CN106179415B - A kind of preparation method of nano-titanium dioxide/molybdenum disulfide composite material film - Google Patents
A kind of preparation method of nano-titanium dioxide/molybdenum disulfide composite material film Download PDFInfo
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- CN106179415B CN106179415B CN201610478492.4A CN201610478492A CN106179415B CN 106179415 B CN106179415 B CN 106179415B CN 201610478492 A CN201610478492 A CN 201610478492A CN 106179415 B CN106179415 B CN 106179415B
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- CWQXQMHSOZUFJS-UHFFFAOYSA-N molybdenum disulfide Chemical compound S=[Mo]=S CWQXQMHSOZUFJS-UHFFFAOYSA-N 0.000 title claims abstract description 57
- 229910052982 molybdenum disulfide Inorganic materials 0.000 title claims abstract description 56
- SOQBVABWOPYFQZ-UHFFFAOYSA-N oxygen(2-);titanium(4+) Chemical compound [O-2].[O-2].[Ti+4] SOQBVABWOPYFQZ-UHFFFAOYSA-N 0.000 title claims abstract description 32
- 239000002131 composite material Substances 0.000 title claims abstract description 18
- 238000002360 preparation method Methods 0.000 title claims abstract description 11
- 239000000084 colloidal system Substances 0.000 claims abstract description 18
- SQGYOTSLMSWVJD-UHFFFAOYSA-N silver(1+) nitrate Chemical compound [Ag+].[O-]N(=O)=O SQGYOTSLMSWVJD-UHFFFAOYSA-N 0.000 claims abstract description 16
- 229910000831 Steel Inorganic materials 0.000 claims abstract description 15
- 239000010959 steel Substances 0.000 claims abstract description 15
- BQCADISMDOOEFD-UHFFFAOYSA-N Silver Chemical compound [Ag] BQCADISMDOOEFD-UHFFFAOYSA-N 0.000 claims abstract description 13
- 229910052709 silver Inorganic materials 0.000 claims abstract description 13
- 239000004332 silver Substances 0.000 claims abstract description 13
- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical compound [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 claims abstract description 11
- 238000004070 electrodeposition Methods 0.000 claims abstract description 10
- 229910002804 graphite Inorganic materials 0.000 claims abstract description 9
- 239000010439 graphite Substances 0.000 claims abstract description 9
- 239000003792 electrolyte Substances 0.000 claims abstract description 8
- 238000007788 roughening Methods 0.000 claims abstract description 8
- 229910001961 silver nitrate Inorganic materials 0.000 claims abstract description 8
- 230000015572 biosynthetic process Effects 0.000 claims abstract description 6
- 229920001343 polytetrafluoroethylene Polymers 0.000 claims abstract description 5
- 238000009210 therapy by ultrasound Methods 0.000 claims abstract description 3
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Chemical compound O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims description 25
- 239000008367 deionised water Substances 0.000 claims description 18
- 229910021641 deionized water Inorganic materials 0.000 claims description 18
- BDERNNFJNOPAEC-UHFFFAOYSA-N propan-1-ol Chemical compound CCCO BDERNNFJNOPAEC-UHFFFAOYSA-N 0.000 claims description 16
- 239000007921 spray Substances 0.000 claims description 14
- VXUYXOFXAQZZMF-UHFFFAOYSA-N titanium(IV) isopropoxide Chemical compound CC(C)O[Ti](OC(C)C)(OC(C)C)OC(C)C VXUYXOFXAQZZMF-UHFFFAOYSA-N 0.000 claims description 14
- 238000006243 chemical reaction Methods 0.000 claims description 13
- 238000003756 stirring Methods 0.000 claims description 13
- 239000000126 substance Substances 0.000 claims description 12
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 claims description 11
- 239000012265 solid product Substances 0.000 claims description 9
- 238000002604 ultrasonography Methods 0.000 claims description 9
- LZZYPRNAOMGNLH-UHFFFAOYSA-M Cetrimonium bromide Chemical compound [Br-].CCCCCCCCCCCCCCCC[N+](C)(C)C LZZYPRNAOMGNLH-UHFFFAOYSA-M 0.000 claims description 7
- KFZMGEQAYNKOFK-UHFFFAOYSA-N Isopropanol Chemical compound CC(C)O KFZMGEQAYNKOFK-UHFFFAOYSA-N 0.000 claims description 7
- 238000002156 mixing Methods 0.000 claims description 6
- UMGDCJDMYOKAJW-UHFFFAOYSA-N thiourea Chemical compound NC(N)=S UMGDCJDMYOKAJW-UHFFFAOYSA-N 0.000 claims description 6
