University of Nottingham
  
JEOL 7100F SEM with operator

Scanning Electron Microscopy (SEM)

The JEOL 7100F FEG-SEM at the Nanoscale and Microscale Research Centre
 

SEM at a glance 

SEM is an imaging technique that uses incident electrons to generate secondary sample irradiance. This can then be detected in a variety of ways to visualise sample surfaces with high depth of field and lateral resolutions of around 1-20nm, as well as analyse the physical and chemical state of the substrate.

  • FIBSEM couples traditional SEM with a focused ion beam that can be used for materials processing and sample preparation (deposition, ablation, sectioning etc.) or at low beam currents, for imaging in its own right.
  • ESEM allows for the imaging of poorly conductive ‘uncoated’, or ‘wet’ samples that cannot be imaged in the high vacuum conditions of a traditional SEM. 
  • Cryo-SEM allows for biological samples to be rapidly frozen, prepared and then SEM imaged. This preserves the initial substrate morphology and chemistry of the fully hydrated specimen by preventing water loss to vacuum operation. 
  • FEGSEM uses a field emission gun electron source to generate a smaller diameter electron beam than standard thermal emission sources. This allows better spatial resolution to be achieved and makes the technique more suitable for nanostructural characterisation.

Applications of SEM

  • Morphological and topographical imaging
  • Compositional contrast imaging
  • Chemical analysis via energy or wavelength dispersive X-ray spectroscopy (EDS, WDS)
  • Dynamic macro-, micro- and nano-structural imaging under temperature, pressure and strain variations
  • Sample manipulation, sectioning and thinning
Scanning Electron Microscopy with cryo-handling capabilities 

How does SEM work?

A fine beam of electrons is used to scan across the specimen surface in synchronism with the spot of a cathode ray tube (CRT). This incident beam leads to elastic and inelastic scattering of electrons, as well as variations of electromagnetic radiation. There are subsequently a host of secondary signals that can be detected, including secondary electrons, backscattered electrons, Auger electrons, cathodoluminescence or X-rays. In general, as the primary electron beam is rastered across a substrate, the intensity of the secondary signal will change depending on the surface morphology, chemistry, physical state etc. The contrast is seen by adjusting the brightness of the CRT spot by the amplified version of this detected signal.

 

 

 

 

Images courtesy of Vladimir Korolkov Photography and Lubrizol Ltd.

 

Our SEM Facilities

Hosted at the Nanoscale and Microscale Research Centre (nmRC). 

Investigate sample morphology, topography and constitution using SEM
Inside the FEI Quanta 650 ESEM
Use a focused ion beam to process samples for imaging and analysis using our FIB-SEM
 

 

The FEI Quanta 650 ESEM
ISAC grants access to multiple SEM instruments tailored to the work to be carried out
Multiple sample mounting for ESEM in water vapour, nitrogen or air.
 

 

JEOL 7100F FEG-SEM

  • JEOL in-lens Schottky field emissions source:
  •         
    • 3.0 nm resolution at 1 kV
    • 1.2 nm resolution at 30 kV
  • GATAN Murano Heating Stage Module with heating up to 950oC. 
  • Oxford Instruments AZtec Energy Advanced X-max 150 EDS System for chemical characterisation.
  • Oxford Instruments AZtec HKL Advanced EBSD System (with NordlysMax3) for crystallographic characterisation.
  • Oxford Instruments INCA Wave 700 WDS System for high resolution elemental mapping and quantification.

 

 

 

ZEISS CROSSBEAM 550 (HR-CAT-SEM) 

