CN105036180A - Preparation method of tin oxide/zinc oxide nanometer flower-shaped composite material - Google Patents
Preparation method of tin oxide/zinc oxide nanometer flower-shaped composite material Download PDFInfo
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- CN105036180A CN105036180A CN201510360841.8A CN201510360841A CN105036180A CN 105036180 A CN105036180 A CN 105036180A CN 201510360841 A CN201510360841 A CN 201510360841A CN 105036180 A CN105036180 A CN 105036180A
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Abstract
The invention discloses a preparation method of a tin oxide/zinc oxide nanometer flower-shaped composite material. The preparation method comprises the steps of firstly, adopting a one-step hydrothermal method, and obtaining a nanometer tin oxide substrate material under an alkaline condition; then, mixing zinc oxide seed crystal liquid and nanometer tin oxide, and enabling a seed crystal to be loaded on the tin oxide substrate material; finally, enabling nanometer zinc oxide to grow on the seed crystal by adopting a hydrothermal method, and then obtaining the tin oxide/zinc oxide nanometer flower-shaped composite material. According to the preparation method disclosed by the invention, a seed crystal growth method and the hydrothermal method are combined, the prepared tin oxide/zinc oxide nanometer material is flower-shaped, and the tin oxide/zinc oxide nanometer flower-shaped composite material can be widely applied to the field of gas sensing, photocatalysis, batteries and the like.
Description
Technical field
The invention belongs to nano composite material technical field, be specifically related to the preparation method of the flower-shaped matrix material of a kind of stannic oxide/zinc-oxide nano.
Background technology
The excellent performance of metal oxide semiconductor nano material, is widely used in the fields such as sensing, catalysis, photoelectricity.Wherein, n-type semiconductor stannic oxide SnO
2with zinc oxide ZnO, there is wider energy gap, higher vapor sensitivity and good optical property, enjoy the concern of scientists.Therefore, study hotspot has just dropped on stannic oxide/zinc oxide composite by people, wishes the excellent properties being given full play to bi-material by recombination energy, and demonstrates the character more more superior than single-material in some aspects.
At present, major part stannic oxide/zinc oxide composite is all prepared by coprecipitation method, method of electrostatic spinning, ball milled, pyrolytic coating method etc., be only and mixed simply by two kinds of materials, the contact interface between stannic oxide and zinc oxide is also insecure.Therefore, a kind of stannic oxide/zinc oxide composite is invented and both synthetic methods of combining closely are extremely important.
Summary of the invention
For overcoming the deficiencies in the prior art, the invention provides the preparation method of the flower-shaped matrix material of a kind of stannic oxide/zinc-oxide nano, seeded growth method is adopted to combine with hydrothermal method, developing zinc oxide on tin oxide base bottom material, thus obtain the stannic oxide/zinc oxide nanometer composite material with floriform appearance.
A preparation method for the flower-shaped matrix material of stannic oxide/zinc-oxide nano, is characterized in that, the concrete steps of the method are:
(1) nano tin dioxide SnO
2the preparation of base material: by two hydration tindichloride SnCl
22H
2the O aqueous solution and sodium hydroxide NaOH aqueous solution, make three mol ratio SnCl
22H
2o:NaOH:H
2o=1:3-5:1250-1750, stirs and is evenly clarified precursor liquid; Reaction soln is transferred in tetrafluoroethylene water heating kettle, in 160 DEG C of hydro-thermal reaction 12-18 hour in an oven; By the precipitate with deionized water that obtains after centrifugal and absolute ethanol washing repeatedly, dry, obtain nano tin dioxide SnO with after agate mortar porphyrize
2base material;
(2) load of zinc oxide crystal seed: compound concentration is the two acetate hydrate zinc Zn (CH of 0.005-0.02mol/L
3cOO)
22H
2the ethanolic soln of O or zinc nitrate hexahydrate Zn (NO
3)
26H
2the ethanolic soln of O is as zinc oxide crystal seed liquid; Crystal seed drop is added nano SnO
2base material also fully grinds, and makes it mix rear drying, and repeatedly, mol ratio Zn (CH
3cOO)
22H
2o:SnO
2or Zn (NO
3)
26H
2o:SnO
2=1:20-50, makes zinc oxide crystal seed be carried on tin oxide base bottom material;
(3) preparation of stannic oxide/zinc oxide nanometer composite material: by zinc nitrate hexahydrate Zn (NO
3)
26H
2the O aqueous solution mixes with hexamethylenetetramine HMT, makes three mol ratio Zn (NO
3)
26H
2o:HMT:H
2o=1:1:1500-2500, stirs and is evenly clarified precursor liquid; By load, the tin oxide base bottom material of zinc oxide crystal seed is placed in tetrafluoroethylene water heating kettle, adds above-mentioned precursor liquid and stirs, in 95-105 DEG C of hydro-thermal reaction 3-6 hour in an oven; By the precipitate with deionized water that obtains after centrifugal and absolute ethanol washing repeatedly, the flower-shaped matrix material of stannic oxide/zinc-oxide nano is drying to obtain.
