CN106390975A - Method for preparing barium titanate nanotube array - Google Patents
Method for preparing barium titanate nanotube array Download PDFInfo
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- CN106390975A CN106390975A CN201610847553.XA CN201610847553A CN106390975A CN 106390975 A CN106390975 A CN 106390975A CN 201610847553 A CN201610847553 A CN 201610847553A CN 106390975 A CN106390975 A CN 106390975A
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- CN
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- Prior art keywords
- barium titanate
- solution
- reactor
- characterization
- preparation
- Prior art date
- Legal status (The legal status is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the status listed.)
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- 239000002071 nanotube Substances 0.000 title claims abstract description 19
- 229910002113 barium titanate Inorganic materials 0.000 title claims abstract description 18
- JRPBQTZRNDNNOP-UHFFFAOYSA-N barium titanate Chemical compound [Ba+2].[Ba+2].[O-][Ti]([O-])([O-])[O-] JRPBQTZRNDNNOP-UHFFFAOYSA-N 0.000 title claims abstract description 17
- 238000000034 method Methods 0.000 title abstract description 8
- SQGYOTSLMSWVJD-UHFFFAOYSA-N silver(1+) nitrate Chemical compound [Ag+].[O-]N(=O)=O SQGYOTSLMSWVJD-UHFFFAOYSA-N 0.000 claims abstract description 20
- 229910052782 aluminium Inorganic materials 0.000 claims abstract description 15
- XAGFODPZIPBFFR-UHFFFAOYSA-N aluminium Chemical compound [Al] XAGFODPZIPBFFR-UHFFFAOYSA-N 0.000 claims abstract description 15
- 229910001961 silver nitrate Inorganic materials 0.000 claims abstract description 10
- 238000006243 chemical reaction Methods 0.000 claims abstract description 9
- IWOUKMZUPDVPGQ-UHFFFAOYSA-N barium nitrate Chemical compound [Ba+2].[O-][N+]([O-])=O.[O-][N+]([O-])=O IWOUKMZUPDVPGQ-UHFFFAOYSA-N 0.000 claims description 22
- 238000009415 formwork Methods 0.000 claims description 19
- HEMHJVSKTPXQMS-UHFFFAOYSA-M Sodium hydroxide Chemical compound [OH-].[Na+] HEMHJVSKTPXQMS-UHFFFAOYSA-M 0.000 claims description 18
- 230000002146 bilateral effect Effects 0.000 claims description 15
- PNEYBMLMFCGWSK-UHFFFAOYSA-N aluminium oxide Inorganic materials [O-2].[O-2].[O-2].[Al+3].[Al+3] PNEYBMLMFCGWSK-UHFFFAOYSA-N 0.000 claims description 13
- 230000003647 oxidation Effects 0.000 claims description 13
- 238000007254 oxidation reaction Methods 0.000 claims description 13
- NBIIXXVUZAFLBC-UHFFFAOYSA-N Phosphoric acid Chemical compound OP(O)(O)=O NBIIXXVUZAFLBC-UHFFFAOYSA-N 0.000 claims description 12
- 238000012512 characterization method Methods 0.000 claims description 12
- 238000002360 preparation method Methods 0.000 claims description 12
- 239000004411 aluminium Substances 0.000 claims description 10
- 229910000147 aluminium phosphate Inorganic materials 0.000 claims description 6
- 238000010438 heat treatment Methods 0.000 claims description 5
- 238000009413 insulation Methods 0.000 claims description 5
- 238000000137 annealing Methods 0.000 claims description 4
- 230000004888 barrier function Effects 0.000 claims description 2
- 239000000376 reactant Substances 0.000 claims description 2
- TWNQGVIAIRXVLR-UHFFFAOYSA-N oxo(oxoalumanyloxy)alumane Chemical compound O=[Al]O[Al]=O TWNQGVIAIRXVLR-UHFFFAOYSA-N 0.000 claims 1
- 238000009792 diffusion process Methods 0.000 abstract description 4
- 150000001768 cations Chemical class 0.000 abstract description 2
- 230000007774 longterm Effects 0.000 abstract description 2
- 239000003381 stabilizer Substances 0.000 abstract description 2
- 125000002091 cationic group Chemical group 0.000 abstract 1
- 238000001879 gelation Methods 0.000 abstract 1
- 230000002035 prolonged effect Effects 0.000 abstract 1
- 239000002689 soil Substances 0.000 abstract 1
