CN101509145A - Method for growing nonpolar a face GaN film on lithium aluminate substrate - Google Patents
Method for growing nonpolar a face GaN film on lithium aluminate substrate Download PDFInfo
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- CN101509145A CN101509145A CNA200910046585XA CN200910046585A CN101509145A CN 101509145 A CN101509145 A CN 101509145A CN A200910046585X A CNA200910046585X A CN A200910046585XA CN 200910046585 A CN200910046585 A CN 200910046585A CN 101509145 A CN101509145 A CN 101509145A
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- lithium aluminate
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- YQNQTEBHHUSESQ-UHFFFAOYSA-N lithium aluminate Chemical compound [Li+].[O-][Al]=O YQNQTEBHHUSESQ-UHFFFAOYSA-N 0.000 title claims abstract description 46
- 238000000034 method Methods 0.000 title claims abstract description 21
- 239000000758 substrate Substances 0.000 title claims description 34
- 239000010410 layer Substances 0.000 claims abstract description 34
- 239000011241 protective layer Substances 0.000 claims abstract description 21
- 239000012298 atmosphere Substances 0.000 claims abstract description 12
- 238000002488 metal-organic chemical vapour deposition Methods 0.000 claims abstract 2
- 229910002601 GaN Inorganic materials 0.000 claims description 59
- 239000012299 nitrogen atmosphere Substances 0.000 claims description 22
- XCZXGTMEAKBVPV-UHFFFAOYSA-N trimethylgallium Chemical compound C[Ga](C)C XCZXGTMEAKBVPV-UHFFFAOYSA-N 0.000 claims description 17
- JMASRVWKEDWRBT-UHFFFAOYSA-N Gallium nitride Chemical compound [Ga]#N JMASRVWKEDWRBT-UHFFFAOYSA-N 0.000 claims description 11
- UFHFLCQGNIYNRP-UHFFFAOYSA-N Hydrogen Chemical compound [H][H] UFHFLCQGNIYNRP-UHFFFAOYSA-N 0.000 claims description 11
- 239000001257 hydrogen Substances 0.000 claims description 11
- 229910052739 hydrogen Inorganic materials 0.000 claims description 11
- IJGRMHOSHXDMSA-UHFFFAOYSA-N Atomic nitrogen Chemical compound N#N IJGRMHOSHXDMSA-UHFFFAOYSA-N 0.000 abstract 4
- 229910001873 dinitrogen Inorganic materials 0.000 abstract 2
- 229910010092 LiAlO2 Inorganic materials 0.000 abstract 1
- 239000007789 gas Substances 0.000 abstract 1
- 229910052757 nitrogen Inorganic materials 0.000 abstract 1
- 229910010093 LiAlO Inorganic materials 0.000 description 7
- 238000005516 engineering process Methods 0.000 description 5
- 239000000463 material Substances 0.000 description 5
- 238000005229 chemical vapour deposition Methods 0.000 description 4
- 229910052751 metal Inorganic materials 0.000 description 4
- 239000002184 metal Substances 0.000 description 4
- 230000003287 optical effect Effects 0.000 description 3
- 238000003860 storage Methods 0.000 description 3
- 230000008901 benefit Effects 0.000 description 2
- 238000005286 illumination Methods 0.000 description 2
- 229910052594 sapphire Inorganic materials 0.000 description 2
- 239000010980 sapphire Substances 0.000 description 2
- 239000004065 semiconductor Substances 0.000 description 2
- 239000007787 solid Substances 0.000 description 2
- 229910045601 alloy Inorganic materials 0.000 description 1
- 239000000956 alloy Substances 0.000 description 1
- 230000002950 deficient Effects 0.000 description 1
- 238000010586 diagram Methods 0.000 description 1
- 230000000694 effects Effects 0.000 description 1
- 230000005611 electricity Effects 0.000 description 1
- 238000001534 heteroepitaxy Methods 0.000 description 1
- 238000004519 manufacturing process Methods 0.000 description 1
- 230000010287 polarization Effects 0.000 description 1
- 230000004223 radioprotective effect Effects 0.000 description 1
- 230000002269 spontaneous effect Effects 0.000 description 1
- 239000000126 substance Substances 0.000 description 1
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Abstract
The invention discloses a method for developing a GaN film of a nonpolar a(11-20) face on the lining of a lithium aluminate(302) face, comprising the following steps: developing a low temperature protective layer in the atmosphere of nitrogen on the lining of LiAlO2(302) face under the protection of gas N2 at the temperature of 800-950 DEG C in an MOCVD system, wherein the pressure of the reaction chamber for the low temperature protective layer is 150-500torr, the flow of TMGa is 1-50sccm corresponding to mole flow of 4E-6mole/min-3E-4mole/min; subsequently lowering the pressure to 100-300torr, and raising the temperature to 1000-1100 DEG C to continue to grow a U-GaN layer in nitrogen gas, wherein the TMGa flow is 10-150sccm corresponding to mole flow of 4E-5mole/min-7.5E-4mole/min; then raising the temperature to 1050-1150 DEG C to grow about 1mum of high temperature U-GaN in nitrogen gas, wherein the TMGa flow is 20-200sccm corresponding to mole flow of 8E-5mole/min-1E-3mole/min. The innovative point of the invention lies in that a novel extending technique is designed according to the characteristic of the lithium aluminate(302) face lining, so that the developed extending film has higher quality and practicality.
