CN112510113B - Method for enhancing photoluminescence signal of antimony-based superlattice material - Google Patents
Method for enhancing photoluminescence signal of antimony-based superlattice material Download PDFInfo
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- 239000000463 material Substances 0.000 title claims abstract description 91
- 238000000034 method Methods 0.000 title claims abstract description 24
- 238000005424 photoluminescence Methods 0.000 title claims abstract description 24
- 230000002708 enhancing effect Effects 0.000 title claims abstract description 13
- 229910052787 antimony Inorganic materials 0.000 title abstract description 6
- WATWJIUSRGPENY-UHFFFAOYSA-N antimony atom Chemical compound [Sb] WATWJIUSRGPENY-UHFFFAOYSA-N 0.000 title abstract description 6
- 229910005542 GaSb Inorganic materials 0.000 claims abstract description 89
- 239000000758 substrate Substances 0.000 claims abstract description 38
- 238000001816 cooling Methods 0.000 claims abstract description 17
- 238000010438 heat treatment Methods 0.000 claims abstract description 13
- 238000000137 annealing Methods 0.000 claims abstract description 9
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Chemical compound O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims abstract description 5
- 229910000673 Indium arsenide Inorganic materials 0.000 claims description 24
- RPQDHPTXJYYUPQ-UHFFFAOYSA-N indium arsenide Chemical compound [In]#[As] RPQDHPTXJYYUPQ-UHFFFAOYSA-N 0.000 claims description 23
- 230000001681 protective effect Effects 0.000 claims description 12
- 229910017115 AlSb Inorganic materials 0.000 claims description 3
- WPYVAWXEWQSOGY-UHFFFAOYSA-N indium antimonide Chemical compound [Sb]#[In] WPYVAWXEWQSOGY-UHFFFAOYSA-N 0.000 claims description 3
- 238000012360 testing method Methods 0.000 abstract description 7
- 238000001514 detection method Methods 0.000 abstract description 3
- 230000001276 controlling effect Effects 0.000 description 10
- 230000006798 recombination Effects 0.000 description 6
- 238000005215 recombination Methods 0.000 description 6
- 238000001451 molecular beam epitaxy Methods 0.000 description 5
- 238000000103 photoluminescence spectrum Methods 0.000 description 4
- 239000013078 crystal Substances 0.000 description 3
- 238000004020 luminiscence type Methods 0.000 description 2
- 238000004519 manufacturing process Methods 0.000 description 2
- 230000005855 radiation Effects 0.000 description 2
- 230000004044 response Effects 0.000 description 2
- 239000004065 semiconductor Substances 0.000 description 2
- 230000009466 transformation Effects 0.000 description 2
- 230000007547 defect Effects 0.000 description 1
- 238000007872 degassing Methods 0.000 description 1
- 230000006866 deterioration Effects 0.000 description 1
- 239000003814 drug Substances 0.000 description 1
- 239000012212 insulator Substances 0.000 description 1
- 239000002184 metal Substances 0.000 description 1
- 238000012986 modification Methods 0.000 description 1
- 230000004048 modification Effects 0.000 description 1
- 238000000628 photoluminescence spectroscopy Methods 0.000 description 1
- 230000000704 physical effect Effects 0.000 description 1
- 238000007781 pre-processing Methods 0.000 description 1
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- 239000000126 substance Substances 0.000 description 1
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- 238000001931 thermography Methods 0.000 description 1
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Abstract
The invention discloses a method for enhancing photoluminescence signals of an antimony-based superlattice material, which comprises the following steps of: pretreating the GaSb substrate to remove water vapor and organic matters; heating the GaSb substrate, and removing an oxide layer of the GaSb substrate at high temperature; cooling the GaSb substrate, and growing a GaSb buffer layer on the GaSb substrate; heating the GaSb buffer layer and then annealing; cooling the GaSb buffer layer, and growing the Sb-based superlattice material on the GaSb buffer layer by controlling the growth temperature, the growth rate, the beam ratio and the growth interface; and cooling the GaSb layer grown on the surface of the Sb-based superlattice material to take out the Sb-based superlattice material. By carrying out photoluminescence test on the Sb-based superlattice material, photoluminescence signals are greatly enhanced, the peak position of a luminous peak is clear, the half-peak width is small, and the band gap of the superlattice material can be accurately tested, so that the Sb-based superlattice material can be widely applied to infrared photoelectric devices, and the detection precision of the infrared photoelectric devices is improved.
