Tables ......................x 1. VersaSCAN Base (VSC-BASE) ..............1 1.1 VSC-BASE Packing List ................. 1 1.2 VersaSCAN Initial Assembly and Set-up ........... 2 1.3 Axis Lockers..................3 1.4 Connectivity and Setting the IP Addresses ..........4 1.5 Getting Started and Home Routine ............5 1.6 Manual Control ..................
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5.3.6 Learning to Position the Probe Manually ........53 5.3.7 Positioning Probe for Line and Area Scans ........54 5.4 Example Area Scan Setup ..............54 6. VersaSCAN LEIS (VSC-LEIS) ..............55 6.1 LEIS Technique Overview and Introduction ..........55 6.2 Applications ..................55 6.3 VSC-LEIS Packing List ................
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7.5.4 Signal Conditioning ..............81 7.5.5 The Lock-In Amplifier ..............82 7.6 VSC-SVET System Test Procedure for Gold Wire Test Sample ....85 8. VersaSCAN SKP (VSC-SKP) ..............91 8.1 SVET Technique Overview and Introduction ........... 91 8.2 Key Points of SKP ................92 8.3 VSC-SKP Packing List .................
9.8 SDC Pump Calibration ..............124 9.9 Reference Electrode ................. 126 9.10 VSC-SDC System Test Procedure for Gold Disk Test Sample ....127 VersaSCAN Optical Surface Profiling (VSC-OSP) ......131 10.1 OSP Technique Overview and Introduction ........... 131 10.2 Applications ..................131 10.3 VSC-OSP Packing List ...............
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VersaSCAN User’s Manual 224213_0H / 082023 Figure 19. Experiment Properties..............21 Figure 20. Experiment Results ..............21 Figure 21. CV of 5mm Gold Sample ............... 22 Figure 22. Current Versus Position for Insulator ..........24 Figure 23. Current Versus Position for Conductor ..........25 Figure 24.
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Figure 168. VersaCAM Camera Showing the Head Being Brought Towards the Sample ......................128 Figure 169. VersaSCAN’s Software Manual Control for Stage Movement ..... 129 Figure 170. SDC Head in Close Proximity to the Sample Forming a Liquid “Microcell” ......................129 Figure 171.
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VersaSCAN User’s Manual 224213_0H / 082023 Figure 184. LEIS Cable Connections ............. 144 Figure 185. V3F ..................144 Figure 186. SVET Cable Connections for Open Circuit Controlled Sample .... 145 Figure 187. SVET Cable Connections for Galvanostatic/Potentiostatic Controlled Sample ....................145 Figure 188.
VersaSCAN BASE (VSC-BASE) This section describes functions of the VSC-BASE. This is the common workstation component of the VersaSCAN platform. General Installation and Setup, Ethernet Communication, home Routine and Manual Control of the positioning system is covered. 1.1 VSC-BASE Packing List Table 1.
224213_0H / 082023 1.2 VersaSCAN Initial Assembly and Set-up The VersaSCAN ships with the XYZ Positioning Stages assembled. Mount the 4 Vibration Resistant feet to the Optical Base. By mounting this first, users can easily lift the base for feet installation without worry of sliding the stages. From there, follow the instructions on the drawing below to help assemble the XYZ Positioning Stages to the Optical Base.
224213_0H / 082023 Chapter 1. VersaSCAN Base (VSC-BASE) Figure 3. Mounting Interface Block to Assembly Connect the 6 cables from the Stages to the Motion Controllers. Note each axis has one cable to command the stage and one cable to read from the linear encoder.
Figure 4. Axis Lockers 1.4 Connectivity and Setting the IP Addresses All IP Addresses should be set at the factory. The VersaSCAN software will look for these specific devices on these addresses, so these are required for proper communication. For reference the default IP Addresses are: Table 2.
224213_0H / 082023 Chapter 1. VersaSCAN Base (VSC-BASE) Setting the IP Addresses is beyond the scope of this document, but Ametek’s Technical Support staff can assist as needed. All Ethernet devices should be connected to the supplied Ethernet hub. All potentiostats should be connected to the USB ports on the computer.
VersaSCAN User’s Manual 224213_0H / 082023 1.6 Manual Control To enable the Manual Control function, click the “Manual Control” button on the top right of the home screen. Figure 6. Home Screen Using this window, users can drive the stages to a given position by either using the mouse to click on the directional arrows or using the keypad for the designated movements.
Additionally, this window displays the Absolute Position of X and Y and Z in millimeters (mm). This document describes the framework of the VersaSCAN software. Details on creating projects and experiments for handling data acquisition as well as graphs for data presentation are provided.
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VersaSCAN SECM (VSC-SECM) The VersaSCAN SECM is a Scanning Electrochemical Microscope (SECM). It requires VSC- BASE and VSC-SECM. It is recommended to use VSC-MLCELL and VSC-CAM. 2.1 SECM Technique Overview and Introduction In a traditional electrochemical measurement, a potentiostat measures an average current over the entire electrode/electrolyte interface.
VersaSCAN User’s Manual 224213_0H / 082023 For imaging experiments, the same kind of approach curve is also used in order to position the tip in the local imaging zone of the sample, without contacting it. The tip-to-sample distance is typically 2 to 4 times the probe diameter for surface imaging experiments. Considering that the tip is 10s of microns, a non-visual means to identify this zone is important.
