CN101327951A - Method for controllable synthesis of pure phase anatase, red schorl, brookite titania nanorod - Google Patents
Method for controllable synthesis of pure phase anatase, red schorl, brookite titania nanorod Download PDFInfo
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Abstract
The invention provides a method for controllably synthesizing pure phase anatase, rutile, brookite titanium dioxide nano-rod. The pure phase anatase, rutile, brookite titanium dioxide nano-rod can be controllably synthesized by controlling the reaction condition of precursor prepared by titanium dioxide powder and alkali solution through a simple hydrothermal method. The method of the invention controllably synthesizes pure phase anatase, rutile, brookite titanium dioxide nano-rod through a simple hydrothermal method at a lower temperature and under a condition without adding any surfactants or templates and has advantages of simply operation, low cost, stable performance, high purity, obvious economic benefit and social benefit which can be synthesized in a large amount.
Description
Technical field
The invention belongs to technical field of nano material, more specifically relate to the method for a kind of controllable synthesis of pure phase anatase, rutile, brookite titania nanorod.
Background technology
Titanium dioxide nano material all has important use to be worth at aspects such as solar cell, lithium ion battery, gas sensor, photocatalysis to degrade organic matter, general template and the hydrothermal method of adopting of tradition carried out the preparation of titanium dioxide nano material, though the titanium dioxide nano material purity height that adopts template to obtain, but preparation process complexity, and need add tensio-active agent and template, the temperature that reaction needed is higher, the raw materials cost height; Adopt the technology of preparing of existing hydrothermal method at present, though preparation process is simple, the titanium dioxide nano material purity of preparing is not enough, and the relevant report of controllable synthesis of pure phase anatase, rutile, brookite titania nanorod is not particularly also arranged at present; In addition, brookite type titanium dioxide generally generates under the occurring in nature high-temperature and high-pressure conditions, is difficult to synthetic pure phase brookite with manual method.Although the synthetic pure phase brookite type titanium dioxide nanoparticle of report is arranged, the brookite type titanium dioxide nanometer rod also is not in the news.
Summary of the invention
The method that the purpose of this invention is to provide a kind of controllable synthesis of pure phase anatase, rutile, brookite titania nanorod, this method is added under the condition of any tensio-active agent and template at a lower temperature and not, with simple hydrothermal method controllable synthesis of pure phase anatase, rutile, brookite titania nanorod, it is easy and simple to handle, cost is low, stable performance, the purity height, can synthesize in a large number.
The method of controllable synthesis of pure phase anatase titanium dioxide nano-rod of the present invention, step is: with 0.5-2g titania powder and concentration is the alkaline solution 10-50mL of 8-12 mol, thorough mixing is even in stainless steel autoclave or polytetrafluoroethylcontainer container, and mixture reacts 24-48h under 363-373K; The product that generates as presoma, is adjusted to 5-7 with the pH value of presoma and is placed on and reacts 48h in stainless steel autoclave or the polytetrafluoroethylcontainer container obtain the pure phase anatase titanium dioxide nano-rod under 433-463K.
The method of controlledly synthesis pure phase rutile titanium dioxide nanometer rod of the present invention, step is: with 0.5-2g titania powder and concentration is the alkaline solution 10-50mL of 8-12 mol, thorough mixing is even in stainless steel autoclave or polytetrafluoroethylcontainer container, and mixture reacts 24-48h under 363-373K; The product that generates as presoma, is added the salpeter solution 50mL of 2-3 mol with presoma, be placed on again in stainless steel autoclave or the polytetrafluoroethylcontainer container that reaction 40-60h obtains pure phase rutile titanium dioxide nanometer rod under 433-463K.
The method of controlledly synthesis pure phase brookite titania nanorod of the present invention, step is: with 0.5-2g titania powder and concentration is the alkaline solution (please replenish the consumption of alkaline solution) of 8-12 mol, thorough mixing is even in stainless steel autoclave or polytetrafluoroethylcontainer container, and mixture reacts 24-48h under 363-373K; The product that generates as presoma, is adjusted to 10-11 with presoma pH value, is placed on again and under 443-473K, reacts 40-60h in stainless steel autoclave or the polytetrafluoroethylcontainer container and obtain the pure phase brookite titania nanorod.
