Document 7004wbY6QaN4mLN3y2N4J71RE
LIA23659
LEAD INDUSTRIES ASSOCIATION, INC.
m MADISON AV KNUI
NEW YORK 17, N, Y.
Kirch 29, 1963
SUBJECTi REPS DO1 OH UAD CERAMIC RESEARCH PAPER.
Tot Member* of ths Lead Industries Association, Inc.i
Wo ex* attaching a reprint frca the Journal of the American Ceramic Society entitled, "Dllatare trie end X-Ray Data for Lead Compounds, II".
As you can see, this Is the aocond In a series of papers on thermal-expansion properties of crystalline lead compounds, die of the authors of this paper is the LIA--Expanded Research Project
fellow at The Pennsylvania State University, working under a ceranlc research grant. The other author la his faculty supervisor and Chairman of the Dept, cf Ceramic Technology.
Printing of this paper In the Ceramic Society Journal has, of course, given It vida distribution throughout the ceramic Industry, and we have purchased only a limited number of reprlnto for dis tribution where we think it will Oe beneficial.
Members can obtain additional copies freo us--up to 25 free of charge--and larger quantities at our cost of 1Of each as Tong as the eupply lasts.
Very truly yours.
r-Y
Jerome P. Smith
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LIA23660
Dt*k<fcu*4 Vfl KAO tNOVtrtllf AlttCUHOH. *C
Jtl M4li A> < H* tw% 17. H*w TM
IkrtMMi^ Nv IW jurtJ 4 TW A*>rt<a Citiaw NvWir. V4, M. Nm. I )try. IMA
Diiatomefric and X-Ray Data for Lead Compounds, II
by J. F. ARCYlt ond F. A. HUMMR
C*I|1 i *****
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tine*/ thermAl-erpgtulon di'j tti presented for PbAJ,Ow Pb;GeO. PbMoO^ PbWOH the pcroe*kile-type structure* PbiMjWO*, PbFeT*0i, and PbJF>,WO,, and the ipAtile-type structure* PbdSiO.UVO.i,, Pb. GeO.hVO.i,, od Pb** tGeO)tPO,)> X*rmjr powder diU *re jirea, Afld lh behxrioc of the compound* ii correlated with
prerioui in'ormttioo from the literature.
L lalrediittlea
T >a a jakntrd out in Part t id tlti> wttr*' that :m*rr data <m
I the thermal ex|*ansVn twhi\>w 4 sTvdalline Wad itim|>>und> ur nor^sjn' t |enlt letter their !*rhav>e to o-*nj.Wi ceramic system* crpmjs-xed4 crystal mixture-* < glassm xtal aggregates
Oat a f< ten amfHind are (*roented in thin jajirr, threr *4 which have the j<rv>kile t*Tc struct ure. three the a|wtste!\j-e structure, and two the whrtliic l>te structure.
IL lMfotvr
(IJ Cwnpwadi
Smdrnskfl. Agram'vskava. and |*u|mv* daimed that
PNMsUft, dWi M^I-U'iV, IVFrTa<\, (IllAi Fr/V-
Ti/V. m<t |1*|Fr.\Vttf
Krtl, \V<M atl had a |wr*V-
iiie lyjw structure.
