TR-SES-200 High Resolution VUV/UV Transmission and Reflection Evaluation System Manual

Document RD-15-11 No: TR-SES-200 High Resolution VUV/UV Transmission and Reflection Evaluation System Manual

TR-SES-200 Manual 1 Table of Contents Table of Contents System Overview Packing List Item Overview Quick Setup and Operational Checkout Hardware Setup Testing of Spectrometer Manually Obtaining a Reference Spectrum Subroutines PMT Signal Optimization for Maximum Signal Sample Rotation Optimization Sample Tilt Optimization for Maximum Signal Obtaining an Optimized Reference Spectrum without Automated Scanning Calibration Calibrating the PMT Stage Calibrating the Sample Rotation Calibrating the Sample Tilt Calibrating the Spectrometer Obtaining Transmission/Reflection Measurements Transmission/Reflection Vs. Wavelength using Automated Scanning Transmission/Reflection Vs. Wavelength without using Automated Scanning Transmission/Reflection Vs. PMT Angle Transmission/Reflection Vs. Sample Tilt Cross Sample Transmission/Reflection Measurement System Summary Appendix System Components Hydrogen Light Source Monochromator PMT Stage Order Sorter Sample Wheel Software Example Scans Contact

TR-SES-200 Manual 2 System Overview The Resonance Ltd. Transmission and Reflection Evaluation System is designed to deliver vacuum-ultraviolet (VUV) to ultraviolet (UV) radiation to a target sample and measure the reflectance, transmission or fluorescence of the target. The system includes a hydrogen lamp emitting from 115 nm to 400 nm, a 200 mm focal length vacuum monochromator with a PC controlled motor drive, a Hamamatsu R8486 photomultiplier tube (PMT) capable of detecting from 115 to 300 nm, Labview TM software and controlling electronics. TR-SES-200 Main System Parts

TR-SES-200 Manual 3 Packing List Below is a list of all the components shipped with the TR-SES-200. If you find any of these items to be missing, please contact Resonance Ltd. to arrange to have it delivered. Item Instruction Manual Tr-SES-200 Assembly including: VM200 Monochromator including: 1200G/mm grating WL adjustment electronics and software along with 2.75 inch Vacuum flange on rear can for pumpout High Vacuum certification VUV/UV test spectra Order sorting filters for 100 to 600 range (see TRSO) 2.75 inch Vacuum flanges for slits and pumpout VUV/UV test spectra NIST Traceable calibration VMMDA VM Motorized wavelength drive with PC interface VMSA Adjustable slit assemblies TRApSAperture stop TRSO VM200 Motorized Order-Sorter including vacuum compatible servo motor TRSC Sample Vacuum chamber end flanges pumping and other ports with CF flanges Interfaces to sample and PMT TRPMT-CsTe VUV CsTe PMT including: Hamamatsu R8486 PMT Hamamatsu C6271 Power Supply Socket Cables TRMT-PMT including motorized turntable vacuum rotation assembly high torque motor with position feedback TRMSWA Motorized Sample wheel assembly 10 x 1 inch sample wheel 20 x ½ inch sample wheel TR-SW-CUST CUSTOM 7 5 3 MM SAMPLE Wheel TRPM-VUV2.75 Parabolic Mirror Collimator TRIR Iris for adjusting light aperture in vacuum chamber

TR-SES-200 Manual 4 TRVID Video Monitor for viewing motion of sample wheel and PMT Toolkit T1 Tools for assembly Hardware Vacuum Gaskets TR-VUV-VLS Lamp system with efficient coupling to VM200 TRPCWE PC with Software installed includes TRSW Software Electronics interface to PMT Sample wheel Iris and VM200 Monitor Samsung SD390HL sn 023WHCPG100822 Keyboard and Mouse TR-SES-200 System Main components 1. Tr-SES-200 main chamber assembly 2. TR-VUV-VLS Lamp system 3. TRPCWE PC PC system, software, monitor keyboard and mouse

TR-SES-200 Manual 5 Quick Setup and Operational Checkout Hardware Setup 1. Unpack system 2. Attach the Tr-SES-200 to the pump (either back or bottom 4.5 inch CF can be used). Figure 3: Vacuum hose and elbow 3. Open the sample wheel door Figure 4: System with Sample wheel door open

