CN107188225B - 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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- CN107188225B CN107188225B CN201710575272.8A CN201710575272A CN107188225B CN 107188225 B CN107188225 B CN 107188225B CN 201710575272 A CN201710575272 A CN 201710575272A CN 107188225 B CN107188225 B CN 107188225B
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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, which includes the following steps：（1）It is dissolved in acid solution after antimonic salt, pink salt and indium salts are mixed, obtains solution A；Alkaline precipitating agent and surfactant are dissolved in deionized water successively, obtain solution B；（2）Solution A is added in solution B under stirring, after reaction, ageing obtains solution C；（3）Solution C is centrifuged, isolated precipitation is washed, is dried, is ground, sintering processes, obtains indium-doped antimony oxidation tin nano-powder.The preparation method of the present invention, simple for process, safety, reaction condition are mild, manufacturing cost is low, are easily industrialized production, and significantly improve the problem of nano-powder is easily reunited in process of production.The grain size 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 usually called TCOs materials.TCOs materials are can
Light-exposed wave-length coverage has good transmissivity, is 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
It is good, there is light-coloured transparent, the film that this material preparation comes out to have good transmitance in visible-range, and to purple
Outside line and infrared ray have good absorption and reflecting properties, and to prevent ultraviolet light and infrared ray from penetrating, 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
Heat-barrier material is received usually to need 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 have 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, generally use binary system produces TCOs materials, in order to solve different metal salt in binary system
And its inconsistent problem of hydrolysate solubility and be extra quality drop to control the method that the size of powder is usually taken
Adduction controls pH value, but this preparation process complexity is not easy to amplify, manufacturing cost is high, is in addition produced using ternary system
When TCOs materials, since ternary system substance is more than the substance of binary system, dissolubility difference also with regard to bigger, and at the same time
The changes in solubility for meeting three kinds of metal salts and three kinds of hydroxide is also a prodigious problem.
Invention content
In order to overcome shortcoming and defect existing in the prior art, the purpose of the present invention is to provide a kind of indium-doped antimony to aoxidize
The preparation method of tin nano-powder, the preparation method is simple for process, and safety, reaction condition is mild, and manufacturing cost is low, largely
Improve the problem of nano-powder is easily reunited in production, be easy to amplification, can realize industrialized production.
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 powders
Body grain size is small, and particle diameter distribution is narrow, and powder reuniting is few, is with a wide range of applications.
The purpose of the invention is achieved by the following technical solution：A kind of preparation method of indium-doped antimony oxidation tin nano-powder,
Include the following steps：
（1）It is dissolved in acid solution after antimonic salt, pink salt and indium salts are mixed, obtains solution A；Alkaline precipitating agent and surface are lived
Property agent is dissolved in successively in deionized water, obtains solution B；
（2）Solution A is added in solution B under stirring, after reaction, ageing obtains solution C；
（3）Solution C is centrifuged, isolated precipitation is washed, is dried, is ground, sintering processes, is obtained indium-doped
Antimony oxidation tin nano-powder.
Then the preparation method of the present invention is occurred altogether using acid solution dissolving antimonic salt, pink salt and indium salts with alkaline precipitating agent
Isolated precipitation is washed, is dried, being ground, sintering processes by precipitation reaction, obtains indium-doped antimony oxidation tin nano powder
Body, simple for process, safety, reaction condition is mild, and manufacturing cost is low, significantly improves nano-powder and easily rolls into a ball in production
Poly- problem is easy to amplification, can realize industrialized production.
Preferably, 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 2.2-3.5 with weight ratio：1.5-2.3:1 compounds, and wherein the weight of surfactant is that alkalinity is heavy
The 0.8%-1.2% of the weight of shallow lake agent.The present invention reduces the surface energy of precipitated product, prevents by using above-mentioned surfactant
Precipitated product wadding is poly-, keeps indium-doped antimony oxidation tin particle diameter of nanometer powder obtained small, and narrowly distributing is reunited small.
