CN105236472A - Preparation method of SnO2 nano-wire array - Google Patents
Preparation method of SnO2 nano-wire array Download PDFInfo
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- CN105236472A CN105236472A CN201510641241.9A CN201510641241A CN105236472A CN 105236472 A CN105236472 A CN 105236472A CN 201510641241 A CN201510641241 A CN 201510641241A CN 105236472 A CN105236472 A CN 105236472A
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Abstract
The invention discloses a preparation method of a SnO2 nano-wire array. The method is characterized in that the SnO2 nano-wire array grows on ITO glass used as a substrate through a hydrothermal process, the length-to-diameter ratio of SnO2 nano-wires in the SnO2 nano-wire array is 4-12, the diameter of the SnO2 nano-wires in the SnO2 nano-wire array is 50-100nm, and the length of the SnO2 nano-wires is 400-600nm. The structure of the SnO2 nano-wire array obtained in the invention is formed by SnO2 mono-crystalline nano-rods with a rutile structure, the microstructure of the SnO2 nano-wire array has compact arrangement and good homogeneity, and can be used as a field emission, photocatalysis, gas-sensitive sensor and lithium ion battery negative material.
Description
Technical field
The invention belongs to field of nanometer material technology, relate to a kind of SnO
2the preparation method of nano-wire array.
Background technology
In recent years, the New Sci-and Tech-Revolution centered by nanometer new science and technology has become the leading of 21 century.Nano material is the subscience that nanosecond science and technology field is dynamic, Research connotation is very abundant, and development nano material is the needs of modern high technology development.Under the requirement of new historical background, the developing direction of electron device is miniaturization, microminiaturization, intellectuality and high integration, and this just has higher requirement to the material manufacturing device, also just makes the size of various material all start to develop towards nano level.
SnO
2belong to rutile crystalline structure, it is a kind of natural direct N-shaped semiconductor material with wide forbidden band, there is following features: there is broad-band gap (Eg=3.6eV) and high exciton bind energy (130meV), (2) SnO under (1) room temperature
2high temperature resistant and radiation, chemical property is stable especially, (3) low cost.SnO
2nano wire small volume, specific surface area are comparatively large, and the structures and characteristics of its uniqueness makes SnO
2there is the advantage of its uniqueness and broad application potential, especially SnO at semiconducter device and field of functional materials
2nano-wire array shows wide application prospect in the negative material of opto-electronic device, gas sensor, Flied emission, information storage, catalyzer, lithium ion battery, absorption of electromagnetic wave etc.At present, a large amount of research workers has been had to be devoted to study SnO
2nanowire array structure also obtains relevant achievement, as Chinese patent CN200810201924.2 discloses a kind of SnO for lithium ion battery
2the preparation method of nano line array electrode, this material has good practical value and application prospect in field of lithium ion battery.Although form array structure, its preparation process is loaded down with trivial details, needs first to utilize magnetron sputtering method to prepare noble metal Au as catalyzer, then in tube furnace with gas-liquid-solid (VLS) mechanism at grown above silicon SnO
2nano-wire array, containing the disagreeableness sulphur powder of environment simultaneously in the reaction starting material adopted.
Summary of the invention
For existing preparation SnO
2the technical defect of nano-wire array and deficiency, the invention provides one without template directly at ITO Grown SnO
2the method of nanowire array structure, solves the loaded down with trivial details and problem of environmental pollution of Chinese patent CN200810201924.2 preparation process.
The technical scheme that the present invention takes is:
A kind of SnO
2the preparation method of nano-wire array, comprising with ito glass is substrate, adopts hydrothermal method to carry out SnO
2nanowire array growth.
Concrete, described SnO
2snO in nano-wire array
2the length-to-diameter ratio of nano wire is 4 ~ 12.
More specifically, described SnO
2snO in nano-wire array
2the diameter of nano wire is 50 ~ 100nm, SnO
2the length of nano wire is 400 ~ 600nm.
In addition, described hydrothermal method carries out SnO
2nanowire array growth comprises: joined by highly basic as reaction source in sn-containing compound solution, carries out hydrothermal growth after ito glass substrate is immersed reaction source at 140 ~ 200 DEG C, and the product washing after growth is dried for neutral and obtain SnO
2nano-wire array.
Further, at 140 ~ 200 DEG C, be incubated 8 ~ 32h after ito glass substrate being immersed reaction source carry out hydrothermal growth.
