International Standard Iso 14644-10:2013(E)

INTERNATIONAL ISO STANDARD 14644-10

First edition 2013-03-01

Cleanrooms and associated controlled environments — Part 10: Classification of surface cleanliness by chemical concentration

Salles propres et environnements maîtrisés apparentés — Partie 10: Classification de la propreté chimique des surfaces --``,`,,,,,,`,,,`,``,,`,,```,`,`-`-`,,`,,`,`,,`---

Reference number ISO 14644-10:2013(E)

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Contents Page

Foreword ...... iv 1 Scope ...... 1 2 Normative references ...... 1 3 Terms and definitions ...... 1 4 Classification ...... 2

controlled environments ...... 2 4.1 Principles for establishing classification of clean surfaces in cleanrooms ...... and 2 4.3 ISO-SCC designation ...... 4 4.24.4 ClassificationConverter for forsubstances surface cleanlinessinto surface by atomic chemical concentration concentration ...... 4 5 Measuring and monitoring the cleanliness of surfaces for chemical contamination and demonstration of compliance ...... 5 5.1 Criteria for good cleanliness assessment ...... 5 5.2 Documentation and reporting ...... 6 Annex A (informative) Conversion between different unit expressions of surface concentration for chemical substances ...... 8 Annex B (informative) Parameters influencing testing and interpretation of results ...... 15 Annex C (informative) Essential considerations for a good cleanliness assessment ...... 16 Annex D (informative) Methods for testing surface cleanliness by chemical concentration ...... 17 Annex E (informative) Test record documentation ...... 28 Bibliography ...... 29

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Foreword

ISO (the International Organization for Standardization) is a worldwide federation of national standards bodiescommittee (ISO hasmember been bodies).established The haswork the of rightpreparing to be International represented Standardson that committee. is normally International carried out through ISO technical committees. Each member body interested in a subject for which a technical

organizations, governmental and non-governmental, in liaison with ISO, also take part in the work. ISO collaborates closely with the International Electrotechnical Commission (IEC) on all matters of electrotechnical standardization. InternationalThe main task Standards of technical are drafted committees in accordance is to prepare with the International rules given inStandards. the ISO/IEC Draft Directives, International Part 2.

Standardscasting a vote. adopted by the technical committees are circulated to the member bodies for voting. Publication as an International Standard requires approval by at least 75 % of the member bodies

Attention is drawn to the possibility that some of the elements of this document may be the subject of patent rights. ISO shall not be held responsible for identifying any orCleanrooms all such patent and associated rights. controlled environments. ISO 14644-10 was prepared by Technical Committee ISO/TC 209, Cleanrooms and associated controlled environments: ISO 14644 consists of the following parts, under the general title — Part 1: Classification of air cleanliness by particle concentration --``,`,,,,,,`,,,`,``,,`,,```,`,`-`-`,,`,,`,`,,`--- — Part 2: Specifications for testing and monitoring to prove continued compliance with ISO 14644-1 — Part 3: Test methods — Part 4: Design, construction and start-up — Part 5: Operations — Part 6: Vocabulary — Part 7: Separative devices (clean air hoods, glove boxes, isolators, mini-environments) — Part 8: Classification of air cleanliness by chemical concentration (ACC) — Part 9: Classification of surface cleanliness by particle concentration — Part 10: Classification of surface cleanliness by chemical concentration The following part is under preparation: — Part 12: Classification of air cleanliness by nanoscale particle concentration

Cleaning of surfaces to achieve defined levels of cleanliness in terms of particle and chemical classifications will form the subject of a future Part 13.

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Cleanrooms and associated controlled environments — Part 10: Classification of surface cleanliness by chemical concentration

1 Scope This part of ISO 14644

particles). This part of ISO defines 14644 the is applicable classification to all system solid surfaces for cleanliness in cleanrooms of surfaces and associated in cleanrooms controlled with

regard to the presence of chemical compounds or elements (including molecules, ions, atoms and--``,`,,,,,,`,,,`,``,,`,,```,`,`-`-`,,`,,`,`,,`---

environments such as walls, ceilings, floors, working environment, tools, equipment and devices. interactionNOTE 1 Forbetween the purpose the contamination of this part of and ISO the 14644, surface. consideration is only given to the chemical characteristics of a particle. The physical properties of the particle are not considered and this part of ISO 14644 does not cover the

NOTE 2 This part of ISO 14644 does not include the contamination generation process and any time-dependent influences (deposition, sedimentation, ageing, etc.) or process-dependent activities such as transportation and handling. Neither does it include guidance on statistical quality control techniques to ensure compliance. 2 Normative references The following referenced documents are recommended for the application of this document. For dated

references, only the edition cited applies. For undated references, the latest edition of the referenced 1) documentISO 14644-1:— (includingCleanrooms any amendments) and associated applies. controlled environments — Part 1: Classification of air cleanliness by particle concentration , Cleanrooms and associated controlled environments — Part 6: Vocabulary

ISO 14644-6, 3 Terms and definitions ISO 14644-6

For3.1 the purposes of this document, the terms and definitions given in and the following apply. air cleanliness by chemical concentration ACC N 3) level, expressed as an ISO Class , which represents the maximum allowable concentration of a given chemical species or group of chemical species, expressed in grams per cubic metre (g/m Note3.2 1 to entry: This definition does not include macromolecules of biological origin, which are judged to be particles. contaminant category

on the surface of interest common name for a group of compounds with a specific and similar deleterious effect when deposited

1) To be published. (Revision of ISO 14644-1:1999.)

