CN104437569B - A kind of based on Ag3PO4The preparation method of the visible light absorbing layer of thin film - Google Patents
A kind of based on Ag3PO4The preparation method of the visible light absorbing layer of thin film Download PDFInfo
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- CN104437569B CN104437569B CN201410657651.8A CN201410657651A CN104437569B CN 104437569 B CN104437569 B CN 104437569B CN 201410657651 A CN201410657651 A CN 201410657651A CN 104437569 B CN104437569 B CN 104437569B
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- 239000010409 thin film Substances 0.000 title claims abstract description 23
- 238000002360 preparation method Methods 0.000 title claims abstract description 17
- 229910000161 silver phosphate Inorganic materials 0.000 claims abstract description 30
- 238000000034 method Methods 0.000 claims abstract description 16
- 239000000843 powder Substances 0.000 claims abstract description 16
- 238000000975 co-precipitation Methods 0.000 claims abstract description 9
- 238000005245 sintering Methods 0.000 claims abstract description 7
- 239000000758 substrate Substances 0.000 claims abstract description 7
- 239000003960 organic solvent Substances 0.000 claims abstract description 4
- 239000001856 Ethyl cellulose Substances 0.000 claims description 9
- ZZSNKZQZMQGXPY-UHFFFAOYSA-N Ethyl cellulose Chemical compound CCOCC1OC(OC)C(OCC)C(OCC)C1OC1C(O)C(O)C(OC)C(CO)O1 ZZSNKZQZMQGXPY-UHFFFAOYSA-N 0.000 claims description 9
- 229920001249 ethyl cellulose Polymers 0.000 claims description 9
- 235000019325 ethyl cellulose Nutrition 0.000 claims description 9
- 239000002243 precursor Substances 0.000 claims description 9
- WUOACPNHFRMFPN-UHFFFAOYSA-N alpha-terpineol Chemical compound CC1=CCC(C(C)(C)O)CC1 WUOACPNHFRMFPN-UHFFFAOYSA-N 0.000 claims description 6
- SQIFACVGCPWBQZ-UHFFFAOYSA-N delta-terpineol Natural products CC(C)(O)C1CCC(=C)CC1 SQIFACVGCPWBQZ-UHFFFAOYSA-N 0.000 claims description 6
- 238000004528 spin coating Methods 0.000 claims description 6
- 229940116411 terpineol Drugs 0.000 claims description 6
- 239000012528 membrane Substances 0.000 claims description 3
- 230000001699 photocatalysis Effects 0.000 abstract description 8
- 239000007788 liquid Substances 0.000 abstract description 7
- 239000000463 material Substances 0.000 abstract description 7
- 239000011941 photocatalyst Substances 0.000 abstract description 6
- 238000006243 chemical reaction Methods 0.000 abstract description 5
- 239000000126 substance Substances 0.000 abstract description 5
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 abstract description 5
- 238000007146 photocatalysis Methods 0.000 abstract description 4
- 239000003344 environmental pollutant Substances 0.000 abstract description 3
- 231100000252 nontoxic Toxicity 0.000 abstract description 3
- 230000003000 nontoxic effect Effects 0.000 abstract description 3
- 231100000719 pollutant Toxicity 0.000 abstract description 3
- 230000015556 catabolic process Effects 0.000 abstract description 2
- 238000006731 degradation reaction Methods 0.000 abstract description 2
- 239000000853 adhesive Substances 0.000 abstract 1
- 230000001070 adhesive effect Effects 0.000 abstract 1
- 239000006185 dispersion Substances 0.000 abstract 1
- 230000005693 optoelectronics Effects 0.000 abstract 1
- 239000010408 film Substances 0.000 description 7
- 238000003756 stirring Methods 0.000 description 6
- UFHFLCQGNIYNRP-UHFFFAOYSA-N Hydrogen Chemical compound [H][H] UFHFLCQGNIYNRP-UHFFFAOYSA-N 0.000 description 4
- 239000011521 glass Substances 0.000 description 4
- 239000001257 hydrogen Substances 0.000 description 4
- 229910052739 hydrogen Inorganic materials 0.000 description 4
- 239000003792 electrolyte Substances 0.000 description 3
- 238000004519 manufacturing process Methods 0.000 description 3
- GWEVSGVZZGPLCZ-UHFFFAOYSA-N titanium dioxide Inorganic materials O=[Ti]=O GWEVSGVZZGPLCZ-UHFFFAOYSA-N 0.000 description 3
- 229940075397 calomel Drugs 0.000 description 2
- 238000006555 catalytic reaction Methods 0.000 description 2
- 238000005253 cladding Methods 0.000 description 2
