CN113304755A - BiVO4/MOOH photoelectric catalyst and preparation method thereof - Google Patents
BiVO4/MOOH photoelectric catalyst and preparation method thereof Download PDFInfo
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- CN113304755A CN113304755A CN202011227227.1A CN202011227227A CN113304755A CN 113304755 A CN113304755 A CN 113304755A CN 202011227227 A CN202011227227 A CN 202011227227A CN 113304755 A CN113304755 A CN 113304755A
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- 229910002915 BiVO4 Inorganic materials 0.000 title claims abstract description 30
- 239000003054 catalyst Substances 0.000 title claims abstract description 11
- 238000002360 preparation method Methods 0.000 title claims description 13
- 239000000758 substrate Substances 0.000 claims abstract description 73
- 238000000151 deposition Methods 0.000 claims abstract description 56
- 229910052797 bismuth Inorganic materials 0.000 claims abstract description 50
- JCXGWMGPZLAOME-UHFFFAOYSA-N bismuth atom Chemical compound [Bi] JCXGWMGPZLAOME-UHFFFAOYSA-N 0.000 claims abstract description 50
- LSGOVYNHVSXFFJ-UHFFFAOYSA-N vanadate(3-) Chemical compound [O-][V]([O-])([O-])=O LSGOVYNHVSXFFJ-UHFFFAOYSA-N 0.000 claims abstract description 50
- 229910052760 oxygen Inorganic materials 0.000 claims abstract description 32
- QVGXLLKOCUKJST-UHFFFAOYSA-N atomic oxygen Chemical compound [O] QVGXLLKOCUKJST-UHFFFAOYSA-N 0.000 claims abstract description 30
- 239000001301 oxygen Substances 0.000 claims abstract description 30
- 238000000034 method Methods 0.000 claims abstract description 29
- PXHVJJICTQNCMI-UHFFFAOYSA-N nickel Substances [Ni] PXHVJJICTQNCMI-UHFFFAOYSA-N 0.000 claims abstract description 28
- 229910052751 metal Inorganic materials 0.000 claims abstract description 17
- 239000002184 metal Substances 0.000 claims abstract description 17
- 229910052759 nickel Inorganic materials 0.000 claims abstract description 17
- 229910052742 iron Inorganic materials 0.000 claims abstract description 13
- 238000000137 annealing Methods 0.000 claims abstract description 12
- 230000008569 process Effects 0.000 claims abstract description 9
- -1 surface-modified bismuth vanadate Chemical class 0.000 claims abstract description 8
- 238000001755 magnetron sputter deposition Methods 0.000 claims abstract description 7
- 229910052782 aluminium Inorganic materials 0.000 claims abstract description 3
- 229910052802 copper Inorganic materials 0.000 claims abstract description 3
- 239000006260 foam Substances 0.000 claims abstract description 3
- 229910052737 gold Inorganic materials 0.000 claims abstract description 3
- 239000002070 nanowire Substances 0.000 claims abstract description 3
- 229910052709 silver Inorganic materials 0.000 claims abstract description 3
- 239000013077 target material Substances 0.000 claims description 59
- 230000008021 deposition Effects 0.000 claims description 53
- XKRFYHLGVUSROY-UHFFFAOYSA-N Argon Chemical compound [Ar] XKRFYHLGVUSROY-UHFFFAOYSA-N 0.000 claims description 52
- 238000010438 heat treatment Methods 0.000 claims description 30
- 229910052786 argon Inorganic materials 0.000 claims description 26
- 239000007789 gas Substances 0.000 claims description 25
- 239000010408 film Substances 0.000 claims description 22
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Chemical compound O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims description 21
- 239000000919 ceramic Substances 0.000 claims description 16
- 238000004544 sputter deposition Methods 0.000 claims description 15
- CSCPPACGZOOCGX-UHFFFAOYSA-N Acetone Chemical compound CC(C)=O CSCPPACGZOOCGX-UHFFFAOYSA-N 0.000 claims description 12
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 claims description 12
- 238000004140 cleaning Methods 0.000 claims description 12
- 239000011941 photocatalyst Substances 0.000 claims description 12
- 239000002131 composite material Substances 0.000 claims description 9
- 238000001035 drying Methods 0.000 claims description 6
- 238000004321 preservation Methods 0.000 claims description 6
- 238000001816 cooling Methods 0.000 claims description 4
- 239000010409 thin film Substances 0.000 claims description 3
- 238000000861 blow drying Methods 0.000 claims description 2
- 229910044991 metal oxide Inorganic materials 0.000 claims description 2
- 238000004506 ultrasonic cleaning Methods 0.000 claims description 2
- 238000000926 separation method Methods 0.000 abstract description 15
- 238000002425 crystallisation Methods 0.000 abstract description 2
- 230000008025 crystallization Effects 0.000 abstract description 2
- 238000011065 in-situ storage Methods 0.000 abstract description 2
- XEEYBQQBJWHFJM-UHFFFAOYSA-N iron Substances [Fe] XEEYBQQBJWHFJM-UHFFFAOYSA-N 0.000 description 16
- 229910002640 NiOOH Inorganic materials 0.000 description 14
- 229910002588 FeOOH Inorganic materials 0.000 description 10
- 230000001699 photocatalysis Effects 0.000 description 9
- 238000005477 sputtering target Methods 0.000 description 9
- UFHFLCQGNIYNRP-UHFFFAOYSA-N Hydrogen Chemical compound [H][H] UFHFLCQGNIYNRP-UHFFFAOYSA-N 0.000 description 7