VersaSCAN User’s Manual 224213_0H / 082023 Cable Connections for a Potentiostatic controlled sample are below. Figure 11. Connection Diagram for VSC-SECM NOTE In Figure 11, the BNC T piece image is shown for reference only. Table 4. Cell Connections for SECM...
Test Sample VersaSTAT 3 Sense (Gray) When multiple potentiostats are connected to the system, the VersaSCAN software must be told which one is connected to the probe and which one is connected to the sample. Once both the potentiostats are located in the System Tab, the Hardware Requirements Tab is accessed by highlighting “Setup”...
VersaSCAN User’s Manual 224213_0H / 082023 2.5 Software Control for VSC-SECM 2.5.1 Comments Any comments that need to be stored with the data file can be entered into this field. Please note that all the Scan and Measurement parameters from the experiments are already stored in each data file, so those are not necessary to be entered here.
“Point” will execute the experiment without moving the probe. 2.5.5 Measurement Mode In a Z-Line experiment, such as used for an Approach Curve experiment, VersaSCAN acquires data in STEP Mode to decrease the opportunity for a tip crash. In “STEP” will oversample and average the data. The probe moves to a given location and remains in that location for the measurement duration.
VersaSCAN User’s Manual 224213_0H / 082023 2.5.6 Start X / Y / Z In this field, the user defines the specific position that the experiment starts. This can be set as “vs. Previous” or “vs. Absolute”. “vs. Previous” will allow the probe to use its current position as the origin point. In this example, 0 / 0 / 0 vs.
Chapter 2. VersaSCAN SECM (VSC-SECM) 224213_0H / 082023 2.5.9 Measurement Mode Setup Figure 17. Measurement Mode Setup 2.5.10 Line Delay The Line Delay allows the user to program a set time delay between each line of data acquisition. This is helpful when waiting for motion in the electrolyte (convection) caused by the return scan to settle.
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Al2O3 suspension. 3. Place the sample in to the VersaSCAN mLCELL and ensure it is a good fit so that it is watertight. If loose, add some PTFE tape to bulk-out the sample and make a fit. If tight, use some water or a small amount of grease placed on the O-ring to ease the sample into the VersaSCAN mLCELL.
4. Now fill the VersaSCAN mLCELL with the Test Solution, to around 70% of maximum. Insert the CE platinum (P/N 233917) and also the Reference electrode (P/N 233795) into the VersaSCAN mLCELL recesses in the PTFE body.
Chapter 3: VSC-SECM System Test Procedure for Gold Disk Test Sample 224213_0H / 082023 Figure 19. Experiment Properties 9. Run the experiment and the following is similar to what users should see: Figure 20. Experiment Results...
VersaSCAN User’s Manual 224213_0H / 082023 The Sigmoid-shaped response is characteristic of an ultramicroelectrode. Note there is virtually no current flowing at the 0.65 Volts vs. Ag/AgCl, because iron exists in solution as the oxidized state Fe3+. When the voltage of the Pt probe is sweep to the reducing potential of -0.25 Volts vs. Ag/AgCl, Fe3+ undergoes an electrochemical reaction to Fe2+ and current flows.
Chapter 3: VSC-SECM System Test Procedure for Gold Disk Test Sample 224213_0H / 082023 3.3 Running Approach Curves Approach Curves define when a probe enters the local imaging area. 1. Select a Z-Line Scan SECM experiment to run an Approach-curve experiment. Move the tip over the Insulating part of the sample (not the gold, but the epoxy region) using the X/Y/Z parameters at the Manual Position window.
VersaSCAN User’s Manual 224213_0H / 082023 Figure 22. Current Versus Position for Insulator 4. Be aware that the probe will be approaching the surface at 10microns every second. It is the users’ responsibility to watch for the decay of current and stop the experiment when the current starts to drop.
Chapter 3: VSC-SECM System Test Procedure for Gold Disk Test Sample 224213_0H / 082023 Figure 23. Current Versus Position for Conductor Then, if these 2 plots are considered together, users can find a maximum difference. Notice that the current starts around the same value of 40nA – the current seen when the probe is in the bulk of the solution (not near a surface).
VersaSCAN User’s Manual 224213_0H / 082023 Figure 24. Insulator Versus Conductor Comparison 9. Now choose a Z-axis point, so that both inhibited and enhanced currents can be seen when over insulating and conducting regions respectively. 3.4 Line Scans and Area Maps 1.
Chapter 3: VSC-SECM System Test Procedure for Gold Disk Test Sample 224213_0H / 082023 Figure 25. Area Maps Notice the current is inhibited over the insulator (i.e., less than 40nA) and enhanced over the gold (i.e., more than 40nA). Please note, the result above was taken with a 25 μm probe. If desired, users can configure an area scan experiment, using their own set-up values.
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4. AC-SECM 4.1 Introduction AC-SECM is a technique based upon impedance. In this experiment, the sample is usually not connected to the potentiostat. The key advantage of this technique versus traditional SECM is there is no requirement for an additional mediator. Therefore, the technique has great appeal to corrosion scientists since a mediator could affect the corrosion properties of the sample during scans.
VersaSCAN User’s Manual 224213_0H / 082023 Figure 27. Limiting Case Number 1 Limiting Case #1: The current flow is shown by RED arrow. The approach curve for this substrate is similar to that of the DC SECM response in which hindered diffusion (migration) of ions results in an increased impedance.
