CN104805503B - Ca-Ti ore type lead titanates/argentum nano composite material and preparation method thereof - Google Patents
Ca-Ti ore type lead titanates/argentum nano composite material and preparation method thereof Download PDFInfo
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- CN104805503B CN104805503B CN201510123312.6A CN201510123312A CN104805503B CN 104805503 B CN104805503 B CN 104805503B CN 201510123312 A CN201510123312 A CN 201510123312A CN 104805503 B CN104805503 B CN 104805503B
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- C—CHEMISTRY; METALLURGY
- C30—CRYSTAL GROWTH
- C30B—SINGLE-CRYSTAL GROWTH; UNIDIRECTIONAL SOLIDIFICATION OF EUTECTIC MATERIAL OR UNIDIRECTIONAL DEMIXING OF EUTECTOID MATERIAL; REFINING BY ZONE-MELTING OF MATERIAL; PRODUCTION OF A HOMOGENEOUS POLYCRYSTALLINE MATERIAL WITH DEFINED STRUCTURE; SINGLE CRYSTALS OR HOMOGENEOUS POLYCRYSTALLINE MATERIAL WITH DEFINED STRUCTURE; AFTER-TREATMENT OF SINGLE CRYSTALS OR A HOMOGENEOUS POLYCRYSTALLINE MATERIAL WITH DEFINED STRUCTURE; APPARATUS THEREFOR
- C30B29/00—Single crystals or homogeneous polycrystalline material with defined structure characterised by the material or by their shape
- C30B29/10—Inorganic compounds or compositions
- C30B29/16—Oxides
- C30B29/22—Complex oxides
- C30B29/32—Titanates; Germanates; Molybdates; Tungstates
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- C—CHEMISTRY; METALLURGY
- C30—CRYSTAL GROWTH
- C30B—SINGLE-CRYSTAL GROWTH; UNIDIRECTIONAL SOLIDIFICATION OF EUTECTIC MATERIAL OR UNIDIRECTIONAL DEMIXING OF EUTECTOID MATERIAL; REFINING BY ZONE-MELTING OF MATERIAL; PRODUCTION OF A HOMOGENEOUS POLYCRYSTALLINE MATERIAL WITH DEFINED STRUCTURE; SINGLE CRYSTALS OR HOMOGENEOUS POLYCRYSTALLINE MATERIAL WITH DEFINED STRUCTURE; AFTER-TREATMENT OF SINGLE CRYSTALS OR A HOMOGENEOUS POLYCRYSTALLINE MATERIAL WITH DEFINED STRUCTURE; APPARATUS THEREFOR
- C30B33/00—After-treatment of single crystals or homogeneous polycrystalline material with defined structure
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Abstract
The present invention relates to Ca-Ti ore type lead titanates/argentum nano composite material and preparation method thereof, the composite is made up of Ca-Ti ore type lead titanates single crystal nanoplate with the Nano silver grain for being deposited on Ca-Ti ore type lead titanates single crystal nanoplate one side.Prepared using Photodeposition, make silver nitrate solution in Ca-Ti ore type lead titanates single crystal nanoplate one side reduction deposition by controlling visible ray intensity of illumination and time, simultaneously, pH value in reaction is regulated and controled by ammoniacal liquor or acetic acid, control deposits the pattern of nano silver particles, obtains Ca-Ti ore type lead titanates/argentum nano composite material that loading nano silvery particle is graininess, sheet and cone.The composite can be effectively increased the utilization ratio of sunshine, be expected to be used for photolysis water hydrogen.
Description
Technical field
The present invention relates to Ca-Ti ore type lead titanates/argentum nano composite material and preparation method thereof, belong to inorganic non-metallic material
Material technical field.
Background technology
Titanium dioxide has superior catalysis activity, chemical stability and the photo-generate electron-hole for lasting a long time due to it
It is right, obtain most commonly used research in catalytic field.But, larger energy gap limits titanium dioxide to solar energy
Effectively utilize, and the rapid of photo-generate electron-hole pair is combined the catalytic efficiency that titanium dioxide has been had a strong impact on dorsad reaction.
