CN114203875B - Patterned composite substrate, preparation method and LED epitaxial wafer - Google Patents
Patterned composite substrate, preparation method and LED epitaxial wafer Download PDFInfo
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- CN114203875B CN114203875B CN202111500526.2A CN202111500526A CN114203875B CN 114203875 B CN114203875 B CN 114203875B CN 202111500526 A CN202111500526 A CN 202111500526A CN 114203875 B CN114203875 B CN 114203875B
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- 239000000758 substrate Substances 0.000 title claims abstract description 146
- 239000002131 composite material Substances 0.000 title claims abstract description 72
- 238000002360 preparation method Methods 0.000 title abstract description 12
- VYPSYNLAJGMNEJ-UHFFFAOYSA-N Silicium dioxide Chemical compound O=[Si]=O VYPSYNLAJGMNEJ-UHFFFAOYSA-N 0.000 claims abstract description 413
- 239000000377 silicon dioxide Substances 0.000 claims abstract description 206
- 235000012239 silicon dioxide Nutrition 0.000 claims abstract description 171
- 229910052594 sapphire Inorganic materials 0.000 claims abstract description 58
- 239000010980 sapphire Substances 0.000 claims abstract description 58
- 229910052731 fluorine Inorganic materials 0.000 claims description 52
- 239000011737 fluorine Substances 0.000 claims description 44
- 238000000034 method Methods 0.000 claims description 44
- YCKRFDGAMUMZLT-UHFFFAOYSA-N Fluorine atom Chemical compound [F] YCKRFDGAMUMZLT-UHFFFAOYSA-N 0.000 claims description 42
- 125000001153 fluoro group Chemical group F* 0.000 claims description 29
- 238000000623 plasma-assisted chemical vapour deposition Methods 0.000 claims description 11
- 238000000059 patterning Methods 0.000 claims description 8
- XPDWGBQVDMORPB-UHFFFAOYSA-N Fluoroform Chemical compound FC(F)F XPDWGBQVDMORPB-UHFFFAOYSA-N 0.000 claims description 7
- 238000000151 deposition Methods 0.000 claims description 7
- WMIYKQLTONQJES-UHFFFAOYSA-N hexafluoroethane Chemical compound FC(F)(F)C(F)(F)F WMIYKQLTONQJES-UHFFFAOYSA-N 0.000 claims description 5
- TXEYQDLBPFQVAA-UHFFFAOYSA-N tetrafluoromethane Chemical compound FC(F)(F)F TXEYQDLBPFQVAA-UHFFFAOYSA-N 0.000 claims description 4
- 238000001755 magnetron sputter deposition Methods 0.000 claims description 3
- 238000002207 thermal evaporation Methods 0.000 claims description 3
- 238000004519 manufacturing process Methods 0.000 claims 2
- 238000005229 chemical vapour deposition Methods 0.000 claims 1
- 125000004122 cyclic group Chemical group 0.000 claims 1
- 239000000463 material Substances 0.000 abstract description 46
- 238000005530 etching Methods 0.000 abstract description 14
- 238000000605 extraction Methods 0.000 abstract description 13
- 238000001312 dry etching Methods 0.000 abstract description 9
- 230000009286 beneficial effect Effects 0.000 abstract description 4
- 229920002120 photoresistant polymer Polymers 0.000 description 24
- 238000010586 diagram Methods 0.000 description 14
- 239000007789 gas Substances 0.000 description 10
- 238000004140 cleaning Methods 0.000 description 6
- 238000009616 inductively coupled plasma Methods 0.000 description 5
- 230000000737 periodic effect Effects 0.000 description 5
- 230000008021 deposition Effects 0.000 description 4
- 238000005516 engineering process Methods 0.000 description 4
- 239000000126 substance Substances 0.000 description 4
- 230000007547 defect Effects 0.000 description 3
- 238000001579 optical reflectometry Methods 0.000 description 3
- BLRPTPMANUNPDV-UHFFFAOYSA-N Silane Chemical compound [SiH4] BLRPTPMANUNPDV-UHFFFAOYSA-N 0.000 description 2
- XUIMIQQOPSSXEZ-UHFFFAOYSA-N Silicon Chemical compound [Si] XUIMIQQOPSSXEZ-UHFFFAOYSA-N 0.000 description 2
- 239000013078 crystal Substances 0.000 description 2
- 230000007423 decrease Effects 0.000 description 2
- 230000000694 effects Effects 0.000 description 2
- 238000003384 imaging method Methods 0.000 description 2
- 229910052710 silicon Inorganic materials 0.000 description 2
- 239000010703 silicon Substances 0.000 description 2
- 238000004088 simulation Methods 0.000 description 2
- BOXJYHMFXVNZMY-UHFFFAOYSA-N [Si](=O)=O.[F] Chemical compound [Si](=O)=O.[F] BOXJYHMFXVNZMY-UHFFFAOYSA-N 0.000 description 1
- 125000004429 atom Chemical group 0.000 description 1
- 238000005452 bending Methods 0.000 description 1
- 230000015572 biosynthetic process Effects 0.000 description 1
- 238000006243 chemical reaction Methods 0.000 description 1
- 239000003153 chemical reaction reagent Substances 0.000 description 1
- 229910052681 coesite Inorganic materials 0.000 description 1
- 229910052906 cristobalite Inorganic materials 0.000 description 1
- 238000002425 crystallisation Methods 0.000 description 1
- 230000008025 crystallization Effects 0.000 description 1
- 230000003247 decreasing effect Effects 0.000 description 1
- 238000005137 deposition process Methods 0.000 description 1
- 239000001307 helium Substances 0.000 description 1
- 229910052734 helium Inorganic materials 0.000 description 1
- SWQJXJOGLNCZEY-UHFFFAOYSA-N helium atom Chemical compound [He] SWQJXJOGLNCZEY-UHFFFAOYSA-N 0.000 description 1
- 125000005842 heteroatom Chemical group 0.000 description 1
- 239000012535 impurity Substances 0.000 description 1
- 238000002347 injection Methods 0.000 description 1
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- 238000012536 packaging technology Methods 0.000 description 1
- 238000001259 photo etching Methods 0.000 description 1
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- 230000001737 promoting effect Effects 0.000 description 1
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- 238000006467 substitution reaction Methods 0.000 description 1
- FAQYAMRNWDIXMY-UHFFFAOYSA-N trichloroborane Chemical compound ClB(Cl)Cl FAQYAMRNWDIXMY-UHFFFAOYSA-N 0.000 description 1
- 229910052905 tridymite Inorganic materials 0.000 description 1
Classifications
