CN106391010B - A kind of Ag/BaTiO3Heterogeneous photocatalyst structure of nano-tube array and preparation method thereof - Google Patents
A kind of Ag/BaTiO3Heterogeneous photocatalyst structure of nano-tube array and preparation method thereof Download PDFInfo
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- CN106391010B CN106391010B CN201610847532.8A CN201610847532A CN106391010B CN 106391010 B CN106391010 B CN 106391010B CN 201610847532 A CN201610847532 A CN 201610847532A CN 106391010 B CN106391010 B CN 106391010B
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- 239000002071 nanotube Substances 0.000 title claims abstract description 33
- 238000002360 preparation method Methods 0.000 title claims abstract description 14
- 239000011941 photocatalyst Substances 0.000 title claims abstract description 13
- 229910002113 barium titanate Inorganic materials 0.000 claims abstract description 45
- PNEYBMLMFCGWSK-UHFFFAOYSA-N Alumina Chemical compound [O-2].[O-2].[O-2].[Al+3].[Al+3] PNEYBMLMFCGWSK-UHFFFAOYSA-N 0.000 claims abstract description 38
- SQGYOTSLMSWVJD-UHFFFAOYSA-N silver(1+) nitrate Chemical compound [Ag+].[O-]N(=O)=O SQGYOTSLMSWVJD-UHFFFAOYSA-N 0.000 claims abstract description 34
- JRPBQTZRNDNNOP-UHFFFAOYSA-N barium titanate Chemical compound [Ba+2].[Ba+2].[O-][Ti]([O-])([O-])[O-] JRPBQTZRNDNNOP-UHFFFAOYSA-N 0.000 claims abstract description 33
- 230000002146 bilateral effect Effects 0.000 claims abstract description 18
- 229910001961 silver nitrate Inorganic materials 0.000 claims abstract description 17
- 238000012512 characterization method Methods 0.000 claims abstract description 13
- 238000009415 formwork Methods 0.000 claims description 25
- IWOUKMZUPDVPGQ-UHFFFAOYSA-N barium nitrate Chemical compound [Ba+2].[O-][N+]([O-])=O.[O-][N+]([O-])=O IWOUKMZUPDVPGQ-UHFFFAOYSA-N 0.000 claims description 18
- HEMHJVSKTPXQMS-UHFFFAOYSA-M Sodium hydroxide Chemical compound [OH-].[Na+] HEMHJVSKTPXQMS-UHFFFAOYSA-M 0.000 claims description 15
- NBIIXXVUZAFLBC-UHFFFAOYSA-N Phosphoric acid Chemical compound OP(O)(O)=O NBIIXXVUZAFLBC-UHFFFAOYSA-N 0.000 claims description 12
- 239000000725 suspension Substances 0.000 claims description 10
- 238000013019 agitation Methods 0.000 claims description 9
- 239000004411 aluminium Substances 0.000 claims description 7
- 229910052782 aluminium Inorganic materials 0.000 claims description 7
- XAGFODPZIPBFFR-UHFFFAOYSA-N aluminium Chemical compound [Al] XAGFODPZIPBFFR-UHFFFAOYSA-N 0.000 claims description 7
- 238000006243 chemical reaction Methods 0.000 claims description 7
- 230000003647 oxidation Effects 0.000 claims description 7
- 238000007254 oxidation reaction Methods 0.000 claims description 7
- 229910000147 aluminium phosphate Inorganic materials 0.000 claims description 6
- 238000000137 annealing Methods 0.000 claims description 6
- 230000004888 barrier function Effects 0.000 claims description 6
- 238000001354 calcination Methods 0.000 claims description 6
- 238000000280 densification Methods 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
- 238000001704 evaporation Methods 0.000 claims description 5
- 239000000843 powder Substances 0.000 claims description 5
- 239000000376 reactant Substances 0.000 claims description 4
- 238000010792 warming Methods 0.000 claims description 4
- 229910000838 Al alloy Inorganic materials 0.000 claims description 2
- QVGXLLKOCUKJST-UHFFFAOYSA-N atomic oxygen Chemical compound [O] QVGXLLKOCUKJST-UHFFFAOYSA-N 0.000 claims description 2
- 239000007788 liquid Substances 0.000 claims description 2
- 229910052760 oxygen Inorganic materials 0.000 claims description 2
- 239000001301 oxygen Substances 0.000 claims description 2
- 238000009792 diffusion process Methods 0.000 abstract description 6
- 238000000034 method Methods 0.000 abstract description 6
- 239000000463 material Substances 0.000 abstract description 4
- 239000002800 charge carrier Substances 0.000 abstract description 2
- 230000000694 effects Effects 0.000 abstract description 2
- 238000007210 heterogeneous catalysis Methods 0.000 abstract description 2
- 239000002086 nanomaterial Substances 0.000 abstract description 2
- 239000003381 stabilizer Substances 0.000 abstract description 2
- FOIXSVOLVBLSDH-UHFFFAOYSA-N Silver ion Chemical compound [Ag+] FOIXSVOLVBLSDH-UHFFFAOYSA-N 0.000 abstract 1
