CN107324389A - A kind of preparation method of molybdenum doping tungstic trioxide nano-film material - Google Patents
A kind of preparation method of molybdenum doping tungstic trioxide nano-film material Download PDFInfo
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- CN107324389A CN107324389A CN201710460372.6A CN201710460372A CN107324389A CN 107324389 A CN107324389 A CN 107324389A CN 201710460372 A CN201710460372 A CN 201710460372A CN 107324389 A CN107324389 A CN 107324389A
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- 238000002360 preparation method Methods 0.000 title claims abstract description 30
- 239000000463 material Substances 0.000 title claims abstract description 29
- ZOKXTWBITQBERF-UHFFFAOYSA-N Molybdenum Chemical compound [Mo] ZOKXTWBITQBERF-UHFFFAOYSA-N 0.000 title claims abstract description 20
- 229910052750 molybdenum Inorganic materials 0.000 title claims abstract description 20
- 239000011733 molybdenum Substances 0.000 title claims abstract description 20
- 239000002120 nanofilm Substances 0.000 title claims abstract description 18
- LYCAIKOWRPUZTN-UHFFFAOYSA-N Ethylene glycol Chemical compound OCCO LYCAIKOWRPUZTN-UHFFFAOYSA-N 0.000 claims abstract description 33
- ZNOKGRXACCSDPY-UHFFFAOYSA-N tungsten trioxide Chemical compound O=[W](=O)=O ZNOKGRXACCSDPY-UHFFFAOYSA-N 0.000 claims abstract description 30
- 239000000758 substrate Substances 0.000 claims abstract description 24
- MHAJPDPJQMAIIY-UHFFFAOYSA-N Hydrogen peroxide Chemical compound OO MHAJPDPJQMAIIY-UHFFFAOYSA-N 0.000 claims abstract description 22
- 238000006243 chemical reaction Methods 0.000 claims abstract description 19
- 239000007788 liquid Substances 0.000 claims abstract description 17
- CMPGARWFYBADJI-UHFFFAOYSA-L tungstic acid Chemical compound O[W](O)(=O)=O CMPGARWFYBADJI-UHFFFAOYSA-L 0.000 claims abstract description 16
- 239000002243 precursor Substances 0.000 claims abstract description 15
- 239000011248 coating agent Substances 0.000 claims abstract description 14
- 238000000576 coating method Methods 0.000 claims abstract description 14
- 239000006193 liquid solution Substances 0.000 claims abstract description 13
- 229910000476 molybdenum oxide Inorganic materials 0.000 claims abstract description 10
- PQQKPALAQIIWST-UHFFFAOYSA-N oxomolybdenum Chemical compound [Mo]=O PQQKPALAQIIWST-UHFFFAOYSA-N 0.000 claims abstract description 10
- 238000001027 hydrothermal synthesis Methods 0.000 claims abstract description 8
- 239000002253 acid Substances 0.000 claims abstract description 7
- 238000003756 stirring Methods 0.000 claims description 14
- 239000007921 spray Substances 0.000 claims description 12
- PNEYBMLMFCGWSK-UHFFFAOYSA-N aluminium oxide Inorganic materials [O-2].[O-2].[O-2].[Al+3].[Al+3] PNEYBMLMFCGWSK-UHFFFAOYSA-N 0.000 claims description 8
- 238000007788 roughening Methods 0.000 claims description 8
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 claims description 6
- 244000137852 Petrea volubilis Species 0.000 claims description 6
- 150000007513 acids Chemical class 0.000 claims description 6
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Chemical compound O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims description 6
- 239000008367 deionised water Substances 0.000 claims description 5
- 229910021641 deionized water Inorganic materials 0.000 claims description 5
- 230000003746 surface roughness Effects 0.000 claims description 4
- 238000005406 washing Methods 0.000 claims description 4
- 238000001816 cooling Methods 0.000 claims description 2
- 230000003647 oxidation Effects 0.000 claims description 2
- 238000007254 oxidation reaction Methods 0.000 claims description 2
- 238000005498 polishing Methods 0.000 claims description 2
- 239000010408 film Substances 0.000 abstract description 16
