Ametek VersaSCAN User guide

VersaSCAN™
Electrochemical Scanning Base
System Manual
AMETEK®Part No. 224213 082023
Manual Revision H Printed in USA

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TABLE OF CONTENTS
Table of Contents............................................................................................ii
Figures............................................................................................................ v
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 .................................................................................... 6
1.7 Probe Position and Experiment Status ..................................................... 7
2. VersaSCAN SECM (VSC-SECM)....................................................................9
2.1 SECM Technique Overview and Introduction............................................. 9
2.2 Applications ...................................................................................... 10
2.3 VSC-SECM Packing List ....................................................................... 11
2.4 Cable Connections for VSC-SECM ......................................................... 11
2.5 Software Control for VSC-SECM ........................................................... 14
2.5.1 Comments................................................................................ 14
2.5.2 Conditioning ............................................................................. 14
2.5.3 Scan Setup............................................................................... 14
2.5.4 Scan Type ................................................................................ 15
2.5.5 Measurement Mode.................................................................... 15
2.5.6 Start X / Y / Z........................................................................... 16
2.5.7 End vs. Start ............................................................................ 16
2.5.8 Step Size ................................................................................. 16
2.5.9 Measurement Mode Setup........................................................... 17
2.5.10 Line Delay...................................................................... 17
2.5.11 Measure Delay ................................................................ 17
2.5.12 Measure Probe and Measure Sample................................... 17
3. VSC-SECM System Test Procedure for Gold Disk Test Sample ..................19
3.1 Materials .......................................................................................... 19
3.2 Setup .............................................................................................. 19
3.3 Running Approach Curves ................................................................... 23
3.4 Line Scans and Area Maps................................................................... 26
4. AC-SECM ..................................................................................................29

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4.1 Introduction...................................................................................... 29
4.2 Example Data ................................................................................... 33
4.2.1 Approach Curves ....................................................................... 34
4.2.2 Feedback Mode X-Y Scan ............................................................ 35
5. VSC-Soft Stylus Probe SECM ....................................................................37
5.1 Technique Overview and Introduction ................................................... 37
5.2 Theory of Operation ........................................................................... 37
5.3 Probe Preparation and Handling ........................................................... 39
5.3.1 Probe Preparation...................................................................... 40
5.3.2 Electrochemistry of the Probes..................................................... 49
5.3.3 Using the Positioning Scales ........................................................ 49
5.3.4 Positioning the Probe ................................................................. 51
5.3.5 Running Constant Distance Mode SECM Experiments....................... 52
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 ........................................................................ 57
6.4 Cable Connections for VSC-LEIS........................................................... 57
6.5 Software Control for VSC-LEIS............................................................. 59
6.5.1 Comments................................................................................ 59
6.5.2 Conditioning ............................................................................. 59
6.5.3 Scan Setup............................................................................... 59
6.5.4 Measurement & Delay ................................................................ 62
6.5.5 Potentiostat Setup ..................................................................... 62
6.5.6 Impedance Setup ...................................................................... 63
6.6 VSC-LEIS System Test Procedure for LEIS Dummy Cell............................ 64
6.7 VSC-LEIS System Test Procedure for Gold Wire Test Sample .................... 68
7. VersaSCAN SVET (VSC-SVET)...................................................................75
7.1 SVET Technique Overview and Introduction ........................................... 75
7.2 Applications ...................................................................................... 75
7.3 VSC-SVET Packing List........................................................................ 76
7.4 Cable Connections for VSC-SVET .......................................................... 77
7.5 Software Control for VSC-SVET ............................................................ 78
7.5.1 Comments................................................................................ 78

