CN107188225A - A kind of indium-doped antimony oxidation tin nano-powder and preparation method thereof - Google Patents
A kind of indium-doped antimony oxidation tin nano-powder and preparation method thereof Download PDFInfo
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- CN107188225A CN107188225A CN201710575272.8A CN201710575272A CN107188225A CN 107188225 A CN107188225 A CN 107188225A CN 201710575272 A CN201710575272 A CN 201710575272A CN 107188225 A CN107188225 A CN 107188225A
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- B82Y—SPECIFIC USES OR APPLICATIONS OF NANOSTRUCTURES; MEASUREMENT OR ANALYSIS OF NANOSTRUCTURES; MANUFACTURE OR TREATMENT OF NANOSTRUCTURES
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- C01P2004/80—Particles consisting of a mixture of two or more inorganic phases
- C01P2004/82—Particles consisting of a mixture of two or more inorganic phases two phases having the same anion, e.g. both oxidic phases
Abstract
The present invention relates to transparent heat-insulated electrical-conductive nanometer field of material technology, and in particular to a kind of indium-doped antimony oxidation tin nano-powder and preparation method thereof, the preparation method comprises the following steps：（1）It is dissolved in after antimonic salt, pink salt and indium salts are mixed in acid solution, obtains solution A；Alkaline precipitating agent and surfactant are dissolved in deionized water successively, solution B is obtained；（2）Solution A is added in solution B under stirring, after reaction terminates, ageing obtains solution C；（3）Solution C is centrifuged, isolated precipitation is washed, dried, is ground, sintering processes, indium-doped antimony oxidation tin nano-powder is obtained.The preparation method of the present invention, technique is simple, safety, reaction condition are gentle, preparation cost is low, be easily achieved industrialized production, and significantly improves the problem of nano-powder is easily reunited in process of production.The particle diameter of indium-doped antimony oxidation tin nano-powder produced by the present invention is small, and particle diameter distribution is narrow, reunites few, is with a wide range of applications.
Description
Technical field
The present invention relates to transparent heat-insulated electrical-conductive nanometer field of material technology, and in particular to a kind of indium-doped antimony oxidation tin nano powder
Body and preparation method thereof.
Background technology
Antimony-doped tin oxide, tin-doped indium oxide, indium antimony-doped tin oxide are all N-type semiconductor materials.This kind of material
Nanometer grade powder has special optical property and electric property, is a kind of novel and multifunctional transparent with tremendous expansion potentiality
Conductive material（TransparentConductiveOxides）, this material is generally called TCOs materials.TCOs materials are can
See that optical wavelength range has good transmissivity, be also equipped with electric conductivity.Therefore TCOs films and coating have in high-tech area
It is widely applied very much, it has stronger advantage than conventional conducting materials and anti-static material.The electric conductivity of TCOs materials is high, when
When addition is seldom, it will make plastics, coating, fiber etc. have anlistatig function.The optical property of TCOs materials
Good, with light-coloured transparent, the film that this material is prepared possesses good transmitance in visible-range, and to purple
Outside line and infrared ray have good absorption and reflecting properties, so that prevent ultraviolet and infrared ray from passing through, therefore its film has
Standby heat-insulation and heat-preservation and radiation resistance, and the influence of its strength of materials light is smaller, thus low emissivity glass for building, infrared suction
Receiving heat-barrier material usually needs to use this material.The stability and weather resistance of TCOs materials are also fine, are commonly used for antistatic
The influence very little of the preparation of material, weather and use environment to it, and acid and alkali-resistance.TCOs materials possess shielding property, root
According to this performance, this material is used to prepare computer room, the shielding protection area of radar, the transparency window of anti-electromagnetic interference.
In the prior art, TCOs materials are generally produced using binary system, in order to solve different metal salt in binary system
And its hydrolysate solubility it is inconsistent the problem of and in order to control the size of powder to be usually taken method be extra quality drop
Adduction controls pH value, but this preparation technology complexity is difficult to amplify, prepares cost height, is produced in addition using ternary system
During TCOs materials, because ternary system material is more more than the material of binary system, its dissolubility difference is also just bigger, while
The changes in solubility for meeting three kinds of metal salts and three kinds of hydroxide is also a very big problem.
