CN102903614A - Method for preparing non-polar A face GaN thin film - Google Patents
Method for preparing non-polar A face GaN thin film Download PDFInfo
- Publication number
- CN102903614A CN102903614A CN2012103111488A CN201210311148A CN102903614A CN 102903614 A CN102903614 A CN 102903614A CN 2012103111488 A CN2012103111488 A CN 2012103111488A CN 201210311148 A CN201210311148 A CN 201210311148A CN 102903614 A CN102903614 A CN 102903614A
- Authority
- CN
- China
- Prior art keywords
- face
- preparing
- gan film
- thin film
- non polarity
- Prior art date
- Legal status (The legal status is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the status listed.)
- Pending
Links
Images
Abstract
The invention provides a method for preparing a non-polar A face GaN thin film. The method comprises the following steps of: preparing an A face ZnO buffering thin film on the surface of a substrate; and preparing the non-polar A face GaN thin film on the prepared A face ZnO buffering thin film. According to the method disclosed by the invention, lattice mismatch and heat lattice mismatch between GaN and the substrate can be coordinated by a ZnO buffering layer, so that the crystallization quality of the prepared GaN thin film is greatly improved.
Description
Technical field
The present invention relates to the semiconductive thin film preparing technical field, relate in particular to a kind of method for preparing the non polarity A face GaN film.
Background technology
Gallium nitride (GaN) belongs to third generation semi-conducting material, belong to the hexagonal wurtzite structure, be the core component of light-emitting diode in the semiconductor lighting, short wavelength laser, ultraviolet detector and high temperature high power device, be prepared in industrial general employing metal-organic chemical vapor deposition equipment method (MOCVD).
Nature lacks natural GaN body monocrystal material, and present work carries out at substrates such as sapphire, SiC, Si mainly that heteroepitaxy carries out.Because lattice mismatch and thermal mismatching between GaN and substrate cause having high dislocation density in the heteroepitaxy GaN film, cause its strain and stress greatly to improve, thereby have greatly affected its performance.
Take at Grown on Sapphire Substrates non polarity A-GaN as example, non polarity A-GaN and sapphire are along GaN[0001] lattice mismatch of direction is 1%, is 16% along the lattice mismatch of [1-100] direction, thermal mismatching is respectively-72% and-25%.Thermal mismatching is-2.6 * 10 along the strain of [0001] direction when dropping to room temperature from growth temperature
-3, and the strain of edge [1-100] direction is-1.8 * 10
-3, its corresponding stress is respectively-0.74GPa and-1.11GPa, so heteroepitaxy is difficult to obtain the film of crystalline quality excellence.
Research in recent years mainly concentrates on the epitaxial quality that how to improve the non polarity A face GaN film.People have adopted a lot of methods to improve the crystalline quality of film, for example spread one deck Si
xN, epitaxial lateral overgrowth is grown in v-LiAlO
2On the substrate, use the nano-pillar epitaxial lateral overgrowth.But, adopt traditional GaN resilient coating technology, be difficult to obtain the A-GaN film of crystalline quality excellence and surfacing.
Summary of the invention
The technical problem that (one) will solve
For solving above-mentioned one or more problems, the invention provides a kind of method for preparing the non polarity A face GaN film.
(2) technical scheme
According to an aspect of the present invention, provide a kind of method for preparing nonpolar GaN film.The method comprises: prepare A face ZnO buffer thin film at substrate surface; A face ZnO buffer thin film preparation non polarity A face GaN film in preparation.
(3) beneficial effect
Can find out from technique scheme, the method that the present invention prepares the non polarity A face GaN film has following beneficial effect:
(1) lattice constant of ZnO and GaN mate very much, its Young's modulus will be far smaller than GaN simultaneously, the ZnO resilient coating can be coordinated lattice mismatch and the thermal mismatching between GaN and the sapphire, thereby has improved greatly the crystalline quality of the non polarity A face GaN film of preparation;
(2) because Zn has diffused into Sapphire Substrate, A-GaN film and R-Al have been improved
3O
2Interface state between the substrate forms the layer that one deck is conducive to increase the chemical state of Ga atomic surface diffusion length;
(3) than the MBE growing technology, MOCVD Material growth technology, because its relatively cheap cost is widely used in suitability for industrialized production, method of the present invention has the high speed of growth, reaches 0.6 μ m/hr, growth quality is better simultaneously.