Preferably, the antimonic salt is SbF3、SbF5、SbCl3And SbCl5One or more of；The pink salt is SnCl4·
5H2O、SnCl2、Sn(NO3)2、Sn(NO3)4And SnF2One or more of；The indium salts are InCl3·4H2O、In(NO3)3、
InF3、InF2And InCl2One or more of.Another preferred, antimonic salt is antimony halides, pink salt is tin halides, indium salts are halogenation
Indium；Another preferred, antimonic salt is antimony trichloride, pink salt is 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, indium-doped antimony oxidation tin particle diameter of nanometer powder obtained is small, narrowly distributing, and reunite small, very great Cheng
Degree improves the problem of nano-powder is easily reunited in process of production.
Preferably, the step（1）In, the molar ratio of antimonic salt, pink salt and indium salts is 15-20：1-4:1；It is another preferred,
The molar ratio of antimonic salt, pink salt and indium salts is 16-18：2-3:1；Another preferred, the molar ratio of antimonic salt, pink salt and indium salts is 18：
2:1, the present invention is by using the ratio between the amount of substance of above-mentioned antimonic salt, pink salt and indium salts, indium-doped antimony oxidation tin nano powder obtained
Body grain size is small, narrowly distributing, reunites small, significantly improves the problem of nano-powder is easily reunited in process of production.
Preferably, the step（1）In, the H of the acid solution+A concentration of 1.8-2.2mol/L, the acid solution
For one or more of 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+A concentration of 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 there is a degree of dissolving in an acidic solution, it
Solubility it is different, and the hydrogen ion that is generated in hydrolytic process of three kinds of metal salts can enhance the acidity of solution again,
It results in during the reaction and is insoluble in the salt of water in solution A if the acidity of solution A becomes too small and will be precipitated；Such as
The acidity of fruit solution A becomes too much, then the hydroxide of three kinds of metals caused by reaction will dissolve so that product is reduced
Or it disappears；If acidity fluctuates, reacting the hydroxide of three kinds of metals of generation will dissolve and be precipitated again, and by
In the different solubility of the hydroxide of three kinds of metals, precipitation sequence is also different, influences the uniformity of product.In order to obtain
One clear mixed solution A needs to keep the acidity for entirely reacting entire reaction system in progress to be at a narrow model
In enclosing, so selection H+Three kinds of metal salt mixed dissolutions are obtained solution A by the acid solution of a concentration of 1.8-2.2mol/L, this
Invention is by selecting H+The acid solution of a concentration of 1.8-2.2mol/L obtains three kinds of metal salt mixed dissolutions uniform clear
Mixed solution A, keeps indium-doped antimony oxidation tin particle diameter of nanometer powder obtained small, and narrowly distributing reunites small, significantly improves and receive
The problem of rice flour body is easily reunited in process of production.
Preferably, the step（1）In, alkaline precipitating agent is alkalescent precipitating reagent, and the alkalescent precipitating reagent is urea
And/or ammonium hydroxide, the amount of the substance of the alkalescent precipitating reagent and the ratio between the amount of the 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 substance of urea and the total object 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, coprecipitation reaction occurs.The present invention makes dissolved antimonic salt, tin by using above-mentioned alkaline precipitating agent
With alkaline precipitating agent coprecipitation reaction can occur for salt and indium salts, and indium-doped antimony oxidation tin particle diameter of nanometer powder obtained is small, distribution
It is narrow, reunite small, significantly improves the problem of nano-powder is easily reunited in process of production.
Preferably, the step（1）In, the process that alkaline precipitating agent and surfactant is dissolved in successively in deionized water
It carries out in a heated state, heating temperature is 75-85 DEG C, another preferred, and heating temperature is 78-82 DEG C, and concrete operations are will
Alkaline precipitating agent is added into three-necked flask, and magnetic agitation uses oil bath heating, and in heating process, three-necked flask adds cooling cycle
Water cooling.Urea is a kind of neutral substance, and urea hardly decomposes 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 to 160 degrees Celsius, can lead to solution boiling production
Raw a large amount of aeration reactions carry out.
