1、BSI Standards PublicationBS ISO 17861:2014Fine ceramics (advancedceramics, advanced technicalceramics) Measurementmethod of spectraltransmittance of fine ceramicsthin films under humidconditionBS ISO 17861:2014 BRITISH STANDARDNational forewordThis British Standard is the UK implementation of ISO 17
2、861:2014. The UK participation in its preparation was entrusted to TechnicalCommittee RPI/13, Advanced technical ceramics.A list of organizations represented on this committee can be obtained on request to its secretary.This publication does not purport to include all the necessary provisions of a c
3、ontract. Users are responsible for its correct application. The British Standards Institution 2014.Published by BSI Standards Limited 2014ISBN 978 0 580 79575 6ICS 81.060.30Compliance with a British Standard cannot confer immunity from legal obligations.This British Standard was published under the
4、authority of the Standards Policy and Strategy Committee on 30 June 2014.Amendments/corrigenda issued since publicationDate T e x t a f f e c t e dBS ISO 17861:2014 ISO 2014Fine ceramics (advanced ceramics, advanced technical ceramics) Measurement method of spectral transmittance of fine ceramics th
5、in films under humid conditionCramiques techniques Mthode de mesurage de la transmittance spectrale des films minces de cramiques fines en conditions humidesINTERNATIONAL STANDARDISO17861First edition2014-06-01Reference numberISO 17861:2014(E)BS ISO 17861:2014ISO 17861:2014(E)ii ISO 2014 All rights
6、reservedCOPYRIGHT PROTECTED DOCUMENT ISO 2014All rights reserved. Unless otherwise specified, no part of this publication may be reproduced or utilized otherwise in any form or by any means, electronic or mechanical, including photocopying, or posting on the internet or an intranet, without prior wr
7、itten permission. Permission can be requested from either ISO at the address below or ISOs member body in the country of the requester.ISO copyright officeCase postale 56 CH-1211 Geneva 20Tel. + 41 22 749 01 11Fax + 41 22 749 09 47E-mail copyrightiso.orgWeb www.iso.orgPublished in SwitzerlandBS ISO
8、17861:2014ISO 17861:2014(E) ISO 2014 All rights reserved iiiContents PageForeword ivIntroduction v1 Scope . 12 Normative references 13 Terms and definitions . 14 Principle 25 Ambient room environment . 26 Test piece 27 Measuring apparatus . 37.1 Apparatus configuration . 37.2 Spectrometer calibratio
9、n . 48 Environmental conditions and control procedures . 49 Optical transmittance measurement procedure. 410 Evaluations of measured spectra 511 Test report . 8Annex A (informative) Structure and function of mini-chamber 9BS ISO 17861:2014ISO 17861:2014(E)ForewordISO (the International Organization
10、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 established has t
11、he 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 standardization.The proc
12、edures used to develop this document and those intended for its further maintenance are described in the ISO/IEC Directives, Part 1. In particular the different approval criteria needed for the different types of ISO documents should be noted. This document was drafted in accordance with the editori
13、al rules of the ISO/IEC Directives, Part 2 (see www.iso.org/directives). 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 or all such patent rights. Details of any patent rights
14、 identified during the development of the document will be in the Introduction and/or on the ISO list of patent declarations received (see www.iso.org/patents). Any trade name used in this document is information given for the convenience of users and does not constitute an endorsement.For an explan
15、ation on the meaning of ISO specific terms and expressions related to conformity assessment, as well as information about ISOs adherence to the WTO principles in the Technical Barriers to Trade (TBT) see the following URL: Foreword - Supplementary informationThe committee responsible for this docume
16、nt is ISO/TC 206, Fine ceramics.iv ISO 2014 All rights reservedBS ISO 17861:2014ISO 17861:2014(E)IntroductionFine ceramics thin films are used in many applications such as anti-reflective coatings, infrared sensor cut filters, X-ray sensor cut filters, and band-pass filters for medical analysis equi
17、pment. Even though spectral transmittance of fine ceramics thin films are specified for each product, the refractive index and optical property change when water vapor or other vapor is adsorbed to the surface of fine ceramics thin films, because, generally, fine ceramics thin films have a columnar
18、and voided structure. For this matter, an International Standard that could evaluate the reliability under a range of humidity was required. This International Standard provides test methods that will easily and accurately evaluate effects of humidity on optical properties of fine ceramic coatings.