Description of drawings
Fig. 1 is the flow chart according to the preparation non polarity A face GaN film of the embodiment of the invention;
Fig. 2 is the swing curve of GaN film edge [0001] and [1-100] both direction of employing method preparation shown in Figure 1;
Fig. 3 is for adopting the PL spectral curve of GaN film when 77K of method preparation shown in Figure 1.
Embodiment
For making the purpose, technical solutions and advantages of the present invention clearer, below in conjunction with specific embodiment, and with reference to accompanying drawing, the present invention is described in more detail.Need to prove, although this paper can provide the demonstration of the parameter that comprises particular value, should be appreciated that, parameter need not definitely to equal corresponding value, but can be similar to corresponding value in acceptable error margin or design constraint.
In one exemplary embodiment of the present invention, provide a kind of method for preparing the non polarity A face GaN film.As shown in Figure 1, this method for preparing the non polarity A face GaN film comprises:
Steps A: process substrate;
In the present embodiment, select the R surface sapphire as substrate, can certainly select SiC, Si etc. and GaN lattice mismatch less than 2% substrate.
Process the impurity that substrate the most important thing is to remove substrate surface, i.e. cleaning step.In this cleaning step, at first used acetone ultrasonic 10 minutes, with deionized water (DIW) flushing for several times; Then at H
2SO
4: HNO
3Boiled in=1: 1 the corrosive liquid 10 minutes, (DIW) rinses substrate well with a large amount of ionized waters; At last, before putting into equipment, with infrared lamp substrate is dried.
Step B: prepare A face ZnO buffer thin film at substrate surface;
Before depositing, need to vacuumize processing to reative cell, need to repeatedly fill and take out reative cell for several times, purpose is to reduce the impact of the inner impurity molecule of reative cell, and when wherein bleeding, the numerical value of pressure about with 100Torr reduces, and that can not take out is too quickly.
Again reative cell is carried out after several vacuumizes processing, in reative cell, inflate to reach the required pressure of growth, chamber pressure maintains 76Torr in the growth course, open simultaneously heater switch, the rising temperature is to 550 degrees centigrade of growth temperatures, after temperature reaches growth temperature, under growth temperature, toasted substrate 30 minutes first, purpose is to remove hydrone and the activation substrate surface that substrate surface absorbs.
Then, open the control valve of zinc source bottle, leave first the gas hand-operated valve, drive again the gas hand-operated valve into, allow the zinc source in pipeline, lead to for a moment first, make it before passing into reative cell, reach air-flow steady.When stoving time reaches 30 minutes, open zinc source shutter, make zinc source air-flow pass into stably reative cell, utilize diethyl zinc and oxygen as reaction source, the zinc source is kept in the stainless steel gas cylinder, and its temperature remains on 18 ℃, pressure remains on 1000Torr, nitrogen is done carrier gas, and the flow of diethyl zinc is 22 μ mol/min, oxygen source O
2Flow be 1SLM (standard Liter Per Minute), growth time is 8 minutes, thickness is 50nm.The A face ZnO resilient coating that makes takes out after keeping being down to room temperature again in 15 minutes under oxygen atmosphere.
In the present embodiment, adopt the MOCVD method to prepare A face ZnO buffer thin film, can certainly adopt other method to prepare A face ZnO buffer thin film, such as: chemical vapour deposition technique (CVD), pulsed laser deposition (PLD) or magnetron sputtering method etc.The thickness of A face ZnO buffer thin film is between between the 10nm to 100nm.
Step C is at the A face ZnO buffer thin film preparation non polarity A face GaN film of preparation;
The A side ZnO film that makes is put into nitride MOCVD equipment as substrate, gallium source and nitrogenous source are respectively trimethyl gallium and ammonia, carrier gas is nitrogen, growth temperature is 1100 ℃, growth pressure is 60Torr, and the gallium source flux is 8 μ mol/min, and ammonia flow is 3SLM, growth time is 1 hour, and measuring thickness of sample after growth finishes is 0.62 μ m.
In the present embodiment, adopt the MOCVD method to prepare the GaN buffer thin film, can certainly adopt other method to prepare non polarity A side GaN buffer thin film, such as: chemical vapour deposition technique (CVD), pulsed laser deposition (PLD) or magnetron sputtering method etc.
