Rigaku SmartLab Operation Procedures

Transcription

1 Working DRAFT Prepared by Lab Manager Jim Connolly (Revision date: 31-May-2013) Rigaku SmartLab General Operating Overview The Rigaku SmartLab is a highly flexible general purpose X-ray diffractometer system. It includes optics for both standard Bragg-Brentano (BB) and parallel-beam (PB) optics for use with thin films, powders and nano-materials. Detectors include a Scintillation counter (SC) and a high-speed 1D silicon strip detector (D/teX). The SC is operable with or without a graphite monochromator that is switchable between curved-crystal or flat modes for use in BB and PB modes, respectively. Stages include a standard single specimen stage, an automated X-Y adjustable stage, a 10-postiton automatic sample changer, a transmission SAXS stage, a capillary spinner stage, an automated five-axis (X-Y-Z--) mini Eulerian cradle, and an advanced experimental stage (Anton Paar XRK900) capable of real-time diffraction experiments in a variety of controlled environment conditions including elevated temperatures and pressures in reactive or non-reactive controlled-gas environments. All stages make use of the SmartLab s automated vertical (Z) adjustment for precise optical and specimen alignments tailored to the requirements of a particular diffraction experiment. Three different X-ray sources including Cu, Mo, and Co are available for the SmartLab, though we expect to use Cu for almost all work on this system. SmartLab Guidance software is used to interact with and control the system and to interact with the operator about what system parts and accessories need to be added and/or changed as setup and data collection proceeds. The general rationale of how this is done is to select the type of analysis required from a large variety of pre-programmed Package Measurement routines (or from custom setups programmed in Macro mode), mount the specimen for analysis and start the process. The system then reads the components in place and requests changes in system parts based on the requirements of the analysis, and guides the user through optical and sample alignment routines for precise system and sample alignment. For most components optical sensors enable the system to recognize when the proper parts are in the correct place and instruct the operator to make required changes. For some components, (i.e., K-β filters, specimen mounts, and a few others) the system instructs the operator to add or remove them, but cannot pre-detect whether the proper items are in place. In the sections that follow related to particular types of analysis, an attempt is made to go through these procedures in a step-by-step manner to clarify how this works. These procedures will not be perfect (certainly at the beginning) but will be modified as we develop the details of the operating procedures. This document is concerned with operation and data collection utilizing the SmartLab Guidance software. Different sections include information about how to best collect data for different types of specimens to be analyzed. It is not concerned with how your data is analyzed or processed.

2 Rigaku Documentation Documentation is available for the Smartlab system and all associated Rigaku software. The help documents for the Smartlab system is a group of Adobe PDF files that are linked in a HTML (webbrowser-based) index. The documentation is available from the SmartLab Guidance Help menu item, and many of the modules offer context sensitive help by clicking on the question mark icon within it. The documentation is locked in that cut and paste, saving of parts of the manual, converting to other formats, etc. is not allowed. All or parts of the manuals may be printed and digital copies may be obtained by lab users for offline use in their work. Contact the lab manager if you are interested in this. Basic documentation includes the following modules that focus on particular types of analysis: 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 Users s Manual (used to simulate diffraction space for setting up configuration of high-resolution multi-axis rocking-curve analyses) The topic Documentation includes the following sections: Utility (Details about operation of various configuration/calibration operations; some of these are done routinely as part of measurement operations, some are done infrequently by service engineers or system administrators.) Film Thickness Analysis (Background and theory of low-angle reflectivity measurements of thin films using parallel beam optics plus details of operations. Detail sections include step-by-step operations on the SmartLab. Note that we currently have only the Ge(220) 2-bounce monochromator available for analyses.) Crystal Quality Analysis (Background and theory of crystal analysis techniques including rocking curve and reciprocal space mapping. Detail sections include operations with PB and standard optics, plus a variety of hi-res monochromators. Note that we currently have only the Ge(220) 2-bounce monochromator available for analyses.) Texture Analysis (Theory operation of pole figure analysis using the Chi-Phi cradle stage to measure orientation and texture in crystalline materials. Detail sections include step by step operations for pole figure and in-plane pole figure measurements.) Powder Phase ID and Structure analysis from Powders (Good general overview of powder diffraction principles involving Bragg-Brentano (BB) and Parallel Beam (PB) sources and a variety of detectors tailored to the SmartLab. Detail sections include step-by-step operations of the many different package management conditions available.) Nano Structural Analysis (General overview of the transmission and reflection small-angle x-ray scattering (SAXS) methods. Detail sections include configuration and operation details for both methods.) SmartLab Operating Procedures Page 2 of 18 Draft Date: 31-May-2013