(?) Apo*iH~Typ* Compound*
Mrrkrf and \Vimltatscbek* shewed that rh,(S*0,HV0)|
r.'d'MlSdV'VM. I1h ((V4
I (WO,
and
l'MGe<U(l,<Vi (dV> (Vo, 17M all had on a|wtitc like
structure They gave (hr and < |suamctcr*. r '< ratio*,
andetmgrurnl melting j*intsas folk***
MIA) SiO, VA Mna twtvlVh APW> tXv-VA
iAl
t W
V XU
lo tet
: x\ o Tt w i r :vj o U\ : :i: o 713
p k Mim
t'>*C4I| wc n>o
1M3
(3) feoV Motybdot* ond 1+&J Jtwyluft
Jargrf ami (Vnn** u^-d heating curses and thermal analvaia !* determine melting imints. inviTsVii*. and li'juidus curve* ir. the system* 11-0 \Vo and II* MA* TIh -v claimed
oaorruent melting ha PtiM<o at H>VC ami for II.WO* at ll.*.i"'C. l*b\VO, a rr;<td l umWrgo a reverwtdc )4\Trvaj>hic tranuttaio at ST*C
(4) 19od Ai\#nmc4$ cad L+oJ Cwmoaoh
(Viler ami Hunting* w.akrtl in the $\`*leiu IlfO-AVh and suggested the eeistenrr t4 a awn|Kjnd n*(>-Al/h This O'jjjj^ajnd lrraks iVw? ra)idlv at lt*trC frm lrta Ala t, jnd Wjuid Thrw tr\rstig4t*av J*inirl 'rut that this Iwrakd n mav true mo^ngnx nt melting < it may he a de es.mj-/-.it i^n am h rated at -7**'* JHai'C Iry the voUtiluatinn
Shutr* claimed that .`11^ (VO. ntrltexj in an AM * cruetWe formed a himojirttMin jVs VrTker and \Vmlra^v'hek, shiWol Out tMT- MV( h ntelted it a |4utinutw crucihle ra(<knv CTystallt/rs. and suggested that the glass nMained tv ^huti* was je4wWv stahibrel hv d>w4\eri AMhff'm the crusSl V.
ktsf'sed Maftl. 14. |!*y, frM^rl rtH rmitnl August jy.
|!'C* C*a*tnt>utaa N* K1 *VJ (f.^n the
*4 Mineral hl-
du'lrtes. The IVnnsxhatua
t'nnrtwtr
The nntrfs arr. trs|xtfrlt. Lead Ki|*amtrd Krwarrh
Prop4in
and |a><(esv<. |W|uitmn( 4 Ceramic Tevh<
n**k*gy. C>4kge <4 Mineral Indu-Oitr*. lte lVno\>Uanu State
I'nivrf 'lv
*j F Aigslr atwl F A llun.iwk IhVl.anetrlc and X Kay
|>ata i'A l.e*d C4ti|<unds. I." J. .{n tYwa. .S*v . 4J jtJ 452-
57 (!Vi*h
' (1 A Sn"lenAt. A 1 Acramn-skat a. and V A. lsupfr,
"New Frimlrrtnis 4 C>aii|4r\ C**nj^stti.>n; HI. lltiMgWO*.
pthlViWOh .id hi,FrTdC f*i T\*t4 JV/u, 1, te.at trj
(IP> : Lu'l*i| Mrtkef and llaus Wofvtratvbek, "C'^ntniundt id
Afutite Tv|s* Strwfure.*'
.Vmrr^l, 45, IA 40 (1PA7).
' K M Jaeger atwl H C (Vetms, "The Sut|hale, Chf>*m4te.
M<4> lMtr amt Tungstate lln.*r) Sj sterns <4 l-e.t|," A**rg m.
flr . Il, US 73 i IWI >
* k F (Wlt*r ami K V Hunting. "Ne|><t >m the S) sterna
U>4'1 Osnle Alumina ami l^-a<( Oswle Ahimma Sdn-a,'* J. Jte>
tear, k \\4tl Har .`CfWu'di. /! {.SJ
-7t 4 ttf|; KP I.Wg;
(>'.. .!*. . 21 |.*l| .VM HM4
* WoMtaitt Shut*. "ISe kristalkhrmische Vetnamftvhaft
jwiwben (Varinauium uml Sdnium tCl)'slal CHeumal K'-latnui
Iteluir rOtiiMniuin ami Sl*c-w ). / M*'1* Ckcw , BJI, V.V.* 30K
(UCUW. (V-j* .ths/e , 1 |tt IS IhWi
1 Meikrt aiwl Hans '.Wlul'ehrk, "Finige FWtner-
kmigvn nun Hl'i-*rth"silikat um) getmanat uml derm Cdasig-
keil" il,rid Orth*filtrate and (Vfmanate, ami Their <VUv.y
Charatt.f
**< ,40 J11J 171 7:1 (
It'S*
N 1907.01
January liflkl
J^iUitomttru n nJ X-ttay Ikihi for I^iu! Comfounds, //
TobU L Cokirwrsg ond firing Trohfrtb. for laod Compound*
C--
III/) MjO-WU, 4FiiO I e^K-Tadk 3|1iO Fe,<K WO, AMKi-SO,- WK MfliO tkA-VA M1.000,-F/X ItiO-WO, Hit) MmO, Hv0AJ,0, :no-(X)i
.__------------------
"~r-
Nil Ml) ftl) 4Zl 1 4<ll 4,VI KVl KV ;.vi Kll
" rr-
pill till 7*i Tin 7m 701 pm JuVi ini 4.wj
7,Me lUI
.'4 *J4 74 74 74 74 74 74 12 12
4
*o
pll HD 7)11 47l 4MI Mu |IMI pon VII) 4MI
1!