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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
-
- 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
-
- 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
- H01L33/10—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 light reflecting structure, e.g. semiconductor Bragg reflector
-
- Y—GENERAL TAGGING OF NEW TECHNOLOGICAL DEVELOPMENTS; GENERAL TAGGING OF CROSS-SECTIONAL TECHNOLOGIES SPANNING OVER SEVERAL SECTIONS OF THE IPC; TECHNICAL SUBJECTS COVERED BY FORMER USPC CROSS-REFERENCE ART COLLECTIONS [XRACs] AND DIGESTS
- Y02—TECHNOLOGIES OR APPLICATIONS FOR MITIGATION OR ADAPTATION AGAINST CLIMATE CHANGE
- Y02P—CLIMATE CHANGE MITIGATION TECHNOLOGIES IN THE PRODUCTION OR PROCESSING OF GOODS
- Y02P70/00—Climate change mitigation technologies in the production process for final industrial or consumer products
- Y02P70/50—Manufacturing or production processes characterised by the final manufactured product
Abstract
The embodiment of the invention discloses a patterned composite substrate, a preparation method and an LED epitaxial wafer. Wherein the substrate comprises: a sapphire substrate; the microstructure protrusions are located on the sapphire substrate and comprise fluorine-doped silicon dioxide, and the refractive index of the fluorine-doped silicon dioxide is smaller than that of the silicon dioxide. According to the patterned composite substrate, the preparation method thereof and the LED epitaxial wafer, the microstructure protrusions made of the fluorine-doped silicon dioxide material are prepared above the sapphire substrate, and as the refractive index of the fluorine-doped silicon dioxide material is lower, the refractive index difference between the substrate and the epitaxial layer material is larger, the total reflection angle is increased, the light extraction rate can be improved, and the brightness of the epitaxial end and the chip end can be improved. In addition, compared with the traditional silicon dioxide substrate material, the fluorine-doped silicon dioxide substrate material with low refractive index is easier to etch under the same condition, has high etching rate and higher etching selectivity ratio, and is beneficial to improving the productivity of dry etching.
Description
Technical Field
The embodiment of the invention relates to the field of semiconductors, in particular to a patterned composite substrate, a preparation method and an LED epitaxial wafer.
Background
The silicon dioxide patterned composite substrate can improve the crystal quality and the light-emitting efficiency of the GaN-based LED device. On the one hand, in epitaxial growth, in order to enable dislocation in GaN material grown at the pattern window to warp along the side of the pattern and then fold at the top of the pattern, the key problem is to avoid GaN material growing on the side of the periodic pattern of the patterned substrate as much as possible, while it is difficult for the conventional Patterned Sapphire Substrate (PSS) to make GaN material not grow on the side of the periodic pattern. However, the silicon dioxide patterned composite substrate has obvious advantages in this respect, and since the silicon dioxide material is not suitable for GaN to grow on, the silicon dioxide material is easy to grow on the side surface of the pattern when growing, thereby promoting bending of dislocation along the side surface of the pattern and folding of dislocation at the top of the pattern, and further improving the crystal quality of the GaN material. On the other hand, PSS forms the reflection grating to improve the light-emitting rate of the LED device, the larger difference between the refractive index of the GaN material and the refractive index of the sapphire material is an important factor influencing the reflection formation, the refractive index of the GaN material is 2.5, the refractive index of the sapphire is 1.76, and the larger difference between the GaN material and the sapphire material forms a larger total reflection angle, so that the light-emitting efficiency of the LED is improved. In this aspect, the silicon dioxide material in the silicon dioxide patterned composite substrate has a larger refractive index difference with GaN, the refractive index of silicon dioxide is 1.46, the total reflection angle formed by the silicon dioxide material and the GaN material is larger, and the formed reflection grating can reflect more light rays, so that the light extraction efficiency is further improved.
With the continuous progress of patterning composite substrates, epitaxial nitride buffer layers and other technologies, the space for improving the quantum efficiency in the epitaxial layers is smaller, and the improvement of the light extraction rate of the substrates is more important.
Disclosure of Invention
The invention provides a patterned composite substrate, a preparation method and an LED epitaxial wafer, which are used for improving the light extraction rate of the patterned composite substrate and improving the light emitting efficiency of an LED.
In a first aspect, an embodiment of the present invention provides a patterned composite substrate, including:
a sapphire substrate;
and the microstructure protrusions are positioned on the sapphire substrate and comprise fluorine-doped silicon dioxide, and the refractive index of the fluorine-doped silicon dioxide is smaller than that of the silicon dioxide.
In a second aspect, an embodiment of the present invention further provides a method for preparing a patterned composite substrate, including:
providing a flat sapphire substrate;
and forming a plurality of microstructure protrusions on the flat piece sapphire substrate, wherein the microstructure protrusions comprise fluorine-doped silicon dioxide, and the refractive index of the fluorine-doped silicon dioxide is smaller than that of the silicon dioxide.
