CN105836793A - SnO2/ZnO nanocomposite and preparation method thereof - Google Patents
SnO2/ZnO nanocomposite and preparation method thereof Download PDFInfo
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- CN105836793A CN105836793A CN201610298192.8A CN201610298192A CN105836793A CN 105836793 A CN105836793 A CN 105836793A CN 201610298192 A CN201610298192 A CN 201610298192A CN 105836793 A CN105836793 A CN 105836793A
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- C01P2002/70—Crystal-structural characteristics defined by measured X-ray, neutron or electron diffraction data
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- C01P2004/03—Particle morphology depicted by an image obtained by SEM
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- C01P2004/60—Particles characterised by their size
- C01P2004/61—Micrometer sized, i.e. from 1-100 micrometer
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- C01P2004/62—Submicrometer sized, i.e. from 0.1-1 micrometer
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- C—CHEMISTRY; METALLURGY
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- 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 SnO2/ZnO nanocomposite and a preparation method thereof. The SnO2/ZnO nanocomposite comprises a ZnO nanorod and an SnO2 nanorod growing on the ZnO nanorod, and is characterized in that the two-level structure SnO2 nanorod directly grows on the main structure ZnO nanorod, the ZnO nanorod in a wurtzite structure is prepared through a microwave-assisted hydrothermal method, the SnO2 nanorod of a rutile structure grows on the ZnO nanorod through a microwave-assisted hydrothermal method, and templates and catalysts are not needed in the microwave-assisted hydrothermal process. The speed is high, the process is simple, the yield is high, cost is low, the SnO2/ZnO nanocomposite is suitable for batch production, and the prepared nanocomposite is uniform in form and tight in coating, and can be used as a radar infrared compatible camouflage material, a photocatalysis material, a solar cell material, a gas sensor material and a lithium ion battery cathode material.
Description
Technical field
The invention belongs to field of nanometer material technology, relate to a kind of SnO2/ ZnO nano composite and preparation side thereof
Method.
Background technology
ZnO and SnO2It is two kinds of important direct wide bandgap semiconductor functional materials.ZnO is that energy gap is
3.37eV exciton bind energy is 60meV, SnO2Energy gap is 3.6eV, and exciton bind energy is 130meV,
ZnO and SnO2Composite be widely used gas sensor, solar cell, photocatalysis, lithium from
Sub-cell negative electrode material and material obsorbing radar waves.By ZnO and SnO2Both materials carry out compound composition
SnO2/ ZnO material, relatively homogenous material are compared, and all increase significantly at the aspect such as air-sensitive, photocatalysis performance,
Therefore in growth course, preferably control ZnO and SnO2The growth acquisition quality of nano material is good and has
The nano composite material of particular hierarchy, significant in application.There is a large amount of scientific research at present
Worker is engaged in ZnO and SnO2Material compound also achieves corresponding achievement, such as Chinese patent
CN200810116624 discloses a kind of one-dimensional SnO2The preparation method of-ZnO alloplasm nanobranch, profit
With gas transport, two step thermal evaporations are at Al2O3On substrate, growth obtains with SnO2For axle, ZnO is branch
SnO2-ZnO alloplasm nanobranch, its preparation process is relatively cumbersome, needs hot environment, and obtains
The SnO arrived2-ZnO alloplasm nanobranch is the most unordered, limits character and the application of material.
Summary of the invention
For defect and the deficiency of existing technology of preparing, the invention provides a kind of directly on ZnO nanorod
Growth SnO2Nano composite material preparation method, its preparation process is simple, aggregate velocity fast, reaction temperature
Monocrystalline SnO prepared by the low and present invention2Nanometer rods is homogeneous, be fitly grown in ZnO nanorod surface,
Be conducive to improving the character of material.
For solving the problems referred to above, the technical scheme that the present invention takes is:
A kind of SnO2/ ZnO nano composite, including ZnO nanorod and be grown in ZnO nanorod surface
On SnO2Nanometer rods.
Further, including monomer, described monomer includes ZnO nanorod and raw on ZnO nanorod
SnO2Nanometer rods.