- HEAUFJZALFKPBA-JPQUDPSNSA-N (3s)-3-[[(2s,3r)-2-[[(2s)-6-amino-2-[[(2s)-2-amino-3-(1h-imidazol-5-yl)propanoyl]amino]hexanoyl]amino]-3-hydroxybutanoyl]amino]-4-[[(2s)-1-[[(2s)-1-[[(2s)-1-[[2-[[(2s)-1-[[(2s)-1-amino-4-methylsulfanyl-1-oxobutan-2-yl]amino]-4-methyl-1-oxopentan-2-yl]amin Chemical compound C([C@@H](C(=O)N[C@H](C(=O)NCC(=O)N[C@@H](CC(C)C)C(=O)N[C@@H](CCSC)C(N)=O)C(C)C)NC(=O)[C@H](CO)NC(=O)[C@H](CC(O)=O)NC(=O)[C@@H](NC(=O)[C@H](CCCCN)NC(=O)[C@@H](N)CC=1NC=NC=1)[C@@H](C)O)C1=CC=CC=C1 HEAUFJZALFKPBA-JPQUDPSNSA-N 0.000 claims description 4
- 101800000399 Neurokinin A Proteins 0.000 claims description 4
- 102100024304 Protachykinin-1 Human genes 0.000 claims description 4
- 238000007605 air drying Methods 0.000 claims description 4
- 239000012300 argon atmosphere Substances 0.000 claims description 3
- 238000010438 heat treatment Methods 0.000 claims description 3
- 235000015393 sodium molybdate Nutrition 0.000 claims description 3
- 239000011684 sodium molybdate Substances 0.000 claims description 3
- TVXXNOYZHKPKGW-UHFFFAOYSA-N sodium molybdate (anhydrous) Chemical compound [Na+].[Na+].[O-][Mo]([O-])(=O)=O TVXXNOYZHKPKGW-UHFFFAOYSA-N 0.000 claims description 3
- 238000001291 vacuum drying Methods 0.000 claims description 3
- 230000008859 change Effects 0.000 claims description 2
- 238000004140 cleaning Methods 0.000 claims description 2
- 238000007865 diluting Methods 0.000 claims description 2
- 229910021389 graphene Inorganic materials 0.000 claims description 2
- 238000005507 spraying Methods 0.000 claims description 2
- 240000007594 Oryza sativa Species 0.000 claims 1
- 235000007164 Oryza sativa Nutrition 0.000 claims 1
- RTAQQCXQSZGOHL-UHFFFAOYSA-N Titanium Chemical compound [Ti] RTAQQCXQSZGOHL-UHFFFAOYSA-N 0.000 claims 1
- 235000013339 cereals Nutrition 0.000 claims 1
- 235000009566 rice Nutrition 0.000 claims 1
- VYPSYNLAJGMNEJ-UHFFFAOYSA-N silicon dioxide Inorganic materials O=[Si]=O VYPSYNLAJGMNEJ-UHFFFAOYSA-N 0.000 claims 1
- 239000000377 silicon dioxide Substances 0.000 claims 1
- BFKJFAAPBSQJPD-UHFFFAOYSA-N tetrafluoroethene Chemical compound FC(F)=C(F)F BFKJFAAPBSQJPD-UHFFFAOYSA-N 0.000 claims 1
- 229910052719 titanium Inorganic materials 0.000 claims 1
- 239000010936 titanium Substances 0.000 claims 1
- GWEVSGVZZGPLCZ-UHFFFAOYSA-N Titan oxide Chemical compound O=[Ti]=O GWEVSGVZZGPLCZ-UHFFFAOYSA-N 0.000 abstract description 30
- 239000004408 titanium dioxide Substances 0.000 abstract description 13
- HGWOWDFNMKCVLG-UHFFFAOYSA-N [O--].[O--].[Ti+4].[Ti+4] Chemical compound [O--].[O--].[Ti+4].[Ti+4] HGWOWDFNMKCVLG-UHFFFAOYSA-N 0.000 abstract description 2
- 230000006872 improvement Effects 0.000 abstract description 2
- 238000003912 environmental pollution Methods 0.000 abstract 1
- 239000000243 solution Substances 0.000 description 68
- 238000000034 method Methods 0.000 description 9
- 239000000463 material Substances 0.000 description 6
- 230000008569 process Effects 0.000 description 6
- -1 12h is placed Substances 0.000 description 5
- 238000001035 drying Methods 0.000 description 5
- 239000011259 mixed solution Substances 0.000 description 5
- 239000003054 catalyst Substances 0.000 description 4
- 150000001875 compounds Chemical class 0.000 description 4
- ZOKXTWBITQBERF-UHFFFAOYSA-N Molybdenum Chemical compound [Mo] ZOKXTWBITQBERF-UHFFFAOYSA-N 0.000 description 3
- 238000005234 chemical deposition Methods 0.000 description 3
- 230000005611 electricity Effects 0.000 description 3
- 239000007789 gas Substances 0.000 description 3
- JEIPFZHSYJVQDO-UHFFFAOYSA-N iron(III) oxide Inorganic materials O=[Fe]O[Fe]=O JEIPFZHSYJVQDO-UHFFFAOYSA-N 0.000 description 3
- 239000000203 mixture Substances 0.000 description 3
- 229910052750 molybdenum Inorganic materials 0.000 description 3
- 239000011733 molybdenum Substances 0.000 description 3
- 229910000510 noble metal Inorganic materials 0.000 description 3
- 239000004065 semiconductor Substances 0.000 description 3
- BOTDANWDWHJENH-UHFFFAOYSA-N Tetraethyl orthosilicate Chemical compound CCO[Si](OCC)(OCC)OCC BOTDANWDWHJENH-UHFFFAOYSA-N 0.000 description 2
- 238000005516 engineering process Methods 0.000 description 2
- 230000004048 modification Effects 0.000 description 2
- 238000012986 modification Methods 0.000 description 2
- 239000002114 nanocomposite Substances 0.000 description 2