- ZOMNIUBKTOKEHS-UHFFFAOYSA-L dimercury dichloride Chemical compound Cl[Hg][Hg]Cl ZOMNIUBKTOKEHS-UHFFFAOYSA-L 0.000 description 2
- 238000006303 photolysis reaction Methods 0.000 description 2
- 230000015843 photosynthesis, light reaction Effects 0.000 description 2
- -1 silver halide Chemical class 0.000 description 2
- 206010070834 Sensitisation Diseases 0.000 description 1
- 229910021607 Silver chloride Inorganic materials 0.000 description 1
- NPNMHHNXCILFEF-UHFFFAOYSA-N [F].[Sn]=O Chemical compound [F].[Sn]=O NPNMHHNXCILFEF-UHFFFAOYSA-N 0.000 description 1
- 239000012298 atmosphere Substances 0.000 description 1
- QVGXLLKOCUKJST-UHFFFAOYSA-N atomic oxygen Chemical compound [O] QVGXLLKOCUKJST-UHFFFAOYSA-N 0.000 description 1
- 230000006399 behavior Effects 0.000 description 1
- 230000009286 beneficial effect Effects 0.000 description 1
- 239000003795 chemical substances by application Substances 0.000 description 1
- 239000011248 coating agent Substances 0.000 description 1
- 238000000576 coating method Methods 0.000 description 1
- 239000004020 conductor Substances 0.000 description 1
- BERDEBHAJNAUOM-UHFFFAOYSA-N copper(I) oxide Inorganic materials [Cu]O[Cu] BERDEBHAJNAUOM-UHFFFAOYSA-N 0.000 description 1
- 239000013078 crystal Substances 0.000 description 1
- KRFJLUBVMFXRPN-UHFFFAOYSA-N cuprous oxide Chemical compound [O-2].[Cu+].[Cu+] KRFJLUBVMFXRPN-UHFFFAOYSA-N 0.000 description 1
- 238000000354 decomposition reaction Methods 0.000 description 1
- 230000007812 deficiency Effects 0.000 description 1
- 238000003912 environmental pollution Methods 0.000 description 1
- AMGQUBHHOARCQH-UHFFFAOYSA-N indium;oxotin Chemical compound [In].[Sn]=O AMGQUBHHOARCQH-UHFFFAOYSA-N 0.000 description 1
- 239000001301 oxygen Substances 0.000 description 1
- 229910052760 oxygen Inorganic materials 0.000 description 1
- 239000002245 particle Substances 0.000 description 1
- 230000002085 persistent effect Effects 0.000 description 1
- 238000013033 photocatalytic degradation reaction Methods 0.000 description 1
- 238000006862 quantum yield reaction Methods 0.000 description 1
- 238000004064 recycling Methods 0.000 description 1
- 230000000630 rising effect Effects 0.000 description 1
- 239000004065 semiconductor Substances 0.000 description 1
- 230000008313 sensitization Effects 0.000 description 1
- 229910052709 silver Inorganic materials 0.000 description 1
- 239000004332 silver Substances 0.000 description 1
- ADZWSOLPGZMUMY-UHFFFAOYSA-M silver bromide Chemical compound [Ag]Br ADZWSOLPGZMUMY-UHFFFAOYSA-M 0.000 description 1
- HKZLPVFGJNLROG-UHFFFAOYSA-M silver monochloride Chemical compound [Cl-].[Ag+] HKZLPVFGJNLROG-UHFFFAOYSA-M 0.000 description 1
- 239000004094 surface-active agent Substances 0.000 description 1
- 238000010345 tape casting Methods 0.000 description 1
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- Application Of Or Painting With Fluid Materials (AREA)
- Catalysts (AREA)
Abstract
A kind of based on Ag3PO4The preparation method of the visible light absorbing layer of thin film, the preparation method belonging to photocatalysis, photoelectric material." co-precipitation spun-dried sintering " four step process are used to be prepared from, step: 1) adopt coprecipitation to obtain Ag3PO4Nano level superfine powder body, the yardstick of powder body is in 20～500nm scope；2) by Ag3PO4Powder ultrasonic is scattered in transparent organic solvent, then is spun in substrate by the colloidal sol shape dispersion liquid of acquisition, obtains prefabricated Ag3PO4Rete；3) by prefabricated Ag3PO4It is dry that rete is placed in the baking oven of 20-80 DEG C, and then load is placed in Muffle furnace to sinter to remove organic substance residues.This Ag3PO4The thickness of visible light absorbing layer, at 0.2～10 μ m, not only has good visible light-responded characteristic and adhesive force, and is easily recycled as photocatalyst, it is possible to for the light anode of photoelectrochemical cell.Bigger application potential is had in fields such as light degradation pollutant, photocatalytic water and opto-electronic conversion.Advantage: method is simple, nontoxic, and easily operated, and cost is low.
