CN105817639A - Tungsten-doped cesium bronze nano-power serving as infrared shelter and preparation method of tungsten-doped cesium bronze nano-power - Google Patents
Tungsten-doped cesium bronze nano-power serving as infrared shelter and preparation method of tungsten-doped cesium bronze nano-power Download PDFInfo
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Abstract
The invention relates to tungsten-doped cesium bronze nano-power serving as an infrared shelter and a preparation method of the tungsten-doped cesium bronze nano-power. The preparation method comprises the following steps that firstly, main raw materials, namely tungstic acid and cesium salt, are weighed, and the molar mass ratio of the tungstic acid to the cesium salt is controlled to be 1:0.01-0.1; secondly, the tungstic acid and the cesium salt are pulverized through a pulverizer and subjected to mixing treatment; thirdly, the pulverized mixed powder is roasted in a sintering furnace under the atmosphere protection; and fourthly, reaction products are washed repeatedly, and target products are obtained after drying and pulverizing. The tungsten-doped cesium bronze nano-power can be applied to outdoor heat insulating materials of buildings, automobiles, trains and the like. The preparation method is low in energy consumption, low in cost, easy to operate, good in environmental friendliness and suitable for large-scale industrial production.
Description
Technical field
The invention belongs to field of nanometer technology, particularly to a kind of caesium Doped Tungsten bronze nano-powder as infrared shield and preparation method thereof.
Background technology
Infrared light has obvious heat effect, is easily caused ambient temperature and raises, and causes building glass, automobile adhesive film, and outdoor facilities etc. needs to reach heat-insulating and energy-saving effect by heat-barrier material.In recent years, tungsten bronze causes people's extensive concern due to the photoelectric properties of its excellence, and the tungsten bronze powder body of the cesium element that adulterates has extremely strong absorption characteristic at region of ultra-red, and the transmitance of visible ray is higher simultaneously, making it cover infrared, the aspect such as glass heat-proof has a wide range of applications.
The caesium Doped Tungsten bronze nano-powder of tradition preparation, to infrared screening rate less than 90%, and uses tungsten chloride or Cesium hydrate. in some processes raw material, cost is high, poor stability, and to human body very bad environmental.
Therefore the invention provides a kind of caesium Doped Tungsten bronze nano-powder as infrared shield and preparation method thereof, product is excellent, technical maturity.
Summary of the invention
For above-mentioned situation, the present invention provides a kind of caesium Doped Tungsten bronze nano-powder as infrared shield and preparation method thereof, overcome the deficiency of existing technique, production cost is low, production efficiency is high, the infrared screening rate of the caesium Doped Tungsten bronze nano-powder of product environment-friendly type reaches 95 ~ 99%, may be directly applied to industrialized mass production.
To achieve these goals, technical scheme is as follows:
Caesium Doped Tungsten bronze nano-powder as infrared shield and preparation method thereof, comprises the following steps:
One, primary raw material wolframic acid and cesium salt are weighed so that it is molal weight ratio controls in 1:0.01 ~ 0.1；
Two, carry out pulverizing and mixing treatment by pulverizer by wolframic acid, cesium salt；
Three, under the mixed powder atmosphere protection after pulverizing, calcine in sintering furnace；
Four, reaction product is carried out cyclic washing, after drying and crushing, i.e. obtain target product.
In the present invention in preferred embodiment, cesium salt can be cesium carbonate, cesium nitrate, cesium sulfate or cesium chloride.
In further preferably implementing, pulverizing batch mixing, pulverize and use jet mill described in step 2, its pulverizing chamber air-pressure controlling is at 0.8 ~ 1.2MPa, and pulverizing speed setting is 5000 ~ 12000 revs/min.
In further preferably implementing, protective atmosphere described in step 3 can be nitrogen, oxygen or argon；Calcining heat maintains 800 ~ 1200 ° of C；Calcining heating rate is 5 ~ 15 ° of C/min, continues heat treatment 5 ~ 10h.
In further preferably implementing, the available deionized water of washing described in step 4 or dehydrated alcohol；Being dried is to carry out 8 ~ 12h under 80 ~ 120 ° of C；Pulverizing and use jet mill, its pulverizing chamber air-pressure controlling is at 0.5 ~ 1.0MPa, and pulverizing speed setting is 2000 ~ 5000 revs/min.
The beneficial effects of the present invention is, the caesium Doped Tungsten bronze nano-powder prepared, good stability, ultraviolet-resistant rate is more than 99.7%, it is seen that light transmission rate 70 ~ 88%, and infrared ray covers and reaches 95 ~ 99%, can be applicable to the outdoor heat-barrier material such as building, automobile, train.This process energy consumption is low, low cost, easily operates, and the feature of environmental protection is good, is suitable for large-scale industrial production.