- 238000005215 recombination Methods 0.000 abstract 1
- 239000002904 solvent Substances 0.000 abstract 1
- 239000000047 product Substances 0.000 description 7
- 238000007146 photocatalysis Methods 0.000 description 6
- 230000001699 photocatalysis Effects 0.000 description 6
- 238000010438 heat treatment Methods 0.000 description 4
- 229910052788 barium Inorganic materials 0.000 description 2
- 150000001875 compounds Chemical class 0.000 description 2
- 230000009977 dual effect Effects 0.000 description 2
- 238000005516 engineering process Methods 0.000 description 2
- 150000002500 ions Chemical class 0.000 description 2
- 230000035484 reaction time Effects 0.000 description 2
- GRYLNZFGIOXLOG-UHFFFAOYSA-N Nitric acid Chemical compound O[N+]([O-])=O GRYLNZFGIOXLOG-UHFFFAOYSA-N 0.000 description 1
- 240000007594 Oryza sativa Species 0.000 description 1
- 235000007164 Oryza sativa Nutrition 0.000 description 1
- 239000012736 aqueous medium Substances 0.000 description 1
- DSAJWYNOEDNPEQ-UHFFFAOYSA-N barium atom Chemical compound [Ba] DSAJWYNOEDNPEQ-UHFFFAOYSA-N 0.000 description 1
- 229910001422 barium ion Inorganic materials 0.000 description 1
- 239000003990 capacitor Substances 0.000 description 1
- 239000003054 catalyst Substances 0.000 description 1
- 230000003197 catalytic effect Effects 0.000 description 1
- 150000001768 cations Chemical class 0.000 description 1
- 230000000052 comparative effect Effects 0.000 description 1
- 230000007812 deficiency Effects 0.000 description 1
- 230000005611 electricity Effects 0.000 description 1
- 238000002474 experimental method Methods 0.000 description 1
- 239000012467 final product Substances 0.000 description 1
- 230000007774 longterm Effects 0.000 description 1
- 229910044991 metal oxide Inorganic materials 0.000 description 1
- 150000004706 metal oxides Chemical class 0.000 description 1
- 229910017604 nitric acid Inorganic materials 0.000 description 1
- 230000001737 promoting effect Effects 0.000 description 1
- 230000005855 radiation Effects 0.000 description 1
- 235000009566 rice Nutrition 0.000 description 1
- 230000000630 rising effect Effects 0.000 description 1
- 238000000926 separation method Methods 0.000 description 1
- 238000001228 spectrum Methods 0.000 description 1
- 238000003756 stirring Methods 0.000 description 1
- 230000002463 transducing effect Effects 0.000 description 1
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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
- B01J23/00—Catalysts comprising metals or metal oxides or hydroxides, not provided for in group B01J21/00
- B01J23/38—Catalysts comprising metals or metal oxides or hydroxides, not provided for in group B01J21/00 of noble metals
- B01J23/54—Catalysts comprising metals or metal oxides or hydroxides, not provided for in group B01J21/00 of noble metals combined with metals, oxides or hydroxides provided for in groups B01J23/02 - B01J23/36
- B01J23/66—Silver or gold
-
- 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
- B01J35/39—Photocatalytic properties
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- Chemical & Material Sciences (AREA)
- Engineering & Computer Science (AREA)
- Materials Engineering (AREA)
- Organic Chemistry (AREA)
- Chemical Kinetics & Catalysis (AREA)
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Abstract
The invention discloses a kind of Ag/BaTiO3Heterogeneous photocatalyst structure of nano-tube array and preparation method thereof.It is template that this method, which is using bilateral porous anodic aluminium oxide, using silver nitrate as Ti (OC4H9)4Stabilizer, prepare Characterization of Barium Titanate Nanotubes array；Use solvent evaporated method in Characterization of Barium Titanate Nanotubes array surface silver nanoparticles loaded again.The present invention utilizes the nano-tube array structure of barium titanate, electric charge carrier diffusion path is set to be elongated, reduce light induced electron and hole-recombination, while using unique surface plasma resonance effect and good electric conductivity possessed by Ag nano materials, building Ag/BaTiO3The heterogeneous catalysis material of nano-tube array, improves the separative efficiency of photo-generate electron-hole.
