CN101330002A - Method for preparing graphical sapphire substrate for nitrifier epitaxial growth - Google Patents
Method for preparing graphical sapphire substrate for nitrifier epitaxial growth Download PDFInfo
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- CN101330002A CN101330002A CNA2007101176171A CN200710117617A CN101330002A CN 101330002 A CN101330002 A CN 101330002A CN A2007101176171 A CNA2007101176171 A CN A2007101176171A CN 200710117617 A CN200710117617 A CN 200710117617A CN 101330002 A CN101330002 A CN 101330002A
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- sapphire substrate
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- Y02P—CLIMATE CHANGE MITIGATION TECHNOLOGIES IN THE PRODUCTION OR PROCESSING OF GOODS
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- Y02P70/50—Manufacturing or production processes characterised by the final manufactured product
Abstract
The invention discloses a production method of the patterned sapphire substrate for the nitride epitaxial growth, which comprises the following steps: a silica coating is deposited on the sapphire substrate used for the nitride epitaxial growth; a general photetch technology is utilized to prepare a mask of photetch patterns; the photetch patterns are etched on the silica coating by utilizing the doped liquid of hydrofluoric acid, ammonium fluoride and H2O; with the patterned silica coating as a mask, the sapphire substrate are etched by adopting the doped liquid of sulphuric acid and phosphoric acid in a wet manner so that the patterns are etched on the sapphire substrate; a dilute hydrofluoric acid solution is used for wet etching so as to remove the residual silica coating and clean the sapphire substrate, and then the preparation of the patterned sapphire substrate is completed. The production method has the advantages of low cost, preventing the sapphire substrate from being damaged by dry etching, etc. The patterned sapphire substrate can be used for the epitaxial growth of nitrides with low dislocation density and high crystal weight.
Description
Technical field
The invention belongs to technical field of semiconductors, be meant a kind of manufacture method that is used for the graphical sapphire substrate of nitride epitaxial growth especially.This graphical sapphire substrate can be used for the epitaxial growth of low-dislocation-density, high-crystal quality nitride.
Background technology
With III-V family gallium nitride (GaN) is the nitride compound semiconductor of representative, has important and application widely as gallium nitride (GaN), aluminium nitride (AlN), indium nitride (InN), aluminium gallium nitride alloy (AlGaN), indium gallium nitride (InGaN), aluminum indium nitride (AlInN) or aluminum indium gallium nitride (AlGaInN) etc. at numerous areas such as UV/blue/green light LED, laser, sunlight blind UV electric explorer and high frequency, high temperature high power electronic devices.Sapphire Substrate is that nitride carries out heteroepitaxial growth substrate the most commonly used at present.Because Sapphire Substrate and nitride epitaxial interlayer exist very macrolattice constant mismatch and thermal expansion coefficient difference, therefore utilize in the nitride epitaxial layer of metal organic chemical vapor deposition (MOCVD), hydride gas-phase epitaxy (HVPE) or molecular beam epitaxy (MBE) homepitaxy technology growth and have very big stress and a lot of crystal defects such as dislocation etc., therefore the crystal mass of material is subjected to very big influence, so deterioration device performance.Adopt the graphic sapphire substrate technology can alleviate in Sapphire Substrate and the nitride epitaxial layer heteroepitaxial growth because the stress that lattice mismatch causes, make it to obtain effective relaxation, reduce the dislocation density in the epitaxially grown nitride material greatly, crystal mass is greatly improved.But the technology of preparing of graphical sapphire substrate is to adopt traditional photoetching process to prepare litho pattern mostly at present, then with silicon dioxide (SiO
2) or silicon nitride (SiN
4) layer be mask, utilize reactive ion (RIE) or inductive couple plasma equipment dry etchings such as (ICP) to form again.Owing to relate to dry etching equipment in the technical process, so complex technical process, cost are higher, and Sapphire Substrate is subject to the dry etching damage and pollutes simultaneously.For the epitaxial growth of the nitride that more effectively is applied to low-dislocation-density, high-crystal quality, development cost graphic sapphire substrate technology low, that be easy to realize is imperative.
Summary of the invention
The objective of the invention is to be to provide a kind of manufacture method that is used for the graphical sapphire substrate of nitride epitaxial growth, this method can reduce the dislocation density in the nitride epitaxial layer effectively, avoid the generation of crackle, improve the crystal mass and the uniformity of epitaxial material, and then can improve the performance of photoelectric device.This technology of preparing does not relate to reactive ion (RIE) or inductive couple plasma dry etching equipment such as (ICP), and it is low to have a cost, is easy to realize advantages such as scale making.
