CN1796287A - Method for preparing Nano granules of stannic oxide - Google Patents
Method for preparing Nano granules of stannic oxide Download PDFInfo
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- CN1796287A CN1796287A CN 200410077780 CN200410077780A CN1796287A CN 1796287 A CN1796287 A CN 1796287A CN 200410077780 CN200410077780 CN 200410077780 CN 200410077780 A CN200410077780 A CN 200410077780A CN 1796287 A CN1796287 A CN 1796287A
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- Prior art keywords
- stannic oxide
- preparation
- citric acid
- nano granules
- microwave heating
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- XOLBLPGZBRYERU-UHFFFAOYSA-N tin dioxide Chemical compound O=[Sn]=O XOLBLPGZBRYERU-UHFFFAOYSA-N 0.000 title claims abstract description 39
- 239000008187 granular material Substances 0.000 title claims description 9
- 238000000034 method Methods 0.000 title abstract description 15
- KRKNYBCHXYNGOX-UHFFFAOYSA-N citric acid Chemical compound OC(=O)CC(O)(C(O)=O)CC(O)=O KRKNYBCHXYNGOX-UHFFFAOYSA-N 0.000 claims abstract description 54
- 239000002243 precursor Substances 0.000 claims abstract description 8
- 150000003839 salts Chemical class 0.000 claims abstract description 6
- 239000002994 raw material Substances 0.000 claims abstract description 4
- LYCAIKOWRPUZTN-UHFFFAOYSA-N Ethylene glycol Chemical compound OCCO LYCAIKOWRPUZTN-UHFFFAOYSA-N 0.000 claims description 26
- 238000010438 heat treatment Methods 0.000 claims description 19
- 238000002360 preparation method Methods 0.000 claims description 15
- -1 polyoxyethylene Polymers 0.000 claims description 14
- 229920003171 Poly (ethylene oxide) Polymers 0.000 claims description 13
- WGCNASOHLSPBMP-UHFFFAOYSA-N hydroxyacetaldehyde Natural products OCC=O WGCNASOHLSPBMP-UHFFFAOYSA-N 0.000 claims description 13
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Chemical compound O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims description 12
- 239000008367 deionised water Substances 0.000 claims description 11
- 229910021641 deionized water Inorganic materials 0.000 claims description 11
- 238000004090 dissolution Methods 0.000 claims description 3
- 239000002184 metal Substances 0.000 claims description 3
- 239000000243 solution Substances 0.000 claims description 3
- 229910021626 Tin(II) chloride Inorganic materials 0.000 claims description 2
- 239000012266 salt solution Substances 0.000 claims description 2
- 239000002105 nanoparticle Substances 0.000 abstract description 14
- 229910001887 tin oxide Inorganic materials 0.000 abstract description 5
- ATJFFYVFTNAWJD-UHFFFAOYSA-N Tin Chemical compound [Sn] ATJFFYVFTNAWJD-UHFFFAOYSA-N 0.000 abstract description 2
- 238000009826 distribution Methods 0.000 abstract description 2
- 239000002245 particle Substances 0.000 abstract description 2
- 238000004220 aggregation Methods 0.000 abstract 1
- 230000002776 aggregation Effects 0.000 abstract 1
- 238000004519 manufacturing process Methods 0.000 abstract 1
- 229920001223 polyethylene glycol Polymers 0.000 abstract 1
- 239000000203 mixture Substances 0.000 description 8
- 238000003756 stirring Methods 0.000 description 8
- 239000000463 material Substances 0.000 description 7
- 229910006404 SnO 2 Inorganic materials 0.000 description 3
- 229910002651 NO3 Inorganic materials 0.000 description 2
- NHNBFGGVMKEFGY-UHFFFAOYSA-N Nitrate Chemical compound [O-][N+]([O-])=O NHNBFGGVMKEFGY-UHFFFAOYSA-N 0.000 description 2
- 239000003054 catalyst Substances 0.000 description 2
- 238000006555 catalytic reaction Methods 0.000 description 2
- 238000009841 combustion method Methods 0.000 description 2
- 239000004020 conductor Substances 0.000 description 2
