CN114038732A - Method for growing GaSb on GaAs substrate by adopting interface mismatch array technology - Google Patents

Method for growing GaSb on GaAs substrate by adopting interface mismatch array technology Download PDF

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CN114038732A
CN114038732A CN202111026677.9A CN202111026677A CN114038732A CN 114038732 A CN114038732 A CN 114038732A CN 202111026677 A CN202111026677 A CN 202111026677A CN 114038732 A CN114038732 A CN 114038732A
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substrate
gaas
gasb
alsb
temperature
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刘国军
徐东昕
李再金
陈浩
赵志斌
曾丽娜
乔忠良
李林
曲轶
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Hainan Normal University
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    • H—ELECTRICITY
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    • H01L21/00—Processes or apparatus adapted for the manufacture or treatment of semiconductor or solid state devices or of parts thereof
    • H01L21/02—Manufacture or treatment of semiconductor devices or of parts thereof
    • H01L21/02104—Forming layers
    • H01L21/02365—Forming inorganic semiconducting materials on a substrate
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    • H—ELECTRICITY
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    • H01L21/02104—Forming layers
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    • H01L21/02365—Forming inorganic semiconducting materials on a substrate
    • H01L21/02612—Formation types
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    • H01L21/02631—Physical deposition at reduced pressure, e.g. MBE, sputtering, evaporation
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Abstract

The invention relates to a method for growing GaSb on a GaAs substrate by adopting an interface mismatch array technology. On a GaAs substrate, GaSb, bright AlSb barrier layers and InAs/GaSb quantum wells clamped between the GaSb and bright AlSb barrier layers are clearly visible, the interface mutation among the material layers is obvious, and no defect or dislocation occurs in the structure, thereby indicating the extremely high material structure quality.