Accompanying drawing explanation
Fig. 1 is the caesium Doped Tungsten bronze nano-powder infrared light transmittance of the infrared shield of embodiment 1 preparation.
Fig. 2 is the caesium Doped Tungsten bronze nano-powder infrared light transmittance of the infrared shield of embodiment 2 preparation.
Fig. 3 is the caesium Doped Tungsten bronze nano-powder infrared light transmittance of the infrared shield of embodiment 3 preparation.
Detailed description of the invention
For the technological means making the present invention realize, creation characteristic, reach purpose and be easy to understand with effect, below in conjunction with being specifically illustrating, the present invention is expanded on further.
See Fig. 1, embodiment 1
One, the molal weight ratio of primary raw material wolframic acid and cesium carbonate controls at 1:0.01；
Two, carrying out pulverizing mixing treatment by pulverizer by wolframic acid, cesium carbonate, use jet mill to pulverize, pulverizing chamber air-pressure controlling is 0.8MPa, and pulverizing speed setting is 5000 revs/min；
Three, under the mixed powder nitrogen protection after pulverizing, calcining in sintering furnace, 5 ° of C/min are warming up to 800 ° of C calcinings, continue heat treatment 5h；
Four, by deionized water, reaction product being carried out cyclic washing, after 90 ° of C oven drying 10h, use jet mill to pulverize, pulverizing chamber air-pressure controlling is 0.6MPa, and pulverizing speed setting is 2000 revs/min；Target product is i.e. obtained after pulverizing.
Embodiment 2
One, the molal weight ratio of primary raw material wolframic acid and cesium nitrate controls at 1:0.03；
Two, carrying out pulverizing mixing treatment by pulverizer by wolframic acid, cesium nitrate, use jet mill to pulverize, pulverizing chamber air-pressure controlling is 0.9MPa, and pulverizing speed setting is 8000 revs/min；
Three, under the mixed powder oxygen protection after pulverizing, calcining in sintering furnace, 8 ° of C/min are warming up to 1200 ° of C calcinings, continue heat treatment 6h；
Four, by dehydrated alcohol, reaction product being carried out cyclic washing, after 80 ° of C oven drying 12h, use jet mill to pulverize, pulverizing chamber air-pressure controlling is 0.8MPa, and pulverizing speed setting is 3000 revs/min；Target product is i.e. obtained after pulverizing.
Embodiment 3
One, the molal weight ratio of primary raw material wolframic acid and cesium sulfate controls at 1:0.05；
Two, carrying out pulverizing mixing treatment by pulverizer by wolframic acid, cesium sulfate, use jet mill to pulverize, pulverizing chamber air-pressure controlling is 1.2MPa, and pulverizing speed setting is 12000 revs/min；
Three, under the mixed powder oxygen protection after pulverizing, calcining in sintering furnace, 10 ° of C/min are warming up to 1000 ° of C calcinings, continue heat treatment 8h；
Four, by dehydrated alcohol, reaction product being carried out cyclic washing, after 100 ° of C oven drying 12h, use jet mill to pulverize, pulverizing chamber air-pressure controlling is 0.9MPa, and pulverizing speed setting is 4000 revs/min；Target product is i.e. obtained after pulverizing.
Embodiment 4
One, the molal weight ratio of primary raw material wolframic acid and cesium chloride controls at 1:0.07；
Two, carrying out pulverizing mixing treatment by pulverizer by wolframic acid, cesium chloride, use jet mill to pulverize, pulverizing chamber air-pressure controlling is 1.20MPa, and pulverizing speed setting is 10000 revs/min；
Three, under the mixed powder argon shield after pulverizing, calcining in sintering furnace, 15 ° of C/min are warming up to 900 ° of C calcinings, continue heat treatment 10h；
Four, by deionized water, reaction product being carried out cyclic washing, after 120 ° of C oven drying 10h, use jet mill to pulverize, pulverizing chamber air-pressure controlling is 1.0MPa, and pulverizing speed setting is 5000 revs/min；Target product is i.e. obtained after pulverizing.
Embodiment 5
One, the molal weight ratio of primary raw material wolframic acid and cesium carbonate controls at 1:0.09；
Two, carrying out pulverizing mixing treatment by pulverizer by wolframic acid, cesium carbonate, use jet mill to pulverize, pulverizing chamber air-pressure controlling is 1.0MPa, and pulverizing speed setting is 8000 revs/min；
Three, under the mixed powder argon shield after pulverizing, calcining in sintering furnace, 10 ° of C/min are warming up to 1000 ° of C calcinings, continue heat treatment 8h；
Four, by deionized water, reaction product being carried out cyclic washing, after 100 ° of C oven drying 12h, use jet mill to pulverize, pulverizing chamber air-pressure controlling is 0.8MPa, and pulverizing speed setting is 2000 revs/min；Target product is i.e. obtained after pulverizing.
