CN102583511A - Nanometer tin oxide compositely doped with ytterbium, bismuth, indium and antimony and preparation method thereof - Google Patents
Nanometer tin oxide compositely doped with ytterbium, bismuth, indium and antimony and preparation method thereof Download PDFInfo
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- CN102583511A CN102583511A CN2012100324726A CN201210032472A CN102583511A CN 102583511 A CN102583511 A CN 102583511A CN 2012100324726 A CN2012100324726 A CN 2012100324726A CN 201210032472 A CN201210032472 A CN 201210032472A CN 102583511 A CN102583511 A CN 102583511A
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Abstract
The invention discloses nanometer tin oxide compositely doped with ytterbium, bismuth, indium and antimony and a preparation method thereof. Four elements which are ytterbium, bismuth, indium and antimony are compositely doped into nanometer tin oxide powder in an ultrasonic chemical method, the advantages of absorption of ytterbium to infrared, good conductivity of indium, good electric conductivity and light transmission performance of bismuth and antimony and the like are combined, the nanometer tin oxide compositely doped with ytterbium, bismuth, indium and antimony is obtained, and the obtained nanometer powder is good in electric conductivity, light transmission rate and thermal insulation effect. The invention further provides the preparation method of the nanometer tin oxide compositely doped with ytterbium, bismuth, indium and antimony, the cavitation effect of ultrasonic is utilized to generate the conditions of high temperature and high pressure, a method of organic solvent washing is combined so that the efficiency of separating a precursor is improved, and the nanometer powder with five elements compositely doped is efficiently prepared. The preparation method is simple, uniformized doping can be achieved, and the prepared powder is little in agglomeration and small in grain size and is dispersed evenly.
Description
Technical field
The present invention relates to field of nanometer material technology, relate in particular to composite mixed nano-stannic oxide of a kind of ytterbium bismuth indium antimony and preparation method thereof.
Background technology
Have lattice distortion easily in the independent stannic oxide nano powder of mixing indium, cause hole mobility to decline to a great extent, the resistivity of the feasible film of processing is difficult to further reduction, restricts the raising of this film conductivity ability.And the ATO that stibium doping stannic oxide makes (Antimony Doped Tin Oxide, tin-antiomony oxide) is when nano-powder is used for the heat-insulation and heat-preservation of building glass, the shortcoming that has that thermal insulation is relatively poor, visible light transmissivity is lower etc.
In addition, the preparation method of nano-powder mainly is liquid-phase coprecipitation, microemulsion method, hydrothermal method, spray pyrolysis etc.But though the coprecipitation method processing parameter is controlled easily, production cost is lower, reunites easily, and diameter of particle is inhomogeneous; The microemulsion method combined coefficient is lower, and the aftertreatment of precursor is difficulty relatively, and cost is also higher; The equipment requirements of hydrothermal method is very high, and the Cl in the hydro-thermal raw material
-Can produce corrosion to kettle, and the corrosion of autoclave further compares danger to what produce; The efficiency ratio of spray pyrolysis is lower, and powder is not had cost advantage.
Therefore, prior art awaits to improve and development.
Summary of the invention
Deficiency in view of above-mentioned prior art; The object of the present invention is to provide composite mixed nano-stannic oxide of a kind of ytterbium bismuth indium antimony and preparation method thereof; Adopt the sonochemistry method to mix nano tin oxide powder to ytterbium, bismuth, indium and four kinds of elements compounding of antimony, method is simple, can realize even doping; The powder reuniting of preparation is few, particle diameter is little, be uniformly dispersed, and is intended to solve existing nano-powder and has problems such as thermal insulation, visible light transmissivity are lower.
Technical scheme of the present invention is following:
The composite mixed nano-stannic oxide of a kind of ytterbium bismuth indium antimony, wherein, the composite mixed nano-stannic oxide of said ytterbium bismuth indium antimony is to have mixed ytterbium, bismuth, indium and four kinds of elements compounding of antimony in the nano tin oxide powder;
The molecular formula of the composite mixed nano-stannic oxide of said ytterbium bismuth indium antimony is Yb
xBi
yIn
zSb
mSn
(1-x-y-z-m)O
2, wherein, described x, y, z and m value sum are 0.03～0.4.
