CN114197055A - InAs/InSb strain superlattice material and preparation method thereof - Google Patents
InAs/InSb strain superlattice material and preparation method thereof Download PDFInfo
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- 229910000673 Indium arsenide Inorganic materials 0.000 title claims abstract description 113
- RPQDHPTXJYYUPQ-UHFFFAOYSA-N indium arsenide Chemical compound [In]#[As] RPQDHPTXJYYUPQ-UHFFFAOYSA-N 0.000 title claims abstract description 113
- WPYVAWXEWQSOGY-UHFFFAOYSA-N indium antimonide Chemical compound [Sb]#[In] WPYVAWXEWQSOGY-UHFFFAOYSA-N 0.000 title claims abstract description 106
- 239000000463 material Substances 0.000 title claims abstract description 46
- 238000002360 preparation method Methods 0.000 title claims abstract description 15
- 239000000758 substrate Substances 0.000 claims abstract description 65
- 238000000034 method Methods 0.000 claims abstract description 35
- 229910005542 GaSb Inorganic materials 0.000 claims description 37
- 238000007872 degassing Methods 0.000 claims description 6
- 230000008859 change Effects 0.000 claims description 5
- 238000010438 heat treatment Methods 0.000 claims description 5
- 230000008569 process Effects 0.000 abstract description 13
- 238000004519 manufacturing process Methods 0.000 abstract description 7
- 230000015572 biosynthetic process Effects 0.000 abstract description 4
- 238000001451 molecular beam epitaxy Methods 0.000 description 8
- 238000001514 detection method Methods 0.000 description 4
- 238000002017 high-resolution X-ray diffraction Methods 0.000 description 4
- 238000001816 cooling Methods 0.000 description 3
- 230000007547 defect Effects 0.000 description 3
- 238000010586 diagram Methods 0.000 description 3
- IJGRMHOSHXDMSA-UHFFFAOYSA-N Atomic nitrogen Chemical compound N#N IJGRMHOSHXDMSA-UHFFFAOYSA-N 0.000 description 2
- 238000010521 absorption reaction Methods 0.000 description 2
- 229910052785 arsenic Inorganic materials 0.000 description 2
- 238000005336 cracking Methods 0.000 description 2
- 238000009792 diffusion process Methods 0.000 description 2
- 230000008595 infiltration Effects 0.000 description 2
- 238000001764 infiltration Methods 0.000 description 2
- 230000009286 beneficial effect Effects 0.000 description 1
- 229910002056 binary alloy Inorganic materials 0.000 description 1
- 150000001875 compounds Chemical class 0.000 description 1
- 230000001276 controlling effect Effects 0.000 description 1
- 238000006392 deoxygenation reaction Methods 0.000 description 1
- 239000003814 drug Substances 0.000 description 1
- 238000005516 engineering process Methods 0.000 description 1
- 238000012986 modification Methods 0.000 description 1
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- 229910052757 nitrogen Inorganic materials 0.000 description 1
- 230000000737 periodic effect Effects 0.000 description 1
- 230000006798 recombination Effects 0.000 description 1
- 238000005215 recombination Methods 0.000 description 1
- 230000001105 regulatory effect Effects 0.000 description 1
- 239000004065 semiconductor Substances 0.000 description 1
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- C—CHEMISTRY; METALLURGY
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- C30B—SINGLE-CRYSTAL GROWTH; UNIDIRECTIONAL SOLIDIFICATION OF EUTECTIC MATERIAL OR UNIDIRECTIONAL DEMIXING OF EUTECTOID MATERIAL; REFINING BY ZONE-MELTING OF MATERIAL; PRODUCTION OF A HOMOGENEOUS POLYCRYSTALLINE MATERIAL WITH DEFINED STRUCTURE; SINGLE CRYSTALS OR HOMOGENEOUS POLYCRYSTALLINE MATERIAL WITH DEFINED STRUCTURE; AFTER-TREATMENT OF SINGLE CRYSTALS OR A HOMOGENEOUS POLYCRYSTALLINE MATERIAL WITH DEFINED STRUCTURE; APPARATUS THEREFOR
- C30B29/00—Single crystals or homogeneous polycrystalline material with defined structure characterised by the material or by their shape
- C30B29/60—Single crystals or homogeneous polycrystalline material with defined structure characterised by the material or by their shape characterised by shape
- C30B29/68—Crystals with laminate structure, e.g. "superlattices"
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- C—CHEMISTRY; METALLURGY
- C30—CRYSTAL GROWTH
- C30B—SINGLE-CRYSTAL GROWTH; UNIDIRECTIONAL SOLIDIFICATION OF EUTECTIC MATERIAL OR UNIDIRECTIONAL DEMIXING OF EUTECTOID MATERIAL; REFINING BY ZONE-MELTING OF MATERIAL; PRODUCTION OF A HOMOGENEOUS POLYCRYSTALLINE MATERIAL WITH DEFINED STRUCTURE; SINGLE CRYSTALS OR HOMOGENEOUS POLYCRYSTALLINE MATERIAL WITH DEFINED STRUCTURE; AFTER-TREATMENT OF SINGLE CRYSTALS OR A HOMOGENEOUS POLYCRYSTALLINE MATERIAL WITH DEFINED STRUCTURE; APPARATUS THEREFOR
- C30B25/00—Single-crystal growth by chemical reaction of reactive gases, e.g. chemical vapour-deposition growth
- C30B25/02—Epitaxial-layer growth
- C30B25/18—Epitaxial-layer growth characterised by the substrate
- C30B25/183—Epitaxial-layer growth characterised by the substrate being provided with a buffer layer, e.g. a lattice matching layer
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- C—CHEMISTRY; METALLURGY
- C30—CRYSTAL GROWTH
