1、raising standards worldwideNO COPYING WITHOUT BSI PERMISSION EXCEPT AS PERMITTED BY COPYRIGHT LAWBSI Standards PublicationDD ISO/TS 25138:2010Surface chemical analysis Analysis of metal oxide filmsby glow-discharge optical-emission spectrometryDD ISO/TS 25138:2010 DRAFT FOR DEVELOPMENTNational forew
2、ordThis Draft for Development is the UK implementation of ISO/TS25138:2010.This publication is not to be regarded as a British Standard.It is being issued in the Draft for Development series of publicationsand is of a provisional nature. It should be applied on thisprovisional basis, so that informa
3、tion and experience of its practicalapplication can be obtained.Comments arising from the use of this Draft for Developmentare requested so that UK experience can be reported to theinternational organization responsible for its conversion toan international standard. A review of this publication wil
4、lbe initiated not later than 3 years after its publication by theinternational organization so that a decision can be taken on itsstatus. Notification of the start of the review period will be made inan announcement in the appropriate issue of Update Standards.According to the replies received by th
5、e end of the review period,the responsible BSI Committee will decide whether to support theconversion into an international Standard, to extend the life of theTechnical Specification or to withdraw it. Comments should be sentto the Secretary of the responsible BSI Technical Committee at BritishStand
6、ards House, 389 Chiswick High Road, London W4 4AL.The UK participation in its preparation was entrusted to TechnicalCommittee CII/60, Surface chemical analysis.A list of organizations represented on this committee can beobtained on request to its secretary.This publication does not purport to includ
7、e all the necessaryprovisions of a contract. Users are responsible for its correctapplication. BSI 2011ISBN 978 0 580 67880 6ICS 71.040.40Compliance with a British Standard cannot confer immunity fromlegal obligations.This Draft for Development was published under the authority ofthe Standards Polic
8、y and Strategy Committee on 31 January 2011.Amendments issued since publicationDate Text affectedDD ISO/TS 25138:2010Reference numberISO/TS 25138:2010(E)ISO 2010TECHNICAL SPECIFICATION ISO/TS25138First edition2010-12-01Surface chemical analysis Analysis of metal oxide films by glow-discharge optical
9、-emission spectrometry Analyse chimique des surfaces Analyse de films doxyde de mtal par spectromtrie dmission optique dcharge luminescente DD ISO/TS 25138:2010ISO/TS 25138:2010(E) PDF disclaimer This PDF file may contain embedded typefaces. In accordance with Adobes licensing policy, this file may
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14、 749 01 11 Fax + 41 22 749 09 47 E-mail copyrightiso.org Web www.iso.org Published in Switzerland ii ISO 2010 All rights reservedDD ISO/TS 25138:2010ISO/TS 25138:2010(E) ISO 2010 All rights reserved iiiContents Page Foreword iv 1 Scope1 2 Normative references1 3 Principle .1 4 Apparatus.2 4.1 Glow-d
15、ischarge optical-emission spectrometer 2 5 Adjusting the glow-discharge spectrometer system settings3 5.1 General .3 5.2 Setting the parameters of a DC source.4 5.3 Setting the discharge parameters of an RF source .5 5.4 Minimum performance requirements6 6 Sampling 8 7 Calibration8 7.1 General .8 7.
