CN115627529A - Low-temperature deoxidation method for GaSb substrate and preparation method for HgCdSe epitaxial material - Google Patents
Low-temperature deoxidation method for GaSb substrate and preparation method for HgCdSe epitaxial material Download PDFInfo
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- 239000000758 substrate Substances 0.000 title claims abstract description 125
- 229910005542 GaSb Inorganic materials 0.000 title claims abstract description 103
- 238000000034 method Methods 0.000 title claims abstract description 67
- 239000000463 material Substances 0.000 title claims abstract description 44
- 238000002360 preparation method Methods 0.000 title claims abstract description 25
- 230000008569 process Effects 0.000 claims abstract description 31
- 238000002128 reflection high energy electron diffraction Methods 0.000 claims description 12
- 238000010438 heat treatment Methods 0.000 claims description 11
- 238000001816 cooling Methods 0.000 claims description 10
- 238000002347 injection Methods 0.000 claims description 8
- 239000007924 injection Substances 0.000 claims description 8
- 238000012544 monitoring process Methods 0.000 claims description 6
- 230000008859 change Effects 0.000 claims description 5
- 238000005507 spraying Methods 0.000 claims description 5
- 239000007921 spray Substances 0.000 claims description 2
- 230000003247 decreasing effect Effects 0.000 claims 1
- 238000005516 engineering process Methods 0.000 abstract description 6
- 239000012535 impurity Substances 0.000 abstract description 5
- IPBWGTSZTNICPQ-UHFFFAOYSA-N [Se].[Cd].[Hg] Chemical compound [Se].[Cd].[Hg] IPBWGTSZTNICPQ-UHFFFAOYSA-N 0.000 abstract description 2
- 238000001451 molecular beam epitaxy Methods 0.000 description 10
- SKJCKYVIQGBWTN-UHFFFAOYSA-N (4-hydroxyphenyl) methanesulfonate Chemical compound CS(=O)(=O)OC1=CC=C(O)C=C1 SKJCKYVIQGBWTN-UHFFFAOYSA-N 0.000 description 8
- 239000000243 solution Substances 0.000 description 7
- 239000011669 selenium Substances 0.000 description 6
- 229910000661 Mercury cadmium telluride Inorganic materials 0.000 description 5
- 230000009286 beneficial effect Effects 0.000 description 4
- 238000010586 diagram Methods 0.000 description 4
- 239000013078 crystal Substances 0.000 description 3
- 238000004519 manufacturing process Methods 0.000 description 3
- 229910004611 CdZnTe Inorganic materials 0.000 description 2
- 238000001465 metallisation Methods 0.000 description 2
- 229910005191 Ga 2 O 3 Inorganic materials 0.000 description 1
- 229910052793 cadmium Inorganic materials 0.000 description 1
- DGJPPCSCQOIWCP-UHFFFAOYSA-N cadmium mercury Chemical compound [Cd].[Hg] DGJPPCSCQOIWCP-UHFFFAOYSA-N 0.000 description 1
- 230000015556 catabolic process Effects 0.000 description 1
- 238000006243 chemical reaction Methods 0.000 description 1
- 150000001875 compounds Chemical class 0.000 description 1
- 230000008094 contradictory effect Effects 0.000 description 1
- 238000000354 decomposition reaction Methods 0.000 description 1
- 230000007547 defect Effects 0.000 description 1
- 230000007123 defense Effects 0.000 description 1
- 238000007872 degassing Methods 0.000 description 1
- 238000006731 degradation reaction Methods 0.000 description 1
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- 238000001514 detection method Methods 0.000 description 1
- 230000007613 environmental effect Effects 0.000 description 1
- VTGARNNDLOTBET-UHFFFAOYSA-N gallium antimonide Chemical compound [Sb]#[Ga] VTGARNNDLOTBET-UHFFFAOYSA-N 0.000 description 1
- 238000012986 modification Methods 0.000 description 1
- 230000004048 modification Effects 0.000 description 1
- 230000000704 physical effect Effects 0.000 description 1
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- 239000004065 semiconductor Substances 0.000 description 1
- 239000000126 substance Substances 0.000 description 1
- 229910052714 tellurium Inorganic materials 0.000 description 1
- PORWMNRCUJJQNO-UHFFFAOYSA-N tellurium atom Chemical compound [Te] PORWMNRCUJJQNO-UHFFFAOYSA-N 0.000 description 1
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Abstract
The invention belongs to the technical field of selenium-cadmium-mercury infrared detectors, and provides a substrate low-temperature deoxidation technology and a preparation method of an epitaxial material. The Ga beam is adopted to carry out low-temperature deoxidation treatment on the GaSb substrate, and the process of Sb beam high-temperature deoxidation treatment in the prior art is replaced, so that the GaSb substrate for the epitaxial preparation of the HgCdSe material is thoroughly deoxidized under the protection of the Sb-free beam, and the pollution of Sb elements to the HgCdSe epitaxial layer is reduced. The deoxidation treatment of the GaSb substrate is carried out under the low-temperature condition, so that the initial temperature of the preparation process of the HgCdSe epitaxial material is greatly reduced, the background impurity concentration of the MBE cavity is favorably reduced, and the electrical property of the HgCdSe epitaxial material is improved.
