CN104416154A - Method for preparing silver cladded zinc metastannate with water bath method - Google Patents
Method for preparing silver cladded zinc metastannate with water bath method Download PDFInfo
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- CN104416154A CN104416154A CN201310407572.7A CN201310407572A CN104416154A CN 104416154 A CN104416154 A CN 104416154A CN 201310407572 A CN201310407572 A CN 201310407572A CN 104416154 A CN104416154 A CN 104416154A
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- zinc metastannate
- solution
- water bath
- metastannate
- silver
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Abstract
The invention discloses a method for preparing silver cladded zinc metastannate with a water bath method. The method comprises the following steps: dissolving zinc sulfate heptahydrate and hexadecyl trimethyl ammonium bromide and then dissolving stannic chloride pentahydrate and sodium hydroxide by using a surface active agent CTAB (Cetyltrimethyl Ammonium Bromide) assisted hydrothermal synthesis method; then carrying out constant-temperature titration; performing reaction for 6 hours at 150 DEG C, carrying out furnace cooling to room temperature to obtain zinc metastannate; carrying out low-temperature reaction at 40 DEG C by using thermostatic water bath in a silver nitrate solution by using the water bath method, and carrying out centrifuging, collecting and drying to finally obtain a finished product. The method disclosed by the invention is simple in principle, convenient to operate, low in cost, short in time consumption, efficient and economic.
Description
Technical field
The invention belongs to technical field of material, more particularly, relate to the coated ZnSnO of Ag
3the preparation method of powder, is mainly used in gas sensitive field tests.
Background technology
Along with the raising of science and technology, people are also increasing for the demand of special material.But present stage material performance can not meet people produce and life needs.Along with going deep into of nanometer-micron technical, people are for the structure updating material, and the performance promoting material has had more deep understanding.Therefore research and develop functional material and have huge development space, meaning is also very great.
Hydrothermal synthesis method is a kind of important wet chemical method, and it can prepare the ZnSnO of different morphologies very easily
3nano/micron structure, causes extensive concern and the interest of the multidisciplinary research personnel comprising materialogy thus.ZnSnO
3as a kind of sensitive material, people are to its application study and propose high performance research further and also never interrupted.At present, hydro-thermal method is adopted to prepare the ZnSnO of varied pattern
3nano/micron labyrinth, more representational as 0 dimension (nanoparticle), 1 dimension (nano wire, nanometer rods), 3 dimensions (Nano microsphere, nano square, nanocage, polyhedron crystallite) etc.ZnSnO
3be a kind of important gas sensitive, have a wide range of applications.It is to CO, H
2s, i-butane, CH
4, LPG, CH
3sH, NO
xdeng there being gas sensing property.ZnSnO
3easily Zn is transformed into more than 700 DEG C
2snO
4and SnO
2.And Zn
2snO
4air-sensitive performance poor, be the product not wishing to obtain.Therefore the preparation method of material has very large impact to the sensitivity of gas and response-turnaround time etc.
Summary of the invention
The object of the invention is to overcome the deficiencies in the prior art, provide a kind of simple and convenient, the with low cost hydro-thermal method that utilizes prepares silver parcel ZnSnO
3method.
