CN115020565B - Preparation method of composite patterned substrate and epitaxial structure with air gap - Google Patents
Preparation method of composite patterned substrate and epitaxial structure with air gap Download PDFInfo
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- CN115020565B CN115020565B CN202210631067.XA CN202210631067A CN115020565B CN 115020565 B CN115020565 B CN 115020565B CN 202210631067 A CN202210631067 A CN 202210631067A CN 115020565 B CN115020565 B CN 115020565B
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- H—ELECTRICITY
- H01—ELECTRIC ELEMENTS
- H01L—SEMICONDUCTOR DEVICES NOT COVERED BY CLASS H10
- H01L33/00—Semiconductor devices with at least one potential-jump barrier or surface barrier specially adapted for light emission; Processes or apparatus specially adapted for the manufacture or treatment thereof or of parts thereof; Details thereof
- H01L33/02—Semiconductor devices with at least one potential-jump barrier or surface barrier specially adapted for light emission; Processes or apparatus specially adapted for the manufacture or treatment thereof or of parts thereof; Details thereof characterised by the semiconductor bodies
- H01L33/20—Semiconductor devices with at least one potential-jump barrier or surface barrier specially adapted for light emission; Processes or apparatus specially adapted for the manufacture or treatment thereof or of parts thereof; Details thereof characterised by the semiconductor bodies with a particular shape, e.g. curved or truncated substrate
- H01L33/22—Roughened surfaces, e.g. at the interface between epitaxial layers
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- H—ELECTRICITY
- H01—ELECTRIC ELEMENTS
- H01L—SEMICONDUCTOR DEVICES NOT COVERED BY CLASS H10
- H01L33/00—Semiconductor devices with at least one potential-jump barrier or surface barrier specially adapted for light emission; Processes or apparatus specially adapted for the manufacture or treatment thereof or of parts thereof; Details thereof
- H01L33/005—Processes
Abstract
The application relates to the field of semiconductors and discloses a composite patterned substrate, a preparation method thereof and an epitaxial structure, wherein a first material layer and a second material layer are sequentially deposited on the surface of a substrate body; then coating positive photoresist to prepare a photoetching window with periodic arrangement; sequentially etching the material layer II, the material layer I and part of the substrate body in the photoetching window by using a first dry etching process to form a spacing groove; and etching out the part of the second material layer covered by the positive photoresist by using a second dry etching process to expose the part of the first material layer, and forming a convex structure to obtain the composite patterned substrate. When the epitaxial structure grows in the subsequent process, the raised structures in the substrate prepared by the method can form a larger air gap between the N-type layer and each raised structure, and light emitted by the LED can be refracted and reflected more in the area at the position of the air gap, so that the light-emitting reflection of the LED can be increased, the light-emitting efficiency is improved, and the brightness is improved.
Description
Technical Field
The application relates to the technical field of semiconductors, in particular to a preparation method of a composite patterned substrate and an epitaxial structure with an air gap.
Background
Semiconductor light-emitting diodes (LEDs) have the advantages of small volume, low energy consumption, long service life, environmental protection, durability and the like, and blue and green light GaN-based LED chips rapidly develop in the fields of display and illumination; domestic LED illumination has replaced common illumination by about 30% and in order to continue to improve the popularity of LEDs in the illumination market, the performance of the LEDs in terms of brightness and light quality needs to be continuously improved. At present, more than 95% of the mainstream blue-green GaN-based LED epitaxial wafer uses a sapphire substrate as a substrate material, and the sapphire substrate is the most dominant substrate material in the mainstream LED market in the future due to the characteristics of high hardness, high light transmittance, mature process and the like. The sapphire substrate adopted at present is basically subjected to patterning (Patterned Sapphire Substrates, PSS) processing and then used for LED epitaxial growth. Because the gallium nitride epitaxial layer is grown on the PSS substrate, the epitaxial defect can be reduced, and the crystal quality of the epitaxial layer is improved so as to improve the electrical characteristics of the LED; in addition, the refractive index of the sapphire is 1.8, the refractive index of the gallium nitride is 2.5, and due to the difference of the refractive indexes, when light enters the sapphire patterned substrate from the gallium nitride epitaxial layer, total reflection is formed, so that the light yield of the GaN-based light emitting diode is improved. The parameters of the LED device made of the epitaxial material based on the PSS substrate show that the optical power of the chip with the same size under the current density of 20A/cm < 2 > is increased by about 30% compared with the optical power of the device made of the sapphire flat substrate, so that the PSS substrate is an effective method for improving the light emitting efficiency of the gallium nitride-based light emitting diode.
