CN108091732A - The preparation method of the visible photodetector of self assembly CuO nanometer sheet on a kind of FTO substrates - Google Patents
The preparation method of the visible photodetector of self assembly CuO nanometer sheet on a kind of FTO substrates Download PDFInfo
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- CN108091732A CN108091732A CN201810095443.1A CN201810095443A CN108091732A CN 108091732 A CN108091732 A CN 108091732A CN 201810095443 A CN201810095443 A CN 201810095443A CN 108091732 A CN108091732 A CN 108091732A
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- 238000001338 self-assembly Methods 0.000 title claims abstract description 26
- 239000000758 substrate Substances 0.000 title claims abstract description 23
- 238000002360 preparation method Methods 0.000 title claims abstract description 17
- 239000011259 mixed solution Substances 0.000 claims abstract description 19
- 239000008367 deionised water Substances 0.000 claims abstract description 12
- 229910021641 deionized water Inorganic materials 0.000 claims abstract description 9
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Chemical compound O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims abstract description 9
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 claims abstract description 8
- VHUUQVKOLVNVRT-UHFFFAOYSA-N Ammonium hydroxide Chemical compound [NH4+].[OH-] VHUUQVKOLVNVRT-UHFFFAOYSA-N 0.000 claims abstract description 6
- 239000000908 ammonium hydroxide Substances 0.000 claims abstract description 6
- 239000000243 solution Substances 0.000 claims abstract description 5
- 238000000151 deposition Methods 0.000 claims abstract description 4
- 238000000643 oven drying Methods 0.000 claims abstract description 4
- 239000000843 powder Substances 0.000 claims abstract description 4
- 238000003756 stirring Methods 0.000 claims abstract description 4
- 238000002207 thermal evaporation Methods 0.000 claims abstract description 4
- 238000002604 ultrasonography Methods 0.000 claims abstract description 4
- 238000005406 washing Methods 0.000 claims abstract description 4
- 238000000034 method Methods 0.000 claims description 6
- 238000000137 annealing Methods 0.000 claims description 3
- 238000007654 immersion Methods 0.000 claims description 2
- 239000007788 liquid Substances 0.000 claims description 2
- 238000002156 mixing Methods 0.000 claims 1
- 238000010521 absorption reaction Methods 0.000 abstract description 5
- 230000015572 biosynthetic process Effects 0.000 abstract description 5
- 238000003786 synthesis reaction Methods 0.000 abstract description 5
- 230000008021 deposition Effects 0.000 abstract 1
- 239000000463 material Substances 0.000 description 5
- 239000010405 anode material Substances 0.000 description 4
- 230000005540 biological transmission Effects 0.000 description 3
- 239000013078 crystal Substances 0.000 description 3
- 230000000694 effects Effects 0.000 description 3
- 238000010586 diagram Methods 0.000 description 2
- 230000005518 electrochemistry Effects 0.000 description 2
- 238000000445 field-emission scanning electron microscopy Methods 0.000 description 2
- 239000004065 semiconductor Substances 0.000 description 2
- 239000003643 water by type Substances 0.000 description 2
- 238000002441 X-ray diffraction Methods 0.000 description 1
- 230000002745 absorbent Effects 0.000 description 1
- 239000002250 absorbent Substances 0.000 description 1
- 238000004458 analytical method Methods 0.000 description 1
- 230000009286 beneficial effect Effects 0.000 description 1
- 230000005684 electric field Effects 0.000 description 1
- 230000005611 electricity Effects 0.000 description 1
- 238000002848 electrochemical method Methods 0.000 description 1
- 238000002003 electron diffraction Methods 0.000 description 1
- 238000005516 engineering process Methods 0.000 description 1
- 238000002474 experimental method Methods 0.000 description 1
- 239000010408 film Substances 0.000 description 1
- 238000002173 high-resolution transmission electron microscopy Methods 0.000 description 1
- 238000004519 manufacturing process Methods 0.000 description 1
- 239000002086 nanomaterial Substances 0.000 description 1
- 230000003287 optical effect Effects 0.000 description 1
- 230000005622 photoelectricity Effects 0.000 description 1
- 238000000053 physical method Methods 0.000 description 1
- 230000005855 radiation Effects 0.000 description 1
- 239000002994 raw material Substances 0.000 description 1
- 230000006798 recombination Effects 0.000 description 1
- 238000005215 recombination Methods 0.000 description 1
- 230000035945 sensitivity Effects 0.000 description 1
- 239000007787 solid Substances 0.000 description 1
