CN102409406A - Growing method for low-dislocation gallium nitride - Google Patents
Growing method for low-dislocation gallium nitride Download PDFInfo
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- CN102409406A CN102409406A CN2011103327933A CN201110332793A CN102409406A CN 102409406 A CN102409406 A CN 102409406A CN 2011103327933 A CN2011103327933 A CN 2011103327933A CN 201110332793 A CN201110332793 A CN 201110332793A CN 102409406 A CN102409406 A CN 102409406A
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- gallium nitride
- nitride template
- hexagonal
- little hole
- low dislocation
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Abstract
The invention discloses a growing method for low-dislocation gallium nitride. The method comprises the following steps of: 1, preparing a base plate, wherein the base plate comprises a substrate and a gallium nitride template manufactured on the substrate; 2, corroding the surface of the gallium nitride template by using corrosive liquid to form a hexangular micro-pit on the surface of the gallium nitride template; 3, coating silicon dioxide gel on the surface of the gallium nitride template with the hexangular micro-pit to cover the hexangular micro-pit, and performing spin coating by using a spin coater; 4, curing the silicon dioxide gel on the gallium nitride template by adopting high-temperature sintering; 5, performing treatment by using the solution of NaOH to remove the silicon dioxide gel outside the micro-pit on the gallium nitride template 11; 6, changing the silicon dioxide gel in the hexangular micro-pit into crystals by adopting the high-temperature sintering again; and 7, extending a gallium nitride material on the treated gallium nitride template to finish the growth of the low-dislocation gallium nitride.
Description
Technical field
The present invention relates to the growth method of a kind of low dislocation gan (GaN), belong to the semiconductor material growing field.
Background technology
GaN base LED has energy-saving and environmental protection, cold light source, colour rendering index is high, response speed is fast, volume is little and outstanding advantage such as long working life, and its green solid light source as a new generation's illumination revolution demonstrates huge application potential.
Sapphire Substrate is that nitride carries out one of the most frequently used substrate of heteroepitaxial growth at present.Owing to have very macrolattice constant mismatch and thermal expansion coefficient difference between Sapphire Substrate and the nitride epitaxial layer; Therefore there are very big unrelieved stress and many lattice defects in the nitride epitaxial layer; Influence the crystal mass of material, limited the further raising of device photoelectric performance.
The present invention is through handling the GaN epitaxial film; Come out in the zone that dislocation is concentrated; After silica dioxide gel filling processing, the dislocation concentrated area is shielded by silica dioxide gel, on the template after the processing, follows extension GaN; Can effectively reduce the dislocation desity of extension GaN layer, improve the crystal mass and the homogeneity of epitaxial material.
Summary of the invention
The growth method that the purpose of this invention is to provide a kind of low dislocation GaN can effectively reduce the dislocation desity of extension GaN layer, improves the crystal mass of epitaxial material.
The present invention provides a kind of growth method of low dislocation gan, comprises the steps:
Step 1: get a substrate, this substrate comprises a substrate and the gallium nitride template of making above that;
Step 2:, form the little hole of hexagonal on the surface of gallium nitride template with the surface of corrosive fluid corrosion gallium nitride template;
Step 3: at the surface-coated silica dioxide gel of gallium nitride template, the little hole of hexagonal is covered, carry out whirl coating with photoresist spinner and handle with the little hole of hexagonal;
Step 4: adopt high temperature sintering that the silica dioxide gel on the gallium nitride template is solidified;
Step 5: use the NaOH solution-treated, remove the silica dioxide gel beyond little hole on the gallium nitride template 11;
Step 6: adopt high temperature sintering again, make the silica dioxide gel in the little hole of hexagonal become crystal;
Step 7: extension gallium nitride material on the gallium nitride template after the processing, accomplish the growth of low dislocation gan.
Wherein corrosive fluid is a KOH solution in the step 2, and temperature is 80 ℃, and etching time is 1-2min, and perhaps the volume ratio of corrosive fluid is H
2SO
4: H
3PO
4=3: 1, temperature is 260 ℃, and etching time is 4-8min.
Wherein the degree of depth in the little hole of hexagonal of step 2 is less than the degree of depth of gallium nitride template.
Wherein whirl coating is treated in the step 3: with the even glue of photoresist spinner, the rotating speed of even glue is 500 commentaries on classics/min, and the time is 5s; Use the photoresist spinner whirl coating again, the rotating speed of whirl coating is 8000 commentaries on classics/min, and the time is 20s.
Wherein the temperature of the high temperature sintering of step 4 is 600 ℃, and silica dioxide gel is solidified.
Wherein the mass ratio of the NaOH solution of step 5 is 30%, and temperature is 60 ℃, and the time is 1-5min.
Wherein the temperature of the high temperature sintering of step 6 is 1100-1300 ℃, makes that silicon-dioxide becomes crystal in the little hole of hexagonal, make its can be in MOCVD high growth temperature.