3 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 Rigaku s documentation. Contact lab manager Jim Connolly for tips on how to access and use the documentation. Organization of this Manual of Procedures This manual is organized into sections based on the type of analysis to be performed. The initial sections deal with General Operations items including system startup, log in for data collection, how to connect with locations for networked data storage, log-off and shutdown. Some of these sections are useful only for system administrators, others are for all system users. These sections include: SmartLab System Startup (from Powered off state) 1 SmartLab login and startup (from idle state) Setting SmartLab to idle state and logoff Shutdown SmartLab (to powered off state) 1 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): Powder Diffraction, Bragg-Brentano, D/teX Detector Powder Diffraction, Bragg-Brentano, Scintillation Detector w. Monochromator Analysis with Parallel Beam (Scintillation Detector w. Monochromator) for powders Use of the ASC-10 Sample Changer for Powder Diffraction 1 These procedures are included as Appendix B SmartLab Operating Procedures Page 3 of 18 Draft Date: 31-May-2013

4 Thin Film analysis including: o Reflectivity Thickness and Roughness measurements o Rocking Curve and Reciprocal Space Mapping o Texture Analysis by pole figures Nano-Structure analysis using Transmission and Reflection SAXS Non-Ambient Analysis with the Anton Paar XRK900 Stage (including elevated temperature and with flow of reactive and non-reactive gases) SmartLab System Startup The SmartLab is left in operating condition (power on, power to the X-ray tube at idle level of 20kV and 2mA). From the powered-off state (without the chillers operating), there is a separate document that details the cold startup procedures. Cold startup should be done only by the Laboratory System Administrator (or other designated personnel who have been trained in proper startup procedures). Any user who enters the lab and finds the system powered off (i.e., Operate light on the SmartLab panel is off and/or the X-Ray On light on the top of the system is off) should contact the Lab Manager immediately. Log-In and Startup The following procedures should be followed when logging in to the SmartLab to collect data. Depending on how the system was run previously, some components may need to be changed based on the type of analyses to be performed. Components (particularly detectors and the Anton Paar controlled environment stage) should only be changed those who have been trained to do so and have sufficient operator privileges. The default setup for the SmartLab is Cu source, Bragg-Brentano (BB) optics, Standard sample stage, and DTeX high-speed 1d detector w. Kβ filter (or the Scintillation Counter with monochromator). Currently Jim Connolly (Connolly@unm.edu; Office Northrop Hall Rm 108) is the main system administrator; Eric Peterson (ejpete@unm.edu) and Darren Dunphy (ddunphy@unm.edu) are also advanced system users. Other advanced System Users will be listed in an addendum to this document as they are certified and added. Each user of the system must have several different accounts set up, listed below. All except for the UNM NetID needs to be set up by a system administrator. Technically the NetID is not currently required for the SmartLab system, but it will be by the end of May, 2013 and is required to use the other workstations in the XRD lab on which analytical software is installed. The EPSCI network account is set up in advance; the other two are created as part of the setup and training. Do not attempt to use the system until all three accounts are set up. 1. UNM NetID (anyone associated with UNM has one of these. Users must know their NetID name and password) 2. Network account on the EPSCI network (enables access to network file storage where collected data files will be stored and accessed for processing) 3. Local login account on the SmartLab control computer SmartLab Operating Procedures Page 4 of 18 Draft Date: 31-May-2013

