CN101148776A - Epitaxy growth method for gallium antimonide on gallium arsenide substrate - Google Patents
Epitaxy growth method for gallium antimonide on gallium arsenide substrate Download PDFInfo
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- CN101148776A CN101148776A CNA2006101522019A CN200610152201A CN101148776A CN 101148776 A CN101148776 A CN 101148776A CN A2006101522019 A CNA2006101522019 A CN A2006101522019A CN 200610152201 A CN200610152201 A CN 200610152201A CN 101148776 A CN101148776 A CN 101148776A
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Abstract
The process of epitaxially growing GaSb on GaAs substrate is one double buffering layer growing process including the following steps: 1. growing a buffering GaAs layer on GaAs substrate at 580 deg.c; 2. growing a buffering AlSb layer on the buffering GaAs layer at 550 deg.c; and 3. growing an epitaxial GaSb layer on the buffering AlSb layer at 400-500 deg.c. The double buffering layer growing process can promote the 2D growth of the epitaxial GaSb layer, and raise the crystal quality and surface smoothness of the epitaxial GaSb layer effectively.
Description
Technical field
The present invention relates to gallium antimonide (GaSb) crystal epitaxy technical field, relate in particular to the method for a kind of employing double-buffering layer growth technique epitaxy GaSb on gallium arsenide (GaAs) substrate.
Background technology
(lattice parameter is the InAs of 6.1 to the GaSb base semiconductor material, GaSb, AlSb and ternary compound thereof), in optical characteristics still is the shortcoming that has all well remedied conventional semiconductor material aspect the electrology characteristic, be preparation high speed, lower powered electron device---the first-selected type material of High Electron Mobility Transistor (HEMT) or mid and far infrared detector and laser apparatus (InAs/GaSb, superlattice infrared eye and laser apparatus).
Though the commercialization of GaSb single-chip owing to there is the cost height, lacks shortcomings such as semi-insulating substrate, so people prepare the GaSb epitaxial film usually on the GaAs substrate.And in the hetero epitaxy process, problem of ubiquity is to have about 7% lattice mismatch and coefficient of thermal expansion mismatch between GaAs substrate and the GaSb epitaxial film, and this GaSb crystal for growing high-quality is a big obstacle.
Current, generally adopt buffer layer technology to alleviate lattice mismatch and thermal mismatching between substrate and the epitaxial film in the world.For the present common method of GaSb extension is high growth temperature GaAs buffer layer on the GaAs substrate, reduces underlayer temperature, at GaAs buffer layer direct growth GaSb epitaxial film, belongs to single buffer layer technology.But have following shortcoming: owing to have about 7% lattice mismatch between GaAs substrate and the GaSb epitaxial film, cause GaSb with three-dimensional island growth, the GaSb material surface that obtains is coarse, and dislocation desity is big, and crystal mass is poor.
And the effect of aluminium antimonide (AlSb) buffer layer is: (1) serves as surfactant, reduced the interfacial free energy between substrate and the epitaxial film, (2) served as an effect of considering plate, suppressed the breeding of dislocation, this does buffer layer with aluminium nitride (AlN) during to growing gallium nitride (GaN) similar reason.
Therefore, how changing single buffer layer technology, make its characteristic that promotes the epitaxial film two-dimensional growth, thereby improve the crystal mass and the surface finish of epitaxial film, is the prerequisite that grows high-quality GaSb layer on the GaAs substrate.
Summary of the invention
(1) technical problem that will solve
In view of this, main purpose of the present invention be to provide a kind of on the GaAs substrate method of epitaxy GaSb, to improve the crystal mass and the surface finish of epitaxial film.
(2) technical scheme
For achieving the above object, technical scheme of the present invention is achieved in that
A kind of on gallium arsenide GaAs substrate the method for epitaxy gallium antimonide GaSb, this method adopts double-buffering layer growth technique, specifically comprises:
A, the GaAs buffer layer of under 580 ℃ of conditions, on the GaAs substrate, growing;
B, the aluminium antimonide AlSb buffer layer of on the GaAs buffer layer of growing under 550 ℃ of conditions, growing;
C, the GaSb epitaxial film of on the AlSb buffer layer of growing under 400 to 500 ℃ of conditions, growing.
Further comprise before the described steps A:
Cleaned GaAs substrate is placed on the molecular beam epitaxy MBE growth room specimen holder, high temperature deoxidation under 580 ℃ of conditions, and the GaAs underlayer temperature risen to 630 ℃ of high-temperature degassing, underlayer temperature is reduced to 580 ℃ then.
