CN104638066A - ZnO/ZnS/FeS 2-core-shell structure array film and preparing method - Google Patents

ZnO/ZnS/FeS 2-core-shell structure array film and preparing method Download PDF

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CN104638066A
CN104638066A CN201510067375.4A CN201510067375A CN104638066A CN 104638066 A CN104638066 A CN 104638066A CN 201510067375 A CN201510067375 A CN 201510067375A CN 104638066 A CN104638066 A CN 104638066A
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CN104638066B (en
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汪牡丹
陈陈旭
方攸同
孟亮
刘嘉斌
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Zhejiang University ZJU
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Abstract

The invention relates to a preparing method of a ZnO/ZnS/FeS 2-core-shell structure array film. The preparing method comprises the following steps that FTO (fluorine-doped tin oxide) conducting glass is used as a substrate, and the substrate is cleaned for use; a uniform and transparent seed layer solution is prepared; the substrate is soaked into the seed layer solution at room temperature, and a uniform ZnO nanometer crystal seed layer is formed on the surface of the substrate; a uniform precursor solution is prepared; the surface of the substrate is provided with a uniform and compact ZnO nanometer rod array film; a ZnO/Fe(OH)3 composite nanometer rod array covers the surface of the substrate; a ZnO/Fe(OH)3 composite nanometer rod array film and sublimed sulfur powder with the purity of 99.5 percent are encapsulated in a quartz tube; the ZnO/Fe(OH)3 composite nanometer rod array is vulcanized to become a ZnO/ZnS/FeS 2-core-shell nanometer rod array. The preparing method has the advantages that visible light with the wavelength greater than 362nm in solar spectrum can be absorbed, and the light absorption and light response performance is good.

