CN112397603A - Yb-based doped TiO2Ultraviolet photoelectric detector made of nano material and preparation method thereof - Google Patents
Yb-based doped TiO2Ultraviolet photoelectric detector made of nano material and preparation method thereof Download PDFInfo
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- 239000002086 nanomaterial Substances 0.000 title claims abstract description 25
- 238000002360 preparation method Methods 0.000 title claims abstract description 19
- 239000000758 substrate Substances 0.000 claims abstract description 55
- OGIDPMRJRNCKJF-UHFFFAOYSA-N titanium oxide Inorganic materials [Ti]=O OGIDPMRJRNCKJF-UHFFFAOYSA-N 0.000 claims abstract description 39
- 239000010453 quartz Substances 0.000 claims abstract description 36
- VYPSYNLAJGMNEJ-UHFFFAOYSA-N silicon dioxide Inorganic materials O=[Si]=O VYPSYNLAJGMNEJ-UHFFFAOYSA-N 0.000 claims abstract description 36
- GWEVSGVZZGPLCZ-UHFFFAOYSA-N titanium dioxide Inorganic materials O=[Ti]=O GWEVSGVZZGPLCZ-UHFFFAOYSA-N 0.000 claims abstract description 31
- 238000000034 method Methods 0.000 claims abstract description 16
- 238000001755 magnetron sputter deposition Methods 0.000 claims abstract description 11
- 238000003980 solgel method Methods 0.000 claims abstract description 7
- 238000004528 spin coating Methods 0.000 claims description 55
- 229920002120 photoresistant polymer Polymers 0.000 claims description 42
- CSCPPACGZOOCGX-UHFFFAOYSA-N Acetone Chemical compound CC(C)=O CSCPPACGZOOCGX-UHFFFAOYSA-N 0.000 claims description 36
- 238000001035 drying Methods 0.000 claims description 26
- 238000004544 sputter deposition Methods 0.000 claims description 26
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 claims description 22
- 239000000463 material Substances 0.000 claims description 22
- XKRFYHLGVUSROY-UHFFFAOYSA-N Argon Chemical compound [Ar] XKRFYHLGVUSROY-UHFFFAOYSA-N 0.000 claims description 14
- QTBSBXVTEAMEQO-UHFFFAOYSA-N Acetic acid Chemical compound CC(O)=O QTBSBXVTEAMEQO-UHFFFAOYSA-N 0.000 claims description 12
- YRKCREAYFQTBPV-UHFFFAOYSA-N acetylacetone Chemical compound CC(=O)CC(C)=O YRKCREAYFQTBPV-UHFFFAOYSA-N 0.000 claims description 12
- 239000008367 deionised water Substances 0.000 claims description 12
- 229910021641 deionized water Inorganic materials 0.000 claims description 12
- 238000001259 photo etching Methods 0.000 claims description 12
- 238000003756 stirring Methods 0.000 claims description 12
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Chemical compound O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims description 12
- 238000011161 development Methods 0.000 claims description 9
- 238000005516 engineering process Methods 0.000 claims description 9
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- 229910052786 argon Inorganic materials 0.000 claims description 7
- 229960000583 acetic acid Drugs 0.000 claims description 6
- 238000007664 blowing Methods 0.000 claims description 6
- YHWCPXVTRSHPNY-UHFFFAOYSA-N butan-1-olate;titanium(4+) Chemical compound [Ti+4].CCCC[O-].CCCC[O-].CCCC[O-].CCCC[O-] YHWCPXVTRSHPNY-UHFFFAOYSA-N 0.000 claims description 6
- 230000000295 complement effect Effects 0.000 claims description 6
- 239000012362 glacial acetic acid Substances 0.000 claims description 6
- 238000005245 sintering Methods 0.000 claims description 6
- 238000009210 therapy by ultrasound Methods 0.000 claims description 6
- 238000005406 washing Methods 0.000 claims description 6
- XIOPWXFTXDPBEY-UHFFFAOYSA-N ytterbium(3+);trinitrate;pentahydrate Chemical compound O.O.O.O.O.[Yb+3].[O-][N+]([O-])=O.[O-][N+]([O-])=O.[O-][N+]([O-])=O XIOPWXFTXDPBEY-UHFFFAOYSA-N 0.000 claims description 6
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- 238000010521 absorption reaction Methods 0.000 abstract description 8
- 239000004065 semiconductor Substances 0.000 abstract description 8
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- 239000002184 metal Substances 0.000 abstract description 2
- -1 drying by blowing Substances 0.000 description 4
- 239000002243 precursor Substances 0.000 description 4
- 238000012360 testing method Methods 0.000 description 4
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- 238000000825 ultraviolet detection Methods 0.000 description 4
- 230000007547 defect Effects 0.000 description 3