- 230000001699 photocatalysis Effects 0.000 description 2
- BASFCYQUMIYNBI-UHFFFAOYSA-N platinum Chemical compound [Pt] BASFCYQUMIYNBI-UHFFFAOYSA-N 0.000 description 2
- RYGMFSIKBFXOCR-UHFFFAOYSA-N Copper Chemical compound [Cu] RYGMFSIKBFXOCR-UHFFFAOYSA-N 0.000 description 1
- 230000009102 absorption Effects 0.000 description 1
- 238000010521 absorption reaction Methods 0.000 description 1
- 150000001336 alkenes Chemical class 0.000 description 1
- 230000015556 catabolic process Effects 0.000 description 1
- 230000003197 catalytic effect Effects 0.000 description 1
- 238000006555 catalytic reaction Methods 0.000 description 1
- 239000007795 chemical reaction product Substances 0.000 description 1
- 239000003795 chemical substances by application Substances 0.000 description 1
- 239000000356 contaminant Substances 0.000 description 1
- 229910052802 copper Inorganic materials 0.000 description 1
- 239000010949 copper Substances 0.000 description 1
- 238000000354 decomposition reaction Methods 0.000 description 1
- 238000006731 degradation reaction Methods 0.000 description 1
- 229960000935 dehydrated alcohol Drugs 0.000 description 1
- 238000000151 deposition Methods 0.000 description 1
- 230000002500 effect on skin Effects 0.000 description 1
- 230000000694 effects Effects 0.000 description 1
- 230000007613 environmental effect Effects 0.000 description 1
- 239000003344 environmental pollutant Substances 0.000 description 1
- 239000012535 impurity Substances 0.000 description 1
- 238000005468 ion implantation Methods 0.000 description 1
- 229910021645 metal ion Inorganic materials 0.000 description 1
- 239000002086 nanomaterial Substances 0.000 description 1
- 239000002135 nanosheet Substances 0.000 description 1
- 230000003287 optical effect Effects 0.000 description 1
- 230000003647 oxidation Effects 0.000 description 1
- 238000007254 oxidation reaction Methods 0.000 description 1
- 238000007146 photocatalysis Methods 0.000 description 1
- 229910052697 platinum Inorganic materials 0.000 description 1
- 231100000719 pollutant Toxicity 0.000 description 1
- 238000004064 recycling Methods 0.000 description 1
- 230000009467 reduction Effects 0.000 description 1
- 230000004044 response Effects 0.000 description 1
- 230000005476 size effect Effects 0.000 description 1
- 238000001179 sorption measurement Methods 0.000 description 1
- 229910001220 stainless steel Inorganic materials 0.000 description 1
- 239000010935 stainless steel Substances 0.000 description 1
- 238000006467 substitution reaction Methods 0.000 description 1
- 238000005406 washing Methods 0.000 description 1
Classifications
-
- 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
- B01J27/047—Sulfides with chromium, molybdenum, tungsten or polonium
- B01J27/051—Molybdenum
-
- B01J35/39—
-
- B01J35/51—
-
- 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
- B01J37/00—Processes, in general, for preparing catalysts; Processes, in general, for activation of catalysts
- B01J37/34—Irradiation by, or application of, electric, magnetic or wave energy, e.g. ultrasonic waves ; Ionic sputtering; Flame or plasma spraying; Particle radiation
- B01J37/348—Electrochemical processes, e.g. electrochemical deposition or anodisation
Abstract
The present invention relates to a kind of nano-titanium dioxide/molybdenum disulfide composite material film preparation methods.The molybdenum disulfide of nanometer titanium dioxide titanium solution and spherical structure is prepared respectively, titanium dioxide/molybdenum disulfide composite material colloid is obtained by ptfe autoclave and ultrasonic treatment, colloid is sprayed on formation nano-titanium dioxide/molybdenum disulfide laminated film on the stainless (steel) wire of roughening, using silver nitrate solution as electrochemical deposition electrolyte, stainless (steel) wire is cathode, graphite is anode, silver nano-grain is deposited on nano-titanium dioxide/molybdenum disulfide laminated film, nano-titanium dioxide/molybdenum disulfide composite material film of silver nano-grain antipoints array is obtained.Nano-titanium dioxide prepared by the present invention/molybdenum disulfide composite material film can be widely used for environmental pollution improvement.
