CN106430292B - A kind of ZnO@SnO2Dendroid heterojunction structure nano material and preparation method thereof - Google Patents
A kind of ZnO@SnO2Dendroid heterojunction structure nano material and preparation method thereof Download PDFInfo
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- 239000002086 nanomaterial Substances 0.000 title claims abstract description 36
- 238000002360 preparation method Methods 0.000 title description 6
- XOLBLPGZBRYERU-UHFFFAOYSA-N SnO2 Inorganic materials O=[Sn]=O XOLBLPGZBRYERU-UHFFFAOYSA-N 0.000 claims abstract description 41
- 239000002070 nanowire Substances 0.000 claims abstract description 33
- 238000006243 chemical reaction Methods 0.000 claims abstract description 14
- 238000000034 method Methods 0.000 claims abstract description 13
- 241000555268 Dendroides Species 0.000 claims abstract description 12
- XLOMVQKBTHCTTD-UHFFFAOYSA-N Zinc monoxide Chemical compound [Zn]=O XLOMVQKBTHCTTD-UHFFFAOYSA-N 0.000 claims description 113
- 239000011787 zinc oxide Substances 0.000 claims description 55
- 239000003708 ampul Substances 0.000 claims description 38
- 239000010453 quartz Substances 0.000 claims description 38
- VYPSYNLAJGMNEJ-UHFFFAOYSA-N silicon dioxide Inorganic materials O=[Si]=O VYPSYNLAJGMNEJ-UHFFFAOYSA-N 0.000 claims description 38
- XUIMIQQOPSSXEZ-UHFFFAOYSA-N Silicon Chemical compound [Si] XUIMIQQOPSSXEZ-UHFFFAOYSA-N 0.000 claims description 30
- 229910052710 silicon Inorganic materials 0.000 claims description 30
- 239000010703 silicon Substances 0.000 claims description 30
- 238000007789 sealing Methods 0.000 claims description 21
- 229910052751 metal Inorganic materials 0.000 claims description 15
- 239000002184 metal Substances 0.000 claims description 15
- 238000005507 spraying Methods 0.000 claims description 15
- HCHKCACWOHOZIP-UHFFFAOYSA-N Zinc Chemical compound [Zn] HCHKCACWOHOZIP-UHFFFAOYSA-N 0.000 claims description 14
- 229910052725 zinc Inorganic materials 0.000 claims description 14
- 239000011701 zinc Substances 0.000 claims description 14
- ATJFFYVFTNAWJD-UHFFFAOYSA-N Tin Chemical compound [Sn] ATJFFYVFTNAWJD-UHFFFAOYSA-N 0.000 claims description 12
- QVGXLLKOCUKJST-UHFFFAOYSA-N atomic oxygen Chemical compound [O] QVGXLLKOCUKJST-UHFFFAOYSA-N 0.000 claims description 10
- 230000004907 flux Effects 0.000 claims description 10
- 229910052760 oxygen Inorganic materials 0.000 claims description 10
- 239000001301 oxygen Substances 0.000 claims description 10
- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical compound [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 claims description 8
- 229910052799 carbon Inorganic materials 0.000 claims description 8
- 230000035484 reaction time Effects 0.000 claims description 8
- 239000000203 mixture Substances 0.000 claims description 5
- 229910001887 tin oxide Inorganic materials 0.000 claims description 4
- 239000000463 material Substances 0.000 abstract description 15
- 238000005229 chemical vapour deposition Methods 0.000 abstract description 6
- 230000004044 response Effects 0.000 abstract description 4
- 238000006555 catalytic reaction Methods 0.000 abstract description 2
- 238000004146 energy storage Methods 0.000 abstract description 2
- 238000009776 industrial production Methods 0.000 abstract description 2
- 239000002114 nanocomposite Substances 0.000 abstract description 2
- 239000002994 raw material Substances 0.000 abstract description 2
- 230000001953 sensory effect Effects 0.000 abstract description 2
- 239000007789 gas Substances 0.000 description 7
- 230000008569 process Effects 0.000 description 6
- 125000005842 heteroatom Chemical group 0.000 description 5
- 241000209094 Oryza Species 0.000 description 3
