CN100345764C - Two-step method for preparing stannic oxide nano material - Google Patents
Two-step method for preparing stannic oxide nano material Download PDFInfo
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- CN100345764C CN100345764C CNB2005100604549A CN200510060454A CN100345764C CN 100345764 C CN100345764 C CN 100345764C CN B2005100604549 A CNB2005100604549 A CN B2005100604549A CN 200510060454 A CN200510060454 A CN 200510060454A CN 100345764 C CN100345764 C CN 100345764C
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- powder
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- mixed powder
- sno
- naoh
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- XOLBLPGZBRYERU-UHFFFAOYSA-N tin dioxide Chemical compound O=[Sn]=O XOLBLPGZBRYERU-UHFFFAOYSA-N 0.000 title claims abstract description 17
- 238000000034 method Methods 0.000 title claims abstract description 14
- 239000002086 nanomaterial Substances 0.000 title claims description 9
- HEMHJVSKTPXQMS-UHFFFAOYSA-M Sodium hydroxide Chemical compound [OH-].[Na+] HEMHJVSKTPXQMS-UHFFFAOYSA-M 0.000 claims abstract description 33
- 239000000843 powder Substances 0.000 claims abstract description 23
- XEEYBQQBJWHFJM-UHFFFAOYSA-N Iron Chemical compound [Fe] XEEYBQQBJWHFJM-UHFFFAOYSA-N 0.000 claims abstract description 14
- 238000000498 ball milling Methods 0.000 claims abstract description 14
- 239000011812 mixed powder Substances 0.000 claims abstract description 10
- 229910052742 iron Inorganic materials 0.000 claims abstract description 7
- 239000008367 deionised water Substances 0.000 claims abstract description 6
- 229910021641 deionized water Inorganic materials 0.000 claims abstract description 6
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Chemical compound O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims abstract description 6
- 238000002425 crystallisation Methods 0.000 claims abstract description 4
- 230000008025 crystallization Effects 0.000 claims abstract description 4
- 239000002245 particle Substances 0.000 claims abstract description 4
- 238000005245 sintering Methods 0.000 claims description 8
- 238000002360 preparation method Methods 0.000 claims description 7
- 229910006404 SnO 2 Inorganic materials 0.000 claims description 6
- 239000000203 mixture Substances 0.000 claims description 4
- 229910021627 Tin(IV) chloride Inorganic materials 0.000 claims description 3
- HPGGPRDJHPYFRM-UHFFFAOYSA-J tin(iv) chloride Chemical compound Cl[Sn](Cl)(Cl)Cl HPGGPRDJHPYFRM-UHFFFAOYSA-J 0.000 claims description 3
- FFBHFFJDDLITSX-UHFFFAOYSA-N benzyl N-[2-hydroxy-4-(3-oxomorpholin-4-yl)phenyl]carbamate Chemical compound OC1=C(NC(=O)OCC2=CC=CC=C2)C=CC(=C1)N1CCOCC1=O FFBHFFJDDLITSX-UHFFFAOYSA-N 0.000 claims 1
- 239000000463 material Substances 0.000 abstract description 9
- 239000007787 solid Substances 0.000 abstract description 4
- 229910001887 tin oxide Inorganic materials 0.000 abstract 1
- KHMOASUYFVRATF-UHFFFAOYSA-J tin(4+);tetrachloride;pentahydrate Chemical compound O.O.O.O.O.Cl[Sn](Cl)(Cl)Cl KHMOASUYFVRATF-UHFFFAOYSA-J 0.000 abstract 1
- 238000002173 high-resolution transmission electron microscopy Methods 0.000 description 9
- 238000002441 X-ray diffraction Methods 0.000 description 8
- 238000005406 washing Methods 0.000 description 4
- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical compound [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 description 3
- RYGMFSIKBFXOCR-UHFFFAOYSA-N Copper Chemical compound [Cu] RYGMFSIKBFXOCR-UHFFFAOYSA-N 0.000 description 3
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 description 3
- 238000013019 agitation Methods 0.000 description 3
- 238000000191 alpha-particle scattering Methods 0.000 description 3
- 229910052799 carbon Inorganic materials 0.000 description 3
- 239000010949 copper Substances 0.000 description 3
- 229910052802 copper Inorganic materials 0.000 description 3
- 229960000935 dehydrated alcohol Drugs 0.000 description 3
- 238000001035 drying Methods 0.000 description 3
- 230000000694 effects Effects 0.000 description 3
- 238000005516 engineering process Methods 0.000 description 3
- 229910021421 monocrystalline silicon Inorganic materials 0.000 description 3
- 238000003756 stirring Methods 0.000 description 3
- 239000000126 substance Substances 0.000 description 3
- 239000013078 crystal Substances 0.000 description 2
- 150000004703 alkoxides Chemical class 0.000 description 1
- 230000009286 beneficial effect Effects 0.000 description 1
- 238000000975 co-precipitation Methods 0.000 description 1
- 238000005354 coacervation Methods 0.000 description 1
- 230000007547 defect Effects 0.000 description 1
- 238000005137 deposition process Methods 0.000 description 1
- 239000003814 drug Substances 0.000 description 1
- 238000001027 hydrothermal synthesis Methods 0.000 description 1
- 239000011858 nanopowder Substances 0.000 description 1
- 230000003287 optical effect Effects 0.000 description 1
- 239000002243 precursor Substances 0.000 description 1
- 239000004065 semiconductor Substances 0.000 description 1
