CN106430292A - ZnO@SnO2 dendritic heterostructure nano material and preparation method thereof - Google Patents
ZnO@SnO2 dendritic heterostructure nano material and preparation method thereof Download PDFInfo
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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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- C01—INORGANIC CHEMISTRY
- C01P—INDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS
- C01P2004/00—Particle morphology
- C01P2004/01—Particle morphology depicted by an image
- C01P2004/03—Particle morphology depicted by an image obtained by SEM
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- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01P—INDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS
- C01P2004/00—Particle morphology
- C01P2004/30—Particle morphology extending in three dimensions
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- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01P—INDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS
- C01P2004/00—Particle morphology
- C01P2004/80—Particles consisting of a mixture of two or more inorganic phases
- C01P2004/82—Particles consisting of a mixture of two or more inorganic phases two phases having the same anion, e.g. both oxidic phases
- C01P2004/84—Particles consisting of a mixture of two or more inorganic phases two phases having the same anion, e.g. both oxidic phases one phase coated with the other
Abstract
The invention discloses a ZnO@SnO2 dendritic heterostructure nano material and a preparation method thereof. The 'trunk' of the ZnO@SnO2 dendritic heterostructure nano material is a ZnO nanowire; the surface of the ZnO nanowire is wrapped by a part of SnO2 in a cover manner; and the other part of the SnO2 grows out from the 'trunk'of the ZnO nanowire in a mode of 'twigs'. A CVD method is adopted, special horizontal tubular furnace equipment is used, the operation is simple and feasible, raw materials are cheap, a process is simple and easy to operate, and large-scale industrial production can be achieved. In addition, as a multi-stage structure is formed for the prepared ZnO@SnO2 dendritic heterostructure nano material, novel nano morphology is generated, a novel heterostructure is generated, a novel interface is formed, and active sites of reactions are increased because of a relatively large specific surface area, so that reaction characteristics of the nano composite material can be improved, and application prospects of the nano composite material in fields of energy storage, catalysis and sensation can be widened.
Description
Technical field
The present invention relates to heterojunction structure nano material field, more particularly to a kind of oxide heterogeneous structure nano material and its
Preparation method.
Background technology
SnO2It is considered as a kind of very potential oxide material for being applied to the present age or even following multiple industrial circles,
In recent years, SnO2Monodimension nanometer material be subjected to the concern from each research field, people are with single SnO2Receive
Rice noodle prepares field-effect transistor as channel layer；By appropriate functionalization means, prepared by the mesh nano line for preparing
Become the NO of excellent performance2Gas sensor, and in tree-shaped SnO2It is found that in nano wire that very strong fluorescence radiation is existing
As.
ZnO is another kind of typically multi-functional oxide material, particularly has very strong application in optoelectronic areas
Prospect, such as blue/UV electronic device etc..Due to its outstanding performance, ZnO also shows in such as plane, spinning electron
The field such as, DSSC, gas sensing, bio-sensing or even lithium ion battery anode material has potential
Application.
Using suitable growing method, many oxide is combined and more complicated one-dimensional nano structure is obtained, for example
Growing the multivariant oxide monodimension nanometer material with dendritic structure may make the material possess special performance, this multiple
The multivariant oxide nanostructured of conjunction can not only have the performance of many oxide concurrently, with bigger specific surface area, and not
Also new cooperative effect may can be produced with the heterojunction structure between oxide, special so as to produce that single oxide do not possess
Advantage.By oxide-based nanomaterial as a example by the application in terms of gas sensing, the material of the oxide heterogeneous structure nano wire of dendroid
Material very may have application prospect, because in the interaction process with gas molecule, it will there is at least three kinds differences
Model of action produce：1）" trunk " and " branch " can produce interaction with gas molecule；2）" trunk " and " trunk ",
The homostyructure potential barrier for contacting formation between " branch " and " branch " will produce special response mode；3）" trunk " and " tree
The heterostructure barriers for contacting formation between branch " can also produce special response mode.This is received in the oxide of one-component
Situation about can not possibly produce in rice noodle.When these three different model of action collaborations are produced, it will so that the ringing in air-sensitive of material
Sensitivity during answering is greatly improved, so as to promote the research of excellent properties gas sensor.