Description
Technical field
The present invention relates to a kind of Ag/BaTiO3Heterogeneous photocatalyst structure of nano-tube array and preparation method thereof, belongs to nanometer
Technical field of material and photocatalysis technology field.
Background technology
Barium titanate is a kind of typical Ferroelectrics, for many years BaTiO3Application study focus primarily upon transducing
The fields such as device, sensing element and capacitor.Predominantly nanocrystalline to the preparation of nm-class barium titanate material, in addition also barium titanate is received
Rice stick, film etc..In recent years, it has been found that BaTiO3As perofskite type oxide and a kind of photochemical catalyst, in ultraviolet light
Or light induced electron and photohole can be equally generated under radiation of visible light, this makes it before photocatalysis field has a wide range of applications
Scape, barium titanate propose its pattern new requirement in the application of photocatalysis field.Nano-tube array structure can be such that charge carries
It flows sub- diffusion path to be elongated, overcomes conventional metal oxides light induced electron and hole and compound disadvantage easily occurs.Anodic oxygen
It is to prepare the common method of nano-tube array, but this method is acted on by the confinement of template to change aluminum alloy pattern plate method, and ion is in mould
Diffusion rate is slow in board channel, and path length, the reaction time is long, and the reaction time is long to be easy to cause template deformation, fracture, reactant
It hydrolyzes.
Invention content
The purpose of the invention is to overcome the deficiencies in the prior art, propose a kind of Ag/BaTiO3Nano-tube array is heterogeneous
Photocatalyst structure and preparation method thereof, to promoting barium titanate to be of great significance in the application of photocatalysis field.
Technical solution is used by realizing the object of the invention：A kind of Ag/BaTiO3The heterogeneous light of nano-tube array is urged
Change structure and preparation method thereof, step is：
Anodic oxidation aluminium formwork 5wt% phosphoric acid dips are removed the alumina barrier layer of bottom densification, obtain bilateral by a
Porous alumina formwork；Bilateral porous alumina formwork is inserted vertically into reactor center and is fixed, makes template that will react
Device is isolated into equal two parts and forms two-way reaction device, ensures the reactant of both sides only by bilateral porous alumina formwork phase
Counterdiffusion；Ti (OC are added in the side of two-compartment reactor4H9)4And silver nitrate solution；Two-compartment reactor the other side be added with
Ti(OC4H9)4Isoconcentration, isometric barium nitrate solution, the pH value of both sides solution are all controlled in 4-6；4-10 is stood in air
Hour；Template is taken out, it is surface wipes are clean and dried under infrared lamp, then with 5 DEG C of heatings per minute in Muffle furnace
Rate is warming up to 750 DEG C and keeps the temperature 1 hour, is made annealing treatment.Anode extra in product is removed with the NaOH solution of 2mol/L
Characterization of Barium Titanate Nanotubes array is obtained after alumina formwork (AAO templates)；
Characterization of Barium Titanate Nanotubes array powder prepared by step a is dissolved in deionized water by b, and ultrasonic agitation 30min forms concentration
For the barium titanate suspension of 0.5g/L-2g/L；
C mixes barium titanate suspension with silver nitrate solution, and ultrasonic agitation is heated to moisture evaporating completely after 1 hour, and
Calcining obtains Ag/BaTiO at 450 DEG C3The heterogeneous photocatalyst structure of nano-tube array.
