CN102211788B - Preparation method of titanium dioxide nano powder and titanium dioxide nano powder prepared by same - Google Patents
Preparation method of titanium dioxide nano powder and titanium dioxide nano powder prepared by same Download PDFInfo
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- CN102211788B CN102211788B CN 201010154384 CN201010154384A CN102211788B CN 102211788 B CN102211788 B CN 102211788B CN 201010154384 CN201010154384 CN 201010154384 CN 201010154384 A CN201010154384 A CN 201010154384A CN 102211788 B CN102211788 B CN 102211788B
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Abstract
The invention provides a preparation method of titanium dioxide nano powder and the titanium dioxide nano powder prepared by the same. The preparation method of micro-spherical titanium dioxide nano powder comprises the following steps of: a) adding titanium precursor into deionized water to obtain titanium precursor solution; b) adding surfactant into the deionized water to obtain surfactant solution; c) adding the surfactant solution into the titanium precursor solution to obtain mixed solution; d) collecting the micro-spherical titanium dioxide nano powder in the mixed solution; and e) drying the micro-spherical titanium dioxide nano powder. By the preparation method of the titanium dioxide nano powder, the titanium dioxide nano powder which is suitable for mass production, is low in preparation cost and has uniform particle sizes can be obtained. The micro-spherical titanium dioxide nano powder prepared by the method can be further used for the preparation of the micro-spherical titanium dioxide nano film.
Description
Technical field
The present invention relates to a kind of preparation method of how ground rice body, relate in particular to the how preparation method of ground rice body and the titanium dioxide that utilizes the method preparation ground rice body how of a kind of titanium dioxide.
Background technology
Global in recent years how meter scientific and technological development is in the ascendant, and the develop of many Nanometer materials has improved people's life really, has also started infinite commercial opportunities.Because the semiconductor energy rank of titanium dioxide (TiO2) have wide can being with, and therefore are widely used for as the multifunctional light catalyst.Although the semiconductor energy rank of zinc oxide also have wide can band, also can be used as the multifunctional catalyst material, its chemical stability relatively poor (for example, not acid resistance solution).Therefore, major part is rice photocatalyst material or take titanium dioxide as main how, and it is present the most widely used Nanometer material.
The titanium dioxide how preparation method of ground rice body is a lot, mainly can be divided into Physical and chemical method.Physical is preparation method the earliest, and it utilizes as the vapor condensation method, reach the physics mode such as high-energy ball milling method and how to obtain the ground rice body.The vapor condensation ratio juris is to utilize variety of way to make material evaporation or evaporate into gas phase, and utilizes special technique condensation (such as liquid nitrogen) nucleation, how to obtain the ground rice body.High, the particle size dispersion of powder purity of in this way preparation evenly, size can control, and is fit to produce high-melting-point how rice metallics or rice grain film how.High-energy ball milling method is the huge energy when utilizing the ball mill rotation and vibration, with raw material pulverizing for how the meter level particle.Its advantage is that simple to operate, easy realization is produced continuously, and shortcoming then is that granular size is inhomogeneous, and easily introduces impurity.Chemical method is how another kind prepares the method for ground rice body, involves some chemical reactions in its process.For the preparation of micro mist and how the chemical method of ground rice body mainly contain the precipitator method, hydrolysis method, sol-gel method, hydrothermal method, spray method, oxidation reduction process, laser synthesis method, and electrochemistry preparation method etc.More than just roughly classification, also can be used the aforesaid method collocation how in the preparation process of ground rice body at titanium dioxide.For example, the precipitator method and spray method often involve hydrolysis reaction and redox reaction; Hydrothermal method is also often in conjunction with the how ground rice body of sol-gel method with the preparation different-shape, such as nanowire, how rice rod, how mitron, Mi Weiqiu etc. how.
