Abstract
In this paper, high quality InAs/InAsSb(Ga-free) type-II superlattice were grown on GaSb substrates by molecular beam epitaxy. The superlattice layers structure consists of 100 periods with 3.8 nm thick InAs layers and 1.4 nm InAs0.66Sb0.34 layers. A specific spike-like defect was found during experiment. The epitaxial layer was characterized and analyzed by high-resolution x-ray diffraction (HRXRD), atomic force microscope (AFM) and Fourier transform infrared spectroscopy (FTIR). The results show that the optimized sample is almost zero lattice mismatched, the FWHM of the zeroth order SL peak is 39.3 arcsec, the RMS surface roughness achieves around 1.72Å over an area of 10 μm×10 μm. The FTIR absorption spectrum shows a 50% cutoff wavelength of 4.28 μm. And PL spectrum shows that the peak of InAs/InAs0.66Sb0.34 SL is at 4.58 μm. These initial results indicate that the grown InAs/InAsSb SL is stable and reproducible, and thus it is worthy of further investigation.
After more than half a century of development, infrared detectors have made great progress by developing infrared detectors and focal planes based on a series of material systems such as HgCdTe, InSb, quantum well and Type-II superlattices (T2SLs). Type-II superlattices have been identified as one of the most promising types of alternative materials
InAs/InAsSb and InAs/GaSb T2SLs have a lot in common: first of all, they both can achieve lattice matching with GaSb substrates (InAs/InAsSb requires adjustment of components); Then, they can cover most of the infrared spectrum; Besides, they both respond to the infrared signal by electron-absorbing photons from the top of the hole microstrip to the bottom of the electronic microstrip. Changing the composition and thickness of the superlattice can adjust the microstrip position and band gap width, thus achieving a similar effect of adjusting the band gap width of the bulk material.
In general, InAs/InAsSb T2SLs are relatively simple to grow, and

Fig.1 Schematic illustration of mechanical shutter sequences used in growing (a) InAs/GaSb and (b) InAs/InAsSb superlattices.
图1 (a) InAs/GaSb和(b) InAs/InAsSb超晶格生长时的简要快门序列
In order to better absorb photons, in the structural design, the periodic thickness of the superlattice needs to be as thin as possible. The increase in Sb components causes the superlattice to produce a compressive strain, requiring more InAs to produce tensile strain to compensate, which in turn causes the InAs layer to thicken, resulting in a thickening of the overall period thickness. Therefore, these parameters should be taken into account when designing the structure to achieve the desired result. In this paper, we use molecular beam epitaxy (MBE) to grow InAs/InAsSb strain-balanced type-II superlattices directly on GaSb substrates, which provides an idea condition for the stable and repeatable growth of InAs/InAsSb T2SLs and lays a solid foundation for the follow-up device research.
MBE(molecular beam epitaxy) is a powerful technique for epitaxial growth with excellent crystalline quality, good compositional and doping uniformity. Given the ability to precisely actuate the shutter sequences, MBE has been successfully applied for superlattice growth where the layer thickness needs to be under perfect control. The doping levels can also be controlled with high precisio


Fig.2 The GaSb substrate surface reconstitution diffraction stripe varies with substrate temperature. (a) 2×5, (b) 1×3
图2 GaSb衬底表面再构条纹随衬底温度的变化 (a) 2×5, (b) 1×3
Ga-free / T2SLs can be strain-balanced on GaSb by adjusting the appropriate combinations of layer thicknesses and alloy compositions. Typically, the tensile strain in InAs is compensated by the compressive strain introduced in leading to a thicker InAs layer compared to the InAsSb one (for antimony concentration > 0.18)
For all the samples, surface morphology was characterized by digital S–II Nano Navi atomic force microscope (AFM) in tapping mode at room temperature in air. The JV-QC3 HRXRD was employed to identify the strain, composition and growth quality of superlattice. The optical properties was measured by Thermo Scientific Nicolet iS-50 Fourier transform infrared spectroscopy (FTIR).
If the InAs/InAs1-xSbx superlattice is regarded as an InAsSb bulk material, it can be calculated that the Sb component in InAs1-xSbx occupies 9% of the total amount of group V elements when matching to a GaSb substrate. However, the Sb component in the InAs1-xSbx layer we designed accounts for 34% and contains more InSb bonds, so it is not appropriate to use high substrate temperature for the InAs/InAs1-xSbx superlattice. And the V/III beam equivalent pressure(BEP)flux ratio was set to about 6 for As:In, 3.1 for Sb:In, based on the theoretical composition. The mechanical shutter sequence during growth is shown in

Fig.3 The mechanical shutter sequence during growth (Contains InSb interface)
图3 生长时的源炉快门开关顺序(插入InSb界面)

Fig. 4 AFM image of spike-like defects in an area of 10µm×10µm:Tc+15°C Tc Tc-15°C Tc-25°C
图4 在10µm×10µm范围内的尖峰状缺陷AFM图像

Fig. 5 Trend of the number of spike-like defects with temperature in a 10µm×10µm area
图5 在10µm×10µm范围尖峰状缺陷数量随温度的变化趋势
Several experiments were carried out to change the Sb:In BEP flux ratio while keeping the As:In BEP flux ratio unchanged. Three sets of InAs/InAsSb SLs (S1, S2, S3) with the same As:In BEP flux ratio of 6 but different Sb:In BEP flux ratio of 3.1, 2, and 1 were grown, respectively. The lattice matching of the samples was analyzed by the HRXRD and the results are shown in

Fig. 6 The high-resolution x-ray diffraction (HRXRD) of the three sets of InAs/InAsSb SLs samples with the BEP flux ratio. S1: Sb/In=3.1, S2: Sb/In=2, S3: Sb/In=1.
图6 不同Ⅴ/Ⅲ比下的InAs/InAsSb超晶格的HRXRD图谱。S1: Sb/In=3.1, S2: Sb/In=2, S3: Sb/In=1.
It can be clearly seen from the above XRD diffraction pattern that the strain is getting closer to the GaSb substrate peak as the Sb:In BEP flux ratio is reduced. The strain between the GaSb substrate peak and the InAs/InAsSb SL zero order peak are (S1) -494 arcsec, (S2) -305 arcsec, (S3) -207 arcsec, respectively. However, even the Sb:In BEP flux ratio is reduced to 1, it still shows compressive strain, indicating that antimony component is greater than 9% in total InAs/InAs1-xSbx SL. There are two reasons resulting in this situation: ① The concentration of the group V element required to grow the best GaSb buffer layer is too high, while the group V concentration required to grow the InAs1-xSbx layer is relatively low. So that the strain of the superlattice is difficult to control; ② Due to the accuracy of the device, the shutter time of 0.5s cannot be accurately controlled, which also caused the background density of antimony to increase. In order to solve the problem of excessive Sb content, the growth process was optimized. We simulated the HRXRD pattern containing the InSb interfacial structure and compared it with the measurement of S3, as shown in


Fig. 7 (a) HRXRD of measurement (black) and simulations (red) of InAs/InAs0.66Sb0.34 SL.:(b) Structure used for HRXRD simulation before shutter sequence optimization
图7 (a) InAs/InAs0.66Sb0.34 超晶格的HRXRD实测(黑)和模拟(红)图谱:(b) 用于HRXRD模拟图的结构(快门顺序优化前)

Fig. 8 The images of the mechanical shutter sequence of each sources cell shutter.( Uninsert InSb interface)
图8 生长时的源炉快门开关顺序(不插入InSb界面)
By removing the 0.5s InSb shutter before and after growing the InAsSb layer , the Sb content was effectively controlled. We still grew three sets of samples (S4, S5, S6) with Sb:In: 3.1, 2, and 1, respectively, and the XRD images are shown in


Fig. 9 (a) HRXRD of three sets of samples with different Sb/In: S1, Sb/In=1; S2, Sb/In=2; S3, Sb/In=3.1; (b) Variation of strain and xsb with Sb/In in InAs/InAs1-xSbx superlattices.
图9 (a) 三组不同Sb/In样品的HRXRD图谱:S1, Sb/In=1; S2, Sb/In=2; S3, Sb/In=3.1;(b) InAs/InAs1-xSbx超晶格中应变和Sb组分随Sb/In的变化
Through the spectral analysis of XRD, the periodic thickness of the superlattice can be calculated by the distance between the adjacent satellite peaks produced by symmetrical diffraction, as shown in
, | (1) |
where D is the periodic thickness, is the wavelength of incident X-ray beam (=1.5406Å), is the separation distance between two adjacent satellite peaks and (30.3634°) is the Bragg angle of the GaSb substrate. was took as the distance between the +1 order peak (the abscissa is 3615 arcsec) and the +2 order peak (the abscissa is 7225 arcsec), and the calculated period thickness of S1 is 51.01Å, which is within the allowable error range of the expected design period thickness.
When the material grows on the substrate, within the elastic range, the lattice grows coherently, which for an atom means that it is stretched or compressed along the growth direction (assumed to be the Z direction), and its vertical strain satisfies
, | (2) |
, | (3) |
where and represent the lattice growth direction (vertical direction), and is the lattice constant of the epitaxial film and substrate, respectively. is the Poisson ratio of the epitaxial film. Δ = - is the distance between the diffraction peak of the epitaxial film and the substrate peak, is the position of the main peak of the superlattice (0th-order peak).
Epitaxial layers are generally considered lattice matched when the peak separation is below 100 arcseconds, or 0.0825% for GaSb substrates


Fig. 10 (a) HRXRD of S1 (black) and simulations (red) of InAs/InAs0.66Sb0.34 SL. The inset shows the separation between the GaSb substrate and SL 0th-order peak.:(b) Structure used for HRXRD simulation after shutter sequence optimization
图10 样品S1的HRXRD实测(黑)和模拟(红)图谱,内嵌图:超晶格0级峰和衬底峰的间距; (b) 用于HRXRD模拟图的结构(快门顺序优化后)
During the growth of InAs/InAs1-xSbx T2SL, substrate temperature has a great influence on the structural quality and optical properties



Fig. 11 AFM images of (a)Tc-15°C, (b)Tc, (c)Tc+15°C InAs/InAs0.66Sb0.34 SL samples surface morphology over 10µm×10µm.
图11 不同生长温度下,InAs/InAs0.66Sb0.34超晶格的AFM图像(10µm×10µm): (a)Tc-15°C, (b)Tc, (c)Tc+15°C
Through AFM analysis, the evolution of the surface morphology was studied. It can be seen from

Fig. 12 The variation trend of 0th-order peak FWHM values and surface RMS roughness at different growth temperatures.
图12 不同生长温度下,零级峰半峰宽和表面均方根粗糙度的变化趋势
In terms of optical properties, the FTIR absorption spectrum and photoluminescence spectra were used to determine the cutoff wavelength or band gap of the sample.

Fig. 13 The FTIR absorption spectrum of InAs/InAs0.66Sb0.34 superlattice.
图13 InAs/InAs0.66Sb0.34超晶格的FTIR吸收谱

Fig. 14 PL spectrum of the InAs/InAs0.66Sb0.34 SL at different temperatures.
图14 InAs/InAs0.66Sb0.34超晶格在不同测试温度下的PL谱
In summary, we have investigated the growth conditions and optical properties of InAs/InAs0.66Sb0.34 type-II superlattice on GaSb substrates by molecular beam epitaxy. Experimental results demonstrate that a suitable and stable V/III BEP flux ratio and substrate temperature are essential for obtaining reproducibly grown InAs/InAsSb superlattices. When V/III BEP flux ratio was As:In=6 and Sb:In=1, with optimized proper growth procedures, the separation between the InAs/InAsSb SL 0 th-order peak and the substrate is only 44 arcsec, almost reaching zero lattice mismatch. The FWHM of the first order SL peak is 42 arcsec in HRXRD pattern. When the optimized growth temperature is Tc, the FWHM of the zeroth order SL peak is 39.3 arcsec, the RMS surface roughness achieves around 1.72Å over an area of 10µm×10 µm. The FTIR absorption spectrum shows the 50% cut-off wavelength is 4.28 µm and the whole absorption edge is relatively smooth. And PL spectrum shows that the peak of InAs/InAs0.66Sb0.34 SL is at 4.58 μm. The above results show that the high-quality strain-balanced InAs/InAsSb type II superlattice was prepared. Therefore, our experimental process and results may be useful for further experimental and theoretical studies on infrared detectors based on InAs/InAsSb superlattice.
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