CN107293615A - The preparation method of flexible tin-oxide photodetector - Google Patents

The preparation method of flexible tin-oxide photodetector Download PDF

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CN107293615A
CN107293615A CN201710354418.6A CN201710354418A CN107293615A CN 107293615 A CN107293615 A CN 107293615A CN 201710354418 A CN201710354418 A CN 201710354418A CN 107293615 A CN107293615 A CN 107293615A
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preparation
cleaned
deionized water
carbon paper
photodetector
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CN107293615B (en
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钱昊宇
蒋圆
史万武
黄芬
夏炜炜
曾祥华
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Yangzhou University
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Yangzhou University
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    • HELECTRICITY
    • H01ELECTRIC ELEMENTS
    • H01LSEMICONDUCTOR DEVICES NOT COVERED BY CLASS H10
    • H01L31/00Semiconductor 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
    • H01L31/18Processes or apparatus specially adapted for the manufacture or treatment of these devices or of parts thereof
    • H01L31/1876Particular processes or apparatus for batch treatment of the devices
    • HELECTRICITY
    • H01ELECTRIC ELEMENTS
    • H01LSEMICONDUCTOR DEVICES NOT COVERED BY CLASS H10
    • H01L31/00Semiconductor 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
    • H01L31/08Semiconductor 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
    • H01L31/09Devices sensitive to infrared, visible or ultraviolet radiation
    • H01L31/095Devices sensitive to infrared, visible or ultraviolet radiation comprising amorphous semiconductors

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  • Physics & Mathematics (AREA)
  • Condensed Matter Physics & Semiconductors (AREA)
  • Electromagnetism (AREA)
  • General Physics & Mathematics (AREA)
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Abstract

The present invention discloses a kind of preparation method of flexible tin-oxide photodetector, comprises the following steps:(10) substrate is cleaned:Carbon paper is cut into required size, is cleaned by ultrasonic after being cleaned with acetone, absolute ethyl alcohol, deionized water;(20) prepared by mixed solution:By proportioning by Na3C6H5O7·2H2O powder, SnCl2·2H2O powder is dissolved in deionized water and absolute ethyl alcohol, is stirred, and obtains mixed solution;(30) nanometer sheet is assembled:Carbon paper is put into fill and mixed in molten reactor, then reactor is taken out and naturally cool to room temperature by hydro-thermal reaction;(40) finished product is dried:Carbon paper is taken out from reactor, is cleaned by ultrasonic with deionized water or absolute ethyl alcohol, is dried, obtain the photodetector of flexible substrate over-assemble Sn3O4 nanometer sheets.The preparation method of the flexible tin-oxide photodetector of the present invention, technique is simple, yield is high, cost is low.