Description
Technical Field
The invention belongs to the technical field of HgCdSe infrared detectors, and particularly relates to a low-temperature deoxidation process method for a GaSb substrate and a preparation method for a HgCdSe epitaxial material.
Background
Infrared detection as a high-precision technology has important and wide application in numerous fields such as aerospace, environmental monitoring, national defense safety and the like. The selenium cadmium mercury (HgCdSe) is a ternary compound semiconductor material similar to the traditional tellurium cadmium mercury (HgCdTe), and has potential application value in the technical development field of infrared detectors. HgCdSe shares many similarities with HgCdTe materials in terms of basic physical properties: the two can realize the adjustment of the forbidden band width by adjusting the ratio of Cd to Hg, and the band gap adjustment range of the HgCdSe material is 0-1.7 eV; both of them have higher electron mobility and minority carrier lifetime, theoretically, better electrical properties can be obtained. The traditional high-quality HgCdTe material is usually prepared on a tellurium-zinc-cadmium (CdZnTe) substrate matched with the crystal lattice of the HgCdTe material, and the cost of the HgCdTe detector is high because the manufacturing cost of the CdZnTe substrate is extremely high and the crystal rounding production is difficult to realize. However, the HgCdSe material is lattice-matched with a relatively mature gallium antimonide (GaSb) substrate, which is easy to implement wafer batch preparation, and can greatly reduce the manufacturing cost of the infrared detector. At present, the mainstream preparation method of the HgCdSe material is to perform Molecular Beam Epitaxy (MBE) on a GaSb substrate with a (211) crystal face. The preparation method comprises the specific steps of degassing and deoxidizing a GaSb substrate, growing a zinc telluride (ZnTe) buffer layer on the GaSb substrate, and finally growing HgCdSe with different components.
However, there is a native oxide layer on the surface of the GaSb substrate, mainly comprising Ga 2 O 3 And Sb 2 O 3 Before MBE growth, the GaSb substrate surface must be subjected to a deoxidation treatment. The traditional GaSb deoxidation mode is realized by utilizing the decomposition and desorption of oxide on the surface of a substrate at high temperature, namely, the thermal deoxidation (TOD) technology is adopted, and the deoxidation temperature of GaSb is usually higher than 580 ℃. In the thermal deoxidation process, a higher Sb beam current is generally required to protect the surface of the GaSb substrate to prevent the subsequent epitaxial layer lattice defects from greatly rising due to rich metallization of the substrate surface due to GaSb pyrolysis. However, for the HgCdSe material, the high-temperature deoxidation method under the protection of Sb beam current has two disadvantages: firstly, sb element is an effective doping source of the HgCdSe material, and the use of Sb element for protection in the deoxidation process of a GaSb substrate can pollute an MBE growth cavity and influence the background impurity concentration of the HgCdSe materialResulting in degradation of electrical properties; secondly, the deoxidation temperature of the GaSb substrate is usually higher than the growth temperature of the ZnTe buffer layer and the HgCdSe epitaxial layer by more than 250 ℃, and the excessive deoxidation temperature can cause the further increase of the background impurity concentration of the cavity and is not beneficial to the control of the background concentration of the HgCdSe epitaxial layer. Therefore, a scheme is needed to solve the problems in the prior art, and the development of a low-temperature deoxidation technology under the Sb-free protection condition of a GaSb substrate is beneficial to the preparation of HgCdSe epitaxial materials.