16、2 Calibration specimens 8 7.3 Validation specimens10 7.4 Determination of the sputtering rate of calibration and validation specimens 11 7.5 Emission intensity measurements of calibration specimens.12 7.6 Calculation of calibration equations .12 7.7 Validation of the calibration .12 7.8 Verification
17、 and drift correction.14 8 Analysis of test specimens 14 8.1 Adjusting discharge parameters .14 8.2 Setting of measuring time and data acquisition rate.14 8.3 Quantifying depth profiles of test specimens 15 9 Expression of results15 9.1 Expression of quantitative depth profile.15 9.2 Determination o
18、f metal oxide mass per unit area 15 9.3 Determination of the average mass fractions of the elements in the oxide16 10 Precision 16 11 Test report17 Annex A (normative) Calculation of calibration constants and quantitative evaluation of depth profiles18 Annex B (informative) Suggested spectral lines
19、for determination of given elements.29 Annex C (informative) Examples of oxide density and the corresponding quantity O30 Annex D (informative) Report on interlaboratory testing of metal oxide films.31 Bibliography36 DD ISO/TS 25138:2010ISO/TS 25138:2010(E) iv ISO 2010 All rights reservedForeword IS
20、O (the International Organization for Standardization) is a worldwide federation of national standards bodies (ISO member bodies). The work of preparing International Standards is normally carried out through ISO technical committees. Each member body interested in a subject for which a technical co
21、mmittee has been established has the right to be represented on that committee. International 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 electro
22、technical standardization. International Standards are drafted in accordance with the rules given in the ISO/IEC Directives, Part 2. The main task of technical committees is to prepare International Standards. Draft International Standards adopted by the technical committees are circulated to the me
23、mber bodies for voting. Publication as an International Standard requires approval by at least 75 % of the member bodies casting a vote. In other circumstances, particularly when there is an urgent market requirement for such documents, a technical committee may decide to publish other types of docu
24、ment: an ISO Publicly Available Specification (ISO/PAS) represents an agreement between technical experts in an ISO working group and is accepted for publication if it is approved by more than 50 % of the members of the parent committee casting a vote; an ISO Technical Specification (ISO/TS) represe
25、nts an agreement between the members of a technical committee and is accepted for publication if it is approved by 2/3 of the members of the committee casting a vote. An ISO/PAS or ISO/TS is reviewed after three years in order to decide whether it will be confirmed for a further three years, revised
26、 to become an International Standard, or withdrawn. If the ISO/PAS or ISO/TS is confirmed, it is reviewed again after a further three years, at which time it must either be transformed into an International Standard or be withdrawn. Attention is drawn to the possibility that some of the elements of
27、this document may be the subject of patent rights. ISO shall not be held responsible for identifying any or all such patent rights. ISO/TS 25138 was prepared by Technical Committee ISO/TC 201, Surface chemical analysis, Subcommittee SC 8, Glow discharge spectroscopy. DD ISO/TS 25138:2010TECHNICAL SP
28、ECIFICATION ISO/TS 25138:2010(E) ISO 2010 All rights reserved 1Surface chemical analysis Analysis of metal oxide films by glow-discharge optical-emission spectrometry 1 Scope This Technical Specification describes a glow-discharge optical-emission spectrometric method for the determination of the th
29、ickness, mass per unit area and chemical composition of metal oxide films. This method is applicable to oxide films 1 nm to 10 000 nm thick on metals. The metallic elements of the oxide can include one or more from Fe, Cr, Ni, Cu, Ti, Si, Mo, Zn, Mg, Mn and Al. Other elements that can be determined
30、by the method are O, C, N, H, P and S. 2 Normative references The following referenced documents are indispensable for the application of this document. For dated references, only the edition cited applies. For undated references, the latest edition of the referenced document (including any amendmen
31、ts) applies. ISO 14284, Steel and iron Sampling and preparation of samples for the determination of chemical composition ISO 14707, Surface chemical analysis Glow discharge optical emission spectrometry (GD-OES) Introduction to use ISO 16962:2005, Surface chemical analysis Analysis of zinc- and/or a
32、luminium-based metallic coatings by glow-discharge optical-emission spectrometry 3 Principle The analytical method described here involves the following processes: a) Cathodic sputtering of the surface metal oxide in a direct-current or radio-frequency glow-discharge device. b) Excitation of the ana
33、lyte atoms in the plasma formed in the glow-discharge device. c) Spectrometric measurement of the intensities of characteristic spectral-emission lines of the analyte atoms as a function of sputtering time (depth profile). d) Conversion of the depth profile in units of intensity versus time to mass
