CN102218315A - Preparation method of porous composite Ag-doped zinc oxide photocatalyst - Google Patents
Preparation method of porous composite Ag-doped zinc oxide photocatalyst Download PDFInfo
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- CN102218315A CN102218315A CN2010101502670A CN201010150267A CN102218315A CN 102218315 A CN102218315 A CN 102218315A CN 2010101502670 A CN2010101502670 A CN 2010101502670A CN 201010150267 A CN201010150267 A CN 201010150267A CN 102218315 A CN102218315 A CN 102218315A
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Abstract
The invention aims at overcoming the defect that the nano-Ag has active property and providing a preparation method of Ag-ZnO composite porous photocatalyst. The preparation method comprises the following steps of preparing mixed metal oxalate by a codeposition method under the condition of room temperature, taking the mixed metal oxalate as a former body; and subsequently carrying out the processing such as roasting, placing the mixed metal oxalate in the air under the room temperature and the like, thus preparing the Ag-ZnO composite porous photocatalyst. The preparation method has a simple production method and low cost; and the Ag-doped zinc oxide composite photocatalyst has the advantages of uniform particle size and good activity. The Ag-doped zinc oxide composite photocatalyst prepared by the method has wood-block shaped particles and coarse surface, has the length of about 4 mcirons, the width of about 1.5 to 2 microns and the height of about 1.5 to 2 microns, and can be used for the production of semiconductor materials, and the like.
Description
[technical field]
The present invention relates to a kind of environment and technical field of semiconductors, specifically is the preparation method of the compound silver-doped zinc oxide photochemical catalyst of a kind of porous.
[background technology]
Zinc oxide is a kind of the have novel broad stopband of excellent performance, semi-conducting material of high excitation energy, and special electronic structure makes it have effects such as excellent electricity, magnetic, light.Zinc oxide is compared with titanium dioxide, and the two energy gap is suitable, but the zinc oxide production technology is simple, with low cost, therefore becomes the photocatalytic semiconductor material that is widely studied at present.Yet that zinc oxide semiconductor material exists is narrow as spectral response range, the easy shortcoming such as compound of greater band gap, electron-hole pair, causes photocatalysis efficiency not high, thereby has limited its application.At zinc oxide particle surface depositing noble metal is a kind of efficient semiconductor photochemical catalyst method of modifying, the electron distributions of the doping of noble metal in can the change system, make Nano semiconductor produce lattice defect and impurity energy level, thereby improve photo-quantum efficiency, improve redox ability, enlarge the spectral absorption scope.The precious metal doping semiconductor energy effectively improves separating of photogenerated charge and photohole, is a focus in the current photochemical catalyst study on the modification.In the present research, the main synthetic method of silver doped zinc oxide composite photo-catalyst has hydro-thermal method, LASER HEATING method, dipping photodissociation method, flame atomizing pyrolysismethod and photochemical precipitation method etc.Wherein, adopt the flame atomizing method to prepare the nano-photocatalyst material of high-ratio surface; The one-dimension zinc oxide nanostructured of carrying silver can be synthetic by one step of solvent thermal process; The surface plasma effect of Ag nano particle is applied to the zinc oxide semi-conductor photocatalysis, has improved the photocatalysis stability and the catalysis of catalysis material greatly.
[summary of the invention]
The character that the objective of the invention is to overcome nanometer Ag is more active, in air, be easy to oxidized existing synthetic method, provide a kind of coprecipitation to prepare the hybrid metal oxalates at ambient temperature, and reveal to put by roasting and air at room temperature as presoma and wait processing, prepare the compound porous photochemical catalyst of Ag-ZnO.Production method of the present invention is simple, and is with low cost; Silver doped zinc oxide composite photo-catalyst of the present invention has uniform particle diameter, active good characteristic.