Preferably, the step（2）In, the process that solution A is added to solution B carries out in a heated state, heating temperature
It is 75-85 DEG C, time for adding 1-3h.It is another preferred, using constant pressure funnel by solution A be slowly dropped into solution B into
Row reaction, after dripping, the reaction was continued 2h.By the present invention in that being instilled solution A in solution B with constant pressure funnel, make anti-
It answers the acidity of solution to maintain a weaker range, B solution slow release ammonia, ammonia under the catalysis of acid is made to be dissolved in solution
Middle generation ammonium hydroxide, ammonium hydroxide can hydroxide corresponding with the generation of the reacting metal salt in solution A, on the one hand generate ammonium hydroxide with it is molten
Acid reaction in liquid A reduces the acidity of solution, and on the other hand, the metal salt hydrolysis in solution A generates H+Acidity can be enhanced 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 made to maintain one
A suitable range, to be copolymerized precipitation reaction, the present invention, in conjunction with the catalysis of acid, is made by the way that the above heating temperature is arranged
Urea generates ammonia in lower temperature, that is, decomposable asymmetric choice net, keeps reaction temperature relatively low, securely and reliably, preparation process is simple, operable
Property it is strong, save energy consumption, keep indium-doped antimony oxidation tin particle diameter of nanometer powder obtained small, narrowly distributing is reunited small, is significantly improved
The problem of nano-powder is easily reunited in process of production, indium-doped antimony oxidation tin particle diameter of nanometer powder obtained is small, narrowly distributing, group
It is poly- small, the problem of nano-powder is easily reunited in process of production is significantly improved, preparation method is simple for this, reaction
Condition is easily-controllable, is convenient for industrialized production and amplification.
Preferably, the step（2）In, digestion time 1.5-3.0h.Another preferred, digestion time is set as 1.5-
2h in ageing process, closes stirring and heating, still aging.The present invention makes coprecipitation reaction by the way that the above digestion time is arranged
More completely, product crystallization is more complete, and indium-doped antimony oxidation tin particle diameter of nanometer powder obtained is small, narrowly distributing, and reunite small, very great Cheng
Degree improves the problem of nano-powder is easily reunited in process of production.
Preferably, 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 ethyl alcohol
It washs.Specifically, by step（3）In obtained reaction product be added in centrifugal bottle, be dispersed with stirring uniformly, with centrifuge,
Go out supernatant liquor and obtain bottom sediment, precipitation is first 6.0-7.0 with deionized water centrifuge washing to pH value, later again to through go from
Ethyl alcohol is added in the precipitation that sub- water washing is crossed, is uniformly mixed simultaneously ultrasonic disperse, then be centrifuged, it is clear to pour out upper layer after the completion
Liquid makes the water in precipitation that will be replaced completely by ethyl alcohol repeatedly several times, further removes in indium-doped antimony oxidation tin nano-powder
Impurity, and washed using ethyl alcohol it is possible to prevente effectively from powder generates hard aggregation in drying sintering process, compared to
The method of the vacuum filtration washing, centrifuge washing that are usually taken, does not have the pressure generated due to the removing of water in washing process,
In addition the high surface energy of nano-powder, so that the nano-powder of generation is easy to, there is a situation where reunite with occurring.The present invention pass through by
It is 6.0-7.0 that precipitation, which is washed with deionized to pH value, after reusing ethyl alcohol washing, indium-doped antimony oxidation tin nano-powder obtained
Grain size is small, narrowly distributing, reunites small, significantly improves the problem of nano-powder is easily reunited in process of production.
Preferably, 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, after precipitation is dried, after being ground with mortar, after drying
Precipitation be placed in Muffle furnace, be sintered, indium-doped antimony oxidation tin nano-powder be made, drying temperature is 70-85 DEG C, when drying
Between be 4-5h, sintering temperature be 580-620 DEG C, sintering time 2-3h.After the present invention is washed by using ethyl alcohol, then carry out low
Temperature is dry, not only can to avoid reunion generation but also the impurity in product can be removed, compared to taking the method for spray drying fast
Rapid-curing cutback is dry to avoid the method reunited, and does not have and generates a large amount of toxic gaseous hydrochlorides gas attack equipment, pollutes environment
The case where side effect, and the method for taking spray drying, the impurity in product is caused also not to be removed.The present invention is by adopting
With the above drying temperature and drying time, sintering temperature and sintering time, indium-doped antimony oxidation tin particle diameter of nanometer powder obtained 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 is using acid solution dissolving antimonic salt, pink salt and indium salts, so
Coprecipitation reaction occurs with alkaline precipitating agent afterwards, isolated precipitation is washed, is dried, is ground, sintering processes, must be mixed
Indium antimony oxidation tin nano-powder, simple for process, safety, reaction condition is mild, and manufacturing cost is low, it is easy to accomplish industrialized production,
And significantly improve the problem of nano-powder is easily reunited in process of production.
