10
Journa / Va t. 2 1, No. 85 ,1 978 X- RAY DIFFRACTION TOPOGRAPHIC OBSERVATIONS OF THE LARGE-ANGLE GRAIN BOUNDARY IN ICE UNDER DEFORMATION By T. HONDOH and A. HIGASHI (Departm e nt of Applied Physi cs, Faculty of Engin ee ring, Hokkaid o University, Sapporo, Japan 060) ABS TRACT . Large-angle tilt grain bound a ries in a rtificia ll y-grow ll i ce bicr ys tal s we re observed by th e method of X-r ay diffraction topography. In bicr ysta ls for which mi sori e nt a tion a ngl es sa tisfy the conditions o fa high-d ensity coincidenc e s it e latt ice (CSL) a t th e bo undar y, th e ima ges of fin e parallel lin e defects app ea r on the topograph taken imme di ately after a ligh t d e fo rmation . Sin ce th ese images di sa ppea r in a time peri od betwee n several hours and a few days and r ea pp ea r aga in at the sa m e sites when the sp ec im en is deformed subseque ntl y, it is co nclud ed th a t these line defec ts are not stable like th e boundary di sloca ti ons but may be steps gen er ated on the bo undar y to for m facets which co in cide w ith th e high-density CS L plane . X-r ay topogr a phi c images of bo undari es which do n ot sa tisfy the co ndition s of a high density CSL are complex and difficult to int erp ret, alth ough so me of the im ages indi cate that ther e ma y be different types of stru ctur es on such bo und a ri es. R EsuME. Observa tion s par topogra/Jhie X d es joints de grains aforte disorientation dall s la glace en coms de difor lllat ioll. On e tudi e l es j o ints de gra ins it forte desorie nt ation dans d e5 bic ri staux de gla ce artifi ciel le p a r topographi c X. Pour les bicris taux dont la d es ori e ntation angula ir e sa tis!a it le cond i tion de gra nde dens it e CS L (reseau de coincid e nce ), juste a pres un e faibl e deformation , o n obse rve d es def a ut s sous forme de fin es li gnes paralleles. Ces li gnes di sparai sse nt dans un l aps de temps co mpri s e ntr e quelqu es he Ul ·e, et plus ieurs jours, puis d ies rea pp araisse nt aux memes e ndroit s lorsqu e I'ec ha ntill on est redeform e. On peut d onc en co nclur e qu e ces defaut s ne so nt pas stables co mm e d es disco ntinuit es des joints de gr a ins, mais pourra ie nt e tr e d es marches creecs s ur le joint pour fo rm e r d es fa cett es co rr espo ndant it un e fort e coinci dence . Les top og r ap hi es d es joints de grain s qui n esa tis font pas les conditi ons d e fo rt e coinciden ce so nt comp lexes e t d iffi c il es a interpr e ter. Cepe ndant, quelques un es d 'e ntr e ell es mont rent qu' il pourrait y avo ir plusicurs so rt es de s tru ctur e dans ces joints. ZUSAMMENFASSUNG. ROlltgeJIt o/ Jographiscit e Beobnchtllllgell der Grosswinkelkomgrell:;:e in Eis unter VClfoTIIlII lIg . Grossw ink e lkippk orngr en ze n in gez i.i chteten Ei s-Zwe ikristallen w urd en mit Hilf e von R o nt ge nbeugungs- topographi c b eo bac ht e t. In Zwcikri sta ll en, deren Fehlo ri ent ierungswink el an der Grcnz fh che die Bedingung I"LIl· ein Koinz id enzs tell engi tte r ( CS L) hoher Di c ht e c rl" i.i llt, crscheinen a uf der Topographi c, d ie unmittdbar n ac h einer Ieic hten Verformung a ul" genomm en w urde, Bilder feiner parallcler Lini en fehlste ll cn. Da di ese Bilder im Zeitra um eini ger Stund en bi s weniger T age verschwinden und na ch darauf fo lgender Verformung der Prob e an den gleichen Ste ll en wieder a uftr e ten , wird gesc hl ossen, d ass diese Linic nl" ehlste llcn nicht sta bil sind wie Korngr enzenversetz un gen , sondcrn Stuf en sein konnen, di e a uf der Grenzn ac he ge bildet wurd en und die sic mit Fa cetten versehen, welche mit der Ebene des Koin ziden zs te ll engitters hoher Di c ht e zusamme n- fallen. Ro ntge ntopogr a phi sch e A ufnahm en einer Ko rngr enze, we lch e die Bedin gung cl er Koin zi de nz- stell e ngitt ers nicht e rf,dlt , s ind schwierig zu de ut en. Dennoch ze igen einige von ihn en an. dass cs a uf dera rti gen Ko rn grenzen e inige ve rschi edene S lrukturt ypen geben mag. I . I NTROD UCTION In spit e of the imp or ta nt role which th e gra in bound ary pl ays in the deformation of polycrystall ine ice, no micros co pic study h as ever bee n carried out into th e s tru cture a nd behaviour of large-angle g rain boundari es in ice. The pr ese nt st ud y is an atte mpt to make cl ear the mi cwsco pi c processes which occur during deform at ion at large-angle boundaries, using the me thod of X-r ay diffraction topog r ap hy. R ece ntly , it was confirmed by elect ron a nd fi eld-ion mi croscopy th at some ordered struc tur es ex ist even in the large-angle gra in boundaries of metals at cert a in special mis- orientation relati onships (see, for exa mpl e, Loberg and Norden , 1976 ). Grain-boundary dislocations on such ordered boundari es were also observ e d. However, X-ray diffract ion topograph y has not been used so far for observations of grain-boundary structures. X-ray topography has advantages ov er el ectron mi croscopy in th at it is se nsitive to sma ll stra in fi eld s, and large specimens can be scanned, al though the reso lution is low. In o rd er to have good images on an X-r ay topograph, it is necessary for th e crystal specim ens to have low 62 9

