I E C 60758 ® I N TE R N ATI ON AL STAN DAR D IEC 60758:201 6-05(en) Syn th eti c q u artz crystal – Speci fi cati on s an d g u i d el i n es for u se Edition 5.0 201 6-05 TH I S P U B L I C ATI O N I S C O P YR I G H T P R O TE C TE D C o p yri g h t © I E C , G e n e va , Sw i t z e rl a n d All rights reserved Unless otherwise specified, no part of this publication may be reproduced or utilized in any form or by any means, electronic or mechanical, including photocopying and microfilm, without permission in writing from either IEC or IEC's member National Committee in the country of the requester If you have any questions about IEC copyright or have an enquiry about obtaining additional rights to this publication, please contact the address below or your local IEC member National Committee for further information IEC Central Office 3, rue de Varembé CH-1 21 Geneva 20 Switzerland Tel.: +41 22 91 02 1 Fax: +41 22 91 03 00 info@iec.ch www.iec.ch Abo u t th e I E C The International Electrotechnical Commission (IEC) is the leading global organization that prepares and publishes International Standards for all electrical, electronic and related technologies Ab o u t I E C p u b l i c a t i o n s The technical content of IEC publications is kept under constant review by the IEC Please make sure that you have the latest edition, a corrigenda or an amendment might have been published I EC C atal og u e - webstore i ec ch /catal o g u e E l ectro ped i a - www el ectro ped i a org The stand-alone application for consulting the entire bibliographical information on IEC International Standards, Technical Specifications, Technical Reports and other documents Available for PC, Mac OS, Android Tablets and iPad The world's leading online dictionary of electronic and electrical terms containing 20 000 terms and definitions in English and French, with equivalent terms in additional languages Also known as the International Electrotechnical Vocabulary (IEV) online I EC pu bl i cati on s search - www i ec ch /search pu b I E C G l o ssary - s td i ec ch /g l ossary The advanced search enables to find IEC publications by a variety of criteria (reference number, text, technical committee,…) It also gives information on projects, replaced and withdrawn publications 65 000 electrotechnical terminology entries in English and French extracted from the Terms and Definitions clause of IEC publications issued since 2002 Some entries have been collected from earlier publications of IEC TC 37, 77, 86 and CISPR I EC J u st Pu bl i s h ed - webstore i ec ch /j u stp u bl i s h ed Stay up to date on all new IEC publications Just Published details all new publications released Available online and also once a month by email I E C Cu s to m er S ervi ce Cen tre - webstore i ec ch /csc If you wish to give us your feedback on this publication or need further assistance, please contact the Customer Service Centre: csc@iec.ch I EC 60758 ® Edition 5.0 201 6-05 I N TER N ATI ON AL STAN DAR D Syn th eti c q u artz crystal – Speci fi cati o n s an d g u i d el i n es for u se INTERNATIONAL ELECTROTECHNICAL COMMISSION ICS 31 40 ISBN 978-2-8322-3395-5 Warn i n g ! M ake su re th at you obtai n ed th i s pu bl i cati on from an au th ori zed d i stri bu tor ® Registered trademark of the International Electrotechnical Commission –2– I EC 60758:201 © I EC 201 CONTENTS FOREWORD I N TRODU CTI ON Scope N ormati ve references Terms an d defin i tions Specification for syn th etic qu artz crystal Standard valu es Sh ape of syn thetic qu artz for optical applicati ons Ori en tation of the seed I nclu sion density Striae in synth etic qu artz for optical applications 4 I n frared qu ality indications of α 500 and α 585 for piezoel ectric applications 4 Grade cl assification by α valu e and Schl ieren m eth od for optical applications Frequ ency-temperatu re ch aracteristics of syn thetic qu artz for piezoelectric