CN115064620A - Efficient deep ultraviolet light-emitting diode with YAlN/AlGaN superlattice p-type layer as step component and preparation method thereof - Google Patents
Efficient deep ultraviolet light-emitting diode with YAlN/AlGaN superlattice p-type layer as step component and preparation method thereof Download PDFInfo
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Abstract
The invention discloses a high-efficiency deep ultraviolet light-emitting diode with a YAlN/AlGaN superlattice p-type layer as a step component, which mainly solves the problem of low luminous efficiency caused by small ionization rate of Mg doped in the p-type layer of the existing deep ultraviolet light-emitting diode. The semiconductor device comprises a substrate (1), a nucleating layer (2), a buffer layer (3), an n-type layer (4), a multi-quantum well layer (5), an electronic barrier layer (6), a p-type layer (7) and an ohmic contact layer (8) from bottom to top, wherein the p-type layer (7) adopts a superlattice of three-step composition YAlN/AlGaN, the number of cycles of the superlattice of each step is the same, the thickness of YAlN is the same, the Al component is unchanged, the thickness of AlGaN is the same, and the Al component is decreased progressively. The invention can enhance the polarization electric field, effectively improve the ionization rate of Mg doping, improve the carrier concentration and the luminous power and efficiency of the device, and can be used for realizing high-performance deep ultraviolet light-emitting diodes and deep ultraviolet light-emitting equipment.
Description
Technical Field
The invention belongs to the technical field of microelectronics, and particularly relates to a high-efficiency deep ultraviolet light-emitting diode which can be used for manufacturing high-efficiency ultraviolet and deep ultraviolet light-emitting equipment.
Technical Field
The AlGaN ternary alloy can be band gap adjusted between 3.43eV and 6.11eV and is suitable for the fabrication of optical devices in the wavelength range of 200nm to 365 nm. Applications in this wavelength range include sterilization, uv curing and printing, phototherapy and medical applications, photocatalyst deodorization and material sensing, etc. So far, the traditional mercury lamp is mainly used for the applications, compared with the mercury lamp, the ultraviolet light emitting diode has the advantages of low cost, small volume, long service life, good stability, high safety, environmental protection and the like, and the ultraviolet light emitting diode based on AlGaN is expected to become a novel ultraviolet light source for replacing the mercury lamp in the future.
The p-type doping beingAn important factor in the efficiency of light emitting diodes, however, good p-type doping has been a problem. Mg is the most commonly used p-type dopant in light emitting diodes, the activation energy of Mg as an acceptor dopant in GaN is 200meV, the activation energy in AlN reaches 630meV as the band gap grows, and the higher activation energy results in a very low ionization rate. In the ultraviolet and deep ultraviolet spectrum regions, the ionization rate of Mg is greatly reduced along with the increase of Al component of AlGaN. At present, the efficient ionization of Mg in AlGaN is very difficult to realize, and the hole concentration in the existing p-type AlGaN is generally low and is generally 10 17 cm -3 On the order of magnitude, the lower hole concentration inhibits the development of high efficiency uv LEDs, and therefore, to increase the efficiency of uv LEDs, it is necessary to increase the hole concentration.
At present, a conventional deep ultraviolet light emitting diode includes a substrate, a nucleation layer, a buffer layer, an n-type layer, a multi-quantum well layer, an electron blocking layer, a p-type layer, and an ohmic contact layer, as shown in fig. 1, wherein the p-type layer mainly adopts a uniformly doped AlGaN material. This device suffers from the following three disadvantages:
firstly, for deep ultraviolet LED, the p-type layer is made of AlGaN with high Al component, the activation energy of Mg is very high, and the ionization efficiency is low, so that the hole activation efficiency is very low, and the luminous efficiency of the LED is influenced.
And secondly, the low hole concentration makes electrons and holes more unbalanced, further aggravates electron leakage and reduces device efficiency.
For the deep ultraviolet LED, the p-type layer is made of AlGaN with high Al component, ohmic contact between the AlGaN with high Al component and a metal electrode is very difficult, a GaN layer is often used as an ohmic contact layer, larger lattice mismatch exists between the AlGaN and the GaN, larger stress exists between layers, the crystal quality is poor, and the difficulty of an epitaxial process is high.
Disclosure of Invention
The invention aims to provide a high-efficiency deep ultraviolet light-emitting diode of a stepped component YAlN/AlGaN superlattice p-type layer and a manufacturing method thereof, aiming at overcoming the defects of the prior art, so that the ionization rate of Mg doping is effectively improved by utilizing a polarization electric field of a superlattice, the carrier concentration is improved, the electron leakage is reduced, the luminous power and the luminous efficiency of a device are effectively improved, and the stress in an epitaxial layer is reduced by adopting the stepped component p-type layer, so that the crystal epitaxial quality is improved.
