Beruflich Dokumente
Kultur Dokumente
Working DRAFT Prepared by Lab Manager Jim Connolly (Revision date: 31-May-2013)
SmartLab Instruction Manual for Thin-Film (an overview of use of the system for thin films)
SmartLab Instruction Manual for Powder (an overview of the use of the system for powders;
largely duplicates the material in the thin film manual with some differences)
SmartLab Reference Manual (a detailed exploration of the Guidance software and its
capabilities)
Diffraction Space Simulation Userss Manual (used to simulate diffraction space for setting up
configuration of high-resolution multi-axis rocking-curve analyses)
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General Measurement (Includes details of setup and data collection for most general package
measurement conditions. Note that conditions for some Hi-res measurements are for
monochromators that we do not currently own.)
Residual Stress (Overview of the principles of residual stress determination, with details of
package measurement conditions and operations.)
In Situ Measurement (This section applies to DSC equipment that we do not have.)
Options (Section focuses on different macro measurement components that can be included in
custom measurement setups that allow specific measurement sequences to be created for
repeatable experiments. Macro setups are required for effective use of the 10-position sample
changer, and are useful for many other types of analyses.)
Links to the help documentation for the SmartLab will be found on all lab computers on which the
Rigaku analytical software suite is installed. This procedures manual contains a tiny fraction of the
procedures that may be found in the Rigaku documentation, and is tailored toward a practical hands-on
operational approach to get users going on the system. All users are encouraged to engage in selftraining using Rigakus documentation. Contact lab manager Jim Connolly for tips on how to access and
use the documentation.
Following the general operations, there are sections specific to data collection unique to particular
materials or specific experimental techniques. In many (but not all cases) different types of analysis
require change of components (optics, stages, detectors) in the system. Some components may be
changed by any trained and qualified system operators, while others may only be changed by
designated and trained system administrators. Each section details what components may or may not
be changed and by whom. These sections (will) include (when completed):
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This check does two things: informs the operator what is installed and reports this information
to the Guidance software. Close the window after the check.
3. Choose Measurement Package. From the Tasks menu, choose Package Measurement, and
choose the package appropriate to the task. In most cases for powders this will be General
(Bragg Brentano focusing) D/teX given the default setup above. The next steps are those in the
standard package measurement conditions. Users may choose to run all steps in the package or
(as is usually the case) only those that are needed for the particular run.
4. Optics Alignment: This is required when optics (BB vs. PB, D/teX vs. Scintillation detector)
have been changed since the last time the system has been run; dont do it if it isnt necessary.
Double-click on Optics Alignment and make sure that the Current Attribute agrees with the
type of analysis you will be doing. If there is any doubt about the alignment, you may select the
correct Optics alignment name for your analysis (i.e. @BB Focusing) and check Change optics
without alignment that uses the latest saved alignment settings for that measurement package.
To perform the alignment, uncheck the box. You will need to add the height reference sample
plate, remove the K filter, and make sure the D/teX beam stop is slid out of the beam path.
The software will instruct you to shift detector-side components; this should already be done
with the D/teX installation, but check the positions anyway. Optics alignment typically takes 10-
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Please note that having the D/teX beam stop in place will cause all alignment procedures to fail. It is located
just to the right of the sample stage and must be slid out of the beam path when doing any alignments.
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In general, 3mm is a good number to enter here. Sometimes if the sample thickness entered is too small, the z
alignment will fail because there is not enough travel on the high (above 0 mm) end of the alignment. If this
occurs, try increasing the sample thickness entered by a mm to get the adjustment within the range of travel.
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Sample Measurement Data: File name is the fully qualified path to the where the file collected
will be saved.5 RAS is the filename for the SmartLab data; files are also saved automatically in
Rigakus ASCII (ASC) and RAW (binary) formats. Sample name and Memo should contain some
information about the data, at a minimum duplicating the File name. Do not leave these boxes
blank. Sample name has a 30 character size limit for most displays of data.