- 238000005215 recombination Methods 0.000 abstract description 6
- 230000005540 biological transmission Effects 0.000 abstract description 5
- 238000010438 heat treatment Methods 0.000 abstract description 4
- 239000011159 matrix material Substances 0.000 abstract description 4
- 230000006798 recombination Effects 0.000 abstract description 4
- 238000005336 cracking Methods 0.000 abstract description 3
- 239000010409 thin film Substances 0.000 abstract description 3
- 238000004519 manufacturing process Methods 0.000 abstract description 2
- 239000012528 membrane Substances 0.000 abstract description 2
- 239000002086 nanomaterial Substances 0.000 abstract description 2
- 239000002105 nanoparticle Substances 0.000 abstract description 2
- 230000005518 electrochemistry Effects 0.000 abstract 1
- 239000002994 raw material Substances 0.000 abstract 1
- 239000011521 glass Substances 0.000 description 9
- 238000001556 precipitation Methods 0.000 description 8
- 239000003643 water by type Substances 0.000 description 8
- 238000002156 mixing Methods 0.000 description 6
- 239000000126 substance Substances 0.000 description 6
- 238000001035 drying Methods 0.000 description 4
- QGLKJKCYBOYXKC-UHFFFAOYSA-N nonaoxidotritungsten Chemical compound O=[W]1(=O)O[W](=O)(=O)O[W](=O)(=O)O1 QGLKJKCYBOYXKC-UHFFFAOYSA-N 0.000 description 3
- 229910001930 tungsten oxide Inorganic materials 0.000 description 3
- 239000013078 crystal Substances 0.000 description 2
- 230000007547 defect Effects 0.000 description 2
- 238000000034 method Methods 0.000 description 2
- 239000002244 precipitate Substances 0.000 description 2
- UFHFLCQGNIYNRP-UHFFFAOYSA-N Hydrogen Chemical compound [H][H] UFHFLCQGNIYNRP-UHFFFAOYSA-N 0.000 description 1
- QVGXLLKOCUKJST-UHFFFAOYSA-N atomic oxygen Chemical compound [O] QVGXLLKOCUKJST-UHFFFAOYSA-N 0.000 description 1
- 239000003054 catalyst Substances 0.000 description 1
- 230000003197 catalytic effect Effects 0.000 description 1
- 238000006555 catalytic reaction Methods 0.000 description 1
- 238000005119 centrifugation Methods 0.000 description 1
- 150000001875 compounds Chemical class 0.000 description 1
- 230000000593 degrading effect Effects 0.000 description 1
- 238000001514 detection method Methods 0.000 description 1
- 230000005611 electricity Effects 0.000 description 1
- 229910052739 hydrogen Inorganic materials 0.000 description 1
- 239000001257 hydrogen Substances 0.000 description 1
- 238000011065 in-situ storage Methods 0.000 description 1
- 231100000252 nontoxic Toxicity 0.000 description 1
- 230000003000 nontoxic effect Effects 0.000 description 1
- 229910052760 oxygen Inorganic materials 0.000 description 1
- 239000001301 oxygen Substances 0.000 description 1
- 239000002245 particle Substances 0.000 description 1
- 230000005622 photoelectricity Effects 0.000 description 1
- 239000000047 product Substances 0.000 description 1
- 239000004065 semiconductor Substances 0.000 description 1
- 230000008054 signal transmission Effects 0.000 description 1
- 238000005245 sintering Methods 0.000 description 1
- GWEVSGVZZGPLCZ-UHFFFAOYSA-N titanium dioxide Inorganic materials O=[Ti]=O GWEVSGVZZGPLCZ-UHFFFAOYSA-N 0.000 description 1
- WFKWXMTUELFFGS-UHFFFAOYSA-N tungsten Chemical compound [W] WFKWXMTUELFFGS-UHFFFAOYSA-N 0.000 description 1
- 229910052721 tungsten Inorganic materials 0.000 description 1
- 239000010937 tungsten Substances 0.000 description 1
Classifications
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- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01G—COMPOUNDS CONTAINING METALS NOT COVERED BY SUBCLASSES C01D OR C01F
- C01G41/00—Compounds of tungsten
- C01G41/02—Oxides; Hydroxides
-
- 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
- B01J23/00—Catalysts comprising metals or metal oxides or hydroxides, not provided for in group B01J21/00
