CN103498193A - Epitaxial growth method for improving crystal quality of material - Google Patents
Epitaxial growth method for improving crystal quality of material Download PDFInfo
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- CN103498193A CN103498193A CN201310446032.XA CN201310446032A CN103498193A CN 103498193 A CN103498193 A CN 103498193A CN 201310446032 A CN201310446032 A CN 201310446032A CN 103498193 A CN103498193 A CN 103498193A
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Abstract
The invention provides an improved epitaxial growth method and a structural design concept, which can greatly and stably improve the crystal quality of an epitaxial material and upgrade the efficiency of a luminescent material and a device. The epitaxial growth method is characterized in that transient growth is firstly performed twice in the early growth process, and the epitaxial growth method mainly comprises the following links: (1) introducing TMGa and NH3 into a reaction chamber in the heating process from 400 DEG C to 900 DEG C, performing epitaxial growth for a period of time, then stopping the introduction of the TMGa and the NH3 and further heating to a high temperature section; and (2) maintaining in the high temperature section for 10-300s, then re-introducing the TMGa and the NH3 and maintaining for 10-200s, and then stopping the introduction and continuously performing treatment in the high temperature section for 10-500s. The epitaxial growth is performed according to the method provided by the invention so as to be favorable to removing inherent mechanical damages on a substrate and a formed initial nucleation center by treatment; the subsequent epitaxial growth process is more favorable to nucleation and continuation of epitaxial growth and further realizes an obvious effect for improving the crystal quality of the material.
Description
Technical field
The invention belongs to material for optoelectronic devices preparation and structure-design technique field, relate generally to a kind of for improving the method for epitaxial material crystal mass.
Background technology
The LED epitaxial wafer refers at one and is heated to the specific monocrystal thin films grown on the substrate base (mainly containing sapphire, SiC, Si etc.) of proper temperature.The upstream link of epitaxial wafer in the LED industrial chain is semiconductor lighting industrial technology content link the highest, that the finished product quality, cost control are had the greatest impact.
The ultimate principle of LED epitaxial wafer growth is: upper at a substrate base (mainly containing sapphire and SiC, Si) that is heated to proper temperature, gaseous substance controlledly is transported to substrate surface, grows specific monocrystal thin films.
LED epitaxial wafer growing technology mainly adopts the Metalorganic chemical vapor deposition method at present.The growth of GaN material is at high temperature, the Ga decomposited by TMGa and NH
3chemical reaction realize, its reversible reaction equation is:
Ga+NH
3=GaN+3/2H
2
Growing GaN needs certain growth temperature, so also need certain NH
3dividing potential drop.
In traditional epitaxial growth technology, the processing of high temperature is first carried out in general all employings to substrate material, the buffer layer that drops to afterwards low-temperature epitaxy one deck low temperature carries out the high temperature anneal for buffer layer afterwards, again at the non-buffer layer of mixing of suitable temperature continued growth, the N-type layer of growing successively afterwards, quantum well layer, P type layer and contact layer.
Concrete early growth process mainly comprises following link:
(1) in reaction chamber, persistently overheating to high temperature section;
(2) maintain 20-800s in high temperature section;
(3) then, be cooled to gradually the growth temperature of buffer layer, start to continue to pass into NH
3, and pass into again the TMGa 120-250s that grown after 50-300s; Then stop passing into TMGa and start heating up, the section of reaching a high temperature is processed the GaN layer of having grown again.
The outer layer growth window of traditional epitaxy technique is very narrow, and the processing condition of layers of material growth need harsh control just can grow crystal mass epitaxial film preferably.
Summary of the invention
The present invention is based on current luminescent device Material growth and structure design, proposed a kind of improved epitaxial growth method and Structural design idea, can significantly stablize the efficiency that improves the epitaxial material crystal mass and promote luminescent material and device.
The solution of the present invention is as follows:
A kind of epitaxial growth method that improves the material crystals quality, be characterized in, the early growth process mainly comprises following link:
(1), in reaction chamber, in 400 degree to 900 degree temperature-rise periods, pass into TMGa and NH
3, carry out epitaxy for some time, then stop passing into the TMGa(trimethyl-gallium) and NH
3, continue to be warming up to high temperature section.Here, not require to start to pass into gas until 900 degree from 400 degree, but emphasize first in this calefactive interzone (arbitrary period), carry out once " passing into TMGa and NH
3".