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3.3 chemical contamination

chemical3.4 (non-particulate) substances that can have a deleterious effect on the product, process or equipment solid surface

boundary3.5 between the solid phase and a second phase surface

boundary between two phases Note3.6 1 to entry: One of the phases is normally a solid phase and the other a gas, a liquid or another solid. surface cleanliness by chemical concentration SCC condition of a surface with respect to its chemical concentration

3.7 surface cleanliness by chemical concentration class NSCC common logarithm (to the base of 10) of the chemical concentration on a surface in grams per square metre (g/m2)

4 Classification

4.1 Principles for establishing classification of clean surfaces in cleanrooms and controlled environments

Classification shall be specified by use of a classification descriptor. This descriptor is designated “ISOconcentration-SCC” and of specifies chemicals the on maximum a surface as total calculated chemical using concentration Formula (1) permitted(given in 4.2) on and a surface expressed for anin g/mindividual2 chemical substance or group of substances. The classification2 of SCC is based upon the

. For calculation of the class, all other units shall be converted_atomic to g/m . In specific cases4.4. where low concentrations need to be specified, the maximum allowable concentration of chemicals on a surface 4.2may be Classification expressed in atoms for surface per square cleanliness centimetre, by ISO-SCC chemical concentration, using Formula (2) in

NSCC NSCC is the common logarithm index of concentration CSCC 2 The SCC class shall be designated by a classification number, , where , expressed in g/m . The SCC classN statementSCC. CSCC shall always be connected with ain chemical terms of substanceNSCC: or group of substances to which it is related. Intermediate concentrations may be specified, with 0,1 being the smallest permitted increment of is determined from Formula (1), 10NSCC CSCC = (1)

log NCSCCS= 10 CC .

CTherefore,SCC is expressed in g/m2. The measured chemical concentration on a surface shall not exceed the maximum , the maximum allowable concentrationCSCC of the specified chemical substance or group of substances, customer and supplier. allowable concentration of SCC, to satisfy the predetermined SCC that is agreed between the

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NSCC class numbers shall include the negative sign.

In all cases, 4.3). NOTE 12 AnFor SCC converting class number from gravimetricis only valid concentrationin connection with(g/m a2 descriptor (see 4.4. ) to numeric concentration (number of atoms, moleculesTable 1 and or Figureions per 1 unit area), see on a surface. further illustrate the ISO-SCC classification as a function of chemical concentration Note also the parameters listed in Annex B

Table that 1 — influence ISO-SCC classification.classes

ISO-SCC class Concentration Concentration Concentration (g/m2) 2) (ng/cm2) 0 100 106 109 (μg/cm 10 105 108 10−1 104 107 −1 10−2 103 106 −2 10−3 102 105 −3 10−4 101 104 −4 10−5 100 103 −5 10−6 10 102 −6 10−7 10−1 101 −7 10−8 10−2 100 −8 10 −9 10−3 10 −9

--``,`,,,,,,`,,,`,``,,`,,```,`,`-`-`,,`,,`,`,,`--- 10−10 10−4 10−1 −10 10−11 10−5 10−2 −11 −12 −6 −3 −12

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X1 +6 X2 X3

Key X1 surface mass concentration (g/m2) X2 2) X3 surface mass concentration (ng/cm2) surface mass concentration (μg/cm Y ISO-SCC class

Figure 1 — ISO-SCC classes as a function of concentration

4.3 ISO-SCC designation

or group of substances for which this class number is valid. The ISO-SCC descriptor is expressed in the Anformat SCC ISO-SCCclass number Class isN (onlyX valid inX isconnection a chemical with substance a descriptor or group that of includes chemical the substances. chemical substance

), where 2. This is within the class limit of 1E-6 g/m2 EXAMPLE 1 With an N-Methyl-2-pyrrolidone (NMP) sample, the measured value of chemical contamination on a surface was 9,8E-7 g/m for Class −6. The designation would be: “ISO-SCC Class −6 (NMP).” 2 of total organic compounds (TOC). This is within the class limit of 1E-4 g/m2 EXAMPLE 2 With an organic compound sample, the measured value was 6E-5 g/m for Class −4. The designation would be: “ISO-SCC Class −4 (TOC).” 4.4 Converter for substances into surface atomic concentration

2 Very low concentrations are usually measured in surface number concentrations in the units of number of molecules, atoms or ions per surface area [1/m ]. For classification purposes, these should be

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2]. This conversion is made using Formula (2): converted into surface mass concentrations in the unit mass per surface area [g/m MC()SCC_number CSCC = Na (2)

where

CSCC_number - 2]; is the surface number concentration = number of molecules, atoms or ions per sur CSCC face area [1/m 2];

Na is the surface mass concentration23 /mol];[g/m

M is Avogadro’s number [6,02 × 10

is the molar mass of atomic, molecular or ionic species [g/mol]. Figure A.4 in Annex A illustrates the relationship between chemical concentration on a surface (expressed in g/m2) and the atomic concentration on a surface (expressed in Foratoms/m information2 purposes,

) for typical substances. 5 Measuring and monitoring the cleanliness of surfaces for chemical contamination and demonstration of compliance

5.1 Criteria for good cleanliness assessment Figure D.2 in Annex D sampling and measuring methods. illustrates how to measure different types of contamination, showing differing

Tests performed to demonstrate compliance shall be conducted in a classified environment where the airborne chemical contaminant and the airborne particle contaminant levels do not negatively influence the classification. Suitable measurement methods and calibrated instruments shall be used for all tests. The environment,Additional test measurement essentials are methods discussed and instruments in Annex C shall beAnnex agreed D upon details between measurement customer methodsand supplier. for demonstrating compliance. , while

The list of typical measurement methods is not exhaustive. Alternative methods that produce results with comparable accuracy may be specified by agreement between customer and supplier. Measurement by different methods, even when those methods are correctly applied, may produce Repeated measurements are recommended as part of the statistical approach. --``,`,,,,,,`,,,`,``,,`,,```,`,`-`-`,,`,,`,`,,`--- different results of equal validity.

Figure D.4 in Annex D. Specific problems such as concentration spikes may occur when measuring high levels of cleanliness. Special quality control techniques will then be required, as explained in enhances chemical deposition onto surfaces. If the surface is neither conductive nor grounded or charge- Precautions should be taken to reduce electrostatic charge around the test zone, as electrostatic charge

neutralized, electrostatic charges might occur. Therefore, test results may vary. to Annex D. For typical methods of measurement for testing surface cleanliness by chemical concentration, refer

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5.2 Documentation and reporting

5.2.1 Principle

Complianceand conditions with of surfacemeasurement. cleanliness Details by chemicalfor demonstrating concentration compliance (SCC) class shall requirements, be agreed upon as specifiedbetween bycustomer the customer, and supplier is verified in advance. by performing measurements and by providing documentation of the results

5.2.2 Testing Tests performed to demonstrate compliance shall be conducted using suitable measurement methods together with calibrated instruments whenever possible. Measurement methods for demonstrating compliance are described in Annex D methods described is not exhaustive. The testing environment shall be agreed between customer and . The list of typical customer and supplier. supplier. Alternative methods of comparable accuracy also may be specified by agreement between

Measurement by different methods, even when correctly applied, may produce different results of equalRepeated validity. measurements are recommended. The testing environment should be agreed between customer and supplier.