- 235000007164 Oryza sativa Nutrition 0.000 description 3
- 235000012149 noodles Nutrition 0.000 description 3
- 235000009566 rice Nutrition 0.000 description 3
- 230000009471 action Effects 0.000 description 2
- 230000008901 benefit Effects 0.000 description 2
- 230000015572 biosynthetic process Effects 0.000 description 2
- 230000002079 cooperative effect Effects 0.000 description 2
- 238000010586 diagram Methods 0.000 description 2
- 230000003993 interaction Effects 0.000 description 2
- HBBGRARXTFLTSG-UHFFFAOYSA-N Lithium ion Chemical compound [Li+] HBBGRARXTFLTSG-UHFFFAOYSA-N 0.000 description 1
- 238000004458 analytical method Methods 0.000 description 1
- 239000010405 anode material Substances 0.000 description 1
- 230000004888 barrier function Effects 0.000 description 1
- 230000008859 change Effects 0.000 description 1
- 239000002131 composite material Substances 0.000 description 1
- 150000001875 compounds Chemical class 0.000 description 1
- 238000005516 engineering process Methods 0.000 description 1
- 230000005669 field effect Effects 0.000 description 1
- 238000007306 functionalization reaction Methods 0.000 description 1
- 229910001416 lithium ion Inorganic materials 0.000 description 1
- 230000005693 optoelectronics Effects 0.000 description 1
- 238000005036 potential barrier Methods 0.000 description 1
- 230000005855 radiation Effects 0.000 description 1
- 230000035945 sensitivity Effects 0.000 description 1
- 239000007787 solid Substances 0.000 description 1
- 238000009987 spinning Methods 0.000 description 1
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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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- C—CHEMISTRY; METALLURGY
- 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
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- Chemical & Material Sciences (AREA)
- Organic Chemistry (AREA)
- Inorganic Chemistry (AREA)
- Crystals, And After-Treatments Of Crystals (AREA)
- Investigating Or Analyzing Materials By The Use Of Fluid Adsorption Or Reactions (AREA)
Abstract
The invention discloses a kind of ZnO@SnO2Dendroid heterojunction structure nano material and its growing method.Wherein ZnO@SnO2" trunk " of dendroid heterojunction structure nano material is ZnO nano-wire, and a SnO2 parts are wrapped in ZnO nano-wire surface in a covered manner, and another part is come out in the form of " branch " from ZnO nano-wire " trunk " superficial growth.The present invention uses CVD method, and simple and easy using special horizontal tube furnace apparatus, raw materials used inexpensive, technique is concise and easily operated, and large-scale industrial production can be achieved.And prepare the ZnO@SnO of gained2The multilevel hierarchy that dendroid heterojunction structure nano material is formed, generate new nanotopography, it is a kind of new heterojunction structure, and cause new interface, its larger specific surface area adds the avtive spot of reaction, so as to lift the response characteristic of the nano composite material, its application prospect in energy storage, catalysis and sensory field is expanded.
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 noodles prepare field-effect transistor as channel layer;By appropriate functionalization means, prepared by the mesh nano line of preparation
As the NO of excellent performance2Gas sensor, and in tree-shaped SnO2It is found that very strong fluorescence radiation shows in nano wire
As.
ZnO is another typical 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 is also shown in such as plane, spinning electron
The fields such as, DSSC, gas sensing, bio-sensing or even lithium ion battery anode material have potential
Using.
