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1. EPITORR User s Guide Version 1 0 December 2006 r CIC Photonics RIGHT TO USE LICENSE AND NON DISCLOSURE AGREEMENT THIS RIGHT TO USE LICENSE AGREEMENT is made and entered into by and between CIC Photonics Inc having its principal place of business in Albuquerque New Mexico hereinafter referred to as Licensor and Applied Materials having a principal place of business at Santa Clara California hereinafter referred to as Licensee Reference P O No 4501245583 SECTION 1 DEFINITIONS Licensed Material means the proprietary SPGAS and SpectraStream and related computer software including executable code and or microcode on the delivered media and all copyrights and other legal rights including trade secret rights in such material Licensed Documentation means any documents materials specifications and information received by Licensee from Licensor relating to the Licensed Material and any copies thereof in whole or in part made by Licensee Licensed Products means the Licensed Material and Licensed Documentation Licensee s Organization means the Licensee legal entity only Designated Customer means any customer of the Licensee to which the Licensed Product is loaned temporarily for test and evaluation purposes SECTION 2 LICENSE GRANTED 2 1 Grant of License Licensor grants to Licensee and Licensee hereby accepts a nonexclusive non transferable license to use Licensed Products on
2. Figure 2 Processes 1 and 2 block diagram The gas analysis process is divided in two main processes Figure 2 One process is in charge of the data collection and the second process is in charge of the data processing Process 1 controls the interaction between the spectrometer and the computer Additionally process 1 interacts with and synchronizes other sub processes that set and control the sampling and the environmental conditions of the spectrometer These sub processes are in charge of controlling the gas handling system and the temperature controller if required 2 0 Unpacking and Installation The EPITORR is a high performance instrument that includes an interferometer laser mirrors windows filters high vacuum seals and electronics Hence it must always be handled with a degree of care and precaution to prevent physical damage and optical misalignments The EPITORR has been built into a Hardigg molded plastic enclosure of the type used in numerous transportable commercial and military instrumentation packages A custom designed vibration and shock mounting structure which is bolted to the walls and floor of the Hardigg enclosure provides isolation of the FTIR spectrometer and 4Runner gas cell subassembly the internal CPU is embedded in the touch screen monitor The enclosure has wheels on its bottom for easy movement within a lab or plant 2 1 Removal from Shipping Crate and Pallet The EPITORR has been shipped inside a wooden
3. 125 C for the bakeout periods The temperature controller has been preset at the factory at 60 C it is manually adjustable to other temperatures For the initial bakeout of the gas cell we recommend 125 C with purge nitrogen for a 24 hour start up conditioning period 4 3 FTIR Spectrometer The FTIR spectrometer is turned on when the system switch is turned on It requires between three to six hours to stabilize for quantitative data collection but it does start operating as soon as the system is turned on The FTIR resolution has been preset at the factory for 2 cm which is the resolution required for use with the SPGAS software therefore do not make any attempt to change the resolution 4 4 Computer System The CPU and touch screen monitor become activated when the computer switch is turned on The first screen to appear will look like Figure 4 Toward the middle upper right of the screen is a Start Stop button which will show Start initially because the computer has already activated the SPGAS software Touching the button alternately starts and stops the operation of the spectrometer At the lower right position are two displays the upper is labeled Show Spectra with options for Background Sample and Absorbance Below it is a display labeled Collecting which indicates one of the following operations Background Moving Mirrors or sample Below it is a
4. Chemraz O rings to high temperatures and acid gases can lead to their degradation 8 3 2 Temperature Controller and Heater If there is indication that the gas cell is not being heated first check the fuse on the temperature controller a blown fuse may indicate a short in the wiring to the heater Using an ohm meter then check the resistance across the leads to the heater a good heater should read approximately 50 ohms Do not overdrive the heating element by exceeding the temperature limit the silicone rubber composition of the sheet heater will start to degrade at 300 C 8 3 3 FTIR Spectrometer For proper operation the spectrometer operating temperature must be kept at or below 30 C and should not exceed 40 C In order to maintain a stable operating temperature heat dissipators have been added to the spectrometer body and with the gas cell enclosure to transfer heat to the circulating air stream which is provided by the two exhaust fans The fans come on when the system switch is activated if they do not come on do not operate the spectrometer shut the system down and call for technical support 8 3 4 CPU and Monitor The computer uses a standard Windows XP professional Operating System any IT Department should be able to troubleshoot it if necessary or call CICP technical support To shut down the CPU first touch the STOP button on the screen then click OK at the screen message and turn off the computer switc
5. DD The Quantification Log files are text files that are easily readable by software like MS Excel A quantification is produced every 30 seconds and stored inside its Quantification Log file One Quantification Log file is produced per day These files are stored inside a folder with the year and month as their name D IRGAS Quantification LogV Y Y MM The quantification calculations are stored in separate archive folders D IRGAS Quantification Log in a similar manner Files are retrieved by their date and hour identification The file sizes have been defined for content size corresponding to a floppy disk so that individual folders can be downloaded 5 4 Downloading Archived Data Records It becomes necessary for the system operator to download archived data about every 30 days in order to free up space on the hard disk Use MS Windows standard procedures to copy files to floppy disks A more efficient way is via the Ethernet 10 100 port for transfer of the data to the system operator s in house network the latter likely requires engaging the assistance of the internal IT Department 6 0 System Shutdown Procedures 6 1 Temporary Shutdown If the EPITORR is being shut down only temporarily and will be used again in the near term then the system switch should be left on so that the FTIR spectrometer power remains on to 18 keep the internal temperature above ambient The computer and heater switches may be turned off