The content of the invention
In order to overcome shortcoming and defect present in prior art, aoxidized it is an object of the invention to provide a kind of indium-doped antimony
The preparation method of tin nano-powder, the preparation method technique is simple, and safety, reaction condition is gentle, and preparation cost is low, largely
Improve the problem of nano-powder is easily reunited in production, it is easy to amplify, industrialized production can be realized.
Another object of the present invention is to provide a kind of indium-doped antimony oxidation tin nano-powder, the indium-doped antimony oxidation tin nano powder
Body particle diameter is small, and particle diameter distribution is narrow, and powder reuniting is few, is with a wide range of applications.
The purpose of the present invention is achieved through the following technical solutions：A kind of preparation method of indium-doped antimony oxidation tin nano-powder,
Comprise the following steps：
（1）It is dissolved in after antimonic salt, pink salt and indium salts are mixed in acid solution, obtains solution A；By alkaline precipitating agent and surfactant
It is dissolved in successively in deionized water, obtains solution B；
（2）Solution A is added in solution B under stirring, after reaction terminates, ageing obtains solution C；
（3）Solution C is centrifuged, isolated precipitation is washed, dried, is ground, sintering processes, indium-doped antimony oxygen is obtained
Change tin nano-powder.
Then the preparation method of the present invention occurs altogether using acid solution dissolving antimonic salt, pink salt and indium salts with alkaline precipitating agent
Precipitation reaction, isolated precipitation is washed, dried, is ground, sintering processes, obtains indium-doped antimony oxidation tin nano powder
Body, technique is simple, and safety, reaction condition is gentle, and preparation cost is low, significantly improves nano-powder and easily rolls into a ball in production
Poly- the problem of, it is easy to amplify, industrialized production can be realized.
It is preferred that, the step（1）In, surfactant is anionic surfactant, the anionic surface
Activating agent is in neopelex, stearic acid, dioctyl succinate disulfonate acid, sodium glycocholate and lauryl sodium sulfate
One or more.Another preferred, surfactant is by neopelex, lauryl sodium sulfate and dioctyl
Sodium sulfosuccinate is using weight ratio as 2.2-3.5：1.5-2.3:1 compounding is formed, and wherein the weight of surfactant is heavy for alkalescence
The 0.8%-1.2% of the weight of shallow lake agent.The present invention reduces the surface energy of precipitated product, prevented by using above-mentioned surfactant
Precipitated product wadding is poly-, makes obtained indium-doped antimony oxidation tin particle diameter of nanometer powder small, and narrowly distributing is reunited small.
It is preferred that, the antimonic salt is SbF3、SbF5、SbCl3And SbCl5In one or more；The pink salt is SnCl4·
5H2O、SnCl2、Sn(NO3)2、Sn(NO3)4And SnF2In one or more；The indium salts are InCl3·4H2O、In(NO3)3、
InF3、InF2And InCl2In one or more.Another preferred, antimonic salt is that antimony halides, pink salt are that tin halides, indium salts are halogenation
Indium；Another preferred, antimonic salt is that trichloride antimony, pink salt are that stannic chloride pentahydrate, indium salts are four water indium trichlorides, and the present invention passes through
Using above-mentioned antimonic salt, pink salt and indium salts, obtained indium-doped antimony oxidation tin particle diameter of nanometer powder is small, narrowly distributing, and reunite small, very great Cheng
That spends improves the problem of nano-powder is easily reunited in process of production.
It is preferred that, the step（1）In, the mol ratio of antimonic salt, pink salt and indium salts is 15-20：1-4:1；It is another preferred,
The mol ratio of antimonic salt, pink salt and indium salts is 16-18：2-3:1；Another preferred, the mol ratio of antimonic salt, pink salt and indium salts is 18：
2:1, the present invention is by using the ratio between amount of material of above-mentioned antimonic salt, pink salt and indium salts, obtained indium-doped antimony oxidation tin nano powder
Body particle diameter is small, narrowly distributing, reunites small, significantly improves the problem of nano-powder is easily reunited in process of production.