Specifically, the draw ratio of described ZnO nanorod is 5～20, SnO2The draw ratio of nanometer rods be 5～
60。
More specifically, a length of 5～10 μm of described ZnO nanorod, ZnO nanorod a diameter of
0.5～1 μm；Described SnO2A length of the 200 of nanometer rods～600nm, SnO2Nanometer rods a diameter of 10～
40nm。
SnO described in preparation2The method of/ZnO nano composite, including using microwave radiation technology hydro-thermal legal system
Standby ZnO nanorod, then microwave radiation technology Hydrothermal Growth SnO on ZnO nanorod2Nanometer rods.
Specifically, described microwave assisted aqueous extraction hot preparation ZnO nanorod includes: is joined by strong base solution and contains
As reaction source in zinc compound solution, reaction source carries out hydro-thermal reaction under microwave condition, and microwave power is
400W, microwave temperature is 200 DEG C, and the microwave time is 15min, washs the product of hydro-thermal reaction for neutrality
And drying i.e. obtains ZnO nanorod.
More specifically, described zinc compound solution is Zn (CH3COOH)2Solution, in reaction source
Zn(CH3COOH)2The concentration of solution is 0.1mol/L, and described strong base solution is NaOH solution, reaction source
The concentration of middle NaOH solution is 1.4mol/L.
Specifically, described employing microwave radiation technology Hydrothermal Growth SnO on ZnO nanorod2Nanometer rods bag
Include: being joined by sn-containing compound solution and obtain growth solution in strong base solution, ZnO nanorod joins
Carrying out microwave hydrothermal reaction in growth solution, microwave power is 400W, and microwave temperature is 180～220 DEG C,
The microwave time is 15～60min, and the product washing reacted by microwave hydrothermal is neutral and drying
SnO2/ZnO nano composite material.
More specifically, described sn-containing compound solution is SnCl4Solution, described strong base solution is NaOH
Solution, NaOH and SnCl in growth solution4Mol ratio be [NaOH]: [SnCl4]=6～10:1, Microwave Water
SnCl in thermal response4It is [SnCl with the mol ratio of ZnO4]: [ZnO]=4～7:1.
Advantages of the present invention is:
(1) SnO that the present invention prepares2/ ZnO nano composite is in a length of 5～10 μm, straight
Footpath about 0.5～1 μm, draw ratio be 5～20 ZnO on grow SnO2Monocrystal nano rod, and SnO2
Monocrystal nano rod is along ZnO superficial growth, SnO2A length of the 200 of nanometer rods～600nm, a diameter of 10～
40nm, its draw ratio is 5～60；From microstructure, SnO2/ ZnO nano composite has the biggest
Specific surface area, can be used as gas sensor, SnO2There is substantial amounts of hetero-junctions in/ZnO nano composite,
Photo-generated carrier is compound to be reduced, and electron hole pair efficiently separates, thus adds life-span and the current-carrying of carrier
Sub-concentration so that SnO2/ ZnO nano composite can be as photocatalysis, gas sensor and lithium ion
Cell negative electrode material.
(2) present invention is at preparation SnO2During/ZnO nano composite, use microwave radiation technology hydro-thermal method at ZnO
Upper growth SnO2Monocrystal nano rod, without any template and catalyst in water-heat process, speed is fast, technique
Simply, productivity is high, and with low cost, is suitable for batch production；
(3) direct growth SnO on ZnO2Nanometer rods, prepared nano composite material form is homogeneous,
Cladding is closely.
Accompanying drawing explanation
Fig. 1 is the XRD spectrum of embodiment 1 in the present invention；
Fig. 2 is the XRD spectrum of embodiment 2 in the present invention；
Fig. 3 is the XRD spectrum of embodiment 3 in the present invention；
Fig. 4 is the SEM photograph of embodiment 1 in the present invention；
Fig. 5 is the SEM photograph of embodiment 2 in the present invention；
Fig. 6 is the SEM photograph of embodiment 3 in the present invention；
Fig. 7 is the XRD spectrum of embodiment 4 in the present invention；
Fig. 8 is the SEM photograph of embodiment 4 in the present invention
Below in conjunction with specification drawings and specific embodiments, the present invention is illustrated.
Detailed description of the invention
SnO prepared by the present invention2/ ZnO nano composite, uses simple microwave radiation technology hydro-thermal without template
Method directly grows SnO on ZnO nanorod2Nanometer rods, with ZnO nanorod as trunk structure, SnO2For secondary
The sandwich of level structure.
