24

Click here to load reader

downloads.semi.orgdownloads.semi.org/.../$FILE/5421A.docx · Web viewIt is the responsibility of the users of the Documents to establish appropriate safety and health practices, and

  • Upload
    lythuy

  • View
    213

  • Download
    0

Embed Size (px)

Citation preview

Page 1: downloads.semi.orgdownloads.semi.org/.../$FILE/5421A.docx · Web viewIt is the responsibility of the users of the Documents to establish appropriate safety and health practices, and

Background Statement for SEMI Draft Document 5421ANew Standard: TEST METHOD FOR PARTICLE REMOVAL PERFORMANCE OF LIQUID FILTER RATED BELOW 30 nm WITH ICP-MS

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 StatementThis document is an extension of Doc. 5297 (published as SEMI C82) which describes the test method for particle removal performance of liquid filter rated 20-50 nm with optical particle counter.

The test particle as tracer material is gold nanoparticle (GNP) certified as National Institute of Science and Technology (NIST) -Reference Material, as similarly used at SEMI C82 standard.

This document describes the test method for below 30 nm-rated filter mainly used for chemical filtration by using GNP and ICP-MS as particle concentration detector.

If you have any questions on this ballot, please contact the following Task Force leaders or SEMI Staff:

Liquid Filter Task Force co-leaders:

Takuya Nagafuchi (Nihon Entegris) at [email protected] Takehito Mizuno (Nihon Pall) at [email protected]

SEMI Staff :

Chie Yanagisawa (SEMI Japan) at [email protected]

The ballot results will be reviewed and adjudicated at the meetings indicated in the table below. Check www.semi.org/standards under Calendar of Events for the latest update.

Review and Adjudication InformationTask Force Review Committee Adjudication

Group: Liquid Filter TF Japan Liquid Chemicals CommitteeDate: Friday, Apr 11, 2014 Friday, Apr 11, 2014Time & Timezone: 14:00-15:00, Japan Time 15:00-17:00, Japan TimeLocation: SEMI Japan Office SEMI Japan OfficeCity, State/Country: Tokyo, Japan Tokyo, JapanLeader(s): Takuya Nagafuchi (Nihon Entegris)

Takehito Mizuno (Nihon Pall)Hiroshi Tomita (Toshiba)Hiroyuki Araki (Dainippon Screen Mfg.)

Standards Staff: Chie Yanagisawa (SEMI Japan)+81.3.3222.5863 / [email protected]

Chie Yanagisawa (SEMI Japan)+81.3.3222.5863 / [email protected]

Page 2: downloads.semi.orgdownloads.semi.org/.../$FILE/5421A.docx · Web viewIt is the responsibility of the users of the Documents to establish appropriate safety and health practices, and

The task force review meeting’s details are subject to change, and additional review sessions may be scheduled if necessary. Contact 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.

If you need a copy of the documents in order to cast a vote, please contact the following person within SEMI. Chie YanagisawaSEMI Standards, SEMI JapanTel: 81.3.3222.5863Email: [email protected]

Page 3: downloads.semi.orgdownloads.semi.org/.../$FILE/5421A.docx · Web viewIt is the responsibility of the users of the Documents to establish appropriate safety and health practices, and

DRAFTDocument Number:

Date: 5/6/23

SEMI Draft Document 5421ANew Standard: TEST METHOD FOR PARTICLE REMOVAL PERFORMANCE OF LIQUID FILTER RATED BELOW 30 nm WITH ICP-MS1 Purpose1.1 This document is to provide a standard of mono-dispersed gold nanoparticle (GNP) challenge test for liquid filter rated below 30 nm using ICP-MS.

2 Scope2.1 This document covers a mono-dispersed GNP challenge test method for below 30 nm rated liquid filter.

2.2 This document defines a test condition for mono-dispersed GNP challenge test.

2.3 The following areas are to be addressed in this document:

The test condition such as fluid, flow rate, pressure, GNP concentration, ligand concentration, membrane treatment etc.

The type of filter evaluated.

The type of gold nanoparticle (GNP)

The method of membrane treatment prior to the test for decreasing the adsorbing effect.

The description of the test result.

