOCl nano-sheet. The preparation method disclosed by the invention is simple and can be used for regulating the size range of nanoparticles by controlling the quantity of HCl, so as to regulate the active exposure faces and the specific surface areas of the nanoparticles. The BiOCl ultra-thin nano-sheet prepared by the method disclosed by the invention, under the irradiation of simulated sunlight or visible light, has good photocatalytic degradation effect on rhodamine (RhB) dye.
Description
Technical field
The present invention relates to a kind of ultra-thin BiOCl nanometer sheet, preparation method and its usage.
Background technology
Photocatalysis technology directly converts solar energy into chemical energy and electric energy by semi-conducting material, and permineralization degraded can be realized to poisonous and harmful organic pollution in environment, be considered to solve one of the human society energy and the potential technical scheme of environmental problem most at present.In recent years, Chinese scholars have developed many novel photocatalysis materials, wherein, Typical Representative oxyhalogen secret system BiOX (X=Cl in lamellar compound, Br, I) catalysis material, especially the BiOCl of layer structure has sufficient space and comes polarized atom and atomic orbital, impel induce dipole moment can separate electronic and hole effectively, thus raising photocatalysis performance, cause BiOCl to have good photocatalytic activity and stability, thus cause the very big concern of the domestic and international scientist of photocatalysis field.The main preparation methods of current micro-nano BiOCl photocatalysis material Tu has: the hot method of Hydrolyze method, solvent-thermal method, alcohol, reverse microemulsion method etc.But want prepared Particle size control a few nanometer or tens nanometers still very difficult.There is certain relevance in the separative efficiencies of factor to its spectral response range and photo-generated carrier such as the structure and morphology of catalysis material, specific area, crystal face are active.The pattern of Effective Regulation BiOCl photocatalytic material, size, micro-structural and vast scale expose active face, greatly can improve the photocatalytic activity of BiOCl.But this area does not also have the ripe preparation method of BiOCl nanometer sheet.
Summary of the invention
The object of this invention is to provide a kind of method of simple, the effective ultra-thin BiOCl nanometer sheet of controlled synthesis.Another object of the present invention is to provide a kind of photocatalytic applications of ultra-thin BiOCl nanometer sheet, and concrete technical scheme is as follows:
A preparation method for ultra-thin BiOCl nanometer sheet, comprises the steps:
(1) by Bi (NO
3)
35H
2o and Na
2c
2o
4soluble in water respectively;
(2) by Na
2c
2o
4solution joins Bi (NO
3)
3to stir in solution;
(3) mixed solution obtained is reacted;
(4) cool;
(5) dry;
(6) calcine;
(7) Bi is got
2o
3be dissolved in HCl solution;
(8) mixed solution obtained is reacted;
(9) cool;
(10) drying obtains ultra-thin BiOCl nanometer sheet.
Further, in step (1), by 1 ~ 5g Bi (NO
3)
35H
2o and 1 ~ 5g Na
2c
2o
4to be dissolved in respectively in 10-30mL distilled water and ultrasonic.
Further, in step (3), in the mixed solution transfer polytetrafluoroethylene (PTFE) reactor obtained, at 100-150 DEG C, react 20-60h.
Further, in step (4) and/or (9), room temperature is naturally cooled to.
Further, in step (5) and/or (10), wash rear 60 DEG C of dry 6h for several times respectively with distilled water and absolute ethyl alcohol.
Further, in step (6), the sample obtained in atmosphere 300-600 DEG C of calcining 2h obtains Bi
2o
3.
Further, in step (7), 0 ~ 0.5g Bi is got
2o
3be dissolved in ultrasonic 3-10min in the HCl solution of 10-40ml 4 ~ 16mmol/L, stir 1h.
Further, in step (8), in the mixed solution transfer polytetrafluoroethylene (PTFE) reactor obtained, at 130-200 DEG C, react 10-20h.
A kind of ultra-thin BiOCl nanometer sheet, adopts above-mentioned method to prepare.
The purposes of above-mentioned ultra-thin BiOCl nanometer sheet, for carrying out photocatalytic degradation to rhodamine (RhB) dyestuff.
Compared with currently available technology, preparation method provided by the invention is simple, and can be regulated and controled the size range of nano particle by the amount of control HCl, thus the active exposure of modulation nano particle and specific area.The BiOCl ultrathin nanometer sheet adopting the inventive method to prepare, under simulated solar irradiation or radiation of visible light, has extraordinary photocatalytic degradation effect to rhodamine (RhB) dyestuff.
