CN111193188A - Preparation method of single ZnO micron band F-P mode ultraviolet laser diode - Google Patents

Preparation method of single ZnO micron band F-P mode ultraviolet laser diode Download PDF

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CN111193188A
CN111193188A CN202010012967.7A CN202010012967A CN111193188A CN 111193188 A CN111193188 A CN 111193188A CN 202010012967 A CN202010012967 A CN 202010012967A CN 111193188 A CN111193188 A CN 111193188A
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zno
micron band
micron
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gan substrate
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姜明明
阚彩侠
万鹏
孙雨周
吴裕庭
季姣龙
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Nanjing University of Aeronautics and Astronautics
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Nanjing University of Aeronautics and Astronautics
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    • H—ELECTRICITY
    • H01—ELECTRIC ELEMENTS
    • H01S—DEVICES USING THE PROCESS OF LIGHT AMPLIFICATION BY STIMULATED EMISSION OF RADIATION [LASER] TO AMPLIFY OR GENERATE LIGHT; DEVICES USING STIMULATED EMISSION OF ELECTROMAGNETIC RADIATION IN WAVE RANGES OTHER THAN OPTICAL
    • H01S5/00—Semiconductor lasers
    • H01S5/30—Structure or shape of the active region; Materials used for the active region
    • H01S5/32—Structure or shape of the active region; Materials used for the active region comprising PN junctions, e.g. hetero- or double- heterostructures
    • H01S5/327—Structure or shape of the active region; Materials used for the active region comprising PN junctions, e.g. hetero- or double- heterostructures in AIIBVI compounds, e.g. ZnCdSe-laser
    • H—ELECTRICITY
    • H01—ELECTRIC ELEMENTS
    • H01S—DEVICES USING THE PROCESS OF LIGHT AMPLIFICATION BY STIMULATED EMISSION OF RADIATION [LASER] TO AMPLIFY OR GENERATE LIGHT; DEVICES USING STIMULATED EMISSION OF ELECTROMAGNETIC RADIATION IN WAVE RANGES OTHER THAN OPTICAL
    • H01S2304/00—Special growth methods for semiconductor lasers

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  • Condensed Matter Physics & Semiconductors (AREA)
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Abstract

The invention discloses a preparation method of a single ZnO micron band F-P mode ultraviolet laser diode. The method comprises the following steps: cleaning a quartz substrate, a glass substrate and a p-GaN substrate; preparing a Ni/Au alloy electrode on one side of a p-GaN substrate; tightly attaching the p-GaN substrate to the quartz substrate, and preparing a gasket on the quartz substrate to ensure that the gasket is tightly attached and level to the p-GaN substrate; moving the n-ZnO Ga micron band on a glass substrate, ensuring that the micron band is attached to the glass substrate, and pressing indium electrodes at two ends of the micron band; directionally sputtering an Ag nano quasi-particle film on the micro-belt; applying voltage on indium electrodes at two ends of the micron band, converting the Ag nano quasi-particle film into AgNPs, and obtaining an AgNPs @ n-ZnO-Ga micron band composite structure; and transferring the micron band composite structure to a p-GaN substrate to obtain the heterojunction diode. The invention realizes high-quality F-P mode ultraviolet laser.

Description

Preparation method of single ZnO micron band F-P mode ultraviolet laser diode
Technical Field
The invention belongs to the field of semiconductor optoelectronic devices, and particularly relates to a preparation method of an ultraviolet laser diode.
Background
ZnO material is used as a direct band gap and wide forbidden band semiconductor material, has high crystallization quality, has an optical resonant cavity, and is widely applied to light-emitting diodes, sensors and detectors. In 1997, the ultraviolet laser is generated by optical pumping excitation in a zinc oxide material for the first time abroad. In 2001, an optically pumped Fabry-Perot (F-P) mode laser was realized abroad using a zinc oxide nanowire. In 2008, zinc oxide micro-wires and nano-wires are utilized at home and abroad to realize low-threshold high-quality laser in an optical pumping WGM mode. The production of electrically pumped F-P mode lasers using zinc oxide nanowire diodes was reported abroad in 2011. In the same year, the Xuchunxiang topic group of southeast university utilizes ZnO micron lines and gallium nitride heterojunction to realize the electrically pumped WGM mode ultraviolet laser radiation. However, the quality factor of both types of electrically pumped laser radiation is low. In 2018, the lesson group where the inventor is located utilizes n-ZnO: Ga micron bands to realize electrically pumped F-P mode ultraviolet laser, but the threshold value is relatively high. Based on the research background, a ZnO microcavity structure with a higher quality factor is designed, and low-threshold and high-quality electrically pumped ZnO ultraviolet laser is realized, which plays an important role in popularizing the application of ZnO in the aspect of ultraviolet lasers.