Technical purpose of the present invention is achieved by following technical proposals:
Immersion method prepares a method for silver-colored coated zinc metastannate, carries out according to following step:
Step 1, by white vitriol (ZnSO
47H
2and softex kw (C O)
16h
33(CH
3)
3nBr, CTAB) be dissolved in 20mL distilled water, form the first solution;
Step 2, by Tin tetrachloride pentahydrate (SnCl
45H
2o) and NaOH (NaOH) dissolve in 20mL distilled water, form the second solution;
Step 3, first solution is placed in 60 DEG C of water bath with thermostatic control magnetic stirring apparatus, after temperature constant, second solution instills in the first solution again, after keeping magnetic agitation 30-60min, suspension is proceeded in reactor, after reacting 6h at being then placed in 150 DEG C, cool to room temperature (namely 20-25 DEG C) with the furnace;
Step 4, by the white precipitate deionized water collected and absolute ethyl alcohol repeatedly centrifugation, removes the foreign ion in precipitation, finally dries under 70 DEG C of air atmospheres and obtains zinc metastannate;
Step 5, is dissolved in distilled water by silver nitrate, ethylene glycol, polyvinylpyrrolidone and sodium borohydride, forms the 3rd solution;
Step 6, adds the zinc metastannate of preparation in the 3rd solution, carries out magnetic agitation and ultrasonic vibration, to make system be uniformly dispersed, afterwards in water bath with thermostatic control at 40 DEG C of lower magnetic force stirring reaction 1-2h;
Step 7, by the precipitate with deionized water collected and absolute ethyl alcohol repeatedly centrifugation, removes the foreign ion in precipitation, finally dries under 70 DEG C of air atmospheres and obtains end product.
In technique scheme, the mass ratio of each medicine is ZnSO
47H
2o:SnCl
45H
2o:CTAB:NaOH is 13:16:5:11, obtains the ZnSnO of simple cubic structure
3, size, between 40-80nm, is evenly distributed.
In technique scheme, the mass ratio of each medicine is ZnSO
47H
2o:SnCl
45H
2o:CTAB:NaOH is 13:16:5:20, obtains the ZnSnO of lamellar structure
3, size, between 100-200nm, is evenly distributed.
In technique scheme, the mass ratio of each medicine is ZnSO
47H
2o:SnCl
45H
2o:CTAB:NaOH is 13:16:5:60, obtains the ZnSnO of 14 body structures
3, size, between 150-250nm, is evenly distributed.
In technique scheme, in step 3, magnetic agitation selects 150-200 turns/min, and rate of addition is 0.1-0.5ml/min.
In technique scheme, in step 5, select 15mL distilled water, add silver nitrate 0.2g, ethylene glycol 15mL, polyvinylpyrrolidone 0.3g and sodium borohydride 0.07g.
In technique scheme, in step 6, select to add zinc metastannate 0.2g.
In technique scheme, in step 6, magnetic agitation selects 150-200 turns/min.
The present invention adopts the method for Surfactant CTAB assisted hydrothermal synthesis, dense by regulation and control soda acid, prepares the ZnSnO of different morphologies of size uniform, better crystallinity degree
3crystal.Based on the ABO that this kind of method is prepared
3the ZnSnO of structure
3nano material, by investigating the impact of change on Product size and pattern of synthesis condition, discloses the formation mechenism of this kind of crystal.Technical solution of the present invention principle is simple, and easy to operate, expense is low, consuming time short, the coated ZnSnO of Ag of generation
3good dispersion and evenly, be a kind of preparation method of high-efficiency and economic.
Accompanying drawing explanation
Fig. 1 is ZnSnO in the present invention
3the stereoscan photograph of preparation embodiment 1 preparing product.
Fig. 2 is ZnSnO in the present invention
3the stereoscan photograph of preparation embodiment 2 preparing product.
Fig. 3 is ZnSnO in the present invention
3the stereoscan photograph of preparation embodiment 3 preparing product.
Fig. 4 is embodiment product ZnSnO prepared by the present invention
3xRD test curve, wherein a is embodiment 1, b be embodiment 2, c is embodiment 3.
Fig. 5 is the stereoscan photograph of the preparation embodiment preparing product of silver-colored coated zinc metastannate in the present invention.
Fig. 6 is the XRD test curve of the preparation embodiment preparing product of silver-colored coated zinc metastannate in the present invention, wherein ● be ZnSnO
3, ◆ be Ag.
Detailed description of the invention
Technical scheme of the present invention is further illustrated below in conjunction with specific embodiment.
First carry out ZnSnO
3preparation embodiment 1-3
Embodiment 1:
The mass ratio of each medicine is: ZnSO
47H
2o:SnCl
45H
2o:CTAB:NaOH is 13:16:5:11.