applicati ons Etch channel density ρ I n tern al transm i ttance for optical appl icati ons Requ irements and measu ri ng methods Ori en tation 2 H andedness Syn th etic qu artz crystal dimensions 4 Seed dim ensions I m perfections Evalu ati on of in frared qual ity by α measuremen t 22 Frequ ency versu s temperature characteristics for piezoelectric applications 24 Striae in synthetic quartz for optical appl ications 25 Growth band in syn thetic quartz for optical appl ications 25 Etch ch annel densi ty 26 1 I n tern al transm i ttance for optical appl icati ons 27 M arking 27 General 27 Sh ipping requ iremen ts 28 Specification for l um bered syn th etic qu artz crystal 28 Standard valu es 28 Tolerance of dimensions 28 Reference su rface flatness 29 An g u lar tolerance of reference su rface 29 Centrali ty of th e seed 30 Requ irements and measu ri ng methods 31 As-g rown qu artz bars u sed for lu mbered qu artz bars 31 2 Dim ensions of lu mbered syn thetic qu artz crystal 31 I den tificati on on reference su rface 31 M easurement of reference surface flatness 31 I EC 60758:201 © I EC 201 –3– M easurement of reference surface an g le tolerance 31 5 Centrali ty of th e seed 31 Deli very conditions 32 General 32 M arking 32 3 Packin g 32 M aking batch 32 I nspection ru le for syn thetic qu artz crystal and lum bered syn th etic qu artz crystal 32 I nspection ru le for as-g rown syn th etic quartz crystal 32 I nspection 32 Lot-by-lot test 32 I nspection ru le for lum bered syn thetic qu artz crystal 33 General 33 2 Lot-by-lot test 34 Gu ideli nes for the u se of syn thetic qu artz crystal for piezoelectric applications 34 General 34 Overvi ew 34 Syn th etic qu artz crystal 34 Sh ape and size of syn theti c qu artz crystal 35 Crystal axis and face design ati on 35 2 Seed 36 Sh apes and di mensions 36 Growth zones 37 Standard method for evalu ati ng th e qu ali ty of syn thetic qu artz crystal 37 Other meth ods for checkin g the qu al i ty of syn thetic qu artz crystal 38 General 38 Vi su al inspection 38 I n frared radiation absorption method 38 4 M iscel laneou s 39 α grade for piezoelectric quartz 40 Opti onal g radin g (only as ordered) , in inclu sions, etch channels, Al ten t 40 I nclu sions 40 Etch ch annels 40 Al conten t 40 Swept qu artz 41 7 Orderin g 42 An nex A (in formati ve) Frequen tl y used sampli ng procedu res 43 A Complete vol u me cou ntin g 43 A Comm odity Y-bar samplin g – M eth od 43 A Comm odity Y-bar samplin g – M eth od 43 A U se of com parative standards for 00 % crystal inspection 44 An nex B (in formati ve) N u merical example 45 An nex C (in formati ve) Example of reference sam ple selection 46 An nex D (in formati ve) Explanations of poin t cal lipers 47 An nex E (i nformati ve) I n frared absorbance α valu e compensation 48 General 48 E E Sample preparation, equ ipmen t set-u p and measu ri ng procedu re 48 E General 48 –4– I EC 60758:201 © I EC 201 Sample preparation 48 E 2 E Equ ipmen t set-up 48 E M easurement procedure 49 E Procedu re to establ ish correction terms 49 E Calcu lation of compensated (corrected) absorbance valu es 51 Annex F (in formati ve) Di fferences of the orthogonal axial system for qu artz between I EC standard and I EEE standard 52 Annex G (in formative) α valu e measu rem en t consistency between dispersive in frared spectrometer and fou rier transform i nfrared spectrometer 54 G General 54 G Experimen t 54 G Experimen tal resu l t 55 Bi bliog raph y 58 Fi gu re – Qu artz crystal axis and cu t direction Fi gu re – I dealized sections of a synth etic quartz crystal g rown on a Z-cu t seed Fi gu re – Typical example of cu tting wafers of AT-cu t plate, or rhom bohedral -cu t plate, X-cu t plate, Y-cu t plate and Z-cu t pl ate 21 Fi gu re – Frequ ency-tem peratu re ch aracteristics deviation rate of the test specimen 25 Fi gu re – Typical sch lieren system setu p 25 Fi gu re – Lu mbered syn thetic qu artz crystal ou