Disclosure of Invention
In order to solve the technical problems mentioned in the background technology, the invention provides a preparation method of a single ZnO micron band F-P mode ultraviolet laser diode.
In order to achieve the technical purpose, the technical scheme of the invention is as follows:
the preparation method of the single ZnO micron band F-P mode ultraviolet laser diode comprises the following steps:
(1) ultrasonic cleaning is carried out on the quartz substrate, the glass substrate and the p-GaN substrate, so that cleanness and tidiness of the quartz substrate, the glass substrate and the p-GaN substrate are guaranteed;
(2) preparing a Ni/Au alloy electrode on one side of the p-GaN substrate to be used as an anode of the diode;
(3) tightly attaching the p-GaN substrate to the quartz substrate, and preparing a gasket on the quartz substrate to ensure that the gasket is tightly attached and level to the p-GaN substrate;
(4) moving an n-ZnO-Ga micron belt to the glass substrate to ensure that one surface of the n-ZnO-Ga micron belt is attached to the glass substrate, and pressing indium electrodes at two ends of the n-ZnO-Ga micron belt;
(5) directionally sputtering an Ag nano quasi-particle film on the n-ZnO-Ga micron belt;
(6) applying voltage to indium electrodes at two ends of the n-ZnO and Ga micron band coated by the Ag nano quasi-particle film obtained in the step (5) until the n-ZnO and Ga micron band emits light, converting the Ag nano quasi-particle film into isolated AgNPs at a light-emitting center to obtain an AgNPs @ n-ZnO and Ga micron band composite structure;
(7) for the AgNPs @ n-ZnO and Ga micron band composite structure, removing an indium electrode, and then moving the structure obtained in the step (3), ensuring that one end of the AgNPs @ n-ZnO and Ga micron band composite structure is arranged on the gasket, and the other end of the AgNPs @ n-ZnO and Ga micron band composite structure is arranged on the p-GaN substrate, and ensuring that the AgNPs @ n-ZnO and Ga micron band composite structure does not contact the Ni/Au alloy electrode of the p-GaN substrate; wherein, an indium electrode is pressed at one end of the AgNPs @ n-ZnO: Ga micron band composite structure positioned on the gasket and used as a cathode of the diode.
Further, in the step (1), the ultrasonic cleaning method is as follows:
respectively putting a sample to be cleaned into a trichloroethylene solution, an acetone solution, an ethanol solution and deionized water, and carrying out ultrasonic cleaning by using an ultrasonic cleaning machine; then the sample is put into an oven for drying and then is dried by nitrogen.
Furthermore, in the step (2), a part of the p-GaN substrate is shielded by a mask plate, a part of the p-GaN substrate is exposed, the exposed part is in a round shape, two layers of electrodes are plated on the exposed part of the p-GaN substrate by an electron beam evaporation method to form a Ni/Au alloy electrode, and the thickness of the Ni/Au alloy electrode is 25-35 nm.
Further, in the step (3), the p-GaN substrate is bonded on the quartz substrate by adopting PMMA, so that the P-GaN substrate is transparent and has no bubbles between the P-GaN substrate and the quartz substrate, and the close fit of the P-GaN substrate and the quartz substrate is realized.
Further, in the step (4), an n-ZnO: Ga micron band is horizontally placed on the glass substrate, and the n-ZnO is operated under a microscopeGa micron band, ensuring that one surface of the n-ZnO Ga micron band is jointed with the glass substrate; pressing indium electrodes at two ends of the n-ZnO, Ga micron band to ensure that the indium electrodes, the n-ZnO, Ga micron band and the glass substrate are compactly attached together to form a metal-semiconductor-metal structure; the electron concentration of the n-ZnO-Ga micron band is 1018～1019/cm3Electron mobility of 15-200 cm2V.s; the thickness of the indium electrode is 1-2 um.