(2), after high temperature section maintains 10-300s, again pass into TMGa and NH
3and maintain 10-200s; Then stop passing into, continue to process 10-500s in high temperature section.
(3) then, be cooled to gradually the growth temperature of buffer layer, start to continue to pass into NH
3, and pass into again the TMGa 120-250s that grown after 50-300s; Then stop passing into TMGa and start heating up, the section of reaching a high temperature is processed the GaN layer of having grown again.
Above-mentioned (3) link, in fact identical in the technique in relevant temperature stage with traditional scheme, and after, also still can complete successively the links such as follow-up epitaxy 3D and uGaN according to traditional scheme, finally make epitaxial wafer.
Based on above-mentioned general planning, the present invention also further does following optimization and limits and improve:
In order to obtain good crystal mass and to strengthen the epitaxy technique window, above step (1)-(3) can be repeated 1-10 time, better for the raising effect of crystal mass, but can increase the extra process time; Therefore preferred 2-3 time.
In (1) link, pass into TMGa and NH
3the optimum temps interval be the 450-850 degree, the time length is respectively 30-150 second;
In (2) link, pass into TMGa and NH
3the optimum temps interval be the 1020-1090 degree, the time length is respectively 25-75 second.
The present invention has the following advantages:
According to the solution of the present invention, carried out the of short duration epitaxy of 2 times in low-temperature zone and high temperature section respectively before original buffer growth, so be conducive to dispose the intrinsic physical abuse of substrate and the nucleation centre at the initial stage of formation, and more be conducive to the continuation of nucleation and extension in follow-up epitaxial process, improve and played obvious effect for the crystal mass of material.
The present invention is optimized improvement by the processing condition to before buffer growth, widened epitaxially grown process window, under the condition that does not increase additional technical steps and time, significantly promoted the epitaxially grown crystal mass of different substrate materials, to obvious the change greatly of selection remaining of substrate selection and technological temperature.Technique and substrate material for large quantities of volume productions are selected to provide good growth basis, have met the needs of current scale operation, can obtain high-quality epitaxial material by this technology, and then promote the device efficiency of material.
The accompanying drawing explanation
The schematic diagram that Fig. 1 is the conventional epitaxial growth method.
Fig. 2 is principle schematic of the present invention.
Embodiment
Principal feature of the present invention is in the early growth process, first carries out the of short duration epitaxy of twice, in rising to the process of pyroprocessing, opens TMGa and NH
3carry out closing after epitaxy for some time, again open TMGa and NH after carrying out for some time in the pyroprocessing stage
3carry out closing after epitaxy for some time, keep afterwards pyroprocessing to continue follow-up buffer layer after for some time, 3D layer and uGaN layer growth get final product.
The solution of the present invention can be applicable to existing various saphire substrate material, below provides several specific embodiments and experimental verification, and the present invention is further described.
Certainly; the solution of the present invention thinking also can be used in other substrate materials as silicon substrate; in the epitaxy of silicon carbide substrates etc., before traditional buffer growth, carry out twice or the epitaxy of above differing temps and carry out follow-up pyroprocessing after continue again the traditional technology growth thinking all belong to protection category of the present invention.
Embodiment mono-
Use the sapphire plane substrate to carry out simultaneous test.
At first use traditional LED technique to carry out epitaxy, that is:
In reaction chamber, begin to warm to 1050 degree from room temperature, heat-up rate is 1.5 degree/second, after 1050 degree high temperature section maintain 435s, is cooled to gradually growth temperature 530 degree of buffer layer, starts to continue to pass into NH
3, and pass into again the TMGa 150s that grown after 120s; Then stop passing into TMGa and begin to warm to 1020 degree, the section of reaching a high temperature is processed the GaN layer of having grown again.
The LED function layers such as follow-up 3D, the U GaN of continued growth afterwards, N GaN, MQW, P GaN get final product; Growth finishes to carry out the XRD test for the LED structure, and (002) (102) crystal face half-breadth is 370arcsec and 413arcsec.
Afterwards, use identical substrate and MOCVD board to carry out simultaneous test.