- 238000001879 gelation Methods 0.000 description 2
- 230000007062 hydrolysis Effects 0.000 description 2
- 238000006460 hydrolysis reaction Methods 0.000 description 2
- 238000001027 hydrothermal synthesis Methods 0.000 description 2
- 230000003647 oxidation Effects 0.000 description 2
- 238000007254 oxidation reaction Methods 0.000 description 2
- 239000000843 powder Substances 0.000 description 2
- 230000005855 radiation Effects 0.000 description 2
- 238000003980 solgel method Methods 0.000 description 2
- 239000004215 Carbon black (E152) Substances 0.000 description 1
- KRKNYBCHXYNGOX-UHFFFAOYSA-K Citrate Chemical compound [O-]C(=O)CC(O)(CC([O-])=O)C([O-])=O KRKNYBCHXYNGOX-UHFFFAOYSA-K 0.000 description 1
- 102000008186 Collagen Human genes 0.000 description 1
- 108010035532 Collagen Proteins 0.000 description 1
- 230000010718 Oxidation Activity Effects 0.000 description 1
- 229910021627 Tin(IV) chloride Inorganic materials 0.000 description 1
- 239000002253 acid Substances 0.000 description 1
- 150000001299 aldehydes Chemical class 0.000 description 1
- 150000004703 alkoxides Chemical class 0.000 description 1
- 150000001735 carboxylic acids Chemical class 0.000 description 1
- 230000003197 catalytic effect Effects 0.000 description 1
- 238000009388 chemical precipitation Methods 0.000 description 1
- 238000006243 chemical reaction Methods 0.000 description 1
- 229920001436 collagen Polymers 0.000 description 1
- 238000009833 condensation Methods 0.000 description 1
- 230000005494 condensation Effects 0.000 description 1
- 239000013078 crystal Substances 0.000 description 1
- 238000002425 crystallisation Methods 0.000 description 1
- 230000008025 crystallization Effects 0.000 description 1
- 238000001035 drying Methods 0.000 description 1
- 238000001704 evaporation Methods 0.000 description 1
- 229930195733 hydrocarbon Natural products 0.000 description 1
- 150000002430 hydrocarbons Chemical class 0.000 description 1
- 238000005984 hydrogenation reaction Methods 0.000 description 1
- 229910010272 inorganic material Inorganic materials 0.000 description 1
- 239000011147 inorganic material Substances 0.000 description 1
- 238000011835 investigation Methods 0.000 description 1
- 150000002576 ketones Chemical class 0.000 description 1
- 238000000593 microemulsion method Methods 0.000 description 1
- 239000002808 molecular sieve Substances 0.000 description 1
- 239000007800 oxidant agent Substances 0.000 description 1
- 238000001556 precipitation Methods 0.000 description 1
- 238000005245 sintering Methods 0.000 description 1
- URGAHOPLAPQHLN-UHFFFAOYSA-N sodium aluminosilicate Chemical compound [Na+].[Al+3].[O-][Si]([O-])=O.[O-][Si]([O-])=O URGAHOPLAPQHLN-UHFFFAOYSA-N 0.000 description 1
- 239000007787 solid Substances 0.000 description 1
- 238000010532 solid phase synthesis reaction Methods 0.000 description 1
- 239000000126 substance Substances 0.000 description 1
- 238000000352 supercritical drying Methods 0.000 description 1
- HPGGPRDJHPYFRM-UHFFFAOYSA-J tin(iv) chloride Chemical compound Cl[Sn](Cl)(Cl)Cl HPGGPRDJHPYFRM-UHFFFAOYSA-J 0.000 description 1
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Abstract
This invention discloses a method to prepare a nano particle of tin oxide. In this method, the salt of tin, citric acid and poly (ethylene glycol) are used as raw materials. After dissolving in DIW, the solution is heated by microwave to form the precursor of gel, which is then baked in muffle furnace to prepare nano particle of tin oxide with good distribution and low aggregation. The average size of the particle is about 17.0 nanometers. The method has the characteristics of simple process, short cycle time of production.
