CN111524787A - Nano cold cathode flat ultraviolet light source device and preparation method thereof - Google Patents
Nano cold cathode flat ultraviolet light source device and preparation method thereof Download PDFInfo
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- CN111524787A CN111524787A CN202010246730.5A CN202010246730A CN111524787A CN 111524787 A CN111524787 A CN 111524787A CN 202010246730 A CN202010246730 A CN 202010246730A CN 111524787 A CN111524787 A CN 111524787A
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- H01J63/06—Lamps with luminescent screen excited by the ray or stream
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- H01J—ELECTRIC DISCHARGE TUBES OR DISCHARGE LAMPS
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- H—ELECTRICITY
- H01—ELECTRIC ELEMENTS
- H01J—ELECTRIC DISCHARGE TUBES OR DISCHARGE LAMPS
- H01J63/00—Cathode-ray or electron-stream lamps
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- H—ELECTRICITY
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Abstract
The invention discloses a nano cold cathode flat ultraviolet light source device which comprises a nano cold cathode substrate and a gallium oxide film anode substrate, wherein the nano cold cathode substrate and the gallium oxide film anode substrate are fixed together in an insulated manner through an isolator and keep a vacuum gap. The invention also discloses a preparation method of the nano cold cathode flat ultraviolet light source device, which comprises the steps of preparing the nano cold cathode substrate and the gallium oxide film anode substrate and assembling. The nano cold cathode and the gallium oxide film have the characteristic of easy large-area preparation, and the flat ultraviolet light source can realize a low-cost large-area plane ultraviolet light source and has important application in the fields of ultraviolet exposure, disinfection, curing and the like.
Description
Technical Field
The invention relates to the field of light sources, in particular to a nano cold cathode flat ultraviolet light source device.
Background
Ultraviolet light is an electromagnetic wave having a wavelength ranging from 100 to 400 nanometers. Ultraviolet light has a shorter wavelength and higher photon energy than visible and infrared light. Thus, ultraviolet light sources are widely used in photolithography, phototherapy, photocuring, disinfection, sterilization, deodorization, optical cleaning, scientific research, and the like.
There have been some studies on the realization of an ultraviolet light source using a cold cathode electron source. For example, Sung Taeyoo et al use carbon nanotubes as cold cathodes and Zn2SiO4The film is used as anode, ultraviolet light source is prepared, and deep ultraviolet light luminescence (J.Vac.Sci.Technol.B 36(2),02C103,2018) with wavelengths of 208, 226 and 244nm is obtained under 7kV anode voltage]. However, the temperature of the preparation process of the carbon nanotube is limited, so that the carbon nanotube is difficult to manufacture on a large-area glass substrate, and the application of the carbon nanotube in a large-area ultraviolet flat light source is limited.
Disclosure of Invention
The invention aims to overcome the problems of the prior ultraviolet light source technology in realizing shorter wavelength ultraviolet light emission and plane light emission, and provides a vacuum plane ultraviolet light source which consists of a large-area nano cold cathode and a gallium oxide film and utilizes the cathode ray luminescence principle and a nano cold cathode flat ultraviolet light source device which can realize short wavelength, high luminous intensity and plane light emission.
The invention adopts the following technical scheme to solve the problems in the prior art:
a nano cold cathode flat ultraviolet light source device comprises a nano cold cathode substrate and a gallium oxide film anode substrate, wherein the nano cold cathode substrate and the gallium oxide film anode substrate are fixed together in an insulated mode through an isolator and keep a vacuum gap.
Gallium oxide is a transparent semiconductor, has a wide bandgap of about 4.9eV at room temperature, corresponds to an intrinsic luminescence wavelength of 253nm, and can be prepared in a large area by a vacuum coating method.
Preferably, the distance between the gallium oxide film anode substrates is 0.1 mm-0.5 mm.
Preferably, the cold cathode substrate comprises a glass substrate, a cathode electrode and a nanowire lattice array distributed on the cathode electrode. The invention can be used for preparing the nano cold cathode on the flat substrate in a large area and a localized manner.
