CN111341887A - GaN base layer and preparation method and application thereof - Google Patents

GaN base layer and preparation method and application thereof Download PDF

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CN111341887A
CN111341887A CN202010135212.6A CN202010135212A CN111341887A CN 111341887 A CN111341887 A CN 111341887A CN 202010135212 A CN202010135212 A CN 202010135212A CN 111341887 A CN111341887 A CN 111341887A
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temperature
base layer
pressure
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CN111341887B (en
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张宇
杨天鹏
张穆萍
康建
杨东
周荣
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Jiangxi Epitop Optoelectronic Co ltd
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Abstract

The invention provides a GaN base layer and a preparation method and application thereof. The invention provides a preparation method of a GaN base layer, which comprises the steps of growing a first GaN layer, a second GaN layer, a third GaN layer, a fourth GaN layer and a fifth GaN layer on an AlN film in sequence, and controlling the temperature and the pressure in each growth step to obtain the final GaN base layer. By the preparation method provided by the invention, the dislocation density of the GaN base layer is reduced, the quality of the GaN base layer is improved, the quality of an LED device is further improved, meanwhile, the GaN base layer is applied to a green LED, and due to the fact that the GaN base layer has good quality, the lattice constant difference between the GaN base layer and InN is reduced, the quality of a green LED product is further improved, and particularly the green LED product with large size is obtained.

Description

GaN base layer and preparation method and application thereof
Technical Field
The invention relates to the technical field of material chemistry, in particular to a GaN base layer and a preparation method and application thereof.
Background
The LED product taking GaN as a basic layer is highly valued by people at present due to the advantages of environmental protection, high efficiency, energy conservation and long service life, and the existing LED technology is to sputter an AlN film on a substrate sapphire, grow a GaN basic layer on the AlN film, and then sequentially grow an N layer, a luminescent layer and a P layer to obtain the final LED product. Therefore, the crystal quality of the GaN foundation layer determines the quality of the following N, light emitting, and P layers, and has an influence on the performance of the final LED device.
At present, when a GaN base layer grows on a sapphire sputtering AlN film, about 14% of lattice mismatch exists between AlN and GaN crystals, so that a great deal of dislocation exists when the GaN base layer grows, wherein the dislocation comprises screw dislocation and edge dislocation, and the larger the sum of the two kinds of dislocation is, the poorer the quality of an LED device is, so that the driving voltage is high, the brightness is poor, and the antistatic performance is weak during working; secondly, In the existing white, blue and green LEDs, the In content In the luminescent layers of the blue and green LEDs is high, and the GaN and the InN have larger lattice constant difference, so that if the GaN base layer for white light is used In the blue and green LED products, the comprehensive yield fluctuation of the products can occur, and the defects of weak antistatic capability, low reverse voltage and the like of the products are shown.
Disclosure of Invention
The invention provides a GaN base layer and a preparation method thereof, which are used for solving the problem of poor quality of an LED device caused by more crystal dislocations of the GaN base layer.
The invention provides a preparation method of a GaN basic layer, which comprises the following steps:
1) controlling the temperature of the reaction chamber at 650 ℃ and the pressure at 400 ℃ and 600torr, introducing carrier gas, a gallium source and an N source, and growing a first GaN layer;
2) increasing the temperature to 1020-1050 ℃ in 480s of 360-480s, reducing the pressure to 150-200torr, introducing carrier gas and N source to convert the first GaN layer into a second GaN layer;
3) reducing the temperature to 1020 ℃ in 60-90s, increasing the pressure to 600torr in 350-;
4) increasing the temperature to 1020-;
5) and controlling the temperature at 1070-.
The invention provides a preparation method of a GaN base layer, which grows the GaN base layer on the basis of a sapphire substrate sputtered with an AlN film, and FIG. 1 is a flow chart of the preparation method of the GaN base layer provided by an embodiment of the invention, as shown in FIG. 1, and comprises the following steps: step 1), controlling the temperature of the reaction chamber to be 500-; step 2), on the basis of the grown first GaN layer, the temperature is increased to 1020-class 1050 ℃ in 360-class 480s, the pressure is reduced to 150-class 200torr, carrier gas and N source are introduced, the introduction of the gallium source is stopped, the first GaN layer is converted into a second GaN layer, and at the moment, the reflectivity of the second GaN layer is detected to be 0.5-1.0%, which indicates that the growth is properly expanded on the basis of the seed crystal in the step 1; step 3), reducing the temperature to 1020 ℃ within 60-90s, increasing the pressure to 600torr within 350-; step 4), increasing the temperature to 1020-; and 5) controlling the temperature at 1070-.