Description
Technical field
The preparation method that the present invention relates to a kind of photocatalysis, photoelectric material, particularly a kind of based on Ag3PO4The preparation method of the visible light absorbing layer of thin 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.Standing in the angle of human society sustainable development, development green environment pollutant abatement technology is extremely urgent with substituting clean energy resource.Current all technology carrying out contrast find, conductor photocatalysis is a kind of quite rising technology, this is because it is readily available the energy in nature light or artificial light source.Catalysis material is a based semiconductor, can produce electronics, hole, and then can be hydrogen and oxygen by water decomposition, or organic wastewater is resolved into innocuous substance under the irradiation of light.In numerous quasiconductor agent, TiO2It is proved to have photocatalytic activity height, stable chemical nature and the advantage such as nontoxic, fully shows advantage in the field such as photocatalytic degradation, hydrogen manufacturing.But, its energy gap is big, can only absorb and account for the ultraviolet light of small part in sunlight.
In recent years, people also develop some successively and have visible light-responded photocatalyst, such as CdS, BiOBr, Cu2O etc..But these materials or be susceptible to photoetch, or photocatalytic activity is not high, and photolysis or light degradation persistent period are long, fall far short from practical application.Until 2009, leaf JINHUA etc. finds a kind of novel photocatalysis materials A g3PO4, 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, but Ag3PO4Based photocatalyst there is also 3 fatefulue deficiencies: first, and the crystal grain general size synthesized is relatively big, adopts surfactant cladding to obtain nanocrystalline despite helping reduction crystallite dimension, but the Organic substance of grain surface cladding is difficult to remove.Second, stability is relatively poor, and not rarely seen light easily decomposes, and is also slightly soluble in water, being susceptible to " photoetch " and forms Ag simple substance particle, thus stoping the incidence of light, passing through Ag in course of reaction3PO4Outer wall form silver halide (AgBr, AgCl etc.) although shell can suppress its " photoetch " behavior, but light stability is still difficult to significantly improve.3rd, Ag3PO4Photocatalyst is generally powder type, is not only difficult to recycle, but also is not easily accomplished photoelectrocatalysis: a kind of catalyzed version more preferably.
From the angle of commercial Application and TiO2Deng in the development course of catalysis material, it is necessary to make thin film or coating form.The material of this form has at least three advantages: one is advantageous for the recycling of photocatalyst, improves service efficiency；Two are made as photoelectrochemistrpool pool (for hydrogen manufacturing or generating), just have visible light-responded because of himself, can not only save dye sensitization link, and be expected to realize better photovoltaic energy conversion.It addition, by Ag3PO4Making form of film, it is achieved photocatalytic water, photovoltaic energy conversion, compare traditional Si, TiO2Base solar cell, preparation cost is lower, and there is no bibliographical information mistake at present.
Summary of the invention
The invention aims to provide a kind of based on Ag3PO4The preparation method of the visible light absorbing layer of thin film, solves current Ag3PO4Based photocatalyst is not easily recycled, and the problem being not easily accomplished 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 spun-dried sintering " four step process to be prepared from；Concrete steps: 1) adopt coprecipitation to obtain Ag3PO4Nanometer grade powder, the yardstick of powder body is in 20～500nm scope；2) by Ag3PO4Powder dissolves and is scattered in transparent organic carrier, it is thus achieved that precursor sol, then utilizes spin-coating method to be spun in substrate the precursor sol of acquisition, obtains prefabricated Ag3PO4Thin film；3) by prefabricated Ag3PO4It is dry that thin film is placed in the baking oven of 20-80 DEG C；4), by dried Ag3PO4Prefabricated 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 terpineol, ethyl cellulose, and their mass ratio is 10:1～5:1.
Ethyl cellulose and Ag in described precursor colloidal sol3PO4The 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 effects of the present invention is as follows:
1. the inventive method is simple, nontoxic, and easily operated.
2. the inventive method need not use inert atmosphere protection, and cost is low, is appropriate to industrialized production.
3. the film adhesion obtained is better, and the thickness of rete is easily controllable.
Accompanying drawing explanation
Fig. 1 is Ag in the embodiment of the present invention 13PO4The XRD figure of base film light anode.
Fig. 2 is Ag in the embodiment of the present invention 13PO4The SEM exterior view of base film light anode.
Fig. 3 is based on Ag in the embodiment of the present invention 13PO4The I-V characteristic curve of the photoelectrochemistrpool pool of light anode.
Fig. 4 is based on Ag in the embodiment of the present invention 13PO4The 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 spun-dried sintering " four step process to be prepared from, step: 1) adopt coprecipitation to obtain Ag3PO4Nanometer grade powder, the yardstick of powder body is in 20～500nm scope；2) by Ag3PO4Powder dissolves and is scattered in transparent organic carrier, it is thus achieved that precursor sol, then utilizes spin-coating method to be spun in substrate the precursor sol of acquisition, obtains prefabricated Ag3PO4Thin film；3) by prefabricated Ag3PO4It is dry that thin film is placed in the baking oven of 20-80 DEG C；4), by dried Ag3PO4Prefabricated membrane is positioned in Muffle furnace and sinters to remove organic solvent residual.
