Background Statement for SEMI Draft Document 5621B

Background Statement for SEMI Draft Document 5621B NEW STANDARD: GUIDE FOR DETERMINING THE QUALITY OF ION EXCHANGE RESIN USED IN POLISH APPLICATIONS OF ULTRAPURE WATER SYSTEM

Notice: This background statement is not part of the balloted item. It is provided solely to assist the recipient in reaching an informed decision based on the rationale of the activity that preceded the creation of this Document.

Notice: Recipients of this Document are invited to submit, with their comments, notification of any relevant patented technology or copyrighted items of which they are aware and to provide supporting documentation. In this context, “patented technology” is defined as technology for which a patent has issued or has been applied for. In the latter case, only publicly available information on the contents of the patent application is to be provided.

Background Statement NOTE: We are answering all the rejects received for Document 5621A. There were many rejects and the majority of them are related, but none of them are technically persuasive. We are changing this document subtype to a Guide and not a Test Method standard because the industry is not familiar with the technique (LNS) that was used in the referenced method validation test for particle analysis at 10 nm. The previously published SEMI C79 has data verifying the accuracy of the LNS method.

Advanced semiconductor manufacturing is becoming more and more susceptible to particulate and organic contamination. Ultrapure water (UPW) piping and piping components undergo rigorous cleanliness testing using the SEMI F57 standard. While ion exchange (IX) resin has a similar surface area to that of the piping material, it is not tested for its contribution to UPW contamination. Ion exchange resin used in UPW Polish loops represents a similar source of contamination to piping materials due to its location in the water-purification process. Fresh ion exchange resin is known to produce significant amounts of contamination when loaded in polishers. Different resin suppliers provide different methods of resin preparation. Therefore, the absence of standardized testing and quality analyses poses the risk of inadequate resin quality. The value of the guide has become particularly important for the industry due to obvious limitations of the existing particle metrology for both UPW quality and wafer defect monitoring. Laser Particle Counters (LPCs) used in high volume semiconductor manufacturing have reached a practical measurement limit of 25 nm, with a counting efficiency of only a few percent at this size. However, even at 25 nm, the size detection is above the half pitch of current technology semiconductor devices, rendering the metrology unable to confirm the presence of potential “killer particles” at the required sizes. The size of the particles to be controlled in UPW is also approaching the capability of the filtration used. Lack of metrology capability, marginal filtration efficiency, and extremely high concentration of the particles shedding from the virgin IX resin (see Appendix 2) substantially increase the risk to the next generation of wafer manufacturing technology. UPW ITRS has suggested a risk-mitigation strategy based on reduction of the particle challenge to the final filters. This document describes a guide prepared to standardize the recommended conditions under which the ion exchange resin quality can be evaluated. It is important to emphasize that the methodology documented in the proposed guide has numerous limitations, described below. However, the task force believes that this guide, even with its limitations, can mitigate the risk of contamination from particle and other impurities. The purpose of this document is to standardize the resin test conditions to compare the performance of different resins. Use of this guide should generate more data to allow for revisions that will improve the method. Not having such a guide or having inadequate particle metrology poses significant risk to advanced semiconductor manufacturing (based on the information from ITRS and SEMETECH) Informational (Blue) Ballot1000AInformational (Blue) Ballot Ballot1000AInformational (Blue) (Blue) Informational Phone: 408.943.6900, Fax:408.943.6900, Phone:408.943.7943 CASan 95134-2127 Jose, 3081 Zanker Road Equipment Semiconductor InternationalMaterials and Standards Staff: Leader(s): State/Country:City, Location: Timezone:Time & Date: Group: Telephone and web information will be distributed to interested parties as the meeting date approaches. If you will you If approaches. necessary. date meeting the as parties interested if to distributed be will information web scheduled and Telephone be may sessions review additional and change, Standards for forcestaff leadersor confirmation. theContact task to subject are details meeting’s *This Information* Adjudication Review and 16nm for HP node Requirements Takeya Shimomura: J.Cepler, Kishimoto, “ Masahiro Aron Thomas Laursen, House, AbbasJohnKadaksham,Matt Report: Jae SEMATECH Lee, Arun Byunghoon Rastegar, Choi, Reference http://www.itrs.net/Links/2013ITRS/2013Chapters/2013Yield.pdf http://www.itrs.net/Links/2013ITRS/2013Tables/Yield_2013Tables.xlsx documents: ITRS References allowing technique. Technologies, accessibilitythis from to wider available Fluid Measurement commercially the type that clarify of to used alsotheIt important PSDSguidetesting is (LNS) in validation instrument now is emsin i rne t erdc ado itiue hs dcmn, i woe r i pr, ny wti h soe f EI nentoa Sadrs cmite (document committee Standards International SEMI of scope the within only part, in or whole in document, Guideline. this Safety or distribute Standard adopted or and/or official reproductiondevelopment) All and/oractivity. other theprior withoutconsent distribution SEMI written prohibited.ofis an reproduce as construed be to to is granted page this is on material No Permission program. Standards International SEMI the of Document Draft a is This contact please telephone/web, by participate to like would but person in meetings staff. Standards these attend to able be not [email protected] 408.943.7019 NA) Michael (SEMI Tran Liquide)Slava Libman(Air San Jose,USA / CA SpringNA Standards 2015Meetings the conjunction with in Headquarters SEMI PM2:00 PM 3:00 to Time) (Pacific Monday, March30,2015 IX TF Resin Task Force Review ”. SEMATECH Albany September”. Albany 2010 SEMATECH Page jn l jn 2 San Jose,USA / CA SpringNA Standards 2015Meetings the conjunction with in Headquarters SEMI PM2:00 PM 5:00 to Time) (Pacific March31,2015 Tuesday, ChapterNA TC Chemicals Liquid Committee Adjudication [email protected] 408.943.7019 NA) Michael (SEMI Tran Frank FlowersPeroxyChem / Frank ICL Parker/ EUV Mask and Blank Cleaning andBlankEUV Cleaning Mask Document Number: Document Doc. Date: 5621A 5/18/2018