  • Specialist cryogenic analytical and transfer (CAT) instrument.
  • High-resolution FIB manipulation / milling with FEG resolution imaging, cryogenic handling capabilites.
  • ZEISS Gemini II (FEG) optics optimised for versatile low kV performance:
      • 1.4 nm resolution at 1kV 
      • 0.7nm resolution at 15kV
    • ZEISS Gemini objective lens design enabling imaging of magnetic materials and during live FIB-milling.
    • Inlens SE, Inlens EsB, ETD (Everhard-Thornley detector), SESI (secondary electron, secondary ion) and aBSD (backscatter) detectors.
    • aSTEM (scanning transmission electron) detector with annular detection diode design. Enables bright field (BF), normal dark field (DF), orientated dark field (ODF), annular dark field (ADF) and high angle annular dark field (HAADF) analysis.
    • Oxford Instruments AZtec Advanced Ultimax 170mm EDS detector.
    • Oxford Instruments Symmetry (EBSD) detector with AZtecHKL nanoanalysis software.
    • ZEISS Xsample holder with SmartEPD software for advanced TEM lamella (sub 20nm) preparation, 3D tomography and nanofabrication.
    • 6-axis super-eucentric sample stage for versatile sample handling.
    • 12 position STEM holder optimised for EDS analysis.
    • 3D EBSD applicable hardware and sample holder.
    • A four gas plus charge compensator, Multi GIS (gas insjector) system. Platinum, carbon mill (water) and carbon precurors available.
    • Quorum Technologies PP3010T cryogenic system for sample freezing, manipulation and transfer.
    • Omniprobe 200 micromanipulator with omniprobe rotation option and omniprobe cryo-lift out capabilities.
 

 

JEOL 7000F FEG-SEM

  • FEG-SEM
  • Oxford Instruments AZtec EDX system
 

 

FEI Quanta200 3D DualBeam FIB/SEM

(Cryo-SEM & ESEM facilities)

  • Thermal emission electron optics with dual-anode source emission geometry and through-the-lens differential pumping.
  • High-resolution (field emission) ion optics (Magnum™ column) with high-volume milling capabilities and an in-situ Omniprobe Model 100.7 nanomanipulator for sample milling, thinning, sectioning and lift-outs for more detailed structural SEM or TEM analysis.
  • Quorum Technologies PP3010T Cryo-SEM Preparation System for cryogenic sample preparation and analysis, including freeze-fracture and freeze-etching.
  • Oxford Instruments integrated INCA Energy 250 Microanalysis System for EDX elemental spectra and mapping.
  • Gaseous secondary and backscattered electron detectors for imaging and analysis in a gaseous environment (ESEM).
  • Gas Chemistry technology for enhanced milling rates including selective carbon Mill.
  • High-precision specimen goniometer with 50 mm travel along the x and y axes.
  • Automation serving unattended sectioning with full access to E-beam, I-beam, patterning and gas chemistry functionality.
  • Tungsten metal deposition, carbon deposition, insulator enhanced etch (XeF2) and selective carbon mill gas injectors (2 fitted at one time)
 

 

FEI Quanta 650 ESEM

  • High performance imaging in three modes: High Vacuum, Low Vacuum and ESEM.
  • Water vapour, air and nitrogen ESEM imaging modes for hydrated or non-coated samples.
  • GATAN in-situ Microtest tensile-compression stage MTEST200VT with loading up to 200N and Peltier temperature range -20oC to 160oC
  • Variable vapour pressures with peltier based temperature control for relative humidity cycling/ adjustment sample freeze thaw cycling
  • Alemnis in-situ Nano Indenter for micropillar compression and scratch testing
  • Oxford Instruments X-Max -150 EDX Detector for high sensitivity chemical analysis.
  • Peltier cooling stage for sample and humidity (gas pressure) control.
  • High performance thermal emission SEM column with dual-anode source emission geometry
  • High vacuum resolution: 3.0nm @ 30kV, 8.0nm @ 3kV
  • Low vacuum resolution:  3.0nm @ 30kV, 10.0nm @ 3kV
  • ESEM resolution: 3.0nm @ 30kV
 

 

FEI Quanta 600 Mineral Liberation Analyser (MLA)

  • Combines EDS software by BRUKER and Mineral Liberation Analysis (MLA) software by JKTech/FEI that allows automated large area analysis of polished specimens to identify and quantify mineral composition and distribution.
  • Outputs include calculated assay, elemental distribution, particle size distribution, modal mineralogy, mineral association, mineral locking etc.
  • Can take up to 14 polished mounts at a time, or samples up to 150mm2 with automated analysis of each sample in turn.
  • HV and LV operational modes with secondary or backscattered electron detection.
  • Resolution reported at 3.5nm @ 30kV
 

 

JEOL JXA-8200 Electron Microprobe

  • High resolution X-ray element mapping and quantification via wavelength dispersive x-ray spectroscopy (WDS).
  • 4 wavelength-dispersive spectrometers (detectable wavelengths of 0.087 to 9.3nm).
  • Detectable element range: B to U
  • Analysable area 80 x 80mm, with  magnification x40 to x300,000 (11mm WD).
  • Specimen stage for 25mm polished blocks or thin sections.
  • Digital secondary electron imaging with 6nm resolution (11mm WD, 30kV). 
  • Energy-dispersive spectrometry (EDX), backscattered electron detection.
 