224213_0H / 082023 Chapter 4: AC-SECM Limiting Case #2: Current can now flow in multiple paths: a) From probe to CE b) From probe to CE via conductor The equivalent circuit has been constructed to show this process – as shown in case #2. Table 8.
VersaSCAN User’s Manual 224213_0H / 082023 Figure 30. High Frequency and/or Low Electrolyte Concentration Graph Typical Tip -Approach curve response for high frequency and/or low electrolyte concentration measurements over a conducting substrate. B) Low Frequency and/or High Electrolyte Concentration In this case, the current is limited by the solution resistance, R1 (current flow is shown in the figure below in the red arrow).
224213_0H / 082023 Chapter 4: AC-SECM Figure 31. Low Frequency and/or High Electrolyte Concentration Current Flow Figure 32. Low Frequency and/or High Electrolyte Concentration Graph Typical Tip – Approach curve response for low frequency and/or high electrolyte concentration measurements over a conducting substrate. 4.2 Example Data For this experiment users will need: Gold Disk Sample, Reference Electrode, counter electrode, 10um or 25um Pt electrode.
VersaSCAN User’s Manual 224213_0H / 082023 4.2.1 Approach Curves 1. Select Potentiostatic EIS technique in the operating mode. Polarize the Probe electrode to 0V vs Open circuit. 2. Chose Single Frequency Technique 3. Set the ac amplitude to 100mV (note – the system is highly linear and therefore large ac amplitudes can be used for this test) 4.
224213_0H / 082023 Chapter 4: AC-SECM Figure 34. AC-SECM Approach Curve Response for an Insulator Figure 35. AC-SECM Approach Curve Response for a Conductor NOTE The magnitude of the change can be quite small from bulk to surface. 4.2.2 Feedback Mode X-Y Scan Position the probe in the local imaging zone as determined by comparing the approach curves over the insulator and conductor.
VersaSCAN User’s Manual 224213_0H / 082023 the VersaSTAT 3F at 0V vs OC. Run an X-Y scan in this Feedback mode configuration (the sample is not polarized). Figure 36. Typical Set of AC-SECM Results Across Insulator/Gold Sample...
5. VSC-SOFT STYLUS PROBE SECM This technique requires Soft Stylus Probe assembly (VSC-STYLUS). 5.1 Technique Overview and Introduction The soft stylus probe was developed by the group of Prof Hubert Girault of EPFL, Switzerland. For a detailed description of the probe technology please consult the papers of the group. The soft probes offer a simple and convenient method of maintaining a constant distance between the probe and the substrate.
VersaSCAN User’s Manual 224213_0H / 082023 Figure 38. Examples of Probe Contact • Figure A: The soft probe is freely suspended. The electrochemical signal is that of the bulk. • Figure B: The soft probe is just in contact with the surface. Notice the classical approach...
224213_0H / 082023 Chapter 5: VSC-Soft Stylus Probe SECM Figure 39. Probe Positioning In the above image, the probe is ‘pushed’ into the surface. This is the correct mode for imaging. The current is independent of probe position in the Z direction for electrochemically homogeneous surfaces.
VersaSCAN User’s Manual 224213_0H / 082023 Figure 40. Probe Handing Example Wear suitable gloves, to avoid smearing on the clear plastic probes. The gloves can be nitrile or vinyl (to avoid allergy issues associated with latex gloves). • Avoid direct contact between the probe and the work surface as debris can scratch the Parylene C coating.
224213_0H / 082023 Chapter 5: VSC-Soft Stylus Probe SECM Figure 41. Probe Cutting Diagram It is necessary to cut the probes to a fine taper using either the surgical scissors provided or a clean, new scalpel. The tapering of the probe will help the movement of the probe during operation. Whilst the width of the probe at the tip is not critical, in general, the smaller the width the better.
VersaSCAN User’s Manual 224213_0H / 082023 Figure 42. Probe Cutting Lines The final probe is shown below. Note the fine tapering of the probe to a point. Figure 43. Final Probe The final stage requires preparation of the electrode surface. The razor tool will be needed for this...
224213_0H / 082023 Chapter 5: VSC-Soft Stylus Probe SECM Figure 44. Razor Tool Supplied with the System Place the probe on a smooth, flat surface. Place the cutting tool at right angles to the probe tip as shown below. With practice, users can reduce the amount of probe cut.
VersaSCAN User’s Manual 224213_0H / 082023 Figure 46. Probe Cutting Direction Apply pressure to the blunt handle using hand pressure in a vertical, downward motion. The blade should simply CUT through the probe. DO NOT USE A SLICING ACTION to cut the probe tip as this might damage the Parylene-C coating.
224213_0H / 082023 Chapter 5: VSC-Soft Stylus Probe SECM The probe may be shipped with writing ‘UP’ on one side. This side is NOT COATED WITH PARYLENE C. If there is no marking, then it is quite easy to identify the correct side. The side with the Parylene C coating is placed in contact with the sample since the thin coating ensures a small tip-substrate separation for better contrast imaging and higher resolution measurements.
VersaSCAN User’s Manual 224213_0H / 082023 Electrode Holder with Stylus Probe Parylene C Coating this side Figure 49. Electrode Loaded into Top Holder Place the copper connection pad on top of the probe followed by the nylon housing and screw down using the three bolts provided.
