Journal of Semiconductors, Volume. 45, Issue 3, 031301(2024)

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
  • 1Laboratory of Solid State Optoelectronics Information Technology, Institute of Semiconductors, Chinese Academy of Sciences, Beijing 100083, China
  • 2College of Materials Science and Opto-Electronic Technology, University of Chinese Academy of Sciences, Beijing 101804, China
  • 3School of Physics Science and Technology, Xinjiang University, Urumqi 830046, China
  • 4School of New Energy and Electronics, Yancheng Teachers University, Yancheng 224002, China
  • 5Key Laboratory of Optoelectronic Materials and Devices, Institute of Semiconductors, Chinese Academy of Sciences, Beijing 100083, China
  • show less
    Figures & Tables(25)
    (Color online) In situ characterization techniques applied in MBE.
    (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.
    (Color online) (a) STM image of the modulated honeycomb 7 × 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 7 × 7 superstructure (in red), the 19 × 19 superstructure (in green), and the 5 × 5 superstructure (in blue). Reproduced with permission. Ref. [48].
    (Color online) STM image of c(6 × 12) reconstructions on wurtzite GaN(0001¯). Reproduced with permission. Ref. [38] Copyright 2014, AIP Publishing.
    (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].
    SnS on graphene substrates as a function of temperature as observed by LEEM. Reproduced with permission. Ref. [60] Copyright 2018, American Chemical Society.
    (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].
    (Color online) RHEED patterns, corresponding STM images, and modeled patterns of GaN films deposited with different I/A ratios. Reproduced with permission. Ref. [54].
    (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.
    (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].
    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.
    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.
    (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].
    (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].
    (Color online) Selected XRD spectra of the sub-free SDD-GaSe film during pressurization. Reproduced with permission. Ref. [127].
    (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.
    (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.
    (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.
    (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.
    (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].
    (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].
    (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].
    (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 (112¯0) a-plane InN growth. Reproduced with permission. Ref. [192] Copyright 2015, Elsevier B.V.
    (Color online) Statistics of in situ characterization techniques involved in publications in recent years.
    • Table 1. A summary of the advantages, disadvantages, and functions of characterization technologies.