Step D after the GaN film preparation is complete, closes the gallium source, drops to below 300 degrees centigrade at reaction chamber temperature and closes nitrogenous source, finishes the growth of A face GaN film.
As a comparison, the sample of traditional GaN buffer growth is 1347arcsecond along the halfwidth that waves of m axle, is 2372arcsecond along the halfwidth that waves of c-axis.And Fig. 2 is the swing curve of GaN film edge [0001] and [1-100] both direction of employing method preparation shown in Figure 1.As shown in Figure 2, in the A-GaN film with the ZnO buffer growth, halfwidth along the m axle is 1558arcsecond, halfwidth along c-axis is 1263arcsecond, and is far smaller than the difference of the sample of growing on traditional A-GaN resilient coating along the difference of the halfwidth of two different solid angle direction.As seen, adopt the sample of ZnO buffer growth, this has illustrated that the anisotropy of the sample of growing on the ZnO resilient coating has obtained very large improvement, and crystalline quality is better than the film that adopts traditional A-GaN buffer growth.
Fig. 3 is for adopting photoluminescence spectrum (PL) curve of GaN film when 77K of method preparation shown in Figure 1.By photoluminescence spectrum (PL) can Knowing material quality condition, because luminescence generated by light has directly been measured the luminous intensity of sample, under identical measuring condition, can make contrast to the relative luminous efficiency of different samples, this detection to light emitting semiconductor device and Laser Devices material identifies to have direct meaning.As shown in Figure 3, the characteristics of luminescence of two samples that have or not the ZnO resilient coating when having contrasted 77K, can find out, its luminous intensity of sample of growing at the ZnO resilient coating will be far longer than the sample that conventional buffer layer is grown, so have preferably optical property with the A-GaN film of ZnO buffer growth.
Above-described specific embodiment; purpose of the present invention, technical scheme and beneficial effect are further described; institute is understood that; the above only is specific embodiments of the invention; be not limited to the present invention; within the spirit and principles in the present invention all, any modification of making, be equal to replacement, improvement etc., all should be included within protection scope of the present invention.
Claims (12)
1. a method for preparing the non polarity A face GaN film is characterized in that, comprising:
Prepare A face ZnO buffer thin film at substrate surface;
A face ZnO buffer thin film preparation non polarity A face GaN film in preparation.
2. the method for preparing the non polarity A face GaN film according to claim 1 is characterized in that, the thickness of described A face ZnO buffer thin film is between between the 10nm to 100nm.
3. the method for preparing the non polarity A face GaN film according to claim 2 is characterized in that, adopts the standby described A face ZnO buffer thin film of metal-organic chemical vapor deposition equipment legal system.
4. the method for preparing the non polarity A face GaN film according to claim 3 is characterized in that, in the standby step of A face ZnO buffer thin film of described employing metal-organic chemical vapor deposition equipment legal system: reaction source is diethyl zinc and oxygen, and carrier gas is nitrogen.
5. the method for preparing the non polarity A face GaN film according to claim 4, it is characterized in that, described employing metal-organic chemical vapor deposition equipment method prepares in the step of A face ZnO buffer thin film, and response parameter is: the flow of diethyl zinc is 22 μ mol/min; Oxygen source O
2Flow be 1SLM; Growth temperature is 550 ℃; Chamber pressure is 76Torr.
6. the method for preparing the non polarity A face GaN film according to claim 5 is characterized in that, the step that described employing metal-organic chemical vapor deposition equipment method prepares A face ZnO buffer thin film also comprises afterwards:
Growth temperature and chamber pressure remain unchanged, and the substrate for preparing A face ZnO buffer thin film was kept 15 minutes under the oxygen atmosphere of reaction chamber.
7. the method for preparing the non polarity A face GaN film according to claim 5 is characterized in that, the step that described employing metal-organic chemical vapor deposition equipment method prepares A face ZnO buffer thin film also comprises before:
After substrate put into reaction chamber, 550 ℃ of lower logical nitrogen baking substrates 30 minutes.
8. the method for preparing the non polarity A face GaN film according to claim 1 is characterized in that, adopts the standby described non polarity A face GaN film of metal-organic chemical vapor deposition equipment legal system.