The present invention is based on above-mentioned background context, devises a kind of ZnO@SnO2Dendroid heterojunction structure nano material,
And adopt chemical vapor deposition（CVD）Method prepares the nano material, is that its application in fields such as gas sensings provides pass
Key material.
Content of the invention
Based on the exploration to growing hetero nano structure, the present invention puts forth effort to obtain a kind of excellent binary oxide of structure different
Matter nanostructured.
The invention provides a kind of ZnO@SnO2Dendroid heterojunction structure nano material, it is characterised in that：" trunk " is ZnO
Nano wire, SnO2A part is wrapped in ZnO nano-wire surface in a covered manner, another part be in the form of " branch " from
ZnO nano-wire " trunk " superficial growth nano wire out.
Further, described a kind of ZnO@SnO2Dendroid heterojunction structure nano material, ZnO nano-wire length is more than 10
μm, a diameter of 100 ~ 200nm, SnO2Dendritic nanowire length is 0.5 ~ 2 μm.
Present invention also offers the ZnO@SnO2The preparation method of dendroid heterojunction structure nano material, its step is such as
Under：
1）Prepare the quartz ampoule of an end closure, with mass ratio as 1：1 zinc oxide（ZnO）And powdered carbon（C）Mixture be
Zinc source, weighs the sealing end that appropriate zinc source is placed in quartz ampoule, and the silicon chip that surface is processed through metal spraying is placed in opening for quartz ampoule
Mouth end, is then positioned over the quartz ampoule in double temperature-area tubular furnaces, the sealing end for placing zinc source is placed in right warm area, place metal spraying
The opening of silicon chip is placed in left warm area, then arranges right warm area temperature for 900 ~ 1000 DEG C, and left warm area temperature is 750 ~ 850 DEG C,
Control chamber pressure 10torr, it is 30min in 1 ~ 5sccm, the response time that oxygen flux is, reaction takes out silicon chip after terminating；
2）By step 1）The silicon chip that surface length has ZnO nano-wire carries out metal spraying again and processes, and is then placed into the opening of quartz ampoule
End, with mass ratio as 1：1 stannum oxide（SnO2）And powdered carbon（C）Mixture be Xi Yuan, weigh appropriate Xi Yuan and be positioned over stone
The sealing end of English pipe, is then positioned over quartz ampoule in tube furnace, and the sealing end for placing Xi Yuan is placed in right warm area, and placing length has
The opening of ZnO nano-wire silicon chip is placed in left warm area, then arranges right warm area temperature for 850 ~ 950 DEG C, and left warm area temperature is 750
~ 850 DEG C, control chamber pressure 10torr, it is 20min in 1 ~ 5sccm, the response time that oxygen flux is, reaction takes out silicon after terminating
Piece, that is, obtain ZnO SnO2Dendroid hetero nano structure.
The useful achievement of the present invention is：
ZnO@SnO described in 1 the inventive method2Dendroid heterojunction structure nano material, is prepared using CVD method, can be by life
The change of long parameter adjusts size and the pattern of nano material, to meet different performance requirements, ZnO@SnO2Dendroid is heterogeneous
Structure nano material can achieve effective controllable standby.
2 ZnO@SnO2Dendroid heterojunction structure nano material is a kind of composite, can have ZnO and SnO concurrently2Bi-material
Advantage, and form new cooperative effect, obtain more preferably combination property.
3 ZnO@SnO2Dendroid heterojunction structure nano material has typical 3-D solid structure, and " trunk " is received for ZnO
Rice noodle, " branch " is SnO2Nano wire, clearly demarcated " tree " " branch " the shape heterojunction structure of this structure, compared to simple ZnO nano
Line and SnO2Nano wire, with being more widely applied field.