Therefore, there is a need to provide a technical solution to solve the above technical problems in the prior art.
Disclosure of Invention
The invention provides a low-temperature deoxidation technology for a GaSb substrate and a preparation method for an HgCdSe epitaxial material, which can at least solve part of problems in the prior art.
To solve the above technical problem, according to an aspect of the present invention, the present invention provides the following technical solutions:
a process method for low-temperature deoxidation of a GaSb substrate comprises the following steps:
s1: heating the GaSb substrate, and keeping the substrate rotating in the heating process;
s2: jetting the surface of the GaSb substrate by using Ga beams;
s3: observing whether the deoxidation of the GaSb substrate is complete;
s4: and if the deoxidation of the GaSb substrate is complete, stopping the injection of the Ga beam, and keeping for a certain time to finish the deoxidation of the GaSb substrate.
As a preferred scheme of the process method for low-temperature deoxidation of the GaSb substrate, the process method comprises the following steps: and S3, monitoring the surface diffraction image change of the GaSb substrate by adopting a reflection high-energy electron diffraction device, and if clear reconstruction stripes appear in the reflection high-energy electron diffraction image of the GaSb substrate, completely deoxidizing the GaSb substrate.
As a preferred scheme of the process method for low-temperature deoxidation of the GaSb substrate, the process method comprises the following steps: in the step S1, the substrate heating temperature is 470-490 ℃, and the rotating speed is 5-20 r/min.
As described in the inventionA preferable scheme of a process method for low-temperature deoxidation of a GaSb substrate is disclosed, wherein: in the step S2, the Ga beam current in the growth cavity is (1-2) multiplied by 10 -7 Torr, and the spraying time is 1 to 2s.
As a preferred scheme of the process method for low-temperature deoxidation of the GaSb substrate, the process method comprises the following steps: the holding time in step S4 is 2-3 min.
As a preferred scheme of the process method for low-temperature deoxidation of the GaSb substrate, the process method comprises the following steps: the step S2 specifically includes:
s21: adopting Ga beam to spray the surface of the GaSb substrate for a certain time;
s22: closing the Ga beam and pausing for a certain time;
the steps S21, S22 are repeated several times.
As a preferred scheme of the process method for low-temperature deoxidation of the GaSb substrate, the process method comprises the following steps: in the step S2, the duration is 1-2S, and the pause time is 15-20S.
In order to solve the above technical problem, according to another aspect of the present invention, the present invention provides the following technical solutions:
a preparation method of HgCdSe epitaxial material is characterized by comprising the following steps: the method comprises the following steps:
s5: cooling the deoxidized GaSb substrate by the process method, and keeping for a certain time;
s6: growing a buffer layer on the GaSb substrate;
s7: cooling the substrate, and growing Hg with required thickness on the basis of the buffer layer 1～x Cd x And (3) Se epitaxial material.
The preferable scheme of the preparation method of the HgCdSe epitaxial material is as follows: and in the step S5, the temperature is reduced to 310-330 ℃, and the holding time is 3-5 min.
The preferable scheme of the preparation method of the HgCdSe epitaxial material is as follows: the thickness of the buffer layer in step S6 is 200-300 nm.
As a preferred scheme of the preparation method of the HgCdSe epitaxial material, the preparation method comprises the following steps: step by stepIn the step S7, the temperature is reduced to 60-130 ℃, hg 1～x Cd x The range of Cd component x in the Se epitaxial material is 0.18-0.37.
The invention has the following beneficial effects:
1. because the GaSb substrate is deoxidized in the Ga beam environment, the high-temperature Sb beam deoxidizing treatment of the GaSb substrate in the prior art is avoided, the GaSb substrate for the epitaxial preparation of the HgCdSe material is thoroughly deoxidized under the protection of Sb-free beams, and the pollution of Sb elements to the HgCdSe epitaxial layer is reduced.
