Residual Stress Measurement Part

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Transcription:

Residual Stress Measurement Part

Contents Contents 1. How to set Part conditions...1 1.1 Setting conditions... 1 1.2 Customizing scan conditions and slit conditions... 8 2. Measurement sequence...19 Residual Stress Measurement Part i

1.2 Customizing scan conditions and slit conditions 1. How to set Part conditions In this chapter, how to set the Residual Stress Measurement (PB/PSA) Part conditions is described. 1.1 Setting conditions Set the basic conditions in the Residual Stress Measurement dialog box. The scan conditions and slit conditions of the residual stress measurement are determined based on the basic conditions. The scan conditions and slit conditions can also be customized. Fig. 1.1.1 Residual Stress 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. Residual Stress Measurement Part 1

1. How to set Part conditions Method Psi points Sample height (mm) Select the method of the residual stress measurement from Iso-inclination (Fixed psi method), Iso-inclination (Fixed psi0 method), Side-inclination (Fixed psi method), or Side-inclination (Fixed psi0 method). Select from Fine, Standard, or Coarse. In ordinary cases, select Coarse. Makes the measurement at nine psi points including psi start and stop angles within the acceptable range determined based on the selected measurement Fine method and specified 2-theta measurement range. Select Fine if you wish to analyze the effects of the texture and coarse crystal grains. Makes the measurement at five psi points including psi start and stop angles within the acceptable range Standard determined based on the selected measurement method and specified 2-theta measurement range. Makes the measurement at the psi start and stop angles of the acceptable range determined based on Coarse the selected measurement method and specified 2-theta measurement range. Select Coarse if you wish to confirm whether residual stress exists. Enter the sample height. Tip: The sample height refers to the dimension (unit: mm) of the sample in the direction shown below. Incident direction of x-ray when φ =0 Sample height Sample width Sample thickness Stress free 2-theta (deg) Enter the diffraction angle of the stress-free sample. Tip: If the sample is registered in a database such as ICDD, enter the diffraction angle registered in the database. If a theta/2-theta scan has already been made, enter the position of a non-overlapped peak in the high angle region. 2 Residual Stress Measurement Part

1.2 Customizing scan conditions and slit conditions 2-theta measurement range (deg) Enter the start and stop angles of the 2-theta scan so that the value in the Stress free 2-theta (deg) box is between the start and stop angles. Tip: Determines the acceptable input range of psi based on the selected measurement method and specified 2-theta measurement range. Duration/point (sec) Select 10000, 5000, 3000, 1000, or 500. In ordinary cases, select 5000. 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. Diffracted beam monochromator Select Not use or Use. In ordinary cases, select Not use. Not use Use 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 the DBM unit (option) for measurements. The diffracted beam monochromator is an optical device (crystal) to monochromatize x-rays using the diffraction. 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. If a pre-measurement (theta/2-theta scan) has been made, select Use specified values. FWHM (deg) If Use specified values is selected, enter the FWHM obtained by the pre-measurement. Residual Stress Measurement Part 3

1. How to set Part conditions Intensity (cps) If Use specified values is selected, enter the intensity obtained by the pre-measurement. Tip: The conditions in the FWHM and intensity settings section are used to determine the step width and duration time of the scan. If Use pre-measurement results is selected, the FWHM and intensity are calculated based on the profile obtained by the pre-measurement. Phi (deg) Enter the angle to drive the phi axis to at the start of the measurement. CAUTION: When Iso-inclination (Fixed psi method) or Iso-inclination (Fixed psi0 method) is selected for Method, the direction of the incident x-rays coincides with that of the residual stress measurement. When Side-inclination (Fixed psi method) or Side-inclination (Fixed psi0 method) is selected for Method, the chi axis will move so that the direction of the incident x-rays becomes perpendicular to that of the residual stress measurement. Therefore, confirm the direction of the sample and secure it to the sample plate not to drop off. To change the direction of residual stress measurement using the Move to origin function, use the wafer sample plate. If the height reference sample plate is used, secure the sample at phi = 0.0000 and change the sample direction manually, because measurement cannot be made at some positions of the phi axis. 4 Residual Stress Measurement Part