6. de de ese de se ee ee se ese een es 6 34 ARUNNERLONGPATHGAS CRL 6 3 5 TEMPERATURE CONTROLLER gear EE NRA ee nate eo ge de uge Ales 7 3 6 CPU AND TOUCH SCREEN MONTIOR eed se ese se ese ee gee ence ge ese ee eae ee ee ee ees 7 3 7 PURGE AND SAMPLE GAS PLUMBING ees se ee se ese dee gee cece ge ese ee ee ede ee ee 8 3 8 SPGAS SYSTEM MANAGEMENT AND GAS QUANTIFICATION SOFTWARE 12 3 9 SPECTRASTREAM FAST RESPONSE SOFTWARE MODULE sesse see se se dee 12 3 10 ELECTRICAL SYSTEMS SESSE ese ee SR ES see ER Bg VEER Vee deg lee eee ees 12 4 0 SYSTEM START UP OPERATIONS eie see ese ese se ese se ese ese se ese ee see se ese se ese ee se ee ee 14 4 1 PURGE GAS FLOW AND SYSTEM SWITCHES eise ese dee sed se dee se ee ee ee ee ee ee 14 42 TEMPERATURE CONTROLLER AND GAS CELL HEATER ii eie ese se sed se see 14 4 3 FLIRSPECTROMETER iis esta ges Soca Wee ee EES Seel N Ge Ee See coeur 14 4 4 COMPUTER SYSTEM cies si cosy es Mee EE Er ERGE Oos see Ee Se EG gee NEEN se VAR GE Se SES ED ge Ged 14 4 5 SPGAS SPECTRASTREAM SOFTWARE DISPLAYS ee ese ese see se ese ee ese ee se ee 16 4 6 gt SYSTEM TESTES is iese gee ene ge guer deg EEN Ha ged es beg ER Se ee see ie 16 5 0 FULL SYSTEM OPERATIONAL PROCRDURES ee eise de es ese ee ese ese see ee ese ee ese ee ee se ee ee 21 3 1 GAS CELE PURGE iis si Haan ees ee Ee de ee EE AE 21 5 2 AUTOMATED DATA COLLECTION AND DiSbtAN ese dee se ese se ee ee ee se ee es 21 5 3 RECORDING ARCHIVIN
7. that the operation of the Licensed Products will meet Licensee requirements EXCEPT AS PROVIDED IN THIS LIMITED WARRANTY LICENSOR MAKES AND LICENSEE RECEIVES NO WARRANTY EXPRESS OR IMPLIED INCLUDING BUT NOT LIMITED TO IMPLIED WARRANTIES OF MERCHANTABILITY AND OR FITNESS FOR A PARTICULAR PURPOSE OR USE 6 1 6 2 7 1 7 2 7 3 71 4 By Signed Name SECTION 6 LIMITATION OF REMEDIES If Licensee reasonably determines that the Licensed Products do not perform as warranted and notifies Licensor of the perceived defect during the aforesaid one 1 year warranty period Licensor s entire liability and Licensee s exclusive remedy shall be for Licensor to i Replace the Licensed Product if determined necessary by Licensor or ii Use best efforts to respond within a reasonable time to telephone inquiries from Licensee with regard to problems with the Licensed Product IN NO EVENT SHALL LICENSOR BE LIABLE TO LICENSEE FOR DAMAGES INCLUDING ANY LOST PROFITS LOST SAVINGS LOST DATA LOST OR DAMAGED LICENSED PRODUCTS OR OTHER INCIDENTAL OR CONSEQUENTIAL DAMAGES ARISING OUT OF THE USE OR INABILITY TO USE THE LICENSED PRODUCTS OR FOR ANY CLAIM BY ANY OTHER PARTY SECTION 7 GENERAL Applicable Software This Agreement applies to all purchases of the SPGAS and SpectraStream software products past present and future by Licensee when purchased in conjunction with IRGAS Systems or separately as software Signature Auth
8. the terms and conditions of this Agreement 2 2 Scope of Authorized Use 2 2 1 Licensed Products Licensee is authorized to use the Licensed Products within Licensee s Organization and at Designated Customer sites only when the Licensed Products remain under the control of the Licensee for INTERNAL PURPOSES ONLY The Licensed Products may not be delivered or provided to any person or persons outside of Licensee s Organization and its Designated Customers without the express written approval of the Licensor 2 2 2 Reverse Engineering Non Competition Licensee agrees not to disassemble decompile or reverse engineer the Licensed Materials and agrees not to allow these actions by its Designated Customers Licensee also agrees that any information obtained in violation of this restriction will be Confidential Information automatically and irrevocably deemed assigned to and owned exclusively by 2 2 3 2 4 3 1 3 2 4 1 Licensor Licensee further agrees not to distribute materials performing functions similar to those of the Licensed Materials without the prior written consent of Licensor Copyright Licensor owns a copyright in the Licensed Products as unpublished works or otherwise and Licensee acknowledges same Assignment of License Licensee s rights in and to the Licensed Software as a result of this Agreement may not be assigned or otherwise transferred voluntarily by operation of law or otherwise without Lice
9. time line showing the Time Left for each of those three operations The SPGAS software is causing the FTIR and transfer mirrors to cycle repeatedly through those three Figure 4 Start Up Screen Display HE IRGAS 100T With SpectraStream Monitor co2 H20 PPB 00 00 Time hh mm Show Spectra C02 H20 E Background i Sample E Absorbance Collecting Stopped Time Left0 Seconds 10 operations With each completed cycle the SPGAS performs a guantitative analysis of the collected data to generate the screen displays of spectra At the Show Spectra display one chooses which of the three options one wants displayed on the main portion of the screen One can switch back and forth between the current background spectrum the current sample spectrum or the calculated absorbance record At the top right of the screen just below the Spectra tream logo is a scan bar which shows on a 0 to 100 scale the percentage of the selected number of scans that have been performed by the FTIR 4 5 SPGAS SpectraStream Software Displays A typical SPGAS screen display is shown in Figure 5 It provides a graphical display of the concentrations of the selected gaseous species as a function of time The gaseous species are those prescribed in advance to the factory for the inclusion of HITRAN calibration data Also presented at the bottom of the screen is the Concentration Log for the selected molecules Two sets