TR-SES-200 Manual 6 4. Carefully remove PMT wheel locking tie 5. Place the sample wheel on the spindle making sure it sits flat by aligning the spindle pin to the alignment hole on the wheel. Tighten the locking nut onto the spindle. Figure 7: Sample wheel placement (shown prior to application of black paint) 6. Close the sample wheel door making sure the vacuum seal o-ring sits flat inside the groove of the door. Fasten the door bolts until there is compression of the o-ring. Figure 8: Vacuum seal O-ring seated in door

TR-SES-200 Manual 7 8. Attach the lamp to the entrance slit flange of the monochromator with the screws and viton gasket provided. Tighten the screws until the gasket compresses and the lamp flange is touching the entrance slit flange. 9. Plug in the main electronics box to AC power.

TR-SES-200 Manual 8 10. Plug in the two electronic D style cables and the two plastic connectors to the Main Electronics case and the vacuum chamber. Follow the color code to insure the cables are plugged into the right connectors. Figure 11: Electronics case connectors 11. Plug in PC to AC power. 12. Attach the Camera and LED mount to the side view port by sliding the case on until it clicks in. Plug in the corresponding USB and LED cables to the PC/electronics box. 13. Plug in USB cable between the Display and the PC/Electronics box. 14. Turn PC on by pushing the PC On/Off button on front panel. The PC Power LED on the Main Electronics box should come on (if not check cables) Figure 12: Power indicator LEDs on electronics case

TR-SES-200 Manual 9 15. Turn on system electronics. The Lamp, PMT and Servos green LEDs on the Main Electronics box should come on. Note: The PC may operate independently from the TR-SES-200 system electronics. When not using the transmissometer for an extended period of time it is recommended to turn off the system electronics. Keep in mind the lamp has a warm-up period. 16. Open the VUV Spectrophotometer software by double clicking the TR-SES-200 icon on the desktop. 17. The indicator lights at the top of the screen should glow green after a few seconds. Figure 14: Software system check indicator lights 18. Make sure there is nothing obstructing any of the stages from rotating.

TR-SES-200 Manual 10 Testing of Spectrometer 19. Observe that the fan turns on when system electronics is on. Figure 16: Lamp Mounted to VM200 20. Allow approximately 20 minutes for the lamp to warm up and stabilize. 21. Meanwhile, carefully close the PMT door and bolt shut until the O-ring compresses. 22. Set aperture to Open Aperture with software. Figure 18: Aperture Wheel (prior to application of black paint)

TR-SES-200 Manual 11 23. Carefully close the sample holder door and bolt shut until the O-ring compresses. 24. Open slits (2) to 800 microns 25. In the program, go to the PMT Rotation tab and set the desired angle to 0 degrees. The PMT rotation motor will make a sound and the displayed PMT angle will start changing. Wait until the PMT reaches zero position. 26. Go to the Sample Rotation tab and set the sample wheel rotation to a vacant sample location. 27. On the Spectrometer tab, set the desired Wavelength to 230nm and press the Scan button in the bottom left corner.

TR-SES-200 Manual 12 28. Click the PMT button to turn on the photomultiplier tube (located in the lower right-hand corner of screen). Set the PMT Gain (adjustable via slider or value input box) to an initial low value and increase accordingly to the PMT signal value so as to not saturate the signal. You should observe the numeric value in the PMT Signal box increase while adjusting the PMT gain to get a peak value below the maximum signal. If the PMT is exposed to a large signal while the voltage is set high, there is a possibility of damaging the detector! Figure 20: PMT gain and signal location 29. After the lamp has been running for 20 minutes, scan the spectrum from 170 to 310nm at a resolution of 0.1nm. One should see the UV portion of the D2 lamp spectrum which peaks at 230 nm.