Wherein, the aperture of the anodic oxidation aluminium formwork described in step a is 50-200nm, the Ti (OC4H9)4And nitric acid
A concentration of 0.01M of barium solution, silver nitrate solution and Ti (OC4H9)4The molar ratio of solution is 1:10；
The molar ratio of silver nitrate and barium titanate described in step c is (0.1-1)：100.
The present invention has the following advantages that compared with prior art：The present invention using the ordered porous alumina of bilateral as template,
Bilateral porous alumina formwork is inserted vertically into reactor center and is fixed, makes template that reactor is isolated into equal two
Divide and form two-way reaction device, ensures the reactant of both sides only by bilateral porous alumina formwork phase counterdiffusion；It is reacted in dual chamber
Device both sides each lead into Ti (OC4H9)4And barium nitrate, mutual expansion of the ion in template duct is realized in a relatively short period of time
It dissipates, it is therefore prevented that alumina formwork is caved in, is broken.Using silver nitrate as stabilizer, Ti (OC are added4H9)4Solution, delay gelating
Time obtains colloidal sol steady in a long-term, it is ensured that reaction terminates preceding Ti (OC4H9)4Exist in the form of colloidal sol, does not flocculate, not water
Solution.
In addition, the present invention considers Ti (OC4H9)4Hold with the difference of viscosity and diffusion rate of the barium nitrate in aqueous medium
Easily make product nonstoichiometry ratio, use concentration offsets method for the first time, Ti (OC are being added4H9)4While be added silver nitrate it is molten
Liquid, control final product realize ideal stoichiometric ratio, it is equal in duct in same time to realize a variety of cations
Even diffusion, to ensure that microstructure, electric property and the photocatalysis characteristic of product.
Characterization of Barium Titanate Nanotubes array structure prepared by the present invention can elongate the diffusion path of electric charge carrier, reduce photoproduction
Electrons and holes are compound；Simultaneously present invention utilizes unique surface plasma resonance effect possessed by Ag nano materials and
Good electric conductivity builds Ag/BaTiO3The heterogeneous catalysis material of nano-tube array, improves the separation of photo-generate electron-hole
Efficiency.
Specific implementation mode
The present invention is described in further detail with reference to embodiment：
Embodiment 1：
By the anodic oxidation aluminium formwork 5wt% phosphoric acid dips that aperture is 50nm, the aluminium oxide barrier of bottom densification is removed
Layer, obtains the porous alumina formwork of bilateral；Bilateral porous alumina formwork is inserted vertically into reactor center and is fixed, is made
Reactor is isolated into equal two parts and forms two-way reaction device by template；The Ti of 0.01M is added in the side of two-compartment reactor
(OC4H9)4With the silver nitrate solution of 0.001M；0.01M and Ti (OC are added in the other side of two-compartment reactor4H9)4Isometric
The pH value of barium nitrate solution, both sides solution is all controlled in 4-6；Stand 4-10 hours in air；Template is taken out, by surface wipes
It dries totally and under infrared lamp, then rising to 750 DEG C of temperature in Muffle furnace with 5 DEG C of heating rates per minute keeps the temperature 1 hour,
It is made annealing treatment.Characterization of Barium Titanate Nanotubes array is obtained after removing AAO templates extra in product with the NaOH solution of 2mol/L；Institute
The Characterization of Barium Titanate Nanotubes array powder of preparation is dissolved in deionized water, and ultrasonic agitation 30min forms the barium titanate of a concentration of 1.0g/L
Suspension；According to Ag and BaTiO3Molar ratio be 0.1:100 ratio mixes barium titanate suspension with silver nitrate solution,
Ultrasonic agitation is heated to moisture evaporating completely after 1 hour, and calcining obtains Ag/BaTiO at 450 DEG C3Nano-tube array is heterogeneous
Photocatalyst structure.
