CN104096580A - Preparation method of nanotube containing rare earth elements - Google Patents
Preparation method of nanotube containing rare earth elements Download PDFInfo
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- CN104096580A CN104096580A CN201410291457.2A CN201410291457A CN104096580A CN 104096580 A CN104096580 A CN 104096580A CN 201410291457 A CN201410291457 A CN 201410291457A CN 104096580 A CN104096580 A CN 104096580A
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Abstract
The invention discloses a preparation method of a nanotube containing rare earth elements. According to the preparation method, bismuth-doped titanium dioxide particles are prepared by adopting a sol-gel method, then a titanic acid nanotube doped with boron, the rare earth and bismuth is prepared by adopting a hydro-thermal method, and finally the titanic acid nanotube doped with the boron, the rare earth and the bismuth is cut off under an ultrasonic wave and microwave synergetic and combinatorial effect. The preparation method of the nanotube containing rare earth elements is adopted to cut off the titanic acid nanotube doped with the boron, the rare earth and the bismuth under the ultrasonic wave and microwave synergetic and combinatorial effect, the obtained short titanic acid nanotubes doped with the boron, the rare earth and the bismuth are even in length, and the minimum length can reach 20 nm.
Description
Technical field
The invention belongs to rare earth applied technical field, relate to a kind of preparation method containing rare earth element nano pipe, specifically the preparation method of a kind of boron, rare earth, bismuth element codope metatitanic acid nanometer short tube.
Background technology
The titanate radical nanopipe with architectural features such as large specific area, hollow duct and stratiforms is a kind of important inorganic functional semiconductor nano materials, there is good photoelectricity, photosensitive, air-sensitive, the characteristic such as pressure-sensitive, be widely used as the processing of environmental wastewater photocatalytic degradation, various sensor, solar cell, organism and plant the aspects such as people's material.The surface of titanate radical nanopipe conventionally can be electronegative, and this also makes titanate radical nanopipe become good substrate or the carrier of fixed catalyst particle.A kind of straightforward procedure of conventionally preparing titanate radical nanopipe is nano TiO 2 powder to be carried out in highly basic to hydro-thermal reaction, product can obtain titanate radical nanopipe through diluted acid ion-exchange, very little 10 nanometers that are about of titanate radical nanopipe caliber that obtain, but the length of nanotube product is very long, the hollow duct of nanotube can not make full use of owing to transporting obstacle, sometimes unordered curling up is difficult to disperse, and this application to them brings very large restriction.Simultaneously the forbidden band energy level of titanate radical nanopipe material is 3.3 eV, and ultraviolet light and the black light that can only be less than 387.5nm by wavelength excite, and ultraviolet light only accounts for 5% of sunshine, and 45% visible ray containing in solar energy cannot utilize.In order to improve the utilization rate of visible ray, conventionally adopt the energy gap of element doping Techniques For Reducing titanate radical nanopipe material, expand spectral response range.Cheng-Ching Hu etc. [Effect of nitrogen doping on the microstructure and visible light photocatalysis of titanate nanotubes by a facile cohydrothermal synthesis via urea treatment, Applied Surface Science 280 (2013) 171 – 178] be take urea and have been obtained nitrogen-doped titanic acid nanotube and had good photocatalysis performance as nitrogenous source adopts hydrothermal method.Song Xuchun [preparation of Transition Element Substituted Titanic Acid Nanotubes and photocatalytic activity, Chinese Journal of Inorganic Chemistry, 2005,2l (12): 1897] has prepared the titanate radical nanopipe of different doped transition metal ionses, and that wherein transition metal ions replaces is the Na of interlayer
+or H
+, and and non-substituted metatitanic acid lattice in Ti
4+.The photocatalytic activity of Cr, the Mn obtaining, Fe, Co, Ni, Cu doped transition metal ions titanate radical nanopipe is all improved.V.C.Ferreira [Synthesis and properties of Co-doped titanate nanotubes and their optical sensitization with methylene blue, Materials Chemistry and Physics 142 (2013) 355-362] to take the titania-doped powder of Co be presoma, adopt hydrothermal method to obtain Co doped titanic acid nanotube, wherein Co element has replaced the Ti in metatitanic acid lattice
4+, these Co doped titanic acid nanotubes present strong absworption peak at visible region.But these doped titanic acid nanotubes all belong to single-element doping, and the length Hen of the titanate radical nanopipe obtaining is long.Length is even, multi-element doping metatitanic acid nanometer short tube not only can reduce the utilization rate of energy gap raising visible ray due to doping, the obstacle that transports that simultaneously can reduce its hollow hole road due to short length is fully used hollow duct, thereby has more wide application prospect.