10. with the performance of the process tool 5 3 Recording Archiving and Recalling of Collected Data Each cycle of background sample and absorbance data is automatically stored in a Grams SPC file format in archive folders on the hard disk of the CPU The spectral records are stored in archive folders D Irgas Spectral Records as the spectra are collected D Spectral Records Filename Convention Background_ TimeStamp spc Sample TimeStamp spc Absorbance TimeStamp spc 16 Figure 9 Single Beam Moisture Background Peak HE IRGAS 100T With SpectraStream 1 658 1 656 1 654 Wavenumbers cm 1 Concentration Log Molecule Concentration ppb c02 0 5 1 2 H20 70 5 Standard Error FCT 29 Standard Error 9 88 15 1 27 8 Show Spectra rd Background E Sample E Absorbance Collecting Background mmm Time Left8 Seconds 17 TimeStamp YY MM DD HH MM SS A file is created about every 30 seconds The Spectra files are stored inside a zip file in 2 hour increments to keep the file size manageable at lt 1 4 mb BackgroundTimeStamp zip Sample TimeStamp zip Absorbance TimeStamp zip The zip files in turn are stored inside a folder with the creation date as their name D IRGAS Spectral Records Date where Date YY MM DD Quantification Log Filename Convention Ouan DateStamp Log DateStamp YY MM
11. 3 2 8 1 14 2 27 4 Collecting Sample E Standard Error Standard Error 5 0 4 Time Left 11 Seconds 13 Figure 7 Single Beam Background Record HE IRGAS 100T With SpectraStream Background Monitor CO2 H20 il Show Spectra 3 500 3 000 2 500 2 000 1 500 1 000 Iv Back groun d Wavenumbers cm 1 i Sample EET E Absorbance Concentrationippb Standard Error 4 1 2 0 5 f d 4 H20 721 85 79 1 28 8 Collecting Sample ee ee ee ee Standard Error 6 Time Left 0 Seconds 14 Figure 8 Single Beam Sample Record Ree 1007 Wan Specuasueen EE Background Sample Absorbance Monitor CC 4 gt Show Spectra 3 500 3 000 2 500 2 000 1 500 1 000 KREIS groun d Wavenumbers cm 1 Sample rd Absorbance FCT Standard Error 0 0 Standard Error 8 77 4 ER Collecting Sample mmm Time Left8 Seconds 15 For the second test display again the Background single beam record and look for the moisture absorption peak at 1653 em Magnify the display of that peak by touching the screen at that point and applying a downward left to right sweep to a scale size that is more easily readable Estimate the effective magnitude of that peak from its peak up to a smoothed curve position on the single beam If the magnitude in arbitrary units is less than 0 05 adequate purging has occurred and one can proceed to sampling process gas for analysis if not then more nitrogen pu
12. 343 9500 Main CEO amp President 509 479 2980 Fax 505 343 1489 Technical Support CIC Photonics Inc 9000 Washington St NE Albuquerque NM 87113 ask cicp com http www irgas com 2002 CIC Photonics Inc No information contained in this document may be reproduced in any form in full or in part without prior written permission from CIC Photonics Inc This document contains product specifications and performance statements that may be in conflict with other CIC Photonics published literature such as product flyers and product catalogs All specifications product characteristics and performance statements included in this document are given as suggestive specifications only In case of conflict between product characteristics given in this document and specifications given in the official CIC Photonics Product Catalogs the latter take precedence CIC Photonics Inc reserves the right to make changes to the specifications of all equipment and software and contents of this document without obligation to notify any person or organization of such changes Every effort has been made to insure that the information contained in this document is current and accurate However no guarantee is given or implied that the document is error free or that the information is accurate CIC Photonics Inc makes no representations or warranties with regard to the product and instructional and reference materials including but not limited to al
13. G AND RECALLING OF COLLECTED DATA 21 54 DOWNLOADING ARCHIVED DATA RECORDS eie ese cece cence cece de ese ene ee 23 6 0 SYSTEM SHUTDOWN PROCEDURES ese ese Ee ence ence cence eee ene see ee dee ee p ee anaes 23 6 1 TEMPORARY SHUTDOWN sesse eg se uses se be Deb de ee Se babes tab Ge eb OG GES ER GER tenes 21 6 2 LONG TERM SHUTDOWN se sesse es ES SEG dE eee bet E Dog De Se de 24 6 3 MOISTURE PROTECTION eis pe desse grees ap eene EE GE Gee DES EN Ge ed dek Gede 24 1 0 PACKING FOR SHIPMENT osse ease eege ek andra GREG EEN EES 24 8 0 SYSTEM DIAGNOSTICS AND TECHNICAL SUPPORT ese see sesse see de es ee se se se sees se ee ees 24 MAER USER TEST Sy anoo ER EE EE ORE tees seer aadeatdeapmeantiebauees 24 8 2 TELEPHONE AND EMAIL SUPPOR D crecian see se ee ese ese gee ee ese ences ee ee se ee ee dee dee 24 8 3 TROUBLE SHOOTING Vi ass NEE ege dE veda AO ee eg ee ER ee Ee 25 8 3 1 GAS CELL DEGRADATION MIRRORS SEALS WINDOWG 25 8 3 2 TEMPERATURE CONTROLLER AND HRATIER eie se se ese esse se de dee 25 8 3 3 FIIR SPECTROMETER eise ES Ke EER Ee Oe SEENEN Ee 25 8 3 4 CPUAND MONITOR ccs os heaves SERS dy GE ENEE Re RE gi be ie Dee vee De di 25 8 3 5 NITROGEN PURIFIER AND GAS LINRS ese ee dee se ese see ge ee ese see ee 25 8 3 6 ELECTRICAL SYSTEM FANS FUSES ese ee se dee ee ge ese de ee ee ee 26 8 3 7 VIBRATION AND SHOCK ISO ATORs ee se ee ee se ese se se ee se ee 26 84 REMOVAL OF GAS CELL FOR WARRANTYVREDAIR ee se se s
14. It is also desirable to keep the nitrogen purge gas flowing through the spectrometer transfer optics and separately through the gas cell 6 2 Long Term Shutdown Before turning off all power switches and terminating flow of purge nitrogen the gas cell should be purged thoroughly with nitrogen using a purge pump out bakeout procedure to rid the gas cell and process gas lines of all traces of the process gas three cycles of purging and pumping with the gas cell temperature elevated is probably adequate Allow the cell to cool to ambient temperature with purge nitrogen before stopping the flow and then cap the input and output lines with VCR caps and seals 6 3 Moisture Protection The above procedures are designed partly to remove all adsorbed moisture from the gas lines and gas cell Residual moisture in the presence of acid gases can be very destructive to the mirrors in the gas cell 7 0 Packing for Shipment The EPITORR should be repacked for shipping forward in the same manner as it was received That entails placing it back on the custom pallet so that the wheels are protected replacing the top cardboard cover tying it down with the four nylon straps and reinstalling the panels of the wooden crate 8 0 System Diagnostics and Technical Support 8 1 User Tests Repeat the tests described in Section 4 6 to ascertain if the system is performing correctly call for technical support if there are any major departures from the prescribed te