1.2 Customizing scan conditions and slit conditions Oscillation conditions Select whether the sample will be oscillated during the residual measurement. This is available only when Iso-inclination (Fixed psi0 method) is selected for the residual stress measurement method. Tip: Set the oscillations conditions such as the oscillation axis and range in the Customize dialog box. 1.2 Customizing scan conditions and slit conditions Run recommended sequence Makes the residual stress measurement using the recommended sequence. Customize conditions Customize Calculated scan duration Makes the residual stress 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 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. Residual Stress Measurement Part 5

1. How to set Part conditions Execute Executes the residual stress measurement under the conditions specified in the Residual Stress Measurement dialog box. CAUTION: Clicking the Cancel button after executing the residual stress measurement does not cancel the specified conditions. Tip: The residual stress measurement is executed with the Residual Stress Measurement dialog box open. While the residual stress 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. 6 Residual Stress Measurement Part

1.2 Customizing scan conditions and slit 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. Residual Stress Measurement Part 7

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 residual stress measurement, set the conditions in the Customize dialog box. Tip: Refer to 2. Measurement sequence to set the scan conditions and slit conditions. Fig. 1.2.1 Customize dialog box 8 Residual Stress Measurement Part

1.2 Customizing scan conditions and slit conditions Method Psi points Sample height (mm) Select the method of the residual stress measurement from Iso-inclination (Fixed psi method), Iso-inclination (Fixed psi0 method), Side-inclination (Fixed psi method), or Side-inclination (Fixed psi0 method). Select Fine, Standard, or Coarse. In ordinary cases, select Coarse. Makes the measurement at nine psi points including psi start and stop angles within the acceptable range determined based on the selected measurement Fine method and specified 2-theta measurement range. Select Fine if you wish to analyze the effects of the texture and coarse crystal grains. Makes the measurement at five psi points including psi start and stop angles within the acceptable range Standard determined based on the selected measurement method and specified 2-theta measurement range. Makes the measurement at the psi start and stop angles of the acceptable range determined based on Coarse the selected measurement method and specified 2-theta measurement range. Select Coarse if you wish to confirm whether residual stress exists. Enter the sample height. Tip: The sample height refers to the dimension (unit: mm) of the sample in the direction shown below. Incident direction of x-ray when φ =0 Sample height Sample width Sample thickness Residual Stress Measurement Part 9

1. How to set Part conditions Stress free 2-theta (deg) Enter the diffraction angle of the stress-free sample. Tip: If the sample is registered in a database such as ICDD, enter the diffraction angle registered in the database. If a theta/2-theta scan has already been made, enter the position of a non-overlapped peak in the high angle region. 2-theta measurement range (deg) Enter the start and stop angles of the 2-theta scan so that the value in the Stress free 2-theta (deg) box is between the start and stop angles. Tip: Determines the acceptable input range of psi based on the selected measurement method and specified 2-theta measurement range. Duration/point (sec) Select 10000, 5000, 3000, 1000, or 500. In ordinary cases, select 5000. 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. Diffracted beam monochromator Select Not use or Use. In ordinary cases, select Not use. Not use Use 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 the DBM unit (option) for measurements. The diffracted beam monochromator is an optical device (crystal) to monochromatize x-rays using the diffraction. 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. If a pre-measurement (theta/2-theta scan) has been made, select Use specified values. FWHM (deg) If Use specified values is selected, enter the FWHM obtained by the pre-measurement. 10 Residual Stress Measurement Part

1.2 Customizing scan conditions and slit conditions Intensity (cps) If Use specified values is selected, enter the intensity obtained by the pre-measurement. Tip: The conditions in the FWHM and intensity settings section are used to determine the step width and duration time of the scan. If Use pre-measurement results is selected, the FWHM and intensity are calculated based on the profile obtained by the pre-measurement. Phi (deg) Enter the angle to drive the phi axis to at the start of the measurement. CAUTION: When Iso-inclination (Fixed psi method) or Iso-inclination (Fixed psi0 method) is selected for Method, the direction of the incident x-rays coincides with that of the residual stress measurement. When Side-inclination (Fixed psi method) or Side-inclination (Fixed psi0 method) is selected for Method, the chi axis will move so that the direction of the incident x-rays becomes perpendicular to that of the residual stress measurement. Therefore, confirm the direction of the sample and secure it to the sample plate not to drop off. To change the direction of residual stress measurement using the Move to origin function, use the wafer sample plate. If the height reference sample plate is used, secure the sample at phi = 0.0000 and change the sample direction manually, because measurement cannot be made at some positions of the phi axis. Tip: When the Close button is clicked after setting the conditions in the Residual stress measurement conditions, FWHM and intensity settings, and Move to origin sections in the Customize dialog box, the conditions in the Residual Stress Measurement dialog box will also be changed. Residual Stress Measurement Part 11

