CN113451447A - Deep ultraviolet amorphous gallium oxide photoelectric detector and preparation method and application thereof - Google Patents

Deep ultraviolet amorphous gallium oxide photoelectric detector and preparation method and application thereof Download PDF

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CN113451447A
CN113451447A CN202110738976.9A CN202110738976A CN113451447A CN 113451447 A CN113451447 A CN 113451447A CN 202110738976 A CN202110738976 A CN 202110738976A CN 113451447 A CN113451447 A CN 113451447A
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film sample
substrate
film
gallium oxide
deposition
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陈朗
叶茂
张立冬
胡松柏
王琪祚
刘奇
李晓文
徐泽东
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Southern University of Science and Technology
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Abstract

The invention provides a deep ultraviolet amorphous gallium oxide photoelectric detector and a preparation method and application thereof, wherein the preparation method comprises the following steps: (1) preparing an amorphous gallium oxide film on the surface of the substrate by adopting a pulse laser deposition method to obtain a film sample; (2) preparing an interdigital electrode on the surface of one side of the film sample by adopting an ultraviolet photoetching method and a magnetron sputtering method in sequence to obtain a deep ultraviolet amorphous gallium oxide photoelectric detector; wherein the oxygen partial pressure of the pulse laser deposition method in the step (1) is 0.13-1.3 Pa. The photoelectric detector comprises a substrate, an amorphous gallium oxide film and an interdigital electrode which are sequentially arranged; the application comprises the fields of analysis and test, environment monitoring, industrial automation control, space communication and missile tracking. The photoelectric detector provided by the invention overcomes the problems of high cost of a homogeneous substrate and large thermal mismatch of a heterogeneous substrate, improves the signal-to-noise ratio and response speed of the device, simplifies the preparation method and is suitable for industrial production and application.

Description

Deep ultraviolet amorphous gallium oxide photoelectric detector and preparation method and application thereof
Technical Field
The invention belongs to the technical field of photoelectric detection, relates to a photoelectric detector, and particularly relates to a deep ultraviolet amorphous gallium oxide photoelectric detector, and a preparation method and application thereof.
Background
In recent years, with the rapid development and wide application of information technology, particularly internet of things technology, the application of a photoelectric detector is expanded to a wider field, so that higher requirements are also made on the performance of the photoelectric detector. The deep ultraviolet photoelectric detector can detect ultraviolet rays with the wavelength of 200-300nm, the ultraviolet rays smaller than the waveband can be absorbed by ozone when passing through the atmosphere, and the ultraviolet rays in the waveband hardly exist on the earth surface, so that the deep ultraviolet photoelectric detector can hardly be interfered by sunlight when in work, the detector has strong anti-interference capability and high detection precision and sensitivity, is widely applied to civil fields such as ultraviolet communication, medical imaging, power grid safety monitoring, flame detection, field search and rescue, and can also be applied to national defense fields such as secret communication, early warning and accurate guidance.
The initial deep ultraviolet detector used a photomultiplier tube, and the characteristics of high sensitivity and low noise made it possible to detect weak light signals, but the photomultiplier tube was bulky, fragile, not stable, and required a large bias voltage, and thus had many limitations in application. For the traditional semiconductor material, it is common practice to add a filter on materials such as silicon and germanium by using a packaging process to limit the response wavelength to the deep ultraviolet band, but this increases the volume and cost of the device, and the device has poor high temperature and high pressure resistance.
With the development of semiconductor materials, wide bandgap semiconductor materials have been gradually adopted as photosensitive materials of deep ultraviolet photodetectors, and the wide bandgap semiconductors have many advantages, such as large forbidden bandwidth, no need of adding an additional optical filter due to the inherent deep ultraviolet absorption characteristics, good thermal conductivity, high electron saturation drift velocity, and high chemical stability and radiation resistance. The deep ultraviolet detector manufactured based on the wide-bandgap semiconductor material can directly respond to ultraviolet photon signals without adding other complex and expensive optical elements, so that the deep ultraviolet detector has the advantages of small volume, high stability, integration capability, high quantum efficiency and the like.
In recent years, a variety of wide bandgap semiconductors have been used to study the design of deep ultraviolet photodetectors, including AlGaN, ZnMgO, Ga2O3Diamond and the like, but the band gap of diamond is too wide to be 5.5eV, and the actual response wavelength is less than 225nm, so the detection efficiency is very low; the band gap width of the ternary alloy materials such as AlGaN and MgZnO can be regulated by regulating the proportion of elements, but the preparation is difficult, the mobility of Al and Ga in AlGaN is different, the components are not uniform, and MgZnO is easy to phase separate, so that the preparation is difficult.
Gallium oxide (Ga)2O3) There are five isomers: alpha, beta, gamma, delta, epsilon-Ga2O3Wherein the beta phase is the most stable crystal phase, the forbidden bandwidth is about 4.9eV, the corresponding ultraviolet wavelength is 254nm, the energy band regulation is not needed, and the absorption coefficient near the absorption edge is as high as 105cm-1Electron mobility up to 300cm2The dielectric constant of the/Vs is as high as 10, the breakdown electric field of 8MV/cm can be resisted at the highest, the material is an ideal deep ultraviolet detection material, and the application of devices can be realized under severe conditions, so the current research is mainly focused on the beta-phase gallium oxide film. But beta-Ga2O3Also faces the problems of expensive homogeneous substrate and large thermal mismatch of heterogeneous substrate, resulting in different substrates and beta-Ga prepared by different methods2O3The detector performance varies greatly.