Description

Method for growing GaSb on GaAs substrate by adopting interface mismatch array technology
Technical Field
The invention discloses a method for growing GaSb on a GaAs substrate by adopting an interface mismatch array technology, belonging to the field of epitaxial growth and manufacturing of semiconductor materials.
Background
Antimony compound semiconductor materials (InAs, InSb, GaSb, AlSb and related compounds) not only have wide-range variable energy band gaps and band gap differences, but also have high electron mobility. These characteristics make this material system very suitable for preparing high-speed and low-power electronic devices and mid-infrared light sources. Heterostructures formed by combining them are generally grown on GaSb or InAs substrates using Molecular Beam Epitaxy (MBE) or metal organic vapor phase epitaxy (MOCVD). However, such substrates have problems of small size, high price, and no semi-insulating substrate for commercial use. In addition, the low thermal conductivity of the substrate material is not favorable for preparing high-power devices.
Based on these factors, there has been interest in the past for a long time in growing antimonide materials epitaxially on other alternative substrates (GaAs or Si). The antimonide material can be grown on GaAs or Si, so that the problems caused by the adoption of a GaSb or InAs substrate can be solved, and the possibility of photoelectronic device integration can be provided. However, the large lattice constant difference (7-8% lattice mismatch) between the antimonide epitaxial material layer and the GaAs or Si substrate results in the formation of a high density of linear dislocations in the epitaxial material layer, which is detrimental to the fabrication of high performance devices.
To overcome this problem, various methods have been used to attempt to reduce the threading dislocation density, including low temperature growth buffer layers, compositionally graded buffer layers, AlSb transition layers, and Interfacial mismatch array (IMF) techniques. Among them, the IMF technique is very effective in stress relief and reduction of the threading dislocation density. The 90-degree pure edge dislocation periodic array is formed at the interface of GaAs and GaSb, so that more than 98% of stress is effectively released on the interface layers of a plurality of molecular monolayers, the probability of generation of 60-degree dislocation causing threading dislocation is reduced, a low dislocation density epitaxial layer is formed, and further, the preparation of a high-performance Sb compound device on a GaAs substrate is possible. Although the IMF technique has a significant effect on the quality improvement of epitaxial antimonide material layers, relatively few reports have been made to date on the study of growth optimization conditions for growing antimonide materials using this technique.
Disclosure of Invention
The invention provides a method for growing GaSb on a GaAs substrate by adopting an interface mismatch array technology. All samples In the experiment are grown on a 2-inch double-side polished (100) -oriented GaAs substrate by adopting an ultrahigh vacuum molecular beam epitaxy system assembled with Ga, In, Al, cracked As and cracked Sb sources. The growth temperature of the sample was measured and monitored using an infrared thermometer and calibrated by the (2x4) to c (4x4) transition point of the surface de-oxidation layer temperature of the GaAs substrate and surface reconstruction near 515 ℃. Growing a narrow bandgap GaSb material on a GaAs substrate results in a significant substrate temperature increase, while maintaining the substrate thermocouple temperature, due to increased infrared radiation absorption. It is particularly noteworthy that this phenomenon is very pronounced at the initial stage of growth of the GaSb material layer. The quality of the antimonide material is very sensitive to the substrate growth temperature. In order to obtain a high quality epitaxial antimonide material layer, the actual substrate temperature measured by an infrared thermometer needs to be kept relatively stable. In this case, the thermocouple temperature of the substrate heater needs to be adjusted and decreased continuously during the growth of the GaSb material layer until the actual substrate temperature is stabilized.
This adjustment of the temperature reduction of the substrate heater thermocouple may be as high as 80 ℃ for growth of GaSb on semi-insulating GaAs substrates, and typically does not exceed 30 ℃ for growth of GaSb on N-type doped GaAs substrates, and the actual substrate temperature may quickly stabilize. In order to avoid the influence on the quality of antimonide materials, which may be caused by a sharp temperature change on a semi-insulating GaAs substrate, an N-type doped GaAs substrate was mainly used in the experiment. In the growth process, cracked As is adopted2And Sb2As a five-family beam source, the growth rates of GaSb and AlSb were fixed at 0.5 micron/hr and 0.16 micron/hr, respectively, and the growth conditions were optimized by varying the growth temperature, Sb: Ga equivalent atomic flux ratio, AlSb transition layer thickness, and GaSb layer thickness. The growth condition optimization values are determined by the quality of the three-axis high resolution x-ray diffraction (HRXRD) measurement sample structure.
The growth process of the material is as follows: firstly, placing a GaAs substrate in a sample feeding bin, degassing at a low temperature of 150 ℃ for not less than 10 hours, then transferring the GaAs substrate into a preparation bin, degassing at a thermocouple temperature of 450 ℃ until the pressure of the preparation bin is lower than 5x10-9The mabr. Thereafter, the substrate was transferred to a growth chamber and heated to 630 ℃ under As overpressure protection (actual substrate temperature measured by an infrared thermometer, the same applies below) and held for 15 minutes. This process ensures that the substrate surface is thoroughly cleaned of oxide and adsorbed gases. After removal of the oxide layer was complete, the substrate temperature was reduced and stabilized at 575 ℃ under continued protection from As overpressure. To obtain a smooth sample surface, a 500 nm thick GaAs buffer layer was grown under an As-rich (2x4) surface reconstruction with the Ga shutter open to ensure the subsequent GaSb layer epitaxial quality. It is to be noted here that the substrate temperature increased to 585 ℃ after the Ga shutter was opened due to the heat radiation from the source furnace. And after the growth of the GaSb buffer layer is finished, closing the Ga shutters and the Sb shutters simultaneously and keeping the thermocouple temperature of the substrate heater unchanged. The shutter is closed to block the heat radiation of the source furnace, and the temperature of the substrate is immediately reduced to about 575 ℃ under the condition that the thermocouple temperature of the substrate heater is not changed. Literature studies have shown that Ga-rich surfaces are a major factor in being able to successfully achieve stress relief using IMF techniques. In order to effectively remove As adsorbed on the substrate surface, the temperature was held constant at 575 ℃ with all shutters and As source needle valves closed until a Ga-rich (4x2) surface reconstruction was observed. Immediately after this phenomenon occurs, the substrate temperature is lowered and stabilized at a predetermined temperature for antimonide growth.
Before the growth of the antimonide material begins, the GaAs surface is irradiated with a Sb beam for 5 seconds to convert it to a Sb-rich surface. After the growth of the antimonide material GaSb or AlSb layer has started, the RHEED diffraction pattern appears as a dot pattern at the initial stage due to the three-dimensional structure growth. This process is of short duration and the RHEED image begins to transform into a typical Sb rich (1x3) surface reconstruction after only a few molecular monolayers for either GaSb or AlSb material layer growth, indicating that a two-dimensional growth pattern of the material layer occurs, but some of the steps are modified to improve the quality of the antimonide material. 585 ℃ was used as the GaAs buffer layer growth temperature. In addition, after the GaAs buffer layer is grown, in the process of lowering the substrate temperature, the existing documents generally adopt As or Sb beam for protection, which may cause a part of As on the surface to remain to some extent. These residual As result in the formation of a thin alloy layer at the interface, affecting not only the epitaxial layer surface roughness but also the stress relief at the interface by the IMF mechanism. Instead of using any beam current protection measures, the substrate surface As is desorbed at high temperature around 575 ℃ and the GaAs buffer layer is converted into a Ga-rich surface. It was found that it took approximately 2 minutes or so to convert the As-rich surface reconstruction of GaAs to a clear Ga-rich surface reconstruction around 575 ℃. The length has enough time to judge the existence of the Ga-rich surface and reduce the temperature of the substrate in time so As to ensure that the GaAs surface does not lose a large amount of As to cause the appearance of excessive Ga or even Ga drops, thereby avoiding affecting the quality of the Sb compound material.
And (3x1) the Sb-rich AlSb epitaxial layer is obtained by growth under the condition of high Sb atom flux. The Al shutter was then turned off by keeping the Sb shutter open, stopping AlSb growth. The Sb atomic flux was reduced stepwise while keeping the substrate temperature and Al flux fixed. After the Sb atomic flux value decreased and stabilized each time, the Al shutter was opened while observing the AlSb surface reconstruction change. When the Sb atomic flux is just insufficient, the Sb-rich surface reconstruction of the AlSb epitaxial layer (3x1) will slowly shift to the Al-rich surface reconstruction of (4x 2). In this case, the Sb atomic flux is further reduced, and the reconstruction transition occurs instantaneously with the opening of the Al shutter, meaning that the Sb atomic flux is severely insufficient, and the Sb atomic flux slightly higher than the vicinity of the reconstruction transition point can well maintain the stable growth of the AlSb layer.
The structure is as follows: the GaAs substrate, grow 10 microns GaSb buffer layer (1), 50 nanometer AlSb layer (2), 5 nanometer GaSb layer and 15 nanometer InAs layer (3), 50 nanometer AlSb layer (2) above the substrate.
Fig. 1 is a TEM measurement result. Although the structures were grown on GaAs substrates, they showed very good structure quality and abrupt interfaces, and TEM measurements confirmed this conclusion further. In a TEM image, bright AlSb barrier layers and an InAs/GaSb quantum well clamped between the AlSb barrier layers are clearly visible, the interface mutation among the material layers is obvious, and no defect or dislocation occurs in the structure, thereby indicating the extremely high quality of the material structure.
Drawings
Fig. 1 shows a schematic structural diagram of TEM measurement results.
Description of the reference numerals
(1) A 10 micron GaSb buffer layer; (2) a 50 nm AlSb layer; (3) a 5 nm GaSb layer and a 15 nm InAs layer.

