In-Plane Pole Figure Measurement Part

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1 In-Plane Pole Figure Measurement Part

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3 Contents Contents 1. How to set Part conditions Setting conditions Customizing scan conditions and slit conditions Measurement sequence...13 In-Plane Pole Figure Measurement Part i

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5 1.1 Setting conditions 1. How to set Part conditions In this chapter, how to set the In-Plane Pole Figure Measurement Part conditions is described. CAUTION: The SmartLab (in-plane) goniometer and either of the following hardware will be required for proper execution of this Part. Standard χ cradle Standard Z stage + χ axis + φ axis 1.1 Setting conditions Set the basic conditions in the In-Plane Pole Figure Measurement dialog box. The scan conditions and slit conditions of the in-plane pole figure measurement are determined based on the basic conditions. The scan conditions and slit conditions can also be customized. Fig In-Plane Pole Figure Measurement dialog box File name Sample name Memo Enter the name of the file to save the measurement data in. Enter the sample name (optional). The sample name entered here will be saved in the measurement data file. Enter the memo (optional). The memo entered here will be saved in the measurement data file. In-Plane Pole Figure Measurement Part 1

6 1. How to set Part conditions Measurement angle (deg) Step Speed Enter the diffraction angle 2-theta to be used for pole figure measurement. If the pre-measurement is made, the data measurement will be made at the diffraction angle 2-theta determined based on the pre-measurement results, regardless of the value entered here. Select the step width from Fine, Standard, or Coarse. In ordinary cases, select Standard. Sets the step widths of the alpha and beta axes Fine to 1 deg. Sets the step widths of the alpha and beta axes Standard to 3 deg. Sets the step widths of the alpha and beta axes Coarse to 5 deg. Select the scan speed from Slow, Standard, or Fast. In ordinary cases, select Standard. Sets the scan speed of the beta axis to 100 Slow deg/min. Sets the scan speed of the beta axis to 150 Standard deg/min. Sets the scan speed of the beta axis to 200 Fast deg/min. Execute the pre-measurement Check the Execute the pre-measurement box to make the pre-measurement to determine the diffraction angle 2-theta for the data measurement. Run recommended sequence Makes the in-plane pole figure measurement using the recommended sequence. Customize conditions Customize Calculated scan duration Makes the in-plane pole figure measurement under the conditions specified in the Customize dialog box. When the Customize conditions radio button is selected, click the Customize button, then set the scan conditions and slit conditions. 1.2 Customizing scan conditions and slit conditions Shows the calculated duration of the in-plane pole figure measurement. 2 In-Plane Pole Figure Measurement Part

7 1.1 Setting conditions Execute Executes the in-plane pole figure measurement under the conditions specified in the In-Plane Pole Figure Measurement dialog box. CAUTION: Clicking the Cancel button after executing the in-plane pole figure measurement does not cancel the specified conditions. Tip: The in-plane pole figure measurement is executed with the In-Plane Pole Figure Measurement dialog box open. While the in-plane pole figure measurement is running, the Part conditions cannot be changed. They can be changed again after the measurement has been completed. The setting of invalid. (Show confirmation messages) on the flow bar becomes Import Loads the saved Part conditions. Clicking the Import button opens the Import dialog box. Select the folder including the file you want to import from the Folder tree view. In the Condition file list, select the condition file you want to import and click the OK button to load the Part conditions. In-Plane Pole Figure Measurement Part 3

8 1. How to set Part conditions Export Saves the specified Part conditions in a file. Clicking the Export button opens the Export dialog box. From the Folder tree view, select a destination folder to save the conditions file then enter a file name in the File name box. Enter comments in the Memo box, if needed. After entering them, click the OK button. OK Sets the conditions and closes the dialog box. Cancel CAUTION: When selecting another Package measurement or switching the task to the Manual Control task, etc. the specified conditions will be cancelled. To save the specified conditions in a file, click the Export button and save the conditions. Does not set the conditions and closes the dialog box. Tip: Clicking the Cancel button also cancels the conditions specified in the Customize dialog box.? Opens the online help of this Part. 4 In-Plane Pole Figure Measurement Part