Accompanying drawing explanation
Fig. 1 is: (a) Bi
2o
3, (f) BiOCl standard card figure, (b) Bi
2o
3, (c) S1, (d) S2, (e) S3 XRD figure;
The SEM that Fig. 2 (A) is Bi2O3 schemes;
The SEM that Fig. 2 (B) is S1 schemes;
The SEM that Fig. 2 (C) is S2 schemes;
The SEM that Fig. 2 (D) is S3 schemes;
Fig. 3 (A) is the TEM photo of ultra-thin BiOCl nanometer sheet (S1);
Fig. 3 (B) is the HRTEM photo of ultra-thin BiOCl nanometer sheet (S1);
Fig. 3 (C) is the atomic diagram of ultra-thin BiOCl nanometer sheet (S1);
Fig. 3 (D) is the crystal growth orientation of ultra-thin BiOCl nanometer sheet (S1);
Fig. 4 is the XPS figure of ultra-thin BiOCl nanometer sheet (S1);
Fig. 5 is ultra-thin BiOCl nanometer sheet formation mechenism figure;
Fig. 6 (A) is S1 ultraviolet-ray visible absorbing collection of illustrative plates to RhB degradation effect under simulated solar irradiation;
Fig. 6 (B) is S1, S2 and S3 degradation effect figure to RhB under simulated solar irradiation;
The ultra-thin BiOCl nanometer sheet of Fig. 7 (A) under simulated solar light action to RhB dyestuff circulation degradation experiment;
Fig. 7 (B) is the XRD diffraction pattern recycling rear ultra-thin BiOCl nanometer sheet for 4 times;
Fig. 8 (A) is for S1 is under visible light to the ultraviolet-ray visible absorbing collection of illustrative plates of RhB degradation effect;
Fig. 8 (B) is for S1, S2 and S3 are under visible light to the degradation effect figure of RhB.
Detailed description of the invention
Describe the present invention with reference to the accompanying drawings below, it is a kind of preferred embodiment in numerous embodiments of the present invention.
By 1 ~ 5g Bi (NO
3)
35H
2o and 1 ~ 5g Na
2c
2o
4be dissolved in 10-30mL distilled water ultrasonic respectively, then by Na
2c
2o
4solution joins Bi (NO
3)
3vigorous stirring in solution, in the mixed solution obtained transfer polytetrafluoroethylene (PTFE) reactor, reacts 20-60h, naturally cools to room temperature at 100-150 DEG C.The product distilled water obtained and absolute ethyl alcohol wash rear 60 DEG C of dry 6h for several times respectively.The sample obtained in atmosphere 300-600 DEG C of calcining 2h obtains Bi
2o
3.
Get 0 ~ 0.5g Bi
2o
3be dissolved in ultrasonic 3-10min in the HCl solution of 10-40ml 4 ~ 16mmol/L, stir 1h, in the mixed solution obtained transfer polytetrafluoroethylene (PTFE) reactor, at 130-200 DEG C, react 10-20h, naturally cool to room temperature.The product distilled water obtained and absolute ethyl alcohol wash rear 60 DEG C of dry 6h for several times respectively, add HCl concentration three samples from less to more called after S1, S2 and S3 respectively.
Fig. 1 can find out that S1, S2 and the S3 obtained is pure BiOCl.Fig. 2 can find out that S1 is ultra-thin laminated structure, and along with the increase of HCl concentration, the thickness of BiOCl nanometer sheet increases.Know from Fig. 5, ultra-thin BiOCl nanometer sheet only has and could be formed under given conditions.99%, S1 photocatalysis efficiency can be reached far away higher than S2 and S3 to the degradation rate of RhB see Fig. 6, S1 catalytic degradation 10min.As can be seen from Figure 7, ultra-thin BiOCl nanometer sheet has good reusing and photostability.Excellent photocatalytic degradation effect is still shown under visible light illumination see Fig. 8, S1 sample.
Above by reference to the accompanying drawings to invention has been exemplary description; obvious specific implementation of the present invention is not subject to the restrictions described above; as long as have employed the various improvement that method of the present invention is conceived and technical scheme is carried out; or directly apply to other occasion, all within protection scope of the present invention without improving.
Claims (10)
1. a preparation method for ultra-thin BiOCl nanometer sheet, is characterized in that, comprise the steps:
(1) by Bi (NO
3)
35H
2o and Na
2c
2o
4soluble in water respectively;
(2) by Na
2c
2o
4solution joins Bi (NO
3)
3to stir in solution;
(3) mixed solution obtained is reacted;
(4) cool;
(5) dry;
(6) calcine;
(7) Bi is got
2o
3be dissolved in HCl solution;
(8) mixed solution obtained is reacted;
(9) cool;
(10) drying obtains ultra-thin BiOCl nanometer sheet.
2. the preparation method of ultra-thin BiOCl nanometer sheet as claimed in claim 1, is characterized in that, in step (1), by 1 ~ 5gBi (NO
3)
35H
2o and 1 ~ 5g Na
2c
2o
4to be dissolved in respectively in 10-30mL distilled water and ultrasonic.
3. the preparation method of ultra-thin BiOCl nanometer sheet as claimed in claim 1 or 2, is characterized in that, in step (3), in the mixed solution transfer polytetrafluoroethylene (PTFE) reactor obtained, at 100-150 DEG C, reacts 20-60h.