A kind of preparation method of the above-mentioned composite mixed nano-stannic oxide of ytterbium bismuth indium antimony wherein, may further comprise the steps:
S1, water-soluble pink salt is mixed with tin-salt solution, adds ytterbium salt, bismuth salt, indium salt and antimonic salt successively, in 50 ℃ ~ 60 ℃ water-bath environment, be stirred to dissolving, add dispersion agent again, be stirred to abundant dissolving;
S2, in above-mentioned solution, add urea, the pH value of conditioned reaction system is stirred to urea and dissolves fully;
S3, above-mentioned solution is washed with argon gas, under 70 ~ 90 ℃ and argon shield, carry out chemical reaction, obtain gelatinous precipitate with the UW radiation;
S4, gelatinous precipitate obtain presoma through ageing, filtration, and said presoma is obtained the composite mixed nano-stannic oxide of said ytterbium bismuth indium antimony through washing, drying, grinding, calcining.
The preparation method of the composite mixed nano-stannic oxide of described ytterbium bismuth indium antimony wherein, is by Yb among the said step S1
xBi
yIn
zSb
mSn
(1-x-y-z-m)O
2Middle x, y, z, m SP take by weighing ytterbium salt, bismuth salt, indium salt, antimonic salt and pink salt;
Said pink salt, bismuth salt, indium salt, ytterbium salt and antimonic salt are water miscible.
The preparation method of the composite mixed nano-stannic oxide of described ytterbium bismuth indium antimony; Wherein, The chlorate that said water-soluble pink salt is a tin, nitrate salt, Citrate trianion or its oxide compound, chlorate or nitrate salt that said ytterbium salt is ytterbium, chlorate or nitrate salt that said bismuth salt is bismuth; Chlorate or nitrate salt that said indium salt is indium, said antimonic salt are the chlorate or the nitrate salt of antimony.
The preparation method of the composite mixed nano-stannic oxide of described ytterbium bismuth indium antimony, wherein, said dispersion agent is polyoxyethylene glycol, USP Kosher or Hydrocerol A, its consumption is 1～2% of a pink salt quality.
The preparation method of the composite mixed nano-stannic oxide of described ytterbium bismuth indium antimony, wherein, the consumption of urea described in the step S2 is n (urea)=4n (Sn
4+)+3n (Bi
3++ In
3++ Sb
3++ Yb
3+), the reaction system endpoint pH is 2～5;
Wherein, temperature of reaction is 50～80 ℃ in the step S2 process.
The preparation method of the composite mixed nano-stannic oxide of described ytterbium bismuth indium antimony, wherein, the time of said argon gas washing is 10 ~ 20min;
Described UW radiation frequency is 20.81kHz, 24.45kHz, 30.10kHz or 40.34kHz;
The said UW radiating time is 2～4h.
The preparation method of the composite mixed nano-stannic oxide of described ytterbium bismuth indium antimony, wherein, the temperature condition of chemical reaction described in the step S3 is 80 ℃.
The preparation method of the composite mixed nano-stannic oxide of described ytterbium bismuth indium antimony, wherein, the aged time described in the step S4 is 4～8 hours;
The process of said washing is for the said presoma of distilled water wash 3 times, and using volume(tric)fraction again is that 10% ethanolic soln washing to filtrating is neutrality, uses twice of absolute ethanol washing at last.
The preparation method of the composite mixed nano-stannic oxide of described ytterbium bismuth indium antimony, wherein said exsiccant mode can be a kind of in forced air drying, vacuum-drying, lyophilize, the microwave drying;
Said incinerating mode is 400 ℃ and is warming up to 600 ℃ of insulation 2h behind the insulation 2h down.