9 1.2 Customizing scan conditions and slit conditions 1.2 Customizing scan conditions and slit conditions If you want to customize the scan conditions and slit conditions of the in-plane pole figure measurement, set the conditions in the Customize dialog box. Tip: Refer to 2. Measurement sequence to set the scan conditions and slit conditions. Fig Customize dialog box In-Plane Pole Figure Measurement Part 5

10 1. How to set Part conditions Measurement angle (deg) Step Speed Enter the diffraction angle 2-theta to be used for pole figure measurement. If the pre-measurement is made, the data measurement will be made at the diffraction angle 2-theta determined based on the pre-measurement results, regardless of the value entered here. Select the step width from Fine, Standard, or Coarse. In ordinary cases, select Standard. Sets the step widths of the alpha and beta axes Fine to 1 deg. Sets the step widths of the alpha and beta axes Standard to 3 deg. Sets the step widths of the alpha and beta axes Coarse to 5 deg. Select the scan speed from Slow, Standard, or Fast. In ordinary cases, select Standard. Sets the scan speed of the beta axis to 100 Slow deg/min. Sets the scan speed of the beta axis to 150 Standard deg/min. Sets the scan speed of the beta axis to 200 Fast deg/min. Execute the pre-measurement Check the Execute the pre-measurement box to make the pre-measurement to determine the diffraction angle 2-theta for the data measurement. Tip: When the Close button is clicked after setting four conditions in the In-plane pole figure measurement conditions section in the Customize dialog box, the conditions in the In-Plane Pole Figure Measurement dialog box will also be changed. 6 In-Plane Pole Figure Measurement Part

11 1.2 Customizing scan conditions and slit conditions Table shows the choices of the aperture angles of the parallel slits and PSA, and the length of the length limiting slit. Soller/PSC (deg) IS L (mm) PSA (deg) Soller (deg) Select the aperture angle of the incident parallel slit. Select the length of the length limiting slit. Select the aperture angle of the PSA. Select the aperture angle of the receiving parallel slit. Table Choices of the length or aperture angle of each slit Slit Soller/PSC (deg) IS length limiting slit (mm) PSA (deg) Soller (deg) Length or aperture angle 5.0, 2.5, 1.0, 0.5, 0.15, Open, None, No_unit 15.0, 10.0, 5.0, 2.0, 0.5, None 1.0, 0.5, 0.114, Open, None, No_unit 5.0, 2.5, 1.0, 0.5, 0.114, Open, None, No_unit Pre-measurement conditions Check the Pre-measurement conditions box to make the pre-measurement to determine the diffraction angle 2-theta for the data measurement. Scan axis Mode Range Start (deg) Select 2-Theta or 2-ThetaChi as the scan axis. Select the scan mode from Continuous or Step. Select the scan range specification method from Absolute or Relative. When Absolute is selected as the scan range specification method, enter the absolute start angle of the scan. When Relative is selected, enter the relative distance of the start angle from the measurement origin. In-Plane Pole Figure Measurement Part 7

