CN116741896A - Submicron-order patterned sapphire substrate and preparation method thereof - Google Patents
Submicron-order patterned sapphire substrate and preparation method thereof Download PDFInfo
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- CN116741896A CN116741896A CN202310661114.XA CN202310661114A CN116741896A CN 116741896 A CN116741896 A CN 116741896A CN 202310661114 A CN202310661114 A CN 202310661114A CN 116741896 A CN116741896 A CN 116741896A
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- 239000000758 substrate Substances 0.000 title claims abstract description 279
- 229910052594 sapphire Inorganic materials 0.000 title claims abstract description 270
- 239000010980 sapphire Substances 0.000 title claims abstract description 270
- 238000002360 preparation method Methods 0.000 title claims abstract description 19
- 239000002131 composite material Substances 0.000 claims abstract description 102
- 238000004528 spin coating Methods 0.000 claims abstract description 25
- 238000004140 cleaning Methods 0.000 claims abstract description 19
- 238000005530 etching Methods 0.000 claims abstract description 18
- 238000012546 transfer Methods 0.000 claims abstract description 13
- 238000000151 deposition Methods 0.000 claims abstract description 12
- 230000007547 defect Effects 0.000 claims abstract description 10
- 238000005516 engineering process Methods 0.000 claims abstract description 7
- 238000000034 method Methods 0.000 claims description 29
- 239000007789 gas Substances 0.000 claims description 27
- MHAJPDPJQMAIIY-UHFFFAOYSA-N Hydrogen peroxide Chemical compound OO MHAJPDPJQMAIIY-UHFFFAOYSA-N 0.000 claims description 26
- QAOWNCQODCNURD-UHFFFAOYSA-N Sulfuric acid Chemical compound OS(O)(=O)=O QAOWNCQODCNURD-UHFFFAOYSA-N 0.000 claims description 26
- 238000001035 drying Methods 0.000 claims description 23
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Chemical compound O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims description 23
- 229920002120 photoresistant polymer Polymers 0.000 claims description 21
- 238000002791 soaking Methods 0.000 claims description 14
- BLRPTPMANUNPDV-UHFFFAOYSA-N Silane Chemical compound [SiH4] BLRPTPMANUNPDV-UHFFFAOYSA-N 0.000 claims description 13
- 239000008367 deionised water Substances 0.000 claims description 13
- 229910021641 deionized water Inorganic materials 0.000 claims description 13
- 229910000077 silane Inorganic materials 0.000 claims description 13
- 238000010023 transfer printing Methods 0.000 claims description 10
- 238000001816 cooling Methods 0.000 claims description 9
- 238000011010 flushing procedure Methods 0.000 claims description 8
- 230000005587 bubbling Effects 0.000 claims description 6
- 238000010438 heat treatment Methods 0.000 claims description 6
- 150000002500 ions Chemical class 0.000 claims description 6
- 238000000623 plasma-assisted chemical vapour deposition Methods 0.000 claims description 6
- 238000005507 spraying Methods 0.000 claims description 6
- 230000033001 locomotion Effects 0.000 claims description 5
- 239000002245 particle Substances 0.000 claims description 5
- 239000012495 reaction gas Substances 0.000 claims description 5
- 239000000853 adhesive Substances 0.000 claims description 4
- 230000001070 adhesive effect Effects 0.000 claims description 4
- 238000001312 dry etching Methods 0.000 claims description 4
- 238000012545 processing Methods 0.000 claims description 4
- 239000002313 adhesive film Substances 0.000 claims description 3
- 230000035484 reaction time Effects 0.000 claims description 3
- 238000002203 pretreatment Methods 0.000 claims 1
- 229910004298 SiO 2 Inorganic materials 0.000 description 4
- 239000010419 fine particle Substances 0.000 description 4
- 239000003292 glue Substances 0.000 description 4
- 238000012360 testing method Methods 0.000 description 4
- 238000004519 manufacturing process Methods 0.000 description 3
- 230000009286 beneficial effect Effects 0.000 description 2
- 150000001875 compounds Chemical class 0.000 description 2
- 230000008021 deposition Effects 0.000 description 2
- 230000000694 effects Effects 0.000 description 2
- 239000000463 material Substances 0.000 description 2
- 238000002488 metal-organic chemical vapour deposition Methods 0.000 description 2
- 239000002904 solvent Substances 0.000 description 2
- 239000011248 coating agent Substances 0.000 description 1
- 238000000576 coating method Methods 0.000 description 1
- 239000013078 crystal Substances 0.000 description 1
- 238000001514 detection method Methods 0.000 description 1
- 238000000407 epitaxy Methods 0.000 description 1
- 238000012986 modification Methods 0.000 description 1
- 230000004048 modification Effects 0.000 description 1
- 238000000465 moulding Methods 0.000 description 1
- 239000004065 semiconductor Substances 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 having potential barriers 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 having potential barriers 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 having potential barriers 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
- H01L33/025—Physical imperfections, e.g. particular concentration or distribution of impurities
-
- H—ELECTRICITY
- H01—ELECTRIC ELEMENTS
- H01L—SEMICONDUCTOR DEVICES NOT COVERED BY CLASS H10
- H01L33/00—Semiconductor devices having potential barriers 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 having potential barriers 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 having potential barriers 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