Description
Technical field
The invention belongs to field of nanometer material technology, the present invention is specifically related to a kind of preparation method of Nano granules of stannic oxide, and this material can be used to prepare gas sensor, electro-conductive material, catalyzer, support of the catalyst etc.
Background technology
Nano tin dioxide is a kind of important inorganic functional material.Stannic oxide has characteristics such as fusing point height, high temperature are difficult for down decomposing, chemical property is stable, difficult and strong acid and strong base reaction, and response speed is fast, is widely used in gas sensitive.As the n N-type semiconductorN, stannic oxide has good photoelectronic property, can be used for electro-conductive material.Stannic oxide also is a kind of good catalyzer and support of the catalyst, not only has stronger complete oxidation ability, selective oxidation activity preferably and hydrothermal stability are also arranged, can be used for the selection hydrogenation of hydrocarbon oxidation, dehydrocyclization, unsaturated aldehyde, ketone or carboxylic acid, the reduction of NOx etc., all widespread uses in this external organic catalysis, photochemical catalysis and the electrocatalysis.
The performance of stannic oxide and specific surface have very strong dependency, obtain the excellent properties stannic oxide materials, must preparation superfine tin oxide powder.Reported method has sol-gel method (Shek C.H.Nanostruct.Mater.1999 at present, 11:887-893), chemical precipitation method (Li Laifeng etc. the investigation of materials journal, 2000,14 (1): 37-41), hydrothermal synthesis method (Wang Chengyuan Nanostruct.Mater.1996,7:421-427), alkoxide hydrolysis (Sophie de Monredon, J.Mater.Chem.2002,12:2396-2400), combustion method of citric acid (Fraigi L.B.Mater.Lett.2001,47:262-266), microemulsion method (Pan Qingyi etc., Journal of Inorganic Materials, 1999,14:83-88), the gas condensation method (Suh S.Thin Solid Films 1999,345:240-249) etc.Relevant at present Chinese patent has 94117467.0 to adopt precipitation from homogeneous solution-supercritical drying drying method preparation to be used for the stannic oxide of low temperature gas sensor; Patent 97114210.6 adopts collosol and gel and hydrolysis method to prepare SnO
2Be used for the normal temperature gas sensor; Patent 200310108633.6 adopts Prepared by Sol Gel Method to be used for the stannic oxide powder of gas sensor; Patent 200310107905.0 adopts hydrothermal method and patent 03118150.3 to adopt solid-phase method for preparing nano-sized SnO
2Deng.
Traditional citric acid sol method prepares nano SnO
2, needing water-bath or the slow evaporating water of other thermals source, gelation time is long.And combustion method of citric acid needs the nitrate of metal to make strong oxidizer, and the nitrate process of preparation tin is more loaded down with trivial details, expends time in.Carry out microwave radiation heating has fast, uniform characteristics, than traditional heating mode special advantages is arranged.Aspect material preparation, utilize carry out microwave radiation heating, can accelerate the synthetic and sintering of stupalith, the catalytic performance etc. that improves the crystallization of molecular sieve and improve catalyzer.The present invention combines the advantage of Citrate trianion method and microwave heating and prepares the tin oxide nano particle.
Summary of the invention
The invention provides the tin oxide nano particulate preparation method that a kind of technology is simple, with low cost, grain-size is little.
It is raw material that the present invention adopts metal pink salt, citric acid, polyoxyethylene glycol, and it mixed dissolution in deionized water, is then made Gel Precursor by microwave heating, this presoma is carried out roasting can obtain granules of stannic oxide.The concentration of the tin-salt solution of configuration is at 0.1～4.0mol L
-1, the mol ratio of pink salt and citric acid is between 1: 2～1: 4, and the amount of the polyoxyethylene glycol of adding is 0.1～0.3g, and solution preparation temperature is normal temperature or heating.Use microwave heating to form gel, the time of microwave heating, microwave heating power was 200～700W at 5～15min.The time of Gel Precursor roasting is 2～6h, and maturing temperature is 450～600 ℃.