Description
Technical field
The present invention relates at a kind of novel substrate (302) LiAlO
2With the method for yield production type MOCVD (metal organic chemical vapor deposition) technology growth GaN film, refer in particular to the method for utilizing the nonpolar a of MOCVD technology growth high quality (11-20) face GaN film on the material.
Background technology
The new generation of semiconductor material that with GaN is representative has obtained people's extensive concern with characteristics such as its wide direct band gap (Eg=3.4eV), high heat conductance, high rigidity, high chemical stability, low-k, radioprotectives, in fields such as solid-state illumination, solid statelaser, optical information storage, ultraviolet detectors huge application potential is arranged all.Calculate by China's electricity consumption situation in 2002,, can save the generated energy of the three gorges hydropower plant in 1 year, huge economy, environment and social benefit are arranged if adopt solid-state illumination to substitute conventional light source; And according to the USDOE measuring and calculating, by 2010, the whole America semiconductor lighting industry output value will reach 50,000,000,000 dollars.Aspect the optical information storage, can increase substantially optical storage density based on the solid blue light laser of GaN.Just because of these advantages, GaN and alloy thereof are placed high hopes.High brightness InGaN/GaN quantum well structure LEDs commercialization.
Substrate material has material impact for the quality of epitaxial film.GaN body monocrystalline material growth is very difficult at present, reports that GaN is that 60-70kbar, temperature are also not melt under 2300 ℃ at pressure.Growth conditions is High Temperature High Pressure normally, costs dearly, and is unfavorable for commercialization, and therefore present application is to do hetero epitaxy at c on sapphire mostly.Using c is that the lattice mismatch of itself and GaN film is up to 13.6% to a sapphire significant drawback, though can remedy this shortcoming by the buffer layer technology, but serious like this mismatch still can cause having in the epitaxial film highdensity defective, thereby reduces device efficiency.
In addition, the GaN film is normally along its polar axis c direction of principal axis growth, and the powerful built in field that is produced by spontaneous polarization and piezoelectric effect has reduced luminous efficiency widely.Adopt novel LiAlO
2Substrate is expected to solve this two problems.LiAlO
2Substrate and GaN film lattice mismatch are little, have only 1.4%, and at LiAlO
2Last growth be nonpolar GaN film, can eliminate the restriction of built in field for luminous efficiency.
Summary of the invention
The technical problem to be solved in the present invention be to provide a kind of on the lithium aluminate substrate method of growing nonpolar a face GaN film; by growing low temperature protective layer and high temperature U-GaN layer; protection lithium aluminate substrate is not destroyed by high temperature, improves film quality, improves surface finish.
