CN108889312A - A kind of sunlight all band photocatalytic nanometer array and preparation method thereof - Google Patents
A kind of sunlight all band photocatalytic nanometer array and preparation method thereof Download PDFInfo
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- 238000002360 preparation method Methods 0.000 title claims abstract description 25
- 230000001699 photocatalysis Effects 0.000 title claims abstract description 24
- GWEVSGVZZGPLCZ-UHFFFAOYSA-N titanium dioxide Inorganic materials O=[Ti]=O GWEVSGVZZGPLCZ-UHFFFAOYSA-N 0.000 claims abstract description 34
- 239000002071 nanotube Substances 0.000 claims abstract description 23
- OGIDPMRJRNCKJF-UHFFFAOYSA-N titanium oxide Inorganic materials [Ti]=O OGIDPMRJRNCKJF-UHFFFAOYSA-N 0.000 claims abstract description 21
- 239000010936 titanium Substances 0.000 claims abstract description 17
- RTAQQCXQSZGOHL-UHFFFAOYSA-N Titanium Chemical compound [Ti] RTAQQCXQSZGOHL-UHFFFAOYSA-N 0.000 claims abstract description 14
- 229910052719 titanium Inorganic materials 0.000 claims abstract description 14
- 238000000034 method Methods 0.000 claims abstract description 13
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 claims description 36
- LYCAIKOWRPUZTN-UHFFFAOYSA-N Ethylene glycol Chemical compound OCCO LYCAIKOWRPUZTN-UHFFFAOYSA-N 0.000 claims description 36
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Chemical compound O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims description 32
- 239000012153 distilled water Substances 0.000 claims description 24
- 238000001035 drying Methods 0.000 claims description 24
- 238000003756 stirring Methods 0.000 claims description 24
- 238000004528 spin coating Methods 0.000 claims description 19
- 238000001816 cooling Methods 0.000 claims description 18
- 235000019441 ethanol Nutrition 0.000 claims description 18
- 239000000758 substrate Substances 0.000 claims description 18
- CSCPPACGZOOCGX-UHFFFAOYSA-N Acetone Chemical compound CC(C)=O CSCPPACGZOOCGX-UHFFFAOYSA-N 0.000 claims description 12
- 230000008569 process Effects 0.000 claims description 8
- VHUUQVKOLVNVRT-UHFFFAOYSA-N Ammonium hydroxide Chemical compound [NH4+].[OH-] VHUUQVKOLVNVRT-UHFFFAOYSA-N 0.000 claims description 6
- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical compound [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 claims description 6
- GSEJCLTVZPLZKY-UHFFFAOYSA-N Triethanolamine Chemical compound OCCN(CCO)CCO GSEJCLTVZPLZKY-UHFFFAOYSA-N 0.000 claims description 6
- 239000000908 ammonium hydroxide Substances 0.000 claims description 6
- 239000003792 electrolyte Substances 0.000 claims description 6
- 238000011010 flushing procedure Methods 0.000 claims description 6
- 229910002804 graphite Inorganic materials 0.000 claims description 6
- 239000010439 graphite Substances 0.000 claims description 6
- 230000003647 oxidation Effects 0.000 claims description 6
- 238000007254 oxidation reaction Methods 0.000 claims description 6
- 238000005498 polishing Methods 0.000 claims description 6
- 238000005245 sintering Methods 0.000 claims description 6
- 150000001412 amines Chemical class 0.000 claims description 3
- UNTBPXHCXVWYOI-UHFFFAOYSA-O azanium;oxido(dioxo)vanadium Chemical compound [NH4+].[O-][V](=O)=O UNTBPXHCXVWYOI-UHFFFAOYSA-O 0.000 claims description 3
- 238000007146 photocatalysis Methods 0.000 abstract description 11
- 230000003197 catalytic effect Effects 0.000 abstract description 6
- 238000004064 recycling Methods 0.000 abstract description 4
- 150000001875 compounds Chemical class 0.000 abstract description 2
- 239000011941 photocatalyst Substances 0.000 abstract description 2
- 239000000843 powder Substances 0.000 abstract description 2