4 ZnO@SnO2The multilevel hierarchy formed by dendroid heterojunction structure nano material, generates new nanotopography,
It is a kind of new heterojunction structure, and causes new interface, and larger specific surface area increased the avtive spot of reaction, so as to
The response characteristic of the nano composite material can be lifted, expands its application prospect in energy storage, catalysis and sensory field.
5 adopt CVD method, and only use level tubular type furnace apparatus, are a kind of industrialized equipment, simple, original used
Material is inexpensive, and technique is simple and clear and easily operated, achievable large-scale industrial production.
Description of the drawings
Fig. 1 is the scanning electron microscope of the ZnO nano-wire material for obtaining in 1 implementation process of embodiment（SEM）Figure.
Fig. 2 is ZnO@SnO obtained in embodiment 12The scanning electron microscope of dendroid heterojunction structure nano material（SEM）
Figure.
Fig. 3 is ZnO@SnO obtained in embodiment 22The scanning electron microscope of dendroid heterojunction structure nano material（SEM）
Figure.
Fig. 4 is ZnO@SnO obtained in embodiment 32The scanning electron microscope of dendroid heterojunction structure nano material（SEM）
Figure.
Fig. 5 is the chemical vapor deposition for adopting in implementation process of the present invention（CVD）Horizontal pipe furnace equipment schematic diagram.In figure
1 is boiler tube, and 2 is quartz ampoule, and 3 is left warm area, and 4 is right warm area.
Specific embodiment
Below in conjunction with specific embodiment, the present invention is further illustrated.
Embodiment 1
1）Prepare the quartz ampoule of an end closure, be placed in as Fig. 5 chemical vapor deposition（CVD）In horizontal tube furnace apparatus, Fig. 5
For the CVD horizontal pipe furnace equipment schematic diagram for adopting in implementation process of the present invention, it is ZnO@SnO of the present invention2Dendroid hetero-junctions
The special-purpose growth equipment of structure nano material.As 2 right-hand member of quartz ampoule sealing in Fig. 5, the sealing that 0.1g zinc source is placed in quartz ampoule is weighed
End, the silicon chip that surface is processed through metal spraying is placed in the opening of quartz ampoule, and in such as Fig. 5,2 left end of quartz ampoule is opening；Then
The quartz ampoule is positioned in double temperature-area tubular furnaces, such as in the CVD equipment of Fig. 5, including left warm area 3 and 4 two warm areas of right warm area,
The sealing end for placing zinc source is placed in right warm area 4, the opening for placing metal spraying silicon chip is placed in left warm area 3, then arranges right warm area
Temperature is 900 DEG C, and left warm area temperature is 750 DEG C, controls chamber pressure 10torr, and oxygen flux is 1sccm, the response time to be
30min, reaction takes out silicon chip after terminating.
2）By step 1）The silicon chip that surface length has ZnO nano-wire carries out metal spraying again and processes, and is then placed into quartz ampoule
Opening, weighs the sealing end that 0.01g Xi Yuan is positioned over quartz ampoule, then quartz ampoule is positioned in tube furnace, will place stannum
The sealing end in source is placed in right warm area, and the opening that placing length has ZnO nano-wire silicon chip is placed in left warm area, then arranges right warm area temperature
Spend for 950 DEG C, left warm area temperature is 850 DEG C, control chamber pressure 10torr, oxygen flux is 3sccm, the response time to be
20min, reaction takes out silicon chip after terminating, that is, obtain ZnO SnO2Dendroid hetero nano structure.
Fig. 1 is the scanning electron microscope of the ZnO nano-wire material for obtaining in 1 implementation process of embodiment（SEM）Figure, ZnO
Nanowire length be more than 10 μm, 100 ~ 200nm of diameter, the ZnO nano-wire for obtaining in other embodiments implementation process also with this
Similar.
Fig. 2 is ZnO@SnO obtained in embodiment 12The scanning electron microscope of dendroid heterojunction structure nano material（SEM）
Figure, SnO2" branch " length about 500nm.
