CN105036180B - A kind of preparation method of the flower-shaped composite of stannum oxide/zinc-oxide nano - Google Patents
A kind of preparation method of the flower-shaped composite of stannum oxide/zinc-oxide nano Download PDFInfo
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- CN105036180B CN105036180B CN201510360841.8A CN201510360841A CN105036180B CN 105036180 B CN105036180 B CN 105036180B CN 201510360841 A CN201510360841 A CN 201510360841A CN 105036180 B CN105036180 B CN 105036180B
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Abstract
The invention discloses the preparation method of a kind of flower-shaped composite of stannum oxide/zinc-oxide nano.First, use one step hydro thermal method, obtain nano tin dioxide base material in the basic conditions；Then, zinc oxide crystal seed liquid is mixed with nano tin dioxide, make crystal seed be carried on tin oxide base bottom material；Finally, use hydro-thermal method growing nano zinc oxide on crystal seed, i.e. can get the flower-shaped composite of stannum oxide/zinc-oxide nano.Seeded growth method is combined by the present invention with hydro-thermal method, and prepared stannum oxide/nano zinc oxide material has floriform appearance, and this composite can be widely applied to the fields such as gas sensing, photocatalysis, battery.
Description
Technical field
The invention belongs to nano composite material technical field, be specifically related to a kind of stannum oxide/zinc-oxide nano flower-shaped compound
The preparation method of material.
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 stannum oxide SnO2With zinc oxide ZnO have wider energy gap, higher vapor sensitivity and
Preferably optical property, enjoys the concern of scientists.Therefore, study hotspot is just fallen multiple at stannum oxide/zinc oxide by people
On condensation material, it is desirable to given full play to the excellent properties of bi-material by recombination energy, and demonstrate in some aspects than single material
Expect the most superior character.
At present, major part stannum oxide/zinc oxide composite is all by coprecipitation, method of electrostatic spinning, ball-milling method, height
The preparations such as temperature spraying process, it is only and two kinds of materials are simply mixed together, contact circle between stannum oxide and zinc oxide
Face is the most insecure.Therefore, invent a kind of stannum oxide/zinc oxide composite and synthetic method that both combine closely is the heaviest
Want.
Summary of the invention
For overcoming the deficiencies in the prior art, the invention provides a kind of flower-shaped composite of stannum oxide/zinc-oxide nano
Preparation method, uses seeded growth method to combine with hydro-thermal method, developing zinc oxide on tin oxide base bottom material, thus is had
There is the stannum oxide/zinc oxide nanometer composite material of floriform appearance.
The preparation method of a kind of flower-shaped composite of stannum oxide/zinc-oxide nano, it is characterised in that the concrete step of the method
Suddenly it is:
(1) nano tin dioxide SnO2The preparation of base material: by two hydration stannum dichloride SnCl2·2H2O aqueous solution and hydrogen
Sodium oxide NaOH aqueous solution, makes three's mol ratio SnCl2·2H2O:NaOH:H2O=1:3-5:1250-1750, stirring obtains
Uniformly clarify precursor liquid；Reaction solution is transferred in politef water heating kettle, in 160 DEG C of hydro-thermal reactions 12-in an oven
18 hours；Will centrifugal after the precipitate with deionized water that obtain and absolute ethanol washing repeatedly, be dried, with agate mortar finely ground after
To nano tin dioxide SnO2Base material；
(2) load of zinc oxide crystal seed: compound concentration is the two acetate hydrate zinc Zn of 0.005-0.02mol/L
(CH3COO)2·2H2The ethanol solution of O or zinc nitrate hexahydrate Zn (NO3)2·6H2The ethanol solution of O is as zinc oxide crystal seed
Liquid；Crystal seed drop is added nano SnO2Base material is also fully ground so that it is is dried after mix homogeneously, and repeatedly, rubs
You are than Zn (CH3COO)2·2H2O:SnO2Or Zn (NO3)2·6H2O:SnO2 =1:20-50, makes zinc oxide crystal seed be carried on oxidation
On tinbase bottom material；
(3) preparation of stannum oxide/zinc oxide nanometer composite material: by zinc nitrate hexahydrate Zn (NO3)2·6H2O aqueous solution
Mix with hexamethylenetetramine HMT, make three mol ratio Zn (NO3)2·6H2O:HMT:H2O=1:1:1500-2500, stirs
To uniformly clarifying precursor liquid；The tin oxide base bottom material having loaded zinc oxide crystal seed is placed in politef water heating kettle, adds
Enter above-mentioned precursor liquid and stir, in 95-105 DEG C of hydro-thermal reaction 3-6 hour in an oven；Will centrifugal after the precipitation that obtains spend from
Sub-water and absolute ethanol washing repeatedly, drying to obtain stannum oxide/flower-shaped composite of zinc-oxide nano.