The technical scheme for realizing the purpose of the invention is as follows:
1. a high-efficiency deep ultraviolet light-emitting diode of a step component YAlN/AlGaN superlattice p-type layer comprises the following components from bottom to top: substrate, nucleation layer, buffer layer, n type layer, multiple quantum well layer, electron barrier layer, p type layer, ohmic contact layer, its characterized in that:
the p-type layer adopts a three-step component YAlN/AlGaN superlattice, and each step of parameters are as follows:
the number of the first-order superlattice cycles is 7-10, the Al component range of the YAlN material in each cycle is 0.6-0.8, the thickness is 3nm-7nm, the Al component range of the AlGaN material in each cycle is 0.5-0.8, and the thickness is 1nm-4 nm;
the number of the second-order superlattice cycles is 7-10, the Al component range of the YAlN material in each cycle is 0.6-0.8, the thickness is 3nm-7nm, the Al component range of the AlGaN material in each cycle is 0.3-0.5, and the thickness is 1nm-4 nm;
the number of the third-order superlattice cycles is 7-10, the Al component range of the YAlN material in each cycle is 0.6-0.8, the thickness is 3nm-7nm, the Al component range of the AlGaN material in each cycle is 0.1-0.3, and the thickness is 1nm-4 nm;
the Al components of the AlGaN materials in the third order are decreased progressively to form a YAlN/AlGaN superlattice p-type layer with a step component, so that the luminous efficiency of the device is effectively improved.
Further, the multiple quantum well layer comprises five periods of quantum wells and quantum barriers, the quantum well in each period is made of AlGaN materials with the thickness of 1.3nm-3nm, the Al component is 0.4-0.79, the quantum barriers in each period are made of AlGaN materials with the thickness of 7nm-12nm, and the Al component is 0.5-0.87.
Further, the substrate is made of c-plane sapphire materials.
Furthermore, the nucleation layer is made of high-temperature AlN material with the thickness of 15nm-35 nm.
Furthermore, the buffer layer is made of AlN material with the thickness of 1-2 μm.
Furthermore, the ohmic contact layer is made of GaN material with the thickness of 10nm-20 nm.
Furthermore, the n-type layer is made of AlGaN material with the thickness of 1.5-2.5 μm, and the Al component is 0.6-0.9.
Furthermore, the electron blocking layer is made of AlGaN material with the thickness of 20nm-30nm, and the Al component is 0.65-0.98.
2. A manufacturing method of a high-efficiency deep ultraviolet light-emitting diode with a step component YAlN/AlGaN superlattice p-type layer is characterized by comprising the following steps:
1) cleaning and nitriding the substrate;
2) growing a nucleation layer with the thickness of 15nm-35nm on the pretreated substrate by utilizing an MOCVD (metal organic chemical vapor deposition) process;
3) growing a buffer layer with the thickness of 1-2 mu m on the nucleating layer by utilizing the MOCVD process;
4) growing an n-type layer of 1.5-2.5 microns on the buffer layer by using an MOCVD (metal organic chemical vapor deposition) process;
5) growing a multi-quantum well layer comprising five periods of quantum wells and quantum barriers on the n-type layer by using an MOCVD (metal organic chemical vapor deposition) process, wherein the thickness of the quantum well in each period is 1.3nm-3nm, and the thickness of the quantum barrier in each period is 7nm-12 nm;
6) growing an electron barrier layer with the thickness of 20nm-30nm on the multi-quantum well layer by utilizing an MOCVD process;
7) on the electron barrier layer, a three-order stepped YAlN/AlGaN superlattice p-type layer with gradually reduced Al components is grown by using an MOCVD process:
7a) growing a first-order superlattice with a period of 7-10 on the electron blocking layer by using an MOCVD (metal organic chemical vapor deposition) process, wherein the thickness of a YAlN material of each period of the first-order superlattice is 3-7 nm, the thickness of an AlGaN material of each period is 1-4 nm, and the Al component range is 0.5-0.8;
7b) growing a second-order superlattice with a period of 7-10 on the first-order superlattice by using an MOCVD (metal organic chemical vapor deposition) process, wherein the thickness of a YAlN material of each period of the second-order superlattice is 3-7 nm, the thickness of an AlGaN material of each period is 1-4 nm, and the Al component range is 0.3-0.5;
7c) growing a third-order superlattice with a period of 7-10 on the second-order superlattice by using an MOCVD (metal organic chemical vapor deposition) process, wherein the thickness of a YAlN material of each period of the third-order superlattice is 3-7 nm, the thickness of an AlGaN material of each period is 1-4 nm, and the Al component range is 0.1-0.3;
8) growing an ohmic contact layer with the thickness of 10nm-20nm on the p-type layer by utilizing an MOCVD process;
9) etching the ohmic contact layer by dry etching, wherein the etching depth is from the surface to the middle part of the n-type layer, and the etching shape is a sector with a central angle of 90 degrees;
10) and depositing metal on the non-etched ohmic contact layer by adopting a metal sputtering method to form a p electrode, and depositing metal on the etched n-type layer by adopting a metal sputtering method to form an n electrode to finish the manufacturing of the LED.
Compared with the prior art, the invention has the following advantages:
1. the invention adopts YAlN/AlGaN superlattice as a p-type layer, and YAlN belongs to transition metal nitride and has strong polarization effect, so that the ionization rate of Mg can be effectively improved by using stronger polarization electric field, the carrier concentration is improved, the electron leakage is improved, and the luminous power and the luminous efficiency of the device are improved.
2. The YAlN/AlGaN superlattice provided by the invention adopts the step components with the gradually decreased Al components, so that the stress in an epitaxial layer is effectively reduced, and the epitaxial quality of crystals is improved.
Drawings
FIG. 1 is an overall structure diagram of a high efficiency deep ultraviolet light emitting diode of the present invention;
FIG. 2 is a schematic structural view of the p-type layer of the YAlN/AlGaN superlattice of the step composition of FIG. 1;
fig. 3 is a schematic flow chart of the manufacturing process of the high-efficiency deep ultraviolet light-emitting diode of fig. 1 according to the present invention.
Detailed Description
Embodiments of the present invention will be described in further detail below with reference to the accompanying drawings.