The present invention is achieved by the following technical solutions:
Silver doped zinc oxide composite photo-catalyst coprecipitation preparation method involved in the present invention comprises the steps:
Step 1 is the solution of some with zinc sulfate hydrate and silver nitrate preparation certain volume metal ion total concentration;
Step 2 adds isopyknic oxalic acid solution under the magnetic agitation condition in the solution of step 1 gained;
Step 3, the system stirring certain hour with the step 2 gained leaves standstill suction filtration;
Step 4 places insulating box with suction filtration products obtained therefrom in the step 3, and dry at a certain temperature certain hour makes its bone dry;
Step 5 moves into the powder of drying in the step 4 in the Muffle furnace time of roasting one fixed length under design temperature;
Step 6, sample is sprawled in leave standstill certain hour on the filter paper under air atmosphere and had both been got product after the calcining of step 5 gained.
Wherein
In the step 1, described mixed solution concentration is 0.020-0.040mol/l.
In the step 1, the volume of described mixed solution is 200ml-500ml.
In the step 2, make in the described solution that the ratio of silver, zinc metal cation amount of substance is 0.03-0.06.
In the step 3, the solution mixing time is at 30min-90min, and time of repose is at 2h-4h.
In the step 4, calorstat temperature is at 80 ℃-120 ℃, and drying time is at 1.5h-4h.
In the step 5, muffle furnace is controlled at 300 ℃-700 ℃, and calcination time is at 2h-3h.
The present invention has following beneficial effect: its composite Nano Zinc oxide powder crystalline size homogeneous, and active good, have the characteristic of loose structure; Simultaneously, preparation method of the present invention is simple, and the energy has been saved in operation easily, and more safe and reliable.
[specific embodiment]
The invention will be further described below in conjunction with embodiment.Production technology of the present invention is to implement easily to this professional people.Present embodiment has provided detailed embodiment and process being to implement under the prerequisite with the technical solution of the present invention, but protection scope of the present invention is not limited to following embodiment.The experimental technique of unreceipted actual conditions in the following example, usually according to normal condition, or the condition of advising according to manufacturer.
Embodiment
With six water zinc sulphates and silver nitrate preparing metal total ion concentration is the solution 200mL of 0.025moL/L.
Adding waits the oxalic acid solution 200mL of amount of substance under the magnetic agitation, and wherein the ratio of silver, zinc metal cation amount of substance is 0.035.
Solution leaves standstill 2h, suction filtration after stirring 30min.
With gained sample 100 ℃ of dry 2h in insulating box.
Drying sample places in the Muffle furnace at 450 ℃ of following roasting 2h.
Sample is sprawled to reveal in the air atmosphere on filter paper and was put 1 day after the roasting.
The silver doped zinc oxide composite photo-catalyst particle that present embodiment obtains presents " wooden unit " shape, and rough surface is about 4 microns, wide, high each about 1.5～2 microns.
Utilize said method can prepare silver doped zinc oxide composite photo-catalyst powder, and reach its distinctive beneficial effect.
Claims (8)
1. the present invention is the preparation method of the compound silver-doped zinc oxide photochemical catalyst of a kind of porous.Zinc oxide product of the present invention has good photocatalytic, and the silver doped zinc oxide composite photo-catalyst particle that obtains presents " wooden unit " shape, and rough surface is about 4 microns, wide, high each about 1.5～2 microns.
2. the preparation method of the compound silver-doped zinc oxide photochemical catalyst of a kind of porous according to claim 1 comprises the steps:
Step 1 is the solution of some with zinc sulfate hydrate and silver nitrate preparation certain volume metal ion total concentration;
Step 2 adds isopyknic oxalic acid solution under the magnetic agitation condition in the solution of step 1 gained;
Step 3, the system stirring certain hour with the step 2 gained leaves standstill suction filtration;
Step 4 places insulating box with suction filtration products obtained therefrom in the step 3, and dry at a certain temperature certain hour makes its bone dry;
Step 5 moves into the powder of drying in the step 4 in the Muffle furnace time of roasting one fixed length under design temperature;
Step 6, sample is sprawled in leave standstill certain hour on the filter paper under air atmosphere and had both been got product after the calcining of step 5 gained.
3. the preparation method of the compound silver-doped zinc oxide photochemical catalyst of a kind of porous according to claim 2 is characterized in that in the step 1 that described mixed solution concentration is 0.020-0.040mol/l.