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- Engineering & Computer Science (AREA)
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- Computer Hardware Design (AREA)
- Microelectronics & Electronic Packaging (AREA)
- Power Engineering (AREA)
- Crystals, And After-Treatments Of Crystals (AREA)
Abstract
The invention discloses a submicron patterned sapphire substrate and a preparation method thereof, wherein the preparation method comprises the following steps: performing flat cleaning on the sapphire substrate; depositing SiO with preset thickness on the surface of the sapphire substrate 2 A layer to obtain a composite sapphire substrate; carrying out spin coating treatment on the composite sapphire substrate; carrying out pattern transfer on the composite sapphire substrate subjected to spin coating treatment by adopting a nano-imprinting technology to obtain a patterned sapphire substrate; and etching the patterned sapphire substrate to obtain the submicron-sized patterned sapphire substrate. The invention can improve the quality and the light-emitting efficiency of the epitaxial layer by reducing the pattern size of the patterned sapphire substrate, reduce the epitaxial defects with low defect density and increase the effective use area. Solves the problem that the prior art can not adoptEffective means to reduce defect density to reduce the pattern size of patterned sapphire substrates.
Description
Technical Field
The invention relates to the technical field of semiconductor devices, in particular to a submicron patterned sapphire substrate and a preparation method thereof.
Background
The patterned sapphire substrate (PatternedSapphireSubstrate, PSS) is a sapphire substrate with a patterned surface etched.
The existing preparation method of the PSS substrate comprises the following steps: coating photoresist on the surface of the sapphire substrate, and exposing and developing the photoresist to obtain a cylindrical photoresist array; the cylindrical photoresist array and the sapphire substrate are etched to form a layer of conical bump array, namely PSS, on the surface of the sapphire substrate.
Under the existing technological conditions, the pattern size of the prepared patterned sapphire substrate is usually in a micron-sized structure, because reducing the pattern size increases the defect density of the patterned sapphire substrate and deteriorates the crystal quality, thereby affecting the light emitting effect, and no effective means is available at present to reduce the defect density to reduce the pattern size of the patterned sapphire substrate.
Disclosure of Invention
Aiming at the defects of the prior art, the invention aims to provide a submicron-level patterned sapphire substrate and a preparation method thereof, and aims to solve the problem that the defect density cannot be reduced by adopting an effective means to reduce the pattern size of the patterned sapphire substrate in the prior art.
A first aspect of the present invention provides a method for preparing a submicron patterned sapphire substrate, which is characterized in that the preparation method comprises:
performing flat cleaning on the sapphire substrate;
depositing SiO with preset thickness on the surface of the sapphire substrate 2 A layer to obtain a composite sapphire substrate;
carrying out spin coating treatment on the composite sapphire substrate;
carrying out pattern transfer on the composite sapphire substrate subjected to spin coating treatment by adopting a nano-imprinting technology to obtain a patterned sapphire substrate;
and etching the patterned sapphire substrate to obtain the submicron-sized patterned sapphire substrate.
According to one aspect of the above technical solution, the step of performing flat cleaning on the sapphire substrate specifically includes:
performing flat processing on the sapphire substrate;
immersing the sapphire substrate subjected to the flat piece treatment in an SPM solution for cleaning; wherein the soaking time is 100s-1500s, the SPM solution comprises sulfuric acid and hydrogen peroxide, and the ratio of the sulfuric acid to the hydrogen peroxide is 2:1-8:1;
placing the cleaned sapphire substrate in a container containing deionized water, and spraying, bubbling and overflowing the sapphire substrate; wherein the water resistance of deionized water is 18 megaohms, and the soaking time is 100s-1500s;
and drying the sapphire substrate after removing ions.
According to one aspect of the above technical solution, a preset thickness of SiO is deposited on the surface of the sapphire substrate 2 A step of obtaining a composite sapphire substrate, comprising:
placing the sapphire substrate in a PECVD reaction chamber under preset conditions, and introducing reaction gas into the PECVD reaction chamber to deposit SiO with preset thickness on the surface of the sapphire substrate 2 A layer to obtain a composite sapphire substrate;
wherein the preset conditions comprise preset pressure, preset radio frequency power and preset cavity temperature, and the reaction gas comprises silane and N 2 O。
According to an aspect of the above technical solution, the preset pressure is 1500Pa-3000Pa, the preset radio frequency power is 500W-2000W, the preset cavity temperature is 250 ℃ to 350 ℃, and the silane and the N are 2 The ratio of O is 1:25-1:60, the concentration of silane is 100%, the reaction time is 1min-2min, and the preset ratio is setThe thickness is 0.5um-1um.