Description
Technical field
The present invention relates to environmental technology fields, and in particular to a kind of nano-titanium dioxide/molybdenum disulfide composite material film
Preparation method.
Background technique
Light-catalyzed reaction is considered as a green pollution treatment technology by catalyst of semiconductor, in numerous semiconductor materials
In, titanium dioxide is most potential photochemical catalyst, but since titanium dioxide is wide band gap semiconducter (~3.2eV), is only capable of inhaling
Receive 3~5% sunlights；Meanwhile photo-generate electron-hole is easily compound in titanium dioxide, so that titanium dioxide optical catalyst pair
Solar energy utilization ratio is lower.
In consideration of it, people using many methods to titania modified and promote its performance, wherein there are three types of most,
First is that material structure nanosizing itself, the skin effect and quantum size effect of nano material make the property of material change；
Second is that it is noble metal decorated, pass through Sol Doping (Nakata K, 2009Mater.Lett 631628), metal ion implantation
(Zheng S K.2002Vacuum65 155), cosputtering surface modification (Zhang X W,
Method 2005Mater.Chem.Phys.9173) is noble metal decorated in titanium dioxide surface by silver, copper, platinum etc..Due to nanometer
The specific surface area of material is larger, and adsorption capacity is stronger, and the surface of synthetic sample can remain more organic agent molecule, simple
The superiority of the nanocomposite of noble metal and titanium dioxide is difficult to give full play to.Third is that semiconductor material is compound.Curing
Molybdenum has excellent catalytic properties, and has been a concern, after the size of molybdenum disulfide reaches nanoscale, in visible region
There are good absorptions, can directly utilize sunlight degradation of contaminant.The mainly curing compound with titanium dioxide at present
Molybdenum nanometer sheet since the marginal layer of molybdenum disulfide in molybdenum disulfide nano sheet/composite titania material is more active, thus is reacted
During pollutant process the decomposition of itself easily occurs for active high, poor chemical stability, leads to the secondary pollution of environment,
It is unfavorable for the recycling and reuse of catalyst.
Summary of the invention
For the above-mentioned problems in the prior art, the purpose of the present invention is to provide a kind of nano-titanium dioxide/bis-
The preparation method of molybdenum sulfide composite material film is interlocked the different of mode by reducing the forbidden bandwidth of titanium dioxide, generating II type
Matter junction structure and reduction meet the generation at center, improve photocatalytic activity and light utilization efficiency；By generating molybdenum disulfide nano
The long-time stability of ball raising composite material.