HL ExpHmn(ol
AD comj***itions were made from cj rivmirak After weighing. the lutchc* were hand mixed in a glav nwetar with acetone ( IS to JO minute*, mir diint. and then heated slowly in a (7Mk u furnace to ,Tii)*C and held f* 4 hours to cxj<d volatile*. The Isatchc* were remixed, given a "first caksnalion" for 31 bur*. rooted, remixed, and given a ''xesmd ralonati<wi,'* a* shown in Tabic l.
After the sro-nd calcination. the luatchc* were ground, mixed with a k'arliowax v>lut*>n. rvwluh/rd through a Jtt mesh sine, and jre*wd into |0- by I- by Nm Ian at 1<*J0
The v|<eeimcn* were fired slowly to the trmja-ratum indicated in Table 1 und held for tl hour* until the liar a* sintered t* a relatively dense condition.
Note that M-srral Volatile oxwlr* (ITiO. WO* \V K. 1W Mi and (Ve*M were involved in the j*crjj/ati><n ( tbs-se pimjanitMU Hv tl>e uw *f rejealnl !* trtn|TJturr cabining. reja-ateil grinding ami miring, and carrfutls chosen f.nal sintering tcinjcralmes f e each O'mj* ritmn. it is highly (pfotuMe that L*s m-s due t* Volatilization mere neghgildr
Thermal ex|sinsi<n run* Were inalc in a Vertical fused silica dilatomctfr, u-ang a heating rate ! I3UCC |<t hour The expansion* sn-re measured hv dial gage* which were asvuratc In t/UVl*! in At least two runs w v t t maik n each xjecimm. Any flattening of the esjunsion xve near it* high trmjefaturr extremity is jrroliahls due to deform*ti'm of the sjevimen un*kf tl>e Wright of ihe fused silica Iran*mission tu!w (abut .VSg).
X rav diffraction jattern* were oMaincd on a N'crki* diflraslomelet Using k*u An railiation. Tlw sjicvimrn* were ground to ;ww t 'JUlmcsh sieve ami packed into sample h'dders in Mich a way a* to mtmntiae the { sMliility of anr jcrfrmd orientation of the crystal aggregate. The sample* were run lwtwn*n III* and n i* J4 al I* |irf minute, thi* fate lring adequate to give jsitlrrnx suitable fnf qualitative tdenttlocation |mrjHH<-s Tlie strongest )<rak of each (vatlefn waa fully accommodated <>n the recording chart hv placing thin nicktl foils in front of the counter till** when jwak inimsiiir* required it High tiin|*rT*turr X-ray jutternt were ob tained with a platinum wound fumaor nvajmedon a Notclm diffractometer. A finely ground s|*ccimrn wa juried into a ft depression slide and sintrred in place for several hur* at a trmjerature aU.ul 50"C higher than the trmjeraiuir sub sequently tised to obtain the diffraction jiattern This jeomhire was iwd |o prrvmt any r/lect of sintering on Ihe jiti`ns or intensities of the X ray rrflivti>n* at elevated ternperatttfe*.
IV. Experimental fteudtt ond Dltcutilaii
[ Ij Prov*i/*e-7yp Sbvctvra*
The linear thcnnal exj*ans..n sxirve* of JlH)-Mg< > W< *. .tl'lil^ cc|t Wt h, and -HfliO-1>J)*- Tu/\ are sltown in Fig.
t. U>iw a^4 4>>ia.0 W yirmtfw
I. .'U'tiO- Fed V \V<H*nd 4 Ha I Fe^ > TiO|ha\t o<ntinuou% exjunsioti curve*. l*ut Jllfl")* MgO-WtS how a disomtinuit v, with a marked negative exjunsim leginning at about to C Snv-lmski!. Agrn*s-ska\a, and Isuiwiv1 claimrtl that Jllit I Mg< W'l | undergoes an antifemelrctric transitwm at X*C. whkh corn sj.axis to the trxnperature below wbirfa thie.xrfnjanmd showa marker! negative exjxnskwj.
