CN101643200B - Preparation method of antimony-doped tin oxide nano-powder - Google Patents
Preparation method of antimony-doped tin oxide nano-powder Download PDFInfo
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- CN101643200B CN101643200B CN2009100752695A CN200910075269A CN101643200B CN 101643200 B CN101643200 B CN 101643200B CN 2009100752695 A CN2009100752695 A CN 2009100752695A CN 200910075269 A CN200910075269 A CN 200910075269A CN 101643200 B CN101643200 B CN 101643200B
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Abstract
The invention discloses a preparation method of antimony-doped tin oxide nano-powder, which belongs to the field of preparation of nanomaterials. The preparation method comprises the following steps: (1) mixing propenoic acid with water according to the ratio of 1-4:1 in parts by weight, and obtaining solution A; (2) weighing soluble antimony salt and tin salt, adding into the solution A, dissolving and obtaining a homogeneous system B, wherein, the ratio of Sb<3+>: Sn<4+> by molar fraction is 1-15:100, and the ratio of tin salt: solution A in parts by weight is 1-25:100; (3) adding water solution of peroxide initiator with weight content of 2-10% into the homogeneous system B for obtaining solution C under the stirring condition; and (4) heating the solution C for 0.1-3h at the temperature of 60-100 DEG C, then drying at the temperature of 80-150 DEG C for obtaining solids, grinding after cooling, and calcining for 1-10h in an air atmosphere at the temperature of 450-900 DEG C. The method has simple process flow, and the prepared powder has even distribution of particle size and higher purity.
Description
Technical field
The present invention relates to the preparation method of a kind of preparation of nanomaterials, particularly antimony-doped tin oxide nano-powder, can be used for fields such as transparent heat insulating dope, anti-static material.
Background technology
Antimony-doped tin oxide materials A ntimony Doped Tin Oxide; Be called for short ATO; It is a kind of Multifunction material that develops rapidly in recent years; Except that having excellent conducting performance and optical property; Also have characteristics such as fusing point height (being about 1200 ℃), Heat stability is good, corrosion-resistant, good mechanical stability, surface adsorption oxygen and carbon monoxide, obtained using widely with aspects such as radiation proof antistatic coating material, INFRARED ABSORPTION heat-barrier material, gas sensor, electrode materials at solar conversion cells, smart window, electrochromic material, anti-static plastic/chemical fibre/coating, display.
The range of application of ATO has further been widened in the development of nanometer technology, for example is reduced to 10nm when following, SnO when ATO powder size
2Gas sensing property significantly improves, and the moment or the trace that can detect gas concentration at normal temperatures change; Nanoscale ATO joins in the transparent polymer matrix in addition, prepares anti-static material with high transparent, transparent heat insulating dope etc. easily.Therefore, the nano-powder of antimony-doped tin oxide has great practical value.
The preparation method of antimony-doped tin oxide nano-powder mainly contains solid phase method and liquid phase method two big classes at present.Solid phase method be with tin oxide and antimony oxide powder machinery mixed evenly after; Obtain caeseous antimony-doped tin oxide nano-powder through high-temperature calcination; This method exists synthesis temperature high, and powder mixes inhomogeneous, and granularity is introduced shortcomings such as impurity greatly, easily; The powder resistance that obtains of solid phase method is difficult to reach the requirement of practicability than higher in addition.Liquid phase method mainly contains chemical coprecipitation, hydro-thermal method etc., is to prepare antimony-doped tin oxide method commonly used at present, but all comes with some shortcomings: such as coprecipitation, because Sb
3+And Sn
4+Hydrolysis is asynchronous, the even doping of the Sb truly of being unrealized; And the very easily hydrolysis of pink salt and antimonic salt exists with the form of ion in order to guarantee tin, antimony, need to add a large amount of strong acid and suppresses its hydrolysis, and then add alkali and make it hydrolytic precipitation, has caused the discharging that production cost is high, the production cycle is long, cause a large amount of waste liquids like this; The powder granule that makes is reunited more serious, is more difficult to get the uniform nano-powder of particle diameter.Hydro-thermal method is because the Cl in the presoma
-, NO
3 -Isoionic existence has influence on electricity, the optical property of ATO powder greatly, and hydro-thermal method requires highly to device ', and there is potential safety hazard in large-scale industrial production.
Summary of the invention
The technical issues that need to address of the present invention be overcome the production cycle that exists among the existing antimony-doped tin oxide nano-powder preparation method long, process route is complicated; The powder doping that makes is inhomogeneous, Impurity removal is difficult, the uneven shortcoming of granularity; A kind of preparation method of antimony-doped tin oxide nano-powder is provided; This method technological process is simple, the cycle short, and prepared powder granularity is evenly distributed, purity is higher.