- 238000006243 chemical reaction Methods 0.000 description 7
- 239000001257 hydrogen Substances 0.000 description 7
- 229910052739 hydrogen Inorganic materials 0.000 description 7
- 239000000463 material Substances 0.000 description 6
- 230000005012 migration Effects 0.000 description 6
- 238000013508 migration Methods 0.000 description 6
- 238000005516 engineering process Methods 0.000 description 5
- 238000007254 oxidation reaction Methods 0.000 description 5
- 239000011521 glass Substances 0.000 description 4
- 238000011068 loading method Methods 0.000 description 4
- 239000000243 solution Substances 0.000 description 4
- GWEVSGVZZGPLCZ-UHFFFAOYSA-N Titan oxide Chemical compound O=[Ti]=O GWEVSGVZZGPLCZ-UHFFFAOYSA-N 0.000 description 3
- 230000000052 comparative effect Effects 0.000 description 3
- 239000013078 crystal Substances 0.000 description 3
- 230000003647 oxidation Effects 0.000 description 3
- 239000002957 persistent organic pollutant Substances 0.000 description 3
- 238000011160 research Methods 0.000 description 3
- 239000001052 yellow pigment Substances 0.000 description 3
- 229910018916 CoOOH Inorganic materials 0.000 description 2
- 230000009286 beneficial effect Effects 0.000 description 2
- 230000005540 biological transmission Effects 0.000 description 2
- RKTYLMNFRDHKIL-UHFFFAOYSA-N copper;5,10,15,20-tetraphenylporphyrin-22,24-diide Chemical compound [Cu+2].C1=CC(C(=C2C=CC([N-]2)=C(C=2C=CC=CC=2)C=2C=CC(N=2)=C(C=2C=CC=CC=2)C2=CC=C3[N-]2)C=2C=CC=CC=2)=NC1=C3C1=CC=CC=C1 RKTYLMNFRDHKIL-UHFFFAOYSA-N 0.000 description 2
- 239000008367 deionised water Substances 0.000 description 2
- 229910021641 deionized water Inorganic materials 0.000 description 2
- 230000000694 effects Effects 0.000 description 2
- 238000004070 electrodeposition Methods 0.000 description 2
- 239000003792 electrolyte Substances 0.000 description 2
- 238000005265 energy consumption Methods 0.000 description 2
- 238000003912 environmental pollution Methods 0.000 description 2
- 235000019441 ethanol Nutrition 0.000 description 2
- 239000011259 mixed solution Substances 0.000 description 2
- 239000000047 product Substances 0.000 description 2
- 239000004065 semiconductor Substances 0.000 description 2
- 239000000126 substance Substances 0.000 description 2
- 238000009825 accumulation Methods 0.000 description 1
- 239000006227 byproduct Substances 0.000 description 1
- 238000004364 calculation method Methods 0.000 description 1
- 239000000969 carrier Substances 0.000 description 1
- 239000002800 charge carrier Substances 0.000 description 1
- 239000011248 coating agent Substances 0.000 description 1
- 238000000576 coating method Methods 0.000 description 1
- 229910017052 cobalt Inorganic materials 0.000 description 1
- 239000010941 cobalt Substances 0.000 description 1
- GUTLYIVDDKVIGB-UHFFFAOYSA-N cobalt atom Chemical compound [Co] GUTLYIVDDKVIGB-UHFFFAOYSA-N 0.000 description 1
- 150000001875 compounds Chemical class 0.000 description 1
- 239000000470 constituent Substances 0.000 description 1
- 239000000356 contaminant Substances 0.000 description 1
- 238000005260 corrosion Methods 0.000 description 1
- 230000000593 degrading effect Effects 0.000 description 1
- 238000011161 development Methods 0.000 description 1
- 238000010586 diagram Methods 0.000 description 1
- 238000005286 illumination Methods 0.000 description 1
- 239000012535 impurity Substances 0.000 description 1
- 238000001727 in vivo Methods 0.000 description 1
- PJXISJQVUVHSOJ-UHFFFAOYSA-N indium(III) oxide Inorganic materials [O-2].[O-2].[O-2].[In+3].[In+3] PJXISJQVUVHSOJ-UHFFFAOYSA-N 0.000 description 1
- 238000004519 manufacturing process Methods 0.000 description 1
- 239000008204 material by function Substances 0.000 description 1
- 238000012986 modification Methods 0.000 description 1
- 230000004048 modification Effects 0.000 description 1
- 230000007935 neutral effect Effects 0.000 description 1
- 238000007146 photocatalysis Methods 0.000 description 1
- 238000005546 reactive sputtering Methods 0.000 description 1
- 230000006798 recombination Effects 0.000 description 1
- 238000005215 recombination Methods 0.000 description 1
- 230000009467 reduction Effects 0.000 description 1
- 238000003756 stirring Methods 0.000 description 1
- LSNNMFCWUKXFEE-UHFFFAOYSA-L sulfite Chemical class [O-]S([O-])=O LSNNMFCWUKXFEE-UHFFFAOYSA-L 0.000 description 1
- 239000004408 titanium dioxide Substances 0.000 description 1
- 230000000007 visual effect Effects 0.000 description 1
- 238000005406 washing Methods 0.000 description 1
- 239000002699 waste material Substances 0.000 description 1
- 229910052845 zircon Inorganic materials 0.000 description 1
- GFQYVLUOOAAOGM-UHFFFAOYSA-N zirconium(iv) silicate Chemical compound [Zr+4].[O-][Si]([O-])([O-])[O-] GFQYVLUOOAAOGM-UHFFFAOYSA-N 0.000 description 1
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- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01J—CHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
- B01J23/00—Catalysts comprising metals or metal oxides or hydroxides, not provided for in group B01J21/00
