CN106892452B - A kind of Ti4O7/Sn5O6The preparation method of composite material - Google Patents
A kind of Ti4O7/Sn5O6The preparation method of composite material Download PDFInfo
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- CN106892452B CN106892452B CN201710030299.9A CN201710030299A CN106892452B CN 106892452 B CN106892452 B CN 106892452B CN 201710030299 A CN201710030299 A CN 201710030299A CN 106892452 B CN106892452 B CN 106892452B
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- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01G—COMPOUNDS CONTAINING METALS NOT COVERED BY SUBCLASSES C01D OR C01F
- C01G23/00—Compounds of titanium
- C01G23/04—Oxides; Hydroxides
- C01G23/043—Titanium sub-oxides
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- C01P2002/00—Crystal-structural characteristics
- C01P2002/70—Crystal-structural characteristics defined by measured X-ray, neutron or electron diffraction data
- C01P2002/72—Crystal-structural characteristics defined by measured X-ray, neutron or electron diffraction data by d-values or two theta-values, e.g. as X-ray diagram
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- C01P—INDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS
- C01P2004/00—Particle morphology
- C01P2004/01—Particle morphology depicted by an image
- C01P2004/03—Particle morphology depicted by an image obtained by SEM
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Abstract
The invention discloses a kind of Ti4O7/Sn5O6The preparation method of composite material, this method include：1) by SnCl4·5H2O is dissolved in deionized water, is stirred evenly, and obtains SnCl4Solution；2) by Ti4O7Powder disperses in glacial acetic acid, and magnetic agitation, obtains Ti4O7Dispersion liquid；3) under magnetic stirring, by SnCl4Solution is added to Ti4O7In dispersion liquid, stir evenly, obtain mixed liquor；4) gained mixed liquor is subjected to hydro-thermal reaction, reaction temperature is 170~190 DEG C, and the reaction time is 16~32h；5) product is taken out after question response, and is washed with ethanol, is then dried in vacuo, drying temperature is 60~90 DEG C, and drying time is 4~8h, obtains Ti4O7/Sn5O6Composite material.The composite material has excellent visible near-infrared wave band absorbing properties, is expected to be applied to photoelectricity (chemistry) fields such as photocatalysis, solar cell.
Description
Technical field
The present invention relates to the preparing technical field of non-stoichiometric oxide composite material.More particularly, to one kind
Ti4O7/Sn5O6The preparation method of composite material.
Background technology
TiOxIt is a series of Magneli phases titanium oxides, this material electronics energy gap is narrow, strong to sun light absorpting ability,
In black-and-blue；Magneli phases TiOxConduct electricity very well, wherein Ti4O7Electric conductivity it is optimal, its monocrystalline electrical conductivity reaches 1500S
cm-1；Ti4O7Surface Lacking oxygen enriches, and adsorption capacity is strong and chemical property is stablized, and is the extraordinary active electrode material of blackness.
Sn5O6Band gap is 2.42eV, is a kind of very promising Van der Waals material.Therefore, how by Ti4O7And Sn5O6It is compound, so as to obtain
Obtaining comprehensive performance includes the more preferable Ti of absorbing properties4O7/Sn5O6Composite material has prominent practical value.But in existing skill
Fail to prepare pure Sn in art5O6And its composite material, the only related SnO with stoichiometric ratio2And TiO2/SnO2It is multiple
Condensation material.
It is true based on more than, it is desirable to provide a kind of Ti4O7/Sn5O6The preparation method of composite material, to make up Ti4O7/
Sn5O6The blank of field of compound material.
The content of the invention
First purpose of the present invention is to provide a kind of Ti4O7/Sn5O6The preparation method of composite material.It is first in the present invention
It is secondary to have synthesized successfully non-stoichiometric Ti4O7/Sn5O6Composite material, and the composite material compares Ti4O7With stronger near red
Outer absorbing properties.
Second object of the present invention is to provide a kind of Ti being prepared by above-mentioned preparation method4O7/Sn5O6It is compound
Material.
To reach above-mentioned first purpose, the present invention uses following technical proposals：
A kind of Ti4O7/Sn5O6The preparation method of composite material, this method comprises the following steps：
1) by SnCl4·5H2O is dissolved in deionized water, is stirred evenly, and obtains SnCl4Solution；
2) by Ti4O7Powder disperses in glacial acetic acid, and magnetic agitation, obtains Ti4O7Dispersion liquid；
3) under magnetic stirring, by the prepared SnCl of step 1)4Solution is added to the Ti that step 2) obtains4O7Dispersion liquid
In, stir evenly, obtain mixed liquor；
4) mixed liquor obtained by step 3) is subjected to hydro-thermal reaction, reaction temperature is 170~190 DEG C, the reaction time for 16~
32h；
5) product is taken out after question response, and is washed with ethanol, is then dried in vacuo, drying temperature is 60~90 DEG C,
Drying time is 4~8h, obtains Ti4O7/Sn5O6Composite material.