- 239000004408 titanium dioxide Substances 0.000 description 2
- 201000004569 Blindness Diseases 0.000 description 1
- XUIMIQQOPSSXEZ-UHFFFAOYSA-N Silicon Chemical compound [Si] XUIMIQQOPSSXEZ-UHFFFAOYSA-N 0.000 description 1
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- 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
- H01L31/10—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 at least one potential-jump barrier or surface barrier, e.g. phototransistors
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- B82Y30/00—Nanotechnology for materials or surface science, e.g. nanocomposites
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- 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
- H01L31/0264—Inorganic materials
- H01L31/032—Inorganic materials including, apart from doping materials or other impurities, only compounds not provided for in groups H01L31/0272 - H01L31/0312
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Abstract
Yb-based doped TiO2A nano-material ultraviolet photoelectric detector and a preparation method thereof belong to the technical field of semiconductor ultraviolet photoelectric detection. From bottom to top, sequentially preparing Yb doped TiO on a quartz plate substrate by a sol-gel method2A nano-material photosensitive layer, Yb doped TiO2The surface of the nano material photosensitive layer is composed of Au interdigital electrodes prepared by a magnetron sputtering method; wherein the quartzThe thickness of the chip substrate is 1-2 mm, and the thickness of the photosensitive layer is 200-300 nm; the invention is realized by adding the titanium oxide into TiO2The nano film is doped with Yb, so that the whole Fermi level of the semiconductor is improved, the Schottky barrier between the metal and the semiconductor is increased, and the dark current can be effectively reduced in a dark state. And with the increase of the doping concentration, the overall absorption wavelength of the device can generate blue shift, thereby providing a new idea for the practical application of the solar blind ultraviolet detector.
Description
Technical Field
The invention belongs to the technical field of ultraviolet photoelectric detection, and particularly relates to a Yb-doped TiO-based probe2A nano-material ultraviolet photoelectric detector and a preparation method thereof.
Background
The high-sensitivity ultraviolet photoelectric detector has important application in the fields of cell detection, remote control, environmental monitoring, photoelectric integrated circuits and the like. With the continuous progress of semiconductor materials and device preparation processes, a new generation of wide bandgap semiconductor ultraviolet detector overcomes the defects of complex structure, large volume, high energy consumption and the like of the traditional photomultiplier, and becomes a focus of attention in the technical field of ultraviolet detection at present. Meanwhile, the wide bandgap material has the visible blindness, so that the disadvantage that a silicon-based device cannot shield visible light by itself is effectively overcome, and the wide bandgap material has a plurality of varieties, particularly comprises a plurality of oxide materials such as ZnO and TiO2And the like, the materials have stable properties, various preparation methods and low cost, and have important application value.
In recent years, ultraviolet detection technology has been studied with a great deal of attention, and among them, titanium dioxide-based ultraviolet detectors have been developed most rapidly, and the research is directed to various aspects. However, due to inherent defects of wide bandgap materials, such as low carrier mobility, short exciton lifetime, and many traps and defects in oxide materials, the device based on a single material gradually fails to meet the requirements of various fields for higher ultraviolet detection performance, and the device needs to break through in dark current, absorption wavelength, and other aspects. Therefore, proper energy band engineering transformation is carried out on the material on the basis of the prior art so as to improve the comprehensive performance of the device, and the method becomes an effective method for the practical application of the ultraviolet detection technology.
