CN107293615B - The preparation method of flexible substrate over-assemble Sn3O4 nanometer sheet for photodetector - Google Patents
The preparation method of flexible substrate over-assemble Sn3O4 nanometer sheet for photodetector Download PDFInfo
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- CN107293615B CN107293615B CN201710354418.6A CN201710354418A CN107293615B CN 107293615 B CN107293615 B CN 107293615B CN 201710354418 A CN201710354418 A CN 201710354418A CN 107293615 B CN107293615 B CN 107293615B
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- 239000000758 substrate Substances 0.000 title claims abstract description 27
- 238000002360 preparation method Methods 0.000 title claims abstract description 22
- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical compound [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 claims abstract description 14
- 229910052799 carbon Inorganic materials 0.000 claims abstract description 14
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Chemical compound O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims abstract description 14
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 claims abstract description 13
- 229960000935 dehydrated alcohol Drugs 0.000 claims abstract description 13
- 239000011259 mixed solution Substances 0.000 claims abstract description 13
- 238000006243 chemical reaction Methods 0.000 claims abstract description 12
- 239000008367 deionised water Substances 0.000 claims abstract description 12
- 229910021641 deionized water Inorganic materials 0.000 claims abstract description 12
- XLYOFNOQVPJJNP-ZSJDYOACSA-N heavy water Substances [2H]O[2H] XLYOFNOQVPJJNP-ZSJDYOACSA-N 0.000 claims abstract description 12
- 239000000843 powder Substances 0.000 claims abstract description 12
- CSCPPACGZOOCGX-UHFFFAOYSA-N Acetone Chemical compound CC(C)=O CSCPPACGZOOCGX-UHFFFAOYSA-N 0.000 claims abstract description 8
- 229910021626 Tin(II) chloride Inorganic materials 0.000 claims abstract description 6
- 238000001027 hydrothermal synthesis Methods 0.000 claims abstract description 6
- 238000002156 mixing Methods 0.000 claims abstract description 6
- 239000001509 sodium citrate Substances 0.000 claims abstract description 6
- AXZWODMDQAVCJE-UHFFFAOYSA-L tin(II) chloride (anhydrous) Chemical compound [Cl-].[Cl-].[Sn+2] AXZWODMDQAVCJE-UHFFFAOYSA-L 0.000 claims abstract description 6
- -1 is stirred evenly Substances 0.000 claims abstract 2
- 238000004140 cleaning Methods 0.000 claims description 4
- 238000003756 stirring Methods 0.000 claims description 4
- 238000001035 drying Methods 0.000 claims description 2
- 230000035484 reaction time Effects 0.000 claims description 2
- 239000000243 solution Substances 0.000 claims description 2
- 238000004506 ultrasonic cleaning Methods 0.000 claims description 2
- IDGUHHHQCWSQLU-UHFFFAOYSA-N ethanol;hydrate Chemical compound O.CCO IDGUHHHQCWSQLU-UHFFFAOYSA-N 0.000 claims 1
- 238000000034 method Methods 0.000 abstract description 10
- 230000005540 biological transmission Effects 0.000 description 4
- 239000013078 crystal Substances 0.000 description 4
- 238000002003 electron diffraction Methods 0.000 description 3
- XOLBLPGZBRYERU-UHFFFAOYSA-N tin dioxide Chemical compound O=[Sn]=O XOLBLPGZBRYERU-UHFFFAOYSA-N 0.000 description 3
- 230000015572 biosynthetic process Effects 0.000 description 2
- 238000002242 deionisation method Methods 0.000 description 2
- 238000010586 diagram Methods 0.000 description 2
- 238000000445 field-emission scanning electron microscopy Methods 0.000 description 2
- 239000000463 material Substances 0.000 description 2
- 230000005622 photoelectricity Effects 0.000 description 2
- 238000003786 synthesis reaction Methods 0.000 description 2
- 238000002604 ultrasonography Methods 0.000 description 2
- 238000012795 verification Methods 0.000 description 2
- 206010034960 Photophobia Diseases 0.000 description 1
- ATJFFYVFTNAWJD-UHFFFAOYSA-N Tin Chemical compound [Sn] ATJFFYVFTNAWJD-UHFFFAOYSA-N 0.000 description 1
- 238000002441 X-ray diffraction Methods 0.000 description 1
- 238000010521 absorption reaction Methods 0.000 description 1
