CN102839417B - A kind of method growing self-stripping gallium nitride film on a sapphire substrate - Google Patents
A kind of method growing self-stripping gallium nitride film on a sapphire substrate Download PDFInfo
- Publication number
- CN102839417B CN102839417B CN201210325765.3A CN201210325765A CN102839417B CN 102839417 B CN102839417 B CN 102839417B CN 201210325765 A CN201210325765 A CN 201210325765A CN 102839417 B CN102839417 B CN 102839417B
- Authority
- CN
- China
- Prior art keywords
- layer
- gallium nitride
- sapphire substrate
- growth
- mocvd device
- 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.)
- Expired - Fee Related
Links
Landscapes
- Crystals, And After-Treatments Of Crystals (AREA)
- Led Devices (AREA)
Abstract
The invention discloses a kind of method growing self-stripping gallium nitride film on a sapphire substrate, utilize MOCVD device close using InGaN interposed layer and GaN low temperature buffer layer as weak bond in r surface sapphire substrate layer growth a surface gallium nitride from stripping film, specifically comprise: get a Sapphire Substrate; In MOCVD device, pass into ammonia, nitrogenize is carried out to Sapphire Substrate, generate one deck nitride layer thereon; In MOCVD device, utilize carrier gas to pass into indium source, gallium source and ammonia, make to obtain InGaN layer on nitride layer; In MOCVD device, carrier gas is utilized to pass into gallium source and ammonia, growth one deck low temperature GaN buffer; In MOCVD device, carrier gas is utilized to pass into gallium source and ammonia, growing gallium nitride epitaxial film.The present invention does weak bonded layer with InGaN interposed layer and low temperature GaN buffer, can obtain high crystalline quality from peeling GaN film.
Description
Technical field
The invention belongs to technical field of semiconductors, refer to that a kind of InGaN interposed layer and low temperature GaN buffer of utilizing uses MOCVD device in r surface sapphire substrate, grow the method certainly peeling off a face GaN film as weak bonded layer especially.
Background technology
Gan, as the representative of third generation semiconductor material with wide forbidden band, can be used for making photodiode, laser diode, the opto-electronic devices such as High Electron Mobility Transistor.Because group III-nitride is hexagonal wurtzite structure, have very large piezoelectricity and spontaneous polarization, have very large polarized electric field along c-axis, this electric field can have a strong impact on the composite efficiency of luminescent device, emission wavelength is also unstable, therefore urgently needs the Material growth of non-polar plane.But often there is stacking fault and the dislocation of very high density in the gallium nitride film of the non-polar plane obtained, cause current gan non-polar plane device can't reach due requirement.The effect that the method being much used for improving c surface gallium nitride defect reported in document is applied in nonpolar a surface gallium nitride film is unsatisfactory.
The single crystal growing difficulty of gan, expensive, the growth of the iso-epitaxy of large-scale still cannot at present; Current growing gallium nitride epitaxial film still adopts hetero epitaxy mostly, and selected foreign substrate has Si, silicon carbide and sapphire.The advantages such as sapphire is because having Heat stability is good, and physical strength is high, does not absorb visible ray, and growing technology is comparatively ripe, moderate, are still best suited for the substrate of III-nitride growth at present.But due to some inferior positions of Sapphire Substrate itself, e.g., large with epitaxial film lattice mismatch and thermal mismatching, hardness is high, poorly conductive, and not easy of integration etc., therefore, in follow-up technique, sapphire existence is a problem that can not be ignored.Now the most frequently used stripping means with laser lift-off technique, Sapphire Substrate and GaN epitaxy sheet is peeled away in the position of buffer layer, and this method will accurately control optical maser wavelength and burst length, adds the difficulty of technique, too increases cost of manufacture.
Summary of the invention
(1) technical problem that will solve
High in order to overcome existing non-polar plane gan defect concentration, and the deficiency of the follow-up making devices complex process of process for sapphire-based gan, the invention provides a kind of InGaN of employing interposed layer and low temperature GaN buffer and grow method from peeling off a surface gallium nitride film on a sapphire substrate as weak bonded layer, adopt the method can obtain the good GaN monocrystal thin films of quality.