15. background moisture level to a minimum level For the first test switch to a background single beam record by touching the Background button under Show Spectra This brings onto the screen a single beam record Figure 7 Take note of or write down the maximum height of the single beam trace in arbitrary units Then switch to the Sample single beam display and take note of its maximum height see Figure 8 If the mirrors are moving in and out of the IR beam the height of the sample single beam should be less than the height of the Background single beam This is a consequence of the fact that in the Sample position the IR beam is traversing a longer distance through the gas cell 11 Figure 5 Typical Screen Display of Concentration vs Time HE IRGAS 100T With SpectraStream Monitor CO2 H2O i 75 70 65 60 55 50 m 45 Q 40 Ve 35 30 25 20 15 10 09 03 09 04 Time hh mm Show Spectra C02 H20 gi Background E Sample E Absorbance Concentration ppb Standard Error FCT Standard Error 2 11 5 0 4 H20 63 2 81 14 2 274 Collecting Background mmm Time Left8 Seconds 12 Figure 6 Multiple and Fast Scan Concentration Displays HE IRGAS 100T With SpectraStream Monitor CO2 H20 PPB 09 03 09 04 Time hh mm Show Spectra _ E Background E Sample E Absorbance FCT Concentrationlppb 2 11 V 4 H20 6
16. ber of scans of the sample gas and store this data as an interferogram Every time an interferogram is completed the computer retrieves this interferogram from the spectrometer and performs the quantitative gas analysis of the impurities Gas Cell A special designed gas sampling compartment Purge Box Used to interconnect the gas cell with the spectrometer inside the spectrometer s sample compartment FTIR Spectrometer Personal Computer Figure 1 FTIR Spectrometer and Personal Computer Interconnection Process 1 Process 2 Wait until there is a System Initialization Interferogram stored interferogram in ys Queue the queue and then retrieve it ER Calculate the absorption spectra of the sample based on the last spectrometer background reading i Perform chemometrics on data from the sampled gas to determine impurity concentrations Set condition to collect a background spectra No collect a new background spectra Collect a background spectra and store it Set and validate A Yes continue kgroun iin Go e l lS background sampling condition for sampling f i spectra valid gases Retrieve data from spectrometer and store it
17. crate mounted on a pallet The top and side walls of the crate should be unscrewed from each other and removed to gain access to the instrument All crate components should be stored for reuse and reshipping The EPITORR has been affixed to a custom wooden pallet with tie down straps over the sides of the enclosure The contractors on the nylon straps should be released and the straps removed from the pallet The straps protective cardboard edge covers and pallet which has been designed for the unit with wheels should be saved to use for later shipments of the system Once the straps and cover are removed the entire enclosure should be lifted off the pallet so that it can be set down on its wheels The total weight of the EPITORR without the pallet is approximately 200 Ibs the enclosure has two handles on each side for lifting and rolling Obviously it may take four persons to lift the unit off of the pallet This should be done before opening the top lid of the enclosure since it adds rigidity to the total physical enclosure 2 2 Electrical Electronic and Gas Connections Once the EPITORR has been removed from the pallet and wheeled to its location for first use then open the lid of the enclosure by disengaging the five locking clips and lifting the lid The lid has one internal guy wire which allows the lid to be lifted back to a stable open position The top panel is fitted with all the electrical electronic and gas connections and
18. ducts to be repaired under warranty are to be shipped back to our factory at user s expense after repair product will be returned at CICP s expense Parts that normally wear out or are consumed or can be damaged in the normal operation of the product such as fragile optical elements and seals lenses windows crystals mirrors filters C seals O rings etc are warranted against defect in manufacture only for a period of 30 days after original delivery to the purchaser Technical assistance for either hardware or software that can be provided by telephone fax or email will be provided by CICP at no time charge to end users for the life of the products After the warranty period has expired CICP offers service either on a time and materials basis or on an annual service and maintenance plan TABLE OF CONTENTS 1 0 INTRODUCTION ee ERG DEE ER eg Ee SE AG ced he dee EE dE e E DE pe Ge hee 1 2 0 UNPACKING AND INSTALLATION 0000 c cece cence cence eee ee ene ee E ese ene SR ee E ee de se 3 2 1 REMOVAL FROM SHIPPING CRATE AND DATIET eise se ese dee se ese ee ee ese se sees 3 2 2 ELECTRICAL ELECTRONIC AND GAS CONNPCTIONS esse se cece cence eee dees 3 3 0 DESCRIPTION OF MAJOR COMPONENTIS ese ee se ese ese se ese eee nee dee see ee ese ene se erase ne ee es 4 3 1 IRGAS SYSTEM OVERVIEW 40 5 Sts ccc ee DE Ne ER ORE poe ENN Joke aan Ve Re ga WEG ge e 4 3 2 IRGAS SYSTEM OPERATIONAL MODERN 6 3 3 BOMEM WORKIR FTIR SPECTROMETER ese de se ese
19. e ese see se ese ee 26 9 0 APPENDICES is Se DE eege EE os Ra Ee RR GR REDE GE EG RE EG dee dda NEG GER EER deca 27 FIGURE 1 FIGURE 2 FIGURE 3 FIGURE 4 FIGURE 5 FIGURE 6 FIGURE 7 FIGURE 8 FIGURE 9 LIST OF FIGURES FTIR SPECTROMETER AND PC INTERCONNECTION 1 PROCESSES 1 AND 2 DIAGRAM sesse ese dees eed vee eg dee geck ge se 2 IRGAS 100T SYSTEM BLOCK DIAOGRAM 0 cece cece ese esse ee ees 5 START UP SCREEN DISPLAY is RR SeSe eg ee DR Ge GE E Aer 14 TYPICAL SCREEN DISPLAY OF CONCENTRATION VS TIME 16 MULTIPLE AND FAST SCAN CONCENTRATION DISPLAYS 17 SINGLE BEAM BACKOGROUNDRBCORID ees se ese ee se sesse ss L8 SINGLE BEAM SAMPLE RECORD se esse see es ee sees ee En 19 SINGLE BEAM MOISTURE BACKGROUND PEAK eise ese see 21 1 0 Introduction The EPITORR Turnkey Gas Analysis System is a transportable version of CIC Photonics Inc e product line of IRGAS Integrated Real Time Gas Analysis Solutions that was especially designed for applied materials The EPITORR has been designed and developed to serve AMAT s need for a high sensitivity fast response time instrument Typically this entails the measurement of gas compositions and impurity species within epitaxial reactors at the low ppb level within seconds The EPITORR is designed for service with the numerous corrosive and toxic gases that are used in epitaxial reactors The heart of the EPITORR is the all stainless steel ARunner H