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 abstract 1
- VKJLWXGJGDEGSO-UHFFFAOYSA-N barium(2+);oxygen(2-);titanium(4+) Chemical compound [O-2].[O-2].[O-2].[Ti+4].[Ba+2] VKJLWXGJGDEGSO-UHFFFAOYSA-N 0.000 description 8
- 239000000047 product Substances 0.000 description 8
- 238000001035 drying Methods 0.000 description 5
- 238000007146 photocatalysis Methods 0.000 description 5
- 230000001699 photocatalysis Effects 0.000 description 5
- 238000007598 dipping method Methods 0.000 description 4
- 230000009977 dual effect Effects 0.000 description 4
- 241001621399 Lampris Species 0.000 description 3
- RTAQQCXQSZGOHL-UHFFFAOYSA-N Titanium Chemical compound [Ti] RTAQQCXQSZGOHL-UHFFFAOYSA-N 0.000 description 2
- 150000002500 ions Chemical class 0.000 description 2
- 239000000463 material Substances 0.000 description 2
- 230000004044 response Effects 0.000 description 2
- 229910000838 Al alloy Inorganic materials 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
- QVGXLLKOCUKJST-UHFFFAOYSA-N atomic oxygen Chemical compound [O] QVGXLLKOCUKJST-UHFFFAOYSA-N 0.000 description 1
- 229910052788 barium Inorganic materials 0.000 description 1
- 229910001422 barium ion Inorganic materials 0.000 description 1
- 230000008901 benefit Effects 0.000 description 1
- 239000003990 capacitor Substances 0.000 description 1
- 238000006555 catalytic reaction Methods 0.000 description 1
- 235000019994 cava Nutrition 0.000 description 1
- 230000008859 change Effects 0.000 description 1
- 230000000052 comparative effect Effects 0.000 description 1
- 150000001875 compounds Chemical class 0.000 description 1
- 230000007812 deficiency Effects 0.000 description 1
- 238000005516 engineering process Methods 0.000 description 1
- 239000012467 final product Substances 0.000 description 1
- 239000003292 glue Substances 0.000 description 1
- 230000007062 hydrolysis Effects 0.000 description 1
- 238000006460 hydrolysis reaction Methods 0.000 description 1
- 239000007788 liquid Substances 0.000 description 1
- 229910044991 metal oxide Inorganic materials 0.000 description 1
- 150000004706 metal oxides Chemical class 0.000 description 1
- 229910052760 oxygen Inorganic materials 0.000 description 1
- 239000001301 oxygen Substances 0.000 description 1
- 239000011941 photocatalyst Substances 0.000 description 1
- 230000005855 radiation Effects 0.000 description 1
- 235000009566 rice Nutrition 0.000 description 1
- 238000001228 spectrum Methods 0.000 description 1
- 239000010409 thin film Substances 0.000 description 1
- 230000002463 transducing effect Effects 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
- B01J23/00—Catalysts comprising metals or metal oxides or hydroxides, not provided for in group B01J21/00
- B01J23/02—Catalysts comprising metals or metal oxides or hydroxides, not provided for in group B01J21/00 of the alkali- or alkaline earth metals or beryllium
-
- B01J35/39—
Abstract
The invention discloses a method for preparing a barium titanate nanotube array. According to the method, the barium titanate nanotube array is prepared through a two-way porous anodised aluminum template in a double-chamber reactor. Through use of silver nitrate as a Ti(OC4H9)4 stabilizer in the reaction process, gelation time is prolonged and soil with long-term stability is obtained. According to a diffusion coefficient and viscosity difference of cations in a water solution, a cationic ratio is adjusted and the barium titanate nanotube array structure with an ideal stoichiometric ratio is obtained.
Description
Technical field
The present invention relates to a kind of preparation method of Characterization of Barium Titanate Nanotubes array, belong to technical field of nanometer material preparation and light
Catalysis technical field.