Al in the prior art 2 O 3 With SiO 2 In the composite substrate, siO 2 Lower surface of (C) and Al 2 O 3 As shown in fig. 1, the composite substrate with pyramid-shaped three-dimensional pattern mainly reflects the light emitted from the LED by the conical surface of the pyramid, and more light emitted from the LED is required to be reflected, so that the pyramid-shaped three-dimensional pattern is more densely arranged on the substrate as possible, but because the sapphire substrate (Al 2 O 3 ) Harder, etching is more difficult, and when the pattern distribution is denser, the etching depth and accuracy are difficult to control.
Disclosure of Invention
The application aims to: aiming at the problems in the prior art, the application provides a preparation method of a composite patterned substrate and an epitaxial structure with air gaps, wherein the area of a middle dielectric film layer of a convex structure in the substrate prepared by the method is larger than the area of the bottom surface of an upper pattern layer and equal to the area of the top surface of a lower pattern layer.
The technical scheme is as follows: the application provides a preparation method of a composite patterned substrate, which comprises a substrate body, wherein the surface of the substrate body is provided with periodically arranged convex structures, and spacing grooves are arranged between adjacent convex structures; the raised structure comprises an upper pattern layer, a middle dielectric film layer and a lower pattern layer, wherein the area of the middle dielectric film layer is larger than the area of the bottom surface of the upper pattern layer and is equal to the area of the top surface of the lower pattern layer; the preparation method comprises the following steps: s1: depositing a first material layer for forming the middle dielectric film layer and a second material layer for forming the upper pattern layer on the surface of the substrate body in sequence; s2: coating positive photoresist on the second material layer, and then sequentially carrying out exposure and development processes to prepare a photoetching window with periodic arrangement on the second material layer; s3: sequentially etching the material layer II, the material layer I and part of the substrate body in the photoetching window by using a first dry etching process to form the interval groove; s4: and etching out part of the second material layer covered by the positive photoresist by using a second dry etching process to expose part of the first material layer, and forming the convex structure to obtain the composite patterned substrate.
Preferably, in S3, the conditions of the first dry etching are: pure boron trichloride (BCl) 3 ) The gas is used as etching gas, the gas flow is 90 sccm-150 sccm, the etching power is 400W-700W, the cavity pressure is 1.5 mT-4 mT, and the time is 5 min-40 min. In the first step of dry etching process, the etching gas is boron trichloride, the etching process is mainly physical bombardment, the lateral chemical etching effect on the first material layer, the second material layer and the substrate body is weak, the slope of the etched composite graph side wall is consistent, and flat interval grooves are easy to form.
Preferably, in S4, the two-step dry etching conditions are:using pure trifluoromethane (CHF) 3 ) The gas is used as etching gas, the gas flow is 50 sccm-200 sccm, the etching power is 200W-500W, the cavity pressure is 3 mT-40 mT, and the time is 1 min-10 min. In the second dry etching, because the energy carried by the trifluoromethane plasma is low, the bombardment etching effect on the surface of the material with high hardness such as sapphire, titanium dioxide, aluminum nitride and the like is not enough, and CHF is generated 3 The gas has chemical corrosion effect on silicon dioxide, so that the whole etching process only carries out lateral chemical corrosion on the material layer II, the material layer I and the substrate body have little etching effect, the material layer II is gradually etched into a cone structure with a small upper part and a large lower part, the material layer I is exposed after the lower part of the material layer II is etched, and a middle dielectric film layer with the area larger than the bottom surface area of the upper pattern layer and equal to the top surface area of the lower pattern layer is formed.
Preferably, the thickness of the positive photoresist is 1000 nm-3000 nm; and/or the thickness of the first material layer is 5 nm-500 nm; and/or the thickness of the second material layer is 500 nm-2500 nm
Preferably, the thickness of the middle dielectric film layer is 10 nm-400 nm.
Preferably, the upper pattern layer is in a cone or pyramid structure, the lower pattern layer is in a truncated cone structure, and the upper pattern layer, the middle dielectric film layer and the lower pattern layer are coaxially arranged.