It is preferred that, the step（1）In, the H of the acid solution+Concentration is 1.8-2.2mol/L, the acid solution
For the one or more in hydrochloric acid, nitric acid, oxalic acid, acetic acid, tartaric acid and citric acid；Another preferred, the acid solution is
Hydrochloric acid, the H of the hydrochloric acid+Concentration is 2mol/L.The hydrolysate of antimonic salt, pink salt and indium salts is antimony hydroxide, hydroxide respectively
Tin and indium hydroxide, three kinds of hydroxide are all insoluble in water, although have a certain degree of dissolving in an acidic solution, but it
Solubility it is different, and the hydrogen ion that three kinds of metal salts are produced in hydrolytic process can strengthen the acidity of solution again,
If result in the acidity of solution A during the course of the reaction becomes too small, then the salt of water is insoluble in solution A to be separated out；Such as
The acidity of fruit solution A becomes too much, then the hydroxide of three kinds of metals produced by reaction will dissolve so that product is reduced
Or disappear；If acidity fluctuates, then the hydroxide for three kinds of metals that reaction is produced will dissolve to be separated out again, and by
In the different solubility of the hydroxide of three kinds of metals, its precipitation order is also different, influences the uniformity of product.In order to obtain
The mixed solution A of one clarification is, it is necessary to keep the acidity of whole reaction system in whole reaction progress to be at a narrow model
In enclosing, so selection H+Concentration for 1.8-2.2mol/L acid solution by three kinds of metal salt mixed dissolutions, obtain solution A, this
Invention is by selecting H+Three kinds of metal salt mixed dissolutions are obtained homogeneous clarification by the acid solution that concentration is 1.8-2.2mol/L
Mixed solution A, makes obtained indium-doped antimony oxidation tin particle diameter of nanometer powder small, and narrowly distributing is reunited small, significantly improves and receive
The problem of ground rice body is easily reunited in process of production.
It is preferred that, the step（1）In, alkaline precipitating agent is alkalescent precipitating reagent, and the alkalescent precipitating reagent is urea
And/or ammoniacal liquor, the ratio between the amount of the material of the alkalescent precipitating reagent and the amount of anion total material of antimonic salt, pink salt and indium salts are
1-5:1.Another preferred, alkaline precipitating agent is urea, the amount of the material of urea and the total thing of anion of antimonic salt, pink salt and indium salts
The ratio between amount of matter is 3-5:1, the cost of urea is relatively low, and urea is a kind of neutral substance, is hardly decomposed at normal temperatures,
Can just slowly release ammonia under the catalysis of acid, using this principle, by the acid solution of antimonic salt, pink salt and indium salts be slowly added dropwise into
In the aqueous solution of urea, occurs coprecipitation reaction.The present invention makes the antimonic salt after dissolving, tin by using above-mentioned alkaline precipitating agent
With alkaline precipitating agent coprecipitation reaction can occur for salt and indium salts, and obtained indium-doped antimony oxidation tin particle diameter of nanometer powder is small, distribution
It is narrow, reunite small, significantly improve the problem of nano-powder is easily reunited in process of production.
It is preferred that, the step（1）In, alkaline precipitating agent and surfactant are dissolved in the process in deionized water successively
Carry out in a heated state, heating-up temperature is 75-85 DEG C, another preferred, heating-up temperature is 78-82 DEG C, and concrete operations are will
Alkaline precipitating agent is added into three-necked flask, and magnetic agitation is used in oil bath heating, heating process, and three-necked flask adds cooling to circulate
Water cooling.Urea is a kind of neutral substance, and urea is hardly decomposed at normal temperatures, only by Urea to 160 degrees Celsius
Left and right urea can just decompose generation ammonia, if the reaction temperature of this reaction is risen into 160 degrees Celsius, can cause solution boiling production
Raw a large amount of aeration reactions are carried out.
It is preferred that, the step（2）In, the process that solution A is added into solution B is carried out in a heated state, heating-up temperature
For 75-85 DEG C, time for adding is 1-3h.It is another preferred, solution A is slowly dropped into solution B using constant pressure funnel
Row reaction, after dripping, continues to react 2h.By the present invention in that being instilled solution A in solution B with constant pressure funnel, make anti-
Answer the acidity of solution to maintain a weaker scope, make B solution slow release ammonia under the catalysis of acid, ammonia is dissolved in solution
Middle generation ammoniacal liquor, ammoniacal liquor can with the corresponding hydroxide of reacting metal salt generation in solution A, on the one hand generation ammoniacal liquor with it is molten
Acid reaction in liquid A reduces the acidity of solution, on the other hand, the metal salt hydrolysis generation H in solution A+Acidity can be strengthened again, led to
The factors such as the concentration for controlling each raw material, reaction temperature, rate of addition, charge ratio are crossed, the acidity of reaction system is maintained one
Individual suitable scope, so as to be copolymerized precipitation reaction, the present invention, with reference to the catalysis of acid, is made by setting above heating-up temperature
Urea is that decomposable asymmetric choice net produces ammonia in relatively low temperature, makes reaction temperature relatively low, safe and reliable, preparation technology is simple, operable
Property it is strong, save energy consumption, make obtained indium-doped antimony oxidation tin particle diameter of nanometer powder small, narrowly distributing is reunited small, significantly improve
The problem of nano-powder is easily reunited in process of production, obtained indium-doped antimony oxidation tin particle diameter of nanometer powder is small, narrowly distributing, group
It is poly- small, the problem of nano-powder is easily reunited in process of production is significantly improved, this preparation method is simple and easy to apply, reacted
Condition is easily-controllable, is easy to industrialized production and amplification.
