CN115732594B - A preparation method for optimizing InAs/GaSb infrared superlattice and InAs/GaSb superlattice - Google Patents
A preparation method for optimizing InAs/GaSb infrared superlattice and InAs/GaSb superlattice Download PDFInfo
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- CN115732594B CN115732594B CN202211308872.5A CN202211308872A CN115732594B CN 115732594 B CN115732594 B CN 115732594B CN 202211308872 A CN202211308872 A CN 202211308872A CN 115732594 B CN115732594 B CN 115732594B
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- 229910005542 GaSb Inorganic materials 0.000 title claims abstract description 108
- 229910000673 Indium arsenide Inorganic materials 0.000 title claims abstract description 77
- RPQDHPTXJYYUPQ-UHFFFAOYSA-N indium arsenide Chemical compound [In]#[As] RPQDHPTXJYYUPQ-UHFFFAOYSA-N 0.000 title claims abstract description 77
- 238000002360 preparation method Methods 0.000 title claims abstract description 22
- 238000000034 method Methods 0.000 claims abstract description 27
- 239000000758 substrate Substances 0.000 claims abstract description 25
- WPYVAWXEWQSOGY-UHFFFAOYSA-N indium antimonide Chemical compound [Sb]#[In] WPYVAWXEWQSOGY-UHFFFAOYSA-N 0.000 claims abstract description 18
- 229910052738 indium Inorganic materials 0.000 claims abstract description 11
- 230000008569 process Effects 0.000 claims abstract description 11
- 238000007872 degassing Methods 0.000 claims abstract description 7
- 229910052785 arsenic Inorganic materials 0.000 claims abstract description 4
- 229910052733 gallium Inorganic materials 0.000 claims abstract description 4
- 238000001451 molecular beam epitaxy Methods 0.000 claims description 6
- 239000013078 crystal Substances 0.000 abstract description 9
- 238000001514 detection method Methods 0.000 abstract description 4
- 239000000463 material Substances 0.000 description 15
- 238000010586 diagram Methods 0.000 description 9
- 238000002441 X-ray diffraction Methods 0.000 description 6
- 238000005336 cracking Methods 0.000 description 5
- 238000010521 absorption reaction Methods 0.000 description 4
- 230000007547 defect Effects 0.000 description 4
- 238000005516 engineering process Methods 0.000 description 4
- 238000000089 atomic force micrograph Methods 0.000 description 3
- 230000009467 reduction Effects 0.000 description 3
- 239000004065 semiconductor Substances 0.000 description 3
- 230000005641 tunneling Effects 0.000 description 3
- 230000009286 beneficial effect Effects 0.000 description 2
- 230000000694 effects Effects 0.000 description 2
- 239000007789 gas Substances 0.000 description 2
- 230000008595 infiltration Effects 0.000 description 2
- 238000001764 infiltration Methods 0.000 description 2
- 238000004519 manufacturing process Methods 0.000 description 2
- 238000000103 photoluminescence spectrum Methods 0.000 description 2
- 229920006395 saturated elastomer Polymers 0.000 description 2
- 229910000661 Mercury cadmium telluride Inorganic materials 0.000 description 1
- 230000004888 barrier function Effects 0.000 description 1
- 230000005540 biological transmission Effects 0.000 description 1
- 230000015572 biosynthetic process Effects 0.000 description 1
- MCMSPRNYOJJPIZ-UHFFFAOYSA-N cadmium;mercury;tellurium Chemical compound [Cd]=[Te]=[Hg] MCMSPRNYOJJPIZ-UHFFFAOYSA-N 0.000 description 1
- 230000001276 controlling effect Effects 0.000 description 1
- 238000009792 diffusion process Methods 0.000 description 1
- 238000000407 epitaxy Methods 0.000 description 1
- 230000006872 improvement Effects 0.000 description 1
- 238000003331 infrared imaging Methods 0.000 description 1
- 238000012986 modification Methods 0.000 description 1
- 230000004048 modification Effects 0.000 description 1
- 230000004297 night vision Effects 0.000 description 1
- 238000005457 optimization Methods 0.000 description 1
- 230000000737 periodic effect Effects 0.000 description 1
- 230000005622 photoelectricity Effects 0.000 description 1
- 238000004886 process control Methods 0.000 description 1
- 230000001105 regulatory effect Effects 0.000 description 1
- 239000000126 substance Substances 0.000 description 1
- 239000004094 surface-active agent Substances 0.000 description 1
- 238000002207 thermal evaporation Methods 0.000 description 1
- 230000008719 thickening Effects 0.000 description 1
- 238000012795 verification Methods 0.000 description 1