Preferably, the bottom diameter d1 of the upper pattern layer is 30% -85% of the period P of the protruding structure; the height h1 is 300nm to 2000 nm; and/or the bottom diameter d2 of the lower pattern layer is 60% -96% of the period P of the protruding structure; the height h2 is 50 nm-500 nm; and/or the period P of the protruding structure is 500 nm-5000 nm.
Preferably, the second material layer is made of silicon dioxide; and/or the first material layer is made of titanium dioxide or aluminum nitride; and/or the lower pattern layer and the substrate body are made of the same material and are made of sapphire.
The application also provides an LED epitaxial structure with an air gap, which comprises the patterned substrate.
Further, the LED epitaxial structure with the air gap further comprises an N-type layer, a light-emitting layer and a P-type layer which are sequentially arranged on the patterned substrate; an air gap is provided between the N-type layer and each of the raised structures.
The beneficial effects are that: in the composite patterned substrate, a middle dielectric film layer is arranged between an upper pattern layer and a lower pattern layer in a convex structure, and the area of the middle dielectric film layer is larger than the area of the bottom surface of the upper pattern layer and is equal to the area of the top surface of the lower pattern layer; in the application, two-step dry etching is used in the preparation of the raised structures, in the first-step dry etching process, the second material layer in the photoetching window is etched firstly, then the first material layer below and part of the substrate body are further etched downwards to form a spacing groove with a smooth bottom surface between every two raised structures, meanwhile, the first-step dry etching can also carry out partial etching on the positive photoresist, the thickness of the positive photoresist is gradually reduced in the etching process, and the area is gradually reduced from the edges of two sides to the middle. And then carrying out second-step dry etching, wherein the second-step dry etching adjusts the etching gas used, so that the second-step etching can only carry out lateral etching on the first material layer and the substrate body, and has no etching effect on the first material layer, thus the second material layer can gradually form an upper pattern layer of a cone structure through the second-step dry etching process, the first material layer surrounding the periphery of the lower part of the upper pattern layer is gradually exposed, and finally, a middle dielectric film layer with the area larger than the area of the bottom surface of the upper pattern layer and equal to the area of the top surface of the lower pattern layer is formed, so that a convex structure is formed.
Because the special structures of the convex structures are arranged, the bottom surfaces of the interval grooves between the adjacent convex structures are smooth planes which are made of the same material as the substrate body, when an N-type layer (N-type gallium nitride) grows on the substrate structure, N can selectively grow in the interval grooves with the smooth bottom surfaces and cannot grow on a rough surface, so that a large air gap is formed among an upper pattern layer, a middle dielectric film layer and the N-type layer of the convex structures after the N-type layer grows, the refractive index of the air gap area is 1, and obvious refractive index difference exists between the air gap area and other material layers, so that light emitted from an LED can generate a larger reflection effect in the area, the reflection of the light emitted from the LED can be increased, the light emitting efficiency is improved, and the brightness is improved.
The preparation process flow of the composite patterned substrate is simple, the processing efficiency is high, the structural performance is stable, the cost is low, and the reliability is good.
Drawings
FIG. 1 is a side cross-sectional view of a prior art sapphire substrate having pyramid-shaped relief patterns;
FIGS. 2 to 5 are schematic process flow diagrams of a method for fabricating a composite patterned substrate according to the present application;
FIG. 6 is a scanning electron microscope image of a composite patterned substrate prepared by the present method;
fig. 7 is a schematic diagram of an LED epitaxial structure with air gaps comprising a composite patterned substrate.
Description of the embodiments
The present application will be described in detail with reference to the accompanying drawings.
The embodiment provides a preparation method of a composite patterned substrate, which comprises the following steps:
s1: as shown in fig. 2, a first material layer 8 for forming a middle dielectric film layer 203 and a second material layer 4 for forming an upper pattern layer 201 are sequentially deposited on the surface of the sapphire substrate body 1; the first material layer 8 is made of titanium dioxide and has the thickness of 100 a nm, the second material layer 4 is made of silicon dioxide and has the thickness of 2000 a nm a.