Disclosure of Invention
The invention aims to provide a Yb-doped TiO-based material2A nano-material ultraviolet photoelectric detector and a preparation method thereof.
The invention is realized by adding TiO into a photosensitive layer2The nano-film is doped with Yb to make Yb in it2O3And Yb and Ti composite oxides exist, and an Au interdigital electrode is prepared on the surface of the device by adopting a magnetron sputtering method to form the device, so that the performance of the ultraviolet detector can be effectively improved, the blue shift of an absorption edge can be realized while the dark current of the device is reduced, and the performance of the device is comprehensively improved. Doping TiO with Yb2As a brand new method, the method provides a new solution for manufacturing the solar blind ultraviolet detector.
The Yb-based doped TiO of the invention2The ultraviolet photoelectric detector of nano-material is characterized in that: from bottom to top, sequentially preparing Yb doped TiO on a quartz plate substrate by a sol-gel method2A nano-material photosensitive layer, Yb doped TiO2The surface of the nano material photosensitive layer is composed of Au interdigital electrodes prepared by a magnetron sputtering method; wherein the thickness of the quartz plate substrate is 1-2 mm, and the photosensitive layer is Yb-doped TiO2The thickness of the photosensitive layer is 200-300 nm, the thickness of the Au interdigital electrode is 100-150 nm, and the electrode length, the electrode distance and the electrode width are respectively 0.8-1.2 mm, 10-30 mu m and 10-30 mu m; the structure of the device is shown in fig. 1.
The Yb-based doped TiO of the invention2The ultraviolet photoelectric detector of the nanometer material, its main theory of operation is: TiO 22The absorption wavelength of (A) is below 400nm, and the forbidden band width is 3.2 eV; yb of2O3The material is a wide-gap semiconductor material, has a gap width of 4.9eV, and has absorption in the ultraviolet range. The whole forbidden band can be adjusted by changing the doping amount in the process of preparing the deviceThe width of the device is changed, so that the whole absorption wavelength of the device is changed, the absorption wavelength of the doped device is subjected to blue shift compared with the absorption wavelength of pure titanium dioxide, and the solar blind type ultraviolet detector is further prepared. And the Fermi level of the whole semiconductor is also improved along with the Yb doping, so that the Schottky barrier formed by the semiconductor and the metal electrode is increased, and the dark current of the device is reduced.
The Yb-based doped TiO of the invention2The preparation method of the ultraviolet photoelectric detector of the nano material comprises the following steps:
(1) cleaning a substrate
Sequentially placing the quartz plate substrate in acetone, ethanol and deionized water, ultrasonically cleaning for 10-20 minutes, and then drying;
(2) preparation of Yb-doped TiO2Nanomaterial photo-sensitive layer
Firstly preparing Yb doped TiO2Sol: adding 0.3-1.8 g of ytterbium pentahydrate nitrate, 5-10 mL of tetrabutyl titanate, 5-10 mL of glacial acetic acid and 5-10 mL of acetylacetone into 50mL of ethanol, fully stirring for 30-45 minutes after each material is added, then adding 5-10 mL of deionized water, and continuously stirring for 12-14 hours; finally, standing the solution in a dark place for 12-14 hours to obtain Yb-doped TiO2Sol;
preparing Yb-doped TiO on the surface of the quartz plate substrate cleaned in the step (1)2Nano-material photosensitive layer: spin coating Yb-doped TiO on the surface of quartz plate substrate2Dissolving the sol and forming a film, wherein the spin coating speed is 2000-3500 rpm, and the spin coating time is 20-30 seconds; then drying the substrate for 10-15 minutes at the temperature of 100-120 ℃, and cooling the substrate to room temperature; repeating the steps of spin coating, drying and substrate cooling for 5-7 times, and finally doping Yb into TiO2Sintering the sol film and the quartz plate substrate at 400-500 ℃ for 2-3 hours to obtain Yb-doped TiO on the surface of the quartz plate substrate2The nano material photosensitive layer is 200-300 nm thick;