TR-SES-200 Manual 13 Manually Obtaining a Reference Spectrum 1. Make sure that all doors to the chamber are closed and that there are no sources of light leakage into the chamber. 2. Go to the Spectrometer tab and set the wavelength to 230 nm. 3. Place the PMT at zero degrees (directly opposite the collimating assembly) 4. Set the PMT gain to a reasonable level (~2V). At this point a signal should be detected. 5. Rotate through 360 degrees on sample wheel to identify the locations of the open sector. 6. Scan to middle of the plateau of a vacant location. Record this angle for future use. 7. Return to the PMT Rotation tab and scan across the peak from -10 to +10 8. Scan up to the middle of the peak to optimize the signal. 9. Perform a scan across the wavelength range to be used in the tes sequence and save as your reference.

TR-SES-200 Manual 14 Subroutines PMT Signal Optimization for Maximum Signal 1. Go to the Spectrometer tab and set the wavelength to 230nm. 2. Go to the Sample Rotation tab and set the sample wheel to a vacant spot for the reference measurement, or to the desired sample location. 3. Scan the PMT from -10 to +10 degrees from the expected angle at a maximum of 0.1 degree increments. Figure 21: Manual scan for PMT alignment

TR-SES-200 Manual 15 4. Take note of the angle where the center of the peak is located. 5. Do another scan with the same step increment, this time ending at the peak of the curve. Figure 22: Optimizing the PMT Signal for maximum signal

TR-SES-200 Manual 16 Sample Rotation Optimization 1. Go to the Spectrometer tab and set the wavelength to 230nm. 2. Go to the Sample Angle tab and set the desired angle to 45 degrees. 3. Go to the PMT Rotation tab and perform the PMT Signal Optimization subroutine at zero degrees 4. Go to the Sample Rotation tab and scan across the full 360 degrees at an increment of 0.5 degrees. 5. Take note of the locations of the centers of any signal plateaus. 6. Starting just before the first plateau, scan at 0.1 degree increments to the recorded center of the plateau. 7. Record this as the optimized of the vacant slots for future use. 8. Return to the PMT Rotation tab and perform the PMT signal Optimization subroutine at 90 degrees. 9. Repeat steps 4-7 recording them as the center of the samples for future use.

TR-SES-200 Manual 17 Sample Tilt Optimization for Maximum Signal 1. Go to the Spectrometer tab and set the wavelength to 230nm. 2. Go to the Sample Rotation tab and set the sample wheel to the desired sample location. 3. Set the PMT to the desired angle. 4. Scan the Sample Tilt from -10 to +10 degrees from the expected angle at a maximum of 0.1 degree increments. Figure 23: Manual scan for PMT alignment

TR-SES-200 Manual 18 5. Take note of the angle where the center of the peak is located. 6. Do another scan with the same step increment, this time ending at the peak of the curve. Obtaining an Optimized Reference Spectrum without Automated Scanning 1. Perform PMT Signal Optimization subroutine. 2. Perform Sample Rotation Optimization subroutine. Calibration If for some reason you suspect that any of the stages may need re-calibration, simply set the PMT gain to an appropriate level and follow the calibration steps below. Calibrating the PMT Stage 1. Go to the Spectrometer tab and set the wavelength to 230nm. 2. Go to the Sample Rotation tab and set the sample wheel to a vacant spot (such as a reference sample location).

TR-SES-200 Manual 19 3. Scan the PMT from -10 to +10 degrees at a maximum of 0.1 degree increments. 4. Take note of the angle where the center of the peak is located. 5. Go into the Settings tab and in the section labelled Conversions, select PMT Rot in the drop-down box. 6. In the Angle textbox, type in the recorded peak angle from Step 4 and press the Convert button at the bottom of the section. 7. Copy the calculated Step Position in the grey box over to the PMT Rotation Offset textbox in the PMT Rotation Constants section. 8. Press the Save Settings button near the bottom of the screen. The green indicator light should turn on if the file has been properly saved.