Embodiment 2：
By the anodic oxidation aluminium formwork 5wt% phosphoric acid dips that aperture is 50nm, the aluminium oxide barrier of bottom densification is removed
Layer, obtains the porous alumina formwork of bilateral；Bilateral porous alumina formwork is inserted vertically into reactor center and is fixed, is made
Reactor is isolated into equal two parts and forms two-way reaction device by template；The Ti of 0.01M is added in the side of two-compartment reactor
(OC4H9)4With the silver nitrate solution of 0.001M；0.01M and Ti (OC are added in the other side of two-compartment reactor4H9)4Isometric
The pH value of barium nitrate solution, both sides solution is all controlled in 4-6；Stand 4-10 hours in air；Template is taken out, by surface wipes
It dries totally and under infrared lamp, being then warming up to 750 DEG C in Muffle furnace with 5 DEG C of heating rates per minute keeps the temperature 1 hour,
It is made annealing treatment.Characterization of Barium Titanate Nanotubes array is obtained after removing AAO templates extra in product with the NaOH solution of 2mol/L；Institute
The Characterization of Barium Titanate Nanotubes array powder of preparation is dissolved in deionized water, and ultrasonic agitation 30min forms the barium titanate of a concentration of 1.0g/L
Suspension；According to Ag and BaTiO3Molar ratio be 0.5:100 ratio mixes barium titanate suspension with silver nitrate solution,
Ultrasonic agitation is heated to moisture evaporating completely after 1 hour, and calcining obtains Ag/BaTiO at 450 DEG C3Nano-tube array is heterogeneous
Photocatalyst structure.
Embodiment 3：
By the anodic oxidation aluminium formwork 5wt% phosphoric acid dips that aperture is 50nm, the aluminium oxide barrier of bottom densification is removed
Layer, obtains the porous alumina formwork of bilateral；Bilateral porous alumina formwork is inserted vertically into reactor center and is fixed, is made
Reactor is isolated into equal two parts and forms two-way reaction device by template；The Ti of 0.01M is added in the side of two-compartment reactor
(OC4H9)4With the silver nitrate solution of 0.001M；0.01M and Ti (OC are added in the other side of two-compartment reactor4H9)4Isometric
The pH value of barium nitrate solution, both sides solution is all controlled in 4-6；Stand 4-10 hours in air；Template is taken out, by surface wipes
It dries totally and under infrared lamp, being then warming up to 750 DEG C in Muffle furnace with 5 DEG C of heating rates per minute keeps the temperature 1 hour,
It is made annealing treatment.Characterization of Barium Titanate Nanotubes array is obtained after removing AAO templates extra in product with the NaOH solution of 2mol/L；Institute
The Characterization of Barium Titanate Nanotubes array powder of preparation is dissolved in deionized water, and ultrasonic agitation 30min forms the barium titanate of a concentration of 1.0g/L
Suspension；According to Ag and BaTiO3Molar ratio be 1:100 ratio mixes barium titanate suspension with silver nitrate solution, surpasses
Sound is heated to moisture evaporating completely after stirring 1 hour, and calcining obtains Ag/BaTiO at 450 DEG C3The heterogeneous light of nano-tube array
Catalytic structure.
Comparative example 1：
By the anodic oxidation aluminium formwork 5wt% phosphoric acid dips that aperture is 50nm, the aluminium oxide barrier of bottom densification is removed
Layer, obtains the porous alumina formwork of bilateral；And bilateral porous alumina formwork is packed among reactor, it is fixed, it will react
Device is isolated into two parts and forms two-compartment reactor；Ti (the OC of 0.01M are added in the side of two-compartment reactor4H9)4；It is anti-in dual chamber
Answer the other side of device that 0.01M and Ti (OC are added4H9)4The pH value of isometric barium nitrate solution, both sides solution is all controlled in 4-6；
Stand 4-10 hours in air.Ti (OC are found after standing 8 hours4H9)4There is flocculent deposit, remaining experimental procedure is the same as real
Apply example 1.The Ag/BaTiO that will be obtained after calcining3The heterogeneous photocatalyst structure of nano-tube array uses discharge plasma atom spectrum
(ICP) atomic ratio is measured, it is found that Ba, Ti molar ratio are more than 1, declaratives Ti4+It is hydrolyzed, not completely and barium ions
React, barium titanate made to deviate from stoichiometric ratio, barium titanate nonstoichiometry than will be to product microstructure, electricity
It learns performance and photocatalysis characteristic generates important influence.