Embodiment 2
1）Prepare the quartz ampoule of an end closure, the sealing end that 0.3g zinc source is placed in quartz ampoule is weighed, by surface through metal spraying
The silicon chip of process is placed in the opening of quartz ampoule, then the quartz ampoule is positioned in double temperature-area tubular furnaces, will place zinc source
Sealing end is placed in right warm area, and the opening for placing metal spraying silicon chip is placed in left warm area, then arranges right warm area temperature for 950 DEG C, left
Warm area temperature is 800 DEG C, controls chamber pressure 10torr, and it is 30min in 3sccm, the response time that oxygen flux is, after reaction terminates
Take out silicon chip.
2）By step 1）The silicon chip that surface length has ZnO nano-wire carries out metal spraying again and processes, and is then placed into quartz ampoule
Opening, weighs the sealing end that 0.05g Xi Yuan is positioned over quartz ampoule, then quartz ampoule is positioned in tube furnace, will place stannum
The sealing end in source is placed in right warm area, and the opening that placing length has ZnO nano-wire silicon chip is placed in left warm area, then arranges right warm area temperature
Spend for 900 DEG C, left warm area temperature is 800 DEG C, control chamber pressure 10torr, oxygen flux is 5sccm, the response time to be
20min, reaction takes out silicon chip after terminating, that is, obtain ZnO SnO2Dendroid hetero nano structure.
Fig. 3 is ZnO@SnO obtained in embodiment 22The scanning electron microscope of dendroid heterojunction structure nano material（SEM）
Figure, SnO2About 1 μm of " branch " length.
Embodiment 3
1）Prepare the quartz ampoule of an end closure, the sealing end that 0.5g zinc source is placed in quartz ampoule is weighed, by surface through metal spraying
The silicon chip of process is placed in the opening of quartz ampoule, then the quartz ampoule is positioned in double temperature-area tubular furnaces, will place zinc source
Sealing end is placed in right warm area, and the opening for placing metal spraying silicon chip is placed in left warm area, then arranges right warm area temperature for 1000 DEG C, left
Warm area temperature is 850 DEG C, controls chamber pressure 10torr, and it is 30min in 5sccm, the response time that oxygen flux is, after reaction terminates
Take out silicon chip.
2）By step 1）The silicon chip that surface length has ZnO nano-wire carries out metal spraying again and processes, and is then placed into quartz ampoule
Opening, weighs the sealing end that 0.1g Xi Yuan is positioned over quartz ampoule, then quartz ampoule is positioned in tube furnace, will place Xi Yuan
Sealing end be placed in right warm area, the opening that placing length has ZnO nano-wire silicon chip is placed in left warm area, then arranges right warm area temperature
For 850 DEG C, left warm area temperature is 750 DEG C, controls chamber pressure 10torr, and it is 20min in 1sccm, the response time that oxygen flux is,
Reaction takes out silicon chip after terminating, that is, obtain ZnO SnO2Dendroid hetero nano structure.
Fig. 4 is ZnO@SnO obtained in embodiment 32The scanning electron microscope of dendroid heterojunction structure nano material（SEM）
Figure, SnO2About 2 μm of " branch " length.
In the various embodiments described above, the zinc source for using is mass ratio for 1：1 zinc oxide（ZnO）And powdered carbon（C）Mixed
Compound, the Xi Yuan for using is mass ratio for 1：1 stannum oxide（SnO2）And powdered carbon（C）Mixture, wherein zinc oxide
（ZnO）, stannum oxide（SnO2）, powdered carbon（C）It is analysis pure.
Claims (5)
1. a kind of ZnO@SnO2Dendroid heterojunction structure nano material, it is characterised in that：The ZnO@SnO2Dendroid heterojunction structure
" trunk " of nano material is ZnO nano-wire, SnO2A part is wrapped in " trunk " ZnO nano-wire surface in a covered manner,
Another part in the form of " branch " from the superficial growth of " trunk " ZnO nano-wire out.
2. a kind of ZnO@SnO according to claim 12Dendroid heterojunction structure nano material, it is characterised in that：" trunk "
ZnO nano-wire length is more than 10 μm, a diameter of 100 ~ 200nm；The SnO of the form of " branch "2Nanowire length is 0.5 ~ 2 μm.