Referring to fig. 1, the deep ultraviolet light emitting diode of the present invention includes a substrate 1, a nucleation layer 2, a buffer layer 3, an n-type layer 4, a multi-quantum well layer 5, an electron blocking layer 6, a YAlN/AlGaN superlattice p-type layer 7, and an ohmic contact layer 8. Wherein:
the substrate 1 is made of c-plane sapphire material;
the nucleating layer 2 is made of high-temperature AlN material, has the thickness of 15nm-35nm and is positioned on the substrate;
the buffer layer 3 is made of AlN material, has the thickness of 1-2 mu m and is positioned on the nucleating layer;
the n-type layer 4 is made of AlGaN material, has an Al component range of 0.6-0.9 and a thickness of 1.5-2.5 μm, and is positioned on the buffer layer;
the multi-quantum well layer 5 comprises five periods of quantum wells and quantum barriers, the quantum well of each period is made of AlGaN material, the Al component range is 0.4-0.79, and the thickness is 1.3-3 nm; the quantum barrier of each period is made of AlGaN material, the Al component range is 0.5-0.87, and the thickness is 7-12 nm; the total thickness of the quantum wells and the quantum barriers of all periods is 41.5nm-75nm, and the quantum wells and the quantum barriers are positioned on the n-type layer;
the electron barrier layer 6 is made of AlGaN material, has an Al component range of 0.65-0.98 and a thickness of 20-30 nm, and is positioned on the multi-quantum well layer;
referring to fig. 2, the YAlN/AlGaN superlattice p-type layer 7 adopts a third-order step composition YAlN/AlGaN superlattice, and each step parameter is as follows:
the number of the first-order superlattice cycles is 7-10, the Al component range of the YAlN material in each cycle is 0.6-0.8, the thickness is 3nm-7nm, the Al component range of the AlGaN material in each cycle is 0.5-0.8, and the thickness is 1nm-4 nm;
the number of the second-order superlattice cycles is 7-10, the Al component range of the YAlN material in each cycle is 0.6-0.8, the thickness is 3nm-7nm, the Al component range of the AlGaN material in each cycle is 0.3-0.5, and the thickness is 1nm-4 nm;
the number of the third-order superlattice cycles is 7-10, the Al component range of the YAlN material in each cycle is 0.6-0.8, the thickness is 3nm-7nm, the Al component range of the AlGaN material in each cycle is 0.1-0.3, and the thickness is 1nm-4 nm;
the Al components of the AlGaN materials in the third order are decreased progressively to form a YAlN/AlGaN superlattice p-type layer with a step component, and the YAlN/AlGaN superlattice p-type layer is positioned on the electron blocking layer;
the ohmic contact layer 8 is made of GaN material, has a thickness of 10nm-20nm, and is located on the p-type layer.
Referring to fig. 3, three examples of the fabrication of high efficiency deep ultraviolet light emitting diodes with graded composition YAlN/AlGaN superlattice p-type layers are presented.
Example 1, a deep ultraviolet light emitting diode having an emission wavelength of 280nm was fabricated.
Step one, preprocessing a substrate.
1.1) cleaning c-plane sapphire substrate, placing the cleaned substrate in an MOCVD reaction chamber, and reducing the vacuum degree of the reaction chamber to 2 x 10 -2 And (3) charging hydrogen into the reaction chamber, heating the substrate to 1050 ℃ under the condition that the pressure of the MOCVD reaction chamber reaches 30Torr, and keeping the temperature for 5min to finish the heat treatment of the substrate.
1.2) placing the substrate after heat treatment in a reaction chamber with the temperature of 1200 ℃, introducing ammonia gas with the flow of 3000sccm, and nitriding for 5min to finish the pretreatment of the substrate.
And step two, extending the nucleation layer, as shown in fig. 3 (a).
And raising the temperature of the reaction chamber to 1250 ℃, keeping the pressure of the reaction chamber at 30Torr, simultaneously introducing a nitrogen source with the flow of 2000sccm and an aluminum source with the flow of 20sccm, and growing the high-temperature AlN nucleating layer 2 with the thickness of 35nm on the c-plane sapphire substrate by adopting an MOCVD method.
And step three, extending the buffer layer, as shown in fig. 3 (b).
Keeping the temperature of the reaction chamber at 1250 ℃, keeping the pressure of the reaction chamber at 30Torr, simultaneously introducing a nitrogen source with the flow of 2000sccm and an aluminum source with the flow of 20sccm, and growing an AlN buffer layer 3 with the thickness of 1 μm on the nucleation layer by adopting an MOCVD method.
Step four, the n-type layer is extended, as shown in fig. 3 (c).
Reducing the temperature of the reaction chamber to 1150 ℃, reducing the pressure of the reaction chamber to 20Torr, simultaneously introducing a nitrogen source with the flow of 2500sccm, a gallium source with the flow of 60sccm, an aluminum source with the flow of 150sccm and a silicon source with the flow of 40sccm, and growing n-type Al with the thickness of 2.5 mu m on the buffer layer by adopting an MOCVD method 0.6 Ga 0.4 And an N layer 4.
And step five, extending the multiple quantum well layer, as shown in fig. 3 (d).