TR-SES-200 Manual 20

TR-SES-200 Manual 21 Calibrating the Sample Rotation 1. Go to the Spectrometer tab and set the wavelength to 230nm. 2. Scan from across the diameter of the desired sample location at a maximum increment of 0.1 degrees. 3. Take note of the angle where the center of the plateau is located. 4. Go into the Settings tab and in the section labelled Conversions, select Sample Rot in the drop-down box. 5. In the Angle textbox, type in the recorded peak angle from Step 3 and press the Convert button at the bottom of the section. 6. Copy the calculated Step Position in the grey box over to the Sample Rotation Offset textbox in the Sample Rotation Constants section. 7. Click the Save Settings button near the bottom of the screen. The green indicator light should turn on if the file has been properly saved.

TR-SES-200 Manual 22 Calibrating the Sample Tilt 1. Place a UV reflective mirror on the sample wheel and note its location. 2. Go to the Sample Rotation tab and set it so that the mirror is in the beam path. 3. Go to the Spectrometer tab and set the wavelength to 230nm. 4. Go to the PMT Rotation tab and set the angle to 45 degrees. 5. Scan the angle tilt from 80-100 at a maximum of 0.1 degree increments. 6. Take note of the angle where the center of the peak is located. 7. Go into the Settings tab and, in the section labelled Conversions, select Sample Tilt in the drop-down box. 8. In the Angle textbox, type in the recorded peak angle from Step 3 and click the Convert button at the bottom of the section and record the calculated step position. 9. Repeat steps 2-6 on the negative side (PMT at -45 and Angle tilt scan from -80 to -100 degrees).

TR-SES-200 Manual 23 10. Calculate the average of the two recorded step positions. This is the location of the zero angle (sample wheel perpendicular to the beam path). 11. Insert the calculated zero angle into the Sample Tilt Offset textbox in the Sample Tilt Constants section. 12. Click the Save Settings button near the bottom of the screen. The green indicator light should turn on if the file has been properly saved. Calibrating the Spectrometer To properly calibrate the spectrometer, at least 3 well defined spectral peaks are required. hydrogen has well known lines at 121.4 nm. For the second and third line, the second and third order diffraction of the 121.4 nm line, at 242.8 nm and 363.2 nm lines will work. 1. Set the PMT to zero degrees. 2. Set the sample wheel to vacant spot (such as a reference location). 3. Turn on the hydrogen lamp and allow 20 minutes to warm up.

TR-SES-200 Manual 24 4. Pump down the system to the 10-3 mbar range. 5. Perform a full range scan, from 100 to 400nm. 6. Identify the three peaks of interest and take note of their displayed wavelength position. 7. Go to the settings tab and, in the Conversions section, determine their corresponding step positions. 8. In the Spectrometer Wavelength Calibration section, insert what the actual wavelength for the peaks should be in the λ1, λ2 and λ3 textboxes, and the calculated step positions in the corresponding textboxes. 9. Click the Calculate button to obtain a new set of constants. 10. Once satisfied with the constants, click on the Apply button. 11. Click the Save Settings button near the bottom of the screen. The green indicator light should turn on if the file had been properly saved.

TR-SES-200 Manual 25 Obtaining Transmission/Reflection Measurements Transmission/Reflection Vs. Wavelength using Automated Scanning 1. Ensure all the stages are properly calibrated. 2. Perform the Sample Rotation Optimization subroutine to determine the location of the samples. 3. Go to the Setup tab. 4. Ensure all the stages have been zeroed. 5. In the Automated Scanning box, select the sample wheel that is being used. 6. Click on the box next to the Sample # for all the samples to be measured. 7. Set the Sample Tilt Angle for the reference and the samples. 8. Set the PMT Angle for the reference and the samples to be measured. 9. Set the Sample Rotation Angle to identify the location of the reference and samples. 10. In the Spectrometer Settings box, set the scan parameters for the measurements: Start and end Wavelength; Wavelength step increment; # of averages per measurement; the delay between readings (only applies if doing more than one averages); and the slit width (for reference only, does not actually set the slit width). 11. Set the PMT Gain to an acceptable level (2.0 is adequate for the majority of situations). 12. In the Signal Selector box, set the input type (PMT Input for standard transmission and reflection measurements, Aux Input for diode sensitivity measurements) and the gain (note: the +/- value indicates the signal limits with that particular gain setting). 13. When all parameters are set, click the Save Parameters button. 14. Click the Measure button to start the scans. The system will go through the scans in the following order: Reference - Sample 1 - Reference - Reference - Sample 2 - Reference... Depending on the settings, this could take from 5 minutes to over and hour.

