Background Statement for SEMI Draft Document 5621B

Semiconductor Equipment and Materials International

3081 Zanker Road

San Jose, CA 95134-2127

Phone: 408.943.6900, Fax: 408.943.7943

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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 guideshould 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)

This is a Draft Document of the SEMI International Standards program. No material on this page is to be construed as an official or adopted Standard or Safety Guideline. Permission is granted to reproduce and/or distribute this document, in whole or in part, only within the scope of SEMI International Standards committee (document development) activity. All other reproduction and/or distribution without the prior written consent of SEMI is prohibited.

Page 1Doc. 5621B SEMI

Semiconductor Equipment and Materials International

3081 Zanker Road

San Jose, CA 95134-2127

Phone: 408.943.6900, Fax: 408.943.7943

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It is also important to clarify that the type of the PSDS instrument (LNS) used in the guide validation testing is now commercially available from Fluid Measurement Technologies, allowing wider accessibility to this technique.

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Semiconductor Equipment and Materials International

3081 Zanker Road

San Jose, CA 95134-2127

Phone: 408.943.6900, Fax: 408.943.7943

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References

ITRS documents:

Page 1Doc. 5621B SEMI

Semiconductor Equipment and Materials International

3081 Zanker Road

San Jose, CA 95134-2127

Phone: 408.943.6900, Fax: 408.943.7943

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Reference SEMATECH Report: Abbas Rastegar, Arun John Kadaksham, Matt House, Byunghoon Lee, Jae Choi, Masahiro Kishimoto, Aron J. Cepler, Thomas Laursen, Takeya Shimomura: “EUV Mask and Blank Cleaning Requirements for 16 nm HP node”. SEMATECH Albany September 2010

Page 1Doc. 5621B SEMI

Semiconductor Equipment and Materials International

3081 Zanker Road

San Jose, CA95134-2127

Phone:408.943.6900, Fax: 408.943.7943

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Review and Adjudication Information*

Task Force Review / Committee Adjudication
Group: / IX Resin TF / NA Liquid Chemicals TC Chapter
Date: / Monday, March 30, 2015 / Tuesday, March 31, 2015
Time & Timezone: / 2:00 PM to 3:00 PM (Pacific Time) / 2:00 PM to 5:00 PM (Pacific Time)
Location: / SEMI Headquarters in conjunction with the NA Standards Spring 2015 Meetings / SEMI Headquarters in conjunction with the NA Standards Spring 2015 Meetings
City, State/Country: / San Jose, CA / USA / San Jose, CA / USA
Leader(s): / Slava Libman (Air Liquide) / Frank Parker / ICL
Frank Flowers / PeroxyChem
Standards Staff: / Michael Tran (SEMI NA)
408.943.7019
/ Michael Tran (SEMI NA)
408.943.7019

*This meeting’s details are subject to change, and additional review sessions may be scheduled if necessary. Contact the task force leaders or Standards staff for confirmation.

Telephone and web information will be distributed to interested parties as the meeting date approaches. If you will not be able to attend these meetings in person but would like to participate by telephone/web, please contact Standards staff.

SEMI Draft Document 5621B

NEW STANDARD: GUIDE FOR DETERMINING THE QUALITY OF ION EXCHANGE RESIN USED IN POLISH APPLICATIONS OF ULTRAPURE WATER SYSTEM

1 Purpose

1.1 This document describes a guide for analysis of virgin high purity ion exchange (HPIX) resin suitable for use in Ultrapure Water (UPW) polish applications. Further information regarding UPW systems can be found in SEMI F61.

1.2 The guide focuses on analysis of ion exchange resin used in UPW. This document defines parameters and test conditions that will minimize the effect of contamination from the resin on the manufacturing process.

1.3 The purpose of the guide is to avoid prolonged rinse-up of the new resin when it is loaded into ion exchange (polish) tanks. The guide results should be representative of full-scale applications.

2 Scope

2.1 This document includes instructions for virgin HPIX resin sample handling and test conditions.

2.2 The document provides an example of the performance of state-of-the-art resins; the data was obtained following this guide. However the quality criteria are expected to be determined by the end user based on the user-specific needs.