It is preferred that, the step（2）In, digestion time is 1.5-3.0h.Another preferred, digestion time is set to 1.5-
In 2h, ageing process, close stirring and heat, it is still aging.The present invention makes coprecipitation reaction by setting above digestion time
More completely, product crystallization is more complete, and obtained indium-doped antimony oxidation tin particle diameter of nanometer powder is small, narrowly distributing, and reunite small, very great Cheng
That spends improves the problem of nano-powder is easily reunited in process of production.
It is preferred that, the step（3）In, it is 6.0-7.0 that precipitation, which makes to be washed with deionized to pH value, then is washed with ethanol
Wash.Specifically, by step（3）In obtained reaction product add in centrifugal bottle, dispersed with stirring is uniform, with centrifuge, falls
Go out supernatant liquor and obtain bottom sediment, precipitation is first 6.0-7.0 with deionized water centrifuge washing to pH value, afterwards again to through go from
Add ethanol in the precipitation that sub- water washing is crossed, be well mixed and ultrasonic disperse, then be centrifuged, after the completion of to pour out upper strata clear
Liquid, is so repeated several times, and the water in precipitation will be replaced completely by ethanol, further removes in indium-doped antimony oxidation tin nano-powder
Impurity, and washed using ethanol it is possible to prevente effectively from powder produces hard aggregation in drying sintering process, compared to
The vacuum filtration being usually taken is washed, the method for centrifuge washing, is not had due to the pressure that the removing of washing process reclaimed water is produced,
In addition the high surface energy of nano-powder, occurs the situation that the nano-powder of generation is easy to reunite.The present invention is by inciting somebody to action
It is 6.0-7.0 that precipitation, which is washed with deionized to pH value, is reused after ethanol washing, obtained indium-doped antimony oxidation tin nano-powder
Particle diameter is small, narrowly distributing, reunites small, significantly improves the problem of nano-powder is easily reunited in process of production.
It is preferred that, the step（3）In, drying temperature is 70-100 DEG C, and the time of drying is 4-8h, and sintering temperature is
550-650 DEG C, the time of sintering is 2-5h.It is another preferred, will be after precipitation drying, after being ground with mortar, after drying
Precipitation be placed in Muffle furnace, be sintered, be made indium-doped antimony oxidation tin nano-powder, drying temperature be 70-85 DEG C, during drying
Between be 4-5h, sintering temperature be 580-620 DEG C, sintering time is 2-3h.After the present invention is washed by using ethanol, then carry out low
Temperature is dried, and can not only avoid that reunites from producing but also can remove the impurity in product, the method for spray drying is fast compared to taking
Rapid-curing cutback is dry to avoid the method reunited, and does not have and produces substantial amounts of toxic gaseous hydrochlorides gas attack equipment, pollutes environment
The situation of side effect, and the method for taking spray drying, cause the impurity in product not also to be removed.The present invention is by adopting
With above drying temperature and drying time, sintering temperature and sintering time, obtained indium-doped antimony oxidation tin particle diameter of nanometer powder is small,
Narrowly distributing, reunites small, significantly improves the problem of nano-powder is easily reunited in process of production.
Another object of the present invention is achieved through the following technical solutions：A kind of indium-doped antimony oxidation tin nano-powder, it is described to mix
Indium antimony oxidation tin nano-powder is made according to above-mentioned preparation method.