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7.5.2 Conditioning ............................................................................. 79
7.5.3 Scan Setup............................................................................... 79
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 ......................................................................... 93
8.4 Cable Connections for VSC-SKP............................................................ 93
8.5 Software Control for VSC-SKP.............................................................. 95
8.5.1 Comments................................................................................ 95
8.5.2 Conditioning ............................................................................. 95
8.5.3 Scan Setup............................................................................... 95
8.5.4 Signal Conditioning .................................................................... 97
8.5.5 Backing Potential Controller ........................................................ 98
8.5.6 Electrometer Gain...................................................................... 99
8.6 The Lock-In Amplifier ......................................................................... 99
8.6.1 Lock-In Input............................................................................ 99
8.6.2 Time Constant ........................................................................ 100
8.6.3 Reference Wave ...................................................................... 100
8.6.4 Measurement & Delay .............................................................. 101
8.7 VSC-SKP System Test Procedure for Zinc/Steel Sample ......................... 102
9. VersaSCAN SDC (VSC-SDC) ....................................................................109
9.1 SDC Technique Overview and Introduction........................................... 109
9.2 Applications .................................................................................... 109
9.3 VSC-SDC Packing List....................................................................... 110
9.4 Cable Connections for VSC-SDC ......................................................... 111
9.5 Preparing the VSC-SDC Head for Use .................................................. 111
9.6 Pump Setup.................................................................................... 115
9.7 SDC Flow Balancing ......................................................................... 120
9.7.1 The Connections...................................................................... 120
9.7.2 The Sample ............................................................................ 121
9.7.3 The Pump .............................................................................. 121
9.7.4 The SDC Reference Electrode .................................................... 122
9.7.5 SDC Head Positioning............................................................... 122
9.7.6 Tube Clamps .......................................................................... 123

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9.8 SDC Pump Calibration ...................................................................... 124
9.9 Reference Electrode ......................................................................... 126
9.10 VSC-SDC System Test Procedure for Gold Disk Test Sample ................... 127
10. 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 ....................................................................... 132
10.4 Cable Connections for VSC-OSP ......................................................... 132
10.5 Software Control for VSC-OSP ........................................................... 133
10.5.1 Comments ................................................................... 133
10.5.2 Conditioning ................................................................. 134
10.5.3 Scan Setup................................................................... 134
10.5.4 Measurement Mode Setup............................................... 136
10.5.5 Optical Sensor Setup ..................................................... 136
10.6 VSC-OSP System Test Procedure for Slip Gauge Samples ....................... 137
11. VersaSCAN mLCELL (VSC-MLCELL)..................................................139
12. VersaSCAN LCELL (VSC-LCELL) .......................................................141
Appendix 1. System Connections for Two Stage Motion Controller .............143
FIGURES
Figure 1. Mount Stage Assembly .....................................................................2
Figure 2. Bubble Level ...................................................................................2
Figure 3. Mounting Interface Block to Assembly .................................................3
Figure 4. Axis Lockers ...................................................................................4
Figure 5. VersaSCAN Warning Message ............................................................ 5
Figure 6. Home Screen ..................................................................................6
Figure 7. Status Bar ...................................................................................... 7
Figure 8. Approach Curve...............................................................................9
Figure 9. Example of Generator-Collector Mode ............................................... 10
Figure 10. SECM Set-up Diagram .................................................................. 11
Figure 11. Connection Diagram for VSC-SECM ................................................. 12
Figure 12. Hardware Requirements Screen...................................................... 13
Figure 13. Comments Field........................................................................... 14
Figure 14. Conditioning................................................................................ 14
Figure 15. Scan Setup Screen ....................................................................... 15
Figure 16. Area Scan Example ...................................................................... 16
Figure 17. Measurement Mode Setup ............................................................. 17
Figure 18. VersaStudio Icon ......................................................................... 20