Summary of the invention
The object of the invention is for the deficiencies in the prior art, provides a kind of preparation method containing rare earth element nano pipe, specifically the preparation method of a kind of boron, rare earth, bismuth element codope metatitanic acid nanometer short tube.
The inventive method comprises the following steps:
Step (1). sol-gel process is prepared bismuth doping titanium dioxide nano particle:
It is in the absolute ethyl alcohol of 20～30 parts that the titanate esters that 1-1. is 10 parts by volume parts joins volume parts, stirs and forms titanate esters alcoholic solution;
Described titanate esters is a kind of in butyl titanate, isopropyl titanate or tetraethyl titanate;
It is in polyethylene glycol-200 of 5～10 parts that 1-2. joins volume parts by bismuth salt, dissolves and forms bismuth salting liquid; Wherein in bismuth salt and step 1-1, the molal volume ratio of titanate esters is 0.03～0.3:10, and unit is mM/mL;
Described bismuth salt is a kind of in bismuth nitrate, bismuth chloride or bismuth acetate;
1-3. is even by the absolute ethyl alcohol and stirring that volume parts is the nitric acid of 1～2 part, deionized water that volume parts is 2～4 parts, volume parts is 20 parts, forms acid solution;
The titanate esters alcoholic solution that the bismuth salting liquid that 1-4. obtains step 1-2 and step 1-1 obtain is uniformly mixed, and then drips the acid solution that step 1-3 obtains, and stirs 2～5 hours under normal temperature, forms gel, and then ageing 20～40 hours; The gel of ageing is dried in vacuum drying chamber and removes ethanol and moisture, through alcohol wash, washing, dry, in Muffle furnace, at 500～600 ℃, calcine 4～6 hours after pulverizing, obtain bismuth doping titanium dioxide nano particle;
Step (2). adopt hydro-thermal method to prepare boron, rare earth, bismuth element codope titanate radical nanopipe:
Bismuth doping titanium dioxide nano particle, borax, rare earth compound are joined to dispersed with stirring in the plastic containers that strong base solution is housed, obtain mixed liquor; Wherein the w/v of the titania-doped particle of bismuth, borax, rare earth compound and strong base solution is 2～5g:0.01～0.05g:0.01～0.05g:100mL; Then mixed liquor is proceeded in the stainless steel cauldron of inner liner polytetrafluoroethylene material and react, reaction temperature is 100～140 ℃, 15～30 hours reaction time; After reaction finishes, be cooled to normal temperature, filter taking precipitate, with the diluted nitric acid aqueous solution washing of 0.1M, then with deionized water washing, be then placed in vacuum drying chamber and dry, pulverize to obtain boron, rare earth, bismuth element codope titanate radical nanopipe;
Described rare earth compound is a kind of in lanthanum chloride, lanthanum nitrate, cerium chloride, cerous nitrate;
Described strong base solution is sodium hydrate aqueous solution, and concentration is 8～15M;
Step (3). ultrasonic wave microwave cooperating combined effect cuts off boron, rare earth, bismuth element codope titanate radical nanopipe:
Boron, rare earth, bismuth element codope titanate radical nanopipe are dispersed in the aqueous solution, are then placed under ultrasonic wave microwave composite reaction instrument normal temperature and cut off processing, precipitate and separate, dry boron, rare earth, the bismuth element codope metatitanic acid nanometer short tube of obtaining; Wherein every 100mL aqueous solution is dispersed with 2～5g sulphur, rare earth, bismuth element codope titanate radical nanopipe;
Described ultrasonic wave microwave composite reaction instrument condition is: ultrasonic frequency is 25KHz, and ultrasonic power control range is 10～100W; Microwave frequency is 2450MHz, and microwave power control range is 10～100W; The work for the treatment of time is 1～5 minute.
