CN102010197A - Method for preparing antimony-doped tin oxide (ATO) nano powder - Google Patents
Method for preparing antimony-doped tin oxide (ATO) nano powder Download PDFInfo
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Abstract
The invention discloses a method for preparing antimony-doped tin oxide (ATO) nano powder, which comprises the following steps of: preparing a precursor under the certain reaction condition; and standing, filtering, eluting, coating, drying, grinding, screening and burning the precursor to obtain ATO nano powder. A coating and drying way is introduced into the preparation process of the powder for the first time, and the obtained ATO nano powder has high dispersibility and less agglomeration; the appearance of the powder is spherical or similarly spherical, and the powder has the grain diameter of 5-10nm, small distributing range of the grain diameter, the resistivity of 1-5ohm.cm and the bulk density of 0.4-1.5g.cm<-3>; and compared with a direct drying way without coating treatment, the invention obviously improves the dispersibility of the powder and reduces the bulk density of the power by half or so. Meanwhile, the invention has the obvious characteristics of simple process, low cost, short reaction period, high yield, easy control of the reaction process and convenience for industrialized mass production.
Description
Technical field
The present invention relates to field of nanometer material technology, relate in particular to a kind of preparation method with antimony-doped tin oxide (ATO) nano-powder of air-sensitive performance and photoelectric properties.
Background technology
Antimony-doped tin oxide, be that ATO is a kind of important gas sensitive, conduction antistatic material and catalyzer and catalyst support material, it is compared with traditional metallic conduction antistatic material, the chemical stability and the weathering resistance of ATO material are better, compare with carbon black, carbon nanotube then to have the more shallow advantage of color; In addition, the electroconductibility of ATO material is higher than the conductive polymer antistatic material.Therefore, the ATO nano-powder more and more causes people's attention in the application in the antistatic field of conduction.It is the main direction that the ATO nano material is used that the ATO nano-powder is distributed to the resistivity that reduces matrix material in insulating plastics or the resin.Deng is superfine, and to mix massfraction in the PET-PEE fiber be 2% ATO powder, makes the ratio resistance of fiber reduce by 5 orders of magnitude, reaches 3.4 * 10
8Ω cm (East China University of Science's journal, 2009,35:p378-384).In recent years, have some about the report of ATO nano-powder at field of textiles.China is the production and consumption big country of chemical fibre, and the man-made fiber antistatic treatment will be the application market of ATO nano-powder maximum.The specific surface area that the ATO nano-powder is huge is easy to attached to fiber surface it, overcome the shortcoming of its fastness and feel difference in field of textiles is used.The ATO particle diameter of nanometer powder is more little, and dispersiveness is good more, and specific surface area is just big more, and antistatic effect is just good more.In addition, the loose density of ATO is more little, and the shared volume of ATO is just big more in the unit volume fiber, thereby can reduce the consumption of ATO nano-powder in fiber, and then reduces cost.
The ATO nano-powder of China's preparation, its loose density minimum is at 0.5gcm
-3About.Japan can prepare loose density and have only 0.4gcm
-3The ATO powder, but price is higher, greatly about about 1000 yuan/Kg.In addition, the antistatic effect of ATO is also closely related with the electroconductibility of ATO itself.
At present, the method for preparing the ATO nano-powder has people such as Zhang Jianrong (Chinese Journal of Inorganic Chemistry, 2004,20 (7): the p801-804) combustion synthesis method of Ti Chuing; People such as D.W.Jung (Applied Surface Science, 2009,255:p5409-5413) the DC arc light plasma splash method of Ti Chuing; People such as Q.H (Micro﹠amp; Nano Letters, 2007,2 (1): the p17-19) chemical precipitation method of Ti Chuing; People such as Gong Sheng (colleges and universities' chemical engineering journal, 2009,23 (3): p460-465) the supercritical fluid drying technology of Ti Chuing; People such as Li Lili (Rare Metals Materials journal, 2006,35 (3): p442-447) the heterogeneous nucleation process of Ti Chuing; People such as T.Nutz (Journal of ChemicalPhysics, 1999,110 (24): p12142-12150) hydrothermal method of Ti Chuing etc.
