CN103449508A - Tungsten doped tin dioxide nano powder and preparation method thereof - Google Patents
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Abstract
The invention discloses tungsten doped tin dioxide nano powder and a preparation method thereof. The tungsten doped tin dioxide nano powder has a molecular formula of WxSn(1-x)O2, wherein the value range of x is 0.02-0.3. A nano thermal insulation coating prepared from the tungsten doped tin dioxide is high in visible light transmittance and good in thermal insulation performance, and the infrared rejection and ultraviolet rejection of the nano thermal insulation coating reach more than 80%. According to the preparation method, an ultrasonic chemical method is adopted to dope tungsten into zinc dioxide to prepare nano powder. By adopting the preparation method, the obtained powder has better electrical conductivity, light transmittance and thermal insulation effect, and a series of defects that agglomeration easily happens and the powder is non-uniform in particle size in a co-precipitation method, the after-treatment of a precursor is difficult and relatively high in cost in a micro-emulsion method, the equipment requirement is high and the corrosivity is strong in a hydro-thermal method, the efficiency of a spray pyrolysis method is low and the like are overcome.
Description
Technical field
The present invention relates to field of nanometer material technology, relate in particular to a kind of tungsten doped stannic oxide nano powder and preparation method thereof.
Background technology
Pure tindioxide is a kind of isolator with broad stopband (3.6 ev), by doping, can make it become semi-conductor or conductor, improves its electroconductibility and spectral selectivity, and then enlarges its range of application.Research is arranged at present by its doping metals indium, antimony etc. are made to transparent heat insulating dope, be coated on glassly, neither affect daylighting, can well stop again the heat transmission, reduce air conditioner load, reach energy-conservation purpose.But, mix in the tindioxide of indium and easily have lattice distortion, cause hole mobility to decline to a great extent, make the resistivity of the film of making be difficult to further reduction, restrict the raising of this film conductivity energy, in addition because indium is precious metal, higher its suitability for industrialized production that limited of cost; Although it is relatively low to mix the film cost that the tindioxide of antimony makes, there are the shortcomings such as thermal insulation is poor, visible light transmissivity is lower during for the heat-insulation and heat-preservation of building glass.
Therefore, prior art has yet to be improved and developed.
Summary of the invention
In view of above-mentioned the deficiencies in the prior art, the object of the present invention is to provide a kind of tungsten doped stannic oxide nano powder and preparation method thereof, be intended to solve the problems such as existing nano-powder thermal insulation is poor, visible light transmissivity is lower.
Technical scheme of the present invention is as follows:
A kind of tungsten doped stannic oxide nano powder, wherein, its molecular formula is W
xsn
(1-x)o
2, wherein, the span of x is 0.02 ~ 0.3.
A kind of preparation method of tungsten doped stannic oxide nano powder as above wherein, comprises the following steps:
S100, to take water-soluble pink salt and tungstate be raw material, presses W
xsn
(1-x)o
2the set(ting)value of middle x takes pink salt and tungstate, adds in the solution that contains dispersion agent, is stirred to abundant dissolving, forms clear solution;
S200, in above-mentioned resulting solution, add urea, be stirred to urea and dissolve fully, the pH value of conditioned reaction system terminal;
S300, above-mentioned solution is washed with argon gas, under argon shield, insert the ultrasonic wave inserting tube and carry out Ultrasonic Radiation, obtain gelatinous precipitate;
S400, by above-mentioned gelatinous precipitate after ageing, after filtration the washing obtain presoma, described presoma drying, grinding, calcining are obtained to described tungsten doped stannic oxide nano powder.
The preparation method of described tungsten doped stannic oxide nano powder, wherein, the chlorate that described pink salt is tin, nitrate or Citrate trianion, described tungstate is sodium wolframate or ammonium tungstate; Described dispersion agent is polyoxyethylene glycol, glycerol or citric acid, 1～2 % that its consumption is the pink salt quality.
The preparation method of described tungsten doped stannic oxide nano powder, wherein, in step S100, described whipping process is to carry out in the water-bath environment of 50 ~ 60 ℃.
The preparation method of described tungsten doped stannic oxide nano powder, wherein, in step S200, described whipping process carries out under 70～90 ℃; Regulation system endpoint pH to 3～5.