Description of drawings
For making the inspector can further understand structure of the present invention, characteristic and purpose thereof, below in conjunction with the detailed description of accompanying drawing and preferred embodiment as after, wherein:
Fig. 1 is a substrate synoptic diagram of the present invention;
Fig. 2 forms the synoptic diagram in the little hole of hexagonal on substrate for the present invention;
Fig. 3 is the sectional view the present invention fills silicon-dioxide in the little hole of hexagonal after;
Fig. 4 is the synoptic diagram of extension gallium nitride material of the present invention.
Embodiment
See also Fig. 1 to shown in Figure 4, the present invention provides a kind of growth method of low dislocation gan, comprises the steps:
Step 1: get a substrate; This substrate comprises a substrate 10 and gallium nitride template 11 (see figure 1)s of making above that; The substrate here can be that sapphire, SiC, Si, GaAS, GaN can be InP at the material of substrate epitaxial; GaAs, ternary, quaternary III-V family and IV-VI compound semiconductors such as GaN, AlN, InN, InGaN, AlGaN, AlInN, AlInGaN.
Step 2: with the surface of corrosive fluid corrosion gallium nitride template 11, form the little hole of hexagonal 20 (see figure 2)s on the surface of gallium nitride template 11, this corrosive fluid is a KOH solution, and temperature is 80 ℃, and etching time is 1-2min, and perhaps the volume ratio of corrosive fluid is H
2SO
4: H
3PO
4=3: 1, temperature is 260 ℃, and etching time is 4-8min, and the degree of depth in the little hole 20 of said hexagonal is less than the degree of depth of gallium nitride template 11; Making most dislocations on gallium nitride template 11 surface, is exactly that all expose in the little hole 20 of hexagonal.
Step 3: in surface-coated silica dioxide gel 30 (see figure 3)s of gallium nitride template 11 with the little hole 20 of hexagonal; The little hole 20 of hexagonal is covered; Carry out whirl coating with photoresist spinner and handle, said whirl coating processed steps is: with the even glue of photoresist spinner, the rotating speed of even glue is 500 commentaries on classics/min; Time is 5s, makes glue that preliminary a distribution can be arranged; Use the photoresist spinner whirl coating again, the rotating speed of whirl coating is 8000 commentaries on classics/min, and the time is 20s, and the glue thought of the little hole 20 of hexagonal can be very thin like this.
Step 4: adopt high temperature sintering that the silica dioxide gel 30 on the gallium nitride template 11 is solidified, the temperature of described high temperature sintering is 600 ℃, and silica dioxide gel 30 is solidified.
Step 5: use the NaOH solution-treated, remove the silica dioxide gel 30 beyond the little hole 20 of hexagonal on the gallium nitride template 11, the mass ratio of described NaOH solution is 30%, and temperature is 60 ℃, and the time is 1-5min.
Step 6: adopt high temperature sintering again; Make the silica dioxide gels 30 in the little hole of hexagonal 20 become crystal, the temperature of described high temperature sintering is 1100-1300 ℃, makes that silicon-dioxide becomes crystal in little hole; Make its can be in MOCVD high growth temperature, so just can not pollute the growth room.
Step 7: extension gallium nitride material 40 (see figure 4)s on the gallium nitride template after the processing 11; Accomplish the growth of low dislocation gan, here 40 also can be ternary, quaternary III-V family and IV-VI compound semiconductors such as InP, GaAs, GaN, AlN, InN, InGaN, AlGaN, AlInN, AlInGaN.Because on the gallium nitride template after the processing 11, originally the dislocation exposed after the corrosion is exactly that the little hole 20 of hexagonal is all filled out in the dust, and the dislocation on the original template 11 can not continue extension gallium nitride material 40 time again.Will obtain the gallium nitride material 40 of low dislocation.
The above; Be merely the embodiment among the present invention, but protection scope of the present invention is not limited thereto, anyly is familiar with this technological people in the technical scope that the present invention disclosed; The conversion that can expect easily or replacement all should be encompassed in of the present invention comprising within the scope.Therefore, protection scope of the present invention should be as the criterion with the protection domain of claims.
Claims (7)
1. the growth method of a low dislocation gan comprises the steps:
Step 1: get a substrate, this substrate comprises a substrate and the gallium nitride template of making above that;
Step 2:, form the little hole of hexagonal on the surface of gallium nitride template with the surface of corrosive fluid corrosion gallium nitride template;
Step 3: at the surface-coated silica dioxide gel of gallium nitride template, the little hole of hexagonal is covered, carry out whirl coating with photoresist spinner and handle with the little hole of hexagonal;
Step 4: adopt high temperature sintering that the silica dioxide gel on the gallium nitride template is solidified;
Step 5: use the NaOH solution-treated, remove the silica dioxide gel beyond little hole on the gallium nitride template 11;
Step 6: adopt high temperature sintering again, make the silica dioxide gel in the little hole of hexagonal become crystal;
Step 7: extension gallium nitride material on the gallium nitride template after the processing, accomplish the growth of low dislocation gan.