In order to solve the problems of the technologies described above, the present invention adopts following technical scheme: a kind of on the lithium aluminate substrate method of growing nonpolar a face GaN film, it is characterized in that: this method may further comprise the steps:
Step 1, the growing low temperature protective layer in the MOCVD system, is done substrate with lithium aluminate (302) face, at N
2Protection is warmed up to 800-950 ℃ down, and growing low temperature protective layer under nitrogen atmosphere, low-temperature protection layer chamber pressure are 150-500torr, and trimethyl-gallium TMGa flow is 1-50sccm, corresponding to molar flow: 4E-6mole/min-3E-4mole/min;
Step 2, the non-Doped GaN layer of growing reduces pressure then to 100-300torr, is warmed up to the 1000-1100 ℃ of non-Doped GaN layer of continued growth under nitrogen atmosphere, the TMGa flow is 10-150sccm, corresponding to molar flow: 4E-5mol/min-7.5E-4mole/min;
Step 3, growth high temperature U-GaN layer is warmed up to 1050-1150 ℃ at last again, and growth thickness is the high temperature U-GaN layer of 1um under hydrogen atmosphere, and the TMGa flow is 20-200sccm, corresponding to molar flow: 8E-5mol/min-1E-3mole/min.
As one of preferred version of the present invention, before carrying out step 1 growing low temperature protective layer, earlier lithium aluminate (302) face substrate is carried out surface heat under 600-900 ℃ and handle.
As one of preferred version of the present invention, on lithium aluminate (302) face substrate, at N
2Protection is warmed up to 800 ℃, growing low temperature protective layer under nitrogen atmosphere down; Reduce pressure then to 100-300torr, be warmed up to 1000 ℃ of non-doped gallium nitride layer of continued growth under nitrogen atmosphere; And then being warmed up to 1050 ℃, growth high temperature U-GaN layer thickness is 1um under hydrogen atmosphere.
As one of preferred version of the present invention, on lithium aluminate (302) face substrate, at N
2Protection is warmed up to 950 ℃, growing low temperature protective layer under nitrogen atmosphere down; Reduce pressure then to 100-300torr, be warmed up to 1100 ℃ of non-doped gallium nitride layer of continued growth under nitrogen atmosphere; And then being warmed up to 1150 ℃, growth high temperature U-GaN layer thickness is 1um under hydrogen atmosphere.
As one of preferred version of the present invention, on lithium aluminate (302) face substrate, at N
2Protection is warmed up to 950 ℃, growing low temperature protective layer under nitrogen atmosphere down; Reduce pressure then to 100-300torr, be warmed up to 1100 ℃ of non-doped gallium nitride layer of continued growth under nitrogen atmosphere; And then being warmed up to 1150 ℃, growth high temperature U-GaN layer thickness is 1um under hydrogen atmosphere.
The present invention is by growing low temperature protective layer and high temperature U-GaN layer, and protection lithium aluminate substrate is not destroyed by high temperature, and improves film quality, has improved the surface finish of GaN film.
Description of drawings
Fig. 1 be the present invention a kind of on lithium aluminate (302) face substrate the structural representation of the nonpolar a of growing high-quality (11-20) face GaN film;
Fig. 2 is the experimental result synoptic diagram of the embodiment of the invention one.
Embodiment
Further specify concrete implementation step of the present invention below in conjunction with accompanying drawing:
Embodiment one
A kind of on lithium aluminate (302) face substrate the method for the nonpolar a of growing high-quality (11-20) face GaN film, in metal organic chemical vapor deposition (MOCVD) system, at lithium aluminate (LiAlO
2) on (302) face substrate, at N
2Protection is warmed up to 800 ℃ down, and growing low temperature protective layer under nitrogen atmosphere, low-temperature protection layer chamber pressure are 150-500torr, and trimethyl-gallium (TMGa) flow is 1-50sccm, corresponding to molar flow: 4E-6mole/min-3E-4mole/min; Reduce pressure then to 100-300torr, be warmed up to the 1000 ℃ of non-doped gallium nitride of continued growth (U-GaN) layers under nitrogen atmosphere, the TMGa flow is 10-150sccm, corresponding to molar flow: 4E-5mol/min-7.5E-4mole/min; And then be warmed up to 1050 ℃, and the about 1um of growth high temperature U-GaN under hydrogen atmosphere, the TMGa flow is 20-200sccm, corresponding to molar flow: 8E-5mol/min-1E-3mole/min.By the growing low temperature protective layer, protection lithium aluminate substrate is not destroyed by high temperature, and high temperature U-GaN layer has improved film quality, improves surface finish.XRD rocking curve peak width at half height 750arcsec.
