Background Statement for SEMI Draft Document 5492

Background Statement for SEMI Draft Document 5492

New Standard: GUIDE FOR ETHYLENE GLYCOL

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.

Introduction

Recent progress in semi-conductor manufacturing technology has led to the introduction of a broad range of solvents into wet processing. Therefore, there are now solvents currently being used for which there are no SEMI guides or standards.

The Solvents in Advanced Processes Task Force held its first meeting in Berlin in 2009 to identify new solvents currently being used and to draft guides for these solvents.

Steps taken

With input from ITRS representatives, semiconductor manufacturers and solvents producers The Solvents in Advanced Processes Task Force initially examined which solvents are currently being used, for which there are no SEMI guides. The task force also examined the properties of these solvents that are important for the process and whether these could be included in a guideline. The Solvents in Advanced Processes Task Force then selected a couple of solvents to focus on initially with the aim of producing guides. Ethylene Glycol was identified as one of those solvents needing standardization. An initial draft of the guide was produced based on task force discussions. That draft is the subject of the current ballot.

Ballot Adjudication Information

This ballot and all responses to it will be adjudicated at the next meeting of the SEMI Standards Europe Gases and Liquid Chemicals Committee to be held in Grenoble, on Tuesday October 7th 2014, in conjunction with SEMICON Europe.

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SEMI Draft Document 5492

New Standard : GUIDE FOR ETHYLENE GLYCOL

1 Purpose

1.1 The purpose of this document is to providea guide for Ethylene Glycol for which a need has been identified.

2 Scope

2.1 The scope of this document covers grades of Ethylene Glycol which are used in the Semiconductor industry

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

4 Referenced Standards and Documents

4.1 SEMI Standards and Safety Guidelines

SEMI C1  Guide for the Analysis of Liquid Chemical.

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

5 Terminology

5.1 Acronyms

5.1.1 EG — Ethylene Glycol (IUPAC : Ethane-1,2-diol)

6 Properties

Table 1Properties of Ethylene Glycol

7 Suggested Values

7.1 The suggested values for Ethylene Glycolfor Tier A and B are listed in Table 3.

8 Grade 1 Procedures

8.1 This section does not apply to this chemical

9 Grade 2 Procedures

9.1 This section does not apply to this chemical.

10 Grade 3 Procedures

10.1 This section does not apply to this chemical.

11 Grade 4 Procedures

11.1 This section does not apply to this chemical.

12 Tier A Procedures

12.1 Standardized test methods are being developed for all parameters at the purity level indicated. Until standardized test methods are published, test methodology shall be determined by user and producer. The Global Liquid Chemicals Committee considers a method to be valid only if method validation according to SEMI C1 has been demonstrated

12.2 Assay

12.2.1 Analyse the sample by gas chromatography (see SEMI C1, in section “Assay by Wide Bore Column Gas Chromatography”). The parameters cited have given satisfactory results.

12.2.2 Column: 50 meter x 320 micron I.D. fused silica capillary coated with 100% dimethyl polysiloxane which has been surface bounded

12.2.3 Column temperature: 80°C isothermal for 3 minutes, then programmed to 260°C at 20°C/min, then isothermal for 5 minutes.

Table 2Chromatography Conditions

12.3 Color

12.3.1 Dilute 2.0 mL of Pt-Co stock solution (APHA 500, see SEMI C1) to 100 mL with DI water. Compare this standard (APHA 10) with 100 mL of sample in Nessler tubes. View vertically over a white background. The sample must be no darker than the standard.

12.4 Water

12.4.1 Analysis performed by coulometric Karl Fisher titration with the use of the appropriate anodic and cathodic coulometric reagents.

12.4.2 Prior to start the analysis, verify the cleanliness of the cell and prevent any exposure of the system to the humidity of the air.

12.4.3 Weigh accurately the sample volume (1.5 +/- 0.001 g) using an analytical balance.

12.4.4 Inject the sample through the septum and start the automatic titration till the equilibrium end-point.

12.5 Residue After Evaporation

12.5.1 Weigh accurately ~ 50 g of sample in a quartz crucible, evaporatecompletely under Nitrogen flow, cool in a desiccator, and weigh (see SEMI C1, Determination of Residue after Evaporation).

12.6 Acidity

12.6.1 To 50 grams of sample in a 250 mL conical flask, add 25 mL of methanol and 0.5 mL of phenolphthalein indicator solution (see SEMI C1). Titrate with 0.1 N methanolic sodium hydroxide solution until a slight pink color persists for at least 15 seconds.

ppm Acidity (CH3COOH) = Volume of NaOH (mL) x Normality of NaOH (mole/L) x 60,000

Mass of sample (g)

12.7 Chloride

12.7.1 The analysis is performed by Ion Chromatography equipped with a guard reversed phase cartridge, a guard column and followed by the analytical anion exchange solvent resistant column with a conductivity detector. The eluent is carbonate / bicarbonate solution. The sample is diluted with DI water (1:4) and the calibration is performed with a NIST traceable chloride standard in water

12.8 Trace metals analysis

12.8.1 The following method has given satisfactory results in determining trace metals impurities for the trace metals as specified using either Inductively coupled plasma optical emission spectroscopy (ICP-OES) or Inductively coupled plasma mass spectroscopy (ICP-MS). Arsenic can also be analyzed by Cold Vapor Atomic Absorption Spectrometry.

12.8.2 The sample preparation is performed by evaporation in a closed PTFE recipient under an inert gas stream.

12.8.3 20 grams of sample are weighed in the recipient and heated on a hot plate at 180°C till nearly dryness. The residue is digested with 2 mL of an HNO3/HCl (10:1) acid solution (hot plate 200°C) for a short amount of time then diluted with DI water and cooled down. To avoid mass interferences when using ICP-MS for determination, make sure to remove all excess Chloride during dissolution process.

12.8.4 It is recommended to run each sample in duplicate. In addition prepare a sample preparation blank for each analysis. It is also recommended to use an internal standard or a spiked sample solution to correct for any matrix effect.

12.9 Particles

12.9.1 Particle measurement method would typically be Optical Particle Counter (OPC).

13 Tier B Procedures

13.1 Assay – See § 12.1

13.2 Color – See § 12.2

13.3 Water – See § 12.3

13.4 Residue After Evaporation – See § 12.4

13.5 Acidity – See § 12.5

13.6 Chloride – See § 12.6

13.7 Trace metals analysis – See § 12.7

14 Tier C Procedures

14.1 This section does not apply to this chemical.

15 Tier D Procedures

15.1 This section does not apply to this chemical.

Table 3Suggested Values and Other Requirements for Ethylene Glycol

#1: bulk shipment – point of filling

NOTICE:SEMI makes no warranties or representations as to the suitability of the Standards and Safety Guidelines set forth herein for any particular application. The determination of the suitability of the Standard or Safety Guideline is solely the responsibility of the user. Users are cautioned to refer to manufacturer’s instructions, product labels, product data sheets, and other relevant literature, respecting any materials or equipment mentioned herein. Standards and Safety Guidelines are subject to change without notice.

By publication of this Standard or Safety Guideline, SEMI takes no position respecting the validity of any patent rights or copyrights asserted in connection with any items mentioned in this Standard or Safety Guideline. Users of this Standard or Safety Guideline are expressly advised that determination of any such patent rights or copyrights and the risk of infringement of such rights are entirely their own responsibility.

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.

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