Zinc oxide crystal seed liquid is two acetate hydrate zinc Zn (CH
3cOO)
22H
2o or zinc nitrate hexahydrate Zn (NO
3)
26H
2the ethanolic soln of O.
Hexamethylenetetramine HMT is adopted to carry out the basicity of regulator solution.
Adopt seeded growth method to combine with hydrothermal method, developing zinc oxide on tin oxide base bottom material, thus obtain the stannic oxide/zinc oxide nanometer composite material with floriform appearance.
Seeded growth method combines with hydrothermal method by the present invention, and prepared stannic oxide/nano zinc oxide material has floriform appearance, and this matrix material can be widely used in the fields such as gas sensing, photochemical catalysis, battery.
Accompanying drawing explanation
Fig. 1 is the scanning electron microscope (SEM) photograph of the flower-shaped matrix material of stannic oxide/zinc-oxide nano that the embodiment of the present invention 1 is synthesized.
Fig. 2 is the scanning electron microscope (SEM) photograph of the flower-shaped matrix material of stannic oxide/zinc-oxide nano of the 2-in-1 one-tenth of the embodiment of the present invention.
Fig. 3 is the transmission electron microscope picture of the flower-shaped matrix material of stannic oxide/zinc-oxide nano that the embodiment of the present invention 3 is synthesized.
Embodiment
The present invention is described in detail by specific examples below, but protection scope of the present invention is not limited to these embodiments.
embodiment 1:
(1) nano tin dioxide SnO
2the preparation of base material: by 1.785gSnCl
22H
2o is dissolved in 170g water and 45ml0.8MNaOH mixed system, and 35 DEG C of stirrings are evenly clarified precursor liquid in 0.5 hour; Reaction soln is transferred in tetrafluoroethylene water heating kettle, in 160 DEG C of hydro-thermal reactions 15 hours in an oven; By the precipitate with deionized water that obtains after centrifugal and absolute ethanol washing repeatedly, dry, obtain nano tin dioxide SnO with after agate mortar porphyrize
2base material.
(2) load of zinc oxide crystal seed: by 0.011gZn (CH
3cOO)
22H
2o is dissolved in 10ml dehydrated alcohol, and 35 DEG C of stirrings obtain zinc oxide crystal seed liquid in 0.5 hour; Get 0.025g nano SnO
2base material is placed in agate mortar, drips 0.1ml zinc oxide crystal seed liquid and fully grinding, makes it mix rear drying, and repeat ten times, make zinc oxide crystal seed be carried on tin oxide base bottom material;
(3) preparation of stannic oxide/zinc oxide nanometer composite material: by 0.263gZn (NO
3)
26H
2o and 0.124gHMT is dissolved in 35g water, stirs and is evenly clarified precursor liquid; By load, the tin oxide base bottom material of zinc oxide crystal seed is placed in tetrafluoroethylene water heating kettle, adds above-mentioned precursor liquid and stirs, in 95 DEG C of hydro-thermal reactions 3 hours in an oven; By the precipitate with deionized water that obtains after centrifugal and absolute ethanol washing repeatedly, the flower-shaped matrix material of stannic oxide/zinc-oxide nano is drying to obtain.Fig. 1 is the stereoscan photograph of this matrix material.
embodiment 2:
(1) nano tin dioxide SnO
2the preparation of base material: by 1.785gSnCl
22H
2o is dissolved in 210g water and 35ml0.8MNaOH mixed system, and 35 DEG C of stirrings are evenly clarified precursor liquid in 0.5 hour; Reaction soln is transferred in tetrafluoroethylene water heating kettle, in 160 DEG C of hydro-thermal reactions 18 hours in an oven; By the precipitate with deionized water that obtains after centrifugal and absolute ethanol washing repeatedly, dry, obtain nano tin dioxide SnO with after agate mortar porphyrize
2base material.
