Iec 60758 2016

INTRODUCTION The re son for ad in s nthetic q artz cry tal for o tical a pl cation to this International Stan ard is as fol ows.. SYNTHETIC QUARTZ CRYSTAL – SPECIFICATIONS AND GUIDELINES

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CONTENTS

FOREWORD 6

INTRODUCTION 8

1 Sco e 9

2 Normative referen es 9

3 Terms an definition 9

4 Sp cification for s nthetic q artz cry tal 13 4.1 Stan ard values 13 4.1.1 Sha e of s nthetic q artz for o tical a pl cation 13 4.1.2 Orientation of the se d 13 4.1.3 In lu ion den ity 13 4.1.4 Stria in s nthetic q artz for o tical a pl cation 14 4.1.5 Infrared q al ty in ication of α 3 5 0 an α 3 5 5 for piezo lectric a plcation 14 4.1 6 Grade clas ification by α value an Sc l eren method for o tical a plcation 15 4.1.7 Freq en y- emp rature c aracteristic of s nthetic q artz for piezo lectric a plcation 15 4.1.8 Etc c an el den ity ρ 15 4.1.9 Internal tran mitan e for o tical a pl cation 16 4.2 Req irements an me s rin method 17 4.2.1 Orientation 17 4.2.2 Han ed es 18 4.2.3 Sy thetic q artz cry tal dimen ion 18 4.2.4 Se d dimen ion 19 4.2.5 Imp rfection 19 4.2.6 Evaluation of infrared q al ty by α me s rement 2

4.2.7 Freq en y vers s temp rature c aracteristic for piezo lectric a plcation 2

4.2.8 Stria in s nthetic q artz for o tical a pl cation 2

4.2.9 Growth b n in s nthetic q artz for o tical a pl cation 2

4.2.10 Etc c an el den ity 2

4.2.1 Internal tran mitan e for o tical a pl cation 2

4.3 Markin 2

4.3.1 General 2

4.3.2 Ship in req irements 2

5 Sp cification for lumb red s nthetic q artz cry tal 2

5.1 Stan ard values 2

5.1.1 Toleran e of dimen ion 2

5.1.2 Referen e s rface flatnes 2

5.1.3 An ular toleran e of referen e s rface 2

5.1.4 Central ty of the se d 3

5.2 Req irements an me s rin method 31

5.2.1 As-grown q artz b rs u ed for lumb red q artz b rs 31

5.2.2 Dimen ion of lumb red s nthetic q artz cry tal 31

5.2.3 Identification on referen e s rface 31

5.2.4 Me s rement of referen e s rface flatnes 31

5.2.5 Me s rement of referen e s rface an le toleran e 31

5.2.6 Central ty of the se d 31

5.3 Del very con ition 3

5.3.1 General 3

5.3.2 Markin 3

5.3.3 Packin 3

5.3.4 Ma in b tc 3

6 In p ction rule for s nthetic q artz cry tal an lumb red s nthetic q artz cry tal 3

6.1 In p ction rule for as-grown s nthetic q artz cry tal 3

6.1.1 In p ction 3

6.1.2 L t by-lot test 32 6.2 In p ction rule for lumb red s nthetic q artz cry tal 33 6.2.1 General 3

6.2.2 L t by-lot test 34 7 Guidel nes for the u e of s nthetic q artz cry tal for piezo lectric a pl cation 3

7.1 General 3

7.1.1 Overview 3

7.1.2 Sy thetic q artz cry tal 3

7.2 Sha e an size of s nthetic q artz cry tal 3

7.2.1 Cry tal axis an face desig ation 3

7.2.2 Se d 3

7.2.3 Sha es an dimen ion 3

7.2.4 Growth zones 3

7.3 Stan ard method for evaluatin the q al ty of s nthetic q artz cry tal 3

7.4 Other method for c eckin the q al ty of s nthetic q artz cry tal 3

7.4.1 General 3

7.4.2 Vis al in p ction 3

7.4.3 Infrared radiation a sorption method 3

7.4.4 Mis el ane u 3

7.5 α grade for piezo lectric q artz 4

7.6 Optional gradin (only as ordered), in in lu ion , etc c an els, Al content 4

7.6.1 In lu ion 40 7.6.2 Etc c an els 4

7.6.3 Al content 40 7.6.4 Swe t q artz 41

7.7 Orderin 4

(informative) Freq ently u ed sampl n proced res 4

An ex A A.1 Complete volume cou tin 4

A.2 Commodity Y-b r sampl n – Method 1 4

A.3 Commodity Y-b r sampl n – Method 2 4

A.4 Use of comp rative stan ard for 10 % cry tal in p ction 4

(informative) Numerical example 4

An ex B (informative) Example of referen e sample selection 4

An ex C (informative) Explanation of p int cal p rs 4

An ex D (informative) Infrared a sorb n e α value comp n ation 4

An ex E E.1 General 4

E.2 Sample pre aration, eq ipment set up an me s rin proced re 48

E.2.2 Sample pre aration 4

E.2.3 Eq ipment set up 4

E.2.4 Me s rement proced re 4

E.3 Proced re to esta l s cor ection terms 4

E.4 Calc lation of comp n ated (cor ected) a sorban e values 51

(informative) Diferen es of the orthogonal axial s stem for q artz b twe n An ex F IEC stan ard an IEEE stan ard 5