Description

The preparation method of flexible tin-oxide photodetector
Technical field
The invention belongs to photoelectric functional material technology field, particularly a kind of technique is simple, the flexibility that yield is high, cost is low The preparation method of tin-oxide photodetector.
Background technology
Tin-oxide is because it has a wide range of applications in fields such as air-sensitive, photoelectricity and causes people greatly to study Interest.But it is due to SnO and SnO2Can be with broadband with larger, it has been limited in photoelectric field.And the tin of mixed valence Oxide has than monovalent state SnO and SnO2Smaller bandwidth, is expected to realize high photoelectric respone under visible light, example Such as:Sn2O3,Sn3O4Deng.
In the prior art, improving the method for photoelectric characteristic has:Light sensitivity is improved, the response to different wavelengths of light is improved, carries The bloom speed of response, induces photoresponse, changes photoconductive direction.Although the several method of above main flow is improved to a certain extent The photoelectric properties of semiconductor, but still have that such as complex steps, products therefrom amount are small, costly problem, thus also limit Its application in industrial circle is made.
The content of the invention
It is an object of the invention to provide a kind of preparation method of flexible tin-oxide photodetector, technique is simple, production Amount is high, cost is low.
The technical solution for realizing the object of the invention is:
A kind of preparation method of flexible tin-oxide photodetector, comprises the following steps:
(10) substrate is cleaned:Carbon paper is cut into required size, ultrasound is clear after being cleaned with acetone, absolute ethyl alcohol, deionized water Wash;
(20) prepared by mixed solution:By proportioning by Na3C6H5O7·2H2O powder, SnCl2·2H2O powder is dissolved in deionization In water and absolute ethyl alcohol, stir, obtain mixed solution;
(30) nanometer sheet is assembled:Carbon paper is put into fill and mixed in molten reactor, then hydro-thermal reaction takes reactor Go out to naturally cool to room temperature;
(40) finished product is dried:Carbon paper is taken out from reactor, is cleaned by ultrasonic with deionized water or absolute ethyl alcohol, is dried, obtain To the photodetector of flexible substrate over-assemble Sn3O4 nanometer sheets.
Compared with prior art, its remarkable advantage is the present invention:
1st, technique is simple:Using simple hydro-thermal method one-step synthesis sample, technique is simple;
2nd, yield is high:A small amount of medicine is only needed to prepare substantial amounts of sample, yield is high;
3rd, cost is low:Involved material price is cheap in preparation process, and production cost is low.
The present invention is described in further detail with reference to the accompanying drawings and detailed description.
Brief description of the drawings
Fig. 1 is the flow chart of the preparation method of the flexible tin-oxide photodetector of the present invention.
Fig. 2 is that the X-ray of the visible photodetector of the flexible substrate over-assemble Sn3O4 nanometer sheets prepared by example is spread out Penetrate figure.
Fig. 3 is the ESEM of the visible photodetector of the flexible substrate over-assemble Sn3O4 nanometer sheets prepared by example Photo figure.
Fig. 4 is the transmission electron microscope of the visible photodetector of the flexible substrate over-assemble Sn3O4 nanometer sheets prepared by example With SEAD figure.
Fig. 5 is the flexible substrate over-assemble Sn prepared by example3O4The UV absorption figure of the visible photodetector of nanometer sheet
Fig. 6 is the photoelectric properties of the visible photodetector of the flexible substrate over-assemble Sn3O4 nanometer sheets prepared by example Figure.
Embodiment
As shown in figure 1, the preparation method of present invention flexibility tin-oxide photodetector, comprises the following steps:
(10) substrate is cleaned:Carbon paper is cut into required size, ultrasound is clear after being cleaned with acetone, absolute ethyl alcohol, deionized water Wash;
In (10) the substrate cleaning step, the ultrasonic cleaning time is 10min.
(20) prepared by mixed solution:By proportioning by Na3C6H5O7·2H2O powder, SnCl2·2H2O powder is dissolved in deionization In water and absolute ethyl alcohol, stir, obtain mixed solution;