Many oxide is combined using suitable growing method and obtains more complicated one-dimensional nano structure, such as
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, have bigger specific surface area, and not
May can also produce new cooperative effect with the heterojunction structure between oxide, so as to produce single oxide do not possess it is special
Advantage.By oxide-based nanomaterial exemplified by the application in terms of gas sensing, the material of the oxide heterogeneous structure nano wire of dendroid
Material may very have application prospect, because in the interaction process with gas molecule, it will there is at least three kinds of differences
The mode of action produce:1)" trunk " and " branch " can produce interaction with gas molecule;2)" trunk " and " trunk ",
The homostyructure potential barrier of formation is contacted between " branch " and " branch " will produce special response mode;3)" trunk " and " tree
The heterostructure barriers of formation are contacted between branch " can also produce special response mode.This is received in the oxide of one-component
Can not possibly caused situation in rice noodles.When these three different mode of action collaborations produce, it will so that material rings in air-sensitive
Sensitivity during answering greatly improves, 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 use chemical vapor deposition(CVD)Method prepares the nano material, and pass is provided for its application in fields such as gas sensings
Key material.
The 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
The nano wire that ZnO nano-wire " trunk " superficial growth comes out.
Further, described a kind of ZnO@SnO2Dendroid heterojunction structure nano material, ZnO nano-wire length are 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, using mass ratio as 1:1 zinc oxide(ZnO)And powdered carbon(C)Mixing
Thing is zinc source, weighs the sealing end that appropriate zinc source is placed in quartz ampoule, and silicon chip of the surface by metal spraying processing is placed in into quartz ampoule
Openend, then the quartz ampoule is positioned in double temperature-area tubular furnaces, the sealing end for placing zinc source is placed in right warm area, placed
The openend of metal spraying silicon chip is placed in left warm area, and it is 900 ~ 1000 DEG C then to set right warm area temperature, and left warm area temperature is 750 ~ 850
DEG C, chamber pressure 10torr is controlled, oxygen flux is 1 ~ 5sccm, reaction time 30min, and reaction takes out silicon chip after terminating;
2)By step 1)Silicon chip of the surface with ZnO nano-wire carries out metal spraying again and handled, and is then placed into quartz ampoule
Openend, using mass ratio as 1:1 tin oxide(SnO2)And powdered carbon(C)Mixture be tin source, weigh appropriate tin source and place
In the sealing end of quartz ampoule, then quartz ampoule is positioned in tube furnace, the sealing end for placing tin source is placed in right warm area, placed
Openend with ZnO nano-wire silicon chip is placed in left warm area, and it is 850 ~ 950 DEG C then to set right warm area temperature, left warm area temperature
For 750 ~ 850 DEG C, chamber pressure 10torr is controlled, oxygen flux is 1 ~ 5sccm, reaction time 20min, and reaction takes after terminating
Go out silicon chip, 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
By the size and pattern of the change regulation nano material of growth parameter(s), to meet different performance requirements, ZnO@SnO2Branch
Shape heterojunction structure nano material can realize effective controllable preparation.
2 ZnO@SnO2Dendroid heterojunction structure nano material is a kind of composite, can have ZnO and SnO concurrently2Two kinds of materials
The advantages of material, and new cooperative effect is formed, 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 noodles, " branch " are SnO2Nano wire, clearly demarcated " tree " " branch " shape heterojunction structure of this structure, compared to simple ZnO nano
Line and SnO2Nano wire, have and be more widely applied field.
4 ZnO@SnO2The multilevel hierarchy that dendroid heterojunction structure nano material is formed, new nanotopography is generated,
It is a kind of new heterojunction structure, and causes new interface, and larger specific surface area adds 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 use CVD method, are a kind of industrialized equipment using only horizontal tube furnace apparatus, simple and easy, used
Raw material is inexpensive, and technique is concise and easily operated, and large-scale industrial production can be achieved.
Brief description of the drawings
Fig. 1 is the SEM of the ZnO nano-wire material obtained in the implementation process of embodiment 1(SEM)Figure.
Fig. 2 is ZnO@SnO made from embodiment 12The SEM of dendroid heterojunction structure nano material(SEM)
Figure.
Fig. 3 is ZnO@SnO made from embodiment 22The SEM of dendroid heterojunction structure nano material(SEM)
Figure.
