CN113880131A - Preparation method of ATO nanocrystalline sol - Google Patents
Preparation method of ATO nanocrystalline sol Download PDFInfo
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- CN113880131A CN113880131A CN202111223484.2A CN202111223484A CN113880131A CN 113880131 A CN113880131 A CN 113880131A CN 202111223484 A CN202111223484 A CN 202111223484A CN 113880131 A CN113880131 A CN 113880131A
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- C—CHEMISTRY; METALLURGY
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- C01G—COMPOUNDS CONTAINING METALS NOT COVERED BY SUBCLASSES C01D OR C01F
- C01G19/00—Compounds of tin
- C01G19/02—Oxides
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B82—NANOTECHNOLOGY
- B82Y—SPECIFIC USES OR APPLICATIONS OF NANOSTRUCTURES; MEASUREMENT OR ANALYSIS OF NANOSTRUCTURES; MANUFACTURE OR TREATMENT OF NANOSTRUCTURES
- B82Y30/00—Nanotechnology for materials or surface science, e.g. nanocomposites
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B82—NANOTECHNOLOGY
- B82Y—SPECIFIC USES OR APPLICATIONS OF NANOSTRUCTURES; MEASUREMENT OR ANALYSIS OF NANOSTRUCTURES; MANUFACTURE OR TREATMENT OF NANOSTRUCTURES
- B82Y40/00—Manufacture or treatment of nanostructures
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- C01P—INDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS
- C01P2002/00—Crystal-structural characteristics
- C01P2002/50—Solid solutions
- C01P2002/52—Solid solutions containing elements as dopants
- C01P2002/54—Solid solutions containing elements as dopants one element only
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- C01P—INDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS
- C01P2004/00—Particle morphology
- C01P2004/60—Particles characterised by their size
- C01P2004/64—Nanometer sized, i.e. from 1-100 nanometer
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- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01P—INDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS
- C01P2006/00—Physical properties of inorganic compounds
- C01P2006/40—Electric properties
Abstract
The invention discloses a preparation method of ATO nanocrystalline sol; dissolving tin stannate in deionized water to obtain a solution A; dissolving antimonic acid antimonic salt in deionized water, and heating for auxiliary dissolution to obtain a solution B; simultaneously adding the solution A and the solution B into deionized water, heating and violently stirring to obtain a solution C; and carrying out hydrothermal reaction treatment on the prepared solution C, adding an organic solvent with small polarity to ensure that ATO obtained by the reaction is subjected to coagulation, washing, and then carrying out solvent replacement and ultrasonic treatment to obtain the ATO nanocrystalline sol. The raw materials are cheap and easy to obtain, the process is simple, the cost is low, and stable ATO nanocrystalline sol with the average grain diameter distributed at 30nm can be obtained without high-temperature calcination and post-dispersion by using a dispersing agent.
Description
Technical Field
The invention relates to ATO (antimony tin oxide) nanocrystals, in particular to a preparation method of ATO nanocrystal sol, belonging to the technical field of tin antimony oxide nanopowder.
Background
ATO is used in the fields of displays, solar cells and transparent thermal barrier coatings as a common Transparent Conductive Oxide (TCO) N-type semiconductor material. More than half of the energy in the sunlight comes from a near-infrared region, ATO is a transparent heat-insulating nano material with great market application prospect, has high transmittance on visible light, and has shielding effects of reflection, absorption and the like on near-infrared light. The ATO is used as a filler and added into the emulsion with high light transmittance, so that the transparent heat-insulating coating which can transmit visible light and shield near infrared light can be obtained, and for countries with large energy consumption, especially countries with high building energy consumption ratio, heat insulation and heat preservation measures for buildings are necessary, but in recent years, large-area glass is adopted for buildings in China, and the application of ATO to the glass heat-insulating coating is undoubtedly a good solution.
The Chinese invention patent CN104263056B provides a preparation method of antimony tin oxide organic nano-slurry, the method utilizes a chemical coprecipitation method, a mixture of tin tetrachloride and antimony trichloride is precipitated by weak base, and then the obtained product is calcined in a muffle furnace at a high temperature of 500-700 ℃ to prepare ATO, and the method has the advantage that ATO powder can be prepared in large quantity. However, the initial particle size of ATO cannot be controlled to a small level due to the chemical precipitation method and the muffle furnace calcination, and the hard agglomeration of the powder is increased. The later dispersion is difficult, high-energy long-time ball milling is needed, the method has high energy consumption, and the initial particle size of the nano powder cannot be well controlled.