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Chemical compound O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 description 1
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- Y—GENERAL TAGGING OF NEW TECHNOLOGICAL DEVELOPMENTS; GENERAL TAGGING OF CROSS-SECTIONAL TECHNOLOGIES SPANNING OVER SEVERAL SECTIONS OF THE IPC; TECHNICAL SUBJECTS COVERED BY FORMER USPC CROSS-REFERENCE ART COLLECTIONS [XRACs] AND DIGESTS
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- Y02P—CLIMATE CHANGE MITIGATION TECHNOLOGIES IN THE PRODUCTION OR PROCESSING OF GOODS
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Abstract
本发明提供了一种优化InAs/GaSb红外超晶格的制备方法，包括：对GaSb衬底除气；对GaSb衬底进行脱氧处理；在脱氧处理后的GaSb衬底上，生长GaSb缓冲层；在GaSb缓冲层上，生长InAs/GaSb超晶格，其中，InAs/GaSb超晶格生长过程按照如下方法控制炉源开关时间：打开Sb炉源的快门6s；同时打开In和Sb炉源的快门0.9s，进行InSb层的生长；关闭Sb炉源快门，同时打开In和As炉源的快门24.2s，进行InAs层的生长；关闭In炉源快门，仅打开As炉源快门6s；同时打开In和Sb炉源快门进行InSb界面层的生长；同时打开Ga和Sb炉源快门，进行GaSb层的外延生长。本发明可有效降低As背景压强扰动对于超晶格生长的影响，精确控制InAs五三比，提高超晶格晶体质量，提高红外探测器件性能。
The invention provides a preparation method for optimizing InAs/GaSb infrared superlattice, comprising: degassing a GaSb substrate; performing deoxidation treatment on the GaSb substrate; growing a GaSb buffer layer on the deoxidation treated GaSb substrate; and growing an InAs/GaSb superlattice on the GaSb buffer layer, wherein, in the growth process of the InAs/GaSb superlattice, the furnace source switching time is controlled according to the following method: opening a shutter of an Sb furnace source for 6 seconds; simultaneously opening shutters of In and Sb furnace sources for 0.9 seconds to grow an InSb layer; closing the Sb furnace source shutter, and simultaneously opening shutters of In and As furnace sources for 24.2 seconds to grow an InAs layer; closing the In furnace source shutter, and only opening the As furnace source shutter for 6 seconds; simultaneously opening the In and Sb furnace source shutters to grow an InSb interface layer; and simultaneously opening the Ga and Sb furnace source shutters to perform epitaxial growth of the GaSb layer. The present invention can effectively reduce the influence of As background pressure disturbance on superlattice growth, accurately control the InAs 5:3 ratio, improve the quality of superlattice crystals, and improve the performance of infrared detection devices.
Description
Technical Field
The invention relates to the technical field of semiconductor photoelectricity, in particular to a preparation method for optimizing an InAs/GaSb infrared superlattice and the InAs/GaSb superlattice.
Background
The long-wave infrared in the range of 3-30 μm is an atmospheric transmission window and is also the region where the characteristic absorption peaks of many chemicals and gases are located. Infrared (IR) detection technology is widely used in the fields of biochemical gas detection, infrared guidance, infrared imaging, night vision, aerospace, and the like. Compared with mercury cadmium telluride materials, the second-class superlattice materials have several advantages: (1)The family lattice constants are close, the lattice mismatch is smaller, and the probability of generating strain and defects is reduced; (2) According to kane theory, the effective mass of a semiconductor material can be roughly considered to be proportional to the band gap, and the effective mass of a semiconductor material with a smaller forbidden band width is smaller. The tunneling current of the infrared detector can have a great influence on the performance, and when the effective mass is smaller, the tunneling current can be increased, and the performance of the detector is reduced. The effective mass of the second-class superlattice material does not completely follow kane theory, the effective mass of the second-class superlattice material is not reduced along with the reduction of the forbidden bandwidth, the larger effective mass is maintained, the tunneling current of the corresponding detector is reduced, and the performance is improved; (3) By adjusting the layer thickness and composition, continuous control of the energy band can be achieved. In addition, the third-generation infrared detector based on the III-V group second superlattice has the advantages of mature growth and processing technology, lower manufacturing cost and the like, and the growth rate and the components in the superlattice growth process can be controlled highly by means of a molecular beam epitaxy technology.