Described MBE growth room is in high vacuum state before GaAs and AlSb buffer growth, pressure is 5 * 10
-9Mbar;
Described MBE growth room is in GaAs and AlSb buffer growth process, and growth room's pressure is in 5 * 10
-8The mbar scope;
Described MBE growth room is when the GaSb outer layer growth, and growth room's pressure is in 8 * 10
-8The mbar scope.
Described steps A comprises: the GaAs substrate equilibrium temperature after the high temperature deoxidation at 580 ℃, is opened Ga source stove shutter, growth GaAs buffer layer on the GaAs substrate.
The temperature of described Ga source when the GaAs buffer growth is 1150 ℃.
The As/Ga line ratio of described GaAs buffer layer when growth is 20, and growth time is 30 minutes, and growth thickness is 0.5 μ m.
Described step B comprises: close Ga source stove shutter, the GaAs underlayer temperature is reduced to 550 ℃, close As source stove shutter, and open Sb source stove shutter and Al source stove shutter, growth AlSb buffer layer on the GaAs buffer layer.
The temperature of described Al source when the AlSb buffer growth is 1180 ℃.
The Al/Sb line ratio of described AlSb buffer layer when growth is 6, and growth time is 12 minutes, and growth thickness is 100nm.
Described step C comprises: close Al source stove shutter, the GaAs underlayer temperature is dropped to 400 to 500 ℃, open Ga source stove shutter, growth GaSb epitaxial film on the AlSb buffer layer.
(3) beneficial effect
From technique scheme as can be seen, the present invention has following beneficial effect:
1, utilizes the present invention, with single buffer layer process reform is double buffer layer process, elder generation is growth GaAs buffer layer on the GaAs substrate, growth AlSb buffer layer on the GaAs buffer layer of growth then, the last GaSb epitaxial film of on the AlSb buffer layer of growth, growing, make its characteristic that promotes the epitaxial film two-dimensional growth, thereby effectively improved the crystal mass and the surface finish of GaSb epitaxial film.
2, the present invention adopts the method for double-buffering layer growth technique epitaxy GaSb on the GaAs substrate, compare with single buffer layer, the epitaxy of carrying out after double-buffering layer growth is finished has formed two-dimensional growth preferably, and the surfaceness of GaSb epitaxial film has had obviously and reduces.
3, the present invention adopts the method for double-buffering layer growth technique epitaxy GaSb on the GaAs substrate, compare with single buffer layer, the halfwidth (FWHM) that the outer GaSb that obtains prolongs twin crystal X-ray diffraction (DCXRD) rocking curve of layer further reduces, and double buffer layer process has significant promoter action to the crystalline quality of epitaxial film.
4, the present invention adopts the method for double-buffering layer growth technique epitaxy GaSb on the GaAs substrate, the GaSb epitaxial film of acquisition, and not only surface finish has had further raising, and the dislocation desity of epitaxial film also obviously descends.Compare with single buffer layer, thereby double-buffering layer has not only formed the surface finish that better two-dimensional growth provides epitaxial film, and its crystallization nucleation and alleviate lattice mismatch and the effect of thermal mismatching has also obviously obtained reinforcement, thereby further reduced the dislocation desity of epitaxial film.
Description of drawings
Fig. 1 is the method flow diagram of the GaSb epitaxial film of growing on the GaAs substrate provided by the invention;
Fig. 2 is the growth structure synoptic diagram of the GaSb epitaxial film of growing on the GaAs substrate provided by the invention;
Fig. 3-1 is the atomic force microscope surface topography map of the GaSb epitaxial film of the single buffer layer technology growth of employing;
Fig. 3-2 is the atomic force microscope surface topography map of the GaSb epitaxial film of employing double buffer layer process growth;
Fig. 4 is the DCXRD rocking curve of GaSb epitaxial film, and wherein curve A is the DCXRD rocking curve of the GaSb epitaxial film of the single buffer layer technology growth of employing, and its halfwidth is 385.4arcsec (second of arc); Curve B is the DCXRD rocking curve of the GaSb epitaxial film of employing double buffer layer process growth, and its halfwidth is 140.5arcsec (second of arc).
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.