tline an d dim ensions along X-, Y- an d Z-axes 29 Fi gu re – An gu lar deviati on for reference su rface 30 Fi gu re – Cen tral ity of the seed with respect to th e dim ension al ong the Z- or Z'-axis 31 Fi gu re – Qu artz crystal axis and face design ati on 36 Fi gu re – Syn th etic quartz crystal g rown on a Z-cu t seed of smal l X-dimensions 37 Fi gu re 1 – Example of a relati on between th e α valu e an d th e Q valu e at wave nu mber 500 cm -1 39 Fi gu re D – Poin t call ipers 47 Fi gu re D – Dig ital poin t cal li pers 47 Fi gu re E – Schematic of measurem ent set-u p 49 Fi gu re E – Graph relationsh ip between averaged α and measu red α at two wave nu m bers of α 500 and α 585 50 Fi gu re F – Left- an d rig h t-handed quartz crystals 53 Fi g ure G – Relationsh ip of α between m easuring val ue and reference valu e 57 Table – I nclusion densi ty grades for pi ezoelectri c applications Table – I nclusion densi ty g rades for optical appl icati ons Table – I n frared absorbance coefficien t grades for pi ezoelectric applicati ons Table – I n frared absorbance coefficien t g rades and Sch l ieren m ethod for optical applications Table – Etch chan nel densi ty g rades for piezoelectric appl ications Table – Test condi ti ons and requ irem en ts for the lot-by-I ot test for grou p A 33 Table – Test condi ti ons and requ irem en ts for the lot-by-lot test for g roup B 33 Table – Test condi ti ons and requ irem en ts for the lot-by-lot test 34 Table B – Comm odity bar sampli ng , method 45 I EC 60758:201 © I EC 201 –5– Table B – Comm odity bar sampli ng 45 Table E – Example of calibration data at α 585 50 Table E – Example of calibration data at α 500 50 –6– I EC 60758:201 © I EC 201 I NTERNATI ONAL ELECTROTECHN I CAL COMMI SSI ON SYNTHETIC QUARTZ CRYSTAL – SPECIFICATIONS AND GUIDELINES FOR USE FOREWORD ) Th e I n tern ati on al El ectrotech n i cal Com m i ssi on (I EC) i s a worl d wi d e org an i zati on for stan dard i zati on com pri si n g al l n ati on al el ectrotech n i cal com m i ttees (I EC N ati on al Com m i ttees) Th e obj ect of I EC i s to prom ote i n tern ati on al co-operati on on al l q u esti on s cern i n g stan d ard i zati on i n th e el ectri cal an d el ectron i c fi el d s To th i s en d an d i n ad d i ti on to oth er acti vi ti es, I EC pu bl i sh es I n tern ati on al Stan d ard s, Tech n i cal Speci fi cati on s, Tech n i cal Reports, Pu bl i cl y Avai l abl e Speci fi cati on s (PAS) an d G u i d es (h ereafter referred to as “I EC Pu bl i cati on (s) ”) Th ei r preparati on i s en tru sted to tech n i cal com m i ttees; an y I EC N ati on al Com m i ttee i n terested i n th e su bj ect d eal t wi th m ay parti ci pate i n th i s preparatory work I n tern ati on al , g overn m en tal an d n on -g overn m en tal org an i zati on s l i si n g wi th th e I EC al so parti ci pate i n th i s preparati on I EC col l aborates cl osel y wi th th e I n tern ati on al Org an i zati on for Stan d ard i zati on (I SO) i n accord an ce wi th d i ti on s d eterm i n ed by ag reem en t between th e two org an i zati on s 2) Th e form al d eci si on s or ag reem en ts of I EC on tech n i cal m atters express, as n earl y as possi bl e, an i n tern ati on al sen su s of opi n i on on th e rel evan t su bj ects si n ce each tech n i cal com m i ttee h as represen tati on from al l i n terested I EC N ati on al Com m i ttees 3) I EC Pu bl i cati on s h ave th e form of recom m en d ati on s for i n tern ati on al u se an d are accepted by I EC N ati on al Com m i ttees i n th at sen se Wh i l e al l reason abl e efforts are m ad e to en su re th at th e tech n i cal ten t of I EC Pu bl i cati on s i s accu rate, I EC can n ot be h el d respon si bl e for th e way i n wh i ch th ey are u sed or for an y m i si n terpretati on by an y en d u ser 4) I n ord er to prom ote i n tern ati on al u n i form i ty, I EC N ati on al Com m i ttees u n d ertake to