1. How to set Part conditions Oscillation Axis Oscillation Range (deg) Oscillation Speed (deg) Select the axis to oscillate. Enter the oscillation width. Enter the oscillation speed. Table 1.2.1 shows the choices of the widths or lengths of the slits and the aperture angles of the parallel slits. Soller/PSC (deg) Select the aperture angle of the incident parallel slit. IS (mm) Enter the width of the incident slit. IS L (mm) Select the length of the length limiting slit. RS1 (mm) Sets the width of the receiving slit # 1 to Open. Otherwise, enter the slit width. PSA (deg) Select the aperture angle of the PSA. Soller (deg) Select the aperture angle of the receiving parallel slit. RS2 (mm) Sets the width of the receiving slit # 2 to Open. Otherwise, enter the slit width. Table 1.2.1 Choices of the width, length, or aperture angle of each slit Slit Width, length, or aperture angle Soller/PSC (deg) 5.0, 2.5, 1.0, 0.5, 0.15, Open IS (mm) Enter the value in mm. IS length limiting slit (mm) 15.0, 10.0, 5.0, 2.0, 0.5, None RS1 (mm) Select Open, or enter the value in mm. PSA (deg) 1.0, 0.5, 0.114, Open, None, No_uinit Soller (deg) 5.0, 2.5, 1.0, 0.5, 0.114, None, No_unit RS2 (mm) Select Open, or enter the value in mm. 12 Residual Stress Measurement Part

1.2 Customizing scan conditions and slit conditions Pre-measurement conditions Check the Pre-measurement conditions box to make the pre-measurement. Step (deg) Speed (deg/min) Attenuator Psi angle (deg) 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 1/10000. Enter the psi angle within the acceptable measurement range of psi for the pre-measurement. Tip: The psi acceptable input range is displayed under Psi acceptable input range in the Measurement psi positions by clicking the Set recommended values button after setting the conditions for Method and 2-theta measurement range. When Iso-inclination (Fixed psi method) or Iso-inclination (Fixed psi0 method) is selected for Method, the omega axis will move. When Side-inclination (Fixed psi method) or Side-inclination (Fixed psi0 method) is selected for Method, the chi axis will move. The position of each axis is given by the following equations: the omega angle = Stress free 2-theta (deg) / 2 + Psi angle (deg) the chi angle = Psi angle (deg) Residual Stress Measurement Part 13

1. How to set Part conditions Mode Step (deg) Select the scan mode from Continuous or Step. 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 1/10000. Checkbox for execution Psi position Allowed psi range Checkbox for execution Psi position Shows the acceptable input range of psi determined based on the selected measurement method and specified 2-theta measurement range. Makes the stress measurement at the entered psi position if the box is checked. Enter the psi position within the psi acceptable input range. 14 Residual Stress Measurement Part

1.2 Customizing scan conditions and slit conditions Auto input Opens the Auto input dialog box. Enter the values in the Psi start angle (deg), Psi stop angle (deg), and Number of psi points boxes, and click the Execute button. Then, the entered number (of psi points) of psi positions will be set in the Measurement psi positions section of the Customize dialog box. When Sin^2 psi constant step is selected, the psi positions will be set so that the values of sin 2 φ are regularly spaced. When Psi constant step is selected, the psi positions will be set so that the values of psi are regularly spaced. Psi0 input Opens the Psi0 input dialog box and shows the acceptable input range of psi0 determined based on the selected measurement method and specified 2-theta measurement range. Enter the value(s) of psi0 and click the Execute button. Then, the psi position(s) corresponding to the entered psi0 value(s) will be set in the Measurement psi positions section of the Customize dialog box. Residual Stress Measurement Part 15