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LETTER (YELLOW) BALLOT Informational (Blue) Ballot1000AInformational (Blue) Ballot Ballot1000AInformational (Blue) (Blue) Informational Phone: 408.943.6900, Fax:408.943.6900, Phone:408.943.7943 CASan 95134-2127 Jose, 3081 Zanker Road Equipment Semiconductor InternationalMaterials and 2.5 manufacturers. of the resin manufacturing processes 2.4 content. residue), andbeads broken (non-volatile evaporation include 2.3 needs.specific user- the on based user end the by determined be to expected are criteria quality the However guide. this following 2.2 2.1 2 full-scale applications. guide of resultsbe(polish) should tanks.representative The 1.3 resin of fromonthe contamination manufacturingprocess. will that the effect conditions minimize 1.2 SEMI in found be can systems F61. UPW regarding information Further applications. polish (UPW) Water Ultrapure 1.1 1 WATER SYSTEM APPLICATIONS OF ULTRAPUREUSED RESIN POLISH IN EXCHANGE DETERMINING OFSTANDARD: ION GUIDE FOR NEW QUALITY THE Draft Document SEMI 5621B emsin i rne t erdc ado itiue hs dcmn, i woe r i pr, ny wti h soe f EI nentoa Sadrs cmite (document committee Standards International SEMI of scope the within only part, in or whole in document, Guideline. this Safety or distribute Standard adopted or and/or official reproductiondevelopment) All and/oractivity. other theprior withoutconsent distribution SEMI written prohibited.ofis an reproduce as construed be to to is granted page this is on material No Permission program. Standards International SEMI the of Document Draft a is This and practices, health and safety other of prior the limitations use. applicability regulatoryor to determine appropriate establish to Documents the of users the of responsibility the is It use. NOTICE: optional required and analyses conduct testing. whetherto which are determine 2.9 equipment. manufacturingtoolsancillary semiconductor in and 2.8 account into taken be the planning testing.when should conditions delivery and storage, life, shelf resin The tanks. beds mixed the in loaded 2.7 a sample usedanalysis. cationic), mixed (anionicis for and form mixed 2.6 estimatetime). the to rinse-up test for leach dynamic used the use be (otherwise established will been tests already has leach quality resin Static virgin baseline volume. when assurance flush quality rinse-up the estimate to used be will tests leach Dynamic needs. user end the by determined is test leach static a or test leach dynamic a either Choosing operation. bed mixed actual the mimicking to closer conditions provide methods test dynamic method; test leach-out dynamic a use to whether decide will user end the quality, resin determine to sufficient is method test leach-out static the Although conditions. Scope Purpose ec-u et mtos r eeecd wti ti ouet poie aus fr bt sai ad dynamic and static both for values provide document this within referenced are methods test Leach-out current the reflects and consideration into resin HPIX virgin of performance wetted-stream the takes guide The method this by assessed parameters quality The resin. HPIX virgin on focus to guide this of intent the is It obtained was data the resins; state-of-the-art of performance the of example an provides document The instructions virginHPIXsample documentand for handling This includes conditions. resin test exchange ion into loaded is it when resin new the of rinse-up prolonged avoid to is guide the of purpose The test and parameters defines document This UPW. in used resin exchange ion of analysis on focuses guide The in use for suitable resin (HPIX) exchange ion purity high virgin of analysis for guide a describes document This hs gie nlds rcmedd aayia tsigta h ed sr a efr; h ed sr should user end the perform; can user end the that testing analytical recommended includes guide This use for intended modules exchange ion (POU) Point-of-Use as well as resin HPIX virgin to applies guide This be to resin HPIX virgin the of representative is tested resin exchange ion virgin the that assumes guide The non- in supplied is resin the When document. this within test the for used is resin HPIX virgin mixed Only quantitative measures of particle contribution, metallic contribution, organics contribution, residue after residue contribution, organics contribution, metallic contribution, particle of measures quantitative SEMI Standards and Safety Guidelines do not purport to address all safety issues associated with their with associated issues safety all address to purport not do Guidelines Safety and Standards SEMI Page jn l jn 3 Document Number: Document Doc. Date: 5621A 5/18/2018

DRAFT  5621A SEMI  LETTER (YELLOW) BALLOT Informational (Blue) Ballot1000AInformational (Blue) Ballot Ballot1000AInformational (Blue) (Blue) Informational Phone: 408.943.6900, Fax:408.943.6900, Phone:408.943.7943 CASan 95134-2127 Jose, 3081 Zanker Road Equipment Semiconductor InternationalMaterials and 3.12 the resin criteriafor tested. user defining be byperformance to the mayconducted end when studies need 3.11 representative fully state-of-the-art resin. future for be 3.10 this considered in been document. treatmentnot have solvent orsystem different 3.9 stated. 3.8 resin quality.measure 3.7 analysis a quality of statistical the resin data. conducting by or supplier resin the with addressed be should inconsistency system. Resin UPW actual the in used resin the from 3.6 3.5 be onsite). vs.mixed bymanufacturer should for theapplication sameit(pre-mixed in done the way actual (mixed) is but document, this of 3.4 scope the beyond are handling onsite the bythe supplier or user.considered of effects The contaminants. add 3.3 the exceed may conditions method test less critical and used primaryother applications. of in resin beds needs mixed specified The tank). UPW the downstream (located only systems (UPW) 3.2 notguide. in components) and beds, included the piping piping are (ion exchange 3.1 3 emsin i rne t erdc ado itiue hs dcmn, i woe r i pr, ny wti h soe f EI nentoa Sadrs cmite (document committee Standards International SEMI of scope the within only part, in or whole in document, Guideline. this Safety or distribute Standard adopted or and/or official reproductiondevelopment) All and/oractivity. other theprior withoutconsent distribution SEMI written prohibited.ofis an reproduce as construed be to to is granted page this is on material No Permission program. Standards International SEMI the of Document Draft a is This forManufacturing Equipment —SafetySEMI S2 Semiconductor Guideline Semiconductor in Processing —GuideUltrapure Water Used SEMI F63 for used Semiconductor —GuideUltrapure Waterin Systems ProcessingSEMI F61 for SystemsDistribution Chemical Liquid and Water Ultrapure in Used Components and Materials Polymer for Specification — F57 SEMI Liquid and Water Ultrapure in Used Components of Evaluation SystemsChemical Distribution for Guide Method Test Particle — F104 SEMI Liquid ForPreparing Components —Practice Testing Chemical SEMI F40 ChemicalDistribution for for Assemblies and Subassemblies,and PipingSEMI E49—Guide HighUltrahigh Purity Performance, Final Purity 4.1 4 of publication bythe date this thecollected limited of amount document. data of fact the account into take should method the of choice the conditions, dynamic under performance resin the of analysis the for representative be may test leach static that suggested 2 Appendix in data Although operation. mixed Polish