The preparation method of described tungsten doped stannic oxide nano powder, wherein, the Ultrasonic Radiation frequency adopted in described Ultrasonic Radiation process is 20.81 kHz, 24.45 kHz, 30.10 kHz or 40.34 kHz, radiated time is 2～6 h.
The preparation method of described tungsten doped stannic oxide nano powder, wherein, in step S300, described excusing from death wave radiation is carried out under 70 ~ 90 ℃.
The preparation method of described tungsten doped stannic oxide nano powder, wherein, the time of described ageing is 5 ~ 24h.
The preparation method of described tungsten doped stannic oxide nano powder, wherein, the process of described filtration washing is to use distilled water wash three times when described gelatinous precipitate is carried out to decompress filter, the ethanolic soln that is 10 % by volume fraction again washs to filtrate and is neutral, finally uses twice of absolute ethanol washing.
The preparation method of described tungsten doped stannic oxide nano powder, wherein, described drying, grinding, calcination process are that drying is after a few hours under 80 ℃, grind into powder, be placed in retort furnace by powder, under 400 ℃ ~ 800 ℃, is incubated 3 ~ 5 h.
Beneficial effect: the invention provides a kind of tungsten doped stannic oxide nano powder, the visible light transmissivity of the nanometer thermal insulation coating made with described tungsten doping stannic oxide is high, heat-proof quality good, and its infrared rays rejection rate and ultraviolet isolating rate all reach more than 80%.And, the preparation method of described tungsten doped stannic oxide nano powder utilizes hyperacoustic cavitation effect to produce the condition of High Temperature High Pressure, realize that the microcosmic between the inhomogeneous reaction thing evenly mixes, promote the generation of solid cenotype, and improve the efficiency of separating presoma in conjunction with the method for organic solvent washing, prepare efficiently nano-powder.The particle diameter of nanometer powder that the present invention obtains is little, it is few to be uniformly dispersed, to reunite, and this technique simple efficient, synthesis cycle is short, favorable reproducibility, is conducive to industrialization.
The accompanying drawing explanation
The XRD figure spectrum that Fig. 1 is tungsten doped stannic oxide nano powder in the embodiment of the present invention 1.
The infrared absorption figure that Fig. 2 is tungsten doped stannic oxide nano powder in the embodiment of the present invention 2.
Embodiment
The invention provides a kind of tungsten doped stannic oxide nano powder and preparation method thereof, clearer, clear and definite for making purpose of the present invention, technical scheme and effect, below the present invention is described in more detail.Should be appreciated that specific embodiment described herein, only in order to explain the present invention, is not intended to limit the present invention.
A kind of tungsten doped stannic oxide nano powder is provided in the present invention, and its molecular formula is W
xsn
(1-x)o
2, wherein, the span of x is 0.02 ~ 0.3.The visible light transmissivity of the nanometer thermal insulation coating that adopts described tungsten doping stannic oxide to make is high, heat-proof quality good, and its infrared rays rejection rate and ultraviolet isolating rate all reach more than 80%.Improved much than its heat-proof quality of ATO, than ITO, greatly saved again production cost.
The preparation method of described tungsten doped stannic oxide nano powder also is provided in the present invention, in the inventive method, adopts the sonochemistry method to carry out the tungsten doping to tindioxide and make nano-powder.The sonochemistry method refers to utilizes hyperacoustic " acoustic cavitation " to act on the condition that produces High Temperature High Pressure in the extremely short time, realizes that the microcosmic between the inhomogeneous reaction thing evenly mixes, and promotes the generation of solid cenotype.This method not only makes the powder electroconductibility, light transmission rate and the effect of heat insulation that obtain better, and made up that coprecipitation method is easily reunited, diameter of particle is inhomogeneous, the aftertreatment of microemulsion method presoma is difficult, cost is higher, a series of shortcomings such as the equipment requirements of hydrothermal method is high, corrodibility is strong, and spray pyrolysis efficiency is low.
Particularly, the preparation method of described tungsten doped stannic oxide nano powder comprises the following steps:
S100, to take water-soluble pink salt and tungstate be raw material, presses W
xsn
(1-x)o
2the set(ting)value of middle x takes pink salt and tungstate, adds in the solution that contains dispersion agent, in the water-bath environment of 50 ~ 60 ℃, is stirred to abundant dissolving, finally forms clear solution.Wherein, the chlorate that described pink salt is tin, nitrate or Citrate trianion, be the quaternary salts of tin, relatively stable; Described tungstate is sodium wolframate or ammonium tungstate, and in the washing of back, filtration procedure, anion ratio is easier to remove, and is beneficial to and obtains high-quality powder; The x value is 0.02 ~ 0.3; Described dispersion agent is polyoxyethylene glycol, glycerol or citric acid, 1～2 % that its consumption is the pink salt quality.