Embodiment two
A kind of on lithium aluminate (302) face substrate the method for the nonpolar a of growing high-quality (11-20) face GaN film, in metal organic chemical vapor deposition (MOCVD) system, at lithium aluminate (LiAlO
2) on (302) face substrate, at N
2Protection is warmed up to 900 ℃ down, and growing low temperature protective layer under nitrogen atmosphere, low-temperature protection layer chamber pressure are 150-500torr, and trimethyl-gallium (TMGa) flow is 1-50sccm, corresponding to molar flow: 4E-6mole/min-3E-4mole/min; Reduce pressure then to 100-300torr, be warmed up to the 1050 ℃ of non-doped gallium nitride of continued growth (U-GaN) layers under nitrogen atmosphere, the TMGa flow is 10-150sccm, corresponding to molar flow: 4E-5mol/min-7.5E-4mole/min; And then be warmed up to 1110 ℃, and the about 1um of growth high temperature U-GaN under hydrogen atmosphere, the TMGa flow is 20-200sccm, corresponding to molar flow: 8E-5mol/min-1E-3mole/min.This novel process makes film surface smooth, XRD rocking curve peak width at half height 720arcsec.
Embodiment three
A kind of on lithium aluminate (302) face substrate the method for the nonpolar a of growing high-quality (11-20) face GaN film, in metal organic chemical vapor deposition (MOCVD) system, at lithium aluminate (LiAlO
2) on (302) face substrate, under the N2 protection, be warmed up to 950 ℃, growing low temperature protective layer under nitrogen atmosphere, low-temperature protection layer chamber pressure is 150-500torr, and trimethyl-gallium (TMGa) flow is 1-50sccm, corresponding to molar flow: 4E-6mole/min-3E-4mole/min; Reduce pressure then to 100-300torr, be warmed up to the 1100 ℃ of non-doped gallium nitride of continued growth (U-GaN) layers under nitrogen atmosphere, the TMGa flow is 10-150sccm, corresponding to molar flow: 4E-5mol/min-7.5E-4mole/min; And then be warmed up to 1150 ℃, and the about 1um of growth high temperature U-GaN under hydrogen atmosphere, the TMGa flow is 20-200sccm, corresponding to molar flow: 8E-5mol/min-1E-3mole/min.This novel process makes film surface smooth, XRD rocking curve peak width at half height 750arcsec.
Other processing condition that relate among the present invention are the common process condition, belong to the category that those skilled in the art are familiar with, and do not repeat them here.
The present invention is by growing low temperature protective layer and high temperature U-GaN layer, and protection lithium aluminate substrate is not destroyed by high temperature, and improves film quality, has improved the surface finish of GaN film.
The foregoing description is the unrestricted technical scheme of the present invention in order to explanation only.Any technical scheme that does not break away from spirit and scope of the invention all should be encompassed in the middle of the patent claim of the present invention.
Claims (5)
1. the method for a growing nonpolar a face GaN film on the lithium aluminate substrate, it is characterized in that: this method may further comprise the steps:
Step 1, growing low temperature protective layer: promptly in the MOCVD system, do substrate with lithium aluminate (302) face, at N
2Protection is warmed up to 800-950 ℃ down, and growing low temperature protective layer under nitrogen atmosphere, low-temperature protection layer chamber pressure are 150-500torr, and trimethyl-gallium TMGa flow is 1-50sccm, corresponding to molar flow: 4E-6mole/min-3E-4mole/min;
Step 2, the non-doped gallium nitride layer of growing: reduce pressure then to 100-300torr, be warmed up to the 1000-1100 ℃ of non-doped gallium nitride layer of continued growth under nitrogen atmosphere, the TMGa flow is 10-150sccm, corresponding to molar flow: 4E-5mol/min-7.5E-4mole/min;
Step 3, growth high temperature U-GaN layer: be warmed up to 1050-1150 ℃ at last again, growth thickness is the high temperature U-GaN layer of 1um under hydrogen atmosphere, and the TMGa flow is 20-200sccm, corresponding to molar flow: 8E-5mol/min-1E-3mole/min.
2. as claimed in claim 1 a kind of on the lithium aluminate substrate method of growing nonpolar a face GaN film, it is characterized in that: before carrying out step 1 growing low temperature protective layer, earlier lithium aluminate (302) face substrate is carried out surface heat under 600-900 ℃ and handle.