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 Limitations3.1 The test procedure is destructive; the filter cannot be returned into operation.

3.2 Fresh filter shall be used for this test procedure.

3.3 Material purity and potential leaching of dissolved contaminants are not addressed by this standard. SEMI F57 does not address this issue for final filters therefore the end user may decide to consider such testing when selecting different types of filters.

3.4 Test parameters affect the outcome of the test described in this standard, therefore test results are a qualitative rather than a quantitative of filter performance. This standard recommends testing filters under the conditions optimized in this standard and describe the conditions in test report.

3.5 Test shall be conducted as side by side comparison using more than one filter. Accordingly, the variability of the challenged particle in size is allowed in this test.

4 Referenced Standards and Documents4.1 SEMI Standards and Safety Guidelines

SEMI F110 — Test Method for Mono-dispersed Polystyrene Latex (PSL) Challenge of Liquid Filters

SEMI C79 — Guide to Evaluate the Efficacy of Sub-15 nm Filters Used in Ultrapure Water (UPW) Distributions Systems

SEMI C82 — Test Method for Particle Removal Performance of Liquid Filter Rated 20 – 50 nm with Liquid-Borne Particle Counter.

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

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 3 Doc. jn l SEMI

Semiconductor Equipment and Materials International3081 Zanker RoadSan Jose, CA 95134-2127Phone: 408.943.6900, Fax: 408.943.7943

Page 4: downloads.semi.orgdownloads.semi.org/.../$FILE/5421A.docx · Web viewIt is the responsibility of the users of the Documents to establish appropriate safety and health practices, and

DRAFTDocument Number:

Date: 5/6/23

5 Terminology5.1 Abbreviations and Acronyms

5.1.1 APD— 2-amino-2-hydroxymethyl-1,3-propanediol

5.1.2 DLS — dynamic light scattering

5.1.3 FM — flow meter

5.1.4 GNP — gold nanoparticle

5.1.5 ICP-MS — inductively coupled plasma – mass spectroscopy

5.1.6 LPM — liter per minute (L/min)

5.1.7 LRV — log reduction value

5.1.8 MSA — Mercaptosuccinic acid

5.1.9 NIST — National Institute of Standards and Technology

5.1.10 OPC — optical particle counter

5.1.11 P — pressure gauge

5.1.12 PSL — polystyrene latex

5.1.13 SAXS — small angle X-ray scattering

5.1.14 T — thermometer

5.1.15 UPW — ultrapure water

5.2 Definitions

5.2.1 background — the gold concentration when feeding the water without GNP.

5.2.2 challenge — the feed the water including GNP and ligand to test filter.

5.2.3 efficiency — particle removal efficiency of filter measured by this test method. It is the effectiveness of the filter in removing the particles, and is measured as (Upstream – Downstream)/Upstream × 100.

5.2.4 ligand — ion or molecule (chemicals) that could bind with the surface of gold nanoparticle.

5.2.5 log reduction value (LRV) — log reduction value of filter measured by test method. This is measured as logarithmic value of ratio of upstream to downstream particle counts.

6 Summary of Test Method6.1 This test method describes that test equipment and procedures for determining the particle removal efficiency of liquid filter (below 30 nm) with the water including ligand and GNP by calculating the difference of the number of challenged particle between upstream and downstream. The concentration of challenged GNP is measured with ICP-MS.

7 Apparatus7.1 Test Device

7.1.1 For this test method, use the schematic shown in Figure 1.

7.1.2 The standard test device shall consist of a pre-filter, flow meters, a particle and ligand injection device, static mixer, pressure gauges, a test filter, a particle counter, flow control valves, a resistivity sensor, a thermometer, and tubing connecting them.

7.1.3 The pore size of a pre-filter shall be equal to or smaller than the pore size of a test filter.

7.1.4 Use a flow meter with an allowable error to less than 5% full scale and of appropriate range.

7.1.5 Use a pressure gauge with an allowable error to less than 1% full scale and of appropriate range.

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 4 Doc. jn l SEMI

Semiconductor Equipment and Materials International3081 Zanker RoadSan Jose, CA 95134-2127Phone: 408.943.6900, Fax: 408.943.7943

Page 5: downloads.semi.orgdownloads.semi.org/.../$FILE/5421A.docx · Web viewIt is the responsibility of the users of the Documents to establish appropriate safety and health practices, and

DRAFTDocument Number:

Date: 5/6/23

7.1.6 Use a thermometer with an allowable error to less than 1% full scale and of appropriate range.

7.1.7 Use a tubing with an inner diameter that does not lead to significant pressure loss for the fluid medium used in the test.