X-RAY DIFFRACTION TOPOGRAPHIC OBSERVATIONS OF THE … · method of X-ray diffraction topography. In bicrystals for which misorientation angles satisfy the conditions ofa high-density

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Page 1: X-RAY DIFFRACTION TOPOGRAPHIC OBSERVATIONS OF THE … · method of X-ray diffraction topography. In bicrystals for which misorientation angles satisfy the conditions ofa high-density

Journa / DIG/aci~/oD, Vat. 2 1, No. 85,1 978

X -RAY DIFFRACTION TOPOGRAPHIC OBSERVATIONS OF THE LARGE-ANGLE GRAIN BOUNDARY IN ICE UNDER

DEFORMATION

By T. HONDOH and A. HIGASHI

(Department of Applied Physics, Faculty of Engineering, Hokkaido University, Sapporo, Japan 060)

ABSTRACT. Large-a ngle tilt grain bounda ri es in a rtificia ll y-growll ice bicrys tal s were o bserved by the method o f X-ray diffraction topography. In bic r ysta ls for which misorienta tion angles sa tisfy the conditions ofa high-density coincidence site lattice (CSL) a t the boundary, the ima ges of fine parallel line defects appea r on the topograph taken immediately after a ligh t d efo rmation . Since th ese images disappea r in a time period between severa l hours and a few days a nd reappea r aga in a t the sam e sites when the sp ecimen is deformed subsequentl y, it is concluded tha t these line defec ts a re not stable like the boundary dislocations but may be steps generated on the boundary to form face ts w hich coincide w ith the high-density CSL p lane . X-ray topogra phic images of boundaries which do not sa ti sfy the conditions o f a high density CSL a re complex and difficu lt to interpret, a lthough some of the images indica te that there may be d ifferen t types o f structures on such bounda ri es.

R EsuME. Observations par topogra/Jhie X desjoints de grains aforte disorientation dalls la glace en coms de diforlllatioll. On e tudie les j o ints de gra ins it forte desorienta tio n d a ns d e5 bicristaux d e glace artifi ciel le p a r topographic X. Pour les bicri staux dont la d esorientation a ngu la ire sa tis!a it le cond ition de grande d ensite CS L (reseau d e coincidence), juste apres une faible deformation , o n observe des defa uts sous forme de fin es lignes paralleles . Ces lignes disparaissent dans un laps de temps compris entre quelques he Ul·e, et plusieurs jours, puis d ies reappa ra issent a ux memes endroits lorsque I'ech a ntillon est redeforme . On peu t donc en conclure que ces defauts ne sont pas stables comm e des discontinuites des joints de gra ins, ma is pourra ie nt e tre des march es creecs sur le joint pour fo rmer d es fa cettes correspondant it une forte coincidence. L es to pographies d es joints d e grains qui nesa tisfont pas les cond itions d e fo rte coinciden ce sont complexes e t d iffic il es a interpre ter. Cependant, quelques unes d 'entre ell es montren t q u ' il pourra it y avoir plusicurs sortes de structure da ns ces joints.