Remarkable advantage of the present invention is:
1) method of the present invention is added under the condition of any tensio-active agent and template at a lower temperature and not, with simple hydrothermal method controllable synthesis of pure phase anatase, rutile, brookite titania nanorod, it is easy and simple to handle, cost is low, stable performance, the purity height, can synthesize in a large number; Controllable synthesis of pure phase anatase, rutile, brookite titania nano material utilize nano titanium oxide to offer help for people detect between the various crystalline phase titanium dioxide contact and better choice.
2) raw material of the present invention and preparation process are scientific and reasonable: at first, and the H on surface
+And OH
-Remarkable influence TiO
6The structure that shows free energy and it form.In reaction process, work as H
+Concentration when higher, it will reduce TiO effectively
6Show free energy; Because the energy of rutile phase is lower, through just forming the rutile phase after the hydro-thermal reaction naturally.When the approaching neutrality of pH value, H
+Concentration to TiO
6Structure influence very little, through after the hydrothermal treatment consists, the titanate condensation of prionodont structure forms anatase phase titanium dioxide.When alkalescence bigger, when just Na+ content is higher, Na in the process of titanate condensation
+Discharge and finally form the titanium dioxide of brookite phase.Secondly, according to a series of experimental result and analysis, we think that formation has the TiO of different crystalline phases and pattern
2Nano material may be the process of a dissolving and recrystallize.At first, the dissolving of sodium titanate nanometer sheet forms [TiO
6] elementary cell.Secondly, [TiO
6] the elementary cell recombine forms different crystalline phases and pattern.Under acidic conditions, help the formation of rutile phase; Under neutrallty condition, help forming the anatase octahedrite phase; Under strong alkaline condition, help forming the brookite phase.
3) the more similar length major part with the rutile nano-stick appearance of synthetic anatase octahedrite of the present invention is a nanometer more than 100, and diameter is about tens nanometers, and the brookite nanometer rod is different from two kinds of nanometer rod of front, is the biconical structure, and length is about 1～2 μ m.Purity is higher than 99%.
Description of drawings
Fig. 1 is the transmission electron microscope photo of rutile nano-stick of the present invention.
Fig. 2 is the transmission electron microscope photo of anatase octahedrite nanometer rod of the present invention.
Fig. 3 is the transmission electron microscope photo of brookite nanometer rod of the present invention.
Embodiment
The controllable synthesis of pure phase anatase titanium dioxide nano-rod: with 0.5-2g titania powder and concentration is the alkaline solution 10-50mL of 8-12 mol, thorough mixing is even in stainless steel autoclave or polytetrafluoroethylcontainer container, and mixture reacts 24-48h under 363-373K; The product that generates as presoma, is adjusted to 5-7 with the pH value of presoma and is placed on and reacts 48h in stainless steel autoclave or the polytetrafluoroethylcontainer container obtain the pure phase anatase titanium dioxide nano-rod under 433-463K.
Alkali in the described alkaline solution is caustic soda.
The pH value of described presoma adopts pH meter control, and described pH value adopts caustic soda or nitric acid to regulate.
Controlledly synthesis pure phase rutile titanium dioxide nanometer rod: with 0.5-2g titania powder and concentration is the alkaline solution 10-50mL of 8-12 mol, thorough mixing is even in stainless steel autoclave or polytetrafluoroethylcontainer container, and mixture reacts 24-48h under 363-373K; The product that generates as presoma, is added the salpeter solution 50mL of 2-3 mol with presoma, be placed on again in stainless steel autoclave or the polytetrafluoroethylcontainer container that reaction 40-60h obtains pure phase rutile titanium dioxide nanometer rod under 433-463K.
Alkali in the described alkaline solution is caustic soda.