- C30B—SINGLE-CRYSTAL GROWTH; UNIDIRECTIONAL SOLIDIFICATION OF EUTECTIC MATERIAL OR UNIDIRECTIONAL DEMIXING OF EUTECTOID MATERIAL; REFINING BY ZONE-MELTING OF MATERIAL; PRODUCTION OF A HOMOGENEOUS POLYCRYSTALLINE MATERIAL WITH DEFINED STRUCTURE; SINGLE CRYSTALS OR HOMOGENEOUS POLYCRYSTALLINE MATERIAL WITH DEFINED STRUCTURE; AFTER-TREATMENT OF SINGLE CRYSTALS OR A HOMOGENEOUS POLYCRYSTALLINE MATERIAL WITH DEFINED STRUCTURE; APPARATUS THEREFOR
- C30B29/00—Single crystals or homogeneous polycrystalline material with defined structure characterised by the material or by their shape
- C30B29/10—Inorganic compounds or compositions
- C30B29/40—AIIIBV compounds wherein A is B, Al, Ga, In or Tl and B is N, P, As, Sb or Bi
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- H—ELECTRICITY
- H01—ELECTRIC ELEMENTS
- H01L—SEMICONDUCTOR DEVICES NOT COVERED BY CLASS H10
- H01L31/00—Semiconductor devices sensitive to infrared radiation, light, electromagnetic radiation of shorter wavelength or corpuscular radiation and specially adapted either for the conversion of the energy of such radiation into electrical energy or for the control of electrical energy by such radiation; Processes or apparatus specially adapted for the manufacture or treatment thereof or of parts thereof; Details thereof
- H01L31/0248—Semiconductor devices sensitive to infrared radiation, light, electromagnetic radiation of shorter wavelength or corpuscular radiation and specially adapted either for the conversion of the energy of such radiation into electrical energy or for the control of electrical energy by such radiation; Processes or apparatus specially adapted for the manufacture or treatment thereof or of parts thereof; Details thereof characterised by their semiconductor bodies
- H01L31/0256—Semiconductor devices sensitive to infrared radiation, light, electromagnetic radiation of shorter wavelength or corpuscular radiation and specially adapted either for the conversion of the energy of such radiation into electrical energy or for the control of electrical energy by such radiation; Processes or apparatus specially adapted for the manufacture or treatment thereof or of parts thereof; Details thereof characterised by their semiconductor bodies characterised by the material
- H01L31/0264—Inorganic materials
- H01L31/0304—Inorganic materials including, apart from doping materials or other impurities, only AIIIBV compounds
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- H01L—SEMICONDUCTOR DEVICES NOT COVERED BY CLASS H10
- H01L31/00—Semiconductor devices sensitive to infrared radiation, light, electromagnetic radiation of shorter wavelength or corpuscular radiation and specially adapted either for the conversion of the energy of such radiation into electrical energy or for the control of electrical energy by such radiation; Processes or apparatus specially adapted for the manufacture or treatment thereof or of parts thereof; Details thereof
- H01L31/0248—Semiconductor devices sensitive to infrared radiation, light, electromagnetic radiation of shorter wavelength or corpuscular radiation and specially adapted either for the conversion of the energy of such radiation into electrical energy or for the control of electrical energy by such radiation; Processes or apparatus specially adapted for the manufacture or treatment thereof or of parts thereof; Details thereof characterised by their semiconductor bodies
- H01L31/0352—Semiconductor devices sensitive to infrared radiation, light, electromagnetic radiation of shorter wavelength or corpuscular radiation and specially adapted either for the conversion of the energy of such radiation into electrical energy or for the control of electrical energy by such radiation; Processes or apparatus specially adapted for the manufacture or treatment thereof or of parts thereof; Details thereof characterised by their semiconductor bodies characterised by their shape or by the shapes, relative sizes or disposition of the semiconductor regions
- H01L31/035236—Superlattices; Multiple quantum well structures
Abstract
The invention provides a preparation method of an InAs/InSb strain superlattice material, which comprises the following steps: s1, providing a substrate; s2, epitaxially growing a buffer layer on the substrate; and S3, epitaxially growing a plurality of periods of InAs/InSb superlattice structures on the buffer layer, wherein each period of InAs/InSb superlattice structure comprises an InAs layer and an InSb layer, and different In source furnaces are adopted for growing the InAs layer and the InSb layer. In addition, the invention also provides an InAs/InSb strain superlattice material obtained based on the preparation method. In the growth process of the InAs/InSb superlattice structure, two different In source furnaces are adopted, so that the speeds of two In sources can be respectively adjusted, the InAs/InSb superlattice structure is respectively suitable for the growth modes of an InAs layer and a thinner InSb layer, the formation of a three-dimensional island structure during the growth of the InAs/InSb superlattice is effectively avoided, the production efficiency of the InAs/InSb superlattice structure can be obviously improved, the production cost is reduced, and the quality and the performance of an InAs/InSb strain superlattice material are improved.