The beneficial effects of the present invention are：The preparation method of the present invention dissolves antimonic salt, pink salt and indium salts using acid solution, so
Occur coprecipitation reaction with alkaline precipitating agent afterwards, isolated precipitation is washed, dried, is ground, sintering processes, must mix
Indium antimony oxidation tin nano-powder, technique is simple, and safety, reaction condition is gentle, prepares cost low, it is easy to accomplish industrialized production,
And significantly improve the problem of nano-powder is easily reunited in process of production.
The particle diameter of indium-doped antimony oxidation tin nano-powder produced by the present invention is small, and particle diameter distribution is narrow, and powder reuniting is few, with wide
General application value.
Indium-doped antimony oxidation tin nano-powder produced by the present invention has very strong shielding to ultraviolet and infrared ray, and right
Visible ray has good permeability, therefore is had broad application prospects in fields such as radiation proof, heat-insulation and heat-preservations.
Brief description of the drawings
Fig. 1 is the SEM image of indium-doped antimony oxidation tin nano-powder produced by the present invention；
Fig. 2 is the XRD scanning spectras of indium-doped antimony oxidation tin nano-powder produced by the present invention；
Fig. 3 is the UV-visible-near infrared absorption of indium-doped antimony oxidation tin nano-powder dispersion liquid produced by the present invention.
Embodiment
For the ease of the understanding of those skilled in the art, further is made to the present invention with reference to embodiment and accompanying drawing 1-3
Explanation, the content that embodiment is referred to not limitation of the invention.
Embodiment 1
A kind of preparation method of indium-doped antimony oxidation tin nano-powder, comprises the following steps：
（1）It is dissolved in after antimonic salt, pink salt and indium salts are mixed in acid solution, obtains solution A；By alkaline precipitating agent and surfactant
It is dissolved in successively in deionized water, obtains solution B；
（2）Solution A is added in solution B under stirring, after reaction terminates, ageing obtains solution C；
（3）Solution C is centrifuged, isolated precipitation is washed, dried, is ground, sintering processes, indium-doped antimony oxygen is obtained
Change tin nano-powder.
The step（1）In, surfactant is neopelex.
The step（1）In, the mol ratio of antimonic salt, pink salt and indium salts is 15：1:1, the antimonic salt is SbF5, the pink salt
For SnCl4·5H2O, the indium salts are InCl3·4H2O。
The step（1）In, the acid solution is the citric acid that concentration is 1.8mol/L；The alkaline precipitating agent is weak
Alkaline precipitating agent, the alkalescent precipitating reagent is ammoniacal liquor, and the amount of the material of ammoniacal liquor is the total of the anion of antimonic salt, pink salt and indium salts
1 times of the amount of material.
The step（1）In, the process that alkaline precipitating agent and surfactant are dissolved in deionized water successively is being heated
Carried out under state, heating-up temperature is 75 DEG C.
The step（2）In, solution A is instilled in solution B by constant pressure funnel, and this process is entered in a heated state
OK, heating-up temperature is 75 DEG C, and time for adding is 1h.
The step（2）In, digestion time is 1.5h.
The step（3）In, it is 6.0-7.0 that precipitation, which makes to be washed with deionized to pH value, then is washed with ethanol.
The step（3）In, drying temperature is 70 DEG C, and time of drying is 8h, and sintering temperature is 550 DEG C, sintering when
Between be 5h.
Embodiment 2
The present embodiment and the difference of embodiment 1 are:
The step（1）In, surfactant is stearic acid.
The step（1）In, the mol ratio of antimonic salt, pink salt and indium salts is 16：2:1, the antimonic salt is SbF3, the pink salt
For SnCl2, the indium salts are In (NO3)3。
The step（1）In, the acid solution is the oxalic acid that concentration is 1.9mol/L；The alkaline precipitating agent is weak base
Property precipitating reagent, the alkalescent precipitating reagent is urea, the amount of the material of urea for the anion of antimonic salt, pink salt and indium salts total thing
3 times of the amount of matter.
The step（1）In, the process that alkaline precipitating agent and surfactant are dissolved in deionized water successively is being heated
Carried out under state, heating-up temperature is 78 DEG C.
The step（2）In, solution A is instilled in solution B by constant pressure funnel, and this process is entered in a heated state
OK, heating-up temperature is 78 DEG C, and time for adding is 1.5h.
The step（2）In, digestion time is 2.0h.
The step（3）In, it is 6.0-7.0 that precipitation, which makes to be washed with deionized to pH value, then is washed with ethanol.