- B01J23/16—Catalysts comprising metals or metal oxides or hydroxides, not provided for in group B01J21/00 of arsenic, antimony, bismuth, vanadium, niobium, tantalum, polonium, chromium, molybdenum, tungsten, manganese, technetium or rhenium
- B01J23/24—Chromium, molybdenum or tungsten
- B01J23/30—Tungsten
-
- 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
-
- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01P—INDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS
- C01P2002/00—Crystal-structural characteristics
- C01P2002/50—Solid solutions
- C01P2002/52—Solid solutions containing elements as dopants
- C01P2002/54—Solid solutions containing elements as dopants one element only
-
- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01P—INDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS
- C01P2006/00—Physical properties of inorganic compounds
- C01P2006/40—Electric properties
-
- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01P—INDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS
- C01P2006/00—Physical properties of inorganic compounds
- C01P2006/60—Optical properties, e.g. expressed in CIELAB-values
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- Chemical & Material Sciences (AREA)
- Organic Chemistry (AREA)
- Engineering & Computer Science (AREA)
- Materials Engineering (AREA)
- Chemical Kinetics & Catalysis (AREA)
- Inorganic Chemistry (AREA)
- Catalysts (AREA)
- Investigating Or Analyzing Materials By The Use Of Fluid Adsorption Or Reactions (AREA)
Abstract
The invention discloses a kind of preparation method of molybdenum doping tungstic trioxide nano-film material, belong to the technical field of nano material.The present invention is first with wolframic acid, molybdenum oxide is raw material, after the reaction of hydrogen peroxide Hybrid Heating, it is dispersed in ethylene glycol solution and reaction precursor liquid solution is made, centrifuged after hydro-thermal reaction, molybdenum doping nano tungsten trioxide coating liquid is made in ultrasonic disperse again, then coating liquid is sprayed into leaf surface after treatment, film is taken off after hot briquetting and obtains molybdenum doping tungstic trioxide nano-film material, thin-film material obtained by the present invention, tungsten trioxide nano particle diameter is reduced by molybdenum doping, improve it and apply membrane stability, again substrate is used as with same element substrate, the power that be combined with each other is good, it will not cause cracking occurs between tungstic acid and matrix in heating process or be broken, and the electric charge transmission of film is fast, it is not susceptible to charge recombination, improve the photoelectrocatalysis of material, electrochemistry and transporting, preparation manipulation simple possible, industrialized production can be met.
Description
Technical field
The invention discloses a kind of preparation method of molybdenum doping tungstic trioxide nano-film material, belong to the skill of nano material
Art field.
Background technology
In recent years, the research of tungstic trioxide nano-film material causes increasing concern.Tungstic acid is a kind of n
Type semi-conducting material, its energy gap is narrower, can responding to visible light, and have and TiO2The characteristics of photochemical catalyst is similar,
I.e. stable, nontoxic, resistance to photetching, cost are low and valence band potential height, photohole oxidability are strong.WO 3 film has photoelectricity
Catalytic performance and sensing capabilities, can be used in photoelectric catalysis degrading organic, decompose aquatic products hydrogen and pH, CH4、NO2Sensor etc..
But the microstructure of WO 3 film decides the PhotoelectrocatalytiPerformance Performance and sensing capabilities of WO 3 film and used
Life-span.