At the above-mentioned various titanium dioxide that prepare how in the method for ground rice body, the spraying cracking process is at present with titanium dioxide one of commercial main processing procedure of ground rice body how, utilizes this processing procedure can obtain uniform particle diameter and stay-in-grade how ground rice body.In addition, utilize sol-gel method and hydrothermal method, the titanium dioxide that can prepare various patterns is the ground rice body how; And can be by pH value, hydrothermal temperature, reaction times and the strength of solution of control reaction soln, how meter ruler is very little to adjust it.This is for obtaining at present the how modal method of rice structure of variation.
Along with the fast development of scientific and technological industry, how the application of ground rice body in each field also increases the titanium dioxide of various patterns day by day.Usually, at preparation microspheroidal titanium dioxide how during the ground rice body, use be hydrothermal method, microemulsion method, and template etc.Yet aforesaid method needs expensive production unit, and is unfavorable for a large amount of and continuous production; In addition, by the prepared powder of these methods, its homogeneity still remains to be improved.Therefore, the how preparation method of ground rice body of a kind of microspheroidal titanium dioxide need to be developed, a large amount of productions can be fit to, how the ground rice body has uniform size for the cheap for manufacturing cost and titanium dioxide that makes.
Summary of the invention
The technical problem to be solved in the present invention provides the how preparation method of ground rice body of a kind of titanium dioxide, utilizes the method can obtain how ground rice body of particle diameter microspheroidal titanium dioxide even, with low cost.
For solving the problems of the technologies described above, embodiments of the invention provide technical scheme as follows:
A kind of microspheroidal titanium dioxide is the preparation method of ground rice body how, comprises the following steps:
(a) a titanium precursor thing is added in the deionized water, obtain a titanium precursor thing solution;
(b) interfacial agent is added in the deionized water, obtain an interfacial activity agent solution;
(c) this interfacial activity agent solution is added in this titanium precursor thing solution, obtain a mixed solution;
(d) collect microspheroidal titanium dioxide ground rice body how in this mixed solution;
(e) how the ground rice body is in addition dry with this microspheroidal titanium dioxide.
Wherein, this titanium precursor thing is titanium tetrachloride.
Wherein, this titanium precursor thing is the titanium alkoxide.
Wherein, the alkyl of this titanium alkoxide has 1 to 6 carbon atom.
Wherein, this interfacial agent is ethylene glycol.
Wherein, this interfacial agent is glycol derivative.
Wherein, step (a) is carried out under 3 to 10 ℃ temperature.
Wherein, step (a) is carried out under a rare gas element.
Wherein, this rare gas element is nitrogen or argon gas.
Further, after obtaining this titanium precursor thing solution, with under the temperature of in 4 to 15 ℃ of this titanium precursor thing solution left standstills 3 to 48 hours.
Wherein, this microspheroidal titanium dioxide how the size of ground rice body be along with the mole of this titanium precursor thing and this interfacial agent than and change.
Embodiments of the invention also provide how ground rice body of a kind of microspheroidal titanium dioxide, be utilize above-mentioned microspheroidal titanium dioxide how the preparation method of ground rice body make.
The present invention also provides how rice thin film technology method of a kind of titanium dioxide, to form how rice film of microspheroidal titanium dioxide at various substrates.
The present invention utilizes hydrolysis method and shallow lake, Shen method with preparation microspheroidal titanium dioxide ground rice body how; In hydrolytic process, adjust the mole ratio of titanium precursor thing and interfacial agent, with the control microspheroidal titanium dioxide size of ground rice body how.Preparation method according to the present invention, the titanium dioxide that can generate at short notice micro-sphere structure is the ground rice body how, and its diameter is between between the 50nm to 2000nm, and has good quality.
With the microspheroidal titanium dioxide that utilizes aforesaid method to make how the ground rice body add among entry, aqueous solvent or the oil-based solvent, add again for example organic molecule, oligomer, high molecular dispersion agent, to form slurry or solution.Wherein, also optionally add anionic and cationic interfacial agent.Then, the modes such as recycling wire mark, rotary coating, spraying form how rice film of microspheroidal titanium dioxide at substrate.