Claims (1)

1. A method for growing GaSb on a GaAs substrate by adopting an interface mismatch array technology is characterized by comprising the following steps:
the invention provides a method for growing GaSb on a GaAs substrate by adopting an interface mismatch array technology, which comprises the steps of firstly placing the GaAs substrate in a sample feeding bin, degassing at a low temperature of 150 ℃ for not less than 10 hours, and then transferring the GaAs substrate into a preparation bin for degassing at a thermocouple temperature of 450 ℃ until the pressure of the preparation bin is lower than 5x10-9A mabr; then, the substrate is conveyed into a growth bin, and is heated to 630 ℃ under As overvoltage protection and kept for 15 minutes; the temperature of the substrate is reduced and stabilized at 575 ℃, a Ga shutter is opened to grow a GaAs buffer layer with the thickness of 500 nanometers under the reconstruction of an As-rich (2x4) surface so As to ensure the epitaxial quality of a next GaSb layer; after the GaAs buffer layer grows, closing the Ga and As shutters at the same time, keeping the thermocouple temperature of the substrate heater unchanged, immediately reducing the substrate temperature to about 575 ℃, and irradiating the GaAs surface for 5 seconds by adopting Sb beam to convert the GaAs surface into a Sb-rich surface; growing under the condition of high Sb atom flux to obtain (3x1) Sb-rich AlSb epitaxial layer; then, the Sb shutter is kept open, the Al shutter is closed, and the growth of AlSb is stopped; reducing Sb atom flux step by step under the condition of keeping the substrate temperature and Al flux fixed; opening an Al shutter after the Sb atomic flux value is reduced and stabilized each time, and observing the reconstruction change condition of the AlSb surface; when the Sb atomic flux is just insufficient, the Sb-rich surface reconstruction of the AlSb epitaxial layer (3x1) will slowly transit to the Al-rich surface reconstruction of (4x2), maintaining stable growth of the AlSb layer.
CN202111026677.9A 2021-09-02 2021-09-02 Method for growing GaSb on GaAs substrate by adopting interface mismatch array technology Pending CN114038732A (en)

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