19、By establishing this International Standard, it aims for a rapid spread of this test method that will then lead to further growth of the industry. ISO 2014 All rights reserved vBS ISO 17861:2014BS ISO 17861:2014Fine ceramics (advanced ceramics, advanced technical ceramics) Measurement method of spec
20、tral transmittance of fine ceramics thin films under humid condition1 ScopeThis International Standard specifies a measurement method of spectral transmittance of fine ceramics thin films under humid condition. This International Standard provides test methods that will easily and accurately evaluat
21、e changes in optical properties of fine ceramic coatings in a humid atmosphere due to water adsorption.2 Normative referencesThe following documents, in whole or in part, are normatively referenced in this document and are indispensable for its application. For dated references, only the edition cit
22、ed applies. For undated references, the latest edition of the referenced document (including any amendments) applies.ISO 9211-1, Optics and photonics Optical coatings DefinitionsISO 8980-3:2013, Ophthalmic optics Uncut finished spectacle lenses Part 3: Transmittance specifications and test methods3
23、Terms and definitionsFor the purposes of this document, the terms and definitions given in ISO 8980-3 and ISO 9211-1, and the following apply.3.1half transmittance wavelength T1/2center of a segment delimited by the wavelengths at which the transmittance is maximal and minimal in a given wavelength
24、range3.2environmental mini-chambersmall chamber to keep the environmental condition of a test piece contained inside the chamberNote 1 to entry: The chamber is equipped with optical feed-through ports with a ball valve for evacuation or air-circulation. The chamber shall be air-tight to keep the cha
25、mber in vacuum or with the atmosphere at a certain humidity by closing the ball valves after evacuation or air-circulating to expose the test piece inside to a certain atmosphere.3.3transmittancefraction of intensity of incident optical beam transferring through the sample3.4monochromatoroptical dev
26、ice that selects light beam with a certain wavelength with a rangeINTERNATIONAL STANDARD ISO 17861:2014(E) ISO 2014 All rights reserved 1BS ISO 17861:2014ISO 17861:2014(E)3.5spectrophotometeroptical instrument that measures spectral transmittance or reflectanceNote 1 to entry: The instrument consist
27、s of optical source, monochromator, sample chamber, optical detector, signal processor, data processor, and interface.3.6double beam spectrophotometertype of spectrophotometer that is utilized to compare the light intensity between the reference sample and the test piecesNote 1 to entry: Compared to
28、 single-beam spectrophotometer measures, a high stability of measurements is obtained. The instrument consists of optics that divide a source light beam into two beams and two detectors. The instability of a source beam mainly due to that of the source lamp is compensated by that of a reference beam
29、.3.7integrating-sphereoptical component consisting of a hollow spherical cavity with its inner surface covered with a diffuse white reflective coatingNote 1 to entry: The cavity is equipped with small holes to set a sample piece and for inlet and outlet of the light beam.4 PrincipleFine ceramics thi
30、n films sometimes possess a voided micro columnar structure, depending on film deposition conditions. If a fine ceramics thin film with a voided structure is exposed to a certain atmosphere with humidity, moisture in the atmosphere adsorbs on surfaces of the columns consisting the voided structures.