Therefore, how to provide a gallium oxide photoelectric detector and a preparation method thereof can overcome the problems of expensive homogeneous substrate and large thermal mismatch of heterogeneous substrate, improve the signal-to-noise ratio and response speed of the device, simplify the preparation method, adapt to industrial production and application, and become the problem which needs to be solved urgently by technical personnel in the field at present.
Disclosure of Invention
The invention aims to provide a deep ultraviolet amorphous gallium oxide photoelectric detector and a preparation method and application thereof, the photoelectric detector overcomes the problems of high cost of a homogeneous substrate and large thermal mismatch of a heterogeneous substrate, simultaneously improves the signal-to-noise ratio and response speed of a device, simplifies the preparation method and is suitable for industrial production and application.
In order to achieve the purpose, the invention adopts the following technical scheme:
in a first aspect, the present invention provides a method for preparing a deep ultraviolet amorphous gallium oxide photodetector, comprising the following steps:
(1) preparing an amorphous gallium oxide film on the surface of the substrate by adopting a pulse laser deposition method to obtain a film sample;
(2) preparing an interdigital electrode on the surface of one side of the film sample by adopting an ultraviolet photoetching method and a magnetron sputtering method in sequence to obtain a deep ultraviolet amorphous gallium oxide photoelectric detector;
the partial pressure of oxygen in the pulsed laser deposition method of step (1) is 0.13-1.3Pa, and may be, for example, 0.13Pa, 0.23Pa, 0.33Pa, 0.43Pa, 0.53Pa, 0.63Pa, 0.73Pa, 0.83Pa, 0.93Pa, 1Pa, 1.1Pa, 1.2Pa or 1.3Pa, but is not limited to the values listed, and other values not listed in the range of values are also applicable.
In the invention, the pulse laser deposition method is adopted to reasonably control the number of surface state defects in the amorphous gallium oxide, so that the surface state defects become a recombination center of electrons and holes, and further the signal-to-noise ratio and the response speed of the photoelectric detector are improved. In addition, compared with crystalline gallium oxide, the amorphous gallium oxide has the advantages of lower required temperature in the preparation process, less limitation by growth conditions and substrates, and simple preparation method.
In the invention, the oxygen partial pressure of the pulsed laser deposition method in the step (1) has obvious influence on both the light dark current and the signal-to-noise ratio (the ratio of the photocurrent to the dark current under the same voltage) of the photodetector. Within the range of 0.13-1.3Pa, along with the increase of the oxygen partial pressure, the oxygen vacancy defect in the film is reduced, the carrier concentration is reduced, and equivalently, the height of a metal-semiconductor interface Schottky barrier is increased, so both the photocurrent and the dark current show a descending trend; however, the change of the number of carriers has more obvious influence on the dark current (the magnitude of the dark current value is small), the dark current is reduced more greatly, and therefore the signal to noise ratio shows an increasing trend. When the oxygen partial pressure is lower than 0.13Pa, the signal-to-noise ratio of the photoelectric detector is too low; when the oxygen partial pressure is higher than 1.3Pa, both the photocurrent and dark current of the photodetector are too low.
Preferably, the pulsed laser deposition method in step (1) is performed in a pulsed laser deposition system, and the specific operations include the following steps:
(a) cleaning and drying the substrate, and then sticking the substrate on a heating support;
(b) placing the heating support on a heating table, and drying the adhesive on the back of the substrate;
(c) and placing the heating support in a cavity, vacuumizing and depositing a thin film.
Preferably, the substrate of step (a) comprises C-plane sapphire.
The invention selects C-plane sapphire (alpha-Al)2O3) As the substrate, the material has good permeability, thermal stability and chemical stability in the visible wavelength range, high mechanical strength, mature production process and low manufacturing cost. Furthermore, although alpha-Al2O3With beta-Ga2O3There is a large lattice mismatch between crystals, but amorphous Ga is produced2O3The film has no problem of lattice mismatch.
Preferably, the substrate of step (a) has a thickness of 0.4-0.6mm, and may be, for example, 0.4mm, 0.42mm, 0.44mm, 0.46mm, 0.48mm, 0.5mm, 0.52mm, 0.54mm, 0.56mm, 0.58mm or 0.6mm, but is not limited to the recited values, and other values not recited within the range of values are equally applicable.
Preferably, the cleaning of step (a) comprises ultrasonic cleaning.
Preferably, the cleaning solution used in the cleaning of step (a) comprises acetone.
Preferably, the drying of step (a) comprises high purity nitrogen blow drying.
Preferably, the adhesive used in the step (a) comprises silver adhesive.
Preferably, the temperature of the drying in step (b) is 100-.
Preferably, the drying time in step (b) is 10-30min, such as 10min, 12min, 14min, 16min, 18min, 20min, 22min, 24min, 26min, 28min or 30min, but not limited to the recited values, and other values not recited in the range of the values are also applicable.
Preferably, the absolute vacuum degree of the vacuum pumping in the step (c) is less than or equal to 5 x 10-4Pa, for example, may be 1X 10-4Pa、1.5×10-4Pa、2×10-4Pa、2.5×10-4Pa、3×10-4Pa、3.5×10-4Pa、4×10-4Pa、4.5×10-4Pa or 5X 10-4Pa, but is not limited to the recited values, and other values within the range are equally applicable.