For problem above, there has been proposed various solutions, such as adulterate to change the energy gap of titanium dioxide, increasing it can
See light utilization ratio；Supported precious metal nano-particle improves the separation of electron hole pair, reduces compound；Sacrifice agent is added to change
The utilization ratio in kind electronics or hole etc..But, can there are a serious problems when these materials are used for photocatalytic water, produce hydrogen
Position with product oxygen is random distribution, this considerably increases the probability for dorsad reacting, seriously limits the efficiency of photocatalytic water.Separately
Outward, the material that can simultaneously improve problem existing for titanium dioxide is also rare at present.
Perovskite-type material and its composite are due to excellent chemical stability and adjustable energy gap, hence it is evident that increase
Effective utilization of sunshine is added, has been catalyzed in photovoltaic cell, organic pollution in recent years and photolysis water hydrogen field is subject to extensive
Concern.Ca-Ti ore type lead titanates has stronger spontaneous polarization due to it, so as to show excellent piezoelectricity, ferroelectric properties.It is expensive
Metal nanoparticle either as plasma enhancing body still as the carrier of composite, due to its special electronics shape
State, considerable influence is had been achieved with characterization method and catalytic field.
Therefore research noble metal has important directive significance with the interaction of the Ca-Ti ore type lead titanates of monocrystalline single domain.
The content of the invention
It is an object of the invention to provide a kind of Ca-Ti ore type lead titanates/Yin Na for being conducive to increasing sun light utilization ratio
Nano composite material and preparation method thereof.
Ca-Ti ore type lead titanates/argentum nano composite material of the invention is by Ca-Ti ore type lead titanates single crystal nanoplate and deposition
Constituted in the Nano silver grain of Ca-Ti ore type lead titanates single crystal nanoplate one side.
The preparation method of Ca-Ti ore type lead titanates/argentum nano composite material of the invention, comprises the following steps：
1）1 ~ 1.5mmol Ca-Ti ore type lead titanates single crystal nanoplates are added in 40 ~ 50mL deionized waters, stirring is obtained
Suspension；
2）Under dark room conditions, in step（1）Ammoniacal liquor or acetic acid are added dropwise in gained suspension, make its pH=3 ~ 12, sealing stirring
After 12 ~ 18h, silver nitrate solution is added, make lead titanates be 10 with the mol ratio of silver nitrate：3~2：1, continue in darkroom stirring 2 ~
8h；
3）By step（2）Gained suspension is placed under the xenon lamp of wavelength X ＞ 400nm, and stirring carries out light deposition reaction, xenon lamp
The distance of bottom and suspension be 10 ~ 12cm, it is 20 ~ 22A, illumination reaction 1h that xenon lamp electric current is adjusted first, then adjusts xenon
Lamp current is 12 ~ 15A, illumination reaction 4h；
4）By step（3）Products therefrom uses deionized water and absolute ethanol washing successively, and drying is incubated at 60 ~ 75 DEG C,
Obtain Ca-Ti ore type lead titanates/argentum nano composite material.
In the present invention, described Ca-Ti ore type lead titanates single crystal nanoplate can use the A of CN 103898607,《A kind of calcium titanium
The preparation method of ore deposit type lead titanate monocrystal nano piece》Disclosed method is obtained.
In the present invention, described ammoniacal liquor, acetic acid are that chemistry is pure, and silver nitrate is pure for analysis.
The present invention is prepared for loading the Ca-Ti ore type metatitanic acid of graininess, sheet and conical silver particles by Photodeposition
Lead/argentum nano composite material.Make silver nitrate solution in Ca-Ti ore type lead titanates list by controlling visible ray intensity of illumination and time
There is reduction deposition in the one side of brilliant nanometer sheet, meanwhile, the pH value of reaction is regulated and controled by ammoniacal liquor or acetic acid, control deposits Nano Silver
The pattern of particle.
Because Ca-Ti ore type lead titanates single crystal nanoplate has one-domain structure and stronger spontaneous polarization, can efficiently separate
Photo-generate electron-hole pair, in Ca-Ti ore type lead titanates single crystal nanoplate single sided deposition graininess, sheet, conical nanometer silver granuel
Son, it is possible to achieve produce hydrogen and produce the segmentation in oxygen region, so as to reduce dorsad react.Therefore, Ca-Ti ore type lead titanates of the invention/
Argentum nano composite material can increase the utilization ratio of sunshine, be expected to be used for photolysis water hydrogen.