In (20) the mixed solution preparation process, the proportioning of mixed solution is:
Na3C6H5O7·2H2O powder, 2.94g,
SnCl2·2H2O powder, 1.073g,
Deionized water, 20ml,
Absolute ethyl alcohol, 20ml.
In (20) the mixed solution preparation process, mixing time 1 hour.
(30) nanometer sheet is assembled:Carbon paper is put into fill and mixed in molten reactor, then hydro-thermal reaction takes reactor Go out to naturally cool to room temperature;
In (30) the nanometer sheet number of assembling steps, the temperature of hydro-thermal reaction is 180 DEG C, and the reaction time 12 is small
(40) finished product is dried:Carbon paper is taken out from reactor, is cleaned by ultrasonic with deionized water or absolute ethyl alcohol, is dried, obtain To the photodetector of flexible substrate over-assemble Sn3O4 nanometer sheets.
It is described that (in (40) finished product drying steps, the carbon paper after cleaning is dried 12 hours at 60 DEG C.
Verification experimental verification:
For verify the inventive method validity, embodiment using D8ADVANCE types XRD (Cu k α radiation,German Bruker-AXS companies) crystal phase structure of sample prepared by measure.Using Hitachi, Ltd (Japan) The type FESEM of S4800 II (FESEM, s-4800 II, Hitachi) are observed the pattern of prepared sample.Using Holland The Tecnai F30 Flied emissions transmission electron microscope (HRTEM, Tecnai F30, FEI) of philips-FEI companies is to the crystalline phase knot of sample Structure intuitively detect and characterize.Using the intensity controlled modulation optical electro-chemistry spectrometers pair of the CIMPS-2 of German ZANNER companies Prepared sample carries out photoelectricity test.
Fig. 2:The X-ray diffraction of the photodetectors of flexible Sn3O4 under visible light prepared by present example Figure.All diffraction maximums as depicted from left to right correspond respectively to anorthic system Sn3O4(101), (111), (- 210), (- 121), (210), (130), (102), (- 301), (- 1-41) crystal face, it is illustrated that XRD illustrates Sn in prepared sample3O4's In the presence of.Illustration is Sn3O4 lattice schematic diagram.
Fig. 3:The stereoscan photograph of the photodetectors of flexible Sn3O4 under visible light prepared by present example Figure.It was found from the figure, the tool of the Sn3O4 structures with high photoelectric properties prepared by example is the nanometer sheet for having bigger serface Shape structure, the thickness of piece is about in 30nm or so, and this pattern is more beneficial for the raising of photoelectric properties.
Fig. 4:The high power transmission electron microscope of the photodetectors of flexible Sn3O4 under visible light prepared by present example With SEAD figure.It can be seen that from the transmission electron microscope and SEAD of high power flexible prepared by example The photodetectors of Sn3O4 under visible light are by pure Sn3O4Constitute.Wherein 0.369nm corresponds to Sn3O4(101) crystal face.
Fig. 5:Flexible substrate over-assemble Sn prepared by present example3O4The visible photodetector of nanometer sheet it is ultraviolet Absorb figure.It may be seen that the forbidden band side of sample is very narrow from figure, its width is 2.7eV.
Fig. 6:The photoelectric properties figure of the photodetectors of flexible Sn3O4 under visible light prepared by present example. The photoswitch time is 10 seconds.It will be seen that the current strength of the visible photodetectors of Sn3O4 of synthesis is with light from figure Strong increase is consequently increased, and photo-current intensity has linear relationship with light intensity.
It can be seen from the studies above result:It is prepared by the photodetectors of the flexible Sn3O4 that we prepare under visible light Program is simple, with low cost, and synthetic quantity is big, possesses good photoelectric response performance under visible light and performance is stable, therefore can Promote and be applied to industrial circle.
Therefore, the present invention is can be seen that from above-mentioned experimental procedure, data and graphic analyses to assemble on flexible substrates first Sn3O4The visible photodetector of nanometer sheet, and preparation process is simple, it is with low cost, possess good light under visible light Electrical response performance energy and performance stabilization, suitable for commercial Application.