2. the growth method of low dislocation gan according to claim 1, wherein corrosive fluid is a KOH solution in the step 2, and temperature is 80 ℃, and etching time is 1-2min, and perhaps the volume ratio of corrosive fluid is H
2SO
4: H
3PO
4=3: 1, temperature is 260 ℃, and etching time is 4-8min.
3. the growth method of low dislocation gan according to claim 1, wherein the degree of depth in the little hole of hexagonal of step 2 is less than the degree of depth of gallium nitride template.
4. the growth method of low dislocation gan according to claim 1, wherein whirl coating is treated in the step 3: with the even glue of photoresist spinner, the rotating speed of even glue is 500 commentaries on classics/min, and the time is 5s; Use the photoresist spinner whirl coating again, the rotating speed of whirl coating is 8000 commentaries on classics/min, and the time is 20s.
5. the growth method of low dislocation gan according to claim 1, wherein the temperature of the high temperature sintering of step 4 is 600 ℃, and silica dioxide gel is solidified.
6. the growth method of low dislocation gan according to claim 1, wherein the mass ratio of the NaOH solution of step 5 is 30%, and temperature is 60 ℃, and the time is 1-5min.
7. the growth method of low dislocation gan according to claim 1, wherein the temperature of the high temperature sintering of step 6 is 1100-1300 ℃, makes that silicon-dioxide becomes crystal in the little hole of hexagonal, make its can be in MOCVD high growth temperature.
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Cited By (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN103866380A (en) * | 2014-03-25 | 2014-06-18 | 山东大学 | Method for carrying out GaN single crystal growth by using graphic annealing porous structure |
| CN107326444A (en) * | 2017-07-21 | 2017-11-07 | 山东大学 | A kind of method that hydro-thermal corrosion porous-substrates grow self-standing gan monocrystalline |
| CN110230102A (en) * | 2018-03-05 | 2019-09-13 | 中国科学院苏州纳米技术与纳米仿生研究所 | Extremely low dislocation density gallium nitride single crystal and its flux growth metrhod growing method |
| CN113445131A (en) * | 2021-06-28 | 2021-09-28 | 中国科学院上海光学精密机械研究所 | Method for inhibiting defects from gallium nitride seed crystal, gallium nitride single crystal and application |
| CN114574960A (en) * | 2022-02-23 | 2022-06-03 | 江苏第三代半导体研究院有限公司 | Nitride epitaxial layer structure, nitride epitaxial wafer and preparation method |
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| CN1434482A (en) * | 2003-02-18 | 2003-08-06 | 华南师范大学 | Method for making gallium nitride crystal |
| CN1560900A (en) * | 2004-03-05 | 2005-01-05 | 长春理工大学 | Method of growing low dislocation gallium nitride on silicon substrate |
| CN1588640A (en) * | 2004-08-19 | 2005-03-02 | 中国科学院物理研究所 | Method for preparing high quality GaN base material on specific saphire pattern substrate |
| JP2011216549A (en) * | 2010-03-31 | 2011-10-27 | Jx Nippon Mining & Metals Corp | METHOD OF MANUFACTURING GaN-BASED SEMICONDUCTOR EPITAXIAL SUBSTRATE |
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2011
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| CN1434482A (en) * | 2003-02-18 | 2003-08-06 | 华南师范大学 | Method for making gallium nitride crystal |
| CN1560900A (en) * | 2004-03-05 | 2005-01-05 | 长春理工大学 | Method of growing low dislocation gallium nitride on silicon substrate |
| CN1588640A (en) * | 2004-08-19 | 2005-03-02 | 中国科学院物理研究所 | Method for preparing high quality GaN base material on specific saphire pattern substrate |
| JP2011216549A (en) * | 2010-03-31 | 2011-10-27 | Jx Nippon Mining & Metals Corp | METHOD OF MANUFACTURING GaN-BASED SEMICONDUCTOR EPITAXIAL SUBSTRATE |
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Cited By (6)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN103866380A (en) * | 2014-03-25 | 2014-06-18 | 山东大学 | Method for carrying out GaN single crystal growth by using graphic annealing porous structure |
| CN103866380B (en) * | 2014-03-25 | 2016-05-11 | 山东大学 | A kind ofly use graphical annealing loose structure to carry out the method for GaN crystal growth |
| CN107326444A (en) * | 2017-07-21 | 2017-11-07 | 山东大学 | A kind of method that hydro-thermal corrosion porous-substrates grow self-standing gan monocrystalline |
| CN110230102A (en) * | 2018-03-05 | 2019-09-13 | 中国科学院苏州纳米技术与纳米仿生研究所 | Extremely low dislocation density gallium nitride single crystal and its flux growth metrhod growing method |
| CN113445131A (en) * | 2021-06-28 | 2021-09-28 | 中国科学院上海光学精密机械研究所 | Method for inhibiting defects from gallium nitride seed crystal, gallium nitride single crystal and application |
| CN114574960A (en) * | 2022-02-23 | 2022-06-03 | 江苏第三代半导体研究院有限公司 | Nitride epitaxial layer structure, nitride epitaxial wafer and preparation method |
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Application publication date: 20120411 |