The step（3）In, drying temperature is 75 DEG C, and time of drying is 7h, and sintering temperature is 580 DEG C, sintering when
Between be 4h.
Embodiment 3
The difference of the present embodiment and Examples 1 and 2 is：
The step（1）In, surfactant is the sour sulphur of neopelex, lauryl sodium sulfate and dioctyl succinate
Sour sodium is using weight ratio as 2.2：1.5:1 compounding is formed.
The step（1）In, the mol ratio of antimonic salt, pink salt and indium salts is 17：3:1, the antimonic salt is SbCl3And SbCl5Press
According to mol ratio 1:1 compounding is formed, and the pink salt is SnCl4·5H2O、SnCl2According to mol ratio 1:1 compounding is formed, the indium salts
For InCl3·4H2O and InCl2According to mol ratio 2:1 compounding is formed.
The step（1）In, the acid solution is citric acid, tartaric acid according to volume ratio 1:2 compoundings are formed, the acid
Property solution concentration be 2mol/L；The alkaline precipitating agent is alkalescent precipitating reagent, and the alkalescent precipitating reagent is urea, urea
The amount of material be 4 times of amount of the total material of the anion of antimonic salt, pink salt and indium salts.
The step（1）In, the process that alkaline precipitating agent and surfactant are dissolved in deionized water successively is being heated
Carried out under state, heating-up temperature is 80 DEG C.
The step（2）In, solution A is instilled in solution B by constant pressure funnel, and this process is entered in a heated state
OK, heating-up temperature is 80 DEG C, and time for adding is 2h.
The step（2）In, digestion time is 2.5h.
The step（3）In, it is 6.0-7.0 that precipitation, which makes to be washed with deionized to pH value, then is washed with ethanol.
The step（3）In, drying temperature is 80 DEG C, and time of drying is 4h, and sintering temperature is 600 DEG C, sintering when
Between be 4h.
Embodiment 4
The difference of the present embodiment and embodiment 1-3 is：
The step（1）In, surfactant is neopelex.
The step（1）In, the mol ratio of antimonic salt, pink salt and indium salts is 18：2:1, the antimonic salt is SbCl3, the tin
Salt is SnCl4·5H2O, the indium salts are InCl3·4H2O。
The step（1）In, the acid solution is the hydrochloric acid that concentration is 2.1mol/L；The alkaline precipitating agent is weak base
Property precipitating reagent, the alkalescent precipitating reagent is urea, the amount of the material of urea for the anion of antimonic salt, pink salt and indium salts total thing
5 times of the amount of matter.
The step（1）In, the process that alkaline precipitating agent and surfactant are dissolved in deionized water successively is being heated
Carried out under state, heating-up temperature is 80 DEG C.
It is preferred that, the step（2）In, solution A is instilled in solution B by constant pressure funnel, and this process is in heating shape
Carried out under state, heating-up temperature is 80 DEG C, and time for adding is 2h.
It is preferred that, the step（2）In, digestion time is 2h.
It is preferred that, the step（3）In, it is 6.0-7.0 that precipitation, which makes to be washed with deionized to pH value, then is washed with ethanol
Wash.
The step（3）In, drying temperature is 80 DEG C, and time of drying is 4h, and sintering temperature is 600 DEG C, sintering when
Between be 2h.
Embodiment 5
The difference that the present embodiment relates to embodiment 1-4 is：
The step（1）In, surfactant is neopelex and sodium glycocholate according to weight ratio 2.2:1.5 compounding
Form.
The step（1）In, the mol ratio of antimonic salt, pink salt and indium salts is 19：3:1, the antimonic salt is SbCl3In one kind
Or it is several, the pink salt is Sn (NO3)2、Sn(NO3)4According to mol ratio 2:1 compounding is formed, and the indium salts are In (NO3)3。
The step（1）In, the acid solution is citric acid, tartaric acid and nitric acid according to volume ratio 1.5:1:0.5 answers
With into the concentration of the acid solution is 2.2mol/L；The alkaline precipitating agent is alkalescent precipitating reagent, and the alkalescent is sunk
Shallow lake agent is ammoniacal liquor, and the amount of the material of ammoniacal liquor is 2 times of the amount of the total material of the anion of antimonic salt, pink salt and indium salts.
The step（1）In, the process that alkaline precipitating agent and surfactant are dissolved in deionized water successively is being heated
Carried out under state, heating-up temperature is 85 DEG C.