- B01J23/70—Catalysts comprising metals or metal oxides or hydroxides, not provided for in group B01J21/00 of the iron group metals or copper
- B01J23/76—Catalysts comprising metals or metal oxides or hydroxides, not provided for in group B01J21/00 of the iron group metals or copper combined with metals, oxides or hydroxides provided for in groups B01J23/02 - B01J23/36
- B01J23/84—Catalysts comprising metals or metal oxides or hydroxides, not provided for in group B01J21/00 of the iron group metals or copper combined with metals, oxides or hydroxides provided for in groups B01J23/02 - B01J23/36 with arsenic, antimony, bismuth, vanadium, niobium, tantalum, polonium, chromium, molybdenum, tungsten, manganese, technetium or rhenium
- B01J23/847—Vanadium, niobium or tantalum or polonium
- B01J23/8472—Vanadium
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01J—CHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
- B01J35/00—Catalysts, in general, characterised by their form or physical properties
- B01J35/30—Catalysts, in general, characterised by their form or physical properties characterised by their physical properties
- B01J35/33—Electric or magnetic properties
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- B01J—CHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
- B01J35/00—Catalysts, in general, characterised by their form or physical properties
- B01J35/30—Catalysts, in general, characterised by their form or physical properties characterised by their physical properties
- B01J35/39—Photocatalytic properties
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- C—CHEMISTRY; METALLURGY
- C23—COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; CHEMICAL SURFACE TREATMENT; DIFFUSION TREATMENT OF METALLIC MATERIAL; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL; INHIBITING CORROSION OF METALLIC MATERIAL OR INCRUSTATION IN GENERAL
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- C23C14/00—Coating by vacuum evaporation, by sputtering or by ion implantation of the coating forming material
- C23C14/0021—Reactive sputtering or evaporation
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- C23C14/00—Coating by vacuum evaporation, by sputtering or by ion implantation of the coating forming material
- C23C14/06—Coating by vacuum evaporation, by sputtering or by ion implantation of the coating forming material characterised by the coating material
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- C23C14/00—Coating by vacuum evaporation, by sputtering or by ion implantation of the coating forming material
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- C23C14/00—Coating by vacuum evaporation, by sputtering or by ion implantation of the coating forming material
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Abstract
The invention relates to BiVO4The thickness of the bismuth vanadate film is 50-500 nm, the metal comprises one or two of Fe, Co and Ni, and the substrate is a transparent conductive electrode FTO, ITO, AZO, ATO or porous electrode foam nickel or a metal nanowire electrode Cu, Au, Ag and Al. Preparing a bismuth vanadate film by magnetron sputtering, obtaining a film with high crystallization quality by a post-annealing process, and depositing an oxygen evolution catalyst MOOH (M = Ni, Co, Fe) on the surface of the prepared bismuth vanadate film, thereby obtaining the surface-modified bismuth vanadate photo-anode film with optimal performanceA film; the MOOH cocatalyst is prepared in situ, so that the combination of the MOOH cocatalyst and BiVO4 is better and more uniform, and the separation of photo-generated electrons and holes at the interface of BiVO4 and MOOH is more facilitated.
Description
Technical Field
The invention relates to the technical field of functional materials, in particular to BiVO4A photoelectric catalyst of/MOOH and a preparation method thereof.
Background
Solar energy is a new renewable clean energy, and has become one of the first-choice alternative energy sources for solving the problems of energy shortage, environmental pollution and the like, but how to efficiently utilize solar energy becomes the key point and the difficulty of the current research.
As early as 1972, Fjulshima and Honda report that a titanium dioxide film can decompose water into hydrogen and oxygen under the condition of illumination so as to realize the conversion of solar energy into chemical energy for the first time, and therefore, a photocatalytic technology enters the visual field of people and attracts extensive attention, thereby becoming one of the current research hotspots. The photocatalytic oxidation technology can effectively utilize clean and renewable solar energy to decompose water to produce hydrogen and oxygen and degrade organic pollutants in water and atmosphere, can effectively reduce energy consumption, and reduces the possibility of byproducts and secondary pollution. It can not only relieve the problem of energy shortage, but also effectively treat environmental pollution, and is a high-efficiency oxidation technology with development prospect.