3. as claimed in claim 1 a kind of on the lithium aluminate substrate method of growing nonpolar a face GaN film, it is characterized in that: on lithium aluminate (302) face substrate, at N
2Protection is warmed up to 800 ℃ down, and growing low temperature protective layer under nitrogen atmosphere reduces pressure then to 100-300torr, is warmed up to 1000 ℃ of non-doped gallium nitride layer of continued growth under nitrogen atmosphere; And then being warmed up to 1050 ℃, growth high temperature U-GaN layer thickness is 1um under hydrogen atmosphere.
4. as claimed in claim 1 a kind of on the lithium aluminate substrate method of growing nonpolar a face GaN film, it is characterized in that: on lithium aluminate (302) face substrate, at N
2Protection is warmed up to 950 ℃ down, growing low temperature protective layer under nitrogen atmosphere; Reduce pressure then to 100-300torr, be warmed up to 1100 ℃ of non-doped gallium nitride layer of continued growth under nitrogen atmosphere; And then being warmed up to 1150 ℃, growth high temperature U-GaN layer thickness is 1um under hydrogen atmosphere.
5. as claimed in claim 1 a kind of on the lithium aluminate substrate method of growing nonpolar a face GaN film, it is characterized in that: on lithium aluminate (302) face substrate, at N
2Protection is warmed up to 950 ℃, growing low temperature protective layer under nitrogen atmosphere down; Reduce pressure then to 100-300torr, be warmed up to 1100 ℃ of non-doped gallium nitride layer of continued growth under nitrogen atmosphere; And then being warmed up to 1150 ℃, growth high temperature U-GaN layer thickness is 1um under hydrogen atmosphere.
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|---|---|---|---|
| CN200910046585XA CN101509145B (en) | 2009-02-24 | 2009-02-24 | Method for growing nonpolar a face GaN film on lithium aluminate substrate |
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|---|---|---|---|
| CN200910046585XA CN101509145B (en) | 2009-02-24 | 2009-02-24 | Method for growing nonpolar a face GaN film on lithium aluminate substrate |
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| CN101509145B CN101509145B (en) | 2011-03-30 |
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Cited By (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101717923B (en) * | 2009-12-10 | 2012-06-06 | 上海蓝光科技有限公司 | Nonpolar GaN membrane and preparation method thereof |
| CN107331743A (en) * | 2017-08-29 | 2017-11-07 | 上海应用技术大学 | It is a kind of to prepare method and its structure based on lithium aluminate substrate Single chip white light LED |
| CN109560085A (en) * | 2018-12-10 | 2019-04-02 | 武汉华星光电半导体显示技术有限公司 | Display panel and display module |
Family Cites Families (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1242091C (en) * | 2002-12-20 | 2006-02-15 | 上海北大蓝光科技有限公司 | Method for growing epitaxial chip of nitride LED structure by MOCVD |
| CN1329955C (en) * | 2004-07-21 | 2007-08-01 | 南京大学 | Method of preparing high quality non-polar GaN self-support substrate |
| CN1657660A (en) * | 2004-12-15 | 2005-08-24 | 中国科学院上海光学精密机械研究所 | Process for preparation large-size high-quality lithium aluminate crystal wafer |
| CN100451181C (en) * | 2006-10-16 | 2009-01-14 | 中国电子科技集团公司第五十五研究所 | Method for carrying out epitaxial growth of single crystal film of nitride by using mask in situ |
| CN101364631B (en) * | 2008-09-25 | 2011-09-14 | 上海蓝光科技有限公司 | Nonpolar GaN film growth method |
-
2009
- 2009-02-24 CN CN200910046585XA patent/CN101509145B/en not_active Expired - Fee Related
Cited By (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101717923B (en) * | 2009-12-10 | 2012-06-06 | 上海蓝光科技有限公司 | Nonpolar GaN membrane and preparation method thereof |
| CN107331743A (en) * | 2017-08-29 | 2017-11-07 | 上海应用技术大学 | It is a kind of to prepare method and its structure based on lithium aluminate substrate Single chip white light LED |
| CN109560085A (en) * | 2018-12-10 | 2019-04-02 | 武汉华星光电半导体显示技术有限公司 | Display panel and display module |
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| CN101509145B (en) | 2011-03-30 |
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