Precise Theta/2-Theta Measurement (PB/PSA) Part

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James Cameron Ferguson
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1 Precise Theta/2-Theta Measurement (PB/PSA) Part

3 Contents Contents 1. How to set Part conditions Setting conditions Customizing scan conditions and slit conditions Measurement sequence...15 Precise Theta/2-Theta Measurement (PB/PSA) Part i

1.1 Setting conditions 1. How to set Part conditions In this chapter, how to set the Precise Theta/2-Theta Measurement (PB/PSA) Part conditions is described. 1.1 Setting conditions Set the basic conditions in the Precise Theta/2-Theta Meas.

5 1.1 Setting conditions 1. How to set Part conditions In this chapter, how to set the Precise Theta/2-Theta Measurement (PB/PSA) Part conditions is described. 1.1 Setting conditions Set the basic conditions in the Precise Theta/2-Theta Meas. (PB/PSA) dialog box. The scan conditions and slit conditions of the precise theta/2-theta measurement are determined based on the basic conditions. The scan conditions and slit conditions can also be customized. Fig Precise Theta/2-Theta Meas. (PB/PSA) 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. Sample form Select the form of sample to be measured from Powder / Bulk / Film, Thin film, or Capillary / Film. Powder / Bulk / Film Performs the theta/2-theta scan. Thin film Performs the 2-theta scan at omega = 1. Capillary / Film Performs the 2-theta scan at omega = 0. Precise Theta/2-Theta Measurement (PB/PSA) Part 1

6 1. How to set Part conditions Sample width (mm) Sample height (mm) Enter the sample width. Enter the sample height. Tip: The sample width and sample height refer to the dimensions (unit: mm) of the sample in the directions shown below. Incident direction of x-ray when φ =0 Sample height Sample width Sample thickness Theta/2-theta measurement range (deg) Enter the range of the precise scan. Enter the start angle in the left box, and the stop angle in the right box. Step (deg) Select 1/10, 1/7, or 1/5. In ordinary cases, select 1/7. Duration time (sec) Select 20000, 10000, 5000, 3000, or In ordinary cases, select Tip: The duration time will be calculated so that the intensity of the highest peak becomes the value (unit: counts) selected in the Duration time (sec) box. Monochromatization Select Multi-layer mirror or Multi-layer mirror + Diffracted beam monochromator. In ordinary cases, select Multilayer mirror. Multi-layer mirror Multi-layer mirror + Diffracted beam monochromator The multi-layer mirror decreases the ratio of Kβ x-rays against Kα x-rays to about 0.5%. If the sample generates a lot of fluorescent x-rays, the background level rises and the P/B ratio becomes bad. In this case, it is recommended to use both the multi-layer mirror and DBM unit (option) for measurements. The diffracted beam monochromator method is to monochromatize x-rays using the diffraction by a crystal. This setting removes almost all x-rays (Kβ x-rays, continuous x-rays, fluorescent x-rays, etc.) other than those of the selected wavelength and provides measurement data with a low background level. 2 Precise Theta/2-Theta Measurement (PB/PSA) Part

7 1.1 Setting conditions FWHM and intensity settings Select Use pre-measurement results or Use specified values to set the FWHM and intensity to calculate the step width and duration time based on. Change thresholds FWHM threshold (deg) Check the Change thresholds box to change the values of the FWHM and intensity thresholds when Use pre-measurement results is selected. Enter the value of the FWHM threshold if the Change thresholds box is checked. The step width of the precise theta/2-theta measurement will be determined as shown in the table below. Minimum FWHM of the peaks obtained by the pre-measurement How to determine the step width Narrower than the FWHM threshold Use the FWHM threshold. Use the minimum FWHM of the peaks Wider than the FWHM threshold obtained by the pre-measurement. Intensity threshold (cps) Enter the value of the intensity threshold if the Change thresholds box is checked. The duration time of the precise theta/2-theta measurement will be determined as shown in the table below. Maximum intensity of the peaks obtained by the pre-measurement How to determine the duration time FWHM (deg) Intensity (cps) Lower than the intensity threshold Use the intensity threshold. Use the maximum intensity of the peaks Higher than the intensity threshold obtained by the pre-measurement. When Use specified values is selected, enter the value of FWHM. The step width of the precise theta/2-theta measurement will be determined based on the value entered here. When Use specified values is selected, enter the value of intensity. The duration time of the precise theta/2-theta measurement will be determined based on the value entered here. Run recommended sequence Makes the precise theta/2-theta measurement using the recommended sequence. Customize conditions Customize Makes the precise theta/2-theta 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. エラー! 参照元が見つかりません Precise Theta/2-Theta Measurement (PB/PSA) Part 3