According to an aspect of the above technical solution, the step of spin-coating the composite sapphire substrate specifically includes:
placing the composite sapphire substrate in a clean water tank, flushing the composite sapphire substrate, and removing particles attached to the surface of the composite sapphire substrate; wherein the flushing time is 5s-30s;
placing the flushed composite sapphire substrate in a photoresist homogenizing groove, and spin-coating negative photoresist with a preset layer number on the surface of the composite sapphire substrate; wherein the negative photoresist adhesive is 2CP-10CP, and the thickness of the uniform adhesive film is 0.3um-1um;
placing the uniformly-glued composite sapphire substrate on a drying device for drying; wherein the drying temperature is 70-130 ℃, and the product is cooled to normal temperature for standby after drying.
According to one aspect of the above technical solution, the step of performing pattern transfer on the composite sapphire substrate after spin coating by using a nanoimprint technology to obtain a patterned sapphire substrate specifically includes:
injecting a template medium into a master template, and vacuumizing, heating, solidifying and cooling the template medium to obtain a soft template for pattern transfer;
and respectively placing the uniformly-treated composite sapphire substrate and the soft template in a carrying platform and a fixing station of the imprinting equipment, and controlling the composite sapphire substrate and the soft template to perform relative movement so as to complete pattern transfer printing to obtain the patterned sapphire substrate.
According to an aspect of the foregoing technical solution, the method further includes:
introducing N between the soft template and the composite sapphire substrate 2 Controlling the carrier to drive the composite sapphire substrate to move towards the soft template so as to be in full contact with the soft template;
controlling an ultraviolet light source to irradiate the composite sapphire substrate to solidify photoresist; wherein the exposure time is 30s-80s;
and controlling the carrier to drive the composite sapphire substrate to move towards one side far away from the soft template and completely separate from the soft template.
Wherein, in the process of transferring the composite sapphire substrate, the temperature of the carrier is 50-120 ℃.
According to one aspect of the above technical solution, the step of etching the patterned sapphire substrate to obtain a final patterned sapphire substrate specifically includes:
placing the patterned sapphire substrate in a reaction chamber of an ICP dry etching device; wherein, the power of the upper electrode is 500W-2000W, the power of the lower electrode is 150W-800W, the internal pressure regulation range is 2.5mT-4mT, the cooling temperature regulation range is 20 ℃ to 40 ℃, and the He gas pressure regulation range is 3T-6T;
introducing BCl into the reaction chamber 3 Gas and CHF gas; wherein, the BCl 3 The flow rate of the gas is 80sccm-200sccm, the flow rate of the CHF gas is 0sccm-20sccm, and the BCl 3 The ratio of the input flow rate of the gas to the CHF gas is 0-30%;
and etching the patterned sapphire substrate to obtain the submicron-sized patterned sapphire substrate.
According to an aspect of the foregoing technical solution, after the step of etching the patterned sapphire substrate to obtain the submicron patterned sapphire substrate, the method further includes:
immersing the patterned sapphire substrate in SPM solution for cleaning; wherein the soaking time is 100s-1500s, the SPM solution comprises sulfuric acid and hydrogen peroxide, and the ratio of the sulfuric acid to the hydrogen peroxide is 2:1-8:1;
placing the patterned sapphire substrate in a container containing deionized water, and spraying, bubbling and overflowing the sapphire substrate; wherein the water resistance of deionized water is 18 megaohms, and the soaking time is 100s-1500s;
and drying the patterned sapphire substrate after removing the ions.
The second aspect of the present invention is to provide a submicron patterned sapphire substrate, where the patterned sapphire substrate is prepared by using the preparation method shown in the above technical solution.
Compared with the prior art, the submicron graphical sapphire substrate and the preparation method thereof have the beneficial effects that:
in the process of manufacturing the patterned sapphire substrate, fine particles attached to the surface of the sapphire substrate are removed by carrying out flat piece and cleaning treatment on the sapphire substrate, and SiO is deposited on the surface of the sapphire substrate 2 The method comprises the steps of obtaining a composite sapphire substrate, conducting spin coating on the composite sapphire substrate, conducting pattern transfer printing on the composite sapphire substrate by means of nanoimprint, obtaining the patterned substrate, and finally etching the patterned substrate, so that a submicron patterned substrate is obtained.
Drawings
The foregoing and/or additional aspects and advantages of the invention will become apparent and may be better understood from the following description of embodiments taken in conjunction with the accompanying drawings in which:
fig. 1 is a flow chart of a method for preparing a submicron patterned sapphire substrate according to an embodiment of the present invention.
