The Hitachi S3200N variable pressure scanning electron microscope (VPSEM) is a conventional high resolution thermionic SEM, which allows the operator to control the specimen chamber vacuum level.

For conductive samples, the instrument is typically operated in high vacuum mode and images are collected with the Everhart-Thornley secondary electron detector.  For insulating samples, the instrument is typically operated in variable pressure mode and images are collected with the Robinson backscattered electron detector.  When operating in variable pressure mode, the chamber is back filled with a gas in order to allow imaging with little or no charging of the sample.  Typically, the back fill gas is either N2 or He, but any non-corrosive, non-reactive gas can be used.  Elemental analysis using the energy dispersive X-ray detector can be done in either high vacuum or variable pressure mode.

The Hitachi S3200N SEM is equipped with the standard Everhard-Thornley secondary electron detector, a Robinson backscattered electron detector, an Oxford energy dispersive X-ray spectrometer, and a GW specimen current meter.  Electrical feedthroughs are also mounted on the chamber to allow powering active electrical devices or observing electron beam induced current (EBIC).  A 4Pi Universal Spectral Engine (electronics set) allows for digital data collection from all of the detectors.

Equipment Specifications

Detectors
  • Everhart-Thornley secondary electron detector
  • Robinson backscattered electron detector
  • Oxford energy dispersive X-ray spectrometer
  • GW Specimen current meter
  • GW ChamberScope
Capabilities
  • Digital imaging of secondary electron images (topographical contrast)
  • Digital imaging of backscattered electron images (atomic number contrast)
  • Digital collection of X-ray spectra
  • Digital X-ray mapping
  • Digital imaging of specimen current
  • EBIC (assumes a means of electrically connecting to the sample!)
Accelerating Voltage
  • 0.3 – 30 kV
Magnification
  • 20X – 300,000X
Resolution (SE)
  • 35 Angsroms @ 30kV in high vacuum mode using the secondary electron detector
Resolution (BSE)
  • 55 Angstroms @ 30kV in variable pressure mode using the backscattered electron detector
Working Distance
  • 3-60 mm
Specimen Stage
  • Eucentric tilt -20º to +90º
  • Rotate 360º
  • x = 60 mm
  • y = 40 mm
  • z = 26 mm
Specimen Considerations
  • Accepts most samples: Conductors, Semiconductors, and Insulators can be observed
    • Including, but not limited to metals, semiconductor devices, ceramics, biological, polymer, textile, pharmaceuticals, even food, etc.
  • Specimens can be up to 150mm in diameter and up to 40mm thick
    • Only the center 60x40mm area can be observed on large specimens

Documentation

Hitachi3200 Operating Instructions

Examples and Instrument Photographs

VPSEM_1RS

Hitachi S-3200N

 

 

ChamberImage_Labeled

Inside the S3200N Chamber

DarkSphere_1

Example Analysis: This sample was taken from waste material at a Cu mine. The question was “is this material rich enough in valuable metals that it should be processed.” The material was mostly composed of dark spheroids with bright spheroidal inclusions. This sphere is composed mostly of oxides of several metals (medium dark contrast areas) and carbon (darkest areas). The bright spheroidal inclusions are Cu-rich.

DarkSphere_1 Probe 1

Example Analysis: Energy dispersive X-ray spectrum (EDS) of a bright spheroidal inclusion in the dark sphere showing that it is composed of mostly Cu.

DarkSphere_1 Probe 2

Example Analysis: EDS spectrum of part of the dark sphere showing it is composed of significant amounts of O, Na, Mg, Al, Si, K, Ca, Ti, and Fe.

DarkSphere_1 Probe 3

Example Analysis: EDS spectrum of the darkest part of the dark sphere showing that this region is mostly C.

 

SandDollar_BSE_50x

Sand Dollar (found at an NC beach) observed with the Robinson BSE detector at 50X.

SandDollar_BSE_500x

Sand Dollar (found at an NC beach) observed with the Robinson BSE detector at 500X.

 

VPSEM_featured_wip2a

Dendritic growth of Ag from a colloidal suspension observed with the Everhart-Thornley SE detector.

etched pearlite

Etched Pearlite. Sample courtesy Lew Reynolds.

framboids

Pyrite (FeS) “framboids” filling the shell of a foraminifera in sediments from the continental shelf seaward of the North Island, New Zealand. Pyrite forms under reducing conditions in shallowly buried, organic-rich marine sediments.
From the work of Lonnie Leithold.

pb-sn_eutectic

Lead-tin eutectic imaged with Robinson BSE detector. The BSE detector is sensitive primarily to changes in atomic number with higher atomic number materials having more contrast. In this case, the Pb is brightest and the Sn is darker. The dark particles observed are polishing media that are embedded in the sample. Sample courtesy Lew Reynolds.

 

pollen

Pollen sample taken from AIF staff member Chuck Mooney’s car.