8 1. How to set Part conditions Calculated scan duration Shows the calculated duration of the pre-measurement when Use pre-measurement results is selected, and shows the calculated duration of the data measurement when Use specified values is selected. Tip: If Use pre-measurement results is selected, the step width and duration time of the data measurement determined based on the pre-measurement results. The calculated duration of the data measurement will be displayed in the History window. Execute Executes the precise theta/2-theta measurement under the conditions specified in the Precise Theta/2-Theta Meas. (PB/PSA) dialog box. CAUTION: Clicking the Cancel button after executing the precise theta/2-theta measurement does not cancel the specified conditions. Tip: The precise theta/2-theta measurement is executed with the Precise Theta/2-Theta Meas. (PB/PSA) dialog box open. While the precise theta/2-theta 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. 4 Precise Theta/2-Theta Measurement (PB/PSA) Part

9 1.1 Setting 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. Precise Theta/2-Theta Measurement (PB/PSA) Part 5

10 1. How to set Part conditions 1.2 Customizing scan conditions and slit conditions If you want to customize the scan conditions and slit conditions of the precise theta/2-theta measurement, set the conditions in the Customize dialog box. Tip: Refer to エラー! 参照元が見つかりません to set the scan conditions and slit conditions. Fig Customize dialog box 6 Precise Theta/2-Theta Measurement (PB/PSA) Part

1.2 Customizing scan conditions and slit conditions Sample form Select the form of sample to be measured from Powder / Bulk / Film, Thin film, or Capillary / Film.

11 1.2 Customizing scan conditions and slit conditions Sample form Select the form of sample to be measured from Powder / Bulk / Film, Thin film, or Capillary / Film. Sample width (mm) Sample height (mm) Powder / Bulk / Film Performs the theta/2-theta scan. Thin film Performs the 2-theta scan at omega = 1. Capillary / Film Performs the 2-theta scan at omega = 0. Enter the sample width. Enter the sample height. Tip: The sample width and sample height refer to the dimensions (unit: mm) of the sample in the directions shown below. Incident direction of x-ray when φ =0 Sample height Sample width Sample thickness Theta/2-theta measurement range (deg) Enter the range of the precise scan. Enter the start angle in the left box, and the stop angle in the right box. Step (deg) Select 1/10, 1/7, or 1/5. In ordinary cases, select 1/7. Duration time (sec) Select 20000, 10000, 5000, 3000, or In ordinary cases, select Tip: The duration time will be calculated so that the intensity of the highest peak becomes the value (unit: counts) selected in the Duration time (sec) box. Precise Theta/2-Theta Measurement (PB/PSA) Part 7

12 1. How to set Part conditions Monochromatization Select Multi-layer mirror or Multi-layer mirror + Diffracted beam monochromator. In ordinary cases, select Multilayer mirror. Multi-layer mirror The multi-layer mirror decreases the ratio of Kβ x-rays against Kα x-rays to about 0.5%. If the sample generates a lot of fluorescent x-rays, the background level rises and the P/B ratio becomes bad. In this case, it is Multi-layer recommended to use both the multi-layer mirror mirror and DBM unit (option) for + measurements. The diffracted beam Diffracted beam monochromator monochromator method is to monochromatize x-rays using the diffraction by a crystal. This setting removes almost all x-rays (Kβ x-rays, continuous x-rays, fluorescent x-rays, etc.) other than those of the selected wavelength and provides measurement data with a low background level. FWHM and intensity settings Select Use pre-measurement results or Use specified values to set the FWHM and intensity to calculate the step width and duration time based on. Change thresholds FWHM threshold (deg) Check the Change thresholds box to change the values of the FWHM and intensity thresholds when Use pre-measurement results is selected. Enter the value of the FWHM threshold if the Change thresholds box is checked. The step width of the precise theta/2-theta measurement will be determined as shown in the table below. Minimum FWHM of the peaks obtained by the pre-measurement How to determine the step width Narrower than the FWHM threshold Use the FWHM threshold. Use the minimum FWHM of the peaks Wider than the FWHM threshold obtained by the pre-measurement. Intensity threshold (cps) Enter the value of the intensity threshold if the Change thresholds box is checked. The duration time of the precise theta/2-theta measurement will be determined as shown in the table below. Maximum intensity of the peaks obtained by the pre-measurement Lower than the intensity threshold Higher than the intensity threshold How to determine the duration time Use the intensity threshold. Use the maximum intensity of the peaks obtained by the pre-measurement. 8 Precise Theta/2-Theta Measurement (PB/PSA) Part