The inventive method adopts ultrasonic wave microwave cooperating combined effect to cut off boron, rare earth, bismuth element codope titanate radical nanopipe, and the boron of acquisition, rare earth, bismuth element codope metatitanic acid nanometer short tube length are even, the shortest 20nm that reaches of length.
The specific embodiment
Below in conjunction with specific embodiment, the present invention is further analyzed.
Embodiment 1.
Step (1). sol-gel process is prepared bismuth doping titanium dioxide nano particle:
1-1. joins 10 mL butyl titanates in 20 mL absolute ethyl alcohols, stirs and forms 30 mL butyl titanate alcoholic solutions;
1-2. joins 0.03mM bismuth nitrate in 5mL polyethylene glycol-200, dissolves and forms bismuth nitrate solution;
1-3. is even by 1mL nitric acid, 4mL deionized water, 20mL absolute ethyl alcohol and stirring, forms 25mL acid solution;
The butyl titanate alcoholic solution that the bismuth nitrate solution that 1-4. obtains step 1-2 and step 1-1 obtain is uniformly mixed, and then drips the acid solution that step 1-3 obtains, and stirs 2 hours under normal temperature, forms gel, and then ageing 20 hours; The gel of ageing is dried in vacuum drying chamber and removes ethanol and moisture, through alcohol wash, washing, dry, in Muffle furnace, at 500 ℃, calcine 6 hours after pulverizing, obtain bismuth doping titanium dioxide nano particle;
Step (2). adopt hydro-thermal method to prepare boron, rare earth, bismuth element codope titanate radical nanopipe:
2g bismuth doping titanium dioxide nano particle, 0.01g borax, 0.01g lanthanum chloride are joined to dispersed with stirring in the plastic containers that 100mL 8M sodium hydrate aqueous solution is housed, obtain mixed liquor; Then mixed liquor is proceeded in the stainless steel cauldron of inner liner polytetrafluoroethylene material and react, reaction temperature is 100 ℃, 30 hours reaction time; After reaction finishes, be cooled to normal temperature, filter taking precipitate, with the diluted nitric acid aqueous solution washing of 0.1M, then with deionized water washing, be then placed in vacuum drying chamber and dry, pulverize to obtain boron, rare earth, bismuth element codope titanate radical nanopipe;
Step (3). ultrasonic wave microwave cooperating combined effect cuts off boron, rare earth, bismuth element codope titanate radical nanopipe:
The 2g boron that step (2) is obtained, rare earth, bismuth element codope titanate radical nanopipe are dispersed in the 100mL aqueous solution, then be placed under ultrasonic wave microwave composite reaction instrument normal temperature and cut off processing, ultrasonic wave microwave composite reaction instrument condition is: ultrasonic frequency is 25KHz, ultrasonic power control range is 10W, microwave frequency is 2450MHz, microwave power control range is 10W, and the work for the treatment of time is 5 minutes; Precipitate and separate, dry boron, rare earth, the bismuth element codope metatitanic acid nanometer short tube of obtaining.
Embodiment 2.