Description
Technical Field
The invention belongs to the field of semiconductor infrared detector materials, and relates to a preparation method of an InAs/InSb strain superlattice material and the InAs/InSb strain superlattice material obtained based on the preparation method.
Background
The infrared detector has been widely applied to the military and civil dual-purpose fields of strategic early warning, missile seeker, laser radar, night vision, remote sensing, medicine, atmospheric monitoring and the like due to the excellent performance of the infrared detector. The InAs/GaSb II type superlattice material is a preferable material of a third-generation infrared focal plane detector, an InAs/GaSb heterogeneous material system has a quite special energy band arrangement structure, and the InAs forbidden band width is smaller than the valence band offset of InAs/GaSb, so that the conduction band bottom of InAs is below the valence band top of GaSb to form II type superlattice. This causes: (1) the electrons and the holes are separated in space, the electrons are limited in the InAs layer, the holes are limited in the GaSb layer, and the effective forbidden bandwidth is the energy difference from the electron microstrip to the heavy-hole microstrip; (2) the effective forbidden bandwidth of the InAs/GaSb superlattice can be effectively adjusted by changing the periodic thickness of the superlattice.
However, devices made from this material have a high recombination-generating (G-R) dark current, so that they do not exhibit the expected performance. The relatively high generation of recombination dark current is due to the low Shockley-Read-hall (SRH) lifetime, which in turn is due to the presence of the initial defects in the GaSb layer. At present, a typical medium wave absorption region material is an InAsSb body material without Ga, but the detection waveband of the InAsSb body material is less than 4.2 mu m, the detection window is narrow, and Sb components only account for 9% when the InAsSb body material is lattice-matched with a GaSb substrate, so that the beam current is small and difficult to control during actual growth. The InAs/InSb superlattice is used as an absorption region, the detection wave band can be expanded to 4.1-4.8 mu m, the technical problem that an InAsSb detection window is narrow is solved, meanwhile, the InAs/InSb superlattice is a superlattice formed by binary alloy, the thickness of an InAs layer and the thickness of an InSb layer are controlled well, and the problem of uneven component control is solved. Theoretically, due to the energy band positions of InAs and InSb, the InAs/InSb superlattice structure has excellent performance in a medium wave band, the conduction band top of InAs and the valence band bottom of InSb are also staggered, so that the InAs/InSb also has the advantages of the class II superlattice of InAs/GaSb, and has no intrinsic defects related to Ga. In addition, the mature molecular beam epitaxial growth technology of III-V group compounds can enable the growth rate and the components of each film layer material in the superlattice to be highly controllable, and provides technical support for the successful preparation of InAs/InSb strain II type superlattice.
At present, the GaSb-based InAs/InSb strain superlattice structure mainly comprises a GaSb layer, an InAs layer and an InSb layer. Wherein the As source and the Sb source are respectively provided by an As cracking furnace with a valve and an Sb cracking furnace with a valve. The reason why the growth difficulty of the InAs/InSb superlattice is large is that: (1) the lattice constant difference between InAs and InSb is too large, so that the InAs and the InSb are called as strain superlattices, and the stress brought by 1ML InSb needs about 9ML InAs to compensate, so that an InSb layer needs to be very thin, and a three-dimensional island structure is very easy to form during epitaxial growth, so that the formation of the InSb layer with good quality is very difficult; (2) as and Sb are easy to interdiffuse in the growth process to form InAsxSb1-x/InAsySb1-y(ii) a (3) In the epitaxial growth process of the superlattice, the growth speed of InSb is very slow, if the growth speed is fast, the InSb is easy to form islands, and if the growth speed is slow, the growth mode of InAs is unfavorable, so the growth speed of InAs and InSb is different, but the growth speed depends on the temperature of a source furnace, the temperature of the source furnace In a conventional MBE system is only 1 In source furnace, and the temperature of the source furnace cannot be changed within a short time for growing the superlattice.