Keeping the temperature of the reaction chamber at 1150 ℃, keeping the pressure of the reaction chamber at 20Torr, simultaneously introducing a nitrogen source with the flow of 2500sccm, and growing Al on the n-type layer for five periods by adopting an MOCVD method 0.4 Ga 0.6 N/Al 0.5 Ga 0.5 N multi quantum well layer 5:
5.1) introducing a gallium source with the flow rate of 120sccm and an aluminum source with the flow rate of 150sccm, and growing a layer of Al with the thickness of 12nm on the n-type layer 0.5 Ga 0.5 An N quantum barrier layer;
5.2) introducing a gallium source with the flow rate of 100sccm and an aluminum source with the flow rate of 120sccm, and growing a layer of Al with the thickness of 3nm on the quantum barrier layer 0.4 Ga 0.6 An N quantum well layer;
5.3) repeating 5.1) and 5.2), and thus alternately growing for five periods, a multiquantum well layer was obtained.
Step six, extending the electron blocking layer, as shown in fig. 3 (e).
The temperature of the reaction chamber was raised to 1200 deg.C, the pressure of the reaction chamber was raised to 30Torr, and a nitrogen source, a gallium source and an aluminum source were introduced at a flow rate of 1800sccm, 50sccm and 120sccm, respectively. Growing Al with the thickness of 30nm on the multi-quantum well layer by adopting an MOCVD method 0.65 Ga 0.35 An N-electron blocking layer 6.
Step seven, the p-type layer is epitaxial, as shown in fig. 3 (f).
Reducing the temperature of the reaction chamber to 1050 ℃, keeping the pressure of the reaction chamber at 30Torr, simultaneously introducing a nitrogen source with the flow of 2500sccm and a magnesium source with the flow of 200sccm, and then growing the three-order step superlattice according to the following process conditions:
7.1) growing a first-order superlattice on the electron blocking layer by using an MOCVD method:
7.1.1) introducing an yttrium source with the flow rate of 50sccm and an aluminum source with the flow rate of 320sccm into the reaction chamber, and growing a layer of Y with the thickness of 6nm on the electron blocking layer 0.2 Al 0.8 N layers;
7.1.2) introducing a gallium source with a flow rate of 150sccm and an aluminum source with a flow rate of 120sccm into the reaction chamber, Y 0.2 Al 0.8 Growing a layer of Al with the thickness of 3nm on the N layer 0.5 Ga 0.5 N layers;
7.1.3) repeating 7.1.1) and 7.1.2), and alternately growing for 10 periods to obtain a first-order superlattice;
7.2) growing a second-order superlattice on the first-order superlattice by adopting an MOCVD method:
7.2.1) introducing an yttrium source with a flow rate of 50sccm and an aluminum source with a flow rate of 300sccm into the reaction chamber, and growing a layer of Y with a thickness of 6nm on the first-order superlattice 0.2 Al 0.8 N layers;
7.2.2) introducing a gallium source with a flow rate of 120sccm and an aluminum source with a flow rate of 150sccm into the reaction chamber, Y 0.2 Al 0.8 Growing a layer of Al with the thickness of 3nm on the N layer 0.3 Ga 0.7 N layers;
7.2.3) repeating 7.2.1) and 7.2.2), and alternately growing for 10 periods to obtain a second-order superlattice;
7.3) growing a third-order superlattice on the second-order superlattice by adopting an MOCVD method:
7.3.1) then introducing an yttrium source with the flow rate of 50sccm and an aluminum source with the flow rate of 300sccm into the reaction chamber, and growing a layer of Y with the thickness of 6nm on the second-order superlattice 0.2 Al 0.8 N layers;
7.3.2) introducing a gallium source with a flow rate of 150sccm and an aluminum source with a flow rate of 60sccm into the reaction chamber, Y 0.2 Al 0.8 Growing a layer of Al with the thickness of 3nm on the N layer 0.1 Ga 0.9 N layers;
7.3.3) repeating 7.3.1) and 7.3.2), and alternately growing for 10 periods to obtain a third-order superlattice;
so far, the epitaxy of the three-step YAlN/AlGaN superlattice p-type layer 7 is completed.
And step eight, extending the ohmic contact layer, as shown in fig. 3 (g).
And keeping the temperature of the reaction chamber at 1050 ℃, keeping the pressure of the reaction chamber at 30Torr, simultaneously introducing a nitrogen source with the flow of 2500sccm, a gallium source with the flow of 150sccm and a magnesium source with the flow of 200sccm, and growing a GaN ohmic contact layer 8 with the thickness of 10nm on the p-type layer by adopting an MOCVD method.
Step nine, etching the horizontal structure, as shown in fig. 3 (h).
And etching the ohmic contact layer by using dry etching, wherein the etching depth is 887nm, the etching is stopped at the middle part of the n-type layer, and the etching shape is a sector with a central angle of 90 degrees.
Step ten, depositing an electrode, as shown in fig. 3 (i).
The temperature of the reaction chamber was maintained at 1200 ℃ in H 2 And annealing for 10min in the atmosphere, depositing metal on the non-etched ohmic contact layer by adopting a metal sputtering method to form a p electrode, depositing metal on the etched n-type layer to form an n electrode, and finishing the manufacture of the deep ultraviolet LED device with the light-emitting wavelength of 280 nm.
Example 2, a deep ultraviolet light emitting diode having an emission wavelength of 255nm was manufactured.
Step 1, preprocessing a substrate.
The specific implementation of this step is the same as step one of example 1.
Step 2, the nucleation layer is epitaxial, as shown in fig. 3 (a).
And raising the temperature of the reaction chamber to 1300 ℃, keeping the pressure of the reaction chamber at 60Torr, introducing a nitrogen source with the flow of 3000sccm and an aluminum source with the flow of 30sccm, and growing the high-temperature AlN nucleating layer 2 with the thickness of 25nm on the c-plane sapphire substrate by adopting an MOCVD method.