Detailed Description
In order to make the objects, features and advantages of the present invention more comprehensible, embodiments accompanied with figures are described in detail below. Several embodiments of the invention are presented in the figures. This invention may, however, be embodied in many different forms and should not be construed as limited to the embodiments set forth herein. Rather, these embodiments are provided so that this disclosure will be thorough and complete.
It will be understood that when an element is referred to as being "mounted" on another element, it can be directly on the other element or intervening elements may also be present. When an element is referred to as being "connected" to another element, it can be directly connected to the other element or intervening elements may also be present. The terms "vertical," "horizontal," "left," "right," and the like are used herein for illustrative purposes only.
Unless defined otherwise, all technical and scientific terms used herein have the same meaning as commonly understood by one of ordinary skill in the art to which this invention belongs. The terminology used herein in the description of the invention is for the purpose of describing particular embodiments only and is not intended to be limiting of the invention. The term "and/or" as used herein includes any and all combinations of one or more of the associated listed items.
Referring to fig. 1, a first aspect of the present invention is to provide a method for preparing a submicron patterned sapphire substrate, which includes steps S11-S15:
step S11, performing flat cleaning on the sapphire substrate;
step S12, depositing SiO with preset thickness on the surface of the sapphire substrate 2 A layer to obtain a composite sapphire substrate;
step S13, carrying out spin coating treatment on the composite sapphire substrate;
step S14, carrying out pattern transfer on the composite sapphire substrate subjected to spin coating treatment by adopting a nano-imprint technology to obtain a patterned sapphire substrate;
and S15, etching the patterned sapphire substrate to obtain the submicron patterned sapphire substrate.
Further, the step of performing flat cleaning on the sapphire substrate specifically includes:
performing flat processing on the sapphire substrate;
immersing the sapphire substrate subjected to the flat piece treatment in an SPM solution for cleaning; wherein the soaking time is 100s-1500s, the SPM solution comprises sulfuric acid and hydrogen peroxide, and the ratio of the sulfuric acid to the hydrogen peroxide is 2:1-8:1;
placing the cleaned sapphire substrate in a container containing deionized water, and spraying, bubbling and overflowing the sapphire substrate; wherein the water resistance of deionized water is 18 megaohms, and the soaking time is 100s-1500s;
and drying the sapphire substrate after removing ions.
Further, depositing SiO with preset thickness on the surface of the sapphire substrate 2 A step of obtaining a composite sapphire substrate, comprising:
placing the sapphire substrate in a PECVD reaction chamber under preset conditions, and introducing reaction gas into the PECVD reaction chamber to deposit SiO with preset thickness on the surface of the sapphire substrate 2 A layer to obtain a composite sapphire substrate;
wherein the preset conditions comprise preset pressure, preset radio frequency power and preset cavity temperature, and the reaction gas comprises silane and N 2 O。
Further, the preset pressure is 1500Pa-3000Pa, the preset radio frequency power is 500W-2000W, the temperature of the preset cavity is 250-350 ℃, and the silane and N are the same as each other 2 The ratio of O is 1:25-1:60, the concentration of silane is 100%, the reaction time is 1min-2min, and the preset thickness is 0.5um-1um.
Further, the step of spin-coating the composite sapphire substrate specifically includes:
placing the composite sapphire substrate in a clean water tank, flushing the composite sapphire substrate, and removing particles attached to the surface of the composite sapphire substrate; wherein the flushing time is 5s-30s;
placing the flushed composite sapphire substrate in a photoresist homogenizing groove, and spin-coating negative photoresist with a preset layer number on the surface of the composite sapphire substrate; wherein the negative photoresist adhesive is 2CP-10CP, and the thickness of the uniform adhesive film is 0.3um-1um;
placing the uniformly-glued composite sapphire substrate on a drying device for drying; wherein the drying temperature is 70-130 ℃, and the product is cooled to normal temperature for standby after drying.
Further, the step of performing pattern transfer on the composite sapphire substrate subjected to spin coating treatment by adopting a nanoimprint technology to obtain a patterned sapphire substrate specifically comprises the following steps:
injecting a template medium into a master template, and vacuumizing, heating, solidifying and cooling the template medium to obtain a soft template for pattern transfer;
and respectively placing the uniformly-treated composite sapphire substrate and the soft template in a carrying platform and a fixing station of the imprinting equipment, and controlling the composite sapphire substrate and the soft template to perform relative movement so as to complete pattern transfer printing to obtain the patterned sapphire substrate.
Further, the method further comprises:
introducing N between the soft template and the composite sapphire substrate 2 Controlling the carrier to drive the composite sapphire substrate to move towards the soft template so as to be in full contact with the soft template;
controlling an ultraviolet light source to irradiate the composite sapphire substrate to solidify photoresist; wherein the exposure time is 30s-80s;
and controlling the carrier to drive the composite sapphire substrate to move towards one side far away from the soft template and completely separate from the soft template.