5 4. Login/User account for the SmartLab Guidance software (that actually controls the system) There are three levels of system control assigned in the Guidance software through user groups: System Manager, System User and Operator. System Managers can do anything on the system including manage users. System Users can do most operations except manage users. Operators can collect data using manual control, package measurements and macros (but cannot modify them), and cannot reconfigure optics or detectors. All new system users after completion of hands-on training on the use of the system users are given System User accounts. After all accounts have been setup by a system manager/administrator, follow these procedures to set up prior to data collection: 1. Log into the SmartLab computer with your computer user account. 2. Map your L: drive as \\eps3\users\your_username following the separate procedure (Appendix A XRD Lab Systems Login that includes some other one-time computer settings 2 ). This should only need to be done once, but each time you log on you should check and make sure your L: drive is present in Computer before you run the Guidance software. 3. Start the SmartLab Guidance software (shortcut on desktop) and login using your account for Guidance. When Guidance starts it will take a few minutes to establish the connection with the system, polling all system conditions and connected hardware. 4. After Guidance has started, check the hardware status window on the left, and note the Tube Voltage and Tube Current settings. Default operating levels are 40kV and 40mA; idle levels are 20kV and 2mA. If the system is idle, from the Control menu, select Aging and select the aging table named Use Everyday and execute the aging routine. This aging table sets the kv and ma to operating levels. This will take about 8 minutes to complete. When done, the system will be ready to collect data. Setting SmartLab to idle state and logoff When data collection is complete for a session, the system should be returned to the idle state (20 kv, 2 ma) with the default component configuration (i.e., standard sample stage, D/teX Detector). There are exceptions to the component configuration dependent on the expertise of the operator and/or system scheduling (for example, only System Managers or Users are allowed to change detectors, or subsequent users may require a specialized setup such as the Anton Paar XRK900 or the - cradle stage). Users who plan to operate using other than the standard configuration will need to contact one of the system manager/administrators to assist them in getting the system set up properly; as part of the training procedure, we may choose to train users to set up the system for the particular types of analysis they will routinely use, including returning it to the default configuration when done. Important: In general, if a user changes components on the system, the appropriate alignment procedures should be executed by that user prior to shutting the system down, and this should be duly noted in the system logbook so that this will not need to be repeated by the subsequent user. This is 2 These procedures are included as Appendix A. SmartLab Operating Procedures Page 5 of 18 Draft Date: 31-May-2013

6 outlined in the general procedure below. If components are not being changed by the user, step 1 may be skipped. 1. If a detector other than the D/teX is mounted, follow the first six steps in the Data Collection for Single-Sample Bragg Brentano D/teX Detector in the next section, using a blank glass or zero background quartz plate sample holder in the standard sample holder. 2. If the Axes are not at the zero position, open the Tasks Manual Control menu, select Meas and Theta/2-Theta under Axis Control, under Move conditions, and click on Move to move to the exchange (zero) axis position. Close the window when done. 3. If you know someone is coming in right after you to use the instrument this step may be skipped: Select Tasks XG Control from the menu, and set the Tube Voltage and Current to idle. First reduce the Current to 2 ma by entering it in the box and executing, then reduce the accelerating potential to 20 kv. Close the window when done. 4. Log-off from the SmartLab control computer. 5. Make sure all of the work that you have done has been properly entered in the system logbook. Failure to properly log your work can lead directly to termination of lab privileges. Data Collection for Single-Sample Bragg Brentano D/teX Detector (Note: These basic procedures are covered in the SmartLab Guidance Help under the General Measurement General (Bragg-Brentano focusing) D/teX section.) This procedure is used for collection of data from powders packed into or dusted on top of glass sample holders, or packed into or dusted on top of any other single rectangular sample holders (including zero-background quartz plates) that fit into the standard stage (Fig. 1). This procedure includes the D/teX detector center adjustment, but is fundamentally the same as that for the Scintillation Counter/Monochromator as discussed in the next section. For completeness, the steps below include installation of the D/teX detector; this may only be done by a System manager or user (not by an operator). With a change of stage attachments, it can also be used for measurement of any material (powders, films, intact and/or irregular materials, etc.) for which standard Bragg-Brentano Figure 1. Specimen mounted on glass slide in single sample holder diffraction data is to be obtained. The D/teX detector should never be SmartLab Operating Procedures Page 6 of 18 Draft Date: 31-May-2013

7 used for angular ranges with lower than 2 2 values (and is not recommended for ranges less than 4 2). Beware of the OK dialog boxes: Through most of the alignment and startup routines, dialog boxes will pop up that you must signal OK in order for the procedure to proceed. Be attentive as the procedures will not run unless you agree to let them. In some cases, the software will instruct you to change components or parts before the procedure will run. Opening and Closing the Smartlab Enclosure: The SmartLab has an automated interlock system. Nothing operates with the door open, and it is opened and closed to remove and replace components. To open the door, press the Door Lock button (Fig. 2). Initially a long beep is heard; when that becomes intermittent, the door may be opened and samples, attachments, etc. changed. Intermittent beeping will continue while the door is open. When done, close the door and press the Door Lock button again; the beeping will stop and the system will be ready. Figure 2. Door lock button Figure 3. Detector adapter position mark (arrow) All components exchangeable by users are changed using a small 2mm Allen wrench (with rubber handle) that is kept just inside the door to the SmartLab. Always leave this tool in place when you are done with it. 1. Install D/teX Detector: (This cannot be done by System operators. ) If the SC is installed (either with or without the monochromator), remove it by loosening the two allen screws at the top of the bracket and pulling it straight out from the mount. Unplug and remove the ROD adapter (first unit after the first slit assembly), and loosen all other adapters to the right (RPS, second receiving slit, attenuator) and slide them to the left. Mount the D/teX by gently pushing it straight into the mount and tightening the two allen screws at the top of the bracket. Adjust the hash mark at the base of the detector adapter to line up at exactly 351mm (Fig. 3). Then adjust the position of the adapters, tightening allen screws sufficiently eliminate any play (but no harder than required). 2. Check system setup. This should always be SmartLab Operating Procedures Page 7 of 18 Draft Date: 31-May-2013

