CN104805503A - Perovskite type lead titanate/silver nanocomposite and preparation method thereof - Google Patents
Perovskite type lead titanate/silver nanocomposite and preparation method thereof Download PDFInfo
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- CN104805503A CN104805503A CN201510123312.6A CN201510123312A CN104805503A CN 104805503 A CN104805503 A CN 104805503A CN 201510123312 A CN201510123312 A CN 201510123312A CN 104805503 A CN104805503 A CN 104805503A
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- lead titanate
- perovskite typed
- xenon lamp
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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
Abstract
The invention relates to a perovskite type lead titanate/silver nanocomposite and a preparation method thereof. The composite comprises a perovskite type lead titanate monocrystal nanosheet and silver nanoparticles deposited on one side of the perovskite type lead titanate monocrystal nanosheet. The nanocomposite is prepared with a photodeposition method, a silver nitrate solution is subjected to reduction deposition on one side of the perovskite type lead titanate monocrystal nanosheet by controlling illumination intensity and time of visible light, meanwhile, the pH value of a reaction is regulated by ammonium hydroxide or acetic acid, shapes of the deposited silver nanoparticles are controlled, and the perovskite type lead titanate/silver nanocomposite loaded with the granular, flaky and conical silver nanoparticles is obtained. The composite can effectively increase the utilization efficiency of sunlight and is expected to be used for hydrogen production through photocatalytic water splitting.
Description
Technical field
The present invention relates to perovskite typed lead titanate/argentum nano composite material and preparation method thereof, belong to technical field of inorganic nonmetallic materials.
Background technology
Titanium dioxide has superior catalytic activity due to it, and chemical stability and life-span longer photo-generate electron-hole pair, obtain at catalytic field and study the most widely.But larger energy gap limits the effective utilization of titanium dioxide to sun power, and the right rapid compound of photo-generate electron-hole and dorsad reaction had a strong impact on the catalytic efficiency of titanium dioxide.For above problem, there has been proposed multiple solution, such as doping changes the energy gap of titanium dioxide, increases its visible ray utilising efficiency; Supported precious metal nano-particle improves the separation of electron-hole pair, reduces compound; Add sacrifice agent to improve utilising efficiency of electronics or hole etc.But can there are serious problems when these materials are used for photocatalytic water, the position of producing hydrogen and product oxygen is stochastic distribution, this considerably increases the probability reacted dorsad, seriously limits the efficiency of photocatalytic water.In addition, the material that simultaneously can improve problem existing for titanium dioxide is also rare at present.
Perovskite-type material and matrix material thereof, owing to having excellent chemical stability and adjustable energy gap, significantly increase effective utilization of sunlight, are subject to extensive concern in recent years in photovoltaic cell, organic pollutant catalysis and photolysis water hydrogen field.Perovskite typed lead titanate has stronger spontaneous polarization due to it, thus shows excellent piezoelectricity, ferroelectric properties.No matter noble metal nano particles is as plasma enhancing body or the carrier as matrix material, due to the electronic state that it is special, obtain considerable influence at characterization method and catalytic field.
Therefore the interaction studying the perovskite typed lead titanate of precious metal and monocrystalline single domain has important directive significance.
Summary of the invention
The object of the present invention is to provide and be a kind ofly conducive to perovskite typed lead titanate/argentum nano composite material increasing sunlight utilising efficiency and preparation method thereof.
Perovskite typed lead titanate/argentum nano composite material of the present invention is made up of perovskite typed lead titanate single crystal nanoplate and the Nano silver grain being deposited on perovskite typed lead titanate single crystal nanoplate one side.
The preparation method of perovskite typed lead titanate/argentum nano composite material of the present invention, comprises the following steps:
1) 1 ~ 1.5mmol perovskite typed lead titanate single crystal nanoplate is joined in 40 ~ 50mL deionized water, stir and obtain suspension liquid;
2) under dark room conditions, drip ammoniacal liquor or acetic acid, make its pH=3 ~ 12 in step (1) gained suspension liquid, after sealing stirring 12 ~ 18h, add silver nitrate solution, the mol ratio making lead titanate and Silver Nitrate is 10:3 ~ 2:1, continues to stir 2 ~ 8h in darkroom;
3) under step (2) gained suspension liquid being placed in the xenon lamp of wavelength X > 400nm, light deposition reaction is carried out in stirring, the bottom of xenon lamp and the distance of suspension liquid are 10 ~ 12cm, first xenon lamp electric current is regulated to be 20 ~ 22A, illumination reaction 1h, then xenon lamp electric current is regulated to be 12 ~ 15A, illumination reaction 4h;
4) step (3) products therefrom is used deionized water and absolute ethanol washing successively, at 60 ~ 75 DEG C, insulation is dried, and obtains perovskite typed lead titanate/argentum nano composite material.