Referenced DocumentsReferenced Limitations This guide application is limited to the ambient temperature UPW system. Other applications, such as Hot UPW as applications, such system.Other UPW ambient temperature the to limitedis guide application This otherwise unless +/-10% are etc.) concentration, rate, flow as (such guide the in used figures the in Tolerances to used techniques analytical the of accuracy the to limited is guide this by generated data the of accuracy The performance their in vary may guide this by specified conditions the under tested samples resin HPIX Virgin specifications. intendedsupersede guidenot to customer This is prepared be should sample The different. be to expected is lab the in mixed vs. resin pre-mixed of Performance may handling “as guidedesigned is theresin assessresinstate;onsite to an received” The in from contamination water ultrapure of system Polishing the in use for intended is guide the following by tested resin HPIX Virgin SEMI Standards SEMI This guide recommends a simplified option of the static leach test versus dynamic leach test, mimicking actual mimicking test, leach dynamic versus test leach static the of option simplified a recommends guide This reproducibility Additional guide. this of application in available currently are data and experience Limited not may and quality resin state-of-the-art 2014 for representative is 2 Appendix in provided data reference The This guide applies solely to virgin HPIX resin testing. Quality and performance of the associated equipment associated the of performance and Quality testing. resin HPIX virgin to solely applies guide This Page jn l jn 4 Document Number: Document Doc. Date: 5621A 5/18/2018

DRAFT  5621A SEMI  LETTER (YELLOW) BALLOT Informational (Blue) Ballot1000AInformational (Blue) Ballot Ballot1000AInformational (Blue) (Blue) Informational Phone: 408.943.6900, Fax:408.943.6900, Phone:408.943.7943 CASan 95134-2127 Jose, 3081 Zanker Road Equipment Semiconductor InternationalMaterials and 6.1.3 6.1.2 6.1.1 SEMIF61. in defined 6.1 1: NOTE 6 5.4 5.3 5.2 5.1 5 NOTICE: Semiconductors Roadmap (ITRS) for Technology International 4.3 Membrane Conductivity Detection and Oxidation Persulfate UV, by Water in Carbon Organic and Carbon, Inorganic Carbon, Total of Method Test Standard — D5904 ASTM High-Purity of Evaporation After Residue of Water Measurement On-line for Method Test Standard — D5544 ASTM Persulfate or (UV) Ultraviolet by Water Purity High Detection Both, and or Oxidation, Infrared in Carbon Inorganic and Organic, Total, — D4779 ASTM 4.2 emsin i rne t erdc ado itiue hs dcmn, i woe r i pr, ny wti h soe f EI nentoa Sadrs cmite (document committee Standards International SEMI of scope the within only part, in or whole in document, Guideline. this Safety or distribute Standard adopted or and/or official reproductiondevelopment) All and/oractivity. other theprior withoutconsent distribution SEMI written prohibited.ofis an reproduce as construed be to to is granted page this is on material No Permission program. Standards International SEMI the of Document Draft a is This 2 http://www.astm.org 1 6.1.16 6.1.15 6.1.14 6.1.13 6.1.12 6.1.11 6.1.10 6.1.9 Appendix) in 6.1.8 6.1.7 6.1.6 6.1.5 6.1.4

http://www.itrs.net/ Harbor International, Conshohocken, Drive,ASTM 100Barr West PAUSA; 610.832.9585, Fax: 610.832.9555, 19428-2959, Telephone: Terminology Units Abbreviations and Acronyms and Abbreviations onethousandth to a millionthor a ofmillimeter. aone meter, Micrometer is lengthequal of unit of 1kg. 1Lapproximately isto equals trillionorParts (ppt) where per ng/L, equivalent pg/mL 1kg. ng/mLμg/L, isto equals billion (ppb) Parts or where per 1Lapproximately equivalent 1kg. 1Lapproximately (ppm)mg/L, million equivalentParts μg/mL per is equals to or where DocumentsOther ASTM Standards HPW —High Purity Water HPW used —High Purity Resin Polish in orHPIX IonPOU Exchange —Differential Mobility AnalyzerDMA LPC —Laser Particle Counter LPC results see – Testing Validation the for used PSDA of (example System Sizing Nano-Particle Liquid — LNS —Liquid OrganicCarbon With DetectorLC-OCD Chromatography Roadmap ForSemiconductors Technology —International ITRS —Inductively MassICP-MS Plasma Coupled Spectrometry —High Volume ManufacturingHVM SEM — Scanning Electron Microscope —Scanning Electron SEM —PolyvinylidenePVDF Fluoride Distribution Analyzer —ParticlePSDA Size UsePOU –Point of —Perfluoroalkoxy PFA or Residue (alsoResidueRAE) AfterEvaporation called NVR —Nonvolatile —NonvolatileResidueNRM Monitor General termsGeneral for systems be in F61.UPW can found SEMI Unless otherwise indicated, all documents cited shall be theversions. latest published otherwise documents all cited be shall Unless indicated, 1