- 230000007613 environmental effect Effects 0.000 abstract 1
- 230000001737 promoting effect Effects 0.000 abstract 1
- 230000002787 reinforcement Effects 0.000 abstract 1
- 230000015556 catabolic process Effects 0.000 description 12
- 238000006731 degradation reaction Methods 0.000 description 12
- MCPLVIGCWWTHFH-UHFFFAOYSA-L methyl blue Chemical compound [Na+].[Na+].C1=CC(S(=O)(=O)[O-])=CC=C1NC1=CC=C(C(=C2C=CC(C=C2)=[NH+]C=2C=CC(=CC=2)S([O-])(=O)=O)C=2C=CC(NC=3C=CC(=CC=3)S([O-])(=O)=O)=CC=2)C=C1 MCPLVIGCWWTHFH-UHFFFAOYSA-L 0.000 description 12
- DLFVBJFMPXGRIB-UHFFFAOYSA-N Acetamide Chemical compound CC(N)=O DLFVBJFMPXGRIB-UHFFFAOYSA-N 0.000 description 6
- 239000003054 catalyst Substances 0.000 description 5
- QGZKDVFQNNGYKY-UHFFFAOYSA-O Ammonium Chemical compound [NH4+] QGZKDVFQNNGYKY-UHFFFAOYSA-O 0.000 description 3
- NINIDFKCEFEMDL-UHFFFAOYSA-N Sulfur Chemical compound [S] NINIDFKCEFEMDL-UHFFFAOYSA-N 0.000 description 3
- 239000005864 Sulphur Substances 0.000 description 3
- 238000012512 characterization method Methods 0.000 description 3
- 230000000694 effects Effects 0.000 description 3
- 238000005286 illumination Methods 0.000 description 3
- 125000002496 methyl group Chemical group [H]C([H])([H])* 0.000 description 3
- 230000005855 radiation Effects 0.000 description 3
- 238000004088 simulation Methods 0.000 description 3
- CURLTUGMZLYLDI-UHFFFAOYSA-N Carbon dioxide Chemical compound O=C=O CURLTUGMZLYLDI-UHFFFAOYSA-N 0.000 description 2
- UFHFLCQGNIYNRP-UHFFFAOYSA-N Hydrogen Chemical compound [H][H] UFHFLCQGNIYNRP-UHFFFAOYSA-N 0.000 description 2
- 238000010521 absorption reaction Methods 0.000 description 2
- QVGXLLKOCUKJST-UHFFFAOYSA-N atomic oxygen Chemical compound [O] QVGXLLKOCUKJST-UHFFFAOYSA-N 0.000 description 2
- 230000008859 change Effects 0.000 description 2
- 238000000354 decomposition reaction Methods 0.000 description 2
- 230000007812 deficiency Effects 0.000 description 2
- 229910052739 hydrogen Inorganic materials 0.000 description 2
- 239000001257 hydrogen Substances 0.000 description 2
- 238000012986 modification Methods 0.000 description 2
- 229910052760 oxygen Inorganic materials 0.000 description 2
- 239000001301 oxygen Substances 0.000 description 2
- 238000001228 spectrum Methods 0.000 description 2
- 206010070834 Sensitisation Diseases 0.000 description 1
- 239000001569 carbon dioxide Substances 0.000 description 1
- 229910002092 carbon dioxide Inorganic materials 0.000 description 1
- 239000002131 composite material Substances 0.000 description 1
- 238000005516 engineering process Methods 0.000 description 1
- 238000003912 environmental pollution Methods 0.000 description 1
- 239000000446 fuel Substances 0.000 description 1
- 238000004519 manufacturing process Methods 0.000 description 1
- 230000004048 modification Effects 0.000 description 1
- 231100000252 nontoxic Toxicity 0.000 description 1
- 230000003000 nontoxic effect Effects 0.000 description 1
- 239000002957 persistent organic pollutant Substances 0.000 description 1
- 239000002096 quantum dot Substances 0.000 description 1
- 230000009467 reduction Effects 0.000 description 1
- 230000008313 sensitization Effects 0.000 description 1
- 230000003595 spectral effect Effects 0.000 description 1
Classifications
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- B01J35/39—
-
- 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
- B01J27/00—Catalysts comprising the elements or compounds of halogens, sulfur, selenium, tellurium, phosphorus or nitrogen; Catalysts comprising carbon compounds
- B01J27/02—Sulfur, selenium or tellurium; Compounds thereof
- B01J27/04—Sulfides
-
- B01J35/40—
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- Chemical & Material Sciences (AREA)
- Engineering & Computer Science (AREA)