20. ee s Organization who must have access to Licensed Products in order to perform their work provided however that Licensee shall have no obligation of confidentiality with respect to Information disclosed to Licensee by Licensor if 5 1 X2 i such information is at the time of disclosure by Licensor to Licensee in the public domain or such information thereafter becomes a part of the public domain without a breach of this Agreement by Licensee or ii such information is known to Licensee at the time Licensor discloses it to Licensee or iii such information is independently developed by Licensee or iv such information is disclosed by Licensor to any third party including the United States Government without restriction as to further disclosure or v such information is disclosed with the written approval of Licensor Should Licensee determine that persons other than employees of Licensee require access to Confidential Information such as employees of any subsidiary or parent company of Licensee such disclosure may only be made with the prior written consent of Licensor This Paragraph 4 1 shall survive the termination of this agreement SECTION 5 LIMITED WARRANTY The Licensed Products are warranted to perform substantially in accordance with the applicable manual provided with the Licensed Products for a period of one 1 year after the date of delivery of the Licensed Products Licensor does not however warrant
21. en preloaded with CIC Photonics SPGAS and SpectraStream software and with HITRAN generated gas calibration data for H2O CO2 CH4 and HF Both H20 and CO2 in ratio can be used to ascertain the presence of any air leakages into a process tool 3 7 Purge and Sample Gas Plumbing VCR connections for the nitrogen purge gas in and for the process gas in and out are accessible at the back of the enclosure on the left and right sides respectively Internally the purge gas line connects to a nitrogen purifier for moisture which reduces the moisture purity of the ultra dry nitrogen supply gas to the ppb level This level of purity of the purge gas is required to ensure the best LOD for moisture in the process gases The nitrogen purifier is provided with a check valve at one end to protect it from air contamination when the nitrogen supply line is not connected a manual shut off valve is also located on the back side of the enclosure The purifier under normal EPITORR usage will last for six to twelve months before regeneration is required it can easily be changed out with a replacement unit Warning The nitrogen purifier should never be exposed to ambient air since air moisture will contaminate the purifier The process gas line is a direct stainless steel plumbing line from the top panel connection to the gas cell and back again without any valves filters or purifiers The user must provide all mass flow controllers and other device
22. h on the top panel If the CPU takes too long to respond after you click OK you may proceed to turn off the panel switch If the Touch screen appears not to be functioning look at the mouse symbol in the lower right bar on the screen observe whether the RED indicator is on the left side of the mouse if not touch the top left of the mouse to activate it The mouse symbol operates like a physical mouse with left and right buttons which you can toggle back and forth 20 To use an on screen keyboard touch the keyboard symbol on the lower right bar To use a physical keyboard open the top panel and use a PS 2 connector to connect to the terminal on the internal CPU If the system software has to be reinstalled a CD Drive is required for connection to the CPU call technical support for a copy of the software 8 3 5 Nitrogen Purifier and Gas Lines The expected lifetime of the nitrogen purifier under normal continuous operation of the system is six to nine months so long as it is not exposed to air Indication that it may becoming saturated with moisture comes from a steady increase in the measured moisture content in the Background records When this occurs to the extent that the background moisture is significantly interfering with quantitative measurements of moisture as an impurity in the process gases the nitrogen purifier should be replaced 8 3 6 Electrical System Fans Fuses The system electrical circuitry is protec
23. hosen for the EPITORR because of its high quality patented interferometer its total compactness and modest weight and its industrial ruggedness Technical features of the WorkIR are provided on the next page The internal optics are KBr and the IR detector is a TE Cooled InAs detector The WorkIR internal compartment should be purged with ultra dry nitrogen at all times Electrical power is provided to the WorkIR when the system switch is turned on it should be left on at all times to keep the spectrometer at a stable operating temperature and to reduce ambient moisture collection on the hydroscopic KBr optics the cooling fans are continuously operating during this time If the EPITORR is stored for any period of time the WorkIR should first be purged and sealed with dry nitrogen A complete Instruction Manual for the WorkIR is provided 3 4 4Runner Long Path Gas Cell The 4Runner Long Path Gas Cell is an all stainless steel cell with stainless steel mirrors that have a custom coating structure of MgF2 Gold Ti onto the stainless steel substrate This configuration provides both high reflectivity in the infrared and chemical resistance to most all corrosive gases The cell includes Chemraz O rings are used in the following places window mounts objective mirrors window seals sight port cap and the top and bottom seals The IR beam input output windows are IR Quartz for high IR transmission The 4Runner gas cell is mounted on a p