(3) preparation of Au interdigital electrode
The main process comprises the steps of spin coating photoresist, photoetching interdigital patterns, developing and sputtering;
firstly doping Yb with TiO2Spin-coating a positive photoresist film with the thickness of 0.5-1 mu m on the surface of the nano material photosensitive layer, wherein the spin-coating rotation speed is 800-1500 rpm, the spin-coating time is 20-30 seconds, and then pre-drying for 10-20 minutes at the temperature of 80-100 ℃; then, placing a photoetching mask plate which is complementary with the Au interdigital electrode structure on the photoresist, carrying out ultraviolet exposure for 60-90 seconds, and removing the exposed photoresist after development for 30-40 seconds; finally, carrying out postbaking treatment at 100-120 ℃ for 10-20 minutes to obtain the photoresist film with the hollowed-out interdigital windows;
preparing Au interdigital electrode by magnetron sputtering technology with vacuum degree of 4.0 × 10-3～8.0×10-3Pa, introducing argon at a flow rate of 20-30 sccm; then adjusting the pressure of the vacuum chamber to be 1-3 Pa, applying bias voltage, sputtering power of 60-120W and sputtering time of 10-15 minutes; after sputtering is finished, obtaining Au interdigital electrodes in the hollow interdigital windows, putting the substrate into acetone for ultrasonic treatment for 10-30 seconds, stripping unexposed photoresist and an Au layer on the unexposed photoresist, washing off the acetone, and drying by blowing to obtain the Yb-doped TiO-based substrate2Ultraviolet photoelectric detector of nanometer material.
Drawings
FIG. 1: the structure of the device is shown schematically;
FIG. 2: the invention relates to a current-voltage characteristic curve of a device (the molar doping concentration of Yb is 5%).
FIG. 3: the invention relates to a current-voltage characteristic curve of a device (the molar doping concentration of Yb is 10%).
FIG. 4: the current-voltage characteristic curve of the device (the molar doping concentration of Yb is 15%) related to the invention.
FIG. 5: the invention relates to a current-voltage characteristic curve of a device (the molar doping concentration of Yb is 20%).
As shown in FIG. 1, the names of the parts are Au interdigital electrode 1 and Yb doped TiO2Nanometer film 2, quartz plate substrate 3, incident ultraviolet 4.
As shown in fig. 2, at a Yb molar doping concentration of 5% in the device, at a bias of 5V,the photocurrent of the device was 0.51 μ A, the dark current was 0.14nA, and the ratio of the dark current to the light was 3.64X 103。
As shown in FIG. 3, when the molar doping concentration of Yb in the device is 10%, the photocurrent of the device is 0.22 μ A, the dark current is 0.61nA, and the ratio of the photocurrent to the dark current is 3.61X 10 at a bias voltage of 5V2。
As shown in FIG. 4, when the Yb molar doping concentration in the device is 15%, the photocurrent of the device is 7.34X 10 under the bias of 5V-2μ A, dark current 0.29nA, light-to-dark current ratio 2.56X 102。
As shown in fig. 5, when the molar doping concentration of Yb in the device was 20%, the photocurrent of the device was 1.48nA, the dark current was 0.24nA, and the ratio of the photodark current was 6.17 under a bias of 5V.
Detailed Description
Example 1:
and (3) sequentially placing the quartz plate substrate with the size of 15mm multiplied by 1mm into acetone, ethanol and deionized water for ultrasonic cleaning for 10 minutes, and then drying.