5.2.3 Test report

Theshall resultsinclude fromas a minimum testing each the following: surface shall be recorded and submitted as a comprehensive report, together with a statement of compliance or non-compliance of the specified SCC class. The test report

a)b) name andof the address person of performing the testing the organization; test; c) measurement environment;

d)e) date,time oftime measurement; and duration of sampling;

f) number and year of publication of this part of ISO 14644, i.e. ISO 14644-10:2013 g) clear identification of the location of the surface measured and specific designations for coordinates of the surface, if applicable; N; h)i) surfaceacceptance cleanliness criteria byfor chemical the clean concentration surface if agreed class between with designation customer andexpressed supplier; as SCC class

j) specified measurement method(s), equipment resolution and detection limits; procedure (if agreed); k) details of the test procedure used, with any available data describing deviations from the test

l)m) identificationnumber of measurements of the instrument(s) performed; used and current calibration certificate(s);

performed; n) test results, including chemical concentration(s) data for given substances, for all measurements

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o) surface condition, i.e. after final cleaning, before or after packaging, with agreement on type and quality of packaging required. Annex E. Other variations of the An example of how this test report may be constructed can be found in test report which are agreeable to both the customer and supplier may be used. --``,`,,,,,,`,,,`,``,,`,,```,`,`-`-`,,`,,`,`,,`---

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Annex A (informative)

Conversion between different unit expressions of surface concentration for chemical substances

A.1 Principle In addition to the unit of surface mass concentration of g/m2 surface number concentration of an organic compound or a group of organics such as molecules/m2 , there2 exist several different units to express composing organic compound(s) under consideration. , based on a number of organic molecules, and atoms C/m , based on a number of atoms of carbon A.2 Examples Tables A.1 to A.3 illustrate how the different units of surface number concentrations (molecules/m2 or atoms C/m2) can be converted into surface mass concentrations Forin terms information of carbon purposes, (g C/m2 ) or whole compound (g/m2

) respectively using the examples of heptane, hexadecaneTable A.1 and— Illustration di (2-ethylhexyl) of the phthalate. relationship between unit of surface concentration [g/m2] and surface number concentration [molecules/m2, atoms C/m2] for heptane (C7H16), CAS No. 142-82-5

Symbol Unit M = 100,2, Nc = 7 Example 1 Example 2 Example 3 Example 4 Surface number molecular Cmolecule 2] concentration --``,`,,,,,,`,,,`,``,,`,,```,`,`-`-`,,`,,`,`,,`--- Surface number concentra- [molecules/m 1,00E+19 1,42E+18 7,16E+16 6,01E+16 2] tion in terms of carbon Ccarbon_number Surface mass concentration [atoms C/m 7,00E+19 1,00E+19 5,00E+17 4,19E+17 2] in terms of carbon Ccarbon_mass

Surface mass concentration CSCC [g C/m2] 1,39E-3 1,98E-4 1,00E-4 8,39E-6

[g/m 1,66E-3 2,36E-4 1,19E-4 1,00E-6 Table A.2 — Illustration of the relationship between unit of surface concentration [g/m2] and surface number concentration [molecules/m2, atoms C/m2] for hexadecane (C17H34), CAS No. 544-76-3

Symbol Unit M = 226,4, Nc = 17 Example 1 Example 2 Example 3 Example 4 Surface number molecular 2] concentration Cmolecule Surface number concentra- [molecules/m 1,00E+19 6,20E+18 3,12E+16 2,60E+16 2] tion in terms of carbon Ccarbon_atom Surface mass concentration [atoms C/m 1,59E+20 1,00E+19 5,00E+17 4,20E+17 2] in terms of carbon Ccarbon_mass

Surface mass concentration CSCC [g C/m2] 3,19E-3 2,00E-4 1,00E-4 8,49E-6

[g/m 3,77E-3 2,35E-4 1,17E-4 1,00E-4

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Table A.3 — Illustration of the relationship between unit of surface concentration [g/m2] and surface number concentration [molecules/m2, atoms C/m2] for di (2-ethylhexyl) phthalate (C24H38O4), CAS No. 117-817-7

Symbol Unit M = 390,6, Nc = 24 Example 1 Example 2 Example 3 Example 4 Surface number molecular 2] concentration Cmolecule Surface number concentra- [molecules/m 1,00E+19 4,20E+18 2,00E+16 1,50E+16 2] tion in terms of carbon Ccarbon_atom Surface mass concentration [atoms C/m 2,39E+20 1,00E+19 4,89E+17 3,60E+17 2] in terms of carbon Ccarbon_mass

Surface mass concentration CSCC [g C/m2] 4,89E-3 2,04E-4 1,00E-4 7,37E-6

Each surface number concentration can[g/m be converted6,62E-3 to the original2,76E-4 surface1,35E-4 concentration1,00E-4 from Formulae (A.1) to (A.3):

22M[]gm/ ol CCSCCmgm// = olecule moleculesm ×     N molecules //mol a [] (A.1) --``,`,,,,,,`,,,`,``,,`,,```,`,`-`-`,,`,,`,`,,`---

C atoms Cm/ 2  2 carbon _atom   M[]gm/ ol CSCC gm/  = ×   N atoms Cm/ olecule N moleculesm/ ol c [ ]] a [] (A.2)

C [/g Cm2]  carbon _ mass  2  Mc [g /mol]  CSCC gm/  = × M [g /mol] (A.3)   Nc [atoms C/molecule] where

Nc is the number of carbon composing organic compound(s) under consideration; and

Mc is the molar mass of carbon.