Beneficial effect: the present invention adopts the sonochemistry method to mix nano tin oxide powder to ytterbium, bismuth, indium and four kinds of elements compounding of antimony; In conjunction with ytterbium to advantages such as the satisfactory electrical conductivity of the good conductivity of infrared absorption, indium, bismuth antimony and photopermeabilities; Obtained the composite mixed nano-stannic oxide of said ytterbium bismuth indium antimony, made the nano-powder electroconductibility, light transmission rate and the effect of heat insulation that obtain better.The preparation method of the composite mixed nano-stannic oxide of said ytterbium bismuth indium antimony also is provided among the present invention; Utilize hyperacoustic cavitation effect to produce the condition of HTHP; And combine the method for organic solvent washing to improve the efficient of separating presoma, prepare five kinds of adulterated nano-powders of elements compounding efficiently.Said preparation method has remedied a series of shortcomings such as coprecipitation method is reunited easily, diameter of particle is inhomogeneous, and the aftertreatment of microemulsion method presoma is difficult, cost is higher, and the equipment requirements of hydrothermal method is high, corrodibility is strong, and spray pyrolysis efficient is low.The inventive method is simple, can realize even doping, and the powder reuniting of preparation is few, particle diameter is little, be uniformly dispersed.
Description of drawings
Fig. 1 is the TEM figure of the composite mixed nano tin oxide powder of ytterbium bismuth indium antimony prepared in the embodiment of the invention 2.
Embodiment
The present invention provides composite mixed nano-stannic oxide of a kind of ytterbium bismuth indium antimony and preparation method thereof, and is clearer, clear and definite for making the object of the invention, technical scheme and effect, below to further explain of the present invention.Should be appreciated that specific embodiment described herein only in order to explanation the present invention, and be not used in qualification the present invention.
Among the present invention, adopt the sonochemistry method to mix nano tin oxide powder to ytterbium, bismuth, indium and four kinds of elements compounding of antimony.This kind method has utilized ytterbium that characteristics such as the satisfactory electrical conductivity of the good conductivity of infrared absorption, indium, bismuth antimony and photopermeability are processed a kind of new-type functional material.This method not only makes the powder electroconductibility, light transmission rate and the effect of heat insulation that obtain better; And remedied that coprecipitation method is reunited easily, 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 efficient is low.The inventive method is simple, can realize even doping, and the powder reuniting of preparation is few, particle diameter is little, be uniformly dispersed.
The composite mixed nano-stannic oxide of wherein said ytterbium bismuth indium antimony is in nano-stannic oxide, mix ytterbium, bismuth, indium and antimony, and its molecular formula is Yb
xBi
yIn
zSb
mSn
(1-x-y-z-m)O
2Wherein, described x, y, z and m value sum are 0.03～0.4.
Said sonochemistry legal system is equipped with the technology of the composite mixed nano tin oxide powder of ytterbium bismuth indium antimony, and its preparation process is following:
S100, water-soluble pink salt is mixed with certain density tin-salt solution; Add quantitative ytterbium salt, bismuth salt, indium salt and antimonic salt successively, in 50 ℃ ~ 60 ℃ water-bath environment, be stirred to dissolving, add certain amount of dispersant again; Be stirred to abundant dissolving, finally form clear solution.
Wherein, said pink salt, bismuth salt, indium salt, ytterbium salt and antimonic salt are water miscible, are to be raw material with pink salt, bismuth salt, indium salt, ytterbium salt and antimonic salt among the step S100, press Yb
xBi
yIn
zSb
mSn
(1-x-y-z-m)O
2Middle x, y, z, m SP take by weighing ytterbium salt, bismuth salt, indium salt, antimonic salt and pink salt, are used to prepare said nano tin oxide powder.The chlorate that said solubility pink salt is a tin, nitrate salt, Citrate trianion or its oxide compound; Chlorate or nitrate salt that said ytterbium salt is ytterbium; Chlorate or nitrate salt that said bismuth salt is bismuth, chlorate or nitrate salt that said indium salt is indium, said antimonic salt are the chlorate or the nitrate salt of antimony.Said dispersion agent is polyoxyethylene glycol, USP Kosher or Hydrocerol A, and its consumption is 1～2% of a pink salt quality.