S2: as shown in fig. 3, a positive photoresist 3 with a thickness of 2400 nm is coated on a second material layer 4, and then exposure and development processes are sequentially performed to prepare a photolithography window 301 with periodic arrangement on the second material layer 4;
s3: as shown in fig. 4, a first dry etching process is used to etch away the second material layer 4 in the photolithography window 301 and further etch away the first material layer 8 and a portion of the substrate body 1, so as to form a spacer trench 101; meanwhile, the positive photoresist 3 with partial thickness is etched, the thickness of the positive photoresist 3 is gradually reduced in the etching process, the edges of the positive photoresist are gradually etched, and the area of the positive photoresist is gradually reduced from the edges of two sides to the middle.
The first dry etching process comprises the following steps: pure boron trichloride gas is used as etching gas, the gas flow is 100 sccm, the etching power is 600W, the cavity pressure is 2 mT, and the time is 20 min. In the one-stage dry etching, the etching gas is BCl 3 The physical bombardment is mainly performed, so that the etching effect is more vertical etching, the vertical etching effect on the material layer two 4, the material layer one 8 and the substrate body 1 is better, and the spacing groove 101 is easier to form.
S4: the positive photoresist 3 and the part of the material layer two 4 covered by it are gradually etched away using a second dry etching process, as shown in fig. 5. The positive photoresist 3 is etched completely, the side wall of the second silicon dioxide material layer 4 below the positive photoresist is etched gradually to form an upper pattern layer 201 with a cone structure towards the middle, the first material layer 8 around the lower part of the positive photoresist is gradually exposed to form a middle dielectric film layer 203, the substrate body 1 below the middle dielectric film layer 203 forms a lower pattern layer 202 with a truncated cone structure, the upper pattern layer 201, the middle dielectric film layer 203 and the lower pattern layer 202 form a convex structure 2 together, and a spacing groove 101 is arranged between every two adjacent convex structures 2.
The second dry etching process comprises the following steps: using pure CHF 3 The gas is used as etching gas, the gas flow is 50 sccm, the etching power is 300W, the cavity pressure is 20 mT, and the time is 5 min. In the second dry etching, since the etching gas is pure CHF 3 The second material layer 4 can only be etched laterally, and hardly acts on the first material layer 8 and the substrate body 1, so that the second material layer 4 can gradually form the upper pattern layer 201 of the cone structure through the second dry etching process, and gradually expose the first material layer 8 surrounding the lower periphery of the upper pattern layer 201, and finally form the middle dielectric film layer 203 with an area larger than the bottom surface area of the upper pattern layer 201 and equal to the top surface area of the lower pattern layer 202, so as to form the protruding structure 2.
As shown in fig. 5, the composite patterned substrate prepared by the above steps includes a sapphire substrate body 1 having periodically arranged bump structures 2 on the surface, and spacer grooves 101 are provided between adjacent bump structures 2; the period of the bump structure 2 was 3000nm. The upper pattern layer 201 of the cone structure, the circular middle medium film layer 203 and the lower pattern layer 202 of the truncated cone structure are coaxially arranged in the bulge structure 2, the area of the middle medium film layer 203 is larger than the area of the bottom surface of the upper pattern layer 201 and equal to the area of the top surface of the lower pattern layer 202, and the lower pattern layer 202 and the substrate body 1 are made of the same material and are made of sapphire. The middle dielectric thin film layer 203 is coaxially arranged with the upper pattern layer 201 and the lower pattern layer 202, the outer diameter of the middle dielectric thin film layer 203 is overlapped with the outer diameter d2 of the lower pattern layer 202, the bottom diameter d1 of the upper pattern layer 201 is about 2300nm, and the height h1 is about 1000nm; the bottom diameter d2 of the lower pattern layer 202 is about 2800nm; the height h2 is about 200nm. Fig. 6 is a top view of a scanning electron microscope of the composite patterned substrate.
And depositing an N-type layer 5, a light-emitting layer 6 and a P-type layer 7 on the surface of the composite patterned substrate in sequence to obtain the LED epitaxial structure with the air gap, as shown in fig. 7. Since the middle dielectric thin film layer 203 is exposed after two-step dry etching, and the bottom surfaces of the interval grooves 101 between the adjacent bump structures 2 are planes made of the same material as the substrate body 1, when the N-type layer (N-type gallium nitride) 5 grows on the substrate structure, the N-type layer 5 selectively grows in the interval grooves 101 and cannot grow on the middle dielectric thin film layer 203, so that a larger air gap 9 is formed between the upper pattern layer 201 and the middle dielectric thin film layer 203 of the bump structures 2 and the N-type layer 5 until the growth is finished, the air in the air gap 9 is different from the surrounding N-type layer 5 and the upper pattern layer 201 and the lower pattern layer 202 in reflectivity, so that more refraction and reflection of light emitted by the LED can occur in the area at the position of the air gap 9, the reflection of the light emitted by the LED can be increased, the light emitting efficiency can be improved, and the brightness can be improved.