Table A.4. The surface number concentration can be obtained fromSurface Formula number (A.4): concentration with different types of unit expression based on Langmuir–Blodgett (LB) film for typical organics is also listed in 2 13//23 CMSCCL_ Bagm/( = /)Nd (A.4)  

where d 3.

is the density of organic compound(s) in g/m

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Table A.4 — Monolayer concentration based on Langmuir–Blodgett film

7 16 17 34 phthalate (C O CAS No. 142-82-5 CAS No. 544-76-3 24 38 4 DiCAS (2-ethylhexyl) No. 117-817-7 Heptane (C H ), Hexadecane (C H ), H ), Surface number molecular concentration Surface number concentration 2,55E+18 1,62E+18 1,34E+18 in terms of carbon Surface mass concentration 1,79E+19 2,59E+19 3,21E+19 in terms of carbon Surface mass concentration 3,56E-4 5,18E-4 6,56E-4

Figures4,24E-4 A.1 to A.4 illustrate 6,10E-4how the different units8,88E-4 of surface number concentrations (molecules/m2 or atoms C/m2) can be converted into surface mass concentrations in termsFor information of carbon (g purposes, C/m2) or whole compound (g/m2

), respectively.

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Key X surface molecular concentration (molecules/m2 2)] Y surface mass concentration (g/m2 2)] ) [surface molecular concentration (molecules/cm ) [surface mass concentration (g/cm 1 heptane (C7 16 • surface concentration corresponding to monolayer based on LB model 2 hexadecane (C17 34 H ), CAS No. 142-82-5 3 24 38O4 H ), CAS No. 544-76-3 di (2-ethylhexyl) phthalate (C H ), CAS No. 117-817-7 Figure A.1 — The relationship between the units of surface mass concentration (g/m2) and surface molecular concentration (molecules/m2) for typical organics --``,`,,,,,,`,,,`,``,,`,,```,`,`-`-`,,`,,`,`,,`---

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Key X surface atomic concentration in terms of mass of carbon (grams C/m2 of mass of carbon (grams C/cm2)] Y surface concentration (g/m2 2)] ) [surface atomic concentration in terms

) [surface concentration (g/cm 1 heptane (C7 16 • surface concentration corresponding to monolayer based on LB model 2 hexadecane (C17 34 H ), CAS No. 142-82-5 3 24 38O4 H ), CAS No. 544-76-3 di (2-ethylhexyl) phthalate (C H ), CAS No. 117-817-7 Figure A.2 — The relationship between the units of surface concentration (g/m2) and surface atomic concentrations, in terms of mass of carbon (grams C/m2) for typical organics --``,`,,,,,,`,,,`,``,,`,,```,`,`-`-`,,`,,`,`,,`---

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Key X surface atomic concentration in terms of numbers of carbon (atoms C/m2 terms of numbers of carbon (atoms C/cm2)] Y surface concentration (g/m2 2)] ) [surface atomic concentration in

) [surface concentration (g/cm 1 heptane (C7 16 • surface concentration corresponding to monolayer based on LB model 2 hexadecane (C17 34 H ), CAS No. 142-82-5 3 24 38O4 H ), CAS No. 544-76-3 di (2-ethylhexyl) phthalate (C H ), CAS No. 117-817-7 Figure A.3 — The relationship between the units of surface concentration (g/m2) and surface atomic concentration, in terms of numbers of carbon (atoms C/m2) for typical organics

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Key X surface atomic concentration in terms of numbers of atoms (atoms/m2 terms of numbers of atoms (atoms/cm2)] Y surface concentration (g/m2 2)] ) [surface atomic concentration in 1 8 15 ) [surface concentration (g/cm 2 9 16 Li (M = 6,9) Ti (M = 47,8) Zn (M = 65,4) 3 10 17 B (M = 10,8) Cr (M = 52,0) As (M = 74,9) 4 11 18 Na (M = 23,0) Mn (M = 54,9) Sn (M = 118,7) 5 12 19 Mg (M = 24,3) Fe (M = 55,9) Ba (M = 137,33) 6 13 Al (M = 27,0) Co (M = 58,9) Pb (M = 207,2) 7 14 K (M = 39,1) Ni (M = 58,7) Ca (M = 40,1) Cu (M = 63,4) Figure A.4 — The relationship between the units of surface mass concentration (g/m2) and surface atomic concentration in terms of numbers of atoms (atoms/m2) for typical substances

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Annex B (informative)

Parameters influencing testing and interpretation of results

B.1 Parameters

Parametersa) skill level influencing of personnel testing doing and sampling interpretation or making of results the test; include the following:

b) reliability, repeatability and capability level of the testing laboratory; c)d) cleanliness level of samplepackaging vessels, used toolsfor shipping and test the equipment; samples;

samples (see Figure D.3 in Annex D); e) use of an agreed sampling, blank and error management procedure for collecting and measuring

f)g) openingunauthorized the sample opening outside of the a sample; controlled environment;

h) quality of chemical or water used to strip the chemical from its substrate; i) loss of analyte during sampling, shipping or testing; j) loss or change of analyte by desorption or thermal decomposition during test heating; l)k) failure errors toin continuallymeasuring recalibrateor calculating test the equipment sample area.or to investigate unusual data excursions (test spikes);

B.2 Considerations The list in B.1 is not comprehensive. --``,`,,,,,,`,,,`,``,,`,,```,`,`-`-`,,`,,`,`,,`---

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Annex C (informative)

Essential considerations for a good cleanliness assessment

C.1 Principle

the assessment: The following considerations should be established, agreed and managed before starting and during

a) surface wettability state, i.e. hydrophilic or hydrophobic; b) substance or group of substances used in the subject material; c)d) substance or group of substances ofused interest in the used maintenance in the subject process; process; e) substance or group of substances found in the outside and inside air;

f)g) existencesubstance of or a group general of chemical/molecularsubstances intended or to product-specific be measured; problem;

h)i) odournature, detection volume and during velocity sampling of the (Precautions air during sampling; should be taken to prevent inhalation.);

j) temperature, relative humidity and pressure levels during sampling; k)l) nanoparticle visualization measurementtest or an ACC priormeasurement to the SCC prior measurement; to the SCC measurement; m) cleaning substance or process used; n) expected level of the measurement result;

o)p) typepoint of of measurement interest representative instrument of needed; the entire sample; q) contamination from the outside environment; r) recontamination from the measurement process or instrument; s) restriction of electrostatic discharge and electrical transients at the measurement site;

t) measurement results within the specification of the classification; u) application of adequate quality control to the collection and measurement of data. C.2 Considerations --``,`,,,,,,`,,,`,``,,`,,```,`,`-`-`,,`,,`,`,,`--- Also see Annex D for detail on measurement methods.