Ligand GNP

T1 P1 P2

UPW

Prefilter

Test filter

FM

Static Mixer

Figure 1 Schematic of Typical Test Setup (Example)

7.2 Particle Injection Device

7.2.1 Use a particle injection device that can inject a particle at a constant flow rate without a pulsation.

7.3 Ligand Injection Device

7.3.1 Use a ligand injection device that can inject a ligand at a constant flow rate without a pulsation.

7.4 ICP-MS

7.4.1 Use an ICP-MS capable of detecting more than 0.1 ppb quantitative limit of gold.

7.4.2 Sample solution containing GNP shall be dissolved with aqua regia prior to injecting into ICP-MS.

8 Reagents and Materials8.1 Ultrapure Water (UPW)

8.1.1 Use the supply UPW with the resistivity more than 17MΩ・cm.

8.1.2 Temperature of the UPW shall be adjusted to 25±5 . ℃1: As some ligands or other surfactants are added to actual challenge solution, there is no need to adhere to the resistivity described in 8.1.1 at challenge test.

8.2 Gold nanoparticle (GNP)

8.2.1 Use the mono-dispersed GNP certified by NIST or the mono-dispersed NIST-traceable GNP.

8.2.2 The mono-dispersed GNP with below 30 nm of particle size is used.

2: In Appendix 2, the average particle size of NIST reference materials (RM) is described

8.3 Ligand

8.3.1 Use a ligand to make colloidal GNP stably disperse and decrease the interaction between GNP and filter media. (please see the Appendix 1)

9 Test Specimens9.1 Use a virgin liquid filter from rating below 30 nm.

9.2 Any size and type of filter, such as disk, capsule or cartridge, can be used in the test.

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 5 Doc. jn l SEMI

Semiconductor Equipment and Materials International3081 Zanker RoadSan Jose, CA 95134-2127Phone: 408.943.6900, Fax: 408.943.7943

Page 6: downloads.semi.orgdownloads.semi.org/.../$FILE/5421A.docx · Web viewIt is the responsibility of the users of the Documents to establish appropriate safety and health practices, and

DRAFTDocument Number:

Date: 5/6/23

10 Procedure 10.1 General Procedures

10.1.1 The filter is evaluated by the following procedures:

Testline background

Filter pretreatment and filter flushing

Background

Challenge

10.2 Testline background

10.2.1 Background testing is required for every test before installing the test filter into the test line (see Figure 1 or Figure 2).

10.2.2 Set the test condition (flow rate and pressure)

UPW (Resistivity: ≥17MΩ・cm, temperature: 25±5 )℃

FM

Choose either standard below:

1. Filter size standard: n L/min at 25.4*n mm-sized (n inch-sized) filter, (n=1,2,3,4,5….)

2. Filter media surface area standard: the flow rate to achieve the flux of >0.1 ml/min/cm2.

P2: ≥100 kPa

3: A downstream pressure of at least 100 kPa has to be maintained in order to eliminate air in the system.

10.2.3 Collect the test line water and measure gold concentration with ICP-MS.

10.2.4 Confirm the concentration becomes below detection limit, and record.

10.3 Filter Pretreatment

10.3.1 Pre-wetting is needed if the test filter is hydrophobic (Follow filter manufacturer's instructions).

10.3.2 Pretreatment fluid is aqueous solution of a ligand used at the challenge test. The concentration shall be same with the concentration at the challenge test. 

4: The condition of ligand concentration to achieve the lowest adsorbing effect depends on membrane type. Accordingly, it is necessary to optimize it in advance. Please see Appendix 1 in terms of how to set the ligand condition.

