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1、DRAFT FOR DEVELOPMENT DD ISO/TR 15969:2001 Surface chemical analysis Depth profiling Measurement of sputtered depth ICS 17.040.20; 71.040.40 NO COPYING WITHOUT BSI PERMISSION EXCEPT AS PERMITTED BY COPYRIGHT LAW Licensed Copy: London South Bank University, London South Bank University, Mon Dec 11 01
2、:19:03 GMT+00:00 2006, Uncontrolled Copy, (c) BSI DD ISO/TR 15969:2001 This Draft for Development, having been prepared under the direction of the Sector Policy and Strategy Committee for Materials and Chemicals, was published under the authority of the Standards Policy and Strategy Committee on 01
3、October 2001 BSI 01 October 2001 ISBN 0 580 38501 9 National foreword This Draft for Development reproduces verbatim ISO/TR 15969:2001. This publication is not to be regarded as a British Standard. It is being issued in the Draft for Development series of publications and is of a provisional nature
4、because the source document is an ISO Technical Report which is not an international standard. It should be applied on this provisional basis, so that information and experience of its practical application may be obtained. Comments arising from the use of this Draft for Development are requested so
5、 that UK experience can be reported to the international organization responsible for its conversion into an international standard. A review of this publication will be initiated 2 years after its publication by the international organization so that a decision can be taken on its status at the end
6、 of its three-year life. The commencement of the review period will be notified by an announcement in Updated Standards. According to the replies received by the end of the review period, the responsible BSI Committee will decide whether to support the conversion into an international standard. Comm
7、ents should be sent in writing to the Secretary of BSI Technical Committee CII/60, Surface chemical analysis, at 389 Chiswick High Road, London W4 4AL, giving the document reference and clause number and proposing, where possible, an appropriate revision of the text. A list of organizations represen
8、ted on this committee can be obtained on request to its secretary. Cross-references The British Standards which implement international or European publications referred to in this document may be found in the BSI Standards Catalogue under the section entitled “International Standards Correspondence
9、 Index”, or by using the “Find” facility of the BSI Standards Electronic Catalogue. Summary of pages This document comprises a front cover, an inside front cover, the ISO/TR title page, pages ii to v, a blank page, pages 1 to 12, an inside back cover and a back cover. The BSI copyright date displaye
10、d in this document indicates when the document was last issued. Amendments issued since publication Amd. No. DateComments Licensed Copy: London South Bank University, London South Bank University, Mon Dec 11 01:19:03 GMT+00:00 2006, Uncontrolled Copy, (c) BSI Reference number ISO/TR 15969:2001(E) TE
11、CHNICAL REPORT ISO/TR 15969 First edition 2001-06-01 Surface chemical analysis Depth profiling Measurement of sputtered depth Analyse chimique des surfaces Profilage dpaisseur Mesurage de lpaisseur bombarde DD ISO/TR 15969:2001 Licensed Copy: London South Bank University, London South Bank Universit
12、y, Mon Dec 11 01:19:03 GMT+00:00 2006, Uncontrolled Copy, (c) BSI ii DD ISO/TR 15969:2001 Licensed Copy: London South Bank University, London South Bank University, Mon Dec 11 01:19:03 GMT+00:00 2006, Uncontrolled Copy, (c) BSI IS/OTR :96951(1002)E iii ContentsPage Foreword.iv 1Scope 1 2Terms and de
13、finitions .1 3Abbreviated terms .2 4Methods of determination of the sputtered depth2 4.1Crater depth measurement after sputter profiling .2 4.2Comparison with sputter profiled samples having interfaces as depth markers.5 4.3Typical applications and uncertainties of the different methods.9 Annex ASur
14、vey of typical applications and uncertainties of the different methods.10 Bibliography11 DD ISO/TR 15969:2001 Licensed Copy: London South Bank University, London South Bank University, Mon Dec 11 01:19:03 GMT+00:00 2006, Uncontrolled Copy, (c) BSI IS/OTR :96951(1002)E iv Foreword ISO (the Internatio
15、nal 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 committee has been
16、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 electrotechnical standar
17、dization. International Standards are drafted in accordance with the rules given in the ISO/IEC Directives, Part 3. The main task of technical committees is to prepare International Standards. Draft International Standards adopted by the technical committees are circulated to the member bodies for v