Disclosure of Invention
The invention relates to a preparation method of an InAs/InSb strain superlattice material and the InAs/InSb strain superlattice material obtained based on the preparation method, which can at least solve part of defects in the prior art.
The invention relates to a method for preparing InAs/InSb strain superlattice material, which comprises the following steps,
s1, providing a substrate;
s2, epitaxially growing a buffer layer on the substrate;
s3, epitaxially growing a plurality of periods of InAs/InSb superlattice structures on the buffer layer, wherein each period of InAs/InSb superlattice structure comprises an InAs layer and an InSb layer, the InAs layer and the InSb layer are grown by a first In source furnace and a second In source furnace respectively, and the growth method of the InAs/InSb superlattice structure comprises the following steps:
s31, adjusting the first In source furnace and the second In source furnace to respective target temperatures, adjusting the As needle valve of the As source furnace and the Sb needle valve of the Sb source furnace to preset opening degrees respectively, opening the first In source furnace shutter and the As source furnace shutter, closing the other source furnace shutters, and keeping the state for t1 time;
s32, closing all source furnace shutters, and keeping the growth interruption state for t2 time;
s33, opening the Sb source furnace shutter and the second In source furnace shutter, and keeping the Sb source furnace shutter and the second In source furnace shutter In the opening state for t3 time;
s34, all source furnace shutters are closed, and the growth interruption state is kept for t4 time so as to enter the next growth cycle.
In one embodiment, the growth speed of the InAs layer is 0.4-0.6 ML/s, the growth speed of the InSb layer is 0.05-0.15 ML/s, and the target temperatures of the two In source furnaces are respectively adapted to the growth speeds of the InAs layer and the InSb layer;
the time t1 is 20-30 s;
the time t2 is 3-6 s;
the time t3 is 10-20 s;
the time t4 is 3-6 s.
In one embodiment, In S32, before closing all source furnace shutters, the As source furnace shutters are closed, and the first In source furnace shutter is kept open for 0.6 to 1.5S;
in S34, before closing all the source furnace shutters, the second In source furnace shutter is closed, and the Sb source furnace shutters are kept open for 0.6-1.5S.
In one embodiment, In S33, the Sb source furnace shutter and the second In source furnace shutter are opened by:
and opening the Sb source furnace shutter for 0.6-1.5 s, and then opening the second In source furnace shutter.
As an embodiment, in S2, the epitaxially growing a buffer layer on the substrate specifically includes:
s21, epitaxially growing a first buffer layer on the substrate and acquiring a reference temperature Tc of epitaxial growth;
and S22, growing a second buffer layer.
As one embodiment, in S21, the method for acquiring the reference temperature Tc includes:
the material of the first buffer layer is GaSb, after the growth of the first buffer layer is finished, the temperature of the substrate is reduced, the reconstruction change condition of the surface of the first buffer layer is observed, after the multiplied by 3 reconstruction of the surface of the first buffer layer is converted into the multiplied by 5 reconstruction and is kept stable, the temperature of the substrate is increased until the multiplied by 5 reconstruction of the surface of the first buffer layer is converted into the multiplied by 3 reconstruction, and the temperature of the substrate at the moment is taken as the reference temperature Tc.
As an embodiment, S22 specifically includes:
heating the substrate to a preset temperature, wherein the preset temperature is higher than the reference temperature Tc, and growing a second buffer layer at the preset temperature, wherein the second buffer layer is a GaSb buffer layer;
and after the second buffer layer is grown, closing a shutter of the Ga source furnace, and reducing the substrate temperature to the reference temperature Tc under the protection of Sb atmosphere to prepare for the growth of the InAs/InSb superlattice structure.
In one embodiment, the substrate is a substrate subjected to degassing and deoxidation treatment in S1.
The invention also relates to an InAs/InSb strain superlattice material, which is prepared by adopting the preparation method.
The invention has at least the following beneficial effects:
in the growth process of the InAs/InSb superlattice structure, two different In source furnaces are adopted, so that the speeds of two In sources can be respectively adjusted, the InAs/InSb superlattice structure is respectively suitable for the growth modes of an InAs layer and a thinner InSb layer, the formation of a three-dimensional island structure during the growth of the InAs/InSb superlattice is effectively avoided, the production efficiency of the InAs/InSb superlattice structure can be obviously improved, the production cost is reduced, and the quality and the performance of an InAs/InSb strain superlattice material are improved.
Drawings
In order to more clearly illustrate the embodiments of the present invention or the technical solutions in the prior art, the drawings used in the description of the embodiments or the prior art will be briefly described below, it is obvious that the drawings in the following description are only some embodiments of the present invention, and for those skilled in the art, other drawings can be obtained according to the drawings without creative efforts.