Description

ZnO/ZnS/FeS 2nucleocapsid structure array film and preparation method
Technical field
The present invention relates to a kind of ZnO/ZnS/FeS 2nuclear shell structure nano rod array film and preparation method thereof.
Technical background
The heterojunction semiconductor of component regulation and control, as superlattice, core/shell structure, and twin shaft nano heterojunction, gather the multifunctionality of independent each component, and the assembling of nanoscale opto-electronic device is subject to increasing concern.Wherein, core/shell structure nano material is at nanometer laser, and light-emitting diode, and the application such as ultraviolet light detector causes and studies interest widely, this depends primarily on structure and the physical and chemical performance of its uniqueness.Sizable effort has been devoted to the design of core/shell structure and has been prepared, especially spheroid and the nemaline core/shell structure of monodimension nano stick/nanometer.One dimension core/shell nanorod structure, due to the specific area that it is larger, and the Debye length suitable with its size, become the field that has special interest.Usually, larger specific area can increase surface trap state quantity significantly and extend the photo-generated carrier life-span.In addition, the reduction energy limiting carrier of dimension zone of action and shorten haulage time.Therefore, the optical device assembled by one dimension core/shell heterojunction shows high sensitivity, high-quantum efficiency and faster response speed usually.
ZnO and ZnS is two kinds of important direct energy-gap semiconductor materials in II-VI main group, due to the photoelectric properties that it is outstanding, the electronic device applications novel on a large scale is widely studied.Large quantity research has concentrated in ZnO/ZnS core/shell nano wire and the preparation method of nanorod heterojunction and the performance of photoelectricity.But, the energy gap (E that ZnO/ZnS heterojunction is larger g (ZnO)=3.4 eV, E g (ZnS)=3.6 eV) seriously limit its utilance to sunlight, this visible ray making it can not absorb solar spectrum medium wavelength to be greater than 362nm.
Summary of the invention
In order to overcome the above-mentioned shortcoming of prior art, the invention provides a kind of visible ray that can absorb solar spectrum medium wavelength and be greater than 362nm, light absorption and the good ZnO/ZnS/FeS of photo absorption property 2nuclear shell structure nano rod array film and preparation method thereof.
ZnO/ZnS/FeS 2the preparation method of nucleocapsid structure array film, comprises the following steps:
1) use FTO electro-conductive glass as substrate, in acetone, absolute ethyl alcohol, deionized water, carry out Ultrasonic Cleaning 15min respectively successively, by for subsequent use after cleaned substrate drying;
2) zinc acetate dihydrate is dissolved in the mixed solution of EGME and monoethanolamine, the mol ratio of monoethanolamine and zinc ion is 1:1, zinc acetate dihydrate, EGME and monoethanolamine mixed solution are stirred to zinc acetate dihydrate at 60 DEG C of lower magnetic forces to be dissolved completely, forms the Seed Layer solution of homogeneous transparent;
3) under room temperature, Seed Layer solution is immersed in substrate, upwards lift plated film with the speed of 200 mm/min, the substrate that 80 DEG C of dry plated films complete, at least repeat aforesaid operations 6 times, substrate is formed at least 6 layers of plated film; In air atmosphere, 350 DEG C of annealing 30min are carried out to the substrate with plated film, thus form one deck uniform ZnO nano crystal seed sublayer at substrate surface;
4) configure the aqueous solution of zinc nitrate and hexamethylenetetramine, the mol ratio of zinc nitrate and hexamethylenetetramine is 1:1, and this aqueous solution of magnetic agitation dissolves completely to zinc nitrate and hexamethylenetetramine, obtains uniform precursor solution;
5) appropriate precursor solution is measured, precursor solution is transferred in reactor, the substrate with ZnO nano crystal seed sublayer is soaked in precursor solution, reactor sealing is placed in thermostatic drying chamber, makes ZnO nano crystal seed sublayer be grown to serve as ZnO nano-rod array; After reaction, reactor is naturally cooled to room temperature, then substrate taken out from reactor, spend deionized water substrate and drying, now, substrate surface has the ZnO nano-rod array film of even compact;
6) configuration concentration is the Fe (NO of 6mmol/L 3) 3solution, immerses this Fe (NO by the substrate with ZnO nano-rod array film under room temperature 3) 3leave standstill in solution, time of repose is within 1min, and now ZnO nano-rod array surface is covered with one deck Fe (OH) 3layer, take out substrate and drying after spending deionized water, the surface coverage of substrate has ZnO/Fe (OH) 3composite nanorod array;