(informative) α value me s rement con isten y b twe n disp rsive infrared An ex G sp ctrometer an fourier tran form infrared sp ctrometer 5

G.1 General 5

G.2 Exp riment 5

G.3 Exp rimental res lt 5

Bibl ogra h 5

Fig re 1 – Quartz cry tal axis an c t direction 17 Fig re 2 – Ide l zed section of a s nthetic q artz cry tal grown on a Z-c t se d 19 Fig re 3 – Typical example of c t in wafers of AT-c t plate, minor rhomb hedral-c t plate, X-c t plate, Y-c t plate an Z-c t plate 21

Fig re 4 – Freq en y- emp rature c aracteristic deviation rate of the test sp cimen 2

Fig re 5 – Typical s hl eren s stem setup 2

Fig re 6 – Lumb red s nthetic q artz cry tal outl ne an dimen ion alon X-, Y- an Z-axes 2

Fig re 7 – An ular deviation for referen e s rface 3

Fig re 8 – Central ty of the se d with resp ct to the dimen ion alon the Z- or Z'-axis 31

Fig re 9 – Quartz cry tal axis an face desig ation 3

Fig re 10 – Sy thetic q artz cry tal grown on a Z-c t se d of smal X-dimen ion 3

Fig re 1 – Example of a relation b twe n the αvalue an the Q value at wave n mb r 3 5 0 cm -1 3

Fig re D.1 – Point cal p rs 4

Fig re D.2 – Digital p int cal p rs 47 Fig re E.1 – Sc ematic of me s rement set up 4

Fig re E.2 – Gra h relation hip b twe n averaged α an me s red α at two wave n mb rs of α 3 5 0 an α 3 5 5 5

Fig re F.1 – L f - an rig t han ed q artz cry tals 5

Fig re G.1 – Relation hip of α b twe n me s rin value an referen e value 5

Ta le 1 – In lu ion den ity grades for piezo lectric a pl cation 14 Ta le 2 – In lu ion den ity grades for o tical a pl cation 14 Ta le 3 – Infrared a sorb n e co f icient grades for piezo lectric a pl cation 14 Ta le 4 – Infrared a sorb n e co f icient grades an Sc l eren method for o tical a pl cation 15 Ta le 5 – Etc c an el den ity grades for piezo lectric a pl cation 16 Ta le 6 – Test con ition an req irements for the lot by-Iot test for group A 3

Ta le 7 – Test con ition an req irements for the lot by-lot test for group B 3

Ta le 8 – Test con ition an req irements for the lot by-lot test 34

Ta le B.2 – Commodity b r sampl n 4

Ta le E.1 – Example of cal bration data at α

3 5 5 5

Ta le E.2 – Example of cal bration data at α

3 5 0 5

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International Stan ard IEC 6 7 8 has b en pre ared by IEC tec nical commit e 4 :

Piezo lectric, dielectric an electrostatic devices an as ociated materials for freq en y

control, selection an detection

This fif h edition can els an re laces the fourth edition, publ s ed in 2 0 This edition

con titutes a tec nical revision

This edition in lu es the fol owin sig ificant tec nical c an es with resp ct to the previou

edition:

• order re r an ement an review of terms an definition ;

• a oltion as a stan ard of the infrared a sorb n e co ficient α

3 410;

• ad ition of the α value me s rement explanation by FT-IR eq ipment in an ex;

• ad ition of the s nthetic q artz cry tal stan ard for o tical a pl cation

The text of this stan ard is b sed on the fol owin doc ments:

Ful information on the votin for the a proval of this stan ard can b fou d in the re ort on

votin in icated in the a ove ta le

This publcation has b en drafed in ac ordan e with the ISO/IEC Directives, Part 2

The commit e has decided that the contents of this publ cation wi remain u c an ed u ti the

sta i ty date in icated on the IEC we site u der "ht p:/we store.iec.c " in the data related to

the sp cific publ cation At this date, the publ cation wi b

INTRODUCTION

The re son for ad in s nthetic q artz cry tal for o tical a pl cation to this International

Stan ard is as fol ows

Quartz cry tal prod ced for o tical a pl cation is prod ced by man of the same s p l ers

man facturin q artz for electronic a pl cation The eq ipment an method to prod ce

o tical q artz are simi ar to those u ed in the prod ction of electronic q artz Also, with a few

ex e tion the c aracterization method of electronic an o tical material are simi ar

Therefore, IEC 6 7 8 serves as the pro er b sis for in lu in ad en a related to q artz cry tal

for o tical a pl cation

SYNTHETIC QUARTZ CRYSTAL –

SPECIFICATIONS AND GUIDELINES FOR USE

This International Stan ard a pl es to s nthetic q artz sin le cry tals inten ed for

man facturin piezo lectric elements for freq en y control, selection an o tical a pl cation

The folowin doc ments, in whole or in p rt, are normatively referen ed in this doc ment an

are in isp n a le for its a pl cation For dated referen es, only the edition cited a pl es For

u dated referen es, the latest edition of the referen ed doc ment (in lu in an amen ments)

a pl es

IEC 6 0 8-1:2 13, En iro me tal testn – Part 1: G e neral a d guida ce

IEC 6 12 -1:2 0 , Quartz crystal unis of as e ssed qual y – Part 1: G en ric sp cificato

IEC 6 410, Sampln pla s a d p rocedures forinsp ecto b y atrib u tes

IEC 619 4 (al p rts), Pie zo lectric a d dielectric de ices for fre uency co trol a d selecto –