TR-SES-200 Manual 26 15. Once the scans are complete for each sample the calculated transmission/reflection graph will be displayed (shown as Measure 1, 2 etc. with the scan plots on the right pane along with reference and sample scans). 16. To save, right click the view window and select a desired File Save Path and File Name. You have the option to save all scanned plots or only the current viewed plots. Ensure you select the appropriate option before clearing data or exiting the program. Click Save and your data will be saved to your selected save path. Transmission/Reflection Vs. Wavelength without using Automated Scanning 1. Ensure all the stages are properly calibrated. 2. Perform the Sample Rotation Optimization subroutine to determine the location of the samples. 3. Set the Sample Rotation to the vacant spot for the reference scan. 4. Set the sample tilt to the desired angle. 5. Perform the PMT Optimization subroutine. 6. Go to the Spectrometer tab and set the scan parameters for the measurements : Start and end Wavelength; Wavelength step increment; # of averages per measurement; the delay between readings (only applies if doing more than one averages; and the PMT gain). 7. Select the type of scan to be performed: Constant Rate or Fastest Speed. Fastest speed will go through the scan as quickly as it can under the set parameters, however the time interval between steps may be inconsistent due to software hand-shaking. Constant rate introduces a delay between steps so that the time interval between steps is consistent throughout the scan. 8. When all parameters are set, click the Start Scan button. 9. When the scan is complete, record the Scan # for future calculation.

TR-SES-200 Manual 27 10. Repeat steps 3-9 for each sample to be measured. It is also recommended to take additional reference scans either after each sample or, at the least, after completing all the sample scans to compensate for any potential lamp drift. 11. When ready, set the scan # for the sample transmission/reflection you want to measure as Plot 2 and set two reference scans (either the ones taken at the start and end of the scan sequence or the ones taken immediately before and after the scan for desired sample) as plots 3 and 4. 12. Setup the function setting to calculate the transmission/reflection of the sample using the average of the two reference scans selected. 13. When you re satisfied with the formula setup, click on the Calculate Result button. The displayed graph will automatically change to the calculated transmission/reflection curve. 14. If the curve is very noisy, you can take the average of multiple data points by setting the number of data point to be used in the text box to the right of the Calculate Result button and pressing the Apply Running Average button above it. 15. Set the File Name and the File Save Path. 16. In the drop box beside the Save button select Result then click the Save button. This will save the transmission data as well as all the spectral data used in the calculation. The green indicator light will turn on to indicate that the file has been saved successfully. 17. If external manipulation of the data is desired, set Post 1, 2, 3 and 4 to the desired scan # s and repeat the save process but setting the Save drop box to the Plot number. This will save each scan in its own individual file.

TR-SES-200 Manual 28 Transmission/Reflection Vs. PMT Angle 1. Ensure all the stages are properly calibrated. 2. Perform the Sample Rotation Optimization subroutine to determine the location of the samples. 3. Set the Sample Rotation to the vacant spot for the reference scan. 4. Set the sample tilt to the desired angle. 5. Set the monochromator to the desired wavelength. 6. Go to the PMT Rotation tab and set the scan parameters for the measurements : Start and End Angle; Angle step increment; # of averages per measurement; the delay between readings (only applies if doing more than one averages; and the PMT gain). 7. Select the type of scan to be performed: Constant Rate or Fastest Speed. Fastest speed will go through the scan as quickly as it can under the set parameters, however the time interval between steps may be inconsistent due to software hand-shaking. Constant rate introduces a delay between steps so that the time interval between steps is consistent throughout the scan. 8. When all parameters are set, click the Start Scan button. 9. When the scan is complete, record the Scan # for future calculation. 10. Repeat steps 3-9 for each sample to be measured. It is also recommended to take additional reference scans either after each sample or, at the least, after completing all the sample scans to compensate for any potential lamp drift. 11. When ready, set the scan # for the sample who s transmission/reflection you want to measure as Plot 2 and set two reference scans (either the ones taken at the start and end of the scan sequence or the ones taken immediately before and after the scan for desired sample) as plots 3 and 4. 12. Setup the function setting to calculate the transmission/reflection of the sample using the average of the two reference scans selected. 13. When you re satisfied with the formula setup, click on the Calculate Result button. The displayed graph will automatically change to the calculated transmission/reflection curve.