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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. Insulator Versus Conductor Comparison........................................... 26
Figure 25. Area Maps .................................................................................. 27
Figure 26. AC-SECM Setup ........................................................................... 29
Figure 27. Limiting Case Number 1 ................................................................ 30
Figure 28. Limiting Case Number 2 ................................................................ 30
Figure 29. High Frequency and/or Low Electrolyte Concentration Current Flow...... 31
Figure 30. High Frequency and/or Low Electrolyte Concentration Graph ............... 32
Figure 31. Low Frequency and/or High Electrolyte Concentration Current Flow...... 33
Figure 32. Low Frequency and/or High Electrolyte Concentration Graph ............... 33
Figure 33. Scan Setup ................................................................................. 34
Figure 34. AC-SECM Approach Curve Response for an Insulator ......................... 35
Figure 35. AC-SECM Approach Curve Response for a Conductor ......................... 35
Figure 36. Typical Set of AC-SECM Results Across Insulator/Gold Sample ............ 36
Figure 37. Cross Section of Carbon Probe After Cutting the Probe ....................... 37
Figure 38. Examples of Probe Contact ............................................................ 38
Figure 39. Probe Positioning ......................................................................... 39
Figure 40. Probe Handing Example ................................................................ 40
Figure 41. Probe Cutting Diagram.................................................................. 41
Figure 42. Probe Cutting Lines ...................................................................... 42
Figure 43. Final Probe.................................................................................. 42
Figure 44. Razor Tool Supplied with the System............................................... 43
Figure 45. Probe Cutting Demonstration ......................................................... 43
Figure 46. Probe Cutting Direction ................................................................. 44
Figure 47. Probe Holder Pieces...................................................................... 44
Figure 48. Delamination of Parylene C Coating................................................. 45
Figure 49. Electrode Loaded into Top Holder.................................................... 46
Figure 50. Copper Pad Place on the Probe ....................................................... 46
Figure 51. Place Gold-Plated Connector .......................................................... 47
Figure 52. Connector in Position .................................................................... 47
Figure 53. Holder Screwed onto Plate............................................................. 48
Figure 54. Probe Mounted on Base Plate and Positioner Stage ............................ 48
Figure 55. Cyclic Voltammogram of FcMeOH in 0.1M KNO3................................. 49
Figure 56. Rotary Optical Positioning Scales .................................................... 50
Figure 57. Example of Probe Angle ................................................................ 50
Figure 58. Probe Scanning Demo................................................................... 51
Figure 59. Correct Probe Bend Versus Incorrect Probe Bend............................... 52
Figure 60. Select Soft Stylus Probe SECM ....................................................... 52

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Figure 61. Manual Control Button .................................................................. 53
Figure 62. Current Versus Height .................................................................. 53
Figure 63. Scan Setup ................................................................................. 54
Figure 64. LEIS Dummy Cell Response - Frequency Sweep ................................ 56
Figure 65. Results from Gold Point-In-Space in Tap Water with 100mV Applied..... 56
Figure 66. LEIS Setup Diagram ..................................................................... 57
Figure 67. LEIS Connections ......................................................................... 58
Figure 68. Software Comments Field.............................................................. 59
Figure 69. Software Conditioning Field ........................................................... 59
Figure 70. Software Scan Setup .................................................................... 60
Figure 71. Area Scan................................................................................... 61
Figure 72. Software Measurement and Delay................................................... 62
Figure 73. Software Potentiostat Setup........................................................... 62
Figure 74. Software Impedance Setup............................................................ 63
Figure 75. Manual Control Settings ................................................................ 65
Figure 76. VersaSCAN Dummy Cell ................................................................ 65
Figure 77. Surface Imaging and Scanning ....................................................... 66
Figure 78. Scan Setup –Select Point.............................................................. 66
Figure 79. Run Icon .................................................................................... 67
Figure 80. LEIS Dummy Cell Test Results........................................................ 68
Figure 81. LEIS Setup for Gold Wire Test Sample ............................................. 69
Figure 82. V3 Connections............................................................................ 69
Figure 83. LEIS Probe Mounting in the PT Wire Counter Electrode ....................... 70
Figure 84. Manual Control Settings ................................................................ 70
Figure 85. Surface Imaging and Scanning ....................................................... 71
Figure 86. Scan Setup ................................................................................. 71
Figure 87. Run Experiment Icon .................................................................... 72
Figure 88. Gold Wire Test Sample Results....................................................... 73
Figure 89. Probe Scan Results....................................................................... 74
Figure 90. Results from Gold Point-in-Space in Tap Water with -10uA Applied....... 75
Figure 91. Results from Bare Metal Corrosion Process ....................................... 76
Figure 92. SVET Setup Diagram .................................................................... 77
Figure 93. SVET Open Circuit Cable Connections .............................................. 77
Figure 94. SVET Galvanostatic/Potentiostatic Controlled Sample Cable Connections78
Figure 95. Software Comments Field.............................................................. 78
Figure 96. Software Conditioning Field ........................................................... 79
Figure 97. Scan Setup ................................................................................. 79
Figure 98. Area Scan................................................................................... 81
Figure 99. Software Signal Conditioning ......................................................... 81
Figure 100.VSC-SVET Signal Conditioning Diagram .......................................... 82
Figure 101. Electrometer Gain Diagram .......................................................... 82
Figure 102. SVET Reference Wave Signal........................................................ 83