In a third aspect, an embodiment of the present invention further provides an LED epitaxial wafer, including the patterned composite substrate provided in any embodiment of the present invention.
According to the technical scheme provided by the embodiment of the invention, the microstructure protrusion formed by the fluorine-doped silicon dioxide material is prepared above the sapphire substrate, and the refractive index difference between the substrate and the epitaxial layer material is larger due to the lower refractive index of the fluorine-doped silicon dioxide material, so that the total reflection angle is increased, the light extraction rate can be improved, and the brightness of the epitaxial end and the chip end can be improved. In addition, compared with the traditional silicon dioxide substrate material, the fluorine-doped silicon dioxide substrate material with low refractive index is easier to etch under the same condition, has high etching rate and higher etching selectivity ratio, and is beneficial to improving the productivity of dry etching.
Drawings
FIG. 1 is a schematic diagram illustrating a simulation of the path of light through different substrates according to an embodiment of the present invention;
FIG. 2 is a schematic structural diagram of a patterned composite substrate according to an embodiment of the present invention;
FIG. 3 is a schematic structural diagram of another patterned composite substrate according to an embodiment of the present invention;
FIG. 4 is a schematic structural diagram of a DBR microstructure protrusion according to an embodiment of the present invention;
FIG. 5 is a graph showing the relationship between fluorine doping concentration and refractive index of fluorine doped silicon dioxide layer according to the embodiment of the present invention;
FIG. 6 is a flowchart of a method for fabricating a patterned composite substrate according to an embodiment of the present invention;
FIG. 7 is a schematic diagram of a method for preparing a patterned composite substrate according to an embodiment of the present invention;
FIG. 8 is a flowchart of another method for fabricating a patterned composite substrate according to an embodiment of the present invention;
FIG. 9 is a schematic diagram of another method for preparing a patterned composite substrate according to an embodiment of the present invention;
fig. 10 is a schematic structural diagram of an LED epitaxial wafer according to an embodiment of the present invention.
Detailed Description
The invention is described in further detail below with reference to the drawings and examples. It is to be understood that the specific embodiments described herein are merely illustrative of the invention and are not limiting thereof. It should be further noted that, for convenience of description, only some, but not all of the structures related to the present invention are shown in the drawings.
In order to further improve the light extraction rate of the patterned composite substrate, the embodiment of the invention simulates the light paths of different substrate materials, fig. 1 is a schematic diagram of the simulation of the light paths of different substrates provided by the embodiment of the invention, the substrate in fig. 1 a) is a sapphire flat sheet, the substrate in fig. 1 b) is a patterned sapphire substrate, and the substrate in fig. 1 c) is a patterned composite substrate. In FIG. 1, the propagation path of light between two materials of different refractive index is shown, the upper layer in FIG. 1 a) being a GaN epitaxial layer, refractive index n GaN 2.5, light is incident from the GaN epitaxial layer to the sapphire flat substrate, and the refractive index of the sapphire substrate is n sapphire 1.78; the upper layer in fig. 1 b) is still a GaN epitaxial layer from which light is incident to the patterned sapphire substrate; in FIG. 1 c) the upper layer material is still a GaN epitaxial layer, where light is incident from the GaN epitaxial layer to the patterned composite substrate, the patterned layer in the patterned composite substrate is silicon dioxide, the refractive index n of the silicon dioxide layer SiO2 1.45. As can be seen from comparison of fig. 1 a) and 1 b), the critical angle θ of the patterned sapphire substrate when light is incident is smaller relative to the sapphire flat sheet, the total reflection angle shown by the solid line in the figure is larger, and the light extraction efficiency is correspondingly improved; as can be seen from a comparison of fig. 1 b) and 1 c), the lower the refractive index of the patterned layer in the substrate, the larger the refractive index difference from the epitaxial layer material layer, the smaller the critical angle θ at which light is incident, the more easily the total reflection phenomenon occurs, and the higher the light extraction rate. Therefore, the light extraction rate of the substrate can be increased by decreasing the refractive index of the patterned composite substrate.
Based on the principle, the invention provides a patterned composite substrate, a preparation method and an LED epitaxial wafer aiming at the problems in the background technology.
Fig. 2 is a schematic structural diagram of a patterned composite substrate according to an embodiment of the present invention, where, as shown in fig. 2, the patterned composite substrate includes: a sapphire substrate 10; a plurality of microstructure protrusions 11 on the sapphire substrate 10, the microstructure protrusions 11 comprising fluorine-doped silica having a refractive index smaller than that of silica.
Wherein, sapphire Ping Pianji plate can be selected as sapphire substrate 10, and the size can be selected according to the requirement. The specific shape of the microstructure protrusion 11 is not limited in the embodiment of the invention, and the microstructure protrusion 11 can be conical, truncated cone-like, polygonal cone-like or polygonal table-like, and the like, and optionally, the side wall of the microstructure protrusion 11 can also have a certain radian, and an epitaxial layer can be grown on a patterned composite substrate formed by the microstructure protrusions 11 with the radian of the side wall, so that lateral epitaxial growth can be better realized, dislocation density of the GaN epitaxial layer can be reduced more, and growth quality of epitaxial layer materials can be improved.
The material of the microstructure protrusion 11 includes fluorine-doped silicon dioxide, and compared with pure silicon dioxide, the fluorine-doped silicon dioxide with fluorine atoms has a lower refractive index, so that the light extraction rate of the substrate can be improved, and the brightness of the epitaxial end and the chip end can be improved.