appl y I EC Pu bl i cati on s tran sparen tl y to th e m axi m u m exten t possi bl e i n th ei r n ati on al an d reg i on al pu bl i cati on s An y d i verg en ce between an y I EC Pu bl i cati on an d th e correspon d i n g n ati on al or reg i on al pu bl i cati on sh al l be cl earl y i n di cated i n th e l atter 5) I EC i tsel f does n ot provi d e an y attestati on of form i ty I n d epen d en t certi fi cati on bodi es provi d e form i ty assessm en t servi ces an d , i n som e areas, access to I E C m arks of form i ty I EC i s n ot respon si bl e for an y servi ces carri ed ou t by i n d epen d en t certi fi cati on bodi es 6) Al l u sers sh ou l d en su re th at th ey h ave th e l atest edi ti on of th i s pu bl i cati on 7) N o l i abi l i ty sh al l attach to I EC or i ts di rectors, em pl oyees, servan ts or ag en ts i n cl u di n g i n d i vi d u al experts an d m em bers of i ts tech n i cal com m i ttees an d I EC N ati on al Com m i ttees for an y person al i n j u ry, property d am ag e or oth er d am ag e of an y n atu re wh atsoever, wh eth er di rect or i n di rect, or for costs (i n cl u di n g l eg al fees) an d expen ses ari si n g ou t of th e pu bl i cati on , u se of, or rel i an ce u pon , th i s I EC Pu bl i cati on or an y oth er I EC Pu bl i cati on s 8) Atten ti on i s d rawn to th e N orm ati ve referen ces ci ted i n th i s pu bl i cati on U se of th e referen ced pu bl i cati on s i s i n di spen sabl e for th e correct appl i cati on of th i s pu bl i cati on 9) Atten ti on i s d rawn to th e possi bi l i ty th at som e of th e el em en ts of th i s I EC Pu bl i cati on m ay be th e su bj ect of paten t ri g h ts I EC sh al l n ot be h el d respon si bl e for i den ti fyi n g an y or al l su ch paten t ri g h ts I n tern ati onal Stan dard I EC 60758 h as been prepared by I EC techn ical commi ttee 49: Pi ezoel ectric, dielectric and electrostatic devices and associated materials for frequ ency trol , selection and detection Th is fi fth edition cancels and replaces the fou rth edition , pu blished in 2008 This edition consti tu tes a techn ical revisi on Th is edi tion i ncludes the fol lowin g sig ni fican t tech nical chang es with respect to the previou s edi tion : • • • • order rearran g ement and review of terms and defin i tions; abolition as a standard of th e i nfrared absorbance coefficien t α 41 0; addi ti on of th e α val ue m easu remen t explan ation by FT-I R equ ipmen t in ann ex; addi tion of th e syn th etic qu artz crystal standards for optical appl ications I EC 60758:201 © I EC 201 –7– The text of this standard i s based on th e foll owing docu men ts: FDI S Report on voti n g 49/1 85/FDI S 49/1 90/RVD Fu ll i n formati on on the votin g for the approval of th is stan dard can be fou nd in the report on votin g i ndicated i n the above table Th is pu blication has been drafted in accordance with th e I SO/I EC Directives, Part The com mi ttee h as decided th at the ten ts of this pu blicati on wil l remain u nch ang ed u n ti l the stabi l ity date in dicated on the I EC website u n der "http://webstore iec ch" in th e data related to th e speci fic publication At th is date, th e pu blication wil l be • recon firmed, • wi thdrawn , • replaced by a revised edition , or • amended A biling u al versi on of th is publication m ay be issu ed at a later date –8– I EC 60758:201 © I EC 201 I NTRODUCTI ON The reason for adding synthetic qu artz crystal for optical appl ication to th is I n ternational Standard is as fol lows Quartz crystal produced for optical applicati ons is produ ced by man y of th e same suppliers m an u factu rin g quartz for el ectron ic applications The equ ipmen t and meth ods to produ ce optical qu artz are si mi lar to those used i n the production of electron ic qu artz Also, wi th a few exceptions th e characterizati on methods of electron ic an d optical m aterial are simi lar Therefore, I