CN104437569A - Preparation method of visible light absorption layer based on Ag3PO4 film - Google Patents
Preparation method of visible light absorption layer based on Ag3PO4 film Download PDFInfo
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- CN104437569A CN104437569A CN201410657651.8A CN201410657651A CN104437569A CN 104437569 A CN104437569 A CN 104437569A CN 201410657651 A CN201410657651 A CN 201410657651A CN 104437569 A CN104437569 A CN 104437569A
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- visible light
- film
- preparation
- ag3po4
- light absorption
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Abstract
The invention discloses a preparation method of a visible light absorption layer based on an Ag3PO4 film, and belongs to a preparation method of photocatalysis and photoelectric materials. The visible light absorption layer is prepared by using a four-step process including coprecipitation, spin coating, drying and sintering, and the method comprises the steps of 1) preparing Ag3PO4 nano-scale ultrafine powder of which the size scale is between 20 and 500 nm by using a coprecipitation method; 2) ultrasonically dispersing the Ag3PO4 powder into transparent organic solvents, and performing spin coating on the obtained sol shaped dispersion liquid on a substrate to obtain a prefabricated Ag3PO4 film layer; and 3) putting the prefabricated Ag3PO4 film layer into an oven at the temperature of 20-80 DEG C for drying, and putting into a muffle furnace for sintering and removing organic residues. The Ag3PO4 visible light absorption layer has a thickness of 0.2-10 microns, and is high in response characteristics and adhesive force of visible light; because the visible light absorption layer is used as a photocatalyst, the visible light absorption layer is easy to recover, can be used for a photo-anode of a photoelectrochemical cell, and has a large application potential on the fields of light degradation pollutants, photolysis of water, photovoltaic conversion and the like. The method is simple, free of toxicity, easy to operate and low in cost.
Description
Technical field
The present invention relates to the preparation method of a kind of photocatalysis, photoelectric material, particularly a kind of based on Ag
3pO
4the preparation method of the visible light absorbing layer of film.
Background technology
Since stepping into the seventies in last century, the problem such as environmental pollution and energy shortage causes people to outburst global the crisis even worry of disaster increasingly.Stand in the angle of human society sustainable development, development green environment pollutant abatement technology and substituting clean energy resource extremely urgent.Current all technology are carried out contrast to find, conductor photocatalysis is a kind of quite rising technology, this is because it is easy to utilize the energy in natural daylight or artificial light source.Catalysis material is a based semiconductor, can produce electronics, hole under the irradiation of light, and then can be hydrogen and oxygen by water decomposition, or organic wastewater is resolved into innocuous substance.In numerous semiconductor agent, TiO
2be proved to be have that photocatalytic activity is high, stable chemical nature and the advantage such as nontoxic, fully show advantage in the field such as photocatalytic degradation, hydrogen manufacturing.But its energy gap is large, can only absorb the ultraviolet light accounting for small part in sunshine.
In recent years, people also develop some successively and have visible light-responded photochemical catalyst, as CdS, BiOBr, Cu
2o etc.But these materials or easily photoetch occurs, or photocatalytic activity is not high, light decompose or the light degradation duration long, fall far short from practical application.Until 2009, leaf golden flower etc. find a kind of novel photocatalysis material---Ag
3pO
4, there is the feature such as visible light-responded (band gap is about 2.4eV), quantum yield high (~ 90%), can by pollutant mineralising within the extremely short time.Although have these advantages, Ag
3pO
4also there are 3 fatefulue deficiencies in based photocatalyst: first, and the crystal grain general size synthesized is comparatively large, although adopt, surfactant is coated to be contributed to reducing crystallite dimension and obtain nanocrystalline, and the coated organic matter of grain surface is difficult to remove.The second, stability is relatively poor, and not rarely seen light easily decomposes, and is also slightly soluble in water, " photoetch " easily occurs in course of reaction and forms Ag simple substance particle, thus stop the incidence of light, pass through Ag
3pO
4outer wall formed silver halide (AgBr, AgCl etc.) although shell can suppress its " photoetch " behavior, photostability is still difficult to remarkable improvement.Three, Ag
3pO
4photochemical catalyst is generally powder type, is not only difficult to recycle, but also is not easy to realize photoelectrocatalysis: a kind of better catalyzed version.
From angle and the TiO of commercial Application
2in development course Deng catalysis material, be necessary to make film or coating form.The material of this form has three advantages at least: one is be conducive to recycling of photochemical catalyst, improves service efficiency; Two is make photoelectrochemistrpool pool (for hydrogen manufacturing or generating), because himself just has visible light-responded, can not only save dye sensitization link, and be expected to realize better photovoltaic energy conversion.In addition, by Ag
3pO
4make form of film, realize photocatalytic water, photovoltaic energy conversion, compare traditional Si, TiO
2base solar cell, preparation cost is lower, and there is no bibliographical information mistake at present.