Preferably, the deposition temperature for the thin film deposition in step (c) is 25-450 ℃, and may be, for example, 25 ℃, 50 ℃, 75 ℃, 100 ℃, 150 ℃, 200 ℃, 250 ℃, 300 ℃, 350 ℃, 400 ℃ or 450 ℃, but is not limited to the recited values, and other values not recited in the range of values are also applicable.
In the invention, the deposition temperature of the film deposition in the step (c) is the temperature in the chamber, the lower limit of the temperature is 25 ℃ which is the temperature of the room temperature, heating is not needed, but when the temperature is higher than 450 ℃, the gallium oxide obtained by deposition is mainly in a crystal state, so that the surface state defects are too few, and the response speed of the photoelectric detector is reduced.
Preferably, the laser energy for the film deposition in step (c) is 1-2J/cm2For example, it may be 1J/cm2、1.1J/cm2、1.2J/cm2、1.3J/cm2、1.4J/cm2、1.5J/cm2、1.6J/cm2、1.7J/cm2、1.8J/cm2、1.9J/cm2Or 2J/cm2However, the numerical values recited are not intended to be limiting, and other numerical values not recited within the numerical range may be equally applicable.
Preferably, the laser frequency of the thin film deposition in step (c) is 8-12Hz, such as 8Hz, 8.5Hz, 9Hz, 9.5Hz, 10Hz, 10.5Hz, 11Hz, 11.5Hz, or 12Hz, but not limited to the values listed, and other values not listed in the range are also applicable.
Preferably, the target material used for the thin film deposition in step (c) is a gallium oxide ceramic target.
Preferably, the gallium oxide ceramic target has a purity of 99.99% or more, and can be, for example, 99.99%, 99.991%, 99.992%, 99.993%, 99.994%, 99.995%, 99.996%, 99.997%, 99.998%, or 99.999%, but is not limited to the recited values, and other values not recited within the range of values are equally applicable.
Preferably, the target spacing for the thin film deposition in step (c) is 50-60mm, such as 50mm, 51mm, 52mm, 53mm, 54mm, 55mm, 56mm, 57mm, 58mm, 59mm or 60mm, but not limited to the recited values, and other values not recited in the range of values are also applicable.
In the invention, because the plasma plumes ejected by the laser bombarding the target material are in axial symmetry and radial distribution in space, and the energy, momentum and quantity of particles (or ions) in the target material are distributed differently along with the difference of radial distance, the target distance of the film deposition in the step (c) can obviously influence the uniformity of the deposited film and needs to be controlled in a reasonable range. When the target pitch is less than 50mm or more than 60mm, uniformity of the deposited thin film is deteriorated to various degrees.
Preferably, the number of pulses for depositing the thin film in step (c) is 8000-.
Preferably, the deposition thickness of the thin film deposition in step (c) is 140-160nm, such as 140nm, 142nm, 144nm, 146nm, 148nm, 150nm, 152nm, 154nm, 156nm, 158nm or 160nm, but not limited to the values listed, and other values not listed in the range are also applicable.
Preferably, the ultraviolet lithography method in step (2) is to expose the film sample under a photolithography plate.
Preferably, the exposure time is 6-8s, and may be, for example, 6s, 6.2s, 6.4s, 6.6s, 6.8s, 7s, 7.2s, 7.4s, 7.6s, 7.8s, or 8s, but is not limited to the recited values, and other values not recited within the range of values are equally applicable.
Preferably, the magnetron sputtering method in the step (2) is to place the film sample in a radio frequency magnetron system for metal deposition, and prepare the interdigital electrode on the surface of one side of the film sample.
Preferably, the material of the interdigital electrode comprises platinum.
The interdigital electrode made of platinum is good in stability, not easy to oxidize, strong in abrasion resistance and corrosion resistance, good in conductivity and good in comprehensive performance.
Preferably, the interdigital electrode has a thickness of 80 to 120nm, and may be, for example, 80nm, 85nm, 90nm, 95nm, 100nm, 105nm, 110nm, 115nm or 120nm, but is not limited to the values listed, and other values not listed in the range of the values are also applicable.
Preferably, the ultraviolet lithography method in the step (2) further comprises sequentially cleaning, drying, spin coating and pre-baking the film sample.
Preferably, the step (2) further comprises, between the ultraviolet lithography method and the magnetron sputtering method, performing post-baking, developing and fixing on the film sample in sequence.
Preferably, the magnetron sputtering method in the step (2) further comprises sequentially peeling and inspecting the film sample.
Preferably, the cleaning means comprises ultrasonic cleaning.
Preferably, the cleaning solution used for cleaning comprises acetone.
Preferably, the drying means comprises high purity nitrogen blow drying.
Preferably, the whirl coating is to place the film sample on a spin coater, drop negative glue on the surface of one side of the film sample and start the rotation operation.
Preferably, the rotation speed of the rotation operation is 3000-5000rpm, for example, 3000rpm, 3200rpm, 3400rpm, 3600rpm, 3800rpm, 4000rpm, 4200rpm, 4400rpm, 4600rpm, 4800rpm or 5000rpm may be used, but the rotation speed is not limited to the enumerated values, and other non-enumerated values in the numerical range are also applicable.
Preferably, the rotation is performed for a time period of 40-80s, for example, 40s, 45s, 50s, 55s, 60s, 65s, 70s, 75s, or 80s, but not limited to the recited values, and other values not recited in the range of values are also applicable.