Further, described sn-containing compound is SnCl
4, SnCl in reaction source
4concentration be 0.02 ~ 0.05mol/L, described highly basic is NaOH, NaOH and SnCl in reaction source
4molar concentration rate be [NaOH]: [SnCl
4]=8 ~ 11:1.
Advantage of the present invention is:
(1) SnO that obtains of the present invention
2nano-wire array is the monocrystalline SnO at ito glass substrate Epitaxial growth
2nano-wire array, its diameter is 50 ~ 100nm, and its length is 400nm ~ 600nm, and length-to-diameter ratio is 4 ~ 12.From microtexture, SnO
2nano-wire array arrangement is fine and close, and homogeneity is good, can be used as Flied emission, photochemical catalysis, gas sensor and lithium ion battery negative material;
(2) the present invention adopts hydrothermal method to prepare SnO
2nano-wire array, without the need to any template and catalyzer in water-heat process, technique is simple, pollution-free, and with low cost, is applicable to batch production;
(3) ito glass is as substrate, direct growth SnO
2nano-wire array, prepared monocrystalline SnO
2nano wire form is homogeneous, homoepitaxial on ito glass substrate.
Accompanying drawing explanation
Fig. 1 is scanning electronic microscope (SEM) photo of the experimental product taking copper sheet as substrate;
Fig. 2 is take copper sheet as substrate, and on the surface of copper sheet substrate first magnetron sputtering one deck SnO
2the SEM photo of the experimental product of film;
Fig. 3 is X-ray diffraction (XRD) collection of illustrative plates of embodiment 1 in the present invention;
Fig. 4 is the XRD figure spectrum of embodiment 2 in the present invention;
Fig. 5 is the XRD figure spectrum of embodiment 3 in the present invention;
Fig. 6 is scanning electronic microscope (SEM) photo of embodiment 1;
Fig. 7 is the SEM photo of embodiment 2;
Fig. 8 is the SEM photo of embodiment 3;
Fig. 9 is a kind of SnO of the present invention
2snO in nanowire array structure
2the typical selected area electron diffraction photo of nano wire.
Below in conjunction with specification drawings and specific embodiments, the present invention is illustrated.
Embodiment
SnO prepared by the present invention
2nanowire array structure is substrate with ito glass, adopts simple hydrothermal method directly on ITO, to prepare SnO without template
2nano-wire array, reaction starting material environmental friendliness, and whole preparation process is carried out in confined conditions.
SnO prepared by the present invention
2nano-wire array take ITO as substrate, direct growth monocrystalline SnO
2nano-wire array, fine and close, homogeneous SnO
2monocrystal nanowire grows along ITO substrate epitaxial.
The present invention mainly adopts hydrothermal method, obtains a kind of SnO by the factor such as concentration, alkali salt ratio, temperature of reaction, reaction times controlling pink salt in reaction system
2the method of nano-wire array, without the need to any template and catalyzer in water-heat process, technique is simple, pollution-free, and with low cost, is applicable to batch production; Ito glass as substrate, direct growth SnO
2nano-wire array, prepared monocrystalline SnO
2nano wire form is homogeneous, homoepitaxial on ito glass substrate.
Fig. 9 is product S nO of the present invention
2snO in nano-wire array
2the selected area electron diffraction photo of nano wire, the diffraction spot on photo discloses this SnO
2nano wire is monocrystalline.
Simple hydrothermal method is adopted directly on ITO, to prepare SnO without template for probing into
2the root of nano-wire array, based on the technical scheme that the present invention takes, contriver attempts to be that substrate is to prepare SnO with copper sheet
2nano-wire array, result all ends in failure.Particularly, based on the processing parameter in the technical scheme that the present invention takes and processing condition, it is desirable to adopt simple hydrothermal method directly on copper sheet, preparing SnO without template
2nano-wire array, the SEM photo of products therefrom as shown in Figure 1, does not see array structure from this picture.But, first magnetron sputtering one deck SnO in copper substrate
2film, and then processing parameter in the technical scheme taked based on the present invention and processing condition, the SEM photo of products therefrom as shown in Figure 2, obviously has array structure to produce, and its XRD figure spectrum (see Fig. 2) shows that products therefrom is SnO
2array, contrasts these two experimental results and shows, SnO
2nano-wire array can generate, and first should have SnO
2seed Layer, but SnO
2the different SnO that the later stage can be caused to grow on the seed layer of forming feature of Seed Layer
2the structure of nano-wire array is different;
Usually, its chemical composition of ito glass market bought is Sn doping In
2o
3, SnO
2with In
2o
3mol ratio be 1:9; Experimental studies have found that through contriver, the preparation technology of ito glass determines SnO
2necessarily equally distributed in ITO, these equally distributed SnO
2become growth unit Sn (OH)
6 2-activity to cast anchor position, based on the SnO of the technical scheme that the present invention takes
2sub-crystalline substance just defines on these activity cast anchor position, and this little crystalline substance has become SnO
2the Seed Layer that nano-wire array is formed.Under processing parameter in the technical scheme that the present invention takes and processing condition, SnO
2the brilliant preferred orientation growth of son, thus define SnO
2nano-wire array.