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Abstract
The present invention relates to a kind of sunlight all band photocatalytic nanometer array and preparation method thereof, which is nanometer VS4Fill TiO2Nano-tube array.Photocatalytic nanometer array made from the method for the present invention is firmly attached to titanium-based on piece, can facilitate recycling and be recycled, and overcomes the difficult problem of traditional powder photocatalyst recycling；The photocatalytic nanometer array is a nanometer VS4Fill TiO2Nano-tube array structure can inhibit the quick compound of photo-generate electron-hole, improve photocatalysis efficiency；Comprehensive TiO simultaneously2With excellent ultraviolet catalytic effect and VS4With excellent visible and near infrared light catalytic effect; nano-array is set to carry out photocatalysis using the sunlight all band from ultraviolet light near infrared light to greatest extent; for promoting nature sunlight photocatalysis technical application, alleviating energy crisis and reinforcement environmental improvement have great importance.
Description
Technical field
The present invention relates to photocatalysis fields, and in particular to a kind of preparation side of sunlight all band photocatalytic nanometer array
Method.
Background technique
Energy shortage and environmental pollution are the significant challenges that current mankind faces, and utilize sunlight catalytic hydrogen production by water decomposition system
Oxygen, reduction carbon dioxide and degradable organic pollutant are the important research hotspots of photocatalysis field.Realizing sunlight catalytic
In the process, construct efficient photochemical catalyst system play the role of it is conclusive.Delivered on Nature since 1972 about
TiO2After under the irradiation of ultraviolet light by water decomposition for hydrogen and oxygen, people are from every field to TiO2Photocatalysis has carried out depth
The principle of photocatalytic process is explored in the research entered, endeavours to improve photocatalysis efficiency.Research shows that TiO2Can be used as it is a kind of efficiently,
Nontoxic, stable photochemical catalyst.But due to TiO2Greater band gap (about 3.2 eV), only urged with the shorter ultraviolet light of wavelength
Change activity.However, ultraviolet light only accounts for about the 4% of total sun light intensity, to limit its extensive use.To make up TiO2Spectrum
The relatively narrow deficiency of absorption region improves catalytic efficiency, and a large amount of research is to TiO2Carry out the surfaces such as fuel sensitization, quantum dot sensitized
Modification.Visible light accounts for about the 48% of total sun light intensity, so people is attracted to adulterate TiO to visible light catalyst2Modification side
The research in face, to widen photochemical catalyst spectral absorption range.However, near infrared light accounts for total sun light intensity in solar spectrum
About 44%, but near infrared light wave band is realized without suitable photochemical catalyst all the time and is efficiently used, so that being unable to maximum limit
Degree carries out photocatalysis using the sunlight all band from ultraviolet light near infrared light.
Summary of the invention
Deficiency in view of the above technology, the present invention provide a kind of sunlight all band（Ultraviolet light, it is seen that light and near-infrared
Light）Photocatalytic nanometer array, the photocatalytic nanometer array are nanometer VS4Fill TiO2The composite material of nano-tube array.Meanwhile
The present invention provides a kind of methods for preparing the sunlight all band photocatalytic nanometer array.