BiVO4The light yellow pigment is an environment-friendly and bright light yellow pigment, and has the characteristics of wide sources of constituent elements, good chemical and thermal stability and the like, particularly has a narrow forbidden band width and a proper valence band position, so that the light yellow pigment shows excellent photocatalytic explanation of organic pollutants and photocatalytic water splitting activity, and has attracted extensive attention of people in recent years. BiVO4There are mainly three kinds of crystal phase structures, which are monoclinic scheelite type, tetragonal scheelite type and tetragonal zircon type, and the three kinds of crystal phases can be mutually converted under a certain temperature condition. Wherein, monoclinic scheelite type BiVO4The structure is the most thermodynamically stable crystal phase structure, and the best photocatalytic activity is shown in the aspects of degrading organic pollutants by visible light and photolyzing water to produce hydrogen and oxygen, so that extensive research is carried out。
Monoclinic scheelite type BiVO4Forbidden band width E ofgEqual to 2.4 eV, the valence band position is sufficient to oxidize water, and the conduction band position is almost coincident with the hydrogen reduction potential, which means BiVO is in the complete Photoelectrochemical (PEC) water splitting process4The energy consumption of hydrogen production is less than that of other visible light semiconductors, and meanwhile, theoretical calculation shows that BiVO4The effective mass of photogenerated electrons and holes in vivo is less than that of other conventional oxide semiconductors, such as TiO2And In2O3And the separation and transmission of photogenerated carriers are facilitated.
However, BiVO4The actual photoelectric conversion efficiency of the photocatalytic material is still far lower than the theoretical value due to some problems of the photocatalytic material, so that the practical application of the photocatalytic material is limited, and the following problems exist: (1) BiVO4The charge transport, and in particular the electron transport rate, in the material is slow, resulting in the recombination of about 60% -80% of the generated charge carriers before they reach the surface of the material; (2) the rate of kinetics of oxygen evolution from this reaction is very slow compared to the oxidation reaction of sulfites.
For BiVO4The accumulation of holes generated at the photoanode/electrolyte interface can often lead to the discovery of the photo-corrosion phenomenon of the photocatalyst, and therefore how to improve BiVO4The surface properties of (2) appear to work very well. Therefore, we propose a BiVO4A photoelectric catalyst of/MOOH and a preparation method thereof.
Disclosure of Invention
The invention mainly aims to provide a BiVO4The bismuth vanadate film prepared based on the method has excellent photo-generated carrier separation and transport capacity, high oxygen kinetic rate and wide application in the fields of photocatalysis, photoelectrocatalysis, electrocatalysis and the like, and compared with a widely used electrodeposition method, the method has higher efficiency and simple preparation process, does not generate waste solution products, is more compact and flat, effectively improves the integral oxidation kinetic rate, and can have the advantages of high efficiency, simple preparation process, high stability and the likeEffectively solves the problems in the background technology.
In order to achieve the purpose, the invention adopts the technical scheme that:
a BiVO4/MOOH photoelectric catalyst comprises a bismuth vanadate thin film and a layered hydroxy metal oxide on a transparent conductive substrate.
Further, the thickness of the bismuth vanadate film is 50-500 nm.
Preferably, the metal comprises one or two of Fe, Co and Ni.
Further, the substrate is a transparent conductive electrode FTO, ITO, AZO, ATO or porous electrode foam nickel or metal nanowire electrode Cu, Au, Ag and Al.
Preparation of BiVO4The method for preparing the/MOOH composite photo-anode film comprises the following steps:
s1, cleaning a substrate and drying;
s2, placing a substrate in a deposition chamber, and then depositing a bismuth vanadate film on the surface of the substrate by adopting a direct-current magnetron sputtering method, wherein the target material is a bismuth vanadate ceramic target, sputtering gases are argon and oxygen, the total pressure is 0.5-2.5 Pa, the oxygen partial pressure is 0-4%, the distance between the target material and the substrate is 7-20 cm, the initial substrate temperature is room temperature, the substrate is heated in the sputtering process, the heating temperature is 350-500 ℃, the power of a direct-current power supply applied to the target material is 50-500W or the power density is 0.6-6.4W/cm2Sputtering a bismuth vanadate ceramic target material for 5-60 min;
s3, preparing MOOH on the surface of the bismuth vanadate film prepared in the step S2 by adopting a direct current magnetron sputtering method, wherein the metal target is one of Fe, Co or Ni targets, the introduced gas with the flow rate of 30-60sccm is argon and the introduced oxygen with the flow rate of 5-10sccm, meanwhile, the introduced water vapor with the flow rate of 5-30sccm is introduced through a micropump, the total pressure is 0.5-2.5 Pa, the distance between the target and the substrate is 7-20 cm, the substrate heating is stopped, and the power of a direct current power supply applied to the target is 50-100W or the power density is 0.2-1.3W/cm2The deposition time is 5-60 min;
s4, after S3 is finished, the temperature of the substrate is reduced to room temperature, the sample is taken out and sent into a muffle furnace for heat treatment, and after the annealing is finished, the sample is waitedThe temperature of the product is reduced to room temperature to prepare BiVO4/MOOH。
Further, the method for cleaning the substrate in S1 is to sequentially use acetone and absolute ethyl alcohol to respectively perform ultrasonic cleaning for at least 30 min; the drying method is compressed air blow drying.
Preferably, the initial background vacuum level in the S2 deposition chamber is less than 10-4 Pa, ensuring that the impurity gas in the cavity is discharged. There will be small amounts of contaminant gases, such as CO2, organics, etc., during the sample loading and unloading process. The local vacuum ensures that the gas can not influence the subsequent reactive sputtering.
Preferably, the heat treatment temperature in S4 is 500-1000 ℃, the heating rate is 1-10 ℃/min, and the heat preservation time is 60-480 min.