Due to magnetron sputtering SnO on copper sheet
2on ITO substrate, SnO is formed under Seed Layer and hydrothermal condition
2seed Layer is two kinds of different preparation methods after all, and processing condition have very large difference naturally, such two kinds of SnO
2seed Layer crystalline state separately, sub brilliant size are inevitable different, which results in the SnO that on two kinds of substrates prepared by hydro-thermal
2structural form have larger difference.
The ito glass buying producer that this experiment adopts is China Electronic Technology Group Corporation No.33 Research Institute;
In order to make objects and advantages of the present invention clearly understand, below in conjunction with drawings and Examples, the present invention is further elaborated.Should be appreciated that specific embodiment described herein only in order to explain the present invention, be not intended to limit the present invention.
Embodiment one
Get the ito glass (note: ito glass size suitably regulates according to teflon-lined volume) of 1cm × 1cm, put into acetone and tetracol phenixin mixing solutions ultrasonic cleaning 30min that volume ratio is 1:1, clean complete ito glass deionized water repeatedly to rinse, be kept in dehydrated alcohol with dehydrated alcohol rinse, and then lie against bottom teflon-lined reactor after ito glass is dried.Then, the NaOH solution of 0.16mol/L is dropwise added dropwise to 0.02mol/LSnCl
45H
2in O solution, precursor solution is obtained after abundant stirring, take out 35ml precursor solution to move into bottom and have in the teflon-lined reactor of ito glass (volume of liner is 50ml), sealed and be placed in 140 DEG C of baking ovens and be incubated 8h and just obtain SnO
2nano-wire array.As shown in Figure 3, electron scanning micrograph as shown in Figure 6 for the X ray diffracting spectrum of this product.
Fig. 3 illustrates that the product of embodiment one is SnO
2, Fig. 6 illustrates that the product of embodiment one is SnO
2nanowire array structure.
Embodiment two
Get the ito glass of 1cm × 1cm, put into acetone and tetracol phenixin mixing solutions ultrasonic cleaning 30min that volume ratio is 1:1, clean complete ito glass deionized water repeatedly to rinse, be kept in dehydrated alcohol with dehydrated alcohol rinse, and then lie against bottom teflon-lined reactor after ito glass is dried.Then, by the NaOH solution of 0.3mol/L by being added dropwise to 0.03mol/LSnCl
45H
2in O solution, precursor solution is obtained after abundant stirring, take out 35ml precursor solution to move into bottom and have in the teflon-lined reactor of ito glass (volume of liner is 50ml), sealed and be placed in 180 DEG C of baking ovens and be incubated 24h and just obtain SnO
2nano-wire array.As shown in Figure 4, electron scanning micrograph as shown in Figure 7 for the X ray diffracting spectrum of this product.
Fig. 4 illustrates that the product of embodiment two is SnO
2, Fig. 7 illustrates that the product of embodiment two is SnO
2nanowire array structure.
Embodiment three
Get the ito glass of 1cm × 1cm, put into acetone and tetracol phenixin mixing solutions ultrasonic cleaning 30min that volume ratio is 1:1, clean complete ito glass deionized water repeatedly to rinse, be kept in dehydrated alcohol with dehydrated alcohol rinse, and then lie against bottom teflon-lined reactor after ito glass is dried.Then, by the NaOH solution of 0.55mol/L by being added dropwise to 0.05mol/LSnCl
45H
2in O solution, precursor solution is obtained after abundant stirring, take out 35ml precursor solution to move into bottom and have in the teflon-lined reactor of ito glass (volume of liner is 50ml), sealed and be placed in 200 DEG C of baking ovens and be incubated 32h and just obtain SnO
2nano-wire array.As shown in Figure 5, electron scanning micrograph as shown in Figure 8 for the X ray diffracting spectrum of this product.