18、oting. Publication as an International Standard requires approval by at least 75 % of the member bodies casting a vote. In exceptional circumstances, when a technical committee has collected data of a different kind from that which is normally published as an International Standard (“state of the ar
19、t“, for example), it may decide by a simple majority vote of its participating members to publish a Technical Report. A Technical Report is entirely informative in nature and does not have to be reviewed until the data it provides are considered to be no longer valid or useful. Attention is drawn to
20、 the possibility that some of the elements of this Technical Report may be the subject of patent rights. ISO shall not be held responsible for identifying any or all such patent rights. ISO/TR 15969 was prepared by Technical Committee ISO/TC 201, Surface chemical analysis, Subcommittee SC 4, Depth p
21、rofiling. DD ISO/TR 15969:2001 Licensed Copy: London South Bank University, London South Bank University, Mon Dec 11 01:19:03 GMT+00:00 2006, Uncontrolled Copy, (c) BSI IS/OTR :96951(1002)E v Introduction This Technical Report is intended to be used as follows: a)For the determination of the depth s
22、cale in sputter depth profiling where signal intensity is obtained as a function of sputtering time (or ion dose density). The sputtered depth per sputtering time is the sputtering rate (typically reported in nm/s). b)To enhance the comparability of depth profiling data obtained with different instr
23、uments and to increase the reliability and use of depth profiling in industrial applications. c)To serve as the basis for the development of International Standards on the measurement of sputtered depth. DD ISO/TR 15969:2001 Licensed Copy: London South Bank University, London South Bank University,
24、Mon Dec 11 01:19:03 GMT+00:00 2006, Uncontrolled Copy, (c) BSI DD ISO/TR 15969:2001 Licensed Copy: London South Bank University, London South Bank University, Mon Dec 11 01:19:03 GMT+00:00 2006, Uncontrolled Copy, (c) BSI TECINHCAL ROPETRIS/OTR :96951(1002)E ISO 1002 All rights rsedevre1 Surface che
25、mical analysis Depth profiling Measurement of sputtered depth 1Scope This Technical Report gives guidelines for measuring the sputtered depth in sputtered depth profiling. The methods of sputtered depth measurement described in this Technical Report are applicable to techniques of surface chemical a
26、nalysis when used in combination with ion bombardment for the removal of a part of a solid sample to a typical sputtered depth of up to several micrometres. 2Terms and definitions For the purposes of this Technical Report, the following terms and definitions apply. NOTEThe terms used in this Technic
27、al Report follow basically the definitions in ASTM E 673-95c1. These definitions are to be modified to conform to those being developed by ISO/TC 201/SC 1 on Terminology. See also 2 and 3. 2.1 sputtered depth distance z (m) (perpendicular to the surface) between the original surface and the analysed
28、 sample surface after removal of a measurable amount of matter as a result of sputter profiling, which is given by m z A ? ? ? (1) where mis the removed sample mass (kg); Ais the sputtered area (m2); ?is the density of the sample (kg/m3) 2.2 crater depth average distance (perpendicular to the surfac
29、e) between the original surface and the region of a crater bottom from which the measured signal is derived NOTEThe crater depth is equal to the sputtered depth if primary-ion implantation and retention, which may cause enlargement (“swelling”) of the sample in the direction perpendicular to the sur
30、face, is negligible5. If the sputtered depth is measured by crater depth measurement outside the analysis chamber, surface reactions (e.g. oxidation) may add to the swelling of the crater bottom, i.e. the crater depth is generally measured as being less than the sputtered depth. DD ISO/TR 15969:2001
31、 1 Licensed Copy: London South Bank University, London South Bank University, Mon Dec 11 01:19:03 GMT+00:00 2006, Uncontrolled Copy, (c) BSI IS/OTR :96951(1002)E 2 ISO 1002 All rights rsedevre 3Abbreviated terms AESAuger electron spectroscopy AFMAtomic force microscopy EDSEnergy dispersive spectrome
32、try EPMAElectron probe microanalysis FIBFocused ion beam GIXRGrazing incidence X-ray reflectivity MEISMedium energy ion scattering RBSRutherford backscattering spectrometry SAMScanning Auger microscopy SEMScanning electron microscopy SIMSSecondary-ion mass spectrometry TEMTransmission electron micro
33、scopy XPSX-ray photoelectron spectroscopy XRFX-ray fluorescence 4Methods of determination of the sputtered depth 4.1Crater depth measurement after sputter profiling 4.1.1General description Usually, the result of sputter profiling is a signal intensity as a function of the sputtering time. The total
34、 sputtering time corresponds to the crater depth and the average sputtering rate is obtained by dividing the crater depth by the sputtering time. Crater depth measurements are usually performed by mechanical stylus profilometry6or, less commonly in use, by optical interferometry. Optical instruments