9. the method for preparing the non polarity A face GaN film according to claim 8 is characterized in that, described employing metal-organic chemical vapor deposition equipment method prepares in the step of non polarity A face GaN film: gallium source and nitrogenous source are respectively trimethyl gallium and ammonia; Carrier gas is nitrogen.
10. the method for preparing the non polarity A face GaN film according to claim 9, it is characterized in that, described employing metal-organic chemical vapor deposition equipment method prepares in the step of non polarity A face GaN film, response parameter is: the flow of trimethyl gallium is 8 μ mol/min, and the flow of ammonia is 3SLM; Growth temperature is 1100 ℃; Chamber pressure is 60Torr.
11. each described method for preparing the non polarity A face GaN film in 10 is characterized in that according to claim 1, described substrate and GaN lattice mismatch are less than 2%.
12. the method for preparing the non polarity A face GaN film according to claim 11 is characterized in that, described substrate is R surface sapphire, SiC or Si.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN2012103111488A CN102903614A (en) | 2012-08-28 | 2012-08-28 | Method for preparing non-polar A face GaN thin film |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN2012103111488A CN102903614A (en) | 2012-08-28 | 2012-08-28 | Method for preparing non-polar A face GaN thin film |
Publications (1)
| Publication Number | Publication Date |
|---|---|
| CN102903614A true CN102903614A (en) | 2013-01-30 |
Family
ID=47575798
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| CN2012103111488A Pending CN102903614A (en) | 2012-08-28 | 2012-08-28 | Method for preparing non-polar A face GaN thin film |
Country Status (1)
| Country | Link |
|---|---|
| CN (1) | CN102903614A (en) |
Cited By (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN103996756A (en) * | 2014-05-30 | 2014-08-20 | 广州市众拓光电科技有限公司 | Film coating method and application thereof |
| CN104993012A (en) * | 2015-05-25 | 2015-10-21 | 中国科学院半导体研究所 | Preparation method of large-size nonpolar A-side GaN self-supporting substrate |
| CN105609604A (en) * | 2016-01-18 | 2016-05-25 | 华中科技大学 | Non-polarized plane ZnO ultraviolet LED device employing p-AlGaN as electron blocking layer |
| CN106299041A (en) * | 2016-08-29 | 2017-01-04 | 华南理工大学 | The preparation method and application of the nonpolar LED being grown in r surface sapphire substrate |
| CN114574961A (en) * | 2022-03-23 | 2022-06-03 | 广东省智能机器人研究院 | Zinc oxide film growth method |
Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US20070254459A1 (en) * | 2006-04-25 | 2007-11-01 | Samsung Electro-Mechanics Co., Ltd. | Method of growing non-polar m-plane nitride semiconductor |
| CN101728248A (en) * | 2008-10-15 | 2010-06-09 | 中国科学院半导体研究所 | Growing method of gallium nitride |
| CN101831613A (en) * | 2010-04-21 | 2010-09-15 | 中国科学院半导体研究所 | Method for growing nonpolar InN film by utilizing nonpolar ZnO buffer layer |
-
2012
- 2012-08-28 CN CN2012103111488A patent/CN102903614A/en active Pending
Patent Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US20070254459A1 (en) * | 2006-04-25 | 2007-11-01 | Samsung Electro-Mechanics Co., Ltd. | Method of growing non-polar m-plane nitride semiconductor |
| CN101728248A (en) * | 2008-10-15 | 2010-06-09 | 中国科学院半导体研究所 | Growing method of gallium nitride |
| CN101831613A (en) * | 2010-04-21 | 2010-09-15 | 中国科学院半导体研究所 | Method for growing nonpolar InN film by utilizing nonpolar ZnO buffer layer |
Non-Patent Citations (2)
| Title |
|---|
| ATSUSHI KOBAYASHI, ET AL.: ""Growth of a-plane GaN on lattice-matched ZnO substrates using a room temperature buffer layer"", 《APPLIDE PHYSICE LETTERS》 * |
| TINGTING JIA, ET AL.: ""Nonpolar a-plane GaN films grown on γ-LiAlO2 (302) substrates by low-pressure MOCVD"", 《JOURNAL OF CRYSTAL GROWTH》 * |
Cited By (7)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN103996756A (en) * | 2014-05-30 | 2014-08-20 | 广州市众拓光电科技有限公司 | Film coating method and application thereof |