Further, in the step (5), shielding the indium-containing electrode parts on two sides of the n-ZnO/Ga micron belt by using a mask plate, sputtering a layer of Ag nano quasi-particle film on the surface of the n-ZnO/Ga micron belt by using a magnetron sputtering instrument, wherein the sputtering target is an Ag target with the purity of 99.9 percent, the working gas is argon, the cavity air pressure is 30-32 Pa, the sputtering current is 28-31 mA, the sputtering time is 300-350 s, and the sputtering area is the n-ZnO/Ga micron belt without indium electrodes on two ends; the thickness of the Ag nano quasi-particle film is 30-50 nm.
Further, in the step (6), the n-ZnO: Ga micron band wrapped by the Ag nano quasi-particle film is placed under a microscope, the microscope is adjusted to enable the n-ZnO: Ga micron band to be a clear image, voltage is applied to indium electrodes at two ends of the n-ZnO: Ga micron band, and the voltage is slowly increased until the n-ZnO: Ga micron band emits light; the source meter for applying the voltage can freely adjust the voltage and the current value, the voltage adjusting range is 0-210V, and the current adjusting range is 0-100 mA.
Further, the thickness of the p-GaN substrate is 300-330 um, and the hole concentration is 5.8 x 1018～1.5*1019/cm3Hole mobility of 20-150 cm2/V·s。
Adopt the beneficial effect that above-mentioned technical scheme brought:
(1) according to the invention, the AgNPs are used for modifying the n-ZnO-Ga micron band, so that the microcavity quality of the n-ZnO-Ga micron band is improved, hot electrons generated by AgNPs mixed quadrupole resonance are injected into the n-ZnO-Ga micron band, the efficiency of the n-ZnO-Ga micron band is greatly improved, and the realization of an electrically pumped n-ZnO-Ga micron band heterojunction diode is facilitated.
(2) According to the invention, by constructing an AgNPs @ n-ZnO/Ga micron band/P-GaN heterojunction diode structure, stable ultraviolet light emission is realized under current injection, when the injection current reaches a certain threshold value, the heterojunction diode generates a lasing phenomenon, high-quality electrically pumped F-P mode ultraviolet laser is obtained, and the application of the ZnO diode in the field of ultraviolet laser is promoted.
Drawings
FIG. 1 is a scanning electron microscope image of a composite structure of AgNPs @ n-ZnO: Ga micron band of the invention;
FIG. 2 is a schematic structural diagram of the AgNPs @ n-ZnO: Ga micron band/p-GaN heterojunction diode of the present invention; description of reference numerals: 1. a quartz substrate; 2. a gasket; 3. a p-GaN substrate; 4. n-ZnO is Ga micron band; 5. an indium electrode; 6. a Ni/Au alloy electrode; 7. n-ZnO is AgNPs on a Ga micron belt;
FIG. 3 is a graph of the IV curve of the AgNPs @ n-ZnO/Ga micron band/p-GaN heterojunction diode of the present invention;
FIG. 4 is a light-emitting diagram of an AgNPs @ n-ZnO/Ga micron band/p-GaN heterojunction diode of the invention;
FIG. 5 is a spectrum of the AgNPs @ n-ZnO/Ga micron band/p-GaN heterojunction diode of the invention.
Detailed Description
The technical scheme of the invention is explained in detail in the following with the accompanying drawings.