According to the patterned composite substrate provided by the embodiment of the invention, the microstructure protrusions above the sapphire substrate are set to be fluorine-doped silicon dioxide, the refractive index of fluorine-doped silicon dioxide material is lower, the refractive index difference between the fluorine-doped silicon dioxide material and the epitaxial layer material is larger, the total reflection angle is increased, the light extraction rate can be improved, and the brightness of the epitaxial end and the chip end is improved. In addition, compared with the traditional silicon dioxide substrate material, the fluorine-doped silicon dioxide substrate material with low refractive index is easier to etch under the same condition, has high etching rate and higher etching selectivity ratio, and is beneficial to improving the productivity of dry etching.
As a preferred embodiment, the microstructure protrusion 11 may be a DBR microstructure protrusion including a periodically layered silicon dioxide layer and a fluorine-doped silicon dioxide layer having a refractive index smaller than that of the silicon dioxide layer. Fig. 3 is a schematic structural diagram of another patterned composite substrate provided by the embodiment of the present invention, fig. 4 is a schematic structural diagram of a DBR microstructure protrusion provided by the embodiment of the present invention, and the patterned composite substrate is described below with reference to fig. 3 and 4.
The DBR microstructure protrusion 12 is referred to herein as a distributed bragg mirror microprotrusion structure. In the embodiment of the present invention, the microstructure protrusion 11 may be a DBR microstructure protrusion 12, and the DBR microstructure protrusion 12 may include a periodically laminated silicon dioxide layer 13 and a fluorine doped silicon dioxide layer 14, where the refractive index of the fluorine doped silicon dioxide layer 14 is smaller than the refractive index of the silicon dioxide layer 13. The structure of the silicon dioxide layer 13 and the fluorine-doped silicon dioxide 14 may be referred to as a silicon dioxide-fluorine-doped silicon dioxide stack. Referring to fig. 4, the DBR microstructure protrusion 12 includes a silicon dioxide layer 13 and a fluorine-doped silicon dioxide layer 14, wherein the hetero layer in the DBR microstructure protrusion 12 near the sapphire substrate 10 is the fluorine-doped silicon dioxide layer 14 with a lower refractive index, and the silicon dioxide layer 13 is above the fluorine-doped silicon dioxide layer 14. The DBR microstructure protrusions 12 formed of two materials having different refractive indexes can further enhance total reflection of light, thereby further improving light reflectivity.
Alternatively, the number of the silica-fluorine doped silica stacks in the DBR microstructure protrusion 12 is not limited, that is, the DBR microstructure protrusion 12 may include n silica-fluorine doped silica stacks, where the specific value of n may be set by those skilled in the art according to the actual situation. As can be seen from fig. 4, the DBR microstructure protrusion 12 includes a plurality of fluorine-doped silica layers 14 and a plurality of silica layers 13, which are alternately stacked, and the number of layers in fig. 4 is merely an example and does not represent the actual situation.
The refractive index of the fluorine-doped silica layer 14 is related to the doping concentration of fluorine atoms therein, and the doping concentration range of fluorine atoms is not particularly limited in the embodiment of the present invention, and can be set by a person skilled in the art according to actual needs. Preferably, in the embodiment of the present invention, the doping concentration of fluorine atoms in the fluorine doped silicon dioxide layer 14 is in the range of 5% -15%.
Alternatively, the source of fluorine atoms may be fluorine source gases such as carbon tetrafluoride (CF 4), hexafluoroethane (C2F 6), and trifluoromethane (CHF 3), and fig. 5 is a graph of the relationship between the doping concentration of fluorine atoms and the refractive index of the fluorine-doped silicon dioxide layer according to the embodiment of the present invention, and the selection of the doping concentration of fluorine atoms in the embodiment of the present invention is illustrated by taking fig. 5 as an example.
Fig. 5 shows the refractive index of the corresponding fluorine doped silica layer 14 at different fluorine atom doping concentrations, wherein the abscissa corresponds to the different fluorine atom doping concentrations and the ordinate corresponds to the refractive index of the fluorine doped silica layer 14. As can be seen from fig. 5, when the fluorine atom doping concentration is zero, the refractive index of the pure silica material is 1.46, and as the fluorine atom doping concentration increases, the refractive index of the fluorine-doped silica layer 14 gradually decreases, and when the fluorine atom doping concentration is 5%, the refractive index of the fluorine-doped silica layer 14 is 1.42, and when the fluorine atom doping concentration increases to 15%, the refractive index of the fluorine-doped silica layer 14 decreases to 1.34. However, it is understood that the doping amount of fluorine atoms cannot be increased without limit, and too much doping amount of fluorine atoms may cause many defects and affect the reliability of the substrate. Therefore, the embodiment of the invention preferably controls the doping concentration of fluorine atoms to 5% -15%, so that the refractive index of the heterogeneous layer can be reduced, and more defects can not be generated to influence the normal use of the patterned composite substrate.
Alternatively, the refractive index of the fluorine doped silica layer 14 may be adjusted by changing the doping concentration of fluorine atoms. In the embodiment of the present invention, the refractive index of the fluorine-doped silica layer 14 is preferably in the range of 1.34 to 1.46.
In addition, the thicknesses of the silicon dioxide layer 13 and the fluorine doped silicon dioxide layer 14 are also related to the respective refractive indexes, and the thicknesses of the silicon dioxide layer 13 and the fluorine doped silicon dioxide layer 14 in the patterned composite substrate are not particularly limited, and may be set by those skilled in the art according to actual needs.
In the embodiments provided by the present invention, the method can be according to formula d 1 ＝λ 0 /4n 1 The thickness of the silicon dioxide layer 13 is calculated, wherein d 1 Thickness of silicon dioxide layer 13Degree, lambda 0 For the central wavelength of incident light, n 1 Is the refractive index of the silicon dioxide layer 13.