The average primary particle size of the ATO powder prepared in the chinese patent application CN 104276598A is about 50nm, but the ATO powder is dispersed by using a surfactant (such as SDS, CTAB) in later-stage dispersion work, the average particle size of the obtained ATO dispersion liquid is about 100 nm, and the too large particle size of the dispersion liquid causes the reduction of light transmittance in the application of glass paint, and affects the lighting effect of architectural glass.
Disclosure of Invention
The invention aims to provide a preparation method of ATO nanocrystalline sol, which has the advantages of low cost, simple process, small particle size and good dispersion.
The purpose of the invention is realized by the following technical scheme:
the technical scheme of the invention is as follows: the preparation method of the ATO nanocrystalline sol comprises the steps of preparing ATO nanocrystalline and preparing the ATO nanocrystalline sol by utilizing solvent replacement.
A preparation method of ATO nanocrystalline sol is characterized by comprising the following steps:
(1) dissolving tin stannate in deionized water to obtain a solution A; dissolving antimonic acid antimonic salt in deionized water, and heating for auxiliary dissolution to obtain a solution B; simultaneously adding the solution A and the solution B into deionized water, heating and violently stirring to obtain a solution C;
(2) and (2) preparing a solution C by utilizing the step (1), performing hydrothermal reaction treatment, adding an organic solvent with small polarity to ensure that ATO obtained by the reaction is subjected to coagulation, washing, and then performing solvent replacement and ultrasonic treatment to obtain the ATO nanocrystalline sol.
To further achieve the object of the present invention, preferably, Sn is contained in the solution C in the step (1)4+The concentration of (b) is 0.5-2 mol/L.
Preferably, Sb in the solution C in the step (1)5+The concentration of (b) is 0.05-0.4 mol/L.
Preferably, the molar ratio of the antimony element to the tin element in the step (1) is 1: 5-1: 20.
Preferably, the heating temperature for heating-assisted dissolution is 60-90 ℃.
Preferably, the heating temperature of the heating and the vigorous stirring is 60-80 ℃.
Preferably, the temperature of the hydrothermal reaction is 150-180 ℃; the reaction time is 5-12 h.
Preferably, the organic solvent with small polarity is one or more of acetone, diethyl ether and petroleum ether.
Preferably, the stannic acid stannate is one or more of potassium stannate trihydrate, sodium stannate trihydrate, potassium stannate, and sodium stannate.
Preferably, the antimony antimonate is one or more of potassium antimonate trihydrate, sodium antimonate trihydrate, potassium antimonate and sodium antimonate.
The preparation method of the ATO nanocrystalline sol firstly mixes tin salt and antimony salt and adds the tin salt and the antimony salt into hot water, so that potassium stannate trihydrate is hydrolyzed into SnO with incompletely formed crystal structure with small particle size in advance2The sol is beneficial to controlling the particle size of nano particles during hydrothermal treatment, small-particle-size monodisperse ATO is prepared by a hydrothermal method, acetone is added for sedimentation, washing is carried out for a plurality of times, and finally the sol of antimony-doped tin dioxide (ATO) nano crystals is obtained by a solvent replacement method. The raw materials of the invention do not contain Cl-Without introduction of Cl-The method can effectively prevent the ATO from generating hard agglomeration in the preparation process, is cheap and easy to obtain, has simple process and low cost, and can obtain stable ATO nanocrystalline sol with the average grain diameter distributed at 30nm without high-temperature calcination and post-dispersion by using a dispersing agent.
Compared with the ATO nanocrystalline sol preparation method in the prior art, the beneficial effects of the invention are that:
1. compared with tin tetrachloride, antimony trichloride and the like used in the traditional method, the tin stannate and antimony antimonate salts used for synthesizing the ATO nanocrystalline in the invention use potassium stannate trihydrate and potassium antimonate trihydrate, and avoid introducing Cl-Ions, which cause hard agglomeration of nanoparticles during synthesis of ATO nanocrystals.