For addressing the above problem, the step that the present invention prepares antimony-doped tin oxide nano-powder comprises:
1. be that 1～4: 1 acrylic acid mixes with water with ratio of weight and number, solution A;
2. take by weighing soluble antimonic salt and pink salt, join in the above-mentioned solution A, dissolving gets homogeneous system B, wherein Sb
3+With Sn
4+The molfraction ratio be 1～15: 100, the ratio of weight and number of pink salt and solution A is 1～25: 100;
3. under stirring condition, be that the aqueous solution of 2～10% peroxide initator joins among the homogeneous system B with weight content, solution C;
4. solution C is heated 0.1～3h at 60～100 ℃, obtain solid 80～150 ℃ of dryings then; Grind cooling back, and under air atmosphere, 450～900 ℃, calcining 1～10h.
Among the present invention, at first in the aqueous solution, form the acrylates of tin and antimony, the thermal decomposition through the polymer salt under the uniform temperature can obtain the homogeneous phase antimony-doped tin oxide nano-powder again.Its chemical equation is:
In the above-mentioned technical process, avoid introducing strong acid, provided cost savings, avoided discharging of waste liquid; Can accelerate polymerization rate through introducing the peroxide initator, shorten the reaction time; Antimony-doped tin oxide obtains through directly directly calcining presoma at a lower temperature; Combustion process through presoma; Impurity such as initator, chlorion will all burn into gas and vapor away; Free from admixture ion residues, purity are higher, and obtain the antimony-doped tin oxide nano-powder of homogeneous phase; Calcining heat is lower, the time is shorter, has practiced thrift the energy; Whole process flow is simple, and equipment is had no special requirements, and can prepare in a large number, is suitable for suitability for industrialized production.Adopt the antimony-doped tin oxide nano-powder lighter color of method for preparing, be the light gray color, be suitable for fields such as transparent heat insulating dope, anti-static material; And the good dispersion of powder, size is even, in 20～500nm scope.
Description of drawings
Fig. 1 is the TEM photo of the antimony-doped tin oxide nano-powder of the embodiment of the invention 1 preparation;
Fig. 2 is the XRD curve of the antimony-doped tin oxide nano-powder of the embodiment of the invention 1 preparation.
The specific embodiment
Below in conjunction with accompanying drawing the present invention is done and to describe in further detail.
Embodiment 1
1. 4 parts by weight of acrylic are dissolved in the deionized water of 1 weight portion, fully dissolving obtains solution A under magnetic agitation;
2. fixedly the ratio of weight and number of butter of tin and solution A is 5: 100, and trichloride antimony and butter of tin were weighed in 5: 100 in molar ratio, joins in the above-mentioned solution A, under magnetic agitation, obtains homogeneous system B;
3. under the magnetic agitation condition, be that the aqueous solution of 5% ammonium persulfate slowly joins among the homogeneous system B that 2. step make with percentage by weight, obtain solution C; Ammonium persulfate that is added and the step acrylic acid weight ratio in 1. is 0.01: 1;
4. the solution C that step is obtained in 3. makes polymerization-filling complete at 100 ℃ of heating 1h; At 80 ℃ of dry 24h, obtain solid then; Grind cooling back, places in the Muffle furnace again, under air atmosphere, 700 ℃, calcined 3 hours, has promptly made caesious antimony-doped tin oxide nano powder.
The transmission electron microscope of this antimony-doped tin oxide nano powder (TEM) photo is as shown in Figure 1, can find out, the good dispersion of the antimony-doped tin oxide powder that said method makes, and size is even, in 100～300nm scope.(XRD) is as shown in Figure 2 for X ray diffracting spectrum, and as can be seen from the figure, the ATO nano-powder has typical cubic rutile structure, and mixing of Sb do not form Sb
2O
3Phase-splitting or change SnO
2Crystal structure.
Accurately take by weighing prepared ATO nano-powder 0.05g, the diameter of packing into is in the mould of 2mm, and behind its resistance of universal meter survey, the specific insulation that calculates its powder is 400 Ω cm.
1. 1 parts by weight of acrylic is dissolved in the deionized water of 1 weight portion, fully dissolving obtains solution A under magnetic agitation;
2. fixedly the ratio of weight and number of butter of tin and solution A is 1: 100, and trichloride antimony and butter of tin were weighed in 15: 100 in molar ratio, joins in the above-mentioned solution A, under magnetic agitation, obtains homogeneous system B;
3. under the magnetic agitation condition, be that the deionized water solution of 10% ammonium persulfate slowly joins among the homogeneous system B that 2. step make with percentage by weight, obtain solution C; Ammonium persulfate that is added and the step acrylic acid weight ratio in 1. is 0.05: 1;
4. the solution C that 3. step is obtained heats 3h at 60 ℃, makes polymerization-filling complete; At 110 ℃ of dry 10h, obtain solid then; Grind cooling back, places in the Muffle furnace again, and under air atmosphere, 450 ℃ of conditions, calcining 10h has promptly made caesious antimony-doped tin oxide nano powder.