EC 60758 serves as the proper basis for including addenda related to quartz crystal for optical appl ications – 48 – I EC 60758:201 © I EC 201 Annex E (informative) Infrared absorbance α value compensation E.1 General I t i s wel l kn own that α valu es measu red in different laboratories usi ng the procedures recom mended in th is stan dard and u sing sim i lar equ ipment to each other resu l t in m easu remen ts with deviations between laboratories beyond th e li m its of accu racy requi red to assu re conformance to th e α requ irements of th is standard To address th is issu e and to establish correl ation between laboratories, a Rou nd Robin was conducted in vol ving fi ve (5) samples wi th a wide ran g e of α valu es an d over twen ty (20) laboratories A procedure to establish correcti on terms based on the di fferences between indi vidual resul ts and th e averag es across laboratories at constan t wave n um bers and sampl es was establ ish ed The same methods described i n Annex E m ay be applied to establ ish correcti on terms i n the fu ture The Rou n d Robin incl uded g ratin g based I R spectroph otometers usi ng a dispersi ve fi g uration and FT-I R equ ipment, th us all owi ng the process to be applied to equ ipmen t using eith er measu ri ng m ethod E.2 Sample preparation, equipment set-up and measuring procedure E.2.1 General To redu ce th e variation between l aboratori es, a set of recomm endati ons concern in g sample preparation , equ ipmen t set-u p, and measu rin g procedu re is described E.2.2 Sample preparation The su gg ested sample preparati on procedu re is as follows: • • sample cu t from th e Z-zone, not inclu ding any porti on of th e seed; • th e th ickness (Y) shou ld be mm ± 0, mm The dimensions for X and Z shoul d be as ven ien t and establish ed in consideration of th e m easuring apertu re; • th e an gu lar devi ation of the surface n orm al on the X and Y faces is less than 30' from the correspondin g crystal axi s; • th e X and Z faces are g rou nd to a rou g h ness ach ieved by mesh #80 diamon d g rit or roug her li g ht propag ation is along th e Y-axis Y-faces are pol ished to a state comm on l y referred to as "optical inspection g rade"; E.2.3 Equipment set-up A diag ram of th e usu al instru men t config uration i s shown i n Fi gu re E I EC 60758:201 © I EC 201 – 49 – Detector Aperture Sample Focal plane of probe beam IEC Figure E.1 – Schematic of measurement set-up The sam ple is posi ti oned so that the beam exi t su rface is within mm of the focal plane and the focal pl ane is between th e test sample and the apertu re The instru men t setting s (scan speed of FTI R, sl it width i n grating spectrometer) shou ld ensu re th at the waveleng th resol u tion is abou t 6, cm –1 ± 0, cm –1 The aperture size is mm × mm The mm di mension is along th e crystal X directi on The apertu re is positioned between the sample an d the focal plane i n su ch a way that the transmission is maximized at the reference wave n u m ber Wi th the sam ple removed, the instru men t is cal ibrated to read 00 % transm ission at all reference and absorption wave nu mber setting s The reference wave n um bers are 800 cm –1 ± cm –1 and 979 cm –1 ± cm –1 The absorption wave nu mbers are 500 cm –1 ± cm –1 and 585 cm –1 ± cm –1 The absorption wave nu m ber settin g for the 585 cm –1 measu rem en t shou ld be adjusted to achieve the l ocal m inim u m valu e of transmission The measu remen t tem peratu re is ° C － 25 ° C The measu remen t relative hu mi dity is 70 % or less E.2.4 Measurement procedure U ncorrected absorbance valu es at any of the two absorption wave nu mbers are calcu lated by using the form u la in T1 is evalu ated at the same reference wave nu mber that was u sed to establish the cali brati on terms described i n Clau se E I n a g rating spectrom eter, the m easu remen ts sh ou ld be m ade withou t scann ing th e wave n u m ber Th e