24. iagram Purge Gas In Process Gas In Process Gas Out Maintenance Valve Purifier Permeation Box Gas Cel Nitrogen Outflow t Check Valve 7 Pressure Flow SS z EN Transfer Optics Z 3 GasFlow DA Pressure Flow ED S N Spectrometer ENE EWE Nitrogen Dutflow 3 2 EPITORR System Operational Modes The EPITORR system takes advantage of the built in security features that Windows XP offers These features allow one to set an account that will run the system in Operational Mode and another account for system Maintenance Mode By logging on in the Operational account the EPITORR system starts automatically and when the EPITORR system is closed it automatically logs off from the Operational account session The Maintenance account for the EPITORR system allows access to all the EPITORR system configuration features The EPITORR system does not start automatically every time the user logs on in the Maintenance account The Maintenance account provides access to the Windows XP standard desktop from which the EPITORR system can be accessed or updated The user can run the EPITORR System by double clicking on the IRGAS icon on the Window s screen 3 3 Bomem WorkIR FTIR Spectrometer The Bomem WorkIR FTIR spectrometer was c
25. l implied warranties of merchantability and fitness for a particular purpose CIC Photonics Inc does not warrant guarantee or make any representations regarding the use or the results of the use of any software or written materials in terms of correctness accuracy reliability currentness or otherwise CIC Photonics Inc shall not be liable for errors or omissions contained in its software or manuals any interruptions of service loss of business or anticipatory profits and or for incidental or consequential damages in connection with the furnishing performance or use of these materials even if CIC Photonics Inc has been advised of the possibility of such damages All equipment software and manuals are sold as is The entire risk as to the results and performance of the equipment and software is assumed by the user Windows is a registered trademark of Microsoft Corporation Workir is a registered trademark of ABB Bomem Inc GRAMS is a registered trademark of Thermo Galactic IRGAS SPGAS and SpectraStream are registered trademarks of CIC Photonics Inc WARRANTY ON PRODUCTS I Il MI IV Since CIC Photonics builds its product to last we warrant them that way If you have a problem with our product within the first year of ownership or within the specified warranty on a specific product that is a result of a defect in workmanship or the wearing out of a component that should not wear out we shall fix it Pro
26. l system for the EPITORR is a standard 120 volt 6 amp system There are three separate switched and fused circuits for the system computer and heater for the gas cell The heater is a stand alone circuit with a 3 amp fuse the computer is a subcircuit 1 amp fuse off the main system fuse 2 amp The system switch turns on and off all components except for the gas cell heater A schematic of the electrical circuits is provided upon request 4 0 System Start up Operations 4 1 Purge Gas Flow and System Switches First start the flow of the ultra dry nitrogen purge gas through the spectrometer and transfer mirror optics and separately through the gas cell then turn on the system and computer switches Purging of the system requires a total of 10 slpm 5 slpm for the spectrometer and 5 slpm for the optical housing assembly Internally the EPITORR has two flow regulators calibrated to provide 5 slpm each at 30 psig Therefore the system requires a constant supply of ultra dry nitrogen at 30 psig at the purge inlet gas port In addition and separately the gas cell needs to be purged before and after any flow of process gases This is best achieved by connecting the process gas line to the process reactor manifold so that either ultra pure nitrogen or hydrogen can be applied as a purge gas 4 2 Temperature Controller and Gas Cell Heater We recommend using 50 C as the on going operational temperature for the gas cell during gas analyses and
27. long path gas cell it provides the direct interface with the reactant gas flows The 4Runner gas cell has a five year track record of high performance in the analysis of all electrical gases in applications all over the world The EPITORR is an industrial turnkey system that provides an automatic on line monitoring analytical tool for the detection of impurities in corrosive and non corrosive gases in real time The system is based on FTIR Spectroscopy and is controlled by SPGAS Specialty Gas Analysis Software which is a sophisticated software running on a personal computer A system architecture was designed to provide the integration and control of the hardware elements as well as the spectral analysis and chemometrics to determine the concentration of impurities in gases FTIR Spectroscopy offers the best characteristics to perform real time detection of moisture and other impurities that may be present in epitaxial reactors Since the infrared light detector is not in contact with the corrosive sample it is not affected and the instrument can therefore be set for a continuous operation and scanning of the sample The real time gas analysis is performed through an FTIR Spectrometer which contains a special gas sample compartment gas cell that is connected directly to a gas line that supplies the sample gas Since the spectrometer is connected directly to a computer see Figure 1 the spectrometer can be set to perform continuously an x num
28. nsor s prior written consent SECTION 3 TERM AND TERMINATION The effective date of this Agreement shall be the date last signed below This Agreement is for the life of the copyrights and trade secret rights to Licensed Products Licensee may terminate this Agreement upon giving written notice to Licensor of its intent to terminate within thirty 30 days and by returning all copies of the Licensed Product in any form within said thirty 30 days Licensor may terminate this License on ten 10 day s written notice for any material breach of this Agreement If a Maintenance Agreement has been purchased and is attached hereto for a period of one 1 year from the effective date of said Maintenance Agreement or until this Agreement is terminated whichever comes first Licensor will send updates and modifications to the Licensee s specified point of contact The Licensee point of contact is Name Address Contact Telephone FAX Maintenance Agreement has has not been purchased and is is not attached hereto SECTION 4 PROPRIETARY INFORMATION Restrictions on Disclosure Licensee acknowledges that the Licensed Products contain proprietary and Confidential Information of Licensor Licensee shall hold Confidential Information in confidence Licensee shall not permit Confidential Information or any part thereof to be disclosed through sale license transfer or otherwise to any third person other than to employees of Licens