- 230000006641 stabilisation Effects 0.000 description 1
- 238000011105 stabilization Methods 0.000 description 1
- 239000010409 thin film Substances 0.000 description 1
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- H01L31/00—Semiconductor devices sensitive to infrared radiation, light, electromagnetic radiation of shorter wavelength or corpuscular radiation and specially adapted either for the conversion of the energy of such radiation into electrical energy or for the control of electrical energy by such radiation; Processes or apparatus specially adapted for the manufacture or treatment thereof or of parts thereof; Details thereof
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- B82Y30/00—Nanotechnology for materials or surface science, e.g. nanocomposites
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- H01L31/0248—Semiconductor devices sensitive to infrared radiation, light, electromagnetic radiation of shorter wavelength or corpuscular radiation and specially adapted either for the conversion of the energy of such radiation into electrical energy or for the control of electrical energy by such radiation; Processes or apparatus specially adapted for the manufacture or treatment thereof or of parts thereof; Details thereof characterised by their semiconductor bodies
- H01L31/0256—Semiconductor devices sensitive to infrared radiation, light, electromagnetic radiation of shorter wavelength or corpuscular radiation and specially adapted either for the conversion of the energy of such radiation into electrical energy or for the control of electrical energy by such radiation; Processes or apparatus specially adapted for the manufacture or treatment thereof or of parts thereof; Details thereof characterised by their semiconductor bodies characterised by the material
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- H—ELECTRICITY
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- H01L31/10—Semiconductor devices sensitive to infrared radiation, light, electromagnetic radiation of shorter wavelength or corpuscular radiation and specially adapted either for the conversion of the energy of such radiation into electrical energy or for the control of electrical energy by such radiation; Processes or apparatus specially adapted for the manufacture or treatment thereof or of parts thereof; Details thereof in which radiation controls flow of current through the device, e.g. photoresistors characterised by potential barriers, e.g. phototransistors
- H01L31/101—Devices sensitive to infrared, visible or ultraviolet radiation
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Abstract
The present invention relates to a kind of preparation method of the visible photodetector of self assembly CuO nanometer sheet on FTO substrates, during making, (1) uses size FTO as substrate, with plasma washing machine hydrophilic treated；(2) Cu (NO are chosen3)2Powder is dissolved in the Cu (NO that 0.12mol/L is configured in deionized water3)2Solution is stirring evenly and then adding into ammonium hydroxide, obtains the first mixed solution；(3) FTO immerses the first mixed solution, is mixed into the second mixed solution, and when nature thermal evaporation 2~3 is small at low temperature by the second mixed solution, then by the second mixed solution cooled to room temperature, deposition is gone up Cu (OH)2FTO be placed on oven drying with deionized water and absolute ethyl alcohol mixed solution ultrasound, obtain dried FTO；(4) FTO is annealed, obtains the visible photodetector of self assembly CuO nanometer sheet on FTO substrates.By the present invention, synthesis for the first time has the FTO CuO heterojunction structures of high light electroresponse, and synthesis temperature is low and yield is big, has larger specific surface area and visible absorption efficiency, and photoelectric response performance is stablized.
Description
Technical field
The present invention relates to a kind of preparation methods of the visible photodetector of self assembly CuO nanometer sheet on FTO substrates, belong to
Photoelectric functional material field, more particularly to PN heterostructure semiconductors material are applied to photoelectric respone device.
Background technology
Traditional photodetector is based primarily upon semiconductor film material, and electricity is deposited by physical method on thin-film material
Pole material structure solid state photodetector, its preparation process is cumbersome and manufacturing cost is high.Solid-liquid circle to grow up in recent years
The photodetector in face assembles three electrodes by electrochemical method can realize photoelectric respone, of low cost to be beneficial to promote.