Step (1). sol-gel process is prepared bismuth doping titanium dioxide nano particle:
1-1. joins 10 mL isopropyl titanates in 30 mL absolute ethyl alcohols, stirs and forms 40mL isopropyl titanate alcoholic solution;
1-2. joins 0.3mM bismuth chloride in 10 mL polyethylene glycol-200, dissolves and forms bismuth chloride solution;
1-3. is even by 1.5mL nitric acid, 3mL deionized water, 20mL absolute ethyl alcohol and stirring, forms 24.5mL acid solution;
The isopropyl titanate alcoholic solution that the bismuth chloride solution that 1-4. obtains step 1-2 and step 1-1 obtain is uniformly mixed, and then drips the acid solution that step 1-3 obtains, and stirs 5 hours under normal temperature, forms gel, and then ageing 40 hours; The gel of ageing is dried in vacuum drying chamber and removes ethanol and moisture, through alcohol wash, washing, dry, in Muffle furnace, at 600 ℃, calcine 4 hours after pulverizing, obtain bismuth doping titanium dioxide nano particle;
Step (2). adopt hydro-thermal method to prepare boron, rare earth, bismuth element codope titanate radical nanopipe:
5g bismuth doping titanium dioxide nano particle, 0.05g borax, 0.05g lanthanum nitrate are joined to dispersed with stirring in the plastic containers that 100mL15M sodium hydrate aqueous solution is housed, obtain mixed liquor; Then mixed liquor is proceeded in the stainless steel cauldron of inner liner polytetrafluoroethylene material and react, reaction temperature is 140 ℃, 15 hours reaction time; After reaction finishes, be cooled to normal temperature, filter taking precipitate, with the diluted nitric acid aqueous solution washing of 0.1M, then with deionized water washing, be then placed in vacuum drying chamber and dry, pulverize to obtain boron, rare earth, bismuth element codope titanate radical nanopipe;
Step (3). ultrasonic wave microwave cooperating combined effect cuts off boron, rare earth, bismuth element codope titanate radical nanopipe:
The 5g boron that step (2) is obtained, rare earth, bismuth element codope titanate radical nanopipe are dispersed in the 100mL aqueous solution, then be placed under ultrasonic wave microwave composite reaction instrument normal temperature and cut off processing, ultrasonic wave microwave composite reaction instrument condition is: ultrasonic frequency is 25KHz, ultrasonic power control range is 100W, microwave frequency is 2450MHz, microwave power control range is 100W, and the work for the treatment of time is 1 minute; Precipitate and separate, dry boron, rare earth, the bismuth element codope metatitanic acid nanometer short tube of obtaining.
Embodiment 3.
Step (1). sol-gel process is prepared bismuth doping titanium dioxide nano particle:
1-1. joins 10 mL tetraethyl titanates in 25 mL absolute ethyl alcohols, stirs and forms tetraethyl titanate alcoholic solution;
1-2. joins 0.1mM bismuth acetate in 8mL polyethylene glycol-200, dissolves and forms bismuth acetate solution; Wherein in bismuth salt and step 1-1, the molal volume ratio of titanate esters is 0.03～0.3:10, and unit is mM/mL,
1-3. is even by 2mL nitric acid, 4mL deionized water, 20mL absolute ethyl alcohol and stirring, forms 26mL acid solution;
The tetraethyl titanate alcoholic solution that the bismuth acetate solution that 1-4. obtains step 1-2 and step 1-1 obtain is uniformly mixed, and then drips the acid solution that step 1-3 obtains, and stirs 4 hours under normal temperature, forms gel, and then ageing 30 hours; The gel of ageing is dried in vacuum drying chamber and removes ethanol and moisture, through alcohol wash, washing, dry, in Muffle furnace, at 550 ℃, calcine 5 hours after pulverizing, obtain bismuth doping titanium dioxide nano particle;
Step (2). adopt hydro-thermal method to prepare boron, rare earth, bismuth element codope titanate radical nanopipe:
3g bismuth doping titanium dioxide nano particle, 0.03g borax, 0.03g cerium chloride are joined to dispersed with stirring in the plastic containers that 100mL 10M sodium hydrate aqueous solution is housed, obtain mixed liquor; Then mixed liquor is proceeded in the stainless steel cauldron of inner liner polytetrafluoroethylene material and react, reaction temperature is 120 ℃, 22 hours reaction time; After reaction finishes, be cooled to normal temperature, filter taking precipitate, with the diluted nitric acid aqueous solution washing of 0.1M, then with deionized water washing, be then placed in vacuum drying chamber and dry, pulverize to obtain boron, rare earth, bismuth element codope titanate radical nanopipe.
Step (3). ultrasonic wave microwave cooperating combined effect cuts off boron, rare earth, bismuth element codope titanate radical nanopipe:
The 3g boron that step (2) is obtained, rare earth, bismuth element codope titanate radical nanopipe are dispersed in the 100mL aqueous solution, then be placed under ultrasonic wave microwave composite reaction instrument normal temperature and cut off processing, ultrasonic wave microwave composite reaction instrument condition is: ultrasonic frequency is 25KHz, ultrasonic power control range is 50W, microwave frequency is 2450MHz, microwave power control range is 50W, and the work for the treatment of time is 4 minutes; Precipitate and separate, dry boron, rare earth, the bismuth element codope metatitanic acid nanometer short tube of obtaining.