Preferably, the pre-baking is performed on a heated platen.
Preferably, the temperature of the pre-baking is 80-100 ℃, for example 80 ℃, 82 ℃, 84 ℃, 86 ℃, 88 ℃, 90 ℃, 92 ℃, 94 ℃, 96 ℃, 98 ℃ or 100 ℃, but is not limited to the recited values, and other values not recited in the range of values are equally applicable.
Preferably, the pre-baking time is 40-80s, for example 40s, 45s, 50s, 55s, 60s, 65s, 70s, 75s or 80s, but not limited to the recited values, and other values not recited in the range of values are equally applicable.
Preferably, the postbaking is carried out on a heated platen.
Preferably, the post-baking temperature is 90-100 ℃, for example 90 ℃, 91 ℃, 92 ℃, 93 ℃, 94 ℃, 95 ℃, 96 ℃, 97 ℃, 98 ℃, 99 ℃ or 100 ℃, but is not limited to the recited values, and other values not recited in the range of values are equally applicable.
Preferably, the post-baking time is 100-140s, and may be, for example, 100s, 105s, 110s, 115s, 120s, 125s, 130s, 135s or 140s, but is not limited to the recited values, and other values not recited in the range of the values are also applicable.
Preferably, the developing solution used for the development comprises an AR300-26 developing solution.
Preferably, the development time is 30-40s, for example 30s, 31s, 32s, 33s, 34s, 35s, 36s, 37s, 38s, 39s or 40s, but is not limited to the recited values, and other values not recited in the range of values are also applicable.
Preferably, the fixing solution used for fixing includes deionized water.
Preferably, the fixing time is 30-60s, for example 30s, 35s, 40s, 45s, 50s, 55s or 60s, but not limited to the recited values, and other values not recited in the range of values are also applicable.
Preferably, the peeling is to soak the film sample in acetone, remove the excess residual glue and blow dry the film sample.
Preferably, the inspection is to use an optical microscope to observe the etched pattern, and confirm whether the size of the interdigital electrode is consistent with the size of the pattern on the photomask.
As a preferred technical solution of the first aspect of the present invention, the preparation method comprises the steps of:
(1) preparing an amorphous gallium oxide film on the surface of a substrate by adopting a pulse laser deposition system to obtain a film sample, and specifically, the method comprises the following steps:
(a) ultrasonically cleaning a C-surface sapphire substrate with the thickness of 0.4-0.6mm by using acetone, drying the substrate by using high-purity nitrogen, and adhering the substrate to a heating support by using silver colloid after drying the substrate by using high-purity nitrogen;
(b) placing the heating support on a heating table, and baking at 100-200 deg.C for 10-30min until the adhesive on the back of the substrate is fully dried;
(c) placing the heating support in the cavity, vacuumizing to an absolute vacuum degree of less than or equal to 510-4Depositing film after Pa, oxygen partial pressure 0.13-1.3Pa, deposition temperature 25-450 deg.C, laser energy 1-2J/cm2The laser frequency is 8-12Hz, the adopted target material is a gallium oxide ceramic target with the purity of more than or equal to 99.99 percent, the target distance is 50-60mm, the pulse frequency is 8000-12000 times, and the deposition thickness is 140-160 nm;
(2) preparing an interdigital electrode on the surface of one side of the film sample to obtain the deep ultraviolet amorphous gallium oxide photoelectric detector, wherein the specific operation comprises the following steps:
(d) cleaning: carrying out ultrasonic cleaning on the film sample by adopting acetone;
(e) and (3) drying: blowing the acetone on the surface of the film sample by high-purity nitrogen;
(f) spin coating: placing a film sample on a spin coater, dropwise adding negative glue on the surface of one side of a film of the film sample, and starting rotation operation, wherein the set rotation speed is 3000 plus 5000rpm, and the time is 40-80 s;
(g) pre-baking: placing the film sample on a heating table, and baking for 40-80s at 80-100 ℃;
(h) ultraviolet photoetching: placing the film sample under a photoetching plate for exposure for 6-8 s;
(i) post-baking: placing the film sample on a heating table, and baking for 140s at 90-100 ℃;
(j) and (3) developing: developing the film sample for 30-40s by using AR300-26 developing solution;
(k) fixing: fixing the film sample for 30-60s by using deionized water;
(l) Magnetron sputtering: placing the film sample in a radio frequency magnetic control system for metal deposition, and preparing an interdigital electrode which is made of platinum and has the thickness of 80-120nm on the surface of one side of the film sample;
(m) peeling: soaking the film sample in acetone, removing redundant residual glue and drying;
(n) checking: and observing the etched pattern by using an optical microscope, and confirming whether the size of the interdigital electrode is consistent with the size of the pattern on the photoetching plate.
In a second aspect, the invention provides a deep ultraviolet amorphous gallium oxide photodetector prepared by the preparation method of the first aspect, wherein the photodetector comprises a substrate, an amorphous gallium oxide thin film and an interdigital electrode, which are sequentially arranged.
In a third aspect, the invention provides a use of the photodetector of the second aspect in the fields of analytical testing, environmental monitoring, industrial automation control, space communication and missile tracking.