According to the method, the dislocation density of the GaN base layer is reduced through the steps 1) to 3), so that the quality of the GaN base layer is improved, the quality of an LED device is further improved, meanwhile, the GaN base layer is applied to a green light LED, and the quality of the GaN base layer is better, the lattice constant difference between the GaN base layer and InN is reduced, and the quality of a green light LED product, particularly a green light LED product with large size is further improved.
In one embodiment, one skilled in the art can sputter grow an AlN film on a sapphire substrate according to the prior art, and transfer the sapphire with the grown AlN film into a reaction chamber to grow a GaN foundation layer according to the above-described method.
Wherein the carrier gas is selected from high purity H2High purity N2One or two of them; the N source is high-purity NH3The gallium source is selected from one of trimethyl gallium (TMGa) or triethyl gallium (TEGa).
In order to ensure the performance of the LED epitaxial wafer and products, the input amount and the growth time of each raw material need to be reasonably set so as to control the thickness of the GaN basic layer.
Specifically, in step 1), the thickness of the first GaN layer is 5 to 15 nm.
In the step 3), the thickness of the third GaN layer is 500-1000 nm.
In the step 4), the thickness of the fourth GaN layer is 600-1000 nm.
In the step 5), the thickness of the fifth GaN layer is 1200-2000 nm.
In the growth process of the GaN base layer, in order to avoid the waste of raw materials, the inventor finds that the growth of the GaN base layer can reach the optimal state by controlling the flow of the gallium source, and the quality of an epitaxial wafer is further improved.
Specifically, in the step 1), the flow rate of the gallium source is 200-.
In the step 3), the flow rate of the gallium source is 600-2000 mu mol/min.
In the step 4), the flow rate of the gallium source is 1500-.
In the step 5), the flow rate of the gallium source is the same as that in the step 4).
The invention does not limit the flow of the carrier gas and the N source, and the carrier gas and the N source can be set by the person skilled in the art, and the description is not repeated.
According to the method, the dislocation density of the GaN base layer is reduced through the steps 1) to 3), so that the quality of the GaN base layer is improved, the quality of an LED device is further improved, meanwhile, the GaN base layer is applied to a green light LED, and the quality of the GaN base layer is better, the lattice constant difference between the GaN base layer and InN is reduced, and the quality of a green light LED product, particularly a green light LED product with large size is further improved.
In a second aspect, the invention provides a GaN foundation layer obtained according to any one of the above-described preparation methods.
The GaN base layer obtained by the preparation method has higher quality due to lower dislocation density, so that the quality of an LED device is further improved.
The invention provides an LED epitaxial structure, which comprises the GaN basic layer obtained by the preparation method or the GaN basic layer.
The invention provides an LED epitaxial structure, wherein an N layer, a luminous layer and a P layer are sequentially grown on a GaN base layer obtained by the preparation method or the GaN base layer according to the existing method to obtain a final LED epitaxial structure and an LED product, and the GaN base layer has lower dislocation density, so that the quality of the GaN base layer is better, and the quality of the LED epitaxial structure and the product is further improved.
The implementation of the invention has at least the following advantages:
1. according to the invention, through the steps 1-3, GaN is fully grown longitudinally, the transverse growth of GaN crystals is inhibited to the greatest extent, and the dislocation of the GaN crystals caused by the simultaneous longitudinal and transverse growth of the traditional GaN base layer is avoided, and through the steps 4-5, the columnar crystal bases obtained through the steps 1-3 are slowly combined and are grown simultaneously transversely and longitudinally on the basis, so that the dislocation density of the GaN base layer is reduced, the quality of the GaN base layer is improved, and the quality of an LED device is further improved;
2. the GaN base layer provided by the invention is applied to the green LED, and the GaN base layer has better quality, so that the lattice constant difference between the GaN base layer and InN is reduced, and the quality of the green LED product is further improved, particularly the green LED product with large size.