FIG. 1 is a schematic diagram of a source furnace shutter switching sequence in a single-cycle InAs/InSb superlattice structure growth procedure provided by an embodiment of the invention;
FIG. 2 is a RHEED (reflection high energy electron diffractometer) screenshot in the InAs/InSb strain superlattice growth process in the embodiment of the invention;
FIG. 3 is a high resolution X-ray diffraction (HRXRD) pattern of an InAs/InSb strained superlattice in an embodiment of the present invention;
fig. 4 is a schematic structural diagram of a molecular beam epitaxy apparatus according to an embodiment of the present invention.
Detailed Description
The technical solutions in the embodiments of the present invention are clearly and completely described below, and it is obvious that the described embodiments are only a part of the embodiments of the present invention, and not all embodiments. All other embodiments, which can be derived by a person skilled in the art from the embodiments given herein without making any creative effort, shall fall within the protection scope of the present invention.
Example one
The embodiment of the invention provides a preparation method of an InAs/InSb strain superlattice material, which comprises the following steps:
s1, providing a substrate;
s2, epitaxially growing a buffer layer on the substrate;
and S3, epitaxially growing a plurality of periods of InAs/InSb superlattice structures on the buffer layer, wherein each period of InAs/InSb superlattice structure comprises an InAs layer and an InSb layer, and different In source furnaces are adopted for growing the InAs layer and the InSb layer.
The substrate is used as a carrier of an epitaxial layer; preferably, the substrate is a GaSb substrate.
Further, the substrate is pretreated and then used in the subsequent process, and in one embodiment, the substrate is degassed and deoxidized, specifically:
in the molecular beam epitaxy apparatus 100, the GaSb substrate is transferred from the sample chamber to the buffer chamber for high temperature degassing; and conveying the degassed GaSb substrate to a growth chamber to remove the oxide layer. In the deoxidation treatment, the substrate temperature is raised to about 380 ℃, an Sb needle valve and an Sb source furnace shutter are opened, the temperature of the GaSb substrate is continuously raised to 700 ℃ under the protection of Sb atmosphere, and the temperature is kept for 10 minutes for deoxidation.
Preferably, in S2, the epitaxially growing the buffer layer on the substrate specifically includes:
s21, epitaxially growing a first buffer layer on the substrate and acquiring a reference temperature Tc of epitaxial growth;
and S22, growing a second buffer layer.
Preferably, the first buffer layer is a GaSb buffer layer; specifically, the deoxidized GaSb substrate is cooled to a preset temperature, and a first GaSb buffer layer is epitaxially grown on the substrate for a certain time; in one embodiment, the first buffer layer has a small thickness, the predetermined temperature is 680 ℃, the first GaSb buffer layer has a growth time of about 3 minutes, and the growth rate is 0.5 ML/s.
Preferably, the method for acquiring the reference temperature Tc includes:
and after the growth of the first buffer layer is finished, reducing the temperature of the substrate, observing the reconstruction change condition of the surface of the first buffer layer, raising the temperature of the substrate until the reconstruction of the layer multiplied by 3 on the surface of the first buffer layer is changed into the reconstruction of the layer multiplied by 5 and is kept stable, and taking the temperature of the substrate at the moment as the reference temperature Tc. In this embodiment, the reconstruction change can be observed using a reflection type high energy electron diffractometer 106.
Further, S22 specifically includes:
heating the substrate to a preset temperature, wherein the preset temperature is higher than Tc, and growing a second buffer layer at the preset temperature, wherein the second buffer layer is a GaSb buffer layer;
and after the second buffer layer is grown, closing the shutter of the Ga source furnace, and reducing the temperature of the substrate to the reference temperature under the protection of Sb to prepare for the growth of the InAs/InSb superlattice structure.
In one embodiment, the predetermined temperature is 680 ℃. For the growth of the second buffer layer, correspondingly opening the Ga source furnace shutter and the Sb source furnace shutter and adjusting the corresponding needle valve opening degree, and keeping the state for a certain time to grow the second GaSb buffer layer; optionally, the growth time of the second GaSb buffer layer is about 40min, and the thickness of the second GaSb buffer layer is 300-400 nm.
Further optimizing the preparation method, the InAs layer and the InSb layer are grown by adopting a first In source furnace 101 and a second In source furnace 102 respectively, and the InAs/InSb superlattice structure growth method comprises the following steps:
s31, adjusting the two In source furnaces to respective target temperatures, adjusting an As needle valve of the As source furnace 103 and an Sb needle valve of the Sb source furnace 104 to preset opening degrees respectively, opening a first In source furnace shutter and an As source furnace shutter, closing the other source furnace shutters, and keeping the state for t1 time;
s32, closing all source furnace shutters, and keeping the growth interruption state for t2 time;
s33, opening the Sb source furnace shutter and the second In source furnace shutter, and keeping the Sb source furnace shutter and the second In source furnace shutter In the opening state for t3 time;
s34, all source furnace shutters are closed, and the growth interruption state is kept for t4 time so as to enter the next growth cycle.