(2) technical scheme
For achieving the above object, the invention provides a kind of method growing self-stripping gallium nitride film on a sapphire substrate, the method utilize MOCVD device close using InGaN interposed layer and GaN low temperature buffer layer as weak bond in r surface sapphire substrate layer growth a surface gallium nitride from stripping film, specifically comprise the following steps:
Step 1: get a Sapphire Substrate;
Step 2: pass into ammonia in MOCVD device, carries out nitrogenize to Sapphire Substrate, generates one deck nitride layer thereon;
Step 3: utilize carrier gas to pass into indium source, gallium source and ammonia in MOCVD device, make to obtain InGaN layer on nitride layer;
Step 4: utilize carrier gas to pass into gallium source and ammonia in MOCVD device, growth one deck low temperature GaN buffer;
Step 5: utilize carrier gas to pass into gallium source and ammonia in MOCVD device, growing gallium nitride epitaxial film.
In such scheme, Sapphire Substrate described in step 1 and 2 is r surface sapphire substrate.
In such scheme, carrier gas described in step 3 to 5 is nitrogen or hydrogen.
In such scheme, described in step 3 during growing InGaN, the growth temperature in MOCVD device is set as 750 DEG C, and reaction chamber pressure controls at 200Torr, and the carrier gas flux in indium source and gallium source is set as 65SCCM and 10SCCM respectively, and growth time is 12 minutes.
In such scheme, during the GaN buffer layer of growing low temperature described in step 4, growth temperature in MOCVD device is set as 550 DEG C, reaction chamber pressure controls at 200Torr, the carrier gas flux in gallium source is set as 20SCCM, growth time is 3 minutes, is then warmed up to 1100 DEG C, and timing is annealed 5 minutes from during intensification.
In such scheme, the surface topography of the weak bonded layer of the LT-GaN/InGaN after annealing is strip.
In such scheme, during the epitaxial film of growing gallium nitride described in step 5, the growth temperature in MOCVD device is set as 1100 DEG C, and reaction chamber pressure controls at 50Torr, and gallium source carrier gas flux is set as 20SCCM.
In such scheme, the growth time of the epitaxial film of growing gallium nitride described in step 5 is 60 minutes.
In such scheme, the thickness of the epitaxial film of growing gallium nitride described in step 5 is about 1.2 μm.
(3) beneficial effect
The present invention, compared with traditional buffer layer technique, graph substrate technology, adopts InGaN interposed layer and low-temperature gan layer as weak bonded layer, has larger advantage.InGaN can decompose in the process of follow-up intensification, In discharges, the weak bonded layer (as shown in Figure 2) of strip is produced between Sapphire Substrate and GaN epitaxy film, the transversal epitaxial growth of GaN can be realized, in the temperature-fall period of epitaxial film after growth terminates, weak bond closes fault rupture, achieves certainly peeling off of monocrystalline high-quality GaN film.Weak bonded layer had both served release stress in process of growth, improved the effect of crystal mass; The automatic stripping of GaN epitaxy film is facilitated again in the process of cooling.The solid colour of the GaN film peeled off and monocrystalline GaN single-chip in the market.Compared with laser lift-off technique the most frequently used at present, this method is owing to automatically completing after the growth was completed, so technique is more simple, also eliminates the cost of laser lift-off equipment.
Accompanying drawing explanation
For further illustrating content of the present invention, below in conjunction with specific embodiment and accompanying drawing, the present invention is described in detail, wherein:
Fig. 1 is the succession schematic diagram growing self-stripping gallium nitride film on a sapphire substrate provided by the invention;
Fig. 2 is the structural representation of the self-stripping gallium nitride film grown on a sapphire substrate provided by the invention.
Embodiment
For making the object, technical solutions and advantages of the present invention clearly understand, below in conjunction with specific embodiment, and with reference to accompanying drawing, the present invention is described in more detail.
For now the most frequently used laser lift-off technique, Sapphire Substrate and GaN epitaxy sheet to accurately be controlled optical maser wavelength and burst length when the position of buffer layer is peeled away, increase the difficulty of technique, the problem of the cost of manufacture also increased, a surface gallium nitride provided by the invention is from stripping means, in the process of cooling after growth terminates, weak bonded layer can rupture, and high-quality gallium nitride epitaxial film strips down from Sapphire Substrate, has departed from Sapphire Substrate.Weak bonded layer serves release stress in process of growth, improves the effect of crystal mass; In the process of cooling, serve crucial effect again to the automatic stripping of GaN epitaxy film, this weak bonded layer is gordian technique place of the present invention.This invention is highly significant for the development of GaN thick film.As this invention being combined with HVPE, the self-stripping gallium nitride thick film of high crystalline quality will be grown.This will be the another quantum jump of field of semiconductor materials.