224213_0H / 082023 Chapter 5: VSC-Soft Stylus Probe SECM Place the gold-plated, spring-loaded connector through the central hole of the other electrode holder plate. This provides electrical connection to the probe itself. Insert the probe in the direction of the arrow. Figure 51.
VersaSCAN User’s Manual 224213_0H / 082023 Screw the holder onto the plate as shown using the bolt to securely fasten the holder to the rotary position stages. Figure 53. Holder Screwed onto Plate Figure 54. Probe Mounted on Base Plate and Positioner Stage...
224213_0H / 082023 Chapter 5: VSC-Soft Stylus Probe SECM 5.3.2 Electrochemistry of the Probes Once the probe is assembled it is recommended to check the electrochemical operation of the cell. 1. Make a solution of 1 or 2mMol Ferrocene Methanol in 0.1M KNO 2.
VersaSCAN User’s Manual 224213_0H / 082023 Figure 56. Rotary Optical Positioning Scales 1. Rotate the body of the holder until ‘0’ on both scales match as shown above. 2. The division on the Right-Hand scale as shown is 10 degrees per major division and 2 degree per minor division.
224213_0H / 082023 Chapter 5: VSC-Soft Stylus Probe SECM 5.3.4 Positioning the Probe It is important to understand the prove movement during MOVEMENT and MEASUREMENT (i.e., when the probe approaches the surface and how it scans across the surface during electrochemical measurements).
VersaSCAN User’s Manual 224213_0H / 082023 Figure 59. Correct Probe Bend Versus Incorrect Probe Bend If the probe is scanned in the wrong direction, bending of the probe will occur and this must be avoided. To avoid this, the correct probe angle MUST be set to the correct value. This is covered in the next section.
224213_0H / 082023 Chapter 5: VSC-Soft Stylus Probe SECM Figure 61. Manual Control Button 3. It is important to tell the software the angle that the probe will make with respect to the surface. To determine the input value, enter 360 – user required value. For example, if it is desired to apply a 20-degree touch angle, input 340 into the Probe Angle Box.
VersaSCAN User’s Manual 224213_0H / 082023 the point at which the probe withdraws for the surface. Use the key to place the probe on the surface. It will approach the surface at the angle specified in the probe angle text box.
(Z). In discussions of LEIS, it is important to understand the different voltages in the system. The V3F with Diff Aux Volt In applies an AC voltage to the sample; the VersaSCAN determines current by measuring the voltage in solution.
VersaSCAN User’s Manual 224213_0H / 082023 Figure 64. LEIS Dummy Cell Response - Frequency Sweep Figure 65. Results from Gold Point-In-Space in Tap Water with 100mV Applied...
VersaSCAN User’s Manual 224213_0H / 082023 Cable Connections for a Potentiostatic controlled sample are below. This assumes that connections for the positioning system are already in place for the motors and encoders. As well the communication cable: Ethernet for the motion controllers and computer;...
224213_0H / 082023 Chapter 6: VersaSCAN LEIS (VSC-LEIS) 6.5 Software Control for VSC-LEIS 6.5.1 Comments Any comments that need to be stored with the data file can be entered into this field. Please note that all the Scan and Measurement parameters from the experiments are already stored in each data file, so those are not necessary to be entered here.
“Point” will execute the experiment without moving the probe. 6.5.3.2 Measurement Mode In LEIS, VersaSCAN acquires data in STEP Mode because of the requirement for calculations of impedance. STEP Mode will oversample and average the data. The probe moves to a given location and remains in that location for the measurement duration.
224213_0H / 082023 Chapter 6: VersaSCAN LEIS (VSC-LEIS) 6.5.3.3 Start X/Y/Z In this field, the user defines the specific position that the experiment starts. This can be set as “vs. Previous” or “vs. Absolute”. “vs. Previous” will allow the probe to use its current position as the origin point. In this example, 0/0/0 vs.
VersaSCAN User’s Manual 224213_0H / 082023 6.5.4 Measurement & Delay Figure 72. Software Measurement and Delay 6.5.4.1 Line Delay The Line Delay allows the user to program a set time delay between each line of data acquisition. This is helpful when waiting for motion in the electrolyte (convection) caused by the return scan to settle.
224213_0H / 082023 Chapter 6: VersaSCAN LEIS (VSC-LEIS) Voltage (or Current): This parameter allows the user to set the DC Bias on which the AC signal is applied. The most common configuration is to run the system with no external DC Bias applied: either 0V vs.
This document assumes that the system has been assembled per instructions in the accompanying guides. 1. Mount and cable the VersaSCAN system as described in the manual. This assumes that connections for the positioning system are already in place for the motors and encoders as well as the communication cable, Ethernet for the motion controllers and computer, and USB for the V3F.
Sync ADC on back of V3F Trig on System Box BNC-to-BNC 2. Use the Manual Control in the VersaSCAN software to position the Electrometer in its maximum Z position as high as possible. Figure 75. Manual Control Settings 3. Mount the cable from the VersaSCAN Dummy Cell (P/N 224211) to the Electrometer (P/N 224077).
Electrochemical Impedance Spectroscopy (LEIS). Figure 77. Surface Imaging and Scanning The file Setup window for the LEIS Step will be displayed. See VersaSCAN LEIS Operator’s Guide for a detailed explanation of all test parameters. 6. Select Scan Type: Point - The starting position parameters are not relevant for this experiment.