13 1.2 Customizing scan conditions and slit conditions FWHM (deg) Intensity (cps) When Use specified values is selected, enter the value of FWHM. The step width of the precise theta/2-theta measurement will be determined based on the value entered here. When Use specified values is selected, enter the value of intensity. The duration time of the precise theta/2-theta measurement will be determined based on the value entered here. Tip: When the Close button is clicked after setting the conditions in the Precise theta/2-theta measurement conditions and FWHM and intensity settings sections in the Customize dialog box, the conditions in the Precise Theta/2-Theta Meas. (PB/PSA) dialog box will also be changed. Table shows the choices of the widths or lengths of the slits and the aperture angles of the parallel slits. Soller/PSC (deg) IS (mm) IS L (mm) RS1 (mm) PSA (deg) Soller (deg) RS2 (mm) Select the aperture angle of the incident parallel slit. Enter the width of the incident slit. Select the length of the length limiting slit. Sets the width of the receiving slit # 1 to Open. Otherwise, enter the slit width. Select the aperture angle of the PSA. Select the aperture angle of the receiving parallel slit. Sets the width of the receiving slit # 2 to Open. Otherwise, enter the slit width. Tip: The slit width can be entered in fractional number such as 1/2, 2/3. Table Choices of the width, length, or aperture angle of each slit Slit Soller/PSC (deg) IS (mm) IS length limiting slit (mm) RS1 (mm) PSA (deg) Soller (deg) RS2 (mm) Width, length, or aperture angle 5.0, 2.5, 1.0, 0.5, 0.15, Open Enter the value in mm. 15.0, 10.0, 5.0, 2.0, 0.5, None Select Open, or enter the value in mm. 1.0, 0.5, 0.114, Open, None, No_uinit 5.0, 2.5, 1.0, 0.5, 0.114, None, No_unit Select Open, or enter the value in mm. Precise Theta/2-Theta Measurement (PB/PSA) Part 9

14 1. How to set Part conditions Pre-measurement conditions Check the Pre-measurement conditions box to make the pre-measurement under the specified conditions. The data measurement will be made under the conditions determined based on the pre-measurement results. Tip: If you want to make the pre-measurement, check the Pre-measurement conditions box. Scan axis Start (deg) Stop (deg) Step (deg) Speed (deg/min) Attenuator If you want to make the data measurement under the customized conditions, uncheck the Pre-measurement conditions box and set the conditions in the Data measurement conditions section. Select the scan axis from Theta/2-Theta, 2-Theta, or 2-Theta/Omega. Enter the start angle of the scan. Enter the stop angle of the scan. Enter the step width of the scan. Enter the scan speed. Select the attenuator to be used for the pre-measurement from Open, 1/70, 1/1000, or 1/ Omega (deg) / delta Omega (deg) When 2-Theta is selected for Scan axis, enter the position of the omega axis. When 2-Theta/Omega is selected for Scan axis, enter the offset angle of the omega axis. Comment Tip: When 2-Theta/Omega is selected for Scan axis, the range of the omega axis is given by the following equations: start angle: (value entered in the Start (deg) box) / 2 + delta Omega stop angle: (value entered in the Stop (deg) box) / 2 + delta Omega Enter the comment (optional). The comment entered here will be saved in the measurement data file. 10 Precise Theta/2-Theta Measurement (PB/PSA) Part

15 1.2 Customizing scan conditions and slit conditions If you want to make the data measurement under the customized conditions without making the pre-measurement, uncheck the Pre-measurement conditions box and set the conditions in the Data measurement conditions section. Scan axis Mode Start (deg) Stop (deg) Step (deg) Select the scan axis from Theta/2-Theta, 2-Theta, Omega, or 2-Theta/Omega. Select the scan mode from Continuous or Step. Enter the start angle of the scan. Enter the stop angle of the scan. 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. Attenuator Select the attenuator to be used for the data measurement from Open, 1/70, 1/1000, or 1/ Omega (deg) / 2-Theta (deg) / delta Omega (deg) When 2-Theta or Omega is selected for Scan axis, enter the position of the omega or 2-theta axis, respectively. When 2-Theta/Omega is selected for Scan axis, enter the offset angle of the omega axis. Comment Tip: When 2-Theta/Omega is selected for Scan axis, the range of the omega axis is given by the following equations: start angle: (value entered in the Start (deg) box) / 2 + delta Omega stop angle: (value entered in the Stop (deg) box) / 2 + delta Omega Enter the comment (optional). The comment entered here will be saved in the measurement data file. Precise Theta/2-Theta Measurement (PB/PSA) Part 11

1. How to set Part conditions Exec. Axis Action When the Exec. box is checked, the selected axis will be oscillating or spinning during the measurement. Select the axis to oscillate or spin.