- 230000035945 sensitivity Effects 0.000 description 1
- 230000005476 size effect Effects 0.000 description 1
- 238000003980 solgel method Methods 0.000 description 1
- 239000007858 starting material Substances 0.000 description 1
- 238000007738 vacuum evaporation Methods 0.000 description 1
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- Compositions Of Oxide Ceramics (AREA)
- Compounds Of Iron (AREA)
Abstract
The present invention discloses a two-step method for preparing the nanometer material of tin oxide. SnCl4.5H2O and NaOH are mixed according to a molar ratio of 1: 4, and then put in a ball milling pot for ball milling for 1 to 3 hours, and the number ratio of iron balls with the diameter of 13mm to iron balls with the diameter of 6.5mm is 1: 2; powder obtained after ball milling is sintered at the temperature of 873K to 1073K so as to obtain nanometer SnO2 mixed powder with the particle size of 3 to 14 nm, and the nanometer SnO2 mixed powder is repeatedly washed and centrifuged by deionized water; finally, the mixed powder is dried into solid powder at the temperature of 75 to 100 DEG C so as to obtain pure nanometer SnO2 powder with perfect crystallization. The two-step method has the advantages of simple adopted equipment, compact flow, easily controlled operation and superfine level product, and is a method worth of popularizing.
Description
Technical field
The present invention relates to technical field of material, relate in particular to the method that a kind of two-step approach prepares stannic oxide nano material.
Background technology
The preparation of nano material and superfine powdery material is one of Materials science research focus in recent years.Nano material generally is meant by fines to be formed, the class material of characteristic dimension size in 1～100nm scope.Because its inner superfine crystal grain and be in crystal boundary in a large number and the existence of the atom of intragranular defect center, make nano material have the effect that common material does not have, as quantum size effect, surface effects and macro quanta tunnel effect, thereby nano material shows the greatest differences with other material on physical and chemical performance, make it obtain using widely, its range of application has now related to a plurality of fields such as national defence, electronics, chemical industry, medicine and Surface Engineering.And SnO
2As a kind of semiconductor functional material of early using, have a wide range of applications at air-sensitive, the aspects such as quick, pressure-sensitive and optical technology that wet.And nano level SnO
2Higher sensitivity, selectivity and stability are arranged in these areas, have more wide application market prospect.At present, research nano SnO
2The preparation method of powder has a lot, for example: sol-gel processing, hydrothermal method, alkoxide process, chemical coprecipitation, solvent-thermal method, vacuum-evaporation coacervation and vapour deposition process etc., every kind of preparation method has characteristics, but under present equipment level and the also immature condition of nano-powder material application market, most methods does not also form the industrial scale that has on the practical significance, and the study sample stage that provides all is provided mostly.
Summary of the invention
The purpose of this invention is to provide the method that technology is simple, cost is low, easy to operate a kind of two-step approach prepares stannic oxide nano material,
The technological step that the present invention adopts is as follows:
One, material mixture ratio
Stannic chloride pentahydrate, SnCl
45H
2O, analytical pure
Sodium hydroxide, NaOH, analytical pure
Two, preparation process
1) with SnCl
45H
2O and NaOH 1: 4 in molar ratio mix to be placed on and carry out ball milling 1～3h in the ball grinder, and diameter is 13mm and the number ratio of the iron ball of 6.5mm is 1: 2;
2) with 1) in the powder that obtains behind the ball milling under 873K～1073K temperature range, carry out sintering, obtain the nano SnO of particle size range at 3～14nm
2Mixed powder;
3) with nano SnO
2Mixed powder is used deionized water wash, centrifugal repeatedly, becomes pressed powder at 75～100 ℃ of down dry 6～8h at last, obtains the pure nano SnO of complete crystallization
2Powder.
The beneficial effect that the present invention has is: use stannic chloride pentahydrate and sodium hydroxide as starting material, carry out ball milling earlier, obtain precursor, carry out sintering again, obtain the nano SnO of different particle sizes by the control sintering temperature
2Powder carries out washing, centrifugal repeatedly, and is dry again, finally obtain complete crystallization, purity better, narrow diameter distribution, the dispersed nano SnO of different scale preferably
2Powder.The equipment that this two-step approach adopts is simple, and flow process is succinct, and is easy to control, and product can reach ultra-fine level, is a kind of method that is worthy to be popularized.