10.3.3 Fill the membrane pore with the pretreatment fluid by flowing after installing into the test line.

10.3.3.1 After ¶10.3.3, soak filters in the pretreatment fluid for a minimum of 30 min.

10.4 Background

10.4.1 Start UPW flow and ligand injection.

10.4.2 Close the air-vent valve after venting air from the filter upstream.

10.4.3 Set the test condition (flow rate and pressure).

UPW (Resistivity: ≥17MΩ・cm, temperature: 25±5 )℃

FM

Choose either standard below:

1. Filter size standard: n L/min at 25.4*n mm-sized (n inch-sized) filter, (n=1,2,3,4,5….)

2. Filter media surface area standard: the flow rate to achieve the flux of >0.1 ml/min/cm2.

P2: ≥100 kPa

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 6 Doc. jn l SEMI

Semiconductor Equipment and Materials International3081 Zanker RoadSan Jose, CA 95134-2127Phone: 408.943.6900, Fax: 408.943.7943

Page 7: downloads.semi.orgdownloads.semi.org/.../$FILE/5421A.docx · Web viewIt is the responsibility of the users of the Documents to establish appropriate safety and health practices, and

DRAFTDocument Number:

Date: 5/6/23

5: A downstream pressure of at least 100 kPa has to be maintained in order to eliminate air in the system.

10.4.4 Collect the downstream of the filter and measure gold concentration with ICP-MS

10.4.4.1 Record the concentration.

6: If the gold concentration does not become below detection limit, terminate the challenge test and re-check test line and other apparatuses. Then, restart the challenge test from 10.4.

10.5 Challenge

10.5.1 Prepare the challenge mono-dispersed GNP. When the challenge solution is diluted, it is necessary to use UPW characterized at 8.1 and agitate sufficiently. The prepared challenge solution shall be used in the test within 24h. Preferably, the particle size in the solution also should be evaluated with the instrument such as DLS, and SAXS in case the particle aggregation might occur. The purpose of this measurement is to confirm that no existence of large aggregated particle in the challenge solution. Large particles may affect removal efficiency of the tested filter, which may cause overestimate the removal capability of the filter. If obviously larger particles than estimated challenge particle size are observed, the challenge test shall be terminated.

10.5.2 Set the test condition (flow rate and pressure).

FM

Choose either standard below:

1. Filter size standard: n L/min at 25.4*n mm-sized (n inch-sized) filter, (n=1,2,3,4,5….)

2. Filter media surface area standard: the flow rate to achieve the flux of >0.1 ml/min/cm2.

P2: ≥100kPa

7: A downstream pressure of at least 100 kPa has to be maintained in order to eliminate air in the system.

10.5.3 Turn on the injection pump which delivers the challenge solution prepared at 10.5.1.

10.5.4 Begin injection at rate to achieve <100 ppb (calculated actual number diluted from the original GNP concentration).

8: The challenge level shall be defined in terms of the concentration at the filter after diluting in the main flow. Record downstream pressure reading.

10.5.5 Run test for achieving below the order of 1010 pcs/cm2 of the number of total challenged particle by tuning challenged GNP concentration and time. Table 1 summarizes examples of the testing condition.

Table 1 Examples of the test condition in terms of concentration filter surface area, and challenging time.GNP size (nm)

GNP concentration (ppb)

GNP particles (pcs/ml)

Flow rate (L/min)

Filter Surface area (cm2)

Time (min)

Accumulated challenge level (pcs/cm2)

Membrane coverage area (cm2)

Membrane Coverage rate(%)

20 10 7.0E+7 10 20,000 60 2.1E+9 131.9 0.710 5 2.9E+8 10 20,000 60 4.3E+9 67.2 0.3

10.5.5.1 Record particle levels in upstream and downstream each.

10.5.5.2 Monitor particle levels downstream of the filter.

10.5.6 Turn off injection pump.

10.5.7 Turn flow off at inlet valve.

10.5.8 Open drain and vent valves.

10.5.9 Remove test filter.

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 7 Doc. jn l SEMI

Semiconductor Equipment and Materials International3081 Zanker RoadSan Jose, CA 95134-2127Phone: 408.943.6900, Fax: 408.943.7943

Page 8: downloads.semi.orgdownloads.semi.org/.../$FILE/5421A.docx · Web viewIt is the responsibility of the users of the Documents to establish appropriate safety and health practices, and

DRAFTDocument Number:

Date: 5/6/23

11 Calculations11.1 Particle removal efficiency (%) and LRV are calculated using the average of the data points from last half for downstream levels and the measured upstream value.