3. a kind of ZnO@SnO described in claim 1 or 2 is prepared2The method of dendroid heterojunction structure nano material, its feature exists
In including step：
1）Prepare the quartz ampoule of an end closure, with the mixture of zinc oxide and powdered carbon as zinc source, weigh appropriate zinc source and put
In the sealing end of quartz ampoule, the silicon chip that surface is processed through metal spraying is placed in the opening of quartz ampoule, then puts the quartz ampoule
It is placed in double temperature-area tubular furnaces, the sealing end for placing zinc source is placed in right warm area, the opening for placing metal spraying silicon chip is placed in left temperature
Area, then arranges right warm area temperature for 900-1000 DEG C, and left warm area temperature is 750-850 DEG C, controls chamber pressure 10torr,
Oxygen flux is 1-5sccm, and the response time is 30min, and reaction takes out length after terminating the silicon chip of ZnO nano-wire；
2）By step 1）The silicon chip that surface length has ZnO nano-wire carries out metal spraying again and processes, and is then placed into the opening of quartz ampoule
End, weighs the sealing end that appropriate Xi Yuan is positioned over quartz ampoule, then quartz ampoule is positioned in tube furnace, will place Xi Yuan's
Sealing end is placed in right warm area, and the opening that placing length has the silicon chip of ZnO nano-wire is placed in left warm area, then arranges right warm area temperature
For 850-950 DEG C, left warm area temperature is 750-850 DEG C, controls chamber pressure 10torr, and oxygen flux is 1-5sccm, during reaction
Between be 20min, reaction terminate after take out silicon chip, that is, obtain ZnO SnO2Dendroid heterojunction structure nano material.
4. ZnO@SnO according to claim 32The preparation method of dendroid heterojunction structure nano material, it is characterised in that：
Step 1）Described zinc source is 1 for mass ratio：1 zinc oxide and the mixture of powdered carbon.
5. ZnO@SnO according to claim 32The preparation method of dendroid heterojunction structure nano material, it is characterised in that：
Step 2）Xi Yuan is with mass ratio as 1:1 stannum oxide and powdered carbon mixture.
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Cited By (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN108828021A (en) * | 2018-05-03 | 2018-11-16 | 吉林大学 | Based on branching SnO2The alcohol gas sensor and preparation method thereof of/ZnO heterojunction structure sensitive material |
| CN108956713A (en) * | 2018-06-29 | 2018-12-07 | 五邑大学 | ZnO/ carbon nanocoils sensitive material of propagation path horizontal distribution and preparation method thereof and high sensitivity sensor |
| CN109133159A (en) * | 2018-08-29 | 2019-01-04 | 浙江大学 | A kind of indium doping Zn2SnO4The preparation method of nano wire |
| CN109382087A (en) * | 2018-11-23 | 2019-02-26 | 西南交通大学 | A kind of stannic oxide-zinc stannate core-shell nano line and preparation method |
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Cited By (7)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN108828021A (en) * | 2018-05-03 | 2018-11-16 | 吉林大学 | Based on branching SnO2The alcohol gas sensor and preparation method thereof of/ZnO heterojunction structure sensitive material |
| CN108956713A (en) * | 2018-06-29 | 2018-12-07 | 五邑大学 | ZnO/ carbon nanocoils sensitive material of propagation path horizontal distribution and preparation method thereof and high sensitivity sensor |
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| CN109133159A (en) * | 2018-08-29 | 2019-01-04 | 浙江大学 | A kind of indium doping Zn2SnO4The preparation method of nano wire |
| CN109133159B (en) * | 2018-08-29 | 2020-06-26 | 浙江大学 | Indium-doped Zn2SnO4Method for preparing nano-wire |
| CN109382087A (en) * | 2018-11-23 | 2019-02-26 | 西南交通大学 | A kind of stannic oxide-zinc stannate core-shell nano line and preparation method |
| CN109382087B (en) * | 2018-11-23 | 2021-06-25 | 西南交通大学 | Tin dioxide-zinc stannate core-shell nanowire and preparation method thereof |
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