8 done when starting a data collection session and any time following a change of components. From the Menu, choose Options Hardware Configuration. The system will check all installed parts and report what is there. Figure 4. SmartLab Hardware Configuration display screen 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; don t do it if it isn t 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 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 Kβ 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- SmartLab Operating Procedures Page 8 of 18 Draft Date: 31-May-2013

9 15 minutes. Occasionally it will fail on the first attempt 3 ; if this happens, just repeat the procedure. 5. D/teX Center Correction does not need to be done unless the detector has recently been changed and not aligned after the change. It should be done if the SC has just been removed and the D/teX installed. If done, choose to use the direct beam using the default scan conditions. Remove the alignment slit if it is present. The detector configuration is the same as for the Optics Alignment above (ROD adapter removed, detector and other optical components shifted to the left) and will be shown in the graphic when this is selected. Center correction takes no more than a minute or two to complete. 6. Sample Alignment: Place your mounted sample in the sample holder, and double click on Sample Alignment. If you will be running a series of samples that are mounted in the same type of holder, you may do this for the first sample only. If samples are mounted in different manners (i.e., powder or film on top of slide, etc.) this should probably done prior to each run. The general rule is that alignment is only required if there is a significant difference in the mount geometry between samples. Choose your approximate sample thickness (including your holder, typically 3 mm 4 ), choose the recommended sequence and Execute. If your sample is not perfectly flat, check the box for Curved Sample (Z scan only) that adjusts only the Z (vertical) position and it will skip the rocking part of the alignment. Full sample alignment typically takes about 10 minutes. (Note: To learn a bit more about the alignment sequence used, click on the? icon in the alignment dialog. This will bring up the help documentation that explains the sequence of tilts and scans used to complete the alignment.) 7. Double-click on General Measurement (BB). A window (below showing default values) will pop up through which data collection is setup and executed. The bullets below the sample window detail everything in this window and what should be entered in the various sections of it: 3 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. 4 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. SmartLab Operating Procedures Page 9 of 18 Draft Date: 31-May-2013

10 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 Rigaku s 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.) 5 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. SmartLab Operating Procedures Page 10 of 18 Draft Date: 31-May-2013

11 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 SmartLab Operating Procedures Page 11 of 18 Draft Date: 31-May-2013

12 shown on the screen. Other windows may be moved out of the way so you can see the data trace as it is collected. 8. After data collection is completed, you may close the general measurement window by clicking Cancel. Important: Do not choose the OK button after your run is done as this can cause your data file to be overwritten. If this is a setup you plan to reuse, you may Export it prior to closing and save it in a location on your L: drive; to reload it later, Import it from the General measurement window. All previous settings (including filenames) are saved in the Export file so these need appropriate editing when reused to avoid overwriting existing data files 9. The SmartLab Guidance software does not incrementally save data to disc as it is collected, but must complete the data collection of the previous step before files are saved. For this reason, it is important to not interrupt the data collection until the system has finished the job. When done, you will have three data files These will be: your_filename.ras, your_filename_theta_2- Theta.RAW, and your_filename_theta_2-theta.asc. 10. If you are done collecting data, check the schedule to see if anyone is coming in to use the instrument immediately after you. If they are, you may log off the system and leave it in full power mode. If nobody is coming in until the next day (or later) follow the procedure for Setting SmartLab to idle state and logoff. Notes on the D/teX Detector: Slits, Background and Beam Stop When used with the D/teX detector the IS, RS1 and RS2 slit settings may be adjusted for optimal performance. What those settings are depend on the particular -2 angular range required for a particular material. Initial tests of the D/teX detector suggest a practical analytical lower 2 limit of 2. At less than 2 2, the IS and RS1 settings must be reduced so much that the advantage of using a 1D detector is effectively lost. At the 2 2 start point, an IS setting of 0.5 and an RS1 setting of 2.0 produces an elevated background at the lower limit that does not cause an overload of the detector 6 and good data in the low angle range. For patterns where start angles are 5 2 or higher, the fully open slits may be used (IS = 7.0mm or ; RS1 and RS2 = 20mm). For samples that require very low 2 angles (under 2 ) the D/teX detector is not the best choice, and the use of the Scintillation counter + monochromator is the preferred setup. Even when possible, the fully open slits may not yield the best data, since in some cases flat specimen errors at low angles can cause peak broadening and axial divergence can induce asymmetry in the peaks. Reducing the IS size while keeping the RS1 and RS2 open can reduce these errors while keeping overall intensities high. Users may need to experiment to see what settings work best. 6 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. SmartLab Operating Procedures Page 12 of 18 Draft Date: 31-May-2013