Preparing Yb-doped TiO on quartz plate substrate by sol-gel method2And (3) a nano film. Firstly preparing Yb doped TiO2Sol: 50mL of ethanol was poured into a conical flask with a volume of 150mL, 0.3459g of ytterbium pentahydrate nitrate, 5mL of tetrabutyl titanate, 5mL of glacial acetic acid, and 5mL of acetylacetone were sequentially poured, and after each material was poured, stirring was performed for 30 minutes, respectively, and then 5mL of deionized water was added, and stirring was continued for 12 hours. Finally, the precursor solution is placed in a dark place and stands for more than 12 hours; spin coating Yb-doped TiO on the surface of quartz plate substrate by spin coating method2Sol and form a film, the spin coating speed is 3000 r/min, and the spin coating time is 30 seconds; then drying at 100 deg.C for 10 min, cooling the substrate to room temperature, repeating the above steps of spin coating and drying for 5 times, and finally doping Yb into TiO2Sintering the sol film and the quartz plate substrate at 450 ℃ for 2 hours to obtain Yb-doped TiO on the surface of the quartz plate substrate2A nano-film with a thickness of 200-300 nm;
by spin-coating photoresist, photoetching interdigital pattern, developing andand sputtering and the like to prepare the Au interdigital electrode. Firstly TiO doped with Yb2Spin-coating a layer of positive photoresist with the thickness of 0.8 mu m on the surface of the film, wherein the spin-coating rotation speed is 1200 rpm, the spin-coating time is 20 seconds, and then pre-baking is carried out for 15 minutes at the temperature of 80 ℃; then, a photoetching mask plate which is complementary with the interdigital electrode structure is placed on the photoresist, ultraviolet exposure is carried out for 80 seconds, and the exposed photoresist is removed after development for 30 seconds; and finally, carrying out postbaking treatment at 120 ℃ for 15 minutes to obtain the photoresist film with the hollow interdigital window. Preparing Au interdigital electrode by magnetron sputtering technology with vacuum degree of 6 multiplied by 10-3Pa, introducing argon at a flow rate of 25 sccm; then adjusting the pressure of the vacuum chamber to 1.5Pa, applying bias voltage, sputtering power of 90W and sputtering time of 12 minutes; and after sputtering is finished, obtaining the Au interdigital electrode in the hollow interdigital window, putting the substrate into acetone for ultrasonic treatment for 15 seconds, stripping the unexposed photoresist and the Au layer on the unexposed photoresist, washing off the acetone, drying by blowing, and finishing the preparation of the device.
And after the device with the Yb molar doping concentration of 5% is prepared, testing the light and dark current-voltage characteristics of the device. In a dark state, the dark current of the device under the bias voltage of 5V is 0.14 nA; at a wavelength of 325nm, the light intensity is 30 muW/cm2Under the irradiation of ultraviolet light, the photocurrent of the device under the bias of 5V is 0.51 muA, and the dark current ratio of the device is 3.64 multiplied by 103。
Example 2:
and (3) sequentially placing the quartz plate substrate with the size of 15mm multiplied by 1mm into acetone, ethanol and deionized water for ultrasonic cleaning for 10 minutes, and then drying.
Preparing Yb-doped TiO on quartz plate substrate by sol-gel method2And (3) a nano film. Firstly preparing Yb doped TiO2Sol: 50mL of ethanol was poured into a conical flask with a volume of 150mL, 0.7303g of ytterbium pentahydrate nitrate, 5mL of tetrabutyl titanate, 5mL of glacial acetic acid, and 5mL of acetylacetone were sequentially poured, and after each material was poured, stirring was performed for 30 minutes, respectively, and then 5mL of deionized water was added, and stirring was continued for 12 hours. Finally, the precursor solution is placed in a dark place and stands for more than 12 hours; spin coating Yb-doped TiO on the surface of quartz plate substrate by spin coating method2Sol and form thinThe spin coating speed of the film is 3000 r/min, and the spin coating time is 30 seconds; then drying at 100 deg.C for 10 min, cooling the substrate to room temperature, repeating the above steps of spin coating and drying for 5 times, and finally doping Yb into TiO2Sintering the sol film and the quartz plate substrate at 450 ℃ for 2 hours to obtain Yb-doped TiO on the surface of the quartz plate substrate2A nano-film with a thickness of 200-300 nm;
the Au interdigital electrode is prepared by the steps of spin coating of photoresist, photoetching of interdigital patterns, development, sputtering and the like. Firstly TiO doped with Yb2Spin-coating a layer of positive photoresist with the thickness of 0.8 mu m on the surface of the film, wherein the spin-coating rotation speed is 1200 rpm, the spin-coating time is 20 seconds, and then pre-baking is carried out for 15 minutes at the temperature of 80 ℃; then, a photoetching mask plate which is complementary with the interdigital electrode structure is placed on the photoresist, ultraviolet exposure is carried out for 80 seconds, and the exposed photoresist is removed after development for 30 seconds; and finally, carrying out postbaking treatment at 120 ℃ for 15 minutes to obtain the photoresist film with the hollow interdigital window. Preparing Au interdigital electrode by magnetron sputtering technology with vacuum degree of 6 multiplied by 10-3Pa, introducing argon at a flow rate of 25 sccm; then adjusting the pressure of the vacuum chamber to 1.5Pa, applying bias voltage, sputtering power of 90W and sputtering time of 12 minutes; and after sputtering is finished, obtaining the Au interdigital electrode in the hollow interdigital window, putting the substrate into acetone for ultrasonic treatment for 15 seconds, stripping the unexposed photoresist and the Au layer on the unexposed photoresist, washing off the acetone, drying by blowing, and finishing the preparation of the device.