S200, in above-mentioned resulting solution, add urea, be stirred to urea and dissolve fully under 70～90 ℃, System forming clear solution, the pH value of conditioned reaction system terminal.
Wherein, regulation system endpoint pH to 3～5, in the preparation process of powder, pH value all has a significant impact pattern and the performance of powder, controls suitable pH value and plays conclusive effect to obtaining high-quality powder.
S300, by argon gas washing 10 ~ 30min for above-mentioned solution, then, under 70 ~ 90 ℃ and argon shield, insert the ultrasonic wave inserting tube and obtain gelatinous precipitate with the Ultrasonic Radiation regular hour of different frequency.
Wherein, the Ultrasonic Radiation frequency of employing can be 20.81 kHz, 24.45 kHz, 30.10 kHz or 40.34 kHz; Radiated time is 2～6 h.
S400, by above-mentioned gelatinous precipitate after ageing, after filtration the washing obtain presoma, described presoma drying, grinding, calcining are obtained to described tungsten doped stannic oxide nano powder.
Wherein, the time of described ageing is 5 ~ 24h, so that powder forms more stable particle.The process of described filtration washing be when described gelatinous precipitate is carried out to decompress filter with distilled water wash three times, then the ethanolic soln that is 10 % with volume fraction washs to filtrate and is neutrality, finally uses twice of absolute ethanol washing.Adopt above-mentioned washing separate mode can obviously accelerate the speed of filtration washing, thereby increase the benefit.Described drying, grinding, calcination process are that drying is after a few hours under 80 ℃, and grind into powder, be placed in retort furnace by powder, under 400 ℃ ~ 800 ℃, is incubated 3 ~ 5 h, and obtaining the tungsten doped stannic oxide nano powder is nanometer WTO powder.
Below in conjunction with embodiment, the present invention is described in detail, but the invention is not restricted to given example.
According to W
xsn
(1-x)in O, x=0.1 is example, takes 3.1410 g SnCl
45H
2o and 0.3300 g Na
2wO
42H
2o is dissolved in the 70 ml deionized waters that contain 0.0315 ~ 0.063 g PEG-600, is placed in the water-bath environment of 60 ℃ to dissolving fully, then adds 2.34 g ureas, is stirred to the formation clear solution; Above-mentioned solution is washed to 20 min with argon gas, then, under 80 ℃ and argon shield, insert the ultrasonic wave inserting tube, Ultrasonic Radiation 4 h that are 20.81 kHz by frequency, obtain gelatinous precipitate; To after gelatinous precipitate ageing 5 h, filter, and in decompress filter with distilled water wash three times, then the ethanolic soln that is 10 % with volume fraction washs to filtrate and is neutrality, finally uses twice of absolute ethanol washing; By gained presoma grind into powder after dry a few hours under 80 ℃, powder is placed in to retort furnace, be incubated 3 ~ 5h under 400 ~ 800 ℃, furnace cooling, obtain little, the finely dispersed nanometer WTO powder of particle diameter.
To the gained material carry out XRD, infrared and atomic absorption is identified, its XRD figure is composed as shown in Figure 1, thereby determines that according to different Absorption Characteristics and the crystal morphology of different elements utilizing the material that this preparation method obtains is the tungsten doped stannic oxide nano powder really.Through detection, the nanometer thermal insulation coating made with the tungsten doping stannic oxide of the present embodiment gained, its visible light transmissivity is about that 85 %, infrared rays rejection rate are about 85 %, the ultraviolet isolating rate is about 99 %, 0 grade of sticking power, hardness > 6 H.The described nanometer thermal insulation coating of the present embodiment ATO powder made the contrast heat insulating coat used with existing market compared, at infrared lamp, irradiate under the condition of 29 min, scribbling the present embodiment receives the temperature of glass of heat insulating coat and reaches 5 ℃ of left and right than the temperature of contrast heat insulating coat is low, and compared with not having cated blank glass, temperature is low nearly 15 ℃.