The invention designs a preparation method of a single ZnO micron band F-P mode ultraviolet laser diode, which comprises the following steps:
step 1: ultrasonic cleaning is carried out on the quartz substrate, the glass substrate and the p-GaN substrate, so that cleanness and tidiness of the quartz substrate, the glass substrate and the p-GaN substrate are guaranteed;
step 2: preparing a Ni/Au alloy electrode on one side of the p-GaN substrate to be used as an anode of the diode;
and step 3: tightly attaching the p-GaN substrate to the quartz substrate, and preparing a gasket on the quartz substrate to ensure that the gasket is tightly attached and level to the p-GaN substrate;
and 4, step 4: moving an n-ZnO-Ga micron belt to the glass substrate to ensure that one surface of the n-ZnO-Ga micron belt is attached to the glass substrate, and pressing indium electrodes at two ends of the n-ZnO-Ga micron belt;
and 5: directionally sputtering an Ag nano quasi-particle film on the n-ZnO-Ga micron belt;
step 6: applying voltage on indium electrodes at two ends of an n-ZnO-Ga micron band coated by the Ag nano quasi-particle film until the n-ZnO-Ga micron band emits light, converting the Ag nano quasi-particle film into isolated AgNPs at a light-emitting center to obtain an AgNPs @ n-ZnO-Ga micron band composite structure;
and 7: for the AgNPs @ n-ZnO and Ga micron band composite structure, removing an indium electrode, and then moving the structure obtained in the step (3) to ensure that one end of the AgNPs @ n-ZnO and Ga micron band composite structure is arranged on the gasket, the other end of the AgNPs @ n-ZnO and Ga micron band composite structure is arranged on the p-GaN substrate, and the AgNPs @ n-ZnO and Ga micron band composite structure is not contacted with the Ni/Au alloy electrode of the p-GaN substrate; wherein, an indium electrode is pressed at one end of the AgNPs @ n-ZnO: Ga micron band composite structure positioned on the gasket and used as a cathode of the diode.
In this embodiment, the step 1 can be implemented by the following preferred scheme:
and ultrasonically cleaning the glass substrate, the quartz substrate and the p-GaN substrate by using trichloroethylene, acetone, ethanol and deionized water for 40 minutes respectively, drying, and then drying by using nitrogen.
In this embodiment, the step 2 can be implemented by the following preferred scheme:
and shielding a part of the p-GaN substrate by using a mask plate, exposing a part of the p-GaN substrate to form a circular exposed part, plating two layers of electrodes on the exposed part of the p-GaN substrate by using an electron beam evaporation method to form a Ni/Au alloy electrode, wherein the thickness of the Ni/Au alloy electrode is 25-35 nm.
In this embodiment, the step 3 can be implemented by the following preferred scheme:
the p-GaN substrate is bonded on the quartz substrate by adopting PMMA (polymethyl methacrylate), so that the P-GaN substrate is transparent and bubble-free between the P-GaN substrate and the quartz substrate, and the close bonding of the P-GaN substrate and the quartz substrate is realized.
In this embodiment, the step 4 can be implemented by the following preferred scheme:
placing an n-ZnO-Ga micron band on a glass substrate horizontally, and operating the n-ZnO-Ga micron band under a microscope to ensure that the n-ZnO-Ga micron band is micro-GaOne surface of the rice strip is attached to the glass substrate; pressing indium electrodes at two ends of the n-ZnO, Ga micron band to ensure that the indium electrodes, the n-ZnO, Ga micron band and the glass substrate are compactly attached together to form a metal-semiconductor-metal structure; the electron concentration of the n-ZnO-Ga micron band is 1018～1019/cm3Electron mobility of 15-200 cm2V.s; the thickness of the indium electrode is 1-2 um.
In this embodiment, the step 5 can be implemented by the following preferred scheme:
shielding the parts containing the indium electrodes on the two sides of the n-ZnO-Ga micron band by using a mask plate, sputtering a layer of Ag nano quasi-particle film on the surface of the n-ZnO-Ga micron band by using a magnetron sputtering instrument, wherein the sputtering target is an Ag target with the purity of 99.9 percent, the working gas is argon, the pressure of a cavity is 30-32 Pa, the sputtering current is 28-31 mA, the sputtering time is 300-350 s, and the sputtering area is the n-ZnO-Ga micron band without the indium electrodes at the two ends; the thickness of the Ag nano quasi-particle film is 30-50 nm.