Controlledly synthesis pure phase brookite titania nanorod: with 0.5-2g titania powder and concentration is the alkaline solution (please replenish the consumption of alkaline solution) of 8-12 mol, thorough mixing is even in stainless steel autoclave or polytetrafluoroethylcontainer container, and mixture reacts 24-48h under 363-373K; The product that generates as presoma, is adjusted to 10-11 with presoma pH value, is placed on again and under 443-473K, reacts 40-60h in stainless steel autoclave or the polytetrafluoroethylcontainer container and obtain the pure phase brookite titania nanorod.
Alkali in the described alkaline solution is caustic soda.
The pH value of described presoma adopts pH meter control, and described pH value adopts caustic soda or nitric acid to regulate.
The more similar length major part with the rutile nano-stick appearance of synthetic anatase octahedrite of the present invention is a nanometer more than 100, and diameter is about tens nanometers, and the brookite nanometer rod is different from two kinds of nanometer rod of front, is the biconical structure, and length is about 1～2 μ m.Purity is higher than 99%.
Below be several embodiments of the present invention, further set forth the present invention, but the present invention be not limited only to this.
Embodiment 1
The controllable synthesis of pure phase anatase titanium dioxide nano-rod
With 0.5g titania powder and concentration is the alkaline solution 10mL of 8 mol, and thorough mixing is even in stainless steel autoclave or polytetrafluoroethylcontainer container, and mixture reacts 24h under 363K; The product that generates as presoma, is adjusted to 5 with the pH value of presoma and is placed on and reacts 48h in stainless steel autoclave or the polytetrafluoroethylcontainer container obtain the pure phase anatase titanium dioxide nano-rod under 433K.
Alkali in the described alkaline solution is caustic soda.
The pH value of described presoma adopts pH meter control, and described pH value adopts caustic soda or nitric acid to regulate.
Synthetic anatase titania nanometer rod length is: 100nm, diameter is: 20nm, purity is: 99%.
Embodiment 2
The controllable synthesis of pure phase anatase titanium dioxide nano-rod
With 2g titania powder and concentration is the alkaline solution 20mL of 12 mol, and thorough mixing is even in stainless steel autoclave or polytetrafluoroethylcontainer container, and mixture reacts 48h under 373K; The product that generates as presoma, is adjusted to 7 with the pH value of presoma and is placed on and reacts 48h in stainless steel autoclave or the polytetrafluoroethylcontainer container obtain the pure phase anatase titanium dioxide nano-rod under 463K.
Alkali in the described alkaline solution is caustic soda.
The pH value of described presoma adopts pH meter control, and described pH value adopts caustic soda or nitric acid to regulate.
Synthetic anatase titania nanometer rod length is: 150nm, diameter is: 30nm, purity is: be higher than 99%.
Embodiment 3
The controllable synthesis of pure phase anatase titanium dioxide nano-rod
With 1-1.5g titania powder and concentration is the alkaline solution 30mL of 10 mol, and thorough mixing is even in stainless steel autoclave or polytetrafluoroethylcontainer container, and mixture reacts 30-40h under 370K; The product that generates as presoma, is adjusted to 6 with the pH value of presoma, is placed on again and under 450-460K, reacts 48h in stainless steel autoclave or the polytetrafluoroethylcontainer container and obtain the pure phase anatase titanium dioxide nano-rod.
Alkali in the described alkaline solution is caustic soda.
The pH value of described presoma adopts pH meter control, and described pH value adopts caustic soda or nitric acid to regulate.
Synthetic anatase titania nanometer rod length is: 150nm, diameter is: 30nm, purity is: be higher than 99%.
Embodiment 4
Controlledly synthesis pure phase rutile titanium dioxide nanometer rod
With 0.5g titania powder and concentration is the alkaline solution 20mL of 8 mol, and thorough mixing is even in stainless steel autoclave or polytetrafluoroethylcontainer container, and mixture reacts 24h under 363K; The product that generates as presoma, is added the salpeter solution 50mL of 2 mol with presoma, be placed on again in stainless steel autoclave or the polytetrafluoroethylcontainer container that reaction 40h obtains pure phase rutile titanium dioxide nanometer rod under 433-K.