The preparation method of existing tungstic trioxide nano-film is mainly to be prepared by the method for hydrothermal chemistry, with representative
The hydrothermal chemistry preparation method of property, its main preparation process includes：（1）Using electro-conductive glass as base material and electric signal transmission base
Body,（2）In electro-conductive glass substrate coat one layer of white tungstic acid colloidal solution and it is sintered obtain tungstic acid crystal seed,（3）It will carry
The electro-conductive glass for having tungstic acid crystal seed is put into the solution of the compound of tungsten carries out hydrothermal chemical reaction under the high temperature conditions, instead
Airing after answering, material obtains electro-conductive glass base tungstic trioxide nano-film after high temperature sintering.But in existing hydrothermal chemistry system
It is the combination between different elemental substances between electro-conductive glass and tungstic acid because substrate uses electro-conductive glass in Preparation Method,
Belong to non-natural combination, mutual adhesion is poor, particularly when being acted on by mechanical external force, or when environment temperature becomes
During change, because material expand coefficient is different, internal stress can be caused to change, so that between tungstic acid and electro-conductive glass matrix
Generation is ftractureed or is broken, or even causes the stripping of WO 3 film and electro-conductive glass substrate.It is non-natural between this different elements
With reference to film, electric charge transmission is slow, easily occur charge recombination, can have a strong impact on PhotoelectrocatalytiPerformance Performance, the chemical property of material
And sensing capabilities etc., and influence it to apply.It would therefore be highly desirable to find a kind of electric charge transmission soon, the three of charge recombination are not susceptible to
Tungsten oxide nanometer thin film.
The content of the invention
The technical problems to be solved by the invention：For being between different elemental substances between electro-conductive glass and tungstic acid
Combination, belong to non-natural combination, the power that be combined with each other is poor, heating be easily caused between tungstic acid and matrix occur cracking or be broken,
And between this different elements non-natural combination film, cause the electric charge of film to transmit slow, easily occur charge recombination, have impact on material
There is provided a kind of molybdenum doping tungstic trioxide nano-film for the defect of the PhotoelectrocatalytiPerformance Performance of material, chemical property and transmission performance
The preparation method of material.
To solve technical problem, the present invention is using technical scheme as described below：
（1）Reaction precursor liquid solution is prepared：Take white tungstic acid, molybdenum oxide to add in hydrogen peroxide, be heated to 95~100 DEG C, stirring is anti-
30~40min is answered, is cooled to after room temperature and adds ethylene glycol solution, continues 1~2h of stirring and obtains reaction precursor liquid solution；
（2）Nano tungsten trioxide coating liquid is prepared：Load hydrothermal reaction kettle after reaction precursor liquid solution is mixed with deionized water
In, 3~5h is reacted at 150~180 DEG C, ultrasonic disperse after washing is centrifuged and in deionized water, obtains nano tungsten trioxide
Coating liquid；
（3）Leaf is pre-processed：Leaf upper surface is polished with sand paper, then upper surface is entered with white fused alumina after being washed with absolute ethyl alcohol
Row roughening treatment, then after leaf is dried, obtain surface preparation substrate：
（4）Film：Surface preparation substrate is placed on warm table and is heated to 160~200 DEG C, then by nano tungsten trioxide film
Liquid is fitted into spray gun, and even application is cleaned and dried after cooling in precondition substrate upper surface, 3~5h of heat growth, obtains molybdenum doping
Tungstic trioxide nano-film material.
Step（1）The white tungstic acid, molybdenum oxide, hydrogen peroxide, the parts by weight of ethylene glycol solution are 5~6 parts of white tungstic acids, 1.5
~1.8 parts of molybdenum oxides, 80~100 parts of mass fractions are that 30% hydrogen peroxide, 100~120 parts of mass fractions are 50% ethylene glycol solution.
Step（3）The roughening treatment degree is that surface roughness Ra is polishing to white fused alumina is 6~8 μm.