Claims (6)

1. a kind of preparation method of flexible tin-oxide photodetector, it is characterised in that comprise the following steps:
(10) substrate is cleaned:Carbon paper is cut into required size, is cleaned by ultrasonic after being cleaned with acetone, absolute ethyl alcohol, deionized water;
(20) prepared by mixed solution:By proportioning by Na3C6H5O7·2H2O powder, SnCl2·2H2O powder is dissolved in deionized water and nothing In water-ethanol, stir, obtain mixed solution;
(30) nanometer sheet is assembled:Carbon paper is put into fill and mixed in molten reactor, then hydro-thermal reaction is taken out reactor certainly So it is cooled to room temperature;
(40) finished product is dried:Carbon paper is taken out from reactor, is cleaned by ultrasonic with deionized water or absolute ethyl alcohol, is dried, obtain soft The photodetector of property substrate over-assemble Sn3O4 nanometer sheets.
2. preparation method according to claim 1, it is characterised in that in (10) the substrate cleaning step, is cleaned by ultrasonic Time is 10min.
3. preparation method according to claim 1, it is characterised in that in (20) the mixed solution preparation process, mixing The proportioning of solution is:
Na3C6H5O7·2H2O powder, 2.94g,
SnCl2·2H2O powder, 1.073g,
Deionized water, 20ml,
Absolute ethyl alcohol, 20ml.
4. preparation method according to claim 1, it is characterised in that in (20) the mixed solution preparation process, stirring 1 hour time.
5. preparation method according to claim 1, it is characterised in that in (30) the nanometer sheet number of assembling steps, hydro-thermal is anti- The temperature answered is 180 DEG C, 12 hours reaction time.
6. preparation method according to claim 1, it is characterised in that described (in (40) finished product drying steps, after cleaning Carbon paper is dried 12 hours at 60 DEG C.
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Cited By (6)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN108649097A (en) * 2018-04-16 2018-10-12 复旦大学 Wearable stretchable spring-like photoelectric detector of one kind and preparation method thereof
CN108878581A (en) * 2018-06-16 2018-11-23 复旦大学 Wearable stretchable spring like photoelectric detector of one kind and preparation method thereof
CN110066117A (en) * 2019-05-13 2019-07-30 扬州大学 It is a kind of novel from connection SnO2Microballoon and preparation method and application
JP2020189764A (en) * 2019-05-21 2020-11-26 国立研究開発法人物質・材料研究機構 Light deterioration inhibitor
CN114180618A (en) * 2022-01-10 2022-03-15 扬州大学 Palm-shaped SnS self-assembled on flexible substrate carbon paper2And method for preparing the same
CN114235931A (en) * 2021-12-17 2022-03-25 湘潭大学 Method for improving performance of flexible photoelectric detector

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CN103877996A (en) * 2014-04-11 2014-06-25 武汉梅斯特工程技术有限公司 Regeneration method of SCR (Selective Catalytic Reduction) catalyst
CN106206828A (en) * 2016-07-14 2016-12-07 扬州大学 A kind of self assembly nucleocapsid SnO2the preparation method of ultraviolet detector

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CN103151176A (en) * 2013-03-08 2013-06-12 厦门大学 Method for preparing three-dimensional spherical anatase type TiO2 photo-anode
CN103877996A (en) * 2014-04-11 2014-06-25 武汉梅斯特工程技术有限公司 Regeneration method of SCR (Selective Catalytic Reduction) catalyst
CN106206828A (en) * 2016-07-14 2016-12-07 扬州大学 A kind of self assembly nucleocapsid SnO2the preparation method of ultraviolet detector

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Cited By (10)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN108649097A (en) * 2018-04-16 2018-10-12 复旦大学 Wearable stretchable spring-like photoelectric detector of one kind and preparation method thereof
CN108878581A (en) * 2018-06-16 2018-11-23 复旦大学 Wearable stretchable spring like photoelectric detector of one kind and preparation method thereof
CN110066117A (en) * 2019-05-13 2019-07-30 扬州大学 It is a kind of novel from connection SnO2Microballoon and preparation method and application
CN110066117B (en) * 2019-05-13 2022-03-01 扬州大学 Novel self-connection SnO2Microsphere and preparation method and application thereof
JP2020189764A (en) * 2019-05-21 2020-11-26 国立研究開発法人物質・材料研究機構 Light deterioration inhibitor
JP7318911B2 (en) 2019-05-21 2023-08-01 国立研究開発法人物質・材料研究機構 Photodegradation inhibitor
CN114235931A (en) * 2021-12-17 2022-03-25 湘潭大学 Method for improving performance of flexible photoelectric detector
CN114235931B (en) * 2021-12-17 2024-01-19 湘潭大学 Method for improving performance of flexible photoelectric detector
CN114180618A (en) * 2022-01-10 2022-03-15 扬州大学 Palm-shaped SnS self-assembled on flexible substrate carbon paper2And method for preparing the same
CN114180618B (en) * 2022-01-10 2024-05-10 扬州大学 Palm-shaped SnS self-assembled on flexible substrate carbon paper2And a method for preparing the same

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