The foregoing embodiments are merely illustrative of the technical concept and features of the present application, and are intended to enable those skilled in the art to understand the present application and to implement the same, not to limit the scope of the present application. All equivalent changes or modifications made according to the spirit of the present application should be included in the scope of the present application.
Claims (9)
1. The preparation method of the composite patterned substrate is characterized in that the composite patterned substrate comprises a substrate body (1) with periodically arranged convex structures (2) on the surface, and spacing grooves (101) are formed between adjacent convex structures (2); the raised structure (2) comprises an upper pattern layer (201), a middle dielectric film layer (203) and a lower pattern layer (202), wherein the area of the middle dielectric film layer (203) is larger than the area of the bottom surface of the upper pattern layer (201) and is equal to the area of the top surface of the lower pattern layer (202); the preparation method comprises the following steps:
s1: depositing a first material layer (8) for forming the middle dielectric film layer (203) and a second material layer (4) for forming the upper pattern layer (201) on the surface of the substrate body (1) in sequence;
s2: coating positive photoresist (3) on the second material layer (4), and then sequentially carrying out exposure and development processes to prepare a photoetching window (301) with periodic arrangement on the second material layer (4);
s3: sequentially etching the second material layer (4), the first material layer (8) and part of the substrate body (1) in the photoetching window (301) by using a first dry etching process to form the interval groove (101);
s4: etching away part of the second material layer (4) covered by the positive photoresist (3) by using a second dry etching process to expose part of the first material layer (8) so as to form the raised structure (2) and obtain the composite graphical substrate;
wherein the second material layer (4) is made of silicon dioxide; and/or the material layer I (8) is made of titanium dioxide or aluminum nitride.
2. The method for preparing a composite patterned substrate according to claim 1, wherein in S3, the conditions of the first dry etching are: pure boron trichloride gas is used as etching gas, the gas flow is 90 sccm-150 sccm, the etching power is 400W-700W, the cavity pressure is 1.5 mT-4 mT, and the time is 5 min-40 min.
3. The method for preparing a composite patterned substrate according to claim 1, wherein in S4, the two-step dry etching conditions are: and pure trifluoromethane gas is used as etching gas, the gas flow is 50 sccm-200 sccm, the etching power is 100-500W, the cavity pressure is 3 mT-40 mT, and the time is 1-10 min.
4. The method for preparing a composite patterned substrate according to claim 1, wherein the positive photoresist (3) has a thickness of 1000nm to 3000 nm;
and/or the thickness of the material layer I (8) is 10 nm-400 nm;
and/or the thickness of the material layer II (4) is 500 nm-2500 nm.
5. The method for preparing a composite patterned substrate according to claim 1, wherein the upper pattern layer (201) has a cone or pyramid structure, the lower pattern layer (202) has a truncated cone structure, and the upper pattern layer (201), the middle dielectric thin film layer (203) and the lower pattern layer (202) are coaxially arranged.
6. The method of manufacturing a composite patterned substrate according to claim 5, wherein the bottom diameter d1 of the upper pattern layer (201) is 30% -85% of the period P of the bump structure (2); the height h1 is 300nm to 2000 nm;
and/or, the bottom diameter d2 of the lower pattern layer (202) is 60% -96% of the period P of the protruding structure (2); the height h2 is 50 nm-500 nm;
and/or the period P of the protruding structure (2) is 500 nm-5000 nm.
7. The method for producing a composite patterned substrate according to any one of claims 1 to 6, wherein,
the lower pattern layer (202) is made of the same material as the substrate body (1) and is made of sapphire.
8. An LED epitaxial structure with air gaps, characterized by comprising a composite patterned substrate prepared by the preparation method of any one of claims 1 to 7.
9. The LED epitaxial structure with air gap of claim 8, further comprising an N-type layer (5), a light emitting layer (6) and a P-type layer (7) disposed in sequence on the patterned substrate; an air gap (9) is provided between the N-type layer (5) and each of the raised structures (2).
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