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Figure 103. Reference Wave Diagram ............................................................ 84
Figure 104. Software Reference Phase Settings ............................................... 84
Figure 105. Measurement and Delay Settings .................................................. 85
Figure 106. VSC SVET Setup for Gold Wire Test Sample.................................... 86
Figure 107. Manual Control Settings .............................................................. 86
Figure 108. Surface Imaging and Scanning ..................................................... 87
Figure 109. SVET Scan Setup ....................................................................... 88
Figure 110. Scanning Area Diagram ............................................................... 88
Figure 111. SVET Signal Conditioning............................................................. 89
Figure 112. Run Icon................................................................................... 89
Figure 113. SVET Test Results ...................................................................... 90
Figure 114. Energy Levels at Different Stages of the SKP Experiment .................. 92
Figure 115. Zinc/Galvanized Steel Response Using VSC-SKP .............................. 92
Figure 116. SKP Setup Diagram .................................................................... 93
Figure 117. SKP Cable Connections................................................................ 94
Figure 118. Software Comment Field ............................................................. 95
Figure 119. Conditioning Tab ........................................................................ 95
Figure 120. Software Scan Setup .................................................................. 96
Figure 121. Area Scan ................................................................................. 97
Figure 122. Signal Conditioning..................................................................... 98
Figure 123. Backing Potential Controller ......................................................... 98
Figure 124. VSC-SKP Signal Conditioning Diagram ........................................... 99
Figure 125. Electrometer Gain Diagram .......................................................... 99
Figure 126. SKP Reference Wave Signal ....................................................... 100
Figure 127. Reference Wave Diagram .......................................................... 100
Figure 128. Software Reference Phase Settings ............................................. 101
Figure 129. Measurement and Delay ............................................................ 101
Figure 130. The SKP Test Sample ................................................................ 102
Figure 131. VSC-LCELL .............................................................................. 103
Figure 132. SKP Test Sample Mounted to Cell................................................ 103
Figure 133. Manual Control Settings ............................................................ 104
Figure 134. 500um SKP Probe @ 100 Microns from the Sample........................ 104
Figure 135. Surface Imaging and Scanning ................................................... 105
Figure 136. SKP Scan Setup ....................................................................... 106
Figure 137. SKP Scan Area......................................................................... 106
Figure 138. SKP Signal Conditioning ............................................................ 107
Figure 139. Backing Potential Controller ....................................................... 107
Figure 140. Run Icon................................................................................. 108
Figure 141. SKP Test Results ...................................................................... 108
Figure 142. Results from Gold Disk in 3M KCl with -500 mV............................. 109
Figure 143. Schematic of the SDC Head with Reference and Counter Electrodes
Installed.................................................................................................. 110