The present invention mainly uses microwave radiation technology hydro-thermal method, by controlling the concentration of pink salt, alkali salt in reaction system
A kind of SnO is obtained than factors such as, pink salt and zinc salt concentration ratio, reaction temperature, reaction time2/ ZnO receives
Nano composite material and the method preparing this material, without any template or catalyst in water-heat process, speed is fast,
Technique is simple, and productivity is high, and with low cost, is suitable for batch production；ZnO nanorod is straight as trunk structure
Deliver a child long SnO2Nanometer rods, prepared monocrystalline SnO2Nanometer rods form is homogeneous, is evenly coated on ZnO.
In order to make objects and advantages of the present invention clearer, below in conjunction with drawings and Examples to this
Bright it is further elaborated.Should be appreciated that specific embodiment described herein is only in order to explain this
Invention, is not intended to limit the present invention.
Embodiment one:
Step one: the NaOH solution of 1.4mol/L is poured into the Zn (CH of 0.1mol/L3COOH)2·2H2O
In solution (volume ratio is 1:1), obtain precursor solution after being sufficiently stirred for, by 30ml precursor solution
Move into the reactor (volume of liner is 100ml) of TFM liner, be sealed against being placed in the microwave merit of 400W
Under rate, 200 DEG C of insulation 15min, product is centrifuged separating treatment, and uses by question response after terminating
Deionized water is washed repeatedly, until the pH=7 of filtrate, is then placed in by products therefrom in baking oven and dries at 60 DEG C
Dry, obtain ZnO nanorod, a length of 5～10 μm, diameter are about 0.5～1 μm.
Step 2, by the SnCl of 0.05mol/L4·5H2The NaOH that O solution is dropwise added dropwise to 0.3mol/L is molten
In liquid, after having titrated, add the ZnO nanorod continuously stirred of step one preparation of 0.01mol/L
(three's mol ratio is [SnCl to 30min4]: [NaOH]: [ZnO]=5:30:1) obtain precursor solution, take
30ml precursor solution moves into the reactor (volume of liner is 100ml) of TFM liner, is placed on 400W
Microwave power under, in 180 DEG C of baking ovens be incubated 15min, product is centrifuged after terminating by question response
Separate, and be washed with deionized repeatedly, until the pH=7 of filtrate, then products therefrom is placed in baking oven
In dry at 60 DEG C, obtain SnO2/ ZnO nano composite.
This product XRD spectrum as it is shown in figure 1, SEM photograph as shown in Figure 4；Fig. 1 illustrates embodiment one
Product be SnO2/ ZnO compound, Fig. 4 illustrates embodiment one product SnO2The pattern of/ZnO, obtains SnO2
A length of the 250 of nanometer rods～300nm, a diameter of 15～20nm.
Embodiment two:
Step one: identical with embodiment one.
Step 2: by the SnCl of 0.1mol/L4·5H2The NaOH that O solution is dropwise added dropwise to 0.9mol/L is molten
In liquid, (three's mol ratio is to add the ZnO continuously stirred 30min of 0.02mol/L after having titrated
[SnCl4]: [NaOH]: [ZnO]=5:45:1) obtain precursor solution, take 30ml precursor solution and move into
The reactor (volume of liner is 100ml) of TFM liner, is placed under the microwave power of 400W, 200 DEG C
Being incubated 30min in baking oven, product is centrifuged separating after terminating by question response, and is washed with deionized water
Wash repeatedly, until the pH=7 of filtrate, then products therefrom is placed in baking oven and dries at 60 DEG C, just obtain
SnO2/ ZnO nano composite.
The X ray diffracting spectrum of this product as in figure 2 it is shown, electron scanning micrograph as shown in Figure 5；
Fig. 2 illustrates that the product of embodiment two is SnO2/ ZnO compound, Fig. 5 illustrates the product of embodiment two
SnO2/ appearance of ZnO, obtains SnO2A length of the 200 of nanometer rods～300nm, a diameter of 10～20nm.
Embodiment three:
Step one: identical with embodiment one.
