PHI 5000 VersaProbe TM Operator s Guide Part No. 705921 Rev. A Copyright 2006 ULVAC-PHI, INC. 370 Enzo, Chigasaki, JAPAN The PHI logo ( ) is a registered trademark of ULVAC-PHI, INC. Physical Electronics, PHI, MultiPak and Watcher are trademarks of ULVAC-PHI, INC.. All other trademarks are the property of their respective owners.
PHI XPS Reservation/Use Policy Reservations can be made up to One Week in advance. A Maximum of 4 hours/session can be reserved between 9am and 5pm Monday thru Friday. There is no restriction on reservation during evenings, early mornings or weekends. You need to arrive at the instrument at the beginning of your reserved time (or earlier). If you do not show up at the instrument and enable Badger within 30 minutes of the start of your reservation another user can consider this a NO SHOW and take that time slot for themselves. If you cancel or cannot use your reserved time, send an email to lamxps_users@lists.stanford.edu letting other users know the time slot has been released. Email messages releasing a reservation need to be sent REGARDLESS of the day or time the instrument is being released. Send an email to lam-xps_users@lists.stanford.edu if you finish running the instrument 30 minutes or more prior to the end of your reserved time letting other users know there is open time on the instrument. Failure to follow any of these rules can result in you being charged for reserved but unused instrument time. To receive email notifications of released time and updates on instrument maintenance go to lists.stanford.edu and subscribe to lam-xps_users.
PHI VersaProbe Scanning XPS System Overview The Main Operating Software is PHI Summitt. It controls the movement of the sample stage, the analysis set-up and acquisition and the control of the ion gun and neutralizer gun. Vacuum Watcher is a separate program that interacts with the PHI Summitt program and is used in conjunction with Summitt to load and transfer samples and to differentially pump the ion gun for ion sputtering. PHI MultiPak is a data reduction program used both for XPS and AES to process spectra, images and profiles acquired on the XPS or AES system. A copy of this program is on the XPS and the AES instrument computers as well as on the stand alone Dell Dimensions offline computer in the lab. The Summitt and Vacuum Watcher programs should always be up and running on the instrument. Do not close these programs without specific instructions from one of the lab supervisors. All three programs can be found on the desktop and on the toolbar at the bottom of the screen. Features The VersaProbe XPS is capable of x-ray beam spot sizes from 10um to 100um and a High Power setting with a beam spot of roughly 1400 x 300um. Secondary electron images can be acquired to locate specific analysis areas on samples with specific features to be analyzed. Computer controlled X, Y, Z, Tilt and Rotate stage control. Auto Z alignment for optimization of x-ray impact and electron extraction. Angle resolved measurements can be done to analyze ultra thin films. Ion sputtering can be done to analyze thicker films or remove surface contamination. Dual beam (electrons and ions) charge neutralization of insulating samples.
Sample Introduction The Vacuum Watcher Program controls the vacuum valve functions required to load and transfer samples in and out of the instrument. Each sample mount has a molybdenum mask secured by small flat-head screws. Loosen the screws and slip the sample under the mask. You can use the mask to secure the sample in place, and you can see it on the image monitor to help you navigate on the sample. If using a mask is not favorable the CuBe clips or silver paste can be used to secure the sample. When working with silver paste use as small an amount as possible to secure the sample. Ensure the silver paste has dried completely prior to introduction into the vacuum system. In the Vacuum Watcher Program, the Backfill Into button is used to vent the intro chamber. The Sample holder is mounted on the end of the transfer arm fork, the chamber cap replaced
and the Pump Intro button is used to pump out the intro chamber. This pumping process takes approximately 5 minutes. After the Vacuum Watcher program indicates the pump intro is complete move the stage to the transfer (Home) position. Go to the SUMMITT Image window and the Stage tab and click the Intro button (Figure below). An Intro dialog box opens (Figure below) and the sample stage will move to the home position. Do not click Up [Z] yet.