S200, in the resulting clear solution of step S100, add urea, the pH value of conditioned reaction system is stirred to urea and dissolves fully.
Wherein, the consumption of said urea is n (urea)=4n (Sn
4+)+3n (Bi
3++ In
3++ Sb
3++ Yb
3+), can improve the agglomeration traits of nano-powder through controlling pH value in reaction, the reaction system endpoint pH is 2～5,50～80 ℃ of temperature of reaction.
S300, above-mentioned solution is washed with argon gas, under 70 ~ 90 ℃ and argon shield, insert the UW inserting tube then, carry out chemical reaction, obtain the oyster white gelatinous precipitate with the UW radiation.
Wherein, the time of said argon gas washing is 10 ~ 20min.Described UW radiation frequency can be each frequency of sonochemistry producer institute fittings, comprises 20.81kHz, 24.45kHz, 30.10kHz, 40.34kHz; The UW radiating time is 2～4h.Carry out chemical reaction with the UW radiation, can make In
3+, Sb
3+, Yb
3+, Bi
3+, Sn
4+Mix and precipitate with the form of oxyhydroxide.
Wherein among the step S300, under 70～90 ℃ and argon shield, carry out chemical reaction with the UW radiation, it is the optimal temperature conditions of chemical reaction that test is found at 80 ℃, reacts more complete, and the product particle diameter of generation is more carefully more even.
The advantage that the sonochemistry method exists in the preparation nano-powder is the speed that cavitation effect of ultrasonic waves can greatly improve inhomogeneous reaction; Realize the microcosmic uniform mixing between the inhomogeneous reaction thing; The diffusion process of accelerated reaction thing and product promotes the generation of solid cenotype, suppresses the crystalline growth velocity; Control particulate size and distribution, the agglomeration between the minimizing powder etc.; In addition, open up technological process efficient, energy-conservation, consumption reduction, might utilize the reinforcement of ultrasonic field to be achieved.Thereby apply to ultrasonic technology in the method for material prepn to compare and have remarkable advantages and distinctive feature with traditional method.
S400, washing separate: with 4～8 hours after-filtration of gelatinous precipitate ageing; The filter cake that obtains after the filtration is presoma; With distilled water wash presoma 3 times, using volume(tric)fraction again is that 10% ethanolic soln washing to filtrating is neutral, uses twice of absolute ethanol washing at last.
Adopt above-mentioned washing separate mode can obviously accelerate the speed of filtration washing, thereby increase the benefit.
S500, with presoma in 80 ℃ of following grind into powders after dry several hours, powder is placed retort furnace calcining several hours, obtain the nanometer powder of the composite mixed nano-stannic oxide of ytterbium bismuth indium antimony.
Said exsiccant mode can be a kind of in forced air drying, vacuum-drying, lyophilize, the microwave drying.Said incinerating mode is 400 ℃ and is warming up to 600 ℃ of insulation 2h behind the insulation 2h down that powder granule good dispersivity, particle diameter that such calcining manners obtains are more even.
Below in conjunction with embodiment the present invention is carried out detailed description, but the invention is not restricted to given example.