Correspondingly, the formula d can also be used 2 ＝λ 0 /4n 2 Calculating the thickness of the fluorine doped silica layer 14, wherein d 2 Lambda is the thickness of the fluorine doped silicon dioxide layer 14 0 Still being the central wavelength of the incident light, n 2 Is the refractive index of the fluorine doped silica layer 14. If the doping concentrations of fluorine atoms are different, the refractive index of the fluorine-doped silica layer 14 is also different, and the thickness of the fluorine-doped silica layer 14 is also different accordingly.
Alternatively, the thickness of the silicon dioxide layer 13 is in the range of 60-90nm and the thickness of the fluorine doped silicon dioxide layer 14 is in the range of 70-100nm.
The thickness of each heterogeneous layer can be set according to actual needs by those skilled in the art. In the embodiment of the invention, the thickness of the silicon dioxide layer 13 is preferably 60-90nm, and the thickness of the fluorine-doped silicon dioxide layer 14 is preferably 70-100nm. In addition, the thickness of the corresponding heterogeneous layer can be set according to the refractive indexes of different heterogeneous layer materials, so that the thickness of the heterogeneous layer is matched with the refractive index of the materials, the thickness of the whole DBR microstructure protrusion 12 meets the requirement of low refractive index, and the light emitting rate of the patterned composite substrate is improved.
As a preferred embodiment, the thickness of the DBR microstructure projection 12 can range from 2.0 μm to 4.0 μm.
The thickness of the silicon dioxide layer 13, the thickness of the fluorine doped silicon dioxide layer 14, the number of layers of the silicon dioxide layer 13, the number of layers of the fluorine doped silicon dioxide layer 14 and the thickness of the entire DBR microstructure protrusion 12 are all related to each other, and the above parameters can be set by those skilled in the art according to experimental results.
The embodiment of the invention also provides a preparation method of the patterned composite substrate, which is used for preparing the patterned composite substrate provided by any embodiment of the invention, and fig. 6 is a flow chart of the preparation method of the patterned composite substrate provided by the embodiment of the invention; fig. 7 is a schematic diagram of a method for preparing a patterned composite substrate according to an embodiment of the present invention, and the method for preparing a patterned composite substrate according to the present invention is described below with reference to fig. 6 and 7:
referring to fig. 6, the method includes:
s110, providing a flat sapphire substrate.
The flat piece sapphire substrate 10 is the same as the sapphire substrate 10 in the above embodiment. Wherein, sapphire Ping Pianji plate can be selected as the flat sapphire substrate 10, and the size can be selected according to the requirement, and the method is not limited. Optionally, the flat sapphire substrate 10 is cleaned before use, and the cleaning mode may be chemical conventional cleaning, plasma cleaning, etc., where the chemical conventional cleaning refers to using a chemical reagent to clean impurities and stains on the sapphire flat substrate; plasma cleaning refers to the treatment of the sample surface by utilizing the properties of the active components in the plasma state substances to improve the surface crystallization of the sapphire flat substrate.
S120, forming a plurality of microstructure protrusions on the flat sapphire substrate, wherein the microstructure protrusions comprise fluorine-doped silicon dioxide, and the refractive index of the fluorine-doped silicon dioxide is smaller than that of the silicon dioxide.
The specific manner of forming the microstructure protrusions 11 on the flat sheet sapphire substrate 10 may be any prior art, and a fluorine-doped silicon dioxide layer may be deposited on the flat sheet sapphire substrate 10 and then patterned.
Alternatively, the process of forming the fluorine-doped silicon dioxide layer may adopt a plasma enhanced chemical vapor deposition, a vacuum thermal evaporation or a magnetron sputtering process, etc., and the embodiment of the invention preferably adopts a plasma enhanced chemical vapor deposition, and the deposition principle of the process is as follows: the gas containing atoms of the film components is ionized by microwaves or radio frequency, plasma is formed locally, the chemical activity of the plasma is strong, and the desired film is deposited on the substrate after the reaction. The plasma enhanced chemical vapor deposition process has high deposition rate, the prepared fluorine-doped silicon dioxide layer has better quality, and the fluorine-doped silicon dioxide layer is not easy to crack in the subsequent patterning process and the like. In addition, the refractive index of fluorine doped silica in the microstructure protrusions 11 in the embodiment of the present invention is lower than that of pure silica.
Further, any prior art may be used to perform patterning on the fluorine-doped silicon dioxide layer, for example, a photoresist layer may be deposited over the fluorine-doped silicon dioxide layer, then the photoresist layer may be subjected to patterning to form periodically arranged photoresist columns, and then a patterned composite substrate with the microstructure protrusions 11 may be obtained through a dry etching process.
Specifically, the photoresist can be uniformly coated on the fluorine-doped silicon dioxide layer through the photoresist, the choice of the photoresist is not limited, and any one of the existing photoresist can be selected, and the photoresist can be positive photoresist or negative photoresist. The thickness of the photoresist layer has a certain influence on the etching of the subsequent microstructure protrusion 11, and a person skilled in the art can set the thickness of the photoresist layer according to practical situations, and in the embodiment of the invention, the thickness of the photoresist layer is preferably set to be 1.0-3.0 μm. By setting a suitable photoresist layer thickness, the desired microstructure protrusions 11 can be ensured to be etched.
Further, the method of patterning the photoresist layer is any of the prior art, and is not limited herein, and may be, for example, photolithography exposure or nanoimprint. In addition, alternatively, the periodic arrangement of the photoresist columns may be any one of periodic square lattice arrangement, periodic hexagonal close-packed arrangement, aperiodic quasicrystal arrangement and random array arrangement, and the corresponding mask pattern may be selected according to actual requirements, which is not limited in the embodiment of the present invention.