sam ples shou l d have th e beam centred inside th e apertu re Consisten t positioni ng of the samples can be ach ieved with dedicated sample-holders E.3 Procedure to establish correction terms The procedu re to establ ish correction terms is perform ed i ndependen tl y for an y of the two absorpti on wave nu mbers, and th e exam pl e here shou ld only discuss the case of 500 cm –1 The samples used for th e Rou nd Robi n or an equ i valen t set of samples are measu red as described in E 2 and E – 50 – I EC 60758:201 © I EC 201 An exampl e of th e cali bration method is shown bel ow A set of fi ve (5) standard samples was tested by several laboratories and an averag e of u ncorrected data determin ed (inclu sive of all instruments) at the two wave nu mber combin ati ons and labell ed "averaged" in Tables E and E The measu remen ts of one laboratory are shown an d l abelled "measu red" Table E.1 – Example of calibration data at α 585 Averag ed Measu red 0, 01 0, 01 5 0, 038 0, 037 0, 062 0, 059 0, 55 0, 53 0, 36 0, 37 Table E.2 – Example of calibration data at α 500 Averag ed Measu red 0, 026 0, 025 0, 038 0, 036 0, 051 0, 047 0, 30 0, 23 0, 07 0, 07 Th is data is g raphical ly sh own i n Fig u re E wi th the corresponding least squ are fit of a lin ear approximation Cal i brati on cu rve at α 585 0, ＝ 0, 994 x ＋ 0, 001 y 0, Averag ed Averag ed α 585 y 0, α 350 0, 20 Cal i brati on cu rve at α 50 0, 05 0, 00 0, 00 0, 05 M easu red 0, 0, α 58 IEC ＝ , 029 9x ＋0, 001 0, 0, 05 0, 00 0, 00 0, 05 M easu red 0, α 50 0, IEC Figure E.2 – Graph relationship between averag ed α and measured α at two wave numbers of α 500 and α 585 The calibration terms calcu lated in th ese two exam ples are factor a = , 029 and offset b = + 0, 001 cm –1 at α 500 , a = 0, 994 an d offset b = + 0, 001 at α 585 I EC 60758:201 © I EC 201 E.4 – 51 – Calculation of compensated (corrected) absorbance values After the correcti on terms are known for the measu rem en t set-u p and waveleng th of in terest, th e sampl e to be evalu ated is m easu red according to E The corrected absorbance valu e α corrected is calcu lated from the u ncorrected m easu remen t α u sing the fol lowin g form u la and th e correcti on terms a and b as defi ned i n Clau se E α corrected = a α + b – 52 – I EC 60758:201 © I EC 201 Annex F (informative) Differences of the orthogonal axial system for quartz between IEC standard and IEEE standard I EEE revised I EEE Stan dard 76-1 946 i n 978 and revised it ag ain to issue i t as I EEE Standard 76-1 987 in 987 The main revision poi n t is th e + X in version of orthog onal crystal axis sh own in Fi g ure F and i t is different from that of th e present I EC 60758 The di fferences between I EEE 76-1 987 and I EC 60758 are gi ven below a) Righ t-handed qu artz is expressed by the righ t-handed orth og onal axi al system , also l eft-h an ded qu artz is expressed by th e left-han ded orthog onal axi al system in I EC 60758 H owever, the rig h t-han ded orth og onal axial system is applied for ri gh t-h anded and l eft-h anded quartz in I EEE 76-1 987 b) For rig h t-han ded qu artz, the relati on between I EC 60758 and I EEE Standard 76-1 987 is th at of rotated 80 deg rees arou nd th e Z-axis For left-han ded quartz, the relation between I EC 60758 and I EEE 76-1 987 is that of reversed Y-axis c) Al l material constan t valu es of left-handed qu artz are th e same as the m aterial constan t valu es of righ t-handed qu artz in I EC 60758 I n I EEE 76-1 987, however, elastic constan t of rig ht-handed qu artz an d left-handed qu artz are the same, bu t the plu s or m inu s si gn of the piezoelectric constan t is reverse to each oth er d) I n I EC 60758, the elastic constan t of C is a n eg ative qu an ti ty and th e piezoelectric constan t of e 1 is a neg ative val ue an d that of e i s a posi ti ve valu e On th e other h and, in I EEE 76-1 987, all these quan ti ties, th at is, C 4, e 