 

Also available:

Philips (FEI) XL30 SEM

  •  Standard imaging with EDX available.

JEOL JSM IT-200 SEM

  • Tungsten electron source capable of < 10 nm resolution
  • Fitted with standard secondary electron (SE) and back-scatter electron (BSE) detectors for routine morphology and atomic number contrast characterisation
  • Low vacuum mode (< 120 Pa) for charge free imaging of non-conductive and non-vacuum compatible materials
  • Sample holders for mounting multiple pin-type stubs or cylindrical holders
  • Easy to use new interface with navigation camera using a photo of actual samples loaded into the chamber. Fitted with a chamberscope integrated into the microscope control software
  • Fitted with an Oxford Instruments Aztec Energy dispersive X-ray analysis (EDX) system and an Ultim-100 silicon drift detector capable of quantitative elemental analysis, X-ray mapping and line scanning and the very useful Aztec Live feature allowing real time chemical imaging. 

JEOL 6490LV SEM

  • Standard and low vacuum imaging with EDX and WDS available.
 

  

Publications of Interest

  • Additive manufacture of complex 3D Au-containing nanocomposites by simultaneous two-photon polymerisation and photoreduction. Hu, Q., Sun, X.-Z., Parmenter, C. D. J., Fay, M. W., Smith, E. F., Rance, G. A., He, Y., Zhang, F., Liu, Y., Irvine, D., Tuck, C., Hague, R. & Wildman, R., Scientific Reports,7, 17150 (2017).
  • Interactions at the Silica–Peptide Interface: Influence of the Extent of Functionalization on the Conformational Ensemble. Sola-Rabada, A., Michaelis, M., Oliver, D. J., Roe, M. J., Colombi Ciacchi, L., Heinz, H. & Perry, C. C., Langmuir,34, 8255–8263 (2018). 
  • Synthesis of hydroxylated group IV metal oxides inside hollow graphitised carbon nanofibers: nano-sponges and nanoreactors for enhanced decontamination of organophosphates. Astle, M. A., Rance, G. A., Fay, M. W., Notman, S., Sambrook, M. R. & Khlobystov, A. N., Journal of Materials Chemistry A,6, 20444–20453 (2018). 
  • Y-Mars: An Astrobiological Analogue of Martian Mudstone. Stevens, A. H., Steer, E., McDonald, A., Amador, E. S. & Cockell, C. S., Earth and Space Science,5, 163–174 (2018). 
  • Flame spheroidisation of dense and porous Ca2Fe2O5 microspheres. Molinar Díaz, J., Samad, S. A., Steer, E., Neate, N., Constantin, H., Islam, M. T., Brown, P. D. & Ahmed, I., Materials Advances,1, 3539–3544 (2020). 
  • Electric Field Induced Biomimetic Transmembrane Electron Transport Using Carbon Nanotube Porins. Hicks, J. M., Yao, Y.-C., Barber, S., Neate, N., Watts, J. A., Noy, A. & Rawson, F. J., Small, 17, 2102517 (2021). 
  • Efficacy of antimicrobial and anti-viral coated air filters to prevent the spread of airborne pathogens. Watson, R., Oldfield, M., Bryant, J. A., Riordan, L., Hill, H. J., Watts, J. A., Alexander, M. R., Cox, M. J., Stamataki, Z., Scurr, D. J. & de Cogan, F., Scientific Reports,12, 2803 (2022). 

     

  • Metallocatanionic vesicle-mediated enhanced singlet oxygen generation and photodynamic therapy of cancer cells. Sharma, B., Jain, A., Pérez-García, L., Watts, J. A., Rawson, F. J., Chaudhary, G. R. & Kaur, G., Journal of Materials Chemistry B, 10, 2160–2170 (2022).

Interface and Surface Analysis Centre (ISAC)

Email: isac@nottingham.ac.uk