Alkali in the described alkaline solution is caustic soda.
Synthetic rutile titanium dioxide nanometer rod length is: 200nm, diameter is: 40nm, purity is: be higher than 99%.
Embodiment 5
Controlledly synthesis pure phase rutile titanium dioxide nanometer rod
With 2g titania powder and concentration is the alkaline solution 30mL of 12 mol, and thorough mixing is even in stainless steel autoclave or polytetrafluoroethylcontainer container, and mixture reacts 48h under 373K; The product that generates as presoma, is added the salpeter solution 50mL of 3 mol with presoma, be placed on again in stainless steel autoclave or the polytetrafluoroethylcontainer container that reaction 60h obtains pure phase rutile titanium dioxide nanometer rod under 463K.
Alkali in the described alkaline solution is caustic soda.
Synthetic rutile titanium dioxide nanometer rod length is: 300nm, diameter is: 40nm, purity is: be higher than 99%.
Embodiment 6
Controlledly synthesis pure phase rutile titanium dioxide nanometer rod
With 1-1.5g titania powder and concentration is the alkaline solution caustic soda of lO-11 mol, and thorough mixing is even in stainless steel autoclave or polytetrafluoroethylcontainer container, and mixture reacts 30-40h under 365-370K; The product that generates as presoma, is added the salpeter solution 50mL of 2.5 mol with presoma, be placed on again in stainless steel autoclave or the polytetrafluoroethylcontainer container that reaction 50-55h obtains pure phase rutile titanium dioxide nanometer rod under 450-460K.
Alkali in the described alkaline solution is caustic soda.
Synthetic rutile titanium dioxide nanometer rod length is: 300nm, diameter is: 40nm, purity is: be higher than 99%.
Embodiment 7
Controlledly synthesis pure phase brookite titania nanorod
With 0.5-2g titania powder and concentration is the alkaline solution 20mL of 8.12 mol, and thorough mixing is even in stainless steel autoclave or polytetrafluoroethylcontainer container, and mixture reacts 24-48h under 363-373K; The product that generates as presoma, is adjusted to 10-11 with presoma pH value, is placed on again and under 443-473K, reacts 40-60h in stainless steel autoclave or the polytetrafluoroethylcontainer container and obtain the pure phase brookite titania nanorod.
Alkali in the described alkaline solution is caustic soda.
The pH value of described presoma adopts pH meter control, and described pH value adopts caustic soda or nitric acid to regulate.
The synthetic brookite titania nanorod is the biconical structure, and length is about 1 gm, and purity is: be higher than 99%.
Embodiment 8
Controlledly synthesis pure phase brookite titania nanorod
With 2g titania powder and concentration is the alkaline solution 30mL of 12 mol, and thorough mixing is even in stainless steel autoclave or polytetrafluoroethylcontainer container, and mixture reacts 48h under 373K; The product that generates as presoma, is adjusted to 11 with presoma pH value, is placed on again and under 443-473K, reacts 60h in stainless steel autoclave or the polytetrafluoroethylcontainer container and obtain the pure phase brookite titania nanorod.
Alkali in the described alkaline solution is caustic soda.
The pH value of described presoma adopts pH meter control, and described pH value adopts caustic soda or nitric acid to regulate.
The synthetic brookite titania nanorod is the biconical structure, and length is about 2 μ m, and purity is: be higher than 99%.
Embodiment 9
Controlledly synthesis pure phase brookite titania nanorod
With 1-1.5g titania powder and concentration is the alkaline solution 50mL of 9.11 mol, and thorough mixing is even in stainless steel autoclave or polytetrafluoroethylcontainer container, and mixture reacts 30-45h under 370K; The product that generates as presoma, is adjusted to 10.5 with presoma pH value, is placed on again and under 450K, reacts 50-55h in stainless steel autoclave or the polytetrafluoroethylcontainer container and obtain the pure phase brookite titania nanorod.