Embodiment 4.
Step (1). sol-gel process is prepared bismuth doping titanium dioxide nano particle:
1-1. joins 10 mL tetraethyl titanates in 22mL absolute ethyl alcohol, stirs and forms tetraethyl titanate alcoholic solution;
1-2. joins 0.2mM bismuth acetate in 6mL polyethylene glycol-200, dissolves and forms bismuth acetate solution;
1-3. is even by 1 mL nitric acid, 2mL deionized water, 20mL absolute ethyl alcohol and stirring, forms 23mL acid solution;
The tetraethyl titanate alcoholic solution that the bismuth acetate solution that 1-4. obtains step 1-2 and step 1-1 obtain is uniformly mixed, and then drips the acid solution that step 1-3 obtains, and stirs 3 hours under normal temperature, forms gel, and then ageing 35 hours; The gel of ageing is dried in vacuum drying chamber and removes ethanol and moisture, through alcohol wash, washing, dry, in Muffle furnace, at 570 ℃, calcine 4.5 hours after pulverizing, obtain bismuth doping titanium dioxide nano particle;
Step (2). adopt hydro-thermal method to prepare boron, rare earth, bismuth element codope titanate radical nanopipe:
4g bismuth doping titanium dioxide nano particle, 0.04g borax, 0.02g cerous nitrate are joined to dispersed with stirring in the plastic containers that 100mL 12M sodium hydrate aqueous solution is housed, obtain mixed liquor; Then mixed liquor is proceeded in the stainless steel cauldron of inner liner polytetrafluoroethylene material and react, reaction temperature is 130 ℃, 20 hours reaction time; After reaction finishes, be cooled to normal temperature, filter taking precipitate, with the diluted nitric acid aqueous solution washing of 0.1M, then with deionized water washing, be then placed in vacuum drying chamber and dry, pulverize to obtain boron, rare earth, bismuth element codope titanate radical nanopipe.
Step (3). ultrasonic wave microwave cooperating combined effect cuts off boron, rare earth, bismuth element codope titanate radical nanopipe:
The 4g boron that step (2) is obtained, rare earth, bismuth element codope titanate radical nanopipe are dispersed in the 100mL aqueous solution, then be placed under ultrasonic wave microwave composite reaction instrument normal temperature and cut off processing, ultrasonic wave microwave composite reaction instrument condition is: ultrasonic frequency is 25KHz, ultrasonic power control range is 60W, microwave frequency is 2450MHz, microwave power control range is 60W, and the work for the treatment of time is 3 minutes; Precipitate and separate, dry boron, rare earth, the bismuth element codope metatitanic acid nanometer short tube of obtaining.
Above-described embodiment is not that the present invention is not limited only to above-described embodiment for restriction of the present invention, as long as meet requirement of the present invention, all belongs to protection scope of the present invention.
Claims (6)
1. containing a preparation method for rare earth element nano pipe, it is characterized in that the method comprises the following steps:
Step (1). sol-gel process is prepared bismuth doping titanium dioxide nano particle:
It is in the absolute ethyl alcohol of 20～30 parts that the titanate esters that 1-1. is 10 parts by volume parts joins volume parts, stirs and forms titanate esters alcoholic solution;
It is in polyethylene glycol-200 of 5～10 parts that 1-2. joins volume parts by bismuth salt, dissolves and forms bismuth salting liquid; Wherein in bismuth salt and step 1-1, the molal volume ratio of titanate esters is 0.03～0.3:10, and unit is mM/mL;
1-3. is even by the absolute ethyl alcohol and stirring that volume parts is the nitric acid of 1～2 part, deionized water that volume parts is 2～4 parts, volume parts is 20 parts, forms acid solution;
The titanate esters alcoholic solution that the bismuth salting liquid that 1-4. obtains step 1-2 and step 1-1 obtain is uniformly mixed, and then drips the acid solution that step 1-3 obtains, and stirs 2～5 hours under normal temperature, forms gel, and then ageing 20～40 hours; The gel of ageing is dried in vacuum drying chamber and removes ethanol and moisture, through alcohol wash, washing, dry, in Muffle furnace, at 500～600 ℃, calcine 4～6 hours after pulverizing, obtain bismuth doping titanium dioxide nano particle;
Step (2). adopt hydro-thermal method to prepare boron, rare earth, bismuth element codope titanate radical nanopipe:
Bismuth doping titanium dioxide nano particle, borax, rare earth compound are joined to dispersed with stirring in the plastic containers that strong base solution is housed, obtain mixed liquor; Wherein the w/v of the titania-doped particle of bismuth, borax, rare earth compound and strong base solution is 2～5g:0.01～0.05g:0.01～0.05g:100mL; Then mixed liquor is proceeded in the stainless steel cauldron of inner liner polytetrafluoroethylene material and react, reaction temperature is 100～140 ℃, 15～30 hours reaction time; After reaction finishes, be cooled to normal temperature, filter taking precipitate, with the diluted nitric acid aqueous solution washing of 0.1M, then with deionized water washing, be then placed in vacuum drying chamber and dry, pulverize to obtain boron, rare earth, bismuth element codope titanate radical nanopipe;
Step (3). ultrasonic wave microwave cooperating combined effect cuts off boron, rare earth, bismuth element codope titanate radical nanopipe:
Boron, rare earth, bismuth element codope titanate radical nanopipe are dispersed in the aqueous solution, are then placed under ultrasonic wave microwave composite reaction instrument normal temperature and cut off processing, precipitate and separate, dry boron, rare earth, the bismuth element codope metatitanic acid nanometer short tube of obtaining; Wherein every 100mL aqueous solution is dispersed with 2～5g sulphur, rare earth, bismuth element codope titanate radical nanopipe.
2. a kind of preparation method containing rare earth element nano pipe as claimed in claim 1, is characterized in that the described titanate esters of step (1) is a kind of in butyl titanate, isopropyl titanate or tetraethyl titanate.
3. a kind of preparation method containing rare earth element nano pipe as claimed in claim 1, is characterized in that the described bismuth salt of step (1) is a kind of in bismuth nitrate, bismuth chloride or bismuth acetate.
4. a kind of preparation method containing rare earth element nano pipe as claimed in claim 1, is characterized in that the described rare earth compound of step (2) is a kind of in lanthanum chloride, lanthanum nitrate, cerium chloride, cerous nitrate.
5. a kind of preparation method containing rare earth element nano pipe as claimed in claim 1, is characterized in that the described strong base solution of step (2) is sodium hydrate aqueous solution, and concentration is 8～15M.
6. a kind of preparation method containing rare earth element nano pipe as claimed in claim 1, is characterized in that the described ultrasonic wave microwave composite reaction instrument condition of step (3) is: ultrasonic frequency is 25KHz, and ultrasonic power control range is 10～100W; Microwave frequency is 2450MHz, and microwave power control range is 10～100W; The work for the treatment of time is 1～5 minute.
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| CN112851116A (en) * | 2021-01-19 | 2021-05-28 | 吉林师范大学 | High-density terbium/cerium-doped scintillation glass and preparation method thereof |
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| JP2008297147A (en) * | 2007-05-30 | 2008-12-11 | Hokkaido Univ | Production method of anatase octahedral titanium oxide fine particle and titanium oxide fine particles |
| CN101664677A (en) * | 2009-09-22 | 2010-03-10 | 陕西科技大学 | Preparation method of samarium-doped titanium dioxide powder |
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| Publication number | Priority date | Publication date | Assignee | Title |
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| JP2008297147A (en) * | 2007-05-30 | 2008-12-11 | Hokkaido Univ | Production method of anatase octahedral titanium oxide fine particle and titanium oxide fine particles |
| CN101664677A (en) * | 2009-09-22 | 2010-03-10 | 陕西科技大学 | Preparation method of samarium-doped titanium dioxide powder |
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| QIULI YUAN等: "Adsorption-induced scission of titanate nanotubes", 《PHYSICA E》, vol. 43, 11 July 2010 (2010-07-11) * |
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| CN112851116A (en) * | 2021-01-19 | 2021-05-28 | 吉林师范大学 | High-density terbium/cerium-doped scintillation glass and preparation method thereof |
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