Preferably, the material of the nano cold cathode lattice array is oxide nanowires. The nanometer cold cathode comprises an array formed by a zinc oxide nanowire, a copper oxide nanowire or a tungsten oxide nanowire lattice which are prepared in a localized mode. The nanometer cold cathode such as zinc oxide nanometer wire can be prepared on a large-area substrate by a thermal oxidation method. The large-area nano cold cathode is used as a cathode, and the gallium oxide film is used as an anode, so that a large-area ultraviolet light source can be realized.
Preferably, the gallium oxide film anode substrate comprises a substrate, an anode electrode and a gallium oxide film, wherein the anode electrode is connected with a lead-out wire connected with an external power supply, and the substrate is ultraviolet transparent. The ultraviolet transparent substrate comprises quartz glass and other crystal substrates with high ultraviolet transmittance and high temperature resistance, and the anode electrode is connected with a lead-out wire connected with an external power supply.
Preferably, the voltage range applied by the external power supply to the nanometer cold cathode substrate and the gallium oxide thin film anode substrate is 1 kV-20 kV. When the nano cold cathode flat ultraviolet light source device works, high voltage is applied to the anode, the cold cathode generates emission current, and emitted electrons bombard the gallium oxide film so as to emit short-wavelength light. The luminous intensity of the light source can be adjusted by the distance between the cathode and the anode, the voltage of the anode and the current of the cathode.
Preferably, the anode electrode is made of a transparent conductive film, the thickness of the transparent conductive film is 50-200 nm, and the thickness of the gallium oxide film is 100-500 nm. Including ITO, IZO, IGZO, etc., which have good conductivity, can effectively conduct away the current bombarded onto the anode without charge accumulation.
The invention also provides a preparation method of the nano cold cathode flat ultraviolet light source device.
S1 preparing a nanometer cold cathode substrate and a gallium oxide film anode substrate,
preparing a nano cold cathode substrate:
preparing a cathode electrode on a substrate, preparing a nano cold cathode dot matrix array on the cathode electrode, and thermally oxidizing the nano cold cathode dot matrix array to obtain a nanowire cold cathode substrate;
preparing a gallium oxide film anode substrate:
preparing an anode electrode on an ultraviolet transparent substrate, preparing a gallium oxide film on the anode electrode, and finally annealing the prepared gallium oxide film at high temperature to obtain a gallium oxide film anode substrate;
s2 assembling:
and the nano cold cathode substrate and the gallium oxide film anode substrate are isolated and fixed by adopting a high-voltage insulating isolator.
Preferably, the annealing temperature of the gallium oxide film is 700-1200 ℃, and the annealing atmosphere of the gallium oxide film is oxidizing gas. The oxidizing gas is air, oxygen, etc. The annealing process of the gallium oxide thin film can convert an amorphous structure of gallium oxide into a polycrystalline structure. The crystallization performance of the gallium oxide film is regulated and controlled through different annealing temperatures and atmospheres, and the gallium oxide film anode substrates with different cathode ray luminescence characteristics are obtained, so that the luminescence wavelength of the flat ultraviolet light source is regulated. The higher the annealing temperature, the better the crystallinity.
Preferably, the preparation process of the nano cold cathode substrate is as follows: and (3) preparing the nano cold cathode lattice array in a localized manner by adopting a method combining a photoetching method and film preparation, and finally performing thermal oxidation growth at the heating temperature of 300-600 ℃. The thermal oxidation growth atmosphere is an oxidizing gas such as air or oxygen. The field emission characteristics of the nanometer cold cathode can be regulated and controlled through different growth temperatures, growth atmosphere concentrations and the like in the thermal oxidation process, so that the nanometer cold cathode substrate with different field emission characteristics is obtained, and the luminous intensity, the luminous power density and the luminous stability of the flat ultraviolet light source are optimized.