The present invention adopts using InGaN interposed layer and low temperature GaN buffer as weak bonded layer, this layer serves the effect of flexible substrate, not only very large release action is served to the stress in epitaxial film, crystal mass is greatly improved, growth technique is had more simple, the advantage easily realized compared with other laterally overgrown.
Key of the present invention is the problem solving the high-quality GaN film of Grown on Sapphire Substrates and epitaxial film stripping.As shown in Figure 1, process of growth comprises the following steps growth structure schematic diagram:
Step 1: get a substrate, this substrate is r (1012) surface sapphire;
Step 2: grow one deck InGaN interposed layer by MOCVD device over the substrate, to discharge the stress in follow-up extension GaN film.Growth temperature is set in 750 DEG C, and reaction chamber pressure controls at 200Torr, and growth time is 12 minutes, indium source, and gallium source carrier gas flux is set as 65SCCM, 10SCCM respectively, and the flow of ammonia is 3SLM;
Step 3: the low temperature GaN buffer of growth skim, growth temperature is set as 550 DEG C, and reaction chamber pressure controls at 200Torr, and growth time is 3min, and the flow in gallium source is 20SCCM, and the flow of ammonia is 3SLM;
Step 4: growing GaN epitaxial film, growth temperature is set as 1100 DEG C, and reaction chamber pressure controls at 50Torr, and growth time is 60min, and the flow in gallium source is 20SCCM, and the flow of ammonia is 0.8SLM.
GaN, as the outstanding a member in wide bandgap semiconductor photoelectric material of new generation, if successfully can prepare the nonpolar monocrystal thin films of high quality, will produce huge application prospect in optics field.But the preparation price of GaN monocrystalline in the market all costly, can not meet the needs of element manufacturing, can not meet large-scale isoepitaxial growth.In order to head it off, introduce in the present invention the weak bonded layer that is made up of InGaN interposed layer and low temperature GaN buffer to realize GaN epitaxy film from peeling off, except growth cost is low, outside technique is simple, the present invention have also been obtained the nonpolar a face GaN film of high quality from peeling off.The method must have very large using value in the actual production in future.
Above-described specific embodiment; object of the present invention, technical scheme and beneficial effect are further described; be understood that; the foregoing is only specific embodiments of the invention; be not limited to the present invention; within the spirit and principles in the present invention all, any amendment made, equivalent replacement, improvement etc., all should be included within protection scope of the present invention.
Claims (3)
1. one kind grows the method for self-stripping gallium nitride film on a sapphire substrate, it is characterized in that, the method utilize MOCVD device close using InGaN interposed layer and GaN low temperature buffer layer as weak bond in r surface sapphire substrate layer growth a surface gallium nitride from stripping film, specifically comprise:
Step 1: get a r surface sapphire substrate;
Step 2: pass into ammonia in MOCVD device, carries out nitrogenize to Sapphire Substrate, generates one deck nitride layer thereon;
Step 3: utilize carrier gas to pass into indium source, gallium source and ammonia in MOCVD device, make to obtain InGaN layer on nitride layer; During wherein said growing InGaN, the growth temperature in MOCVD device is set as 750 DEG C, and reaction chamber pressure controls at 200Torr, and the carrier gas flux in indium source and gallium source is set as 65SCCM and 10SCCM respectively, and growth time is 12 minutes;
Step 4: utilize carrier gas to pass into gallium source and ammonia in MOCVD device, growth one deck low temperature GaN buffer; During wherein said growing low temperature GaN buffer layer, the growth temperature in MOCVD device is set as 550 DEG C, and reaction chamber pressure controls at 200Torr, the carrier gas flux in gallium source is set as 20SCCM, growth time is 3 minutes, is then warmed up to 1100 DEG C, and timing is annealed 5 minutes from during intensification;
Step 5: utilize carrier gas to pass into gallium source and ammonia in MOCVD device, growing gallium nitride epitaxial film, in the temperature-fall period after epitaxy of gallium nitride layer growth completes, obtains a surface gallium nitride film from peeling off;
During the epitaxial film of growing gallium nitride described in step 5, the growth temperature in MOCVD device is set as 1100 DEG C, and reaction chamber pressure controls at 50Torr, and gallium source carrier gas flux is set as 20SCCM; The growth time of described growing gallium nitride epitaxial film is 60 minutes; The thickness of described growing gallium nitride epitaxial film is 1.2 μm.