TR-SES-200 Manual 29 14. If the curve is very noisy, you can take the average of multiple data points by setting the number of data point to be used in the text box to the right of the Calculate Result button and click the Apply Running Average button above it. 15. Set the File Name and the File Save Path. 16. In the drop box beside the Save button select Result then click the Save button. This will save the transmission data as well as all the spectral data used in the calculation. The green indicator light will turn on to indicate that the file has been saved successfully. 17. If external manipulation of the data is desired, set Post 1, 2, 3 and 4 to the desired scan # s and repeat the save process but setting the Save drop box to the Plot number. This will save each scan in its own individual file. Transmission/Reflection Vs. Sample Tilt 1. Ensure all the stages are properly calibrated. 2. Perform the Sample Rotation Optimization subroutine to determine the location of the samples. 3. Set the Sample Rotation to the vacant spot for the reference scan. 4. Set the PMT to the desired angle. 5. Set the monochromator to the desired wavelength. 6. Go to the Sample Tilt tab and set the scan parameters for the measurements : Start and End Angle; Angle step increment; # of averages per measurement; the delay between readings (only applies if doing more than one averages; and the PMT gain). 7. Select the type of scan to be performed: Constant Rate or Fastest Speed. Fastest speed will go through the scan as quickly as it can under the set parameters, however the time interval between steps may be inconsistent due to software hand-shaking. Constant rate introduces a delay between steps so that the time interval between steps is consistent throughout the scan. 8. When all parameters are set, click the Start Scan button. 9. When the scan is complete, record the Scan # for future calculation.

TR-SES-200 Manual 30 10. Repeat steps 3-9 for each sample to be measured. It is also recommended to take additional reference scans either after each sample or, at the least, after completing all the sample scans to compensate for any potential lamp drift. 11. When ready, set the scan # for the sample who s transmission/reflection you want to measure as Plot 2 and set two reference scans (either the ones taken at the start and end of the scan sequence or the ones taken immediately before and after the scan for desired sample) as plots 3 and 4. 12. Setup the function setting to calculate the transmission/reflection of the sample using the average of the two reference scans selected. 13. When you re satisfied with the formula setup, click on the Calculate Result button. The displayed graph will automatically change to the calculated transmission/reflection curve. 14. If the curve is very noisy, you can take the average of multiple data points by setting the number of data point to be used in the text box to the right of the Calculate Result button and click the Apply Running Average button above it. 15. Set the filename and the File Save Path. 16. In the drop box beside the Save button select Result then click the Save button. This will save the transmission data as well as all the spectral data used in the calculation. The green indicator light will turn on to indicate that the file has been saved successfully. 17. If external manipulation of the data is desired, set Post 1, 2, 3 and 4 to the desired scan # s and repeat the save process but setting the Save drop box to the Plot number. This will save each scan in its own individual file.

TR-SES-200 Manual 31 Cross Sample Transmission/Reflection Measurement 1. Ensure all the stages are properly calibrated. 2. Perform the Sample Rotation Optimization subroutine to determine the location of the ends of the vacant spot and samples. 3. Set the Sample Rotation to the vacant spot for the reference scan. 4. Set the sample tilt to the desired angle. 5. Set the monochromator to the desired wavelength. 6. Perform the PMT Optimization subroutine. 7. Go to the Sample Rotation tab and set the scan parameters for the measurements: Start and End Angle; Angle step increment; # of averages per measurement; the delay between readings (only applies if doing more than one averages; and the PMT gain). 8. Select the type of scan to be performed: Constant Rate or Fastest Speed. Fastest speed will go through the scan as quickly as it can under the set parameters, however the time interval between steps may be inconsistent due to software hand-shaking. Constant rate introduces a delay between steps so that the time interval between steps is consistent throughout the scan. 9. When all parameters are set, click the Start Scan button. 10. When the scan is complete, record the Scan # for future calculation. 11. Repeat steps 3-9 for each sample to be measured. It is also recommended to take additional reference scans either after each sample or, at the least, after completing all the sample scans to compensate for any potential lamp drift. 12. When ready, set the scan # for the sample who s transmission/reflection you want to measure as Plot 2 and set two reference scans (either the ones taken at the start and end of the scan sequence or the ones taken immediately before and after the scan for desired sample) as plots 3 and 4. 13. Setup the function setting to calculate the transmission/reflection of the sample using the average of the two reference scans selected.