16 1. How to set Part conditions Exec. Axis Action When the Exec. box is checked, the selected axis will be oscillating or spinning during the measurement. Select the axis to oscillate or spin. Select the action of the selected axis from Oscillation or Spin. Range Tip: The available actions depend on the selected axis. When Oscillation is selected as the action of the selected axis, select Absolute or Relative as the oscillation range specification method. Origin (Center)(deg) Oscillation rang (+/-)(deg) Start (deg) Stop (deg) Speed (deg/min) When Oscillation is selected as the action of the selected axis and Relative is selected as the oscillation range specification method, enter the oscillation center. When Oscillation is selected as the action of the selected axis and Relative is selected as the oscillation range specification method, enter the oscillation width. When Oscillation is selected as the action of the selected axis and Absolute is selected as the oscillation range specification method, enter the oscillation start angle. When Oscillation is selected as the action of the selected axis and Absolute is selected as the oscillation range specification method, enter the oscillation stop angle. Enter the oscillation or spin speed. 12 Precise Theta/2-Theta Measurement (PB/PSA) Part

17 1.2 Customizing scan conditions and slit conditions Calculated scan duration Set recommended values Close If the pre-measurement is made, shows the calculated duration of the pre-measurement. If only the data measurement is made, shows the calculated duration of the data measurement. 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 Sample form, Sample width, Sample height, Step, and Duration time. The recommended values are shown in Tables through Closes the Customize dialog box. Table Recommended slit conditions Sample form Soller/PSC IS IS L RS1 PSA / Soller RS2 Powder / Bulk / Film Thin film Capillary / Film 5 deg Determined based on the sample form, sample width and start angle. Determined based on the sample height. Open deg / None or 0.5 deg / 5 deg Open Table Recommended conditions (pre-measurement, data measurement) Sample form Scan axis 2-Theta / Omega / delta Omega Powder / Bulk / Film Theta/2-Theta 0 deg Thin film 2-Theta Omega = 1 deg Capillary / Film 2-Theta Omega = 0 deg Table Recommended pre-measurement conditions Mode Start Stop Step Speed Attenuator Continuous Specified range deg deg/min Open Precise Theta/2-Theta Measurement (PB/PSA) Part 13

18 1. How to set Part conditions Table Recommended data measurement conditions (when Use pre-measurement results is selected) Mode Start Stop Step Duration time Attenuator Determined based on the FWHM Determined based on the intensity Step Specified range obtained by the pre-measurement and step width specified in the Precise theta/2-theta obtained by the pre-measurement and duration time specified in the Precise theta/2-theta Open measurement conditions section. measurement conditions section. Table Recommended data measurement conditions (when Use specified values is selected) Mode Start Stop Step Duration time Attenuator Determined based on the Determined based on the Step Specified range specified FWHM and step width specified in the Precise theta/2-theta measurement specified intensity and duration time specified in the Precise theta/2-theta measurement Open conditions section. conditions section. 14 Precise Theta/2-Theta Measurement (PB/PSA) Part

19 1.2 Customizing scan conditions and slit conditions 2. Measurement sequence The precise theta/2-theta measurement is performed automatically. However, the length limiting slit, parallel slit, etc. must be installed (or removed) manually as instructed by messages displayed on the screen. (1) When Multi-layer mirror is selected as the monochromatization method, install the scintillation counter onto the counter adaptor as instructed by the message. θs IS RS1 ATT RS2 θd T S Z S Zd Fig. 2.1 Monochromatization (multi-layer mirror only) When Multi-layer mirror + Diffracted beam monochromator is selected as the monochromatization method, install the DBM unit (Flat) onto the counter adaptor as instructed by the message. CAUTION: The DBM unit is an option. θs IS RS1 ATT RS2 No monochromator slit (Flat) θd T S Z S Zd Fig. 2.2 Monochromatization (multi-layer mirror + diffracted beam monochromator) (2) Make the data measurement under the conditions specified in the Precise Theta/2-Theta Meas. (PB/PSA) dialog box. θ/2θ scan RS1 RS2 IS,IS L Soller/PSC PSA Soller Fig. 2.3 Theta/2-theta measurement using the multi-layer mirror only Precise Theta/2-Theta Measurement (PB/PSA) Part 15

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