- 238000004458 analytical method Methods 0.000 description 1
- 229940079593 drug Drugs 0.000 description 1
- 239000003814 drug Substances 0.000 description 1
- 230000005518 electrochemistry Effects 0.000 description 1
- 238000005516 engineering process Methods 0.000 description 1
- 238000002474 experimental method Methods 0.000 description 1
- 238000002173 high-resolution transmission electron microscopy Methods 0.000 description 1
- 208000013469 light sensitivity Diseases 0.000 description 1
- 238000004519 manufacturing process Methods 0.000 description 1
- 230000003287 optical effect Effects 0.000 description 1
- 230000005855 radiation Effects 0.000 description 1
- 239000004065 semiconductor Substances 0.000 description 1
- 230000006641 stabilisation Effects 0.000 description 1
- 238000011105 stabilization Methods 0.000 description 1
- 229910001887 tin oxide Inorganic materials 0.000 description 1
Classifications
-
- H—ELECTRICITY
- H01—ELECTRIC ELEMENTS
- H01L—SEMICONDUCTOR DEVICES NOT COVERED BY CLASS H10
- 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
- H01L31/18—Processes or apparatus specially adapted for the manufacture or treatment of these devices or of parts thereof
- H01L31/1876—Particular processes or apparatus for batch treatment of the devices
-
- H—ELECTRICITY
- H01—ELECTRIC ELEMENTS
- H01L—SEMICONDUCTOR DEVICES NOT COVERED BY CLASS H10
- 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
- H01L31/08—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
- H01L31/09—Devices sensitive to infrared, visible or ultraviolet radiation
- H01L31/095—Devices sensitive to infrared, visible or ultraviolet radiation comprising amorphous semiconductors
Abstract
The present invention discloses a kind of preparation method of flexible substrate over-assemble Sn3O4 nanometer sheet for photodetector, include the following steps: that (10) substrate cleans: carbon paper being cut into required size, is cleaned by ultrasonic after being cleaned with acetone, dehydrated alcohol, deionized water；(20) prepared by mixed solution: according to the ratio by Na3C6H5O7·2H2O powder, SnCl2·2H2O powder is dissolved in deionized water and dehydrated alcohol, is stirred evenly, and mixed solution is obtained；(30) nanometer sheet assembles: carbon paper being put into and is filled in the molten reaction kettle of mixing, then reaction kettle is taken out cooled to room temperature by hydro-thermal reaction；(40) finished product is dry: carbon paper is taken out from reaction kettle, is cleaned by ultrasonic with deionized water or dehydrated alcohol, it is dry, and obtain the photodetector of flexible substrate over-assemble Sn3O4 nanometer sheet.The preparation method of flexible substrate over-assemble Sn3O4 nanometer sheet for photodetector of the invention, simple process, yield are high, at low cost.
Description
Technical field
The invention belongs to photoelectric functional material technology field, especially a kind of simple process, yield is high, at low cost is used for
The preparation method of the flexible substrate over-assemble Sn3O4 nanometer sheet of photodetector.
Background technique
Tin-oxide causes people greatly to study since it has a wide range of applications in fields such as air-sensitive, photoelectricity
Interest.But due to SnO and SnO2With biggish energy band broadband, 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, the method for improving photoelectric characteristic has: improving light sensitivity, improves the response to different wavelengths of light, mention
The bloom speed of response induces photoresponse, changes photoconductive direction.Although the several method of the above mainstream improves to a certain extent
The photoelectric properties of semiconductor, but still have that such as complex steps, products therefrom amount are small, expensive problem, thus also limit
It has been made in the application of industrial circle.
Summary of the invention
The purpose of the present invention is to provide a kind of systems of flexible substrate over-assemble Sn3O4 nanometer sheet for photodetector
Preparation Method, simple process, yield are high, at low cost.