The invention provides a kind of manufacture method that is used for the graphical sapphire substrate of nitride epitaxial growth, it is characterized in that, comprise the steps:
Step 1: be used for deposit layer of silicon dioxide film on the Sapphire Substrate of nitride epitaxial growth;
Step 2: utilize conventional photoetching technique to prepare the mask of litho pattern;
Step 3: utilize hydrofluoric acid+ammonium fluoride+H
2The O mixed liquor etches into litho pattern on the silicon dioxide film;
Step 4: as mask, adopt the mixed liquor wet etching Sapphire Substrate of sulfuric acid and phosphoric acid with the figure silicon dioxide film, with pattern etching on Sapphire Substrate;
Step 5: utilize the dilute hydrofluoric acid solution wet etching to remove remaining silicon dioxide film, and Sapphire Substrate is cleaned up, finish the preparation of graphical sapphire substrate.
Wherein said Sapphire Substrate is any in (0001) or c face, (1102) or r face, (1010) or m face, (1120) or a surface sapphire substrate.
Wherein the thickness of silicon dioxide film is 20 nanometers-2 micron.
Wherein litho pattern is the periodic pattern array, and the unit of its litho pattern is by any or several the combining in circular, square, regular hexagon, rhombus, triangle or the irregular figure.
Wherein the size of each unit and spacing are 1 micron-10 microns in the litho pattern.
Wherein the structure of litho pattern is any or two kinds of combinations in mesa shaped or the groove shape.
Wherein the temperature of the mixed liquor wet etching of sulfuric acid and phosphoric acid is between 320 ℃-520 ℃, and the time of etching is 30 seconds-30 minutes.
The nitride that wherein is used for nitride epitaxial growth is any or several combination of gallium nitride, aluminium nitride, indium nitride, aluminium gallium nitride alloy, indium gallium nitride, aluminum indium nitride or aluminum indium gallium nitride.
The method that wherein is used for nitride epitaxial growth is any or several combinations of the method for metal organic chemical vapor deposition method, hydride gas-phase epitaxy method or molecular beam epitaxy.
The manufacture method that is used for the graphical sapphire substrate of nitride epitaxial growth of the present invention, have cost low, make Sapphire Substrate avoid advantages such as dry etching damage.This graphical sapphire substrate can be used for the epitaxial growth of low-dislocation-density, high-crystal quality nitride.
Description of drawings
In order to further specify content of the present invention, below in conjunction with the example of implementing the present invention is done a detailed description, wherein:
Fig. 1 is the structural profile schematic diagram that is used for behind the Sapphire Substrate litho pattern of nitride epitaxial growth; 1 is Sapphire Substrate among the figure, the 2nd, and silicon dioxide film, the 3rd, photoresist layer;
Fig. 2 is to be mask with the photoresist layer, utilizes hydrofluoric acid (HF)+ammonium fluoride (NH
4F)+H
2Generalized section behind the O mixed liquor corrode silicon dioxide film; 1 is Sapphire Substrate among the figure, the 2nd, and silicon dioxide layer, the 3rd, photoresist layer;
Fig. 3 utilizes patterned silicon dioxide film to be mask, adopts sulfuric acid and phosphoric acid mixed liquor wet etching sapphire, with the generalized section of figure transfer after the Sapphire Substrate; 1 is Sapphire Substrate among the figure, the 2nd, and silicon dioxide film;
Fig. 4 is that diluted hydrofluoric acid (HF) wet etching removes remaining silicon dioxide film, and substrate is cleaned up, and is prepared into the generalized section behind the graphical sapphire substrate; 1 is Sapphire Substrate among the figure.