Light anode material as electrochemistry photodetector needs to have several features：(1) structure possesses superior light
The micro-nano structure of absorbent properties can allow incident light that can carry out Multiple Scattering in light anode material, increase the light path of incident light；
(2) realize that light anode material there can be good electron propagation ducts to charge-trapping pole, reduce the scattering of light induced electron；(3) solve
The certainly probability of recombination of the light anode material surface of photo-generated carrier increases effective collection of photo-generated carrier.
Based on the above idea on to improving photoelectric properties, we construct p-n junction type ultraviolet detector.It and p-
N junction type solar cell principles are identical, photovoltaic effect of the operation principle based on p-n junction.When ultraviolet lighting is mapped to p-n junction area
When, under the action of internal electric field, photo-generated carrier forms electric current.Such photovoltaic junction type ultraviolet detector high sensitivity, on-off ratio
The big and response time is short.Therefore we introduce N-type FTO and p-type CuO, and self assembly generation PN heterojunction structures, which has larger
Specific surface area and visible absorption efficiency, experimental result show that the structure possesses good photoelectric response performance under visible light
And performance is stablized.
The content of the invention
The purpose of the present invention invents aiming at the above-mentioned prior art, develops the self assembly P on N-type FTO substrates are gone out for the first time
The preparation method of the visible photodetector of type CuO nanometer sheet provides self assembly CuO nanometer sheet on a kind of FTO substrates
It can be seen that the preparation method of photodetector.
The object of the present invention is achieved like this, the visible photodetector of self assembly CuO nanometer sheet on a kind of FTO substrates
Preparation method, it is characterized in that, comprise the following steps：
(1) size FTO is used as substrate, by FTO plasma washing machine hydrophilic treateds 5~10 minutes；
(2) Cu (NO are chosen3)2Powder is dissolved in the Cu (NO that 0.12mol/L is configured in deionized water3)2Solution, stirring are equal
The ratio of addition ammonium hydroxide after even, ammonium hydroxide and deionized water is 1:20, obtain the first mixed solution；
(3) the first mixed solution that will be obtained through step (1) treated FTO immersions through step (2), it is mixed to be mixed into second
Solution is closed, when nature thermal evaporation 2~3 is small at low temperature by the second mixed solution, is then naturally cooled to the second mixed solution
Room temperature, the upper Cu (OH) of deposition2FTO be placed on oven drying with deionized water and absolute ethyl alcohol mixed solution ultrasound, obtain
Dried FTO；
(4) dried FTO is placed in Muffle furnace and annealed, obtain the visible ray of self assembly CuO nanometer sheet on FTO substrates
Electric explorer.
In step (1), the size of FTO is 1cm × 1cm.
In step (3), in deionized water and absolute ethyl alcohol mixed solution, deionized water is 1 with absolute ethyl alcohol proportioning:1.
In step (3), the temperature in baking oven is 60 DEG C.
In step (4), when dried FTO annealing times in Muffle furnace are 1 small.
The advanced science of the method for the present invention, the advantage of the invention is that the PN junction photodetector of synthesis, the prices of raw materials
Cheap and environmental-friendly, preparation process is simple, and synthesis temperature is low and yield is big, and sample has larger specific surface area and visible ray
Absorption efficiency, and photoelectric response performance is stablized, and can promote and applied to industrial circle.
The superior part of the present invention will be further illustrated in following description of the drawings and specific embodiment.
Description of the drawings
Fig. 1 is the FTO-CuO schematic diagrames of self assembly in a low temperature of the embodiment of the present invention is prepared.
Fig. 2 is the FTO-CuO flat scanning electron microscopes of self assembly in a low temperature of the embodiment of the present invention is prepared.
Fig. 3 is the FTO-CuO cross-sectional scans electron microscopes of self assembly in a low temperature of the embodiment of the present invention is prepared.
Fig. 4 is the FTO-CuO transmission electron microscope pictures of self assembly in a low temperature of the embodiment of the present invention is prepared.
Fig. 5 is the FTO-CuOX- x ray diffration pattern xs of self assembly in a low temperature of the embodiment of the present invention is prepared.
Fig. 6 is the FTO-CuO ultraviolet-visible absorption figures of self assembly in a low temperature of the embodiment of the present invention is prepared.
Fig. 7 is the tri- electrode photochemical effect performance maps of FTO-CuO of self assembly in a low temperature of the embodiment of the present invention is prepared.