Description of drawings
Fig. 1 is the SnO according to the embodiment preparation
2The XRD diffractogram of nanometer powder;
Fig. 2 is the SnO according to the embodiment preparation
2The HRTEM photo of nanometer powder.
Embodiment
Embodiment 1
With the mole proportioning 1: 4 SnCl
45H
2O and NaOH put into the ball grinder ball milling 1h of Spex8000 type ball mill, and diameter is 13mm and the number ratio of the iron ball of 6.5mm is 1: 2.Powder behind the ball milling is put into the SRJX high temperature box furnace carry out sintering, under 873K, be incubated 2h, obtain SnO by the heat-up rate of 5 ℃/min
2Mixed powder, under 78HW-3 type constant temperature magnetic agitation instrument, stir then and use deionized water wash, pass through the centrifugal 10min of 10000r/min whizzer (SORVALL LEGEND-T) again, washing once more, the solid 75 ℃ of down dry 8h in loft drier that obtain after 4～5 times become 3nmSnO so repeatedly
2Powder.The sample of X-ray diffraction analysis (XRD) does not have for the exsiccant powder places on the back of the body monocrystalline silicon piece at the end, the laboratory apparatus of employing be Rigaku D Max-2200, adopt Cu K alpha scattering, sweep interval is 20-80 °, step-length is 0.02 °, per sweep time in step 4s.The specimen that high resolution transmission electron microscopy (HRTEM, model is JEM-2010) is observed is dried sample ultrasonic to be handled be dispersed in the dehydrated alcohol, the drips of solution after will disperseing then on the copper mesh that is coated with carbon film, drying at room temperature.
Embodiment 2
With the mole proportioning 1: 4 SnCl
45H
2O and NaOH put into the ball grinder ball milling 2h of Spex8000 type ball mill, and diameter is 13mm and the number ratio of the iron ball of 6.5mm is 1: 2.Resultant behind the ball milling is put into the SRJX high temperature box furnace carry out sintering, under 973K, be incubated 2h, obtain SnO by the heat-up rate of 5 ℃/min
2Mixed powder, under 78HW-3 type constant temperature magnetic agitation instrument, stir then and use deionized water wash, pass through the centrifugal 10min of 10000r/min whizzer (SORVALL LEGEND-T) again, washing once more, the solid 85 ℃ of down dry 6h in loft drier that obtain after 4～5 times become 8nmSnO so repeatedly
2Powder.The sample of X-ray diffraction analysis (XRD) does not have for the exsiccant powder places on the back of the body monocrystalline silicon piece at the end, the laboratory apparatus of employing be Rigaku D Max-2200, adopt Cu K alpha scattering, sweep interval is 20-80 °, step-length is 0.02 °, per sweep time in step 4s.The specimen that high resolution transmission electron microscopy (HRTEM, model is JEM-2010) is observed is dried sample ultrasonic to be handled be dispersed in the dehydrated alcohol, the drips of solution after will disperseing then on the copper mesh that is coated with carbon film, drying at room temperature.
Embodiment 3
With the mole proportioning 1: 4 SnCl
45H
2O and NaOH put into the ball grinder ball milling 3h of Spex8000 type ball mill, and diameter is 13mm and the number ratio of the iron ball of 6.5mm is 1: 2.Resultant behind the ball milling is put into the SRJX high temperature box furnace carry out sintering, under 1073K, be incubated 2h, obtain SnO by the heat-up rate of 5 ℃/min
2Mixed powder, under 78HW-3 type constant temperature magnetic agitation instrument, stir then and use deionized water wash, pass through the centrifugal 10min of 10000r/min whizzer (SORVALL LEGEND-T) again, washing once more, the solid 100 ℃ of down dry 6h in loft drier that obtain after 4～5 times become 14nmSnO so repeatedly
2Powder.The sample of X-ray diffraction analysis (XRD) does not have for the exsiccant powder places on the back of the body monocrystalline silicon piece at the end, the laboratory apparatus of employing be Rigaku D Max-2200, adopt Cu K alpha scattering, sweep interval is 20-80 °, step-length is 0.02 °, per sweep time in step 4s.The specimen that high resolution transmission electron microscopy (HRTEM, model is JEM-2010) is observed is dried sample ultrasonic to be handled be dispersed in the dehydrated alcohol, the drips of solution after will disperseing then on the copper mesh that is coated with carbon film, drying at room temperature.
Fig. 1 is the SnO for preparing according to embodiment 1,2,3 modes
2The XRD diffractogram of nanometer powder.
