CN107638886A - The method that ion-exchange prepares bismoclite/bismuth oxyiodide composite ultra-thin nanometer sheet - Google Patents
The method that ion-exchange prepares bismoclite/bismuth oxyiodide composite ultra-thin nanometer sheet Download PDFInfo
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Abstract
The invention discloses a kind of method that ion-exchange prepares bismoclite/bismuth oxyiodide composite ultra-thin nanometer sheet, five nitric hydrate bismuths and polyvinylpyrrolidone are dissolved in ethylene glycol solution, it is stirred at room temperature to being completely dissolved, saturated nacl aqueous solution is taken to be added in above-mentioned solution, continue stirring and obtain white opacity solution, it is transferred in hydrothermal reaction kettle in 140 180 DEG C of reactions, product bismoclite ultrathin nanometer piece is made then at 60 DEG C of vacuum drying, bismoclite ultrathin nanometer piece is distributed in saturated solution of potassium iodide, 3 12h are stirred in 25 50 DEG C, and target product bismoclite/bismuth oxyiodide composite ultra-thin nanometer sheet is made.Operation is simple and reproducible by the present invention, the bismoclite of synthesis/bismuth oxyiodide composite ultra-thin nanometer sheet has ultra-thin two-dimension structure, specific surface area is big, and bismoclite/bismuth oxyiodide composite ultra-thin nanometer sheet band gap is suitable, photoresponse wider range, thus in optics, electrically and thermally etc. association area has preferable application prospect.
Description
Technical field
The invention belongs to the synthesis technical field of composite photocatalyst material, and in particular to a kind of ion-exchange prepares chlorine oxygen
Change the method for bismuth/bismuth oxyiodide composite ultra-thin nanometer sheet.
Background technology
In recent years, environmental pollution and energy shortage are the significant challenges that current mankind faces.Photocatalysis technology can be direct
Normal-temperature deep reaction is carried out as optical drive using solar energy, therefore with wide in terms of the depollution of environment and new energy development
Development prospect.Using conductor oxidate as catalyst, electric energy and chemical energy are converted light energy into we provide a kind of ideal
Using energy source and environmental pollution improvement method.But subject matter present in Study on photocatalyst is photoproduction
Electron-hole pair recombination probability is high and photoresponse scope is narrower.
Bismuth system catalysis material issues because having special layer structure and narrower energy gap in the irradiation of visible ray
Raw electronics and the separation in hole.Bismuth series photocatalyst mainly includes bismuth oxide, BiOX, the oxysalt of bismuth and multiple at present
Mould assembly bismuth catalyst etc., wherein most representative is BiOX（BiOX, X=F, Cl, Br, I）Series compound, they because
Cheap, photocatalysis performance is high and the advantages such as stability is good, has potential practical value；Bismoclite high anisotropy
Layer structure make it have good, stable photocatalytic activity, but its energy gap is wider；Bismuth oxyiodide band gap is minimum, tool
There are unique Open architecture and the simultaneous structure of indirect transition pattern, be advantageous to hole-electron to efficiently separating
And electric charge transfer, so with very high visible light photocatalysis active.
Application No. CN201210082112.7 patent discloses a kind of preparation of porous bismuth oxyiodide nano-photo catalytic
Method, primarily to solve technical problem of the existing bismuth oxyiodide in visible region light degradation property difference, but party's legal system
Standby process is cumbersome and has used a large amount of organic solvents to be unfavorable for mass producing, and this method is simply prepared for specific surface area slightly in addition
Big bismuth oxyiodide, changes the photocatalysis performance of bismuth oxyiodide not from root, and room for promotion is limited.Publication No.
CN101724839A patent provides the method for preparing BiOCl films using vapour deposition and chemical oxidization method, obtained thin
Film has a flower-like structure, but preparation process need to need special instrument and equipment and high-purity by the processes of physical vapor deposition of complexity
Gas does protection gas, and cost is higher, complex operation.Publication No. CN101857382A patent is anti-using the absorption of continuous ionic layer
Answer legal system to obtain BiOI membrane electrodes, there is application potential in area of solar cell, but this method need to pass through repeatedly
Film needed for being made, operating process are relatively complicated.Publication No. CN102974373 A patent discloses a kind of oxychloride
The preparation method of bismuth/bismuth oxyiodide hetero-junctions visible light catalytic material, there is high catalytic activity and stability mainly for providing
Material, but prepare predecessor bismoclite and take tediously long, later stage and bismuth oxyiodide, which react, will also pass through calcining, the nanometer of formation
Piece is thicker and is unfavorable for efficiently separating for electron-hole.