Chemical precipitation method is compared advantages such as to have technology simple, and cost is low, and output is big with additive method, but the gained powder is easy to reunite, and is dispersed bad, seriously limited its application.The introducing of supercritical fluid drying technology, interpolation dispersion agent, heterogeneous one-tenth nuclear technique can obviously improve powder dispersity.It is the simplest wherein to add dispersion agent, most widely used.The supercritical fluid drying The Application of Technology is subjected to the influence of equipment complexity, be unfavorable for applying, though but not the homogeneous nucleation method can reduce reunion, improve dispersedly, effect is general.Given this, seek a kind of simply efficient, the gained diameter of particle is little, good dispersity, and the good novel process of electrical properties becomes a difficult problem that needs to be resolved hurrily.
Summary of the invention
In view of existing in prior technology the problems referred to above, the present invention is intended to disclose a kind of preparation method of ATO nano-powder, and this method relates to utilizes chemical coprecipitation method, prepares target powder by adding dispersion agent and wrapping up drying mode; Gained ATO nano-powder has good dispersity, and particle diameter is little, and loose density is low, the characteristics that electrical properties is good.
Technical solution of the present invention is achieved in that
A kind of preparation method of antimony-doped tin oxide nano-powder comprises the steps:
(1) preparation presoma: with the solution of certain density antimony ion and tin ion, with certain molar ratio, mix, mixing solutions and certain density ammonia soln are added drop-wise in the deionized water that fills the finite concentration dispersion agent simultaneously, under certain reaction temperature, reaction times, pH value and stirring velocity, synthesize flaxen precipitation presoma;
(2) described presoma is left standstill for some time after, filter, the gained filter cake is respectively through deionized water and dehydrated alcohol drip washing;
(3) parcel is dry: the presoma filter cake is wrapped up dry 0.5-5h under 50-150 ℃ with encapsulate substances;
(4) presoma after the oven dry sieves through grinding, calcines 0.5-4h down at 500-900 ℃, gets blue antimony-doped tin oxide, i.e. ATO nano-powder;
In the step (1), the concentration of antimony ion is 0.05-5mol/L in the solution, and the concentration of tin ion is 0.05-5mol/L, and the concentration of ammonia soln is 0.05-13mol/L, and the mol ratio of described antimony ion and tin ion is 3-30%, and preferred version is 5-20%; Described temperature of reaction is 40-100 ℃, and the reaction times is 0.5-4h, and the pH value is 2-11, and preferred version is 3-4; Stirring velocity is 5-30rps;
In the step (2), the time of leaving standstill is 0.05-48h;
In the step (4), the particle diameter of gained ATO nano-powder is 5-10nm, and resistivity is 1-5 Ω cm, and the powder loose density is at 0.4-1.5gcm
-3
Further, in the step (1), described antimony ion is metallic antimony, antimonous oxide or antimony peroxide and hydrochloric acid, nitric acid or effect of sulfuric acid and get, or the compound dissolution of butter of antimony or antimony pentachloride and getting; Described tin ion is metallic tin and hydrochloric acid, nitric acid or effect of sulfuric acid and get, or the compound dissolution of tin protochloride, tin tetrachloride and getting.
Described dispersion agent is one or more mixing in polyvinyl alcohol, polyoxyethylene glycol, the polyvinyl lactam, and the ratio of the quality of dispersion agent and metallic tin (or tin ion) quality is between 2-10%.
In the step (3), described encapsulate substances is a qualitative filter paper, or quantitative paper, or material such as towel, cloth, oilpaper.
In the step (4), need through grinding 200 mesh sieves after the presoma oven dry.