2.3 It is the intent of this guide to focus on virgin HPIX resin. The quality parameters assessed by this method include quantitative measures of particle contribution, metallic contribution, organics contribution, residue after evaporation (non-volatile residue), and broken beads content.

2.4 The guide takes the wetted-stream performance of virgin HPIX resin into consideration and reflects the current manufacturing processes of the resin manufacturers.

2.5 Leach-out test methods are referenced within this document provide values for both static and dynamic conditions. Although the static leach-out test method is sufficient to determine resin quality, the end user will decide whether to use a dynamic leach-out test method; dynamic test methods provide conditions closer to mimicking the actual mixed bed operation. Choosing either a dynamic leach test or a static leach test is determined by the end user needs. Dynamic leach tests will be used to estimate the rinse-up flush volume. Static leach tests will be used for quality assurance when baseline virgin resin quality has already been established (otherwise use the dynamic leach test to estimate the rinse-up time).

2.6 Only mixed virgin HPIX resin is used for the test within this document. When the resin is supplied in non-mixed form (anionic and cationic), a mixed sample is used for analysis.

2.7 The guide assumes that the virgin ion exchange resin tested is representative of the virgin HPIX resin to be loaded in the mixed beds tanks. The resin shelf life, storage, and delivery conditions should be taken into account when planning the testing.

2.8 This guide applies to virgin HPIX resin as well as Point-of-Use (POU) ion exchange modules intended for use in semiconductor manufacturing tools and ancillary equipment.

2.9 This guide includes recommended analytical testing that the end user can perform; the end user should determine which analyses are required and whether to conduct optional testing.

NOTICE:SEMI Standards and Safety Guidelines do not purport to address all safety issues associated with their use. It is the responsibility of the users of the Documents to establish appropriate safety and health practices, and determine the applicability of regulatory or other limitations prior to use.

3 Limitations

3.1 This guide applies solely to virgin HPIX resin testing. Quality and performance of the associated equipment (ion exchange beds, piping and piping components) are not included in the guide.

3.2 Virgin HPIX resin tested by following the guide is intended for use in the Polishing system of ultrapure water (UPW) systems only (located downstream the UPW tank). The specified test method conditions may exceed the needs of resin used in primary mixed beds and other less critical applications.

3.3 The guide is designed to assess contamination from the resin in an “as received” state; onsite resin handling may add contaminants. The effects of the onsite handling are beyond the scope of this document, but should be considered by the supplier or user.

3.4 Performance of pre-mixed resin vs. mixed in the lab is expected to be different. The sample should be prepared (mixed) in the same way it is done for the actual application (pre-mixed by manufacturer vs. mixed on site).

3.5 This guide is not intended to supersede customer specifications.

3.6 Virgin HPIX resin samples tested under the conditions specified by this guide may vary in their performance from the resin used in the actual UPW system. Resin inconsistency should be addressed with the resin supplier or by conducting a statistical analysis of the resin quality data.

3.7 The accuracy of the data generated by this guide is limited to the accuracy of the analytical techniques used to measure resin quality.

3.8 Tolerances in the figures used in the guide (such as flow rate, concentration, etc.) are +/-10% unless otherwise stated.

3.9 This guide application is limited to the ambient temperature UPW system. Other applications, such as Hot UPW system or different treatment solvent have not been considered in this document.

3.10 The reference data provided in Appendix 2 is representative for 2014 state-of-the-art resin quality and may not be fully representative for future state-of-the-art resin.

3.11 Limited experience and data are currently available in application of this guide. Additional reproducibility studies may need to be conducted by the end user when defining performance criteria for the resin tested.

3.12 This guide recommends a simplified option of the static leach test versus dynamic leach test, mimicking actual Polish mixed operation. Although data in Appendix 2 suggested that static leach test may be representative for the analysis of the resin performance under dynamic conditions, the choice of the method should take into account the fact of the limited amount of data collected by the date of publication of this document.