In conclusion, the invention provides the GaN base layer and the preparation method thereof, through the steps 1-3, GaN is fully grown longitudinally, the transverse growth of GaN crystal is inhibited to the greatest extent, the dislocation density of the GaN base layer is reduced, and the quality of an LED device is improved.
Drawings
Fig. 1 is a flowchart of a method for fabricating a GaN foundation layer according to an embodiment of the present invention.
Detailed Description
In order to make the objects, technical solutions and advantages of the present invention clearer, the technical solutions in the embodiments of the present invention will be clearly and completely described below with reference to the embodiments of the present invention. All other embodiments, which can be derived by a person skilled in the art from the embodiments given herein without making any creative effort, shall fall within the protection scope of the present invention.
Example 1
1. A30 nm AlN film was sputtered on a 2 inch PSS, placed in a graphite tray, transferred to the reaction chamber and the MOCVD system was ready.
2.1, increasing the temperature of the reaction chamber to 550 ℃, introducing 5.357mol/min H under the pressure of 500torr2And 1.339mol/min of N2Trimethyl gallium at 502. mu. mol/min, NH at 2mol/min3Continuously growing a first GaN layer of 10 nm;
2.2, the temperature is increased to 1030 ℃ within 420s, the pressure is reduced to 200torr, and 3.357mol/min H is introduced2And 1.339mol/min of N22mol/min NH3Stopping introducing trimethyl gallium, and converting the first GaN layer into a second GaN layer, wherein the reflectivity of the surface of the second GaN layer is 0.5%;
2.3, reducing the temperature to 1010 ℃ within 60s, increasing the pressure to 400torr, and introducing 5.357mol/min H2And 1.339mol/min of N21116 μmol/min of trimethylgallium, 2mol/min NH3Growing a third GaN layer with the thickness of 800nm for 1500s continuously, wherein the reflectivity of the whole GaN oscillates between 0.5 and 1.0 percent;
2.4, increasing the temperature to 1080 ℃ in 360s, reducing the pressure to 150torr, and introducing 5.357mol/min H2And 1.339mol/min of N22mol/min NH3Uniformly increasing the flow rate of trimethyl gallium to 3000 mu mol/min, and continuously growing a fourth GaN layer with the thickness of 800nm for 350s, wherein the integral reflectivity of GaN is increased from 1.0% to 6%;
2.5, keeping the temperature at 1080 ℃ and the pressure at 150torr, and introducing 5.357mol/min of H2And 1.339mol/min of N22mol/min NH3And 3000 mu mol/min trimethyl gallium continuously grows a fifth GaN layer with the thickness of 1600nm for 900s to obtain a GaN basic layer, wherein the reflectivity of the whole GaN is increased from 6.0% to 22%, and the reflectivity of the whole GaN oscillates between 16% and 22% along with the increase of time.
3. On the basis of step 2.5, the temperature of the reaction chamber is reduced to 970 ℃, the pressure is 100torr, and simultaneously, 5mol/min of N is introduced20.5mol/min NH3500. mu. mol/min of trimethylgallium, 500. mu. mol/min of 200ppm SiH4Continuously growing a dopant, namely 100 mu mol/min of trimethylaluminum for 180s to obtain an N-type AlGaN layer with the thickness of 100 nm;
wherein the Si doping concentration in the N-type AlGaN layer is about 5E +18atoms/cm3(ii) a The atomic number percentage of Al is about 10%.