Fig. 4 is ZnO@SnO made from embodiment 32The SEM of dendroid heterojunction structure nano material(SEM)
Figure.
Fig. 5 is the chemical vapor deposition used in implementation process of the present invention(CVD)Horizontal pipe furnace equipment schematic diagram.In figure
1 is boiler tube, and 2 be quartz ampoule, and 3 be left warm area, and 4 be right warm area.
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 such as Fig. 5 chemical vapor depositions(CVD)Horizontal tube furnace apparatus
In, Fig. 5 is the CVD horizontal pipe furnace equipment schematic diagrams used in implementation process of the present invention, is ZnO@SnO of the present invention2Dendroid
The special-purpose growth equipment of heterojunction structure nano material.Such as the right-hand member of quartz ampoule 2 sealing in Fig. 5, weigh 0.1g zinc source and be placed in quartz ampoule
Sealing end, silicon chip of the surface by metal spraying processing is placed in the openend of quartz ampoule, as the left end of quartz ampoule 2 is opening in Fig. 5
End;Then the quartz ampoule is positioned in double temperature-area tubular furnaces, as Fig. 5 CVD equipment in, including 4 liang of left warm area 3 and right warm area
Individual warm area, the sealing end for placing zinc source is placed in right warm area 4, the openend for placing metal spraying silicon chip is placed in left warm area 3, then sets
Right warm area temperature is 900 DEG C, and left warm area temperature is 750 DEG C, chamber pressure 10torr, oxygen flux 1sccm is controlled, during reaction
Between be 30min, reaction terminate after take out silicon chip.
2)By step 1)Silicon chip of the surface with ZnO nano-wire carries out metal spraying again and handled, and is then placed into quartz ampoule
Openend, the sealing end that 0.01g tin sources are positioned over quartz ampoule is weighed, then quartz ampoule is positioned in tube furnace, tin will be placed
The sealing end in source is placed in right warm area, places the openend with ZnO nano-wire silicon chip and is placed in left warm area, then sets right warm area temperature
Spend for 950 DEG C, left warm area temperature is 850 DEG C, controls chamber pressure 10torr, oxygen flux 3sccm, the reaction time is
20min, reaction take out silicon chip after terminating, that is, obtain ZnO SnO2Dendroid hetero nano structure.
Fig. 1 is the SEM of the ZnO nano-wire material obtained in the implementation process of embodiment 1(SEM)Figure, ZnO
Nanowire length be more than 10 μm, 100 ~ 200nm of diameter, the ZnO nano-wire obtained in other embodiments implementation process also with this
It is similar.
Fig. 2 is ZnO@SnO made from embodiment 12The SEM of dendroid heterojunction structure nano material(SEM)
Figure, SnO2" branch " length about 500nm.
Embodiment 2
1)Prepare the quartz ampoule of an end closure, weigh the sealing end that 0.3g zinc source is placed in quartz ampoule, surface is passed through
The silicon chip of metal spraying processing is placed in the openend of quartz ampoule, and then the quartz ampoule is positioned in double temperature-area tubular furnaces, will place zinc
The sealing end in source is placed in right warm area, and the openend for placing metal spraying silicon chip is placed in left warm area, and it is 950 then to set right warm area temperature
DEG C, left warm area temperature is 800 DEG C, controls chamber pressure 10torr, oxygen flux 3sccm, reaction time 30min, reaction
Silicon chip is taken out after end.
2)By step 1)Silicon chip of the surface with ZnO nano-wire carries out metal spraying again and handled, and is then placed into quartz ampoule
Openend, the sealing end that 0.05g tin sources are positioned over quartz ampoule is weighed, then quartz ampoule is positioned in tube furnace, tin will be placed
The sealing end in source is placed in right warm area, places the openend with ZnO nano-wire silicon chip and is placed in left warm area, then sets right warm area temperature
Spend for 900 DEG C, left warm area temperature is 800 DEG C, controls chamber pressure 10torr, oxygen flux 5sccm, the reaction time is
20min, reaction take out silicon chip after terminating, that is, obtain ZnO SnO2Dendroid hetero nano structure.