The technical solution that the present invention takes: a kind of preparation method of nano-titanium dioxide/molybdenum disulfide composite material film,
Step 1: diluting titanium isopropoxide with 2- propyl alcohol, solution A is obtained；
Step 2: solution A is added dropwise in 2- aqueous propanol solution, stands 10h-12h and obtain solution B；
Step 3: CTAB is dissolved in deionized water in stirring, then GOS is added in CTAB solution while stirring,
Stirring for 24 hours, obtains solution C；
Step 4: sodium molybdate is added in solution C while stirring, thiocarbamide then is added after ultrasound 30min, ultrasound is straight again
To the uniform solution D of acquisition；
Step 5: deionized water is added into solution D obtains solution E, so that the concentration of CTAB is maintained in E solution
0.02mol/L；
Solution F is obtained for 24 hours in 220 DEG C of reactions step 6: solution E is transferred in ptfe autoclave, wait react
After kettle naturally cools to room temperature, solution F is transferred in beaker；
Step 7: doing centrifuging treatment to solution F, black solid product G is obtained；
Step 8: first cleaning 3 black solid product G with deionized water, then with washes of absolute alcohol 3 times；
Step 9: the black solid product G after washes of absolute alcohol is put into 80 DEG C of dry 12h in vacuum oven；
Step 10: 800 DEG C of heat treatment 2h obtain spherical shape to the black solid product G after dry under argon atmosphere in tube furnace
The molybdenum disulfide of structure；
Step 11: the molybdenum disulfide of solution B and spherical structure is blended in 2- aqueous propanol solution, 10h is quickly stirred,
Obtain Solution H；
Step 12: Solution H is put into reaction kettle, 25h is reacted at 150 DEG C -250 DEG C and obtains solution I, certainly to reaction kettle
After being so cooled to room temperature, solution I is transferred in beaker；
Step 13: doing centrifuging treatment to solution I, substance J is obtained；
Step 14: after substance J is washed 3 times with deionized water, put dry at 100 DEG C -150 DEG C in a vacuum drying oven
20h obtains substance K；
Step 15: substance K is put into deionized water, doing ultrasonic treatment makes the two uniformly mixing, obtains colloid L；
Step 16: colloid K is sprayed on formation nano-titanium dioxide/molybdenum disulfide THIN COMPOSITE on the stainless (steel) wire of roughening
Film, air drying 30min；
Step 17: repeating the 16th step, make nano-titanium dioxide/molybdenum disulfide laminated film with a thickness of 500-600nm；
Step 18: stainless (steel) wire is cathode using silver nitrate solution as electrochemical deposition electrolyte, graphite is anode, will
Silver nano-grain is deposited on nano-titanium dioxide/molybdenum disulfide laminated film, obtains the nanometer of silver nano-grain antipoints array
Titanium dioxide/molybdenum disulfide composite material film.
When the solution B is mixed with the molybdenum disulfide of spherical structure, the mass fraction of molybdenum disulfide is 2%-10%.
The 2- aqueous propanol solution, the volume ratio of the third alcohol and water of 2- are 2: 1-2: 3.
Spray power of the colloid E in spraying is 100W, spray pressure 0.3-1.8kg/cm2.
The quick speed of agitator is 3000r/min-5000r/min.
The utility model has the advantages that
1. introducing molybdenum disulfide impurity energy level in titanium dioxide forbidden band, the forbidden bandwidth of titanium dioxide, raising pair are reduced
The absorptivity of visible light；
2. depositing silver-colored antipoints array on nano-titanium dioxide/molybdenum disulfide film surface, light induced electron will be from titanium dioxide
Titanium is migrated to silver, so that light induced electron and hole are separated, is reduced complex centre and is generated, improve photo-quantum efficiency and photocatalysis
Activity；
3. titanium dioxide, the top of valence band of molybdenum disulfide and conduction band bottom will form II type interlock mode heterojunction structure not only
The response range of visible light can be increased, and generate electron-hole clock synchronization in visible light stimulus, avoid the fast of photo-generated carrier
Reply immediately conjunction；
4. the molybdenum disulfide of spherical structure has better stability relative to the molybdenum disulfide of laminated structure.
Specific embodiment
Below with reference to embodiment, the present invention will be further described.
Ethyl orthosilicate (2.4mmol) is dissolved in 60ml deionized water in stirring first, it then while stirring will oxidation
Graphene (6mmol) is added in teos solution.Mixture stirs for 24 hours so that ethyl orthosilicate is adsorbed in graphite oxide
Alkene surface.Sodium molybdate (3mmol) is dissolved in mixture in stirring later, is added after ultrasonic 30min thiocarbamide (12mmol) and again
Ultrasonic 30min is to obtain uniform solution.Deionized water is subsequently added into until the volume of mixture is about 120ml (so that CTAB
Concentration be maintained at 0.02mol/l) and be transferred in 200ml ptfe autoclave 220 DEG C reaction for 24 hours.To reaction kettle
After cooled to room temperature, the isolated black solid product of centrifuge washing respectively cleans 3 times simultaneously with deionized water and dehydrated alcohol
80 DEG C of dry 12h in a vacuum drying oven.800 DEG C of heat treatment 2h obtain curing to end product under argon atmosphere in tube furnace
Molybdenum.