Compared with the prior art, the invention has the following beneficial effects:
the invention provides a BiVO modified by MOOH (M = Ni, Co, Fe) oxygen evolution catalyst4A photo-anode film and a preparation method thereof are disclosed, wherein a bismuth vanadate film is prepared by magnetron sputtering, a film with high crystallization quality is obtained by a post-annealing process, and a layer of oxygen evolution catalyst MOOH (M = Ni, Co, Fe) is deposited on the surface of the prepared bismuth vanadate film, so that a surface modified bismuth vanadate photo-anode film with the best performance is obtained; the MOOH cocatalyst is prepared in situ, so that the MOOH cocatalyst is combined with BiVO4 better and more uniformly, and the separation of photo-generated electrons and holes at the interface of BiVO4 and MOOH is facilitated;
secondly, the magnetron sputtering process has mild conditions, simple process and short period, can be used for continuous preparation, is not limited by the size, texture and appearance of the substrate, has high preparation efficiency in the whole process and few process steps, and avoids secondary pollution possibly generated in the subsequent preparation process;
compared with the conventional hydrothermal deposition or electrodeposition, the method has the advantages that trace water is introduced in the sputtering process, the MOOH is chemically synthesized under the assistance of plasma glow, the preparation procedure is simpler, the popularization is easier, the MOOH layer is deposited to modify the bismuth vanadate film, the interface oxidation reaction can be promoted, and the photoelectrocatalysis efficiency is improved.
Drawings
FIG. 1 MOOH/BiVO4Structural schematic diagram of double-layer film
FIG. 2 shows the photocurrent curves of different MOOH-modified bismuth vanadate films in neutral electrolyte.
Detailed Description
In order to make the technical means, the creation characteristics, the achievement purposes and the effects of the invention easy to understand, the invention is further described with the specific embodiments.
The equipment used in the following examples is a three-target co-sputtering coating machine with model number MSP-3200, which is assembled by Wennan Wei Ke technology of Beijing, the system can comprise a deposition chamber, a sample chamber, a plurality of target heads, a tray, a plurality of direct current power supplies and a series of vacuum pumps, wherein the target heads and a substrate plate form a certain angle, and the direct current power supplies are connected with the target heads; and the equipment is placed in a room with constant temperature of 22 ℃.
The following examples refer to argon and oxygen with a purity of 99.99%.
Example 1
S1, ultrasonically cleaning the substrate (FTO glass), respectively ultrasonically cleaning the substrate with acetone and absolute ethyl alcohol for 30min, orderly fixing the substrate on a tray, putting the substrate into a sample chamber, and then opening a gate to load the substrate until the vacuum degree (background vacuum degree) reaches 10－4 In a deposition chamber below Pa;
s2, introducing a mixed gas of argon of 60sccm and oxygen of 1sccm into the deposition chamber, wherein the pressure is 0.6 Pa, the target material is a pure bismuth vanadate target material, the distance between the target material and the substrate is 8cm, the chamber is heated to 500 ℃, a direct current power supply (the electric power is 200W) is started, the deposition time is 10 min, and the bismuth vanadate ceramic target material is sputtered;
s3, introducing a mixed gas of 60sccm argon and 10sccm oxygen into the deposition chamber at a flow ratio of 6:1, introducing water vapor of 20sccm through a micropump, wherein the total pressure is 1.5 Pa, the distance between the target and the substrate is 8cm, the sputtering target is a metal nickel target, stopping heating the substrate, and the power of a direct-current power supply applied to the target is 100W, wherein the deposition time is 20 min;
s4, after the deposition is finished, when the temperature of the substrate is reduced to room temperature, taking out the sample, sending the sample into a muffle furnace, carrying out heat treatment on the sample, wherein the temperature rise speed is 5 ℃/min, the annealing temperature is 500 ℃, and the heat preservation time is 240 min; after the annealing is completed, the temperature of the sample is cooled back to the room temperature, and the sample is taken out. The sample is a bismuth vanadate photocatalyst modified by the surface of NiOOH, the size and the thickness of the NiOOH are matched with the migration distance of a photon-generated carrier, and the separation efficiency and the separation speed of the sample can be obviously improved. The BiVO4/NiOOH photocurrent curve is shown in FIG. 2.
Example 2
S1, the same as the embodiment 1;
s2, introducing pure argon into the deposition chamber, wherein the flow is 60sccm, the pressure is 0.6 Pa, the target material is a pure bismuth vanadate target material, the distance between the target material and the substrate is 8cm, the chamber is heated to 500 ℃, a direct-current power supply (the electric power is 200W) is started, the deposition time is 10 min, and sputtering a bismuth vanadate ceramic target material;
s3, introducing a mixed gas of 60sccm argon and 10sccm oxygen into the deposition chamber at a flow ratio of 6:1, introducing water vapor of 20sccm through a micropump, wherein the total pressure is 1.5 Pa, the distance between the target and the substrate is 8cm, the sputtering target is a metal nickel target, stopping heating the substrate, and the power of a direct-current power supply applied to the target is 100W, wherein the deposition time is 10 min;
s4 Heat treatment is carried out in the same manner as in example 1. The sample is a bismuth vanadate photocatalyst modified by the surface of NiOOH, the size and the thickness of the NiOOH are matched with the migration distance of a photon-generated carrier, and the separation efficiency and the separation speed of the sample can be obviously improved.