2. Before hydrothermal treatment, the tin stannate and antimony antimonate are added into hot water and stirred vigorously to form monodisperse sol in the hot water, so that the tin stannate and antimony antimonate have numerous crystal nucleus growth sites in subsequent hydrothermal reaction, and particle size control is facilitated.
3. The method adopts hydrothermal reaction, compared with the traditional sol-gel method, the monodisperse ATO nanocrystalline with small particle size can be obtained by adopting the hydrothermal reaction without high-temperature calcination in the later period, the problem of hard agglomeration of particles caused by high-temperature calcination is avoided, stable ATO nanocrystalline sol is obtained by using a solvent replacement method, and the later redispersion processes such as ball milling and the like are not needed, so that the energy consumption can be greatly reduced.
4. Compared with the prior art in which an alcohol solvent is used for preparing the ATO nanocrystalline, the solvent adopted by the invention is deionized water, so that the price is low, and the preparation method is environment-friendly.
5. Compared with the traditional method of drying the ATO nanocrystalline and then performing ball milling dispersion, the ATO nanocrystalline sol prepared by the method of solvent replacement saves energy consumption, does not need to add a dispersing agent for post dispersion, greatly saves cost and is beneficial to industrial application.
Drawings
FIG. 1 is a particle size distribution diagram of the ATO nanocrystalline sol obtained in example 1 of the present invention.
FIG. 2 shows the Zeta potential of the ATO nanocrystalline sol obtained in example 1 of the present invention.
Detailed Description
For better understanding of the present invention, the present invention is further illustrated by the following examples, which are not intended to limit the scope of the claims of the present invention, and other examples obtained by those skilled in the art without inventive efforts shall fall within the scope of the present invention.
Example 1: synthesis of ATO nanocrystalline sol
0.596g of K2SnO3·3H2O was dissolved in 3g of water, while 0.079g of KSbO was added3·3H2O was added to 10g of deionized water and heated to 60 ℃ and stirred for 20min to aid dissolution. And simultaneously pouring the prepared potassium stannate trihydrate solution and potassium antimonate trihydrate solution into deionized water at 70 ℃, stirring at the rotating speed of 500rpm for 20min to obtain a precursor solution of ATO nanocrystalline, adding the precursor solution into a 75ml lining of a polytetrafluoroethylene hydrothermal reaction kettle, and sealing the liner. And in an electrically heated forced-air ovenReacting for 5 hours at 160 ℃, and pouring out the supernatant to obtain the ATO nanocrystal.
Adding acetone with the mass of 5% of the precursor solution to precipitate ATO nanocrystals, washing with deionized water, centrifuging at 7000rpm for 20min, repeating the operation for 3 times, washing unreacted substances and other impurities, adding deionized water to replace the solvent, adjusting the solid content to 20%, and finally obtaining stable ATO nanocrystal sol. Fig. 1 is a distribution diagram of the particle size of the ATO nanocrystal sol obtained in example 1 of the present invention, and it can be seen from fig. 1 that the average particle size of the obtained ATO nanocrystal sol is distributed between 30nm and 50 nm. FIG. 2 is a Zeta potential diagram of the ATO nanocrystalline sol obtained in example 1 of the present invention, and it can be seen from FIG. 2 that the Zeta potential of the obtained ATO nanocrystalline sol is also at-38 mV, indicating that the ATO nanocrystalline sol is in a stable state. The particle size distribution and zeta potential of the ATO nanocrystalline sol obtained in the following examples are substantially similar to those of example 1, and are not provided.
Example 2: synthesis of ATO nanocrystalline sol
Adding 0.533g of Na2SnO3·3H2O was dissolved in 3g of water, while 0.074g of NaSbO was added3·3H2O was added to 10g of deionized water and heated to 90 ℃ and stirred for 1h to aid dissolution. And simultaneously pouring the prepared sodium stannate trihydrate solution and the prepared sodium antimonate trihydrate solution into deionized water at 60 ℃, stirring at the rotating speed of 1000rpm for 20min to obtain a precursor solution of ATO nanocrystalline, adding the precursor solution into a 75ml inner liner of a polytetrafluoroethylene hydrothermal reaction kettle, and sealing the inner liner. And reacting for 5 hours in an electric heating blast oven at the temperature of 150 ℃, and pouring out the supernatant to obtain the ATO nanocrystalline.