4. The temperature is raised to 1010 ℃ and the pressure is maintained at 150torr, while simultaneously introducing 5mol/min of H2And 2mol/min of N2As carrier gas, 3000. mu. mol/min of trimethyl gallium, 3mol/min of NH31200. mu. mol/min of 200ppm SiH4Continuously growing a dopant for 2000s to obtain an N-type GaN layer with the thickness of 4000 nm;
wherein the doping concentration of Si in the N-type GaN layer is about 1.2E +20atoms/cm3。
5. Growing a light-emitting layer:
5.1.1, the temperature is reduced to 850 ℃, the pressure is maintained at 200torr, and 3mol/min N is introduced23mol/min NH3Stopping introducing trimethyl gallium and SiH4A dopant;
5.1.2. maintaining the temperature at 850 deg.C and the pressure at 200torr, and introducing 3mol/min N2，3mol/min NH3800. mu. mol/min of trimethylgallium, 4. mu. mol/min of SiH at a concentration of 200ppm4A dopant to grow a 200nm N-type GaN layer, wherein the Si doping concentration is about 1.2E +18atoms/cm3；
5.2, reducing the temperature by 720 ℃, keeping the pressure at 200torr, and introducing 3mol/min of N2，3mol/min NH3Stopping introducing trimethyl gallium and SiH 4;
5.3, reducing the temperature by 720 ℃, keeping the pressure at 200torr, and introducing 3mol/min of N23mol/min NH3200 mu mol/min of triethyl gallium and 800 mu mol/min of trimethyl indium, and growing an InGaN layer with the thickness of 3.5nm, wherein the In content is 22 percent;
5.4, increasing the temperature to 870 ℃, keeping the pressure at 200torr, and introducing 3mol/min of N2，3mol/min NH3Stopping introducing the triethyl gallium;
5.5, keeping the pressure and the temperature unchanged, and introducing 3mol/min N2, 3mol/min NH3600. mu. mol/min of triethylgallium, 0.2. mu. mol/min of 200ppm SiH4A dopant, growing nGaN layer with thickness of 13nm and Si doping concentration of about 5E +16atoms/cm3；
5.6, repeating the steps of 5.2-5.5 for 12 periods to obtain an InGaN/nGaN periodic layer;
5.7, reducing the temperature to 720 ℃, keeping the pressure at 200torr, and introducing 3mol/min of N23mol/min NH3Keeping the pressure at 200torr, and stopping introducing the triethyl gallium and the SiH4；
5.8, reducing the temperature to 720 ℃, keeping the pressure at 200torr, and introducing 3mol/min of N23mol/min NH3200 mu mol/min of triethyl gallium, 800 mu mol/min of trimethyl indium, growing an InGaN layer with a thickness of 3.5nm, wherein the content of In is about 22%;
5.9, the temperature is raised to 870 ℃, the pressure is maintained at 200torr, and 3mol/min N is introduced23mol/min NH3Stopping introducing trimethyl gallium and trimethyl indium;
5.10, holding pressureThe temperature is not changed, and 3mol/min N is introduced23mol/min NH3Growing a GaN layer with the thickness of 16nm by using 600 mu mol/min of triethyl gallium;
6. on the basis of step 5.10, the temperature is reduced to 750 ℃, the pressure is kept at 200torr, the MO source is stopped being introduced, and 5mol/min H is introduced23mol/min of N2As carrier gas, 1200. mu. mol/min of trimethylgallium, 3mol/min of NH3Cp of 10. mu. mol/min2A Mg dopant, growing a low temperature type P type GaN layer with a thickness of 60nm, wherein the Mg doping concentration is about 2E +20atoms/cm3；
7. The temperature is raised to 970 ℃, the pressure is maintained at 100torr, and 5mol/min of N is introduced20.5mol/min NH3Trimethyl gallium at 1200. mu. mol/min, CP at 0.2. mu. mol/min2Mg dopant, 120 mu mol/min trimethyl aluminum, and continuously growing a P-type AlGaN layer with the thickness of 100nm, wherein the Mg doping concentration is 5E +17atoms/cm3(ii) a The atomic number content of Al in the AlGaN layer accounts for 14 percent;
8. controlling the temperature at 950 ℃ and the pressure at 200torr, and introducing 3mol/min of N25mol/min of H23mol/min NH3150 μmol/min of triethyl gallium, 0.3 μmol/min of CP2Mg dopant, continuously growing a high temperature type P type GaN layer with the thickness of 30nm, wherein the Mg doping concentration is about 5E +17atoms/cm3；
9. The temperature is reduced to 880 ℃, the pressure is maintained at 200torr, and 3mol/min N is introduced25mol/min of H23mol/min NH350 μmol/min of triethylgallium, 10 μmol/min of Cp2Mg dopant, continuously growing a high temperature type P type GaN layer with the thickness of 5nm, wherein the Mg doping concentration is about 3E +20atoms/cm3；
10. The temperature is reduced to 800 ℃, the pressure is maintained at 200torr, and 5mol/min N is introduced21.33mol/min NH3Then reducing the temperature to 750 ℃ for 4-5 minutes, and annealing the epitaxial layer;
11. the temperature is reduced to 500 ℃, the pressure is maintained at 200torr, and 10mol/min N is introduced2Then the temperature is reduced to 450 DEG CAnd closing a power supply of the heating wire, cooling the grown epitaxial wafer along with the furnace, and then taking out the graphite tray to obtain the LED epitaxial wafer D1.