(2) load of zinc oxide crystal seed: by 0.06gZn (NO
3)
26H
2o be dissolved in 10ml dehydrated alcohol, 35 DEG C of stirrings obtain zinc oxide crystal seed liquid in 0.5 hour; Get 0.025g nano SnO
2base material is placed in agate mortar, drips 0.1ml zinc oxide crystal seed liquid and fully grinding, makes it mix rear drying, and repeat four times, make zinc oxide crystal seed be carried on tin oxide base bottom material;
(3) preparation of stannic oxide/zinc oxide nanometer composite material: by 0.263gZn (NO
3)
26H
2o and 0.124gHMT is dissolved in 30g water, stirs and is evenly clarified precursor liquid; By load, the tin oxide base bottom material of zinc oxide crystal seed is placed in tetrafluoroethylene water heating kettle, adds above-mentioned precursor liquid and stirs, in 100 DEG C of hydro-thermal reactions 6 hours in an oven; By the precipitate with deionized water that obtains after centrifugal and absolute ethanol washing repeatedly, the flower-shaped matrix material of stannic oxide/zinc-oxide nano is drying to obtain.Fig. 2 is the stereoscan photograph of this matrix material.
embodiment 3:
(1) nano tin dioxide SnO
2the preparation of base material: by 1.785gSnCl
22H
2o is dissolved in 147g water and 40ml0.8MNaOH mixed system, and 35 DEG C of stirrings are evenly clarified precursor liquid in 0.5 hour; Reaction soln is transferred in tetrafluoroethylene water heating kettle, in 160 DEG C of hydro-thermal reactions 12 hours in an oven; By the precipitate with deionized water that obtains after centrifugal and absolute ethanol washing repeatedly, dry, obtain nano tin dioxide SnO with after agate mortar porphyrize
2base material.
(2) load of zinc oxide crystal seed: by 0.022gZn (CH
3cOO)
22H
2o is dissolved in 10ml dehydrated alcohol, and 35 DEG C of stirrings obtain zinc oxide crystal seed liquid in 0.5 hour; Get 0.025g nano SnO
2base material is placed in agate mortar, drips 0.1ml zinc oxide crystal seed liquid and fully grinding, makes it mix rear drying, and repeat four times, make zinc oxide crystal seed be carried on tin oxide base bottom material;
(3) preparation of stannic oxide/zinc oxide nanometer composite material: by 0.263gZn (NO
3)
26H
2o and 0.124gHMT is dissolved in 25g water, stirs and is evenly clarified precursor liquid; By load, the tin oxide base bottom material of zinc oxide crystal seed is placed in tetrafluoroethylene water heating kettle, adds above-mentioned precursor liquid and stirs, in 105 DEG C of hydro-thermal reactions 3 hours in an oven; By the precipitate with deionized water that obtains after centrifugal and absolute ethanol washing repeatedly, the flower-shaped matrix material of stannic oxide/zinc-oxide nano is drying to obtain.Fig. 3 is the transmission electron microscope photo of this matrix material.
Claims (4)
1. a preparation method for the flower-shaped matrix material of stannic oxide/zinc-oxide nano, is characterized in that, the concrete steps of the method are:
(1) nano tin dioxide SnO
2the preparation of base material: by two hydration tindichloride SnCl
22H
2the O aqueous solution and sodium hydroxide NaOH aqueous solution, make three mol ratio SnCl
22H
2o:NaOH:H
2o=1:3-5:1250-1750, stirs and is evenly clarified precursor liquid; Reaction soln is transferred in tetrafluoroethylene water heating kettle, in 160 DEG C of hydro-thermal reaction 12-18 hour in an oven; By the precipitate with deionized water that obtains after centrifugal and absolute ethanol washing repeatedly, dry, obtain nano tin dioxide SnO with after agate mortar porphyrize
2base material;
(2) load of zinc oxide crystal seed: compound concentration is the two acetate hydrate zinc Zn (CH of 0.005-0.02mol/L
3cOO)
22H
2the ethanolic soln of O or zinc nitrate hexahydrate Zn (NO
3)
26H
2the ethanolic soln of O is as zinc oxide crystal seed liquid; Crystal seed drop is added nano SnO
2base material also fully grinds, and makes it mix rear drying, and repeatedly, mol ratio Zn (CH
3cOO)
22H
2o:SnO
2or Zn (NO
3)
26H
2o:SnO
2=1:20-50, makes zinc oxide crystal seed be carried on tin oxide base bottom material;
(3) preparation of stannic oxide/zinc oxide nanometer composite material: by zinc nitrate hexahydrate Zn (NO
3)
26H
2the O aqueous solution mixes with hexamethylenetetramine HMT, makes three mol ratio Zn (NO
3)
26H
2o:HMT:H
2o=1:1:1500-2500, stirs and is evenly clarified precursor liquid; By load, the tin oxide base bottom material of zinc oxide crystal seed is placed in tetrafluoroethylene water heating kettle, adds above-mentioned precursor liquid and stirs, in 95-105 DEG C of hydro-thermal reaction 3-6 hour in an oven; By the precipitate with deionized water that obtains after centrifugal and absolute ethanol washing repeatedly, the flower-shaped matrix material of stannic oxide/zinc-oxide nano is drying to obtain.