G los ary

3 Terms and definitions

For the purp ses of this doc ment, the terms an definition given in IEC 619 4 an the

fol owin a ply

3.1

hy roth rmal cry tal growth

cry tal growth in the presen e of water, elevated temp ratures an pres ures by a cry tal

growth proces b l eved to proce d ge logical y within the e rth's cru t

Note 1 to e try: Th in ustrial sy th tic q artz growth pro es es uti ze alk ln water solutio s c nfin d within

a to la es at su ercritic l temp ratures (3 0 °C to 4 0 °C) a d pres ures (7 0to 2 0 0 atmosp eres)

Note 2 to e try: Th a to la e isdivid dinto twoc amb rs: th dis olvin c amb r, c ntainin raw q artz c ipsat

th hig er temp rature; th growin c amb r, c ntainin c t se ds at th lower temp rature (se 7.1.2)

3.2

s nth tic quartz cry tal

sin le cry tal of α q artz grown by the h drothermal method

Note 1 to e try: Culture q artz h s th same me nin as sy th tic q artz crystal

3.3

a -grown s nthetic q artz cry tal

state of s nthetic q artz cry tal prior to grin in or c t in

3.4

a -grown Y-bar

cry tals whic are grown by u in lon stick se d in the Y-direction

3.5

a -grown Z-bar

cry tals whic are grown by u in Z-c t se d

3.6

s nth tic quartz cry tal batc

s nthetic q artz cry tals grown at the same time in one autoclave

orie tation of a s nthetic quartz cry tal

orientation of the se d of a s ntheticq artz cry tal with resp ct to the orthogonal axes sp cified

in 3.7

3.10

orthogonal a ial s stem of α q artz cry tal

orthogonal axis s stem con istin of thre axes with a mutual y vertical X axis, Y axis an Z axis

an foreig material within a s nthetic q artz cry tal, visible by examination of s atered l g t

from a brig t source with the cry tal immersed in a refractive in ex-matc in l q id

Note 1 to e try: A p rtic larly c mmo in lusio is mainly th min rals c le a mite a d emele site

ad itive u ed in the growth proces whic may c an e the cry tal ha it, c emical comp sition,

ph sical or electrical pro erties of the s nthetic q artz b tc

3.2

pre-dime sion d bar

b r whose as-grown dimen ion have b en altered by sawin , grin in , la pin , etc to me t a

p rtic lar dimen ional req irement

3.2

impurity conc ntration

con entration of impurities relative to si con atoms

ves el for the hig -pres ure an hig - emp rature con ition req ired for growth of a s nthetic

q artz cry tal

right-ha d d quartz or lef -h nde quartz

han ed es of q artz cry tal as determined by o servin the sen e of han ed es of the

o tical rotation in the p larized l g t

Note 1 to e try: Rig t h n e q artz is th crystal of d xtrorotatory a d lef h n e q artz is th crystal of

infrare absorption coef icie t α v lue

co f icient (refer ed to as the α value) esta l s ed by determinin the relation hip b twe n

a sorption of two wave n mb rs

Note 1 to e try: On wa e n mb r is minimal a sorptio d e to OH imp rity, th oth r is hig a sorptio d e to

prese c of OH imp rities in th crystal latic Th OH imp rity cre tes me h nic l los in reso ators a d its

prese c is c relate toth prese c of oth r los -in u in imp rities.Th αv lu isa me sureof OH c n e tratio

a d is c relate with e p cte me h nic l los esd e to material imp rities

Note 2 to e try: For th c eficie t d fin d h re, th lo arithm b se 10 is use Th infrare a sorptio c eficie t

v lu α is d termin d usin th folowin e u tio :

α=1

푡푙푙푙

1

�푇

lumbere s nth tic quartz cry tal

s nthetic q artz cry tal whose X- an Z- or Z'- s rfaces in the as-grown con ition have b en

proces ed flat an p ralel by sawin , grin in , la pin , etc to me t sp cified dimen ion an

orientation

3.31

refere c s rfa e

s rface of the lumb red b r pre ared to sp cific flatnes an orientation with resp ct to a

cry tal ogra hic direction ( ypical y the X-direction)

3.3

s nthetic quartz for optic l appl c tions

s nthetic q artz whic satisfies the req irements for the u e of o tical pickups, o tical lowp s

fi ters (OLPF) an wave plates for digital sin le-len reflex camera, monitorin camera, digital

vide camera an o tical commu ication mod le o eratin in the 3 0 nm – 1 7 0 nm wave

len th (5 8 2 cm

-1

-1

internal tra smit a c

internal tran mitan e whic do s not in lu e los of s rface refraction

Note 1 to e try: This d finitio a ples to sy th tic q artz for o tic l a plc tio s o ly Intern ltra smis io v lu s

re uire stateme t of sample thic n s for whic th v lu is c lc late , e.g 2 mm

3.3

stria

s ort ran e deviation of refractive in ex inq artz, growin defects in whic the refractive in ex

flu tuates with a typical p riod of fraction of one mi imetre to several mi imetres

Note 1 to e try: This d finitio a ples to sy th tic q artz for o tic l a plc tio s o ly

