CN108545960A - A kind of Y doping zinc oxide nanometers stick array preparation method - Google Patents
A kind of Y doping zinc oxide nanometers stick array preparation method Download PDFInfo
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- C03C17/00—Surface treatment of glass, not in the form of fibres or filaments, by coating
- C03C17/34—Surface treatment of glass, not in the form of fibres or filaments, by coating with at least two coatings having different compositions
- C03C17/3411—Surface treatment of glass, not in the form of fibres or filaments, by coating with at least two coatings having different compositions with at least two coatings of inorganic materials
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- C03C2217/00—Coatings on glass
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- C03C2217/21—Oxides
- C03C2217/211—SnO2
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- C03C—CHEMICAL COMPOSITION OF GLASSES, GLAZES OR VITREOUS ENAMELS; SURFACE TREATMENT OF GLASS; SURFACE TREATMENT OF FIBRES OR FILAMENTS MADE FROM GLASS, MINERALS OR SLAGS; JOINING GLASS TO GLASS OR OTHER MATERIALS
- C03C2217/00—Coatings on glass
- C03C2217/20—Materials for coating a single layer on glass
- C03C2217/21—Oxides
- C03C2217/216—ZnO
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- C03—GLASS; MINERAL OR SLAG WOOL
- C03C—CHEMICAL COMPOSITION OF GLASSES, GLAZES OR VITREOUS ENAMELS; SURFACE TREATMENT OF GLASS; SURFACE TREATMENT OF FIBRES OR FILAMENTS MADE FROM GLASS, MINERALS OR SLAGS; JOINING GLASS TO GLASS OR OTHER MATERIALS
- C03C2217/00—Coatings on glass
- C03C2217/20—Materials for coating a single layer on glass
- C03C2217/21—Oxides
- C03C2217/24—Doped oxides
- C03C2217/241—Doped oxides with halides
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- C03C2217/00—Coatings on glass
- C03C2217/20—Materials for coating a single layer on glass
- C03C2217/21—Oxides
- C03C2217/24—Doped oxides
- C03C2217/242—Doped oxides with rare earth metals
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- C—CHEMISTRY; METALLURGY
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- C03C—CHEMICAL COMPOSITION OF GLASSES, GLAZES OR VITREOUS ENAMELS; SURFACE TREATMENT OF GLASS; SURFACE TREATMENT OF FIBRES OR FILAMENTS MADE FROM GLASS, MINERALS OR SLAGS; JOINING GLASS TO GLASS OR OTHER MATERIALS
- C03C2217/00—Coatings on glass
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- C03C2218/00—Methods for coating glass
- C03C2218/10—Deposition methods
- C03C2218/11—Deposition methods from solutions or suspensions
- C03C2218/111—Deposition methods from solutions or suspensions by dipping, immersion
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- C03C2218/00—Methods for coating glass
- C03C2218/30—Aspects of methods for coating glass not covered above
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Abstract
The invention discloses a kind of preparation methods of Y doping zinc oxide nanometers stick array.Zinc acetate is dissolved in absolute ethyl alcohol, monoethanolamine is added and as stabilizer and stirs, ZnO film is plated on FTO electro-conductive glass using dip-coating method, then annealing obtains ZnO seed layers；Zinc nitrate and hexamethylenetetramine are dissolved in deionized water and are stirred, the rear yttrium nitrate that is added obtains growth solution；The above-mentioned FTO electro-conductive glass for having plated ZnO seed layers is placed in growth solution and carries out hydrothermal growth, taking-up, which is placed in ethanol solution, after the completion of growth is ultrasonically treated and is dried up, and finally annealing obtains the Y doping zinc oxide nanometer stick arrays.Present invention light absorption in UV, visible light optical range is improved, and greatly improve quantum dot sensitized ZnO solar battery light anodes catches light efficiency.Raw material sources are wide, and reaction condition is mild, easily controllable, environmental-friendly without adding activating agent, are conducive to marketization application and promote.
Description
Technical field
The present invention relates to semiconductor nano material preparing technical fields, and in particular to a kind of Y doping zinc oxide nanometers stick array
Preparation method.