Zinc oxide crystal seed liquid is two acetate hydrate zinc Zn (CH3COO)2·2H2O or zinc nitrate hexahydrate Zn (NO3)2·6H2O
Ethanol solution.
Hexamethylenetetramine HMT is used to regulate the basicity of solution.
Seeded growth method is used to combine with hydro-thermal method, developing zinc oxide on tin oxide base bottom material, thus had
There is the stannum oxide/zinc oxide nanometer composite material of floriform appearance.
Seeded growth method is combined by the present invention with hydro-thermal method, and prepared stannum oxide/nano zinc oxide material has flower
Shape pattern, this composite can be widely applied to the fields such as gas sensing, photocatalysis, battery.
Accompanying drawing explanation
Fig. 1 is the scanning electron microscope (SEM) photograph of the flower-shaped composite of stannum oxide/zinc-oxide nano of the embodiment of the present invention 1 synthesis.
Fig. 2 is the scanning electron microscope (SEM) photograph of the flower-shaped composite of stannum 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 composite of stannum oxide/zinc-oxide nano of the embodiment of the present invention 3 synthesis.
Detailed description of the invention
The present invention is described in detail by following instantiation, but protection scope of the present invention is not only restricted to these in fact
Execute example.
Embodiment 1:
(1) nano tin dioxide SnO2The preparation of base material: by 1.785 g SnCl2·2H2O be dissolved in 170 g water and
In 45 ml 0.8 M NaOH mixed systems, 35 DEG C of stirrings are uniformly clarified precursor liquid in 0.5 hour；Reaction solution is transferred to
In politef water heating kettle, in 160 DEG C of hydro-thermal reaction 15 hours in an oven；The precipitate with deionized water obtained after being centrifuged
With absolute ethanol washing repeatedly, be dried, with agate mortar finely ground after obtain nano tin dioxide SnO2Base material.
(2) load of zinc oxide crystal seed: by 0.011 g Zn (CH3COO)2·2H2O is dissolved in 10 ml dehydrated alcohol,
35 DEG C of stirrings obtain zinc oxide crystal seed liquid in 0.5 hour；Take 0.025 g nano SnO2Base material is placed in agate mortar, drips 0.1
Ml zinc oxide crystal seed liquid is also fully ground so that it is is dried after mix homogeneously, and repeats ten times, makes zinc oxide crystal seed be carried on oxygen
Change on tinbase bottom material；
(3) preparation of stannum oxide/zinc oxide nanometer composite material: by 0.263 g Zn (NO3)2·6H2O and 0.124 g
HMT is dissolved in 35g water, and precursor liquid is uniformly clarified in stirring；The tin oxide base bottom material having loaded zinc oxide crystal seed is placed in
In politef water heating kettle, add above-mentioned precursor liquid and stir, in 95 DEG C of hydro-thermal reaction 3 hours in an oven；After being centrifuged
The precipitate with deionized water obtained and absolute ethanol washing repeatedly, drying to obtain stannum oxide/flower-shaped composite wood of zinc-oxide nano
Material.Fig. 1 is the stereoscan photograph of this composite.
Embodiment 2:
(1) nano tin dioxide SnO2The preparation of base material: by 1.785 g SnCl2·2H2O be dissolved in 210 g water and
In 35 ml 0.8 M NaOH mixed systems, 35 DEG C of stirrings are uniformly clarified precursor liquid in 0.5 hour；Reaction solution is transferred to
In politef water heating kettle, in 160 DEG C of hydro-thermal reaction 18 hours in an oven；The precipitate with deionized water obtained after being centrifuged
With absolute ethanol washing repeatedly, be dried, with agate mortar finely ground after obtain nano tin dioxide SnO2Base material.
(2) load of zinc oxide crystal seed: by 0.06 g Zn (NO3)2·6H2O be dissolved in 10 ml dehydrated alcohol, 35
DEG C stirring obtains zinc oxide crystal seed liquid in 0.5 hour；Take 0.025 g nano SnO2Base material is placed in agate mortar, drips 0.1 ml
Zinc oxide crystal seed liquid is also fully ground so that it is is dried after mix homogeneously, and is repeated four times, makes zinc oxide crystal seed be carried on stannum oxide
On base material；
(3) preparation of stannum oxide/zinc oxide nanometer composite material: by 0.263 g Zn (NO3)2·6H2O and 0.124 g
HMT is dissolved in 30g water, and precursor liquid is uniformly clarified in stirring；The tin oxide base bottom material having loaded zinc oxide crystal seed is placed in
In politef water heating kettle, add above-mentioned precursor liquid and stir, in 100 DEG C of hydro-thermal reaction 6 hours in an oven；Will be centrifugal
After the precipitate with deionized water that obtains and absolute ethanol washing repeatedly, drying to obtain stannum oxide/zinc-oxide nano is flower-shaped compound
Material.Fig. 2 is the stereoscan photograph of this composite.