ZUSAMMENFASSUNG. ROlltgeJIto/Jographiscite Beobnchtllllgell der Grosswinkelkomgrell:;:e in Eis unter VClfoTIIlIIlIg. G rosswinkelkippkorngrenzen in gez i.i ch teten Eis-Zweikristall en wurde n mit Hilfe von R o ntgenbeugungs­topographic beobachtet. I n Zwcikrista ll en, deren F ehlo ri entierungswinke l an der Grcnz fh ch e die Bedingung I"LIl· ein K o inzidenzs tell eng itte r (CS L) hoher Dichte c rl"i.i llt, crscheinen a uf der Topographi c, d ie unmittdbar nach eine r Ieichten Verformung a ul"genomme n w urde, Bilder feiner p a ra llcler Linien fe hls te ll cn. Da diese Bilder im Zeitra um einiger Stunden bis wenige r T age verschwinden und nach darauf fo lgender Verformung der Probe a n d en gleichen Ste lle n wieder a uftre ten , wird geschlossen, d ass diese Linicnl"e h lste llcn nicht stabil sind wie Korngrenzenverse tzungen, sondcrn Stufen se in konnen, di e a uf d er Grenznac he gebildet wurden und die sic mit Facetten verseh e n, welche mit der Ebene des Koinzidenzs tellengitters hoher Di chte zusammen­fallen. R ontgentopographisch e Aufnahmen e ine r Korngrenze, welche die Bedingung cle r Koinzidenz­stellengitte rs n icht erf,dlt, s ind sch wierig zu d euten. Dennoch zeige n e inige von ihne n an. dass cs a uf dera rtigen K o rng renzen einige verschiedene S lrukturtypen geben mag.

I . I NTROD UCTION

In spite of the importa nt role which the grain bounda ry plays in the d eformation of polycrystall ine ice, no microscopic study has ever been carried out into the structure and behaviour of large-angle grain boundaries in ice. The present study is an attempt to make clear the micwscopic processes which occur during deform ation at large-a ng le boundaries, using the m e thod of X-ray diffraction topog raphy.

R ecently, it was confirmed by electron a nd field-ion microscopy th at som e ordered structures exist even in the la rge-angle gra in boundaries of metals at certa in special mis­orientation relationships (see, for example, Loberg and Norden, 1976). Grain-boundary dislocations on such ordered boundaries were a lso observed. However, X-ray diffraction topography has not been used so far for observations of grain-boundary structures. X-ray topography has advantages over electron microscopy in tha t it is sensitive to small strain fields, and large specimens can be scanned , a lthough the resolution is low. In order to have good images on an X-ray topograph , it is n ecessary for the crystal specimens to have low

629

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J OU R NA L OF GL AC I O L O GY

dislocation densities; It IS this requirement which might have prevented the observa tion of grain boundaries by X-ray topography. Since ice is compa ra tively transparent to X-rays and a technique for growing bicrystals of ice with a low disloca tion density h as been developed in our la boratory, X-ray diffraction topography has become a good m ethod by which to observe grain boundaries in ice.

Grain boundaries of som e bicrys ta ls were observed by X -ray diffraction topography in the as-grown state and after successive deforma tions. Differences between images and the behaviour of images with d eformation and subsequent annealing are discu ssed in terms of the coincidence-site la ttice concept (CSL). Two kinds of bicrystal were grown , with tilt gra in bounda ri es having c-axis misorientations a round the ( 1010 ) ro tation axis of 34° and 47 °. The 34 ° boundary is expec ted to have an ordered structure in CSL and the 47 ° boundary is not.

2. E XPE RIMENTAL PROCED UR E

Since grain-boundary defects, in general, cause only sm all strain fields, it is difficult to distinguish their images from those of la ttice dislocations if dislocation densities are high in the grains on both sides of the boundary. Therefore, it is n ecessary to use bicrystals with Iow dislocation densities for studies of grain-boundary structures. It is also n ecessary to have a fixed misorientation rela tion in the bicrystals together with a very fl at gra in-boundary plane . Althoug h it was not an easy task to obtain good bicrys ta ls, exp eriments in our la boratory have made it possible.

I ce bicrystals which h ad ( 1010) tilt large-angle gra in boundaries were g rown para llel to the < JO I 0 ) axis by the Czochralski method . A seed bicrys tal was made by growing two sing le crysta ls of Iow dislocation density in such a way that the c-axes rota ted e a round the < I 0 I 0 )

axis. When the growth direction was norma l to the rota tion axis w, the gra in-boundary pla n e tended to curve strongly a nd many sm a ll-angle gra in b oundaries were emitted from i t. On the o ther hand, when the growth direction was pa rallel to w, the bounda ry extended as a plane in the direction of growth . It grew a lmost exactly p arallel to the direction of w bu t sometimes bent slightly in the direction n ormal to w a nd a few small-angle grain boundaries were emitted from the curve of the boundary. Good portions cut from a bicrys tal grown para llel to w were used for seeds as well as for the experiments. Good bicrysta ls were obta ined in which the dislocation densities were b e tween 106 m - 2 a nd 108 m- ' .