The present invention utilizes the liquid phase chemical coprecipitation method to prepare a kind of ATO nano-powder material that can be used for fields such as gas sensor, conduction static inhibitor, transparency conductive electrode, catalyzer and support of the catalyst, will wrap up drying mode first to be incorporated in the powder preparing process; Because water and ethanol all have certain surface tension and capillary force, these reactive forces can cause that particulate is reunited and the increase of particle diameter.The parcel dry technology makes the enveloped high pressure to a certain degree that formed when drying, gas density is big under the high pressure, and the molecule discontinuity equalization degree in the fluid surface layer is reduced, and surface tension of liquid diminishes.The solubleness of gas in liquid strengthens under the high pressure in addition, has changed the composition of liquid, has also reduced surface tension.The influence of pressure then is both comprehensive results, capillaryly reduces to have reduced that particulate is reunited and growth velocity, thereby has improved dispersiveness.
Compared with prior art, preparation method's disclosed in this invention characteristics are very outstanding:
By the ATO nano-powder good dispersity that the present invention obtains, it is few to reunite; Morphology microstructure is sphere or class sphere, and particle diameter is between 5-10nm, and particle size distribution range is little, and resistivity is between 1-5 Ω cm, and the powder loose density is at 0.4-1.5gcm
-3Between; Compare with the convection drying mode of not wrapping up processing, the dispersiveness of powder is improved significantly and the loose density of powder has reduced about half.
And its technology is simple, and cost is low, and reaction time is short, the productive rate height, and reaction process is easy to control, is convenient to industrialized mass production.
Description of drawings
Fig. 1 a is not for wrapping up the selected area electron diffraction (left side) and the transmission electron micrograph (right side) of the dry ATO powder that makes;
Fig. 1 b is selected area electron diffraction (left side) transmission electron micrograph (stone) of the dry ATO powder that makes of parcel;
Fig. 2 is not for wrapping up loose density comparison diagram dry and the dry ATO powder that makes respectively of parcel.
Embodiment
Take by weighing metallic tin grain 11.87g, measure the nitric acid 40ml of 7.5mol/L, the hydrochloric acid 50ml of 6mol/L, 80 degrees centigrade of reactions 30 minutes obtain tin ion solution with metallic tin dissolving.Weighing butter of antimony 1.2g is with obtaining antimony ion solution after the dissolving of 10ml concentrated hydrochloric acid.Weighing polyvinyl alcohol 0.6g obtains polyvinyl alcohol solution with the 100mL deionized water dissolving.Tin ion solution and the mixing of antimony ion solution are obtained mixing solutions, simultaneously dropwise be added drop-wise in the polyvinyl alcohol solution ammonia soln of mixing solutions and 13mol/L, control reaction temperature is 65 ℃, stir and obtained faint yellow colloid shape precipitation presoma in 1 hour, this presoma is left standstill 24 hours after-filtration.The filter cake that filtration obtains again with after the deionized water drip washing 5 times with dehydrated alcohol drip washing 2 times, select two kinds of drying modes, a kind of for filter cake is wrapped up with the middling speed qualitative filter paper, the second way is without filter paper parcel filter cake, with parcel and not the filter cake of parcel be placed into simultaneously in the loft drier in 100 ℃ dry 5 hours down, grind and cross 200 mesh sieves after the presoma that obtains after the drying is cooled to room temperature.The presoma that obtains that will sieve at last promptly obtains blue ATO nano-powder in 600 ℃ of calcinings after 2 hours.Drying mode is to ATO powder structure and dispersed influence, and as shown in Figure 1, the result shows that two kinds of powders are nano-multicrystal, have cubic rutile-type stannic oxide structure, parcel exsiccant powder dispersity is better, without any reunion, powder is spherical, and particle diameter is about 8nm, shown in Fig. 1 b; Bao Guo powder dispersity is not relatively poor, has agglomeration, and particle diameter is also about 8nm, as shown in Figure 1a.Contrast the loose density of two kinds of prepared two kinds of powders of drying mode, as shown in Figure 2, the result shows that parcel exsiccant powder loose density is less, at 0.67gcm
-3It is bigger not wrap up exsiccant powder loose density, at 1.22gcm
-3The powder resistance rate that other wraps up that desiccating method obtains is 5 Ω cm, and the dry powder resistance rate that obtains of parcel is not 2.4 Ω cm.
