Tektronix KEITHLEY EC-UPGRADE User manual

Keithley Instruments
28775 Aurora Road
Cleveland, Ohio 44139
1-800-935-5595
tek.com/keithley
SMU Potentiostats and EC-UPGRADE Kit
Quick Start Guide
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Description
The Keithley Instruments SMU (source-measure unit) Potentiostats are designed to make electrochemical
measurements easily and accurately. Included with your Model 2450, 2460, or 2461 Interactive SourceMeterTM
Instrument and other hardware is a USB flash drive containing electrochemistry test scripts or applications.
When running, each application can be user-configured to meet your specific test requirements.
The EC-UPGRADE kit lets you use an existing Keithley Instruments 2450, 2460, or 2461 SourceMeter as a
potentiostat or galvanostat.
The following applications are installed on your instrument or on the supplied USB flash drive.
▪Cyclic Voltammetry: Potential is swept at a user-programmable scan rate between two to four defined
potential vertices, and the resulting current is measured.
▪Open Circuit Potential: Measures the cell potential difference between two electrodes with high-input
impedance as a function of time.
▪Potential Pulse and Square Wave: Sources potential at programmable peak and base levels while
current is recorded at the pulse peak level, and the resulting current is measured.
▪Current Pulse and Square Wave: Sources current at programmable peak and base levels, and the
potential is recorded at the pulse peak level.
▪Chronoamperometry: Potential is stepped to a programmed value, and the resulting current is measured
as a function of time.
▪Chronopotentiometry: Current is stepped to a programmed value, and the resulting potential is
measured as a function of time.
This kit is not intended to be used with a SMU interlock enabled. To prevent electric shock
and possible damage to the test cable assembly or test setup, do not activate the Keithley
Instruments 2450, 2460, or 2461 interlock.
When the interlock is not engaged on the 2450, 2460, or 2461 the nominal output is limited to
±42 V. However, review the Safety Precautions (on page 23) section of this document to
ensure responsible operation.

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What you should have received
Below is a list of what you should have received. If you only ordered the EC-UPGRADE kit, a SMU instrument
is not included.
Model number
Quantity
2450, 2460, or 2461
1
01217440x
1
013042100
4
2450-800x
1
Description
Keithley Instruments 2450, 2460, or 2461
Interactive SourceMeter SMU Instrument
with power cable
1 m connectorized cable assembly
Insulated miniature alligator clips
Interactive Sourcemeter Electrochemistry
Kit USB Flash Drive and Instructions (not
pictured)
Figure 1: EC-UPGRADE kit shipping contents

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Getting started
Before you can run an electrochemistry test, you will need to configure the instrument and make basic
connections. The following topics will explain how to set up and configure your instrument.
The 2450-EC or 2460-EC instrument must have firmware version 1.5.0 or later to run the
electrochemistry test applications. The 2461-EC must have firmware version 1.6.0 or later.
Scripts with version numbers lower than 189427 are compatible with firmware versions 1.5.0
(1.6.0 for 2461) to 1.6.7. Scripts with version numbers of 189427 and higher are compatible with
firmware versions 1.5.0 (1.6.0 for 2461) to 1.6.7 and version 1.7.2 and higher. The script version
number is displayed near the top right corner of an application's Home screen.
To view the firmware version, press the MENU key, then select Info/Manage under System.
The firmware version is at the upper-left of your display. The latest firmware is available from the
Keithley Instruments website (tek.com/keithley).
Power the instrument on or off
Follow the steps below to connect the SMU to line power and turn on the instrument. The SMU operates from a
line voltage of 100 V to 240 V at a frequency of 50 Hz or 60 Hz. It automatically senses line voltage and
frequency. Make sure the operating voltage in your area is compatible.
You must turn on the SMU and allow it to warm up for at least one hour to achieve rated accuracies.
Operating the instrument on an incorrect line voltage may cause damage to the instrument,
possibly voiding the warranty.
The power cord supplied with the 2450-EC, 2460-EC, and 2461-EC contains a separate
protective earth (safety ground) wire for use with grounded outlets. When proper connections
are made, the instrument chassis is connected to power-line ground through the ground wire
in the power cord. In addition, a redundant protective earth connection is provided through a
screw on the rear panel. This terminal should be connected to a known protective earth. In
the event of a failure, not using a properly grounded protective earth and grounded outlet
may result in personal injury or death due to electric shock.
Do not replace detachable mains supply cords with inadequately rated cords. Failure to use
properly rated cords may result in personal injury or death due to electric shock.