Description
Technical Field
The invention relates to the technical field of semiconductor infrared detectors, in particular to a method for enhancing photoluminescence signals of Sb-based superlattice materials.
Background
The infrared thermal imaging has the characteristics of strong anti-interference performance, long identification distance, thermal radiation detection and the like, and is widely applied to the fields of security, industry, medicine, automatic driving and the like in recent years.
The infrared photoelectric device is made of wide range of materials, and metal, insulator and superconductor can be used for making infrared detector. Wherein, the antimony (symbol Sb) based superlattice material has special physical properties which are very suitable for manufacturing infrared photoelectric devices. The Sb-based superlattice infrared detector can respond to light radiation from near infrared to short-wave infrared, medium-wave infrared, long-wave infrared and far infrared through energy band engineering, can effectively inhibit Auger recombination, and improves the performance and the working temperature of the infrared detector. In addition, Sb-based materials are considered to be one of the most ideal materials for manufacturing the new generation of infrared focal plane detectors due to low cost, good stability and uniformity.
The response wavelength is an important indicator of an infrared detector. And the band gap of the Sb-based superlattice material determines the response wavelength of an infrared detector prepared from the Sb-based superlattice material. Therefore, the bandgap test is an indispensable part of characterizing Sb-based superlattice materials. The most common method for characterizing the band gap of semiconductor materials is photoluminescence spectroscopy. However, the Sb-based superlattice material has serious surface recombination, so that photoluminescence signals are weakened, the photoluminescence signals are not obvious, and the positions of luminescence peaks and the band gaps of the superlattice material are difficult to determine.
Disclosure of Invention
Aiming at the defects of the prior art, the technical problem to be solved by the invention is to provide a method for enhancing photoluminescence signals of an antimony-based superlattice material so as to reduce surface recombination, improve luminous peak intensity and accurately test a bandgap of the superlattice material.
In order to achieve the purpose, the invention adopts the following technical scheme:
the embodiment of the invention provides a method for enhancing photoluminescence signals of an Sb-based superlattice material, which comprises the following steps of:
pretreating the GaSb substrate to remove water vapor and organic matters;
heating the GaSb substrate, and removing an oxide layer of the GaSb substrate at high temperature;
cooling the GaSb substrate, and growing a GaSb buffer layer on the GaSb substrate;
heating the GaSb buffer layer and then annealing;
cooling the GaSb buffer layer, and growing the Sb-based superlattice material on the GaSb buffer layer by controlling the growth temperature, the growth rate, the beam ratio and the growth interface;
and cooling the GaSb layer grown on the surface of the Sb-based superlattice material to take out the Sb-based superlattice material.
Preferably, the GaSb substrate is a GaSb (100) substrate.
Preferably, when the oxide layer of the GaSb substrate is removed at high temperature, the GaSb substrate needs to be heated, Sb protective beams are opened at 400 ℃, the heating is continued, and the oxide is removed in the range of 540-580 ℃.
Preferably, when the GaSb buffer layer grows on the GaSb substrate, the temperature needs to be reduced to 500 ℃ to grow the GaSb buffer layer, and the Sb/Ga beam ratio ranges from 8 to 12; the growth thickness is 100 nm-2 μm.
Preferably, the conditions for heating the GaSb buffer layer and annealing are that the temperature is increased to 510-530 ℃ and high-temperature annealing is carried out for 3 min-2 h.
Preferably, when the Sb-based superlattice material grows on the GaSb buffer layer, the Sb/Ga beam current ratio and the As/In beam current ratio range from 2 to 8; GaSb and InAs growth rates of
The growth thickness is 10-300 cycles; the growth interface is an InSb type interface.