4 Referenced Documents

4.1 SEMI Standards

SEMI E49 —Guide for High Purity and Ultrahigh Purity Piping Performance, Subassemblies, and Final Assemblies

SEMI F40 — Practice For Preparing Liquid Chemical Distribution Components for Chemical Testing

SEMI F104 —Particle Test Method Guide for Evaluation of Components Used in Ultrapure Water and Liquid Chemical Distribution Systems

SEMI F57 — Specification for Polymer Materials and Components Used in Ultrapure Water and Liquid Chemical Distribution Systems

SEMI F61 — Guide for Ultrapure Water Systems used in Semiconductor Processing

SEMI F63 —Guide for Ultrapure Water Used in Semiconductor Processing

SEMI S2 — Safety Guideline for Semiconductor Manufacturing Equipment

4.2 ASTM Standards[1]

ASTM D4779 — Total, Organic, and Inorganic Carbon in High Purity Water by Ultraviolet (UV) or Persulfate Oxidation, or Both, and Infrared Detection

ASTM D5544 — Standard Test Method for On-line Measurement of Residue After Evaporation of High-Purity Water

ASTM D5904 — Standard Test Method of Total Carbon, Inorganic Carbon, and Organic Carbon in Water by UV, Persulfate Oxidation and Membrane Conductivity Detection

4.3 Other Documents

International Technology Roadmap for Semiconductors (ITRS)[2]

NOTICE: Unless otherwise indicated, all documents cited shall be the latest published versions.

5 Units

5.1 Parts per million (ppm) is equivalent to μg/mL or mg/L, where 1 L approximately equals 1 kg.

5.2 Parts per billion (ppb) is equivalent to ng/mL or μg/L, where 1 L approximately equals 1 kg.

5.3 Parts per trillion (ppt) is equivalent to pg/mL or ng/L, where 1 L approximately equals 1 kg.

5.4 Micrometer is a unit of length equal to one millionth of a meter, or one thousandth of a millimeter.

6 Terminology

NOTE 1:General terms for UPW systems can be found in SEMI F61.

6.1 Abbreviations and Acronyms—General terms and acronyms used in this standard are listed below and may be defined in SEMI F61.

6.1.1 DMA — Differential Mobility Analyzer

6.1.2 HPIX — High Purity Ion Exchange Resin used in Polish or POU

6.1.3 HPW — High Purity Water

6.1.4 HVM — High Volume Manufacturing

6.1.5 ICP-MS — Inductively Coupled Plasma Mass Spectrometry

6.1.6 ITRS — International Technology Roadmap For Semiconductors

6.1.7 LC-OCD— Liquid Chromatography With Organic Carbon Detector

6.1.8 LNS — Liquid Nano-Particle Sizing System (example of PSDA used for the Validation Testing – see results in Appendix)

6.1.9 LPC — Laser Particle Counter

6.1.10 NRM — Nonvolatile Residue Monitor

6.1.11 NVR — Nonvolatile Residue (also called Residue After Evaporation or RAE)

6.1.12 PFA —Perfluoroalkoxy

6.1.13 POU – Point of Use

6.1.14 PSDA — Particle Size Distribution Analyzer

6.1.15 PVDF —Polyvinylidene Fluoride

6.1.16 SEM — Scanning Electron Microscope

6.1.17 TOC — Total Organic Carbon

6.1.18 UPW — Ultra Pure Water

6.2 Definition

6.2.1 Background — the contaminant concentrations in the test system reported by analyzers such as PSDA, NRM, TOC, and others. Background is measured in the static leach test containers or when UPW flows through the dynamic leach test skid (after rinsed and cleaned components have reached a steady-state of background contamination). Background includes contributions from the UPW and the test equipment components.

6.2.2 Delta Measurement— the UPW contaminant analyte concentration difference between the inlet of the resin column and the outlet of the resin column. Useful when the inlet analyte concentration is too unstable during the test period to allow the proper use of an average background measurement. Delta Measurement can be achieved by using two calibrated analyzers that have had their responses matched on the same water sample.

6.2.3 Dynamic Leach Test Skid (see Figure 1) — the system providing resin-evaluation test analysis. The test skid includes piping, resin column, flow meters, pressure gauges, valves, regulators, sample ports, etc.

6.2.4 Virgin HPIX Resin — an unused high quality ion exchange resin that has not been regenerated.