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To connect the power cord:
1. Make sure that the front-panel POWER switch is in the off (O) position.
2. Connect the female end of the supplied power cord to the AC receptacle on the rear panel.
3. Connect the male end of the power cord to a grounded AC outlet.
To turn the instrument on or off:
1. Before turning the instrument on, disconnect any devices under test (DUTs) from the instrument.
2. To turn your instrument on, press the front-panel POWER switch to place it in the on (|) position. The
instrument displays a status bar as it powers on. The home screen is displayed when power on is
complete.
3. To turn your instrument off, press the front-panel POWER switch to place it in the off (O) position.
On some sensitive or easily damaged devices under test (DUTs), the instrument power-up and
power-down sequence can apply transient signals to the DUT that may affect or damage it. When
testing this type of DUT, do not make final connections to it until the instrument has completed its
power-up sequence and is in a known operating state. When testing this type of DUT, disconnect it
from the instrument before turning the instrument off.
To prevent any human contact with a live conductor, connections to the DUT must be fully insulated and the
final connections to the DUT must only use safety-rated safety jack socket connectors that do not allow bodily
contact.
Select the high-impedance, output-off state
Before making physical connections from the instrument to the test cell, set the output of the instrument to the
high-impedance, output-off state. When the high-impedance output-off state is selected, the output relay opens,
disconnecting the instrument from the load.
To set the output of your SMU to the high-impedance output-off state:
1. Press the MENU key.
2. Under Source, select Settings.
3. Select Output Off.
4. Choose High Z (high impedance).
You may receive a notification about making measurements with the output turned off. Select OK to
clear the message or select Details to see more information.

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Copy a script to the instrument
Your SMU is shipped with all test applications and supporting scripts loaded into memory.
If you accidentally delete a test application or a supporting script (EC_Framework.tsp or
EC_Images.tsp), you can copy the files from the flash drive to your instrument.
If you are upgrading your SMU with the EC-UPGRADE kit, you can run the test applications from the flash drive
or copy the files from the flash drive to the instrument. If you choose to copy the applications, you must also
copy the support files (EC_Framework.tsp and EC_Images.tsp) to your SMU.
To copy a script to the SMU:
1. Insert the USB flash drive into the USB port on the front panel.
2. Press the MENU key.
3. Under Scripts, select Manage. The Manage Scripts menu opens. Your list of Internal Scripts may appear
different than the following figure.
Figure 2: Manage Scripts menu
4. In the USB Scripts list, select the test script you want to copy to the SMU. For this example, you will copy
the cyclic voltammetry test script.
Figure 3: Selecting the test script to be copied

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5. Select <. The test script is transferred to the instrument, and the corresponding filename is displayed in the
Internal Scripts list.
Figure 4: Copying the file to the instrument
Connections and usage
The cable assembly can be used with Keithley SMUs for electrochemistry applications. Each connector of the
assembly is labeled according to its function:
Figure 5: Cable assembly connector labels and definitions

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Make the SMU connections
To connect to the instrument (all tests):
The front panel of your SMU has four banana-style input and output jacks. You use the supplied cable to
connect your electrochemical cell to these jacks.
The SENSE terminals are used to measure voltage at the device under test (DUT). When you use sense leads,
the voltage drop across the force leads is eliminated from a measurement. This produces more accurate
voltage sourcing and measurement at the DUT. Plug the SHI and SLO connectors into the SENSE terminals.
The FORCE terminals are used to source or sink voltage or current to or from a DUT. Plug the HI and LO
connectors into the FORCE terminals.
Plug the four SMU-side cable connectors into the front of your SMU instrument as shown in the below graphic.
Figure 6: Connecting SMU-side cable connectors to the SMU front-panel inputs
Make the device connections
The test cable lets you make connections to test cells with two, three, or four electrodes.
For two-electrode applications, the device-side cable connectors are used in stacked pairs. Connect the WE
and WES pair to the working electrode of your electrochemical cell, and connect the CE and RE pair to the
counter electrode of the cell.
Figure 7: Two-electrode cell testing cable connections

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For three-electrode applications, the WE and WES connectors are stacked and attached to the working
electrode. The CE and RE connectors connect to the counter electrode and reference electrode, respectively.
Figure 8: Three-electrode cell testing cable connections
For four-electrode applications, each device-side cable connector is used separately.
Figure 9: Four-electrode cell testing cable connections
Attach the alligator clips
Four insulated alligator clips are supplied. You can attach these clips to the ends of the device-side connectors,
as shown in the following graphic. The clips provide a safe, secure way to connect to your device.
Figure 10: Alligator clip attached to accessory cable connector
For small cells and electrodes, you can use commercially available banana-to-microclip connectors by plugging
them directly into the cable connectors.
Once the appropriate connectors or clips are attached, you are ready to connect to the test cell.