Step（4）The quantity for spray is 0.25~0.30mL/cm2。
The method have the benefit that：
The present invention reduces tungsten trioxide nano particle diameter by molybdenum doping, improves its and applies membrane stability, then with same element substrate conduct
Substrate, each other with natural combination attribute, is firmly combined between substrate and tungsten oxide, and skill is sprayed with reference to in-situ thermal oxidation
Art, is eliminated on the premise of film nano grain structure is kept in the Lacking oxygen defect largely existed in particle, heating process
Will not cause between tungstic acid and matrix occur cracking or be broken, reduce electronics and the probability of hole-recombination so that electronics with
Hole-recombination probability is reduced, and the impedance that electronics is transmitted in the film is reduced, so as to improve the PhotoelectrocatalytiPerformance Performance of material, electricity
Chemical property and transmission performance, preparation method simple possible can meet industrialized production.
Embodiment
Weigh 5~6g white tungstic acids, 1.5~1.8g molybdenum oxides are added during 80~100mL mass fractions are 30% hydrogen peroxide, plus
Heat is cooled to addition 100~120mL matter after room temperature to 95~100 DEG C, and with 300~400r/min, 30~40min of stirring reaction
Amount fraction is 50% ethylene glycol solution, continues to stir 1~2h, obtains reaction precursor liquid solution；Measure 150~200mL precursors
Solution, is added in 150~200mL deionized waters, to load hydro-thermal reaction after 300~400r/min stirring mixing, 10~15min
In kettle, 3~5h is reacted at 150~180 DEG C, is cooled to after room temperature and is transferred in centrifuge, with 6000~8000r/min centrifugations point
It from 15~20min, must precipitate, precipitation be washed with deionized 3~5 times, then precipitation is added in 10~12L deionized waters, with
300W ultrasonic echographies disperse 1~2h, obtain nano tungsten trioxide coating liquid；Take one piece of 5cm × 10cm leaf, and by its upper surface
Polished with sand paper, then wash with absolute ethyl alcohol upper surface 3~5 times, roughening treatment is then carried out to upper surface to table with white fused alumina
Surface roughness Ra is 6~8 μm, then leaf is placed in drying box, and 3~5h is dried at 55~60 DEG C, surface preparation base is obtained
Piece；Surface preparation substrate is placed on warm table and is heated to 160~200 DEG C, then measures the nanometer of 12.5~15.0mL preparations
Tungstic acid coating liquid is fitted into spray gun, and even application is in precondition substrate upper surface, and it is 0.25~0.30mL/ to control quantity for spray
cm2, 3~5h of heat growth is cooled to after room temperature, leaf upper surface is washed with deionized 2~3 times, then continues in baking oven,
3~4h is toasted at 300~400 DEG C, is cooled to after room temperature and obtains molybdenum doping tungstic trioxide nano-film material.
Example 1
Weigh 6g white tungstic acids, 1.8g molybdenum oxides are added during 100mL mass fractions are 30% hydrogen peroxide, be heated to 100 DEG C, and with
400r/min stirring reaction 40min, it is 50% ethylene glycol solution to be cooled to after room temperature and add 120mL mass fractions, continues to stir
2h, obtains reaction precursor liquid solution；200mL reaction precursor liquid solutions are measured, adds in 200mL deionized waters, is stirred with 400r/min
It is fitted into after mixing mixing 15min in hydrothermal reaction kettle, reacts 5h at 180 DEG C, be cooled to after room temperature and be transferred in centrifuge, with
8000r/min centrifuges 20min, must precipitate, and precipitation is washed with deionized 5 times, then precipitation is added into 12L deionized waters
In, 2h is disperseed with 300W ultrasonic echographies, nano tungsten trioxide coating liquid is obtained；Take one piece of 5cm × 10cm leaf, and by its upper table
Face is polished with sand paper, then washs with absolute ethyl alcohol upper surface 5 times, and roughening treatment is then carried out to upper surface to surface with white fused alumina
Roughness Ra is 8 μm, then leaf is placed in drying box, and 5h is dried at 60 DEG C, surface preparation substrate is obtained；Surface is located in advance
Reason substrate, which is placed on warm table, is heated to 200 DEG C, then measures the nano tungsten trioxide coating liquids of 15.0mL preparations and be fitted into spray gun,
Even application is in precondition substrate upper surface, and it is 0.30mL/cm to control quantity for spray2, heat growth 5h is cooled to after room temperature, is used
Deionized water washing leaf upper surface 3 times, then continues in baking oven, 4h is toasted at 400 DEG C, be cooled to after room temperature and obtain molybdenum doping
Tungstic trioxide nano-film material.