Embodiment 1
According to title product Yb
0.03Bi
0.03In
0.03Sb
0.03Sn
0.88O
2Claim appearance, n (Yb)+n (Bi)+n (In)+n (Sb)/[n (Yb)+n (Bi)+n (In)+n (Sb)+n (Sn)]=0.12 takes by weighing 3.1g SnCl
45H
2O adds the 100mL deionized water, is mixed with the solution of 0.088mol/L.In solution, add 0.11gYbCl more successively
35H
2O, 0.15gBi (NO
3)
35H
2O, 0.094gInCl
35H
2O, 0.096gSbCl
35H
2O places 50 ℃ water-bath environment to be stirred to raw material and dissolves fully, adds 0.031g PEG-600 (polyoxyethylene glycol), fully stirs to form clear solution; In above-mentioned solution, add the 2.328g urea, be stirred to the formation clear solution; Above-mentioned solution is washed 10min with argon gas, under 70 ℃ and argon shield, insert the UW inserting tube then, use the UW radiation 4h of frequency, obtain the oyster white gelatinous precipitate as 20.81kHz; With gelatinous precipitate ageing 4h after-filtration, and with distilled water wash twice, using volume(tric)fraction again is that 10% ethanolic soln washing to filtrating is neutral, uses twice of absolute ethanol washing at last; With gained presoma grind into powder after under 80 ℃ dry several hours, powder is placed retort furnace, be warming up to 600 ℃ of insulation 2h behind the insulation 2h down in 400 ℃, furnace cooling obtains the composite mixed nano tin oxide powder of rutile phase ytterbium bismuth indium antimony.TEM shows that the particle diameter of nanometer powder of gained disperses about 28nm more even, and seldom reunite.And more existing adulterated nano-powders when being lower than 30nm, disperse bad and agglomeration is serious.
To the gained material carry out XRD, infrared and atomic absorption is identified, thereby absorb characteristic and crystal morphology confirms that the material that utilizes this preparation method to obtain is the powder of the composite mixed nano-stannic oxide of ytterbium bismuth indium antimony really according to the difference of different elements.Compared with existing nano-powder, the nano-powder resistivity of present embodiment gained is lower than 10
-4Ucm, visible light transmissivity are about 84%, the infrared rays rejection rate is about 80%, the ultraviolet isolating rate is about 99%, 0 grade of sticking power, Ying Du>5H.
Embodiment 2
According to title product Yb
0.04Bi
0.04In
0.06Sb
0.06Sn
0.8O
2Claim appearance, take by weighing 2.8g SnCl
45H
2O adds the 100mL deionized water, is made into 0.080mol/L solution; In solution, add 0.148gYbCl more successively
35H
2O, 0.194gBi (NO
3)
35H
2O, 0.188gInCl
35H
2O, 0.192gSbCl
35H
2O; Place 60 ℃ water-bath environment to be stirred to raw material and dissolve fully, add 0.055gPEG-600, fully stir and form clear solution; In above-mentioned solution, add the 2.28g urea, be stirred to the formation clear solution; Above-mentioned solution is washed 20min with argon gas, under 80 ℃ and argon shield, insert the UW inserting tube then, use the UW radiation 2h of frequency, obtain the oyster white gelatinous precipitate as 30.10kHz; With gelatinous precipitate ageing 5h after-filtration, and, be neutral with certain density ethanolic soln washing to filtrating again, use twice of absolute ethanol washing at last with distilled water wash twice; With gained presoma grind into powder after under 80 ℃ dry several hours, powder is placed retort furnace, be warming up to 600 ℃ of insulation 2h behind the insulation 2h down in 400 ℃, furnace cooling obtains the composite mixed nano tin oxide powder of ytterbium bismuth indium antimony.Fig. 1 is the TEM photo of present embodiment gained powder; From photo, can find out the composite mixed nano-silica diameter of particle of synthetic ytterbium bismuth indium antimony about 24nm, have distribute and disperse more even, littler and reunite still less compared to existing numerous adulterated particle diameter of nanometer powder.
To the gained material carry out XRD, infrared and atomic absorption is identified, thereby absorb characteristic and crystal morphology confirms that the material that utilizes this preparation method to obtain is the powder of the composite mixed nano-stannic oxide of ytterbium bismuth indium antimony really according to the difference of different elements.Compared with existing nano-powder, the nano-powder resistivity of present embodiment gained is lower than 10
-4Ucm, visible light transmissivity are about 87%, the infrared rays rejection rate is about 82%, the ultraviolet isolating rate is about 99.5%, 0 grade of sticking power, Ying Du>5H.