And after the device with the Yb molar doping concentration of 10% is prepared, testing the light and dark current-voltage characteristics of the device. In a dark state, the dark current of the device under the bias voltage of 5V is 0.14 nA; at a wavelength of 325nm, the light intensity is 30 muW/cm2Under the irradiation of ultraviolet light, the photocurrent of the device under the bias of 5V is 0.51 muA, and the dark current ratio of the device is 3.61 multiplied by 102。
Example 3:
and (3) sequentially placing the quartz plate substrate with the size of 15mm multiplied by 1mm into acetone, ethanol and deionized water for ultrasonic cleaning for 10 minutes, and then drying.
Preparing Yb-doped TiO on quartz plate substrate by sol-gel method2And (3) a nano film. Firstly preparing Yb doped TiO2Sol: 50mL of ethanol was poured into a conical flask with a volume of 150mL, 1.1598g of ytterbium pentahydrate nitrate, 5mL of tetrabutyl titanate, 5mL of glacial acetic acid, and 5mL of acetylacetone were sequentially poured, and after each material was poured, stirring was performed for 30 minutes, respectively, and then 5mL of deionized water was added, and stirring was continued for 12 hours. Finally, the precursor solution is placed in a dark place and stands for more than 12 hours; spin coating Yb-doped TiO on the surface of quartz plate substrate by spin coating method2Sol and form a film, the spin coating speed is 3000 r/min, and the spin coating time is 30 seconds; then drying at 100 deg.C for 10 min, cooling the substrate to room temperature, repeating the above steps of spin coating and drying for 5 times, and finally doping Yb into TiO2Sintering the sol film and the quartz plate substrate at 450 ℃ for 2 hours to obtain Yb-doped TiO on the surface of the quartz plate substrate2A nano-film with a thickness of 200-300 nm;
the Au interdigital electrode is prepared by the steps of spin coating of photoresist, photoetching of interdigital patterns, development, sputtering and the like. Firstly TiO doped with Yb2Spin-coating a layer of positive photoresist with the thickness of 0.8 mu m on the surface of the film, wherein the spin-coating rotation speed is 1200 rpm, the spin-coating time is 20 seconds, and then pre-baking is carried out for 15 minutes at the temperature of 80 ℃; then, a photoetching mask plate which is complementary with the interdigital electrode structure is placed on the photoresist, ultraviolet exposure is carried out for 80 seconds, and the exposed photoresist is removed after development for 30 seconds; and finally, carrying out postbaking treatment at 120 ℃ for 15 minutes to obtain the photoresist film with the hollow interdigital window. Preparing Au interdigital electrode by magnetron sputtering technology with vacuum degree of 6 multiplied by 10-3Pa, introducing argon at a flow rate of 25 sccm; then adjusting the pressure of the vacuum chamber to 1.5Pa, applying bias voltage, sputtering power of 90W and sputtering time of 12 minutes; and after sputtering is finished, obtaining the Au interdigital electrode in the hollow interdigital window, putting the substrate into acetone for ultrasonic treatment for 15 seconds, stripping the unexposed photoresist and the Au layer on the unexposed photoresist, washing off the acetone, drying by blowing, and finishing the preparation of the device.