12 1. How to set Part conditions Stop (deg) Step (deg) When Absolute is selected as the scan range specification method, enter the absolute stop angle of the scan. When Relative is selected, enter the relative distance of the stop angle from the measurement origin. Enter the step width of the scan. Speed (deg/min) / Duration time (sec) When Continuous is selected as the scan mode, enter the scan speed. When Step is selected as the scan mode, enter the duration time per measurement point. IS (mm) Enter the width of the incident slit. RS1 (mm) Enter the width of the receiving slit # 1. RS2 (mm) Enter the width of the receiving slit # 2. Attenuator Select the attenuator to be used for the data measurement from Open, 1/70, 1/1000, 1/10000, or Auto. Tip: If Auto is selected, an automatic attenuator scan is performed while the attenuator is automatically switched based on intensity. Measurement origin Check the Measurement origin box to drive the five axes (2-theta, omega, chi, 2-theta-chi, phi) to the positions entered in the 2-Theta (deg), Omega (deg), Chi (deg), 2-ThetaChi (deg), and Phi (deg) boxes before executing the pre-measurement. CAUTION: The 2-ThetaChi (deg) box is disabled when 2-Theta is selected as the scan axis in the Pre-measurement conditions section. 2-Theta (deg) Enter the position to drive the 2-theta axis to. Omega (deg) Chi (deg) 2-ThetaChi (deg) Phi (deg) Enter the position to drive the omega axis to. Enter the position to drive the chi axis to. Enter the position to drive the 2-theta-chi axis to. Enter the position to drive the phi axis to. 8 In-Plane Pole Figure Measurement Part

13 1.2 Customizing scan conditions and slit conditions Read current positions Sets the current position of each axis in the 2-Theta (deg), Omega (deg), Chi (deg), 2-ThetaChi (deg), and Phi (deg) boxes. Mode Range Start (deg) Stop (deg) Step (deg) Select the scan mode from Continuous or Step. Select the scan range specification method from Absolute or Relative. When Absolute is selected as the scan range specification method, enter the absolute start angle of the scan. When Relative is selected, enter the relative distance of the start angle from the measurement origin. When Absolute is selected as the scan range specification method, enter the absolute stop angle of the scan. When Relative is selected, enter the relative distance of the stop angle from the measurement origin. Enter the step width of the scan. Speed (deg/min) / Duration time (sec) When Continuous is selected as the scan mode, enter the scan speed. When Step is selected as the scan mode, enter the duration time per measurement point. IS (mm) Enter the width of the incident slit. RS1 (mm) Enter the width of the receiving slit # 1. RS2 (mm) Enter the width of the receiving slit # 2. Attenuator Select the attenuator to be used for the data measurement from Open, 1/70, 1/1000, 1/10000, or Auto. Tip: If Auto is selected, an automatic attenuator scan is performed while the attenuator is automatically switched based on intensity. In-Plane Pole Figure Measurement Part 9

14 1. How to set Part conditions Set the measurement origin when Relative is selected in the Range box in the Data measurement conditions section. 2-ThetaB (deg) Alpha (deg) Beta (deg) Calculate 2-Theta (deg) Omega (deg) 2-ThetaChi (deg) Phi (deg) Read current positions Enter the position of the 2-thetaB axis (a pole figure axis). When the Pre-measurement conditions box is checked, the data measurement is made at the diffraction angle 2-theta determined based on the pre-measurement results (the 2-ThetaB (deg) box is disabled). Enter the position of the alpha axis. Enter the position of the beta axis. Calculates the positions of the pole figure axes based on the angles of the four measurement axes. Enter the position of the 2-theta axis. Enter the position of the omega axis. Enter the position of the 2-theta-chi axis. Enter the position of the phi axis. Sets the current position of each axis in the 2-Theta (deg), Omega (deg), 2-ThetaChi (deg), and Phi (deg) boxes. Exec. Axis Width (+/-) (deg) Speed (deg/min) If the sample will be oscillated during the measurement, check the Exec. box and set the oscillation conditions. Select the axis to oscillate. Enter the oscillation width. Enter the oscillation speed. 10 In-Plane Pole Figure Measurement Part