Compared with the prior art, the invention has the following beneficial effects:
(1) the gallium oxide film prepared by the invention is amorphous, the absorption edge is in the deep ultraviolet band, the obtained deep ultraviolet photoelectric detector can respond under deep ultraviolet light, and the signal-to-noise ratio can reach 10 at most4
(2) The invention adopts the pulse laser deposition method to prepare the amorphous gallium oxide film, has flexible and adjustable process parameters, short deposition period and high efficiency, and is suitable for industrial production application.
Drawings
Fig. 1 is a schematic structural diagram of a deep ultraviolet amorphous gallium oxide photodetector provided by the present invention.
Wherein: 1-a substrate; 2-amorphous gallium oxide thin film; 3-interdigital electrode.
Detailed Description
The technical solution of the present invention is further explained by the following embodiments. It should be understood by those skilled in the art that the examples are only for the understanding of the present invention and should not be construed as the specific limitations of the present invention.
Example 1
The present embodiment provides a deep ultraviolet amorphous gallium oxide photodetector and a method for manufacturing the same, as shown in fig. 1, the photodetector includes a substrate 1, an amorphous gallium oxide thin film 2, and an interdigital electrode 3, which are sequentially disposed; the preparation method comprises the following steps:
(1) preparing an amorphous gallium oxide film 2 on the surface of a substrate 1 by adopting a pulse laser deposition system to obtain a film sample, and specifically, the method comprises the following steps:
(a) ultrasonically cleaning a C-surface sapphire substrate 1 with the thickness of 0.5mm by using acetone, drying the substrate 1 by using high-purity nitrogen, and sticking the substrate on a heating support by using silver colloid after drying the substrate by using high-purity nitrogen;
(b) placing the heating support on a heating table, and baking at 150 ℃ for 20min until the adhesive on the back surface of the substrate 1 is fully dried;
(c) placing the heating support in a chamber, and vacuumizing to an absolute vacuum degree of 2.5 × 10-4Depositing the film after Pa, the oxygen partial pressure is 0.7Pa, the deposition temperature is 240 ℃, and the laser energy is 1.5J/cm2The laser frequency is 10Hz, the adopted target material is a gallium oxide ceramic target with the purity of 99.995 percent, the target spacing is 55mm, the pulse frequency is 10000 times, and the deposition thickness is 150 nm;
(2) preparing an interdigital electrode 3 on the surface of one side of the film sample to obtain the deep ultraviolet amorphous gallium oxide photoelectric detector, wherein the specific operation comprises the following steps:
(d) cleaning: carrying out ultrasonic cleaning on the film sample by adopting acetone;
(e) and (3) drying: blowing the acetone on the surface of the film sample by high-purity nitrogen;
(f) spin coating: placing a film sample on a spin coater, dropwise adding negative glue on the surface of one side of a film of the film sample, and starting rotation operation, wherein the set rotation speed is 4000rpm, and the time is 60 s;
(g) pre-baking: placing the film sample on a heating table, and baking for 60s at 90 ℃;
(h) ultraviolet photoetching: placing the film sample under a photoetching plate for exposure for 7 s;
(i) post-baking: placing the film sample on a heating table, and baking for 120s at 95 ℃;
(j) and (3) developing: developing the film sample for 35s by using AR300-26 developing solution;
(k) fixing: fixing the film sample for 45s by using deionized water;
(l) Magnetron sputtering: placing the film sample in a radio frequency magnetic control system for metal deposition, and preparing an interdigital electrode 3 which is made of platinum and has the thickness of 100nm on the surface of one side of the film sample;
(m) peeling: soaking the film sample in acetone, removing redundant residual glue and drying;
(n) checking: and observing the etched pattern by using an optical microscope, and confirming whether the size of the interdigital electrode is consistent with the size of the pattern on the photoetching plate.
Example 2
The present embodiment provides a deep ultraviolet amorphous gallium oxide photodetector and a method for manufacturing the same, as shown in fig. 1, the photodetector includes a substrate 1, an amorphous gallium oxide thin film 2, and an interdigital electrode 3, which are sequentially disposed; the preparation method comprises the following steps:
(1) preparing an amorphous gallium oxide film 2 on the surface of a substrate 1 by adopting a pulse laser deposition system to obtain a film sample, and specifically, the method comprises the following steps:
(a) ultrasonically cleaning a C-surface sapphire substrate 1 with the thickness of 0.4mm by using acetone, drying the substrate 1 by using high-purity nitrogen, and sticking the substrate on a heating support by using silver colloid after drying the substrate by using high-purity nitrogen;
(b) placing the heating support on a heating table, and baking for 30min at 100 ℃ until the adhesive on the back of the substrate 1 is fully dried;
(c) placing the heating support in a chamber, vacuumizing to an absolute vacuum degree of 1 × 10-4Carrying out film deposition after Pa, wherein the oxygen partial pressure is 1.3Pa, the deposition temperature is 25 ℃, and the laser energy is 2J/cm2The laser frequency is 8Hz, the adopted target material is a gallium oxide ceramic target with the purity of 99.99 percent, the target distance is 50mm, the pulse frequency is 12000 times, and the deposition thickness is 160 nm;
(2) preparing an interdigital electrode 3 on the surface of one side of the film sample to obtain the deep ultraviolet amorphous gallium oxide photoelectric detector, wherein the specific operation comprises the following steps:
(d) cleaning: carrying out ultrasonic cleaning on the film sample by adopting acetone;
(e) and (3) drying: blowing the acetone on the surface of the film sample by high-purity nitrogen;
(f) spin coating: placing a film sample on a spin coater, dropwise adding negative glue on the surface of one side of a film of the film sample, and starting rotation operation, wherein the set rotation speed is 3000rpm and the time is 80 s;
(g) pre-baking: placing the film sample on a heating table, and baking for 80s at 80 ℃;
(h) ultraviolet photoetching: placing the film sample under a photoetching plate for exposure for 6 s;
(i) post-baking: placing the film sample on a heating table, and baking for 140s at 90 ℃;
(j) and (3) developing: developing the film sample for 30s by using AR300-26 developing solution;
(k) fixing: fixing the film sample for 30s by using deionized water;
(l) Magnetron sputtering: placing the film sample in a radio frequency magnetic control system for metal deposition, and preparing an interdigital electrode 3 which is made of platinum and has the thickness of 80nm on the surface of one side of the film sample;
(m) peeling: soaking the film sample in acetone, removing redundant residual glue and drying;
(n) checking: and observing the etched pattern by using an optical microscope, and confirming whether the size of the interdigital electrode is consistent with the size of the pattern on the photoetching plate.