Embodiment 6
One, the molal weight ratio of primary raw material wolframic acid and cesium nitrate controls at 1:1.0；
Two, carrying out pulverizing mixing treatment by pulverizer by wolframic acid, cesium nitrate, use jet mill to pulverize, pulverizing chamber air-pressure controlling is 0.8MPa, and pulverizing speed setting is 12000 revs/min；
Three, under the mixed powder nitrogen protection after pulverizing, calcining in sintering furnace, 5 ° of C/min are warming up to 800 ° of C calcinings, continue heat treatment 10h；
Four, by deionized water, reaction product being carried out cyclic washing, after 80 ° of C oven drying 12h, use jet mill to pulverize, pulverizing chamber air-pressure controlling is 0.6MPa, and pulverizing speed setting is 4000 revs/min；Target product is i.e. obtained after pulverizing.
The ultimate principle of the present invention, principal character and advantages of the present invention have more than been shown and described.Skilled person will appreciate that of the industry; the present invention is not restricted to the described embodiments; the principle of the simply present invention described in above-described embodiment and description; the present invention also has various changes and modifications without departing from the spirit and scope of the present invention, and these changes and improvements both fall within the range of claimed invention.The protection domain of application claims is defined by appending claims and equivalent thereof.
Claims (9)
1. as the caesium Doped Tungsten bronze nano-powder and preparation method thereof of infrared shield, it is characterised in that comprise the steps:
One, primary raw material wolframic acid and cesium salt are weighed so that it is molal weight ratio controls in 1:0.01 ~ 0.1；
Two, carry out pulverizing mixing treatment by pulverizer by wolframic acid, cesium salt；
Three, under the mixed powder atmosphere protection after pulverizing, calcine in sintering furnace；
Four, reaction product is carried out cyclic washing, after drying and crushing, i.e. obtain target product.
Caesium Doped Tungsten bronze nano-powder as infrared shield the most according to claim 1 and preparation method thereof, it is characterised in that cesium salt described in step one can be cesium carbonate, cesium nitrate, cesium sulfate or cesium chloride.
Caesium Doped Tungsten bronze nano-powder as infrared shield the most according to claim 1 and preparation method thereof, it is characterized in that pulverizing described in step 2 batch mixing, pulverize and use jet mill, its pulverizing chamber air-pressure controlling is at 0.8 ~ 1.2MPa, and pulverizing speed setting is 5000 ~ 12000 revs/min.
Caesium Doped Tungsten bronze nano-powder as infrared shield the most according to claim 1 and preparation method thereof, it is characterised in that protective atmosphere described in step 3 can be nitrogen, oxygen or argon.
Caesium Doped Tungsten bronze nano-powder as infrared shield the most according to claim 1 and preparation method thereof, it is characterised in that calcining described in step 3, temperature maintains 800 ~ 1200 ° of C.
Caesium Doped Tungsten bronze nano-powder as infrared shield the most according to claim 5 and preparation method thereof, it is characterised in that described calcining heating rate is 5 ~ 15 ° of C/min, continues heat treatment 5 ~ 10h.
Caesium Doped Tungsten bronze nano-powder as infrared shield the most according to claim 1 and preparation method thereof, it is characterised in that the available deionized water of washing described in step 4 or dehydrated alcohol.
Caesium Doped Tungsten bronze nano-powder as infrared shield the most according to claim 1 and preparation method thereof, it is characterised in that being dried described in step 4 is to carry out 8 ~ 12h under 80 ~ 120 ° of C.
Caesium Doped Tungsten bronze nano-powder as infrared shield the most according to claim 1 and preparation method thereof, it is characterized in that step 4 is pulverized and use jet mill, its pulverizing chamber air-pressure controlling is at 0.5 ~ 1.0MPa, and pulverizing speed setting is 2000 ~ 5000 revs/min.
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Cited By (4)
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| CN107541187A (en) * | 2017-09-29 | 2018-01-05 | 沪本新材料科技（上海）有限公司 | Nano ceramics infrared barrier material |
| CN110534620A (en) * | 2019-09-05 | 2019-12-03 | 保定嘉盛光电科技股份有限公司 | A kind of energy-saving photovoltaic module manufacture craft |
| CN111547771A (en) * | 2019-07-17 | 2020-08-18 | 中国科学院上海硅酸盐研究所 | Transparent heat-shielding fine particles, fine particle dispersion, process for producing the same, and use thereof |
| WO2021008564A1 (en) * | 2019-07-17 | 2021-01-21 | 中国科学院上海硅酸盐研究所 | Transparent heat-shielding material, transparent heat-shielding microparticle dispersion, preparation method therefor and use thereof |
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