      View table
      View in Article

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

      TechniqueAdvantagesDisadvantagesFunctions
      STMHigh spatial resolution; morphology and electronic structure analysisLimited to conductive samples, requires ultra-high vacuumSurface morphology, electronic structure analysis
      SEMHigh depth of field, for conductive and non-conductive samplesLower resolution than STM, sample preparation challengesMorphology analysis of various samples
      AFMHigh resolution in both lateral and vertical directionsRelatively slow imaging, tip wear and contamination effectsSurface morphology analysis, material property studies
      LEEMHigh spatial resolution, real-time imaging of surface dynamicsLimited to conductive samples, complex instrumentationSurface morphology analysis, real-time imaging
      RHEEDReal-time monitoring, provides crystal structure informationLimited to conducting samples, surface sensitivity variabilityThin-film growth monitoring, surface structure determination
      LEEDHigh sensitivity for surface structure determinationRequires ultra-high vacuum, limited to ordered surfacesCrystallography studies, surface structure analysis
      GIFADProvides structural information for surfacesLimited to specific incident angles, complex instrumentationSurface structure analysis, studies of ordered surfaces
      NFSNondestructive, element-specific, sensitive to vibrationsFor certain isotopes, relatively low scattering cross sectionStudy of vibrational dynamics, element-specific analysis
      RASReal-time monitoring, sensitive to surface changesRequires careful data analysis, limited to specific materialsMonitoring of surface processes, surface structure analysis
      XRSProvides atomic arrangement information in crystalsRequires a crystalline sample, limited to periodic structuresCrystallography studies
      XRDHigh precision in determining crystal structuresFor crystalline samples, bulk analysis lack surface specificityCrystallography studies, analysis of crystalline materials
      RSMDetailed information on crystal lattice parametersRequires crystalline samples, complex instrumentationStrain analysis, determination of crystal lattice parameters
      XANESProvides local electronic structure informationFor elements with absorption edges in the X-ray rangeStudy of local electronic structure in various materials
      RSNondestructive, applicable to a wide range of materialsLow spatial resolution, susceptibility to fluorescence interferencemolecular structures analysis
      SEHigh sensitivity, nondestructiveRequires accurate modeling, limited to certain sample typesFilm thickness and optical constant determination
      STM/STSProvides electronic structure, density of states informationLimited to conductive samples, sample preparation challengesSurface electronic structure, density of states analysis
      QMSHigh sensitivity to mass changes, real-time analysisLimited to gas-phase analysis, may require sample ionizationGas composition analysis
      DMSProvides real-time information on desorbed species analysisLimited to studying desorption phenomena, sample-dependentSurface desorption analysis, study of desorption processes
      PESHigh surface sensitivity, elemental composition analysisRequires ultra-high vacuum, limited to surface analysisSurface composition analysis, chemical state determination
      XPSSurface-sensitive for elemental composition analysisLimited depth of analysis, sample charging affect resultsSurface composition analysis, chemical state determination
      UPSProvides information about valence band, surface-sensitiveRequires ultra-high vacuum, limited to surface analysisValence band electronic structure analysis, surface chemical analysis
      ARPESProvides detailed information about electronic band structureRequires ultra-high vacuum, limited to surface analysisElectronic band structure analysis, surface electronic states
      CEMSProvides information on chemical environment, Mössbauer-active nucleiLimited to specific isotopes, requires cryogenic temperaturesStudy of chemical environments, Mössbauer-active nuclei analysis
      MOKESensitive to magnetic properties and domain structuresLimited to magnetic materials, complex instrumentationMagnetic domain structure, magnetic properties analysis
      XASProvides information on local electronic and geometric structureRequires synchrotron radiation, complex data analysisLocal electronic and geometric structure analysis
      XPDProvides structural information at the atomic level, surface-sensitiveRequires ultra-high vacuum, limited to surface analysisSurface structural analysis, study of atomic arrangement
      AESElemental and chemical state analysis of surfaces, high sensitivityLimited depth of analysis, surface sensitivitySurface composition analysis, chemical state determination
      EELSProvides information on electronic excitations and bonding, high spatial resolutionRequires sophisticated instrumentation, complex data analysisElectronic structure analysis, study of electronic excitations
      AIPESProvides angle-integrated information on electronic structureLimited to angle-integrated data, lack angular informationElectronic structure analysis, study of electronic states
      CMMeasures surface curvature, provides strain informationLimited to surface propertiesStrain analysis, characterization of curved surfaces
      MOSSimultaneous measurement of multiple parametersSystem complexity may require careful calibrationMultifaceted parameter monitoring, simultaneous data acquisition
      4PCAccurate measurement of electrical conductivityRequires precise sample preparationElectrical conductivity analysis, study of conductive materials
      BEMMonitors changes in band structure during processesSpecific to semiconductor materials, requires precise control of growth conditionsReal-time monitoring of band structure changes during thin-film growth
      XPEEMCombines high-resolution imaging with surface-sensitive spectroscopyRequires ultra-high vacuum conditions, limited to surface analysisSurface chemical composition analysis, electronic structure imaging
      CLProbes luminescent properties of materials under electron beam excitationLimited to materials with luminescent properties, resolution may be limitedStudy of bandgap, defects, and luminescent properties of materials
      XMCDSensitive to magnetic properties and magnetic moments of elementsRequires synchrotron radiation for high-quality data, limited to magnetic materialsStudy of magnetic properties, magnetic moment determination
      DRSSensitive to changes in the optical properties of materialsData analysis may require careful consideration of multiple factorsMonitoring changes in optical properties, surface and interface analysis
    Tools

    Get Citation

    Copy Citation Text

    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

    Download Citation

    EndNote(RIS)BibTexPlain Text
    Save article for my favorites
    Paper Information

    Category: Articles

    Received: Jul. 29, 2023

    Accepted: --

    Published Online: Apr. 24, 2024

    The Author Email: Sun Zhenyu (ZYSun), Zhao Chao (CZhao)

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

    Topics