In this embodiment, the step 6 can be implemented by the following preferred scheme:
placing the n-ZnO and Ga micron band wrapped by the Ag nano quasi-particle film under a microscope, adjusting the microscope to enable the n-ZnO and Ga micron band to form a clear image, applying voltage to indium electrodes at two ends of the n-ZnO and Ga micron band, and slowly increasing the voltage until the n-ZnO and Ga micron band emits light; the source meter for applying the voltage can freely adjust the voltage and the current value, the voltage adjusting range is 0-210V, and the current adjusting range is 0-100 mA. Due to joule heat effect, the Ag quasi-particle film of the light-emitting center of the n-ZnO-Ga micron band becomes isolated AgNPs, and an AgNPs @ n-ZnO-Ga micron band composite structure is obtained, wherein a scanning electron microscope image of the AgNPs @ n-ZnO-Ga micron band composite structure is shown in figure 1, and in figure 1, (a) is a scanning electron microscope image of a single n-ZnO-Ga micron band; (b) scanning electron microscope images of the n-ZnO and Ga micron bands at the junction of a luminous zone and a non-luminous zone in the x direction after the Ag quasi-particle film is sputtered; (c) is an AgNPs scanning electron microscope picture of a light emitting area of the Ga micron band in the y direction; (d) is a scanning electron microscope image of large-size AgNPs in a light-emitting area of n-ZnO and Ga micron.
In this embodiment, the step 7 can be implemented by the following preferred scheme:
and (3) removing the indium electrode under a microscope and displacing the structure obtained in the step (3) to ensure that one end of the micron-band composite structure is arranged on the gasket and the other end is arranged on the p-GaN and ensure that the micron-band composite structure does not contact the Ni/Au electrode on the p-GaN. And pressing indium particles on the micron band of the gasket to form an indium electrode as a cathode of the heterojunction diode, thus forming the complete AgNPs @ n-ZnO: Ga micron band diode, wherein the structure of the diode is shown in figure 2.
In the embodiment, the thickness of the p-GaN substrate is 300-330 um, and the hole concentration is 5.8 x 1018～1.5*1019/cm3Hole mobility of 20-150 cm2V.s. The size of the quartz substrate: L-W is 7.0-3.5 cm; size of glass substrate: L-W is 2.0-1.0 cm; size of p-GaN substrate: L-W is 2.0-1.0 cm; l represents a length and W represents a width.
The AgNPs @ n-ZnO: Ga micron band diode formed in the step 7 is electrically tested, and the IV curve is shown in figure 3. An image of the light emitted by the AgNPs @ n-ZnO Ga micron band diode is taken, as shown in FIG. 4. The spectrum of the AgNPs @ n-ZnO: Ga micron band diode is shown in FIG. 5. As can be seen from the IV curve, the AgNPs @ n-ZnO: Ga micron band diode has good rectification characteristics. As can be seen from FIG. 4, a coherent halo appears at the AgNPs @ n-ZnO: Ga micron band when the injection current is 18 mA. It can be seen from the spectrum of fig. 5 that when the current exceeds 13.5mA, lasing peaks appear at 410nm and 425nm, and the full width at half maximum is only around 1 nm. As the injection current continues to increase, the lasing intensity becomes greater.
The embodiments are only for illustrating the technical idea of the present invention, and the technical idea of the present invention is not limited thereto, and any modifications made on the basis of the technical scheme according to the technical idea of the present invention fall within the scope of the present invention.

Claims (8)

1. The preparation method of the single ZnO micron band F-P mode ultraviolet laser diode is characterized by comprising the following steps of:
(1) ultrasonic cleaning is carried out on the quartz substrate, the glass substrate and the p-GaN substrate, so that cleanness and tidiness of the quartz substrate, the glass substrate and the p-GaN substrate are guaranteed;
(2) preparing a Ni/Au alloy electrode on one side of the p-GaN substrate to be used as an anode of the diode;
(3) tightly attaching the p-GaN substrate to the quartz substrate, and preparing a gasket on the quartz substrate to ensure that the gasket is tightly attached and level to the p-GaN substrate;
(4) moving an n-ZnO-Ga micron belt to the glass substrate to ensure that one surface of the n-ZnO-Ga micron belt is attached to the glass substrate, and pressing indium electrodes at two ends of the n-ZnO-Ga micron belt;
(5) directionally sputtering an Ag nano quasi-particle film on the n-ZnO-Ga micron belt;
(6) applying voltage to indium electrodes at two ends of the n-ZnO and Ga micron band coated by the Ag nano quasi-particle film obtained in the step (5) until the n-ZnO and Ga micron band emits light, converting the Ag nano quasi-particle film into isolated AgNPs at a light-emitting center to obtain an AgNPs @ n-ZnO and Ga micron band composite structure;
(7) for the AgNPs @ n-ZnO and Ga micron band composite structure, removing an indium electrode, and then moving the structure obtained in the step (3), so that one end of the AgNPs @ n-ZnO and Ga micron band composite structure is arranged on the gasket, the other end of the AgNPs @ n-ZnO and Ga micron band composite structure is arranged on the p-GaN substrate, and the AgNPs @ n-ZnO and Ga micron band composite structure is not in contact with the Ni/Au alloy electrode of the p-GaN substrate; wherein, an indium electrode is pressed at one end of the AgNPs @ n-ZnO: Ga micron band composite structure positioned on the gasket and used as a cathode of the diode.