— General terms and acronyms used in this standard are listed below and may be may and below listed are standard this in used acronyms and terms General — Page jn l jn 5 2 Document Number: Document Doc. Date: 5621A 5/18/2018

DRAFT  5621A SEMI  LETTER (YELLOW) BALLOT Informational (Blue) Ballot1000AInformational (Blue) Ballot Ballot1000AInformational (Blue) (Blue) Informational Phone: 408.943.6900, Fax:408.943.6900, Phone:408.943.7943 CASan 95134-2127 Jose, 3081 Zanker Road Equipment Semiconductor InternationalMaterials and 6.2.4 piping, gauges, sample meters,regulators, ports, etc. resinincludes pressure valves, flow column, 6.2.3 by achieved be can Measurement Delta measurement. background average watersample. hadonthe same have their that matched responses twocalibratedanalyzers using an of use proper the allow to period background of steady-state test the during unstable too is concentration analyte inlet the when Useful column. resin the of outlet the and column a reached have 6.2.2 components cleaned and the through rinsed flows UPW (after when theequipmentcomponents. test contributions the Background UPW and from includes contamination). or skid containers test test leach static leach the dynamic in measured is Background others. and TOC, 6.2.1 6.2 6.1.18 6.1.17 emsin i rne t erdc ado itiue hs dcmn, i woe r i pr, ny wti h soe f EI nentoa Sadrs cmite (document committee Standards International SEMI of scope the within only part, in or whole in document, Guideline. this Safety or distribute Standard adopted or and/or official reproductiondevelopment) All and/oractivity. other theprior withoutconsent distribution SEMI written prohibited.ofis an reproduce as construed be to to is granted page this is on material No Permission program. Standards International SEMI the of Document Draft a is This Definition Virgin HPIX Resin HPIX Virgin Skid Test Leach Dynamic Measurement Delta Background UPW UPW —Ultra PureUPW Water OrganicCarbon —Total TOC 48" Long 48" 1" I.D. 1" — the contaminant concentrations in the test system reported by analyzers such as PSDA, NRM, PSDA, as such analyzers by reported system test the in concentrations contaminant the — Vent to Vent Vent to Vent — an unused highregenerated. has —anthat been exchange not unused ion resin quality drain drain — the UPW contaminant analyte concentration difference between the inlet of the resin the of inlet the between difference concentration analyte contaminant UPW the — General Test Schematic Diagram for DynamicGeneral for TestLeach Test Diagram Schematic flow rate - 420 + 20 mL/min 20 + 420 - rate flow P1 (see Figure 1) — the system providing resin-evaluation test analysis. The test skid test The analysis. test resin-evaluation providing system the — 1) Figure (see Total effluent Total _ P2 Figure 1 Figure UPW return or drain or return UPW Page Temp jn l jn 6 UPW Sizing/Counting Residue Monitor Residue Carbon Monitor Carbon Total Organic Total Non-volatile Monitor Particle UPW return or drain or return UPW Document Number: Document UPW return or drain or return UPW drain or return UPW Doc. UPW return or drain or return UPW Date: 5621A 5/18/2018

DRAFT  5621A SEMI  LETTER (YELLOW) BALLOT Informational (Blue) Ballot1000AInformational (Blue) Ballot Ballot1000AInformational (Blue) (Blue) Informational Phone: 408.943.6900, Fax:408.943.6900, Phone:408.943.7943 CASan 95134-2127 Jose, 3081 Zanker Road Equipment Semiconductor InternationalMaterials and enclosed ISO Class 7 (per current revision of ISO 14644, roughly equivalent to FED STD 209E Class 10,000), or 10,000), Class 209E STD FED to equivalent roughly 14644, ISO of revision current (per 7 Class ISO enclosed 7.6.6 2) Appendix A2-2, Figure (see expectations performance resin the by dictated are PSDA by measured levels particle 7.6.5 7.6.4 7.6.3 7.6.2 7.6.1 7.6 avoid gas to bubbles.testing 7.5 adequate that ensure 7.4 to skid test leach assemblingthe E49when system. SEMI within designingand recommendations dynamic the to source 7.3 leak and safety (for construction of materials prevention). the upon depends potential limit reduce pressure to psig) high 45 The – formation. (30 kPa micro-bubble 207-310 be should column the to side feed the on Pressure contamination. avoid to sidestream or downstream meters flow and gauges pressure the Install kPa). (172 psig 25 typically column, 7.2 theequipment. UPW theto and column system PFAanalytical connecting with tubing PVDF of made is column exchange ion The skid. the of configuration required the presents 1 Figure requirements. 7.1 7 emsin i rne t erdc ado itiue hs dcmn, i woe r i pr, ny wti h soe f EI nentoa Sadrs cmite (document committee Standards International SEMI of scope the within only part, in or whole in document, Guideline. this Safety or distribute Standard adopted or and/or official reproductiondevelopment) All and/oractivity. other theprior withoutconsent distribution SEMI written prohibited.ofis an reproduce as construed be to to is granted page this is on material No Permission program. Standards International SEMI the of Document Draft a is This 8.2.3 the drums. anddrip Allowtheoff water to storage. during transport 8.2.2 8.2.1 8.2 8.1 8 supply the theyinstrumentation enter lines. before gas prevent to skid test bubbles divert and capture to stand the test the in included be must Provisions separation. resin prevent to bottom the to vent and top the from be vertically must column exchange ion column the through flow UPW exchange Exception: formation. bubble ion and accumulation the Position entrapment. bubble limit to 7.6.8 frequency. and the manufacturers’ with procedures accordance while 7.6.7 user, end more the follow should by testing approved exacting more be requiring may users requirements. stringent testing End conditions environment. these clean the from of intent Deviation the testing. maintaining the during or system, test the of part any handling when better, or 7, Class ISO maintain to necessary procedures Follow environment. better,