Embodiment 3:
(1) nano tin dioxide SnO2The preparation of base material: by 1.785 g SnCl2·2H2O be dissolved in 147 g water and
In 40 ml 0.8 M NaOH mixed systems, 35 DEG C of stirrings are uniformly clarified precursor liquid in 0.5 hour；Reaction solution is transferred to
In politef water heating kettle, in 160 DEG C of hydro-thermal reaction 12 hours in an oven；The precipitate with deionized water obtained after being centrifuged
With absolute ethanol washing repeatedly, be dried, with agate mortar finely ground after obtain nano tin dioxide SnO2Base material.
(2) load of zinc oxide crystal seed: by 0.022 g Zn (CH3COO)2·2H2O is dissolved in 10 ml dehydrated alcohol,
35 DEG C of stirrings obtain zinc oxide crystal seed liquid in 0.5 hour；Take 0.025 g nano SnO2Base material is placed in agate mortar, drips 0.1
Ml zinc oxide crystal seed liquid is also fully ground so that it is is dried after mix homogeneously, and is repeated four times, makes zinc oxide crystal seed be carried on oxygen
Change on tinbase bottom material；
(3) preparation of stannum oxide/zinc oxide nanometer composite material: by 0.263 g Zn (NO3)2·6H2O and 0.124 g
HMT is dissolved in 25g water, and precursor liquid is uniformly clarified in stirring；The tin oxide base bottom material having loaded zinc oxide crystal seed is placed in
In politef water heating kettle, add above-mentioned precursor liquid and stir, in 105 DEG C of hydro-thermal reaction 3 hours in an oven；Will be centrifugal
After the precipitate with deionized water that obtains and absolute ethanol washing repeatedly, drying to obtain stannum oxide/zinc-oxide nano is flower-shaped compound
Material.Fig. 3 is the transmission electron microscope photo of this composite.
Claims (1)
1. the preparation method of the flower-shaped composite of stannum oxide/zinc-oxide nano, it is characterised in that the concrete steps of the method
For:
(1) nano tin dioxide SnO2The preparation of base material: by two hydration stannum dichloride SnCl2·2H2O aqueous solution and hydroxide
Sodium NaOH aqueous solution, makes three's mol ratio SnCl2·2H2O:NaOH:H2O=1:3-5:1250-1750, stirring obtains uniformly
Clarification precursor liquid；Reaction solution is transferred in politef water heating kettle, in 160 DEG C in an oven hydro-thermal reaction 12-18 little
Time；Will centrifugal after the precipitate with deionized water that obtain and absolute ethanol washing repeatedly, be dried, with agate mortar finely ground after received
Rice stannum oxide SnO2Base material；
(2) load of zinc oxide crystal seed: compound concentration is the two acetate hydrate zinc Zn (CH of 0.005-0.02mol/L3COO)2·
2H2The ethanol solution of O or zinc nitrate hexahydrate Zn (NO3)2·6H2The ethanol solution of O is as zinc oxide crystal seed liquid；By crystal seed liquid
It is added dropwise to nano SnO2Base material is also fully ground so that it is be dried after mix homogeneously, and repeatedly, mol ratio Zn
(CH3COO)2·2H2O:SnO2Or Zn (NO3)2·6H2O:SnO2 =1:20-50, makes zinc oxide crystal seed be carried at the bottom of tin oxide base
On material；
(3) preparation of stannum oxide/zinc oxide nanometer composite material: by zinc nitrate hexahydrate Zn (NO3)2·6H2O aqueous solution and six
Methine tetramine HMT mixes, and makes three mol ratio Zn (NO3)2·6H2O:HMT:H2O=1:1:1500-2500, stirring obtains all
Even clarification precursor liquid；The tin oxide base bottom material having loaded zinc oxide crystal seed is placed in politef water heating kettle, in addition
State precursor liquid and stir, in 95-105 DEG C of hydro-thermal reaction 3-6 hour in an oven；The precipitate with deionized water obtained after being centrifuged
With absolute ethanol washing repeatedly, drying to obtain stannum oxide/flower-shaped composite of zinc-oxide nano.
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| CN105381802B (en) * | 2015-12-23 | 2018-10-02 | 哈尔滨工业大学 | One kind preparing dandelion shape Fe based on heterogeneous nucleation means3O4The methods and applications of@ZnO nucleocapsid compounds |
| 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 |
| 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 |
| CN108593167B (en) * | 2018-03-20 | 2019-12-24 | 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 |
| CN110487847B (en) * | 2019-08-26 | 2022-08-09 | 济南大学 | ZnO/Sn 3 O 4 Gas sensitive material, preparation method thereof and application thereof in sensor |
| CN114047230A (en) * | 2021-10-15 | 2022-02-15 | 光华临港工程应用技术研发(上海)有限公司 | Gas-sensitive nanomaterial with branched nanowire structure, preparation method and application thereof |
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