Compared with the prior art, the invention has the beneficial effects that:
the nano cold cathode flat ultraviolet light source device provided by the invention adopts the nano cold cathode to realize large-area uniform high field emission current, and can realize low-cost preparation of large-area flat light emitting devices. By adjusting the voltage applied to the device, the luminous intensity and the optical power density of the ultraviolet light source device can be adjusted. The light-emitting wavelength of the flat ultraviolet light source can be adjusted by adjusting and controlling the crystallization property of the gallium oxide film through different annealing temperatures and atmospheres in the gallium oxide film annealing process.
The nano cold cathode and the gallium oxide film have the characteristic of easy large-area preparation, so the flat ultraviolet light source can realize a low-cost large-area plane ultraviolet light source, and has important application in the fields of ultraviolet exposure, disinfection, curing and the like.
Drawings
FIG. 1 is a schematic structural diagram of a nano cold cathode flat ultraviolet light source device,
FIG. 2 is a flow chart of a process for preparing a ZnO nanowire cold cathode array,
FIG. 3 is an SEM topography of a ZnO nanowire cold cathode array. (a) Low magnification; (b) the high magnification factor is obtained by the following steps,
FIG. 4 is a flow chart of the preparation of a gallium oxide thin film anode substrate,
FIG. 5 is a light-emitting working diagram of a nanometer cold cathode flat ultraviolet light source device,
FIG. 6 is an enlarged view of the light-emitting condition of the nano cold cathode flat ultraviolet light source device,
FIG. 7 XRD patterns of gallium oxide films annealed at different temperatures,
FIG. 8 shows the luminescence spectra of gallium oxide films at different annealing temperatures under electron bombardment,
description of the reference numerals
The cathode substrate 11, the cathode electrode 12, the nanometer cold cathode array 13, the separator 14, the gallium oxide film 15, the anode electrode 16, the anode substrate 17, the power supply 18, the photoresist 23, the Zn film 24 and the ZnO nanowire 25.
Detailed Description
The present invention will be further described with reference to the following embodiments.
Example 1
The flat ultraviolet light source device of the invention mainly comprises a cold cathode substrate prepared with a nanometer cold cathode and an anode substrate prepared with a gallium oxide film (figure 1). And a cathode electrode and a nano cold cathode electron source array are directly prepared on the cold cathode substrate. An anode electrode and a gallium oxide film are sequentially prepared on the anode substrate. The cathode substrate and the anode substrate are fixed together in an insulated manner by a separator, and a vacuum gap is maintained between the cathode substrate and the anode substrate.
Firstly, a cold cathode substrate is prepared, and fig. 2 is a flow chart of a preparation process of the ZnO nanowire cold cathode array. The cold cathode substrate is a glass substrate, and an ITO electrode 22 is first prepared on the glass substrate by a magnetron sputtering method as shown in fig. 2 (b). The thickness of the ITO film layer is about 540nm, and the prepared ITO film is subjected to heat preservation annealing at 450 ℃ for 3 hours, so that the conductivity of the ITO film is improved. And then preparing the ZnO nanowire lattice array in a localized manner by adopting a photoetching method. The method comprises the following steps of firstly, carrying out ultrasonic cleaning series on an ITO-plated glass sample, then, carrying out spin coating on photoresist 23 as shown in figure 2(c), then, baking the sample at the temperature of 120 ℃ for 2min, taking out the sample after baking, cooling to room temperature, exposing the sample by using an exposure machine, then, immersing the sample in a developing solution for developing, finally, cleaning by using deionized water and drying by blowing to obtain a dot matrix pattern of a required zinc film as shown in figure 2 (d); a Zn thin film 24 having a thickness of about 1.2 μm is deposited on a glass substrate, on which a cathode lattice pattern is lithographed, using an electron beam evaporation technique, as shown in fig. 2 (e). As shown in fig. 2(f), a lift-off process is adopted to form a Zn film pattern lattice, a sample plated with a Zn film is soaked in an acetone solution, a non-lattice area of the Zn film naturally falls off to form the Zn film lattice, and the Zn film lattice is cleaned and dried by deionized water; finally, the sample is placed in the middle of a rapid heating box furnace, thermal oxidation is carried out under the oxygen atmosphere, the temperature rising curve is set to rise from the initial temperature of 20 ℃ to 470 ℃ at about 2.5 ℃/min for 3 hours, then heat preservation is carried out for 3 hours, and oxygen with the flow rate of 3.6slm is introduced within 6 hours. And then stopping ventilation, opening the cavity door, and naturally cooling to room temperature to obtain the ZnO nanowire cold cathode substrate, as shown in fig. 2 (g). The morphology of the ZnO nanowire cold cathode array prepared by the process in a Scanning Electron Microscope (SEM) is shown in figure 3. The growth height of the ZnO nanowire is about 3.7 μm, and the tip diameter is about 25 nm.