Preferably, the Sb-based superlattice material comprises one or a combination of InAs/Ga (in) Sb, InAs/AlSb and InAs/InAsSb.
Preferably, the thickness of the GaSb layer grown on the surface of the Sb-based superlattice material is
Preferably, when the Sb-based superlattice material is taken out through cooling, the Sb-based superlattice material is taken out after the Sb-based superlattice material is cooled in the Sb protective atmosphere, the Sb protective beam is closed when the temperature is reduced to 400 ℃, and the Sb-based superlattice material is taken out after the temperature is continuously reduced to below 150 ℃.
By adopting the method for enhancing the photoluminescence signal of the antimony-based superlattice material, disclosed by the embodiment of the invention, the Sb-based superlattice material grows on the GaSb buffer layer by controlling the growth temperature, the growth rate, the beam ratio and the growth interface, so that the strain of the superlattice material can be adjusted, and the quality of superlattice crystals is prevented from being deteriorated due to strain relaxation; meanwhile, a layer of wide-band-gap GaSb material grows on the surface of the superlattice material at low temperature, so that the surface recombination of the superlattice material can be effectively inhibited, and a photoluminescence signal is enhanced. By carrying out photoluminescence test on the superlattice material, photoluminescence signals are greatly enhanced, the peak position of a luminous peak is clear, the half-peak width is small, and the band gap of the superlattice material can be accurately tested, so that the Sb-based superlattice material can be widely applied to infrared photoelectric devices, and the detection precision of the infrared photoelectric devices 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 embodiments of the present invention, and for those skilled in the art, other drawings can be obtained according to the provided drawings without creative efforts.
FIG. 1 is a schematic flow chart of a method for enhancing photoluminescence signals of Sb-based superlattice materials according to the invention;
FIG. 2 is a schematic flow chart of another method for enhancing photoluminescence signals of Sb-based superlattice materials provided by the invention;
FIG. 3 is a photoluminescence spectrum of a medium-wave InAs/GaSb superlattice material provided by the invention;
FIG. 4 is a photoluminescence spectrum of the long-wave InAs/GaSb superlattice material provided by the invention.
Detailed Description
The technical solutions in the embodiments of the present invention will be clearly and completely described below with reference to the drawings in the embodiments of the present invention, and it is obvious that the described embodiments are only a part of the embodiments of the present invention, and not all of the 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.
As shown in fig. 1, the method for enhancing photoluminescence signals of Sb-based superlattice materials provided by the present invention comprises the following steps:
step 101, preprocessing the GaSb substrate to remove water vapor and organic matters. In this step, a GaSb (100) substrate is used as the GaSb substrate. The GaSb (100) substrate is loaded into a molecular beam epitaxy system (MBE) sample chamber, enters a buffer chamber after degassing treatment, and enters a growth chamber.
And 102, removing the oxide layer of the GaSb substrate at high temperature. In the step, the GaSb substrate in the growth chamber is heated to a preset temperature, then the Sb protective beam is opened, the temperature is continuously raised, and when the temperature is in the range of 540-580 ℃, different types of oxides can be removed.
And 103, cooling to grow a GaSb buffer layer on the GaSb substrate. The Sb/Ga beam ratio of the grown GaSb buffer layer ranges from 8 to 12; the growth thickness is 100 nm-2 μm.
And 104, heating the GaSb buffer layer for annealing treatment. And (3) continuously raising the temperature on the basis of the temperature reduction in the step 103, raising the temperature by 10-30 ℃, and then annealing at high temperature for 3 min-2 h.
And 105, cooling the GaSb buffer layer, and growing the Sb-based superlattice material on the GaSb buffer layer by controlling the growth temperature, the growth rate and the beam current ratio. Wherein, the GaSb buffer layer is cooled to the temperature near the reconstruction transformation point again, and the Sb-based superlattice material grows. Controlling the Sb/Ga beam current ratio and the As/In beam current ratio to be 2-8 In the growth process of the Sb-based superlattice material, wherein the growth rates of GaSb and InAs are
The growth thickness of the superlattice material is 10-300 cycles. The Sb-based superlattice material may be an Sb-based superlattice material such as InAs/Ga (in) Sb, InAs/AlSb, InAs/InAsSb and the like.