As shown in Figure 1, Fig. 1 is the method flow diagram of the GaSb epitaxial film of growing on the GaAs substrate provided by the invention, and this method adopts double-buffering layer growth technique, specifically may further comprise the steps:
Step 101: the GaAs buffer layer of under 580 ℃ of conditions, on the GaAs substrate, growing;
Step 102: at the AlSb buffer layer of on the GaAs buffer layer of growth, growing under 550 ℃ of conditions;
Step 103: at the GaSb epitaxial film of on the AlSb buffer layer of growth, growing under 400 to 500 ℃ of conditions.
Further comprise before the above-mentioned steps 101: cleaned GaAs substrate is placed on the MBE growth room specimen holder, high temperature deoxidation under 580 ℃ of conditions, and the GaAs underlayer temperature risen to 630 ℃ of high-temperature degassing, underlayer temperature is reduced to 580 ℃ then.
Described MBE growth room is in high vacuum state before GaAs and AlSb buffer growth, pressure is 5 * 10
-9Mbar; Described MBE growth room is in GaAs and AlSb buffer growth process, and growth room's pressure is in 5 * 10
-8The mbar scope; Described MBE growth room is when the GaSb outer layer growth, and growth room's pressure is in 8 * 10
-8The mbar scope.
Above-mentioned steps 101 comprises: the GaAs substrate equilibrium temperature after the high temperature deoxidation at 580 ℃, is opened Ga source stove shutter, growth GaAs buffer layer on the GaAs substrate.The temperature of described Ga source when the GaAs buffer growth is 1150 ℃.The As/Ga line ratio of described GaAs buffer layer when growth is 20, and growth time is 30 minutes, and growth thickness is 0.5 μ m.
Above-mentioned steps 102 comprises: close Ga source stove shutter, the GaAs underlayer temperature is reduced to 550 ℃, close As source stove shutter, and open Sb source stove shutter and Al source stove shutter, growth AlSb buffer layer on the GaAs buffer layer.The temperature of described Al source when the AlSb buffer growth is 1180 ℃.The Al/Sb line ratio of described AlSb buffer layer when growth is 6, and growth time is 12 minutes, and growth thickness is 100nm.
Above-mentioned steps 103 comprises: close Al source stove shutter, the GaAs underlayer temperature is dropped to 400 to 500 ℃, open Ga source stove shutter, growth GaSb epitaxial film on the AlSb buffer layer.
Method flow diagram based on the GaSb epitaxial film of on the GaAs substrate, growing shown in Figure 1, Fig. 2 shows the growth structure synoptic diagram of the GaSb epitaxial film of growing provided by the invention on the GaAs substrate, Fig. 3-1 shows the atomic force microscope surface topography map of the GaSb epitaxial film that adopts single buffer layer technology growth, and Fig. 3-2 shows the atomic force microscope surface topography map of the GaSb epitaxial film that adopts the double buffer layer process growth.
Compare with single buffer layer, the epitaxy of carrying out after double-buffering layer growth is finished has formed two-dimensional growth preferably, and showing as surfaceness has had obviously and reduce.Fig. 3-1 shows the atomic force microscope surface topography map of the GaSb epitaxial film that adopts single buffer layer technology growth, and the rootmean-square surfaceness is 1.74 , and concave-convex surface shows tangible three dimensional growth feature.Fig. 3-2 shows the atomic force microscope surface topography map of the GaSb epitaxial film that adopts the double buffer layer process growth, has an even surface, and can see atomic steps clearly, and the rootmean-square surfaceness is 1.07 , and more single buffer layer is greatly improved.
From Fig. 3-1 and Fig. 3-2 as can be seen, the planeness on the epitaxial film GaSb surface that double buffer layer process obtains further improves, and the surface topography of Fig. 3-1 and Fig. 3-2 has than big-difference, the epitaxial film GaSb surface that shows as the single buffer layer of Fig. 3-1 use exists tangible screw dislocation hole and screw dislocation boundary line, shows the epitaxial film GaSb height of its dislocation desity than Fig. 3-2 double-buffering layer.
In addition, compare with single buffer layer, the epitaxial film GaSb that adopts double buffer layer process to obtain, the halfwidth (FWHM) of its twin crystal X-ray diffraction (DCXRD) rocking curve further reduces, and shows that double buffer layer process has significant promoter action to the crystalline quality of epitaxial film.Fig. 4 shows the DCXRD rocking curve of GaSb epitaxial film, and wherein curve A is the DCXRD rocking curve of the GaSb epitaxial film of the single buffer layer technology growth of employing, and its halfwidth is 385.4arcsec (second of arc); Curve B is the DCXRD rocking curve of the GaSb epitaxial film of employing double buffer layer process growth, and its halfwidth is 140.5arcsec (second of arc).