1 and e , are posi ti ve valu es e) According to I EC 60758, for example AT-cu t at rig h t-handed qu artz is call ed + 35° rotated Y-cu t H owever, accordin g to I EEE 76-1 987, i t shou ld be called –35° rotated Y-cu t N ow, in al l i n ternational academic papers, quartz m aterial constants are wri tten based on I EEE Standard 76-1 987 Care shoul d be taken to avoid confusion wh ich m ay be cau sed by the expression di fferences of m aterial constan ts and crystal axes between I EEE 76-1 987 and I EC 60758 I EC 60758:201 © I EC 201 – 53 – ANSI/IEEE Std 76-1 987 987 IEEE Z +X +X +X r r Y AXIS Z +X Z Z Y AXIS r r Z Z +X AXIS +X AXIS Z AXIS z –MINOR FACE r x Z + r –MAJOR FACE Z AXIS z –MINOR FACE +X AXIS r Z x +X AXIS DT AT CT GT a) – Left-Handed Quartz s + ON TENSION ON COMPRESSION BT r –MAJOR FACE BT DT AT CT GT b) – Right-Handed Quartz Figure F.1 – Left- and right-handed quartz crystals IEC – 54 – I EC 60758:201 © I EC 201 Annex G (informative) α value measurement consistency between dispersive infrared spectrometer and fourier transform infrared spectrometer G.1 General Dispersive in frared spectrometer has been mainly ven tion al measu rin g equ ipm en t for the determi nation of infrared absorpti on of α coeffici en t H owever, the Dispersi ve I n frared Spectrometer, wh ich was applied for th e measurement method in Annex E, h as n ot been comm onl y on the sale an ymore for th e last decade Fou rier transform infrared spectrometer (FT-I R) is now availabl e to measu re in frared absorbance of the materi al I EC 60758:2008 an d J apanese N ation al Stan dard J I S C 6704 [33] were revised in 999 I n th e correspondin g version , α was also measu red by FT-I R meth od and i ts resu l t was verified that the same resu lt can be obtain ed as on e by I n frared Spectrometer I n the m easurement, th e du al beam system i n the FT-I R system was appl ied The dual beam system u ses one beam as a reference ligh t, and si mu ltaneousl y cali brates the measured sig nal of the sample Therefore the base line drift was compensated H owever, the corresponding system was not a comm on FT-I R Spectroscopy Common FT-I R Spectroscopy is g enerall y sing le-beam system , i n which the stabi li ty of base l ine is believed to be in ferior to a du al beam system To firm that the ven tional sing le beam FT-I R spectroscopy is also appl icabl e, the re-exam in ati on test was execu ted G.2 Experiment The same qu artz crystal specim ens, which were u sed i n a Round Robi n test in Annex E, were measured by both I nfrared spectrometer and FT-I R Spectroscopy I n this experiment, FT-I R equ ipmen t comm ercially avail able of fou r companies was employed Those resu lts were carefu l ly exam i ned The criteria valu e to determ in e a satisfyin g dition was a tolerance value of the m easu rem en t performed in a Rou n d Robi n test in An nex E, wh ich were ± 2, % for 585 cm –1 and ± % for 500 cm –1 Measurin g conditions for FT-I R measurem en t are reconsidered as foll ows (refer to an d Annex E) : a) The sample sh all be placed u nder th e dition , where (a) th e l ig h t emerg ence plane is posi tioned wi th in mm from focal plan e an d, (b) th e focu s poin t shall be l ocated between the speci men and the apertu re b) The scan speed of FT-I R shal l be adjusted to m ake the resolu ti on of wave n um ber i n a rang e from , cm –1 to 4, cm –1 The apertu re size shall be from mm φ to mm φ The ligh t shal l be al ig ned along Y axi s The X axis of specimen shall be upward The accum u lation nu mbers for FT-I R system shal l be more th an ti mes The apertu re is posi tioned between th e sam ple and the focal plan e i n such a way that the transm ission is maximized at the reference wave n um ber g ) With the sam ple removed, the i nstru men t is calibrated to read 00 % transm ission at all reference and absorption wave nu mber setti ng s c) d) e) f) h ) The reference wave n u mbers are 