Claims (3)
1. a kind of Ag/BaTiO3The preparation method of the heterogeneous photocatalyst structure of nano-tube array, it is characterised in that：The preparation method
Include the following steps：
The anodic oxidation aluminium formwork in the apertures 50-200nm 5wt% phosphoric acid dips are removed the aluminium oxide barrier of bottom densification by a
Layer, obtains the porous alumina formwork of bilateral；Bilateral porous alumina formwork is inserted vertically into reactor center and is fixed, is made
Reactor is isolated into equal two parts and forms two-way reaction device by template, ensures the reactant of both sides only by the porous oxygen of bilateral
Change aluminum alloy pattern plate phase counterdiffusion；Silver nitrate solution and Ti (OC is added in the side of two-compartment reactor4H9)4Solution；In two-compartment reactor
The other side be added with Ti (OC4H9)4Isoconcentration, isometric barium nitrate solution, the pH value of both sides solution are all controlled in 4-6；
It is stood in air；It takes out surface wipes are clean after template and is dried under infrared lamp, then made annealing treatment；Use 2mol/L
NaOH solution remove in product after extra alumina formwork to obtain Characterization of Barium Titanate Nanotubes array；Wherein, the silver nitrate is molten
Liquid and Ti (OC4H9)4The molar ratio of solution is 1:10, Ti (OC4H9)4With a concentration of 0.01M of barium nitrate solution；
Characterization of Barium Titanate Nanotubes array powder prepared by step a is dissolved in deionized water by b, and ultrasonic agitation 30min forms a concentration of
The barium titanate suspension of 0.5g/L-2g/L；
C mixes barium titanate suspension with silver nitrate solution, and ultrasonic agitation is heated to moisture evaporating completely after 1 hour, and 450
Calcining obtains Ag/BaTiO at DEG C3The heterogeneous photocatalyst structure of nano-tube array.
2. Ag/BaTiO as described in claim 13The preparation method of the heterogeneous photocatalyst structure of nano-tube array, it is characterised in that：
Time of repose is in air described in step a：4-10 hours, annealing condition was：With 5 DEG C of liters per minute in Muffle furnace
Warm rate is warming up to 750 DEG C and keeps the temperature 1 hour.
3. Ag/BaTiO as described in claim 13The preparation method of the heterogeneous photocatalyst structure of nano-tube array, it is characterised in that：
The molar ratio of silver nitrate and barium titanate described in step c is (0.1-1):100.
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| CN1690257A (en) * | 2004-04-30 | 2005-11-02 | 中国科学技术大学 | La1-XPbXMnO3 compound ordered nano-line array and method for preparing same |
| CN101279767A (en) * | 2008-04-28 | 2008-10-08 | 哈尔滨工业大学 | Preparation of lanthanide series rare-earth doped bismuth titanate nano-tube |
| CN102251232A (en) * | 2011-07-18 | 2011-11-23 | 同济大学 | Method for preparing silver nanowire array in ordered porous alumina template |
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| CN1690257A (en) * | 2004-04-30 | 2005-11-02 | 中国科学技术大学 | La1-XPbXMnO3 compound ordered nano-line array and method for preparing same |
| CN101279767A (en) * | 2008-04-28 | 2008-10-08 | 哈尔滨工业大学 | Preparation of lanthanide series rare-earth doped bismuth titanate nano-tube |
| CN102251232A (en) * | 2011-07-18 | 2011-11-23 | 同济大学 | Method for preparing silver nanowire array in ordered porous alumina template |
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