Adding ether with the mass of 10% of that of the precursor solution to precipitate ATO nanocrystals, washing with deionized water, centrifuging at 7000rpm for 20min, repeating the operation for 3 times, washing unreacted substances and other impurities, adding deionized water to replace the solvent, adjusting the solid content to 20%, and finally obtaining the stable ATO nanocrystal sol.
Example 3: synthesis of ATO nanocrystalline sol
0.848g of Na2SnO3Dissolved in 3g of water while 0.079g of KSbO was added3·3H2O was added to 10g of deionized water and heated to 90 ℃ and stirred for 1h to aid dissolution. And simultaneously pouring the prepared sodium stannate solution and potassium antimonate trihydrate solution into 80 ℃ deionized water rapidly, stirring at the rotating speed of 500rpm for 20min to obtain a precursor solution of ATO nanocrystalline, adding the precursor solution into a 75ml inner liner of a polytetrafluoroethylene hydrothermal reaction kettle, and sealing the inner liner. And reacting for 12 hours in an electric heating blast oven at 160 ℃, and pouring out the supernatant to obtain the ATO nanocrystalline.
Adding petroleum ether accounting for 8% of the mass of the precursor solution to enable the ATO nanocrystalline to be difficultly dispersed in the petroleum ether, performing coagulation and washing by deionized water, centrifuging at the rotating speed of 7000rpm for 20min, repeating the operation for 3 times, washing unreacted substances and other impurities, adding deionized water to perform solvent replacement, adjusting the solid content to 20%, and finally obtaining the stable ATO nanocrystalline sol.
The ATO nanocrystals with small particle size (about 30 nm) can be prepared by the above examples 1-3, and the impurities remained in the reaction are removed by a solvent replacement method to obtain a stable ATO nanocrystal sol. The invention utilizes tin stannate and antimony antimonate as raw materials for preparing ATO, and avoids introducing chloride ions to cause hard agglomeration of nano particles, which is different from the traditional method of utilizing tin tetrachloride, antimony trichloride and other salts as raw materials. And under the condition that a surfactant is not used as a reaction template, the monodisperse spherical ATO with small particle size can be prepared by only using water as a solvent, the ATO nanocrystalline is obtained without high-temperature calcination, the problem of hard agglomeration of particles caused by high-temperature calcination is avoided, stable ATO nanocrystalline sol is obtained by using a solvent replacement method, and the process of ball milling and other later redispersion is not needed, so that the energy consumption can be greatly reduced. In the chinese patent CN104263056B, tin tetrachloride and antimony trichloride are used as raw materials, alkali is added to promote hydrolysis of antimony salt and tin salt, and a high-temperature calcination method is also used to prepare the ATO nanocrystal, which all causes the particle size of ATO to be increased due to hard agglomeration. Even though the secondary dispersion is carried out on the ATO powder by using the ball milling and the dispersing agent, the grain diameter is as high as 90 nm. In the Chinese patent CN110003685A, ATO is ball-milled for 1-24 hours by using a ball mill to prepare ATO sol, and the stable ATO nanocrystalline sol can be obtained only by carrying out solvent replacement. In the Chinese patent CN106315666A, isopropanol is used as a solvent to synthesize ATO, and compared with the method that water is used as a solvent to participate in hydrothermal reaction, the method of the invention uses an organic solvent as a solvent, which can generate a large amount of consumption, not only is not beneficial to saving cost, but also is not beneficial to environmental protection.