3.3

growth ba d

contrastin den ity b n that can b o served in the Y-c t cry tal by Sc l eren an simi ar

o tical method

Note 1 to e try: Th c use of thisc ntrast isth t eleme tssu h as aluminium,so ium, lthiuma d iro are tra p d

in th crystal wh n a crystal is growin

Note 2 to e try: L rg r amo nts of tra p d imp rities ty ic ly c use a in re se in α

Note 3 to e try: Growth b n s c n ot b o serv d wh n α

3 5 5

is les th n 0,16 or α

3 5 0

isles th n 0,12

Note 4 to e try: Thisd finitio a ples to sy th tic q artz for o tic l a plc tio s o ly

4 Specification for s nthetic quartz cry tal

4.1 Sta dard v lue

4.1.1 Shape of s nthetic quartz for optic l appl c tions

A se d cry tal is removed an the growth faces are mac ined to a sp cified u iform s rface

rou h es an to a sp cified flatnes with the sp cified cry tal ogra hic orientation

4.1.3.1 Inclusion de sity of s nthetic qu rtz for piezoele tric appl c tions

The in lu ion den ity (me s red as in 4.2.5.3)for e c grade s al not ex e d the fig res inan

req ired size ran e for that grade l sted in Ta le 1

Table 1 – In lusion de sity gra e for piezoele tric appl c tions

Users req irin a grade in only one or more of the size ran es may desig ate their req irement

as the grade fol owed by the a pro riate size ran e

4.1.3.2 Inclusion de sity of s nthetic q artz for o tic l appl c tions

The in lu ion den itygrade of s nthetic q artz for o ticala pl cation s al b s own at Ta le 2

Table 2 – In lusion de sity gra e for o tic l ap l c tions

4.1.4 Stria in s nth tic quartz for optic l ap l c tion

A size, contrastin den ity an q antity s ould not ex e d a lmit sample A l mit sample s ould

b defined b twe n the man facturer an the u er

4.1.5 Infrare qual ty indic tions of α

3 5 0

3 5 5for piezoele tric ap l c tion

An infrared extin tion co ficient value (α value) of s nthetic q artz (me s red as in 4.2.6) s al

b as l sted u der the a pro riate he din for α

35 0

or α

3 5 5

in Ta le 3 for the variou grades:

Table 3 – Infrare absorba c coef icie t gra e for piezoele tric appl c tions

Th se Q v lu s were o tain d from α me sureme ts a d empiric l c relatio , a d were in c mmo usa e

prior to 19 7 Th se are in lu e h re as th pre io s la els to maintain c ntin ity thro g th c a g in

emp asizin α la els α is th p ysic l me sureme t n w use to c ntrol a d sp cify q alty in sy th tic

q artz

The test lmits a ove either cor esp n to or are u c an ed(ex e t in the cases of grades B an

D) from the α

3 5 0

Iimits that cor esp n to the Q value grades l sted IEC 6 7 8:19 3 This fif h

edition of IEC 6 7 8 desig ated some of the same grades in terms of minimum in icated Q's in

4.1.6 Gra e cla sific tion by α v lue a d Sc l ere method for optic l appl c tions

Grade clas ification is s own at Ta le 4

Table 4 – Infrare absorba c coef icie t gra e

a d Sc l ere method for optic l appl c tions

The freq en y- emp rature c aracteristic of s nthetic q artz cry tal u its s al b as es ed

by determination of the fractional freq en y deviation me s red at 15 °C an 3 °C with

resp ct to the series resonan e freq en y at 2 °C The fractional deviation s al satisfy the

4.1.8.1 Etc c a nel d nsity ρ for piezoele tric ap l c tion

When req ired, the etc c an el den ity, ρ, p r cm

2

(me s red as in 4.2.8) for e c grade,

s al comply with the l stin s in Ta le 3

Table 5 – Etc c a nel d nsity gra e for piezoele tric appl c tions

4.1.9 Intern l tra smit a c for optic l ap l c tion

At the wavelen th 4 0 nm, 5 0 nm, 6 0 nm an 1 5 0 nm, internal tran mitan e s ould b

0,9 8 or more for a 2 mm thick sample

Figure 1 – Quartz cry tal a is a d c t dire tion

(ey epie e r otatin clo k w ise)

In p larisc p : a aly ser r otate

c u ter clo k w ise

The dimen ion alon the Z or Z'-axis s al b me s red by a p int cal p r an it s al b

sp cified as the maximum dimen ion alon the Z or Z'-axis in the gre ter X zone (se

There s al b no cracks or fractures in the u a le region The existen e of cracks an

fractures s al b c eck d by vis al in p ction

cry tal u in a stere binoc lar micros o e o eratin at 3 × to 4 × mag ification eq ip ed

for cou tin within either a circ lar or a s uare field an with a cal brated retic le s ale for

determinin p rticle sizes, inten e side i umination (s c as halogen lamps) over a

reces ed black mat b ckgrou d, an in ex matc in lq id (n = 1,5 , a proximately) for

tran p ren y, an me n of me s rin the dimen ion of the sample volumes cou ted An

example for the referen e sample selection proced re is given in An ex B

b) Method 2

In case it is dific lt to a ply method 1, cry tals are comp red with referen e samples

a pro riately re resentin e c grade ran e, immersin within an in ex matc in l q id