Take by weighing metallic tin grain 11.87g, measure the nitric acid 45ml of 6mol/L, the hydrochloric acid 40ml of 8mol/L, 80 degrees centigrade of reactions 30 minutes obtain tin ion solution with metallic tin dissolving.Weighing butter of antimony 4.8g is with obtaining antimony ion solution after the dissolving of 30ml concentrated hydrochloric acid.Weighing polyvinyl alcohol 0.6g obtains polyvinyl alcohol solution with the 100mL deionized water dissolving.Tin ion solution and the mixing of antimony ion solution are obtained mixing solutions, simultaneously dropwise be added drop-wise in the polyvinyl alcohol solution ammonia soln of mixing solutions and 13mol/L, control reaction temperature is 65 degrees centigrade, stir and obtained faint yellow colloid shape precipitation presoma in 1 hour, this presoma is left standstill 24 hours after-filtration.The filter cake that filtration obtains again with after the deionized water drip washing 3 times with dehydrated alcohol drip washing 1 time, with the middling speed qualitative filter paper filter cake is wrapped up, with the filter cake of parcel be placed in the loft drier in 100 ℃ dry 5 hours down, grind and cross 200 mesh sieves after the presoma that obtains after the drying is cooled to room temperature.The presoma that obtains that will sieve at last promptly obtains blue ATO nano-powder in 600 ℃ of calcinings after 2 hours.Measuring result shows that the ATO diameter of particle that obtains is at 5.8nm, and loose density is 0.42gcm
-3, resistivity is 4.3 Ω cm.
Embodiment 3
Take by weighing metallic tin grain 11.87g, measure the nitric acid 45ml of 6mol/L, the hydrochloric acid 40ml of 8mol/L, 80 degrees centigrade of reactions 30 minutes obtain tin ion solution with metallic tin dissolving.Weighing butter of antimony 3.6g is with obtaining antimony ion solution after the dissolving of 25ml concentrated hydrochloric acid.Weighing polyvinyl alcohol 0.6g obtains polyvinyl alcohol solution with the 100mL deionized water dissolving.Tin ion solution and the mixing of antimony ion solution are obtained mixing solutions, simultaneously dropwise be added drop-wise in the polyvinyl alcohol solution ammonia soln of mixing solutions and 13mol/L, control reaction temperature is 65 degrees centigrade, stir and obtained faint yellow colloid shape precipitation presoma in 1 hour, this presoma is left standstill 24 hours after-filtration.The filter cake that filtration obtains again with after the deionized water drip washing 4 times with dehydrated alcohol drip washing 2 times, with the middling speed qualitative filter paper filter cake is wrapped up, with the filter cake of parcel be placed in the loft drier in 100 ℃ dry 5 hours down, grind and cross 200 mesh sieves after the presoma that obtains after the drying is cooled to room temperature.The presoma that obtains that will sieve at last promptly obtains blue ATO nano-powder in 600 ℃ of calcinings after 2 hours.The result shows that the ATO diameter of particle that obtains is at 6.5nm, and loose density is 0.5gcm
-3, resistivity is 3 Ω cm.