2. The method can realize deoxidation treatment of the GaSb substrate under the condition of low temperature, so that the initial temperature of the preparation process of the HgCdSe epitaxial material is greatly reduced, the background impurity concentration of the MBE cavity is favorably reduced, and the electrical property of the HgCdSe epitaxial material is 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 structures shown in the drawings without creative efforts.
FIG. 1 is a schematic view of a temperature control curve for an epitaxial substrate according to the present invention;
FIG. 2 is a schematic diagram illustrating the control of a Ga source switch in the deoxidation process of the GaSb substrate according to the present invention;
FIG. 3 is a typical RHEED diffraction reconstruction pattern during the deoxidation process of the GaSb substrate of the present invention;
FIG. 4 shows the Atomic Force Microscope (AFM) morphology of 300nm buffer layer grown on deoxidized GaSb substrate.
The implementation, functional features and advantages of the objects of the present invention will be further explained with reference to the accompanying drawings.
Detailed Description
The following will clearly and completely describe the technical solutions in the embodiments, 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.
It should be noted that, if directional indications (such as up, down, left, right, front, and back … …) are involved in the embodiment of the present invention, the directional indications are only used to explain the relative position relationship between the components, the motion situation, and the like in a specific posture (as shown in the drawing), and if the specific posture is changed, the directional indication is changed accordingly.
In addition, if there is a description of "first", "second", etc. in an embodiment of the present invention, the description of "first", "second", etc. is for descriptive purposes only and is not to be construed as indicating or implying relative importance or implicitly indicating the number of technical features indicated. Thus, a feature defined as "first" or "second" may explicitly or implicitly include at least one such feature. In addition, technical solutions between various embodiments may be combined with each other, but must be realized by a person skilled in the art, and when the technical solutions are contradictory or cannot be realized, such a combination should not be considered to exist, and is not within the protection scope of the present invention.
The invention provides a low-temperature deoxidation method for a GaSb substrate and a preparation method for an HgCdSe epitaxial material, which can realize that the GaSb substrate is thoroughly deoxidized under the protection of Sb-free beam, reduce the pollution of Sb elements to the HgCdSe epitaxial layer, and greatly reduce the initial temperature of the preparation process of the HgCdSe epitaxial material, thereby being beneficial to reducing the background impurity concentration of an MBE cavity and improving the electrical property of the HgCdSe epitaxial material.
Taking fig. 1-2 as an example, fig. 1 shows a schematic diagram of a temperature control curve of a GaSb substrate in a process of preparing an HgCdSe epitaxial material, and fig. 2 shows a schematic diagram of switching control of a Ga source in a process of performing surface deoxidation on the GaSb substrate.
A preparation method of HgCdSe epitaxial material comprises the following steps:
the method comprises the following steps of (1) loading a GaSb substrate into a growth cavity of a Molecular Beam Epitaxy (MBE) system, and monitoring the surface diffraction image change of the GaSb substrate by adopting a reflection high-energy electron diffraction (RHEED) device;
heating the GaSb substrate at 470-490 deg.c while maintaining the rotation speed of 5-20 rpm;
using (1-2) × 10 -7 The Ga beam current of Torr is 0-t 1 Spraying the GaSb substrate surface within the time, wherein the spraying time is 1-2 s;
closing Ga beam at t 1 -t 2 Pausing for 15-20 s within the time;
repeating the step of Ga beam injection and the step of closing Ga beam and pausing for N times, or not repeating the step of Ga beam injection and the step of closing Ga beam and pausing until clear reconstruction stripes appear in RHEED images of the GaSb substrate, indicating that the GaSb substrate is completely deoxidized, and stopping the injection of Ga beam to complete the deoxidation treatment of the GaSb substrate;
closing the Ga beam, keeping for 2-3 min, and completing the deoxidation of the GaSb substrate;
subjecting the low-temperature deoxidized GaSb substrate to t 2 -t 3 Cooling to 310-330 ℃ within a period of time, and keeping for 3-5 min;
t 3 -t 4 growing a buffer layer on the GaSb substrate within the time, wherein the thickness of the buffer layer is 200-300 nm;
to the substrate at t 4 -t 5 Cooling to 60-130 deg.C within a certain time, and growing Hg with the thickness required by the device on the basis of the buffer layer 1～x Cd x Se epitaxial material for t 4 -t 5 ，Hg 1～x Cd x The range of Cd component x in the Se epitaxial material is 0.18-0.37.