The grain size 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, has wide
General application value.
Indium-doped antimony oxidation tin nano-powder produced by the present invention has very strong shielding to ultraviolet light and infrared ray, and right
Visible light has good permeability, therefore has broad application prospects in fields such as radiation protection, heat-insulation and heat-preservations.
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 ultraviolet-visible-near infrared absorption light of indium-doped antimony oxidation tin nano-powder dispersion liquid produced by the present invention
Spectrum.
Specific implementation mode
For the ease of the understanding of those skilled in the art, the present invention is made with reference to embodiment and attached drawing 1-3 further
Explanation, the content that embodiment refers to not is limitation of the invention.
Embodiment 1
A kind of preparation method of indium-doped antimony oxidation tin nano-powder, includes the following steps：
（1）It is dissolved in acid solution after antimonic salt, pink salt and indium salts are mixed, obtains solution A；Alkaline precipitating agent and surface are lived
Property agent is dissolved in successively in deionized water, obtains solution B；
（2）Solution A is added in solution B under stirring, after reaction, ageing obtains solution C；
（3）Solution C is centrifuged, isolated precipitation is washed, is dried, is ground, sintering processes, is obtained indium-doped
Antimony oxidation tin nano-powder.
The step（1）In, surfactant is neopelex.
The step（1）In, the molar 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 of a concentration of 1.8mol/L；The alkaline precipitating agent is weak
Alkaline precipitating agent, the alkalescent precipitating reagent are ammonium hydroxide, and the amount of the substance of ammonium hydroxide is the total of the anion of antimonic salt, pink salt and indium salts
1 times of the amount of substance.
The step（1）In, the process that alkaline precipitating agent and surfactant are dissolved in successively in deionized water is being heated
It is carried out under state, heating temperature is 75 DEG C.
The step（2）In, solution A by constant pressure funnel instill solution B in, this process in a heated state into
Row, heating temperature are 75 DEG C, time for adding 1h.
The step（2）In, digestion time 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 ethyl alcohol.
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 embodiment 1 difference lies in:
The step（1）In, surfactant is stearic acid.
The step（1）In, the molar 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 of a concentration of 1.9mol/L；The alkaline precipitating agent is weak base
Property precipitating reagent, the alkalescent precipitating reagent is urea, and the amount of the substance of urea is total object of the anion of antimonic salt, pink salt and indium salts
3 times of the amount of matter.
The step（1）In, the process that alkaline precipitating agent and surfactant are dissolved in successively in deionized water is being heated
It is carried out under state, heating temperature is 78 DEG C.
The step（2）In, solution A by constant pressure funnel instill solution B in, this process in a heated state into
Row, heating temperature are 78 DEG C, time for adding 1.5h.
The step（2）In, digestion time 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 ethyl alcohol.
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 present embodiment and Examples 1 and 2 difference lies in：
The step（1）In, surfactant is neopelex, lauryl sodium sulfate and dioctyl succinate
Disulfonate acid is with weight ratio for 2.2：1.5:1 compounds.
The step（1）In, the molar ratio of antimonic salt, pink salt and indium salts is 17：3:1, the antimonic salt is SbCl3And SbCl5It presses
According to molar ratio 1:1 compounds, and the pink salt is SnCl4·5H2O、SnCl2According to molar ratio 1:1 compounds, the indium salts
For InCl3·4H2O and InCl2According to molar ratio 2:1 compounds.