Specific embodiment
See also Fig. 1-shown in Figure 4, a kind of manufacture method that is used for the graphical sapphire substrate of nitride epitaxial growth of the present invention comprises the steps:
Step 1: deposit layer of silicon dioxide film 2 on the Sapphire Substrate 1 that is used for nitride epitaxial growth; Wherein said Sapphire Substrate 1 is any in (0001) or c face, (1102) or r face, (1010) or m face, (1120) or a surface sapphire substrate 1; Wherein the thickness of silicon dioxide film 2 is 20 nanometers-2 micron; This nitride that is used for nitride epitaxial growth is any or several combination of gallium nitride, aluminium nitride, indium nitride, aluminium gallium nitride alloy, indium gallium nitride, aluminum indium nitride or aluminum indium gallium nitride; Any or several combinations of the method that this method that is used for nitride epitaxial growth is metal organic chemical vapor deposition method, hydride gas-phase epitaxy method or molecular beam epitaxy;
Step 2: utilize conventional photoetching technique to prepare the mask 3 of litho pattern; Wherein litho pattern is the periodic pattern array, and the unit of its litho pattern is by any or several the combining in circular, square, regular hexagon, rhombus, triangle or the irregular figure; The size of each unit and spacing are 1 micron-10 microns in this litho pattern; The structure of this litho pattern is any or two kinds of combinations in mesa shaped or the groove shape;
Step 3: utilize hydrofluoric acid+ammonium fluoride+H
2The O mixed liquor etches into litho pattern on the silicon dioxide film 2;
Step 4: as mask, adopt the mixed liquor wet etching Sapphire Substrate 1 of sulfuric acid and phosphoric acid with figure silicon dioxide film 2, with pattern etching on Sapphire Substrate 1; The temperature of the mixed liquor wet etching of this sulfuric acid and phosphoric acid is between 320 ℃-520 ℃, and the time of etching is 30 seconds-30 minutes;
Step 5: utilize the dilute hydrofluoric acid solution wet etching to remove remaining silicon dioxide film 2, and Sapphire Substrate 1 is cleaned up, finish the preparation of graphical sapphire substrate 1.
Further set forth technical characterstic of the present invention and obvious improvement below by two specific embodiments.
Please consult Fig. 1-Fig. 4 again, present embodiment is a kind of manufacture method that is used for the figure c surface sapphire substrate 1 of nitride epitaxial growth.C surface sapphire substrate 1 is one of the most frequently used backing material of present epitaxial growth nitride.
The silicon dioxide film 2 of 0.3 micron of using plasma chemical gas-phase deposition enhanced (PECVD) deposition techniques on 2 inches c surface sapphire substrate 1 at first, on silicon dioxide film 2, utilize conventional photoetching technique resist coating layer 3, form circular array by exposure imaging.The size of this circular array cellular construction and spacing are 3 microns, and the structural profile after the photoetching as shown in Figure 1;
Then utilize photoresist layer 3 as the figure mask, use hydrofluoric acid (HF)+ammonium fluoride (NH
4F)+H
2The O mixed liquor etches into litho pattern on the silicon dioxide film 2, and its structural profile as shown in Figure 2;
Be the figure mask with silicon dioxide film 2 then, utilize sulfuric acid and phosphoric acid mixed liquor 400 ℃ of following wet etching c surface sapphire substrate 1, etch period is 10 minutes, and structural profile as shown in Figure 3; The volume ratio of this sulfuric acid and phosphoric acid mixed liquor 3: 1.
Utilize diluted hydrofluoric acid (HF) that silicon dioxide film 2 wet etchings of remnants are removed at last, promptly can be made into figure c surface sapphire substrate 1, structural profile as shown in Figure 4.
The graphic element of this Sapphire Substrate 1 is a mesa structure, and table surface height is 1.3 microns, and the side is because the anisotropy of wet etching is nearly equilateral triangle structure, by { 11-20}, { 2110} and { the 1-210} crystal face constitutes, and the surface is the round-shaped of photo etched mask.This c surface sapphire substrate 1 with periodic pattern array can be used for the epitaxial growth of low-dislocation-density, high-crystal quality nitride.
Present embodiment is a kind of manufacture method that is used for the figure r surface sapphire substrate 1 of nitride epitaxial growth.R surface sapphire substrate 1 can be used for the nonpolar nitride of epitaxial growth.Nonpolar nitride can be avoided the internal electric field that strain effect causes on the vertical-growth direction, thereby strengthens the radiation recombination probability of charge carrier, improves the performance of photoelectric device.