Embodiment 2
According to W
xsn
(1-x)o
2middle x=0.15 is example, takes 3.1410 g SnCl
45H
2o and 0.5241 g Na
2wO
42H
2o is dissolved in the 70 mL deionized waters that contain 0.0315 ~ 0.063 g PEG-600, is placed in the water-bath environment of 70 ℃ to dissolving fully, then adds 2.4459 g ureas, is stirred to the formation clear solution; Above-mentioned solution is washed to 30 min with argon gas, then, under 90 ℃ and argon shield, insert the ultrasonic wave inserting tube, Ultrasonic Radiation 6 h that are 30.10 kHz by frequency, obtain gelatinous precipitate; To after gelatinous precipitate ageing 10 h, filter, and in decompress filter with distilled water wash three times, then the ethanolic soln that is 10 % with volume fraction washs to filtrate and is neutrality, finally uses twice of absolute ethanol washing; By gained presoma grind into powder after dry a few hours under 80 ℃, powder is placed in to retort furnace, calcine 3 ~ 5h under 400 ~ 800 ℃, furnace cooling, obtain the nano-powder of tungsten doping stannic oxide.
To the gained material carry out XRD, infrared and atomic absorption is identified, its middle infrared absorption figure is as shown in Figure 2.Thereby determine that according to different Absorption Characteristics and the crystal morphology of different elements utilizing the material that this preparation method obtains is the nano-powder of tungsten doping stannic oxide really.The described nanometer thermal insulation coating of the present embodiment the contrast heat insulating coat made with existing market ATO powder used compared, at infrared lamp, irradiate under the condition of 29 min, scribbling the present embodiment receives the temperature of glass of heat insulating coat and reaches 7 ℃ of left and right than the temperature of contrast heat insulating coat is low, and compared with not having cated blank glass, temperature is low nearly 17 ℃.
In sum, the tungsten doped stannic oxide nano powder thermal insulation provided in the present invention is good, visible light transmissivity is higher.And the present invention adopts the sonochemistry method to carry out tungsten doping to tindioxide to make nano-powder, this method is simple, synthesis cycle is short, can realize Uniform Doped, the powder reuniting made is few, particle diameter is little, be uniformly dispersed, this method not only makes the powder electroconductibility, light transmission rate and the effect of heat insulation that obtain better, and made up that coprecipitation method is easily reunited, diameter of particle is inhomogeneous, the aftertreatment of microemulsion method presoma is difficult, cost is higher, a series of shortcomings such as the equipment requirements of hydrothermal method is high, corrodibility is strong, and spray pyrolysis efficiency is low.
Should be understood that, application of the present invention is not limited to above-mentioned giving an example, and for those of ordinary skills, can be improved according to the above description or convert, and all these improvement and conversion all should belong to the protection domain of claims of the present invention.
Claims (10)
1. a tungsten doped stannic oxide nano powder, is characterized in that, its molecular formula is W
xsn
(1-x)o
2, wherein, the span of x is 0.02 ~ 0.3.
2. the preparation method of a tungsten doped stannic oxide nano powder as claimed in claim 1, is characterized in that, comprises the following steps:
S100, to take water-soluble pink salt and tungstate be raw material, presses W
xsn
(1-x)o
2the set(ting)value of middle x takes pink salt and tungstate, adds in the solution that contains dispersion agent, is stirred to abundant dissolving, forms clear solution;
S200, in above-mentioned resulting solution, add urea, be stirred to urea and dissolve fully, the pH value of conditioned reaction system terminal;
S300, above-mentioned solution is washed with argon gas, under argon shield, carry out Ultrasonic Radiation, obtain gelatinous precipitate;
S400, by above-mentioned gelatinous precipitate after ageing, after filtration the washing obtain presoma, described presoma drying, grinding, calcining are obtained to described tungsten doped stannic oxide nano powder.
3. according to the preparation method of tungsten doped stannic oxide nano powder as claimed in claim 2, it is characterized in that, the chlorate that described pink salt is tin, nitrate or Citrate trianion, described tungstate is sodium wolframate or ammonium tungstate; Described dispersion agent is polyoxyethylene glycol, glycerol or citric acid, 1～2 % that its consumption is the pink salt quality.
4. according to the preparation method of tungsten doped stannic oxide nano powder as claimed in claim 2, it is characterized in that, in step S100, described whipping process is to carry out in the water-bath environment of 50 ~ 60 ℃.