(n = 1,5 a proximately) for tran p ren y, or a plyin s c l q id to the s rface The

referen e samples s al b agre d up n b twe n the s p l er an the u er An example for

the referen e sample selection proced re is given in An ex C

4.2.5.3.2 Sampl ng

Becau e of the con idera le costs in time, la our an money, some plan for sampln b th b rs

an region within the b rs is normal y u ed by agre ment b twe n the s p l er an the bu er

when q al ty control of either in lu ion den ity or etc c an el den ity is req ired

Cle rly, the prefera le low-cost in p ction situation is the one in whic the den ities of

in lu ion or etc c an els are wel b low the test lmits, an infreq ent samples can b

ju tified Sin e s c situation are not alway at aina le, more rigorou in p ction strategies

wi sometimes b req ired for a pro riate den ity control, an s al b fou d, work d out, an

agre d up n b twe n the s p l er an the u er

Sou d statistical method are req ired in order to me t a pro riate agre d-up n as ured

q al ty level tests an en ure that the cry tals an the volumes cou ted within them are

s f iciently re resentative Sin e sampl n proced res an statistical confiden e tests are

des rib d in the l terature, their prin iples wi not b re e ted here

4.2.5.3.3 Batc s mpl n

In most b tc sampl n , a s ita le sample b r or group of b rs is c osen to re resent the b tc

p pulation The n mb r of b rs s al de en on the n mb r in the b tc , the typ of cry tal,

the inten ed a pl cation, the se aration b twe n the me n an the target in lu ion den ities

an the AQL (ac e table q al ty level) confiden e level req irement ne ded to provide

s f icient as uran e that the b tc in lu ion den ity in e c size ran e s al b b low their

a pl ca le grade test l mits The sample b r group s al re sona ly re resent the b tc with

resp ct to in lu ion den ities Deviation , if an , are al owed an s al b toward hig er, not

lower, in lu ion den ities for safe as uran e

4.2.5.3.4 Volume within a bar

A group of volumes within e c sample b r is next c osen for in lu ion cou tin The

b u daries of the volumes are defined by the are of the focal field of the micros o e (or the

outl ne of a s uare retic le) an either the heig t of the b r or the len th ran e of the de th

adju tment of the micros o e c osen for u e It is neces ary to determine an total the

volumes throu hout whic cou ts are ac umulated The volumes selected for cou tin s ould

in lu e mainly region (u ual y Z-growth zones as in Fig re 3) whose material wi b present

an active in the finis ed devices an s ould not avoid den e in lu ion volumes within these

region The n mb r of volumes p r b r s al b at le st six or more for re sona le statistical

The sample volume location within a b r s al b a pro riately distributed in its X-, Y-, Z-axes

to in lu e the variation of the in lu ion den ity with these in e en ent varia les Typical

s nthetic q artz b rs (Fig re 3 ) are lon in the Y- an smal in the X- an Z-axes dimen ion

Normal y, the gre test variation of in lu ion den ity a p ars over a zone's grown direction, for

example the Z-dimen ion in the Z-zone (Fig res 1a an 3) Th s, for large Z-cry tals, the

sampled region s al b located at varied Z-distan es from the se d to en ure that the b r's

ran e of Z is wel -re resented by the group of sample volumes Simi arly, an noted variation

over Y or X s al b sampled, if s c variation are present

a) – L c tio of AT-c t plate in rig th n ed s nth tic

b) – L c tio of X-c t plate, Y-c t plate an Z-c t plate

Fig re 3 – Typic l e ample of c t ing wafers of AT-c t plate, minor

rhomboh dral-c t plate, X-c t plate, Y-c t plate a d Z-c t plate

To aid in distributin sample volumes within a typical b r, its les er X-s rface is mark d with

tran verse Z'-l nes, p rp n ic lar to the se d at reg lar 10 mm intervals over the Y-len th of

the s rface Sample volumes for in lu ion cou tin are c osen as ne ded from within e c

rectan le formed by the marks an the cry tal s rfaces To locate the sample volumes at varied

distan es from the se d, in smal cry tals (where a Z-zone me s res les than double the field

diameter of the micros o e), they s ould b alternated ne r an far from the se d For larger

cry tals, the volumes s ould b seq en ed in Z over its ran e to en ure that e c in lu ion

b n is re resented in the sample volumes Several freq ently u ed sampl n plan are

4.2.5.3.5 Inclusion countin

The circ lar or s uare field of view c osen for cou tin within its mark d rectan le is s an ed

vertical y over its c osen X-heig t within the micros o e's ran e of de th adju tment, as

fol ows

If the sample is a Y-b r with a relatively smal X-heig t, the s an wi b at a series of sites

varied in Z alon its len th (u der side i umination, with its les er X-s rface up) Begin in in a

rectan le p sitioned at one en of the u a le zone, an in lu ion cou t is ta en in an X-c l n er

(or p ralelel pip d) volume Startin sl g tly b low the les er X-s rface (an not cou tin

s rface material), al visible in lu ion in foc s are categorized an cou ted in e c of the size

categories req ired by the c stomer's order: 10 µm to 3 µm, 3 µm to 7 µm, 7 µm to