4. the preparation method of the compound silver-doped zinc oxide photochemical catalyst of a kind of porous according to claim 2 is characterized in that in the step 1 that the volume of described mixed solution is 200ml-500ml.
5. the preparation method of the compound silver-doped zinc oxide photochemical catalyst of a kind of porous according to claim 2 is characterized in that in the step 2, makes in the described solution that the ratio of silver, zinc metal cation amount of substance is 0.03-0.06.
6. the preparation method of the compound silver-doped zinc oxide photochemical catalyst of a kind of porous according to claim 2 is characterized in that in the step 3 that the solution mixing time is at 30min-90min, and time of repose is at 2h-4h.
7. the preparation method of the compound silver-doped zinc oxide photochemical catalyst of a kind of porous according to claim 2 is characterized in that in the step 4, and calorstat temperature is at 80 ℃-120 ℃, and drying time is at 1.5h-4h.
8. the preparation method of the compound silver-doped zinc oxide photochemical catalyst of a kind of porous according to claim 2 is characterized in that in the step 5, and muffle furnace is controlled at 300 ℃-700 ℃, and calcination time is at 2h-3h.
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| Application Number | Priority Date | Filing Date | Title |
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| CN2010101502670A CN102218315A (en) | 2010-04-16 | 2010-04-16 | Preparation method of porous composite Ag-doped zinc oxide photocatalyst |
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| CN2010101502670A CN102218315A (en) | 2010-04-16 | 2010-04-16 | Preparation method of porous composite Ag-doped zinc oxide photocatalyst |
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Cited By (6)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN102553587A (en) * | 2011-11-11 | 2012-07-11 | 西华师范大学 | Ag/ZnO-SnO2 composite nanocatalyst and production method thereof |
| TWI494159B (en) * | 2012-11-02 | 2015-08-01 | Ind Tech Res Inst | Photocatalyst material and method for fabricating the same |
| US9724675B2 (en) | 2012-11-02 | 2017-08-08 | Industrial Technology Research Institute | Photocatalyst material and method for fabricating the same |
| CN108993501A (en) * | 2018-08-09 | 2018-12-14 | 苏州汉力新材料有限公司 | A kind of silver-silver oxide-zinc oxide photocatalysis material preparation method |
| CN111018365A (en) * | 2019-12-30 | 2020-04-17 | 黑龙江省科学院高技术研究院 | Method for in-situ preparation of silver nanoparticle loaded ZnO nano-foam |
| CN115246709A (en) * | 2022-08-01 | 2022-10-28 | 河北浩锐陶瓷制品有限公司 | High-flatness ceramic tile and production process thereof |
-
2010
- 2010-04-16 CN CN2010101502670A patent/CN102218315A/en active Pending
Cited By (7)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN102553587A (en) * | 2011-11-11 | 2012-07-11 | 西华师范大学 | Ag/ZnO-SnO2 composite nanocatalyst and production method thereof |
| CN102553587B (en) * | 2011-11-11 | 2014-07-09 | 西华师范大学 | Ag/ZnO-SnO2 composite nanocatalyst and production method thereof |
| TWI494159B (en) * | 2012-11-02 | 2015-08-01 | Ind Tech Res Inst | Photocatalyst material and method for fabricating the same |
| US9724675B2 (en) | 2012-11-02 | 2017-08-08 | Industrial Technology Research Institute | Photocatalyst material and method for fabricating the same |
| CN108993501A (en) * | 2018-08-09 | 2018-12-14 | 苏州汉力新材料有限公司 | A kind of silver-silver oxide-zinc oxide photocatalysis material preparation method |
| CN111018365A (en) * | 2019-12-30 | 2020-04-17 | 黑龙江省科学院高技术研究院 | Method for in-situ preparation of silver nanoparticle loaded ZnO nano-foam |
| CN115246709A (en) * | 2022-08-01 | 2022-10-28 | 河北浩锐陶瓷制品有限公司 | High-flatness ceramic tile and production process thereof |
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Application publication date: 20111019 |