Embodiment according to the present invention, in step 1), the SnCl4·5H2The addition of O for 0.1~
1mmol, the addition of deionized water is 4~8mL.
Preferred embodiment according to the present invention, in step 1), the addition of the deionized water is 5mL.
Embodiment according to the present invention, in step 2), the Ti4O7The addition of powder for 0.8~
1.2mmol, the addition of glacial acetic acid is 20~30mL.
Preferred embodiment according to the present invention, in step 2), the Ti4O7The addition of powder is 1mmol, ice
The addition of acetic acid is 20~25mL.
Preferred embodiment according to the present invention, in step 4), the reaction temperature is 180~185 DEG C, instead
It is 20~24h between seasonable.
More preferably embodiment according to the present invention, in step 4), the reaction temperature is 180 DEG C, during reaction
Between be 24h.
Preferred embodiment according to the present invention, in step 5), the drying temperature is 60~65 DEG C, when dry
Between be 6~8h.
More preferably embodiment according to the present invention, in step 5), the drying temperature is 60 DEG C, drying time
For 8h.
Preferred embodiment according to the present invention, in step 5), the number of the ethanol washing is three times.
To reach above-mentioned second purpose, the present invention provides the Ti that above-mentioned preparation method is prepared4O7/Sn5O6It is compound
Material.
The Ti4O7/Sn5O6Composite material compares Ti4O7With improved near infrared light absorbance, it can be achieved that to it is visible-
The absorption and utilization of near infrared light, are expected to be applied to photoelectricity (chemistry) fields such as photocatalysis, solar cell.
Unless otherwise specified, each raw material used in the present invention can be by commercially available commercially available.In addition, the preparation side of the present invention
The process and device therefor being not specifically mentioned in method can use the conventional equipment in fields or showing with reference to fields
There is technology progress.
Beneficial effects of the present invention are as follows：
In the present invention, by the selection to raw material, SnCl is selected4·5H2O and Ti4O7For raw material, in hydrothermal reaction process
In, creative utilizes Ti4O7Reproducibility, and the further restriction to process conditions, such as SnCl4·5H2O and Ti4O7Add
The stringent control of amount, hydrothermal temperature and time etc., and the selection of dispersion liquid dispersant, so as to successfully be prepared first
Non-stoichiometric Ti4O7/Sn5O6Composite material, and the composite material has excellent near-infrared absorption performance, being expected to should
For the photoelectricity such as photocatalysis, solar cell (chemistry) field.
Brief description of the drawings
The embodiment of the present invention is described in further detail below in conjunction with the accompanying drawings.
Fig. 1 shows the Ti that the embodiment of the present invention 1 is prepared4O7/Sn5O6The scanning electron microscope (SEM) photograph of composite material.
Fig. 2 shows the Ti that the embodiment of the present invention 1 is prepared4O7/Sn5O6The XRD spectra of composite material.
Fig. 3 shows the Ti that the embodiment of the present invention 1 is prepared4O7/Sn5O6The abosrption spectrogram of composite material.
Embodiment
In order to illustrate more clearly of the present invention, the present invention is done further with reference to preferred embodiments and drawings
It is bright.Similar component is indicated with identical reference numeral in attached drawing.It will be appreciated by those skilled in the art that institute is specific below
The content of description is illustrative and be not restrictive, and should not be limited the scope of the invention with this.
Embodiment 1
A kind of Ti4O7/Sn5O6The preparation method of composite material, includes the following steps：
1) SnCl of 0.24mmol is taken4·5H2O is dissolved in 5mL deionized waters, is stirred evenly, and obtains SnCl4Solution；
2) 1mmolTi is taken4O7Powder is dispersed in 25mL glacial acetic acid, and magnetic agitation is uniform, obtains Ti4O7Dispersion liquid；
3) under conditions of magnetic agitation, by the prepared SnCl of step 1)4Solution is added to the Ti that step 2) obtains4O7
In dispersion liquid, stir evenly, obtain mixed liquor；
4) mixed liquor obtained by step 3) being placed in reaction kettle, carries out hydro-thermal reaction, the temperature of hydro-thermal reaction is 180 DEG C,
Reaction time is 24h；
5) product is taken out after question response, and is washed repeatedly three times with ethanol, then vacuum is done in vacuum drying chamber
Dry, drying temperature is 60 DEG C, and drying time 8h, obtains Ti4O7/Sn5O6Composite material.
The Ti being prepared4O7/Sn5O6The scanning electron microscope (SEM) photograph of composite material is as shown in Figure 1.
The Ti being prepared4O7/Sn5O6The XRD spectra of composite material is as shown in Figure 2.As can be known from Fig. 2, the composite material
In contain Ti4O7Phase and Sn5O6Phase.
The Ti being prepared4O7/Sn5O6The abosrption spectrogram of composite material is as shown in Figure 3.As can be known from Fig. 3, this implementation
For composite material in example in the range of 800nm wavelengths above, absorbance is better than pure Ti4O7Absorbance in this wave-length coverage.