10 µm, an gre ter than 10 µm The micros o e is then lowered an the newly foc sed

in lu ion cou ted an ad ed into their size categories This proces is contin ed throu h the

c osen X-heig t; the proced re is re e ted at the next sample p sition, an so on

The cou ts from the b r's sample sites in e c of the four size categories are s mmed by

category an divided by the calc lated total of the sampled volumes, to o tain an average

cou t p r cm

3

for e c category in one b r The cou t averages in e c category from al the

sample b rs from a ru are averaged an recorded as required to re resent the size

distribution for the ru Maximum an minimum b r averages may also b recorded, if desired

or req ired A n merical example is given in An ex B

4.2.6 Ev luation of infrare qual ty by α me s reme t

The infrared a sorption p r centimetre at one or more of 3 5 0 or 3 5 5 wave n mb rs is

me s red in a Y-c t slce s an as the diferen e b twe n the a sorption at the c osen wave

n mb r an a sorption in the b ckgrou d outside the b n , at 3 8 0 cm

–1

or at 3 9 9 cm

–1

when u in a sin le b am in trument Sin e those α are k own to vary directly with the total

Z-growth size distribution of the cry tals in one b tc , a maximum Z-cry tal ( or worst case

maximum α me s rement is u ed to c aracterize the b tc Other cry tals, the average

Z-cry tal for example, may b me s red to further c aracterize the b tc

Two method have b en u ed for IR me s rements in q artz The first was disp rsive, a set up

in whic a monoc romator res lts in the exp s re of the test sample to a sin le b am sp ctrum

of sp cified wavelen th (wave n mb r) L ter, Fourier tran form infrared sp ctro hotometers

(FTIR) were develo ed al owin al relevant wavelen th to b sampled simultane u ly This

method u es an interferometer to col ect tran mis ion acros a wide sp ctrum The detector

sig al is sent to a computer integrated into the test setup, an an algorithm cal ed a Fourier

tran form is p rformed on the interferogram to con ert it into a sin le b am sp ctrum, with the

tran mis ion data so o tained u ed to estimate the alpha extin tion co ficient Today, the

FTIR is u ed more widely than disp rsive IR eq ipment

Both the disp rsive Infrared Sp ctrometer an FTIR method may b u ed to me s re the

whole sample at a sin le, fixed wave n mb r In this o tion, the sample is s an ed a out the Z

direction u in a nar ow b am to me s re infrared a sorption p int by-p int, then con tru tin

a ma of a sorption vers s Z-p sition

4.2.6.2 Preparation of th Y c t sl c

The s nthetic q artz cry tal to b sampled is mou ted on a s bstrate then sl ced with a q artz

saw to yield at le st one Y-c t sl ce whose thicknes afer la pin and p l s in wi fal in the

ran e of 5 mm to 10 mm The 5 mm thicknes is a pro riate for hig α-material, to resolve its

α-variation ; the mid-ran e for medium α; an the 10 mm thicknes is a pro riate for the

lowest α-material to me s re its smal a sorption

Afer sawin , the sl ce is la p d on b th major s rfaces: first, with a homogenized mixture of

2 µm a rasive; secon , with a homogenized mixture of 3 µm a rasive Further la pin to

p l s is o tional an is prefer ed for low α

4.2.6.3 Cal bration of a sta dard Y-c t sl c in a infrare spe trophotometer

The infra-red sp ctro hotometer is turned on, al owed to warm an fuly sta i ze, then

cal brated The normal dai y calbration in lu es its tran mis ion (0 % – 10 %) or a sorb n e

(log T = 1,0 – 0) l mit setin s, c art sp ed an s n hronized sample s an in ar an ement

For evaluation an normal u e, a 1,5 mm width a erture is located in the sample b am For the

lowest α value me s rements, a 5 mm width a erture may b req ired The a erture's heig t

s al not ex e d the X-dimen ion of the se d or 5,0 mm A p l s ed Y-c t stan ard referen e

sl ce is placed first in the sample holder, whic is then mou ted in the s an in device

The wave n mb r control is set at a b ckgrou d set in (outside, but ne r the OH a sorption

b n ), u ual y (3 8 0 ± 3) cm

–1

, an the sample is tran lated throu h the b am with

s n hronized c art ad an e at the fixed wave n mb r Su h s an in is done only in the

Z-growth zones of the Y-c t sl ce (i u trated in Fig res 1 an 3) In certain cases where

b ckgrou d noise may b a pro lem, s c as sin le b am o eration, a hig er b ckgrou d

wave n mb r (3 7 ± 3) cm

–1

may b u ed for lowered b ckgrou d noise If the b ckgrou d

s an trace is not re sona ly flat outside the original se d's b u daries, a thin fi m of fluorolub

gre se s al b a pled to b th major s rfaces of the semi-p ls ed Y-c t slce Basel ne

The sample is returned to its original p sition an

the c art p p r rerol ed to the p sition where its wave n mb r s an b gan The sample is then

s an ed to plot its infra-red a sorption at this wave n mb r in the a sorption b n

The cal bration α values (maximum an minimum) are calc lated from this referen e s an,

(1/T).To c n ert this v lu to ln ar a sorptio c eficie t,asd fin d in IEV 8 5-0 -7 ,c resp n in to th

in re se in a sorptio c eficie t at th sp cifie wa ele gth, α is multiple with a fa tor 10 *n(10) = 2 0,3 Th

fa tor 10 c n erts from cm

–1

to m–1

a d ln(10) = 1/lo

10(e) from b se 10 to e

The sp ctro hotometer is con idered in pro er cal bration if its α

ma

min

re din s are

re e ta le within ± ,0 4 u its of the stan ard's values for them A stan ardization cor ection

may b calc lated as ne ded to brin the in trument's re din on a stan ard sl ce to an

ac e ted value an u ed whi e c r ent

4.2.6.4 Te t me s reme t of a Y-c t sl c

Afer s c es ful cal bration, e c pre ared (prefera ly p l s ed) u known sl ce is s an ed at

the b ckgrou d an c osen OH a sorption b n wave n mb rs, u in a thin fi m of oi as

ne ded in cases where there is only a semi-p l s Their p rtinent α values are calc lated

u in the eq ation a ove Region ex lu ed from this determination are ± ,0 mm from the