Embodiment 4
Take by weighing metallic tin grain 11.87g, measure the nitric acid 45ml of 6mol/L, the hydrochloric acid 40ml of 8mol/L, 80 degrees centigrade of reactions 30 minutes obtain tin ion solution with metallic tin dissolving.Weighing butter of antimony 1.2g is with obtaining antimony ion solution after the dissolving of 25ml concentrated hydrochloric acid.Weighing polyvinyl alcohol 0.8g obtains polyvinyl alcohol solution with the 100mL deionized water dissolving.Tin ion solution and the mixing of antimony ion solution are obtained mixing solutions, simultaneously dropwise be added drop-wise in the polyvinyl alcohol solution ammonia soln of mixing solutions and 13mol/L, control reaction temperature is 50 degrees centigrade, stir and obtained faint yellow colloid shape precipitation presoma in 1 hour, this presoma is left standstill 24 hours after-filtration.The filter cake that filtration obtains again with after the deionized water drip washing 4 times with dehydrated alcohol drip washing 2 times, with the middling speed qualitative filter paper filter cake is wrapped up, with the filter cake of parcel be placed in the loft drier in 100 ℃ dry 5 hours down, grind and cross 200 mesh sieves after the presoma that obtains after the drying is cooled to room temperature.The presoma that obtains that will sieve at last promptly obtains blue ATO nano-powder in 600 ℃ of calcinings after 2 hours.The result shows that the ATO diameter of particle that obtains is at 8nm, and loose density is 0.9gcm
-3, resistivity is 1.5 Ω cm.
Embodiment 5
Take by weighing metallic tin grain 11.87g, measure the nitric acid 45ml of 6mol/L, the hydrochloric acid 40ml of 8mol/L, 80 degrees centigrade of reactions 30 minutes obtain tin ion solution with metallic tin dissolving.Weighing butter of antimony 1.2g is with obtaining antimony ion solution after the dissolving of 25ml concentrated hydrochloric acid.Measure polyoxyethylene glycol-4000.6ml, it is mixed obtaining polyvinyl alcohol solution with the 100mL deionized water.Tin ion solution and the mixing of antimony ion solution are obtained mixing solutions, simultaneously dropwise be added drop-wise in the polyglycol solution ammonia soln of mixing solutions and 13mol/L, control reaction temperature is 75 degrees centigrade, stir and obtained faint yellow colloid shape precipitation presoma in 0.5 hour, this presoma is left standstill 24 hours after-filtration.The filter cake that filtration obtains again with after the deionized water drip washing 4 times with dehydrated alcohol drip washing 2 times, with the middling speed qualitative filter paper filter cake is wrapped up, with the filter cake of parcel be placed in the loft drier in 100 degrees centigrade ℃ dry 5 hours down, grind and cross 200 mesh sieves after the presoma that obtains after the drying is cooled to room temperature.The presoma that obtains that will sieve at last promptly obtains blue ATO nano-powder in 700 ℃ of calcinings after 2 hours.The result shows that the ATO diameter of particle that obtains is at 9nm, and loose density is 0.8gcm
-3, resistivity is 1.9 Ω cm.
Embodiment 6
Take by weighing stannic chloride pentahydrate 26g, obtain tin ion solution with the 100ml deionized water dissolving.Weighing butter of antimony 1.2g is with obtaining antimony ion solution after the dissolving of 25ml concentrated hydrochloric acid.Measure polyvinyl lactam 0.6g, it is mixed obtaining polyvinyl lactam solution with the 100mL deionized water.Tin ion solution and the mixing of antimony ion solution are obtained mixing solutions, the ammonia soln of mixing solutions and 13mol/L dropwise is added drop-wise in the polyvinyl lactam solution simultaneously, control reaction temperature is 75 degrees centigrade, stir and obtained faint yellow colloid shape precipitation presoma in 0.5 hour, this presoma is left standstill 24 hours after-filtration.The filter cake that filtration obtains again with after the deionized water drip washing 4 times with dehydrated alcohol drip washing 2 times, with the middling speed qualitative filter paper filter cake is wrapped up, with the filter cake of parcel be placed in the loft drier in 120 ℃ dry 3 hours down, grind and cross 200 mesh sieves after the presoma that obtains after the drying is cooled to room temperature.The presoma that obtains that will sieve at last promptly obtains blue ATO nano-powder in 700 ℃ of calcinings after 2 hours.The result shows that the ATO diameter of particle that obtains is at 7nm, and loose density is 0.6gcm
-3, resistivity is 2.5 Ω cm.