The step（1）In, the acid solution is citric acid, tartaric acid according to volume ratio 1:2 compound, the acid
A concentration of 2mol/L of property solution；The alkaline precipitating agent is alkalescent precipitating reagent, and the alkalescent precipitating reagent is urea, urea
The amount of substance be 4 times of amount of total material of anion of antimonic salt, pink salt and indium salts.
The step（1）In, the process that alkaline precipitating agent and surfactant are dissolved in successively in deionized water is being heated
It is carried out under state, heating temperature is 80 DEG C.
The step（2）In, solution A by constant pressure funnel instill solution B in, this process in a heated state into
Row, heating temperature are 80 DEG C, time for adding 2h.
The step（2）In, digestion time 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 ethyl alcohol.
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 present embodiment and embodiment 1-3 difference lies in：
The step（1）In, surfactant is neopelex.
The step（1）In, the molar 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 of a concentration of 2.1mol/L；The alkaline precipitating agent is weak base
Property precipitating reagent, the alkalescent precipitating reagent is urea, and the amount of the substance of urea is total object of the anion of antimonic salt, pink salt and indium salts
5 times of the amount of matter.
The step（1）In, the process that alkaline precipitating agent and surfactant are dissolved in successively in deionized water is being heated
It is carried out under state, heating temperature is 80 DEG C.
Preferably, the step（2）In, solution A is instilled by constant pressure funnel in solution B, this process is in heating shape
It is carried out under state, heating temperature is 80 DEG C, time for adding 2h.
Preferably, the step（2）In, digestion time 2h.
Preferably, 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 ethyl alcohol
It washs.
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 present embodiment relate to embodiment 1-4 difference lies in：
The step（1）In, surfactant is neopelex and sodium glycocholate according to weight ratio 2.2:1.5
It compounds.
The step（1）In, the molar 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 molar ratio 2:1 compounds, 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 is multiple
With into a concentration of 2.2mol/L of the acid solution；The alkaline precipitating agent is alkalescent precipitating reagent, and the alkalescent is heavy
Shallow lake agent is ammonium hydroxide, and the amount of the substance of ammonium hydroxide 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 successively in deionized water is being heated
It is carried out under state, heating temperature is 85 DEG C.
The step（2）In, solution A by constant pressure funnel instill solution B in, this process in a heated state into
Row, heating temperature are 85 DEG C, time for adding 3.0h.
The step（2）In, digestion time 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 ethyl alcohol.
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 present embodiment and embodiment 1-5 difference lies in：
The step（1）In, surfactant is neopelex, lauryl sodium sulfate and dioctyl succinate
Disulfonate acid is with weight ratio for 3.5：2.3:1 compounds.
The step（1）In, the molar ratio of antimonic salt, pink salt and indium salts is 20：4:1, the antimonic salt is SbCl3And SbCl5
According to molar ratio 1:3 compound, and the pink salt is SnF2One or more of, the indium salts are InF3And InF2According to rubbing
That ratio 1:1 compounds.
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
State a concentration of 2mol/L of acid solution；The alkaline precipitating agent is alkalescent precipitating reagent, and the alkalescent precipitating reagent is urea,
The amount of the substance 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 successively in deionized water is being heated
It is carried out under state, heating temperature is 85 DEG C.
The step（2）In, solution A by constant pressure funnel instill solution B in, this process in a heated state into
Row, heating temperature are 85 DEG C, time for adding 2.5h.
The step（2）In, digestion time 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 ethyl alcohol.
The step（3）In, drying temperature is 100 DEG C, and time of drying is 5.5h, and sintering temperature is DEG C, sintering when
Between be 2.5h.
Embodiment 7
（1）Weigh urea：（0.405mol, 24.3g）, neopelex（0.2g）, it is dissolved in going for 60ml successively
In ionized water；Aqueous solution of urea is added in 500ml three-necked flasks, magnetic agitation, 80 DEG C of oil bath heating, top adds cooling cycle
Water cooling.