In the process of epitaxy of the second-class superlattice material, the growth temperature, the five-three beam ratio and the growth rate have very important influences on the interface and the components of each layer. In the prior art, an InSb-like interface and a GaAs-like interface are inserted between superlattice InAs and GaSb layers by a growth interruption method, a surface mobility enhancement method and a five-group element infiltration method, so that the superlattice interface is optimized, the superlattice crystal quality is further regulated, and the effects of factors such as interruption time, infiltration beam size and the like on the type and the components of the interface are mainly explored.
Disclosure of Invention
In order to solve the technical problems of insufficient As voltage and small five-three ratio in the initial growth stage of the superlattice in the prior art, the invention aims to provide a preparation method for optimizing an InAs/GaSb infrared superlattice, which comprises the following steps:
step S1, degassing a GaSb substrate;
s2, deoxidizing the GaSb substrate;
step S3, growing a GaSb buffer layer on the deoxidized GaSb substrate;
step S4, growing InAs/GaSb superlattice on the GaSb buffer layer, wherein the growth process of the InAs/GaSb superlattice controls the switching time of a furnace source according to the following method:
step S41, opening a shutter 6S of the Sb furnace source;
s42, simultaneously opening shutters of In and Sb furnace sources for 0.9S, and growing an InSb layer;
s43, closing a shutter of an Sb furnace source, and simultaneously opening shutters of In and As furnace sources for 24.2 seconds to grow an InAs layer;
step S44, closing the In furnace shutter, and opening only the As furnace shutter 6S;
s45, simultaneously opening In and Sb furnace source shutters to grow InSb interface layers;
and step S46, simultaneously opening the Ga and Sb furnace source shutters, and performing epitaxial growth of the GaSb layer.
Preferably, in step S4, the vacuum degree of the vacuum growth chamber is greater than 2×10 -9 mbar。
Preferably, in step S4, the InAs/GaSb superlattice is grown using a molecular beam epitaxy method.
Preferably, in step S1, the GaSb substrate is degassed at 300℃in a degassing chamber for about 1-2 hours.
Preferably, in step S2, the GaSb substrate is introduced into a vacuum growth chamber and deoxidized at a temperature of 520 ℃ for 10min.
Another object of the present invention is to provide an InAs/GaSb infrared superlattice structure prepared by a method of the present invention for optimizing the preparation of an InAs/GaSb infrared superlattice, comprising a GaSb substrate, a GaSb buffer layer, an InSb layer, an InAs layer, an InSb interface layer, and a GaSb epitaxial layer from bottom to top.
According to the preparation method for optimizing the InAs/GaSb infrared superlattice and the InAs/GaSb superlattice, provided by the invention, on the basis of a traditional process method, the on-off control of an As needle valve is further optimized aiming at the characteristics of the specificity of an As cracking source furnace structure of Molecular Beam Epitaxy (MBE) equipment and the large saturated vapor pressure of five-group element As, and the problems of insufficient As pressure and small five-three ratio in the initial growth stage of the superlattice are solved by increasing the opening size of the As needle valve in the initial growth stage of the superlattice. The large As needle valve opening size in the initial growth stage is beneficial to the improvement of the surface atomic diffusion length, is more beneficial to the reduction of defect density and effectively improves the crystal quality. As atom surfactant, the mobility of Sb atoms is increased, the formation probability of Sb clusters is reduced, and the superlattice is ensured to grow on an atomically flat surface.