In a word, as can be seen, adopt the ATO nano-powder of preparation method's gained of the present invention to have the branch good dispersity, few distinguishing feature of reuniting, the pattern of gained powder is sphere or class sphere, particle diameter is 5-10nm, particle size distribution range is little, and loose density is 0.4-1.5gcm
-3, resistivity is 1-5 Ω cm; Do not wrap up the exsiccant mode with tradition and compare, the gained powder has littler diameter of particle and loose density.
The above; only be the preferable embodiment of the present invention; but protection scope of the present invention is not limited thereto; anyly be familiar with those skilled in the art in the technical scope that the present invention discloses; be equal to replacement or change according to technical scheme of the present invention and inventive concept thereof, all should be encompassed within protection scope of the present invention.
Claims (7)
1. the preparation method of an antimony-doped tin oxide nano-powder comprises the steps:
(1) preparation presoma: with the solution of certain density antimony ion and tin ion, with certain molar ratio, mix, mixing solutions and certain density ammonia soln are added drop-wise in the deionized water that fills the finite concentration dispersion agent simultaneously, under certain reaction temperature, reaction times, pH value and stirring velocity, synthesize flaxen precipitation presoma;
(2) described presoma is left standstill for some time after, filter, the gained filter cake is respectively through deionized water and dehydrated alcohol drip washing;
(3) parcel is dry: the presoma filter cake is wrapped up dry 0.5-5h under 50-150 ℃ with encapsulate substances;
(4) presoma after the oven dry sieves through grinding, calcines 0.5-4h down at 500-900 ℃, gets blue antimony-doped tin oxide, i.e. ATO nano-powder;
In the step (1), the concentration of antimony ion is 0.05-5mol/L in the solution, and the concentration of tin ion is 0.05-5mol/L, and the concentration of ammonia soln is 0.05-13mol/L, and the mol ratio of described antimony ion and tin ion is 3-30%; Described temperature of reaction is 40-100 ℃, and the reaction times is 0.5-4h, and the pH value is 2-11, and stirring velocity is 5-30rps;
In the step (2), the time of leaving standstill is 0.05-48h;
In the step (4), the particle diameter of gained ATO nano-powder is 5-10nm, and resistivity is 1-5 Ω cm, and the powder loose density is at 0.4-1.5gcm
-3
2. the preparation method of antimony-doped tin oxide nano-powder according to claim 1 is characterized in that:
In the step (3), described encapsulate substances is a qualitative filter paper, or quantitative paper, or towel, cloth, oilpaper.
3. the preparation method of antimony-doped tin oxide nano-powder according to claim 1 is characterized in that:
In the step (1), described antimony ion is metallic antimony, antimonous oxide or antimony peroxide and hydrochloric acid, nitric acid or effect of sulfuric acid and get, or the compound dissolution of butter of antimony or antimony pentachloride and getting; Described tin ion is metallic tin and hydrochloric acid, nitric acid or effect of sulfuric acid and get, or the compound dissolution of tin protochloride, tin tetrachloride and getting.
4. the preparation method of antimony-doped tin oxide nano-powder according to claim 1 is characterized in that:
In the step (1), the mol ratio of described antimony ion and tin ion is 5-20%.
5. the preparation method of antimony-doped tin oxide nano-powder according to claim 1 is characterized in that:
In the step (1), described pH value is 3-4.
6. the preparation method of antimony-doped tin oxide nano-powder according to claim 1 is characterized in that:
In the step (1), described dispersion agent is one or more mixing in polyvinyl alcohol, polyoxyethylene glycol, the polyvinyl lactam, and the ratio of the quality of dispersion agent and metallic tin (or tin ion) quality is between 2-10%.
7. the preparation method of antimony-doped tin oxide nano-powder according to claim 1 is characterized in that:
In the step (4), need through grinding 200 mesh sieves after the presoma oven dry.
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