7) by ZnO/Fe (OH) 3composite Nano rod array film and purity be 99.5% sublimed sulfur powder be packaged in quartz ampoule, be evacuated to before encapsulation lower than 1 X 10 -2pa, and applying argon gas is replaced 5-8 time repeatedly;
8) encapsulation after sample in constant-temperature oven, carry out vulcanizing treatment, curing temperature lower than 600 DEG C, ZnO/Fe (OH) 3composite nanorod is array switching is ZnO/ZnS/FeS 2core-shell nanometer rod array, each ZnO/ZnS/FeS 2core-shell nanometer rod is from inside to outside followed successively by ZnO kernel, ZnS layer and FeS 2nano-particle layer, substrate surface covers ZnO/ZnS/FeS 2core-shell nano rod array film.
Further, the thickness of the substrate in step (1) is 2.2 mm, and resistance is less than 14 Ω, and light transmittance is greater than 90%, and conductive layer thickness is 350 nm.Conductive layer is fluorine-doped tin dioxide layer SnO 2: F.Substrate described in step (1) needs to carry out Ultrasonic Cleaning, to remove surperficial grease, is beneficial to the uniform fold of film, increases the adhesive force of film and substrate.
Further, in the Seed Layer solution described in step (2), zinc acetate concentration is the zinc acetate dissolving 0.05mol in the mixed solution of 50ml EGME and monoethanolamine.
Further, the annealing in process described in step (3), temperature is 350 DEG C, and the time is 30min.
Further, the precursor solution described in step (4), zinc nitrate concentration is 0.025M.
Further, in step (5), the substrate with ZnO nano crystal seed sublayer is placed in inner liner of reaction kettle and answers conducting surface to rest on obliquely on reactor wall down.
Further, the standing certain hour described in step (6), the time is 30s.
Further, the vulcanizing treatment described in step (8), sulphur steam pressure is 5 kPa, and curing temperature is 350 DEG C, and cure time is 1h, and heating rate is 2 DEG C/min.
ZnO/ZnS/FeS 2nuclear shell structure nano rod array film, is characterized in that: comprise the substrate of being made up of FTO electro-conductive glass, substrate is coated with ZnO/ZnS/FeS 2core-shell nanometer rod array, each ZnO/ZnS/FeS 2nanometer rods is by FeS 2the ZnO/ZnS core-shell nano bar construction of particle sensitization; Each ZnO/ZnS/FeS 2core-shell nanometer rod is from inside to outside followed successively by ZnO kernel, ZnS layer and FeS 2nano-particle layer.
The invention has the advantages that: by one deck FeS additional on ZnO/ZnS nuclear shell structure nano rod 2nano particle, as photosensitizer, carrys out sensitization wide bandgap semiconductor ZnO/ZnS nuclear shell structure nano rod, thus improves light absorption and the photo absorption property of ZnO/ZnS nuclear shell structure nano rod.It is highly sensitive that the present invention has light, and quantum efficiency is high and response speed is high and can absorb the visible ray that solar spectrum medium wavelength is greater than 362nm, light absorption and the good advantage of photo absorption property.
Accompanying drawing explanation
Fig. 1 is making ZnO/ZnS/FeS 2the flow chart of nanometer stick array.
Fig. 2 is the ZnO/ZnS/FeS that prepared ZnO and vulcanizing treatment obtain 2nano-stick array thin film crystal structure X-ray diffraction spectrum.
Fig. 3 is the scanning electron microscopic picture of prepared ZnO nano-rod array film.
Fig. 4 is prepared ZnO/Fe (OH) 3the scanning electron microscopic picture of nano-stick array thin film.
Fig. 5 is prepared ZnO/ZnS/FeS 2the scanning electron microscopic picture of nano-stick array thin film.
Fig. 6 is prepared ZnO/ZnS/FeS 2the transmission electron microscope picture of nano-stick array thin film.
Fig. 7 (a) is prepared ZnO/ZnS/FeS 2the optical absorption spectra of nano-stick array thin film.
Fig. 7 (b) is prepared ZnO/ZnS/FeS 2the photocurrent response spectrum of nano-stick array thin film.
Embodiment
With reference to accompanying drawing, further illustrate the present invention:
ZnO/ZnS/FeS 2the preparation method of nucleocapsid structure array film, comprises the following steps:
1) use FTO electro-conductive glass as substrate, in acetone, absolute ethyl alcohol, deionized water, carry out Ultrasonic Cleaning 15min respectively successively, by for subsequent use after cleaned substrate drying;
2) zinc acetate dihydrate is dissolved in the mixed solution of EGME and monoethanolamine, the mol ratio of monoethanolamine and zinc ion is 1:1, zinc acetate dihydrate, EGME and monoethanolamine mixed solution are stirred to zinc acetate dihydrate at 60 DEG C of lower magnetic forces to be dissolved completely, forms the Seed Layer solution of homogeneous transparent;
3) under room temperature, Seed Layer solution is immersed in substrate, upwards lift plated film with the speed of 200 mm/min, the substrate that 80 DEG C of dry plated films complete, at least repeat aforesaid operations 6 times, substrate is formed at least 6 layers of plated film; In air atmosphere, 350 DEG C of annealing 30min are carried out to the substrate with plated film, thus form one deck uniform ZnO nano crystal seed sublayer at substrate surface;