Manual exchange slit conditions: Includes options for: Soller/PSC Slit (Incident); Incident Slit;
PSA adapter; and Soller Slits (Diffracted). Different options are available here depending on the
package measurement conditions chosen. Read current slits polls the installed slits and
reports any changes. Slits may also be changed here and the system will prompt you for the
proper item before executing. Sometimes parameters input will prompt the system for a
change in components (i.e., change in sample size parameters can produce a request to a
change in the incident slit).
Monochromatization: Options to use K-beta filter or diffracted beam monochromator (former
used for D/teX, later preferred for use with Scintillation Counter SC). Changing from the
installed method will prompt a change in hardware before proceeding. (Note: Operators
cannot change this setting because it requires a detector change.)
We strongly recommend using a location on our network for storing your data rather than a place on the local
hard drive of the system computer. If you have followed the procedure to map your network User folder as the
L: drive it will be easy to enter this drive as the destination for your data. This will make it much easier to access
your data from other computer systems used for data analysis.
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Measurement Conditions: For a single sample, choose one line to configure and check the
Exec. Box. Clicking on the ? icon pulls up the help for the measurement settings dialog.
Parameters for analysis include:
o Scan Axis: Specifies scan mode. /2 coupled is default and usual
o Mode: Choices are continuous or step. D/teX always should be continuous; either mode
is possible with SC.
o Range: Specifies range mode of scan as Absolute or Relative. Always choose
absolute for normal scans.
o Start: Specifies start (low) angle (2) for scan. Because of angular range of D/teX,
angles here less of than 2 can produce extreme low-angle background (or detector
shutdown depending on the slit sizes chosen). Use of the low-angle (slide-out) beam
stop for the D/teX is recommended for all scans below 4 2.
o Stop: Specify stop(high) angle (2) for scan. Upper limit is 158.
o Step: Specifies step size in 2 over which data is sampled for collection. Default is
0.02 and is generally best for most uses; may be varied to adjust resolution (smaller for
slow scans or larger for fast scans).
o Speed Duration time: Indicates rate of scan in /min for continuous scan or time spent
per step for a step scan. DteX scan rates are typically 4 to 8/min or faster.
o IS (Incident Slit): Pulldown selects automatic slit control to maintain a consistent
angular aperture (deg) or select a fixed aperture (mm). Maximum fixed aperture is
7mm. Large apertures can lead to some angular divergence and/or flat specimen errors
in low-angle data. We will add some suggestions on IS and RS settings about optimal
settings for different angular conditions (as we experiment with different materials).
o RS1 (Rec. Slit 1): Pulldown selects automatic slit control to maintain a consistent angular
aperture (deg) or select a fixed aperture (mm); Maximum (20mm) is typically used for
D/teX; this can be reduced for materials with peaks at extremely low 2 angles.
o RS2 (Rec. Slit 2): Selects fixed fixed aperture (mm); Maximum (20mm) is typically used
for DteX
o Attenuator: Typically open (no attenuator)
o Comment: Optionally attaches comment to data for this run
o Options: Allows setting specialized options for stages with those capabilities (i.e.,
rotations, tilts, postions, etc.)
o Voltage (kV): Operating kV for scan (40kV is default)
o Current (mA): Operating mA for scan (30kV is default; we recommend setting at 40mA)
o Check the box for Drive the 4 axes to the current zero positions after the measurement
is completed. Not absolutely necessary except for last run (if doing multiple samples).
7. When a single measurement line is checked in which all parameters are set as desired, click on
the Execute button to start collecting data. This system will pop up a dialog box that you must
click OK in before data collection starts. After that your initial data file (RAS) will be created
and data collection will be initiated. After a few seconds a real-time display of your data will be
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An overload of the detector is evidenced by a message Error Code (2) RCD Error on Communication at the start
of data collection, and is caused by overloading the D/teX by too much direct X-ray intensity at the start angle.
This error causes the detector to shut down to protect itself from damage. Should this error be encountered, reset
the IS and RS1 settings to lower values and try again.