Sample Recommendations Sample Dynamic LeachDynamic ConfigurationSkid Test The UPW should be in compliance with theminimum following with UPWbe compliance should in requirements:The during psig) (20 kPa 138 be should skid test leach dynamic the of downstream pressure operating Minimum thesystemlead test particle-backgroundcounts. high excessive to vibrationwhichProtect could from UPW the from paths flow wetted all in systems piping low-shedding low-TOC, low-particle, ultrapure, Use exchange ion the of downstream instruments the feed quality to sufficient F57 be should SEMI pressure operating meeting Minimum components, purity high of made be should skid test leach dynamic The To take a virgin resin samplethe endlocation,follow a this from user virgin resin To take the procedure: drums at consideration. exchange fromunder ion virginresin the representative batch sample Test a To ensure a stable background level, before beginning the test install and rinse the ion exchange column in an in column exchange ion the rinse and install test the beginning before level, background stable a ensure To ( particle/ml <1 level: background particle-concentration recommended Maximum 0.2ppb. < NVR: > 0.05 0.05 Doc.  m). Background m). Date: 5621A 5/18/2018

DRAFT  5621A SEMI  LETTER (YELLOW) BALLOT Informational (Blue) Ballot1000AInformational (Blue) Ballot Ballot1000AInformational (Blue) (Blue) Informational Phone: 408.943.6900, Fax:408.943.6900, Phone:408.943.7943 CASan 95134-2127 Jose, 3081 Zanker Road Equipment Semiconductor InternationalMaterials and 9.1.1 9.1 9 practices handling packaging of theand by resin in manufacturer accordance thewith typical processes. manufacturing sticker. shipment). Add “FRAGILE” 8.5 8.4 8.3 8.2.7.5 8.2.7.4 8.2.7.3 8.2.7.2 8.2.7.1 8.2.7 to drumresults. more in representative thanobtain one sample order 8.2.6.2 one sample. more test to may than need 8.2.6.1 8.2.6 8.2.5 should the particulates,outer lowgas qualifiedlower bags have permeability). for while be 8.2.4 emsin i rne t erdc ado itiue hs dcmn, i woe r i pr, ny wti h soe f EI nentoa Sadrs cmite (document committee Standards International SEMI of scope the within only part, in or whole in document, Guideline. this Safety or distribute Standard adopted or and/or official reproductiondevelopment) All and/oractivity. other theprior withoutconsent distribution SEMI written prohibited.ofis an reproduce as construed be to to is granted page this is on material No Permission program. Standards International SEMI the of Document Draft a is This from the tank being measured.concentration polish the for the particledilutes tanks additionalfrom out leach particle year aover spread is change-out the resin concentration If effluent. tank particle acceptable the estimate can user end the retention, particle some provide will 9.1.4 yields. decreasing thereby process, photolithography the disrupt as well as surfaces critical and devices contaminate can resin HPIX virgin the from UPW 9.1.3 The tanks. polish parallel the of one only in replaced tank with thefromvirginresin. TOC tanks dilutes additional the new is resin the if insignificant considered is ppb 9.1.2.1.1 UPW quality.final 9.1.2.1 or nitride silicon of (CVD) deposition thin deposition.other film vapor chemical (ALD), deposition layer atomic growth, epitaxial voltage, breakdown oxide gate resist, the of adhesion cleaning, mask and wafer uniformity, etching affects oxidation, silicon 9.1.2 exchangeapplications. used ion performance ofin polish typicalresins rangeof indicate the actual and polish exchange ion onthestudy benchmarking in 2arebased Appendix thein data 2.The Appendix design,results system provided and the contamination, to sensitivity process-specific the upon based requirements quality define NOTE 1: Test Methodology Test Leach-Out ParametersLeach-Out in week one exceed not (do delivery direct fast using lab the to ship and cooler a in sample resin the Place it resin protect during shipping. samplebubble to wrap in Wrap the bagthe bag. clean and prepared seal the resin a Place in This document does not provide specific quality requirements for leachable parameters. The end user must user end The parameters. leachable for requirements quality specific provide not does document This you open immediately the drum. resin Sample after insidedrum. open bags the the protective drum aand representative Open unopened from a resin drum. previously Take should bags inner (the packaging double-bagged Use shipping. and sampling resin the for bags clean Prepare Based upon the UPW particle concentration target (in particles perandthe that final (inthefilter particles assumption liter) upontheconcentrationtarget UPW particle Based by released Particles technology. and process manufacturing user’s end the to specific is size particle Critical causes compounds organic by Contamination release. particle and TOC for considerations criteria Success Loading virgin HPIX resin for applications with tight target levels for TOC and particles poses risk to the to risk poses particles and TOC for levels target tight with applications for resin HPIX virgin Loading the gentle resin motionUse avoidbeads. damaging to resin sampleambientcontamination. exposureof to Minimize the a test staticleach 1Lfor dynamic the test. resin leach a and 1Lsample of for Take resin approximatelythe upper layer. 5cm (2”)of Remove sample. fromwith to frombeing taken excessliquid ofthe the top prevent the sample drum Take to need may you used, be to resin the of amount total the of 10% < is drum single a in resin of amount the If you conditions, different under stored was or batches different from supplied is testing for prepared resin If Resin sample handlingResin and sample may impact test packaging submittedthe results. Samples for should standard testing reflect In HVM facility where a number of parallel polish mixed beds are used, TOC contribution of less than 0.3 than less of contribution TOC used, are beds mixed polish parallel of number a where facility HVM In Page jn l jn 8 Document Number: Document Doc. Date: 5621A 5/18/2018