The preparation process of the gallium oxide film anode substrate is shown in fig. 4. The anode substrate is composed of an anode quartz glass substrate 31, an anode electrode 32 and a gallium oxide film 33, wherein the anode electrode 32 is an ITO electrode. The preparation process comprises the following steps: firstly, ultrasonic cleaning is carried out on a quartz glass substrate, an area needing film coating on the substrate is exposed, an ITO film is deposited on the area by using a magnetron sputtering instrument, and the thickness of the ITO film layer is about 540nm, as shown in figure 4 (b). Then, the ITO is annealed at 450 ℃ for 3 hours, so that the light transmittance and the conductivity of the ITO are improved. After the ITO-coated quartz glass sample was subjected to an ultrasonic cleaning series, a gallium oxide film having a thickness of about 100nm was deposited on the exposed area of the anode electrode using electron beam evaporation, as shown in fig. 4 (c). And finally, annealing the gallium oxide film by adopting a rapid heating tube type electric furnace at 900 ℃ for 2 hours.
The prepared anode and cathode substrates were separated by a separator and assembled together, the distance between the nano cold cathode substrate and the gallium oxide thin film anode substrate was 0.25mm in this example, the prepared device was placed in a vacuum with a degree of vacuum maintained at 1 × 10-5Pa, then connecting a lead wire on an ITO electrode of the anode to be connected with an external power supply, wherein the voltage applied on the ITO electrode is 1 kV-20 kV. Fig. 5 is a photograph of the device during light emitting operation, fig. 6(a) is an enlarged view of the light emitting condition of the device, and it can be seen from fig. 6(b) that the light source realizes uniform and stable light emission over a large area as a function of time.
Example 2
In order to explore the influence of different annealing temperatures on the crystallization performance of a gallium oxide film and realize the regulation and control of the luminescence wavelength, a gallium oxide film sample is prepared by an electron beam evaporation technology, and the film is annealed for 2 hours in the atmosphere of a tubular furnace at 800 ℃ and 1050 ℃ respectively. Figure 7 is an XRD pattern of a gallium oxide film annealed at two temperature conditions. As can be seen from fig. 7(a), the XRD pattern of the non-annealed gallium oxide shows no significant peak position of the crystal phase, indicating that the structure is an amorphous structure. As shown in fig. 7(b), the XRD pattern of the gallium oxide thin film with the annealing temperature of 800 ℃ clearly shows the peak position of (002) crystal orientation at about 31.5 °. The XRD pattern of the gallium oxide thin film with the annealing temperature of 1050 deg.c, as shown in fig. 7(c), is larger in the peak intensity of (002) crystal orientation at 31.5 deg.. XRD results of the gallium oxide thin film annealed under the two temperature conditions show that the crystallinity of the gallium oxide thin film annealed at 1050 ℃ is better than that of the gallium oxide thin film annealed at 800 ℃, namely the crystallinity of the thin film can be adjusted by the annealing temperature, and the higher the annealing temperature is, the better the crystallinity is.