Step 2: by the SnCl of 0.3mol/L4·5H2The NaOH that O solution is dropwise added dropwise to 1.8mol/L is molten
In liquid, (three's mol ratio is to add the ZnO continuously stirred 30min of 0.05mol/L after having titrated
[SnCl4]: [NaOH]: [ZnO]=6:36:1) obtain precursor solution, take 30ml precursor solution and move into
The reactor (volume of liner is 100ml) of TFM liner, is placed under the microwave power of 400W, 220 DEG C
Being incubated 60min in baking oven, product is centrifuged separating after terminating by question response, and is washed with deionized water
Wash repeatedly, until the pH=7 of filtrate, then products therefrom is placed in baking oven and dries at 60 DEG C, just obtain
SnO2/ ZnO nano composite.
The X ray diffracting spectrum of this product as it is shown on figure 3, electron scanning micrograph as shown in Figure 6；
Fig. 3 illustrates that the product of embodiment three is SnO2/ ZnO compound, Fig. 6 illustrates the product of embodiment three
SnO2/ appearance of ZnO, SnO2A length of the 300 of nanometer rods～600nm, a diameter of 20～40nm.
Embodiment four: comparative example
Step one: identical with embodiment one.
Step 2: by the SnCl of 0.1mol/L4·5H2The NaOH that O solution is dropwise added dropwise to 0.9mol/L is molten
In liquid, add after having titrated 0.025mol/L ZnO continuously stirred 30min (three's mol ratio is 4:
36:1), by mixed solution, take 30ml precursor solution and move into the reactor (appearance of liner of TFM liner
Amass as 100ml), it is placed under the microwave power of 400W, 160 DEG C of baking ovens are incubated 60min, question response
It is centrifuged product after end separating, and is washed with deionized repeatedly, until the pH=7 of filtrate,
Then products therefrom is placed in baking oven and dries at 60 DEG C.
The X ray diffracting spectrum of this product as it is shown in fig. 7, electron scanning micrograph as shown in Figure 8；
Fig. 7 illustrates that the product of embodiment four is ZnSn (OH)6Compound with ZnO, it is clear that do not have SnO2Generate.
Fig. 8 illustrates the product morphology of embodiment four, and it is octahedral ZnSn (OH)6With bar-shaped ZnO.Obviously,
In present case, SnO2/ ZnO structure can not be formed at 160 DEG C.
In sum, the present invention relates to a kind of SnO2The preparation method of/ZnO nano-structure compound, is adopted
Hydro-thermal preparation process technique simple, speed is fast, and controllability is strong, and productivity is high, with low cost, is suitable for batch
Amount produces.
The above is only the preferred embodiment of the present invention, it is noted that common for the art
For technical staff, under the premise without departing from the principles of the invention, it is also possible to make some improvements and modifications,
These improvements and modifications also should be regarded as protection scope of the present invention.
Claims (9)
1. a SnO2/ ZnO nano composite, it is characterised in that include ZnO nanorod and be grown in
SnO on ZnO nanorod surface2Nanometer rods.
2. SnO as claimed in claim 12/ ZnO nano composite, it is characterised in that include monomer,
Described monomer includes ZnO nanorod and raw at the SnO on ZnO nanorod2Nanometer rods.
3. SnO as claimed in claim 1 or 22/ ZnO nano composite, it is characterised in that described
The draw ratio of ZnO nanorod be 5～20, SnO2The draw ratio of nanometer rods is 5～60.
4. SnO as claimed in claim 1 or 22/ ZnO nano composite, it is characterised in that described
A length of 5～10 μm of ZnO nanorod, a diameter of 0.5～1 μm of ZnO nanorod；Described SnO2
A length of the 200 of nanometer rods～600nm, SnO2A diameter of the 10 of nanometer rods～40nm.
5. preparation SnO described in claim 1,2,3 or 42The method of/ZnO nano composite, its
It is characterised by, prepares ZnO nanorod, then microwave on ZnO nanorod including using microwave radiation technology hydro-thermal method
Assisting alcohol-hydrothermal method growth SnO2Nanometer rods.
Prepare SnO the most as claimed in claim 52The method of/ZnO nano composite, it is characterised in that
Described microwave assisted aqueous extraction hot preparation ZnO nanorod includes: strong base solution joins zinc compound solution
Middle as reaction source, reaction source carries out hydro-thermal reaction under microwave condition, and microwave power is 400W, microwave
Temperature is 200 DEG C, and the microwave time is 15min, is washed by the product of hydro-thermal reaction and i.e. obtains for neutral and drying
Obtain ZnO nanorod.