2. The method for preparing the single ZnO micron band F-P mode ultraviolet laser diode as claimed in claim 1, wherein in the step (1), the sample to be cleaned is respectively put into trichloroethylene solution, acetone solution, ethanol solution and deionized water, and ultrasonic cleaning is carried out by an ultrasonic cleaning machine; then the sample is put into an oven for drying and then is dried by nitrogen.
3. The method for preparing a single ZnO micron band F-P mode ultraviolet laser diode as claimed in claim 1, wherein in the step (2), a part of the P-GaN substrate is shielded by a mask plate, a part of the P-GaN substrate is exposed, the exposed part is in a round shape, two layers of electrodes are plated on the exposed part of the P-GaN substrate by an electron beam evaporation method to form a Ni/Au alloy electrode, and the thickness of the Ni/Au alloy electrode is 25-35 nm.
4. The method for preparing a single ZnO micron band F-P mode ultraviolet laser diode as claimed in claim 1, wherein in step (3), PMMA is adopted to adhere the P-GaN substrate to the quartz substrate, so that PMMA is transparent and bubble-free between the P-GaN substrate and the quartz substrate, and the P-GaN substrate and the quartz substrate are tightly attached.
5. The preparation method of the single ZnO micron band F-P mode ultraviolet laser diode as claimed in claim 1, wherein in the step (4), a n-ZnO: Ga micron band is horizontally placed on a glass substrate, and the n-ZnO: Ga micron band is operated under a microscope to ensure that one surface of the n-ZnO: Ga micron band is attached to the glass substrate; pressing indium electrodes at two ends of the n-ZnO, Ga micron band to ensure that the indium electrodes, the n-ZnO, Ga micron band and the glass substrate are compactly attached together to form a metal-semiconductor-metal structure; the electron concentration of the n-ZnO-Ga micron band is 1018～1019/cm3Electron mobility of 15-200 cm2V.s; the thickness of the indium electrode is 1-2 um.
6. The preparation method of the single ZnO micron band F-P mode ultraviolet laser diode as claimed in claim 1, wherein in the step (5), the part of the n-ZnO and Ga micron band containing the indium electrodes on the two sides is shielded by a mask plate, a magnetron sputtering instrument is used for sputtering a layer of Ag nano quasi-particle film on the surface of the n-ZnO and Ga micron band, the sputtering target is an Ag target with the purity of 99.9 percent, the working gas is argon, the cavity pressure is 30-32 Pa, the sputtering current is 28-31 mA, the sputtering time is 300-350 s, and the sputtering area is the n-ZnO and Ga micron band without the indium electrodes on the two ends; the thickness of the Ag nano quasi-particle film is 30-50 nm.
7. The method for preparing the single ZnO micron band F-P mode ultraviolet laser diode as claimed in claim 1, wherein in the step (6), the n-ZnO: Ga micron band wrapped by the Ag nano quasi-particle film is placed under a microscope, the microscope is adjusted to enable the n-ZnO: Ga micron band to form a clear image, voltage is applied to indium electrodes at two ends of the n-ZnO: Ga micron band, and the voltage is slowly increased until the n-ZnO: Ga micron band emits light; the source meter for applying the voltage can freely adjust the voltage and the current value, the voltage adjusting range is 0-210V, and the current adjusting range is 0-100 mA.
8. The method for preparing a single ZnO micron band F-P mode ultraviolet laser diode as claimed in claim 1, wherein the thickness of the P-GaN substrate is 300-330 um, and the hole concentration is 5.8 x 1018～1.5*1019/cm3Hole mobility of 20-150 cm2/V·s。
CN202010012967.7A 2020-01-07 2020-01-07 Preparation method of single ZnO micron band F-P mode ultraviolet laser diode Pending CN111193188A (en)

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