Embodiment 2
A kind of Ti4O7/Sn5O6The preparation method of composite material, includes the following steps：
1) SnCl of 0.4mmol is taken4·5H2O is dissolved in 5mL deionized waters, is stirred evenly, and obtains SnCl4Solution；
2) 0.8mmolTi is taken4O7Powder is dispersed in 25mL glacial acetic acid, and magnetic agitation is uniform, obtains Ti4O7Dispersion liquid；
3) under conditions of magnetic agitation, by the prepared SnCl of step 1)4Solution is added to the Ti that step 2) obtains4O7
In dispersion liquid, stir evenly, obtain mixed liquor；
4) mixed liquor obtained by step 3) being placed in reaction kettle, carries out hydro-thermal reaction, the temperature of hydro-thermal reaction is 180 DEG C,
Reaction time is 24h；
5) product is taken out after question response, and is washed repeatedly three times with ethanol, then vacuum is done in vacuum drying chamber
Dry, drying temperature is 70 DEG C, and drying time 7h, obtains Ti4O7/Sn5O6Composite material.The pattern of gained composite material, phase group
Into and absorbing properties it is close with embodiment 1.
Obviously, the above embodiment of the present invention is only intended to clearly illustrate example of the present invention, and is not pair
The restriction of embodiments of the present invention, for those of ordinary skill in the field, may be used also on the basis of the above description
To make other variations or changes in different ways, all embodiments can not be exhaustive here, it is every to belong to this hair
Row of the obvious changes or variations that bright technical solution is extended out still in protection scope of the present invention.
Claims (5)
- A kind of 1. Ti4O7/Sn5O6The preparation method of composite material, it is characterised in that this method comprises the following steps：1) by SnCl4·5H2O is dissolved in deionized water, is stirred evenly, and obtains SnCl4Solution；2) by Ti4O7Powder disperses in glacial acetic acid, and magnetic agitation, obtains Ti4O7Dispersion liquid；3) under magnetic stirring, by the prepared SnCl of step 1)4Solution is added to the Ti that step 2) obtains4O7In dispersion liquid, stir Mix uniformly, obtain mixed liquor；4) mixed liquor obtained by step 3) is subjected to hydro-thermal reaction, reaction temperature is 170~190 DEG C, and the reaction time is 16~32h；5) product is taken out after question response, and is washed with ethanol, is then dried in vacuo, drying temperature is 60~90 DEG C, dry Time is 4~8h, obtains Ti4O7/Sn5O6Composite material；In step 1), the SnCl4·5H2The addition of O is 0.1~1mmol, and the addition of deionized water is 4~8mL；In step 2), the Ti4O7The addition of powder is 0.8~1.2mmol, and the addition of glacial acetic acid is 20~30mL.
- 2. preparation method according to claim 1, it is characterised in that in step 2), the Ti4O7The addition of powder is 1mmol, the addition of glacial acetic acid is 20~25mL.
- 3. preparation method according to claim 1, it is characterised in that in step 4), the reaction temperature for 180~ 185 DEG C, the reaction time is 20~24h.
- 4. preparation method according to claim 1, it is characterised in that in step 5), the drying temperature is 60~65 DEG C, drying time is 6~8h.
- 5. the Ti being prepared such as Claims 1 to 4 any one of them preparation method4O7/Sn5O6Composite material.
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Citations (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101773853A (en) * | 2009-01-14 | 2010-07-14 | 中国科学院大连化学物理研究所 | Non-supported catalyst pulp, preparation method and application thereof |
| CN104556210A (en) * | 2015-01-19 | 2015-04-29 | 陕西科技大学 | Method for preparing Sm2Sn2O7/SnO2 nano composite by microwave-assisted solvothermal two-step process |
| CN104556209A (en) * | 2015-01-09 | 2015-04-29 | 太原理工大学 | Preparation method for spherical tin dioxide self-assembled from nano-fragments |
| CN105417572A (en) * | 2015-11-09 | 2016-03-23 | 上海纳米技术及应用国家工程研究中心有限公司 | Method for preparing p-n type SnO2/CuO composite microspheres |
Family Cites Families (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| KR101548190B1 (en) * | 2013-08-19 | 2015-08-31 | 한국에너지기술연구원 | Metal complex of fluorinated tin oxide and titanium oxide and preparation method thereof |
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Patent Citations (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101773853A (en) * | 2009-01-14 | 2010-07-14 | 中国科学院大连化学物理研究所 | Non-supported catalyst pulp, preparation method and application thereof |
| CN104556209A (en) * | 2015-01-09 | 2015-04-29 | 太原理工大学 | Preparation method for spherical tin dioxide self-assembled from nano-fragments |
| CN104556210A (en) * | 2015-01-19 | 2015-04-29 | 陕西科技大学 | Method for preparing Sm2Sn2O7/SnO2 nano composite by microwave-assisted solvothermal two-step process |
| CN105417572A (en) * | 2015-11-09 | 2016-03-23 | 上海纳米技术及应用国家工程研究中心有限公司 | Method for preparing p-n type SnO2/CuO composite microspheres |
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