A kind of preparation method of sunlight all band photocatalytic nanometer array, specifically synthesizes according to the following steps：
（One）,TiO2The preparation of nano-tube array
Abrasive paper for metallograph polishing will be carried out to titanium sheet first, then be cleaned by ultrasonic respectively with ethyl alcohol, acetone and distilled water, then with titanium sheet
For anode, graphite is to electrode, 1% NH4The ethylene glycol of F and the mixed liquor of water are electrolyte, in 1 h of oxidation at voltages of 50 V
Afterwards, it is successively cleaned up with ethyl alcohol and distilled water, then 80 DEG C of drying calcine 2 h under 400 DEG C of air, obtain hole after cooling
Diameter is about the TiO of 100 nm, regular appearance2Nano-tube array；
（Two）,VS4The preparation of colloidal sol
A certain amount of ammonium metavanadate is dissolved in distilled water and ethyl alcohol and stirs evenly to form solution A；By a certain amount of thioacetyl
Amine and triethanolamine, which are dissolved in ethylene glycol, to stir evenly to form solution B；Solution A is entered in solution B dropwise, is stirred when being added dropwise；
After being added dropwise, continue to stir 30 min, ammonium hydroxide is then added dropwise and adjusts pH=9.8 ~ 11.2, stops stirring；In 60 DEG C of water-baths
Lower place to the viscosity of colloidal sol is 2 ~ 5 mPas；
（Three）,TiO2/VS4The preparation of nano-array
By step（One）TiO obtained2Nano-tube array is adsorbed on the vacuum chuck of sol evenning machine, a dropping step（Two）It is configured
VS4Colloidal sol, 20 ~ 50s of spin coating under 3000 ~ 5000 r/min rotation speeds；The good substrate of spin coating is placed in 120 in drying box
~ 200 DEG C of 1 h of drying time use distilled water flushing substrate surface after cooling；Substrate is placed on sol evenning machine again after natural drying
On, in 300 ~ 500 DEG C of 2 h of vacuum-sintering after repeating above-mentioned spin coating process 2 ~ 5 times, TiO is obtained after cooling2/VS4Nano-array.
The present invention has the following advantages that：
One, photocatalytic nanometer array made from the method for the present invention is firmly attached to titanium-based on piece, can facilitate recycling and be recycled,
Overcome the difficult problem of traditional powder photocatalyst recycling；
Two, photocatalytic nanometer array of the invention is a nanometer VS4Fill TiO2Nano-tube array structure can inhibit photoproduction electric
Son-hole is quick compound, improves photocatalysis efficiency；
Three, the comprehensive TiO of the present invention2With excellent ultraviolet catalytic effect and VS4It is urged with excellent visible and near infrared light
Change effect, nano-array is made to carry out photocatalysis using the sunlight all band from ultraviolet light near infrared light to greatest extent.
Specific embodiment
Here is that in conjunction with specific embodiments, the present invention is further explained.These embodiments are merely to illustrate the present invention, but not
For limiting the scope of the invention.