Wherein, in the process of transferring the composite sapphire substrate, the temperature of the carrier is 50-120 ℃.
Further, the step of etching the patterned sapphire substrate to obtain a final patterned sapphire substrate specifically includes:
placing the patterned sapphire substrate in a reaction chamber of an ICP dry etching device; wherein, the power of the upper electrode is 500W-2000W, the power of the lower electrode is 150W-800W, the internal pressure regulation range is 2.5mT-4mT, the cooling temperature regulation range is 20 ℃ to 40 ℃, and the He gas pressure regulation range is 3T-6T;
introducing BCl into the reaction chamber 3 Gas and CHF gas; wherein, the BCl 3 Flow rate of gas80sccm-200sccm, the flow rate of CHF gas is 0sccm-20sccm, and the BCl 3 The ratio of the input flow rate of the gas to the CHF gas is 0-30%;
and etching the patterned sapphire substrate to obtain the submicron-sized patterned sapphire substrate.
Further, after the step of etching the patterned sapphire substrate to obtain the submicron patterned sapphire substrate, the method further includes:
immersing the patterned sapphire substrate in SPM solution for cleaning; wherein the soaking time is 100s-1500s, the SPM solution comprises sulfuric acid and hydrogen peroxide, and the ratio of the sulfuric acid to the hydrogen peroxide is 2:1-8:1;
placing the patterned sapphire substrate in a container containing deionized water, and spraying, bubbling and overflowing the sapphire substrate; wherein the water resistance of deionized water is 18 megaohms, and the soaking time is 100s-1500s;
and drying the patterned sapphire substrate after removing the ions.
The second aspect of the present invention is to provide a submicron patterned sapphire substrate, where the patterned sapphire substrate is prepared by using the preparation method shown in the above technical solution.
Example 1
Referring to fig. 1, a first embodiment of the present invention provides a method for preparing a submicron patterned sapphire substrate, wherein the preparation method is used for preparing a submicron patterned sapphire substrate with low defect density, namely a submicron PSS substrate with low defect density, and the preparation method comprises steps S11-S15:
step S11, performing flat cleaning on the sapphire substrate;
wherein, the flat sheet cleaning of the sapphire substrate comprises flat sheet treatment and cleaning treatment.
In the embodiment, when the sapphire substrate is cleaned, the sapphire substrate is placed in an SPM solution, the soaking time of the sapphire substrate in the SPM solution is 600s, and the ratio of sulfuric acid to hydrogen peroxide in the SPM solution is 4:1;
in addition, the soaking time of placing the sapphire substrate in deionized water was 600s.
Through the mode, the sapphire substrate is cleaned, fine particles attached to the surface of the sapphire substrate can be effectively removed, and the number of the fine particles attached to the surface of the sapphire substrate is less than 50 particles after detection.
Step S12, depositing SiO with preset thickness on the surface of the sapphire substrate 2 A layer to obtain a composite sapphire substrate;
wherein, siO is deposited on the surface of the sapphire substrate 2 The purpose of the layer is to reduce the refractive index of the sapphire substrate to light, the lower the refractive index, the greater the improvement in the epitaxial brightness.
In this embodiment, siO is deposited on the surface of the cleaned sapphire substrate 2 The layers, in particular deposited by means of an MOCVD tool, comprise the following deposition parameters:
placing a sapphire substrate in a reaction chamber of MOCVD equipment, controlling the reaction temperature in the reaction chamber to be 300 ℃, the reaction pressure to be 2000Pa and the radio frequency power to be 1100W;
360sccm of Silane (SiH) was introduced into the reaction chamber 4 ) 10000sccm of N 2 0, and 1800sccm of N 2 。
By depositing SiO on the surface of the sapphire substrate in the above manner 2 Layer, through testing, the SiO 2 The refractive index of the layer was 1.479 and the improvement in the epitaxial brightness was 4.3%.
Step S13, carrying out spin coating treatment on the composite sapphire substrate;
in this embodiment, siO is deposited on the surface of the sapphire substrate 2 After the composite sapphire substrate is obtained, the composite sapphire substrate needs to be cleaned before spin coating is performed on the composite sapphire substrate.
Wherein, clean compound sapphire substrate, include:
placing the composite sapphire substrate in a water purifying tank, flushing the composite sapphire substrate, and removing particles attached to the surface of the composite sapphire substrate; wherein the flushing time is 5s-30s.
Wherein, carry out even glue processing to the compound sapphire substrate after the cleaning, include:
placing the flushed composite sapphire substrate in a spin coating groove, controlling the composite sapphire substrate to rotate, and spin coating negative photoresist with a preset layer number on the surface of the composite sapphire substrate; wherein, the negative photoresist adhesive is 3CP, and the thickness of the photoresist homogenizing film is 0.5um;
placing the uniformly-glued composite sapphire substrate on a drying device for drying so as to remove the solvent; wherein the drying temperature is 90 ℃, and the product is cooled to normal temperature for standby after drying.