15 1.2 Customizing scan conditions and slit conditions Set recommended values Calculated scan duration Close Checks the Pre-measurement conditions box, and sets the conditions in the Slit conditions, Pre-measurement conditions, and Data measurement conditions sections to the recommended values based on the conditions specified for Measurement angle (deg), Step, and Speed. The recommended values are shown in Tables through Shows the calculated duration of the in-plane pole figure measurement. Closes the Customize dialog box. Table Recommended conditions of the manual exchange slits Optics attribute Soller/ PSC IS length limiting slit PSA Soller Medium resolution parallel beam/rs Medium resolution parallel beam/psa 0.5 deg The length used in the High resolution parallel beam Ge(220)x2/RS High resolution parallel beam Ge(400)x2/RS 0.5 deg Sample Alignment Open 0.5 deg Ultra-high resolution parallel beam Ge(220)x4/RS Ultra-high resolution parallel beam Ge(440)x4/RS Part (or 10 mm) Table Recommended conditions of the pre-measurement Scan Mode Range Start Stop Step Speed IS RS1 RS2 Attenuator axis theta Continuous Relative Auto deg deg deg deg/min mm mm mm Table Recommended positions of the pre-measurement origin when the Measurement origin box is unchecked (scan axis is 2-theta) Origin Unchecked 2-theta Omega Chi 2-ThetaChi Phi Measurement axis The value entered in the Measurement angle (deg) in the In-plane pole figure measurement conditions section. Half the value entered in the Measurement angle (deg) in the In-plane pole figure measurement conditions section. 0 deg 0 deg In-Plane Pole Figure Measurement Part 11

16 1. How to set Part conditions Table Recommended positions of the pre-measurement origin when the Measurement origin box is unchecked (scan axis is 2-theta-chi) Origin Unchecked 2-theta Omega Chi 2-ThetaChi Phi Measurement axis 0.5 deg 0.5 deg 0 deg The value entered in the Measurement angle (deg) in the In-plane pole figure measurement conditions section. Half the value entered in the Measurement angle (deg) in the In-plane pole figure measurement conditions section. Table Recommended conditions of the data measurement Scan Attenuator Mode Range Start Stop Step Speed IS RS1 RS2 axis 1 deg (Fine) Alpha Absolute 0 deg 5 deg (Coarse) 90 3 deg deg (Standard) 1 deg (Fine) 100 deg/min (Slow) Beta Conti deg 150 deg/min Absolute 0 deg nuous deg (Standard) (Standard) 1 mm 2 mm 2 mm Auto 5 deg (Coarse) 200 deg/min (Fast) Table Recommended positions of the data measurement origin when Absolute is selected for Range in the Data measurement conditions section Pole figure axis Measurement axis The value entered The value entered 2-thetaB in the Measurement angle (deg) in the Measurement angle (deg) 2-theta in the In-plane pole figure in the In-plane pole figure measurement conditions section. measurement conditions section. Alpha 90 deg Omega Half the value entered in the Measurement angle (deg) in the In-plane pole figure measurement conditions section. Beta 0 deg Chi 0 deg Phi 0 deg 12 In-Plane Pole Figure Measurement Part

17 2. Measurement sequence The in-plane pole figure measurement is performed automatically when Run recommended sequence is selected in the In-Plane Pole Figure Measurement dialog box. Described below is the measurement sequence when Run recommended sequence is selected. CAUTION: If the sample is changed, execute sample alignment using the In-Plane Sample Alignment Part before executing this Part as a general rule. (1) Set the widths of the slits (IS, RS1, RS2), the length of the incident length limiting slit (IS L), and the aperture angles of the Soller slits to the recommended values. IS, IS L(recommended value) RS1 (recommended value) RS2 (recommended value) Soller/PSC (recommended value) Fig. 2.1 PSA (recommended value) Soller (recommended value) Setting the slits and Soller slits CAUTION: Figure 2.1 shows the medium resolution parallel beam/rs optics, which may differ from the current optics. (2) Make the pre-measurement (2-theta scan) under the recommended conditions. 2θ scan IS, IS length limiting slit RS1 RS2 Soller/PSC PSA Soller Fig. 2.2 Pre-measurement (2-theta scan) (3) Determine the diffraction angle 2-theta used for the data measurement based on the obtained measurement profile. (4) Make the data measurement at the diffraction angle determined in step (3). β(φ) scan at every α(χ) step IS, IS length limiting slit RS1 RS2 Soller/PSC PSA Soller Fig. 2.3 Data measurement In-Plane Pole Figure Measurement Part 13