The content of the invention
Present invention solves the technical problem that it there is provided the ion exchange that a kind of preparation technology is simple and condition is easily controllable
Method prepares the method for bismoclite/bismuth oxyiodide composite ultra-thin nanometer sheet, obtained bismoclite/bismuth oxyiodide composite
With ultra-thin two-dimension nanostructured, there is larger specific surface area, surface atom exposure is more, is advantageous to photo-generate electron-hole
To generation and separation.
The present invention adopts the following technical scheme that ion-exchange prepares bismoclite/iodine oxygen to solve above-mentioned technical problem
Change the method for bismuth composite ultra-thin nanometer sheet, it is characterised in that concretely comprise the following steps：By the nitric hydrate bismuths of 0.2-0.6g five and 0.3-
0.8g polyvinylpyrrolidones are dissolved in 25mL ethylene glycol solutions, are stirred at room temperature to being completely dissolved, and take 5mL saturated nacl aqueous solutions
It is added in above-mentioned solution, continues stirring and obtain white opacity solution, gained white opacity solution is transferred to hydrothermal reaction kettle
In in 140-180 DEG C react 3-6h, be cooled to centrifugation after room temperature and the white precipitate for reacting generation used into deionized water and second respectively
Alcohol washs, and product bismoclite ultrathin nanometer piece is made then at 60 DEG C of vacuum drying, then takes the oxychloride obtained by 0.1-2g
Bismuth ultrathin nanometer piece is distributed in 10-50mL saturated solution of potassium iodide, and stirring 3-12h in 25-50 DEG C is made target product chlorine oxygen
Change bismuth/bismuth oxyiodide composite ultra-thin nanometer sheet.
Further preferably, the preparation method of the bismoclite/bismuth oxyiodide composite ultra-thin nanometer sheet, it is characterised in that tool
Body step is：The nitric hydrate bismuths of 0.486g five and 0.4g polyvinylpyrrolidones are dissolved in 25mL ethylene glycol solutions, room temperature is stirred
Mix to dissolving completely, take 5mL saturated nacl aqueous solutions to be added in above-mentioned solution, continue stirring and obtain white opacity solution, will
Gained white opacity solution is transferred in hydrothermal reaction kettle reacts 3h in 160 DEG C, and generation will be reacted by being cooled to centrifugation after room temperature
White precipitate is washed with deionized water and ethanol respectively, and the ultra-thin bismoclite nanometer sheet of product is made then at 60 DEG C of vacuum drying,
Then the bismoclite ultrathin nanometer piece obtained by 0.1-2g is taken to be distributed in 10-50mL saturated solution of potassium iodide, in 25-50 DEG C
Stir 3-12h and target product bismoclite/iodine oxidation composite ultra-thin nanometer sheet is made.
The present invention has the advantages that compared with prior art：Operation is simple and reproducible by the present invention, closes
Into bismoclite/bismuth oxyiodide composite ultra-thin nanometer sheet there is ultra-thin two-dimension structure, specific surface area is big, and bismoclite/iodine
Bismuth oxide composite ultra-thin nanometer sheet band gap is suitable, photoresponse wider range, thus in optics, the association area tool such as electrically and thermally
There is preferable application prospect.
Brief description of the drawings
Fig. 1 be comparative example 1 be made bismoclite ultrathin nanometer piece SEM figure, picture multiplication factor be respectively 20000 times and
5000 times；
Fig. 2 is the SEM figures that bismoclite/bismuth oxyiodide composite ultra-thin nanometer sheet is made in embodiment 1, and picture multiplication factor is respectively
2000 times and 10000 times；
Fig. 3 is that bismoclite ultrathin nanometer piece is made in comparative example 1 and bismoclite/bismuth oxyiodide composite ultra-thin is made in embodiment 1
The XRD of nanometer sheet.
Embodiment
The above of the present invention is described in further details by the following examples, but this should not be interpreted as to this
The scope for inventing above-mentioned theme is only limitted to following embodiment, and all technologies realized based on the above of the present invention belong to this hair
Bright scope.