1. How to set Part conditions Calculated scan duration Shows the calculated duration of the residual stress measurement. Set recommended values Sets the conditions in the Pre-measurement conditions and Data measurement conditions sections to the recommended values based on the conditions specified for Method, Psi points, and Sample height. The recommended values are shown in Tables 1.2.2 through 1.2.7. Close Closes the Customize dialog box. Table 1.2.2 Recommended slit conditions Soller/PSC IS IS L RS1 PSA Soller RS2 Determined based on the selected 0.5 5 deg 1.000 mm Open 5 deg Open measurement method and sample height. deg Table 1.2.3 Recommended conditions (pre-measurement, data measurement) Method Scan axis Start Stop Iso-inclination (Fixed psi method) 2-Theta/Omega Enter the values in the 2-theta Iso-inclination (Fixed psi0 method) 2-Theta measurement range (deg) boxes Side-inclination (Fixed psi method) Theta/2-Theta in the Residual stress Side-inclination (Fixed psi0 method) 2-Theta measurement conditions section. Table 1.2.4 Recommended pre-measurement conditions Mode Step Speed Attenuator Psi angle Continuous 0.0100 deg 3.0000 deg/min Open 0.0000 deg Table 1.2.5 Recommended data measurement conditions (when Use pre-measurement results is selected) Mode Step Duration time Attenuator Step Determined based on the FWHM obtained by the pre-measurement and step width specified in the Residual stress measurement conditions section. Determined based on the intensity obtained by the pre-measurement and duration time specified in the Residual stress measurement conditions section. Open 16 Residual Stress Measurement Part

1.2 Customizing scan conditions and slit conditions Table 1.2.6 Recommended data measurement conditions (when Use specified values is selected) Mode Step Duration time Attenuator Determined based on the FWHM specified in the FWHM and intensity Determined based on the intensity specified in the FWHM and intensity Step settings section and step settings section and width specified in the duration time specified in Open Residual stress measurement conditions section. the Residual stress measurement conditions section. Table 1.2.7 Measurement psi positions Psi positions Determined based on the selected measurement method and specified 2-theta measurement range (Psi points: Fine = 9, Standard = 5, Coarse = 2 points). Checkbox for execution Check the boxes for all the calculated psi positions. Residual Stress Measurement Part 17

2. Measurement sequence The residual stress 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. Described below is the measurement sequence when Use pre-measurement results and Run recommended sequence are selected in the Residual Stress Measurement dialog box. (1) If the diffracted beam monochromator is not used, install the optical devices or detector as instructed by the message. θs IS, IS L (recommended value) RS2 (recommended value) RS1 (recommended value) ATT θd T S Soller/PSC (recommended value) Z S PSA (recommended value) Soller (recommended value) Fig. 2.1 When the diffracted beam monochromator is not used If the diffracted beam monochromator is used, install the DBM unit (Flat) onto the counter adaptor as instructed by the message. CAUTION: The DBM unit is an option. θs IS, IS L (recommended value) RS2 (recommended value) RS1 (recommended value) No monochromator slit (Flat) θd T S Z S Soller/PSC (recommended value) PSA (recommended value) Zd Soller (recommended value) Fig. 2.2 When the diffracted beam monochromator is used Residual Stress Measurement Part 19

2. Measurement sequence (2) Make the pre-measurement (2-theta/omega, 2-theta, or theta/2-theta scan) under the recommended conditions. RS2 RS1 Soller Soller/PSC IS, IS L PSA ϕ = 0.0000 Fig. 2.3 Pre-measurement (theta/2-theta scan) (3) Determine the step width and duration time of the data measurement based on the obtained profile. (4) Execute the data measurement from psi = 0.0000 under the conditions determined in step (3). The data measurements (2-theta/omega, 2-theta, or theta/2-theta scan) are made at various positions of psi under the conditions determined based on the conditions specified for Method, Psi points, and 2-theta measurement range (deg). RS2 Soller RS1 RS1 PSA Soller/PSC IS, IS L ϕ (recommended values) Fig. 2.4 Residual stress measurement (iso-inclination method) 20 Residual Stress Measurement Part