| CN103996756B (en) * | 2014-05-30 | 2017-01-18 | 广州市众拓光电科技有限公司 | Film coating method and application thereof |
| CN104993012A (en) * | 2015-05-25 | 2015-10-21 | 中国科学院半导体研究所 | Preparation method of large-size nonpolar A-side GaN self-supporting substrate |
| CN104993012B (en) * | 2015-05-25 | 2017-04-12 | 中国科学院半导体研究所 | Preparation method of large-size nonpolar A-side GaN self-supporting substrate |
| CN105609604A (en) * | 2016-01-18 | 2016-05-25 | 华中科技大学 | Non-polarized plane ZnO ultraviolet LED device employing p-AlGaN as electron blocking layer |
| CN106299041A (en) * | 2016-08-29 | 2017-01-04 | 华南理工大学 | The preparation method and application of the nonpolar LED being grown in r surface sapphire substrate |
| CN114574961A (en) * | 2022-03-23 | 2022-06-03 | 广东省智能机器人研究院 | Zinc oxide film growth method |
Similar Documents
| Publication | Publication Date | Title |
|---|---|---|
| US6423983B1 (en) | Optoelectronic and microelectronic devices including cubic ZnMgO and/or CdMgO alloys | |
| Kinoshita et al. | Performance and reliability of deep-ultraviolet light-emitting diodes fabricated on AlN substrates prepared by hydride vapor phase epitaxy | |
| CN103887381B (en) | A kind of growing method for lifting ultraviolet LED epitaxial material crystalline quality | |
| CN103022295B (en) | Aluminum nitride film growing on silicon substrate and preparation method and application thereof | |
| CN104112803B (en) | Semi-polarity surface gallium nitride based light-emitting diode and preparation method thereof | |
| CN102903614A (en) | Method for preparing non-polar A face GaN thin film | |
| CN104037284A (en) | GaN thin film growing on Si substrate and preparation method and applications thereof | |
| CN105023979A (en) | A GaN-based LED epitaxial wafer and a manufacturing method thereof | |
| CN106299041A (en) | The preparation method and application of the nonpolar LED being grown in r surface sapphire substrate | |
| Hussain et al. | Applications and synthesis of zinc oxide: an emerging wide bandgap material | |
| CN106384763B (en) | Nonpolar InGaN/GaN multiple quantum wells nano-pillar and its preparation method | |
| TW202127687A (en) | Epitaxial substrate with 2D material interposer, manufacturing method and manufacturing assembly including a polycrystalline substrate, a polycrystalline 2D ultra-thin material interposer and an AlN, AlGaN or GaN based epitaxial layer | |
| CN107369748A (en) | A kind of LED epitaxial growth methods based on graphene | |
| CN107799640B (en) | High-light-efficiency P-type nonpolar AlN film and preparation method thereof | |
| CN111354629B (en) | AlN buffer layer structure for ultraviolet LED and manufacturing method thereof | |
| JP2012169621A (en) | METHOD FOR GROWING AlInGaN LAYER AND, OPTOELECTRONIC, PHOTOVOLTAIC AND ELECTRONIC DEVICES | |
| CN104538509A (en) | Method for growing three-dimensional structural layer of light-emitting diode | |
| CN105097451A (en) | Preparation method for low-dislocation density Al<x>Ga<1-x>N epitaxial thin film | |
| CN102185049B (en) | Preparation method of ZnO-based light-emitting device | |
| CN102185071B (en) | Non-polar ZnO-based luminescent device and manufacturing method thereof | |
| CN106299045B (en) | A kind of LED extensions contact layer growing method | |
| CN103882526B (en) | Direct growth is from the method for peeling GaN monocrystalline on sic substrates | |
| CN209045597U (en) | A kind of light emitting diode being grown on nanometic zinc oxide rod array compound substrate | |
| CN203179936U (en) | GaN film grown on Si substrate and electrical apparatus element containing GaN film | |
| JP2007096200A (en) | Compound semiconductor element |
Legal Events
| Date | Code | Title | Description |
|---|---|---|---|
| C06 | Publication | ||
| PB01 | Publication | ||
| C10 | Entry into substantive examination | ||
| SE01 | Entry into force of request for substantive examination | ||
| C05 | Deemed withdrawal (patent law before 1993) | ||
| WD01 | Invention patent application deemed withdrawn after publication |
Application publication date: 20130130 |