Description of drawings
Fig. 1 is the how scanning type electron microscope image of ground rice body of embodiments of the invention microspheroidal titanium dioxide, and microspheroidal titanium dioxide shown in 1 (a) the how particle diameter of ground rice body is 650 to 750nm; Microspheroidal titanium dioxide shown in 1 (b) the how particle diameter of ground rice body is 550 to 650nm; Microspheroidal titanium dioxide shown in 1 (c) the how particle diameter of ground rice body is 450 to 550nm; Microspheroidal titanium dioxide shown in 1 (d) the how particle diameter of ground rice body is 300 to 400nm;
Fig. 2 is the how X-ray diffraction chart of ground rice body of embodiments of the invention microspheroidal titanium dioxide;
Fig. 3 is the microspheroidal titanium dioxide sweep electron microscope image of rice film how that is configured on the base material.
Embodiment
For technical problem, technical scheme and advantage that embodiments of the invention will be solved is clearer, be described in detail below in conjunction with the accompanying drawings and the specific embodiments.
Embodiments of the invention are for preparation microspheroidal titanium dioxide in the prior art how during the ground rice body, need expensive production unit, and be unfavorable for reaching in a large number the quantity-produced problem, the how preparation method of ground rice body and the titanium dioxide that utilizes the method preparation ground rice body how of a kind of microspheroidal titanium dioxide is provided, can obtains to be fit to produce in a large number, cheap for manufacturing cost and titanium dioxide with uniform size ground rice body how.
The deionized water of 200mL is remained on temperature under the ice bath environment between 3 to 10 ℃, and can optionally pass into nitrogen or argon gas.In the time of with high-speed stirring, dropwise the titanium precursor thing is added in the deionized water with the speed of per second 1 to several, can obtain titanium precursor thing solution.In one embodiment, the titanium precursor thing is the titanium alkoxide, and wherein the alkyl in the titanium alkoxide may have 1 to 6 carbon atom.In another embodiment, the titanium precursor thing is titanium tetrachloride.Continued stir about 1 to 5 hour; Then under 4 to 15 ℃ temperature, leaving standstill 3 to 48 hours.To add in the deionized water as the ethylene glycol of interfacial agent, can obtain the interfacial activity agent solution.This interfacial activity agent solution is added in the above-mentioned titanium precursor thing solution again, and stirred 5 to 100 minutes, wherein the mole of titanium precursor thing/ethylene glycol ratio is 1: 3.In another embodiment, can make spent glycol oligomer or ethylene glycol polymer to replace ethylene glycol.The mixed solution that obtains is sealed with preservative film and aluminium-foil paper, put into temperature between 10 to 90 ℃ baking oven reaction 10 to 200 minutes; Then utilize and filter or centrifugal and so on mode is collected powder.With above-mentioned powder with washed with de-ionized water at least three times, to remove residual solvent; In addition dry with the baking oven of temperature between 60 to 500 ℃ again, thereby obtain how ground rice body of microspheroidal titanium dioxide of the present invention, it has uniform size, between 650 to 750nm.Fig. 1 (a) shows how sweep electron microscope (scanning electron microscope, the SEM) image of ground rice body of this microspheroidal titanium dioxide, and Fig. 2 shows its X-ray diffraction chart.
Change the mole ratio of titanium precursor thing and ethylene glycol, can change the how size of ground rice body of microspheroidal titanium dioxide.As shown in table 1.
Table 1
| Mole is than (titanium precursor thing/ethylene glycol) | Microspheroidal titanium dioxide is the size of ground rice body how | The SEM image |
| 1∶3 | 650 to 750nm | Fig. 1 (a) |
| 1∶5 | 550 to 650nm | Fig. 1 (b) |
| 1∶7 | 450 to 550nm | Fig. 1 (c) |
| 1∶9 | 300 to 400nm | Fig. 1 (d) |
How ground rice body 6g mixes with the acetic acid of 1mL with above-mentioned microspheroidal titanium dioxide, stirs three minutes; Add the deionized water of 5mL, stir and made it even mixing in 3 minutes; Then add 15mL ethanol, 20g Terpineol 350, and the 30g ethyl cellulose after, stir and made it Uniform Dispersion in 12 hours, namely finish the how preparation of Rice ﹠ peanut milk material of microspheroidal titanium dioxide.