Example 3
The present embodiment provides a deep ultraviolet amorphous gallium oxide photodetector and a method for manufacturing the same, as shown in fig. 1, the photodetector includes a substrate 1, an amorphous gallium oxide thin film 2, and an interdigital electrode 3, which are sequentially disposed; the preparation method comprises the following steps:
(1) preparing an amorphous gallium oxide film 2 on the surface of a substrate 1 by adopting a pulse laser deposition system to obtain a film sample, and specifically, the method comprises the following steps:
(a) ultrasonically cleaning a C-surface sapphire substrate 1 with the thickness of 0.6mm by using acetone, drying the substrate 1 by using high-purity nitrogen, and sticking the substrate on a heating support by using silver colloid after drying the substrate by using high-purity nitrogen;
(b) placing the heating support on a heating table, and baking for 10min at 200 ℃ until the adhesive on the back surface of the substrate 1 is fully dried;
(c) placing the heating support in a chamber, and vacuumizing to an absolute vacuum degree of 5 × 10-4Depositing the film after Pa, oxygen partial pressure is 0.13Pa, deposition temperature is 450 ℃, and laser energy is 1J/cm2The laser frequency is 12Hz, the adopted target material is a gallium oxide ceramic target with the purity of 99.999 percent, the target distance is 60mm, the pulse frequency is 8000 times, and the deposition thickness is 140 nm;
(2) preparing an interdigital electrode 3 on the surface of one side of the film sample to obtain the deep ultraviolet amorphous gallium oxide photoelectric detector, wherein the specific operation comprises the following steps:
(d) cleaning: carrying out ultrasonic cleaning on the film sample by adopting acetone;
(e) and (3) drying: blowing the acetone on the surface of the film sample by high-purity nitrogen;
(f) spin coating: placing a film sample on a spin coater, dropwise adding negative glue on the surface of one side of a film of the film sample, and starting rotation operation, wherein the set rotation speed is 5000rpm, and the time is 40 s;
(g) pre-baking: placing the film sample on a heating table, and baking for 40s at 100 ℃;
(h) ultraviolet photoetching: placing the film sample under a photoetching plate for exposure for 8 s;
(i) post-baking: placing the film sample on a heating table, and baking for 100s at 100 ℃;
(j) and (3) developing: developing the film sample for 40s by using AR300-26 developing solution;
(k) fixing: fixing the film sample for 60s by using deionized water;
(l) Magnetron sputtering: placing the film sample in a radio frequency magnetic control system for metal deposition, and preparing an interdigital electrode 3 which is made of platinum and has the thickness of 120nm on the surface of one side of the film sample;
(m) peeling: soaking the film sample in acetone, removing redundant residual glue and drying;
(n) checking: and observing the etched pattern by using an optical microscope, and confirming whether the size of the interdigital electrode is consistent with the size of the pattern on the photoetching plate.
Example 4
The present embodiment provides a deep ultraviolet amorphous gallium oxide photodetector and a method for manufacturing the same, as shown in fig. 1, the photodetector includes a substrate 1, an amorphous gallium oxide thin film 2, and an interdigital electrode 3, which are sequentially disposed; the preparation method is the same as that of example 1 except that the deposition temperature in step (c) is increased to 500 ℃, and thus the description is omitted.
Example 5
The present embodiment provides a deep ultraviolet amorphous gallium oxide photodetector and a method for manufacturing the same, as shown in fig. 1, the photodetector includes a substrate 1, an amorphous gallium oxide thin film 2, and an interdigital electrode 3, which are sequentially disposed; the preparation method is the same as that of example 1 except that the target pitch in step (c) is changed to 45mm, and thus the description is omitted.
Example 6
The present embodiment provides a deep ultraviolet amorphous gallium oxide photodetector and a method for manufacturing the same, as shown in fig. 1, the photodetector includes a substrate 1, an amorphous gallium oxide thin film 2, and an interdigital electrode 3, which are sequentially disposed; the preparation method is the same as that of example 1 except that the target pitch in step (c) is changed to 65mm, and thus the description is omitted.
Comparative example 1
The present comparative example provides a deep ultraviolet amorphous gallium oxide photodetector and a method for manufacturing the same, as shown in fig. 1, the photodetector includes a substrate 1, an amorphous gallium oxide thin film 2, and an interdigital electrode 3, which are sequentially disposed; the preparation method is the same as that of example 1 except that the oxygen partial pressure in step (c) is changed to 0.1Pa, and thus the details are not repeated herein.