The invention provides a low-temperature deoxidation technology of a GaSb substrate without Sb beam protection and a preparation method of HgCdSe epitaxial material 2 O 3 And Sb 2 O 3 React at a certain temperature to form volatile Ga 2 O and monoSb, gaseous Ga 2 O is pumped away by an MBE vacuum system, the simple substance Sb is bound on the surface of the substrate by Ga atoms, and finally the deoxidation treatment of the GaSb substrate is realized. The excessive Ga atoms sprayed on the surface of the GaSb substrate can cause excessive Ga atoms participating in the reaction on the surface of the substrate to be rich in metallization. Therefore, the Ga atoms are sprayed under the condition of lower beam current, and proper pause is introduced to help the Ga atoms to migrate and react on the surface of the substrate; and the oxide on the surface of the substrate is thoroughly removed by adopting multiple times of spraying and stopping of Ga atoms.
Because the growth temperature of the HgCdSe epitaxial layer and the buffer layer is lower than 350 ℃, under the low-temperature condition, the adhesion coefficient of Ga atoms is about equal to 1, and the saturated vapor pressure is lower than 10 -12 Torr, so that MBE epitaxial samples hold residual Ga atoms almost negligible for the background concentration of HgCdSe epitaxial layer.
Example 1
A process method for low-temperature deoxidation of a GaSb substrate comprises the following steps:
the method comprises the following steps of (1) loading a GaSb substrate into a growth cavity of a Molecular Beam Epitaxy (MBE) system, and monitoring the surface diffraction image change of the GaSb substrate by adopting a reflection high-energy electron diffraction (RHEED) device;
heating the GaSb substrate at 470 ℃, wherein the substrate is kept rotating at a rotating speed of 10 r/min in the heating process;
using 1X 10 -7 Jetting the surface of the GaSb substrate by the Ga beam of Torr for 1s;
closing the Ga beam, stopping 15s, and stopping the injection of the Ga beam, wherein clear reconstruction stripes appear in the RHEED image of the GaSb substrate;
closing the Ga beam, keeping for 2min, and finishing the deoxidation treatment of the GaSb substrate.
Example 2
A process method for low-temperature deoxidation of a GaSb substrate comprises the following steps:
the method comprises the following steps of (1) loading a GaSb substrate into a growth cavity of a Molecular Beam Epitaxy (MBE) system, and monitoring the surface diffraction image change of the GaSb substrate by adopting a reflection high-energy electron diffraction (RHEED) device;
heating the GaSb substrate at 490 ℃, wherein the substrate is kept rotating at a rotating speed of 10 r/min in the heating process;
using a 2X 10 -7 Injecting the Ga beam of Torr on the surface of the GaSb substrate for 1-2 s;
closing the Ga beam and pausing for 20s;
repeating the step of Ga beam injection and the step of closing the Ga beam and pausing for 3 times, wherein clear reconstruction stripes appear in RHEED images of the GaSb substrate, and the Ga beam injection is stopped;
closing the Ga beam, keeping for 3min, and finishing the deoxidation treatment of the GaSb substrate.
Fig. 3 shows the RHEED diffraction reconstructed image of the GaSb substrate after deoxidation treatment in example 2, and it can be seen from fig. 3 that obvious reconstructed clear stripes appear on the substrate surface after deoxidation treatment of the GaSb substrate, which shows that after the GaSb substrate is treated by the Ga beam, the oxide layer on the substrate surface has been completely removed, and the deoxidation treatment of the substrate is realized.