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Prepare the analyte and assemble the test cell
Before connecting to the DUT, make sure to prepare the analyte and assemble the test cell for your test.
Connect to the DUT
The next figure shows the connections from a SMU to a three-electrode test cell.
Figure 11: Front panel connections
Run a test
Once you have configured your SMU and connected a test cell, you are ready to run a test. For this example,
you will run the Cyclic Voltammetry test.
To run a test:
1. Press the HOME key.
2. Select the active script indicator at the top of your home screen. If there is no script activity, the indicator
displays "No Script."
Figure 12: Active script indicator

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3. Select the preloaded Cyclic Voltammetry test script or connect the supplied USB drive to your SMU
instrument to locate the included Cyclic Voltammetry test. If you connect the USB drive, scripts on the drive
are displayed with usb1/ before the script file name, which includes the .tsp file extension.
Figure 13: Available test scripts
4. Select CyclicVoltammetry. The test application runs and the Cyclic Voltammetry home screen is
displayed.
Figure 14: Cyclic voltammetry home screen
Review the test home screen controls
All test home screen controls include:
End App
Select this control to immediately stop the test and return to normal SMU
operation.
Autoscale
Select this control to define the graph based upon the plotted data. This is
useful for constraining all of the data to the screen's viewing size.
Start Test
Select this control to immediately begin the test. This option becomes Stop
Test when the test runs.
Save Data
Select this control to save the test data to a .csv file on a flash drive. This
option is only visible after the test runs.
Cursor
Select this control to cycle through the available cursor placements: None,
Vertical, Horizontal, and Both.

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Define the potential scan parameters
You will define the potential scan parameters: Number of vertices, vertex potentials, potential reference, scan
rate, and number of cycles.
An example of a potential scan performed during a cyclic voltammetry test is shown in the next figure.
You can select up to four voltage potential vertices, which are defined as E1 (or E initial), E2, E3, and E4 in the
next figure. The slope of the lines is determined by the scan rate that you use. You will set the scan rate later in
this step of the test.
Figure 15: Potential sweep versus time of cyclic voltammetry example
For this step, you will set the Number of vertices, define their potentials, and specify the potential reference.
To select the Number of Vertices:
1. Press the MENU key, then select Scan Settings.
2. Select Number of Vertices.
Figure 16: Scan Settings menu

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3. Enter the number of potential vertices. You can define two, three, or four vertices.
4. The vertex selections will change based on the number of vertices you choose. Select each vertex to enter
its potential. For this example, you will define four vertices.
Figure 17: Scan Settings menu, defining four vertices
5. Enter each vertex value in the range of ±20 V.
After you define the vertices, select the potential reference: Eref or Eoc. If you select Eref, the applied potential
is relative to the potential at the reference electrode. If you select Eoc, the applied potential is relative to the
open-circuit potential of the cell (Eoc), which is measured immediately before the scan begins.
To select the potential reference:
1. From the Scan Settings menu, select Reference.
Figure 18: Scan Settings menu, selecting Reference
2. Select Eref or Eoc.

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Define the scan settings
You can specify the scan rate in units of millivolts per second. The scan rate, defined as the change of the
potential as a function of time (∆E/∆t), determines the rate at which the potential is linearly scanned during the
experiment. You can select a scan rate of 0.1 mV per second to 3500 mV per second.
To select the scan rate:
1. From the scan Settings menu, select Scan Rate
Figure 19: Scan Settings menu, selecting Scan Rate
2. Enter a value.
3. Select OK.
After entering the scan rate, you will choose the number of cycles, from 1 to 100. The number of cycles
determines how many times each scan is repeated.
To select the number of scan cycles:
1. From the Scan Settings screen, select Number of Cycles.
Figure 20: Scan Settings menu, selecting the Number of Cycles
2. Enter a value.
3. Select OK.

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The following figure shows an example of a potential versus time graph showing three cycles of a three-vertex
voltage sweep.
Figure 21: Example potential versus time graph
Modify the measure settings
Specify how often to make measurements during the scan by selecting one of the sampling rate units shown in
the following table and setting a value for the sampling rate. The acquired measurements are stored in the
active buffer of the instrument, cvBuffer. The buffer can hold a maximum of 100,000 readings.
The following table describes the available interval units and accompanying range of values.
Sampling rate unit
Description
Sampling rate range of values
points/test
The number of points acquired during a test,
regardless of how many cycles
10 to 10,000
points/cycle
The number of points acquired in each cycle
10 to 10,000
s/point
The number of seconds per each point
0.01 to 100
points/s
The number of points taken per second
0.01 to 100