Example 4: application of ATO nanocrystalline sol
Mixing and stirring the ATO nanocrystalline sol obtained in the example 1 and the water-based silicone-acrylic emulsion, wherein the mass percent of the ATO nanocrystalline sol is 20%, the mass percent of the water-based silicone-acrylic emulsion is 60%, the mass percent of the film-forming additive dodecyl alcohol ester is 5%, the mass percent of the defoaming agent is 0.01%, the mass percent of the leveling agent is 0.1%, the mass percent of the pH regulator is 0.03%, and then adding 14.86% of deionized water and carrying out magnetic stirring for 0.5 hour to ensure that the ATO nanocrystalline sol and the water-based silicone-acrylic emulsion are uniformly dispersed. Finally, respectively scrubbing the float glass by using 10 wt% of sodium hydroxide and 10 wt% of sulfuric acid, washing the float glass by using deionized water for 2 times, and drying the float glass for later use. Respectively coating the prepared transparent heat-insulating coating and the water-based silicone-acrylic emulsion without filler on float glass with the thickness of 100mm multiplied by 3mm by using different thickness surfaces of a BGD four-surface preparation device to prepare a sample with the coating thickness of 30um, forming a film in an electrothermal blowing constant-temperature drying oven with the temperature of 80 ℃ for 3 days, and carrying out a comparative test:
the paint film properties were tested according to the standard:
the visible light transmittance of the paint film was measured using a Hitachi UV-3900 UV-visible spectrophotometer.
And (3) testing the heat insulation effect of the heat insulation coating by using a self-made temperature difference testing instrument.
The hardness of the coating was tested according to the national standard GB/T6739-1996.
The adhesion of the coating was tested by the cross-hatch method, according to the specifications of the national standard GB/T9286-1998.
The water resistance of the coating was tested as specified in the national Standard GB/T1733-1993A method.
The acid resistance of the coating was tested as specified in the national standard GB/T9274-1988A.
The coatings were tested for alkali resistance as specified in the national standard GB/T9274-1998A.
The experimental results are shown in table 1 below.
It can be seen from table 1 that the thermal insulation temperature difference of the transparent thermal insulation coating prepared by mixing the prepared ATO nanocrystalline sol and the single-component silicone-acrylic emulsion according to a certain proportion can reach 4.2 ℃ at most, and the visible light transmittance is maintained at 89.0%. Meanwhile, with the addition of the nano filler, the hardness of a paint film of the transparent heat-insulating coating reaches 2H, and the adhesive force also reaches 0 level. Compared with a pure silicon acrylic paint film without filler, the comprehensive performance is comprehensively improved, and various weather resistance tests are passed. The results of the ATO nanocrystalline sol tests using examples 2 and 3 are similar to those of the present example and are not provided.
TABLE 1
| Detecting the index | Self-made transparent heat-insulating coating | Blank group-silicone acrylic emulsion | |
| Appearance of the coating | Light blue transparent | Colorless and transparent | |
| Average visible light transmittance | 89.0％ | 99.8％ | |
| Highest partitionThermal temperature difference | 4.2℃ | Without heat insulation effect | |
| Hardness of pencil | 2H | H | |
| | Level | 0 | Level 1 |
| Water resistance (7d) | No bubbling and no color change | No bubbling and no color change | |
| Acid resistance (10% H)2SO4，2d) | No bubbling and no color change | No bubbling and no color change | |
| Alkali resistance (20% NaOH, 3d) | No bubbling and no color change | No bubbling and no color change |
It should be noted that the present invention is not limited by the above-mentioned embodiments, and various changes and modifications can be made in the present invention without departing from the spirit and scope of the present invention, and these changes and modifications fall into the protection scope of the claimed invention; the scope of the invention is defined by the following claims.
Claims (10)
1. A preparation method of ATO nanocrystalline sol is characterized by comprising the following steps:
(1) dissolving tin stannate in deionized water to obtain a solution A; dissolving antimonic acid antimonic salt in deionized water, and heating for auxiliary dissolution to obtain a solution B; simultaneously adding the solution A and the solution B into deionized water, heating and violently stirring to obtain a solution C;
(2) and (2) preparing a solution C by utilizing the step (1), performing hydrothermal reaction treatment, adding an organic solvent with small polarity to ensure that ATO obtained by the reaction is subjected to coagulation, washing, and then performing solvent replacement and ultrasonic treatment to obtain the ATO nanocrystalline sol.
2. The method for preparing an ATO nanocrystal sol according to claim 1, characterized in that: sn in the solution C in the step (1)4+The concentration of (b) is 0.5-2 mol/L.
3. The method for preparing an ATO nanocrystal sol according to claim 1, characterized in that: sb in the solution C in the step (1)5+The concentration of (b) is 0.05-0.4 mol/L.
4. The method for preparing an ATO nanocrystal sol according to claim 1, characterized in that: the molar ratio of the antimony element to the tin element in the step (1) is 1: 5-1: 20.