Background technology
ZnO is direct band-gap semicondictor material, and band gap at room temperature 3.37eV, exciton bind energy 60meV have good
Chemical stability and thermal stability, have in the fields such as ultraviolet detector, solar cell, pressure-sensitive nano ceramics extensive
Using.Especially Low-Dimensional ZnO Nanomaterials not only have big specific surface area, and have small-size effect and quantum size
Effect.Therefore, Low-Dimensional ZnO Nanomaterials also have unique electricity, optics and change other than the excellent specific property with body material
Learn property.The ZnO nano-rod array of ordered arrangement is widely used in the light anode of quantum dot sensitized solar cell, mainly
The reason is as follows that some：
1) electron mobility of ZnO is about 205~1000cm2·V-1·s-1, compare TiO2(0.1~4cm2·V-1·s-1)
High 2~3 orders of magnitude, are conducive to the transmission of light induced electron；
2) ZnO has higher conduction band bottom current potential, advantageously reduces Carrier recombination and forms larger open-circuit voltage；
3) ZnO nano-rod array can enhance the scattering of incident sunlight, improve the capture rate of photon；
4) the direct transmission channel for providing light induced electron, is effectively shortened the transmission path of electronics.
However pure ZnO nano material only has absorption as optoelectronic pole material to ultraviolet light, limits it to the effective of sunlight
It utilizes.
Invention content
There are problems that only thering is light absorption, the present invention to provide a kind of Y doping zinc oxide nanometers stick array to ultraviolet for pure ZnO
Preparation method, prepared Y doping zinc oxide nanometer stick arrays light absorption in UV-visible range is improved, greatly carries
High quantum dot sensitized ZnO solar battery light anodes catch light efficiency.The raw material sources that this method uses are wide, reaction condition temperature
With it is easily controllable, it is environmental-friendly without adding activating agent, be conducive to the marketization application and promote.
In order to achieve the above objectives, as follows using technical solution：
A kind of Y doping zinc oxide nanometers stick array preparation method, includes the following steps：
1) prepared by ZnO seed layers
Zinc acetate is dissolved in absolute ethyl alcohol, monoethanolamine is added and as stabilizer and stirs, using dip-coating method
ZnO film is plated on FTO electro-conductive glass, then annealing obtains ZnO seed layers；
2) configuration of Y growth solutions is mixed
Zinc nitrate and hexamethylenetetramine are dissolved in deionized water and are stirred, the rear yttrium nitrate that is added obtains growth solution；
3) preparation of Y doping zinc oxide nanometers stick array
The above-mentioned FTO electro-conductive glass for having plated ZnO seed layers is placed in growth solution and carries out hydrothermal growth, after the completion of growth
Taking-up, which is placed in ethanol solution, to be ultrasonically treated and is dried up, and finally annealing obtains the Y doping zinc oxide nanometer stick battle arrays
Row.
By said program, monoethanolamine and the molar ratio of zinc acetate are 1 in step 1:1, Zn2+Molar concentration is 0.5mol/
L。
By said program, the dip time of dip-coating method is 4~6min in step 1, and pull rate is 60~70mm/
min。
By said program, annealing specimen temperature is 300~400 DEG C in step 1, and the time is 2~3h.
By said program, the molar ratio of zinc nitrate and hexamethylenetetramine is 1 in step 2 growth solution:1, zinc nitrate
Molar concentration is 0.03~0.07mol/L, and the molar concentration that yttrium nitrate is added is 0.01~0.1mol/L.
By said program, 45 ° of inclinations are placed in growth to the conducting surface (ZnO crystal seeds level) of FTO electro-conductive glass downward in step 3
In solution.
By said program, step 3 hydrothermal growth temperature is 95~100 DEG C, and growth time is 4.5~5.5h.
By said program, step 3 ultrasonic power is 80~100W, and sonication treatment time is 3~5s.
By said program, step 3 sample annealing temperature is 350~450 DEG C, and the time is 2~3h.
Effect of the invention is that：
Using the Y doping zinc oxide nanometer stick arrays of Hydrothermal Growth, in nanometer stick array growth course, Y3+Ion adds
Enter so that cation concn increases, causes to be nucleated during crystallization nucleation more dense, the nanometer rods of growth are also more dense.Y3+It mixes
It is miscellaneous to enter in ZnO lattices, due to Y3+Radius be more than Zn2+There is intensive hole so that nanometer rods in nanometer rods in radius
Specific surface area increases, and improves quantum dot deposition on ZnO nanorod, light absorption is carried in UV-visible range
The light induced electron of height, generation increases, and the photoelectric conversion efficiency of quantum dot sensitized solar cell can be improved.Experimental provision is simply easy
Operation, does not need surfactant, environmentally safe, and manufacturing cost is low, and reaction condition is controllable.