Embodiment 1:
5ml titanium isopropoxide is measured, is diluted with the 2- propyl alcohol of 45ml, is obtained solution A, solution A is added dropwise to
In 26ml2- propyl alcohol and 26ml water mixed solution, 12h is placed, solution B is obtained；The molybdenum disulfide of solution B and 2wt% are blended in
In the 2- aqueous propanol solution that 20 milliliters of volume ratios are 1: 1,5h is stirred under the revolving speed of 3000r/min, obtains solution C, then by solution C
It is put into reaction kettle, is reacted at 200 DEG C for 24 hours, is washed with deionized 3 times 3, drying for 24 hours, obtains substance D at 105 DEG C；It will
Substance D is added in deionized water, is uniformly mixed using 750 watts of ultrasounds, obtains colloid E；Colloid E is sprayed on the stainless of roughening
Nano-titanium dioxide/molybdenum disulfide laminated film is formed on steel mesh, wherein spray power is 100w, spray pressure 0.6kg/
Cm2, air drying 30min, the process are repeated 4 times, and film thickness is 500 nanometers；Using silver nitrate solution as electrochemical deposition
Electrolyte, stainless (steel) wire are cathode, and graphite is anode, and it is compound that silver nano-grain is deposited on nano-titanium dioxide/molybdenum disulfide
On film, electrochemical deposition voltage is 12v.
Embodiment 2:
5ml titanium isopropoxide is measured, is diluted with the 2- propyl alcohol of 45ml, is obtained solution A, solution A is added dropwise to
In 26ml2- propyl alcohol and 26ml water mixed solution, 12h is placed, solution B is obtained；The molybdenum disulfide of solution B and 4wt% are blended in
In the 2- aqueous propanol solution that 20ml volume ratio is 1: 1,5h is stirred under the revolving speed of 3000r/min, obtains solution C, then solution C is put
Enter reaction kettle, reacted at 200 DEG C for 24 hours, is washed with deionized 3 times 3, drying for 24 hours, obtains substance D at 105 DEG C；By object
Matter D is added in deionized water, using the uniformly mixing of 750w ultrasound, obtains colloid E；Colloid E is sprayed on the stainless (steel) wire of roughening
Upper formation nano-titanium dioxide/molybdenum disulfide laminated film, wherein spray power is 100w, spray pressure 0.8kg/cm2, sky
Dry 30min, the process are repeated 4 times in gas, film thickness 500nm；Using silver nitrate solution as electrochemical deposition electrolyte, no
Rust steel mesh is cathode, and graphite is anode, and silver nano-grain is deposited on nano-titanium dioxide/molybdenum disulfide laminated film, electricity
Chemical deposition voltage is 12v.
Embodiment 3:
5ml titanium isopropoxide is measured, is diluted with the 2- propyl alcohol of 45ml, is obtained solution A, solution A is added dropwise to
In 26ml2- propyl alcohol and 26ml water mixed solution, 12h is placed, solution B is obtained；The molybdenum disulfide of solution B and 6wt% are blended in
In the 2- aqueous propanol solution that 20ml volume ratio is 1: 1,5h is stirred under the revolving speed of 3000r/min, obtains solution C, then solution C is put
Enter reaction kettle, reacted at 200 DEG C for 24 hours, is washed with deionized 3 times 3, drying for 24 hours, obtains substance D at 105 DEG C；By object
Matter D is added in deionized water, using the uniformly mixing of 750w ultrasound, obtains colloid E；Colloid E is sprayed on the stainless (steel) wire of roughening
Upper formation nano-titanium dioxide/molybdenum disulfide laminated film, wherein spray power is 100w, spray pressure 1.1kg/cm2, sky
Dry 30min, the process are repeated 4 times in gas, film thickness 500nm；Using silver nitrate solution as electrochemical deposition electrolyte, no
Rust steel mesh is cathode, and graphite is anode, and silver nano-grain is deposited on nano-titanium dioxide/molybdenum disulfide laminated film, electricity
Chemical deposition voltage is 12v.