In the method, the residual V-group elements in the cavity can be reduced and the diffusion of As and Sb can be inhibited by controlling the opening and closing sequence of the shutter in the epitaxial process and combining the regulation and control modes of element infiltration, growth interruption and the like, so that the interface of the superlattice structure and the material quality are improved.
In the method, the time t 1-t 4 is mainly determined by the growth rate, and the growth rate is mainly determined by the temperature of the source furnace. In one embodiment, the target temperature adjusted by the two In source furnaces is within the range of 750-900 ℃, and the corresponding growth rates are as follows: 0.4-0.6 ML/s InAs layer and 0.05-0.15 ML/s InSb layer; on the basis, the time t1 is 20-30 s, the time t2 is 3-6 s, the time t3 is 10-15 s, and the time t4 is 3-6 s.
In S31, the Sb needle valve opening degree is preferably controlled within a relatively small range, for example, less than 30%; in one embodiment, the opening degree of the Sb needle valve is 15-25%. The opening degree of the As needle valve can be determined and adjusted according to specific conditions, such As the requirement of the thickness of the InAs layer, the requirement of the growth speed and the like.
Further, In S32, before closing all the source furnace shutters, the As source furnace shutters are closed, the first In source furnace shutter is kept open for 0.6-1.5S, and then the first In source furnace shutter is closed, even if all the source furnace shutters are closed. In S34, before closing all the source furnace shutters, the second In source furnace shutter is closed, the opening of the Sb source furnace shutter is kept for 0.6-1.5S, and then the second In source furnace shutter is closed, even if all the source furnace shutters are closed.
Further, In S33, the manner of opening the Sb source furnace shutter and the second In source furnace shutter is as follows:
and opening the Sb source furnace shutter for 0.6-1.5 s, and then opening the second In source furnace shutter.
In the method, after InAs grows up, a first In source furnace shutter is continuously opened for a certain time to enable the InAs surface to be In an In-rich state, then the growth is interrupted for a certain time to reduce the As pressure In the cavity, then an Sb source furnace shutter and a second In source furnace shutter are sequentially opened, the Sb source furnace shutter is opened firstly to carry out Sb infiltration, and the growth of an InSb layer can be regulated and controlled; therefore, the diffusion of As and Sb can be effectively suppressed, and the interface of the superlattice and the quality of the material can be improved.
In one embodiment, 100 periods of InAs/InSb superlattice structures are grown, namely S31-S34 which are repeatedly performed for 100 times.
In the method, InAs layers and InSb layers are alternately grown in sequence; in one embodiment, the thickness ratio of the InAs layer and the InSb layer is controlled to be (8-10): 1, and further preferably controlled at 9:1, so that the stress in the growth process of the InAs/InSb superlattice structure can be effectively controlled; in one embodiment, the thickness of the InAs layer is 11-13 ML, the thickness of the InSb layer is 1.2-1.4 ML, the growth speed of the InAs layer is 0.4-0.6 ML/s, and the growth speed of the InSb layer is 0.05-0.15 ML/s; further optionally, the thickness of the InAs layer is 12ML, the thickness of the InSb layer is 1.3ML, the growth rate of the InAs layer is 0.5ML/s, and the growth rate of the InSb layer is 0.1 ML/s.
In the preparation method provided by the embodiment, In the growth process of the InAs/InSb superlattice structure, two different In source furnaces are adopted, and the speeds of two In sources can be respectively adjusted to be suitable for the growth modes of the InAs layer and the thinner InSb layer, so that the formation of a three-dimensional island structure during the growth of the InAs/InSb superlattice is effectively avoided, the production efficiency of the InAs/InSb superlattice structure can be remarkably improved, the production cost is reduced, and the quality and the performance of an InAs/InSb strain superlattice material are improved.
Preferably, in the growth process of the InAs/InSb superlattice structure, the ratio of the V-group element beam to the III-group element beam is: As/In1=5~10，Sb/In2= 2-5, Sb/Ga = 3-12. In a more specific embodiment, As/In1=7.5，Sb/In2=3，Sb/Ga=5。
Example two
The following is a specific embodiment of the first example:
the embodiment provides a method for growing InAs/InSb strain superlattice material by molecular beam epitaxy, which comprises the following steps:
step 1: selecting a GaSb substrate as a carrier of an epitaxial layer;
step 2: degassing and deoxidizing the substrate;
(1) degassing: the GaSb substrate was loaded into the sample chamber of the molecular beam epitaxy apparatus 100 and subjected to a high temperature degassing treatment.
(2) And (3) deoxidation: transferring the degassed GaSb substrate into a growth chamber to remove an oxide layer, raising the substrate temperature to 380 ℃ at the heating rate of 30 ℃/min, opening the Sb needle valve to 77%, and opening the Sb source furnace shutterCorresponding beam current of 3.6X 10-6 And Torr, continuously heating the GaSb substrate to 700 ℃ under the protection of Sb atmosphere, and keeping the temperature for 10min for deoxidation. The temperature of the Ga source was increased to tip/base =1005/905 ℃ during deoxygenation.