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Figure 144. SDC Setup Diagram.................................................................. 111
Figure 145. SDC Cable Connections ............................................................. 111
Figure 146. Parts Required for Preliminary/SDC Head Assembly ....................... 112
Figure 147. Placing the PTFE Tape ............................................................... 112
Figure 148. Fittings with PTFE Tape ............................................................. 113
Figure 149. SDC Head with its Fittings Properly Installed................................. 113
Figure 150. Cord Grip with Caps Removed .................................................... 114
Figure 151. Looking into Counter Electrode Opening on SDC Head .................... 115
Figure 152. Positioning Electrodes in SDC Head ............................................. 115
Figure 153. Steps for Releasing Cassette Button ............................................ 116
Figure 154. Peristaltic Pump Cassette with PVC Tubing Set Properly Installed ..... 116
Figure 155. Steps for Reinserting Pump Cassette ........................................... 117
Figure 156. Tubing Connected to SDC Head .................................................. 117
Figure 157. General Schematic of Liquid Flow Through the SDC System ............ 118
Figure 158. Semi-Transparent View of SDC Head and Solution Flow Path ........... 119
Figure 159. Closeup of SDC Head’s Tip ......................................................... 119
Figure 160. Proper Positioning of Reference Electrode in SDC Head ................... 122
Figure 161. Proper Clamp Location .............................................................. 123
Figure 162. General Flow Schematic for SDC System...................................... 124
Figure 163. Peristaltic Pump Interface .......................................................... 125
Figure 164. Flow Calibration Example........................................................... 125
Figure 165. Removing the Reference Electrode Sheath.................................... 126
Figure 166. Inspection of Frit...................................................................... 127
Figure 167. SDC (and SECM) Standard Test Sample ....................................... 128
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. SDC Test Showing SDC Results Over the Whole 5mm Au SDC Test Sample
............................................................................................................. 130
Figure 172. OSP Setup Diagram .................................................................. 132
Figure 173. OSP Cable Connections ............................................................. 133
Figure 174. Comment Field ........................................................................ 133
Figure 175. Conditioning Tab ...................................................................... 134
Figure 176. Scan Setup ............................................................................. 134
Figure 177. Area Scan ............................................................................... 136
Figure 178. Measurement and Delay ............................................................ 136
Figure 179. Optical Sensor Setup ................................................................ 136
Figure 180. VSC-MLCELL Parts Diagram ....................................................... 139
Figure 181. VSC-LCELL Parts Diagram.......................................................... 141
Figure 182. Complete VSC-LCELL ................................................................ 142
Figure 183. Connection Diagram for VSC-SECM ............................................. 143

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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. SKP Cable Connections.............................................................. 146
Figure 189. SDC Cable Connections ............................................................. 146
TABLES
Table 1. VSC-BASE Packing List ...................................................................... 1
Table 2. Default IP Addresses .........................................................................4
Table 3. VSC-SECM Packing List .................................................................... 11
Table 4. Cell Connections for SECM................................................................ 12
Table 5. Potentiostat Connections for VSC-SECM in Feedback Mode .................... 13
Table 6. Potentiostat Connections for VSC-SECM in Generator-Collector Mode ...... 13
Table 7. Limiting Case Number 1 Circuit Element Definitions .............................. 30
Table 8. Limiting Case Number 2 Circuit Element Definitions .............................. 31
Table 9. VSC-LEIS Packing List ..................................................................... 57
Table 10. Cell Connections for LEIS................................................................ 58
Table 11. LEIS Cable Connections for LEIS Dummy Cell .................................... 65
Table 12. LEIS Cable Connections for Gold Wire Test Sample ............................. 69
Table 13. VSC-SVET Packing List ................................................................... 76
Table 14. VSC-SKP Packing List..................................................................... 93
Table 15. Cell Connections for SKP ................................................................ 94
Table 16. SKP Cable Connections ................................................................ 103
Table 17. VSC-SDC Packing List .................................................................. 110
Table 18. VSC-OSP Packing List .................................................................. 132
Table 19. VSC-MLCELL Parts List ................................................................. 140
Table 20. VSC-LCELL Parts List ................................................................... 142
Table 21. Cable Connections for VSC-SECM With System Control Box, Using Bypass
Cable...................................................................................................... 143
Table 22. Cable Connections for VSC-SECM without System Control Box............ 144