In the present invention, described perovskite typed lead titanate single crystal nanoplate can adopt CN 103898607 A, and a kind of " preparation method of perovskite typed lead titanate single crystal nanoplate " disclosed method obtains.
In the present invention, described ammoniacal liquor, acetic acid are chemical pure, and Silver Nitrate is analytical pure.
The present invention has prepared the perovskite typed lead titanate/argentum nano composite material of loaded particle shape, sheet and conical silver particles by Photodeposition.By control visible ray intensity of illumination and time chien shih silver nitrate solution there is reduction deposition in the one side of perovskite typed lead titanate single crystal nanoplate, meanwhile, by the pH value of ammoniacal liquor or acetic acid regulation and control reaction, control the pattern of institute's depositing nano silver particles.
Because perovskite typed lead titanate single crystal nanoplate has one-domain structure and stronger spontaneous polarization, can effectively be separated photoproduction electron-hole pair, at perovskite typed lead titanate single crystal nanoplate single sided deposition particulate state, sheet, conical nano silver particles, can realize the segmentation of producing hydrogen and producing oxygen region, thus minimizing is reacted dorsad.Therefore, perovskite typed lead titanate/argentum nano composite material of the present invention can increase the utilising efficiency of sunlight, is expected to for photolysis water hydrogen.
Preparation method of the present invention is easy and simple to handle, with low cost, and the pattern of load silver has controllability.
Accompanying drawing explanation
The SEM photo of perovskite typed lead titanate/argentum nano composite material when Fig. 1 is pH=12;
The SEM photo of perovskite typed lead titanate/argentum nano composite material when Fig. 2 is pH=10;
The SEM photo of perovskite typed lead titanate/argentum nano composite material when Fig. 3 is pH=5.
Embodiment
The inventive method is further illustrated below in conjunction with embodiment.
Embodiment 1
1) 1.2mmol perovskite typed lead titanate single crystal nanoplate is joined in 45mL deionized water, stir and obtain suspension liquid;
2) under dark room conditions, drip ammoniacal liquor, make its pH=12 in step (1) gained suspension liquid, sealing adds the silver nitrate solution of 15mL, 40mmol/L, continues to stir 8h in darkroom after stirring 18h;
3) under step (2) gained suspension liquid being placed in the xenon lamp of wavelength X > 400nm, light deposition reaction is carried out in stirring, the bottom of xenon lamp and the distance of suspension liquid are 10cm, first xenon lamp electric current is regulated to be 22A, illumination reaction 1h, then xenon lamp electric current is regulated to be 12A, illumination reaction 4h;
4) by step (3) products therefrom deionized water wash 3 times, then use absolute ethanol washing 1 time, at 60 DEG C, insulation is dried, and obtains perovskite typed lead titanate/argentum nano composite material.The load that this example obtains is in the Nano silver grain conically (see figure 1) of perovskite typed lead titanate single crystal nanoplate one side.
Embodiment 2
1) 1mmol perovskite typed lead titanate single crystal nanoplate is joined in 50mL deionized water, stir and obtain suspension liquid;
2) under dark room conditions, drip ammoniacal liquor, make its pH=10 in step (1) gained suspension liquid, sealing adds the silver nitrate solution of 10mL, 40mmol/L, continues to stir 2h in darkroom after stirring 12h;
3) under step (2) gained suspension liquid being placed in the xenon lamp of wavelength X > 400nm, light deposition reaction is carried out in stirring, the bottom of xenon lamp and the distance of suspension liquid are 11cm, first xenon lamp electric current is regulated to be 22A, illumination reaction 1h, then xenon lamp electric current is regulated to be 15A, illumination reaction 4h;
4) by step (3) products therefrom deionized water wash 3 times, use absolute ethanol washing again 1 time, at 70 DEG C, insulation is dried, obtain perovskite typed lead titanate/argentum nano composite material, the load that this example obtains is in the Nano silver grain (see figure 2) in the form of sheets of perovskite typed lead titanate single crystal nanoplate one side.
Embodiment 3
1) 1.5mmol perovskite typed lead titanate single crystal nanoplate is joined in 40mL deionized water, stir and obtain suspension liquid;
2) under dark room conditions, drip ammoniacal liquor, make its pH=5 in step (1) gained suspension liquid, sealing adds the silver nitrate solution of 18mL, 40mmol/L, continues to stir 5h in darkroom after stirring 15h;
3) under step (2) gained suspension liquid being placed in the xenon lamp of wavelength X > 400nm, light deposition reaction is carried out in stirring, the bottom of xenon lamp and the distance of suspension liquid are 10cm, first xenon lamp electric current is regulated to be 20A, illumination reaction 1h, then xenon lamp electric current is regulated to be 15A, illumination reaction 4h;
4) by step (3) products therefrom deionized water wash 4 times, use absolute ethanol washing again 2 times, at 75 DEG C, insulation is dried, obtain perovskite typed lead titanate/argentum nano composite material, the load that this example obtains is particulate state (see figure 3) at the Nano silver grain of perovskite typed lead titanate single crystal nanoplate one side.