Step 3, extending the buffer layer, as shown in fig. 3 (b).
Keeping the temperature of the reaction chamber at 1300 ℃, keeping the pressure of the reaction chamber at 60Torr, simultaneously introducing a nitrogen source with the flow of 3000sccm and an aluminum source with the flow of 30sccm, and growing an AlN buffer layer 3 with the thickness of 1.5 μm on the nucleation layer by adopting an MOCVD method.
And step 4, extending the n-type layer, as shown in fig. 3 (c).
Reducing the temperature of the reaction chamber to 1200 ℃, keeping the pressure of the reaction chamber at 60Torr, simultaneously introducing a nitrogen source with the flow of 3000sccm, a gallium source with the flow of 30sccm, an aluminum source with the flow of 120sccm and a silicon source with the flow of 30sccm, and growing n-type Al with the thickness of 2 mu m on the buffer layer by adopting an MOCVD method 0.8 Ga 0.2 And an N layer 4.
And step 5, extending the multiple quantum well layer, as shown in fig. 3 (d).
Keeping the temperature of the reaction chamber at 1200 ℃, keeping the pressure of the reaction chamber at 60Torr, introducing a nitrogen source with the flow of 3000sccm, and growing Al on the n-type layer for five periods by adopting an MOCVD method 0.6 Ga 0.4 N/Al 0.75 Ga 0.25 The N multi-quantum well layer 5 is formed by introducing a gallium source with the flow rate of 40sccm and an aluminum source with the flow rate of 130sccm, and growing a layer of Al with the thickness of 10nm on the N-type layer 0.75 Ga 0.25 An N quantum barrier layer; then a gallium source with the flow rate of 60sccm and an aluminum source with the flow rate of 120sccm are introduced, and a layer of Al with the thickness of 2nm grows on the quantum barrier layer 0.6 Ga 0.4 An N quantum well layer; thus, a multiple quantum well layer was obtained by growing the layers alternately for five periods.
Step 6, extending the electron blocking layer, as shown in fig. 3 (e).
The temperature of the reaction chamber was raised to 1250 ℃, the pressure in the reaction chamber was maintained at 60Torr, and the nitrogen source at a flow rate of 2500sccm, the gallium source at a flow rate of 15sccm, and the aluminum source at a flow rate of 170sccm were introduced. Growing Al with the thickness of 25nm on the multi-quantum well layer by adopting an MOCVD method 0.95 Ga 0.05 An N-electron blocking layer 6.
Step 7, the p-type layer is epitaxial, as shown in fig. 3 (f).
Reducing the temperature of the reaction chamber to 1200 ℃, keeping the pressure of the reaction chamber at 60Torr, simultaneously introducing a nitrogen source with the flow of 3000sccm and a magnesium source with the flow of 300sccm, and then growing the three-order step superlattice according to the following process conditions:
7a) growing a first-order superlattice on the electron blocking layer by MOCVD method, namely introducing yttrium source with the flow rate of 60sccm and aluminum source with the flow rate of 280sccm, and growing a layer of Y with the thickness of 5nm on the electron blocking layer 0.3 Al 0.7 N layers; then introducing a gallium source with the flow rate of 60sccm and an aluminum source with the flow rate of 120sccm into the reactor at Y 0.3 Al 0.7 Growing a layer of Al with the thickness of 2nm on the N layer 0.6 Ga 0.4 N layers; repeating the process for 8 periods to obtain a first-order superlattice;
7b) growing a second-order superlattice on the first-order superlattice by MOCVD method, namely introducing 60sccGrowing a layer of Y with the thickness of 5nm on the first-order superlattice by using a yttrium source of m and an aluminum source with the flow rate of 280sccm 0.3 Al 0.7 N layers; then introducing a gallium source with the flow rate of 130sccm and an aluminum source with the flow rate of 150sccm into the reactor at Y 0.3 Al 0.7 Growing a layer of Al with the thickness of 2nm on the N layer 0.4 Ga 0.6 N layers; repeating the process for 8 periods to obtain a second-order superlattice;
7c) growing a third-order superlattice on the second-order superlattice by MOCVD method, namely introducing an yttrium source with the flow rate of 60sccm and an aluminum source with the flow rate of 280sccm, and growing a layer of Y with the thickness of 5nm on the second-order superlattice 0.3 Al 0.7 N layers; then introducing a gallium source with the flow rate of 180sccm and an aluminum source with the flow rate of 120sccm into the reactor at Y 0.3 Al 0.7 Growing a layer of Al with the thickness of 2nm on the N layer 0.2 Ga 0.8 N layers; repeating the process for 8 cycles to obtain a third-order superlattice;
so far, the epitaxy of the three-step YAlN/AlGaN superlattice p-type layer 7 is completed.
And 8, extending the ohmic contact layer, as shown in figure 3 (g).
Keeping the temperature of the reaction chamber at 1200 ℃, keeping the pressure of the reaction chamber at 60Torr, simultaneously introducing a nitrogen source with the flow of 3000sccm, a gallium source with the flow of 240sccm and a magnesium source with the flow of 300sccm, and growing a GaN ohmic contact layer 8 with the thickness of 15nm on the p-type layer by adopting an MOCVD method.
Step 9, etch the horizontal structure, as shown in fig. 3 (h).
And etching the ohmic contact layer by using dry etching, wherein the etching depth is 813nm, the etching is stopped at the middle part of the n-type layer, and the etching shape is a sector with a central angle of 90 degrees.