Example 2
1. A30 nm AlN film was sputtered on a 2 inch PSS, placed in a graphite tray, transferred to the reaction chamber and the MOCVD system was ready.
2.1, increasing the temperature of the reaction chamber to 550 ℃, introducing 5.357mol/min H under the pressure of 500torr2And 1.339mol/min of N2Trimethyl gallium at 502. mu. mol/min, NH at 2mol/min3Continuously growing a first GaN layer of 10 nm;
2.2, the temperature is increased to 1030 ℃ in 420s, the pressure is reduced to 200torr, and 3.357mol/min H is introduced2And 1.339mol/min of N22mol/min NH3Stopping introducing trimethyl gallium, and converting the first GaN layer into a second GaN layer, wherein the reflectivity of the surface of the second GaN layer is about 0.5%;
2.3, the temperature is reduced to 1010 ℃ in 60s, the pressure is increased to 500torr, and 5.357mol/min H is introduced2And 1.339mol/min of N21116 μmol/min of trimethylgallium, 2mol/min NH3Growing a third GaN layer with the thickness of 800nm for 1200s, wherein the reflectivity of the whole GaN oscillates between 0.5% and 1.0%;
2.4, increasing the temperature to 1070 ℃ in 360s, reducing the pressure to 150torr, and introducing 5.357mol/min H2And 1.339mol/min of N22mol/min NH as carrier gas3Uniformly increasing the flow rate of trimethyl gallium to 3000 mu mol/min, and continuously growing a fourth GaN layer with the thickness of 800nm for 350s, wherein the integral reflectivity of GaN is increased from 1.0% to 6%;
2.5, increasing the temperature to 1080 ℃, keeping the pressure at 150torr, and introducing 5.357mol/min of H2And 1.339mol/min of N2，2mol/min NH3And 3000 mu mol/min trimethyl gallium continuously grows a fifth GaN layer with the thickness of 1600nm for 900s to obtain a GaN basic layer, wherein the reflectivity of the whole GaN is increased from 6.0% to 22%, and the reflectivity of the whole GaN oscillates between 16% and 22% along with the increase of time.
An LED epitaxial wafer D2 was prepared in the same manner as in step 3 to step 11 provided in example 1.
Example 3
1. A30 nm AlN film was sputtered on a 2 inch PSS, placed in a graphite tray, transferred to the reaction chamber and the MOCVD system was ready.
2.1, increasing the temperature of the reaction chamber to 550 ℃, introducing 5.357mol/min H under the pressure of 500torr2And 1.339mol/min of N2Trimethyl gallium at 502. mu. mol/min, NH at 2mol/min3Continuously growing a first GaN layer of 10 nm;
2.2, the temperature is increased to 1030 ℃ in 420s, the pressure is reduced to 200torr, and 3.357mol/min H is introduced2And 1.339mol/min of N22mol/min NH3Stopping introducing trimethyl gallium, and converting the first GaN layer into a second GaN layer, wherein the reflectivity of the surface of the second GaN layer is about 0.5%;
2.3, the temperature is reduced to 1010 ℃ in 60s, the pressure is increased to 400torr, and 5.357mol/min H is introduced2And 1.339mol/min of N21116 μmol/min of trimethylgallium, 2mol/min of NH3Growing a third GaN layer with the thickness of 800nm for 1500s continuously, wherein the reflectivity of the whole GaN oscillates between 0.5 and 1.0 percent;
2.4, increasing the temperature to 1070 ℃ in 360s, reducing the pressure to 150torr, and introducing 5.357mol/min H2And 1.339mol/min of N22mol/min NH3Uniformly increasing the flow rate of trimethyl gallium to 1500 mu mol/min, and continuously growing a fourth GaN layer with the thickness of 800nm for 700s, wherein the integral reflectivity of GaN is increased from 1.0% to 6%;
2.5, increasing the temperature to 1080 ℃, keeping the pressure at 150torr, and introducing 5.357mol/min of H2And 1.339mol/min of N22mol/min NH3And trimethyl gallium of 1500 mu mol/min continuously grows a fifth GaN layer with the thickness of 1600nm for 1800s to obtain a GaN basic layer, wherein the reflectivity of the whole GaN is increased from 6.0 percent to 22 percent, and the reflectivity of the whole GaN oscillates between 16 percent and 22 percent along with the increase of time.