5. according to the preparation method of tungsten doped stannic oxide nano powder as claimed in claim 2, it is characterized in that, in step S200, described whipping process carries out under 70～90 ℃; Regulation system endpoint pH to 3～5.
6. according to the preparation method of tungsten doped stannic oxide nano powder as claimed in claim 2, it is characterized in that, the Ultrasonic Radiation frequency adopted in described Ultrasonic Radiation process is 20.81 kHz, 24.45 kHz, 30.10 kHz or 40.34 kHz, and radiated time is 2～6 h.
7. according to the preparation method of tungsten doped stannic oxide nano powder as claimed in claim 2, it is characterized in that, in step S300, described excusing from death wave radiation is carried out under 70 ~ 90 ℃.
8. according to the preparation method of tungsten doped stannic oxide nano powder as claimed in claim 2, it is characterized in that, the time of described ageing is 5 ~ 24h.
9. according to the preparation method of tungsten doped stannic oxide nano powder as claimed in claim 2, it is characterized in that, the process of described filtration washing is to use distilled water wash three times when described gelatinous precipitate is carried out to decompress filter, the ethanolic soln that is 10 % by volume fraction again washs to filtrate and is neutral, finally uses twice of absolute ethanol washing.
10. according to the preparation method of tungsten doped stannic oxide nano powder as claimed in claim 2, it is characterized in that, described drying, grinding, calcination process are under 80 ℃ after dry a few hours, grind into powder, powder is placed in to retort furnace, under 400 ℃ ~ 800 ℃, is incubated 3 ~ 5 h.
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| CN106189365A (en) * | 2016-07-15 | 2016-12-07 | 深圳大学 | Modified Fxmnysn(1 x y)o2nano-powder and the preparation method of modified aqueous polyurethane emulsion |
| CN106219552A (en) * | 2015-11-30 | 2016-12-14 | 沪本新材料科技（上海）有限公司 | A kind of nano-powder preparation method absorbing blue light |
| CN108465465A (en) * | 2018-04-04 | 2018-08-31 | 广东工业大学 | A kind of semiconductive thin film and preparation method thereof |
| CN109650438A (en) * | 2019-01-18 | 2019-04-19 | 昆明理工大学 | Nanometer witch culture tin dioxide powder and preparation method thereof |
| CN109722653A (en) * | 2019-01-02 | 2019-05-07 | 华南理工大学 | A kind of method that solwution method prepares witch culture tin oxide transparent conductive film |
| CN110282654A (en) * | 2019-07-30 | 2019-09-27 | 云南大学 | A kind of pentagonal pyramid shape SnO2The preparation method and application of nano-array composite hierarchical structure tectosome nano material |
| CN115259295A (en) * | 2022-08-12 | 2022-11-01 | 上海纳米技术及应用国家工程研究中心有限公司 | Electrode manufacturing method for degrading resorcinol by electrocatalysis, product and application |
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| CN106219552A (en) * | 2015-11-30 | 2016-12-14 | 沪本新材料科技（上海）有限公司 | A kind of nano-powder preparation method absorbing blue light |
| CN106189365A (en) * | 2016-07-15 | 2016-12-07 | 深圳大学 | Modified Fxmnysn(1 x y)o2nano-powder and the preparation method of modified aqueous polyurethane emulsion |
| CN106189365B (en) * | 2016-07-15 | 2018-06-22 | 深圳大学 | Modified FxMnySn(1-x-y)O2The preparation method of nano-powder and modified aqueous polyurethane emulsion |
| CN108465465A (en) * | 2018-04-04 | 2018-08-31 | 广东工业大学 | A kind of semiconductive thin film and preparation method thereof |
| CN109722653A (en) * | 2019-01-02 | 2019-05-07 | 华南理工大学 | A kind of method that solwution method prepares witch culture tin oxide transparent conductive film |
| CN109650438A (en) * | 2019-01-18 | 2019-04-19 | 昆明理工大学 | Nanometer witch culture tin dioxide powder and preparation method thereof |
| CN110282654A (en) * | 2019-07-30 | 2019-09-27 | 云南大学 | A kind of pentagonal pyramid shape SnO2The preparation method and application of nano-array composite hierarchical structure tectosome nano material |
| CN115259295A (en) * | 2022-08-12 | 2022-11-01 | 上海纳米技术及应用国家工程研究中心有限公司 | Electrode manufacturing method for degrading resorcinol by electrocatalysis, product and application |
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