% Efficiency = (Upstream – Downstream)/Upstream × 100% (1)

LRV = Log(Upstream/Downstream) (2)

12 Report 12.1 Include the system setup, which includes the particle data system settings.

12.2 Include calculated efficiencies and LRV, shown in Table 1 (sample data).

12.3 Report resistivity, temperature and flux.

Table 2 Sample Data Format (Example)

Filter / Filter size/ Lot number AAverage GNP size (nm) and Coefficient variation (-) 30, < 20%GNP manufacturer/ Lot number AGNP concentration (N/ml) 1E+8Water resistivity (MΩ) 18.2Water temperature (℃) 23Challenging time (min) 60Ligand / Ligand concentration (mmol/L) MSA / 0.3Main flow rate (L/min) 10Side flow rate (L/min) 0.1Flux (ml/min/cm2) 0.5ICP-MS manufacturer/ Model number ABackground Average (ppb) < DLUpstream Average (ppb) 50Downstream Average (ppb) 0.05Efficiency (%) 99.9LRV (-) 3

#1 Downstream values were calculated by averaging last half data recorded.

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 8 Doc. jn l SEMI

Semiconductor Equipment and Materials International3081 Zanker RoadSan Jose, CA 95134-2127Phone: 408.943.6900, Fax: 408.943.7943

Page 9: downloads.semi.orgdownloads.semi.org/.../$FILE/5421A.docx · Web viewIt is the responsibility of the users of the Documents to establish appropriate safety and health practices, and

DRAFTDocument Number:

Date: 5/6/23

APPENDIX 1Ligand additionNOTICE: The material in this Appendix is an official part of SEMI [designation number] and was approved by full letter ballot procedures on [A&R approval date].

A1-1 Purpose of ligand additionA1-1.1 As the GNP used in this standard has very small size, some disturbance such as concentration change, contamination of foreign object, and pH change could easily cause aggregation or sedimentation of GNP. Also, the interaction between GNP and filter media is extremely high and GNP could be adsorbed on the surface of filter media.

A1-1.2 In order to stabilize GNP colloidal system and prevent filter media from adsorbing GNP, it is preferable to use ligand technique. Precious metal like gold and platinum can bind with sulfur element and the molecule including amino group with a coordination bond 1) 2). Thus, the gold surface could be easily modified by molecules including thiol or amino functional groups.

A1-2 Polyethylene filterA1-2.1 For polyethylene filter, a branched or bulky ligand like Mercaptosuccinic acid (MSA) including carboxyl group could reduce adsorbing effect 3). Figure A1-1 shows the schematic drawing of atomic configuration of MSA molecule combing with GNP. GNP is entirely covered with MSA ligand by adding the ligand into GNP challenge solution, and the GNP covered with MSA is difficult to approach to filter media surface by steric effect. Furthermore, when the GNP challenge solution including MSA is injected into main line, it is expected that the colloidal system might be instable because MSA concentration is rapidly decreased. Therefore, previously adding MSA ligand into main line at upstream of GNP injection line.

A1-2.2 Also, p-mercaptobenzoic acid can be used as acting similar with MSA 3). Table A1-1 summarizes the representative ligands which have an ability to reduce adsorptive interaction between GNP and PE membrane.

Figure A1-1Schematic drawing of atomic configuration of MSA molecule combining with GNP. Sulfur element is

combined with gold element.

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 9 Doc. jn l SEMI

Semiconductor Equipment and Materials International3081 Zanker RoadSan Jose, CA 95134-2127Phone: 408.943.6900, Fax: 408.943.7943

Page 10: downloads.semi.orgdownloads.semi.org/.../$FILE/5421A.docx · Web viewIt is the responsibility of the users of the Documents to establish appropriate safety and health practices, and

DRAFTDocument Number:

Date: 5/6/23

Table A1-2 Representative ligands to have an ability to reduce adsorbing effect between GNP and polyethylene media.