4.2.6.5 Compe s tion of α v lue by sta dard s mple

Cor elation b twe n the test eq ipment of e c man facturer can ot b as ured by strict

ad eren e to u iform me s rin con ition an proced res Therefore, it is neces ary to

esta l s a comp n ation value for α The recommen ed comp n ation value is determined by

e c man facturer referen in the proced re des rib d in An ex E

4.2.7 Fre ue c v rsu temperature c ara teristic for piezoele tric ap l c tion

The sp cification for the q artz cry tal u it for evaluatin the freq en y-vers s- temp rature

c aracteristic s al b as fol ows, an me s rements s al b made as sp cified in

IEC 6 12 -1:

• orientation of plate AT c t 3 ° 15' ± 3 ";

• finis of s rface la p d (average p rticle size of a rasive s al b les

than 3 µm), then etc ed by 2 0 kHz;

• flatnes of s rface when i uminated with monoc romatic l g t throu h an

o tical flat glas an examined within a circ lar zone

of 6 mm diameter, the prod ct of the frin e c rvature

an the freq en y expres ed in MHz s al not ex e d

5 if me s red with yel ow l g t or 6 if me s red with

gre n lg t;

stan ard atmospheric con ition for temp rature an

pres ure (se 4.1 of IEC 6 0 8-1:2 13)

The sp cification s al state the minimum an maximum slo e of freq en y- emp rature

c aracteristic (Fig re 4)

Figure 4 – Fre ue c -temperature c ara teristic

de iation rate of the te t spe ime

4.2.8 Stria in s nth tic quartz for optic l ap l c tion

Stria inlumb redq artz cry talare o servedin the white lg t withthe lq id of whic refractive

in ex is almost the same as that of q artz, s c as si con oi Lumb red q artz cry tal is

p sitioned b twe n the cros nicol p larizers an stria can b o served from Z direction The

q antity, size an colour stren th of the stria s ould b comp red with those l mit samples

They can b also o served in the p l s ed Y-c t sample of several mi imetres thicknes by

u in s hl eren or simi ar eq ipment Typical o tical set up for testin of s hl eren is s own at

Fig re 5

Figure 5 – Typic l s hl ere s stem s tup

4.2.9 Growth ba d in s nthetic quartz for optic l appl c tions

Sample’s c t in direction is p rp n ic lar to Y axis an its b th Y face s ould b p l s ed By

u in s hl eren or simiar eq ipment growth b n s ould b o served

4.2.10 Etc c a nel d nsity

4.2.10.1 Ge eral

The etc c an el den ity is me s red by cou tin c an els in an etc ed AT-c t sample sl ce of

the sampled q artz cry tal as se n u der a binoc lar micros o e at up to 3 × mag ification

4.2.10.2 Sampl ng the cry tals from a batc

Sampl n a b tc to ac ieve a sp cified statistical confiden e level req ires the u e of AQL

confiden e statistic a pro riate in this, the etc c an el case, b cau e the etc c an el

p pulation de en s on b th the c an els in the se d an the proces that grows the material

on the se d It is prefera le to pre-sort an group se d for their etc c an el den ities an

record their group location in autoclaves or en ure that there is an adeq ate sample of the

se d as wel as the growth on them, b cau e of the p s ibi ty that some of the se d may

dif er gre tly from the others, u les intentional y control ed d rin plantin

4.2.10.3 Preparation of AT c t sl c for etc in

A sample s nthetic q artz cry tal is c t to yield an AT-c t sl ce (at 3 ,2 ° ± ° to the Y-plane) of

a thicknes to finis at 10 mm The slce s ould prefera ly contain ful se d heig t, althou h

thin er sl ces an les er se d heig ts may b u ed in sp cial cases, provided the sp cified

amou t of material is removed in e c la pin The sl ce's identity s ould b mark d with a

diamon s rib , prefera ly on its les er X-s rface, to an adeq ate de th to en ure that the

identity wi not b lost in la pin an etc in

Afer sawin an markin , the slce is la p d on b th major s rfaces; first, with a homogenized

mixture of 2 µm a rasive, then on a cle ned la with a homogenized mixture of 1 ,5 µm

a rasive A minimum of 0,2 mm total thicknes of q artz s al b removed in the first a rasive

la pin , an of 0,10 mm total thicknes in the secon a rasive la pin The slce is then

cle ned to en ure a u iform etc in rate over its s rfaces, as eviden ed by its u iform mat

a p aran e af er etc in

4.2.10.4 Etc ing proc dure for lappe AT-c t sl c

Within a fume ho d, u in a pro riate safety eq ipment (in lu in a ron, gloves, eyeglas es,

an splater s ield ), an ex es of ammonium bifluoride is ad ed to deionized water in a

s ita le container to ma e a saturated solution at 7 °C ± 2 °C The ammonium bifluoride is

maintained at the 7 °C ± 2 °C temp rature, with the u e of a con tant temp rature l q id b th