The antimony-doped tin oxide nano powder good dispersion that adopts method provided by the invention to prepare, size is even, and in 20～100nm scope, the specific insulation of powder is 50 Ω cm.
Embodiment 3
1. 2 parts by weight of acrylic are dissolved in the deionized water of 1 weight portion, fully dissolving obtains solution A under magnetic agitation;
2. fixedly the weight ratio of butter of tin and solution A is 25: 100, and trichloride antimony and butter of tin were weighed in 1: 100 in molar ratio, joins in the above-mentioned solution A, under magnetic agitation, obtains homogeneous system B;
3. under the magnetic agitation condition, be that the aqueous solution of 2% ammonium persulfate slowly joins among the homogeneous system B that 2. step make with percentage by weight, obtain solution C; Ammonium persulfate that is added and the step acrylic acid weight ratio in 1. is 0.1: 1;
4. the C solution that 3. step is obtained heated 0.1 hour at 80 ℃, made polymerization-filling complete; At 150 ℃ of dry 5h, obtain solid then; Grind the cooling back, places in the Muffle furnace again, under air atmosphere, 900 ℃ of conditions, calcines 1h, has promptly made caesious antimony-doped tin oxide nano powder.
The antimony-doped tin oxide nano powder good dispersion that adopts method for preparing to obtain, size is even, and in 100～500nm scope, the specific insulation of powder is 3000 Ω cm.
Embodiment 4
1. 4 parts by weight of acrylic are dissolved in the deionized water of 1 weight portion, fully dissolving obtains solution A under magnetic agitation;
2. fixedly the weight ratio of tin tetrabromide and solution A is 5: 100, and trichloride antimony and tin tetrabromide were weighed in 5: 100 in molar ratio, joins in the above-mentioned solution A, under magnetic agitation, obtains homogeneous system B;
3. under the magnetic agitation condition, be that the deionized water solution of 5% potassium peroxydisulfate slowly joins among the homogeneous system B that 2. step make with percentage by weight, obtain solution C; Potassium peroxydisulfate that is added and the step acrylic acid weight ratio in 1. is 0.01: 1;
4. the solution C that 3. step is obtained heats 1h at 100 ℃, makes polymerization-filling complete; At 80 ℃ of dry 24h, obtain solid then; Grind cooling back, places in the Muffle furnace again, at air atmosphere, 700 ℃ calcining 3h down, has promptly made caesious antimony-doped tin oxide nano powder.
The antimony-doped tin oxide nano powder good dispersion that adopts method for preparing to obtain, size is even, and in 50～200nm scope, the specific insulation of powder is 300 Ω cm.
Embodiment 5
1. 4 parts by weight of acrylic are dissolved in the deionized water of 1 weight portion, fully dissolving obtains solution A under magnetic agitation;
2. fixedly the weight ratio of tin tetrafluoride and solution A is 5: 100, and antimony acetate and tin tetrafluoride were weighed in 5: 100 in molar ratio, joins in the above-mentioned solution A, under magnetic agitation, obtains homogeneous system B;
3. be that the deionized water solution of 5% potassium peroxydisulfate slowly joins under the magnetic agitation condition among the homogeneous system B that 2. step make with percentage by weight, obtain solution C; Potassium peroxydisulfate that is added and the step acrylic acid weight ratio in 1. is 0.01: 1;
4. the solution C that 3. step is obtained heats 1h at 100 ℃, makes polymerization-filling complete; At 80 ℃ of dry 24h, obtain solid then; Grind cooling back, places in the Muffle furnace again, and under air atmosphere, 700 ℃ of conditions, calcining 3h has promptly made caesious antimony-doped tin oxide nano powder.
The antimony-doped tin oxide nano powder good dispersion that adopts method for preparing to obtain, size is even, and in 50～300nm scope, the specific insulation of powder is 500 Ω cm.