Fig. 2 is the SnO for preparing according to 1,2,3 modes of enforcement
2The HRTEM photo of nanometer powder.(a) and (b), (c) obtain when being respectively 873K, 973K and 1073K temperature sintering nano SnO
2The HRTEM photo.
Claims (1)
1, a kind of two-step approach prepares the method for stannic oxide nano material, it is characterized in that the step of this method is as follows:
One, material mixture ratio
Stannic chloride pentahydrate, SnCl
45H
2O, analytical pure;
Sodium hydroxide, NaOH, analytical pure;
Two, preparation process
1) with SnCl
45H
2O and NaOH 1: 4 in molar ratio mix to be placed on and carry out ball milling 1～3h in the ball grinder, and diameter is 13mm and the number ratio of the iron ball of 6.5mm is 1: 2;
2) with 1) in the powder that obtains behind the ball milling under 873K～1073K temperature range, carry out sintering, obtain the nano SnO of particle size range at 3～14nm
2Mixed powder;
3) with nano SnO
2Mixed powder is used deionized water wash, centrifugal repeatedly, becomes pressed powder at 75～100 ℃ of down dry 6～8h at last, obtains the pure nano SnO of complete crystallization
2Powder.
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| Application Number | Priority Date | Filing Date | Title |
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| CNB2005100604549A CN100345764C (en) | 2005-08-23 | 2005-08-23 | Two-step method for preparing stannic oxide nano material |
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| CNB2005100604549A CN100345764C (en) | 2005-08-23 | 2005-08-23 | Two-step method for preparing stannic oxide nano material |
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| CN1762827A CN1762827A (en) | 2006-04-26 |
| CN100345764C true CN100345764C (en) | 2007-10-31 |
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Families Citing this family (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN102030362B (en) * | 2010-10-08 | 2012-08-29 | 四川大学 | Method for preparing SnO2 nanomaterial by hydride deposition |
| CN104132987B (en) * | 2014-05-30 | 2016-11-16 | 中国石油化工股份有限公司青岛安全工程研究院 | Preparation method for the gas sensor of hydrocarbon gas detection |
| CN105600818B (en) * | 2016-01-12 | 2017-06-23 | 济南大学 | The method and products obtained therefrom of a kind of stannic oxide nanometer powder prepared rich in Lacking oxygen |
| CN108726559A (en) * | 2018-06-20 | 2018-11-02 | 新疆大学 | A kind of method that solid phase prepares stannic oxide-ZnO heterojunction nano flower |
| CN108928848A (en) * | 2018-06-20 | 2018-12-04 | 新疆大学 | A kind of solid phase prepares stannic oxide-tourmaline hetero-junctions porous material method |
Citations (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| JPH02248489A (en) * | 1989-03-22 | 1990-10-04 | Japan Exlan Co Ltd | Manufacture of conductive white powder |
| US6503475B1 (en) * | 1998-05-15 | 2003-01-07 | Advanced Nano Technologies Pty Ltd. | Process for the production of ultrafine powders of metal oxides |
| CN1446862A (en) * | 2003-01-13 | 2003-10-08 | 华东理工大学 | Aquosity pulp of tin dioxide with nano stibonium being adulterated to |
| CN1454709A (en) * | 2003-03-06 | 2003-11-12 | 天津大学 | Method of preparing SnO2 cladded Tio2 nano particle photocatalyst |
| CN1530325A (en) * | 2003-03-10 | 2004-09-22 | 中南大学 | Method for preparing stannic anhydride nanometer crystal with solid phase reaction |
-
2005
- 2005-08-23 CN CNB2005100604549A patent/CN100345764C/en not_active Expired - Fee Related
Patent Citations (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| JPH02248489A (en) * | 1989-03-22 | 1990-10-04 | Japan Exlan Co Ltd | Manufacture of conductive white powder |
| US6503475B1 (en) * | 1998-05-15 | 2003-01-07 | Advanced Nano Technologies Pty Ltd. | Process for the production of ultrafine powders of metal oxides |
| CN1446862A (en) * | 2003-01-13 | 2003-10-08 | 华东理工大学 | Aquosity pulp of tin dioxide with nano stibonium being adulterated to |
| CN1454709A (en) * | 2003-03-06 | 2003-11-12 | 天津大学 | Method of preparing SnO2 cladded Tio2 nano particle photocatalyst |
| CN1530325A (en) * | 2003-03-10 | 2004-09-22 | 中南大学 | Method for preparing stannic anhydride nanometer crystal with solid phase reaction |
Non-Patent Citations (1)
| Title |
|---|
| Gas sensing properties of nanosized tin oxide synthesised bymechanochemical processing L.M. Cukrov et al,Sensors and Actuators,Vol.77 2001 * |
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| CN1762827A (en) | 2006-04-26 |
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