In this embodiment, the drying device is a baking tray, and the composite sapphire substrate is placed on the baking tray to be baked, so that moisture and solvent on the surface of the composite sapphire substrate can be effectively dried, and after the composite sapphire substrate is dried by using the baking tray, the composite sapphire substrate also needs to be cooled by a cold tray, so that the composite sapphire substrate is cooled to normal temperature on the cold tray.
Step S14, carrying out pattern transfer on the composite sapphire substrate subjected to spin coating treatment by adopting a nano-imprint technology to obtain a patterned sapphire substrate;
in this embodiment, after the composite sapphire substrate is subjected to spin coating treatment to obtain a spin coated composite sapphire substrate, the spin coated composite sapphire substrate is further subjected to pattern transfer printing to obtain a patterned sapphire substrate, i.e., a ps substrate. In this embodiment, the nano-imprint is used to perform pattern transfer on the composite sapphire substrate, which includes two steps of soft mold fabrication and pattern transfer.
Wherein the soft molding comprises:
and (3) injecting a template medium into the master template, and vacuumizing, heating, solidifying and cooling the template medium to obtain the soft template for pattern transfer printing.
Specifically, the template medium is AB glue, the AB glue is uniformly stirred and dripped onto a master template, the master template pattern is a cylindrical pattern with a period of 1.0um or less, the cylindrical bottom width is 0.1um-1um, the cylindrical height is 0.5um-1.5um, the weight of the AB glue is 40g-120g, and the soft template corresponding to the master template is obtained through vacuumizing, heating, solidifying and cooling, wherein the heating temperature is 100-150 ℃.
Wherein, the graphic transfer printing includes:
and respectively placing the uniformly-treated composite sapphire substrate and the prepared soft template in a carrying platform and a fixing station of the imprinting equipment, and controlling the composite sapphire substrate and the soft template to perform relative movement so as to complete pattern transfer printing to obtain the patterned sapphire substrate.
In this embodiment, the step of controlling the relative motion of the composite sapphire substrate and the soft template to realize the pattern transfer printing, to obtain the patterned sapphire substrate specifically includes:
introducing N between the soft template and the composite sapphire substrate 2 Controlling a carrier of the imprinting equipment to drive the composite sapphire substrate to move towards the soft template, so that the composite sapphire substrate is in full contact with the soft template;
controlling an ultraviolet light source to irradiate the composite sapphire substrate to solidify photoresist coated on the surface of the substrate; the exposure time of the ultraviolet light source is 30s-80s, and in this embodiment, the exposure time of the ultraviolet light source is 40s, for example;
and after the ultraviolet light source irradiates and the photoresist is solidified, the carrier is controlled to drive the composite sapphire substrate to move towards one side far away from the soft template, so that the composite sapphire substrate and the soft template are mutually separated, and the patterned substrate is obtained.
And S15, etching the patterned sapphire substrate to obtain the submicron patterned sapphire substrate.
In this embodiment, etching the patterned sapphire substrate specifically includes:
placing the patterned sapphire substrate in a reaction chamber of an ICP dry etching device; wherein, the power of the upper electrode is 500W-2000W, the power of the lower electrode is 150W-800W, the internal pressure regulation range is 2.5mT-4mT, the cooling temperature regulation range is 20 ℃ to 40 ℃, and the He gas pressure regulation range is 3T-6T;
introducing BCl into the reaction chamber 3 Gas and CHF gas; wherein BCl 3 The flow rate of the gas is 80sccm-200sccm, the flow rate of CHF gas is 0sccm-20sccm, and BCl 3 The ratio of the input flow rate of the gas to the CHF gas is 0-30%;
and etching the patterned sapphire substrate to obtain the submicron-sized patterned sapphire substrate.
Compared with the prior art, the preparation method of the submicron-level patterned sapphire substrate shown in the embodiment has the beneficial effects that:
in the process of manufacturing the patterned sapphire substrate, fine particles attached to the surface of the sapphire substrate are removed by carrying out flat piece and cleaning treatment on the sapphire substrate, and SiO is deposited on the surface of the sapphire substrate 2 The method comprises the steps of obtaining a composite sapphire substrate, conducting spin coating on the composite sapphire substrate, conducting pattern transfer printing on the composite sapphire substrate by means of nanoimprint, obtaining the patterned substrate, and finally etching the patterned substrate, so that a submicron patterned substrate is obtained.
Example two
The second embodiment of the present invention also provides a method for preparing a submicron patterned sapphire substrate, which is different from the preparation method shown in the first embodiment in that:
in this embodiment, the reaction temperature in the reaction chamber is controlled to 300 ℃, the reaction pressure is 1800Pa, and the radio frequency power is 1100W;
360sccm of Silane (SiH) was introduced into the reaction chamber 4 ) 9000sccm of N 2 0, and 1500sccm of N 2 。
By depositing SiO on the surface of the sapphire substrate in the above manner 2 Layer, through testing, the SiO 2 The refractive index of the layer was 1.497 and the improvement in the epitaxial brightness was 4.0%.