5. The method for preparing an ATO nanocrystal sol according to claim 1, characterized in that: the heating temperature for heating-assisted dissolution is 60-90 ℃.
6. The method for preparing an ATO nanocrystal sol according to claim 1, characterized in that: the heating temperature for heating and violent stirring is 60-80 ℃.
7. The method for preparing an ATO nanocrystal sol according to claim 1, characterized in that: the temperature of the hydrothermal reaction is 150-180 ℃; the reaction time is 5-12 h.
8. The method for preparing an ATO nanocrystal sol according to claim 1, characterized in that: the organic solvent with small polarity is one or more of acetone, diethyl ether and petroleum ether; the addition amount of the organic solvent with low polarity is 5-10% of the mass of the solution C.
9. The method for preparing an ATO nanocrystal sol according to claim 1, characterized in that: the stannic acid stannate is one or more of potassium stannate trihydrate, sodium stannate trihydrate, potassium stannate and sodium stannate.
10. The method for preparing an ATO nanocrystal sol according to claim 1, characterized in that: the antimonic acid antimonic salt is one or more of potassium antimonate trihydrate, sodium antimonate trihydrate, potassium antimonate and sodium antimonate.
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Citations (7)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US3346468A (en) * | 1964-05-08 | 1967-10-10 | M & T Chemicals Inc | Tin electrodeposition process |
| JPH07257922A (en) * | 1994-03-22 | 1995-10-09 | Sumitomo Osaka Cement Co Ltd | Hydrophobic antimony containing tin oxide, heat ray shielding coating liquid and each production thereof |
| JPH1111947A (en) * | 1997-06-26 | 1999-01-19 | Mitsubishi Materials Corp | Production of antimony doped tin oxide powder and coating material containing the same |
| CN1994965A (en) * | 2006-12-08 | 2007-07-11 | 中南大学 | Process for preparing antimony doped stannic oxide nano powder |
| CN103613976A (en) * | 2013-12-03 | 2014-03-05 | 浙江大学 | Preparation method of antimony tin oxide water/oil amphiprotic slurry |
| CN105540650A (en) * | 2016-02-25 | 2016-05-04 | 攀枝花学院 | Tungsten-doped stannic oxide sol nanocrystalline and preparing method thereof |
| CN108751737A (en) * | 2018-05-30 | 2018-11-06 | 西安理工大学 | Tin dope nickel oxide-stannic oxide composite nanocrystalline film and preparation method thereof |
-
2021
- 2021-10-20 CN CN202111223484.2A patent/CN113880131A/en active Pending
Patent Citations (7)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US3346468A (en) * | 1964-05-08 | 1967-10-10 | M & T Chemicals Inc | Tin electrodeposition process |
| JPH07257922A (en) * | 1994-03-22 | 1995-10-09 | Sumitomo Osaka Cement Co Ltd | Hydrophobic antimony containing tin oxide, heat ray shielding coating liquid and each production thereof |
| JPH1111947A (en) * | 1997-06-26 | 1999-01-19 | Mitsubishi Materials Corp | Production of antimony doped tin oxide powder and coating material containing the same |
| CN1994965A (en) * | 2006-12-08 | 2007-07-11 | 中南大学 | Process for preparing antimony doped stannic oxide nano powder |
| CN103613976A (en) * | 2013-12-03 | 2014-03-05 | 浙江大学 | Preparation method of antimony tin oxide water/oil amphiprotic slurry |
| CN105540650A (en) * | 2016-02-25 | 2016-05-04 | 攀枝花学院 | Tungsten-doped stannic oxide sol nanocrystalline and preparing method thereof |
| CN108751737A (en) * | 2018-05-30 | 2018-11-06 | 西安理工大学 | Tin dope nickel oxide-stannic oxide composite nanocrystalline film and preparation method thereof |
Non-Patent Citations (2)
| Title |
|---|
| RIDDHIMAN MEDHI ET AL.: ""Uniformly Spherical and Monodisperse Antimony- and Zinc-Doped Tin Oxide Nanoparticles for Optical and Electronic Applications"", 《ACS APPLIED NANO MATERIALS》 * |
| 蔡昭军等: "纳米ATO粉体制备及其悬浮液的分散稳定性", 《材料科学与工程学报》 * |
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