And step 3: and growing a first GaSb buffer layer. And after the deoxidation is finished, cooling the temperature of the substrate to 680 ℃, opening the reflection type high-energy electron diffractometer 106, opening a Ga source furnace shutter when the temperature of the substrate is stabilized at 680 ℃, growing a first GaSb buffer layer with the thickness of 30nm, and then stopping the rotation of the substrate.
And 4, step 4: the reference temperature for epitaxial growth, i.e., the reconstruction temperature Tc, is determined. Adjusting the angle of the substrate to enable the multiplied by 3 reconstruction stripes on the surface of the GaSb to be clearly visible, then reducing the temperature of the substrate to 490 ℃, enabling the surface of the substrate to display clear multiplied by 5 reconstruction stripes, adjusting the temperature change rate to 5 ℃/min, and in turn, raising the temperature of the GaSb substrate again until the multiplied by 5 reconstruction stripes on the surface are converted into multiplied by 3 reconstruction stripes, determining the temperature 500 ℃ at the moment as the reconstruction temperature Tc of the GaSb, and taking the Tc as the reference temperature of epitaxial growth.
And 5: and raising the temperature of the substrate to 680 ℃ at a variable temperature rate of 30 ℃/min, changing the rotating speed to 10 revolutions per minute, and waiting for epitaxial growth.
Step 6: editing a growth program:
(1) the substrate temperature was set at 680 deg.C, Ga source temperature tip/base =1005/905 deg.C, and Sb needle valve was opened to 77%. And opening the Ga source furnace shutter and the Sb source furnace shutter, closing the other shutters, keeping for 40min, and growing a second GaSb buffer layer. Raising the temperature of the first In source furnace 101 and the second In source furnace 102 to tip/base =870/870 ℃ and 772/772 ℃ respectively during the growth of the second buffer layer;
(2) closing a shutter of the Ga source furnace, reducing the substrate temperature to Tc under the protection of Sb, and then changing the opening value of an Sb needle valve to 20 percent, wherein the corresponding beam current is 2.51 multiplied by 10-7 Torr, prepare to grow InAs/InSb II type superlattice. FIG. 1 is a schematic diagram of a shutter opening and closing sequence of a single InAs/InSb period;
(3) the As needle valve opening value is adjusted to 54 percent, and the corresponding beam current is 1.65 multiplied by 10-6Torr, Sb needle valve opening degree is still 20%, and the first In source furnace shutter and As source furnace shutter are opened and kept In this state 25s, the other shutters are closed;
(4) closing the As shutter, keeping the first In source furnace shutter to be continuously opened for 1s, and closing the rest shutters;
(5) all shutters are closed, and growth interruption is kept for 4 s;
(6) opening the Sb source furnace shutter, keeping for 1s, and closing the other shutters;
(7) simultaneously opening a second In source furnace shutter and an Sb source furnace shutter, keeping for 13s, and closing the other shutters;
(8) closing a second In source furnace shutter, keeping the Sb source furnace shutter to be continuously opened for 1s, and closing the other shutters;
(9) all shutters are closed, and growth interruption is kept for 4 s;
(10) repeating the processes (3) to (9) for 100 cycles, after the processes are completed, opening the Sb source furnace shutter, cooling the substrate temperature to 380 ℃ under the protection of Sb, changing the opening value of the Sb needle valve to 0, closing the Sb source furnace shutter, and continuously cooling the substrate temperature to 200 ℃;
(11) and (4) transferring the substrate out of the sample chamber, filling nitrogen into the sample chamber to break vacuum, and taking out the grown sample.
Fig. 2 is a RHEED screenshot in the growth process of the material of this embodiment, which shows a clear × 3 reconstruction and obvious stripes, and shows that the material state is two-dimensional growth and has a high flatness at this time.
Fig. 3 is a graph of InAs/InSb (12ML/1.3ML) superlattice high resolution X-ray diffraction (HRXRD) in this embodiment, and it can be seen that the satellite peak is clear and sharp, the half-peak width of the 1-order peak is only 43 arcsec, and the distance between the substrate peak and the superlattice 0-order peak is only 54 arcsec, which shows that the material quality is good and almost 0 lattice mismatch is achieved. The period thickness of the InAs/InSb (12ML/1.3ML) class ii superlattice in this embodiment is theoretically calculated as 40.56 a, and the actual period thickness of the material of this embodiment can be calculated as 39.96 a from the positive and negative 1-order peak positions in fig. 3, which are within the error range and meet the expected results. The data show that the InAs/InSb II type superlattice material is successfully prepared by the method, and the growth quality is higher.
EXAMPLE III
The embodiment of the invention provides an InAs/InSb strain superlattice material, and the InAs/InSb strain superlattice material is prepared by the preparation method provided by the first embodiment or the second embodiment.