Description of the drawings
Fig. 1：The X-ray diffractogram of 1 products therefrom of comparative example 1 and embodiment；
Fig. 2：The x-ray photoelectron spectroscopy figure of Y doping zinc oxide nanometer stick arrays prepared by embodiment 1；
Fig. 3：The scanning electron microscope (SEM) photograph of undoped ZnO nano-rod array prepared by comparative example 1；
Fig. 4：The scanning electron microscope (SEM) photograph of the ZnO nano-rod array of Y doping prepared by embodiment 1；
Fig. 5：The uv-visible absorption spectroscopy figure of 1 products therefrom of comparative example 1 and embodiment；
Specific implementation mode
Following embodiment further illustrates technical scheme of the present invention, but not as limiting the scope of the invention.
Comparative example 1
A kind of preparation method of the ZnO nanorod of undoped Y, is as follows：
(1) ZnO seed layers are prepared：It weighs 10.95g acetic acid dihydrate zinc and is dissolved in magnetic agitation in 100mL absolute ethyl alcohols
0.5h, be added dropwise 3mL monoethanolamine stirring until solution clarify completely, ZnO precursor sol is obtained, by FTO electro-conductive glass
It is placed in Best-Effort request in ZnO precursor sol, obtained sample is transferred to 350 in Muffle furnace by pull rate 60mm/min
DEG C heat treatment 2h, obtain ZnO seed layers.
(2) growth solution of ZnO nanorod is prepared：Weigh the zinc nitrate hexahydrate of 1.485g and six methines four of 0.7g
Amine is dissolved separately in 50mL deionized waters, and magnetic agitation is mixed stirring after being completely dissolved, and obtains ZnO growth solutions.
(3) Y doping zinc oxide nanometer stick arrays are prepared：Growth solution obtained is poured into polytetrafluoroethyllining lining, is coated with
45 ° of the FTO electro-conductive glass of ZnO seed layers is downwardly inclined and is placed in growth solution (ZnO seed layers this down), and liner is shifted
To reaction kettle, is taken out after 95 DEG C of reaction 5h to room temperature, substrate of glass is put into ultrasound 5s in absolute ethyl alcohol, it is anti-with deionized water
The bulky grain of sample surfaces is washed out and is dried up by multiple rinse, and obtained sample is transferred to 400 DEG C of heat treatment 2h in Muffle furnace,
Y doping zinc oxide nanometer stick arrays are obtained in FTO Conducting Glass.
Embodiment 1
1.149g is added after zinc nitrate hexahydrate and hexamethylenetetramine are mixed evenly in 1 step 2 of comparative example
Six nitric hydrate yttriums stir to clarify, and obtain the ZnO growth solutions of Y doping, other steps prepared by Y doping zinc oxide nanometer stick arrays
Suddenly it is prepared with the ZnO nanorod undoped with Y identical.
Fig. 1 is the X ray diffracting spectrum (1# of prepared doped and undoped ZnO nanorod：It is undoped；2#：Y mixes
It is miscellaneous).From the comparative example 1 of Fig. 1 and the XRD spectrum of embodiment 1 it is found that all diffraction maximums have typical hexagonal wurtzite knot
Structure.(002) peak intensity bigger of Y doping zinc oxide nanometers stick array more sharp (see 2# in Fig. 1) and do not find Y's in embodiment 1
Mutually and impurity diffraction maximum, show its be along c-axis preferential growth and crystallinity it is more preferable, Y3+Ion is combined into the position of zinc.
X-ray photoelectron spectroscopy figure (XPS) (see Fig. 2) is the figure of the Y doping zinc oxide nanometer stick arrays prepared by embodiment 1
Spectrum.Wherein show that the XPS peak values of Y doping zinc oxide nanometer stick array samples are located at combination energy of the peak corresponding to Y3d of 161.88eV,
Which demonstrate the Y presence in ZnO nanorod.