29. of concentration and standard error numbers are listed The first set to the left are the concentration in ppb and its associated standard error from the long term or multiple scan collection of data The second set to the right presents the FCT fast concentration tracker results and associated standard error The FCT numbers are generated by SpectraStream from single scan data collection to provide the fast response early warning detection of changes in gas composition or impurity levels The associated standard errors are greater because fewer data points are used in the calculations These numbers are continuously updated as the SPGAS analyses proceeds Above the graphical display are one or more buttons for the selected calibration gases Touching one of these buttons brings up a display for that gas of both the multiple scan and the fast scan concentrations as a function of time One such display is shown in Figure 6 The solid curve presents the multiple scan results and the dashed curve presents the single scan results 4 6 System Tests There are two easy system tests that will reveal if the EPITORR is performing correctly Both are based upon displays of single beam background data curves One test determines if the movable mirrors in the optical transfer box actually move in and out of the IR beam as controlled by the SpectraStream module The second test determines if the nitrogen purging of the spectrometer and optics has reduced the
30. ority Licensor and Licensee acknowledge that the person signing this Agreement for each party has been properly authorized and empowered to enter into this Agreement Entire Agreement This Agreement constitutes the entire agreement between the parties in connection with the subject matter hereof and supersedes all prior and contemporaneous agreements understandings negotiations or discussions whether oral or written of the parties Applicable Law This Agreement shall be construed and interpreted under the laws of the State of New Mexico and the parties agree that any lawsuit instituted based on this Agreement shall be brought in Albuquerque New Mexico in a court of proper jurisdiction CIC Photonics Inc By Signed Richard T Meyer Name Title CEO amp President Title Date Date FOREWORD COPYRIGHT DISCLAIMER TRADEMARKS Thank you for purchasing a CICP Photonics gas analysis system We strive to build the best gas analyzers available and believe that you will be pleased with the performance of the IRGAS System Should you have any difficulties at all please call 505 343 1489 for technical assistance We should be able to help you immediately If you have any comments on this or any of our other products we would like to hear from you We can be reached at the address telephone numbers or e mail address as given below Thank you again for you business Richard T Meyer 505
31. rging may be required See Figure 9 5 0 Full System Operational Procedures 5 1 Gas Cell Purge The gas cell should have been purged with ultra pure nitrogen or hydrogen from the process tool manifold prior to and between the additions of the reactor treatment gases 5 2 Automated Data Collection and Display As indicated in the start up procedures once the system is turned on data collection begins immediately and continues to cycle between background data collection and sample data collection with a quantification analysis of absorbance performed for each complete cycle The absorbance data are then converted to concentrations via the HITRAN gas calibrations and the resulting concentration values are displayed on the screen as a function of absolute time The EPITORR is based upon the system operator being an active observer of the displays of gas concentrations to determine if departures from expected concentration levels occur Such departures may occur due to changes in the quality of the supply gases deterioration of inline gas purifiers leaks in the gas lines or gas manifold components degradation of seals in the process tool alterations in the operating performance of the process tool etc The EPITORR is also dependent on the system operator keeping an independent log of operational changes with the process tool as a function of absolute time this is necessary so that data archived by the EPITORR can be correlated at any later time
32. s that may be required for handling the process gas In addition a separate connection to a house supply of purified ultra dry nitrogen is required for purging the 4Runner gas cell between process gas samples and for recording background spectra 3 8 SPGAS System Management and Gas Quantification Software The complete version of CIC Photonics proprietary software SPGAS provides both system management of the hardware components and advanced gas quantification capability The version installed in the EPITORR requires some manual operations of the hardware components e g setting the temperature controller opening closing gas valves etc As stated above the SPGAS software for the EPITORR has HITRAN generated calibration data preinstalled for H2O CH4 HF and CO2 The installed reference calibrations for both species are 1 ppm Beer s Law is integrated to calculate all other concentrations for matching observed data with calculated data 3 9 SpectraStream Fast Response Software Module SpectraStream is a proprietary U S Patent Application Serial No 09 731 550 add on module to SPGAS It provides a fast response early warning indication of sudden changes within seconds in the composition of the streaming gas that might arise from supply gas purity variations system leakages process tool failures etc Use of SpectraStream requires the motorized transfer mirror assembly described above 3 10 Electrical Systems The electrica