Step 10, depositing an electrode, as shown in FIG. 3 (i).
The specific completion of the step is the same as the step of the embodiment 1, and the manufacturing of the deep ultraviolet LED device with the light-emitting wavelength of 255nm is completed.
Example 3, a deep ultraviolet light emitting diode having an emission wavelength of 227nm was manufactured.
And step A, preprocessing the substrate.
The specific implementation of this step is the same as the first step of example 1.
Step B, the nucleation layer is epitaxial, as shown in fig. 3 (a).
And raising the temperature of the reaction chamber to 1350 ℃, raising the pressure of the reaction chamber to 100Torr, simultaneously introducing a nitrogen source with the flow rate of 4000sccm and an aluminum source with the flow rate of 40sccm, and growing the high-temperature AlN nucleating layer 2 with the thickness of 15nm on the c-plane sapphire substrate by adopting an MOCVD method.
Step C, epitaxial buffer layer, as shown in FIG. 3 (b).
Keeping the temperature of the reaction chamber at 1350 ℃, keeping the pressure of the reaction chamber at 100Torr, simultaneously introducing a nitrogen source with the flow of 4000sccm and an aluminum source with the flow of 40sccm, and growing an AlN buffer layer 3 with the thickness of 2 μm on the nucleation layer by adopting an MOCVD method.
And step D, extending the n-type layer, as shown in figure 3 (c).
Keeping the temperature of the reaction chamber at 1350 ℃, keeping the pressure of the reaction chamber at 100Torr, simultaneously introducing a nitrogen source with the flow of 4000sccm, a gallium source with the flow of 50sccm, an aluminum source with the flow of 180sccm and a silicon source with the flow of 50sccm, and growing n-type Al with the thickness of 2.5 μm on the buffer layer by adopting an MOCVD method 0.9 Ga 0.1 And an N layer 4.
Step E, the multiple quantum well layer is epitaxial as shown in fig. 3 (d).
Keeping the temperature of the reaction chamber at 1350 ℃, keeping the pressure of the reaction chamber at 100Torr, simultaneously introducing a nitrogen source with the flow of 4000sccm, and growing Al on the n-type layer for five periods by adopting an MOCVD method 0.79 Ga 0.21 N and Al 0.87 Ga 0.13 N multi quantum well layer 5:
E1) introducing a gallium source with the flow rate of 40sccm and an aluminum source with the flow rate of 170sccm, and growing a layer of Al with the thickness of 7nm on the n-type layer 0.87 Ga 0.13 N quantum barrier layer
E2) Introducing a gallium source with the flow rate of 60sccm and an aluminum source with the flow rate of 180sccm, and growing a layer of Al with the thickness of 1.3nm on the quantum barrier layer 0.79 Ga 0.21 N quantum well layer
E3) E1) and E2) were repeated, thus alternately growing for five cycles, to obtain a multiple quantum well layer.
Step F, the electron blocking layer is epitaxial, as shown in fig. 3 (e).
The temperature of the reaction chamber was raised to 1400 ℃ and the pressure in the reaction chamber was maintained at 100Torr, while introducing a nitrogen source at a flow rate of 4000sccm, a gallium source at a flow rate of 10sccm and an aluminum source at a flow rate of 180 sccm. Growing Al with the thickness of 20nm on the multi-quantum well layer by adopting an MOCVD method 0.98 Ga 0.02 An N-electron blocking layer 6.
Step G, the p-type layer is epitaxial, as shown in FIG. 3 (f).
Reducing the temperature of the reaction chamber to 1350 ℃, keeping the pressure of the reaction chamber at 100Torr, simultaneously introducing a nitrogen source with the flow of 4000sccm and a magnesium source with the flow of 400sccm, and then growing the three-order stepped superlattice according to the following process conditions:
G1) growing a first-order superlattice on the electron blocking layer by using an MOCVD method:
g1.1) introducing an yttrium source with the flow rate of 80sccm and an aluminum source with the flow rate of 280sccm into the reaction chamber, and growing a layer of Y with the thickness of 7nm on the electron blocking layer 0.4 Al 0.6 N layers;
g1.2) introducing a gallium source with a flow rate of 60sccm and an aluminum source with a flow rate of 150sccm into the reaction chamber, and introducing a gallium source with a flow rate of 150sccm into the reaction chamber 0.4 Al 0.6 Growing a layer of Al with the thickness of 4nm on the N layer 0.8 Ga 0.2 N layers;
g1.3) repeating G1.1) and G1.2), and alternately growing for 7 periods to obtain a first-order superlattice;
G2) growing a second-order superlattice on the first-order superlattice by using an MOCVD method:
g2.1) introducing an yttrium source with the flow rate of 80sccm and an aluminum source with the flow rate of 280sccm into the reaction chamber, and growing a layer of Y with the thickness of 7nm on the first-order superlattice 0.4 Al 0.6 N layers;
g2.2) introducing a gallium source with the flow rate of 80sccm and an aluminum source with the flow rate of 120sccm into the reaction chamber, and introducing a gallium source with the flow rate of 120sccm into the reaction chamber 0.4 Al 0.6 Growing a layer of Al with the thickness of 4nm on the N layer 0.5 Ga 0.5 N layers;
g2.3) repeating G2.1) and G2.2), and alternately growing for 7 periods to obtain a second-order superlattice;
G3) growing a third-order superlattice on the second-order superlattice by using an MOCVD method:
g3.1) introducing an yttrium source with the flow rate of 80sccm and an aluminum source with the flow rate of 280sccm into the reaction chamber, and growing a layer of Y with the thickness of 7nm on the second-order superlattice 0.4 Al 0.6 N layers;
g3.2) introducing a gallium source with the flow rate of 120sccm and an aluminum source with the flow rate of 100sccm into the reaction chamber, and introducing a gallium source with the flow rate of 100sccm into the reaction chamber 0.4 Al 0.6 Growing a layer of Al with the thickness of 4nm on the N layer 0.3 Ga 0.7 N layers;
g.3.3) repeating G3.1) and G3.2), and alternately growing for 7 periods to obtain a third-order superlattice;
so far, the epitaxy of the three-step YAlN/AlGaN superlattice p-type layer 7 is completed.
