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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...
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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.
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SEM Quick Start Revision No.2 May 2014 Page 1 of 16 Zeiss ΣIGMA VP-FE-SEM User Guide May 2014 Jeremy Hilgar, Darlene Usi...
SEM Quick Start Revision No.2 May 2014 Page 3 of 16 Zeiss VP-FE-SEM Quick Start Guide Procedural Section 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.
SEM Quick Start Revision No.2 May 2014 Page 4 of 16 are all fairly simple. Perhaps the most convenient instrument used to deposit spots on the support is the mechanical micropipette. The exact volume of the spot will naturally vary depending on the situation.
1.2.1 Software Startup The microscope is controlled entirely by the SmartSEM software suite developed by Zeiss. The software requires users to login to an account before use. User accounts are important for both logging operator actions as well as saving personalized user interface preferences. Once opened and logged in, the software will automatically show a view of the vacuum chamber as well as the status of the instrument.
SEM Quick Start Revision No.2 May 2014 Page 6 of 16 The pressure of the sample chamber can be viewed under the Vacuum tab on the right sidebar. Pressure units can be cycled through to the user’s preference by left-clicking the vacuum pressure status boxes. The microscope requires a vacuum below 0.009 Pa before extra high tension (EHT) can be enabled, which is required to produce an image.
Many of the procedures listed in this section will make use of both the Zeiss SEM keyboard and the SEM Stage Control board. The adjustments made using these input boards can be performed in either coarse or fine modes.
SEM Quick Start Revision No.2 May 2014 Page 8 of 16 detector to be discussed is the STEM detector, which is composed of both dark-field and bright-field components. The STEM detector collects electrons that travel through the sample while mounted on STEM- compatible carousel and support film.
SEM Quick Start Revision No.2 May 2014 Page 9 of 16 operator is comfortable with. Be sure to select the TV detector channel while making changes to the working distance. The larger control stick on the right is responsible for moving the stage through three degrees of freedom.
(higher resolution) without having to wait for the entire frame to be scanned after making changes. To enable the reduced raster window, click the Reduced button directly above the Magnification knob on the left-hand side of the Zeiss SEM...
Mag = Y X. Changing the magnification of the image is done using the dial labelled Magnification on the left-hand side of the Zeiss SEM keyboard. It is sometimes convenient to zoom all the way out while switching between samples (Sections 1.3.2 and 1.3.3).
Focus upon the selected scene and correct for any apparent beam astigmatism. Once sufficiently focused, locate and press the button labelled Wobble on the top portion of the Zeiss SEM Keyboard. A reduced raster box will appear showing an amplification of the current focus wobble.
SEM Quick Start Revision No.2 May 2014 Page 13 of 16 low and the noise reduction method should be set to line average. To freeze a frame, open the Scanning tab on the SEM Control side-panel and select Freeze on = End Frame from the first dropdown menu in the Noise Reduction box.
SEM Quick Start Revision No.2 May 2014 Page 14 of 16 switching to the TV detector channel (Section 1.3.1), open the Stage Points List tool and double click the stage point labelled $STEM_SAFE_ZONE. The stage will move to an area in the chamber that is safe for detector arm insertion.
SEM Quick Start Revision No.2 May 2014 Page 15 of 16 Logging Off Finishing a session with the microscope is roughly the reverse of the startup process. The following sections will briefly outline the steps to safely log off the instrument. 1.5.1 Stage Positioning and STEM Detector The first steps to safely logging off the instrument involves stowing the stage and disabling the control sticks.
Venting the vacuum chamber can be accomplished by clicking the Vac status textbox at the bottom right portion of the Zeiss SmartSEM window and selecting the Vent option. The roughing pump will promptly switch off and the vacuum chamber will begin to vent. After a short time the chamber door can be opened if the operator wishes to retrieve any samples.
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