Adopt the technical process of similar embodiment 1, using plasma chemical gas-phase deposition enhanced (PECVD) deposition techniques silicon dioxide film 2, conventional photoetching technique litho pattern, hydrofluoric acid (HF)+ammonium fluoride (NH on r surface sapphire substrate 1
4F)+H
2O mixed liquor corrode silicon dioxide film 2, sulfuric acid and phosphoric acid mixed liquor corrode r surface sapphire substrate 1 down at 400 ℃, etch period is 6 minutes, utilize diluted hydrofluoric acid (HF) that silicon dioxide film 2 wet etchings of remnants are removed at last, promptly can be made into patterned r surface sapphire substrate 1.
The graphic element of this Sapphire Substrate 1 is a mesa structure, and the table surface height of graphic element is about 0.6 micron, because the anisotropy of wet etching, its surface becomes semilune by the circle of litho pattern.This graphical r surface sapphire substrate 1 can be used for the epitaxial growth of low-dislocation-density, the nonpolar nitride of high-crystal quality.
The foregoing description has been described the graphical c face that is used for nitride epitaxial growth and the manufacture method of r surface sapphire substrate.Owing to do not relate to dry etching processes such as RIE or ICP, therefore the graphical sapphire substrate of preparation can avoid the dry etching damage.Simultaneously, this wet etching technique does not relate to expensive device, have cost low, be easy to advantages such as scale making.Adopt the graphic sapphire substrate technology can alleviate the stress that causes owing to lattice mismatch in the heteroepitaxial growth process between Sapphire Substrate and nitride, reduce the defect concentration of nitride epitaxial layer, improve crystal mass, and then improve the performance of device.
Claims (9)
1, a kind of manufacture method that is used for the graphical sapphire substrate of nitride epitaxial growth is characterized in that, comprises the steps:
Step 1: be used for deposit layer of silicon dioxide film on the Sapphire Substrate of nitride epitaxial growth;
Step 2: utilize conventional photoetching technique to prepare the mask of litho pattern;
Step 3: utilize hydrofluoric acid+ammonium fluoride+H
2The O mixed liquor etches into litho pattern on the silicon dioxide film;
Step 4: as mask, adopt the mixed liquor wet etching Sapphire Substrate of sulfuric acid and phosphoric acid with the figure silicon dioxide film, with pattern etching on Sapphire Substrate;
Step 5: utilize the dilute hydrofluoric acid solution wet etching to remove remaining silicon dioxide film, and Sapphire Substrate is cleaned up, finish the preparation of graphical sapphire substrate.
2, the manufacture method that is used for the graphical sapphire substrate of nitride epitaxial growth according to claim 1, it is characterized in that wherein said Sapphire Substrate is any in (0001) or c face, (1102) or r face, (1010) or m face, (1120) or a surface sapphire substrate.
3, the manufacture method that is used for the graphical sapphire substrate of nitride epitaxial growth according to claim 1 is characterized in that, wherein the thickness of silicon dioxide film is 20 nanometers-2 micron.
4, the manufacture method that is used for the graphical sapphire substrate of nitride epitaxial growth according to claim 1, it is characterized in that, wherein litho pattern is the periodic pattern array, and the unit of its litho pattern is by any or several the combining in circular, square, regular hexagon, rhombus, triangle or the irregular figure.
5, the manufacture method that is used for the graphical sapphire substrate of nitride epitaxial growth according to claim 1 is characterized in that, wherein the size of each unit and spacing are 1 micron-10 microns in the litho pattern.
6, the manufacture method that is used for the graphical sapphire substrate of nitride epitaxial growth according to claim 1 is characterized in that, wherein the structure of litho pattern is any or two kinds of combinations in mesa shaped or the groove shape.
7, the manufacture method that is used for the graphical sapphire substrate of nitride epitaxial growth according to claim 1 is characterized in that, wherein the temperature of the mixed liquor wet etching of sulfuric acid and phosphoric acid is between 320 ℃-520 ℃, and the time of etching is 30 seconds-30 minutes.
8, the manufacture method that is used for the graphical sapphire substrate of nitride epitaxial growth according to claim 1, it is characterized in that the nitride that wherein is used for nitride epitaxial growth is any or several combination of gallium nitride, aluminium nitride, indium nitride, aluminium gallium nitride alloy, indium gallium nitride, aluminum indium nitride or aluminum indium gallium nitride.
9, the manufacture method that is used for the graphical sapphire substrate of nitride epitaxial growth according to claim 1, it is characterized in that the method that wherein is used for nitride epitaxial growth is any or several combinations of the method for metal organic chemical vapor deposition method, hydride gas-phase epitaxy method or molecular beam epitaxy.
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