Background technology
Barium metatitanate. is a kind of typical Ferroelectrics, BaTiO for many years3Applied research focus primarily upon transducing
The fields such as device, sensing element and capacitor.Preparation to nm-class barium titanate material is predominantly nanocrystalline, and in addition also Barium metatitanate. is received
Rice rod, thin film etc..In recent years it has been found that BaTiO3It is also a class photocatalyst as perofskite type oxide, in ultraviolet light
Or equally can produce light induced electron and photohole under radiation of visible light, this makes it before photocatalysis field has a wide range of applications
Scape, Barium metatitanate. proposes new requirement in the application of photocatalysis field to its pattern.Nano-tube array structure can make electric charge carry
Flow sub- the evolving path to be elongated, overcome conventional metal oxides light induced electron and hole easily occurs compound shortcoming.Anodic oxygen
Changing aluminum alloy pattern plate method is to prepare the common method of nano-tube array, but this method is subject to the confinement of template to act on, and ion is in mould
Board channel internal diffusion speed is slow, path length, and the response time is long, and the response time is long to be easily caused template deformation, fracture, reactant
Hydrolyze.
Content of the invention
The invention aims to overcoming the deficiencies in the prior art, a kind of preparation side of Characterization of Barium Titanate Nanotubes array is proposed
Method, makes Barium metatitanate. have a wide range of applications in photocatalysis field.
Realizing the technical solution that the object of the invention adopted is：A kind of preparation method of Characterization of Barium Titanate Nanotubes array,
Its preparation process is：
A, by anodic oxidation aluminium formwork 5wt% phosphoric acid dip, removes the fine and close alumina barrier layer in bottom, obtains bilateral
Porous alumina formwork；And bilateral porous alumina formwork is loaded in the middle of reactor, and fixing, reactor is isolated into two
Divide and form two-compartment reactor；Add Ti (OC in the side of two-compartment reactor according to certain mol ratio4H9)4And silver nitrate solution；
Add finite concentration, isopyknic barium nitrate solution in the opposite side of two-compartment reactor, the pH value of both sides solution all controls in 4-
6；Stand 4-10 hour, Ti (OC in atmosphere4H9)4With barium nitrate phase counterdiffusion in two lateral pattern hole roads respectively, change
Learn reaction and generate Barium metatitanate.；
B takes out template, by clean for surface wipes and drying under infrared lamp, with 5 DEG C of intensifications per minute in Muffle furnace
Speed rises to 750 DEG C and is incubated 1 hour.Remove unnecessary anodic oxidation aluminium formwork (AAO mould in product with the NaOH solution of 2mol/L
Plate) after Characterization of Barium Titanate Nanotubes array；
Wherein, the aperture of the anodic oxidation aluminium formwork described in step a is 50-200nm；The concentration of described barium nitrate solution
For 0.01M, Ti (OC4H9)4The concentration of solution is 0.012M-0.016M；The concentration of described silver nitrate solution and Ti (OC4H9)4
The concentration ratio of solution is 1:10.
The present invention compared with prior art has the advantage that：The present invention with the ordered porous alumina of bilateral as template,
Bilateral porous alumina formwork is inserted vertically into reactor central authorities and fixes, make template that reactor is isolated into equal two
Divide and form two-way reaction device, each lead into Ti (OC in two-compartment reactor both sides4H9)4And barium nitrate, realize in the short period of time
Phase counterdiffusion in template duct for the ion is it is therefore prevented that alumina formwork caves in, ruptures.Using silver nitrate as stabilizer, plus
Enter Ti (OC4H9)4Solution, the delay gelating time, obtains colloidal sol steady in a long-term it is ensured that reaction terminates front Ti (OC4H9)4With molten
Presented in glue, do not flocculate, do not hydrolyze.
In addition, the present invention considers Ti (OC4H9)4Hold with the difference of viscosity in aqueous medium for the barium nitrate and diffusion rate
Easily make product nonstoichiometry ratio, adopt concentration offsets method first, add Ti (OC4H9)4While add silver nitrate molten
Liquid, controls final product to realize preferable stoichiometric proportion it is achieved that multiple cation is equal in duct in same time
Even diffusion, thus ensure that the microstructure of product, electric property and photocatalysis characteristic.
Specific embodiment
With reference to embodiment, further illustrate the present invention.
