CN105645465A - Process for preparing stannic oxide nano-powder through sintering method - Google Patents
Process for preparing stannic oxide nano-powder through sintering method Download PDFInfo
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- CN105645465A CN105645465A CN201610053656.9A CN201610053656A CN105645465A CN 105645465 A CN105645465 A CN 105645465A CN 201610053656 A CN201610053656 A CN 201610053656A CN 105645465 A CN105645465 A CN 105645465A
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- stannic oxide
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- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- 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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- 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
- C01P2006/60—Optical properties, e.g. expressed in CIELAB-values
- C01P2006/64—Optical properties, e.g. expressed in CIELAB-values b* (yellow-blue axis)
Abstract
The invention relates to the field of preparation of stannic oxide powder, in particular to a process for preparing stannic oxide nano-powder through an intermittent water heating method. The process includes the steps of dissolving SnCl4.5H2O in deionized water to prepare a solution, putting the solution in a constant-temperature water bath, dropwise adding ammonia to the solution, conducting stirring and reacting to generate sol Sn(OH)4, washing the sol Sn(OH)4 with deionized water, then conducting centrifugal separation, conducting ultrasonic dispersion on deposit obtained through separation to obtain a precursor, washing the precursor with absolute ethyl alcohol, conducting centrifugal separation, drying and grinding a separated-out product, and putting ground powder in a furnace to be sintered to obtain the stannic oxide nano-powder. The stannic oxide precursor is prepared through SnCl4 and ammonia, chloride ion removal and dispersion are conducted on the precursor, and a firm foundation is laid for preparing the stannic oxide nano-powder; meanwhile, by sintering the precursor, nanometer products small in granularity and uniform in distribution are prepared, and preparation efficiency is improved.
Description
Technical field
The present invention relates to the preparation field of tin dioxide powder, the technique that specifically roasting method prepares stannic oxide nano powder.
Background technology
At present, one of nano-stannic oxide study hotspot having become as nano material. It is take reliable and effective technological parameter and preparation method that microscopic characteristics such as preparing the structure of stannic oxide nano powder, granularity, pattern, particle size distribution is carried out autotelic regulation and control that stannic oxide nano powder obtains efficient and wide variety of premise, and then meets its application requirement at specific area; And the effective way improving every application performance of stannic oxide nano powder is to prepare the nano-powder that particle diameter is less.
Its optical property is had significant impact by the particle diameter of usual nano-powder, when particle diameter of nanometer powder is less than 20nm, nano-powder has good optical property, and namely quantum size effect can affect the optical property of nano-powder, making optical absorption spectra generation blue shift, quasiconductor energy gap increases. Tin dioxide nanometer material is one of a few oxide semiconductor being easily achieved quantum size effect, when the tin dioxide powder prepared is closely sized to its Bohr radius, has obvious quantum size effect.
The existing research about stannic oxide nano powder preparation method is a lot, and including solid phase method, vapor phase method and liquid phase method etc., wherein liquid phase method has that cost is low, reaction condition is gentle, simple operation and other advantages, is widely adopted. Liquid preparation methods Nanometer Tin Dioxide Particles generally includes precursor power and two steps of crystallization, and the properties of product prepared all are had a great impact by the technological parameter of precursor preparation and crystallization process. Owing to existing method exists bigger shortcoming in technology controlling and process etc., cause that the properties of product of stannic oxide nano powder produced are not good enough.
Summary of the invention
For the problems referred to above, the present invention provides a kind of and produces the technique that the less roasting method of particle diameter prepares stannic oxide nano powder.
This invention address that the technical scheme that above-mentioned technical problem adopts is: roasting method prepares the technique of stannic oxide nano powder, comprises the following steps:
(1) by SnCl4��5H2O is dissolved in deionized water and is configured to solution;
(2) being placed in water bath with thermostatic control by above-mentioned solution, and drip ammonia in this solution, stirring reaction generates Sn(OH)4Colloidal sol;
(3) by Sn(OH)4The laggard row centrifugation of colloidal sol deionized water wash, then by separating obtained precipitate ultrasonic disperse, obtain tin ash presoma;
(4) use absolute ethanol washing precursor again, be then centrifuged for separating, isolated product is dried, grinds;
(5) powder body after grinding is placed in kiln roasting, obtains stannic oxide nano powder.