Example 3
S1, the same as the embodiment 1;
s2, introducing a mixed gas of argon of 60sccm and oxygen of 2sccm into the deposition chamber, wherein the pressure is 0.6 Pa, the target material is a pure bismuth vanadate target material, the distance between the target material and the substrate is 8cm, the chamber is heated to 500 ℃, a direct current power supply (the electric power is 200W) is started, the deposition time is 10 min, and the bismuth vanadate ceramic target material is sputtered;
s3, introducing a mixed gas of argon of 60sccm and oxygen of 10sccm into the deposition chamber at a flow ratio of 6:1, introducing water vapor of 20sccm through a micropump, wherein the total pressure is 1.5 Pa, the distance between the target and the substrate is 8cm, the sputtering target is a metal nickel target, stopping heating the substrate, and the power of a direct current power supply applied to the target is 100W, wherein the deposition time is 30 min;
s4 Heat treatment is carried out in the same manner as in example 1. The sample is a bismuth vanadate photocatalyst modified by the surface of NiOOH, the size and the thickness of the NiOOH are matched with the migration distance of a photon-generated carrier, and the separation efficiency and the separation speed of the sample can be obviously improved.
Example 4
S1, the implementation mode is the same as that of the embodiment 1 except that the base material is ITO;
s2, introducing pure argon into the deposition chamber, wherein the flow is 60sccm, the pressure is 0.6 Pa, the target material is a pure bismuth vanadate target material, the distance between the target material and the substrate is 8cm, the chamber is heated to 500 ℃, a direct current power supply (the electric power is 200W) is started, the deposition time is 10 min, and sputtering the bismuth vanadate ceramic target material;
s3, introducing a mixed gas of argon of 60sccm and oxygen of 10sccm into the deposition chamber at a flow ratio of 6:1, introducing water vapor of 20sccm through a micropump, wherein the total pressure is 1.5 Pa, the distance between the target and the substrate is 8cm, the sputtering target is a metal iron target, stopping heating the substrate, and the power of a direct current power supply applied to the target is 100W, wherein the deposition time is 5 min;
s4, the heat treatment mode is the same as that of the embodiment 1. The sample is a bismuth vanadate photocatalyst modified by FeOOH surface, the size and thickness of FeOOH are matched with the migration distance of a photon-generated carrier, and the separation efficiency and speed of the sample can be obviously improved.
Example 5
S1, the same as the embodiment 1;
s2, introducing a mixed gas of argon of 60sccm and oxygen of 1sccm into the deposition chamber, wherein the pressure is 0.6 Pa, the target material is a pure bismuth vanadate target material, the distance between the target material and the substrate is 8cm, the chamber is heated to 500 ℃, a direct current power supply (the electric power is 200W) is started, the deposition time is 10 min, and the bismuth vanadate ceramic target material is sputtered;
s3, introducing a mixed gas of 60sccm argon and 10sccm oxygen into the deposition chamber at a flow ratio of 6:1, introducing 20sccm steam through a micropump, wherein the total pressure is 1.5 Pa, the distance between the target and the substrate is 8cm, the sputtering target is a metal cobalt target, heating of the substrate is stopped, the power of a direct current power supply applied to the target is 100W, and the deposition time is 10 min;
s4, the heat treatment mode is the same as that of the embodiment 1. The sample is a bismuth vanadate photocatalyst modified by a CoOOH surface, the size and the thickness of the CoOOH are matched with the migration distance of a photon-generated carrier, and the separation efficiency and the separation speed of the sample can be obviously improved.
Example 6
S1, except that the substrate is ATO, the implementation manner is the same as that of the embodiment 1;
s2, introducing a mixed gas of argon of 60sccm and oxygen of 1sccm into the deposition chamber, wherein the pressure is 0.6 Pa, the target material is a pure bismuth vanadate target material, the distance between the target material and the substrate is 8cm, the chamber is heated to 500 ℃, a direct current power supply (the electric power is 200W) is started, the deposition time is 10 min, and the bismuth vanadate ceramic target material is sputtered;
s3, introducing a mixed gas of 60sccm argon and 10sccm oxygen into the deposition chamber at a flow ratio of 6:1, introducing water vapor of 20sccm through a micropump, wherein the total pressure is 1.5 Pa, the distance between the target and the substrate is 8cm, the sputtering target is a metal iron target, stopping heating the substrate, and the power of a direct current power supply applied to the target is 100W, wherein the deposition time is 15 min.
S4, the heat treatment mode is the same as that of the embodiment 1. The photocurrent curve of BiVO4/FeOOH is shown in FIG. 2.
Example 7
S1, the same as the embodiment 1;
s2, introducing a mixed gas of argon of 60sccm and oxygen of 2sccm into the deposition chamber, wherein the pressure is 0.6 Pa, the target material is a pure bismuth vanadate target material, the distance between the target material and the substrate is 8cm, the chamber is heated to 350 ℃, a direct current power supply (the electric power is 200W) is started, the deposition time is 10 min, and the bismuth vanadate ceramic target material is sputtered;
s3, introducing a mixed gas of 60sccm argon and 10sccm oxygen into the deposition chamber at a flow ratio of 6:1, introducing water vapor of 20sccm through a micropump, wherein the total pressure is 1.5 Pa, the distance between the target and the substrate is 8cm, the sputtering target is a metal iron target and a nickel target, stopping heating the substrate, and applying 100W of power of a direct current power supply to the target, wherein the deposition time is 15 min.