And step H, extending the ohmic contact layer, as shown in figure 3 (g).
Keeping the temperature of the reaction chamber at 1350 ℃, keeping the pressure of the reaction chamber at 100Torr, simultaneously introducing a nitrogen source with the flow of 4000sccm, a gallium source with the flow of 300sccm and a magnesium source with the flow of 400sccm, and growing a GaN ohmic contact layer 8 with the thickness of 20nm on the p-type layer by adopting an MOCVD method.
Step I, etch the horizontal structure, as shown in FIG. 3 (h).
And etching the ohmic contact layer by using dry etching, wherein the etching depth is 778nm, the etching is stopped at the middle part of the n-type layer, and the etching shape is a sector with a central angle of 90 degrees.
Step J, depositing an electrode, as shown in FIG. 3 (i).
The specific completion of the step is the same as the step ten of the embodiment 1, and the manufacturing of the deep ultraviolet LED device with the light emitting wavelength of 227nm is completed.
The foregoing description is only three specific examples of the present invention and should not be construed as limiting the invention in any way, and it will be apparent to those skilled in the art that various modifications and variations in form and detail can be made without departing from the principle and structure of the invention, but these modifications and variations will still fall within the scope of the appended claims.
Claims (10)
1. A high-efficiency deep ultraviolet light-emitting diode of a step component YAlN/AlGaN superlattice p-type layer comprises the following components from bottom to top: substrate (1), nucleation layer (2), buffer layer (3), n type layer (4), multiple quantum well layer (5), electron barrier layer (6), p type layer (7), ohmic contact layer (8), its characterized in that:
the p-type layer (7) adopts a three-step component YAlN/AlGaN superlattice, and each step of parameters are as follows:
the number of the first-order superlattice cycles is 7-10, the Al component range of the YAlN material in each cycle is 0.6-0.8, the thickness is 3nm-7nm, the Al component range of the AlGaN material in each cycle is 0.5-0.8, and the thickness is 1nm-4 nm;
the number of the second-order superlattice cycles is 7-10, the Al component range of the YAlN material in each cycle is 0.6-0.8, the thickness is 3nm-7nm, the Al component range of the AlGaN material in each cycle is 0.3-0.5, and the thickness is 1nm-4 nm;
the number of the third-order superlattice cycles is 7-10, the Al component range of the YAlN material in each cycle is 0.6-0.8, the thickness is 3nm-7nm, the Al component range of the AlGaN material in each cycle is 0.1-0.3, and the thickness is 1nm-4 nm;
the Al components of the AlGaN materials in the third order are decreased progressively to form a YAlN/AlGaN superlattice p-type layer with a step component, so that the luminous efficiency of the device is effectively improved.
2. The diode of claim 1, wherein: the multiple quantum well layer (5) comprises five periods of quantum wells and quantum barriers, wherein the quantum well in each period is made of AlGaN materials with the thickness of 1.3nm-3nm, the Al component is 0.4-0.79, the quantum barriers in each period are made of AlGaN materials with the thickness of 7nm-12nm, and the Al component is 0.5-0.87.
3. The diode of claim 1, wherein:
the substrate (1) is made of c-plane sapphire material;
the nucleating layer (2) is made of high-temperature AlN material with the thickness of 15nm-35 nm;
the buffer layer (3) is made of AlN material with the thickness of 1-2 mu m;
the ohmic contact layer (8) is made of GaN material with the thickness of 10nm-20 nm.
4. The diode of claim 1, wherein:
the n-type layer (4) is made of AlGaN material with the thickness of 1.5-2.5 μm, and the Al component is 0.6-0.9;
the electron blocking layer (6) is made of AlGaN material with the thickness of 20nm-30nm, and the Al component is 0.65-0.98.