Example III
The third embodiment of the present invention also provides a method for preparing a submicron patterned sapphire substrate, which is different from the preparation method shown in the first embodiment in that:
in this embodiment, the reaction temperature in the reaction chamber is controlled to be 300 ℃, the reaction pressure is controlled to be 1500Pa, and the radio frequency power is controlled to be 1500W;
360sccm of Silane (SiH) was introduced into the reaction chamber 4 ) 10000sccm of N 2 0, and 1800sccm of N 2 。
By depositing SiO on the surface of the sapphire substrate in the above manner 2 Layer, through testing, the SiO 2 The refractive index of the layer was 1.474 and the improvement in the epitaxial brightness was 4.5%.
Example IV
The fourth embodiment of the present invention also provides a method for preparing a submicron patterned sapphire substrate, which is different from the preparation method shown in the first embodiment in that:
in this embodiment, the reaction temperature in the reaction chamber is controlled to 320 ℃, the reaction pressure is 2500Pa, and the radio frequency power is 1200W;
300sccm of Silane (SiH) was introduced into the reaction chamber 4 ) 10000sccm of N 2 0, and 1500sccm of N 2 。
By depositing SiO on the surface of the sapphire substrate in the above manner 2 Layer, through testing, the SiO 2 The refractive index of the layer was 1.471 and the improvement in the epitaxial brightness was 5.2%.
Table 1 shows SiO in the first to fourth embodiments of the present invention 2 A comparison of the deposition conditions of the layers and their effect on epitaxy.
In combination with examples one through four and Table 1, siO was deposited over a flat sheet clean treated sapphire substrate 2 When the layer is formed, when the reaction temperature in the reaction chamber is controlled to be 300 ℃, the radio frequency power is 1200W, the reaction pressure is 2500Pa, and 300sccm SiH is respectively introduced 4 10000sccm of N 2 N of 0 and 1500sccm 2 To obtain a composite sapphire substrate, and detecting the SiO in the composite sapphire substrate 2 The refractive index of the layer was 1.471, which is the smallest of the various embodiments, and the ratio of improvement to the epitaxial brightness was the largest, reaching 5.2%.
In the description of the present specification, a description referring to terms "one embodiment," "some embodiments," "examples," "specific examples," or "some examples," etc., means that a particular feature, structure, material, or characteristic described in connection with the embodiment or example is included in at least one embodiment or example of the present invention. In this specification, schematic representations of the above terms do not necessarily refer to the same embodiments or examples. Furthermore, the particular features, structures, materials, or characteristics described may be combined in any suitable manner in any one or more embodiments or examples.
The foregoing examples illustrate only a few embodiments of the invention, and are described in detail, but are not to be construed as limiting the scope of the invention. It should be noted that it is possible for those skilled in the art to make several variations and modifications without departing from the spirit of the invention, which are all within the scope of the invention. Accordingly, the scope of protection of the present invention is to be determined by the appended claims.
Claims (10)
1. A method for preparing a submicron patterned sapphire substrate, which is used for preparing a submicron patterned sapphire substrate, characterized in that the preparation method comprises the following steps:
performing flat cleaning on the sapphire substrate;
depositing a pre-treatment on the surface of the sapphire substrateSiO of a set thickness 2 A layer to obtain a composite sapphire substrate;
carrying out spin coating treatment on the composite sapphire substrate;
carrying out pattern transfer on the composite sapphire substrate subjected to spin coating treatment by adopting a nano-imprinting technology to obtain a patterned sapphire substrate;
and etching the patterned sapphire substrate to obtain the submicron-sized patterned sapphire substrate.
2. The method for preparing a submicron patterned sapphire substrate according to claim 1, wherein the step of performing a flat cleaning on the sapphire substrate comprises:
performing flat processing on the sapphire substrate;
immersing the sapphire substrate subjected to the flat piece treatment in an SPM solution for cleaning; wherein the soaking time is 100s-1500s, the SPM solution comprises sulfuric acid and hydrogen peroxide, and the ratio of the sulfuric acid to the hydrogen peroxide is 2:1-8:1;
placing the cleaned sapphire substrate in a container containing deionized water, and spraying, bubbling and overflowing the sapphire substrate; wherein the water resistance of deionized water is 18 megaohms, and the soaking time is 100s-1500s;
and drying the sapphire substrate after removing ions.