31、 The quantity of adsorbed water is affected by hydrostatic vapor pressure in the atmosphere. Depending on the quantity of water adsorbed, the refractive index of thin films changes, resulting in the change in transmittance and reflectance. To evaluate effects of water adsorption on to surface of voi
32、ds of fine ceramics films on film optical properties, it is necessary to measure optical properties under a certain atmosphere, typically in an atmosphere with a high humidity. In addition to the measurements under a high humidity, for the sake of comparison, it is also necessary to measure the prop
33、erties in vacuum, i.e. under the condition without water adsorption and low humidity. By comparing optical transmittance measured in vacuum, low humidity, and high humidity conditions, the stability of fine ceramics thin films shall be evaluated.5 Ambient room environmentThe test shall be carried ou
34、t under an ambient laboratory room atmosphere where deviations in the temperature and humidity are small. In particular, to prevent the condensation of water in the environmental mini-chamber, after removing the mini-chamber from the humidity-temperature control chamber to the laboratory room, the a
35、mbient temperature should be controlled to a certain range. Recommended laboratory room conditions are the following:a) temperature: 23 C 2 C;b) relative humidity: below 70 %.NOTE Attention is needed to dew condensation when environment temperature is low compared to that in the humidity-temperature
36、 control chamber.6 Test pieceThe test piece shall comprise a single layer or multilayer of thin films of fine ceramic deposited on to the surface of a plate or film substrate, such as glass, polymer material, with no restriction of material for 2 ISO 2014 All rights reservedBS ISO 17861:2014ISO 1786
37、1:2014(E)the substrate if it is enough transparent in a certain range to measure transmittance of thin films. If it fits the environmental mini-chamber, in terms of size and shape, any test piece is acceptable.7 Measuring apparatus7.1 Apparatus configurationa) Spectrophotometer: Double beam method,
38、wavelength accuracy 0,2 nm or less at UV-visible light and 1,0 nm or less at near-infrared range, repeatability of wavelength setting 0,1 nm or less at UV-visible light and 0,5 nm or less at near infrared range. For UV-visible and near-infrared range measurements, the range of 300 nm to approximatel
39、y 2 500 nm is desirable. The use of the integrating sphere for photometer is recommended. In the case of measurements in a range in infrared and far-infrared, the wavelength range can be expanded by using an appropriate spectrometer.b) Environmental mini-chamber: An airtight container which could ma
40、intain the test sample in vacuum and low- and high-humidity environments for the measurements of the spectral of each environment. Build two windows with transparent quartz glass with the sample fixed inside the chamber for the measurement of light transmittance. Also build an air inlet and exhaust
41、ports, each with a valve. It is necessary to confirm that there is no vacuum leak from the chamber when all the valves are closed. In case of necessity, check the leak rate of the chamber by using a vacuum gauge.The spectrometry device configuration is shown in Figure 1. Example of the blueprint is
42、shown in Annex A.LSWS CMD SPDPRBVLMCSCTBSQWKeyLS light source TB test beamCM chopper mirror RB reference beamWS wavelength selector (monochrometer) MC environmental mini-chamberSC specimen compartment VL valveD detector QW quartz windowSP signal processor S specimenDP data processorFigure 1 device c
43、onfiguration for spectral transmittance measurement ISO 2014 All rights reserved 3BS ISO 17861:2014ISO 17861:2014(E)c) A vacuum evacuation (exhaust) equipment: A rotary pump or a dry pump shall be used. The type does not matter only if the ultimate pressure is less than 40 Pa and if the pumping spee
44、d is larger than 1,0 l/s.d) Temperature/humidity controlled chamber: Use types that can set the temperature at 23 C and that can set the relative humidity range from 40 % to 80 %. It is desirable to measure the humidity around the test sample using a hygrometer.7.2 Spectrometer calibrationPerform a
45、wavelength and transmittance calibration for the spectrophotometer apparatus as followsa) Wavelength calibration: The test method which uses optical glass filter, didymium, or holmium oxides shall be applied. For an infrared range, polystyrene can be used as a wavelength standard.b) Baseline correct
46、ion: Set spectral transmittance to 100 % in the range of the measuring wavelength by using the baseline adjustment function of the apparatus by measuring the transmittance of the environmental mini-chamber without setting a test piece in the chamber.Other baseline correction methods, e.g. correction
47、 for air, are acceptable, though the method applied should be reported.8 Environmental conditions and control proceduresEvacuate or expose the test piece to a required environmental condition in a temperature/humidity control chamber prior to optical transmittance measurements. The test piece should
48、 not be taken out from the environmental mini-chamber during a series of measurements of vacuum, low-humidity, and high-humidity conditions. Measurement environmental conditions recommended are vacuum, temperature of 23 C 2 C and R.H. of 80 % 2 %, and temperature of 23 C 2 C and R.H. of 40 % 2 % as
49、described in the following list. If necessary, the environmental test sequence may be modified.a) Vacuum: Evacuate the environmental mini-chamber containing a test piece inside by connecting one of its ports to a vacuum pump. Evacuate the chamber for longer than 30 min.NOTE To reduce the amount of water remaining in thin films after the evacuation, the environmental mini-chamber may be heated up to 130 C during evacuation. However, the mini-chamber is cooled to room temperature prior to the transmittance measurement.b)