Example 2
Weigh 5g white tungstic acids, 1.5g molybdenum oxides are added during 80mL mass fractions are 30% hydrogen peroxide, be heated to 95 DEG C, and with
300r/min stirring reaction 30min, it is 50% ethylene glycol solution to be cooled to after room temperature and add 100mL mass fractions, continues to stir
1h, obtains reaction precursor liquid solution；150mL reaction precursor liquid solutions are measured, adds in 150mL deionized waters, is stirred with 300r/min
It is fitted into after mixing mixing 10min in hydrothermal reaction kettle, reacts 3h at 150~180 DEG C, be cooled to after room temperature and be transferred in centrifuge,
15min is centrifuged with 6000r/min, must be precipitated, precipitation is washed with deionized 3 times, then precipitation is added into 10L deionized waters
In, 1h is disperseed with 300W ultrasonic echographies, nano tungsten trioxide coating liquid is obtained；Take one piece of 5cm × 10cm leaf, and by its upper table
Face is polished with sand paper, then washs with absolute ethyl alcohol upper surface 3 times, and roughening treatment is then carried out to upper surface to surface with white fused alumina
Roughness Ra is 6 μm, then leaf is placed in drying box, and 3h is dried at 55 DEG C, surface preparation substrate is obtained；Surface is located in advance
Reason substrate, which is placed on warm table, is heated to 160 DEG C, then measures the nano tungsten trioxide coating liquids of 12.5 preparations and be fitted into spray gun,
Even to be sprayed on precondition substrate upper surface, it is 0.25mL/cm to control quantity for spray2, heat growth 3h is cooled to after room temperature, spends
Ion water washing leaf upper surface 2 times, then continues in baking oven, 3h is toasted at 300 DEG C, is cooled to after room temperature and obtains molybdenum doping three
Tungsten oxide nanometer thin film material.
Example 3
5~6g white tungstic acids are weighed, 1.5~1.8g molybdenum oxides add 80~100mL mass fractions in 30% hydrogen peroxide, to be heated to
95~100 DEG C, and with 300~400r/min, 30~40min of stirring reaction, be cooled to after room temperature and add 100~120mL mass point
Number is 50% ethylene glycol solution, continues to stir 1~2h, obtains reaction precursor liquid solution；Measure 150~200mL precursors molten
Liquid, is added in 150~200mL deionized waters, to load hydrothermal reaction kettle after 300~400r/min stirring mixing, 10~15min
In, 3~5h is reacted at 150~180 DEG C, is cooled to after room temperature and is transferred in centrifuge, is centrifuged with 6000~8000r/min
15~20min, must be precipitated, and precipitation be washed with deionized 3~5 times, then precipitation is added in 10~12L deionized waters, with
300W ultrasonic echographies disperse 1~2h, obtain nano tungsten trioxide coating liquid；Take one piece of 5cm × 10cm leaf, and by its upper surface
Polished with sand paper, then wash with absolute ethyl alcohol upper surface 3~5 times, roughening treatment is then carried out to upper surface to table with white fused alumina
Surface roughness Ra is 6~8 μm, then leaf is placed in drying box, and 3~5h is dried at 55~60 DEG C, surface preparation base is obtained
Piece；Surface preparation substrate is placed on warm table and is heated to 160~200 DEG C, then measures 12.5~15.0mL）The nanometer of preparation
Tungstic acid coating liquid is fitted into spray gun, and even application is in precondition substrate upper surface, and it is 0.25~0.30mL/ to control quantity for spray
cm2, 3~5h of heat growth is cooled to after room temperature, leaf upper surface is washed with deionized 2~3 times, then continues in baking oven,
3~4h is toasted at 300~400 DEG C, is cooled to after room temperature and obtains molybdenum doping tungstic trioxide nano-film material.