Case study on implementation 3
According to title product Yb
0.06Bi
0.09In
0.09Sb
0.06Sn
0.6O
2Claim appearance, take by weighing 2.1g SnCl
45H
2O adds the 100mL deionized water, is mixed with the solution of 0.069mol/L.In solution, add 0.22gYbCl more successively
35H
2O, 0.44gBi (NO
3)
35H
2O, 0.28gInCl
35H
2O, 0.19gSbCl
35H
2O places 55 ℃ water-bath environment to be stirred to raw material and dissolves fully, adds 0.042g PEG-600 (polyoxyethylene glycol), fully stirs to form clear solution; In above-mentioned solution, add the 1.98g urea, be stirred to the formation clear solution; Above-mentioned solution is washed 15min with argon gas, under 90 ℃ and argon shield, insert the UW inserting tube then, use the UW radiation 3h of frequency, obtain the oyster white gelatinous precipitate as 20.81kHz; With gelatinous precipitate ageing 8h after-filtration, and with distilled water wash twice, using volume(tric)fraction again is that 10% ethanolic soln washing to filtrating is neutral, uses twice of absolute ethanol washing at last; With gained presoma grind into powder after under 90 ℃ dry several hours, powder is placed retort furnace, be warming up to 600 ℃ of insulation 2h behind the insulation 2h down in 400 ℃, furnace cooling obtains the composite mixed nano tin oxide powder of ytterbium bismuth indium antimony.The particle diameter that the TEM photo shows the gained powder is about 29nm and good dispersivity, reunite fewly, and more existing adulterated nano-powders when being lower than 30nm, disperse bad and agglomeration is serious.
To the gained material carry out XRD, infrared and atomic absorption is identified, thereby absorb characteristic and crystal morphology confirms that the material that utilizes this preparation method to obtain is the powder of the composite mixed nano-stannic oxide of ytterbium bismuth indium antimony really according to the difference of different elements.Compared with existing nano-powder, the nano-powder resistivity of present embodiment gained is lower than 10
-4Ucm, visible light transmissivity are about 85%, the infrared rays rejection rate is about 81%, the ultraviolet isolating rate is about 99 %, 0 grade of sticking power, Ying Du>5H.
Should be understood that application of the present invention is not limited to above-mentioned giving an example, concerning those of ordinary skills, can improve or conversion that all these improvement and conversion all should belong to the protection domain of accompanying claims of the present invention according to above-mentioned explanation.
Claims (10)
1. the composite mixed nano-stannic oxide of ytterbium bismuth indium antimony is characterized in that, the composite mixed nano-stannic oxide of said ytterbium bismuth indium antimony is to have mixed ytterbium, bismuth, indium and four kinds of elements compounding of antimony in the nano tin oxide powder;
The molecular formula of the composite mixed nano-stannic oxide of said ytterbium bismuth indium antimony is Yb
xBi
yIn
zSb
mSn
(1-x-y-z-m)O
2, wherein, described x, y, z and m value sum are 0.03～0.4.
2. the preparation method of the composite mixed nano-stannic oxide of ytterbium bismuth indium antimony as claimed in claim 1 is characterized in that, may further comprise the steps:
S1, water-soluble pink salt is mixed with tin-salt solution, adds ytterbium salt, bismuth salt, indium salt and antimonic salt successively, in 50 ℃ ~ 60 ℃ water-bath environment, be stirred to dissolving, add dispersion agent again, be stirred to abundant dissolving;
S2, in above-mentioned solution, add urea, the pH value of conditioned reaction system is stirred to urea and dissolves fully;
S3, above-mentioned solution is washed with argon gas, under 70 ~ 90 ℃ and argon shield, carry out chemical reaction, obtain gelatinous precipitate with the UW radiation;
S4, gelatinous precipitate obtain presoma through ageing, filtration, and said presoma is obtained the composite mixed nano-stannic oxide of said ytterbium bismuth indium antimony through washing, drying, grinding, calcining.
3. the preparation method of the composite mixed nano-stannic oxide of ytterbium bismuth indium antimony according to claim 2 is characterized in that, is by Yb among the said step S1
xBi
yIn
zSb
mSn
(1-x-y-z-m)O
2Middle x, y, z, m SP take by weighing ytterbium salt, bismuth salt, indium salt, antimonic salt and pink salt;
Said bismuth salt, indium salt, ytterbium salt and antimonic salt are water miscible.