Specific embodiment
Below in conjunction with attached drawing and description of the drawings, the present invention is further illustrated.
The preparation method of the visible photodetector of self assembly CuO nanometer sheet on a kind of FTO substrates, first using 1cm ×
The FTO of 1cm sizes is as substrate, with plasma washing machine hydrophilic treated 5min；Choose Cu (NO3)2Powder 1.165g is dissolved in
In 40ml deionized waters, after stirring evenly, 2mL ammonium hydroxide is added in；FTO is immersed into solution again, 3h nature thermal evaporations at 70 DEG C；Then
Cooled to room temperature is taken out, the upper Cu (OH) of deposition2FTO deionized waters and absolute ethyl alcohol 1:After 1 mixed solution ultrasound
60 DEG C of oven dryings are placed in, product is finally placed in 200 DEG C of annealing 1h in Muffle furnace, obtains on FTO substrates self assembly CuO nanometers
The visible photodetector of piece.
As shown in Fig. 2, Fig. 3, Fig. 4, Fig. 5, using S4800 II type FESEM (FESEM, the s-4800 of Hitachi, Ltd (Japan)
II, Hitachi) pattern of prepared sample (the visible photodetector of self assembly CuO nanometer sheet on FTO substrates) is seen
It examines；It is right using the Tecnai F30 Flied emissions transmission electron microscope (HRTEM, Tecnai F30, FEI) of Dutch philips-FEI companies
The crystal phase structure of sample intuitively detect and characterize；Using D8ADVANCE types XRD (Cu k α radiation,German Bruker-AXS companies) crystal phase structure of sample prepared by measure；Using German ZANNER companies
The intensity controlled modulation optical electro-chemistry spectrometers of CIMPS-2 carry out photoelectricity test to prepared sample.
Result of the test shows：
Fig. 1：The pictorial diagram of FTO-CuO prepared by the embodiment of the present invention, it is seen that the sample homoepitaxial of preparation is in FTO tables
Face.
Fig. 2：The scanning electron microscope (SEM) photograph of FTO-CuO planes prepared by the embodiment of the present invention, it was found from the figure, embodiment is made
The standby tools of the FTO-CuO with high photoelectric properties are the flaky nanometer structures for having bigger serface, this pattern is more advantageous to light
The raising of electrical property.
Fig. 3：The scanning electron microscope (SEM) photograph in the FTO-CuO sections prepared by the embodiment of the present invention, the thickness in section is about 4 μm.
Fig. 4：The high power transmission electron microscope of FTO-CuO prepared by the embodiment of the present invention and selective electron diffraction figure, can from figure
To find out that the FTO-CuO prepared by embodiment is made of pure CuO nanometer sheet.
Fig. 5：The x-ray diffraction pattern of FTO-CuO prepared by the embodiment of the present invention, all diffraction maximums as depicted
From left to right correspond respectively to (- 110) of CuO, (002), (111), (200), (- 202), (202), (- 113), (- 311) and
(- 220) crystal face, it is illustrated that XRD illustrates the presence of CuO in prepared sample.
Fig. 6：The ultraviolet-visible absorption figure of FTO-CuO prepared by the embodiment of the present invention, from figure it may be seen that
The forbidden band side of sample is very narrow, width 1.2eV.
Fig. 7：The three electrode luminous effect performance maps of FTO-CuO prepared by the embodiment of the present invention, photoswitch time are 10 seconds.
It will be seen that the current strength of the visible photodetector of hetero-junctions of synthesis also increases therewith with the increase of light intensity from figure
Add, there is linear relationships with light intensity for photo-current intensity.
It understands according to the above results：It is prepared by the photodetectors of FTO-CuO manufactured in the present embodiment under visible light
Program is simple, of low cost, and synthetic quantity is big, possesses good photoelectric response performance under visible light and performance is stablized, therefore can
It promotes and is applied to industrial circle.
Therefore, the present invention is can be seen that for the first time in FTO substrate over-assembles from above-mentioned experimental procedure, data and graphic analyses
The visible photodetector of CuO nanometer sheet, and preparation process is simple, it is of low cost, possess good light under visible light
Electrical response performance energy and performance stabilization, suitable for commercial Application.