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Remember that the beam stop must be removed from the beam path when doing alignments
procedures and put it in place only when you actually doing your analyses. Having the beam stop in
place during sample alignment will cause the procedure to fail.
With the D/teX detector, samples with high Fe content can produce significantly elevated background as
a consequence of the fluorescence of Fe in Cu K X-rays. For samples that are not amorphous (and for
which the high background is not masking something you are hoping to see) the elevated background
tends to be rather flat and thus relatively easy to deal with as long as the characteristic peaks in the
pattern are well defined. How this fluorescence-related background might influence quantitative
(Rietveld or similar) analyses with Fe-rich samples is something that needs further investigation.
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Sample Measurement Data: File name is the fully qualified path to the where the file collected
will be saved. A network location (like your personal L: drive) should be used for saving the
data collected (as discussed in the D/teX data collection section). RAS is the filename for the
SmartLab data; files are also saved automatically in Rigakus ASCII (ASC) and RAW formats.
Sample name and Memo should contain some information about the data, minimally
duplicating the file name; do not leave any of these fields blank. Sample name has a 30
character size limit for most displays of data.
Manual exchange slit conditions: Includes options for: Soller/PSC Slit (Incident); Incident Slit;
PSA adapter; and Soller Slits (Diffracted). Slits shown are defaults for BB with SC/Mono
combination for most standard powders.
Monochromatization: For SC/Mono combination select Diffracted beam monochromator
method. Changing from the installed method will prompt a change in hardware before
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proceeding. (Note: Operators cannot change this setting because it requires detector
reconfiguration, adding or removing the monochromator.)
Measurement Conditions: For a single sample, choose one line to configure and check the
Exec. Box. Clicking on the ? box pulls up the help for the measurement settings dialog.
Parameters for analysis include:
o Scan Axis: Specifies scan mode. Theta/2-Theta coupled is default and usual
o Mode: Choices are continuous or step. Either mode is possible with SC. Do not use step
scan for scans faster than 1 deg/min (i.e., 1.2 sec/step with a 0.02 step size.
o Range: Specifies range mode of scan as Absolute or Relative. Always choose
absolute for normal scans.
o Start: Specifies start (low) angle (2) for scan. SC/Monochromator combination can go
as low as 1 or less.
o Stop: Specify stop(high) angle (2) for scan. Upper limit is 158.
o Step: Specifies step size in 2 over which data is sampled for collection. Default is
0.02 and is generally best for most uses; may be varied to adjust resolution (smaller for
slow scans or larger for fast scans).
o Speed Duration time: Indicates rate of scan in /min for continuous scan or time spent
per step for a step scan. SC/Monochromator scan rates are typically 4/min or slower.
High-resolution data will require much slower scan rates.
o IS (Incident Slit): Pulldown selects automatic slit control to maintain a consistent
angular aperture (deg) or select a fixed aperture (mm). For SC/Mono the default of 2/3
is generally a good choice.
o RS1 (Rec. Slit 1): Pulldown selects automatic slit control to maintain a consistent angular
aperture (deg) or select a fixed aperture (mm). For SC/Mono the default 2/3 is a good
choice.
o RS2 (Rec. Slit 2): For the SC/Mono the default of 0.3mm is a good choice in BB mode.
o Attenuator: Typically open (no attenuator)
o Comment: Optionally attaches comment to data for this run
o Options: Allows setting specialized options for stages with those capabilities (i.e.,
rotations, tilts, postions, etc.)
o Voltage (kV): Operating kV for scan (40kV is default)
o Current (mA): Operating mA for scan (30kV is default; typically should be set at 40mA)
o Check the box for Drive the 4 axes to the current zero positions after the measurement
is completed. This is only required after your final run to put the instrument is default
mode.
5. When a single measurement line is checked in which all parameters are set as desired, click on
the Execute button to start collecting data. This system will pop up a dialog box that you must
click OK in before data collection starts. After that your initial data file (RAS) will be created
and data collection will be initiated. After a few seconds a real-time display of your data will be
shown on the screen. Other windows may be moved out of the way so you can see the data
trace as it is collected.
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