The step（2）In, solution A is instilled in solution B by constant pressure funnel, and this process is entered in a heated state
OK, heating-up temperature is 85 DEG C, and time for adding is 3.0h.
The step（2）In, digestion time is 3.0h.
The step（3）In, it is 6.0-7.0 that precipitation, which makes to be washed with deionized to pH value, then is washed with ethanol.
The step（3）In, drying temperature is 90 DEG C, and time of drying is 6h, and sintering temperature is 620 DEG C, sintering when
Between be 3h.
Embodiment 6
The difference of the present embodiment and embodiment 1-5 is：
The step（1）In, surfactant is the sour sulphur of neopelex, lauryl sodium sulfate and dioctyl succinate
Sour sodium is using weight ratio as 3.5：2.3:1 compounding is formed.
The step（1）In, the mol ratio of antimonic salt, pink salt and indium salts is 20：4:1, the antimonic salt is, SbCl3And SbCl5
According to mol ratio 1:3 compoundings are formed, and the pink salt is SnF2In one or more, the indium salts be InF3And InF2According to rubbing
You compare 1:1 compounding is formed.
The step（1）In, the acid solution is hydrochloric acid, oxalic acid, acetic acid, tartaric acid according to volume ratio 1:1:1:1, institute
The concentration for stating acid solution is 2mol/L；The alkaline precipitating agent is alkalescent precipitating reagent, and the alkalescent precipitating reagent is urea,
The amount of the material of urea is 3.5 times of the amount of the total material of the anion of antimonic salt, pink salt and indium salts.
The step（1）In, the process that alkaline precipitating agent and surfactant are dissolved in deionized water successively is being heated
Carried out under state, heating-up temperature is 85 DEG C.
The step（2）In, solution A is instilled in solution B by constant pressure funnel, and this process is entered in a heated state
OK, heating-up temperature is 85 DEG C, and time for adding is 2.5h.
The step（2）In, digestion time is 3.0h.
The step（3）In, it is 6.0-7.0 that precipitation, which makes to be washed with deionized to pH value, then is washed with ethanol.
The step（3）In, drying temperature is 100 DEG C, and time of drying is 5.5h, sintering temperature for DEG C, sintering when
Between be 2.5h.
Embodiment 7
（1）Weigh urea：（0.405mol, 24.3g）, neopelex（0.2g）, 60ml deionization is dissolved in successively
In water；Aqueous solution of urea is added in 500ml three-necked flasks, magnetic agitation, 80 DEG C of oil bath heating, top adds cooling circulating water cold
But.
（2）Weigh SnCl4·5H2O（0.0225mol, 7.875g）；SbCl3（0.0025mol, 0.47g）；InCl3·4H2O
（0.00125mol, 0.49g）；The ratio between amount of material of three kinds of raw materials is 18：2：1；Three kinds of raw material mixed dissolutions are dense in 15ml
Spend in the hydrochloric acid for 2mol/L, the mixing hydrochloric acid solution of three kinds of metal salts of indium tin antimony is slowly dropped into step with constant pressure funnel
（1）In three-necked flask in, time for adding is 2h, is reacted again after dripping off and is aged 2h after the completion of 2h, reaction.
（3）By step（2）In obtained reaction product add in centrifugal bottle, dispersed with stirring is uniform, with centrifuge, falls
Go out supernatant liquor and obtain bottom sediment, precipitation is first 6.0-7.0 with deionized water centrifuge washing to pH value, afterwards again with ethanol from
The heart is washed；It will be deposited in after the completion of washing at 80 DEG C and dry 4h, be ground afterwards with mortar, finally by the precipitated powder after grinding
End is placed in Muffle furnace, 600 DEG C of sintering 2h, and indium-doped antimony oxidation tin nano-powder is made.
If Fig. 1 is the SEM image of indium-doped antimony oxidation tin nano-powder produced by the present invention, it can be seen that this reality
The average grain diameter for applying indium-doped antimony oxidation tin nano-powder made from example is 10nm-12nm, and pattern is ball-type, and particle diameter is small, particle diameter point
Cloth is narrower, and powder is more loose, soft-agglomerated less, hard aggregation-free.