Ligand

Mercaptosuccinic acid (MSA)

Mercaptobenzoic acid

A1-3 Nylon filterA1-3.1 As nylon molecular has an amide linkage with high positive polarity in the structure. It is well known that nylon could adsorb various colloidal particles dispersing in liquid because those particles are almost negatively charged in their surface. Studies show that the ligand with amino group, which directly combines with gold surface, has a repulsive force against nylon molecular structure 3). Below table A1-2 shows the ligand examples for nylon filter evaluation.

Table A1-1 Representative ligands to have an ability to reduce adsorbing effect between GNP and nylon media.

Ligand

2-amino-2-hydroxymethyl-1,3-propanediol (APD)

2-amino-2-methyl-1,3-propanediol

2-amino-2-methyl-1-propanol

2-amino-1,3-propanediol

3-amino-1,2-propanediol

(R)-(-)02-amino-1-propanol

(S)-(+)-2-amino-1-propanol

A1-4 PTFE filterA1-4.1 PTFE itself has lower surface tension and adsorbing capability; however, MSA ligand is suitable to reduce the interaction between GNP and PTFE media.

A1-5 Investigation of proper ligand concentrationA1-5.1 As described in this document, the ligand condition to achieve the lowest adsorbing effect is varied with membrane type. Though ligands probably some influence the membrane surface as well as challenge particle, it is uncertain that which parameter or property of membrane has an impact in regard to particle removal efficiency. However, it is supposed that pore size and surface etc. are key parameter in order to conduct at proper condition.

A1-5.2 Thus, it is necessary to examine proper condition in advance. Please refer to following example showing particle penetration ratio is varied with ligand concentration.

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 10 Doc. jn l SEMI

Semiconductor Equipment and Materials International3081 Zanker RoadSan Jose, CA 95134-2127Phone: 408.943.6900, Fax: 408.943.7943

Page 11: downloads.semi.orgdownloads.semi.org/.../$FILE/5421A.docx · Web viewIt is the responsibility of the users of the Documents to establish appropriate safety and health practices, and

DRAFTDocument Number:

Date: 5/6/23

A1-5.2.1 (Example 1)

A1-5.2.1.1 Filter type: Polyethylene Membrane sheet, 47 mm in diameter

A1-5.2.1.2 Challenge GNP specification : 10 nm – 2.9E+10 pcs/mL

A1-5.2.1.3 Ligand – MSA 0 – 1.0 mmol/L, MSA solution was added to GNP solution.

A1-5.2.1.4 Filtration was performed by challenging with GNP solution containing MSA after prewetting the membrane with Isopropyl alcohol at a flow rate of 5 mL/min. The schematic diagram of filtration equipment is shown in Figure A1-2. Figure A1-3 shows that the penetration ratio of 10 nm GNP through polyethylene membrane. The penetration ratio increased with an increase of MSA concentration. On the contrary, the gradual decrease of the penetration ratio was observed at more than 0.3 mmol/L of MSA concentration. In this case, around 0.2 mmol/L of MSA concentration is suitable to achieve the lowest adsorbing effect between GNP and membrane surface.

Figure A1-1 The schematic diagram of the filtration equipment installed with 47 mm in diameter disk membrane.

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 11 Doc. jn l SEMI

Semiconductor Equipment and Materials International3081 Zanker RoadSan Jose, CA 95134-2127Phone: 408.943.6900, Fax: 408.943.7943

Page 12: downloads.semi.orgdownloads.semi.org/.../$FILE/5421A.docx · Web viewIt is the responsibility of the users of the Documents to establish appropriate safety and health practices, and

DRAFTDocument Number:

Date: 5/6/23

Figure A1-2 The penetration ratio of 10 nm GNP through polyethylene membrane. At around 0.2 mmol/L of MSA

concentration, the highest penetration ratio could be observed.

A1-5.2.2 (Example 2)

A1-5.2.2.1 Filter type: Nylon6, 6 membrane sheet, 47 mm in diameter

A1-5.2.2.2 Challenge GNP specification : 5 nm – 2.5E+11 pcs/mL

A1-5.2.2.3 Ligand – APD 0 – 1.0 mmol/L, APD solution was added to GNP solution.