The X rav diffraction data for these three oenjaiunds a/e shown in Table 11
(2) AfiatrH-Typa Sbvcfvrwa
The linear thermal exjunsion characteristics of 5l*b0- t^b PiOv olliO SiOi V/V and .MlAJ OHH-VA are
Tobl* R. X-Ray Oiffioctioo Data for Compowndi with frovvkiU-Typ Structure
4/Sai f rUW u
rrvo frviH T
jrw> wg< wcw
4> A)
l 1.
ii A) t /.
' 4iM
in
3 99
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3 33
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34 6 3
100 3 7 IX 4 16
14 4 3 3
31 14
1 410 1 3M l 274 t 264 l 1M
10
1 6 4 4
LI A23662
12
Journal oj 13te Amrruan Crriimir Snnrty AriyL- anJ Uummrl
Vol 4t*( No.
TobU UL X-Rgy Dffroct*oo &ola foe Compound* with Apotita-Typ* Structure
irv<i <x. rax
irw> <Xh v a
irwi-JMv va\
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4< A)
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in 34
2 92
un
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2 23 2 ) 2 14
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1 ot\\ t 9(5
1 K*2 I > 1 iM5 1 Ml I fJ<1 ) Ml
t M3 I Oli 1 5(U
47 4
4 9 3
1X1 13
7 2
14 in jo 10 3
& 5 3
1 54^
t 342 1 3TU
3 m 9
x r ft 37
4 A
4 4ft 4 3.1
4 13 3. tin
3 .19 3 29 3 19 3 13
J V9 2 V7 2 * 3.AS 2 7ft 2 39 2 24 2 21 2.1ft
2 `W 2 2 2 lai 1 J W9 1 * 1 77
I X13 1.749 1 c m2 1 ft. 1 U39
t fox 1 3K1 1 37* I .Vtt 1 VA l M3 1 39*
3 32
30 13
30 42 la
pit 99 !A 6?
3 4 11 9 It
.m 13 n 2ft 22 U 27
1ft
1f1t
& A
9
9ft
4 Ift 9 1.1
3 34
&
4 31 4 19 4 11 3 Aft 3 47 3 3* 3 27
3 no 3m 2 UH 2 urt 2 Mt 2
2 37 2 2ft 2 20 2 Ift 2 11 2 ** 2 *1 1 9*3 1 Wl I 914
| WU 1 Soft 1 ICJ*
34 &
33 a 3 31 a
n & p>t w S3 3
3 3 9 X 3 .11 13 ft 22 22
IX 25 X
1 ft.14 1 K23 1 i-O I .v**
1 .VA l Vd 1 M4 1 M9
X 9 9 2
3 12 9 12
shown io Fig. I. All the curve* ire continuous and the three nmj*>und* have almost identical linear thermal rxjsiftuont I>uring the final firing of these liar *|rimetis it vu noted that the edge* lecamr slightly roumlrd almVr ft)il 3*il"C; the firing therefore w** halted at this tnnj>eraturT since good sintering had already j*uduced a suitable raian^m f|>ed* men I'ndu the optical ir.tcrmcnj< or.lv the {jlite phie wu <ilnerved in these sjicciniens. making it highly likely that the routi 'ing ( roccs* was due to Ik s of oxide c.mijwnent* from the >j*'.:i>efl surface. Piflermtial thermal analysis mm ere nude on small portion* of llie lsr letimens, giving melting tcmjcfaturr of h7.1*C (.MliO-SfOfXW, WS"C (Mid) OO, P/V, and lv5*C (MliO-OeO,-VA); each tmijerature a* 7* to X' lirlow thv re^-ifled hy Metier and Wondratschek.*
The X ray dilTraelion data fur these omijuninds are shown in Table 111.