Push the Transfer Sample Button in Watcher. A Watcher message pops up. Click Yes on the Watcher Task Message ("Pump Intro Complete. Transfer Sample?") (Figure below). V1 will open. If No is selected the sample transfer will be aborted and V1 will not be opened. When V1 opens another Watcher Task Message ("Introduce the sample now.") will popup (Figure below), click OK. ATTENTION: Do not move the stage while moving the intro rod. While watching through the viewport, slowly slide the intro rod all the way into the vacuum chamber. The sample holder will move into position over the stage. In the Intro dialog box (Figure below) click the Up [Z] button. The stage will move Z up and the sample holder will be held by the stage clip.
Verify through the viewport that the sample holder is secure on the stage. Slide the Intro rod completely out of the chamber. The V1 gate valve will be closed automatically. Sample Extraction Click the Pump Intro button in the Vacuum Tasks section of Watcher (Figure below). The Pump Intro routine takes approximately 6 minutes; when complete, "Task Pump Intro complete" will be displayed in the Vacuum Task area. Note: Prior to pumping the intro users must ensure that there is no Argon leaking into the system (Ion Gun off and Thermo Valve Ctrl set to Limit). When the Intro chamber is pumped Watcher will stop Differentially Pumping the Ion Gun which would cause a rapid increase in system pressure if Argon was being leaked into the system
Click the Extract button in the Stage tab of the Image window (Figure below). The stage will move to the home (transfer) position. An Extract dialog box opens (Figure below). Do not click Down [Z] yet. Click the Transfer Sample button in the Watcher Vacuum Tasks section. The "Pump Intro Complete and Transfer Sample?" dialog box will popup (Figure below). Click the Yes button; V1 will open. If No is selected the sample transfer will be aborted and V1 will not be opened.
When V1 opens another Watcher Task Message ("Introduce the sample now.") will popup (Figure below), click OK. ATTENTION: Do not move the stage while moving the intro rod. While watching through the viewport, slowly slide the intro rod all the way into the vacuum chamber. Watch through the viewport as the fork on the Intro engages the sample holder. Ensure that the fork is fully engaged before proceeding. In the Extract dialog box (Figure below) click the Down [Z] button. The stage will move Z down and the sample holder will remain on the Intro rod fork. Ensure that the stage clip is below the sample holder and clear prior to pulling the intro rod out of the chamber. Slide the Intro rod completely out of the chamber. The V1 gate valve will be closed automatically. In the vacuum tasks section of Watcher Click the Backfill Intro button. If V2 remains red (closed), check to see that the intro probe is fully withdrawn from the main chamber. When the Backfill Intro task is complete the intro cover may be removed. If you do not intend to introduce another sample, replace the Intro cover and pump it down.
Sample Navigation The center of the CCD camera image is aligned to the center of the analysis area and focused at the analyzer focal point. When using the camera to move the stage to a desired analysis area; care should be taken to ensure that the stage is at the correct Z height (approximately 16 to17mm with a 1 flat sample holder). The software joystick may be used to move the stage or coordinates may be entered on the Stage tab (the stage will move to the entered coordinates when Move is clicked). The Auto-Z routine is used to determine the correct Z height for each sample. Clicking the Auto-Z button on the right side of the Image window starts the routine. The automated routine acquires spectra, moves the stage Z axis and acquires another spectrum. Spectra are compared at Z heights higher and lower than the current position. The stage is automatically set to the Z position with the maximum count rate. The recommended X-ray setting for the Auto-Z routine is 100um25W15kV. Clicking the SXI button will acquire a secondary electron image from the scanned X-ray source (text in the SXI button turns green while acquiring an image). During acquisition of a secondary electron image, the text in the SXI button turns green. Analysis points, lines, and maps are defined using the SXI image. Click the SXI button a second time to stop acquiring an image (SXI button text returns to black). The SXI button can not be clicked when a high power X-ray setting is selected. There are three modes for collecting SXI images: Slow, Fast, and Average. Slow and Fast modes display a new image with every frame. Average mode adds frames in a persisted image which is used to enhance image quality. The persisted image will be re-acquired if the Refresh button is clicked. Magnification is chosen by selecting the desired raster size from the drop down menu next to the frame rate window.