Prepare SnO the most as claimed in claim 62The method of/ZnO nano composite, it is characterised in that
Described zinc compound solution is Zn (CH3COOH)2Solution, Zn (CH in reaction source3COOH)2Solution
Concentration is 0.1mol/L, and described strong base solution is NaOH solution, the concentration of NaOH solution in reaction source
For 1.4mol/L.
Prepare SnO the most as claimed in claim 52The method of/ZnO nano composite, it is characterised in that
Described uses microwave radiation technology Hydrothermal Growth SnO on ZnO nanorod2Nanometer rods includes: by stanniferousization
Polymer solution joins and obtains growth solution in strong base solution, and ZnO nanorod joins in growth solution
Row microwave hydrothermal react, microwave power is 400W, and microwave temperature is 180～220 DEG C, the microwave time be 15～
60min, the product washing reacted by microwave hydrothermal is neutral and the nano combined material of drying SnO2/ZnO
Material.
Prepare SnO the most as claimed in claim 82The method of/ZnO nano composite, it is characterised in that
Described sn-containing compound solution is SnCl4Solution, described strong base solution is NaOH solution, grows molten
NaOH and SnCl in liquid4Mol ratio be [NaOH]: [SnCl4]=6～10:1, SnCl in microwave hydrothermal reaction4
It is [SnCl with the mol ratio of ZnO4]: [ZnO]=4～7:1.
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Cited By (6)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN106517315A (en) * | 2016-08-17 | 2017-03-22 | 安徽建筑大学 | One-dimensional nanometer complex metal oxide gas-sensitive material and preparation method thereof |
| CN107352575A (en) * | 2017-05-24 | 2017-11-17 | 江苏时瑞电子科技有限公司 | A kind of preparation method of ZnO nanoparticle for gas sensor |
| CN108205004A (en) * | 2016-12-16 | 2018-06-26 | 南京理工大学 | Enzyme-free glucose electrochemical sensing nanocomposite and preparation method thereof |
| CN109694101A (en) * | 2019-02-14 | 2019-04-30 | 西北大学 | A kind of SnO2@ZnO nano composite material and preparation method |
| CN109967075A (en) * | 2019-03-29 | 2019-07-05 | 昆明理工大学 | A kind of ZnO-SnO of doping metals platinum2The preparation method of composite photocatalyst material |
| CN110040766A (en) * | 2019-04-02 | 2019-07-23 | 重庆大学 | The gas-sensitive nano material and gas sensor of high moisture resistance |
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Cited By (10)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN106517315A (en) * | 2016-08-17 | 2017-03-22 | 安徽建筑大学 | One-dimensional nanometer complex metal oxide gas-sensitive material and preparation method thereof |
| CN106517315B (en) * | 2016-08-17 | 2018-01-12 | 安徽建筑大学 | 1-dimention nano composite metal oxide gas-sensing material and preparation method thereof |
| CN108205004A (en) * | 2016-12-16 | 2018-06-26 | 南京理工大学 | Enzyme-free glucose electrochemical sensing nanocomposite and preparation method thereof |
| CN107352575A (en) * | 2017-05-24 | 2017-11-17 | 江苏时瑞电子科技有限公司 | A kind of preparation method of ZnO nanoparticle for gas sensor |
| CN109694101A (en) * | 2019-02-14 | 2019-04-30 | 西北大学 | A kind of SnO2@ZnO nano composite material and preparation method |
| CN109694101B (en) * | 2019-02-14 | 2021-05-28 | 西北大学 | SnO (stannic oxide)2@ ZnO nano composite material and preparation method thereof |
| CN109967075A (en) * | 2019-03-29 | 2019-07-05 | 昆明理工大学 | A kind of ZnO-SnO of doping metals platinum2The preparation method of composite photocatalyst material |
| CN109967075B (en) * | 2019-03-29 | 2021-12-03 | 昆明理工大学 | ZnO-SnO doped with metal platinum2Preparation method of composite photocatalytic material |
| CN110040766A (en) * | 2019-04-02 | 2019-07-23 | 重庆大学 | The gas-sensitive nano material and gas sensor of high moisture resistance |
| CN110040766B (en) * | 2019-04-02 | 2021-09-03 | 重庆大学 | Preparation method of high-humidity-resistance nano gas-sensitive material and gas-sensitive sensor |
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