Embodiment 4:
5ml titanium isopropoxide is measured, is diluted with the 2- propyl alcohol of 45ml, is obtained solution A, solution A is added dropwise to
In 26ml2- propyl alcohol and 26ml water mixed solution, 12h is placed, solution B is obtained；The molybdenum disulfide of solution B and 8wt% are blended in
In the 2- aqueous propanol solution that 20ml volume ratio is 1: 1,5h is stirred under the revolving speed of 3000r/min, obtains solution C, then solution C is put
Enter reaction kettle, reacted at 200 DEG C for 24 hours, is washed with deionized 3 times 3, drying for 24 hours, obtains substance D at 105 DEG C；By object
Matter D is added in deionized water, using the uniformly mixing of 750w ultrasound, obtains colloid E；Colloid E is sprayed on the stainless (steel) wire of roughening
Upper formation nano-titanium dioxide/molybdenum disulfide laminated film, wherein spray power is 10w, spray pressure 1.3kg/cm2, sky
Dry 30min, the process are repeated 4 times in gas, film thickness 500nm；Using silver nitrate solution as electrochemical deposition electrolyte, no
Rust steel mesh is cathode, and graphite is anode, and silver nano-grain is deposited on nano-titanium dioxide/molybdenum disulfide laminated film, electricity
Chemical deposition voltage is 12v.
Embodiment 5:
5ml titanium isopropoxide is measured, is diluted with the 2- propyl alcohol of 45ml, is obtained solution A, solution A is added dropwise to
In 26ml2- propyl alcohol and 26ml water mixed solution, 12h is placed, solution B is obtained；Solution B is mixed with the molybdenum disulfide of 10wt%
It is to stir 5h in 1: 1 2- aqueous propanol solution under the revolving speed of 3000r/min, obtain solution C in 20ml volume ratio, then by solution C
It is put into reaction kettle, is reacted at 200 DEG C for 24 hours, is washed with deionized 3 times 3, drying for 24 hours, obtains substance D at 105 DEG C；It will
Substance D is added in deionized water, using the uniformly mixing of 750w ultrasound, obtains colloid E；Colloid E is sprayed on the stainless steel of roughening
Online to form nano-titanium dioxide/molybdenum disulfide laminated film, wherein spray power is 100w, spray pressure 1.5kg/cm2,
Air drying 30min, the process are repeated 4 times, film thickness 500nm；Using silver nitrate solution as electrochemical deposition electrolyte,
Stainless (steel) wire is cathode, and graphite is anode, and silver nano-grain is deposited on nano-titanium dioxide/molybdenum disulfide laminated film,
Electrochemical deposition voltage is 12v.
The foregoing is merely a specific embodiment of the invention, are not intended to restrict the invention, all on basis of the invention
On, any modification, equivalent substitution, improvement and etc. done should all be included in the protection scope of the present invention.
Claims (5)
1. a kind of nano-titanium dioxide/molybdenum disulfide composite material film preparation method, it is characterised in that:
Step 1: diluting titanium isopropoxide with 2- propyl alcohol, solution A is obtained；
Step 2: solution A is added dropwise in 2- aqueous propanol solution, stands 10h-12h and obtain solution B；
Step 3: CTAB is dissolved in deionized water in stirring, CTAB solution is then added graphene oxide into while stirring
In, stirring for 24 hours, obtains solution C；
Step 4: sodium molybdate is added in solution C while stirring, thiocarbamide then is added after ultrasound 30min, ultrasound is until obtaining again
Obtain uniform solution D；
Step 5: deionized water is added into solution D obtains solution E, so that the concentration of CTAB is maintained at 0.02mol/ in E solution
L；
Solution F is obtained for 24 hours in 220 DEG C of reactions step 6: solution E is transferred in ptfe autoclave, certainly to reaction kettle
After being so cooled to room temperature, solution F is transferred in beaker；
Step 7: doing centrifuging treatment to solution F, black solid product G is obtained；
Step 8: first cleaning 3 black solid product G with deionized water, then with washes of absolute alcohol 3 times；
Step 9: the black solid product G after washes of absolute alcohol is put into 80 DEG C of dry 12h in vacuum oven；
Step 10: 800 DEG C of heat treatment 2h obtain spherical structure to the black solid product G after dry under argon atmosphere in tube furnace
Molybdenum disulfide；
Step 11: the molybdenum disulfide of solution B and spherical structure is blended in 2- aqueous propanol solution, 10h is quickly stirred, is obtained
Solution H；
Step 12: Solution H is put into ptfe autoclave, 25h is reacted at 150 DEG C -250 DEG C and obtains solution I, to poly-
After tetrafluoroethene reaction kettle naturally cools to room temperature, solution I is transferred in beaker；
Step 13: doing centrifuging treatment to solution I, substance J is obtained；
Step 14: after substance J is washed 3 times with deionized water, dry 20h at 100 DEG C -150 DEG C in a vacuum drying oven is put,
Obtain substance K；
Step 15: substance K is put into deionized water, doing ultrasonic treatment makes the two uniformly mixing, obtains colloid L；
Step 16: colloid K is sprayed on formation nano-titanium dioxide/molybdenum disulfide laminated film on the stainless (steel) wire of roughening,
Air drying 30min；
Step 17: repeating the 16th step, make nano-titanium dioxide/molybdenum disulfide laminated film with a thickness of 500-600nm；
Step 18: stainless (steel) wire is cathode using silver nitrate solution as electrochemical deposition electrolyte, graphite is anode, and silver is received
Rice grain is deposited on nano-titanium dioxide/molybdenum disulfide laminated film, obtains the nano-silica of silver nano-grain antipoints array
Change titanium/molybdenum disulfide composite material film.