Alkali in the described alkaline solution is caustic soda.
The pH value of described presoma adopts pH meter control, and described pH value adopts caustic soda or nitric acid to regulate.The synthetic brookite titania nanorod is the biconical structure, and length is about 1.5 μ m, and purity is: be higher than 99%.
Claims (9)
1. the method for a controllable synthesis of pure phase anatase titanium dioxide nano-rod, it is characterized in that: the step of described method is: with 0.5-2g titania powder and concentration is the alkaline solution 10-50mL of 8-12 mol, thorough mixing is even in stainless steel autoclave or polytetrafluoroethylcontainer container, and mixture reacts 24-48h under 363-373K; The product that generates as presoma, is adjusted to 5-7 with the pH value of presoma and is placed on and reacts 48h in stainless steel autoclave or the polytetrafluoroethylcontainer container obtain the pure phase anatase titanium dioxide nano-rod under 433-463K.
2. the method for controllable synthesis of pure phase anatase titanium dioxide nano-rod according to claim 1 is characterized in that: the alkali in the described alkaline solution is caustic soda.
3. the method for controllable synthesis of pure phase anatase titanium dioxide nano-rod according to claim 1 is characterized in that: the pH value of described presoma adopts pH meter control, and described pH value adopts caustic soda or nitric acid to regulate.
4. the method for a controlledly synthesis pure phase rutile titanium dioxide nanometer rod, it is characterized in that: the step of described method is: with 0.5-2g titania powder and concentration is the alkaline solution 10-50mL of 8-12 mol, thorough mixing is even in stainless steel autoclave or polytetrafluoroethylcontainer container, and mixture reacts 24-48h under 363-373K; The product that generates as presoma, is added the salpeter solution 50mL of 2-3 mol with presoma, be placed on again in stainless steel autoclave or the polytetrafluoroethylcontainer container that reaction 40-60h obtains pure phase rutile titanium dioxide nanometer rod under 433-463K.
5. the method for controlledly synthesis pure phase rutile titanium dioxide nanometer rod according to claim 4 is characterized in that: the alkali in the described alkaline solution is caustic soda.
6. the method for a controlledly synthesis pure phase brookite titania nanorod, it is characterized in that: the step of described method is: with 0.5-2g titania powder and concentration is the alkaline solution 10-50mL of 8-12 mol, thorough mixing is even in stainless steel autoclave or polytetrafluoroethylcontainer container, and mixture reacts 24-48h under 363-373K; The product that generates as presoma, is adjusted to 10-11 with presoma pH value, is placed on again and under 443-473K, reacts 40-60h in stainless steel autoclave or the polytetrafluoroethylcontainer container and obtain the pure phase brookite titania nanorod.
7. the method for controlledly synthesis pure phase brookite titania nanorod according to claim 6 is characterized in that: the alkali in the described alkaline solution is caustic soda.
8. the method for controlledly synthesis pure phase brookite titania nanorod according to claim 6 is characterized in that: the pH value of described presoma adopts pH meter control, and described pH value adopts caustic soda or nitric acid to regulate
9. the method for controlledly synthesis pure phase brookite titania nanorod according to claim 6 is characterized in that: described pure phase brookite titania nanorod is the biconical structure, and length is 1～2 μ m.