1
1. 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. VSC-BASE Packing List
Description
Ametek PN
Quantity (Each)
XYZ Stages Motor Controllers
233776
1
Optical Breadboard
233752
1
Vibration Resistant Feet
233916
4
Stages to Board Mounting
VersaSCAN Stage Interface Plate
224060
1
Screw M6x12mm
233194
4
Washer M6 Split, 9.9mm OD
233784
4
Washer M6 Flat, 12mm OD
233783
4
Bracket to Stages Mounting
VersaSCAN Mounting Block
224061
1
Screw M5x0.8-14mm
233785
4
Washer M5 Split, 8.8mm OD
233787
4
Washer M5 Flat, 10mm OD
233786
4
Level
Level, Bull’s Eye 7/8 Dia. Flanged
233865
1
Laptop
Laptop
224123
1
Communications Cables
Ethernet Switch, 5-port, 10/100
233794
1
Ethernet Cables
683730
3
Power Cables
Power Cord
233950
2
Extension Cord
803937
2
Outlet Strip IEC320
233948
1
Power Supply, Desktop, 12V 2A
233949
1
Shipping and Documentation
VersaSCAN Base XYZ Pelican Case
244170
1
VersaSCAN Software
224102
1
VersaSCAN Manual
224213
1
NOTE Internal mounting hardware, such as screws, etc. are not included in this
packing list.

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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. Mounting
the stages to the base will require a 5mm Allen Wrench.
Figure 1. Mount Stage Assembly
Use the bubble level provided to level the optical base.
Figure 2. Bubble Level
Take this opportunity to position and mount the supplied Interface Block to the Z Stage with the
following instructions.

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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 thestage and one cableto read from the linear encoder.
These are labeled “X” or “Y” or “Z” and mount to either “Motor” or “Encoder”. Note to ensure that
the encoder does connect to “Encoder” and not “S/C Encoder”. The difference in Motor and Encoder
cables are easily identified as they will not mount incorrectly.
1.3 Axis Lockers
In shipment, the stages are locked into position with an Axis Locker on each stage.
It is crucial that all 3 of these are removed before the stages are moved. Take this opportunity to
remove them now with a Philips head screwdriver. Store the Axis Lockers as these will be needed
if the system is ever transported to a new location.

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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. Default IP Addresses
XYZ Controller
192.168.10.11
Supplied with VSC-BASE
Lock-in Amplifier
192.168.10.9
Supplied with VSC-SVET, VSC-SKP
Laser Profiler
192.168.10.10
Supplied with VSC-OSP
Pstat 1
USB
Connection
Drivers installed through VersaStudio software
package, supplied with VSC-SECM, VSC-SDC
Pstat 2
USB
Connection
Drivers installed through VersaStudio software
package, supplied with VSC-SECM, VSC-SDC
Computer
The CPU needs to be set to the same local network as the other
components. This is the 192.168.10.X setting where “X” is a numeric value
that is different to all other computers and devices, e.g., 192.168.10.100.
NOTE If the system has TWO motion controller boxes, please refer to Appendix 1 for
set-up diagrams.

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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.
1.5 Getting Started and Home Routine
Separate documents fully describe the functions of the software and describe the data file structure,
Projects, Experiments, Steps, etc.
When the power is turned off to the controllers, they lose their knowledge of absolute position.
When this happens a Home Routine needs to be performed, so that the controllers validate their
current position and the limits on the scan parameters.
Users will see a message such as this:
Figure 5. VersaSCAN Warning Message
By acknowledging this message (clicking “OK” button) users command the positioning system to
drive the stages to the extreme value. This is to its limit to the left (-X); and back (-Y); and up (+Z).
It uses this position as it is the most likely not to create physical contact with samples, cells, or
cables such as those between the SECM probe and cell etc. However, please consider that the
travel on these stages is 100 mm x 100 mm x 100 mm; so please ensure there is proper clearance
prior to running this Home Routine.
Users can also “Cancel” the Home Routine and remove possible obstructions before commencing
the Home Routine.
Also, consider this is only required when the Motion Controllers are powered off. If they are left in
the Powered (on) state; the system maintains its knowledge of the axial positions and will not need
to perform another Home Routine.
After the system finds these absolute limits, it will return to the position where the Home Routine
started. It is now ready for experiments or other manual control.