Embodiment 6
1. 4 parts by weight of acrylic are dissolved in the deionized water of 1 weight portion, fully dissolving obtains solution A under magnetic agitation;
2. fixedly the weight ratio of tin tetrafluoride and solution A is 5: 100, and antimony sulfate and tin tetraiodide were weighed in 5: 100 in molar ratio, joins in the above-mentioned solution A, under magnetic agitation, obtains homogeneous system B;
3. under the magnetic agitation condition, be that the deionized water solution of 5% ammonium persulfate slowly joins among the homogeneous system B that 2. step make with percentage by weight, obtain solution C; Ammonium persulfate that is added and the step acrylic acid weight ratio in 1. is 0.01: 1;
4. the C solution that 3. step is obtained heated 1 hour at 100 ℃, made polymerization-filling complete; At 80 ℃ of dry 24h, obtain solid then; Grind cooling back, places in the Muffle furnace again, and under air atmosphere, 700 ℃ of conditions, calcining 3h has promptly made caesious antimony-doped tin oxide nano powder.
The antimony-doped tin oxide nano powder good dispersion that adopts method for preparing to obtain, size is even, and in 100～300nm scope, the specific insulation of powder is 450 Ω cm.
To sum up, adopt the antimony-doped tin oxide nano-powder lighter color of technical scheme preparation of the present invention, be the light gray color; And the purity of powder is higher, good dispersion, and size is even, in 20～500nm scope.
Claims (3)
1. the preparation method of an antimony-doped tin oxide nano-powder is characterized in that, may further comprise the steps:
1. be that 1～4: 1 acrylic acid mixes with water with ratio of weight and number, solution A;
2. take by weighing soluble antimonic salt and pink salt, join in the above-mentioned solution A, dissolving gets homogeneous system B, wherein Sb
3+With Sn
4+The molfraction ratio be 1～15: 100, the ratio of weight and number of pink salt and solution A is 1～25: 100;
3. under stirring condition, be that the aqueous solution of 2～10% peroxide initator joins among the homogeneous system B with weight content, solution C; Said peroxide initator is potassium peroxydisulfate or ammonium persulfate; Said peroxide initator and acrylic acid weight ratio are 0.01～0.1: 1;
4. solution C is heated 0.1～3h at 60～100 ℃, obtain solid 80～150 ℃ of dryings then; Grind cooling back, and under air atmosphere, 450～900 ℃, calcining 1～10h.
2. the preparation method of antimony-doped tin oxide nano-powder according to claim 1; It is characterized in that: the antimonic salt of step described in 2. is antimony chloride, antimony acetate or antimony sulfate, and described pink salt is butter of tin, tin tetrabromide, tin tetrafluoride or tin tetraiodide.
3. the preparation method of antimony-doped tin oxide nano-powder according to claim 1 is characterized in that: the calcining of step described in 4. is in Muffle furnace.
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| CN102976396A (en) * | 2012-12-21 | 2013-03-20 | 苏州大学 | Method for preparing stibium doped stannic oxide nano-powder |
| CN104710883B (en) * | 2015-03-23 | 2018-05-04 | 苏州卫优知识产权运营有限公司 | A kind of glass door and window clear dope and preparation method thereof |
| CN107473263A (en) * | 2016-06-07 | 2017-12-15 | 杭州聚力氢能科技有限公司 | The preparation method of superfine high-purity degree antimony-doped tin oxide nano powder |
| CN112624182B (en) * | 2020-12-15 | 2023-03-31 | 佛山欧神诺陶瓷有限公司 | Antistatic material and preparation method and application thereof |
| CN114685861A (en) * | 2022-03-14 | 2022-07-01 | 太原理工大学 | Fly ash loaded nano antimony doped tin oxide composite material and preparation method thereof |
| CN115287040A (en) * | 2022-08-05 | 2022-11-04 | 佛山市兰可馨环保科技有限公司 | Preparation method of anti-static composite material |
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| CN1891633A (en) * | 2005-07-01 | 2007-01-10 | 中南大学 | Method for preparing nano antimony-doped tin dioxide powder |
| CN101037224A (en) * | 2007-02-15 | 2007-09-19 | 苏州大学 | Preparation process of antimony doped stannum oxide nano-crystal |
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Patent Citations (4)
| Publication number | Priority date | Publication date | Assignee | Title |
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| CN1891633A (en) * | 2005-07-01 | 2007-01-10 | 中南大学 | Method for preparing nano antimony-doped tin dioxide powder |
| CN101037224A (en) * | 2007-02-15 | 2007-09-19 | 苏州大学 | Preparation process of antimony doped stannum oxide nano-crystal |
| WO2009047302A1 (en) * | 2007-10-09 | 2009-04-16 | Chemip B.V. | Dispersion of nanoparticles in organic solvents |
| CN101428849A (en) * | 2008-12-03 | 2009-05-13 | 江苏柏鹤涂料有限公司 | Stibium doped tin dioxide nano-powder and method for producing the same |
Non-Patent Citations (1)
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