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|---|---|---|---|---|
| CN101880057A (en) * | 2010-06-04 | 2010-11-10 | 山东轻工业学院 | Method for preparing high-purity brookite titanium dioxide with controlled appearance |
| CN101550595B (en) * | 2009-04-03 | 2011-07-20 | 哈尔滨工业大学 | Method for preparing pure rutile-phase titanium dioxide single crystalline nanorod without template under low temperature |
| CN102285685A (en) * | 2011-05-18 | 2011-12-21 | 福州大学 | Nanorod rutile TiO2 mesocrystalline and preparation method and application thereof |
| CN102336435A (en) * | 2011-09-13 | 2012-02-01 | 福州大学 | Porous rutile TiO2 mesomorphase and preparation method and application thereof |
| CN103058273A (en) * | 2011-10-20 | 2013-04-24 | 中国科学院福建物质结构研究所 | Monodispersed brookite phase titanium dioxide nanometer spindle body powder and preparation method thereof |
| CN103848457A (en) * | 2012-11-29 | 2014-06-11 | 中国科学院合肥物质科学研究院 | Nitrogen-doped anatase crystal form titanium dioxide nanopowder and preparation method thereof |
| CN104760995A (en) * | 2015-03-13 | 2015-07-08 | 首都师范大学 | Preparation method of brookite titanium doxide nano-rod |
| CN104925750A (en) * | 2015-05-07 | 2015-09-23 | 南京文钧医疗科技有限公司 | Preparation method for TiO2 nanowire-Ag/AgCl-Fe3O4 composite material with Yolk-Shell structures |
| CN105056925A (en) * | 2015-09-07 | 2015-11-18 | 黑龙江大学 | Preparation method of black titanium dioxide nano rod visible light catalyst |
| CN106348340A (en) * | 2016-07-28 | 2017-01-25 | 安徽师范大学 | TiO2 single-crystal hollow square nanocone material and preparation method and application thereof |
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| CN114804197A (en) * | 2021-01-28 | 2022-07-29 | 中国科学院大连化学物理研究所 | Brookite titanium dioxide nanorod and preparation method thereof |
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| CN101550595B (en) * | 2009-04-03 | 2011-07-20 | 哈尔滨工业大学 | Method for preparing pure rutile-phase titanium dioxide single crystalline nanorod without template under low temperature |
| CN101880057A (en) * | 2010-06-04 | 2010-11-10 | 山东轻工业学院 | Method for preparing high-purity brookite titanium dioxide with controlled appearance |
| CN102285685A (en) * | 2011-05-18 | 2011-12-21 | 福州大学 | Nanorod rutile TiO2 mesocrystalline and preparation method and application thereof |
| CN102285685B (en) * | 2011-05-18 | 2013-04-17 | 福州大学 | Nanorod rutile TiO2 mesocrystalline and preparation method and application thereof |
| CN102336435A (en) * | 2011-09-13 | 2012-02-01 | 福州大学 | Porous rutile TiO2 mesomorphase and preparation method and application thereof |
| CN103058273A (en) * | 2011-10-20 | 2013-04-24 | 中国科学院福建物质结构研究所 | Monodispersed brookite phase titanium dioxide nanometer spindle body powder and preparation method thereof |
| CN103848457A (en) * | 2012-11-29 | 2014-06-11 | 中国科学院合肥物质科学研究院 | Nitrogen-doped anatase crystal form titanium dioxide nanopowder and preparation method thereof |
| CN104760995A (en) * | 2015-03-13 | 2015-07-08 | 首都师范大学 | Preparation method of brookite titanium doxide nano-rod |
| CN104925750A (en) * | 2015-05-07 | 2015-09-23 | 南京文钧医疗科技有限公司 | Preparation method for TiO2 nanowire-Ag/AgCl-Fe3O4 composite material with Yolk-Shell structures |
| CN105056925A (en) * | 2015-09-07 | 2015-11-18 | 黑龙江大学 | Preparation method of black titanium dioxide nano rod visible light catalyst |
| CN106348340A (en) * | 2016-07-28 | 2017-01-25 | 安徽师范大学 | TiO2 single-crystal hollow square nanocone material and preparation method and application thereof |
| CN107043127A (en) * | 2017-05-18 | 2017-08-15 | 武汉工程大学 | A kind of TiO as obtained by nitric acid neutralisation treatment regulates and controls alkaline hydro-thermal method2The method of nano particle pattern |
| CN107043127B (en) * | 2017-05-18 | 2019-05-03 | 武汉工程大学 | A kind of TiO as obtained by nitric acid neutralisation treatment regulation alkaline hydro-thermal method2The method of nano particle pattern |
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