As preferably, the volume ratio adding hydrochloric acid, hydrochloric acid and deionized water in the deionized water in step (1) is 1:70.
As preferably, the SnCl of preparation in step (1)4The concentration of solution is 0.05 0.1mol/L.
As preferably, the temperature of water bath with thermostatic control in step (2) keeps 30--40 DEG C.
As preferably, the ammonia concn that step (2) drips is 5 10wt%, and after having reacted, the pH value of solution is 7.5 8.5.
As preferably, during dry in step (4), in thermostatic drying chamber, carry out 80 DEG C of dry 12h.
As preferably, sintering temperature is 200--400 DEG C, and roasting time is 2 4h.
The present invention passes through SnCl4Prepare tin ash presoma with ammonia, and precursor is carried out removing chloride and dispersion, lay a solid foundation for preparing stannic oxide nanometer; Meanwhile, roasting presoma of the present invention, not only prepare the nanometer product that particle diameter is less and is evenly distributed, and improve preparation efficiency.
Detailed description of the invention
The present invention is described more detail below, and illustrative examples and explanation in this present invention are used for explaining the present invention, but not as a limitation of the invention.
The roasting method of the present invention prepares the technique of stannic oxide nano powder, comprises the following steps:
(1) by SnCl4��5H2It is 0.05 0.1mol/LSnCl that O be dissolved in deionized water to be configured to concentration4Solution, as solution concentration increases again, the tin ash particle diameter of preparation can increase, and affects performance; As concentration is too little, then can affect response speed, increase cost, and the tin ash change of size of preparation and inconspicuous; Wherein adopting the volume ratio that should add a small amount of hydrochloric acid, hydrochloric acid and deionized water during deionized water preparation solution is 1:70, can prevent SnCl4Hydrolysis.
(2) above-mentioned solution is placed in 30--40 DEG C of water bath with thermostatic control, in this solution, drips the ammonia of 5 10wt% while stirring, until the pH value of solution is 7.5 8.5, in the solution of this pH value, (OH)��Concentration is relatively big, and is centered around around crystal grain, (OH)��Repulsive interaction between ion can suppress the increase of crystal grain, thus the granule of less particle diameter can be obtained; Ammonia as precipitant, in 30--40 DEG C ionizable go out more (OH)��, and the concentration of employing 5 10wt%, make the OH that ionization goes out)��Increasing the saturation of solution, improve nucleation rate, reducing the response time, thus suppressing the increase of crystal grain; Concentration such as ammonia is excessive, the Sn(OH of generation)4Settling velocity speeds, and moment generates substantial amounts of micelle, and substantial amounts of micelle has little time dispersion and is susceptible to reunite, and is easily formed bigger granule; Course of reaction should make solution mixing fully, make the Sn(OH of generation)4Precipitation particles is grown perfect, granule uniform-spherical.
(3) by Sn(OH)4Colloidal sol deionized water wash, removes out impurity, it is to avoid affect follow-up reaction; Carrying out centrifugation after washing, after centrifugal, gained supernatant can remove chloride ion with silver nitrate; And separating obtained precipitate can adopt ultrasonic disperse so that the tin ash presoma arrived is better effects if when reaction.
(4) use absolute ethanol washing precursor again, be then centrifuged for separating, isolated product is dried, grinds;Adopt dehydrated alcohol to replace the moisture in precipitate, reduce granule degree of focus in dry run; Time dry, thermostatic drying chamber carries out 80 DEG C of dry 12h; Through twice washing, it is completely removed the impurity on presoma, improves the new energy of crystallization of presoma.
(5) powder body after grinding being placed in kiln roasting, obtain stannic oxide nano powder, sintering temperature is 200--400 DEG C, and roasting time is 2 4h.