DRAFT  5621A SEMI  LETTER (YELLOW) BALLOT Informational (Blue) Ballot1000AInformational (Blue) Ballot Ballot1000AInformational (Blue) (Blue) Informational Phone: 408.943.6900, Fax:408.943.6900, Phone:408.943.7943 CASan 95134-2127 Jose, 3081 Zanker Road Equipment Semiconductor InternationalMaterials and 9.3.2 9.3.1.6 9.3.1.5 9.3.1.4 9.3.1.3 9.3.1.2 9.3.1.1 9.3 95% andofbeads. > unbroken ofnon-crackedbeads contains >wholeresin 90% and 9.2.1.1 9.2.1 9.2 Appendix (per 2). Application stringent may of affect requirements andschedule cost. 2: NOTE practice. is it applications, 9.1.7 critical less For performance. class” in 2. “best 2 Appendix Appendix in indicated as limits, detection the below be to metals all with on used is extraction UPW that recommended based criteria quality using 9.1.6 critical and devices microelectronic etch or failure. orcorrode immediate device future during fabrication,causing surfaces and devices microelectronic of properties electrical the alter 9.1.5 emsin i rne t erdc ado itiue hs dcmn, i woe r i pr, ny wti h soe f EI nentoa Sadrs cmite (document committee Standards International SEMI of scope the within only part, in or whole in document, Guideline. this Safety or distribute Standard adopted or and/or official reproductiondevelopment) All and/oractivity. other theprior withoutconsent distribution SEMI written prohibited.ofis an reproduce as construed be to to is granted page this is on material No Permission program. Standards International SEMI the of Document Draft a is This of indicative not is and components and resin temperatures. service exchange ion for data comparable achieve to used is specification 9.4.2 between required. themay TOC be andfor the inlet outlet column measurement delta a period, test the during fluctuates level TOC UPW source the If testing. particle with 9.4.1.4 9.4.1.3 LC-OCD chromatogramshown Appendix of in the 2. example an concentrations. Referto high unusually 9.4.1.2 Nitrogen, Sulfur, Phosphorus,andtheirinclude in structures. Chlorine 9.4.1.1 to required be may LC-OCD, as such contaminants. organic the identificationofassess individual TOC, measuring than other Methods growth. bacterial increase the to of nutrient structure the on depend can compounds potential a is individual water ultrapure in compound organic Any the processes. manufacturing semiconductor the and of molecules, effects actual the but 0.5ppb < be should levels 9.4.1 9.4 requirements. user’s the end meet to levels particle bring to required UPW of volume the of indication an provides and mode flushing continuous NOTE 2: Particle Contribution Test Test Particle Contribution Parameters Other

The Dynamic Leach Test evaluates particle contribution performance of the virgin ion exchange resin in a in resin exchange ion virgin the of performance contribution particle evaluates Test Leach Dynamic The whole-bead areprovided estimatingcontent. recommendations following for the The industry common the on based period time acceptable maximum the considered is time rinse week One leach HCl an conduct should user end the contamination, metals to susceptible applications purity high For can contamination Metallic specifications. metal user end the upon depends also consideration leach Metal The temperature of virgin ion exchange resin during a static leach test should be 40 ± 3°C. A temperature A 3°C. ± 40 be should test leach static a during resin exchange ion virgin of temperature The TOC maximum materials; organic for method screening quality water common a is TOC of measurement The Organic Contamination Organic Use the dynamic leach test to evaluate the TOC rinse-up volume, this is effective when done in conjunction in done when effective is this volume, rinse-up TOC the evaluate to test leach dynamic the Use in present are that for virginion evaluate resinAppendix to using test 2data thequality, reference. staticleach exchange Use compounds those or compounds organic unusual either identify to LC-OCD Use also that compounds organic in contained Carbon organic the measure correctly must analyzer TOC The SEM Sample Grab PSDA Sample Grab LPC sample Grab mostNVR =In-situ particles) (if of NRM the In-situ PSDA isemployed: forThe testing. instruments following contribution UPW used the particle are the if tanks polish in use for acceptable considered is resin exchange ion virgin the content: bead Whole Using the performance quality criteria, “best in class” HPIX resin is recommended where tightest quality is required is quality tightest where recommended is resin HPIX class” in “best criteria, quality performance the Using If virgin resin the not HPIX does meet user requirements,end quality end should the the user consult resin supplier. Page jn l jn 9 Document Number: Document Doc. Date: 5621A 5/18/2018

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Broken Beads Beads Broken (B) (A) Using deionized water and a representative sample of the virgin HPIX resin, prepare four microscope slides. microscope four prepare resin, HPIX virgin the of sample representative a and water deionized Using in clogging cause and process handling or manufacturing resin the in problem a indicate may Beads Broken tested resin of liter per contamination of micrograms in contamination metallic of values measured Report the and UPW for 3°C ± 40 be should test leach static a during resin exchange ion of virgin of temperature The tests. staticleach UPW for or either acid the Use ( tested resin of liter per contamination of micrograms in TOC of values measured Report Metallic ContaminationTest is total counted as: of defined beads The number or to (equal fragments broken and beads, whole but cracked beads, perfect whole of number the Count susceptible metalcontamination. for to HCl awith test processes staticleach Use semiconductor all UPW awith for test applications. staticleach Use metals no test, leach static the UPW a In specifications. user’s end the to conform should resin HPIX Virgin samples resin virgin exchange ion for needed be may testing and specifications contamination Metallic Division of broken beads by a factor of 2 implies that the bead is split into two pieces and both are counted. Although counted. are both and pieces two into split is bead the that implies 2 of factor a by beads broken of Division The leachstatic test UPW HCl,even using or one a duration,has valuesof 15-hour limitations. The measured a using The leachstatic test UPW,even using one a15-hour limitations.The of duration, has values using staticmeasured a Results: and Calculation