Comparative example 2
The present comparative example provides a deep ultraviolet amorphous gallium oxide photodetector and a method for manufacturing the same, as shown in fig. 1, the photodetector includes a substrate 1, an amorphous gallium oxide thin film 2, and an interdigital electrode 3, which are sequentially disposed; the preparation method is the same as that of example 1 except that the oxygen partial pressure in step (c) is changed to 1.5Pa, and thus the details are not repeated herein.
Comparative example 3
The present comparative example provides a method for preparing a deep ultraviolet amorphous gallium oxide photodetector using a magnetron sputtering system, the method comprising the steps of:
(1) cleaning a substrate and then placing the substrate on a sample holder in a pre-vacuum chamber;
(2) evacuating the pre-vacuum chamber to 2X 10-6Torr below;
(3) sending the sample to a main vacuum chamber and vacuumizing to 1 × 10-6Torr below;
(4) adjusting the oxygen flow to be 2sccm, the sputtering power to be 50W and the sputtering time to be 30 min;
(5) and (5) sputtering and sampling after the sputtering is finished.
In the present invention, the pulsed laser deposition system described in examples 1-6 and comparative examples 1-2 was of the type PLD-450, and the pulsed laser in the deposition system was of the type COMPEX Pro 102F.
The photocurrent and dark current generated by the photodetectors obtained in examples 1 to 6 and comparative examples 1 to 3 under the irradiation of ultraviolet light in the deep ultraviolet band were measured using a semiconductor analytical tester (Keithley, 4200-SCS), and the signal-to-noise ratio of each device was calculated as shown in table 1.
TABLE 1
Figure BDA0003142464190000161
As can be seen from Table 1: with the increase of the oxygen partial pressure, the oxygen vacancy in the film is reduced, when the oxygen partial pressure is 1.3Pa, the device performance is optimal, and the signal-to-noise ratio can reach 1 x 104(ii) a When the target distance is 55mm, the plasma plume is deposited on the thin film on the substrate and is uniformly distributed, and the quality and the performance are better; when the temperature is above 450 ℃, the film begins to crystallize, the photoresponse gain is reduced, and the signal-to-noise ratio is reduced.
Therefore, the gallium oxide film prepared by the invention is amorphous, the absorption edge is positioned in the deep ultraviolet band, the obtained deep ultraviolet photoelectric detector can respond under deep ultraviolet light, and the signal-to-noise ratio can reach 10 at most4(ii) a In addition, the invention adopts the pulse laser deposition method to prepare the amorphous gallium oxide film, has flexible and adjustable process parameters, short deposition period and high efficiency, and is suitable for industrial production application.
The applicant declares that the above description is only a specific embodiment of the present invention, but the scope of the present invention is not limited thereto, and it should be understood by those skilled in the art that any changes or substitutions that can be easily conceived by those skilled in the art within the technical scope of the present invention are within the scope and disclosure of the present invention.

Claims (10)

1. A preparation method of a deep ultraviolet amorphous gallium oxide photoelectric detector is characterized by comprising the following steps:
(1) preparing an amorphous gallium oxide film on the surface of the substrate by adopting a pulse laser deposition method to obtain a film sample;
(2) preparing an interdigital electrode on the surface of one side of the film sample by adopting an ultraviolet photoetching method and a magnetron sputtering method in sequence to obtain a deep ultraviolet amorphous gallium oxide photoelectric detector;
wherein the oxygen partial pressure of the pulse laser deposition method in the step (1) is 0.13-1.3 Pa.
2. The preparation method according to claim 1, wherein the pulsed laser deposition method of step (1) is carried out in a pulsed laser deposition system, and the specific operation comprises the following steps:
(a) cleaning and drying the substrate, and then sticking the substrate on a heating support;
(b) placing the heating support on a heating table, and drying the adhesive on the back of the substrate;
(c) and placing the heating support in a cavity, vacuumizing and depositing a thin film.
3. The method of claim 2, wherein step (a) the substrate comprises C-plane sapphire;
preferably, the substrate of step (a) has a thickness of 0.4-0.6 mm;
preferably, the cleaning of step (a) comprises ultrasonic cleaning;
preferably, the cleaning solution used in the cleaning in the step (a) comprises acetone;
preferably, the drying of step (a) comprises high purity nitrogen blow drying;
preferably, the adhesive used in the step (a) comprises silver adhesive;
preferably, the temperature for drying in step (b) is 100-;
preferably, the drying time in the step (b) is 10-30 min.
4. The method of claim 2 or 3, wherein the degree of vacuum of step (c) is less than or equal to 5 x 10-4Pa;
Preferably, the deposition temperature of the thin film deposition of the step (c) is 25-450 ℃;
preferably, the laser energy for the film deposition in step (c) is 1-2J/cm2
Preferably, the laser frequency of the film deposition in the step (c) is 8-12 Hz;
preferably, the target material for the film deposition in the step (c) is a gallium oxide ceramic target;
preferably, the purity of the gallium oxide ceramic target is more than or equal to 99.99 percent;
preferably, the target spacing for the thin film deposition of step (c) is 50-60 mm;
preferably, the number of pulses for depositing the thin film in step (c) is 8000-;
preferably, the deposition thickness of the thin film deposition in the step (c) is 140-160 nm.