13 The low-angle detector overload problem (i.e., Error code (2)) may be ameliorated by the use of a special knife-edge attachment that is designed to limit the low angle direct beam impingement on the detector. This attachment can only be used with perfectly flat specimens and the combination of knifeedge height adjustment and appropriate IS and RS1 slit settings to produce optimal results without overload errors. As we learn more about optimal settings, this section will be modified and expanded. Another option (and one that is generally recommended by Rigaku) is to use the low-angle beam stop when using the D/teX detector at low angles. This will eliminate the possibility of detector overload. This device is located immediately to the right of the sample stage (Fig. 5) and slides in and out of the beam path, limiting low angle X-rays from entering the detector, allowing low start angles at wide-open slit settings. With the beam stop in place and fully open slits (IS=7mm, RS1 & RS2=20mm), there is no signal to the detector until ~1.8 2, and Figure 5. D/teX Beam stop in position for analysis signal is notably reduced until ~ An operational problem noted when using the beam stop with a zero-background plate is the presence of a small peak slightly above background (but clearly present) that is at ~ that appears to be related to the presence of the beam stop. If using the beam stop, users are encouraged to do a quick scan on a blank sample holder to assure that all sample peaks are truly from the sample. 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. SmartLab Operating Procedures Page 13 of 18 Draft Date: 31-May-2013

14 Data Collection for Single-Sample Bragg Brentano SC+Monochromator (Note: These basic procedures are covered in the SmartLab Guidance Help under the General Measurement General (Bragg-Brentano focusing) section.) This section is for collection of data utilizing BB optics and the scintillation counter + monochromator 0D combination instead of the D/teX 1D detector. These procedures are almost identical to those in the previous section except for items specific to the detector setup. 1. Install the Scintillation Counter with Monochromator. Remove the D/teX detector. Remove (if installed) the direct-install bracket from the SC. Mount the SC into the Monochromator and attach the monochromator to the optical bench, making sure the adjustment mark is positioned at exactly 351.5mm. Install the Monochromater slit (labeled BBM) in the monochromator. When done, Check system setup (From the Menu, choose Options Hardware Configuration) to make sure the system recognizes the changes. The detector should be identified as the SC- 70. Close the window after the check. 2. Choose Measurement Package. From the Tasks menu, choose Package Measurement, and choose the package appropriate to the task. With the SC/Monochromator in place, choose General (Bragg Brentano focusing). This setup can also be used for a multitude of other types of analysis as discussed later; different types of analysis require different optics to be added or removed in the next step. There will be a series of steps that are followed under standard package measurement conditions. 3. 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; don t do it if it isn t 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 Focusing) and check Change optics without alignment that uses the latest saved alignment settings for that measurement package. To perform the alignment, make sure the Change optics without alignment box is not checked and select execute. You will need to add the height reference sample plate, add (and plug in) the ROD adapter and shift detector-side components as instructed by the software before it will perform the alignment. Make sure all the allen screws that hold the components in place are sufficiently tight to hold everything in place (i.e., nothing wobbles on the component bench). Optics alignment typically takes minutes. 4. Sample Alignment: Place your mounted sample in the sample holder, and double click on Sample Alignment. If you will be running a series of samples that are mounted in the same type of holder, you may do this for the first sample only. If samples are mounted in different manners (i.e., powder or film on top of slide, etc.) this should probably done prior to each run. The general rule is that alignment is only required if there is a significant difference in the mount geometry between samples. Choose your approximate sample thickness (including your holder, typically 2-3 mm), choose the recommended sequence and Execute. If your sample is notably irregular, check the box for Curved Sample (Z scan only) that adjusts only the Z (vertical) position and it will skip the rocking part of the alignment (which will often fail for SmartLab Operating Procedures Page 14 of 18 Draft Date: 31-May-2013