800 cm –1 ± cm –1 and 979 cm –1 ± cm –1 i) The air in a sample cham ber shall be replaced wi th a dried air I EC 60758:201 © I EC 201 G.3 – 55 – Experimental result Japanese N ational Comm ittee has performed a rou nd Robin test i n five qu artz crystal compan ies Fi ve sam ples wi th variou s α valu es, wh ich were exactly the same samples u sed in a roun d Robin test in 999, were prepared for measu ring infrared absorption coefficien ts Th en averag ed valu es, Maximu m valu es, and im um valu es obtained from the test were referred by th e n ew testin g system Th e perm issibl e levels were defin ed so that th e m easured valu es cou ld be plotted with in the range between th e m axi mu m and m i ni mum valu es of referred resu lts Au tocorrelation graph between reference α and measured α for wave leng th of 500 cm –1 are shown in Fig u res G a) to G d) The dotted line represents th e recomm en ded reference val u e and the sol id li ne is a measu red valu e Measu red α val ues were plotted in a range between the m aximu m an d m in imu m valu es of referred resul ts Al l measu red resu l ts were in perm issi ble l evels so that th e measuri ng system u sing FT-I R system is precise enoug h u nder the condition sh own in Clau se G I n additi on , Fi g ures G e) -G h) show the au tocorrel ati on plot of reference α and m easu red α for th e wave l en g th of 585 cm –1 Measu red α valu es were plotted in a ran g e between the m aximu m an d m in im u m valu es of referred resul ts Al l measu red resu l ts were in perm issi ble l evels as in th e 500 cm –1 measu rem en t The precise measu remen t was performed in the same way as 500 cm –1 wave l en g th case The absorbance peak at 585 cm –1 is di fficu lt to detect wi th poor wave l eng th resolu tion , si nce th e peak is very sh arp and narrow Therefore the m easu remen t using 585 cm –1 is on e of the m ost di fficul t m ethods by u sin g in frared spectrometer U p to now, 500 cm –1 wave len g th was rather ch osen for obtaini ng α valu es in conven ti onal m easu remen ts, because this absorbance peak is pretty sh allow an d easy to m easure absorbance The wave leng th resolu ti on in FT-I R m easu ring system is theoretical ly very h ig h, th erefore measu red peak i n a spectrum at 585 cm –1 was very sharp and the measured α had small errors after several measurem en ts All m easu red valu es are wi th in th e reference values wi th small tolerances An d the resu l ts are also i den tical to ones from I n frared spectroscopy These resu lts sh owed the FT-I R measuremen t curren tl y avai lable was firmed to be applicable for th e determ in ation of α valu es – 56 – IEC a) – Maker A 20 times accumulation α 50 IEC c) – Maker C times accumulation α 500 I EC 60758:201 © I EC 201 IEC b) – Maker B times accumulation α 50 IEC d) – Maker D 20 times accumulation α 500 IEC e) – Maker A 20 times accumulation α 585 IEC f) – Maker B times accumulation α 585 I EC 60758:201 © I EC 201 – 57 – IEC IEC g) – Maker C times accumulation α 585 h) – Maker D 20 times accumulation α 585 Figure G.1 – Relationship of α between measuring value and reference value – 58 – I EC 60758:201 © I EC 201 Bibliography General [1 ] R A Laudise an d J W N ielsen : H ydroth erm al Crystal Growth (Academ ic Press I nc : Sol id State Ph ysics, v 2, p 49) [2] W J Spencer: Observation of Resonan t Vibrati ons and Defect Stru ctu re in Sing le Crystals by X-ray Di ffracti on Topog raph y (Academ ic Press: Ph ysical Acoustics, v 5, p 111) [3] D B Fraser: I m purities and Anelasticity i n Crystall i ne Qu artz (Academ ic 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Measurement of reflectance of plane surfaces and transmittance of plane parallel elements _ I N TE RN ATI O N AL E LE C TR OTE C H N I C AL CO M M I S SI O N , ru e d e Vare m bé PO Box 31 CH -1 21 G e n e va S wi tze rl an d Te l : + 41 Fax: + 22 9 1 22 9 0 i n fo @ i e c ch www i e c ch