Kf I. Uw ax>w*i a i.Ow
9* *t+**r**+-+ir* *rn*A fsO ?r>o 0*0*
X-ray riifTracti'Hi data were Own otKaincd Iwtwten n*>oi
tnnjwrjture and `.V** C a* sh-.w n in Table 1V. 11 is interest mg
to note that Ufth 11AVO, and ri.MnO, a/lrf relatively rajrid
coding to n>m tiinjsfalufc on tvr-r tis*n trinj-ctaturtr* do
ivc/t give pa* term which ague with the original r>>tn tm*
jwrature jxtlctns (which are in rvwntial agos-imm with
.VSTM data* /* |lie I wo uanja Airjilst If. h>>w v\ if. the sfwvr-
ttwti i* left osenuglit. \crv rV-w agnnnml with tile nginal
|*allcm is obtained IIh -w tlala indicate I |>fiJulilr rr-
arrar., emi-nt of Ihr 1h *m\ miial a*<*ni* in these (aui-amds
at high tcmjrialurrs and a \i-rv j*n mourned thjwndrtice
in time in returning to ther<>ni tmi|s-r.itme <a;ligur-ati.o *
71e line splitting lernrd in
at high trm|cT*aJnrr*
mjv indicate a transition fr.-m the tctfag-mal vhrelitr struc
ture to one of lower symmetry.
The two o4/t|a>onds have the same sfuve gr**up *' CaWO
-- /I, al and simiUr lattnv |ararmtrTsas follow*:
CaWtt, PbMoO.
Hi WO*
3 242 5 4X\
41 5 PUft A 44
11 372 12 11 12 m 4 2 o4ft 12 m
v,
<*l <*) <91 tX) <9)
Arali* has shown that the Hi i*ns are as\iunHricully urrocnWd hy oxygen* in HiMotl*, similar to other lead mm-
(3) 190J TvnptM* and Uod MoJyidoft
The linear thermal -expansion curves of PbWO, and HiMofh are shown in Fig 2. Jaeger and (Terms* claimed that IlilVO* has a reversible inversion at X77C. hul the j>tcsent rsjwnsioti curve doc* not s Im.w an inflection ut thi* joint and a DTA run sltowed no Ih *a I eflect.
* AST.M l>ata File*. Americ-an Swirl) U<t Tr>tlnf *ml Ma- .
teriaW. Philadelphia. IS * L 11 Sr.rn and Anna IJsa X\landrf. "Ossgrti ISisJthms
In Tungstate* amt M'-liUlaOv with SlM-rhtr Structuir," .Irlir. Ktmi. Mtnftal Gr,4 , 17A HI I .*7 I lUWj.
" Tak diaru Ar.ki. "Cn .*! Slfu* Hire <4 WuHenitr, |tiM**0.`* Mfm (W/ \i rM Kv.4....V< fl.ii, t.Vi Onth:;Mi Fnglohl
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l)iJttlomiln( tnui A'-/My l\tUt /or /.aW t nm/xMrm/*, // TcbU IV. X-Ray OiffToeiion Dole f*v PbWO orrd PblAoOi
It.WO,
r*v*
wc IwXfll
rn*c
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|wMich a* ihc <>\i.l<, f.4 rxaiH|.lr Inlrtxln* * <( b-ad into the Mnnturr imt dv etjamU the latticr (r|<via!lv in the f dirivtiotil hat al lirin^'* n^xit a chjn^r in the Viral rmifomnmt <4 the W\ <n and in ilir ynmietty <4 the MnulHrr at hi^b tcMijxiaUirr rrLitiw- to fciii lemi-cr alurr
The hi^h ti-mja-rjtmr dilTraili'St |ialt-m* <4 |'h\V<l, a*id H.M.4 l( wrfr ohlamed l.v funning at l"* jef MiitJUtr, and at trni|>rfaturrs the vjx-iintrm may not have l*een fullv r.|ui!it<airil to llu- ct'mt needed for g.**! thermal rxjan\*<i dal* `live hi>:h temjK^atuir X ray data therefore were tv*t UM-tl f>r the rah .ilation i4 a amt < expansion ox fli.-K-tm *r for eoiH}ari-fi with the linear dilatoinelrir data
(4) (tod OoemoooN at*J 1+oJ AJvmmat* Thr litirur thermal et|ans>on rharatleri it in `4 -MlfOvVOi
tnd 1*14 ) Aid h irr 4h ih in Fig. 2 `l he X niv 'hflra1t*m dati f**r -I*14)-(VOj and It/l-AljO*
are slmwn in Table V. TIk - daia f.r HiO-Al/h art in (nod agreement with tin- |reviom work <4 Celler and Hunting.*
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