S4, the heat treatment mode is the same as that of the embodiment 1. The sample is a bismuth vanadate photocatalyst compositely modified by FeOOH/NiOOH, the size and thickness of the FeOOH/NiOOH are matched with the migration distance of a photon-generated carrier, the separation efficiency and speed of the sample can be obviously improved, and the photoelectric conversion efficiency of the BiVO4 composite film is improved. The photocurrent curve is shown in fig. 2, which has the best photoelectric conversion efficiency.
Example 8
S1, the same as the embodiment 1;
s2, introducing pure argon into the deposition chamber, wherein the flow is 60sccm, the pressure is 0.6 Pa, the target material is a pure bismuth vanadate target material, the distance between the target material and the substrate is 8cm, the chamber is heated to 500 ℃, a direct current power supply (the electric power is 200W) is started, the deposition time is 10 min, and sputtering the bismuth vanadate ceramic target material;
s3, introducing a mixed gas of 60sccm of argon and 10sccm of oxygen into the deposition chamber at a flow ratio of 6:1, and introducing 5sccm of water vapor through the micro pump. The total pressure is 1.5 Pa, the distance between the target material and the substrate is 8cm, the sputtering target materials are a metal iron target and a nickel target, the substrate is stopped to be heated, the power of a direct current power supply applied to the target material is 100W, and the deposition time is 15 min;
s4, the heat treatment mode is the same as that of the embodiment 1. The sample is a bismuth vanadate photocatalyst compositely modified by FeOOH/NiOOH, and at the moment, the size of a formed sheet-shaped compound is smaller, but the sample still shows good photoelectric conversion efficiency.
Example 9
S1, the same as the embodiment 1;
s2, introducing a mixed gas of argon of 60sccm and oxygen of 2sccm, keeping the pressure at 0.6 Pa, wherein the target material is a pure bismuth vanadate target material, the distance between the target material and the substrate is 8cm, heating the chamber to 500 ℃, starting a direct current power supply (the electric power is 200W), and sputtering the bismuth vanadate ceramic target material, wherein the deposition time is 10 min;
s3, introducing a mixed gas of argon of 60sccm and oxygen of 10sccm into the deposition chamber at a flow ratio of 6:1, introducing water vapor of 30sccm through a micropump, wherein the total pressure is 1.5 Pa, the distance between the target and the substrate is 8cm, the sputtering target materials are a metal iron target and a nickel target, the initial substrate temperature is room temperature, the power of a direct current power supply applied to the target material is 100W, and the deposition time is 15 min;
s4, the heat treatment mode is the same as that of the embodiment 1. The sample is the thick-sheet FeOOH/NiOOH composite modified bismuth vanadate photocatalyst. At the moment, the supported FeOOH/NiOOH composite cocatalyst has longer growth time and thicker thickness, and is not beneficial to the separation and transmission of photo-generated electrons; the more water vapor that is not passed in, the better.
Comparative example 1
Ultrasonically cleaning substrate (FTO glass), respectively ultrasonically cleaning the substrate with acetone and anhydrous ethanol for 30min, sequentially fixing on a tray, placing into a sample chamber, opening a gate, and loading until vacuum degree (background vacuum degree) reaches 10－4 In a deposition chamber below Pa;
introducing pure argon gas with the flow of 60sccm and the pressure of 0.6 Pa, wherein the target material is a pure bismuth vanadate target material, the distance between the target material and the substrate is 8cm, the initial chamber temperature is kept at room temperature, a direct current power supply (with the electric power of 200W) is started, and the deposition time is 10 min. Sputtering bismuth vanadate ceramic target material, keeping the substrate at room temperature;
the sample was then sent to a muffle furnace and heat treated. The heating speed is 5 ℃/min, the annealing temperature is 500 ℃, and the heat preservation time is 240 min. After the annealing is completed, the temperature of the sample is cooled back to the room temperature, and the sample is taken out. The pure BiVO4 photocurrent curve is shown in figure 2.
Comparative example 2
Ultrasonically cleaning substrate (FTO glass), respectively ultrasonically cleaning the substrate with acetone and anhydrous ethanol for 30min, sequentially fixing on a tray, placing into a sample chamber, opening a gate, and loading until vacuum degree (background vacuum degree) reaches 10－4 In a deposition chamber below Pa;
introducing pure argon gas with the flow of 60sccm and the pressure of 0.6 Pa, wherein the target material is a pure bismuth vanadate target material, the distance between the target material and the substrate is 8cm, the initial chamber temperature is kept at room temperature, a direct current power supply (with the electric power of 200W) is started, and the deposition time is 10 min. Sputtering bismuth vanadate ceramic target material, keeping the substrate at room temperature;
the sample was then sent to a muffle furnace and heat treated. The heating speed is 5 ℃/min, the annealing temperature is 500 ℃, and the heat preservation time is 240 min. After the annealing is finished, cooling the sample to the room temperature, and taking out the sample;
subsequently, Fe (NO) was prepared3)2·6H2O and Ni (NO)3)2·6H2And taking 50ml of the mixed solution with the O concentration of 30mM out, placing the mixed solution in a beaker, and downloading the surface deposition of the thin film for 45s by constant potential-1V of the CHI-600 electrochemical workstation. Repeatedly washing with deionized water and ethanol after deposition is finished, and finally 60 in a vacuum ovenoC drying for 1 hour. Finally preparing the FeOOH/NiOOH composite modified bismuth vanadate photocatalyst. The photocurrent at 1.23V relative to the standard hydrogen electrode was 0.5 mA/cm2Much smaller than the magnitude of the photocurrent in example 2 of this patent (fig. 2).