Claims (5)
1. the preparation method of the visible photodetector of self assembly CuO nanometer sheet on a kind of FTO substrates, it is characterized in that, including with
Lower step：
(1) size FTO is used as substrate, by FTO plasma washing machine hydrophilic treateds 5~10 minutes；
(2) Cu (NO are chosen3)2Powder is dissolved in the Cu (NO that 0.12mol/L is configured in deionized water3)2Solution adds after stirring evenly
Enter ammonium hydroxide, the ratio of ammonium hydroxide and deionized water is 1:20, obtain the first mixed solution；
(3) the first mixed solution that will be obtained through step (1) treated FTO immersions through step (2), it is molten to be mixed into the second mixing
Liquid, by the thermal evaporation 2~3 natural at low temperature of the second mixed solution it is small when, then by the second mixed solution cooled to room temperature,
The upper Cu (OH) of deposition2FTO be placed on oven drying with deionized water and absolute ethyl alcohol mixed solution ultrasound, after being dried
FTO；
(4) dried FTO is placed in Muffle furnace and annealed, obtain the visible ray electrical resistivity survey of self assembly CuO nanometer sheet on FTO substrates
Survey device.
2. the preparation side of the visible photodetector of self assembly CuO nanometer sheet on a kind of FTO substrates according to claim 1
Method, it is characterized in that, in step (1), the size of FTO is 1cm × 1cm.
3. the preparation side of the visible photodetector of self assembly CuO nanometer sheet on a kind of FTO substrates according to claim 1
Method, it is characterized in that, in step (3), in deionized water and absolute ethyl alcohol mixed solution, deionized water is 1 with absolute ethyl alcohol proportioning:
1。
4. the preparation side of the visible photodetector of self assembly CuO nanometer sheet on a kind of FTO substrates according to claim 1
Method, it is characterized in that, in step (3), the temperature in baking oven is 60 DEG C.
5. the preparation side of the visible photodetector of self assembly CuO nanometer sheet on a kind of FTO substrates according to claim 1
Method, it is characterized in that, in step (4), when dried FTO annealing times in Muffle furnace are 1 small.
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Cited By (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN110665503A (en) * | 2019-09-30 | 2020-01-10 | 扬州大学 | Degradable CO2Preparation method of semiconductor photocatalyst |
| CN111495365A (en) * | 2020-05-29 | 2020-08-07 | 扬州大学 | Novel n-Cu2Preparation method of O/CuO semiconductor photocatalyst |
| CN111640581A (en) * | 2020-05-29 | 2020-09-08 | 扬州大学 | n-Cu2O/TiO2Preparation method of nanorod array PEC type photoelectric detector |
Citations (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN103117378A (en) * | 2013-01-25 | 2013-05-22 | 浙江大学 | Method for preparing copper oxide (CuO) nanosheet and carbon nanotube composite material through electrostatic self-assembly and application of composite material |
| CN103771485A (en) * | 2014-01-21 | 2014-05-07 | 中国计量学院 | Controllable preparation method for three-dimensional nano self-assembly of copper oxide |
-
2018
- 2018-01-31 CN CN201810095443.1A patent/CN108091732B/en active Active
Patent Citations (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN103117378A (en) * | 2013-01-25 | 2013-05-22 | 浙江大学 | Method for preparing copper oxide (CuO) nanosheet and carbon nanotube composite material through electrostatic self-assembly and application of composite material |
| CN103771485A (en) * | 2014-01-21 | 2014-05-07 | 中国计量学院 | Controllable preparation method for three-dimensional nano self-assembly of copper oxide |
Cited By (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN110665503A (en) * | 2019-09-30 | 2020-01-10 | 扬州大学 | Degradable CO2Preparation method of semiconductor photocatalyst |
| CN110665503B (en) * | 2019-09-30 | 2022-07-26 | 扬州大学 | Degradable CO 2 Preparation method of semiconductor photocatalyst |
| CN111495365A (en) * | 2020-05-29 | 2020-08-07 | 扬州大学 | Novel n-Cu2Preparation method of O/CuO semiconductor photocatalyst |
| CN111640581A (en) * | 2020-05-29 | 2020-09-08 | 扬州大学 | n-Cu2O/TiO2Preparation method of nanorod array PEC type photoelectric detector |
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