And 106, growing a GaSb layer on the surface of the Sb-based superlattice material, and cooling to take out the Sb-based superlattice material. Wherein, after the growth of the Sb-based superlattice material is finished, a GaSb layer continues to grow, and the thickness is
Here, a GaSb layer is grown on the surface of the Sb-based superlattice material. The GaSb layer is a wide band gap, so that the surface recombination of the Sb-based superlattice material can be inhibited, and a photoluminescence signal is enhanced. And (3) when the temperature is reduced in the Sb protective atmosphere, closing the Sb protective beam when the temperature reaches a certain temperature, and then continuously reducing the temperature to be below 150 ℃ to take out the Sb-based superlattice material. It should be noted here that the Sb protection beam current is not turned off until step 107 after the Sb protection beam current is turned on in step 102. Then scribing the Sb-based superlattice material, and measuring the Sb-based superlattice material by a photoluminescence spectrometerAnd (6) testing.
The technical content of the present invention will be further described in detail with reference to a specific embodiment. Referring to fig. 2, the method for enhancing the photoluminescence signal of the Sb-based superlattice material provided in the embodiment of the present invention specifically includes the following steps:
step 201, a GaSb (100) substrate is loaded into a molecular beam epitaxy system (MBE) sample chamber.
Step 202, the GaSb (100) substrate enters a growth chamber after being degassed through a sample chamber and a buffer chamber.
And step 203, heating the GaSb (100) substrate, opening the Sb protective beam at 400 ℃, continuing to heat, and respectively staying the GaSb (100) substrate at 540 ℃ and 560 ℃ for 5min and 15min to remove the oxide layer.
And step 204, cooling to 500 ℃, and growing a GaSb buffer layer on the GaSb (100) substrate, wherein the Sb/Ga beam flow ratio is 10, and the growth thickness is 0.5 mu m.
Step 205, heating to 520 ℃, and annealing at high temperature for 15 min;
in step 206, the temperature is reduced to the vicinity of the temperature of the reconstruction transformation point again, and the InAs/Ga (in) Sb superlattice material is grown.
Step 207, controlling the Sb/Ga beam current ratio and As/In beam current ratio range to be 4 In the growth of InAs/Ga (In) Sb superlattice material, and controlling the growth rate of GaSb to be
InAs growth rate of
The source furnace in the growth chamber is controlled by a computer, and the interface of the superlattice material is controlled to be an InSb type interface by regulating and controlling the opening and closing sequence and time of a baffle of the source furnace. The strain of the InAs/Ga (in) Sb superlattice material can be adjusted by controlling the interface of the superlattice material, and the deterioration of the superlattice crystal quality caused by strain relaxation is prevented. The superlattice material is grown to a thickness of 100 periods thick.
Step 208, after the InAs/Ga (in) Sb superlattice material is grown, a GaSb layer is continuously grown to the thickness of
And 209, cooling in the Sb protective atmosphere, closing the Sb protective beam when the temperature is 400 ℃, and continuously cooling to below 150 ℃ to take out the InAs/Ga (in) Sb superlattice material.
Step 210, scribing the InAs/Ga (in) Sb superlattice material to meet the test requirement, and testing by using a photoluminescence spectrometer. Fig. 3 and 4 respectively show photoluminescence spectra of the InAs/GaSb superlattice material generated by the method of the embodiment of the invention at different wavelengths. As can be seen from the figure, the peak position of the photoluminescence spectrum luminescence peak of the InAs/GaSb superlattice material generated by the invention is clear and the half-peak width is small no matter in medium wave or long wave, so that the band gap of the InAs/GaSb superlattice material can be accurately tested and obtained.