Take the ZnSO of 0.259g
47H
2o powder, puts into 40ml beaker, adds 20ml distilled water, and is placed on magnetic stirring apparatus and constantly stirs, and after it dissolves completely, slowly adds the CTAB of 0.1g, 10min is stirred in 60 DEG C of water-baths, until temperature is permanent steady.Separately get a beaker, take the SnCl of 0.316g
45H
2o powder, be placed in 40ml beaker, add 20ml distilled water, and be placed on magnetic stirring apparatus and constantly stir, after it dissolves completely, slowly add 0.23gNaOH, after it dissolves completely, with dropper, solution is slowly added dropwise to (magnetic agitation selects 150 turns/min, and rate of addition is 0.5ml/min) in the beaker of water-bath, now has a large amount of white precipitate to produce.After 60 DEG C of water bath with thermostatic control magnetic agitation 30-60min, suspension is proceeded in the reactor of 60ml, be then placed in after 150 DEG C of drying boxes react 6h and cool to room temperature with the furnace.By the white precipitate deionized water collected and absolute ethyl alcohol repeatedly centrifugation, remove the foreign ion in precipitation.Finally under 70 DEG C of air atmospheres, dry more than 10h obtains end product, and as shown in Figure 1, the structure shown in accompanying drawing 1 is the ZnSnO of simple cubic structure
3, size, between 40-80nm, is evenly distributed.
Embodiment 2:
The mass ratio of each medicine is: ZnSO
47H
2o:SnCl
45H
2o:CTAB:NaOH is 13:16:5:20.
Take the ZnSO of 0.259g
47H
2o powder, puts into 40ml beaker, adds 20ml distilled water, and is placed on magnetic stirring apparatus and constantly stirs, and after it dissolves completely, slowly adds the CTAB of 0.1g, 10min is stirred in 60 DEG C of water-baths, until temperature is permanent steady.Separately get a beaker, take the SnCl of 0.316g
45H
2o powder, be placed in 40ml beaker, add 20ml distilled water, and be placed on magnetic stirring apparatus and constantly stir, after it dissolves completely, slowly add 0.4gNaOH, after it dissolves completely, with dropper, solution is slowly added dropwise to (magnetic agitation selects 200 turns/min, and rate of addition is 0.1ml/min) in the beaker of water-bath, now has a large amount of white precipitate to produce.After 60 DEG C of water bath with thermostatic control magnetic agitation 30-60min, suspension is proceeded in the reactor of 60ml, be then placed in after 150 DEG C of drying boxes react 6h and cool to room temperature with the furnace.By the white precipitate deionized water collected and absolute ethyl alcohol repeatedly centrifugation, remove the foreign ion in precipitation.Finally under 70 DEG C of air atmospheres, dry more than 10h obtains end product, and as shown in Figure 2, the structure shown in accompanying drawing 2 is the ZnSnO of lamellar structure
3, size, between 100-200nm, is evenly distributed.
Embodiment 3:
The mass ratio of each medicine is: ZnSO
47H
2o:SnCl
45H
2o:CTAB:NaOH is 13:16:5:60.
Take the ZnSO of 0.259g
47H
2o powder, puts into 40ml beaker, adds 20ml distilled water, and is placed on magnetic stirring apparatus and constantly stirs, and after it dissolves completely, slowly adds the CTAB of 0.1g, 10min is stirred in 60 DEG C of water-baths, until temperature is permanent steady.Separately get a beaker, take the SnCl of 0.316g
45H
2o powder, be placed in 40ml beaker, add 20ml distilled water, and be placed on magnetic stirring apparatus and constantly stir, after it dissolves completely, slowly add 0.6gNaOH, after it dissolves completely, with dropper, solution is slowly added dropwise to (magnetic agitation selects 180 turns/min, and rate of addition is 0.3ml/min) in the beaker of water-bath, now has a large amount of white precipitate to produce.After 60 DEG C of water bath with thermostatic control magnetic agitation 30-60min, suspension is proceeded in the reactor of 60ml, be then placed in after 150 DEG C of drying boxes react 6h and cool to room temperature with the furnace.By the white precipitate deionized water collected and absolute ethyl alcohol repeatedly centrifugation, remove the foreign ion in precipitation.Finally under 70 DEG C of air atmospheres, dry more than 10h obtains end product, and as shown in Figure 3, the structure shown in accompanying drawing 3 is the ZnSnO of 14 body structures
3, size, between 150-250nm, is evenly distributed.