Scanning electron microscope (SEM) figure (see Fig. 3 and Fig. 4) is the result shows that ZnO nano-rod array prepared by the two is each perpendicular to serve as a contrast
Bottom direction is grown, and is matched with XRD analysis result, it can be seen that pure ZnO nano-rod array average length is 1.88 μm (Fig. 3), Y
Doping zinc oxide nanometer stick average length is 2.6 μm and growth is more dense, and multiple hole structure (Fig. 4) occur in nanometer rods, illustrates that Y is adulterated
Into in ZnO nanorod.
Uv-visible absorption spectroscopy figure (1#：It is undoped；2#：Y is adulterated) (see Fig. 5).The result shows that synthesized Y mixes
The miscellaneous purer ZnO nano-rod array of ZnO nano-rod array has better optical absorption in ultraviolet-visible light region.
Embodiment 2
A kind of preparation method of Y doping zinc oxide nanometers stick array, steps are as follows：
(1) ZnO seed layers are prepared：It weighs 10.95g acetic acid dihydrate zinc and is dissolved in magnetic agitation in 100mL absolute ethyl alcohols
0.5h is added dropwise the stirring of 3mL monoethanolamine and obtains ZnO precursor sol until solution is clarified completely, FTO electro-conductive glass is set
Obtained sample is transferred to 350 ° of heat in Muffle furnace by the Best-Effort request in ZnO precursor sol, pull rate 60mm/min
Handle to obtain 2h to ZnO seed layers.
(2) growth solution of Y doping zinc oxide nanometer sticks is prepared：Weigh 1.485g zinc nitrate hexahydrate and six times of 0.7g
Tetramine is dissolved separately in 50mL deionized waters, and magnetic agitation is mixed after being completely dissolved stirs 0.5h, is added
Six nitric hydrate yttriums of 1.915g stir to clarify, and obtain the ZnO growth solutions containing Y.
(3) Y doping zinc oxide nanometer stick arrays are prepared：Growth solution obtained is poured into polytetrafluoroethyllining lining, is coated with
45 ° of inclinations of FTO electro-conductive glass of ZnO seed layers are placed in growth solution (ZnO seed layers this down), and liner is transferred to instead
It answers in kettle, is taken out after 95 DEG C of reaction 5h to room temperature, substrate of glass is put into ultrasound 5s in absolute ethyl alcohol, is rushed repeatedly with deionized water
It washes and the bulky grain of sample surfaces is washed out and dried up, obtained sample is transferred to 400 DEG C of heat treatment 2h in Muffle furnace, is led in FTO
Y doping zinc oxide nanometer stick arrays are obtained in electric glass substrate.
Embodiment 3
A kind of preparation method of Y doping zinc oxide nanometers stick array, steps are as follows：
(1) ZnO seed layers are prepared：It weighs 10.95g acetic acid dihydrate zinc and is dissolved in magnetic agitation in 100mL absolute ethyl alcohols
0.5h is added dropwise the stirring of 3mL monoethanolamine and obtains ZnO precursor sol until solution is clarified completely, FTO electro-conductive glass is set
Obtained sample is transferred to 350 ° of heat in Muffle furnace by the Best-Effort request in ZnO precursor sol, pull rate 60mm/min
Handle to obtain 2h to ZnO seed layers.
(2) growth solution of Y doping zinc oxide nanometer sticks is prepared：Weigh 1.485g zinc nitrate hexahydrate and six times of 0.7g
Tetramine is dissolved separately in 50mL deionized waters, and magnetic agitation is mixed after being completely dissolved stirs 0.5h, is added
Six nitric hydrate yttriums of 2.681g stir to clarify, and obtain the ZnO growth solutions containing Y.
(3) Y doping zinc oxide nanometer stick arrays are prepared：Growth solution obtained is poured into polytetrafluoroethyllining lining, is coated with
45 ° of inclinations of FTO electro-conductive glass of ZnO seed layers are placed in growth solution (ZnO seed layers this down), and liner is transferred to instead
It answers in kettle, is taken out after 95 DEG C of reaction 5h to room temperature, substrate of glass is put into ultrasound 5s in absolute ethyl alcohol, is rushed repeatedly with deionized water
It washes and the bulky grain of sample surfaces is washed out and dried up, obtained sample is transferred to 400 DEG C of heat treatment 2h in Muffle furnace, is led in FTO
Y doping zinc oxide nanometer stick arrays are obtained in electric glass substrate.