Embodiment 1
By SnCl4��5H2It is 0.05mol/LSnCl that O be dissolved in deionized water to be configured to concentration4Solution, in deionized water, the volume ratio of hydrochloric acid and deionized water is 1:70; Above-mentioned solution is placed in 30 DEG C of waters bath with thermostatic control, in solution, drips the ammonia of 5wt% while stirring, until the pH value of solution is 7.5, it is thus achieved that Sn(OH)4Colloidal sol; Then by Sn(OH)4Colloidal sol deionized water wash, centrifugation, separating obtained precipitate adopts ultrasonic disperse, it is thus achieved that presoma; Again by precursor absolute ethanol washing, being then centrifuged separating, be placed in thermostatic drying chamber by the product of centrifugation and carry out 80 DEG C of dry 12h, be then ground, finally the roasting 4h when 200 DEG C, obtains stannic oxide nano powder. By analysis, this diameter of particle is all between 4 8nm.
Embodiment 2
By SnCl4��5H2It is 0.08mol/LSnCl that O be dissolved in deionized water to be configured to concentration4Solution, in deionized water, the volume ratio of hydrochloric acid and deionized water is 1:70; Above-mentioned solution is placed in 35 DEG C of waters bath with thermostatic control, in solution, drips the ammonia of 8wt% while stirring, until the pH value of solution is 8, it is thus achieved that Sn(OH)4Colloidal sol; Then by Sn(OH)4Colloidal sol deionized water wash, centrifugation, separating obtained precipitate adopts ultrasonic disperse, obtain presoma, again by precursor absolute ethanol washing, then it is centrifuged separating, the product of centrifugation is placed in thermostatic drying chamber and carries out 80 DEG C of dry 12h, be then ground, the last roasting 3h when 300 DEG C, obtains stannic oxide nano powder. By analysis, this diameter of particle is all between 1 5nm.
Embodiment 3
By SnCl4��5H2It is 0.1mol/LSnCl that O be dissolved in deionized water to be configured to concentration4Solution, in deionized water, the volume ratio of hydrochloric acid and deionized water is 1:70; Above-mentioned solution is placed in 40 DEG C of waters bath with thermostatic control, in solution, drips the ammonia of 10wt% while stirring, until the pH value of solution is 8.5, it is thus achieved that Sn(OH)4Colloidal sol; Then by Sn(OH)4Colloidal sol deionized water wash, centrifugation, separating obtained precipitate adopts ultrasonic disperse, it is thus achieved that presoma; Again by precursor absolute ethanol washing, being then centrifuged separating, be placed in thermostatic drying chamber by the product of centrifugation and carry out 80 DEG C of dry 12h, be then ground, finally the roasting 2h when 400 DEG C, obtains stannic oxide nano powder. By analysis, this diameter of particle is all between 1 3nm.
The technical scheme above embodiment of the present invention provided is described in detail, principle and the embodiment of the embodiment of the present invention are set forth by specific case used herein, and the explanation of above example is only applicable to help to understand the principle of the embodiment of the present invention; Simultaneously for one of ordinary skill in the art, according to the embodiment of the present invention, all will change in detailed description of the invention and range of application, in sum, this specification content should not be construed as limitation of the present invention.
Claims (7)
1. roasting method prepares the technique of stannic oxide nano powder, comprises the following steps:
(1) by SnCl4��5H2O is dissolved in deionized water and is configured to solution;
(2) being placed in water bath with thermostatic control by above-mentioned solution, and drip ammonia in this solution, stirring reaction generates Sn(OH)4Colloidal sol;
(3) by Sn(OH)4The laggard row centrifugation of colloidal sol deionized water wash, then by separating obtained precipitate ultrasonic disperse, obtain tin ash presoma;
(4) use absolute ethanol washing precursor again, be then centrifuged for separating, isolated product is dried, grinds;
(5) powder body after grinding is placed in kiln roasting, obtains stannic oxide nano powder.