Therefore, grow with two-dimensional approach in order to make epitaxial film, obtain even curface, effective means is to change current single buffer growth technology of generally using, and the new approaches of proposition double buffer layer process, both under higher temperature growth regulation one deck buffer layer to obtain better crystallization nucleation substrate, growth second layer buffer layer holds big lattice mismatch under low slightly temperature then, obtaining accurate preferably two-dimensional growth plane, so that provide better growth substrate for the GaSb epitaxial film that obtains atomically flating.
Below in conjunction with specific embodiment method of growing the GaSb epitaxial film on the GaAs substrate provided by the invention is further described.
Embodiment 1
After the GaAs substrate that cleans up is carried out high temperature deoxidation and degasification, the GaAs underlayer temperature is dropped to 580 ℃, open Ga source stove shutter, 1150 ℃ of Ga source temperatures carry out the crystalline growth of GaAs high temperature buffer layer on the GaAs substrate.The growth time of GaAs buffer layer 30 minutes, thickness 0.5 μ m.
Close Ga source stove shutter then, underlayer temperature is reduced to about 550 ℃, close As source stove shutter, open Sb source stove shutter, open Al source stove shutter, 1180 ℃ of Al source temperatures, growing low temperature AlSb buffer layer on the GaAs buffer layer, growth time 12 minutes, thickness is about 100nm.
Close Al source stove shutter then, underlayer temperature drops to 500 ℃, opens Ga source stove shutter, carries out the growth of epitaxial film GaSb on the AlSb buffer layer, and the surface finish of gained GaSb epitaxial film further provides, and dislocation desity also significantly reduces.
Embodiment 2,3
The outer layer growth temperature of lesser temps is respectively 460 ℃, 480 ℃, and all the other are with embodiment 1, and the value of a half width that surfaceness that atomic force microscope is measured and DCXRD rocking curve are measured is listed in table 1.
| Embodiment | The double-buffering layer underlayer temperature | The outer layer growth underlayer temperature | AFM(2×2μm 2) | DCXRD | |
| The GaAs buffer layer | The AlSb buffer layer | RMS(nm) | FWHM(arcsec) | ||
| 1 | 580℃ | 550℃ | 500℃ | 1.11 | 59.8 |
| 2 | 580℃ | 550℃ | 460℃ | 1.38 | 94.5 |
| 3 | 580℃ | 550℃ | 480℃ | 1.26 | 76.1 |
Table 1
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 being made, be equal to replacement, improvement etc., all should be included within protection scope of the present invention.
Claims (10)
1. the method for an epitaxy gallium antimonide GaSb on gallium arsenide GaAs substrate is characterized in that, this method adopts the double-buffering layer growth technique, and this method specifically comprises:
A, the GaAs buffer layer of under 580 ℃ of conditions, on the GaAs substrate, growing;
B, the aluminium antimonide AlSb buffer layer of on the GaAs buffer layer of growing under 550 ℃ of conditions, growing;
C, the GaSb epitaxial film of on the AlSb buffer layer of growing under 400 to 500 ℃ of conditions, growing.
2. according to claim 1 on the GaAs substrate method of epitaxy GaSb, it is characterized in that, further comprise before the described steps A:
Cleaned GaAs substrate is placed on the molecular beam epitaxy MBE growth room specimen holder, high temperature deoxidation under 580 ℃ of conditions, and the GaAs underlayer temperature risen to 630 ℃ of high-temperature degassing, underlayer temperature is reduced to 580 ℃ then.
3. according to claim 2 on the GaAs substrate method of epitaxy GaSb, it is characterized in that,
Described MBE growth room is in high vacuum state before GaAs and AlSb buffer growth, pressure is 5 * 10
-9Mbar;
Described MBE growth room is in GaAs and AlSb buffer growth process, and growth room's pressure is in 5 * 10
-8The mbar scope;
Described MBE growth room is when the GaSb outer layer growth, and growth room's pressure is in 8 * 10
-8The mbar scope.
4. according to claim 2 on the GaAs substrate method of epitaxy GaSb, it is characterized in that described steps A comprises:
GaAs substrate equilibrium temperature after the high temperature deoxidation at 580 ℃, is opened Ga source stove shutter, growth GaAs buffer layer on the GaAs substrate.
5. according to claim 4 on the GaAs substrate method of epitaxy GaSb, it is characterized in that the temperature of described Ga source when the GaAs buffer growth is 1150 ℃.