Based on the above, the method for enhancing the photoluminescence signal of the Sb-based superlattice material provided by the embodiment of the present invention removes water vapor and organic substances by pretreating the GaSb substrate in the molecular beam epitaxy system; then removing the oxide layer at high temperature in a growth chamber, and growing a high-quality GaSb buffer layer; and then cooling to grow the Sb-based superlattice material on the GaSb buffer layer. The Sb-based superlattice material can obtain an optimized growth condition by controlling the growth temperature, the growth rate and the beam current ratio, and then the strain of the superlattice material is adjusted by controlling an interface, so that the quality of the superlattice crystal is prevented from being deteriorated due to strain relaxation; finally, a layer of wide-band-gap GaSb material grows on the surface of the superlattice material at low temperature, so that the surface recombination of the superlattice material can be effectively inhibited, and a photoluminescence signal is enhanced.
The previous description of the disclosed embodiments is provided to enable any person skilled in the art to make or use the present invention. Various modifications to these embodiments will be readily apparent to those skilled in the art, and the generic principles defined herein may be applied to other embodiments without departing from the spirit or scope of the invention. Thus, the present invention is not intended to be limited to the embodiments shown herein but is to be accorded the widest scope consistent with the principles and novel features disclosed herein.
Claims (9)
1. A method for enhancing photoluminescence signals of Sb-based superlattice materials is characterized by comprising the following steps:
pretreating the GaSb substrate to remove water vapor and organic matters;
heating the GaSb substrate, and removing an oxide layer of the GaSb substrate at high temperature;
cooling the GaSb substrate, and growing a GaSb buffer layer on the GaSb substrate;
heating the GaSb buffer layer and then annealing;
cooling the GaSb buffer layer, and growing the Sb-based superlattice material on the GaSb buffer layer by controlling the growth temperature, the growth rate, the beam ratio and the growth interface;
and cooling the GaSb layer grown on the surface of the Sb-based superlattice material to take out the Sb-based superlattice material.
2. The method of claim 1, wherein the GaSb substrate is a GaSb (100) substrate.
3. The method according to claim 1, wherein the GaSb substrate is heated when the oxide layer of the GaSb substrate is removed at a high temperature, the Sb protective beam is turned on at 400 ℃, the heating is continued, and the oxide is removed at a temperature ranging from 540 ℃ to 580 ℃.
4. The method according to claim 1, wherein when growing the GaSb buffer layer on the GaSb substrate, the temperature is reduced to 500 ℃ to grow the GaSb buffer layer, and the Sb/Ga beam ratio is in a range of 8-12; the growth thickness is 100 nm-2 μm.
5. The method according to claim 1, wherein the annealing treatment is carried out by heating the GaSb buffer layer to 510-530 ℃ for 3 min-2 h.
6. The method according to claim 1, wherein when the Sb-based superlattice material is grown on the GaSb buffer layer, the Sb/Ga beam flow ratio and the As/In beam flow ratio are both In the range of 2-8; GaSb and InAs growth rates of
The growth thickness is 10-300 cycles; the growth interface is an InSb type interface.
7. The method of claim 1 or 6, wherein the Sb-based superlattice material comprises one or a combination of InAs/ga (in) Sb, InAs/AlSb, InAs/InAsSb.
8. The method of claim 1, wherein the thickness of the GaSb layer grown on the surface of the Sb-based superlattice material is
9. The method according to claim 1, wherein the temperature of the Sb-based superlattice material is reduced to be taken out, the Sb-based superlattice material is required to be reduced in an Sb protective atmosphere, the Sb protective beam is closed when the temperature is reduced to 400 ℃, and the Sb-based superlattice material is taken out after the temperature is continuously reduced to be below 150 ℃.
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| CN208422929U (en) * | 2018-05-02 | 2019-01-22 | 嘉兴风云科技有限责任公司 | A kind of II-class superlattices infrared detector absorption plot structure |
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| CN208422929U (en) * | 2018-05-02 | 2019-01-22 | 嘉兴风云科技有限责任公司 | A kind of II-class superlattices infrared detector absorption plot structure |
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