35、 and scanned-probe microscopes give a two- dimensional view of the crater and its non-uniformities. 4.1.2Mechanical stylus crater depth measurement Mechanical stylus profilometers convert the deflection of a stylus in mechanical contact with the surface into a voltage that is amplified and then disp
36、layed directly on a strip chart, or digitized and processed in a computer. In some instruments, the stylus is scanned across the sample containing the crater, and in others the sample is scanned under the stylus. Profilometers typically produce one-dimensional line scans, though some modern instrume
37、nts and scanned probe microscopes are capable of producing two-dimensional scans by making an automated series of closely spaced one-dimensional scans. Stylus profilometry is appropriate for measuring the depths of craters in which the roughness of the original surface and that of the crater bottom
38、are small compared to the crater depth. It is commonly used for craters made in semiconductors during SIMS depth profiling. The minimum depth that can be measured successfully depends on the acoustic and electronic noise of the profilometer as well as the surface roughness. In modern instruments the
39、 minimum depth may be as small as 10 nm, and the maximum may be as great as 100?m. To perform a crater depth measurement with a one-dimensional profilometer, a scan is made through the centre of the crater and over a sufficient distance of the unsputtered top surface on either side to establish an a
40、ccurate DD ISO/TR 15969:2001 2 Licensed Copy: London South Bank University, London South Bank University, Mon Dec 11 01:19:03 GMT+00:00 2006, Uncontrolled Copy, (c) BSI IS/OTR :96951(1002)E ISO 1002 All rights rsedevre3 baseline, as shown in Figure 1. Multiple scans are made over different traces th
41、rough the crater centre to determine the repeatability of the crater depth measurement. The depth is measured on a computerized profilometer by determining the average height difference between a region in the centre of the crater at A and two regions of the reference surface on opposite sides at B
42、and C. Figure 1 shows an example of a computerized profilometer trace of a sputtered crater in single crystal silicon approximately 0,5?m in depth. The three pairs of vertical cursor lines indicate the regions over which the depth is averaged. Figure 1 Example of stylus profilometry trace of a 0,5?
43、? ? ?m deep crater in silicon The depth scale of the stylus profilometer is calibrated with standard step-heights or grooves that are traceable to fundamental length standards (wavelength of light). A typical calibration uncertainty is 1 % for a 1?m standard gauge. The uncertainty of a crater depth
44、measurement is a combination of calibration uncertainty and profilometer noise. In a recent round-robin experiment on craters in silicon, uncertainties ranged from?1,3 % for a 2?m crater to?4,7 % for a 0,1?m crater6. NOTEFor the purposes of this Technical Report, typical uncertainties are given as o
45、ne-standard-deviation uncertainties. Advantages of stylus profilometry for crater depth measurements are that it is rapid, requires no sample preparation, and reveals the size, shape, and flatness of the crater bottom which are measures of the ion beam current density. A disadvantage is that correct
46、ions may be necessary to convert crater depth to sputtered depth in the case of non-negligible swelling or oxidation. In the case of layered structures with different sputtering rates, separate craters must be made for each interface so that the individual sputtering rates can be determined. Otherwi
47、se only an average sputtering rate is obtained. 4.1.3Optical interferometry crater depth measurement Optical interferometry is a simple and convenient non-contact method of crater depth measurement for which the equipment is relatively cheap to buy and easy to use. This method utilizes a metallurgic
48、al microscope equipped with an interference attachment (Mireau or Michelson objective, sample tilting stage and monochromatic light source/interference filter) and is only applicable to smooth flat samples, for example flat glass, coatings on glass and semiconductor wafers. Generally, metal samples
49、are too rough for this method to be suitable. The crater to be measured is placed on the microscope sample stage, which usually is capable of producing a controlled tilting movement of the sample as well as the usual x-y translation. Using the interference objective or a normal objective, the crater of interest is located and placed at the centre of the field of view. This operation can be done with white light illumination. If a normal objective has been used, the interference objective is then put in place DD ISO/TR 15969:2001 3 Licensed Copy: