J. Semicond. > 2024, Volume 45 > Issue 3 > 031301
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REVIEWS

Development of in situ characterization techniques in molecular beam epitaxy

Chao Shen1, 3, Wenkang Zhan1, 2, Manyang Li1, 2, Zhenyu Sun1, 2, , Jian Tang4, Zhaofeng Wu3, Chi Xu5, Bo Xu1, 2, Chao Zhao1, 2, and Zhanguo Wang1, 2

+ Author Affiliations

 Corresponding author: Zhenyu Sun, zsun@semi.ac.cn; Chao Zhao, zhaochao@semi.ac.cn

DOI: 10.1088/1674-4926/45/3/031301

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Abstract: Ex situ characterization techniques in molecular beam epitaxy (MBE) have inherent limitations, such as being prone to sample contamination and unstable surfaces during sample transfer from the MBE chamber. In recent years, the need for improved accuracy and reliability in measurement has driven the increasing adoption of in situ characterization techniques. These techniques, such as reflection high-energy electron diffraction, scanning tunneling microscopy, and X-ray photoelectron spectroscopy, allow direct observation of film growth processes in real time without exposing the sample to air, hence offering insights into the growth mechanisms of epitaxial films with controlled properties. By combining multiple in situ characterization techniques with MBE, researchers can better understand film growth processes, realizing novel materials with customized properties and extensive applications. This review aims to overview the benefits and achievements of in situ characterization techniques in MBE and their applications for material science research. In addition, through further analysis of these techniques regarding their challenges and potential solutions, particularly highlighting the assistance of machine learning to correlate in situ characterization with other material information, we hope to provide a guideline for future efforts in the development of novel monitoring and control schemes for MBE growth processes with improved material properties.

Key words: epitaxial growth, thin film, in situ characterization, molecular beam epitaxy (MBE)



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Fig. 1.  (Color online) In situ characterization techniques applied in MBE.

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Fig. 2.  (Color online) STM images of filled states obtained after sequential depositions at 500 °C: (a) 0.6 ML ErSb on a GaSb (001) surface, followed by (b) 2 ML of GaSb, and then followed by (c) an additional 0.6 ML ErSb. STM images acquired after depositing additional GaSb on the surface shown in (a). (d) 4 ML of GaSb and (e) 10 ML of GaSb. Higher-resolution STM insets (10 nm × 10 nm) reveal the surface reconstruction of the ErSb sites, with (a–c) showing exposed ErSb and (d-e) showing GaSb coverage over the ErSb sites. Reproduced with permission. Ref. [44] Copyright 2013, American Chemical Society.

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Fig. 3.  (Color online) (a) STM image of the modulated honeycomb $ \sqrt{7} $ × $ \sqrt{7} $ superstructure with a close-up in the bottom left corner. (b) The LEED pattern of (a). (c) Schematic representation of one-sixth of the pattern, where filled dots represent the hidden (0, 0) spot and integer-order spots, and open circles represent spots corresponding to the $ \sqrt{7} $ × $ \sqrt{7} $ superstructure (in red), the $ \sqrt{19} $ × $ \sqrt{19} $ superstructure (in green), and the 5 × 5 superstructure (in blue). Reproduced with permission. Ref. [48].

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Fig. 4.  (Color online) STM image of c(6 × 12) reconstructions on wurtzite GaN($000\bar{1} $). Reproduced with permission. Ref. [38] Copyright 2014, AIP Publishing.

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Fig. 5.  (Color online) In situ AFM images for as-grown NiO on Ni(110) in (a) air, (b) water, and (c) 10 mM Pb-contained solution for 15 h. MBE-grown NiO on MgO(001) in (d) air, (e) water, and (f) 10 mM Pb-contained solution for 15 h. Reproduced with permission. Ref. [58].

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Fig. 6.  SnS on graphene substrates as a function of temperature as observed by LEEM. Reproduced with permission. Ref. [60] Copyright 2018, American Chemical Society.

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Fig. 7.  (Color online) RHEED patterns taken after the growth of (a) CaTi5O11 and (b) TiO2-B films on (001) SrTiO3 substrates. Reproduced with permission. Ref. [66].

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Fig. 8.  (Color online) RHEED patterns, corresponding STM images, and modeled patterns of GaN films deposited with different I/A ratios. Reproduced with permission. Ref. [54].

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Fig. 9.  (Color online) RHEED patterns of Fe1−xZnx films deposited on MgO (001) substrates: (a) and (b) pure Fe, (c) and (d) low Zn concentration, (e) and (f) moderate Zn concentration with α to Γ phase transition and (g) and (h) Fe0.29Zn0.71 with Γ phase. Reproduced with permission. Ref. [81] Copyright 2011, AIP Publishing.

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Fig. 10.  (Color online) (a) RHEED images of the SrTiO3(001) substrate. RHHED images of the SrCoO2.5 grown on substrate with different Co/Sr ratios: (b) Co/Sr = 1.00, (c) Co/Sr = 1.30, and (d) Co/Sr = 0.90. Reproduced with permission. Ref. [88].

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Fig. 11.  REELS spectra, RHEED patterns, and AFM images of AlN: (a) a smooth surface, (b) a rougher surface. Reproduced with permission. Ref. [70] Copyright 2011, AIP Publishing.

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Fig. 12.  Evolution of LEED patterns of coronene monolayers on Cu(110) surface during (A−G) the heating and (H) cooling process. Reproduced with permission. Ref. [102] Copyright 2010, American Chemical Society.

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Fig. 13.  (Color online) Typical LEED patterns of the silicene-stanene on Ag(111) during hetero-epitaxy. (a) Post preparation at incident energy. (b) After Si deposition. (c) After Sn deposition. (d) After non-reactive Al2O3 encapsulation. Reproduced with permission. Ref. [105].

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Fig. 14.  (Color online) Specular rod for LSAT(001) measured with X-rays and calculated profiles. (a) Calculated rod for AO-terminated LSAT Substrates with varying La0.18Sr0.82O surface coverage. (b) Calculated rod with varying topmost plane displacement relative to the bulk LSAT lattice parameter at growth temperature. (c) Calculated rod accounting for both surface coverage and surface relaxation. Reproduced with permission. Ref. [117].

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Fig. 15.  (Color online) Selected XRD spectra of the sub-free SDD-GaSe film during pressurization. Reproduced with permission. Ref. [127].

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Fig. 16.  (Color online) Diffraction intensity as a function of time, in nanowires annealed at 610 °C. Reproduced with permission. Ref. [130] Copyright 2019, American Chemical Society.

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Fig. 17.  (Color online) Results of the in situ XANES measurements. (a) The single-phase brownmillerite-structured SrCoO2.5. (b) Two-phase brownmillerite-structured SrCoO2.5 and Sr3Co2O6±δ films. Reproduced with permission. Ref. [119] Copyright 2018, American Chemical Society.

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Fig. 18.  (Color online) Layer-dependent STS reveals the transition from semiconductor to semimetal as the layer number increases from one to six in PtSe2 on highly oriented pyrolytic graphite (HOPG). Reproduced with permission. Ref. [147] Copyright 2021, Wiley-VCH GmbH.

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Fig. 19.  (Color online) Desorption during the growth of InxGa1–xN/GaN nanowires by MBE. (a) Calibration of full desorption and background pressure at 800 °C, with the growth of a segment at 604 °C. (b) Comparison of InxGa1–xN quantum well (QW) (blue line) and extended NW segment (red line) growth at the same temperature. (c) In desorption during InxGa1–xN QW growth at different substrate temperatures. Reproduced with permission. Ref. [151] Copyright 2012, American Chemical Society.

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Fig. 20.  (Color online) (a) Valence band maximum measured by UPS for Cu2O with nominal thickness of 42 nm. (b) Core-level energy spectrum measured by XPS for Cu2O with nominal thickness of 42 nm. Reproduced with permission. Ref. [162].

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Fig. 21.  (Color online) A series of ARPES spectra of YbAl3 was collected along the (0, 0) to (0, π) direction at kz ≈ Γ, spanning temperatures from 255 down to 21 K. Reproduced with permission. Ref. [168].

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Fig. 22.  (Color online) (a) Angle-integrated photoemission spectroscopy (PES) of various SIO−STO SLs and the SIO-214 film. The dotted black line represents the Fermi energy (EF), while the blue (orange) shaded region corresponds to the peak position of the Jeff = 1/2 (Jeff = 3/2) bands. (b) Schematic model illustrating the bandwidth-control Mott transition in SIO−STO SLs and the SIO-214 film. Reproduced with permission. Ref. [184].

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Fig. 23.  (Color online) (a) In situ reflectivity profiles of samples B to E, exhibiting significant variations in GR and N/In ratio. (b) The extracted 1 st reflectivity profiles of samples B to E during ($ 11\bar{2} 0$) a-plane InN growth. Reproduced with permission. Ref. [192] Copyright 2015, Elsevier B.V.

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Fig. 24.  (Color online) Statistics of in situ characterization techniques involved in publications in recent years.

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Table 1.   A summary of the advantages, disadvantages, and functions of characterization technologies.

Technique Advantages Disadvantages Functions
STM High spatial resolution; morphology and electronic structure analysis Limited to conductive samples, requires ultra-high vacuum Surface morphology, electronic structure analysis
SEM High depth of field, for conductive and non-conductive samples Lower resolution than STM, sample preparation challenges Morphology analysis of various samples
AFM High resolution in both lateral and vertical directions Relatively slow imaging, tip wear and contamination effects Surface morphology analysis, material property studies
LEEM High spatial resolution, real-time imaging of surface dynamics Limited to conductive samples, complex instrumentation Surface morphology analysis, real-time imaging
RHEED Real-time monitoring, provides crystal structure information Limited to conducting samples, surface sensitivity variability Thin-film growth monitoring, surface structure determination
LEED High sensitivity for surface structure determination Requires ultra-high vacuum, limited to ordered surfaces Crystallography studies, surface structure analysis
GIFAD Provides structural information for surfaces Limited to specific incident angles, complex instrumentation Surface structure analysis, studies of ordered surfaces
NFS Nondestructive, element-specific, sensitive to vibrations For certain isotopes, relatively low scattering cross section Study of vibrational dynamics, element-specific analysis
RAS Real-time monitoring, sensitive to surface changes Requires careful data analysis, limited to specific materials Monitoring of surface processes, surface structure analysis
XRS Provides atomic arrangement information in crystals Requires a crystalline sample, limited to periodic structures Crystallography studies
XRD High precision in determining crystal structures For crystalline samples, bulk analysis lack surface specificity Crystallography studies, analysis of crystalline materials
RSM Detailed information on crystal lattice parameters Requires crystalline samples, complex instrumentation Strain analysis, determination of crystal lattice parameters
XANES Provides local electronic structure information For elements with absorption edges in the X-ray range Study of local electronic structure in various materials
RS Nondestructive, applicable to a wide range of materials Low spatial resolution, susceptibility to fluorescence interference molecular structures analysis
SE High sensitivity, nondestructive Requires accurate modeling, limited to certain sample types Film thickness and optical constant determination
STM/STS Provides electronic structure, density of states information Limited to conductive samples, sample preparation challenges Surface electronic structure, density of states analysis
QMS High sensitivity to mass changes, real-time analysis Limited to gas-phase analysis, may require sample ionization Gas composition analysis
DMS Provides real-time information on desorbed species analysis Limited to studying desorption phenomena, sample-dependent Surface desorption analysis, study of desorption processes
PES High surface sensitivity, elemental composition analysis Requires ultra-high vacuum, limited to surface analysis Surface composition analysis, chemical state determination
XPS Surface-sensitive for elemental composition analysis Limited depth of analysis, sample charging affect results Surface composition analysis, chemical state determination
UPS Provides information about valence band, surface-sensitive Requires ultra-high vacuum, limited to surface analysis Valence band electronic structure analysis, surface chemical analysis
ARPES Provides detailed information about electronic band structure Requires ultra-high vacuum, limited to surface analysis Electronic band structure analysis, surface electronic states
CEMS Provides information on chemical environment, Mössbauer-active nuclei Limited to specific isotopes, requires cryogenic temperatures Study of chemical environments, Mössbauer-active nuclei analysis
MOKE Sensitive to magnetic properties and domain structures Limited to magnetic materials, complex instrumentation Magnetic domain structure, magnetic properties analysis
XAS Provides information on local electronic and geometric structure Requires synchrotron radiation, complex data analysis Local electronic and geometric structure analysis
XPD Provides structural information at the atomic level, surface-sensitive Requires ultra-high vacuum, limited to surface analysis Surface structural analysis, study of atomic arrangement
AES Elemental and chemical state analysis of surfaces, high sensitivity Limited depth of analysis, surface sensitivity Surface composition analysis, chemical state determination
EELS Provides information on electronic excitations and bonding, high spatial resolution Requires sophisticated instrumentation, complex data analysis Electronic structure analysis, study of electronic excitations
AIPES Provides angle-integrated information on electronic structure Limited to angle-integrated data, lack angular information Electronic structure analysis, study of electronic states
CM Measures surface curvature, provides strain information Limited to surface properties Strain analysis, characterization of curved surfaces
MOS Simultaneous measurement of multiple parameters System complexity may require careful calibration Multifaceted parameter monitoring, simultaneous data acquisition
4PC Accurate measurement of electrical conductivity Requires precise sample preparation Electrical conductivity analysis, study of conductive materials
BEM Monitors changes in band structure during processes Specific to semiconductor materials, requires precise control of growth conditions Real-time monitoring of band structure changes during thin-film growth
XPEEM Combines high-resolution imaging with surface-sensitive spectroscopy Requires ultra-high vacuum conditions, limited to surface analysis Surface chemical composition analysis, electronic structure imaging
CL Probes luminescent properties of materials under electron beam excitation Limited to materials with luminescent properties, resolution may be limited Study of bandgap, defects, and luminescent properties of materials
XMCD Sensitive to magnetic properties and magnetic moments of elements Requires synchrotron radiation for high-quality data, limited to magnetic materials Study of magnetic properties, magnetic moment determination
DRS Sensitive to changes in the optical properties of materials Data analysis may require careful consideration of multiple factors Monitoring changes in optical properties, surface and interface analysis
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    Received: 29 July 2023 Revised: 13 November 2023 Online: Accepted Manuscript: 12 December 2023Uncorrected proof: 13 December 2023Published: 15 March 2024

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      Article Navigation >  Journal of Semiconductors  > 2024  >  45(3): 031301
      Chao Shen, Wenkang Zhan, Manyang Li, Zhenyu Sun, Jian Tang, Zhaofeng Wu, Chi Xu, Bo Xu, Chao Zhao, Zhanguo Wang. Development of in situ characterization techniques in molecular beam epitaxy[J]. Journal of Semiconductors, 2024, 45(3): 031301. doi: 10.1088/1674-4926/45/3/031301 ****Chao Shen, Wenkang Zhan, Manyang Li, Zhenyu Sun, Jian Tang, Zhaofeng Wu, Chi Xu, Bo Xu, Chao Zhao, Zhanguo Wang, Development of in situ characterization techniques in molecular beam epitaxy[J]. Journal of Semiconductors, 2024, 45(3), 031301 doi: 10.1088/1674-4926/45/3/031301
      Citation:
      Chao Shen, Wenkang Zhan, Manyang Li, Zhenyu Sun, Jian Tang, Zhaofeng Wu, Chi Xu, Bo Xu, Chao Zhao, Zhanguo Wang. Development of in situ characterization techniques in molecular beam epitaxy[J]. Journal of Semiconductors, 2024, 45(3): 031301. doi: 10.1088/1674-4926/45/3/031301 ****
      Chao Shen, Wenkang Zhan, Manyang Li, Zhenyu Sun, Jian Tang, Zhaofeng Wu, Chi Xu, Bo Xu, Chao Zhao, Zhanguo Wang, Development of in situ characterization techniques in molecular beam epitaxy[J]. Journal of Semiconductors, 2024, 45(3), 031301 doi: 10.1088/1674-4926/45/3/031301
      shu

      Development of in situ characterization techniques in molecular beam epitaxy

      DOI: 10.1088/1674-4926/45/3/031301
      • 1.

        Laboratory of Solid State Optoelectronics Information Technology, Institute of Semiconductors, Chinese Academy of Sciences, Beijing 100083, China

      • 2.

        College of Materials Science and Opto-Electronic Technology, University of Chinese Academy of Sciences, Beijing 101804, China

      • 3.

        School of Physics Science and Technology, Xinjiang University, Urumqi 830046, China

      • 4.

        School of New Energy and Electronics, Yancheng Teachers University, Yancheng 224002, China

      • 5.

        Key Laboratory of Optoelectronic Materials and Devices, Institute of Semiconductors, Chinese Academy of Sciences, Beijing 100083, China

      More Information
      • Chao Shen obtained his bachelor’s degree from Yancheng Teachers University in 2020. Currently, he is pursuing a master's degree at Xinjiang University and has been actively engaged in research at the Key Laboratory of Semiconductor Materials Science since July 2022. His primary focus lies in in-situ characterization techniques and machine learning within the realm of semiconductor materials science
      • Zhenyu Sun is currently an associate professor in Institute of Semiconductors, Chinese Academy of Sciences. He received his B.E. in Information Engineering from Zhejiang University in 2010 and Ph.D. in Electrical Engineering from Texas Tech University in 2019. His research interests include Ⅲ–Ⅴ compound semiconductor materials and optoelectronic devices
      • Chao Zhao is a full professor in Institute of Semiconductors, Chinese Academy of Sciences. He has a long and distinguished record of achievements in the fields of Ⅲ–Ⅴ compound semiconductor materials and optoelectronic devices. He is a IOP Fellow and holds senior memberships at The Optical Society (OSA) and IEEE
      • Corresponding author: zsun@semi.ac.cn; zhaochao@semi.ac.cn
      • Received Date: 2023-07-29
      • Revised Date: 2023-11-13
        • Available Online: 2023-12-12

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