Further, the fluorine doped silicon dioxide layer having the photoresist pillars may be etched by an inductively coupled plasma (Inductively Coupled Plasma, ICP) dry etching method to form the desired microstructure protrusions 11. The specific etching parameters in the ICP process can be set according to actual conditions. In addition, the specific shape of the etched microstructure protrusion 11 is not limited in the embodiment of the present invention, and preferably, a certain radian is provided on the sidewall of the microstructure protrusion 11, and the specific radian can be set according to practical situations. The microstructure protrusions 11 with the side wall radians can better utilize the scattering effect to scatter emergent light of the LED active region, break through the total reflection limit of the emergent light interface, improve the effective scattering area of the microstructure to light and improve the emergent light efficiency of the LED.
According to the preparation method of the imaging composite substrate, the plurality of microstructure protrusions comprising fluorine-doped silicon dioxide are formed on the flat sapphire substrate, and as the refractive index of the fluorine-doped silicon dioxide is smaller than that of the silicon dioxide, the difference between the refractive index of the imaging composite substrate formed based on the fluorine-doped silicon dioxide and that of an epitaxial layer material is larger, the total reflection angle is increased, the light extraction rate can be improved, and the brightness of an epitaxial end and a chip end can be improved. In addition, compared with the traditional silicon dioxide substrate material, the fluorine-doped silicon dioxide substrate material with low refractive index is easier to etch under the same condition, has high etching rate and higher etching selectivity ratio, and is beneficial to improving the productivity of dry etching.
On the basis of the above embodiment, the embodiment of the present invention further provides another method for preparing a patterned composite substrate, fig. 8 is a flowchart of another method for preparing a patterned composite substrate provided by the embodiment of the present invention, and fig. 9 is a schematic diagram of another method for preparing a patterned composite substrate provided by the embodiment of the present invention. In this method, the microstructure protrusions 11 may be provided as DBR microstructure protrusions 12. Referring to fig. 8, the method includes:
s210, providing a flat sapphire substrate.
S220, forming a DBR film layer on the flat sapphire substrate, wherein the DBR film layer comprises a silicon dioxide layer and a fluorine-doped silicon dioxide layer which are laminated periodically, and the refractive index of the fluorine-doped silicon dioxide layer is smaller than that of the silicon dioxide layer.
In this embodiment, the DBR film 15 may be formed on the flat sapphire substrate 10, and the DBR film 15 includes the silicon dioxide layer 13 and the fluorine-doped silicon dioxide layer 14 which are periodically stacked, wherein the refractive index of the fluorine-doped silicon dioxide layer 14 is smaller than the refractive index of the silicon dioxide layer 13. The patterned composite substrate formed by the DBR film layer 15 of the present embodiment can further enhance the light reflectivity due to the low refractive index of the fluorine-doped silica.
Alternatively, the silicon dioxide layer 13 and the fluorine-doped silicon dioxide layer 14 can be sequentially and alternately deposited by adopting a plasma enhanced chemical vapor deposition, a vacuum thermal evaporation or a magnetron sputtering process, and the thickness d of the silicon dioxide layer 13 1 The method meets the following conditions: d, d 1 ＝λ 0 /4n 1 Thickness d of fluorine doped silica layer 14 2 The method meets the following conditions: d, d 2 ＝λ 0 /4n 2 The method comprises the steps of carrying out a first treatment on the surface of the Wherein lambda is 0 For the center wavelength of incident light incident on the patterned composite substrate, n 1 Refractive index of silicon dioxide layer 13, n 2 Is the refractive index of the fluorine-doped silica 14.
Referring to fig. 9, a fluorine doped silicon dioxide layer 14 may be deposited on a flat piece of sapphire substrate 10, followed by deposition of a silicon dioxide layer 13 over the fluorine doped silicon dioxide layer 14. The number of the fluorine-doped silicon dioxide layer 14 and the silicon dioxide layer 13 can be set according to actual conditions.
Alternatively, the silicon dioxide layer 13 and the fluorine-doped silicon dioxide layer 14 are sequentially and alternately deposited by adopting a plasma enhanced chemical vapor deposition process; fluorine source gases in plasma enhanced chemical vapor deposition processes include CF4, C2F6, and CHF3.
The deposition methods of the silicon dioxide layer 13 and the fluorine doped silicon dioxide layer 14 can adopt a plasma enhanced chemical vapor deposition process. In preparing the fluorine-doped silica layer 14, a fluorine source gas may be introduced, and the fluorine source gas may be any gas capable of realizing fluorine atom injection, for example, may be: one of CF4, C2F6, and CHF3.
The refractive index of the fluorine-doped silica layer 14 is related to the doping concentration of fluorine atoms therein, and the doping concentration range of fluorine atoms is not particularly limited in the embodiment of the present invention, and can be set by a person skilled in the art according to actual needs. Preferably, in the embodiment of the present invention, the doping concentration of fluorine atoms in the fluorine doped silicon dioxide layer 14 is in the range of 5% -15%.
The relationship between the fluorine atom doping concentration and the refractive index of the fluorine doped silica layer 14 has been described in the above embodiments, and will not be described here again. The doping concentration of fluorine atoms can be adjusted by changing the introduction time, the introduction rate and the like of fluorine source gas in the deposition process.
In the embodiment of the invention, the doping concentration range of fluorine atoms is controlled to be 5% -15%, so that the refractive index of the DBR film layer 15 can be reduced, and more defects can not be generated to influence the normal use of the patterned composite substrate.
Alternatively, the refractive index of the fluorine doped silica layer 14 may be adjusted by changing the doping concentration of fluorine atoms. In the embodiment of the present invention, the refractive index of the fluorine-doped silica layer 14 is preferably in the range of 1.34 to 1.46.
In addition, the thicknesses of the silicon dioxide layer 13 and the fluorine doped silicon dioxide layer 14 are also related to the respective refractive indexes, and the thicknesses of the silicon dioxide layer 13 and the fluorine doped silicon dioxide layer 14 in the patterned composite substrate are not particularly limited, and may be set by those skilled in the art according to actual needs.
In the embodiments provided by the present invention, the method can be according to formula d 1 ＝λ 0 /4n 1 The thickness of the silicon dioxide layer 13 is calculated, wherein d 1 Thickness of silicon dioxide layer lambda 0 For the central wavelength of incident light, n 1 Is the refractive index of the silicon dioxide layer 13.
Correspondingly, the formula d can also be used 2 ＝λ 0 /4n 2 Calculating the thickness of the fluorine doped silica layer 14, wherein d 2 Lambda is the thickness of the fluorine doped silicon dioxide layer 14 0 Still being the central wavelength of the incident light, n 2 Is the refractive index of the fluorine doped silica layer 14. If the doping concentrations of fluorine atoms are different, the refractive index of the fluorine-doped silica layer 14 is also different, and the thickness of the fluorine-doped silica layer 14 is also different accordingly.
Alternatively, the thickness of the silicon dioxide layer 13 is in the range of 60-90nm and the thickness of the fluorine doped silicon dioxide layer 14 is in the range of 70-100nm.
The thickness of each heterogeneous layer can be set according to actual needs by those skilled in the art. In the embodiment of the invention, the thickness of the silicon dioxide layer 13 is preferably 60-90nm, and the thickness of the fluorine-doped silicon dioxide layer 14 is preferably 70-100nm. In addition, the thickness of the corresponding heterogeneous layer can be set according to the refractive indexes of different heterogeneous layer materials, so that the thickness of the heterogeneous layer is matched with the refractive index of the materials, the thickness of the whole DBR microstructure protrusion 12 finally obtained meets the requirement of low refractive index, and the light emitting rate of the patterned composite substrate is improved.
S230, patterning the DBR film layer to form a plurality of DBR microstructure protrusions.
Further, after the DBR film layer 15 is deposited, a photoresist layer 16 may be deposited over the DBR film layer 15, and then the photoresist layer 16 may be patterned to form periodically arranged photoresist pillars, and then a patterned composite substrate with DBR microstructure protrusions 12 may be obtained through a dry etching process.
As a preferred embodiment, the thickness of the DBR microstructure projection 12 can range from 2.0 μm to 4.0 μm. The thickness of the DBR microstructure protrusion 12 can be adjusted by adjusting various parameters in the dry etching process.
The thickness of the silicon dioxide layer 13, the thickness of the fluorine doped silicon dioxide layer 14, the number of layers of the silicon dioxide layer 13, the number of layers of the fluorine doped silicon dioxide layer 14 and the thickness of the entire DBR microstructure protrusion 12 are all related to each other, and the above parameters can be set by those skilled in the art according to experimental results.
The patterning method for the DBR film 15 is the same as that in the above embodiment, and will not be described here again.
According to the preparation method of the patterned composite substrate, provided by the embodiment of the invention, a fluorine source gas is introduced above a flat sapphire substrate to prepare a fluorine-doped silicon dioxide layer, a silicon dioxide layer is deposited above the fluorine-doped silicon dioxide layer, two film layers are sequentially and alternately deposited to form a DBR film layer, and the DBR film layer is subjected to patterned etching, so that the patterned composite substrate is finally obtained. Because the refractive index of the fluorine-doped silicon dioxide is low, the patterned composite substrate after the fluorine-doped silicon dioxide layer is introduced can further increase the total reflection of light, so that the light reflectivity is further improved.
As a specific embodiment, the preparation process of the patterned composite substrate may be described as follows:
after cleaning a sapphire flat sheet with the thickness of 600-1000mm, depositing a fluorine-doped silicon dioxide layer by utilizing a plasma enhanced chemical vapor deposition process, wherein the thickness of the fluorine-doped silicon dioxide layer is 60-90nm, the upper radio frequency power is 500-5000W, the SiH4 flow is 200-500sccm, the N2O flow is 6000-15000sccm, the N2 flow is 1000-3000sccm, the C2F6 flow is 500-5000sccm, and the chamber temperature is 200-400 ℃.
And then a silicon dioxide layer is deposited on the fluorine-doped silicon dioxide layer by utilizing a plasma enhanced chemical vapor deposition process, wherein the thickness of the silicon dioxide layer is 60-90nm, the upper radio frequency power is 500-5000W, the SiH4 flow is 200-500sccm, the N2O flow is 6000-15000sccm, the N2 flow is 1000-3000sccm, and the chamber temperature is 200-400 ℃.
And repeating the two steps of deposition steps to prepare n silicon dioxide-fluorine doped silicon dioxide laminates, namely DBR film layers, wherein the total thickness of the DBR film layers can be 2-3 mu m, and cylindrical photoresist columns which are arranged in a hexagonal period are prepared on the sapphire substrate on which the DBR film layers are deposited through photoresist homogenizing exposure and development, the thickness range of the photoresist homogenizing film is 2-3 mu m, and the period range of the photoetching plate is 1-3.5 mu m.
And carrying out ICP dry etching on the substrate with the photoresist column and the DBR film layer to prepare the required patterned composite substrate. Wherein the pressure of the etching chamber is 2.0-2.0 mTorr, the power range of the upper radio frequency electrode is 500-2000W, the power range of the lower radio frequency electrode is 300-850W, the flow rate of boron trichloride gas is 40-120sccm, the flow rate of trifluoromethane is 0-20sccm, the back helium gas pressure is 3-7 Torr, and the temperature of the cooler is 0-40 ℃. Because the etching rate of the fluorine-doped silicon dioxide is faster than that of the conventional silicon dioxide, the etching time of the composite substrate is shorter than that of the conventional silicon dioxide-sapphire composite substrate.