It is of the invention the specific steps are：
（One）,TiO2The preparation of nano-tube array
Abrasive paper for metallograph polishing will be carried out to titanium sheet first, then be cleaned by ultrasonic respectively with ethyl alcohol, acetone and distilled water, then with titanium sheet
For anode, graphite is to electrode, 1% NH4The ethylene glycol of F and the mixed liquor of water are electrolyte, in 1 h of oxidation at voltages of 50 V
Afterwards, it is successively cleaned up with ethyl alcohol and distilled water, then 80 DEG C of drying calcine 2 h under 400 DEG C of air, obtain hole after cooling
Diameter is about the TiO of 100 nm, regular appearance2Nano-tube array；
（Two）,VS4The preparation of colloidal sol
A certain amount of ammonium metavanadate is dissolved in distilled water and ethyl alcohol and stirs evenly to form solution A；By a certain amount of thioacetyl
Amine and triethanolamine, which are dissolved in ethylene glycol, to stir evenly to form solution B；Solution A is entered in solution B dropwise, is stirred when being added dropwise；
After being added dropwise, continue to stir 30 min, ammonium hydroxide is then added dropwise and adjusts pH=9.8 ~ 11.2, stops stirring；In 60 DEG C of water-baths
Lower place to the viscosity of colloidal sol is 2 ~ 5 mPas；
（Three）,TiO2/VS4The preparation of nano-array
By step（One）TiO obtained2Nano-tube array is adsorbed on the vacuum chuck of sol evenning machine, a dropping step（Two）It is configured
VS4Colloidal sol, 20 ~ 50 s of spin coating under 3000 ~ 5000 r/min rotation speeds；The good substrate of spin coating is placed in drying box
120 ~ 200 DEG C of 1 h of drying time use distilled water flushing substrate surface after cooling；Substrate is placed on spin coating again after natural drying
On machine, in 300 ~ 500 DEG C of 2 h of vacuum-sintering after repeating above-mentioned spin coating process 2 ~ 5 times, TiO is obtained after cooling2/VS4Nano-array.
It can be prepared through the invention with sunlight all band（Ultraviolet light, it is seen that light and near infrared light）Photocatalysis effect
TiO2/VS4Nano-array.
Specific embodiment one：
（One）,TiO2The preparation of nano-tube array
Abrasive paper for metallograph polishing will be carried out to titanium sheet first, then be cleaned by ultrasonic respectively with ethyl alcohol, acetone and distilled water, then with titanium sheet
For anode, graphite is to electrode, 1% NH4The ethylene glycol of F and the mixed liquor of water are electrolyte, in 1 h of oxidation at voltages of 50 V
Afterwards, it is successively cleaned up with ethyl alcohol and distilled water, then 80 DEG C of drying calcine 2 h under 400 DEG C of air, obtain hole after cooling
Diameter is about the TiO of 100 nm, regular appearance2Nano-tube array；
（Two）,VS4The preparation of colloidal sol
1.17 g ammonium metavanadates are dissolved in 20 ml distilled water and 20 ml ethyl alcohol and stir evenly to form solution A；By 3.75 g sulphur
It is dissolved in 50ml ethylene glycol for acetamide and 3.725 g triethanolamines and stirs evenly to form solution B；Solution A is entered into solution B dropwise
In, it is stirred when being added dropwise；After being added dropwise, continue to stir 30 min, ammonium hydroxide is then added dropwise and adjusts pH=9.8, stops stirring
It mixes；Being placed under 60 DEG C of water-baths to the viscosity of colloidal sol is 3 mPas；
（Three）,TiO2/VS4The preparation of nano-array
By step（One）TiO obtained2Nano-tube array is adsorbed on the vacuum chuck of sol evenning machine, and 1 ml step is added dropwise（Two）Institute
The VS of configuration4Colloidal sol, 30 s of spin coating under 4000 r/min rotation speeds；The good substrate of spin coating is placed in drying box 150 DEG C
1 h of drying time uses distilled water flushing substrate surface after cooling；Substrate is placed on sol evenning machine again after natural drying, is repeated
In 400 DEG C of 2 h of vacuum-sintering after above-mentioned spin coating process 5 times, TiO is obtained after cooling2/VS4Nano-array.
XRD characterization is carried out to sample prepared by embodiment one, detects TiO2Object phase, VS4Object phase and Ti object phase；It is right
Sample prepared by embodiment one carries out Methyl blueness test, under 30 min ultraviolet lights, methyl blue
Degradation rate is 100%；Under 30 min radiation of visible light, the degradation rate of methyl blue is 46%；Under 30 min near infrared lights,
The degradation rate of methyl blue is 22%；In the case where the big solar illumination of 30 min simulation is penetrated, the degradation rate of methyl blue is 34%.