Fig. 3 is ZnO@SnO made from embodiment 22The SEM 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, weigh the sealing end that 0.5g zinc source is placed in quartz ampoule, surface is passed through
The silicon chip of metal spraying processing is placed in the openend of quartz ampoule, and then the quartz ampoule is positioned in double temperature-area tubular furnaces, will place zinc
The sealing end in source is placed in right warm area, and the openend for placing metal spraying silicon chip is placed in left warm area, and it is 1000 then to set right warm area temperature
DEG C, left warm area temperature is 850 DEG C, controls chamber pressure 10torr, oxygen flux 5sccm, reaction time 30min, reaction
Silicon chip is taken out after end.
2)By step 1)Silicon chip of the surface with ZnO nano-wire carries out metal spraying again and handled, and is then placed into quartz ampoule
Openend, the sealing end that 0.1g tin sources are positioned over quartz ampoule is weighed, then quartz ampoule is positioned in tube furnace, tin source will be placed
Sealing end be placed in right warm area, place the openend with ZnO nano-wire silicon chip and be placed in left warm area, then right warm area temperature is set
For 850 DEG C, left warm area temperature is 750 DEG C, controls chamber pressure 10torr, oxygen flux 1sccm, reaction time 20min,
Reaction takes out silicon chip after terminating, that is, obtains ZnO SnO2Dendroid hetero nano structure.
Fig. 4 is ZnO@SnO made from embodiment 32The SEM of dendroid heterojunction structure nano material(SEM)
Figure, SnO2About 2 μm of " branch " length.
In the various embodiments described above, the zinc source used is that mass ratio is 1:1 zinc oxide(ZnO)And powdered carbon(C)It is mixed
Compound, the tin source used are that mass ratio is 1:1 tin oxide(SnO2)And powdered carbon(C)Mixture, wherein zinc oxide
(ZnO), tin oxide(SnO2), powdered carbon(C)It is that analysis is pure.
Claims (2)
- A kind of 1. 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 is come out in the form of " branch " from " trunk " ZnO nano-wire superficial growth;Wherein " trunk " ZnO nano-wire length is big In 10 μm, a diameter of 100~200nm;The SnO of the form of " branch "2Nanowire length is 0.5~2 μm.
- 2. prepare a kind of ZnO@SnO described in claim 12The method of dendroid heterojunction structure nano material, it is characterised in that bag Include step:1) prepare the quartz ampoule of an end closure, using the mixture of zinc oxide and powdered carbon as zinc source, weigh appropriate zinc source and put In the sealing end of quartz ampoule, silicon chip of the surface by metal spraying processing is placed in the openend of quartz ampoule, then put 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 openend for placing metal spraying silicon chip is placed in left temperature Area, it is 900-1000 DEG C then to set right warm area temperature, and left warm area temperature is 750-850 DEG C, controls chamber pressure 10torr, Oxygen flux is 1-5sccm, reaction time 30min, and reaction takes out the silicon chip with ZnO nano-wire after terminating;2) silicon chip of the step 1) surface with ZnO nano-wire is carried out into metal spraying again to handle, is then placed into the opening of quartz ampoule End, weighs the sealing end that appropriate tin source is positioned over quartz ampoule, then quartz ampoule is positioned in tube furnace, will place tin source Sealing end is placed in right warm area, and the openend for placing the silicon chip with ZnO nano-wire is placed in left warm area, then sets right warm area temperature For 850-950 DEG C, left warm area temperature is 750-850 DEG C, chamber pressure 10torr, oxygen flux 1-5sccm is controlled, during reaction Between be 20min, reaction terminate after take out silicon chip, that is, obtain ZnO SnO2Dendroid heterojunction structure nano material;Zinc source wherein described in step 1) is that mass ratio is 1:1 zinc oxide and the mixture of powdered carbon;Tin source described in step 2) For using mass ratio as 1:1 tin oxide and powdered carbon mixture.
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