224213_0H / 082023 Chapter 6: VersaSCAN LEIS (VSC-LEIS) 7. The new experiment now needs to be configured. The LEIS experiment Potentiostat and Impedance Setup window will be displayed. See the VSC-LEIS Users Guide for details on the controls. Suggested parameters for the LEIS Dummy Cell.
VSC-MLCELL and the circular PT Counter Electrode leaves a very small scan area available. 1. Mount and cable the VersaSCAN system as described in the manual. This assumes that connections for the positioning system are already in place for the motors and encoders, as well as the communication cable, Ethernet for the motion controllers and computer, and USB for the V3F.
Figure 81. LEIS Setup for Gold Wire Test Sample Figure 82. V3 Connections 2. Mount the VersaSCAN Gold Wire Test Sample (P/N 224116) into the cell and level it. 3. Fill the cell with suitable electrolyte. Drinking water with a typical conductivity of 150µS/cm is suitable for the test sample.
Counter (Red) to the Counter electrode. Circular Pt Counter is supplied. 7. Use the Manual Control in the VersaSCAN software to position the tip of the LEIS probe such that it is aligned above the gold wire of the test sample by approximately 100 micrometers.
Electrochemical Impedance Spectroscopy (LEIS). Figure 85. Surface Imaging and Scanning The file Setup window for the LEIS Step will be displayed. See VersaSCAN LEIS Operator’s Guide for a detailed explanation of all test parameters. 9. If the LEIS probe is positioned directly over the gold wire, these parameters will cause a 10 mm Line Scan in X with the gold being centered.
VersaSCAN User’s Manual 224213_0H / 082023 10. The new experiment now needs to be configured. The LEIS experiment Potentiostat and Impedance Setup window will be displayed. See the VSC-LEIS Users Guide for details on the controls. Suggested parameters for the Gold Wire Test Sample.
224213_0H / 082023 Chapter 6: VersaSCAN LEIS (VSC-LEIS) Figure 88. Gold Wire Test Sample Results NOTE The impedance results decrease over the gold wire. 13. After successfully running a Line Scan experiment in LEIS in the X-direction, users position the probe directly over the gold in X, by moving it to the position of lowest...
7. VersaSCAN SVET (VSC-SVET) The VersaSCAN SVET is a Scanning Vibrating Electrode Technique (SVET). It requires VSC- BASE and VSC-SVET. It is recommended to use VSC-CAM and VSC-LCELL or VSC-mLCELL. 7.1 SVET Technique Overview and Introduction The Scanning Vibrating Electrode Technique uses a single wire to measure potential field gradient drop in solution.
224213_0H / 082023 Chapter 7: VersaSCAN SVET (VSC-SVET) 7.4 Cable Connections for VSC-SVET NOTE If the system has TWO motion controller boxes, please refer to Appendix 1 for set-up diagrams. The diagrams are additionally available as part of the “Setup” of each experiment.
VersaSCAN User’s Manual 224213_0H / 082023 Figure 94. SVET Galvanostatic/Potentiostatic Controlled Sample Cable Connections 7.5 Software Control for VSC-SVET 7.5.1 Comments Any comments that need to be stored with the data file can be entered into this field. Please note that all the Scan and Measurement parameters from the experiments are already stored in each data file, so those are not necessary to be entered here.
224213_0H / 082023 Chapter 7: VersaSCAN SVET (VSC-SVET) 7.5.2 Conditioning The Conditioning tab allows the user to set the time for the system to delay before any measurement in the Step is started. Note this programmed delay occurs once before the experiment starts.
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VersaSCAN User’s Manual 224213_0H / 082023 7.5.3.2 Measurement Mode In this field, the user defines if the experiment is ran in “Step” or “Sweep”. “STEP” will oversample and average the data. The probe moves to a given location and remains in that location for the measurement duration.
224213_0H / 082023 Chapter 7: VersaSCAN SVET (VSC-SVET) Figure 98. Area Scan 7.5.4 Signal Conditioning In order to tune to Signal Conditioning most effectively, the probe should be positioned in X,Y over the most active region (highest signal). Figure 99. Software Signal Conditioning...
Voltage is applied to the piezo unit from the System Box to drive the vibrations. A Lock-in Amplifier measures an AC input and provides a DC output proportional to its magnitude. VersaSCAN uses a Signal Recovery Lock-in Amplifier 7230, but all Ethernet LIA from Signal Recovery are compatible.
224213_0H / 082023 Chapter 7: VersaSCAN SVET (VSC-SVET) The default setting for this value is “Linked”. This scales the Lock-In Input to response levels from the Electrometer. 7.5.5.2 Time Constant. The Time Constant sets the amount of filtering on the data.
VersaSCAN User’s Manual 224213_0H / 082023 Figure 103. Reference Wave Diagram Manual adjustment of the Reference Phase should follow an AC response. This is a good additional check that the measured response is dominated by signal and not noise. Figure 104. Software Reference Phase Settings The Up and Down arrows will move the Reference Phase in 5-degree increments.
This document assumes that the system has been assembled per instructions in the accompanying guides. 1. Mount the VersaSCAN Gold Wire Test Sample (P/N 224116) into the cell and level it. NOTE Both the L-Cell and mL-Cell are compatible. 2. Fill the cell with suitable electrolyte. Drinking water with a typical conductivity of 150µS/cm is suitable for the test sample.