Specific embodiment two：
（One）,TiO2The preparation of nano-tube array
Abrasive paper for metallograph polishing will be carried out to titanium sheet first, then be cleaned by ultrasonic respectively with ethyl alcohol, acetone and distilled water, then with titanium sheet
For anode, graphite is to electrode, 1% NH4The ethylene glycol of F and the mixed liquor of water are electrolyte, in 1 h of oxidation at voltages of 50 V
Afterwards, it is successively cleaned up with ethyl alcohol and distilled water, then 80 DEG C of drying calcine 2 h under 400 DEG C of air, obtain hole after cooling
Diameter is about the TiO of 100 nm, regular appearance2Nano-tube array；
（Two）,VS4The preparation of colloidal sol
1.17 g ammonium metavanadates are dissolved in 30 ml distilled water and 10 ml ethyl alcohol and stir evenly to form solution A；By 3.75 g sulphur
It is dissolved in 50 ml ethylene glycol for acetamide and 3.725 g triethanolamines and stirs evenly to form solution B；Solution A is entered into solution dropwise
In B, stirred when being added dropwise；After being added dropwise, continue to stir 30 min, ammonium hydroxide is then added dropwise and adjusts pH=11.2, stops stirring
It mixes；Being placed under 60 DEG C of water-baths to the viscosity of colloidal sol is 5 mPas；
（Three）,TiO2/VS4The preparation of nano-array
By step（One）TiO obtained2Nano-tube array is adsorbed on the vacuum chuck of sol evenning machine, and 5 ml steps are added dropwise（Two）Institute
The VS of configuration4Colloidal sol, 50 s of spin coating under 5000 r/min rotation speeds；The good substrate of spin coating is placed in drying box 200 DEG C
1 h of drying time uses distilled water flushing substrate surface after cooling；Substrate is placed on sol evenning machine again after natural drying, is repeated
In 500 DEG C of 2 h of vacuum-sintering after above-mentioned spin coating process 2 times, TiO is obtained after cooling2/VS4Nano-array.
XRD characterization is carried out to sample prepared by embodiment two, detects TiO2Object phase, VS4Object phase and Ti object phase；It is right
Sample prepared by embodiment two carries out Methyl blueness test, under 30 min ultraviolet lights, methyl blue
Degradation rate is 100%；Under 30 min radiation of visible light, the degradation rate of methyl blue is 57%；Under 30 min near infrared lights,
The degradation rate of methyl blue is 29%；In the case where the big solar illumination of 30 min simulation is penetrated, the degradation rate of methyl blue is 43%.
Specific embodiment three：
（One）,TiO2The preparation of nano-tube array
Abrasive paper for metallograph polishing will be carried out to titanium sheet first, then be cleaned by ultrasonic respectively with ethyl alcohol, acetone and distilled water, then with titanium sheet
For anode, graphite is to electrode, 1% NH4The ethylene glycol of F and the mixed liquor of water are electrolyte, in 1 h of oxidation at voltages of 50 V
Afterwards, it is successively cleaned up with ethyl alcohol and distilled water, then 80 DEG C of drying calcine 2 h under 400 DEG C of air, obtain hole after cooling
Diameter is about the TiO of 100 nm, regular appearance2Nano-tube array；
（Two）,VS4The preparation of colloidal sol
1.17 g ammonium metavanadates are dissolved in 10 ml distilled water and 30 ml ethyl alcohol and stir evenly to form solution A；By 3.75 g sulphur
It is dissolved in 50ml ethylene glycol for acetamide and 3.725 g triethanolamines and stirs evenly to form solution B；Solution A is entered into solution B dropwise
In, it is stirred when being added dropwise；After being added dropwise, continue to stir 30 min, ammonium hydroxide is then added dropwise and adjusts pH=10.5, stops stirring
It mixes；Being placed under 60 DEG C of water-baths to the viscosity of colloidal sol is 2 mPas；
（Three）,TiO2/VS4The preparation of nano-array
By step（One）TiO obtained2Nano-tube array is adsorbed on the vacuum chuck of sol evenning machine, and 3 ml steps are added dropwise（Two）Institute
The VS of configuration4Colloidal sol, 20 s of spin coating under 3000 r/min rotation speeds；The good substrate of spin coating is placed in drying box 120 DEG C
1 h of drying time uses distilled water flushing substrate surface after cooling；Substrate is placed on sol evenning machine again after natural drying, is repeated
In 300 DEG C of 2 h of vacuum-sintering after above-mentioned spin coating process 3 times, TiO is obtained after cooling2/VS4Nano-array.