An LED epitaxial wafer D3 was prepared in the same operation as in step 3 to step 11 provided in example 1.
Example 4
1. A30 nm AlN film was sputtered onto 4 inches of PSS, placed in a graphite tray, transferred into the reaction chamber and the MOCVD system was ready.
2.1, increasing the temperature of the reaction chamber to 550 ℃, introducing 5.357mol/min H under the pressure of 500torr2And 1.339mol/min of N2Trimethyl gallium at 502. mu. mol/min, NH at 2mol/min3Continuously growing a first GaN layer of 10 nm;
2.2, the temperature is increased to 1030 ℃ in 420s, the pressure is reduced to 200torr, and 3.357mol/min H is introduced2And 1.339mol/min of N22mol/min NH3Stopping introducing trimethyl gallium, and converting the first GaN layer into a second GaN layer, wherein the reflectivity of the surface of the second GaN layer is about 0.5%;
2.3, the temperature is reduced to 1010 ℃ in 60s, the pressure is increased to 400torr, and 5.357mol/min H is introduced2And 1.339mol/min of N21116 μmol/min of trimethylgallium, 2mol/min of NH3Growing a third GaN layer with the thickness of 800nm for 1500s continuously, wherein the reflectivity of the whole GaN oscillates between 0.5 and 1.0 percent;
2.4, increasing the temperature to 1080 ℃ in 360s, reducing the pressure to 150torr, and introducing 5.357mol/min H2And 1.339mol/min of N22mol/min NH as carrier gas3Uniformly increasing the flow rate of trimethyl gallium to 3000 mu mol/min, and continuously growing a fourth GaN layer with the thickness of 800nm for 350s, wherein the integral reflectivity of GaN is increased from 1.0% to 6%;
2.5, increasing the temperature to 1080 ℃, keeping the pressure at 150torr, and introducing 5.357mol/min of H2And 1.339mol/min of N22mol/min NH3And 3000 mu mol/min trimethyl gallium continuously grows a fifth GaN layer with the thickness of 1600nm for 900s to obtain a GaN basic layer, wherein the reflectivity of the whole GaN is increased from 6.0% to 22%, and the reflectivity of the whole GaN oscillates between 16% and 22% along with the increase of time.
An LED epitaxial wafer D4 was prepared in the same operation as in step 3 to step 11 provided in example 1.
The LED epitaxial wafers D1-D4 are subjected to XRD test, and the test results are shown in Table 1.
TABLE 1 XRD test results of LED epitaxial wafers D1-D4 obtained in examples 1-4
Figure BDA0002397026450000101
As can be seen from table 1, the dislocation numbers of the 102 or 002 planes of the GaN foundation layer in the LED epitaxial wafers obtained in examples 1 to 4 are both 230 or less, while the dislocation numbers of the 102 or 002 planes of the conventional GaN foundation layer are generally about 300 to 350, so that the dislocation density of the GaN foundation layer provided by the present invention is low, and the quality of the epitaxial wafer can be effectively improved; furthermore, the data of the light-emitting layer (MQW) in the above table show that the epitaxial wafers D1-D4 provided in examples 1-4 have good quality, which indirectly demonstrates that the GaN foundation layer provided by the present invention can effectively improve the quality of the epitaxial wafer.
On the basis of the epitaxial wafers D1-D4, 4 samples are prepared for each group of epitaxial wafers to carry out repeated experiments, and the same preparation process is adopted to evaporate an ITO layer of about 1200 angstroms, evaporate a Cr/Pt/Au electrode of about 16000 angstroms and evaporate a protective layer of SiO on each epitaxial wafer2About 800 angstroms, 16 wafer samples were prepared, which contained several grains of the same size, the grain size was 965.2 μm 965.2 μm (38mi 38mil), and then all the grains on the wafer were measured by placing the wafer in a point measurement machine, and the driving voltage, brightness, wavelength, antistatic property, etc. of the grains were obtained under the constant current driving of 350mA, and the test results are shown in table 2.