A1-5.2.2.4 Filtration was performed by challenging with GNP solution containing APD after prewetting the membrane with Isopropyl alcohol at a flow rate of 5 mL/min. Figure A1-4 shows that the penetration ratio of 5 nm GNP through nylon6,6 membrane. The penetration ratio was at constant at more than 0.05mmol/l of APD concentration.

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 12 Doc. jn l SEMI

Semiconductor Equipment and Materials International3081 Zanker RoadSan Jose, CA 95134-2127Phone: 408.943.6900, Fax: 408.943.7943

Page 13: downloads.semi.orgdownloads.semi.org/.../$FILE/5421A.docx · Web viewIt is the responsibility of the users of the Documents to establish appropriate safety and health practices, and

DRAFTDocument Number:

Date: 5/6/23

Figure A1-1 The penetration ratio of 5 nm GNP through nylon6,6 membrane.

A1-5.2.3 (Example 3)

A1-5.2.3.1 Filter type: PTFE membrane sheet, 47 mm in diameter

A1-5.2.3.2 Challenge GNP specification : 10 nm – 2.9E+9 pcs/mL

A1-5.2.3.3 Ligand – MSA 0 – 1.0 mmol/L, MSA solution was added to GNP solution.

A1-5.2.3.4 Filtration was performed by challenging with GNP solution containing MSA after prewetting the membrane with Isopropyl alcohol at a flow rate of 5 mL/min. Figure A1-5 shows that the penetration ratio of 5 nm GNP through PTFE membrane.

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 13 Doc. jn l SEMI

Semiconductor Equipment and Materials International3081 Zanker RoadSan Jose, CA 95134-2127Phone: 408.943.6900, Fax: 408.943.7943

Page 14: downloads.semi.orgdownloads.semi.org/.../$FILE/5421A.docx · Web viewIt is the responsibility of the users of the Documents to establish appropriate safety and health practices, and

DRAFTDocument Number:

Date: 5/6/23

Figure A1-1 The penetration ratio of 10 nm GNP through PTFE membrane.

A1-6 Filter pretreatment A1-6.1 Ligands shall be injected into UPW main line. It is expected to have an effect of filter pretreatment decreasing adsorbing effect before GNP challenge test. Also, stabilizing effect of GNP solution could be expected when injecting GNP into main line. Please refer to SEMI C82 for more information.

A1-7 Hydrodynamic diameter of GNP dispersed in challenge solutionA1-7.1 Figure A1-6 and A1-7 shows the hydrodynamic diameter of 30nm-GNP dispersed in the solution containing MSA and APD ligand, respectively. 1.0E+8 pcs/ml of GNP solution with a variety of MSA concentration were prepared, and the hydrodynamic diameter was measured with DLS.

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 14 Doc. jn l SEMI

Semiconductor Equipment and Materials International3081 Zanker RoadSan Jose, CA 95134-2127Phone: 408.943.6900, Fax: 408.943.7943

Page 15: downloads.semi.orgdownloads.semi.org/.../$FILE/5421A.docx · Web viewIt is the responsibility of the users of the Documents to establish appropriate safety and health practices, and

DRAFTDocument Number:

Date: 5/6/23

Figure A1-1

The hydrodynamic diameter of 30nm-GNP dispersed in MSA ligand solution with a variety of the ligand concentration.

Figure A1-2

The hydrodynamic diameter of 30nm-GNP dispersed in APD ligand solution with a variety of the ligand concentration.

A1-8 ReferencesA1-8.1 G. Schmid, “Nanoparticles – From Theory to Application”, Wiley-Vch Verlag GmbH & Co. KgaA (2004).

A1-8.2 G. T. Hermanson, “Bioconjugate Techniques”, Elsevier (2008).

A1-8.3 T. Mizuno et al., “A novel filter rating method using less than 30-nm gold nanoparticle and protective ligand”, IEEE/TSM, vol. 22, No. 4, (2009) 452-461.