% Whole = Number of Whole Perfect Beads × 100 / Total 100/ Beads WholeBeads WholeNumber of × Perfect = % % Cracked = Number of Cracked But Whole Beads × Whole Total But 100/ Beads Cracked NumberCracked Beads of % =  g/L) should be reported for all measured values of TOC. g/L) bemeasured all values should reported for Number of Broken Beads 2 Broken / Number of Page jn l jn 10 (1)

Document Number: Document Doc. (2)  Date: g/L). Detection g/L). 5621A (3) 5/18/2018

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DRAFT  5621A SEMI  LETTER (YELLOW) BALLOT Informational (Blue) Ballot1000AInformational (Blue) Ballot Ballot1000AInformational (Blue) (Blue) Informational Phone: 408.943.6900, Fax:408.943.6900, Phone:408.943.7943 CASan 95134-2127 Jose, 3081 Zanker Road Equipment Semiconductor InternationalMaterials and reclaim it; to prevent bubbles from being introduced, do not allow effluent to enter the on-line metrology. To avoid To metrology. on-line the enter to effluent allow not do introduced, being from bubbles prevent to it; reclaim 11.1.1.9 onthetapping walls). 11.1.1.8 FED to 10,000). 209EClass STD equivalent 11.1.1.7 skid test = NVR and PSDA for level) noise the background level. (at non-detect, Particles level. background skid test = TOC met. 11.1.1.6 11.1.1.5 put bed on-line. 3: NOTE 11.1.1.4 11.1.1.3 column §7for depth. See details. 11.1.1.2 11.1.1.1 of (seeAppendixan data). test 2for example resin 11.1.1 11.1 11 emsin i rne t erdc ado itiue hs dcmn, i woe r i pr, ny wti h soe f EI nentoa Sadrs cmite (document committee Standards International SEMI of scope the within only part, in or whole in document, Guideline. this Safety or distribute Standard adopted or and/or official reproductiondevelopment) All and/oractivity. other theprior withoutconsent distribution SEMI written prohibited.ofis an reproduce as construed be to to is granted page this is on material No Permission program. Standards International SEMI the of Document Draft a is This Background results. test the of values the than lower significantly should higher limits includedthe report. in thanvalues detection be or limits detection than less either be should 11.2.1.2 for and be qualified theto tests conducted. cleaned 11.2.1.1 11.2.1 11.2 beads.the resin 11.1.1.15 criteria. 11.1.1.14 data. TOC the incoming downstream the actual (instantaneous)from TOC 0.1 ppb,subtract ± than more by varies TOC incoming If ppb). 0.1 ± than more by vary not does TOC (incoming test the throughout 11.1.1.13 11.1.1.12 11.1.1.11 11.1.1.10 of andthe column. top bottom the from excess air while venting the top from the column fillSlowly valves. UPW the open slowly shock, hydraulic TestProcedure Dynamic Leach Leach Dynamic Static LeachStatic Preparations/Equipment: HPIX virgin the rinse to required time and volume UPW projected the determines test leach dynamic The If the polish tank is rinsed under lower flow than the normal operation flow, the particle level may increase once the once increase may level particle the flow, operation normal the than flow lower under rinsed is tank polish the If Container Material: High purity PFA to minimize background contamination. The container must be pre- be must container The contamination. background minimize to PFA purity High Material: Container by load you as (pack column the agitate not Do resin. the of slurry roughly make not 14644, do separation, ISO avoid of To revision current (per environment better, or 7 Class ISO an in column Pack are parameters required the all until column empty the through UPW running by baseline test a Establish TOC. NRM, Metrology: PSDA, tanks Representativeof0.049m/s full-scalepolish Hydraulic conditions: (20 gpm/ft §7.1. to refer Column Material: bed (4ft) cm 121.92 by diameter (1inch) cm 2.54 tank polish full-scale a represent dimensions Column Preparations/Equipment: The criteria for the qualification imply that all the parameters tested in the container filled with UPW with filled container the in tested parameters the all that imply qualification the for criteria The The linear log-log slope may change as the surface rinse mechanism can be replaced with diffusion out of out diffusion with replaced be can mechanism rinse surface the as change may slope log-log linear The success the achieve to taken time the extrapolate and regression linear log/log a Plot maintained Report: Prepare is background stable a provided data test the from values TOC background Subtract columnfrom TOC. collectNRM, UPW daysPSDA, Collection:data throughthree Run Data the and for measuring to and effluent. the flow 0.42LPM start Reduce to rate minutes. and thethree UPW 1LPM flush offlow for full theis water,increase column When Column pre-flush: Install the test column in the test apparatus (see Figure 1). Direct effluent to a drain or drain a to effluent Direct 1). Figure (see apparatus test the in column test the Install pre-flush: Column The Test Method Process Flow Process TestThe Method Figure 2 Figure Page jn l jn 12 Document Number: Document 2 ). ). Doc. Date: 5621A 5/18/2018

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Cracked Beads Perfect Beads Perfect Figure A1.2 Figure A1.1 Page jn l jn 16 Document Number: Document Doc. Date: 5621B 5/18/2018

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Resin Sample Resin

e l c i t r a P e v i t a l u m u C d e d d A n o i t a r t n e c n o C Average “ Cv (%)

1.9 ) m n 0 1 > L m / # ( Background Levels D A C B E F Spool” represents Spool” the resin with resin.test column no 1e+5 1e+6 1e+7 1e+8 1e+9 Cumulative Particle Concentration Measured in Dynamic LeachTest in Measured Dynamic Cumulative Particle Concentration 1 TOC (ppb) 13.6% 0.18 0.09 0.67 0.66 0.49 0.68 0.71 0.79 0.65 0.69 10 Flush Volume (liters UPW) FlushVolume Figure A2.1 Page jn l jn 18