2. a kind of preparation method of nano-titanium dioxide/molybdenum disulfide composite material film according to claim 1, special
Sign is: when the solution B is mixed with the molybdenum disulfide of spherical structure, the mass fraction of molybdenum disulfide is 2%-10%.
3. a kind of preparation method of nano-titanium dioxide/molybdenum disulfide composite material film according to claim 1, special
Sign is: the 2- aqueous propanol solution, and the volume ratio of the third alcohol and water of 2- is 2: 1-2: 3.
4. a kind of preparation method of nano-titanium dioxide/molybdenum disulfide composite material film according to claim 1, special
Sign is: spray power of the colloid E in spraying is 100W, spray pressure 0.3-1.8kg/cm2。
5. a kind of preparation method of nano-titanium dioxide/molybdenum disulfide composite material film according to claim 1, special
Sign is: the quick speed of agitator is 3000r/min-5000r/min.
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| CN107723777B (en) * | 2017-10-16 | 2019-04-16 | 南通纺织丝绸产业技术研究院 | The preparation method of the TiO 2 nanotubes modified array of electro-deposition molybdenum disulfide quantum dot |
| CN107803209A (en) * | 2017-10-20 | 2018-03-16 | 上海应用技术大学 | A kind of preparation method of individual layer molybdenum disulfide and nano titania hetero-junctions |
| CN107744818A (en) * | 2017-10-23 | 2018-03-02 | 南昌航空大学 | Molybdenum disulfide loads the preparation method of silver-colored photochemical catalyst |
| CN108579768B (en) * | 2018-01-12 | 2020-08-04 | 合肥师范学院 | Few-layer MoS2Modified Ag-TiO2Preparation method of nano composite film |
| CN108642541A (en) * | 2018-04-11 | 2018-10-12 | 哈尔滨工程大学 | The preparation method of titanium doped molybdenum disulfide film with ultraviolet absorption peak |
| CN109704406A (en) * | 2019-02-22 | 2019-05-03 | 西安工业大学 | A kind of preparation method of nano molybdenum disulfide |
| CN110404565A (en) * | 2019-08-28 | 2019-11-05 | 中国科学院上海硅酸盐研究所湖州先进材料产业创新中心 | A kind of titanium oxide/sulfur-rich vacancy molybdenum sulfide composite material and preparation method and application |
| CN115067358B (en) * | 2022-06-21 | 2024-03-19 | 重庆德强化工有限公司 | Ag/Zn ion loaded black titanium dioxide composite molybdenum disulfide nanosheet nanomaterial |
Citations (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN105195133A (en) * | 2015-09-18 | 2015-12-30 | 黑龙江大学 | Preparation method of molybdenum disulfide-black titanium dioxide composite visible-light-driven photocatalyst for hydrogen production |
| CN107297214A (en) * | 2017-07-06 | 2017-10-27 | 陕西科技大学 | A kind of preparation method of the titanium dioxide composite photocatalyst of molybdenum disulfide modification |
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Patent Citations (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN105195133A (en) * | 2015-09-18 | 2015-12-30 | 黑龙江大学 | Preparation method of molybdenum disulfide-black titanium dioxide composite visible-light-driven photocatalyst for hydrogen production |
| CN107297214A (en) * | 2017-07-06 | 2017-10-27 | 陕西科技大学 | A kind of preparation method of the titanium dioxide composite photocatalyst of molybdenum disulfide modification |
Non-Patent Citations (2)
| Title |
|---|
| Synergetic Effect of MoS2 and Graphene as Cocatalysts for Enhanced Photocatalytic H2 Production Activity of TiO2 Nanoparticles;Quanjun Xiang等;《JACS》;20120418;第134卷(第15期);第6575-6578页 |
| 基于水热法制备的TiO2 /MoS2复合光催化剂及其光催化制氢活性;齐中等;《环境化学》;20160515;第35卷(第5期);第1027-1034页 |
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