5. Set the Galvanostat to generate a constant current of -10µA. 6. Use the Manual Control in the VersaSCAN software to position the tip of the SVET probe such that it is aligned above the gold wire of the test sample by approximately 100 micrometers.
224213_0H / 082023 Chapter 7: VersaSCAN SVET (VSC-SVET) 7. In the VersaSCAN software select the menu option “File” and select “New Project”. Within the “Project” an Experiment is created. Insert a Step of the Scanning Vibrating Electrode Technique (SVET). Figure 108. Surface Imaging and Scanning The file Setup window for the SVET Step will be displayed.
VersaSCAN User’s Manual 224213_0H / 082023 Figure 109. SVET Scan Setup Figure 110. Scanning Area Diagram 8. The new experiment now needs to be configured. The SVET experiment Signal Configuration window will be displayed. See the VSC-SVET Users Guide for details on the controls.
224213_0H / 082023 Chapter 7: VersaSCAN SVET (VSC-SVET) Figure 111. SVET Signal Conditioning Please note that the reference phase will need to be adjusted to the optimum value. The use of Auto will select a Reference Phase that gives the maximum positive signal.
8. VERSASCAN SKP (VSC-SKP) The VersaSCAN SKP is a Scanning Kelvin Probe (SKP). It requires VSC-BASE and VSC-SKP. It is recommended to use VSC-CAM and VSC-LCELL or VSC-mLCELL. 8.1 SVET Technique Overview and Introduction The Scanning Kelvin Probe technique works on the principle of capacitor. The VSC-SKP uses a tungsten wire as its measurement element.
VersaSCAN User’s Manual 224213_0H / 082023 Figure 114. Energy Levels at Different Stages of the SKP Experiment Figure 115. Zinc/Galvanized Steel Response Using VSC-SKP 8.2 Key Points of SKP General statements about Scanning Kelvin Probe • Non-destructive • Non-contact •...
VersaSCAN User’s Manual 224213_0H / 082023 Figure 117. SKP Cable Connections Table 15. Cell Connections for SKP CABLE Motion Controller (XYZ) System Box (XYZ) 37-PIN to 37-PIN Top of Electrometer System Box (Electrometer) 9-Pin Male to Male Top of Piezo...
224213_0H / 082023 Chapter 8: VersaSCAN SKP (VSC-SKP) 8.5 Software Control for VSC-SKP 8.5.1 Comments Any comments that need to be stored with the data file can be entered into this field. Please note that all the Scan and Measurement parameters from the experiments are already stored in each data file, so those are not necessary to be entered here.
VersaSCAN User’s Manual 224213_0H / 082023 Figure 120. Software Scan Setup 8.5.3.1 Scan Type The “Scan type” allows the user to define if the experiment is going to be executed in a single line axis or in an area as a series of line experiments. “X Line” would be a single line of data in X, while maintaining a constant Y and Z position.
224213_0H / 082023 Chapter 8: VersaSCAN SKP (VSC-SKP) This can be set as “vs. Previous” or “vs. Absolute”. “vs. Previous” will allow the probe to use its current position as the origin point. In this example, 0/0/0 vs. Previous starts the experiment from the probe’s current position.
VersaSCAN User’s Manual 224213_0H / 082023 Figure 122. Signal Conditioning 8.5.5 Backing Potential Controller The Backing Potential Controller (BPC) is the electronics that applies the nulling voltage to the sample. This is accessed through DAC2 on the back of the SR 7230 Lock-in Amplifier.
Voltage is applied to the piezo unit from the System Box to drive the vibrations. A Lock-In Amplifier measures an AC input and provides a DC output proportional to its magnitude. VersaSCAN uses a Signal Recovery Lock-in Amplifier 7230, but all Ethernet LIA from Signal Recovery are compatible.
VersaSCAN User’s Manual 224213_0H / 082023 The default setting for this value is “Linked”. This scales the Lock-In Input to response levels from the Electrometer. 8.6.2 Time Constant The Time Constant sets the amount of filtering on the data. The longer the Time Constant, the more filtering is done.
224213_0H / 082023 Chapter 8: VersaSCAN SKP (VSC-SKP) Manual adjustment of the Reference Phase should follow an AC response. This is a good additional check that the measured response is dominated by signal and not noise. Figure 128. Software Reference Phase Settings The Up and Down arrows will move the Reference Phase in 5-degree increments.
2” port on the Lock-in Amplifier. This is the Backing Potential Controller. The Piezo (P/N 233737) is mounted to the VersaSCAN Mounting Block (P/N 224061). The Electrometer (P/N 224077) is mounted directly to the Piezo. The SKP probe (P/N 224112 or...
224213_0H / 082023 Chapter 8: VersaSCAN SKP (VSC-SKP) Cable Connections Table 16. SKP CABLE Motion Controller (XY) System Box (XY) 25-Pin to 25-Pin Motion Controller (Z) System Box (Z) 25-Pin to 25-Pin Top of Electrometer System Box (Electrometer) 9-Pin Male to Male...
5. Use the Manual Stage in the VersaSCAN software to position the tip of the SKP probe such that it is aligned above the center of the test sample, in the center of the etched area. The probe tip to sample distance should be approximately 100 micrometers.