Embodiment 1：
By the aperture 5wt% phosphoric acid dip of the anodic oxidation aluminium formwork for 100nm, obtain the porous oxidation aluminum dipping form of bilateral
Plate；And bilateral porous alumina formwork is loaded in the middle of reactor, and fixing, reactor is isolated into two parts and forms dual chamber reaction
Device.Add the barium nitrate solution of 0.01M in the side of two-compartment reactor；Add the Ti of 0.012M in the opposite side of two-compartment reactor
(OC4H9)4With 1.2 × 10-3The silver nitrate solution of M；The pH value of both sides solution all controls in 4-6；Stand 6 hours in atmosphere；Take
Go out template, clean for surface wipes and drying under infrared lamp rises to 750 with 5 DEG C of heating rates per minute in Muffle furnace
DEG C insulation 1 hour；Removed with the NaOH solution of 2mol/L and after unnecessary AAO template in product, obtain Characterization of Barium Titanate Nanotubes array.
Embodiment 2：
By the aperture 5wt% phosphoric acid dip of the anodic oxidation aluminium formwork for 100nm, obtain the porous oxidation aluminum dipping form of bilateral
Plate；And bilateral porous alumina formwork is loaded in the middle of reactor, and fixing, reactor is isolated into two parts and forms dual chamber reaction
Device.Add the barium nitrate solution of 0.01M in the side of two-compartment reactor；Add the Ti of 0.014M in the opposite side of two-compartment reactor
(OC4H9)4With 1.4 × 10-3The silver nitrate solution of M；The pH value of both sides solution all controls in 4-6；Stand 6 hours in atmosphere；Take
Go out template, clean for surface wipes and drying under infrared lamp rises to 750 with 5 DEG C of heating rates per minute in Muffle furnace
DEG C insulation is made annealing treatment for 1 hour.Received with obtaining Barium metatitanate. after unnecessary AAO template in the NaOH solution removing product of 2mol/L
Mitron array.
Embodiment 3：
By the aperture 5wt% phosphoric acid dip of the anodic oxidation aluminium formwork for 100nm, obtain the porous oxidation aluminum dipping form of bilateral
Plate；And bilateral porous alumina formwork is loaded in the middle of reactor, and fixing, reactor is isolated into two parts and forms dual chamber reaction
Device.Add the barium nitrate solution of 0.01M in the side of two-compartment reactor；Add the Ti of 0.016M in the opposite side of two-compartment reactor
(OC4H9)4With 1.6 × 10-3The silver nitrate solution of M；The pH value of both sides solution all controls in 4-6；Stand 6 hours in atmosphere；Take
Go out template, clean for surface wipes and drying under infrared lamp rises to 750 with 5 DEG C of heating rates per minute in Muffle furnace
DEG C insulation is made annealing treatment for 1 hour.Received with obtaining titanate after unnecessary AAO template in the NaOH solution removing product of 2mol/L
Mitron array.
Comparative example 1：
By the aperture 5wt% phosphoric acid dip of the anodic oxidation aluminium formwork for 100nm, obtain the porous oxidation aluminum dipping form of bilateral
Plate；And bilateral porous alumina formwork is loaded in the middle of reactor, and fixing, reactor is isolated into two parts and forms dual chamber reaction
Device.Add the barium nitrate solution of 0.01M in the side of two-compartment reactor；Add the Ti of 0.016M in the opposite side of two-compartment reactor
(OC4H9)4Solution；The pH value of both sides solution all controls in 4-6；Stand 6 hours in atmosphere；Standing finds Ti after 6 hours
(OC4H9)4Flocculent deposit occurs, takes out template, by clean for surface wipes and drying under infrared lamp, with 5 DEG C in Muffle furnace
Heating rate per minute rises to 750 DEG C of insulations and is made annealing treatment for 1 hour.Removed many in product with the NaOH solution of 2mol/L
Titanate nanotube array is obtained after remaining AAO template.The Characterization of Barium Titanate Nanotubes obtaining array is adopted discharge plasma atom
Spectrum (ICP) measures atomic ratio, finds that Ba, Ti mol ratio is more than 1, declaratives Ti4+There occurs hydrolysis, incomplete and barium
Ion reacts, and makes Barium metatitanate. deviate from stoichiometric proportion, and Barium metatitanate. nonstoichiometry ratio will be tied to the microcosmic of product
Structure, electric property and photocatalysis characteristic produce important impact.