33. st results There is a built in diagnostic to determine if the transfer mirrors in the gas cell purge box are functioning properly that is providing the movement in and out of the IR beam position This diagnostic is provided at the following location D IRGAS PurgeBoxDiagnostic exe 8 2 Telephone and Email Support Telephone technical support is available Monday through Friday 8 30 am to 5 30 pm U S Mountain Time by calling 505 343 1489 343 9520 or 343 9500 fax 509 479 2980 Inquiries may also be sent at anytime to jperez cicp com with copy to jgarcia cicp com 19 8 3 Trouble shooting 8 3 1 Gas Cell Degradation Mirrors Seals Windows The best way to track any degradation of the gas cell mirrors and windows is to keep a daily or weekly record of the energy throughput in a ratio measurement of the single beam magnitude for the IR beam through the empty cell a Sample reading compared to that for the IR beam bypassing the cell a Background reading When that ratio decreases to less than two thirds of the value recorded for the cell when brand new then there is some indication that either the windows are becoming coated or the mirror reflectivity is diminishing At that point fax or email your records to CIC Photonics for examination Occasional testing of the gas cell and plumbing lines with a helium leak detector will provide assurances that the VCR fittings and Chemraz O rings are intact Long term exposure of the
34. switches that are required for integrating the EPITORR with a user s test station all points of connection are labeled and include the following Electrical power connector 120 volts 6 amps three prong twist lock male System switch 2 amps flip switch Computer switch 1 amp flip switch Heater switch 3 amps flip switch Data terminal Ethernet 10 100 female plug Floppy disk port for transferring archiving data Nitrogen purge connector male VCR fitting to source of high purity N2 gas Process gas IN connector male VCR fitting to source of process gas Process gas OUT connector male VCR fitting to process gas exhaust Also mounted on the top panel are Two fans for exhausting cooling air from the internal volume Air filter washable for input of cooling air Touch screen monitor Gas cell temperature indicator controller 3 0 Description of Major Components 3 1 EPITORR System Overview A System Block Diagram is provided in Figure 3 As will be seen the use and operation of the EPITORR System are in general quite simple and easy to perform EPITORR offers a robust design and works under Microsoft s Windows XP professional Operating System The minimum requirements of the system are as follow SPGAS Minimum Hardware Requirements Pentium or AMD 133 Mhz 64 MB Ram One ISA slot free 100 MB of free hard drive space Software Requirements e Windows XP Professional Figure 3 EPITORR System Block D
35. ted with a combination of three fuses 1 2 and 3 amp If any of these fail a thorough check of the associated circuit should be conducted 8 3 7 Vibration and Shock Isolators The internal instrument package CPU and nitrogen purifier are mounted within the system enclosure by means of a vibration and shock isolator assembly The top panel may be removed to inspect the inside if there is any indication that some component may have come loose Call for technical support if that occurs 8 4 Removal of Gas Cell for Warranty Repair Should it become necessary to return the gas cell due to degradation of mirrors windows or seals please call technical support for instructions The gas cell can be removed and returned without having to return the entire IRGAS system In brief what is involved is 1 flushing the cell well with purge nitrogen 2 removing the blue anodized cover box which encloses the gas cell 3 disconnecting the VCR fittings and capping them 4 disconnecting the optical couplers at the purge box and 5 lifting the cell off the spectrometer and out of the system enclosure Then special packing and shipping procedures are to be followed 21
36. tion of its moisture dry status Actual testing has shown that the system will maintain its dry condition for up to an hour or longer In most cases this is long enough to move the system from one process line to another and to reconnect the system for application 3 5 Temperature Controller The 4Runner cell body is controlled with a 1 16 DIN Microprocessor Based Auto Tuning Controller It drives a sheet heater with an imbedded Type K thermocouple that is mounted cylindrically on the cell body The temperature setting is manually adjustable with touch switches on the face of the controller The preset readout is in C Normal operating temperature range is ambient to 200 C Warning The Chemraz O rings are only rated to 260 C for continuous use Always operate the temperature controller in the auto tune mode with a preset temperature maximum that ensures that the temperature does not exceed the safe limit for the heater and the O rings A brief description of the operation of the controller is included in the 4Runner User s Guide and a complete User s Manual is provided 3 6 CPU and Touch screen Monitor The CPU is located inside the touch screen monitor An electronic cable connects it to the touch screen monitor which is mounted on the top lid but can removed to the top panel for easier use These units function in the same general manner as most PCs The installed operating system is Microsoft XP professional The CPU has be
37. urge box containing a two position transfer mirror assembly The transfer mirrors are moved in and out of the IR beam by means of an electronically driven motor and gear drive When the mirrors are aligned with the IR beam the IR beam is transferred into and out of the gas cell through the IR Quartz windows When the mirrors are moved out of the IR beam a wire mesh filter moves into the beam to prevent saturation of the InAs detector The cycling of the mirrors is controlled by the SPGAS SpectraStream software program The 4Runner is optically coupled to the WorkIR using the optical housings provide with the spectrometer This assembly of components is enclosed in a blue anodized aluminum Permeation Cover The permeation cover and its volume are flushed continuously with the purge nitrogen that escapes from the 4Runner purge box which significantly reduces and or eliminates air moisture permeation through the Chemraz O rings into the gas cell volume The WorkIR 4Runner purge box and optical housings and the permeation cover should be continuously purged with ultra dry nitrogen at all times The 4Runner gas cell volume should also be continuously purged when not being used to measure a process gas stream Once the EPITORR System has been conditioned with ultra dry nitrogen purging the system can subsequently be closed off from the sample and purge gas supply lines and transported to another in plant location without significant deteriora

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