6. according to claim 4 on the GaAs substrate method of epitaxy GaSb, it is characterized in that the As/Ga line ratio of described GaAs buffer layer when growth is 20, growth time is 30 minutes, growth thickness is 0.5 μ m.
According to claim 1 or 4 described on the GaAs substrate method of epitaxy GaSb, it is characterized in that described step B comprises:
Close Ga source stove shutter, the GaAs underlayer temperature is reduced to 550 ℃, close As source stove shutter, and open Sb source stove shutter and Al source stove shutter, growth AlSb buffer layer on the GaAs buffer layer.
8. according to claim 7 on the GaAs substrate method of epitaxy GaSb, it is characterized in that the temperature of described Al source when the AlSb buffer growth is 1180 ℃.
9. according to claim 7 on the GaAs substrate method of epitaxy GaSb, it is characterized in that the Al/Sb line ratio of described AlSb buffer layer when growth is 6, growth time is 12 minutes, growth thickness is 100nm.
10. according to claim 7 on the GaAs substrate method of epitaxy GaSb, it is characterized in that described step C comprises:
Close Al source stove shutter, the GaAs underlayer temperature is dropped to 400 to 500 ℃, open Ga source stove shutter, growth GaSb epitaxial film on the AlSb buffer layer.
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| CN104409463A (en) * | 2014-11-09 | 2015-03-11 | 北京工业大学 | Optical detector for modulating channel current based on HEMT (High Electron Mobility Transistor) structure |
| CN106298577A (en) * | 2016-10-18 | 2017-01-04 | 中国工程物理研究院激光聚变研究中心 | A kind of method of monocrystal thin films sedimentation rate on-line determination and application |
| RU2623832C1 (en) * | 2016-04-27 | 2017-06-29 | Федеральное государственное бюджетное учреждение науки Научно-технологический центр микроэлектроники и субмикронных гетероструктур Российской академии наук (НТЦ микроэлектроники РАН) | Method of obtaining antimonide gallium with a large specific electrical resistance |
| CN107634000A (en) * | 2013-02-15 | 2018-01-26 | 弗赖贝格化合物原料有限公司 | Method, gallium arsenide substrate for preparing gallium arsenide substrate and application thereof |
| CN110246754A (en) * | 2019-06-20 | 2019-09-17 | 江苏能华微电子科技发展有限公司 | A kind of preparation method and epitaxial structure of HEMT epitaxial structure |
| CN113823551A (en) * | 2020-06-19 | 2021-12-21 | 中国科学院半导体研究所 | Method for growing GaSb epitaxial wafer on GaAs substrate and GaAs-based substrate |
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- 2006-09-18 CN CNA2006101522019A patent/CN101148776A/en active Pending
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| CN107634000A (en) * | 2013-02-15 | 2018-01-26 | 弗赖贝格化合物原料有限公司 | Method, gallium arsenide substrate for preparing gallium arsenide substrate and application thereof |
| CN107634000B (en) * | 2013-02-15 | 2022-09-23 | 弗赖贝格化合物原料有限公司 | Method for producing a gallium arsenide substrate, gallium arsenide substrate and use thereof |
| CN104409463A (en) * | 2014-11-09 | 2015-03-11 | 北京工业大学 | Optical detector for modulating channel current based on HEMT (High Electron Mobility Transistor) structure |
| RU2623832C1 (en) * | 2016-04-27 | 2017-06-29 | Федеральное государственное бюджетное учреждение науки Научно-технологический центр микроэлектроники и субмикронных гетероструктур Российской академии наук (НТЦ микроэлектроники РАН) | Method of obtaining antimonide gallium with a large specific electrical resistance |
| CN106298577A (en) * | 2016-10-18 | 2017-01-04 | 中国工程物理研究院激光聚变研究中心 | A kind of method of monocrystal thin films sedimentation rate on-line determination and application |
| CN106298577B (en) * | 2016-10-18 | 2019-03-12 | 中国工程物理研究院激光聚变研究中心 | A kind of method and application of monocrystal thin films deposition rate on-line determination |
| CN110246754A (en) * | 2019-06-20 | 2019-09-17 | 江苏能华微电子科技发展有限公司 | A kind of preparation method and epitaxial structure of HEMT epitaxial structure |
| CN113823551A (en) * | 2020-06-19 | 2021-12-21 | 中国科学院半导体研究所 | Method for growing GaSb epitaxial wafer on GaAs substrate and GaAs-based substrate |
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