“Project” an Experiment is created; Insert a Step of the Scanning Kelvin Probe (SKP). Figure 135. Surface Imaging and Scanning The file Setup window for the SKP Step will be displayed. See VersaSCAN Operator’s Guide to detailed explanation of all test parameters.
VersaSCAN User’s Manual 224213_0H / 082023 Figure 136. SKP Scan Setup Figure 137. SKP Scan Area The new experiment now needs to be configured. The SKP experiment Signal Configuration window will be displayed. See the VSC-SKP Users Guide for details on the controls.
224213_0H / 082023 Chapter 8: VersaSCAN SKP (VSC-SKP) Figure 138. SKP Signal Conditioning Figure 139. Backing Potential Controller Please note that the reference phase will need to be adjusted to the optimum value. The use of Auto will select a Reference Phase that gives the maximum positive signal.
VersaSCAN User’s Manual 224213_0H / 082023 Figure 140. Run Icon 11. The screenshot below shows the typical data obtained from the test experiment. Figure 141. SKP Test Results Please note that the SKP measurement is a relative measurement between the Probe work function and the surface work function, absolute values cannot be measured with this technique.
9. VERSASCAN SDC (VSC-SDC) The VersaSCAN SDC is a Scanning Droplet Cell (SDC). It requires VSC-BASE and VSC-SDC. It is recommended to use VSC-CAM and VSC-LCELL. 9.1 SDC Technique Overview and Introduction The Scanning Droplet Cell (SDC) is a technique of the VersaSCAN Scanning Electrochemical Workstation.
233767 Scr M3x0.5-14mm 233792 Electrodes Reference Electrode, AG/AGCL 233795 Counter Electrode, PT Wire 233917 Control Box Bypass Cable, Adapter, VersaSCAN Sys Box 224145 Test Sample VersaSCAN Gold Disk Test Sample 224115 Connectivity and Power Cables* Extension Cord 803937 Cable, BNC-BNC SC0033 *Indicates that item is used on multiple techniques and will not be duplicated in shipment.
224213_0H / 082023 Chapter 9: VersaSCAN SDC (VSC-SDC) 9.4 Cable Connections for VSC-SDC NOTE If the system has TWO motion controller boxes, please refer to Appendix 1 for set-up diagrams. The diagrams are additionally available as part of the “Setup” of each experiment.
VersaSCAN User’s Manual 224213_0H / 082023 Place the PTFE SDC Head in a bath of clean deionized water and ultrasonically clean the head for 10 – 15 minutes prior to use if the SDC Head has been used previously. This will help to...
224213_0H / 082023 Chapter 9: VersaSCAN SDC (VSC-SDC) Repeat this process for the two miniature Bayonet Hose Connectors and the other Cord Grip. It is important to ensure the solution’s flow is not obstructed with PTFE tape over the fittings’...
VersaSCAN User’s Manual 224213_0H / 082023 NOTE Note that the Bayonet Hose Connectors will not thread completely into the SDC Head. Simply ensure that they are threaded in tightly by hand. Prepare to install the Reference Electrode (see Reference Electrode Setup Section if working with a new electrode for its preparation prior to installation into the SDC Head) and Counter Electrode by removing only the Cord Grip caps as shown in the photo below.
224213_0H / 082023 Chapter 9: VersaSCAN SDC (VSC-SDC) Figure 151. Looking into Counter Electrode Opening on SDC Head Insert the Reference Electrode into the body of the SDC head as indicated in the picture below. Gently insert the Reference Electrode into the SDC head to the point where it stops on the internal seat, and then remove the Reference Electrode by ~ 1 mm.
VersaSCAN User’s Manual 224213_0H / 082023 Figure 153. Steps for Releasing Cassette Button Once the two cassettes have been removed from the pump housing, the PVC tubing sets need to be installed by stretching one PVC tubing set over each of the semi-circular cassette’s end points as shown below.
224213_0H / 082023 Chapter 9: VersaSCAN SDC (VSC-SDC) Figure 155. Steps for Reinserting Pump Cassette NOTE The cassettes should be inserted into the pump such that the metal clips on them are all on the same end. The arrows on the caseates which indicate the direction of the solution flow should all be facing the same direction.
VersaSCAN User’s Manual 224213_0H / 082023 NOTE It is often easier, especially with new tubing, to attach the tubing to the Inlet and Outlet Bayonet Hose connectors when the SDC Head is dismounted from the Stage. Ensure that the end of the tube is pushed as fully onto the Bayonet Hose connector as possible.
224213_0H / 082023 Chapter 9: VersaSCAN SDC (VSC-SDC) and installed and all seals remain airtight, the solution’s path should be uninterrupted by air bubbles. IMPORTANT Air entering the SDC Head at any of the various sealing points can make Flow Balancing and maintaining a consistent drop at the tip very difficult.
The best way to avoid such air leaks is to properly seal each of the threaded joints connecting to the SDC Head with PTFE tape as shown in the “Using the VersaSCAN in SDC Mode” section of the manual. This should always be the first step in setting up the SDC...
See the “Using the VersaSCAN in SDC Mode” section of the manual for guidance on how to remove and reinstall the pump cassettes. Swap the PVC tubing set from one cassette with the PVC tubing set held in the other cassette, keeping the cassettes themselves in the same location in the pump housing.