The technical solution for realizing the aim of the invention is as follows:
A kind of preparation method of the flexible substrate over-assemble Sn3O4 nanometer sheet for photodetector, includes the following steps:
(10) substrate cleans: carbon paper being cut into required size, ultrasound is clear after being cleaned with acetone, dehydrated alcohol, deionized water
It washes；
(20) prepared by mixed solution: according to the ratio by Na3C6H5O7·2H2O powder, SnCl2·2H2O powder is dissolved in deionization
It in water and dehydrated alcohol, stirs evenly, obtains mixed solution；
(30) nanometer sheet assembles: carbon paper being put into and is filled in the molten reaction kettle of mixing, then hydro-thermal reaction takes reaction kettle
Cooled to room temperature out；
(40) finished product is dry: carbon paper is taken out from reaction kettle, is cleaned by ultrasonic with deionized water or dehydrated alcohol, it is dry, and it obtains
To the photodetector of flexible substrate over-assemble Sn3O4 nanometer sheet.
Compared with prior art, the present invention its remarkable advantage are as follows:
1, simple hydro-thermal method one-step synthesis sample, simple process simple process: are used；
2, yield is high: only needing a small amount of drug that can prepare a large amount of sample, yield is high；
3, at low cost: material price involved in preparation process is cheap, and production cost is low.
The present invention is described in further detail with reference to the accompanying drawings and detailed description.
Detailed description of the invention
Fig. 1 is process of the present invention for the preparation method of the flexible substrate over-assemble Sn3O4 nanometer sheet of photodetector
Figure.
Fig. 2 is that the X-ray of the visible photodetector of flexible substrate over-assemble Sn3O4 nanometer sheet prepared by example is spread out
Penetrate figure.
Fig. 3 is the scanning electron microscope of the visible photodetector of flexible substrate over-assemble Sn3O4 nanometer sheet prepared by example
Photo figure.
Fig. 4 is the transmission electron microscope of the visible photodetector of flexible substrate over-assemble Sn3O4 nanometer sheet prepared by example
With selective electron diffraction figure.
Fig. 5 is 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 flexible substrate over-assemble Sn3O4 nanometer sheet prepared by example
Figure.
Specific embodiment
As shown in Figure 1, preparation method of the present invention for the flexible substrate over-assemble Sn3O4 nanometer sheet of photodetector,
Include the following steps:
(10) substrate cleans: carbon paper being cut into required size, ultrasound is clear after being cleaned with acetone, dehydrated alcohol, deionized water
It washes；
In (10) the substrate cleaning step, the ultrasonic cleaning time is 10min.
(20) prepared by mixed solution: according to the ratio by Na3C6H5O7·2H2O powder, SnCl2·2H2O powder is dissolved in deionization
It in water and dehydrated alcohol, stirs evenly, obtains mixed solution；
In (20) the mixed solution preparation step, the proportion of mixed solution are as follows:
Na3C6H5O7·2H2O powder, 2.94g,
SnCl2·2H2O powder, 1.073g,
Deionized water, 20ml,
Dehydrated alcohol, 20ml.
In (20) the mixed solution preparation step, mixing time 1 hour.
(30) nanometer sheet assembles: carbon paper being put into and is filled in the molten reaction kettle of mixing, then hydro-thermal reaction takes reaction kettle
Cooled to room temperature out；
In (30) the nanometer sheet assembling steps, the temperature of hydro-thermal reaction is 180 DEG C, and the reaction time 12 is small
(40) finished product is dry: carbon paper is taken out from reaction kettle, is cleaned by ultrasonic with deionized water or dehydrated alcohol, it is dry, and it obtains
To the photodetector of flexible substrate over-assemble Sn3O4 nanometer sheet.
It is described that (in (40) finished product drying steps, the carbon paper after cleaning is 12 hours dry at 60 DEG C.
Verification experimental verification:
For the validity for verifying the method for the present invention, embodiment using D8ADVANCE type XRD (Cu k α radiation,German Bruker-AXS company) measure the crystal phase structure of prepared sample.Using Hitachi, Ltd (Japan)
II type FESEM of S4800 (FESEM, s-4800 II, Hitachi) observes the pattern of prepared sample.Using Holland
The Tecnai F30 Flied emission transmission electron microscope (HRTEM, Tecnai F30, FEI) of philips-FEI company is to the crystal phase knot of sample
Structure is intuitively detected and is characterized.Using the intensity controlled modulation optical electro-chemistry spectrometer pair of the CIMPS-2 of German ZANNER company
Prepared sample carries out photoelectricity test.