Claims (3)
1. perovskite typed lead titanate/argentum nano composite material, is characterized in that being made up of perovskite typed lead titanate single crystal nanoplate and the Nano silver grain being deposited on perovskite typed lead titanate single crystal nanoplate one side.
2. prepare the method for perovskite typed lead titanate/argentum nano composite material according to claim 1, comprise the following steps:
1) 1 ~ 1.5mmol perovskite typed lead titanate single crystal nanoplate is joined in 40 ~ 50mL deionized water, stir and obtain suspension liquid;
2) under dark room conditions, drip ammoniacal liquor or acetic acid, make its pH=3 ~ 12 in step (1) gained suspension liquid, after sealing stirring 12 ~ 18h, add silver nitrate solution, the mol ratio making lead titanate and Silver Nitrate is 10:3 ~ 2:1, continues to stir 2 ~ 8h in darkroom;
3) under step (2) gained suspension liquid being placed in the xenon lamp of wavelength X > 400nm, light deposition reaction is carried out in stirring, the bottom of xenon lamp and the distance of suspension liquid are 10 ~ 12cm, first xenon lamp electric current is regulated to be 20 ~ 22A, illumination reaction 1h, then xenon lamp electric current is regulated to be 12 ~ 15A, illumination reaction 4h;
4) step (3) products therefrom is used deionized water and absolute ethanol washing successively, at 60 ~ 75 DEG C, insulation is dried, and obtains perovskite typed lead titanate/argentum nano composite material.
3. the preparation method of perovskite typed lead titanate/argentum nano composite material according to claim 2, it is characterized in that described ammoniacal liquor, acetic acid is chemical pure, Silver Nitrate is analytical pure.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
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| CN201510123312.6A CN104805503B (en) | 2015-03-20 | 2015-03-20 | Ca-Ti ore type lead titanates/argentum nano composite material and preparation method thereof |
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| CN201510123312.6A CN104805503B (en) | 2015-03-20 | 2015-03-20 | Ca-Ti ore type lead titanates/argentum nano composite material and preparation method thereof |
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| CN104805503A true CN104805503A (en) | 2015-07-29 |
| CN104805503B CN104805503B (en) | 2017-05-31 |
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Cited By (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 |
| CN105289604A (en) * | 2015-10-16 | 2016-02-03 | 浙江大学 | Preparation method of silver oxide/lead titanate nanocomposite |
| CN105731531A (en) * | 2016-01-11 | 2016-07-06 | 浙江大学 | Preparation method of lead titanate nano sheet-platinum nano particle composite material |
| CN107999053A (en) * | 2017-11-06 | 2018-05-08 | 哈尔滨理工大学 | A kind of lanthanium titanate lead/pucherite and preparation method |
| CN114062445A (en) * | 2021-11-12 | 2022-02-18 | 福州大学 | Preparation method of nano-silver surface modified two-dimensional lead titanate material for high-sensitivity ammonia sensing at room temperature |
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| 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 |
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| 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)
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| DAVID ARNEY,ET AL.: "Effects of Particle Surface Areas and Microstructures on Photocatalytic H2 and O2 Production over PbTiO3", 《J. AM. CERAM. SOC.》 * |
| 张漫: "Pb(ZrxTi1-x)O3铁电薄膜光阴极光还原Ag+及其光电化学特性", 《中国优秀硕士学位论文全文数据库（基础科学辑）》 * |
Cited By (9)
| 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 |
| CN105289604A (en) * | 2015-10-16 | 2016-02-03 | 浙江大学 | Preparation method of silver oxide/lead titanate nanocomposite |
| 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 |
| CN105731531A (en) * | 2016-01-11 | 2016-07-06 | 浙江大学 | Preparation method of lead titanate nano sheet-platinum nano particle 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 |
| CN107999053A (en) * | 2017-11-06 | 2018-05-08 | 哈尔滨理工大学 | A kind of lanthanium titanate lead/pucherite and preparation method |
| CN107999053B (en) * | 2017-11-06 | 2020-06-16 | 哈尔滨理工大学 | Lead lanthanum titanate/bismuth vanadate and preparation method thereof |
| CN114062445A (en) * | 2021-11-12 | 2022-02-18 | 福州大学 | Preparation method of nano-silver surface modified two-dimensional lead titanate material for high-sensitivity ammonia sensing at room temperature |
| 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 |
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| CN104805503B (en) | 2017-05-31 |
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