Example four
Referring to fig. 4, an apparatus for performing the manufacturing method according to the first embodiment or the second embodiment of the present invention includes a molecular beam epitaxy device 100, and the molecular beam epitaxy device 100 includes a Ga source furnace 105, an Sb source furnace 104, an As source furnace 103, a first In source furnace 101, and a second In source furnace 102. Other structures of the molecular beam epitaxy apparatus 100 are conventional in the art and will not be described herein.
The above description is only for the purpose of illustrating the preferred embodiments of the present invention and is not to be construed as limiting the invention, and any modifications, equivalents, improvements and the like that fall within the spirit and principle of the present invention are intended to be included therein.
Claims (9)
1. A method for preparing InAs/InSb strain superlattice material is characterized by comprising the following steps,
s1, providing a substrate;
s2, epitaxially growing a buffer layer on the substrate;
s3, epitaxially growing a plurality of periods of InAs/InSb superlattice structures on the buffer layer, wherein each period of InAs/InSb superlattice structure comprises an InAs layer and an InSb layer, the InAs layer and the InSb layer are grown by a first In source furnace and a second In source furnace respectively, and the growth method of the InAs/InSb superlattice structure comprises the following steps:
s31, adjusting the first In source furnace and the second In source furnace to respective target temperatures, adjusting the As needle valve of the As source furnace and the Sb needle valve of the Sb source furnace to preset opening degrees respectively, opening the first In source furnace shutter and the As source furnace shutter, closing the other source furnace shutters, and keeping the state for t1 time;
s32, closing all source furnace shutters, and keeping the growth interruption state for t2 time;
s33, opening the Sb source furnace shutter and the second In source furnace shutter, and keeping the Sb source furnace shutter and the second In source furnace shutter In the opening state for t3 time;
s34, all source furnace shutters are closed, and the growth interruption state is kept for t4 time so as to enter the next growth cycle.
2. The method for preparing an InAs/InSb strained superlattice material as claimed in claim 1, wherein:
the growth speed of the InAs layer is 0.4-0.6 ML/s, the growth speed of the InSb layer is 0.05-0.15 ML/s, and the target temperatures of the two In source furnaces are respectively adapted to the growth speeds of the InAs layer and the InSb layer;
the time t1 is 20-30 s;
the time t2 is 3-6 s;
the time t3 is 10-20 s;
the time t4 is 3-6 s.
3. The method for preparing an InAs/InSb strained superlattice material as claimed in claim 1, wherein:
in S32, before closing all source furnace shutters, closing As source furnace shutters, and keeping the first In source furnace shutter open for 0.6-1.5S;
in S34, before closing all the source furnace shutters, the second In source furnace shutter is closed, and the Sb source furnace shutters are kept open for 0.6-1.5S.
4. The method for preparing an InAs/InSb strained superlattice material as claimed In claim 1, wherein In S33, the manner of opening the Sb source furnace shutter and the second In source furnace shutter is as follows:
and opening the Sb source furnace shutter for 0.6-1.5 s, and then opening the second In source furnace shutter.
5. The method for preparing an InAs/InSb strained superlattice material as claimed in claim 1, wherein in S2, epitaxially growing a buffer layer on the substrate specifically comprises:
s21, epitaxially growing a first buffer layer on the substrate and acquiring a reference temperature Tc of epitaxial growth;
and S22, growing a second buffer layer.
6. The method for preparing an InAs/InSb strained superlattice material as claimed in claim 5, wherein in S21, the method for obtaining the reference temperature Tc comprises:
the material of the first buffer layer is GaSb, after the growth of the first buffer layer is finished, the temperature of the substrate is reduced, the reconstruction change condition of the surface of the first buffer layer is observed, after the multiplied by 3 reconstruction of the surface of the first buffer layer is converted into the multiplied by 5 reconstruction and is kept stable, the temperature of the substrate is increased until the multiplied by 5 reconstruction of the surface of the first buffer layer is converted into the multiplied by 3 reconstruction, and the temperature of the substrate at the moment is taken as the reference temperature Tc.
7. The method for preparing an InAs/InSb strained superlattice material as claimed in claim 5, wherein S22 specifically comprises:
heating the substrate to a preset temperature, wherein the preset temperature is higher than the reference temperature Tc, and growing a second buffer layer at the preset temperature, wherein the second buffer layer is a GaSb buffer layer;
and after the second buffer layer is grown, closing a shutter of the Ga source furnace, and reducing the substrate temperature to the reference temperature Tc under the protection of Sb atmosphere to prepare for the growth of the InAs/InSb superlattice structure.
8. The method for preparing an InAs/InSb strained superlattice material as claimed in claim 1, wherein: in S1, the substrate is a substrate after degassing and deoxidizing.
9. An InAs/InSb strain superlattice material is characterized in that: the InAs/InSb strain superlattice material is prepared by the preparation method of any one of claims 1 to 8.
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