4. the preparation method of the ultra-thin BiOCl nanometer sheet according to any one of claim 1-3, is characterized in that, in step (4) and/or (9), naturally cools to room temperature.
5. the preparation method of the ultra-thin BiOCl nanometer sheet according to any one of claim 1-4, is characterized in that, in step (5) and/or (10), washs rear 60 DEG C of dry 6h for several times respectively with distilled water and absolute ethyl alcohol.
6. the preparation method of the ultra-thin BiOCl nanometer sheet according to any one of claim 1-5, is characterized in that, in step (6), the sample obtained in atmosphere 300-600 DEG C of calcining 2h obtains Bi
2o
3.
7. the preparation method of the ultra-thin BiOCl nanometer sheet according to any one of claim 1-6, is characterized in that, in step (7), gets 0 ~ 0.5g Bi
2o
3be dissolved in ultrasonic 3-10min in the HCl solution of 10-40ml 4 ~ 16mmol/L, stir 1h.
8. the preparation method of the ultra-thin BiOCl nanometer sheet according to any one of claim 1-7, is characterized in that, in step (8), in the mixed solution transfer polytetrafluoroethylene (PTFE) reactor obtained, at 130-200 DEG C, reacts 10-20h.
9. a ultra-thin BiOCl nanometer sheet, is characterized in that, adopts the method as described in claim 1-8 to prepare.
10. the purposes of ultra-thin BiOCl nanometer sheet as claimed in claim 9, is characterized in that, for carrying out photocatalytic degradation to rhodamine (RhB) dyestuff.
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Cited By (8)
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|---|---|---|---|---|
| CN106268877A (en) * | 2016-08-09 | 2017-01-04 | 石家庄中实验学校 | A kind of BiOCl with visible light catalysis activity and preparation method thereof |
| CN106669741A (en) * | 2015-11-11 | 2017-05-17 | 孙文彬 | Visual light driven semiconductor photocatalyst as well as preparation method and application thereof |
| CN106732327A (en) * | 2016-11-24 | 2017-05-31 | 陕西科技大学 | A kind of mesoporous BiOCl/Bi2O3Composite granule and its preparation method and application |
| CN107904660A (en) * | 2017-09-25 | 2018-04-13 | 北京航空航天大学 | Bismuth oxygen chlorine method for preparing single crystal |
| CN108502926A (en) * | 2018-05-15 | 2018-09-07 | 安徽师范大学 | BiOCl nano-rings and its synthetic method |
| CN110560097A (en) * | 2019-09-30 | 2019-12-13 | 中国科学院青岛生物能源与过程研究所 | Method for preparing BiOCl ultrathin nanosheets under mild conditions and application thereof |
| CN112058246A (en) * | 2020-09-09 | 2020-12-11 | 天津城建大学 | Micro-nano Fe3O4@ BiOCl composite material and synthesis method thereof |
| CN113479934A (en) * | 2021-07-28 | 2021-10-08 | 中国科学院上海硅酸盐研究所 | BiOCl nanosheet and preparation method and application thereof |
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| CN102220637A (en) * | 2011-05-31 | 2011-10-19 | 国家纳米科学中心 | Micron/nanometer hierarchical structure of BiOCl, BiOBr and Bi2S3 |
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Cited By (10)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN106669741A (en) * | 2015-11-11 | 2017-05-17 | 孙文彬 | Visual light driven semiconductor photocatalyst as well as preparation method and application thereof |
| CN106268877A (en) * | 2016-08-09 | 2017-01-04 | 石家庄中实验学校 | A kind of BiOCl with visible light catalysis activity and preparation method thereof |
| CN106732327A (en) * | 2016-11-24 | 2017-05-31 | 陕西科技大学 | A kind of mesoporous BiOCl/Bi2O3Composite granule and its preparation method and application |
| CN107904660A (en) * | 2017-09-25 | 2018-04-13 | 北京航空航天大学 | Bismuth oxygen chlorine method for preparing single crystal |
| CN108502926A (en) * | 2018-05-15 | 2018-09-07 | 安徽师范大学 | BiOCl nano-rings and its synthetic method |
| CN108502926B (en) * | 2018-05-15 | 2019-11-05 | 安徽师范大学 | BiOCl nano-rings and its synthetic method |
| CN110560097A (en) * | 2019-09-30 | 2019-12-13 | 中国科学院青岛生物能源与过程研究所 | Method for preparing BiOCl ultrathin nanosheets under mild conditions and application thereof |
| CN112058246A (en) * | 2020-09-09 | 2020-12-11 | 天津城建大学 | Micro-nano Fe3O4@ BiOCl composite material and synthesis method thereof |
| CN113479934A (en) * | 2021-07-28 | 2021-10-08 | 中国科学院上海硅酸盐研究所 | BiOCl nanosheet and preparation method and application thereof |
| CN113479934B (en) * | 2021-07-28 | 2023-07-07 | 中国科学院上海硅酸盐研究所 | BiOCl nano-sheet and preparation method and application thereof |
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Application publication date: 20150506 |