RE is not pressed against the seat and that a gap of ~ 1 mm is in place between the bottom of the RE and the seat. Instructions on positioning the RE can be found in the “Using the VersaSCAN in SDC Mode” section of the manual. Figure 160. Proper Positioning of Reference Electrode in SDC Head 9.7.5 SDC Head Positioning...
224213_0H / 082023 Chapter 9: VersaSCAN SDC (VSC-SDC) 9.7.6 Tube Clamps Partially clamping the PVC tubes to and from the peristaltic pump is an option that offers a further degree of control for balancing, although it should not be used as a cure-all. If reasonable...
Arrange the pump and the SDC fluidics system as described in the “Using the VersaSCAN in SDC Mode” section of the manual and approach the sample surface as described in “Running the SDC Test Sample”...
224213_0H / 082023 Chapter 9: VersaSCAN SDC (VSC-SDC) Once the system appears to be operating correctly, stop the peristaltic pump and completely empty the graduated cylinder of its contents. Select a number of flow rates that will help calibrate the pump across the interest range.
VersaSCAN User’s Manual 224213_0H / 082023 9.9 Reference Electrode When a new Reference Electrode (RE) is first received, it arrives with a protective sheath on it to seal the frit/junction preventing internal filling solution from draining and the frit/junction from drying out while the electrode is being shipped or stored.
Prior to running this procedure, the VersaSCAN must be configured for the SDC System as described in the “Using the VersaSCAN in SDC Mode” section of the manual. It will also be very useful to review the section entitled “SDC Principle of Operation” prior to running this test.
224213_0H / 082023 Figure 167. SDC (and SECM) Standard Test Sample Once the VersaSCAN System is fully configured and ready to run in SDC Mode, use the manual to maneuver the SDC Head’s tip to a close proximity to the surface. The stage controls SDC Standard Test Sample must be polished prior to testing.
224213_0H / 082023 Chapter 9: VersaSCAN SDC (VSC-SDC) Figure 169. VersaSCAN’s Software Manual Control for Stage Movement When the SDC Head is located too far from the sample surface, the liquid being pumped to the tip will likely well out from the tip covering more surface area than it would if the tip were ideally located very close to the surface.
10. VERSASCAN OPTICAL SURFACE PROFILING (VSC-OSP) 10.1 OSP Technique Overview and Introduction The goal of the Optical Surfacing Profiling measurement is to measure the topography (height differences in Z) of a sample. This is a laser-based measurement which is generally made in air, but under the correct conditions could be made through liquid electrolyte.
Ametek PN Quantity (Each) Potentiostats VSC-OSP Laser Head 233734 VSC-OSP Laser Controller 233735 Cable, 2M, VSC-OSP to VersaSCAN System Box 233736 System Control Box and Internal Assemblies VersaSCAN System Control Assy 224118 VersaSCAN Sys Box Cable Assy, Laser Controller 224151...
The external cable connections for the VSC-OSP are straight-forward. Figure 173. OSP Cable Connections There is a single interface cable that connects the VersaSCAN System Control Box (P/N 224118) to VSC-OSP laser head (P/N 233734). Additionally, there is a standard Ethernet cable connected from “LAN” port on the VersaSCAN System Control Box to the Ethernet Hub of the VersaSCAN system.
VersaSCAN User’s Manual 224213_0H / 082023 10.5.2 Conditioning The conditioning tab allows the user to set the time for the system to delay before any measurement in the Step is started. Note this programmed delay occurs once before the experiment starts. The Measurement & Delay window allows other specific delays between each line and between each point to be programmed.
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224213_0H / 082023 Chapter 10: VersaSCAN Optical Surface Profiling (VSC-OSP) 10.5.3.2 Measurement Mode “STEP” will oversample and average the data. The probe moves to a given location and remains in that location for the measurement duration. Then, it moves stepwise to the new location (1 x Step Size;...
VersaSCAN User’s Manual 224213_0H / 082023 Figure 177. Area Scan 10.5.4 Measurement Mode Setup Figure 178. Measurement and Delay 10.5.4.1 Line Delay The Line Delay allows the user to program a set time delay between each line of data acquisition.
224213_0H / 082023 Chapter 10: VersaSCAN Optical Surface Profiling (VSC-OSP) Measurement This parameter is the measured value of the laser displacement sensor. This is the value that is recorded in the VSC-OSP experiment. Measure Mode The VSC-OSP can be operated in Diffuse, Translucent, Transparent 1, Transparent 2, and Multi-Reflective Modes.
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APPENDIX 1. SYSTEM CONNECTIONS FOR TWO STAGE MOTION CONTROLLER The following chapter describes the system connections for two stage motion controllers. Only follow these instructions if the system has separate X/Y and Z stage motion control boxes. This applies to all units shipped BEFORE MARCH 2016 . For reference the default IP Addresses are: XY Controller: 192.168.10.11.
VersaSCAN User’s Manual 224213_0H / 082023 Without the System Box in Place: Table 22. Cable Connections for VSC-SECM without System Control Box CABLE Motion Controller I/O (XY) T-BNC 25-Pin to 25-Pin + Motion Controller I/O (Z) Pigtail BNC P/N 224145...
Appendix 1. System Connections for Two Stage Motion Controller 224213_0H / 082023 A.3 SVET Cable Connections for an Open Circuit controlled sample are below. Figure 186. SVET Cable Connections for Open Circuit Controlled Sample Cable Connections for a Galvanostatic/Potentiostatic controlled sample are below. Figure 187.