2. the method growing self-stripping gallium nitride film on a sapphire substrate according to claim 1, it is characterized in that, carrier gas described in step 3 to 5 is nitrogen or hydrogen.
3. the method growing self-stripping gallium nitride film on a sapphire substrate according to claim 1, is characterized in that, the surface topography of the weak bonded layer of the LT-GaN/InGaN after annealing is strip.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201210325765.3A CN102839417B (en) | 2012-09-05 | 2012-09-05 | A kind of method growing self-stripping gallium nitride film on a sapphire substrate |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201210325765.3A CN102839417B (en) | 2012-09-05 | 2012-09-05 | A kind of method growing self-stripping gallium nitride film on a sapphire substrate |
Publications (2)
| Publication Number | Publication Date |
|---|---|
| CN102839417A CN102839417A (en) | 2012-12-26 |
| CN102839417B true CN102839417B (en) | 2015-09-09 |
Family
ID=47367126
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| CN201210325765.3A Expired - Fee Related CN102839417B (en) | 2012-09-05 | 2012-09-05 | A kind of method growing self-stripping gallium nitride film on a sapphire substrate |
Country Status (1)
| Country | Link |
|---|---|
| CN (1) | CN102839417B (en) |
Families Citing this family (7)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN103215647A (en) * | 2013-03-27 | 2013-07-24 | 上海萃智科技发展有限公司 | Non-polar a-side GaN film growth method |
| CN109728139A (en) * | 2019-02-20 | 2019-05-07 | 江苏晶曌半导体有限公司 | A kind of GaN epitaxy film and Sapphire Substrate are from stripping means |
| CN110429019B (en) * | 2019-06-24 | 2021-11-19 | 北京工业大学 | Epitaxial growth method for improving quality of nonpolar GaN material by inserting InGaN layer |
| CN111223763B (en) * | 2020-01-19 | 2024-04-12 | 镓特半导体科技（上海）有限公司 | Semiconductor structure, self-supporting gallium nitride layer and preparation method thereof |
| CN112233969A (en) * | 2020-10-21 | 2021-01-15 | 国网山东省电力公司电力科学研究院 | Method for preparing low-stress GaN film |
| CN113628953A (en) * | 2021-06-17 | 2021-11-09 | 中国电子科技集团公司第十三研究所 | Method for preparing nitride material and nitride semiconductor device |
| CN115036402B (en) * | 2022-08-12 | 2022-10-25 | 江苏第三代半导体研究院有限公司 | Induction-enhanced Micro-LED homoepitaxial structure and preparation method thereof |
Citations (6)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1996556A (en) * | 2006-12-01 | 2007-07-11 | 北京大学 | A method for preparing the gallium nitride single crystal wafer |
| CN101154570A (en) * | 2006-09-30 | 2008-04-02 | 中国科学院合肥物质科学研究院 | Preparation method of self-stripping gallium nitride substrate material |
| CN101364482A (en) * | 2008-09-19 | 2009-02-11 | 南京大学 | Visible light InGaN based photoelectrochemical cell and preparation |
| CN102220640A (en) * | 2011-06-09 | 2011-10-19 | 青岛铝镓光电半导体有限公司 | Preparation method of gallium nitride single crystal |
| CN102226985A (en) * | 2011-05-08 | 2011-10-26 | 北京大学 | Method for manufacturing GaN (gallium nitride) substrate |
| CN102244156A (en) * | 2011-06-16 | 2011-11-16 | 清华大学 | Epitaxial growth method of InGaN quantum dot and single photon source obtained thereby |
Family Cites Families (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| JPH088185A (en) * | 1994-06-15 | 1996-01-12 | Furukawa Electric Co Ltd:The | Multilayer structure and growth method of gan-based compound semiconductor thin film |
| KR101204029B1 (en) * | 2005-09-14 | 2012-11-27 | 삼성코닝정밀소재 주식회사 | Preparation of single crystalline gallium nitride thick film |
-
2012
- 2012-09-05 CN CN201210325765.3A patent/CN102839417B/en not_active Expired - Fee Related
Patent Citations (6)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101154570A (en) * | 2006-09-30 | 2008-04-02 | 中国科学院合肥物质科学研究院 | Preparation method of self-stripping gallium nitride substrate material |
| CN1996556A (en) * | 2006-12-01 | 2007-07-11 | 北京大学 | A method for preparing the gallium nitride single crystal wafer |