Product prepared by embodiment 1-3 is carried out XRD test, and result is by shown in accompanying drawing 4, although the pattern of product is shown as three kinds of different patterns, the end product of three kinds of preparation methods is ZnSnO
3.
The lamellar ZnSnO utilizing above-described embodiment to prepare
3powder carries out Ag parcel
Take the AgNO of 0.2g
3be dissolved in the distilled water of 15ml, after to be dissolved, add 0.3gpvp(K-90), then in above-mentioned solution, add 15ml ethylene glycol (C
2h
6o
2), magnetic agitation is dissolved to evenly, then adds the NaBH of 0.07g
4to dissolving the mixed liquor forming 30ml completely.The lamellar ZnSnO of 0.2g is added in the mixed liquor of above-mentioned 30ml
3powder, magnetic agitation 5min, then ultrasonic vibration 10min, form suspension.Suspension is placed in 40 DEG C of water-baths, and with magnetic agitation 2h, until color becomes ash.By the white precipitate deionized water collected and absolute ethyl alcohol repeatedly centrifugation, remove the foreign ion in precipitation.Finally under 70 DEG C of air atmospheres, dry more than 10h obtains end product, and as shown in Figure 5, its XRD as shown in Figure 6 for SEM.
Above to invention has been exemplary description; should be noted that; when not departing from core of the present invention, any simple distortion, amendment or other those skilled in the art can not spend the equivalent replacement of creative work all to fall into protection scope of the present invention.
Claims (3)
1. immersion method prepares a method for silver-colored coated zinc metastannate, it is characterized in that, carries out according to following step:
Step 1, is dissolved in white vitriol and softex kw in 20mL distilled water, forms the first solution;
Step 2, dissolves Tin tetrachloride pentahydrate and NaOH in 20mL distilled water, forms the second solution;
Step 3, is placed in 60 DEG C of water bath with thermostatic control magnetic stirring apparatus, after temperature constant by the first solution, second solution instills in the first solution again, after keeping magnetic agitation 30-60min, suspension is proceeded in reactor, after reacting 6h at being then placed in 150 DEG C, cool to room temperature with the furnace;
Step 4, by the white precipitate deionized water collected and absolute ethyl alcohol repeatedly centrifugation, removes the foreign ion in precipitation, finally dries under 70 DEG C of air atmospheres and obtains zinc metastannate;
Step 5, is dissolved in distilled water by silver nitrate, ethylene glycol, polyvinylpyrrolidone and sodium borohydride, forms the 3rd solution;
Step 6, adds the zinc metastannate of preparation in the 3rd solution, carries out magnetic agitation and ultrasonic vibration, to make system be uniformly dispersed, afterwards in water bath with thermostatic control at 40 DEG C of lower magnetic force stirring reaction 1-2h;
Step 7, by the precipitate with deionized water collected and absolute ethyl alcohol repeatedly centrifugation, removes the foreign ion in precipitation, finally dries under 70 DEG C of air atmospheres and obtains end product;
Wherein the mass ratio of each medicine is white vitriol: Tin tetrachloride pentahydrate: softex kw: NaOH is 13:16:5:11, and obtain the zinc metastannate of simple cubic structure, size, between 40-80nm, is evenly distributed; The mass ratio of each medicine is white vitriol: Tin tetrachloride pentahydrate: softex kw: NaOH is 13:16:5:20, and obtain the zinc metastannate of lamellar structure, size, between 100-200nm, is evenly distributed; The mass ratio of each medicine is white vitriol: Tin tetrachloride pentahydrate: softex kw: NaOH is 13:16:5:60, and obtain the zinc metastannate of 14 body structures, size, between 150-250nm, is evenly distributed; In described step 5, select 15mL distilled water, add silver nitrate 0.2g, ethylene glycol 15mL, polyvinylpyrrolidone 0.3g and sodium borohydride 0.07g; In described step 6, select to add zinc metastannate 0.2g.