And after the device with the Yb molar doping concentration of 15% is prepared, testing the light and dark current-voltage characteristics of the device. In a dark state, the dark current of the device under the bias voltage of 5V is 0.29 nA; at wavelength 325nm, light intensity of 30 μ W/cm2Under the irradiation of ultraviolet light, the photocurrent of the device under the bias of 5V is 7.34 multiplied by 10-2μ A, the dark current ratio of the device is 2.56 × 102。
Example 4:
and (3) sequentially placing the quartz plate substrate with the size of 15mm multiplied by 1mm into acetone, ethanol and deionized water for ultrasonic cleaning for 10 minutes, and then drying.
Preparing Yb-doped TiO on quartz plate substrate by sol-gel method2And (3) a nano film. Firstly preparing Yb doped TiO2Sol: 50mL of ethanol was poured into a conical flask with a volume of 150mL, 1.6431g of ytterbium pentahydrate nitrate, 5mL of tetrabutyl titanate, 5mL of glacial acetic acid, and 5mL of acetylacetone were sequentially poured, and after each material was poured, stirring was performed for 30 minutes, respectively, and then 5mL of deionized water was added, and stirring was continued for 12 hours. Finally, the precursor solution is placed in a dark place and stands for more than 12 hours; spin coating Yb-doped TiO on the surface of quartz plate substrate by spin coating method2Sol and form a film, the spin coating speed is 3000 r/min, and the spin coating time is 30 seconds; then drying at 100 deg.C for 10 min, cooling the substrate to room temperature, repeating the above steps of spin coating and drying for 5 times, and finally doping Yb into TiO2Sintering the sol film and the quartz plate substrate at 450 ℃ for 2 hours to obtain Yb-doped TiO on the surface of the quartz plate substrate2A nano-film with a thickness of 200-300 nm;
the Au interdigital electrode is prepared by the steps of spin coating of photoresist, photoetching of interdigital patterns, development, sputtering and the like. Firstly TiO doped with Yb2Spin-coating a layer of positive photoresist with the thickness of 0.8 mu m on the surface of the film, wherein the spin-coating rotation speed is 1200 rpm, the spin-coating time is 20 seconds, and then pre-baking is carried out for 15 minutes at the temperature of 80 ℃; then, a photoetching mask plate which is complementary with the interdigital electrode structure is placed on the photoresist, ultraviolet exposure is carried out for 80 seconds, and the exposed photoresist is removed after development for 30 seconds; and finally, carrying out postbaking treatment at 120 ℃ for 15 minutes to obtain the photoresist film with the hollow interdigital window. Preparing Au interdigital electrode by magnetron sputtering technology with vacuum degree of 6 multiplied by 10-3Pa, introducing argon at a flow rate of 25 sccm; then the pressure of the vacuum chamber was adjusted to 1.5Pa, applying bias voltage, wherein the sputtering power is 90W, and the sputtering time is 12 minutes; and after sputtering is finished, obtaining the Au interdigital electrode in the hollow interdigital window, putting the substrate into acetone for ultrasonic treatment for 15 seconds, stripping the unexposed photoresist and the Au layer on the unexposed photoresist, washing off the acetone, drying by blowing, and finishing the preparation of the device.
And after the device with the Yb molar doping concentration of 20% is prepared, testing the light and dark current-voltage characteristics of the device. In a dark state, the dark current of the device under the bias voltage of 5V is 0.24 nA; at a wavelength of 325nm, the light intensity is 30 muW/cm2Under the irradiation of ultraviolet light, the photocurrent of the device under the bias voltage of 5V is 1.48nA, and the ratio of the dark current of the device is 6.17.
Claims (5)
1. Yb-based doped TiO2The ultraviolet photoelectric detector of nano-material is characterized in that: from bottom to top, sequentially preparing Yb doped TiO on a quartz plate substrate by a sol-gel method2A nano-material photosensitive layer, Yb doped TiO2The surface of the nano material photosensitive layer is composed of Au interdigital electrodes prepared by a magnetron sputtering method.