XRD characterization is carried out to sample prepared by embodiment three, detects TiO2Object phase, VS4Object phase and Ti object phase；It is right
Sample prepared by embodiment three carries out Methyl blueness test, under 30 min ultraviolet lights, methyl blue
Degradation rate is 100%；Under 30 min radiation of visible light, the degradation rate of methyl blue is 50%；Under 30 min near infrared lights,
The degradation rate of methyl blue is 26%；In the case where the big solar illumination of 30 min simulation is penetrated, the degradation rate of methyl blue is 38%.
Claims (1)
1. a kind of sunlight all band photocatalytic nanometer array and preparation method thereof, it is characterised in that the nano-array is nanometer VS4
Fill TiO2The preparation method of nano-tube array, the nano-array includes the following steps：
（One）,TiO2The preparation of nano-tube array
Abrasive paper for metallograph polishing will be carried out to titanium sheet first, then be cleaned by ultrasonic respectively with ethyl alcohol, acetone and distilled water, then with titanium sheet
For anode, graphite is to electrode, 1% NH4The ethylene glycol of F and the mixed liquor of water are electrolyte, in 1 h of oxidation at voltages of 50 V
Afterwards, it is successively cleaned up with ethyl alcohol and distilled water, then 80 DEG C of drying calcine 2 h under 400 DEG C of air, obtain hole after cooling
Diameter is about the TiO of 100 nm, regular appearance2Nano-tube array；
（Two）,VS4The preparation of colloidal sol
A certain amount of ammonium metavanadate is dissolved in distilled water and ethyl alcohol and stirs evenly to form solution A；By a certain amount of thioacetyl
Amine and triethanolamine, which are dissolved in ethylene glycol, to stir evenly to form solution B；Solution A is entered in solution B dropwise, is stirred when being added dropwise；
After being added dropwise, continue to stir 30 min, ammonium hydroxide is then added dropwise and adjusts pH=9.8 ~ 11.2, stops stirring；In 60 DEG C of water-baths
Lower place to the viscosity of colloidal sol is 2 ~ 5 mPas；
（Three）,TiO2/VS4The preparation of nano-array
By step（One）TiO obtained2Nano-tube array is adsorbed on the vacuum chuck of sol evenning machine, a dropping step（Two）It is configured
VS4Colloidal sol, 20 ~ 50 s of spin coating under 3000 ~ 5000 r/min rotation speeds；The good substrate of spin coating is placed in drying box
120 ~ 200 DEG C of drying time 1h use distilled water flushing substrate surface after cooling；Substrate is placed on sol evenning machine again after natural drying
On, in 300 ~ 500 DEG C of 2 h of vacuum-sintering after repeating above-mentioned spin coating process 2 ~ 5 times, TiO is obtained after cooling2/VS4Nano-array.
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| CN110240222A (en) * | 2019-05-24 | 2019-09-17 | 同济大学 | A kind of photoelectrocatalytioxidation oxidation system and its conversion of degradable organic pollutant orientation to synthesis gas method |
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| CN110240222A (en) * | 2019-05-24 | 2019-09-17 | 同济大学 | A kind of photoelectrocatalytioxidation oxidation system and its conversion of degradable organic pollutant orientation to synthesis gas method |
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