The present invention adopts tin tetrachloride, citric acid, poly(oxyethylene glycol) 400 or 600 to be raw material, and it mixed dissolution in deionized water, is then made Gel Precursor with crossing microwave heating, and then the roasting Gel Precursor promptly obtains nano particle in retort furnace.
Processing condition: SnCl
4Volumetric molar concentration be 0.1～4.0mol L
-1The mol ratio of pink salt and citric acid is between 1: 2～1: 4, the amount of the polyoxyethylene glycol that adds is 0.1～0.3g, solution preparation temperature is normal temperature or heating, the time of microwave heating is at 5～15min, microwave heating power is 200～700W, and the time of Gel Precursor roasting is 2～6h, and maturing temperature is 450～600 ℃.
Nanoparticle features: grain diameter is little, crystal grain is about 17.0nm, size distribution is more even, adopt the mode of microwave heating, gelation time is shortened to about 10min by 1 original～3d, and the collagen amount is good, the time and the energy have been saved, improve efficient, simplified operation, expanded application and the nanometer particle process method of microwave aspect material preparation
Description of drawings
Fig. 1: the XRD figure of the sample of different maturing temperatures;
Fig. 2: the TEM figure of 450 ℃ of roasting samples;
Fig. 3: the TEM figure of 500 ℃ of roasting samples;
Fig. 4: the TEM figure of 600 ℃ of roasting samples;
Embodiment
Example:
1, gets SnCl
45H
2The about 7.0188g of O, citric acid 8.4065g, polyoxyethylene glycol (400) 0.3g add in the 10ml deionized water and mix, and stir, and put into microwave oven then and adopt behind the medium heats 9min under 600 ℃ at retort furnace roasting 3h.According to the result of XRD, trying to achieve the nano particle grain size by the Scherrer equation is 17.4nm.
2, get SnCl
45H
2The about 7.0188g of O, citric acid 8.4056g, polyoxyethylene glycol (400) 0.3g add in the 10ml deionized water and mix, and stir, and put into microwave oven then and adopt behind the medium heats 13min under 500 ℃ at retort furnace roasting 4h.According to the result of XRD, trying to achieve the nano particle grain size by the Scherrer equation is 18.3nm
3, get SnCl
45H
2The about 7.0188g of O, citric acid 16.8112g, polyoxyethylene glycol (600) 0.3g add in the 15ml deionized water and mix, and stir, and put into microwave oven then and adopt behind the medium heats 11min under 500 ℃ at retort furnace roasting 4h.According to the result of XRD, trying to achieve the nano particle grain size by the Scherrer equation is 16.8nm.
4, get SnCl
45H
2The about 7.0188g of O, citric acid 12.6084g, polyoxyethylene glycol (600) 0.3g add in the 12ml deionized water and mix, and stir, and put into microwave oven then and adopt behind the medium heats 9min under 600 ℃ at retort furnace roasting 2h.According to the result of XRD, trying to achieve the nano particle grain size by the Scherrer equation is 18.1nm.
5, get SnCl
45H
2The about 7.0188g of O, citric acid 8.4065g, polyoxyethylene glycol (400) 0.3g add in the 10ml deionized water and mix, and stir, and put into microwave oven then and adopt behind the medium heats 9min under 450 ℃ at retort furnace roasting 4h.According to the result of XRD, trying to achieve the nano particle grain size by the Scherrer equation is 14.1nm.
6, get SnCl
45H
2The about 7.0188g of O, citric acid 8.4065g, polyoxyethylene glycol (400) 0.3g add in the 10ml deionized water and mix, and stir, and put into microwave oven then and adopt behind the medium heats 7min under 500 ℃ at retort furnace roasting 4h.According to the result of XRD, trying to achieve the nano particle grain size by the Scherrer equation is 14.5nm.