FIGS. 8(a) and (b) are the luminescence spectra of the two annealed samples, respectively, under electron beam bombardment. Can be seen. The above results show that the luminescence peak of the 800 ℃ annealed gallium oxide film is 422nm, and the luminescence peak of the 1050 ℃ annealed gallium oxide film is 372nm and 411 nm. The light-emitting peak position of gallium oxide is deviated at different temperatures, and the higher the annealing temperature is, the shorter the wavelength of the light-emitting peak position is. That is, the crystalline characteristics of gallium oxide can be improved by high temperature annealing, so that the luminescence peak position is closer to the intrinsic peak position of the material. Therefore, the crystallization performance of the gallium oxide film can be regulated and controlled through different annealing temperatures and atmospheres, so that the light-emitting wavelength of the flat ultraviolet light source can be regulated.
It should be understood that the above-described embodiments of the present invention are merely examples for clearly illustrating the present invention, and are not intended to limit the embodiments of the present invention. Other variations and modifications will be apparent to persons skilled in the art in light of the above description. And are neither required nor exhaustive of all embodiments. Any modification, equivalent replacement, and improvement made within the spirit and principle of the present invention should be included in the protection scope of the claims of the present invention.
Claims (10)
1. A nano cold cathode flat ultraviolet light source device is characterized by comprising a nano cold cathode substrate and a gallium oxide film anode substrate, wherein the nano cold cathode substrate and the gallium oxide film anode substrate are fixed together in an insulated mode through an isolator, and a vacuum gap is kept.
2. The device of claim 1, wherein the distance between the cold cathode substrate and the gallium oxide thin film anode substrate is 0.1 mm-0.5 mm.
3. The device as claimed in claim 1, wherein the cold cathode substrate comprises a glass substrate, a cathode electrode and a matrix array of cold cathodes distributed on the cathode electrode.
4. The device as claimed in claim 1, wherein the material of the nano cold cathode lattice array is oxide nanowires.
5. The device of claim 1, wherein the gallium oxide thin film anode substrate comprises a substrate, an anode electrode and a gallium oxide thin film, the anode electrode is connected with a lead-out wire connected with an external power supply, and the substrate is ultraviolet transparent.
6. The device of claim 5, wherein the voltage applied by the external power source to the cold cathode nano-substrate and the gallium oxide thin film anode substrate is in a range of 1kV to 20 kV.
7. The gallium oxide thin film anode substrate according to claim 6, wherein the anode electrode is made of a transparent conductive film, the thickness of the transparent conductive film is 50-200 nm, and the thickness of the gallium oxide thin film is 100-500 nm.
8. A method for preparing the ultraviolet light source device with the nano cold cathode flat plate as claimed in claim 1,
s1 preparing a nanometer cold cathode substrate and a gallium oxide film anode substrate,
preparing a nano cold cathode substrate:
preparing a cathode electrode on a substrate, preparing a nano cold cathode dot matrix array on the cathode electrode, and thermally oxidizing the nano cold cathode dot matrix array to obtain a nanowire cold cathode substrate;
preparing a gallium oxide film anode substrate:
preparing an anode electrode on a substrate, preparing a gallium oxide film on the anode electrode, and finally annealing the prepared gallium oxide film at high temperature to obtain a gallium oxide film anode substrate;
s2 assembling:
and the nanometer cold cathode substrate and the gallium oxide film anode substrate are isolated and fixed by adopting a high-voltage insulating isolator.
9. The method for preparing a nano cold cathode flat ultraviolet light source device according to claim 8, wherein the annealing temperature of the gallium oxide film is 700-1200 ℃, and the annealing atmosphere of the gallium oxide film is oxidizing gas.
10. The method for manufacturing a nano cold cathode flat ultraviolet light source device according to claim 8, wherein the manufacturing process of the nano cold cathode substrate is as follows: and (3) preparing the nano cold cathode lattice array in a localized manner by adopting a method combining a photoetching method and film preparation, and finally performing thermal oxidation growth at the heating temperature of 300-600 ℃.
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2020
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Application publication date: 20200811 |