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Annex D (informative)

Methods for testing surface cleanliness by chemical concentration

D.1 Method selection

D.1.1 Principle

methods should be selected. In some cases where quantitative information cannot be ascertained for a In order to obtain quantitative information regarding surface cleanliness, appropriate measurement Clause 5. surface, it is possible at least to obtain a qualitative result. Qualitative results cannot be used for surface D.1.2cleanliness Measurement by chemical concentrationmatrix classification as defined in Figure D.1 chemical concentration. provides a matrix for selecting an appropriate method for measuring surface cleanliness by

SCC

Specific Substrate Specific Substrate Representative Witness

Real Time Measurement Measurement After Exposure

Analysis Method Options?

Direct Method Indirect Method

Figure D.1 — Analysis of surface cleanliness by chemical concentration: measurement matrix chart

D.1.3 General application range of principal measurement methods Figure D.2

--``,`,,,,,,`,,,`,``,,`,,```,`,`-`-`,,`,,`,`,,`--- methods are appropriate for measuring particular substances. illustrates how to measure different types of contamination, indicating which measurement

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Key X surface chemical contamination Y main measurement methods Z detection depth (nm) P particles O organics M metals I a TOF-SIMS ions, i.e. acids and bases b XPS time of flight–secondary ion mass spectrometry c AES X-ray photo-electron spectroscopy d SEM Auger electron spectroscopy e SEM-EDX scanning electron microscopy f SEM-WDX SEM–energy dispersive X-ray spectroscopy g TXRF SEM–wavelength dispersive X-ray spectroscopy h total reflection X-ray fluorescence spectroscopy i TD-IMS/MS TD-GC/MS thermal desorption–gas chromatography/mass spectrometry FTIR TD–ion mobility spectroscopy/MS k MIR-FTIR j Fourier transform infrared spectroscopy l multiple interlayer reflection–FTIR m SAW surface acoustic wave QCM quartz crystal microbalance n VPD-ICP/MS vapour phase decomposition–inductive coupled plasma/MS o SIMS p VPD-TXRF vapour phase decomposition–TXRF secondary ion mass spectrometry q SE-IC/MS r solvent extraction–ion chromatography/MS SE-HPLC SE–high-performance liquid chromatography Figure D.2 — General application range of principal measurement methods

--``,`,,,,,,`,,,`,``,,`,,```,`,`-`-`,,`,,`,`,,`---

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D.2 Criteria for the measurement of surface cleanliness by chemical concentration

D.2.1 General

chemical contamination has been measured. The classification of surface cleanliness by chemical concentration can be determined as soon as the

As a measurable and quantitative criterion for the evaluation and classification of the surface cleanliness, D.2.2the number Requirements and type of all of adherent the measurement chemical substances method should be determined.

The measurement method is selected according to criteria determined by the surface being tested and its characteristics. Some of the most important requirements are summarized as follows: a) information regarding chemical characteristics and resistance (e.g. material, concentration); b) feasible measuring positions (direct, real-time measuring device such as an SAW instrument); c)d) testingfeasible speed measuring and effort positions involved (indirect, (i.e. use analytical of random measuring sampling device or series such testing); as an SEM stub zone);

components); e) flexibility (i.e. whether the method can be rapidly implemented on various surfaces of different

f) little or no surface alteration caused by the measurement procedure (i.e. measurement surfaces are not altered as a result of being wetted with flushing fluids). Due to requirements a) through f) in D.2.2, the measurement methods described in D.2.3 could be D.2.3classified Direct and be or limited indirect for eachmeasurement of the applications. methods

D.2.3.1 Principle

Ideally,measure surface the surface cleanliness cleanliness: by chemical concentration is best assessed when the test surface can be accessed by the chosen measurement device. In principle, the following methods can be utilized to a) direct methods;

b) indirect methods where a pre-treatment technique may also be introduced. Direct methods that do not require sample pre-treatment should generally be given priority. Generally, these methods involve less measurement activity and are also associated with fewer errors, thus giving --``,`,,,,,,`,,,`,``,,`,,```,`,`-`-`,,`,,`,`,,`--- moredetermine reproducible the chemical results cleanliness than indirect of a surface. methods. However, depending on component and sampling feasibility for complex components, indirect methods are often the only possible alternative in order to

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D.2.3.2 Collection method

The1) chemicaltotal product contamination — where the under whole consideration contaminated may specimen be presented is sent in to one test; of three groups: 2)

3) deposition sample — from proximity exposure onto witness discs or wafers;

extractedextraction. sample — collected from materials, work tops or equipment, using appropriate physical

tools such as swabs, scalpels or adhesive tapes of predetermined contamination level or by solvent --``,`,,,,,,`,,,`,``,,`,,```,`,`-`-`,,`,,`,`,,`---

D.2.3.3 Detachment techniques Figure D.3

“Total product”-type contamination may be collected and analysed as per , using either wet or dry techniques. Deposition samples may also follow the same procedure, wherein the contaminant is either displaced by surfactant in a water solution or dissolved by an organic solvent. The resulting analyteinto the instrument. is then fed into the appropriate test system for indirect assessment. Alternatively if “dry” assessment is to be made, the material will be cut into appropriately sized pieces and loaded directly

The third type — extracted samples — requires the contaminant to be transferred to adhesive tapes or SEM stubs that can be directly loaded into the instrument. Low-tack adhesive is used for this work, which involvescleanroom placing gloves the should tape beor usedstub whenover thetaking surface the sample. and making Depending firm contact on the extractionwith the film. method The usedadhesive and or stub is then placed in a clean, sealed transport pouch for shipment to the laboratory. Non-leaching

the contamination form, either analysis can be carried out directly by placing the physical collection sample intoD.2.4 the Packaginganalytical instrument, of test samples or further preparation by chemical or thermal techniques will be required.