2. The Yb-doped TiO-based material of claim 12The ultraviolet photoelectric detector of nano-material is characterized in that: the thickness of the quartz plate substrate is 1-2 mm, the thickness of the photosensitive layer is 200-300 nm, the thickness of the Au interdigital electrode is 100-150 nm, and the electrode length, the electrode spacing and the electrode width are respectively 0.8-1.2 mm, 10-30 microns and 10-30 microns.
3. Yb-based doped TiO according to claim 1 or 22The preparation method of the ultraviolet photoelectric detector of the nano material comprises the following steps:
(1) cleaning a substrate
Sequentially placing the quartz plate substrate in acetone, ethanol and deionized water, ultrasonically cleaning for 10-20 minutes, and then drying;
(2) preparation of Yb-doped TiO2Nanomaterial photo-sensitive layer
0.3-1.8 g of ytterbium pentahydrate nitrate is added into 50mL of ethanol5-10 mL of tetrabutyl titanate, 5-10 mL of glacial acetic acid and 5-10 mL of acetylacetone, fully stirring for 30-45 minutes after each material is added, then adding 5-10 mL of deionized water, and continuously stirring for 12-14 hours; finally, standing the solution in a dark place for 12-14 hours to obtain Yb-doped TiO2Sol;
spin coating Yb-doped TiO on the surface of quartz plate substrate2Dissolving the sol and forming a film, wherein the spin coating speed is 2000-3500 rpm, and the spin coating time is 20-30 seconds; then drying the substrate for 10-15 minutes at the temperature of 100-120 ℃, and cooling the substrate to room temperature; repeating the steps of spin coating, drying and substrate cooling for 5-7 times, and finally doping Yb into TiO2Sintering the sol film and the quartz plate substrate at 400-500 ℃ for 2-3 hours to obtain Yb-doped TiO on the surface of the quartz plate substrate2The nano material photosensitive layer is 200-300 nm thick;
(3) preparation of Au interdigital electrode
The main process comprises the steps of spin coating photoresist, photoetching interdigital patterns, developing and sputtering;
firstly doping Yb with TiO2Spin-coating a positive photoresist film with the thickness of 0.5-1 mu m on the surface of the nano material photosensitive layer, wherein the spin-coating rotation speed is 800-1500 rpm, the spin-coating time is 20-30 seconds, and then pre-drying for 10-20 minutes at the temperature of 80-100 ℃; then, placing a photoetching mask plate which is complementary with the Au interdigital electrode structure on the photoresist, carrying out ultraviolet exposure for 60-90 seconds, and removing the exposed photoresist after development for 30-40 seconds; finally, carrying out postbaking treatment at 100-120 ℃ for 10-20 minutes to obtain the photoresist film with the hollowed-out interdigital windows;
preparing Au interdigital electrode by magnetron sputtering technology with vacuum degree of 4.0 × 10-3～8.0×10-3Pa, introducing argon at a flow rate of 20-30 sccm; then adjusting the pressure of the vacuum chamber to be 1-3 Pa, applying bias voltage, sputtering power of 60-120W and sputtering time of 10-15 minutes; after sputtering is finished, obtaining Au interdigital electrodes in the hollow interdigital windows, putting the substrate into acetone for ultrasonic treatment for 10-30 seconds, stripping unexposed photoresist and an Au layer on the unexposed photoresist, washing off the acetone, and drying by blowing to obtain the Yb-doped T-based substrateiO2Ultraviolet photoelectric detector of nanometer material.
4. The Yb-doped TiO of claim 32The preparation method of the nano material ultraviolet photoelectric detector is characterized by comprising the following steps: forming Yb doped TiO on quartz plate surface by spin coating method2The spin coating speed of the sol film is 2000-3500 rpm, and the spin coating time is 20-30 seconds.
5. The Yb-doped TiO of claim 42The preparation method of the nano material ultraviolet photoelectric detector is characterized by comprising the following steps: the vacuum degree of the Au interdigital electrode prepared by adopting the magnetron sputtering technology is 4.0 multiplied by 10-3～8.0×10-3Pa, introducing argon at a flow rate of 20-30 sccm; adjusting the pressure of the vacuum chamber to 1-3 Pa, applying bias voltage, sputtering power to 60-120W, and sputtering time to 10-15 minutes.
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