34、fraction versus depth by means of calibration functions (quantification). Calibration of the system is achieved by measurements on calibration specimens of known chemical composition and measured sputtering rate. DD ISO/TS 25138:2010ISO/TS 25138:2010(E) 2 ISO 2010 All rights reserved4 Apparatus 4.1
35、Glow-discharge optical-emission spectrometer 4.1.1 General The required instrumentation includes an optical-emission spectrometer system consisting of a Grimm type1or similar glow-discharge source (direct-current or radio-frequency powered) and a simultaneous optical spectrometer as described in ISO
36、 14707, capable of providing suitable spectral lines for the analyte elements. The inner diameter of the hollow anode of the glow-discharge source shall be in the range 2 mm to 8 mm. A cooling device for thin specimens, such as a metal block with circulating cooling liquid, is also recommended, but
37、not strictly necessary for implementation of the method. Since the principle of determination is based on continuous sputtering of the surface metal oxide, the spectrometer shall be equipped with a digital readout system for time-resolved measurement of the emission intensities. A system capable of
38、a data acquisition speed of at least 500 measurements/second per spectral channel is recommended, but, for a large number of applications, speeds of 50 measurements/second per spectral channel are acceptable. 4.1.2 Selection of spectral lines For each analyte to be determined, there exist a number o
39、f spectral lines which can be used. Suitable lines shall be selected on the basis of several factors, including the spectral range of the spectrometer used, the analyte mass fraction range, the sensitivity of the spectral lines and any spectral interference from other elements present in the test sp
40、ecimens. For applications where several of the analytes of interest are major elements in the specimens, special attention shall be paid to the occurrence of self-absorption of certain highly sensitive spectral lines (so-called resonance lines). Self-absorption causes non-linear calibration curves a
41、t high analyte mass fraction levels, and strongly self-absorbed lines should therefore be avoided for the determination of major elements. Suggestions concerning suitable spectral lines are given in Annex B. Spectral lines other than those listed may be used, so long as they have favourable characte
42、ristics. 4.1.3 Selection of glow-discharge source type 4.1.3.1 Anode size Most GD-OES instruments on the market are delivered with options to use various anode diameters, 2 mm, 4 mm and 8 mm being the most common. Some older instruments have one anode only, usually 8 mm, while the most commonly used
43、 anode in modern instruments is 4 mm. A larger anode requires larger specimens and higher power during analysis; therefore the specimen is heated to a greater extent. On the other hand, a larger anode gives rise to a plasma of larger volume that emits more light, resulting in lower detection limits
44、(i.e. higher analytical sensitivity). In a large number of applications, the 4 mm anode is a good compromise. However, in surface analysis applications it is rather common to encounter problems of overheating of the specimens due to e.g. surface layers of poor heat conductivity and/or very thin spec
45、imens. In such cases, the smaller 2 mm anode is preferable, even if there is some loss of analytical sensitivity. 4.1.3.2 Type of power supply The glow-discharge source can be either a type powered by a direct-current (DC) power supply or a radio-frequency (RF) type. The most important difference is
46、 that the RF type can sputter both conductive and non-conductive specimens; hence this is the only type that can be used for e.g. polymer coatings and insulating oxide layers. On the other hand, it is technically simpler to measure and control the electrical source parameters (voltage, current, powe
47、r) of a DC type. Several commercially available GD-OES systems can be delivered with the option to switch between DC and RF operation, but RF-only systems are becoming increasingly common. In short, there are a very large number of applications where DC or RF sources can be used and several where on
48、ly an RF source can be used. DD ISO/TS 25138:2010ISO/TS 25138:2010(E) ISO 2010 All rights reserved 34.1.3.3 Mode of operation Both DC and RF sources can be operated in several different modes with respect to the control of the electrical parameters (current, voltage, power) and the pressure. There a
49、re several reasons for this: “historical” reasons (older instruments have simpler but functional power supplies, while the technology has evolved so newer models have more precise and easier-to-operate source control); different manufacturers have chosen different solutions for source control; there are some application-related issues where a particular mode of operation is to be preferred. This Technical Specification gives instructions for optimizing the source parameters based on several available modes of operation. The