4) configure the aqueous solution of zinc nitrate and hexamethylenetetramine, the mol ratio of zinc nitrate and hexamethylenetetramine is 1:1, and this aqueous solution of magnetic agitation dissolves completely to zinc nitrate and hexamethylenetetramine, obtains uniform precursor solution;
5) appropriate precursor solution is measured, precursor solution is transferred in reactor, the substrate with ZnO nano crystal seed sublayer is soaked in precursor solution, reactor sealing is placed in thermostatic drying chamber, makes ZnO nano crystal seed sublayer be grown to serve as ZnO nano-rod array; After reaction, reactor is naturally cooled to room temperature, then substrate taken out from reactor, spend deionized water substrate and drying, now, substrate surface has the ZnO nano-rod array film of even compact;
6) configuration concentration is the Fe (NO of 6mmol/L 3) 3solution, immerses this Fe (NO by the substrate with ZnO nano-rod array film under room temperature 3) 3leave standstill in solution, time of repose is 30s, and now ZnO nano-rod array surface is covered with one deck Fe (OH) 3layer, take out substrate and drying after spending deionized water, the surface coverage of substrate has ZnO/Fe (OH) 3composite nanorod array; Leave standstill 30s, can make to immerse Fe (NO in substrate 3) 3in the process of reacting in solution, Fe 3+hydrolysis forms Fe (OH) 3and be attached to ZnO nanorod surface, can H be avoided again +znO is corroded completely, thus forms ZnO/Fe (OH) 3composite Nano rod array film.
7) by ZnO/Fe (OH) 3composite Nano rod array film and purity be 99.5% sublimed sulfur powder be packaged in quartz ampoule, be evacuated to before encapsulation lower than 1 X 10 -2pa, and applying argon gas is replaced 5-8 time repeatedly;
8) sample after encapsulation carries out vulcanizing treatment in constant-temperature oven, and sulphur steam pressure is 5kPa, and curing temperature is 350 DEG C, and cure time is 1h, and heating rate is 2 DEG C/min; ZnO/Fe (OH) 3composite nanorod is array switching is ZnO/ZnS/FeS 2core-shell nanometer rod array, each ZnO/ZnS/FeS 2core-shell nanometer rod is from inside to outside followed successively by ZnO kernel, ZnS layer and FeS 2nano-particle layer, substrate surface covers ZnO/ZnS/FeS 2core-shell nano rod array film.Curing temperature is 350 DEG C, and cure time is 1h, can ensure ZnO nanorod only outer surface cure as one deck ZnS layer, ZnO/ZnS/FeS 2core-shell nanometer rod array.
The thickness of the substrate in step (1) is 2.2 mm, and resistance is less than 14 Ω, and light transmittance is greater than 90%, and conductive layer thickness is 350 nm.Conductive layer is fluorine-doped tin dioxide layer SnO 2: F.Substrate described in step (1) needs to carry out Ultrasonic Cleaning, to remove surperficial grease, is beneficial to the uniform fold of film, increases the adhesive force of film and substrate.
In Seed Layer solution described in step (2), zinc acetate concentration is the zinc acetate dissolving 0.05mol in the mixed solution of 50ml EGME and monoethanolamine.
Annealing in process described in step (3), temperature is 350 DEG C, and the time is 30min.
Precursor solution described in step (4), zinc nitrate concentration is 0.025M.
In step (5), the conducting surface with the substrate of ZnO nano crystal seed sublayer is rested on reactor wall down obliquely.
ZnO/ZnS/FeS 2nuclear shell structure nano rod array film, is characterized in that: comprise the substrate of being made up of FTO electro-conductive glass, substrate is coated with ZnO/ZnS/FeS 2core-shell nanometer rod array, each ZnO/ZnS/FeS 2nanometer rods is by FeS 2the ZnO/ZnS core-shell nano bar construction of particle sensitization; Each ZnO/ZnS/FeS 2core-shell nanometer rod is from inside to outside followed successively by ZnO kernel, ZnS layer and FeS 2nano-particle layer.
The invention has the advantages that: by one deck FeS additional on ZnO/ZnS nuclear shell structure nano rod 2nano particle, as photosensitizer, carrys out sensitization wide bandgap semiconductor ZnO/ZnS nuclear shell structure nano rod, thus improves light absorption and the photo absorption property of ZnO/ZnS nuclear shell structure nano rod.It is highly sensitive that the present invention has light, and quantum efficiency is high and response speed is high and can absorb the visible ray that solar spectrum medium wavelength is greater than 362nm, light absorption and the good advantage of photo absorption property.
Content described in this specification embodiment is only enumerating the way of realization of inventive concept; protection scope of the present invention should not be regarded as being only limitted to the concrete form that embodiment is stated, protection scope of the present invention also and conceive the equivalent technologies means that can expect according to the present invention in those skilled in the art.