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To select the sampling rate units:
1. From the Menu screen, select Measure Settings.
2. Select Sampling Rate Units.
Figure 22: Measure Settings menu, selecting Sampling Rate Units
3. Select the units you want to use for the test. You can now set a sampling rate.
To set the sampling rate:
1. From the Measure Settings screen, select Sampling Rate.
2. Enter a value.
3. Select OK.
Now you will select the current range to measure the current from the scan. Choose the range based upon the
largest current magnitude you expect during the test.
To select the current measurement range:
1. From the Measure Settings screen, select Current Range.
Figure 23: Measure Settings menu, selecting Current Range

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When the test runs, your potentiostat will limit the magnitude of the maximum current that can flow in
the test circuit to 100 percent of the selected current range. This could affect your experiment results.
If your expected current is near the full scale of a range, select the next highest current range to
minimize the influence of your potentiostat on the test.
2. Choose a value. Note that the choices are different depending on your potentiostat model.
Figure 24: Selecting the current range
Although rare, you may encounter overshoot, ringing, or other instability on the output of your SMU potentiostat
depending the electrical impedance of your chemical cell. This is particularly an issue when the impedance is
capacitive and you are forcing voltage and measuring relatively low currents, as with the cyclic voltammetry
test.
In these cases, you can use the high-capacitance mode to minimize overshoot, ringing, and instability. See
your 24XX Interactive SourceMeterTM Reference Manual for more information.
To select the high-capacitance mode:
1. From the Menu screen, select Measure Settings.
2. Select High Capacitance.
Figure 25: High Capacitance Mode selection
3. Select Off or On.

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Save or load the test parameter data
You can save your test parameters to the front-panel flash drive at any time. Up to five test parameter
configurations can be stored.
To save the test parameters:
1. From the Menu screen, select Save Settings.
If you have saved a settings file previously with the same File Selection number, you will be
prompted to overwrite it.
Figure 26: Selecting Save Settings
2. Select a file number and then select Save Settings. You are notified when the save is complete, as shown
in the next figure. Select OK to clear the prompt.
Figure 27: Successful file save

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To load saved test parameters:
Test parameters can only be loaded to the same instrument model on which they were created and
saved. For example, you cannot load test parameter settings created with a 2450-EC to a 2460-EC.
1. From the Menu screen, select Load Settings.
Figure 28: Selecting Load Settings
2. Select a file by choosing File Selection and then a file number.
Figure 29: Choosing a file to load
3. Select Load Settings. You are notified when the load completes. Select OK to clear the prompt.

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Run the test and view the graph
To run the test and view the graph:
1. Press the HOME key.
2. Select Start Test. The output turns on automatically, and the display shows the current measurements
plotting in real time, along with a progress bar at the bottom of the screen. The Start Test control also
changes to Stop Test for the duration of the test.
The output turns off when the test completes. The following graphic shows the test home screen during the
test. You can return to this home screen at any time when the test is running by selecting the Run / Graph
option from the Menu screen.
Figure 30: Cyclic voltammetry test results graph
You can use the touchscreen to manipulate the graph or add cursors. See your Interactive
SourceMeterTM Instrument Reference Manual for more information.
You can save a screen capture to a flash drive inserted into the USB port of the potentiostat by simultaneously
pressing the HOME key and the ENTER key. The file name has the format imgmmdd_hhmmss.png, where
hhmmss represents the instrument hour (in 24-hour notation), month, and day.
To end the test before the run completes, select Stop Test at any time. This stops the test and turns
off the potentiostat output. You can then select End App to exit the test and return to normal SMU
operation. If there is a long interval between consecutive samples, there may be a long delay
between selecting Stop Test and when the test stops, as the current operation must complete.

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Make sure to select Stop Test before selecting End App. Stop Test turns off the instrument's
output.
Hazardous voltages may be present on all output and guard terminals. To prevent electrical
shock that could cause injury or death, never make or break connections to the instrument
while the power is turned on. Turn off the equipment from the front panel or disconnect the
main power cord from the rear of the instrument before handling cables. Putting the
equipment into an output-off state does not guarantee that the outputs are powered off if a
hardware or software fault occurs.
Acquire the open-circuit potential (Eoc)
If you selected Eoc as the potential reference for the scan, then the open-circuit potential will be measured
immediately after starting the test. You are prompted by the test application, as shown in the next figure.
Figure 31: Prompt for Eoc measurement
If you select Yes, the instrument measures the open-circuit potential (Eoc) of your electrochemical cell. If you
select No, the test stops. After the Eoc is measured, the value is displayed in a prompt, as shown in the next
figure. Figure 32: Eoc measurement displayed
If this value is acceptable, then select Yes to start the scan. If you select No, the test will stop. The measured
Eoc value is saved in the eocBuffer internal buffer of the instrument.