| CN101364482A (en) * | 2008-09-19 | 2009-02-11 | 南京大学 | Visible light InGaN based photoelectrochemical cell and preparation |
| CN102226985A (en) * | 2011-05-08 | 2011-10-26 | 北京大学 | Method for manufacturing GaN (gallium nitride) substrate |
| CN102220640A (en) * | 2011-06-09 | 2011-10-19 | 青岛铝镓光电半导体有限公司 | Preparation method of gallium nitride single crystal |
| CN102244156A (en) * | 2011-06-16 | 2011-11-16 | 清华大学 | Epitaxial growth method of InGaN quantum dot and single photon source obtained thereby |
Non-Patent Citations (1)
| Title |
|---|
| Growth of a-plane GaN on r-plane sapphire by self-patterned nanoscale epitaxial lateral overgrowth;zhiwei Li et al.;《Journal of Crystal Growth》;20120404;第348卷(第1期);参见对比文件1摘要，第2部分"Experiments"第1段 * |
Also Published As
| Publication number | Publication date |
|---|---|
| CN102839417A (en) | 2012-12-26 |
Similar Documents
| Publication | Publication Date | Title |
|---|---|---|
| CN102839417B (en) | A kind of method growing self-stripping gallium nitride film on a sapphire substrate | |
| JP3352712B2 (en) | Gallium nitride based semiconductor device and method of manufacturing the same | |
| CN100505165C (en) | A method for preparing the gallium nitride monocrystal substrate | |
| JP5679494B2 (en) | Nitride semiconductor structure and manufacturing method thereof | |
| US20200181799A1 (en) | Method for Preparing GaN Substrate Material | |
| US5923950A (en) | Method of manufacturing a semiconductor light-emitting device | |
| TWI744038B (en) | Epitaxy substrate with 2D material interposer and preparation method and production element | |
| EP2251464B1 (en) | Epitaxial substrate for semiconductor device, semiconductor device, and method of manufacturing epitaxial substrate for semiconductor device | |
| WO2020207234A1 (en) | Single crystal substrate using 2d-material epitaxy to eliminate defects, and fabricating method therefor and components thereof | |
| US20230343890A1 (en) | Epitaxial wafer for ultraviolet light emitting device, method for producing metal bonded substrate for ultraviolet light emitting device, method for producing ultraviolet light emitting device, and method for producing ultraviolet light emitting device array | |
| EP2802002B1 (en) | Method for the manufacturing of a substrate having a hetero-structure | |
| CN114242815A (en) | N-polarity GaN/AlGaN heterojunction epitaxial structure and preparation method thereof | |
| KR100583163B1 (en) | Nitride semiconductor and fabrication method for thereof | |
| JP7069584B2 (en) | Manufacturing method for board products | |
| CN100550302C (en) | A kind of III hi-nitride semiconductor material and growing method thereof | |
| CN105762061B (en) | Epitaxial growth method of nitride | |
| JPH11298039A (en) | Method of growing gan layer ad buffer layer and structure thereof | |
| US8048786B2 (en) | Method for fabricating single-crystalline substrate containing gallium nitride | |
| CN213150800U (en) | Aluminum nitride nucleation layer structure with nano interlayer | |
| CN212991102U (en) | Composite substrate structure | |
| US8026517B2 (en) | Semiconductor structures | |
| JP4333092B2 (en) | Manufacturing method of nitride semiconductor | |
| KR100834698B1 (en) | Method of forming gan layer and gan substrate manufactured using the same | |
| CN103094421A (en) | Method for improving quality of aluminumnitride (AlN) of face a by utilizing of aluminium nitride indium (AlInN) self-imaging pattern | |
| JP4099093B2 (en) | Nitride semiconductor growth method |
Legal Events
| Date | Code | Title | Description |
|---|---|---|---|
| C06 | Publication | ||
| PB01 | Publication | ||
| C10 | Entry into substantive examination | ||
| SE01 | Entry into force of request for substantive examination | ||
| C14 | Grant of patent or utility model | ||
| GR01 | Patent grant | ||
| CF01 | Termination of patent right due to non-payment of annual fee | ||
| CF01 | Termination of patent right due to non-payment of annual fee |
Granted publication date: 20150909 Termination date: 20160905 |