Described transparent organic carrier is made up of terpineol, ethyl cellulose, and their mass ratio is 10:1～5:1.
Ethyl cellulose and Ag in described precursor sol3PO4The 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, adds 0.4g ethyl cellulose in 5mL terpineol, stirs 24h, obtain clear viscous liquids, take Ag prepared by 0.5g coprecipitation under room temperature3PO4Grind 30min, join in the 375 above-mentioned clear viscous liquids of μ L, stir 2h, obtain 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 thin film with the high rotating speed spin coating 60s of 3000r/min.By thin film good for spin coating dry 12h in 60 DEG C of baking ovens, it is subsequently placed in Muffle furnace and sinters.From room temperature with the ramp of 1 DEG C/min to 125 DEG C, it is incubated 30min, then with the ramp of 10 DEG C/min to 400 DEG C, is incubated 90min, naturally cools to room temperature, obtain stronger thin film.Ag by preparation3PO4Base film is in DSSC, and Pt electrode is as to electrode, and many iodide ions are as electrolyte.This thin film has certain photoresponse as light anode, as shown in Figure 4.
Embodiment 2: using indium tin oxide (ITO) electro-conductive glass as substrate, adds 0.4g ethyl cellulose in 4.5mL terpineol, stirs 12h, obtain clear viscous liquids, take 0.4gAg at 60 DEG C3PO4Grind 30min, join in the 225 above-mentioned clear viscous liquids of μ L, stir 2h, obtain gel.Obtaining thin film by knife coating, in 50 DEG C of baking ovens, dry 12h, is subsequently placed in Muffle furnace and sinters.From room temperature with the ramp of 1 DEG C/min to 125 DEG C, it is incubated 30min, then with the ramp of 10 DEG C/min to 375 DEG C, is incubated 90min, naturally cools to room temperature, obtain stronger thin film.Ag by preparation3PO4Base film light anode is 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 terpineol, stirs 12h, obtain clear viscous liquids, take 0.45gAg at 60 DEG C3PO4Grind 30min, join in the 275 above-mentioned clear viscous liquids of μ L, stir 2h, obtain gel.Obtaining thin film by czochralski method, in 80 DEG C of baking ovens, dry 12h, is subsequently placed in Muffle furnace and sinters.From room temperature with the ramp of 1 DEG C/min to 125 DEG C, it is incubated 30min, then with the ramp of 10 DEG C/min to 400 DEG C, is incubated 90min, naturally cools to room temperature, obtain stronger thin film.Ag by preparation3PO4During base film light anode is used in electrochemical workstation, Pt electrode is as to electrode, and calomel electrode is as reference electrode, and 0.1M Alkitrate is as electrolyte.
Claims (3)
1. one kind based on Ag3PO4The preparation method of the visible light absorbing layer of thin film, it is characterised in that: the preparation method of visible light absorbing layer is: use " co-precipitation spun-dried sintering " four step process to be prepared from；Concrete steps: 1) adopt coprecipitation to obtain Ag3PO4Nanometer grade powder, the yardstick of powder body is in 20 ~ 500nm scope；2) by Ag3PO4Powder dissolves and is scattered in transparent organic carrier, it is thus achieved that precursor sol, then utilizes spin-coating method to be spun in substrate the precursor sol of acquisition, obtains prefabricated Ag3PO4Thin film；3) by prefabricated Ag3PO4It is dry that thin film is placed in the baking oven of 20-80 DEG C；4), by dried Ag3PO4Prefabricated membrane is positioned in Muffle furnace and sinters to remove organic solvent residual；Two step temperature method sintering are adopted to form；
Described transparent organic carrier is made up of terpineol, ethyl cellulose, and both mass percents are in 10:1 ~ 5:1 scope.
2. according to claim 1 based on Ag3PO4The preparation method of the visible light absorbing layer of thin film, it is characterised in that: ethyl cellulose and Ag in described precursor sol3PO4The mass percent of powder is in 0.03:1 ~ 0.1:1 scope.
3. according to claim 1 based on Ag3PO4The preparation method of the visible light absorbing layer of thin film, it is characterised in that: two described step temperature methods, 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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| 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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| CN104014355A (en) * | 2014-06-19 | 2014-09-03 | 中国矿业大学 | Preparation method of visible-light catalyst |
| CN104014354A (en) * | 2014-06-16 | 2014-09-03 | 中国矿业大学 | Improve Ag3PO4Method for visible light catalytic performance |
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| 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 |
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