Comparative example 3
Ultrasonically cleaning substrate (FTO glass), respectively ultrasonically cleaning the substrate with acetone and anhydrous ethanol for 30min, sequentially fixing on a tray, placing into a sample chamber, opening a gate, and loading until vacuum degree (background vacuum degree) reaches 10－4 In a deposition chamber below Pa;
introducing pure argon gas with the flow of 60sccm and the pressure of 0.6 Pa, wherein the target material is a pure bismuth vanadate target material, the distance between the target material and the substrate is 8cm, the initial chamber temperature is kept at room temperature, a direct current power supply (with the electric power of 200W) is started, and the deposition time is 10 min. Sputtering bismuth vanadate ceramic target material, keeping the substrate at room temperature;
the sample was then sent to a muffle furnace and heat treated. The heating speed is 5 ℃/min, the annealing temperature is 500 ℃, and the heat preservation time is 240 min. After the annealing is finished, cooling the sample to the room temperature, and taking out the sample;
then, Fe (NO) was taken out separately3)2·6H2O and Ni (NO)3)2·6H2O was prepared as a 10mM solution and a clear solution was obtained by constant stirring. The above BiVO4 film and 40ml of the above solution were put into a hydrothermal kettle, 120oAnd C, preserving the heat for 6 hours. After the reaction was complete, the sample was removed and repeatedly rinsed with deionized water and ethanol, and finally in a vacuum oven 60oC drying for 1 hour. Finally preparing the FeOOH/NiOOH composite modified bismuth vanadate photocatalyst. The photocurrent at 1.23V relative to the standard hydrogen electrode was 0.6 mA/cm2Much less than the photocurrent of example 7 of this patentSize (fig. 2).
The foregoing shows and describes the general principles and broad features of the present invention and advantages thereof. It will be understood by those skilled in the art that the present invention is not limited to the embodiments described above, which are described in the specification and illustrated only to illustrate the principle of the present invention, but that various changes and modifications may be made therein without departing from the spirit and scope of the present invention, which fall within the scope of the invention as claimed. The scope of the invention is defined by the appended claims and equivalents thereof.
Claims (8)
1. A BiVO4/MOOH photoelectric catalyst, which is characterized by comprising a bismuth vanadate thin film and a layered hydroxyl metal oxide on a transparent conductive substrate.
2. BiVO according to claim 14the/MOOH photoelectric catalyst is characterized in that the thickness of the bismuth vanadate film is 50-500 nm.
3. BiVO according to claim 14the/MOOH photocatalyst is characterized in that the metal comprises one or two of Fe, Co and Ni.
4. BiVO according to claim 14The photoelectric catalyst of/MOOH is characterized in that the substrate is a transparent conductive electrode FTO, ITO, AZO, ATO or porous electrode foam nickel or metal nanowire electrodes Cu, Au, Ag and Al.
5. Preparation of BiVO as claimed in claims 1 to 44The method for preparing the/MOOH composite photo-anode film is characterized by comprising the following steps of:
s1, cleaning a substrate and drying;
s2, placing the substrate in a deposition chamber, and then depositing a bismuth vanadate film on the surface of the substrate by adopting a direct-current magnetron sputtering method, wherein the target material is a bismuth vanadate ceramic target, sputtering gases are argon and oxygen, the total pressure is 0.5-2.5 Pa, and the oxygen partial pressure is 0.5-2.5 Pa0-4%, the distance between the target and the substrate is 7-20 cm, the initial substrate temperature is room temperature, the substrate is heated in the sputtering process, the heating temperature is 350-500 ℃, and the power of a direct current power supply applied to the target is 50-500W or the power density is 0.6-6.4W/cm2Sputtering a bismuth vanadate ceramic target material for 5-60 min;
s3, preparing MOOH on the surface of the bismuth vanadate film prepared in the step S2 by adopting a direct current magnetron sputtering method, wherein the metal target is one of Fe, Co or Ni targets, the introduced gas with the flow rate of 30-60sccm is argon and the introduced oxygen with the flow rate of 5-10sccm, meanwhile, the introduced water vapor with the flow rate of 5-30sccm is introduced through a micropump, the total pressure is 0.5-2.5 Pa, the distance between the target and the substrate is 7-20 cm, the substrate heating is stopped, and the power of a direct current power supply applied to the target is 50-100W or the power density is 0.2-1.3W/cm2The deposition time is 5-60 min;
s4, after S3, cooling the temperature of the substrate to room temperature, taking out the sample, sending the sample into a muffle furnace for heat treatment, and after the annealing is finished, cooling the temperature of the sample to room temperature to obtain BiVO4/MOOH。
6. A method of preparing BiVO according to claim 54The method for cleaning the substrate in the S1 is characterized in that acetone and absolute ethyl alcohol are sequentially used for ultrasonic cleaning for at least 30 min; the drying method is compressed air blow drying.
7. A method of preparing BiVO according to claim 54The method for preparing the/MOOH composite photo-anode film is characterized in that the initial background vacuum degree in the S2 deposition chamber is lower than 10-4 Pa。
8. A method of preparing BiVO according to claim 54The method for preparing the MOOH composite photo-anode film is characterized in that the heat treatment temperature in S4 is 500-1000 ℃, the heating rate is 1-10 ℃/min, and the heat preservation time is 60-480 min.
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