2. a kind of immersion method according to claim 1 prepares the method for silver-colored coated zinc metastannate, it is characterized in that, in described step 3, magnetic agitation selects 150-200 turns/min, and rate of addition is 0.1-0.5ml/min.
3. a kind of immersion method according to claim 1 prepares the method for silver-colored coated zinc metastannate, it is characterized in that, in described step 6, magnetic agitation selects 150-200 turns/min.
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Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN106044843A (en) * | 2016-06-02 | 2016-10-26 | 景德镇学院 | Preparing method of porous zinc metastannate nanosheet |
| CN110180526A (en) * | 2019-05-10 | 2019-08-30 | 重庆第二师范学院 | A kind of photocatalyst Li2SnO3Preparation method and its degradation antibiotic in utilization |
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|---|---|---|---|---|
| CN1043830A (en) * | 1989-10-16 | 1990-07-11 | 云南大学 | The manufacture method of zinc metastannate gas |
| CN101251508A (en) * | 2008-04-01 | 2008-08-27 | 重庆大学 | Method for manufacturing gas sensor for testing hydrogen |
| CN102126745A (en) * | 2011-01-24 | 2011-07-20 | 济南大学 | Nano zinc metastannate air-sensitive material with hollow fiber structure and preparation method thereof |
| KR20130104173A (en) * | 2012-03-13 | 2013-09-25 | 인하대학교 산학협력단 | Znsno3 nanorods coated with palladium particles, a preparation method thereof, and gas sensor using the same |
-
2013
- 2013-09-09 CN CN201310407572.7A patent/CN104416154B/en not_active Expired - Fee Related
Patent Citations (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1043830A (en) * | 1989-10-16 | 1990-07-11 | 云南大学 | The manufacture method of zinc metastannate gas |
| CN101251508A (en) * | 2008-04-01 | 2008-08-27 | 重庆大学 | Method for manufacturing gas sensor for testing hydrogen |
| CN102126745A (en) * | 2011-01-24 | 2011-07-20 | 济南大学 | Nano zinc metastannate air-sensitive material with hollow fiber structure and preparation method thereof |
| KR20130104173A (en) * | 2012-03-13 | 2013-09-25 | 인하대학교 산학협력단 | Znsno3 nanorods coated with palladium particles, a preparation method thereof, and gas sensor using the same |
Cited By (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN106044843A (en) * | 2016-06-02 | 2016-10-26 | 景德镇学院 | Preparing method of porous zinc metastannate nanosheet |
| CN106044843B (en) * | 2016-06-02 | 2017-06-23 | 景德镇学院 | The preparation method of porous zinc metastannate nanometer sheet |
| CN110180526A (en) * | 2019-05-10 | 2019-08-30 | 重庆第二师范学院 | A kind of photocatalyst Li2SnO3Preparation method and its degradation antibiotic in utilization |
| CN110180526B (en) * | 2019-05-10 | 2022-03-25 | 重庆第二师范学院 | Photocatalyst Li2SnO3The preparation method and the application thereof in degrading antibiotics |
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| CN104416154B (en) | 2016-08-10 |
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Inventor after: Liang Yanqin Inventor after: Cui Zhenduo Inventor after: Yang Xianjin Inventor after: Zhu Shengli Inventor after: Zheng Jing Inventor before: Zheng Jing Inventor before: Cui Zhenduo Inventor before: Yang Xianjin Inventor before: Zhu Shengli Inventor before: Liang Yanqin |
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