The preparation method for optimizing the InAs/GaSb infrared superlattice and the InAs/GaSb superlattice provided by the invention can effectively reduce the problem of the reduction of the crystal quality of the infrared detector superlattice caused by the fluctuation of the background pressure of group five, and provide great advantages for preparing infrared detectors with uniform and reliable components.
The preparation method for optimizing the InAs/GaSb infrared superlattice and the InAs/GaSb superlattice provided by the invention can effectively reduce the influence of As background pressure disturbance on the superlattice growth, accurately control the InAs five-three ratio, improve the superlattice crystal quality and further improve the infrared detection device performance.
Drawings
In order to more clearly illustrate the embodiments of the present invention or the technical solutions in the prior art, the drawings that are needed in the description of the embodiments or the prior art will be briefly described, and it is obvious that the drawings in the description below are some embodiments of the present invention, and other drawings can be obtained according to the drawings without inventive effort for a person skilled in the art.
Fig. 1 schematically shows a schematic of the partial pressure of As over time during multicycle superlattice growth.
Fig. 2 shows a schematic diagram of an InAs/GaSb infrared superlattice structure in an embodiment of the invention.
Figure 3 shows a schematic time sequential diagram of the growth of an InAs/GaSb superlattice per period in one embodiment of the invention.
Fig. 4 shows a schematic structural diagram of a superlattice infrared detector fabricated by using a method for optimizing the preparation of the InAs/GaSb infrared superlattice in an embodiment of the invention.
Fig. 5 shows an X-ray diffraction contrast plot of an nBn type InAs/GaSb superlattice in accordance with the invention and an InAs/GaSb infrared superlattice.
Fig. 6 shows an atomic force microscopic comparison of an nBn-type InAs/GaSb superlattice with an inventive InAs/GaSb infrared superlattice.
Figure 7 shows a photoluminescence spectrum of an InAs/GaSb infrared superlattice in one embodiment of the invention.
Detailed Description
To further clarify the above and other features and advantages of the present invention, a further description of the invention will be rendered by reference to the appended drawings. It should be understood that the specific embodiments presented herein are for purposes of explanation to those skilled in the art and are intended to be illustrative only and not limiting.
In order to solve the technical problems of insufficient As voltage and small five-three ratio in the initial growth stage of the superlattice in the prior art, a preparation method for optimizing the InAs/GaSb infrared superlattice and the InAs/GaSb superlattice are provided.
Description of the principles
For GaSb substrates, gaSb thickness has less strain effect on the superlattice, which is mainly related to interface structure and InAs layer thickness, variation in InAs layer thickness creates superlattice mismatch problems. An increase in the InAs layer thickness requires a larger lattice constant InSb layer to compensate, and thickening of the InSb layer can lead to an increase in defects and dislocations. Because of lattice mismatch between InAs and GaSb and the interface defect state caused by a complex heterojunction interface structure, stress regulation and control can be performed by controlling the thickness of each layer and the interface technology (valve switching sequence), so that the stress balance superlattice is realized. Therefore, in order to obtain the superlattice material with high crystal quality and strain balance, the accurate regulation and control of the InAs five-three ratio and the components are also important.
During the growth of the superlattice, an As source and an Sb source are respectively provided by cracking a cracking source furnace with an As needle valve and an Sb needle valve. The vapor pressure of the thermal evaporation source furnace and the Sb cracking source furnace is relatively low, and the required beam value is easy to reach. As the saturated vapor pressure of the As cracking source is higher, the As pressure is easily unstable when the As needle valve is opened and closed, so that the uniformity of the crystal components of the superlattice material is deteriorated, and the crystal quality is reduced. The thickness of the absorbing layer of an infrared detector is related to the length of light absorbed by the detector, typically a few microns, involving the growth of a superlattice of a few hundred cycles.
As partial pressure of As changes with time in the multi-period superlattice growth process As shown in figure 1, the partial pressure of As measured by a beam monitor changes with time in the multi-period superlattice growth process, and the partial pressure of As measured by the beam monitor is always in an elevated state in the first few superlattice growth periods and is not in a stable state until twenty to thirty periods, which causes non-uniformity of superlattice material components.