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 15 Doc. jn l SEMI

Semiconductor Equipment and Materials International3081 Zanker RoadSan Jose, CA 95134-2127Phone: 408.943.6900, Fax: 408.943.7943

Page 16: downloads.semi.orgdownloads.semi.org/.../$FILE/5421A.docx · Web viewIt is the responsibility of the users of the Documents to establish appropriate safety and health practices, and

DRAFTDocument Number:

Date: 5/6/23

APPENDIX 2Particle size of NIST Reference MaterialNOTICE: The material in this Appendix is an official part of SEMI [designation number] and was approved by full letter ballot procedures on [A&R approval date].

A2-1 Particle size of NIST Reference Material (RM)A2-1.1 Table A2-1 and A2-2 summarize reference value mean size and expanded uncertainty of RM8011 and RM8012.

Table A2-1 Reference value mean size and expanded uncertainty of RM8011 (10 nm)Technique Analyte Form Mean Particle size

(nm)Expanded

UncertaintyAtomic Force Microscopy Dry, deposited on substrate 8.5 ± 0.3Scanning Electron Microscopy Dry, deposited on substrate 9.9 ± 0.1Transmission Electron Microscopy Dry, deposited on substrate 8.9 ± 0.1Differential Mobility Analysis Dry, aerosol 11.3 ± 0.1Dynamic Light Scattering Liquid suspension 13.5 ± 0.1Small-Angle X-ray Scattering Liquid suspension 9.1 ± 1.8

Table A2-2 Reference value mean size and expanded uncertainty of RM8012 (30 nm)Technique Analyte Form Mean Particle size

(nm)Expanded

UncertaintyAtomic Force Microscopy Dry, deposited on substrate 24.9 ± 1.1Scanning Electron Microscopy Dry, deposited on substrate 26.9 ± 0.1Transmission Electron Microscopy Dry, deposited on substrate 27.6 ± 2.1Differential Mobility Analysis Dry, aerosol 28.4 ± 1.1Dynamic Light Scattering173º scattering angle (backscatter)

Liquid suspension 28.6 ± 0.9

Dynamic Light Scattering90º scattering angle

Liquid suspension 26.5 ± 3.6

Small-Angle X-ray Scattering Liquid suspension 24.9 ± 1.2

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 16 Doc. jn l SEMI

Semiconductor Equipment and Materials International3081 Zanker RoadSan Jose, CA 95134-2127Phone: 408.943.6900, Fax: 408.943.7943

Page 17: downloads.semi.orgdownloads.semi.org/.../$FILE/5421A.docx · Web viewIt is the responsibility of the users of the Documents to establish appropriate safety and health practices, and

DRAFTDocument Number:

Date: 5/6/23

APPENDIX 3Actual filtration dataNOTICE: The material in this Appendix is an official part of SEMI [designation number] and was approved by full letter ballot procedures on [A&R approval date].

A3-1 Actual filtration dataA3-1.1 Actual filtration results are summarized in Table A3-1.

Table A3-1 Actual filtration result (Examples)

Filter / Filter size/ Lot number Polyethylene A / disk Nylon B / disk PTFE C / cartridgeAverage GNP size (nm) and coefficient variation (%)

10nm, < 10% 20nm, < 20% 20, < 20%

GNP manufacturer/ Lot number A A AGNP concentration (N/ml) 2.9E+9 3.5E+8 3.5E+7Water resistivity (MΩ) 18.2 18.2 18.2Water temperature (℃) 23 23 23Challenging time (min) 4 4 60Ligand / Ligand concentration (mmol/L) MSA / 0.5 APD / 1.0 MSA / 6.7E-3Main Flow rate 5 ml/min 5 ml/min 10 L/minSide flow rate - - 0.1 L/minFlux (ml/min/cm2) 0.5 0.5 0.5ICP-MS manufacturer/ Model number A A ABackground Average (ppb) < DL < DL < DLUpstream Average (ppb) 54.4 52.0 5.28Downstream Average (ppb) 3.0 0.021 0.008Efficiency (%) 94.5 > 99.9 99.8LRV (-) 1.3 > 3 2.3

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.

Page 17 Doc. jn l SEMI

Semiconductor Equipment and Materials International3081 Zanker RoadSan Jose, CA 95134-2127Phone: 408.943.6900, Fax: 408.943.7943