Analysis areas can be defined on the SXI image by selecting Point (or Area), Line, or Map. When creating an analysis Point or Area, click the point button on the right side of the Image window. An analysis point will be placed in the center of the SXI image. Analysis points can be changed to areas with a right click (on the point) then selecting area. Analysis points or areas can be added by clicking in the SXI image (adds a point where the mouse is clicked) or by clicking Add in the Point/Area tab under Point Center (adds a point in the center of the image). Analysis points and areas can be moved by clicking (holding the mouse button) and dragging them to the desired location, or by right clicking on the point or area and changing the coordinates. Users can define up to 20 points or areas. To define an analysis line, click the Line button on the right side of the Image window. Vertical, Horizontal, and Free Line mode can be chosen by right clicking on the line and selecting the desired option. Selecting the Map button will create a map area on the SXI image. To change the size and position of the area the user may click and drag edges of the box or drag the whole box. A right click on the map area will bring up a sub menu; selecting coordinates will allow the user to directly enter coordinates and window size.
The SXI/Auto-Z tab on the lower part of the Image window contains the X-ray parameter setting for SXI imaging and Auto-Z tab. The X-ray Setting pull-down list box in the Setting group allows to you to select the predefined X-ray beam setting to use for data collection.
Data Acquisition Acquisition Setting Window Region Name: You can enter the Transition Name (e.g. Ag3d5). Other energy region parameters will be set automatically if the region parameters are registered in Element Table described later. Pass Energy (ev): The Pass Energy pull-down list box allows to you to select the energy resolution (Pass Energy) with which to collect data. Lower (ev): The Lower edit box allows to you to set the lower binding energy of energy region. Range (ev): The Range edit box allows to you to set the energy width of the energy region.
Energy Step (ev): The Energy Step edit box allows to you to set the energy difference (step) between adjacent data points. Repeats: The Repeats edit box allows to you to set the number of times to accumulate the collecting data. Check Boxes: The check boxes left side of the energy region parameters allows to you to select or deselect the energy region settings. Clicking the Folder button opens a file name and folder setting dialog box that allows you to select the data folder and file name to store the data. (Figure below) Clicking the Acquire button to start to collect the data with established acquisition settings.
Starting the Ion Gun Starting the Ion Gun a. In the Watcher vacuum tasks section, select Diff vlv open to start differentially pumping the Ion Gun.
b. Choose the ion gun file desired. Set the Ion Gun to Standby. c. Turn the RVG050 power on and set to limit switch to Set point (Extractor Pressure should regulate to ~10mPa in a few minutes).
To shut off the Ion Gun, switch the RVG050 to limit and turn the Ion Gun off. The ion gun may be used to do a timed sputtering of the surface by setting the sputter time in minutes I the ion gun menu and clicking the Sputter button. The gun may be used in a depth profile mode by setting the sputter conditions in the acquisition menu In Acquisition Setting window, toggling the Sputter Mode button will expand the window and allow for the sputter conditions setup: Sputter Mode: Options are alternating and continuous. In the alternating mode, data acquisition and sputtering are performed in alternating time intervals. In the continuous mode, data acquisition and sputtering occur simultaneously Sputter Time: Specifies the total time the ion gun will sputter. This does not include the time needed to acquire the data in an alternating sputter profile Interval Time: The length of time the ion gun will sputter between data acquisition cycles. This parameter appears only when the alternating sputter mode is selected. This parameter is only available when the alternating sputter mode is selected Delayed Acq. Time: Specify a delay time, in seconds, after sputtering is completed and before data acquisition is performed. A time delay may be required for some insulating samples in order for all surface potentials to reach a new steady state condition following sputtering. This parameter is only available when the alternating sputter mode is selected. Num (Presputter): Specifies the number of spectral acquisition to be done prior to the first sputter interval. X-Ray while sputtering: Allows the X-ray beam to stay on while sputtering. This option should be left off if there is a risk of sample damage as a result of prolonged X-ray irradiation.