5. A manufacturing method of a high-efficiency deep ultraviolet light-emitting diode of a YAlN/AlGaN superlattice p-type layer is characterized by comprising the following steps:
1) carrying out cleaning and nitriding pretreatment on the substrate (1);
2) growing a nucleation layer (2) with the thickness of 15nm-35nm on the pretreated substrate by using an MOCVD (metal organic chemical vapor deposition) process;
3) growing a buffer layer (3) with the thickness of 1-2 mu m on the nucleation layer by utilizing the MOCVD process;
4) growing an n-type layer (4) with the thickness of 1.5-2.5 mu m on the buffer layer by utilizing an MOCVD process;
5) growing a multi-quantum well layer (5) comprising five periods of quantum wells and quantum barriers on the n-type layer by using an MOCVD process, wherein the thickness of the quantum well in each period is 1.3nm-3nm, and the thickness of the quantum barrier in each period is 7nm-12 nm;
6) growing an electron barrier layer (6) with the thickness of 20nm-30nm on the multi-quantum well layer by utilizing an MOCVD process;
7) growing a three-order stepped YAlN/AlGaN superlattice p-type layer (7) with gradually decreased Al components on the electronic barrier layer by using an MOCVD process:
7a) growing a first-order superlattice with a period of 7-10 on the electron blocking layer by using an MOCVD (metal organic chemical vapor deposition) process, wherein the thickness of a YAlN material of each period of the first-order superlattice is 3-7 nm, the thickness of an AlGaN material of each period is 1-4 nm, and the Al component range is 0.5-0.8;
7b) growing a second-order superlattice with a period of 7-10 on the first-order superlattice by using an MOCVD (metal organic chemical vapor deposition) process, wherein the thickness of a YAlN material of each period of the second-order superlattice is 3-7 nm, the thickness of an AlGaN material of each period is 1-4 nm, and the Al component range is 0.3-0.5;
7c) growing a third-order superlattice with a period of 7-10 on the second-order superlattice by using an MOCVD (metal organic chemical vapor deposition) process, wherein the thickness of a YAlN material of each period of the third-order superlattice is 3-7 nm, the thickness of an AlGaN material of each period is 1-4 nm, and the Al component range is 0.1-0.3;
8) growing an ohmic contact layer (8) with the thickness of 10nm-20nm on the p-type layer by using an MOCVD process;
9) etching the ohmic contact layer by dry etching, wherein the etching depth is from the surface to the middle part of the n-type layer, and the etching shape is a sector with a central angle of 90 degrees;
10) and depositing metal on the non-etched ohmic contact layer by adopting a metal sputtering method to form a p electrode, and depositing metal on the etched n-type layer by adopting a metal sputtering method to form an n electrode to finish the manufacturing of the LED.
6. The method as claimed in claim 5, wherein the MOCVD process adopted in the steps 2) and 3) is to set the following condition parameters for the reaction chamber:
the temperature of the reaction chamber is 1250-1350 ℃,
the pressure in the reaction chamber is maintained at 30-100Torr,
introducing a nitrogen source with the flow rate of 2000-4000sccm and an aluminum source with the flow rate of 20-40sccm into the reaction chamber.
7. The method as claimed in claim 5, wherein the MOCVD process adopted in the step 4) is to set the following condition parameters for the reaction chamber:
the temperature of the reaction chamber is 1150-,
the pressure in the reaction chamber is maintained at 20-100Torr,
and introducing a nitrogen source with the flow rate of 2500-4000sccm, a gallium source with the flow rate of 30-60sccm, an aluminum source with the flow rate of 120-180sccm and a silicon source with the flow rate of 30-50sccm into the reaction chamber.
8. The method as claimed in claim 5, wherein the MOCVD process adopted in the step 5) is to set the following condition parameters for the reaction chamber:
the temperature of the reaction chamber is 1150-1350 ℃,
the pressure in the reaction chamber is maintained at 20-100Torr,
and introducing a nitrogen source with the flow rate of 2500-4000sccm, a gallium source with the flow rate of 40-120sccm and an aluminum source with the flow rate of 120-180sccm into the reaction chamber.
9. The method of claim 5, wherein the MOCVD process conditions used in step 7 are as follows:
the temperature, the pressure and the gas of the 7a), the 7b) and the 7c) are the same, namely the temperature of the reaction chamber is 1050-1350 ℃, the pressure of the reaction chamber is kept at 30-100Torr, the introduced gas is a nitrogen source, a gallium source, an aluminum source, an yttrium source and a magnesium source, the flow rate of the nitrogen source is 2500-4000sccm, the flow rate of the yttrium source is 50-80sccm, and the flow rate of the magnesium source is 200-400 sccm;
the flow rates of the introduced gallium source and the introduced aluminum source of the 7a), 7b) and 7c) are different, namely:
in the step 7a), the gallium source flow rate is 60-150sccm, and the aluminum source flow rate is 120-320 sccm.
In step 7b), the flow rate of the gallium source is 80-130sccm, and the flow rate of the aluminum source is 120-300 sccm.
In the step 7c), the flow rate of the gallium source is 120-180sccm and the flow rate of the aluminum source is 60-300 sccm.
10. The method of claim 5, wherein:
the MOCVD process adopted in the step 6) is to set the temperature of the reaction chamber at 1200-;
the MOCVD process adopted in the step 8) is to set the temperature of the reaction chamber at 1050-.
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| CN116314510A (en) * | 2023-05-23 | 2023-06-23 | 江西兆驰半导体有限公司 | Composite undoped AlGaN layer, preparation method, epitaxial wafer and LED |
| CN116364819A (en) * | 2023-05-31 | 2023-06-30 | 江西兆驰半导体有限公司 | LED epitaxial wafer, preparation method thereof and LED |
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| Publication number | Priority date | Publication date | Assignee | Title |
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| CN116314510A (en) * | 2023-05-23 | 2023-06-23 | 江西兆驰半导体有限公司 | Composite undoped AlGaN layer, preparation method, epitaxial wafer and LED |
| CN116314510B (en) * | 2023-05-23 | 2023-08-15 | 江西兆驰半导体有限公司 | Composite undoped AlGaN layer, preparation method, epitaxial wafer and LED |
| CN116364819A (en) * | 2023-05-31 | 2023-06-30 | 江西兆驰半导体有限公司 | LED epitaxial wafer, preparation method thereof and LED |
| CN116364819B (en) * | 2023-05-31 | 2023-12-15 | 江西兆驰半导体有限公司 | LED epitaxial wafer, preparation method thereof and LED |
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