2. the preparation method of the flower-shaped matrix material of a kind of stannic oxide/zinc-oxide nano according to claim 1, is characterized in that, zinc oxide crystal seed liquid is two acetate hydrate zinc Zn (CH
3cOO)
22H
2o or zinc nitrate hexahydrate Zn (NO
3)
26H
2the ethanolic soln of O.
3. the preparation method of the flower-shaped matrix material of a kind of stannic oxide/zinc-oxide nano according to claim 1, is characterized in that, adopts hexamethylenetetramine HMT to carry out the basicity of regulator solution.
4. the preparation method of the flower-shaped matrix material of a kind of stannic oxide/zinc-oxide nano according to claim 1, it is characterized in that, seeded growth method is adopted to combine with hydrothermal method, developing zinc oxide on tin oxide base bottom material, thus obtain the stannic oxide/zinc oxide nanometer composite material with floriform appearance.
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Cited By (7)
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|---|---|---|---|---|
| CN105381802A (en) * | 2015-12-23 | 2016-03-09 | 哈尔滨工业大学 | Method for preparing dandelion-shaped Fe3O4@ZnO core-shell structure compound on basis of heterogeneous nucleation method and application |
| CN105529455A (en) * | 2016-01-25 | 2016-04-27 | 陕西科技大学 | Prismatic assembly ball shaped SnO2 sodium-ion battery anode material and preparation method thereof |
| CN106966605A (en) * | 2017-03-30 | 2017-07-21 | 陕西科技大学 | The zinc oxide of a kind of diamond structure/tin ash optoelectronic pole and its preparation method and application |
| CN107159218A (en) * | 2017-05-10 | 2017-09-15 | 同济大学 | The preparation method of nanometer copper sheet/Zinc oxide nano sheet composite and application |
| CN110487847A (en) * | 2019-08-26 | 2019-11-22 | 济南大学 | A kind of ZnO/Sn3O4Gas sensitive and preparation method thereof and application in the sensor |
| CN110987260A (en) * | 2018-03-20 | 2020-04-10 | 武汉铂纳智感科技有限公司 | Flexible electronic skin capable of sensing pressure and air sensitivity simultaneously and preparation method thereof |
| WO2023060742A1 (en) * | 2021-10-15 | 2023-04-20 | 光华临港工程应用技术研发(上海)有限公司 | Gas-sensitive nanomaterial having branched nanowire structure, preparation method therefor and application thereof |
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Cited By (10)
| Publication number | Priority date | Publication date | Assignee | Title |
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| CN105381802A (en) * | 2015-12-23 | 2016-03-09 | 哈尔滨工业大学 | Method for preparing dandelion-shaped Fe3O4@ZnO core-shell structure compound on basis of heterogeneous nucleation method and application |
| CN105529455A (en) * | 2016-01-25 | 2016-04-27 | 陕西科技大学 | Prismatic assembly ball shaped SnO2 sodium-ion battery anode material and preparation method thereof |
| CN105529455B (en) * | 2016-01-25 | 2018-07-17 | 陕西科技大学 | A kind of spherical SnO of prism assembling2Anode material of lithium-ion battery and preparation method thereof |
| CN106966605A (en) * | 2017-03-30 | 2017-07-21 | 陕西科技大学 | The zinc oxide of a kind of diamond structure/tin ash optoelectronic pole and its preparation method and application |
| CN106966605B (en) * | 2017-03-30 | 2019-09-24 | 陕西科技大学 | A kind of zinc oxide of diamond structure/stannic oxide optoelectronic pole and its preparation method and application |
| CN107159218A (en) * | 2017-05-10 | 2017-09-15 | 同济大学 | The preparation method of nanometer copper sheet/Zinc oxide nano sheet composite and application |
| CN110987260A (en) * | 2018-03-20 | 2020-04-10 | 武汉铂纳智感科技有限公司 | Flexible electronic skin capable of sensing pressure and air sensitivity simultaneously and preparation method thereof |
| CN110987260B (en) * | 2018-03-20 | 2021-04-30 | 武汉铂纳智感科技有限公司 | Flexible electronic skin capable of sensing pressure and air sensitivity simultaneously and preparation method thereof |
| CN110487847A (en) * | 2019-08-26 | 2019-11-22 | 济南大学 | A kind of ZnO/Sn3O4Gas sensitive and preparation method thereof and application in the sensor |
| WO2023060742A1 (en) * | 2021-10-15 | 2023-04-20 | 光华临港工程应用技术研发(上海)有限公司 | Gas-sensitive nanomaterial having branched nanowire structure, preparation method therefor and application thereof |
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