D.2.4.1 Packaging of samples for chemical examination Samples that are to be assessed for SCC outside the area of origin should be packaged as follows: a) Preparation should take place inside the area of origin. The preparer should wear appropriate cleanroom clothing.

b) To handle samples, a technician should wear a new pair of washed nitrile or latex cleanroom gloves and use tweezers or vacuum pickup. wrapping in clean aluminium foil. c) When a cleaning process has been used, the samples should be allowed to cool and dry before

d) Each sample should be foil-wrapped separately before being placed in a cleanroom bag. used. The minimum thickness of the bags should be 80 µm to avoid tearing. e) Cleanroom-produced polyethylene bags with a fully detailed chemical test certificate should be

f) The bag should be sealed with specified adhesive tape and an identity label should be fixed to the outside, worded to prevent the bag from being opened outside a controlled environment. contamination. g) A second cleanroom bag should then be placed over the first bag to eliminate particulate

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D.2.4.2 Removal from packaging

a)b) The exteriorinterior bagbag shouldshould notbe removedbe removed immediately before arrival before in enteringthe controlled the controlled test environment. test environment.

interior pack. c) Full cleanroom garments, including hood and face mask, should be worn when handling the d) A new pair of washed nitrile or latex cleanroom gloves should be worn when examining the samples.

D.2.5 Pre-treatment methods

Figure D.3. In situations where a direct measurement technique is not practical, it may be necessary to condition theExamples sample of before pre-treatment measurement are: using an additional surface refinement technique. See also

a) Field-ion beam (FIB) microscopy — a preparation technique using an ion beam to create a cross sectionelectron in microscope the specimen (STEM). which is then analysed using a high-resolution microscope such as a scanning electron microscope (SEM), a transmission electron microscope (TEM), or a scanning transmission

b) Thermal desorption (TD) spectroscopy — the contaminant is thermally evaporated into a gaseous substance, which is then analysed using controlled analytical methods. Derivatives of this are: — TD-GC/MS, used on inorganic and metallic surfaces where the final analysis is carried out using gas chromatography with mass spectrometry; spectrometer; — TD-QMS, using thermal desorption and measuring ion intensity with a quadrupole mass

— TD-API-MS, using a Thermally Desorbed Atomic Pressure Ionization Mass Spectrometer; c) —Solvent wafer extraction thermal (SE)desorption — a suitable (WTD), solvent used for is usedsemiconductor to dissolve wafers. the surface contaminant creating a

test solution for use in one of the following wet microanalysis methods: — solvent dissolution (SD), where both the contaminant and the substrate matrix are dissolved by the solvent for a few nanometres depth, as shown in D.2.8; — vapour phase decomposition (VPD), where the contaminant is dissolved using vaporized D.2.6 Comparativehydrofluoric acid test and methods tested as shown in D.2.8.

Table D.1 lists direct test methods and Table D.2 The following tables are for guidance only and are not intended to be exhaustive or comprehensive. D.2.7 Direct measurements lists indirect methods, which may include pretreatment. Complex methods: X/Y

(for example, GC/MS), where X is the main measuring method to be used and chromatographic separation (qualification) and determination (quantification) are the basic functions. The classification is based on the ‘X’ process. ‘Y’ describes the additional functions, e.g. sensitivity of mass spectrometry for each chromatogram peak to make up quantification. Additional information for ‘X’, such as a mass chromatogram or the mass spectra of each peak to ascertain qualification, may also be shown.

--``,`,,,,,,`,,,`,``,,`,,```,`,`-`-`,,`,,`,`,,`---

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Table D.1 — Direct measurement methods and their applications

Information Resolution lateral Quantitative Typical applica- Technique Acronym Principle Sensitivity gained depth analysis? tions Method in which an electron spec- - trometer is used Semi-quan- Auger tion of surface to measure the Structure electron AES < 10 nm 20 nm Characterizacontaminants; - composition standard - tion of Auger tifiedmaterials with 0,1 at % ture energyelectrons distribu emitted spectroscopy multilayer struc from a surface

Method in which of organic and an electron spec- Surfaceinorganic analysis mate-

trometer is used rials or residues; electron to measure the X-ray photo- Semi-quan- - (also known XPS (or elemental tion of photoelec- < 10nm < 10 nm depthcomposition; profiling spectroscopyas electron ESCA) Quantifiedand oxidation standard energytrons and distribu Auger foroxide thin-film thickness state tifiedmaterials with electrons emitted 0,1 at % measurements for chemical from a surface (SiO O ); spectroscopy 2 2 3 determination of , Al - analysis) irradiated by mer groups X-ray photons functional poly Trace con- Mass spectrom- tamination of measure the mass- Elemen- etryto-charge is used quotient to surfaces,structures thin and ion mass SIMS and abundance ppm-ppb 2 nm 30 nm with stand- inorganic films,interfaces; multilayer Secondary Quantifiedard materials tal,molecules simple composition and emitted from - spectrometry ofsample secondary after ionions urements of thin bombardment impurity meas

films organic and inor- Semi-quan- Elemental Microanalysisganic materials; of TOF-SIMS Same as SIMS and molecu- ppm-ppb <5 nm mass spectra Time-of-flightmass spec- standard lar direct from sur- secondary ion tifiedmaterials with <0,2 µm faces; ion surface imaging trometry

of micro-struc- Scanning microscope using Characterizationtural surface Structure and electron SEM High-powera focused scanned N/A N/A N/A N/A electron beam to produce images topography,and contamina - morphology microscopy graintion size, oxides - Elemental. - Analyticalsolid-state capacooled - persive bility that uses a bined with Elemental SEM EDX Energy-dis- detect and meas- Mayimaging be com tools detector system to 0,1 % ≅ 1 µm ≅ 1 µm yes X-ray spec emitted during STEM). microanalysis troscopy ureSEM X-ray interaction. pulses (SEM, TEM, - - mental screen- eter measuring Qualitativeing of unknown ele X-ray spectrom- - metallic surface energy distribu TXRF 10 ppb 1 nm 1 mm with stand- samples,contamination Total reflec tionfrom of surface fluorescent. irra- elemental Quantifiedard materials on semicon- tion X-ray X-rays emitted Quantified fluorescence composition spectroscopy diatedcondition by primaryof total ductor wafers, X-rays under

--``,`,,,,,,`,,,`,``,,`,,```,`,`-`-`,,`,,`,`,,`--- ratios of binary reflection. thin films

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Table D.1 (continued)