Embodiment 1
The nitric hydrate bismuths of 0.486g five and 0.4g polyvinylpyrrolidones are dissolved in 25mL ethylene glycol solutions, are stirred at room temperature to molten
Solution is complete, takes 5mL saturated nacl aqueous solutions to be slowly added into above-mentioned solution, continues stirring and obtain white opacity solution, by institute
White opacity solution is transferred in hydrothermal reaction kettle and reacts 3h in 160 DEG C, the white of generation will be reacted by being cooled to centrifugation after room temperature
Color precipitation is washed with deionized water and ethanol respectively, product bismoclite ultrathin nanometer piece is made then at 60 DEG C of vacuum drying, so
Take the bismoclite ultrathin nanometer piece obtained by 0.1g to be distributed in 15mL saturated solution of potassium iodide afterwards, be stirred at room temperature 3h after
Target product bismoclite/bismuth oxyiodide composite ultra-thin nanometer sheet BOC/BOI-NS1 is made in 60 DEG C of vacuum drying.
Embodiment 2
The nitric hydrate bismuths of 0.486g five and 0.4g polyvinylpyrrolidones are dissolved in 25mL ethylene glycol solutions, are stirred at room temperature to molten
Solution is complete, takes 5mL saturated nacl aqueous solutions to be slowly added into above-mentioned solution, continues stirring and obtain white opacity solution, by institute
White opacity solution is transferred in hydrothermal reaction kettle and reacts 3h in 160 DEG C, the white of generation will be reacted by being cooled to centrifugation after room temperature
Color precipitation is washed with deionized water and ethanol respectively, product bismoclite ultrathin nanometer piece is made then at 60 DEG C of vacuum drying, so
The bismoclite ultrathin nanometer piece obtained by 0.5g is taken to be distributed in 50mL saturated solution of potassium iodide afterwards, in 40 DEG C of stirred in water bath
Target product bismoclite/bismuth oxyiodide composite ultra-thin nanometer sheet BOC/BOI-NS2 is made after 60 DEG C of vacuum drying in 6h.
Embodiment 3
The nitric hydrate bismuths of 0.486g five and 0.4g polyvinylpyrrolidones are dissolved in 25mL ethylene glycol solutions, are stirred at room temperature to molten
Solution is complete, takes 5mL saturated nacl aqueous solutions to be slowly added into above-mentioned solution, continues stirring and obtain white opacity solution, by institute
White opacity solution is transferred in hydrothermal reaction kettle and reacts 3h in 160 DEG C, the white of generation will be reacted by being cooled to centrifugation after room temperature
Color precipitation is washed with deionized water and ethanol respectively, product bismoclite ultrathin nanometer piece is made then at 60 DEG C of vacuum drying, so
The bismoclite ultrathin nanometer piece obtained by 2g is taken to be distributed in 50mL saturated solution of potassium iodide afterwards, in 50 DEG C of stirred in water bath
Target product bismoclite/bismuth oxyiodide composite ultra-thin nanometer sheet BOC/BOI-NS3 is made after 60 DEG C of vacuum drying in 12h.
Comparative example 1
The nitric hydrate bismuths of 0.486g five and 0.4g polyvinylpyrrolidones are dissolved in 25mL ethylene glycol solutions, are stirred at room temperature to molten
Solution is complete, takes 5mL saturated nacl aqueous solutions to be slowly added into above-mentioned solution, continues stirring and obtain white opacity solution, by institute
White opacity solution is transferred in hydrothermal reaction kettle and reacts 3h in 160 DEG C, the white of generation will be reacted by being cooled to centrifugation after room temperature
Color precipitation is washed with deionized water and ethanol respectively, and product bismoclite ultrathin nanometer piece BOC is made then at 60 DEG C of vacuum drying.
Embodiment above describes the general principle of the present invention, main features and advantages, the technical staff of the industry should
Understand, the present invention is not limited to the above embodiments, the original for simply illustrating the present invention described in above-described embodiment and specification
Reason, under the scope for not departing from the principle of the invention, various changes and modifications of the present invention are possible, and these changes and improvements are each fallen within
In the scope of protection of the invention.
Claims (2)
1. the method that ion-exchange prepares bismoclite/bismuth oxyiodide composite ultra-thin nanometer sheet, it is characterised in that specific steps
For：The nitric hydrate bismuths of 0.2-0.6g five and 0.3-0.8g polyvinylpyrrolidones are dissolved in 25mL ethylene glycol solutions, room temperature is stirred
Mix to being completely dissolved, take 5mL saturated nacl aqueous solutions to be added in above-mentioned solution, continue stirring and obtain white opacity solution, will
Gained white opacity solution is transferred in hydrothermal reaction kettle reacts 3-6h in 140-180 DEG C, and centrifugation will reaction after being cooled to room temperature
The white precipitate of generation is washed with deionized water and ethanol respectively, is made that product bismoclite is ultra-thin to be received then at 60 DEG C of vacuum drying
Rice piece, then takes the bismoclite ultrathin nanometer piece obtained by 0.1-2g to be distributed in 10-50mL saturated solution of potassium iodide, in
Target product bismoclite/bismuth oxyiodide composite ultra-thin nanometer sheet is made in 25-50 DEG C of stirring 3-12h.