Example 3
A preparation method of HgCdSe epitaxial material comprises the following steps:
cooling the low-temperature deoxidized GaSb substrate obtained in the embodiment 1 to 310 ℃ and keeping the temperature for 3min;
growing a ZnTe buffer layer of zinc telluride on a GaSb substrate, wherein the thickness of the buffer layer is 200nm;
cooling the substrate to 60 ℃, and growing Hg with the thickness required by the device on the basis of the buffer layer 1～x Cd x And (3) Se epitaxial material.
Example 4
A preparation method of HgCdSe epitaxial material comprises the following steps:
cooling the low-temperature deoxidized GaSb substrate obtained in example 2 to 330 ℃ and keeping for 5min;
growing a ZnTe zinc telluride buffer layer on a GaSb substrate, wherein the thickness of the buffer layer is 300nm;
cooling the substrate to 130 ℃, and growing Hg with the thickness required by the device on the basis of the buffer layer 1～x Cd x And (3) Se epitaxial material.
Fig. 4 is a morphology diagram of the buffer layer 300nm ZnTe deposited on the GaSb substrate and detected by an atomic force microscope in example 4, and it can be seen from the figure that after the buffer layer is deposited on the GaSb substrate processed by the Ga beam, the obtained buffer layer has low film roughness and good film uniformity.
The above description is only a preferred embodiment of the present invention, and not intended to limit the scope of the present invention, and all modifications and equivalents of the present invention, which are made by the present specification and directly/indirectly applied to other related technical fields within the spirit of the present invention are included in the scope of the present invention.
Claims (10)
1. A process method for low-temperature deoxidation of a GaSb substrate is characterized by comprising the following steps:
s1: heating the GaSb substrate, and keeping the substrate rotating in the heating process;
s2: jetting the surface of the GaSb substrate by using Ga beams;
s3: observing whether the deoxidation of the GaSb substrate is complete;
s4: and if the deoxidation of the GaSb substrate is complete, stopping the injection of the Ga beam, and keeping for a certain time to finish the deoxidation of the GaSb substrate.
2. The process method for deoxidizing a GaSb substrate at a low temperature as claimed in claim 1, wherein in step S3, a reflection high-energy electron diffraction device is used for monitoring the surface diffraction image change of the GaSb substrate, and if clear reconstruction stripes appear in the reflection high-energy electron diffraction image of the GaSb substrate, the deoxidation of the GaSb substrate is complete.
3. The process method for low-temperature deoxidation of the GaSb substrate according to claim 1, wherein in the step S1, the substrate heating temperature is 470-490 ℃ and the rotation speed is 5-20 r/min.
4. The process method for low-temperature deoxidation of GaSb substrate according to claim 1, wherein in step S2, the Ga beam current is (1-2) x 10 -7 Torr, and the spraying time is 1-2 s。
5. The process method for low-temperature deoxidation of the GaSb substrate according to claim 1, wherein the holding time in the step S4 is 2-3 min.
6. The process method for low-temperature deoxidation of the GaSb substrate according to claim 1, wherein the step S2 specifically comprises:
s21: adopting Ga beam to spray the surface of the GaSb substrate for a certain time;
s22: closing the Ga beam and pausing for a certain time;
the steps S21, S22 are repeated several times.
7. The process method for low-temperature deoxidation of the GaSb substrate according to claim 6, wherein the duration time in the step S2 is 1-2S, and the dwell time is 15-20S.
8. A preparation method of HgCdSe epitaxial material is characterized by comprising the following steps: the method comprises the following steps:
s5: cooling the deoxidized GaSb substrate by the process method of any one of claims 1 to 7, and keeping the substrate for a certain time;
s6: growing a buffer layer on the GaSb substrate;
s7: cooling the substrate, and growing Hg with required thickness on the basis of the buffer layer 1～x Cd x And (3) Se epitaxial material.
9. The method for preparing HgCdSe epitaxial material of claim 8, wherein the temperature is decreased to 310-330 ℃ in step S5, and the temperature is maintained for 3-5 min.
10. The method for preparing HgCdSe epitaxial material as claimed in claim 8, wherein the temperature is reduced to 60-130 ℃ in step S7, and Hg is Hg 1～x Cd x The range of Cd component x in the Se epitaxial material is 0.18-0.37.
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