Preparation method of the present invention is easy to operate, with low cost, and the pattern for loading silver has controllability.
Brief description of the drawings
The SEM photograph of Ca-Ti ore type lead titanates/argentum nano composite material when Fig. 1 is pH=12；
The SEM photograph of Ca-Ti ore type lead titanates/argentum nano composite material when Fig. 2 is pH=10；
The SEM photograph of Ca-Ti ore type lead titanates/argentum nano composite material when Fig. 3 is pH=5.
Specific embodiment
The inventive method is further illustrated with reference to embodiments.
Embodiment 1
1）1.2mmol Ca-Ti ore type lead titanates single crystal nanoplates are added in 45mL deionized waters, stirring obtains suspended
Liquid；
2）Under dark room conditions, in step（1）Ammoniacal liquor is added dropwise in gained suspension, makes its pH=12, after sealing stirring 18h, plus
Enter the silver nitrate solution of 15mL, 40mmol/L, 8h is stirred in continuation in darkroom；
3）By step（2）Gained suspension is placed under the xenon lamp of wavelength X ＞ 400nm, and stirring carries out light deposition reaction, xenon lamp
The distance of bottom and suspension be 10cm, it is 22A, illumination reaction 1h that xenon lamp electric current is adjusted first, then adjusts xenon lamp electric current
It is 12A, illumination reaction 4h；
4）By step（3）Products therefrom is washed with deionized 3 times, then with absolute ethanol washing 1 time, is incubated at 60 DEG C
Drying, obtains Ca-Ti ore type lead titanates/argentum nano composite material.Ca-Ti ore type lead titanates nanometer monocrystalline is supported on obtained in this example
The Nano silver grain of piece one side is in cone（See Fig. 1）.
Embodiment 2
1）1mmol Ca-Ti ore type lead titanates single crystal nanoplates are added in 50mL deionized waters, stirring obtains suspension；
2）Under dark room conditions, in step（1）Ammoniacal liquor is added dropwise in gained suspension, makes its pH=10, after sealing stirring 12h, plus
Enter the silver nitrate solution of 10mL, 40mmol/L, 2h is stirred in continuation in darkroom；
3）By step（2）Gained suspension is placed under the xenon lamp of wavelength X ＞ 400nm, and stirring carries out light deposition reaction, xenon lamp
The distance of bottom and suspension be 11cm, it is 22A, illumination reaction 1h that xenon lamp electric current is adjusted first, then adjusts xenon lamp electric current
It is 15A, illumination reaction 4h；
4）By step（3）Products therefrom is washed with deionized 3 times, then with absolute ethanol washing 1 time, is incubated at 70 DEG C
Drying, obtains Ca-Ti ore type lead titanates/argentum nano composite material, and Ca-Ti ore type lead titanates nanometer monocrystalline is supported on obtained in this example
The Nano silver grain of piece one side is in the form of sheets（See Fig. 2）.
Embodiment 3
1）1.5mmol Ca-Ti ore type lead titanates single crystal nanoplates are added in 40mL deionized waters, stirring obtains suspended
Liquid；
2）Under dark room conditions, in step（1）Ammoniacal liquor is added dropwise in gained suspension, makes its pH=5, after sealing stirring 15h, plus
Enter the silver nitrate solution of 18mL, 40mmol/L, 5h is stirred in continuation in darkroom；
3）By step（2）Gained suspension is placed under the xenon lamp of wavelength X ＞ 400nm, and stirring carries out light deposition reaction, xenon lamp
The distance of bottom and suspension be 10cm, it is 20A, illumination reaction 1h that xenon lamp electric current is adjusted first, then adjusts xenon lamp electric current
It is 15A, illumination reaction 4h；
4）By step（3）Products therefrom is washed with deionized 4 times, then with absolute ethanol washing 2 times, is incubated at 75 DEG C
Drying, obtains Ca-Ti ore type lead titanates/argentum nano composite material, and Ca-Ti ore type lead titanates nanometer monocrystalline is supported on obtained in this example
The Nano silver grain of piece one side is in granular form（See Fig. 3）.