2. the method that ion-exchange according to claim 1 prepares bismoclite/bismuth oxyiodide composite ultra-thin nanometer sheet,
It is characterized in that concretely comprise the following steps：It is molten that the nitric hydrate bismuths of 0.486g five and 0.4g polyvinylpyrrolidones are dissolved in 25mL ethylene glycol
In liquid, it is stirred at room temperature to dissolving completely, takes 5mL saturated nacl aqueous solutions to be added in above-mentioned solution, continue stirring and obtain white
Turbid solution, gained white opacity solution is transferred in hydrothermal reaction kettle and reacts 3h in 160 DEG C, centrifugation will after being cooled to room temperature
The white precipitate of reaction generation is washed with deionized water and ethanol respectively, and the ultra-thin oxychloride of product is made then at 60 DEG C of vacuum drying
Bismuth nanometer sheet, the bismoclite ultrathin nanometer piece obtained by 0.1-2g is then taken to be distributed in 10-50mL saturated solution of potassium iodide,
3-12h is stirred in 25-50 DEG C, and target product bismoclite/iodine oxidation composite ultra-thin nanometer sheet is made.
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Cited By (4)
| Publication number | Priority date | Publication date | Assignee | Title |
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| CN108906085A (en) * | 2018-07-17 | 2018-11-30 | 河南师范大学 | A kind of Bi2S3The preparation method and applications of/BiOBr composite photocatalyst material |
| CN109621990A (en) * | 2018-06-14 | 2019-04-16 | 河南师范大学 | A kind of preparation method of three-dimensional structure bismuth oxychloride@bismuth oxybromide composite ultra-thin nanometer sheet |
| CN114839760A (en) * | 2022-05-06 | 2022-08-02 | 深圳市华科创智技术有限公司 | Light valve and preparation method thereof |
| CN115845882A (en) * | 2022-11-17 | 2023-03-28 | 北京师范大学 | Double-vacancy and interface electric field synergistic ultrathin nanosheet and preparation method and application thereof |
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| CN102974373A (en) * | 2012-12-24 | 2013-03-20 | 山东大学 | Visible-light photocatalytic material and preparation method thereof |
| CN103752332A (en) * | 2014-01-22 | 2014-04-30 | 玉林师范学院 | Dried persimmon-shaped visible-light-driven photocatalyst BiOBr and preparation method thereof |
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| CN102974373A (en) * | 2012-12-24 | 2013-03-20 | 山东大学 | Visible-light photocatalytic material and preparation method thereof |
| CN103752332A (en) * | 2014-01-22 | 2014-04-30 | 玉林师范学院 | Dried persimmon-shaped visible-light-driven photocatalyst BiOBr and preparation method thereof |
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| HAILI LIN, ET AL: "Facile anion-exchange synthesis of BiOI/BiOBr composite with enhanced photoelectrochemical and photocatalytic properties", 《CERAMICS INTERNATIONAL》 * |
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Cited By (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN109621990A (en) * | 2018-06-14 | 2019-04-16 | 河南师范大学 | A kind of preparation method of three-dimensional structure bismuth oxychloride@bismuth oxybromide composite ultra-thin nanometer sheet |
| CN108906085A (en) * | 2018-07-17 | 2018-11-30 | 河南师范大学 | A kind of Bi2S3The preparation method and applications of/BiOBr composite photocatalyst material |
| CN114839760A (en) * | 2022-05-06 | 2022-08-02 | 深圳市华科创智技术有限公司 | Light valve and preparation method thereof |
| CN115845882A (en) * | 2022-11-17 | 2023-03-28 | 北京师范大学 | Double-vacancy and interface electric field synergistic ultrathin nanosheet and preparation method and application thereof |
| CN115845882B (en) * | 2022-11-17 | 2024-03-15 | 北京师范大学 | Ultrathin nanosheet with cooperation of double vacancies and interfacial electric field as well as preparation method and application thereof |
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