3. The method for preparing a submicron patterned sapphire substrate according to claim 1, wherein a preset thickness of SiO is deposited on the surface of the sapphire substrate 2 A step of obtaining a composite sapphire substrate, comprising:
placing the sapphire substrate in a PECVD reaction chamber under preset conditions, and introducing reaction gas into the PECVD reaction chamber to deposit SiO with preset thickness on the surface of the sapphire substrate 2 A layer to obtain a composite sapphire substrate;
wherein the preset conditions comprise preset pressure, preset radio frequency power and preset cavity temperature, and the reaction gasComprising silane and N 2 O。
4. The method for preparing a submicron patterned sapphire substrate according to claim 3, wherein the preset pressure is 1500Pa-3000Pa, the preset rf power is 500W-2000W, the preset cavity temperature is 250 ℃ to 350 ℃, and the silane and N are the same 2 The ratio of O is 1:25-1:60, the concentration of silane is 100%, the reaction time is 1min-2min, and the preset thickness is 0.5um-1um.
5. The method for preparing a submicron patterned sapphire substrate according to claim 1, wherein the step of spin-coating the composite sapphire substrate comprises:
placing the composite sapphire substrate in a clean water tank, flushing the composite sapphire substrate, and removing particles attached to the surface of the composite sapphire substrate; wherein the flushing time is 5s-30s;
placing the flushed composite sapphire substrate in a photoresist homogenizing groove, and spin-coating negative photoresist with a preset layer number on the surface of the composite sapphire substrate; wherein the negative photoresist adhesive is 2CP-10CP, and the thickness of the uniform adhesive film is 0.3um-1um;
placing the uniformly-glued composite sapphire substrate on a drying device for drying; wherein the drying temperature is 70-130 ℃, and the product is cooled to normal temperature for standby after drying.
6. The method for preparing a submicron patterned sapphire substrate according to claim 1, wherein the step of performing pattern transfer on the composite sapphire substrate after spin coating by using a nanoimprint technique to obtain a patterned sapphire substrate comprises the following steps:
injecting a template medium into a master template, and vacuumizing, heating, solidifying and cooling the template medium to obtain a soft template for pattern transfer;
and respectively placing the uniformly-treated composite sapphire substrate and the soft template in a carrying platform and a fixing station of the imprinting equipment, and controlling the composite sapphire substrate and the soft template to perform relative movement so as to complete pattern transfer printing to obtain the patterned sapphire substrate.
7. The method of preparing a sub-micron patterned sapphire substrate of claim 6, further comprising:
introducing N between the soft template and the composite sapphire substrate 2 Controlling the carrier to drive the composite sapphire substrate to move towards the soft template so as to be in full contact with the soft template;
controlling an ultraviolet light source to irradiate the composite sapphire substrate to solidify photoresist; wherein the exposure time is 30s-80s;
controlling the carrier to drive the composite sapphire substrate to move towards one side far away from the soft template and completely separate from the soft template;
wherein, in the process of transferring the composite sapphire substrate, the temperature of the carrier is 50-120 ℃.
8. The method for preparing a patterned sapphire substrate of submicron order according to claim 1, wherein the step of etching the patterned sapphire substrate to obtain a final patterned sapphire substrate comprises:
placing the patterned sapphire substrate in a reaction chamber of an ICP dry etching device; wherein, the power of the upper electrode is 500W-2000W, the power of the lower electrode is 150W-800W, the internal pressure regulation range is 2.5mT-4mT, the cooling temperature regulation range is 20 ℃ to 40 ℃, and the He gas pressure regulation range is 3T-6T;
introducing BCl into the reaction chamber 3 Gas and CHF gas; wherein, the BCl 3 The flow rate of the gas is 80sccm-200sccm, the flow rate of the CHF gas is 0sccm-20sccm, and the BCl 3 The ratio of the input flow rate of the gas to the CHF gas is 0-30%;
and etching the patterned sapphire substrate to obtain the submicron-sized patterned sapphire substrate.
9. The method of preparing a patterned sapphire with low defect density according to any of claims 1-8, wherein after the step of etching the patterned sapphire substrate to obtain a patterned sapphire substrate with submicron dimensions, the method further comprises:
immersing the patterned sapphire substrate in SPM solution for cleaning; wherein the soaking time is 100s-1500s, the SPM solution comprises sulfuric acid and hydrogen peroxide, and the ratio of the sulfuric acid to the hydrogen peroxide is 2:1-8:1;
placing the patterned sapphire substrate in a container containing deionized water, and spraying, bubbling and overflowing the sapphire substrate; wherein the water resistance of deionized water is 18 megaohms, and the soaking time is 100s-1500s;
and drying the patterned sapphire substrate after removing the ions.
10. A submicron patterned sapphire substrate, characterized in that the patterned sapphire substrate is prepared by the preparation method as set forth in any one of claims 1 to 9.
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| CN117410168B (en) * | 2023-12-13 | 2024-03-29 | 江西兆驰半导体有限公司 | Patterned sapphire substrate and preparation method thereof |
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