Claims (9)
1. a kind of Y doping zinc oxide nanometers stick array preparation method, it is characterised in that include the following steps：
1) prepared by ZnO seed layers
Zinc acetate is dissolved in absolute ethyl alcohol, monoethanolamine is added and as stabilizer and stirs, using dip-coating method in FTO
ZnO film is plated on electro-conductive glass, then annealing obtains ZnO seed layers；
2) configuration of Y growth solutions is mixed
Zinc nitrate and hexamethylenetetramine are dissolved in deionized water and are stirred, the rear yttrium nitrate that is added obtains growth solution；
3) preparation of Y doping zinc oxide nanometers stick array
The above-mentioned FTO electro-conductive glass for having plated ZnO seed layers is placed in growth solution and carries out hydrothermal growth, is taken out after the completion of growth
It is placed in ethanol solution and is ultrasonically treated and is dried up, finally annealing obtains the Y doping zinc oxide nanometer stick arrays.
2. Y doping zinc oxide nanometers stick array preparation method as described in claim 1, it is characterised in that monoethanolamine and second in step 1
The molar ratio of sour zinc is 1:1, Zn2+Molar concentration is 0.5mol/L.
3. Y doping zinc oxide nanometers stick array preparation method as described in claim 1, it is characterised in that dip-coating method in step 1
Dip time is 4~6min, and pull rate is 60~70mm/min.
4. Y doping zinc oxide nanometers stick array preparation method as described in claim 1, it is characterised in that annealing specimen temperature in step 1
It it is 300~400 DEG C, the time is 2~3h.
5. Y doping zinc oxide nanometers stick array preparation method as described in claim 1, it is characterised in that nitric acid in step 2 growth solution
The molar ratio of zinc and hexamethylenetetramine is 1:1, the molar concentration of zinc nitrate is 0.03~0.07mol/L, and yttrium nitrate is added
Molar concentration is 0.01~0.1mol/L.
6. Y doping zinc oxide nanometers stick array preparation method as described in claim 1, it is characterised in that FTO electro-conductive glass in step 3
Conducting surface (ZnO crystal seeds level) 45 ° of inclinations are placed in growth solution downward.
7. Y doping zinc oxide nanometers stick array preparation method as described in claim 1, it is characterised in that step 3 hydrothermal growth temperature is
95~100 DEG C, growth time is 4.5~5.5h.
8. Y doping zinc oxide nanometers stick array preparation method as described in claim 1, it is characterised in that step 3 ultrasonic power be 80~
100W, sonication treatment time are 3~5s.
9. Y doping zinc oxide nanometers stick array preparation method as described in claim 1, it is characterised in that step 3 sample annealing temperature is
350~450 DEG C, the time is 2~3h.
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Cited By (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN113517403A (en) * | 2021-07-26 | 2021-10-19 | 南京信息工程大学滨江学院 | Novel organic PN heterojunction liquid phase growth method |
| CN113999475A (en) * | 2021-12-03 | 2022-02-01 | 苏州鼎奕通材料科技有限公司 | Sunlight-resistant anti-UV material and preparation method thereof |
| CN114163138A (en) * | 2021-12-16 | 2022-03-11 | 南京工程学院 | Preparation method of spectrum conversion nanorod array |
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Cited By (6)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN113517403A (en) * | 2021-07-26 | 2021-10-19 | 南京信息工程大学滨江学院 | Novel organic PN heterojunction liquid phase growth method |
| CN113517403B (en) * | 2021-07-26 | 2024-02-27 | 南京信息工程大学滨江学院 | Novel organic PN heterojunction liquid phase growth method |
| CN113999475A (en) * | 2021-12-03 | 2022-02-01 | 苏州鼎奕通材料科技有限公司 | Sunlight-resistant anti-UV material and preparation method thereof |
| CN113999475B (en) * | 2021-12-03 | 2022-12-06 | 苏州鼎奕通材料科技有限公司 | Sunlight-resistant anti-UV material and preparation method thereof |
| CN114163138A (en) * | 2021-12-16 | 2022-03-11 | 南京工程学院 | Preparation method of spectrum conversion nanorod array |
| CN114163138B (en) * | 2021-12-16 | 2023-03-03 | 南京工程学院 | Preparation method of spectrum conversion nanorod array |
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Application publication date: 20180918 |