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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. It is important to
consider the speed at which the probe will move when one of these directional movements
is activated.
The Step (distance) and Speed are set using the sliding bar on the left.
Users can use the check box to enable these to be locked in step. Therefore, 1 click moves the
distance of 1 step at the given distance. Or these can be independently set.
It is highly recommended that users familiarize themselves with the mechanics of this Manual
Control before mounting a probe to the system. Users can see how fast the different movements
are and the response time required as the probe moves.
Generally, the user gradually decreases the Step and Speed as the probe approaches the sample.
The slide-bar makes it easy to reduce the Step from e.g., 1 mm →100 um →10 um →1 um. This
is a typical progression for these movements. Note that the piezoelectric motors produce a more
audible sound at lower speeds.

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1.7 Probe Position and Experiment Status
This Status Bar displays the active step in the Experiment, here labeled as “Idle”.
Figure 7. Status Bar
The Time section gives a real-time value of the duration of the current Step in the Experiment.
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.
An accompanying document provides specific information on hardware set-up and specifics of each
technique.

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2. 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. Rarely is a sample homogenous. Samples often consist
of local sites of passivate/active nature or sites of anodic/cathodic character. This is needed to
investigate localized electrochemistry led to the development of the Scanning Electrochemical
Microscope (SECM).
The SECM integrates a positioning system, a bipotentiostat, and an ultramicroelectrode tip. The
positioning system moves the tip close to the surface of the sample. The bipotentiostat polarizes
both the sample and the tip independently and measures both resulting currents. The tip is an
ultramicroelectrode with a specific tapered polish and active radius lower than 100 microns. The
positioning system scans the measurement tip and charts position with measured
electrochemical parameters, creating a data map of local current.
One SECM experiment is the Approach Curve in Feedback Mode. In this experiment, a redox
active salt, the mediator, is introduced into the electrolyte. A single potentiostat polarizes the tip
to cause an electrochemical reaction; however, the sample itself is not polarized. The resulting
current is recorded as the tip is incremented towards the sample. When the tip is appropriately
close to the sample, a local response is seen. If the location on the sample is conductive, the
Nernstian response of the sample causes an increase in current when compared to the bulk
current. This is called ‘positive feedback’. If the location on the sample is insulating, mass
transport to the electrode of the tip is hindered and a decrease in current is observed when
compared to the bulk current. This is called ‘negative feedback’. Intermediate behaviors may
occur above different samples. Quantitative analysis of such approach curves allows very
accurate local surface kinetics analysis.
Figure 8. Approach Curve

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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.
In Generator-Collector mode, the SECM uses the second channel of the bipotentiostat to
polarize the sample and actively control the redox reactions in the system. As an example, if the
redox species exists in bulk solution in oxidation state Ox, the sample can be polarized to
electrochemically convert species Ox to species Red. If the tip is polarized to a different level, it
is sufficient to cause an electrochemical reaction with Red. Initially no bulk current is generated
at the tip, as the initial concentration of Red is negligible. However, when the tip enters a space
where the products of the electrochemical reaction at the sample (Red) do exist, current will be
generated at the probe. This provides an imaging mechanismfor the probe to determine spatially
where on the surface of the sample is most efficiently undergoing the electrochemical reactions.
A high current at the tip is due to more concentration of Red at the probe, which is in turn due to
a more active Ox→Red transition in that position.
Figure 9. Example of Generator-Collector Mode
2.2 Applications
Since the imaging mechanism is electrochemistry, the applications of a SECM are as varied as
the applications of electrochemistry itself. Some key applications are biological sensors, reaction
kinetics, porous membrane study, fuel cell catalysts, and corrosion mechanisms.