In reaction chamber, begin to warm to 1050 degree from room temperature, heat-up rate is 1.5 degree/second, when temperature arrival 500 is spent, passes into TMGa and NH
3carry out epitaxy, when temperature reaches 650, close TMGa and NH while spending
3, logical reactant TMGa and NH
3about 100s of time; Then stop passing into the TMGa(trimethyl-gallium) and NH
3, continue to be warming up to high temperature section 1050 degree;
After 1050 degree high temperature section maintain 150s, again pass into TMGa and NH
3and maintain 35s; Then stop passing into reactant, continue to process 250s in high temperature section;
Then, be cooled to gradually growth temperature 530 degree of buffer layer, start to continue to pass into NH
3, and pass into again the TMGa 150s that grown after 120s; Then stop passing into TMGa and begin to warm to 1020 degree, the section of reaching a high temperature is processed the GaN layer of having grown again.
The LED function layers such as follow-up 3D, the U GaN of continued growth afterwards, N GaN, MQW, P GaN get final product; Growth finishes to carry out the XRD test for the LED structure, and (002) (102) crystal face half-breadth is 230arcsec and 249arcsec.
Simultaneously for the structure of growth LED under two kinds of conditions, carry out the photoelectric properties test, after assay optimization under LED structure 20mA brightness risen to 70unit by 50unit, promote 40%; The percent of pass that simultaneously leaks electricity has risen to more than 95% by original 75%;
Embodiment bis-
Use A producer and the patterned Sapphire Substrate of B producer to carry out simultaneous test.
At first use traditional LED technique to carry out epitaxy to the patterned Sapphire Substrate of A producer and B producer, that is:
In reaction chamber, begin to warm to 1050 degree from room temperature, heat-up rate is 1.5 degree/second, after 1050 degree high temperature section maintain 435s, is cooled to gradually growth temperature 530 degree of buffer layer, starts to continue to pass into NH
3, and pass into again the TMGa 150s that grown after 120s; Then stop passing into TMGa and begin to warm to 1020 degree, the section of reaching a high temperature is processed the GaN layer of having grown again.
The LED function layers such as follow-up 3D, the U GaN of continued growth afterwards, N GaN, MQW, P GaN get final product; Growth finishes to carry out the XRD test for the LED structure, and (002) (102) crystal face half-breadth of A producer substrate epitaxial is 370arcsec and 350arcsec.(002) (102) crystal face half-breadth of B producer substrate epitaxial is 570arcsec and 600arcsec, and the extension outward appearance of B producer is class polycrystalline shape;
Afterwards, use the A producer patterned Sapphire Substrate identical with B producer and identical MOCVD board to carry out simultaneous test.
In reaction chamber, begin to warm to 1060 degree from room temperature, heat-up rate is 1.6 degree/second, when temperature arrival 520 is spent, passes into TMGa and NH
3carry out epitaxy, when temperature reaches 600, close TMGa and NH while spending
3, logical reactant TMGa and NH
3about 50s of time; Then stop passing into the TMGa(trimethyl-gallium) and NH
3, continue to be warming up to high temperature section 1060 degree;
After 1050 degree high temperature section maintain 150s, again pass into TMGa and NH
3and maintain 45s; Then stop passing into reactant, continue to process 275s in high temperature section;
Then, be cooled to gradually growth temperature 530 degree of buffer layer, start to continue to pass into NH
3, and pass into again the TMGa 150s that grown after 120s; Then stop passing into TMGa and begin to warm to 1020 degree, the section of reaching a high temperature is processed the GaN layer of having grown again.
The LED function layers such as follow-up 3D, the U GaN of continued growth afterwards, N GaN, MQW, P GaN get final product; Growth finishes to carry out the XRD test for the LED structure, and (002) (102) crystal face half-breadth of A producer substrate epitaxial is 250arcsec and 243arcsec.(002) (102) crystal face half-breadth of B producer substrate epitaxial is 249arcsec and 237arcsec, and epitaxial surface is all smooth smooth;
Simultaneously for the structure of growth LED under two kinds of conditions, carry out the photoelectric properties test, after assay optimization under LED structure 20mA brightness risen to 90unit/85unit by 75unit/35unit, promoted respectively 20% and 140%; The percent of pass that simultaneously leaks electricity has risen to respectively more than 95% by original 85%/15%;
From above-described embodiment, can find out, the present invention, by carried out the process optimization processing before buffer layer, for different substrate materials, all can still make crystalline material possess higher quality, and promote the efficiency of luminescent material and device when stable mass production.
Processing by present method, can make the crystal mass of GaN material increase substantially, use the epitaxial film of different substrate materials growth, (102) (002) crystal face halfwidth all has by original 500-700arcsec and is reduced to below 250arcses, the smooth smooth zero defect of epi-layer surface.