TR-SES-200 Manual 32 14. When you re satisfied with the formula setup, click on the Calculate Result button. The displayed graph will automatically change to the calculated transmission/reflection curve. 15. If the curve is very noisy, you can take the average of multiple data points by setting the number of data point to be used in the text box to the right of the Calculate Result button and click the Apply Running Average button above it. 16. Set the filename and the File Save Path. 17. In the drop box beside the Save button select Result then press the Save button. This will save the transmission data as well as all the spectral data used in the calculation. The green indicator light will turn on to indicate that the file has been saved successfully. 18. If external manipulation of the data is desired, set Post 1, 2, 3 and 4 to the desired scan # s and repeat the save process but setting the Save drop box to the Plot number. This will save each scan in its own individual file.

TR-SES-200 Manual 33 System Summary The TR-SES-200 is a spectrophotometer that has four main system elements: 1. VUV, UV tuneable light source (TLS) consisting of: a. Hydrogen light source with power module for 100 to 240 V operation b. Motorized VM200 Monochromator with 200 nm and 285 nm order sorter filter switch (for continuous operation from 110 to 400 nm). c. Collimating Assembly 2. Motorized sample wheel that can tilt and rotate: a. Tilt and rotate drive mechanism b. 2 inch and 1 inch sample wheels 3. Rotating Detector: a. PMT plus HV power supply and Amplifier. b. Periscope to increase rotation angle to within 6 degrees of beam. c. Rotating PMT stage with motor drive. 4. Electronics/Computing System: a. Main Electronics for motor control PMT and Diode monitoring Telemetry. b. PC.

TR-SES-200 Manual 34 Appendix System Components Hydrogen Light Source The system is provided with a Resonance Ltd. D2ArCM-L hydrogen light source, supplying radiation ranging from 115 nm to 400 nm, with a photon flux of approximately 2 x 10 15 photons/sec/str. The lamp is mounted adaptor and is located on the entrance slit arm of the monochromator. A separate manual describing lamp operation and specs is provided as support documentation. Monochromator A Resonance VM200 scanning monochromator is supplied to act a The VM200 monochromator contains a concave holographic grating optimized for the 100 to 300 range with the following specifications: No. of lines/mm: 1200 l/mm Size: 40 x 45 mm Coating: Al/MgF2 Spectral range of operation: 115 400 nm Input Focal length: la : 200 mm Output Focal length:: lb : 187.9 mm Reciprocal Linear Dispersion: 3.09 nm/mm (123 nm), 3.03 nm/mm (159 nm) 2.88 nm/mm (246 nm) The grating is rotated by a servo motor with an multi-turn absolute encoder. The grating is installed in a bucket and the spectrometer has two long arms at the end of which the entrance and the exit adjustable slits are installed. PMT Stage The TR-SES-200 uses a Hamamatsu R8486 28 mm, side-on PMT. This PMT is sensitive from 115 to 320 nm with a typical quantum efficiency of 22.5% at 122 nm. It is powered using a Hamamatsu C6271 high voltage power supply socket assembly. A 10-turn potentiometer is mounted on the front plate of the electronics rack to control the high voltage output to the PMT. It is best to keep the control voltage set low and increase it as needed. If the PMT is exposed to a large signal while the voltage is set high, there is a possibility of damaging the detector!