NVR (ppt) NVR 9.5% 100 228 238 197 226 241 262 209 220 42 22 Document Number: Document Particles ≥ Particles nm 10 ≥ (#/ml) Spool ResinF ResinE ResinD ResinC ResinB ResinA 1000 2.60E+00 1.33E+00 1.31E+07 1.51E+07 1.14E+07 1.40E+07 1.40E+07 1.22E+07 1.20E+07 1.29E+07 Doc. 10.1% Date: 5621B 5/18/2018

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emsin i rne t erdc ado itiue hs dcmn, i woe r i pr, ny wti h soe f EI nentoa Sadrs cmite (document committee Standards International SEMI of scope the within only part, in or whole in document, Guideline. this Safety or distribute Standard adopted or and/or official reproductiondevelopment) All and/oractivity. other theprior withoutconsent distribution SEMI written prohibited.ofis an reproduce as construed be to to is granted page this is on material No Permission program. Standards International SEMI the of Document Draft a is This

) t p p ( e u d i s e r e l i t a l o v - n o N

Cumulative Particle Concentration Measured in Dynamic LeachTest in (linear coordinates) Measured Dynamic Cumulative ParticleConcentration

n o i t a r t n e c n o C e l c i t r a P e v i t a l u m u 1000 2000 3000 4000 5000 C

) m n 0 1 > L m / # ( 0 Non-volatile Residue Measured inNon-volatile (linear ResidueMeasured Dynamiccoordinates) LeachTest 1e+10 1e+6 1e+7 1e+8 1e+9 0 500 500 FlushVolume (liters) Flush Volume (liters UPW) Figure A2.2 Figure A2.3 Page jn l jn 19 1000 1000

1500 AveBackground Spool Resin F Resin E Resin D Resin C Resin B Resin A 1500 Ave. Background Ave. Spool F Resin E Resin D Resin C Resin B Resin A Resin Document Number: Document 2000 Doc. Date: 5621B 2000 5/18/2018

) t p p ( d e d d a e u d i s e r e l i t a l o v - n o N

) b p p ( C O T 100 10 Non-volatile Residue Measured in Dynamic LeachTest in (log-logNon-volatile coordinates) ResidueMeasured Dynamic 1 10 12 14 8 0 2 4 6 1 TOC Measured in (linear-log Measured Dynamic coordinates)TOC LeachTest 10 10 FlushVolume (Liters) Flush Volume (liters) Figure A2.5 Figure A2.4 Page jn l jn 20 100 100 Ave. Background Spool Resin F Resin E Resin D Resin C Resin B Resin A 1000 Document Number: Document Spool F Resin E Resin D Resin C Resin B Resin A Resin 1000 Doc. Date: 5621B 5/18/2018

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Sample ID Sample ) b p p ( d e d d a C O T Spool Unstable TOC values at the end of the experiments were due to the effect of the UPW temperature on the TOC the on temperature UPW the of effect the to due were experiments the of end the at values TOC Unstable D C A E B F 0.01 100 Dynamic LeachSummary 0.1 10 1 1 added (liters 1E+7/ml UPW) 1020 140 190 250 170 16 3 Particles ≥ Particles 10nm ≥ TOC Measured in (log-log Measured Dynamiccoordinates)TOC LeachTest added (liters added 1E+6/ml UPW) >2000 1100 900 820 760 50 40 10 FlushVolume (Liters) added (liters 500 ppt 500 Figure A2.6 UPW) 140 240 190 Page <1 <1 <1 2 jn l jn 21 NVR added (liters added 50 ppt 50 UPW) >2000 100 <10 <10 <10 300 160 NA 1 ppb added (liters UPW)(liters 205 215 140 <1 80 25 65 Document Number: Document TOC Spool F Resin E Resin D Resin C Resin B Resin A Resin 1000 added (liters 0.2 0.2 ppb Doc. >1800 >1800 >1800 >1800 UPW 1000 120 <1 Date: 5621B 5/18/2018

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rel. Signal Response 0,5 1,5 2,5 3,5 0 1 2 3 4

0 Balazs_130 Project:

-- OND -- UVD -- OCD --

Resin 14-00960 Resin 14-00958 Resin Resin 14-00944 Resin 14-00938 Resin Resin Lot CHS CHS Lot Resin 14-00943 Resin Bypass 50007 D E F B C A

Biopolymers 50

Building Blocks RetentionTime in Minutes LC-OCD ChromatogramLC-OCD LMW Acids Figure A1.1 Page 100 jn l jn

X3 Document Number: Document

Ammonium Doc. Date: 5621B 200 5/18/2018

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) L m / # ( n o i t a r t n e c n o C r e b m u N e v i t a l u m u C 1e+6 1e+7 1e+8 1e+9 Table A1.2 Table A1.2 10 Resin ID Blank D C A E B F Grab Sample Particle LeachAnalysis Particle Sample LNSGrab by Grab Sample Particle Leach Analysis byLNS Grab SampleParticleLeach ≥ ≥ 3052 10 nm 125 121 225 20 Cumulative Concentration 10 Cumulative x 31 87 65 Particle Diameter (nm) Diameter Particle Figure A1.3 Page jn l jn 30 25 ≥ ≥ 20 nm 40 92.6 30.0 18.0 11.6 2.7 9.7 4.5 50 6 (#/mL) ≥ ≥ 60 30 nm Blank Blank F Resin E Resin D Resin C Resin B Resin A Resin Number: Document 0.51 26.8 7.02 1.29 6.42 0.27 1.32 80 100 Doc. Date: 5621B 5/18/2018

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2.6 49 ± 49 5 ± 49 5 ± F 49 ± 5 ± 49 * <49 <49 <49 ND µm >1 >1

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