5. The production method according to any one of claims 1 to 4, wherein the UV lithography in the step (2) is exposure by placing a film sample under a reticle;
preferably, the exposure time is 6-8 s;
preferably, the magnetron sputtering method in the step (2) is to place the film sample in a radio frequency magnetron system for metal deposition, and prepare an interdigital electrode on the surface of one side of the film sample;
preferably, the material of the interdigital electrode comprises platinum;
preferably, the thickness of the interdigital electrode is 80-120 nm.
6. The method according to any one of claims 1 to 5, wherein the UV lithography in step (2) further comprises sequentially cleaning, drying, spin coating and pre-baking the film sample;
preferably, the step (2) further comprises the steps of performing post-baking, developing and fixing on the film sample in sequence between the ultraviolet lithography method and the magnetron sputtering method;
preferably, the magnetron sputtering method in the step (2) further comprises sequentially peeling and inspecting the film sample.
7. The production method according to claim 6, wherein the cleaning means includes ultrasonic cleaning;
preferably, the cleaning solution used for cleaning comprises acetone;
preferably, the drying mode comprises high-purity nitrogen blow drying;
preferably, the whirl coating is to place the film sample on a spin coater, drip negative glue on the surface of one side of the film sample and start the rotation operation;
preferably, the rotating speed of the rotating operation is 3000-;
preferably, the time of the rotating operation is 40-80 s;
preferably, the pre-baking is performed on a heated platen;
preferably, the temperature of the pre-baking is 80-100 ℃;
preferably, the pre-baking time is 40-80 s;
preferably, the postbaking is performed on a heated platen;
preferably, the temperature of the postbaking is 90-100 ℃;
preferably, the time of the post-drying is 100-140 s;
preferably, the developing solution used for developing comprises AR300-26 developing solution;
preferably, the development time is 30-40 s;
preferably, the fixing solution used for fixing comprises deionized water;
preferably, the fixing time is 30-60 s;
preferably, the peeling is to soak the film sample in acetone, remove the redundant residual glue and blow dry the film sample;
preferably, the inspection is to use an optical microscope to observe the etched pattern, and confirm whether the size of the interdigital electrode is consistent with the size of the pattern on the photomask.
8. The method of any one of claims 1 to 7, comprising the steps of:
(1) preparing an amorphous gallium oxide film on the surface of a substrate by adopting a pulse laser deposition system to obtain a film sample, and specifically, the method comprises the following steps:
(a) ultrasonically cleaning a C-surface sapphire substrate with the thickness of 0.4-0.6mm by using acetone, drying the substrate by using high-purity nitrogen, and adhering the substrate to a heating support by using silver colloid after drying the substrate by using high-purity nitrogen;
(b) placing the heating support on a heating table, and baking at 100-200 deg.C for 10-30min until the adhesive on the back of the substrate is fully dried;
(c) placing the heating support in a cavity, vacuumizing to an absolute vacuum degree of less than or equal to 5 multiplied by 10-4Depositing film after Pa, oxygen partial pressure 0.13-1.3Pa, deposition temperature 25-450 deg.C, laser energy 1-2J/cm2The laser frequency is 8-12Hz, the adopted target material is a gallium oxide ceramic target with the purity of more than or equal to 99.99 percent, the target distance is 50-60mm, the pulse frequency is 8000-12000 times, and the deposition thickness is 140-160 nm;
(2) preparing an interdigital electrode on the surface of one side of the film sample to obtain the deep ultraviolet amorphous gallium oxide photoelectric detector, wherein the specific operation comprises the following steps:
(d) cleaning: carrying out ultrasonic cleaning on the film sample by adopting acetone;
(e) and (3) drying: blowing the acetone on the surface of the film sample by high-purity nitrogen;
(f) spin coating: placing a film sample on a spin coater, dropwise adding negative glue on the surface of one side of a film of the film sample, and starting rotation operation, wherein the set rotation speed is 3000 plus 5000rpm, and the time is 40-80 s;
(g) pre-baking: placing the film sample on a heating table, and baking for 40-80s at 80-100 ℃;
(h) ultraviolet photoetching: placing the film sample under a photoetching plate for exposure for 6-8 s;
(i) post-baking: placing the film sample on a heating table, and baking for 140s at 90-100 ℃;
(j) and (3) developing: developing the film sample for 30-40s by using AR300-26 developing solution;
(k) fixing: fixing the film sample for 30-60s by using deionized water;
(l) Magnetron sputtering: placing the film sample in a radio frequency magnetic control system for metal deposition, and preparing an interdigital electrode which is made of platinum and has the thickness of 80-120nm on the surface of one side of the film sample;
(m) peeling: soaking the film sample in acetone, removing redundant residual glue and drying;
(n) checking: and observing the etched pattern by using an optical microscope, and confirming whether the size of the interdigital electrode is consistent with the size of the pattern on the photoetching plate.
9. The deep ultraviolet amorphous gallium oxide photoelectric detector prepared by the preparation method according to any one of claims 1 to 8, wherein the photoelectric detector comprises a substrate, an amorphous gallium oxide film and interdigital electrodes which are sequentially arranged.
10. Use of the photodetector of claim 9 in the fields of analytical testing, environmental monitoring, industrial automation control, space communication and missile tracking.
CN202110738976.9A 2021-06-30 2021-06-30 Deep ultraviolet amorphous gallium oxide photoelectric detector and preparation method and application thereof Pending CN113451447A (en)

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