Claims (9)

1.ZnO/ZnS/FeS 2the preparation method of nucleocapsid structure array film, comprises the following steps:
1) use FTO electro-conductive glass as substrate, in acetone, absolute ethyl alcohol, deionized water, carry out Ultrasonic Cleaning 15min respectively successively, by for subsequent use after cleaned substrate drying;
2) zinc acetate dihydrate is dissolved in the mixed solution of EGME and monoethanolamine, the mol ratio of monoethanolamine and zinc ion is 1:1, zinc acetate dihydrate, EGME and monoethanolamine mixed solution are stirred to zinc acetate dihydrate at 60 DEG C of lower magnetic forces to be dissolved completely, forms the Seed Layer solution of homogeneous transparent;
3) under room temperature, Seed Layer solution is immersed in substrate, upwards lift plated film with the speed of 200 mm/min, the substrate that 80 DEG C of dry plated films complete, at least repeat aforesaid operations 6 times, substrate is formed at least 6 layers of plated film; In air atmosphere, 350 DEG C of annealing 30min are carried out to the substrate with plated film, thus form one deck uniform ZnO nano crystal seed sublayer at substrate surface;
4) configure the aqueous solution of zinc nitrate and hexamethylenetetramine, the mol ratio of zinc nitrate and hexamethylenetetramine is 1:1, and this aqueous solution of magnetic agitation dissolves completely to zinc nitrate and hexamethylenetetramine, obtains uniform precursor solution;
5) appropriate precursor solution is measured, precursor solution is transferred in reactor, the substrate with ZnO nano crystal seed sublayer is soaked in precursor solution, reactor sealing is placed in thermostatic drying chamber, makes ZnO nano crystal seed sublayer be grown to serve as ZnO nano-rod array; After reaction, reactor is naturally cooled to room temperature, then substrate taken out from reactor, spend deionized water substrate and drying, now, substrate surface has the ZnO nano-rod array film of even compact;
6) configuration concentration is the Fe (NO of 6mmol/L 3) 3solution, immerses this Fe (NO by the substrate with ZnO nano-rod array film under room temperature 3) 3leave standstill in solution, time of repose is within 1min, and now ZnO nano-rod array surface is covered with one deck Fe (OH) 3layer, take out substrate and drying after spending deionized water, the surface coverage of substrate has ZnO/Fe (OH) 3composite nanorod array;
7) by ZnO/Fe (OH) 3composite Nano rod array film and purity be 99.5% sublimed sulfur powder be packaged in quartz ampoule, be evacuated to before encapsulation lower than 1 X 10 -2pa, and applying argon gas is replaced 5-8 time repeatedly;
8) encapsulation after sample in constant-temperature oven, carry out vulcanizing treatment, curing temperature lower than 600 DEG C, ZnO/Fe (OH) 3composite nanorod is array switching is ZnO/ZnS/FeS 2core-shell nanometer rod array, each ZnO/ZnS/FeS 2core-shell nanometer rod is from inside to outside followed successively by ZnO kernel, ZnS layer and FeS 2nano-particle layer, substrate surface covers ZnO/ZnS/FeS 2core-shell nano rod array film.
2. ZnO/ZnS/FeS as claimed in claim 1 2the preparation method of nucleocapsid structure array film, is characterized in that: ZnO/ZnS/FeS 2the thickness of the substrate in preparation method's step 1) of nucleocapsid structure array film is 2.2 mm, and resistance is less than 14 Ω, and light transmittance is greater than 90%, and conductive layer thickness is 350 nm.
3. ZnO/ZnS/FeS as claimed in claim 2 2the preparation method of nucleocapsid structure array film, is characterized in that: in the Seed Layer solution described in step (2), zinc acetate concentration is the zinc acetate dissolving 0.05mol in the mixed solution of 50ml EGME and monoethanolamine.
4. ZnO/ZnS/FeS as claimed in claim 3 2the preparation method of nucleocapsid structure array film, is characterized in that: the annealing in process described in step (3), and temperature is 350 DEG C, and the time is 30min.
5. ZnO/ZnS/FeS as claimed in claim 4 2the preparation method of nucleocapsid structure array film, is characterized in that: the precursor solution described in step (4), and zinc nitrate concentration is 0.025M.
6. ZnO/ZnS/FeS as claimed in claim 5 2the preparation method of nucleocapsid structure array film, is characterized in that: in step (5), the substrate with ZnO nano crystal seed sublayer is placed in inner liner of reaction kettle and answers conducting surface to rest on obliquely on reactor wall down.
7. ZnO/ZnS/FeS as claimed in claim 6 2the preparation method of nucleocapsid structure array film, is characterized in that: the standing certain hour described in step (6), and the time is 30s.
8. ZnO/ZnS/FeS as claimed in claim 7 2the preparation method of nucleocapsid structure array film, is characterized in that: the vulcanizing treatment described in step (8), and sulphur steam pressure is 5 kPa, and curing temperature is 350 DEG C, and cure time is 1h, and heating rate is 2 DEG C/min.
9. the ZnO/ZnS/FeS belonging to one of claim 1-8 2the array film that the preparation method of nuclear shell structure nano rod array film obtains, is characterized in that: comprise the substrate of being made up of FTO electro-conductive glass, substrate is coated with ZnO/ZnS/FeS 2core-shell nanometer rod array, each ZnO/ZnS/FeS 2nanometer rods is by FeS 2the ZnO/ZnS core-shell nano bar construction of particle sensitization; Each ZnO/ZnS/FeS 2core-shell nanometer rod is from inside to outside followed successively by ZnO kernel, ZnS layer and FeS 2nano-particle layer.
CN201510067375.4A 2015-02-09 2015-02-09 ZnO/ZnS/FeS 2-core-shell structure array film and preparing method Expired - Fee Related CN104638066B (en)

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CN109399725A (en) * 2017-08-15 2019-03-01 中国石油化工股份有限公司 A kind of preparation method and applications of the nano-structure array of dregs containing zinc
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CN111816716A (en) * 2020-07-21 2020-10-23 中国人民解放军国防科技大学 Preparation method of core-shell heterojunction array electrode with efficient photoelectric detection performance
CN111816716B (en) * 2020-07-21 2021-08-31 中国人民解放军国防科技大学 Preparation method of core-shell heterojunction array electrode with efficient photoelectric detection performance
CN114182281A (en) * 2021-12-10 2022-03-15 黑龙江省科学院高技术研究院 Preparation method of mono-crystal-like bismuth vanadate nanorod array with [010] dominant growth orientation

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