2. the technique preparing stannic oxide nano powder according to claim 1, it is characterised in that: the volume ratio adding hydrochloric acid, hydrochloric acid and deionized water in the deionized water in step (1) is 1:70.
3. the technique preparing stannic oxide nano powder according to claim 1, it is characterised in that: the SnCl of preparation in step (1)4The concentration of solution is 0.05 0.1mol/L.
4. the technique preparing stannic oxide nano powder according to claim 1, it is characterised in that: the temperature of water bath with thermostatic control in step (2) keeps 30--40 DEG C.
5. the technique preparing stannic oxide nano powder according to claim 1, it is characterised in that: the ammonia concn that step (2) drips is 5 10wt%, and after having reacted, the pH value of solution is 7.5 8.5.
6. the technique preparing stannic oxide nano powder according to claim 1, it is characterised in that: in thermostatic drying chamber, carry out 80 DEG C of dry 12h during dry in step (4).
7. the technique preparing stannic oxide nano powder according to claim 6, it is characterised in that: sintering temperature is 200--400 DEG C, and roasting time is 2 4h.
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Cited By (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN106766676A (en) * | 2016-12-20 | 2017-05-31 | 西北稀有金属材料研究院 | A kind of drying means of tin oxide precursor powder |
| CN110921699A (en) * | 2019-12-10 | 2020-03-27 | 山东工商学院 | Method for preparing flat plate type gas sensor based on pollen structure tin dioxide |
| CN113697848A (en) * | 2021-07-13 | 2021-11-26 | 芜湖映日科技股份有限公司 | Method for manufacturing tin oxide powder of ITO target material |
Citations (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1724383A (en) * | 2005-06-21 | 2006-01-25 | 电子科技大学 | Process for preparing one-dimensional nano tin dioxide material |
| CN101643238A (en) * | 2009-06-22 | 2010-02-10 | 云南锡业集团（控股）有限责任公司 | Method for producing tin dioxide |
| CN103739006A (en) * | 2013-12-12 | 2014-04-23 | 宁夏东方钽业股份有限公司 | Preparation method of superfine highly-pure tin oxide |
| CN104528811A (en) * | 2015-01-20 | 2015-04-22 | 天津大学 | One-step hydrothermal method for preparing highly dispersed tin oxide (SnO2) nanoparticles |
-
2016
- 2016-01-27 CN CN201610053656.9A patent/CN105645465A/en active Pending
Patent Citations (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1724383A (en) * | 2005-06-21 | 2006-01-25 | 电子科技大学 | Process for preparing one-dimensional nano tin dioxide material |
| CN101643238A (en) * | 2009-06-22 | 2010-02-10 | 云南锡业集团（控股）有限责任公司 | Method for producing tin dioxide |
| CN103739006A (en) * | 2013-12-12 | 2014-04-23 | 宁夏东方钽业股份有限公司 | Preparation method of superfine highly-pure tin oxide |
| CN104528811A (en) * | 2015-01-20 | 2015-04-22 | 天津大学 | One-step hydrothermal method for preparing highly dispersed tin oxide (SnO2) nanoparticles |
Non-Patent Citations (2)
| Title |
|---|
| HONGLIANG ZHU等: "A simple hydrothermal route for synthesizing SnO2 quantum dots", 《NANOTECHNOLOGY》 * |
| 曾秋花: "水热法制备二氧化锡纳米粉体研究", 《中国优秀硕士学位论文全文数据库 工程科技Ⅰ辑》 * |
Cited By (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN106766676A (en) * | 2016-12-20 | 2017-05-31 | 西北稀有金属材料研究院 | A kind of drying means of tin oxide precursor powder |
| CN110921699A (en) * | 2019-12-10 | 2020-03-27 | 山东工商学院 | Method for preparing flat plate type gas sensor based on pollen structure tin dioxide |
| CN113697848A (en) * | 2021-07-13 | 2021-11-26 | 芜湖映日科技股份有限公司 | Method for manufacturing tin oxide powder of ITO target material |
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Application publication date: 20160608 |