Summary of the invention
The object of the invention is to provide a kind of based on Ag
3pO
4the preparation method of the visible light absorbing layer of film, solves current Ag
3pO
4based photocatalyst not easily reclaims, and is not easy the problem realizing photovoltaic energy conversion, photolysis water hydrogen.
Realize the technical scheme of the object of the invention: the preparation method of visible light absorbing layer is: use " co-precipitation-spin coating-drying-sintering " four step process to be prepared from; Concrete steps: 1) adopt coprecipitation to obtain Ag
3pO
4nanometer grade powder, the yardstick of powder is in 20 ~ 500nm scope; 2) by Ag
3pO
4powder dissolution is scattered in transparent organic carrier, obtains precursor sol, then utilizes spin-coating method to be spun in substrate the precursor sol of acquisition, obtain prefabricated Ag
3pO
4film; 3) by prefabricated Ag
3pO
4film is placed in the baking oven drying of 20-80 DEG C; 4), by dried Ag
3pO
4prefabricated membrane is positioned in Muffle furnace and sinters to remove organic solvent residual, adopts two step temperature method sintering to form.
Described transparent organic carrier is made up of terpinol, ethyl cellulose, and their mass ratio is 10:1 ~ 5:1.
Ethyl cellulose and Ag in described precursor colloidal sol
3pO
4the mass ratio of powder is 0.03:1 ~ 0.1:1.
The holding stage of two described step temperature methods is divided into two, and low-temperature zone is at 125-150 DEG C, and high temperature section is then positioned at 350-400 DEG C of scope.
Beneficial effect of the present invention is as follows:
1. the inventive method is simple, nontoxic, and is easy to operation.
2. the inventive method does not need to use inert atmosphere protection, and cost is low, is applicable to carrying out suitability for industrialized production.
3. the film adhesion obtained is better, and the thickness of rete is easy to control.
Accompanying drawing explanation
Fig. 1 is Ag in the embodiment of the present invention 1
3pO
4the XRD figure of base film light anode.
Fig. 2 is Ag in the embodiment of the present invention 1
3pO
4the SEM exterior view of base film light anode.
Fig. 3 is based on Ag in the embodiment of the present invention 1
3pO
4the I-V characteristic curve of the photoelectrochemistrpool pool of light anode.
Fig. 4 is based on Ag in the embodiment of the present invention 1
3pO
4the photoresponse curve of the photoelectrochemistrpool pool of light anode.
Detailed description of the invention
The preparation method of visible light absorbing layer is: use " co-precipitation-spin coating-drying-sintering " four step process to be prepared from, step: 1) adopt coprecipitation to obtain Ag
3pO
4nanometer grade powder, the yardstick of powder is in 20 ~ 500nm scope; 2) by Ag
3pO
4powder dissolution is scattered in transparent organic carrier, obtains precursor sol, then utilizes spin-coating method to be spun in substrate the precursor sol of acquisition, obtain prefabricated Ag
3pO
4film; 3) by prefabricated Ag
3pO
4film is placed in the baking oven drying of 20-80 DEG C; 4), by dried Ag
3pO
4prefabricated membrane is positioned in Muffle furnace and sinters to remove organic solvent residual.
Described transparent organic carrier is made up of terpinol, ethyl cellulose, and their mass ratio is 10:1 ~ 5:1.
Ethyl cellulose and Ag in described precursor sol
3pO
4the mass ratio of powder is 0.03:1 ~ 0.1:1.
The holding stage of described sintering process is divided into two, and low-temperature zone is at 125-150 DEG C, and high temperature section is then positioned at 350-400 DEG C of scope.
Embodiment 1: using fluorine tin-oxide (FTO) electro-conductive glass as substrate, add 0.4g ethyl cellulose in 5mL terpinol, stirred at ambient temperature 24h, obtains clear viscous liquids, gets Ag prepared by 0.5g coprecipitation
3pO
4grinding 30min, joins in the above-mentioned clear viscous liquids of 375 μ L, stirs 2h, obtains gel.FTO electro-conductive glass is placed on sol evenning machine, drips gel in centre, with the slow-speed of revolution spin coating 10s of 1000r/min, then obtain film with the high rotating speed spin coating 60s of 3000r/min.By film good for spin coating dry 12h in 60 DEG C of baking ovens, be then placed in Muffle furnace and sinter.From room temperature with the ramp to 125 DEG C of 1 DEG C/min, insulation 30min, then with the ramp to 400 DEG C of 10 DEG C/min, insulation 90min, naturally cools to room temperature, obtains more firmly film.By the Ag of preparation
3pO
4base film is used in DSSC, and Pt electrode is as to electrode, and many iodide ions are as electrolyte.This film has certain photoresponse as light anode, as shown in Figure 4.