Information Resolution lateral Quantitative Typical applica- Technique Acronym Principle Sensitivity gained depth analysis? tions

molecular struc- Measurement for tureIdentification organic of infrared absorp- Fourier Chemical tion spectra in transform bonding and 1E-19 carbon 10– FTIR which a spec- with stand- compounds,powders liquids; infrared molecular atoms/m2 100 µm trometer is used Quantifiedards films, particles, structure 0,1– to measure the 2,5 µm quantification - spectroscopy of O and H in Si infrared energy wafers;wafers quantifi cation of H in SiN -

OpticallyFTIR; low-angle modi Multiple fiedincident version IR is of Less than internal Similar to above MIR-FTIR As above 1E-18 carbon As above As above As above between infrared on surfaces atoms/m2 FTIR multi-reflectedtransparent prism reflection and substrate surface to enhance

detectionDevice in whichactivity Vibration - - piezoelectricrespond to the Molecular is compared its of gaseous tal micro- quartzcondensation crystals of - ng/cm2 N/A N/A frequencywith refer- Thincontaminants film depos Quartzbalance crys ment ence materi- QCM flux measure -Hz als of known detector surface gasses by reducing concentration onto quartz operatingrelationship Hz in a linear mass-to-Hz Acoustic - wave is com- its of gaseous Surface Molecular pared with 2- Thincontaminants film depos acoustic wave SAW Item as above - N/A N/A reference onto a detec- detector ment materials of 0,01 ng/cm tor substrate flux measure known con- Hz surface --``,`,,,,,,`,,,`,``,,`,,```,`,`-`-`,,`,,`,`,,`--- centration Atomic force Shape and AFM Visual imaging microscope

molecule size wavelength of Measuringelements of X-ray atomic Element dis- number of lithium tribution can Wavelength during SEM inter- be combined dispersive SEM-WDX action; measuring with imaging Visual imaging - elements > atomic X-ray spec X-raynumber wavelength of lithium toolsetc.) (SEM, troscopy during SEM inter- TEM, STEM, action

NOTE Resolution and sensitivity are interdependent parameters. Resolution is related to the concentration on the sample. Sensitivity can be influenced by optimizing the sample area.

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D.2.8 Indirect measurement methods (pre-treatment and measurement)

Table D.2 — Indirect measurement methods and their applications

Information Typical sensi- Typical quantitative analysis appli- Technique Acronym Principle gained tivity cations Contaminants on substrate surface are organic species; evalu- Thermal desorption– concentrated into a spe- Traceation ofanalysis contaminants of thermally desorbed and 10 ng/m2 with stand- molecular on silicon wafers Quantifiedards Quantified (wafer thermal des- gas chromatography/ TD-GC/MS cificare then absorption introduced column to a mass spectrometry andgas chromatograph/massanalyte. Concentrates spectrometer. orption GC/MS) --``,`,,,,,,`,,,`,``,,`,,```,`,`-`-`,,`,,`,`,,`--- Contaminants on Trace ionic contamina- substrate surface are dis- - solved in an appropriate urement of extractable Solvent dissolution– - tionionic analysis; constituents meas of SD-IC/MS tion stage if required. An 10 ng/m2 with stand- ionic - solvent,optimum via amount a concentra of solu- Quantifiedards Quantified tion compounds and ion chromatography/ powders, encapsula mass spectrometry an ion chromatograph/ tionmass is spectrometer. then injected into glasses, after sample Contaminants on preparation by reflux substrate surface are

are introduced to an ion thermally desorbed and Thermal desorp- Contaminants are decom- parts per billion 3 and TD-IMS mobilityposed using spectrometer. (ppb) in gas with stand- organic contaminants - phase 1 µg/m2 Quantifiedards onInorganic substrate NH surface tion–ion mobility - spectrometry βrated rays according into ionized to theirfrag ments, which are sepa determined with quadru- ionpole mobility. mass detector. Ions are then The contaminants are - priate solvent and are dissolved by an appro Solvent dissolution– electrophoresis (CE). - SD-CE/MS introducedThe contaminants into capillary are 200 ng/m2 resis-mass spectrom- separated from each capillary electropho other according to their conductive properties etry spectrometer. and evaluated by mass The contaminants are dissolved with appropriate solvent and are Solvent dissolution– Measurement of introduced to high-per- high performance liq- 2000 ng/m2 with stand- extractable organic formance liquid chroma- Quantifiedards components tograph to be separated SD-HPLC from each other and uid chromatography evaluated

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Table D.2 (continued)

Information Typical sensi- Typical quantitative analysis appli- Technique Acronym Principle gained tivity cations The contaminants on the substrate surface are dis- Solvent dissolution– solved with appropriate 500 ng/m2 to

solvent. 2 A portion of solvent is gas chromatography/ SD-GC/MS 10,000 ng/m mass spectrometry introduced to GC/MS. - Vapour-phaseon the surface hydrofluoto dissolve ricthe acid SiO2 (HF) with is the condensed contam- Vapour phase decom- contamination forms a VPD-ICP/MS 1E-14 atoms/m2 metallic contaminants coupled plasma/mass inantsdroplet in on it. the The resultant HF with elemental Ultraon silicon trace wafers analysis of position– inductively Quantified

spectrometry hydrophobicappropriate method surface. to Thisthe measuring is transferred instru- by ment ICP/MS.

--``,`,,,,,,`,,,`,``,,`,,```,`,`-`-`,,`,,`,`,,`---

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D.2.9 Sampling, analysis and associated quality control (QC) elements

Sampling and Analysis QC Process Steps Taking the Sample Pre- Analysis Results Sample treatment

Plan and prepare Adjust sample size to take sample if required

Prepare sample for chosen DRY analytical YES technique Incorporate relevant QC adjustments Target surface/ Apply pre- substrate is treatment if sampled required

Final analytical Is analytical calculations technique dry or wet? Analyse all samples

Is analysis to be performed within Determination the sampling of sample environment? surface chemical Apply pre- cleanliness treatment if required

NO WET

Prepare and , package sample Extraction, substrate and makeup and travel blanks adjustments

Figure D.3 — Overview flowchart of sampling, analysis and associated QC elements

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D.2.10 Analysis quality control

A ddition of spike Blanksamples samples Substratecleaningifrequired;e.g. atmosphere exposure test

Substrateblank Sample spike

Sampling of thesubstrate sample

Travel blank Travel spike

Transportand storage from exposure/samplinglocationto analytical source/laboratory