Claims (5)
1. an epitaxial growth method that improves the material crystals quality, it is characterized in that: its early growth process mainly comprises following link:
(1), in reaction chamber, in 400 degree to 900 degree temperature-rise periods, pass into TMGa and NH
3, carry out epitaxy for some time, then stop passing into TMGa and NH
3, continue to be warming up to high temperature section;
(2), after high temperature section maintains 10-300s, again pass into TMGa and NH
3and maintain 10-200s; Then stop passing into, continue to process 10-500s in high temperature section;
(3) then, be cooled to gradually the growth temperature of buffer layer, start to continue to pass into NH
3, and pass into again the TMGa 120-250s that grown after 50-300s; Then stop passing into TMGa and start heating up, the section of reaching a high temperature is processed the GaN layer of having grown again.
2. epitaxial growth method according to claim 1, is characterized in that: this early growth process repetition 1-10 time.
3. epitaxial growth method according to claim 2, is characterized in that: in (1) link, pass into TMGa and NH
3temperature range be the 450-850 degree, the time length is respectively 30-150 second; In (2) link, pass into TMGa and NH
3temperature range be the 1020-1090 degree, the time length is respectively 25-75 second.
4. epitaxial growth method according to claim 3, is characterized in that, this epitaxial growth method is based on the sapphire plane substrate to carry out:
In reaction chamber, begin to warm to 1050 degree from room temperature, heat-up rate is 1.5 degree/second, when temperature arrival 500 is spent, passes into TMGa and NH
3carry out epitaxy, when temperature reaches 650, close TMGa and NH while spending
3; Then continue to be warming up to high temperature section 1050 degree;
After 1050 degree high temperature section maintain 150s, again pass into TMGa and NH
3and maintain 35s; Then stop passing into TMGa and NH
3, continue to process 250s in high temperature section;
Then, be cooled to gradually growth temperature 530 degree of buffer layer, start to continue to pass into NH
3, and pass into again the TMGa 150s that grown after 120s; Then stop passing into TMGa and begin to warm to 1020 degree, the section of reaching a high temperature is processed the GaN layer of having grown again.
5. epitaxial growth method according to claim 3, is characterized in that, this epitaxial growth method is based on patterned Sapphire Substrate to carry out:
In reaction chamber, begin to warm to 1060 degree from room temperature, heat-up rate is 1.6 degree/second, when temperature arrival 520 is spent, passes into TMGa and NH
3carry out epitaxy, when temperature reaches 600, close TMGa and NH while spending
3; Then continue to be warming up to high temperature section 1060 degree;
After 1050 degree high temperature section maintain 150s, again pass into TMGa and NH
3and maintain 45s; Then stop passing into TMGa and NH
3, continue to process 275s in high temperature section;
Then, be cooled to gradually growth temperature 530 degree of buffer layer, start to continue to pass into NH
3, and pass into again the TMGa 150s that grown after 120s; Then stop passing into TMGa and begin to warm to 1020 degree, the section of reaching a high temperature is processed the GaN layer of having grown again.
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Cited By (6)
| Publication number | Priority date | Publication date | Assignee | Title |
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| CN104790030A (en) * | 2015-03-30 | 2015-07-22 | 苏州新纳晶光电有限公司 | Method for improving GaN epitaxial yield after MOCVD outage |
| CN105719946A (en) * | 2014-12-03 | 2016-06-29 | 广东昭信半导体装备制造有限公司 | GaN composite substrate preparation method |
| CN106206869A (en) * | 2016-07-25 | 2016-12-07 | 华灿光电（浙江）有限公司 | Growth method of GaN-based light emitting diode epitaxial wafer |
| CN106229397A (en) * | 2016-07-25 | 2016-12-14 | 华灿光电（浙江）有限公司 | Growth method of light-emitting diode epitaxial wafer |
| CN107887255A (en) * | 2017-09-18 | 2018-04-06 | 中国电子科技集团公司第五十五研究所 | A kind of method of high resistant GaN film epitaxial growth |
| CN111952419A (en) * | 2020-06-30 | 2020-11-17 | 华灿光电（浙江）有限公司 | Preparation method of light-emitting diode epitaxial wafer |
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| CN111952419B (en) * | 2020-06-30 | 2021-11-05 | 华灿光电（浙江）有限公司 | Preparation method of light-emitting diode epitaxial wafer |
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