The X-ray diffraction of Fig. 2: Sn3O4 flexible prepared by present example photodetector under visible light
Figure.All diffraction maximums as shown in the figure from left to right correspond respectively to anorthic system Sn3O4(101), (111), (- 210),
(- 121), (210), (130), (102), (- 301), (- 1-41) crystal face, diagram XRD illustrate Sn in prepared sample3O4's
In the presence of.Illustration is the lattice schematic diagram of Sn3O4.
The stereoscan photograph of Fig. 3: Sn3O4 flexible prepared by present example photodetector under visible light
Figure.It was found from the figure that the Sn3O4 structure tool prepared by example with high photoelectric properties is the nanometer sheet for having bigger serface
Shape structure, for the thickness of piece about in 30nm or so, this pattern is more advantageous to the raising of photoelectric properties.
The high power transmission electron microscope of Fig. 4: Sn3O4 flexible prepared by present example photodetector under visible light
With selective electron diffraction figure.It can be seen that from the transmission electron microscope and selective electron diffraction of high power flexible prepared by example
The photodetector of Sn3O4 under visible light is by pure Sn3O4It constitutes.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, width 2.7eV.
The photoelectric properties figure of Fig. 6: Sn3O4 flexible prepared by present example photodetector under visible light.
The photoswitch time is 10 seconds.It will be seen that the current strength of the visible photodetector of Sn3O4 of synthesis is with light from figure
Strong increase is consequently increased, and there is linear relationships for photo-current intensity and light intensity.
Known to according to the above results: the photodetector preparation of the Sn3O4 flexible that we prepare under visible light
Program is simple, low in cost, and synthetic quantity is big, has good photoelectric response performance under visible light and performance is stablized, therefore can
It promotes and is applied to industrial circle.
Therefore, it can be seen that the present invention from above-mentioned experimental procedure, data and graphic analyses to assemble on flexible substrates for the first time
Sn3O4The visible photodetector of nanometer sheet, and preparation process is simple, it is low in cost, have good light under visible light
Electrical response performance energy and performance stabilization, are suitable for industrial application.
Claims (6)
1. a kind of preparation method of the flexible substrate over-assemble Sn3O4 nanometer sheet for photodetector, which is characterized in that including
Following steps:
(10) substrate cleans: carbon paper being cut into required size, is cleaned by ultrasonic after being cleaned with acetone, dehydrated alcohol, deionized water；
(20) prepared by mixed solution: according to the ratio by Na3C6H5O7·2H2O powder, SnCl2·2H2O powder is dissolved in deionized water and nothing
It in water-ethanol, stirs evenly, obtains mixed solution；
(30) nanometer sheet assembles: carbon paper being put into and is filled in the molten reaction kettle of mixing, then hydro-thermal reaction is taken out reaction kettle certainly
So it is cooled to room temperature；
(40) finished product is dry: carbon paper is taken out from reaction kettle, is cleaned by ultrasonic with deionized water or dehydrated alcohol, it is dry, and it obtains soft
Property substrate over-assemble Sn3O4 nanometer sheet.
2. preparation method according to claim 1, which is characterized in that in (10) the substrate cleaning step, ultrasonic cleaning
Time is 10min.
3. preparation method according to claim 1, which is characterized in that in (20) the mixed solution preparation step, mixing
The proportion of solution are as follows:
Na3C6H5O7·2H2O powder, 2.94g,
SnCl2·2H2O powder, 1.073g,
Deionized water, 20ml,
Dehydrated alcohol, 20ml.
4. preparation method according to claim 1, which is characterized in that in (20) the mixed solution preparation step, stirring
Time 1 hour.
5. preparation method according to claim 1, which is characterized in that in (30) the nanometer sheet assembling steps, hydro-thermal is anti-
The temperature answered is 180 DEG C, the reaction time 12 hours.
6. preparation method according to claim 1, which is characterized in that in (40) the finished product drying steps, after cleaning
Carbon paper is 12 hours dry at 60 DEG C.
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| 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 |
| CN110066117B (en) * | 2019-05-13 | 2022-03-01 | 扬州大学 | Novel self-connection SnO2Microsphere and preparation method and application thereof |
| 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 |
| CN114235931B (en) * | 2021-12-17 | 2024-01-19 | 湘潭大学 | Method for improving performance of flexible photoelectric detector |
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| CN103877996B (en) * | 2014-04-11 | 2016-05-25 | 武汉梅斯特工程技术有限公司 | A kind of renovation process of SCR catalyst |
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