（2）Weigh SnCl4·5H2O（0.0225mol, 7.875g）；SbCl3（0.0025mol, 0.47g）；InCl3·4H2O
（0.00125mol, 0.49g）；The ratio between amount of substance of three kinds of raw materials is 18：2：1；Three kinds of raw material mixed dissolutions are dense in 15ml
Degree is that the mixing hydrochloric acid solution of three kinds of metal salts of indium tin antimony is slowly dropped into step with constant pressure funnel in the hydrochloric acid of 2mol/L
（1）In three-necked flask in, time for adding 2h reacts 2h again after dripping off, 2h is aged after the completion of reaction.
（3）By step（2）In obtained reaction product be added in centrifugal bottle, be dispersed with stirring uniformly, with centrifuge,
Go out supernatant liquor and obtain bottom sediment, precipitation is first 6.0-7.0 with deionized water centrifuge washing to pH value, use again later ethyl alcohol from
The heart washs；It will be deposited in after the completion of washing at 80 DEG C and dry 4h, be ground later with mortar, finally by the precipitated powder after grinding
End is placed in Muffle furnace, and indium-doped antimony oxidation tin nano-powder is made in 600 DEG C of sintering 2h.
If Fig. 1 is the SEM image of indium-doped antimony oxidation tin nano-powder produced by the present invention, it can be seen from the figure 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 grain size is small, grain size point
Cloth is relatively narrow, 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 from the figure that
The crystal form of indium-doped antimony oxidation tin nano-powder made from the present embodiment belongs to tetragonal structure, is all gold with undoped stannic oxide
Red stone configuration, but crystallinity decreases, the reason is that resulting 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 from the figure that prepared indium-doped antimony oxidation tin nano-powder dispersion liquid has higher visible light transmittance, and
Being penetrated to ultraviolet and near-infrared has extremely excellent blocking effect.
Above-described embodiment is the preferable implementation of the present invention, and in addition to this, the present invention can be realized with other manner,
Any obvious replacement is not departed under the premise of present inventive concept within protection scope of the present invention.
Claims (7)
1. a kind of preparation method of indium-doped antimony oxidation tin nano-powder, it is characterised in that：Include the following steps：
（1）It is dissolved in acid solution after antimonic salt, pink salt and indium salts are mixed, obtains solution A；By alkaline precipitating agent and surfactant
It is dissolved in deionized water successively, obtains solution B；
（2）Solution A is added in solution B under stirring and is reacted, after reaction, ageing obtains solution C；
（3）Solution C is centrifuged, isolated precipitation is washed successively, is dried, is ground and sintering processes, must be mixed
Indium antimony oxidation tin nano-powder；
The step（1）In, the H of the acid solution+A concentration of 1.8-2.2mol/L, the alkaline precipitating agent are heavy for alkalescent
Shallow lake agent, the alkalescent precipitating reagent are urea, the amount of the amount of the substance of urea and the anion total material of antimonic salt, pink salt and indium salts
The ratio between be 3-5:1；The molar ratio of the antimonic salt, pink salt and indium salts is 15-20：1-4:1；The weight of the surfactant is alkali
The 0.8%-1.2% of the weight of property precipitating reagent；The step（2）In, solution A is instilled in solution B using constant pressure funnel, it will
The process that solution B is added in solution A carries out in a heated state, and heating temperature is 75-85 DEG C；The step（3）In, washing uses
It is 6.0-7.0 that deionized water, which is washed to pH value, then is washed with ethyl alcohol；Indium-doped antimony oxidation tin nano-powder made from the preparation method
Average grain diameter be 10nm-12nm；The crystal form of the indium-doped antimony oxidation tin nano-powder belongs to tetragonal structure.
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 dodecyl benzene sulfonic acid
One or more of 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 antimonic salt is SbF3、SbF5、SbCl3And SbCl5One or more of；The pink salt is SnCl4·5H2O、
SnCl2、Sn(NO3)2、Sn(NO3)4And SnF2One or more of；The indium salts are InCl3·4H2O、In(NO3)3、InF3、
InF2And InCl2One or more of.
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 acid solution is one or more of hydrochloric acid, nitric acid, oxalic acid, acetic acid, tartaric acid and citric acid.
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, alkaline precipitating agent and surfactant are dissolved in the process in deionized water successively and carried out in a heated state, heating temperature
Degree is 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, digestion time 1.5-3.0h.
7. 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。
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