Reference examples：The WO 3 film material prepared using hydro-thermal method
Phototranstormation efficiency, the photoelectric current-voltage curve of WO 3 film material prepared by example 1 to example 3 and reference examples
Deng being detected, data such as table 1 is detected.
Table 1
| Detection project | Reference examples | Example 1 | Example 2 | Example 3 |
| The magnitude of current in 0.4V（mA） | 0.7 | 0.9 | 1.0 | 1.1 |
| Phototranstormation efficiency（When voltage is 0.4V）% | 0.5 | 0.8 | 0.75 | 0.78 |
As can be seen from Table 1, the WO 3 film material PhotoelectrocatalytiPerformance Performance that prepared by the present invention is good, and chemical property is superior.
Claims (4)
1. a kind of preparation method of molybdenum doping tungstic trioxide nano-film material, it is characterised in that specifically preparation process is：
（1）Reaction precursor liquid solution is prepared：Take white tungstic acid, molybdenum oxide to add in hydrogen peroxide, be heated to 95~100 DEG C, stirring is anti-
30~40min is answered, is cooled to after room temperature and adds ethylene glycol solution, continues 1~2h of stirring and obtains reaction precursor liquid solution；
（2）Nano tungsten trioxide coating liquid is prepared：Load hydrothermal reaction kettle after reaction precursor liquid solution is mixed with deionized water
In, 3~5h is reacted at 150~180 DEG C, ultrasonic disperse after washing is centrifuged and in deionized water, obtains nano tungsten trioxide
Coating liquid；
（3）Leaf is pre-processed：Leaf upper surface is polished with sand paper, then upper surface is entered with white fused alumina after being washed with absolute ethyl alcohol
Row roughening treatment, then after leaf is dried, obtain surface preparation substrate：
（4）Film：Surface preparation substrate is placed on warm table and is heated to 160~200 DEG C, then by nano tungsten trioxide film
Liquid is fitted into spray gun, and even application is cleaned and dried after cooling in precondition substrate upper surface, 3~5h of heat growth, obtains molybdenum doping
Tungstic trioxide nano-film material.
2. a kind of preparation method of molybdenum doping tungstic trioxide nano-film material as claimed in claim 1, it is characterised in that step
Suddenly（1）The white tungstic acid, molybdenum oxide, hydrogen peroxide, the parts by weight of ethylene glycol solution are 5~6 parts of white tungstic acids, 1.5~1.8 parts of oxidations
Molybdenum, 80~100 parts of mass fractions are that 30% hydrogen peroxide, 100~120 parts of mass fractions are 50% ethylene glycol solution.
3. a kind of preparation method of molybdenum doping tungstic trioxide nano-film material as claimed in claim 1, it is characterised in that step
Suddenly（3）The roughening treatment degree is that surface roughness Ra is polishing to white fused alumina is 6~8 μm.
4. a kind of preparation method of molybdenum doping tungstic trioxide nano-film material as claimed in claim 1, it is characterised in that step
Suddenly（4）The quantity for spray is 0.25~0.30mL/cm2。
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Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN112495401A (en) * | 2020-11-30 | 2021-03-16 | 华南理工大学 | Mo-doped MoO3@ZnIn2S4Z-system photocatalyst and preparation method and application thereof |
| CN113054168A (en) * | 2019-12-28 | 2021-06-29 | 湖南杉杉能源科技股份有限公司 | Tungsten-molybdenum composite coated ternary cathode material and preparation method thereof |
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