Embodiment 2: using indium tin oxide (ITO) electro-conductive glass as substrate, add 0.4g ethyl cellulose in 4.5mL terpinol, stir 12h at 60 DEG C, obtain clear viscous liquids, get 0.4gAg
3pO
4grinding 30min, joins in the above-mentioned clear viscous liquids of 225 μ L, stirs 2h, obtains gel.Obtain film by knife coating, dry 12h in 50 DEG C of baking ovens, be then placed in Muffle furnace and sinter.From room temperature with the ramp to 125 DEG C of 1 DEG C/min, insulation 30min, then with the ramp to 375 DEG C of 10 DEG C/min, insulation 90min, naturally cools to room temperature, obtains more firmly film.By the Ag of preparation
3pO
4base film light anode is used in electrochemical workstation, and Pt electrode is as to electrode, and calomel electrode is as reference electrode, and 0.1M Alkitrate is as electrolyte.
Embodiment 3:FTO electro-conductive glass, as substrate, adds 0.5g ethyl cellulose in 6mL terpinol, stirs 12h, obtain clear viscous liquids at 60 DEG C, gets 0.45g Ag
3pO
4grinding 30min, joins in the above-mentioned clear viscous liquids of 275 μ L, stirs 2h, obtains gel.Obtain film by czochralski method, dry 12h in 80 DEG C of baking ovens, be then placed in Muffle furnace and sinter.From room temperature with the ramp to 125 DEG C of 1 DEG C/min, insulation 30min, then with the ramp to 400 DEG C of 10 DEG C/min, insulation 90min, naturally cools to room temperature, obtains more firmly film.By the Ag of preparation
3pO
4base film light anode is used in electrochemical workstation, and Pt electrode is as to electrode, and calomel electrode is as reference electrode, and 0.1M Alkitrate is as electrolyte.
Claims (4)
1. one kind based on Ag
3pO
4the preparation method of the visible light absorbing layer of film, is characterized in that: the preparation method of visible light absorbing layer is: use " co-precipitation-spin coating-drying-sintering " four step process to be prepared from; Concrete steps: 1) adopt coprecipitation to obtain Ag
3pO
4nanometer grade powder, the yardstick of powder is in 20 ~ 500 nm scopes; 2) by Ag
3pO
4powder dissolution is scattered in transparent organic carrier, obtains precursor sol, then utilizes spin-coating method to be spun in substrate the precursor sol of acquisition, obtain prefabricated Ag
3pO
4film; 3) by prefabricated Ag
3pO
4film is placed in the baking oven drying of 20-80 DEG C; 4), by dried Ag
3pO
4prefabricated membrane is positioned in Muffle furnace and sinters to remove organic solvent residual; Two step temperature method sintering are adopted to form.
2. according to claim 1 based on Ag
3pO
4the preparation method of the visible light absorbing layer of film, is characterized in that: described transparent solvent is made up of terpinol, ethyl cellulose, and both mass percents are in 10:1 ~ 5:1 scope.
3. according to claim 1 based on Ag
3pO
4the preparation method of the visible light absorbing layer of film, is characterized in that: ethyl cellulose and Ag in described precursor sol
3pO
4the mass percent of powder is in 0.03:1 ~ 0.1:1 scope.
4. according to claim 1 based on Ag
3pO
4the preparation method of the visible light absorbing layer of film, is characterized in that: two described step temperature methods, and wherein first paragraph is in 125-150 DEG C of interval, and second step is then positioned at 350-400 DEG C of interval.
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|---|---|---|---|
| CN201410657651.8A CN104437569B (en) | 2014-11-18 | 2014-11-18 | A kind of based on Ag3PO4The preparation method of the visible light absorbing layer of thin film |
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| CN104437569A true CN104437569A (en) | 2015-03-25 |
| CN104437569B CN104437569B (en) | 2016-07-06 |
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Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN106944107A (en) * | 2017-03-30 | 2017-07-14 | 常州大学 | A kind of preparation method of silver phosphate photocatalyst film |
| CN110563990A (en) * | 2019-09-17 | 2019-12-13 | 广西科技大学 | Preparation method and application of silver-containing cellulose composite material with photodegradation function |
Citations (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN104014354A (en) * | 2014-06-16 | 2014-09-03 | 中国矿业大学 | Improve Ag3PO4Method for visible light catalytic performance |
| CN104014355A (en) * | 2014-06-19 | 2014-09-03 | 中国矿业大学 | Preparation method of visible-light catalyst |
-
2014
- 2014-11-18 CN CN201410657651.8A patent/CN104437569B/en not_active Expired - Fee Related
Patent Citations (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN104014354A (en) * | 2014-06-16 | 2014-09-03 | 中国矿业大学 | Improve Ag3PO4Method for visible light catalytic performance |
| CN104014355A (en) * | 2014-06-19 | 2014-09-03 | 中国矿业大学 | Preparation method of visible-light catalyst |
Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN106944107A (en) * | 2017-03-30 | 2017-07-14 | 常州大学 | A kind of preparation method of silver phosphate photocatalyst film |
| CN110563990A (en) * | 2019-09-17 | 2019-12-13 | 广西科技大学 | Preparation method and application of silver-containing cellulose composite material with photodegradation function |
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| CN104437569B (en) | 2016-07-06 |
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