If Fig. 2 is the XRD scanning spectras of indium-doped antimony oxidation tin nano-powder produced by the present invention, it can be seen that
The crystal formation of indium-doped antimony oxidation tin nano-powder belongs to tetragonal structure made from the present embodiment, with undoped with tin ash be all gold
Red stone configuration, but crystallinity decreases, reason is to result in distortion of lattice after doping.
If Fig. 3 is ultraviolet-visible-near infrared absorption light of indium-doped antimony oxidation tin nano-powder dispersion liquid produced by the present invention
Spectrum, it can be seen that prepared indium-doped antimony oxidation tin nano-powder dispersion liquid has higher visible light transmissivity, and
Ultraviolet and near-infrared is passed through with extremely excellent blocking effect.
Above-described embodiment is the present invention preferably implementation, and in addition, the present invention can be realized with other manner,
Any obvious replacement is within protection scope of the present invention on the premise of not departing from present inventive concept.
Claims (10)
1. a kind of preparation method of indium-doped antimony oxidation tin nano-powder, it is characterised in that：Comprise the following steps：
（1）It is dissolved in after antimonic salt, pink salt and indium salts are mixed in acid solution, obtains solution A；By alkaline precipitating agent and surfactant
It is dissolved in successively in deionized water, obtains solution B；
（2）Solution A is added under stirring and reacted in solution B, after reaction terminates, ageing obtains solution C；
（3）Solution C is centrifuged, isolated precipitation is washed successively, dried, is ground and sintering processes, must be mixed
Indium antimony oxidation tin nano-powder.
2. the preparation method of indium-doped antimony oxidation tin nano-powder according to claim 1, it is characterised in that：The step
（1）In, surfactant is anionic surfactant, and the anionic surfactant is DBSA
One or more in sodium, stearic acid, dioctyl succinate disulfonate acid, sodium glycocholate and lauryl sodium sulfate.
3. the preparation method of indium-doped antimony oxidation tin nano-powder according to claim 1, it is characterised in that：The step
（1）In, the mol ratio of antimonic salt, pink salt and indium salts is 15-20：1-4:1；The antimonic salt is SbF3、SbF5、SbCl3And SbCl5In
One or more；The pink salt is SnCl4·5H2O、SnCl2、Sn(NO3)2、Sn(NO3)4And SnF2In one or more；
The indium salts are InCl3·4H2O、In(NO3)3、InF3、InF2And InCl2In one or more.
4. the preparation method of indium-doped antimony oxidation tin nano-powder according to claim 1, it is characterised in that：The step
（1）In, the H of the acid solution+Concentration is 1.8-2.2mol/L, and the acid solution is hydrochloric acid, nitric acid, oxalic acid, acetic acid, wine
One or more in stone acid and citric acid；The alkaline precipitating agent is alkalescent precipitating reagent, and the alkalescent precipitating reagent is urine
The ratio between element and/or ammoniacal liquor, the amount of the material of the alkalescent precipitating reagent and amount of anion total material of antimonic salt, pink salt and indium salts
For 1-5:1.
5. the preparation method of indium-doped antimony oxidation tin nano-powder according to claim 1, it is characterised in that：The step
（1）In, the process that alkaline precipitating agent and surfactant are dissolved in deionized water successively is carried out in a heated state, heating temperature
Spend for 75-85 DEG C.
6. the preparation method of indium-doped antimony oxidation tin nano-powder according to claim 1, it is characterised in that：The step
（2）In, the process that solution A is added into solution B is carried out in a heated state, and heating-up temperature is 75-85 DEG C, and time for adding is 1-
3h。
7. the preparation method of indium-doped antimony oxidation tin nano-powder according to claim 1, it is characterised in that：The step
（2）In, digestion time is 1.5-3.0h.
8. the preparation method of indium-doped antimony oxidation tin nano-powder according to claim 1, it is characterised in that：The step
（3）In, it is 6.0-7.0 that washing, which makes to be washed with deionized to pH value, then is washed with ethanol.
9. the preparation method of indium-doped antimony oxidation tin nano-powder according to claim 1, it is characterised in that：The step
（3）In, drying temperature is 70-100 DEG C, and the time of drying is 4-8h, and sintering temperature is 550-650 DEG C, and the time of sintering is 2-
5h。
10. a kind of indium-doped antimony oxidation tin nano-powder, it is characterised in that：The indium-doped antimony oxidation tin nano-powder will according to right
The preparation method described in any one of 1-9 is asked to be made.
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