The embodiment of the invention also provides an LED epitaxial wafer, and fig. 10 is a schematic structural diagram of the LED epitaxial wafer provided by the embodiment of the invention, where the LED epitaxial wafer includes any patterned composite substrate 20 provided by the embodiment of the invention and an epitaxial layer 30 formed on the patterned composite substrate 20. The patterned composite substrate 20 includes a sapphire substrate 10 and a microstructure bump 11.
For different substrate materials, different LED epitaxial wafer growth technologies, chip processing technologies and device packaging technologies are required, and for the patterned composite substrate 20 provided by the embodiment of the present invention, the epitaxial layer 30 on the corresponding LED epitaxial wafer may be GaN, an AIGaN epitaxial layer, or the like.
According to the LED epitaxial wafer provided by the embodiment of the invention, the plurality of microstructure protrusions comprising fluorine-doped silicon dioxide are formed on the flat sapphire substrate, and as the refractive index of the fluorine-doped silicon dioxide is smaller than that of silicon dioxide, the difference between the refractive index of the patterned composite substrate formed based on the fluorine-doped silicon dioxide and that of an epitaxial layer material is larger, the total reflection angle is increased, the light extraction rate can be improved, and the brightness of an epitaxial end and a chip end can be improved.
Note that the above is only a preferred embodiment of the present invention and the technical principle applied. It will be understood by those skilled in the art that the present invention is not limited to the particular embodiments described herein, and that various obvious changes, rearrangements, combinations, and substitutions can be made by those skilled in the art without departing from the scope of the invention. Therefore, while the invention has been described in connection with the above embodiments, the invention is not limited to the embodiments, but may be embodied in many other equivalent forms without departing from the spirit or scope of the invention, which is set forth in the following claims.
Claims (7)
1. A patterned composite substrate, comprising:
a sapphire substrate;
a plurality of microstructure protrusions on the sapphire substrate, the microstructure protrusions comprising fluorine-doped silica having a refractive index less than a refractive index of the silica;
the microstructure protrusion is a DBR microstructure protrusion, the DBR microstructure protrusion comprises a silicon dioxide layer and a fluorine-doped silicon dioxide layer which are periodically laminated, and the refractive index of the fluorine-doped silicon dioxide layer is smaller than that of the silicon dioxide layer; in the DBR microstructure protrusion, the fluorine-doped silicon dioxide layer is attached to the sapphire substrate, and the fluorine-doped silicon dioxide layer and the silicon dioxide layer are alternately arranged;
the doping concentration range of fluorine atoms in the fluorine-doped silicon dioxide layer is 5% -15%; the refractive index of the fluorine-doped silicon dioxide layer ranges from 1.34 to 1.46.
2. The patterned composite substrate according to claim 1, wherein the thickness of the silicon dioxide layer is in the range of 60-90nm and the thickness of the fluorine doped silicon dioxide layer is in the range of 70-100nm.
3. A patterned composite substrate according to claim 1, wherein the DBR microstructure protrusions have a thickness in the range of 2.0-4.0 μm.
4. A method of preparing a patterned composite substrate, comprising:
providing a flat sapphire substrate;
forming a plurality of microstructure protrusions on the flat sapphire substrate, wherein the microstructure protrusions comprise fluorine-doped silicon dioxide, and the refractive index of the fluorine-doped silicon dioxide is smaller than that of the silicon dioxide;
the microstructure protrusions are DBR microstructure protrusions; forming a plurality of microstructure protrusions on the flat sheet sapphire substrate, comprising:
forming a DBR film layer on the flat sapphire substrate, wherein the DBR film layer comprises a silicon dioxide layer and a fluorine-doped silicon dioxide layer which are periodically laminated, and the refractive index of the fluorine-doped silicon dioxide layer is smaller than that of the silicon dioxide layer;
wherein, form the DBR rete on the flat piece sapphire substrate, the DBR rete includes cyclic stack's silica layer and fluorine doped silica layer, includes:
sequentially and alternately depositing the fluorine-doped silicon dioxide layer and the silicon dioxide layer on the surface of the flat sapphire substrate to form the DBR film layer;
patterning the DBR film layer to form a plurality of DBR microstructure protrusions;
the doping concentration range of fluorine atoms in the fluorine-doped silicon dioxide layer is adjusted to be 5% -15%, and the refractive index range of the fluorine-doped silicon dioxide layer is 1.34-1.46.
5. The method of fabricating a patterned composite substrate according to claim 4, wherein forming a DBR film layer on the flat sheet sapphire substrate comprises:
by means of plasmaThe silicon dioxide layer and the fluorine-doped silicon dioxide layer are sequentially and alternately deposited by enhanced chemical vapor deposition, vacuum thermal evaporation or magnetron sputtering process, and the thickness d of the silicon dioxide layer 1 The method meets the following conditions: d, d 1 ＝λ 0 /4n 1 Thickness d of the fluorine-doped silica layer 2 The method meets the following conditions: d, d 2 ＝λ 0 /4n 2 The method comprises the steps of carrying out a first treatment on the surface of the Wherein lambda is 0 For the center wavelength of the incident light incident on the patterned composite substrate, n 1 N is the refractive index of the silicon dioxide layer 2 Is the refractive index of the fluorine-doped silica.
6. The method of fabricating a patterned composite substrate according to claim 5, wherein the silicon dioxide layer and the fluorine-doped silicon dioxide layer are alternately deposited in sequence using a plasma enhanced chemical vapor deposition process; the fluorine source gas in the plasma enhanced chemical vapor deposition process comprises CF4, C2F6 and CHF3.
7. An LED epitaxial wafer comprising the patterned composite substrate of any one of claims 1-3.
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