15 irregular samples). Full sample alignment typically takes about 10 minutes, Curved Sample alignment takes about 5 minutes. (Note: To learn a bit more about the alignment sequence used, click on the? icon in the alignment dialog. This will bring up the help documentation that explains the sequence used.) Double-click on General Measurement (BB). A window (below showing default values) will pop up through which data collection is setup and executed: 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 Rigaku s 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 SmartLab Operating Procedures Page 15 of 18 Draft Date: 31-May-2013

16 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. SmartLab Operating Procedures Page 16 of 18 Draft Date: 31-May-2013

17 6. When collecting multiple patterns repeat the procedure, changing filenames and data collection parameters as appropriate for your samples. Failure to change the filename will cause previously collected data to be over written. 7. After data collection is completed, you may close the general measurement window by clicking Cancel. Important: Do not choose the OK button after your run is done as this can cause your data file to be overwritten. If this is a setup you plan to reuse, you may Export it prior to closing and save it in a location on your L: drive; to reload it later, Import it from the General measurement window. All previous settings (including filenames) are saved in the Export file so these need appropriate editing when reused to avoid overwriting existing data files 8. The SmartLab Guidance software does not incrementally save data to disc as it is collected, but must complete the data collection of the previous step before files are saved. For this reason, it is important to not interrupt the data collection until the system has finished the job. When done, you will have three data files These will be: your_filename.ras, your_filename_theta_2- Theta.RAW, and your_filename_theta_2-theta.asc. 9. If you are done collecting data, check the schedule to see if anyone is coming in to use the instrument immediately after you. If they are, you may log off the system and leave it in full power mode. If nobody is coming in until the next day (or later) follow the procedure for Setting SmartLab to idle state and logoff. Analysis with Parallel Beam (Scintillation Detector w. Monochromator) for powders and other materials (Note: These basic procedures are covered in the SmartLab Guidance Help under the General (medium resolutions PB/PSA) section.) (For powders, procedures are fundamentally the same as those for powders using the Scintillation and D/teX detectors, with some variations in how the optics alignments are handled. Parallel Beam analysis requires the use of the Scintillation counter, preferably with monochromator; PB is not compatible with the D/teX detector. Details for this section are Under Development.) Thin Film analysis: Reflectivity Thickness and Roughness measurements (Note: These basic procedures are covered in the SmartLab Guidance Help under the Film thickness analysis section.) (Details for this section are Under Development. As configured, our instrument includes the Medium Resolution optics and the high resolution Ge(220)x2 optics.) Thin Film analysis: Rocking Curve and Reciprocal Space Mapping SmartLab Operating Procedures Page 17 of 18 Draft Date: 31-May-2013

18 (Note: These basic procedures are covered in the SmartLab Guidance Help under the Crystal Quality analysis section.) (Details for this section are Under Development. Our instrument includes the Medium Resolution optics and the high resolution Ge(220)x2 optics.) Thin Film analysis: Texture Analysis by pole figures (Note: These basic procedures are covered in the SmartLab Guidance Help under the Texture analysis section.) (Details for this section are Under Development. Our instrument is capable of doing a standard Pole Figure analysis with our 5-axis chi-phi stage utilizing medium resolution parallel beam optics.) Nano-Structure analysis using Transmission and Reflection SAXS (Note: These basic procedures are covered in the SmartLab Guidance Help under the Nano-Structural analysis section.) (Our instrument is capable transmission and reflection SAXS. Procedures for effective utilization of this method for different materials are under development.) Non-Ambient Analysis with the Anton Paar XRK900 Stage (including elevated temperature and with flow of reactive and non-reactive gases) (Eric Peterson ejpete@unm.edu is developing methods and procedures for the use of this stage for non-ambient analysis under controlled temperature and gas environments to include a gas-handling flow and delivery system that is being installed. Interested users should contact Eric if interested in learning about and using this capability.) Advanced System Users Qualified to Change Stages, Detectors and other System Components (This list current as of 31-May-2013) Jim Connolly (Connolly@unm.edu) Eric Peterson (ejpete@unm.edu) Darren Dunphy (ddunphy@unm.edu) SmartLab Operating Procedures Page 18 of 18 Draft Date: 31-May-2013