EPA/600/R-14/211 | October 2014 | www.epa.gov/research
Zeiss ΣIGMA VP-FE-SEM
User Guide
R E S E A R C H A N D D E V E L O P M E N T
Zeiss ΣIGMA VP-FE-SEM
User Guide
Prepared for
Jeremy Hilgar, Darlene Usi and Katrina Varner
U.S. Environmental Protection Agency
Office of Research and Development
National Exposure Research Laboratory
Environmental Sciences Division
Las Vegas, NV 89119
Although this work was reviewed by EPA and approved for publication, it may not necessarily reflect
official Agency policy. Mention of trade names and commercial products does not constitute
endorsement or recommendation for use.
U.S. Environmental Protection Agency
Office of Research and Development
Washington, DC 20460
Zeiss ΣIGMA VP-FE-SEM
User Guide
May 2014
By:
Jeremy Hilgar, Darlene Usi
SEM Quick Start
Revision No.2
May 2014
Page 1 of 16
SEM Quick Start
Revision No.2
May 2014
Page 2 of 16
TABLE OF CONTENTS
Section Page
1.0 Procedural Section ............................................................................................................................................ 3
1.1 Sample Preparation and Loading ............................................................................................................. 3
1.1.1 Support Selection ................................................................................................................ 3
1.1.2 Sample Deposition .............................................................................................................. 3
1.1.2.1 Liquid Samples ..................................................................................................... 3
1.1.2.2 Solid Samples ....................................................................................................... 4
1.1.3 Loading the Carousel .......................................................................................................... 4
1.2 Instrument Startup .................................................................................................................................... 5
1.2.1 Software Startup ................................................................................................................. 5
1.2.2 Gas Pressure and Vacuum Control ..................................................................................... 5
1.2.3 Accelerating Voltage .......................................................................................................... 6
1.3 Producing an Image .................................................................................................................................. 7
1.3.1 Detectors ............................................................................................................................. 7
1.3.2 Stage Control and Working Distance using Analog Controls............................................. 8
1.3.3 Stage Control Using SmartSEM’s Stage Navigation .......................................................... 9
1.3.4 Scan Speed and Noise Reduction ..................................................................................... 10
1.3.5 Reduced Raster ................................................................................................................. 10
1.3.6 Brightness and Contrast .................................................................................................... 11
1.3.7 Magnification and Focus .................................................................................................. 11
1.3.8 Stigmation and Focus Wobbles ........................................................................................ 11
1.3.9 Saving an Image ............................................................................................................... 12
1.4 STEM Mode ........................................................................................................................................... 13
1.4.1 Stage Navigation and the STEM Detector ........................................................................ 13
1.4.2 Imaging Modes ................................................................................................................. 14
1.5 Logging Off ............................................................................................................................................ 15
1.5.1 Stage Positioning and STEM Detector ............................................................................. 15
1.5.2 Accelerating Voltage ........................................................................................................ 15
1.5.3 Vacuum Control and Gas Pressure ................................................................................... 16
1.5.4 Closing the Software ......................................................................................................... 16
2.0 References ...................................................................................................................................................... 16
1.0 Procedural Section
1.1 Sample Preparation and Loading
Note: The cleanliness of the vacuum chamber is very important. It is encouraged
that the investigator wear gloves while handling objects that will enter the
vacuum chamber, specifically the sample carousels. It is also good practice to
keep the chamber door closed as often as possible. This practice reduces the
contamination rate of the chamber.
Sample preparation consists of two basics steps and will vary depending
on both the nature of the analyte and the information required from the analyte
SEM Quick Start
Revision No.2
May 2014
Page 3 of 16
Zeiss VP-FE-SEM Quick Start Guide
1.1.1 Support Selection
Sample supports and films are most broadly categorized by
whether or not they are STEM-compatible. STEM-compatible films and
grids are always slotted to allow the passage (transmission) of electrons to
a detector. The most commonly used STEM-compatible support film is
the lacey carbon copper grid. These grids can come equipped with a
Formvar resin to enhance the stability of the lacey carbon network. The
usage of STEM-compatible support films often proves convenient given
that these sample mounts can also be used in normal SEM mode. The
selection of an appropriate support medium for a given task is often a
process of trial and error.
1.1.2 Sample Deposition
1.1.2.1 Liquid Samples
Liquid samples are deposited onto the appropriate support
in a drop-by-drop fashion using a variety of tools. Given that
sample supports are often large enough to house several different
analytes, it is often desirable to control both the location and size
of the spots deposited. The tools used to reach this end vary, but
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