Claims (2)
1. the method for preparing Ca-Ti ore type lead titanates/argentum nano composite material, the composite is by Ca-Ti ore type lead titanates list
Brilliant nanometer sheet and the Nano silver grain composition for being deposited on Ca-Ti ore type lead titanates single crystal nanoplate one side, its preparation include following step
Suddenly：
1）1 ~ 1.5mmol Ca-Ti ore type lead titanates single crystal nanoplates are added in 40 ~ 50mL deionized waters, stirring obtains suspended
Liquid；
2）Under dark room conditions, in step（1）Ammoniacal liquor or acetic acid are added dropwise in gained suspension, make its pH=3 ~ 12, sealing stirring 12 ~
After 18h, silver nitrate solution is added, make lead titanates be 10 with the mol ratio of silver nitrate：3~2：1, continue to stir 2 ~ 8h in darkroom；
3）By step（2）Gained suspension is placed under the xenon lamp of wavelength X ＞ 400nm, and stirring carries out light deposition reaction, the bottom of xenon lamp
Portion is 10 ~ 12cm with the distance of suspension, and it is 20 ~ 22A, illumination reaction 1h that xenon lamp electric current is adjusted first, then adjusts xenon lamp electricity
It is 12 ~ 15A to flow, illumination reaction 4h；
4）By step（3）Products therefrom uses deionized water and absolute ethanol washing successively, and drying is incubated at 60 ~ 75 DEG C, obtains
Ca-Ti ore type lead titanates/argentum nano composite material.
2. the preparation method of Ca-Ti ore type lead titanates/argentum nano composite material according to claim 1, it is characterized in that described
Ammoniacal liquor, acetic acid be chemistry it is pure, silver nitrate for analysis it is pure.
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Families Citing this family (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN105215374A (en) * | 2015-10-16 | 2016-01-06 | 浙江大学 | The preparation method of silver/lead titanates nano composite material |
| CN105289604B (en) * | 2015-10-16 | 2017-11-07 | 浙江大学 | A kind of preparation method of silver oxide/lead titanates nano composite material |
| CN105731531B (en) * | 2016-01-11 | 2017-07-14 | 浙江大学 | A kind of lead titanates nanometer sheet and the preparation method of nano platinum particle composite |
| CN107999053B (en) * | 2017-11-06 | 2020-06-16 | 哈尔滨理工大学 | Lead lanthanum titanate/bismuth vanadate and preparation method thereof |
| CN114062445B (en) * | 2021-11-12 | 2023-03-03 | 福州大学 | Preparation method of nano-silver surface modified two-dimensional lead titanate material for high-sensitivity ammonia sensing at room temperature |
Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN103007932A (en) * | 2012-12-11 | 2013-04-03 | 山东大学 | Method for preparing titanium dioxide nanobelt load thermometal integral catalyst |
| CN103898607A (en) * | 2014-03-28 | 2014-07-02 | 浙江大学 | Preparation method of perovskite type lead titanate monocrystal nanosheet |
| CN104117355A (en) * | 2014-07-14 | 2014-10-29 | 王丹军 | A bismuth tungstate photocatalyst surface-modified by nanometer silver and a preparing method thereof |
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2015
- 2015-03-20 CN CN201510123312.6A patent/CN104805503B/en active Active
Patent Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN103007932A (en) * | 2012-12-11 | 2013-04-03 | 山东大学 | Method for preparing titanium dioxide nanobelt load thermometal integral catalyst |
| CN103898607A (en) * | 2014-03-28 | 2014-07-02 | 浙江大学 | Preparation method of perovskite type lead titanate monocrystal nanosheet |
| CN104117355A (en) * | 2014-07-14 | 2014-10-29 | 王丹军 | A bismuth tungstate photocatalyst surface-modified by nanometer silver and a preparing method thereof |
Non-Patent Citations (2)
| Title |
|---|
| Effects of Particle Surface Areas and Microstructures on Photocatalytic H2 and O2 Production over PbTiO3;David Arney,et al.;《J. Am. Ceram. Soc.》;20110531;第94卷(第5期);第1483-1489页 * |
| Pb(ZrxTi1-x)O3铁电薄膜光阴极光还原Ag+及其光电化学特性;张漫;《中国优秀硕士学位论文全文数据库（基础科学辑）》;20150115(第1期);第A005-193页 * |
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