Optimizing process
As shown in fig. 2, which is a schematic diagram of an InAs/GaSb infrared superlattice structure in an embodiment of the present invention, according to an embodiment of the present invention, there is provided a preparation method for optimizing an InAs/GaSb infrared superlattice, the preparation method including:
step S1, degassing the GaSb substrate 101.
The GaSb substrate 101 is degassed at 300 ℃ for about 1-2 hours to remove water vapor on the surface of the GaSb substrate 101.
Step S2, deoxidizing the GaSb substrate 101.
The GaSb substrate 101 is transferred into a vacuum growth cavity, deoxidized for 10min at the temperature of 520 ℃ and the oxide layer on the surface of the GaSb substrate 101 is removed.
And step S3, growing a GaSb buffer layer 102 on the deoxidized GaSb substrate, wherein the thickness of the GaSb buffer layer 102 is 500nm.
And S4, growing InAs/GaSb superlattice on the GaSb buffer layer.
Fig. 3 shows a schematic time sequence diagram of the growth of the InAs/GaSb superlattice per period in one embodiment of the invention, and in step S4, the InAs/GaSb superlattice is grown by using a molecular beam epitaxy method. The InAs/GaSb superlattice growth process controls the furnace source switching time according to the following method:
step S41, opening a shutter 6S of the Sb furnace source.
Step S42, shutter of In and Sb furnace source is opened for 0.9S at the same time, and InSb layer 103 is grown.
And S43, closing the shutter of the Sb furnace source, and simultaneously opening the shutters of the In furnace source and the As furnace source for 24.2 seconds to grow the InAs layer 104.
Step S44, the In furnace shutter is closed, and only the As furnace shutter 6S is opened.
And step S45, simultaneously opening In and Sb furnace source shutters to grow the InSb interface layer 105.
And step S46, simultaneously opening the Ga and Sb furnace source shutters, and performing epitaxial growth of the GaSb epitaxial layer 106.
In the growth process of InAs/GaSb superlattice, the growth rates of GaSb and InAs are as followsThe vacuum degree of the vacuum growth cavity is more than 2 multiplied by 10 -9 mbar。
According to an embodiment of the present invention, as shown in fig. 2, an InAs/GaSb infrared superlattice structure is prepared in one growth cycle by the above-described optimized preparation process, and includes a GaSb substrate 101, a GaSb buffer layer 102, an InSb layer 103, an InAs layer 104, an InSb interface layer 105, and a GaSb epitaxial layer 106 from bottom to top.
Superlattice infrared detector
Fig. 4 is a schematic structural diagram of a superlattice infrared detector fabricated by using a method for optimizing the fabrication of an InAs/GaSb infrared superlattice in an embodiment of the invention. According to an embodiment of the present invention, a superlattice infrared detector is provided, which includes a GaSb substrate 101, a GaSb buffer layer 102, a first N-type doped type-two superlattice layer, an absorption layer, a barrier layer, a second N-type doped type-two superlattice layer, and a cap layer from bottom to top.
The first N-type doped type II superlattice layer, the absorption layer and the second N-type doped type II superlattice layer are all used for carrying out a plurality of periodic growth of InAs/GaSb superlattice through the steps S41 to S46. Namely: the first N-type doped second-type superlattice layer, the absorption layer and the second N-type doped second-type superlattice layer comprise an InSb layer 103, an InAs layer 104, an InSb interface layer 105 and a GaSb epitaxial layer 106 in an InAs/GaSb infrared superlattice structure which grow in a plurality of cycles.
The cover layer is an InAs cover layer grown on the second N-type doped type II superlattice layer.
Result verification
By adopting the preparation method, the five-family atmosphere of the MBE cavity can be stabilized to the greatest extent, the five-three ratio of superlattice growth can be precisely controlled, and the crystal quality of the superlattice can be greatly improved.
An X-ray diffraction contrast pattern of an nBn-type InAs/GaSb superlattice as shown in fig. 5, wherein (a) an X-ray diffraction pattern (XRD pattern) of an inventive InAs/GaSb infrared superlattice; (b) An X-ray diffraction pattern (XRD pattern) of an nBn type InAs/GaSb superlattice.