Fig. 5 illustrates that the product of embodiment three is SnO
2, Fig. 8 illustrates that the product of embodiment three is SnO
2nanowire array structure.
In sum, the present invention relates to a kind of SnO
2nano-wire array and hydrothermal preparing process thereof, the hydro-thermal preparation process technique adopted is simple, and controllability is strong, pollution-free, with low cost, is applicable to batch production.
The above is only the preferred embodiment of the present invention; it should be pointed out that for those skilled in the art, under the premise without departing from the principles of the invention; can also make some improvements and modifications, these improvements and modifications also should be considered as protection scope of the present invention.
Claims (6)
1. a SnO
2the preparation method of nano-wire array, is characterized in that, comprising with ito glass is substrate, adopts hydrothermal method to carry out SnO
2nanowire array growth.
2. SnO as claimed in claim 1
2the preparation method of nano-wire array, is characterized in that, described SnO
2snO in nano-wire array
2the length-to-diameter ratio of nano wire is 4 ~ 12.
3. SnO as claimed in claim 1 or 2
2the preparation method of nano-wire array, is characterized in that, described SnO
2snO in nano-wire array
2the diameter of nano wire is 50 ~ 100nm, SnO
2the length of nano wire is 400 ~ 600nm.
4. SnO as claimed in claim 1 or 2
2the preparation method of nano-wire array, is characterized in that, described hydrothermal method carries out SnO
2nanowire array growth comprises: joined by highly basic as reaction source in sn-containing compound solution, carries out hydrothermal growth after ito glass substrate is immersed reaction source at 140 ~ 200 DEG C, and the product washing after growth is dried for neutral and obtain SnO
2nano-wire array.
5. SnO as claimed in claim 4
2the preparation method of nano-wire array, is characterized in that, is incubated 8 ~ 32h and carries out hydrothermal growth after ito glass substrate is immersed reaction source at 140 ~ 200 DEG C.
6. SnO as claimed in claim 4
2the preparation method of nano-wire array, is characterized in that, described sn-containing compound is SnCl
4, SnCl in reaction source
4concentration be 0.02 ~ 0.05mol/L, described highly basic is NaOH, NaOH and SnCl in reaction source
4molar concentration rate be [NaOH]: [SnCl
4]=8 ~ 11:1.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201510641241.9A CN105236472A (en) | 2015-09-30 | 2015-09-30 | Preparation method of SnO2 nano-wire array |
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| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201510641241.9A CN105236472A (en) | 2015-09-30 | 2015-09-30 | Preparation method of SnO2 nano-wire array |
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|---|---|
| CN105236472A true CN105236472A (en) | 2016-01-13 |
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Cited By (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN105948105A (en) * | 2016-05-06 | 2016-09-21 | 西北大学 | SnO2/ZnO nano composite material and preparation method thereof |
| CN110117027A (en) * | 2019-05-28 | 2019-08-13 | 北华航天工业学院 | A kind of SnO2Nanometer rods and preparation method thereof |
| CN111116232A (en) * | 2019-12-13 | 2020-05-08 | 苏州麦茂思传感技术有限公司 | Synthesis method of formaldehyde gas sensor sensitive material |
| CN114583118A (en) * | 2020-11-30 | 2022-06-03 | 松山湖材料实验室 | Carbon-coated tin nanowire array cathode material and preparation method and application thereof |
-
2015
- 2015-09-30 CN CN201510641241.9A patent/CN105236472A/en active Pending
Non-Patent Citations (1)
| Title |
|---|
| 杨伟光 等: "SnO2 纳米柱状阵列的微波水热法合成及表征", 《铜业工程》 * |
Cited By (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN105948105A (en) * | 2016-05-06 | 2016-09-21 | 西北大学 | SnO2/ZnO nano composite material and preparation method thereof |
| CN110117027A (en) * | 2019-05-28 | 2019-08-13 | 北华航天工业学院 | A kind of SnO2Nanometer rods and preparation method thereof |
| CN110117027B (en) * | 2019-05-28 | 2021-08-24 | 北华航天工业学院 | SnO (stannic oxide)2Nano-rod and preparation method thereof |
| CN111116232A (en) * | 2019-12-13 | 2020-05-08 | 苏州麦茂思传感技术有限公司 | Synthesis method of formaldehyde gas sensor sensitive material |
| CN114583118A (en) * | 2020-11-30 | 2022-06-03 | 松山湖材料实验室 | Carbon-coated tin nanowire array cathode material and preparation method and application thereof |
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