TR-SES-200 Manual 35 Order Sorter/Aperture Wheel As higher wavelength ranges are scanned, 2 nd and 3 rd order features can appear, making it difficult to obtain accurate spectral measurements. To prevent this, the system is equipped with order sorter filters which filter out lower wavelengths before their 2 nd order signal is reached. The filters are part of the aperture wheel and are software selectable. Quartz filters (transmission drops off around 180 nm) and Pyrex filters (drops off around 310 nm) to block off lower wavelength light are installed. Sample Wheel The system is provided with wheels to accommodate 1 and 2 diameter samples. Accessories are available for alternate sample sizes. Software The TR-SES-200 uses a LabView 8.2 based executable program that is compatible with Windows XP, Vista and Windows 7 and Windows 8.

TR-SES-200 Manual 36 Example Scans Measurement Scans Reference Scans

TR-SES-200 Manual 37 Contact Resonance Ltd. stands behind every product we sell. We welcome feedback and encourage any of our customers to contact us with questions, or concerns. Resonance Ltd. 143 Ferndale Drive North Barrie, ON L4N 9V9 Tel: 705-733-3633 Fax: 705-733-1388 Email: sales@resonance.on.ca Web: www.resonance.on.ca

TR-SES-200 Manual 38 Appendix 1 TR-SES-200 Subassemblies 1 VM200 VM200 W/standard 1200G/mm grating manually interchangeable slit, WL adjustment dial, 2.75 inch Vacuum flanges for slits and pump out, High-Vacuum-certified, VUV/UV test spectra, NIST Traceable calibration 2 VMMDA VM Motorized wavelength drive PC electrical interface, software drivers (PC is separate) 3 VMASA VM Adjustable Slit Assemblies (entrance and exit slits) for VM200 10 microns to 5 mm 4 TRApS Aperture Stop (Trims slit height for collimation) 5 TRSO VM200 Motorized Order-Sorter including vacuum compatible servo motor filter arm with 180 and 300 nm cutoff filters for 100 to 600 nm range 6 TRSC Sample vacuum chamber plus end flanges, pumping light and electrical io ports with CF flanges, end doors with interfaces for sample wheels and photomultiplier system 7 TRPMT-CsTe VUV CsTe Photomultiplier System with Hamamatsu R8486 PMT and C6271 Power Supply Socket in PMT rotation assy 8 TRMT-PMT Motorized PMT turntable with 360 degree rotation for control of angle of reflectance from sample surface, including vacuum feedthrough of motion, high torque motor with position feedback. 9 TRMSWA Motorized sample wheel assembly including wheel with 10x 1 inch samples with hole patterns for random sample sizes and holes for standard 25 mm sized samples and wheel with 20 x 1/2 inch with holes for 12-mm samples. Sample wheel spindle with rotation motor drive and Sample tilt arm with tilt motor drive. Two motors allow continuous rotation of sample wheel and continuous tilting 10 TRMRC Motorized sample wheel Tilt system including Vacuum servo motor with position feedback to accurately change the angle of incidence onto samples 11 TR-SW-Cust Custom 7mm, 5mm, 3mm sample wheel with capacity of xxx samples at each size.

TR-SES-200 Manual 39 12 TRPM-VUV2.75 Parabolic Mirror Collimator in 2.75-inch Conflat Flange with Vacuum housing, order sorter housing with vacuum electrical feedthroughs, VUV reflecting parabolic collimator 13 TREI-200 Electronics Interface including 16 bit picoammeter with 4 ranges, programmable HV Power supply for PMT, Power drivers for PMT tilt, sample tilt and sample rotation motors, saftey interlock controls for chamber A to D and D to A converters with PC interface 14 TRSW Software for Transmissometer System Control and Acquisition including reflection and transmission spectra, reference spectra, dark subtract, phase sensitive detection, signals vs. angles and signal vs sample positon, export to CSV, Excel, real time monitoring 15 TRPCWE PC with software installed and tested 16 TRVid Video monitor, with and vacuum viewport for checking position of sample wheel and PMT 17 TR-VUVUV-CLS VUV/UV Lamp system with efficient coupling to VM200 with spectral range of 113 to 400 nm, modulation and sync outputs for phase sensitive detection 18 TRSYSCAL System calibration and documentation package for transmission and reflectance of test samples in 113 to 300 nm region