Cleanupblank Cleanupspike

Sample make up and adjustm ents for analysis(calibrationblank sigma x 30)

Injectionblank Injectionspike

Pre-treatmentinwafer thermal desorption apparatus

Calibration Calibrationblank standardsat4 concentration levels A nalysis by gaschromatograph/ mass spectrometer

Measurementofintensity

Figure D.4 — Analysis quality control flowchart using silicon wafer TD-GC/MS

In general, spike samples are introduced at critical sampling and analysis stages in order to monitor method performance or quantify the variance and bias of preparation and testing stages. The analysis method will describe spike levels at each stage. In this example of a silicon wafer, intensity and total ion chromatogram (TIC) of an injection spike analyte should be the same as that of the calibration standard, ofpattern the same (see amountReference added,14] within the required reliability range. For example, a 100-ng injection spike added to wafer thermal desorption is equivalent to a 100-ng calibration standard in intensity and TIC [ in the Bibliography).

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Annex E (informative)

Test record documentation

Table E.1 is an example of how a test report might be constructed. Other variations of the test report

which are agreeableTable E.1 to —both Supporting the customer documentat and supplierion formay testing be used. surface cleanliness by chemical concentration

Formalities Title: Date: Tester: Customer: Environmental conditions/ cleanroom conditions Temperature: Relative humidity: Locations used for the measurements: References of standards and guidelines consulted: Specimen Description of the operating facility and identiLication: IdentiLication of the test object: Test set-up (photo and/or sketch) Description of operating parameters: Description of measurement points and measurement methods: Measurement devices IdentiLication number of measuring device: Measurement range of measuring devices used; equipment resolution and detection limits: Reference of calibration certiLicate: Performing the test Test and measurement procedure: Noticeable observations made during the measurement where applicable: Test duration and sampling time: Reference to ACC or nanoparticle measurements if applicable: Results and analysis Measurement values and/or their analysis:

--``,`,,,,,,`,,,`,``,,`,,```,`,`-`-`,,`,,`,`,,`--- Visual inspection of the test surface before and after the measurement, where applicable:

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Bibliography

Cleanrooms and associated controlled environments — Part 8: Classification of air cleanliness by chemical concentration (ACC) [1] ISO 14644-8, Cleanrooms and associated controlled environments — Part 9: Classification of surface cleanliness by particle concentration [2] ISO 14644-9, Surface chemical analysis — Vocabulary — Part 1: General terms and terms used in spectroscopy [3] ISO 18115-1, ISO 17052 Rubber, raw — Determination of residual monomers and other volatile low-molecular-mass compounds by capillary gas chromatography — Thermal desorption (dynamic headspace) method [4] , ISO 18116 Surface chemical analysis — Guidelines for preparation and mounting of specimens for analysis [5] , Ambient air — Determination of asbestos fibres — Direct transfer transmission electron microscopy method [6] ISO 10312, Standard for evaluation methods on substrate surface contamination in cleanrooms and associated controlled environments [7] JACA 43, Test method for the determination of organic contamination from minienvironments using ion mobility spectrometry (IMS) [8] SEMI E46-0307, T.Airborne Molecular Contamination: Contamination on Substrates and the Environment in Semiconductors and Other Industries. In: Developments [9] in Fujimoto Surface ContaminationT., Takeda K., and Nonaka Cleaning: Fundamentals and Applied Aspects

, (Kohli R., & Mittal K.L.eds.). William Andrew Publishing, Norwich, New York, 2007, pp. 329–474. Developments in Surface Contamination and Cleaning: Fundamentals and Applied Aspects [10] Birch W., Carre A., Mittal K.L.Wettability in Surface Contamination and Cleaning. In: , (Kohli R., & Mittal K.L.eds.). William Andrew Publishing, Norwich, New York, 2007, pp. 693–724. and on Substrate Surfaces.” Proceedings of the 18th ICCCS [11] Fujimoto T., Nonaka T., Takeda K. et al. “Study on Airborne Molecular Contaminants in Atmosphere . Beijing: International Symposium on Contamination Control, 2006 [12] Proceedings Beckhoff B., of Fabry ALTECH L. et 2003 al. “Ultra-Trace Analysis of Light Elements and Speciation of Minute Organic Contaminants on Silicon Wafer Surfaces by Means of TXRF in Combination with NEXFS.” (Analytical Techniques for Semiconductor Materials and Process Characterization IV), 203rd Electrochemical Society Meeting, Paris, 27 April–2 May,Proceedings 2003 of the 2001 SPWCC [13] Wang J., Balazs M. et al. “How Low Can the Detection Limit Go with VPD-TXRF?” (Semiconductor Pure Water Chemicals Conference), 362–369. Pennington, New Jersey: The ElectrochemicalMethod for Society,determination 2001 of tetra- through octa-chlorodibenzo-p-dioxins, tetra- through octa-chlorodibenzofurans and co-planar polychlorobiphenyls in stationary source emissions [14] JIS K 0311:2005, Microelectronics Failure Analysis: Desk Reference [15] Evans K., Anderson T.A. Instrumental analysis techniques. In: , (Electronic Device Failure Analysis Society Desk Reference Committee, ed.) ASM International, Materials Park, Ohio, Fourth Edition, 1999,Microelectronics pp. 343–51. Failure Analysis: Desk Reference [16] Vanderlinde W. Energy dispersive X-ray analysis. In: , (Electronic Device Failure Analysis Society Desk Reference Committee, ed.), ASM International, Materials Park, Ohio, Fifth Edition, 2004, pp. 628–39.

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IMS/MS and .” Proceedings of SEMICON Europa [17] Budde K., Holtzapfel W. “Determination of Contaminants on Substrate Surface Using GC/MS (1997 and 2000, Munich, Germany).San Jose, California: SEMI, 2000 Contamination- Free Manufacturing for Semiconductors and Other Precision Products [18] Chia V.K.F., Edgell M.J. On-Wafer Measurement of Molecular Contaminants. In: , (Donavan R.P., ed.). M. Dekker Press, New York, 2001, pp. 117–48. --``,`,,,,,,`,,,`,``,,`,,```,`,`-`-`,,`,,`,`,,`---

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ICS 13.040.35 Price based on 30 pages

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