By screen painting, how the Rice ﹠ peanut milk material is coated on the transparent conducting glass base material with aforesaid microspheroidal titanium dioxide, and utilizes high temperature sintering to remove organic substance, and sintering temperature is between 300 to 600 ℃, and sintering time is then between 1 to 5 hour; Then be cooled to room temperature, can form how rice film of microspheroidal titanium dioxide at base material, thickness is 1 to 10 micron, and it can be used in for example transparency electrode of solar cell.The hardness of this film is between the pencil hardness of 3B to 6H.Fig. 3 is the microspheroidal titanium dioxide sweep electron microscope image of rice film how that is disposed on the base material.
In each embodiment of the method for the present invention; the sequence number of described each step can not be used for limiting the sequencing of each step; for those of ordinary skills, under the prerequisite of not paying creative work, the priority of each step is changed also within protection scope of the present invention.
The above is preferred implementation of the present invention; should be pointed out that for those skilled in the art, under the prerequisite that does not break away from principle of the present invention; can also make some improvements and modifications, these improvements and modifications also should be considered as protection scope of the present invention.
Claims (8)
1. the microspheroidal titanium dioxide preparation method of ground rice body how is characterized in that, comprises the following steps:
(a) a titanium precursor thing is added in the deionized water, obtain a titanium precursor thing solution, with under the temperature of in 4 to 15 ℃ of this titanium precursor thing solution left standstills 3 to 48 hours;
(b) interfacial agent is added in the deionized water, obtain an interfacial activity agent solution, this interfacial agent is ethylene glycol;
(c) this interfacial activity agent solution is added in this titanium precursor thing solution, obtain a mixed solution;
(d) collect microspheroidal titanium dioxide ground rice body how in this mixed solution;
(e) how the ground rice body is in addition dry with this microspheroidal titanium dioxide.
2. the microspheroidal titanium dioxide according to claim 1 preparation method of ground rice body how is characterized in that, this titanium precursor thing is titanium tetrachloride.
3. the microspheroidal titanium dioxide according to claim 1 preparation method of ground rice body how is characterized in that, this titanium precursor thing is the titanium alkoxide.
4. the microspheroidal titanium dioxide according to claim 3 preparation method of ground rice body how is characterized in that, the alkyl of this titanium alkoxide has 1 to 6 carbon atom.
5. the microspheroidal titanium dioxide according to claim 1 preparation method of ground rice body how is characterized in that, step (a) is carried out under 3 to 10 ℃ temperature.
6. the microspheroidal titanium dioxide according to claim 1 preparation method of ground rice body how is characterized in that, step (a) is carried out under a rare gas element.
7. the microspheroidal titanium dioxide according to claim 6 preparation method of ground rice body how is characterized in that, this rare gas element is argon gas.
8. the microspheroidal titanium dioxide according to claim 1 preparation method of ground rice body how is characterized in that, this microspheroidal titanium dioxide how the size of ground rice body be along with the mole of this titanium precursor thing and this interfacial agent than and change.
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| Publication number | Priority date | Publication date | Assignee | Title |
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| CN1248550A (en) * | 1999-05-12 | 2000-03-29 | 中国科学院上海硅酸盐研究所 | Process for preparing titanic schorl phase titanium dioxide nanometer crystal under room temp. |
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| CN1248550A (en) * | 1999-05-12 | 2000-03-29 | 中国科学院上海硅酸盐研究所 | Process for preparing titanic schorl phase titanium dioxide nanometer crystal under room temp. |
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