4. the preparation method of the composite mixed nano-stannic oxide of ytterbium bismuth indium antimony according to claim 2; It is characterized in that; The chlorate that said water-soluble pink salt is a tin, nitrate salt, Citrate trianion or its oxide compound, chlorate or nitrate salt that said ytterbium salt is ytterbium, chlorate or nitrate salt that said bismuth salt is bismuth; Chlorate or nitrate salt that said indium salt is indium, said antimonic salt are the chlorate or the nitrate salt of antimony.
5. the preparation method of the composite mixed nano-stannic oxide of ytterbium bismuth indium antimony according to claim 2 is characterized in that said dispersion agent is polyoxyethylene glycol, USP Kosher or Hydrocerol A, and its consumption is 1～2% of a pink salt quality.
6. the preparation method of the composite mixed nano-stannic oxide of ytterbium bismuth indium antimony according to claim 2 is characterized in that the consumption of urea described in the step S2 is n (urea)=4n (Sn
4+)+3n (Bi
3++ In
3++ Sb
3++ Yb
3+), the reaction system endpoint pH is 2～5;
Wherein, temperature of reaction is 50～80 ℃ in the step S2 process.
7. the preparation method of the composite mixed nano-stannic oxide of ytterbium bismuth indium antimony according to claim 2 is characterized in that, the time of said argon gas washing is 10 ~ 20min;
Described UW radiation frequency is 20.81kHz, 24.45kHz, 30.10kHz or 40.34kHz;
The said UW radiating time is 2～4h.
8. the preparation method of the composite mixed nano-stannic oxide of ytterbium bismuth indium antimony according to claim 2 is characterized in that the temperature condition of chemical reaction described in the step S3 is 80 ℃.
9. the preparation method of the composite mixed nano-stannic oxide of ytterbium bismuth indium antimony according to claim 2 is characterized in that the aged time described in the step S4 is 4～8 hours;
The process of said washing is for the said presoma of distilled water wash 3 times, and using volume(tric)fraction again is that 10% ethanolic soln washing to filtrating is neutrality, uses twice of absolute ethanol washing at last.
10. the preparation method of the composite mixed nano-stannic oxide of ytterbium bismuth indium antimony according to claim 2 is characterized in that, said exsiccant mode can be a kind of in forced air drying, vacuum-drying, lyophilize, the microwave drying;
Said incinerating mode is 400 ℃ and is warming up to 600 ℃ of insulation 2h behind the insulation 2h down.
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Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN107188225A (en) * | 2017-07-14 | 2017-09-22 | 广东拓扑中润科技发展有限公司 | A kind of indium-doped antimony oxidation tin nano-powder and preparation method thereof |
| CN111205758A (en) * | 2020-02-26 | 2020-05-29 | 南京君弘新材料有限公司 | Transparent antistatic liquid and preparation method thereof |
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| CN1673096A (en) * | 2005-02-25 | 2005-09-28 | 昆明理工大学 | Prepn process of nano In-Sn oxide powder |
| WO2010139910A1 (en) * | 2009-06-05 | 2010-12-09 | Centre National De La Recherche Scientifique (C.N.R.S.) | Method for preparing a water-compatible composition of metal oxide nanocrystals |
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| CN107188225A (en) * | 2017-07-14 | 2017-09-22 | 广东拓扑中润科技发展有限公司 | A kind of indium-doped antimony oxidation tin nano-powder and preparation method thereof |
| CN107188225B (en) * | 2017-07-14 | 2018-11-02 | 广东拓扑中润科技发展有限公司 | A kind of indium-doped antimony oxidation tin nano-powder and preparation method thereof |
| CN111205758A (en) * | 2020-02-26 | 2020-05-29 | 南京君弘新材料有限公司 | Transparent antistatic liquid and preparation method thereof |
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