7, get SnCl
45H
2The about 3.5094g of O, citric acid 4.2033g, polyoxyethylene glycol (400) 0.1g add in the 10ml deionized water and mix, and stir, and put into microwave oven then and adopt behind the medium heats 9min under 500 ℃ at retort furnace roasting 4h.According to the result of XRD, trying to achieve the nano particle grain size by the Scherrer equation is 14.7nm.
8, get SnCl
45H
2The about 7.0188g of O, citric acid 8.4065g, polyoxyethylene glycol (400) 0.25g add in the 10ml deionized water and mix, and stir, and put into microwave oven then and adopt behind the medium heats 9min under 500 ℃ at retort furnace roasting 6h.According to the result of XRD, trying to achieve the nano particle grain size by the Scherrer equation is 17.2nm.
Claims (4)
1, a kind of preparation method of Nano granules of stannic oxide, it is characterized in that: adopting metal pink salt, citric acid, polyoxyethylene glycol is raw material, it mixed dissolution in deionized water, is then made Gel Precursor by microwave heating, this presoma is carried out roasting can obtain granules of stannic oxide.
2, by the preparation method of the described a kind of Nano granules of stannic oxide of claim 1, it is characterized in that: the concentration of the tin-salt solution of configuration is at 0.1～4.0mol L
-1, the mol ratio of pink salt and citric acid is between 1: 2～1: 4, and the amount of the polyoxyethylene glycol of adding is 0.1～0.3g, and solution preparation temperature is normal temperature or heating.
3, by the preparation method of claim 1 or 2 described a kind of Nano granules of stannic oxide, it is characterized in that: use microwave heating to form gel, the time of microwave heating, microwave heating power was 200～700W at 5～15min.
4, by the preparation method of claim 1 or 2 described a kind of Nano granules of stannic oxide, it is characterized in that: the time of Gel Precursor roasting is 2～6h, and maturing temperature is 450～600 ℃.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CNB2004100777806A CN100482591C (en) | 2004-12-30 | 2004-12-30 | Method for preparing Nano granules of stannic oxide |
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| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CNB2004100777806A CN100482591C (en) | 2004-12-30 | 2004-12-30 | Method for preparing Nano granules of stannic oxide |
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| Publication Number | Publication Date |
|---|---|
| CN1796287A true CN1796287A (en) | 2006-07-05 |
| CN100482591C CN100482591C (en) | 2009-04-29 |
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Cited By (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN102923765A (en) * | 2012-10-08 | 2013-02-13 | 中山大学 | Indium tin oxide (ITO) nano powder and preparation method thereof |
| CN104211107A (en) * | 2014-08-26 | 2014-12-17 | 洛阳市方德新材料科技有限公司 | Preparation method for nano tin oxide powder |
| CN107293411A (en) * | 2017-06-08 | 2017-10-24 | 东南大学 | A kind of quick method for preparing tin ash two dimension carbonization titanium composite material |
Family Cites Families (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| DE19828692A1 (en) * | 1997-06-27 | 1999-01-07 | Ami Doduco Gmbh | Tin oxide powder granulation by microwave heat treatment |
| CN1251969C (en) * | 2003-11-14 | 2006-04-19 | 中国科学院上海硅酸盐研究所 | Stannic oxide powder preparation method |
-
2004
- 2004-12-30 CN CNB2004100777806A patent/CN100482591C/en not_active Expired - Fee Related
Cited By (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN102923765A (en) * | 2012-10-08 | 2013-02-13 | 中山大学 | Indium tin oxide (ITO) nano powder and preparation method thereof |
| CN104211107A (en) * | 2014-08-26 | 2014-12-17 | 洛阳市方德新材料科技有限公司 | Preparation method for nano tin oxide powder |
| CN107293411A (en) * | 2017-06-08 | 2017-10-24 | 东南大学 | A kind of quick method for preparing tin ash two dimension carbonization titanium composite material |
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| Publication number | Publication date |
|---|---|
| CN100482591C (en) | 2009-04-29 |
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