Claims (4)
1. a kind of preparation method of Characterization of Barium Titanate Nanotubes array it is characterised in that：Described preparation method comprises the steps：
A, by anodic oxidation aluminium formwork 5wt% phosphoric acid dip, removes the fine and close alumina barrier layer in bottom, obtains the many of bilateral
Porous aluminum oxide template；Bilateral porous alumina formwork is inserted vertically into reactor central authorities fixing, make template by reactor every
Form two-way reaction device from becoming equal two parts it is ensured that the reactant of both sides is only mutually expanded by bilateral porous alumina formwork
Dissipate；Add silver nitrate and Ti (OC in the side of two-compartment reactor4H9)4Solution；Add and Ti in the opposite side of two-compartment reactor
(OC4H9)4Isopyknic barium nitrate solution, the pH value of both sides solution all controls in 4-6；Stand in atmosphere, take out template, will
Surface wipes are clean and dry under infrared lamp, remove unnecessary anodic oxidation aluminium formwork in product with the NaOH solution of 2mol/L
Obtain Characterization of Barium Titanate Nanotubes array afterwards.
2. Characterization of Barium Titanate Nanotubes array as claimed in claim 1 preparation method it is characterised in that：Described silver nitrate solution
With Ti (OC4H9)4The mol ratio of solution is 1:10, Ti (OC4H9)4The concentration of solution is 0.012M-0.016M, barium nitrate solution
Concentration is 0.01M.
3. Characterization of Barium Titanate Nanotubes array as claimed in claim 1 preparation method it is characterised in that：Described anodised aluminium
The aperture of template is 50-200nm.
4. Characterization of Barium Titanate Nanotubes array as claimed in claim 1 preparation method it is characterised in that：Described in the air standing
Time is：4-10 hour, annealing condition is：Rise to 750 DEG C of insulations 1 with 5 DEG C of heating rates per minute in Muffle furnace
Hour.
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| CN201610847553.XA CN106390975B (en) | 2016-09-26 | 2016-09-26 | A kind of preparation method of Characterization of Barium Titanate Nanotubes array |
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|---|---|---|---|
| CN201610847553.XA CN106390975B (en) | 2016-09-26 | 2016-09-26 | A kind of preparation method of Characterization of Barium Titanate Nanotubes array |
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| CN106390975B CN106390975B (en) | 2018-12-04 |
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| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1824844A (en) * | 2006-01-16 | 2006-08-30 | 中山大学 | Self-supporting bi-pass nano-aluminium oxide form and preparing method thereof |
| US20070138459A1 (en) * | 2005-10-13 | 2007-06-21 | Wong Stanislaus S | Ternary oxide nanostructures and methods of making same |
| CN101037229A (en) * | 2007-04-28 | 2007-09-19 | 首都师范大学 | Preparation method of TiO2 nano material using anode alumina as template by sol-gel process |
| CN101224870A (en) * | 2008-01-23 | 2008-07-23 | 中国科学院化学研究所 | Method for preparing inorganic nano-tube by employing porous templates |
| CN101948144A (en) * | 2010-09-14 | 2011-01-19 | 安徽工程大学 | Preparation method of cobalt sulfide nanotubes or nanowires based on porous anodic aluminum oxide template |
| CN103173764A (en) * | 2013-03-22 | 2013-06-26 | 天津大学 | TiO2 through hole nanotube and CdS compound array film and preparation method thereof |
-
2016
- 2016-09-26 CN CN201610847553.XA patent/CN106390975B/en active Active
Patent Citations (6)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US20070138459A1 (en) * | 2005-10-13 | 2007-06-21 | Wong Stanislaus S | Ternary oxide nanostructures and methods of making same |
| CN1824844A (en) * | 2006-01-16 | 2006-08-30 | 中山大学 | Self-supporting bi-pass nano-aluminium oxide form and preparing method thereof |
| CN101037229A (en) * | 2007-04-28 | 2007-09-19 | 首都师范大学 | Preparation method of TiO2 nano material using anode alumina as template by sol-gel process |
| CN101224870A (en) * | 2008-01-23 | 2008-07-23 | 中国科学院化学研究所 | Method for preparing inorganic nano-tube by employing porous templates |
| CN101948144A (en) * | 2010-09-14 | 2011-01-19 | 安徽工程大学 | Preparation method of cobalt sulfide nanotubes or nanowires based on porous anodic aluminum oxide template |
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| CHIEN CHON CHEN ET AL.: "Template assisted fabrication of TiO2 and BaTiO3 nanotubes", 《APPLIED MECHANICS AND MATERIALS》 * |
| YING-YU CHEN ET AL.: "Template-based fabrication of SrTiO3 and BaTiO3 nanotubes", 《INORGANIC CHEMISTRY》 * |
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