As can be seen from FIG. 5, the XRD of the InAs/GaSb infrared superlattice and the full structure of the invention shows sharp diffraction peaks and obvious satellite peaks.
An atomic force microscopic comparison diagram of the nBn type InAs/GaSb superlattice and the InAs/GaSb infrared superlattice according to the invention is shown in fig. 6, wherein (a) is an atomic force microscopic diagram (AFM diagram) of the InAs/GaSb infrared superlattice according to the invention; (b) Atomic force microscopy images (AFM images) of nBn type InAs/GaSb superlattice.
As can be seen from FIG. 5, the atomic force micrograph of the InAs/GaSb infrared superlattice of the invention shows that the bright spots are obviously reduced, the height of the bright spots is reduced and the surface is quite smooth after the AFM observation of the superlattice which grows optimally.
As shown in FIG. 7, the photoluminescence spectrum of the InAs/GaSb infrared superlattice in one embodiment of the invention has a peak position of 4.78 μm at 77K, corresponding to 0.25eV, and a half-width of only 22.3meV.
According to the preparation method for optimizing the InAs/GaSb infrared superlattice and the InAs/GaSb superlattice, the proper larger As needle valve opening size is selected in the first few periods of superlattice growth, so that the cavity pressure is effectively stabilized, the influence of the partial pressure disturbance of the five-group element on the superlattice growth is reduced, the surface of the material is effectively protected, the uniformity and the stability of the surface of the superlattice material can be greatly improved, and the area uniformity and the quality stability of the large-area array superlattice infrared detector are further improved. The superlattice material growth optimization method can be used for preparing the full-structure material of the infrared detector, and the full-structure material is subjected to subsequent process processing, so that the high-performance superlattice infrared detector can be finally obtained.
While embodiments of the present invention have been shown and described above, it will be understood that the above embodiments are illustrative and not to be construed as limiting the invention, and that variations, modifications, alternatives and variations may be made to the above embodiments by one of ordinary skill in the art within the scope of the invention.
Claims (6)
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Citations (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101576413A (en) * | 2008-05-09 | 2009-11-11 | 中国科学院半导体研究所 | GaAs based InAs/GaSb superlattice near infrared photodetector and manufacturing method thereof |
| CN101777601A (en) * | 2010-02-03 | 2010-07-14 | 中国科学院半导体研究所 | InAs/GaSb superlattice infrared photoelectric detector and manufacturing method thereof |
| CN103233271A (en) * | 2013-04-18 | 2013-08-07 | 中国科学院半导体研究所 | Method for epitaxial growth of InAs/GaSb type-II superlattice on GaAs substrate |
| CN113358677A (en) * | 2021-06-06 | 2021-09-07 | 南京国科半导体有限公司 | Method for measuring growth speed of InAs layer grown on GaSb substrate |
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| Publication number | Priority date | Publication date | Assignee | Title |
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| US20090224227A1 (en) * | 2008-03-06 | 2009-09-10 | Manijeh Razeghi | TYPE-II InAs/GaSb SUPERLATTICE PHOTODIODE AND METHOD OF OPTIMIZING QUANTUM EFFICIENCY |
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Patent Citations (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101576413A (en) * | 2008-05-09 | 2009-11-11 | 中国科学院半导体研究所 | GaAs based InAs/GaSb superlattice near infrared photodetector and manufacturing method thereof |
| CN101777601A (en) * | 2010-02-03 | 2010-07-14 | 中国科学院半导体研究所 | InAs/GaSb superlattice infrared photoelectric detector and manufacturing method thereof |
| CN103233271A (en) * | 2013-04-18 | 2013-08-07 | 中国科学院半导体研究所 | Method for epitaxial growth of InAs/GaSb type-II superlattice on GaAs substrate |
| CN113358677A (en) * | 2021-06-06 | 2021-09-07 | 南京国科半导体有限公司 | Method for measuring growth speed of InAs layer grown on GaSb substrate |
Non-Patent Citations (1)
| Title |
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| "Interface engineered MBE grown InAs/GaSb based type-II superlattice heterostructures";Puspashree Mishra 等;《Journal of Alloys and Compounds》;20210824;第889卷;全文 * |
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