Figure BDA0002397026450000121
From the parameters and the comprehensive yield provided by table 2, the comprehensive yield of the wafer is 91.1-97.6%, while the comprehensive yield of the green wafer of most chip manufacturers can only reach about 85% at present, so that the epitaxial wafer obtained by the preparation method provided by the invention has good comprehensive performance and repeatability, can meet the use requirement of green LED products, and has certain economic benefit.
Finally, it should be noted that: the above embodiments are only used to illustrate the technical solution of the present invention, and not to limit the same; while the invention has been described in detail and with reference to the foregoing embodiments, it will be understood by those skilled in the art that: the technical solutions described in the foregoing embodiments may still be modified, or some or all of the technical features may be equivalently replaced; and the modifications or the substitutions do not make the essence of the corresponding technical solutions depart from the scope of the technical solutions of the embodiments of the present invention.

Claims (10)

1. A preparation method of a GaN base layer is characterized by comprising the following steps:
1) controlling the temperature of the reaction chamber at 650 ℃ and the pressure at 400 ℃ and 600torr, introducing carrier gas, a gallium source and an N source, and growing a first GaN layer;
2) increasing the temperature to 1020-1050 ℃ in 480s of 360-480s, reducing the pressure to 150-200torr, introducing carrier gas and N source to convert the first GaN layer into a second GaN layer;
3) reducing the temperature to 1020 ℃ in 60-90s, increasing the pressure to 600torr in 350-;
4) increasing the temperature to 1020-;
5) and controlling the temperature at 1070-.
2. The method according to claim 1, wherein in step 1), the first GaN layer has a thickness of 5 to 15 nm.
3. The method as claimed in claim 1, wherein the thickness of the third GaN layer in step 3) is 500-1000 nm.
4. The method as claimed in claim 1, wherein in step 4), the thickness of the fourth GaN layer is 600-1000 nm.
5. The method as claimed in claim 1, wherein the thickness of the fifth GaN layer in step 5) is 1200-2000 nm.
6. The method as claimed in claim 1, wherein the flow rate of the gallium source in step 1) is 200-1000 μmol/min.
7. The method as claimed in claim 1, wherein the flow rate of the gallium source in step 3) is 600-2000 μmol/min.
8. The method as claimed in claim 1, wherein the flow rate of the gallium source in step 4) is 1500-.
9. A GaN foundation layer characterized by being obtained by the production method according to any one of claims 1 to 8.
10. An LED epitaxial structure comprising a GaN foundation layer obtained by the production method according to any one of claims 1 to 8 or the GaN foundation layer according to claim 9.
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Cited By (1)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN113322448A (en) * 2021-05-21 2021-08-31 聚灿光电科技股份有限公司 Graphite plate

Citations (4)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN104022199A (en) * 2014-05-30 2014-09-03 华灿光电(苏州）有限公司 Epitaxial structure of light emitting diode
CN108598226A (en) * 2018-02-28 2018-09-28 华灿光电（浙江）有限公司 A kind of LED epitaxial slice and preparation method thereof
CN110098290A (en) * 2019-05-22 2019-08-06 湘能华磊光电股份有限公司 A kind of growing method of LED epitaxial structure
CN110504340A (en) * 2019-09-18 2019-11-26 福建兆元光电有限公司 A kind of growing method of gallium nitride light-emitting diode LED epitaxial wafer

Patent Citations (4)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN104022199A (en) * 2014-05-30 2014-09-03 华灿光电(苏州）有限公司 Epitaxial structure of light emitting diode
CN108598226A (en) * 2018-02-28 2018-09-28 华灿光电（浙江）有限公司 A kind of LED epitaxial slice and preparation method thereof
CN110098290A (en) * 2019-05-22 2019-08-06 湘能华磊光电股份有限公司 A kind of growing method of LED epitaxial structure
CN110504340A (en) * 2019-09-18 2019-11-26 福建兆元光电有限公司 A kind of growing method of gallium nitride light-emitting diode LED epitaxial wafer

Cited By (1)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN113322448A (en) * 2021-05-21 2021-08-31 聚灿光电科技股份有限公司 Graphite plate

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