A p lytetrafluoro th lene (PT E) co ted thermometer in the solution is u ed for monitorin the

temp rature If dif erent etc temp ratures are prefer ed, the etc time wi b adju ted

a pro riately to comply with the stock removal req irement b low

The la p d an cle ned AT-c t sl ce is immersed into the saturated ammonium bifluoride

solution u in PT E-co ted ton s or an inert etc in sl ce holder The solution s ould b

agitated or the sample slowly moved (a proximately 2 mm p r secon ) d rin the etc in

proces An etc in time of a out 4 h s ould b s ficient, de en in on the agitation an the

n mb r of slces, to remove not les than 0,10 mm (minimum) or more than 0,12 mm (maximum)

total thicknes Uniform etc rate is a req irement The q artz sl ce s al b c eck d

p riodicaly for etc u iformity b th in time an over the are of the sl ce Afer etc in is

completed, the slce is removed from the etc solution with the PT E-co ted ton s, rin ed with

hot water (8 °C), then cle ned with acetone an other cle nin agents, if ne ded, to pre are

the sample for u o stru ted vis al in p ction

4.2.10.5 Etc c a nel counting proc dure

A s uare grid of known dimen ion in the ran e of 0,2 cm × 0,2 cm to 0,5 cm × 0,5 cm is

mark d on the AT-c t sl ce within the Z-growth zone as identified in Fig re 3 If prefer ed, the

grid p tern may b drawn only over the rectan ular p rtion of the Z-zones matc in the

heig t of the se d No grid s uares s ould b cou ted that fal within ± mm of the centre l ne

of the se d

Eac sl ce is viewed with a binoc lar micros o e u in 3 × to 4 × mag ification, an a stron

l g t source directed into the sl ce in its les er X-direction Care s al b ta en to foc s the

micros o e on the up er s rface of the sample, th s avoidin cou tin the etc c an el

intersection with the lower sample s rface The etc c an els are cou ted an recorded in

e c an every s uare are with the micros o e's zo m adju tment set for a con enient

viewin mag ification Afer al the grid are s inten ed for cou tin are cou ted, their average

cou t is calc lated, an con erted to an average p r cm

4.2.1 Intern l tra smit a c for optic l ap l c tion

Internal tran mit an e is me s red by the folowin proced re

a) Two samples are c t from the same q artz b r;

b) Direction of c t in is p rp n ic lar to Y-axis ± 6 ’;

c) Thicknes of samples are 5 mm an 10 mm;

d) Both Y- ace of two samples is mir or p l s ed;

e) Tran mis ion is me s red throu h b th samples u in a sp ctro hotometer at the

wavelen th 4 0 nm, 5 0 nm, 6 0 nm, an 1 5 0 nm.Internal tran mitan e is me s red by

a sp ctro hotometer at wavelen th 4 0 nm, 5 0 nm, 6 0 nm an 1 5 0 nm

f The internal tran mit an e for a 5 mm lon sample is calc lated u in the folowin formula:

휏 =푇

tran mitan e in lu in s rface refraction los of 10 mm sample;

Internal tran mit an e values for other thicknes es can b calc lated u in the fol owin

ex the natural exp nent fu ction;

5 mm the thicknes for whic τ was original y calc lated;

t the thicknes of sample for whic the internal tran mitan e is calc lated (e.g.2 mm)

4.3 Marking

Eac s nthetic q artz cry tal s al have the fol owin information cle rly mark d on a major or

les er X-s rface:

a) man facturer's name or trade mark;

b) orientation of material;

c) han ed es of material;

RH stan s for rig t han ed q artz;

LH stan s for lef -han ed q artz

d) other information, if sp cified, to b mark d s c as;

1) b tc identification;

2) α grade;

for piezo lectric a pl cation : Aa, A, B, C, D or E;

for o tical a pl cation : OPT A, OPT B, OPT C or OPT D

3) in lu ion den ity;

for piezo lectric a pl cation : Ia, Ib, l, Il or I I

for o tical a pl cation ：OPT l, OPT Il or OPT I

4) etc c an el den ity;

for piezo lectric a pl cation : 1a ,1a,1, 2, 3 or 4;

for o tical a pl cation : 1a ,1a,1, 2 or 3

4.3.2 Shippin re uireme ts

These req irements s al b sp cified up n agre ment b twe n the s p l er an the u er

5 Specification for lumbered sy thetic quartz crystal

5.1 Sta dard v lue

5.1.1 Tolera c of dime sions

Deviation from the sp cified dimen ion alon the X- an Z- or Z'- axes s al b les than

0,2 mm (se Fig re 6)

a) – Smal X-dimensio s ed

b) – Larg X-dimensio s ed

Figure 6 – Lumbere s nth tic quartz cry tal outl n

a d dime sions along X-, Y- a d Z-a e

5.1.2 Refere c s rfa e flatne s

Referen e s rface s al b flat to within 0,2 mm or as sp cified Care s ould b exercised in

the selection of the method of me s rement to isolate me s res of referen e s rface

deviation from those of the o p site side (p ral el sm)

5.1.3 An ular tolera c of refere c s rfa e

An ular deviation of the referen e s rface s al b les than 15’ from the sp cified

cry tal ogra hic direction (se Fig re 7)

Fig re 7 – Angular de iation for refere c s rfa e

Th a g lar d viatio

of th refere c surfa e

from th Z-a is

L s th n ±15′