The rota tion angle e was fixed a t a pproximately 34° (C SL) or 47° (no t CSL). The grain­bounda r y plane should coincide with the (12 1 I) plane in the case of 8 = 34°, but for 8 = 47 ° the grain boundary does not coincide with a ny plane of low indices if the boundary pla ne bi­sects the rota tion angle.

Specimens used in this work were cut a nd formed by band sawing a nd planing bu t withou t chemical polishing. Dislocations, which are genera ted a t the surface due to the mecha nical stress which accompanies su ch preparation m ethods, disappeared after ageing for a few days and did no t affect the ob servations.

All observa tions and deformations were carried out in a cold room a t - 20°C . X-ray diffraction topographs were taken using a la rge Lang cam era (scanning a r ea 8 X 10 cm') with a powerful rota ting X-ray source (Mo ta rget) opera ted a t 50 kV and go mA. Genera lly, a pair of topographs was taken having th e same diffracting plane for both crystal gra ins in order to observe both sides of the boundary.

Bicrys tal specimens, wi th a scanned a r ea of several squa re centimetres a nd a thickness of severa l millimetres (as illustra ted in Figures 1, 2 , and 4) were subjected to sm all uniaxial com ­pressive strains. Applied stresses are given in the figure captions together with the dura tion of deforma tion.

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OBSE R VAT I ONS OF I CE GRA I N BOUN D A RI ES

3. R ESULTS

3. I. Specimens with 8 = 34° T he pair of topographs shown in Figure I (a) was taken with a [1010] g-vector for both

grains. T he grain-boundar y p la ne ABeD can b e clearly identified by the Pende116sung fringes, a nd very few dislocation im ages can be seen in both grains. After a light deformation with shear stress of a bout 2. 3 X IQ5 Pa (2-4 kg/cm 2) acting on the grain boundary for a bout 10 s, many fine lines (parallel to I - I ' as shown in Figure I (b)) appeared on the bounda ry plane in

A 91 [10101,

A

B B

~ 91 [10TOh

(a)

A 91 [10TO], A

~/' , . 0

B

91 [1010]2

( b)

A

B

(e) Fig. I. L ine defects on a [IOIO] /3 ,t till grain boundary.

(a ) A pair of X -ray di/fracliontopographs taken with [1010] g -veclor of both grains before the specimen was deformed. (b) T opographs of the specimen just (ifter the first light deformation. Note parallel line images l - l ' . (c) Topographs taken with (2I IO ) diffracting plane of the specimen just after the second light defonnation. Note parallel line

images 2-2'.

(d ) Topographs of the specimCll aged for 2 d after a deformation for a long period : shear stress of 9.8 X 10' P a ( l kg/cm' ) on the boundary for I h.

(e) Schematic illustration of the specimen.

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JO URNAL OF GLACIOLOGY

topographs taken with the same diffraction conditions as those in Figure I (a). Since these para llel line images are recognized in both topographs of grains I and 2, it is clear that these images originated from strain fields around grain-bounda ry defects genera ted by deforma tion. Most of them extended from one end of the boundary p lane to the other, but some of them terminated in the middle of the boundary plane. These images disappeared within a few hours, during ageing at - 20°C, so it is difficult to obtain topographs of these defects taken with various diffraction conditions to determine the Burgers vector.

When this specimen was subjected to subsequent d eformation, almost the same images again a ppeared on the topographs. Figure I (c) shows a topograph taken with a [21 10] g-vector immediately after the second deformation. W e can observe another type of parallel line defect (designated 2 - 2') on this topograph in addition to those of Figure I (b). The crystallography of this specimen is shown in Figure I (e) . The rotation axes w, determined

A

c (c)

Fig. 2. Line difects on a bent [10;0] 134° tilt boundary.

(a) A topograph taken with ( TOIO ) diffracting plane just after a light diformation, compressive stress ,, ~ 2.0 X IOS Pa ( 2.1 kglcm' ) was applied as shown on (b) for 10 s. Shear stress in the regions of AB and BC was approximately I X IOS Pa ( r kglcm' ).

(b) Schematic illustration of the specimen. (c) Misorientations of the boundary planes AB and BC with respects to basal planes cif both grains.

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OBSE R VAT IO NS OF I CE G R A I N BOUN D ARIES

to be [IO I 0] for both grains, a re parallel to each other to within about 1°. Since w is approxi­mately on the boundary p la ne ABeD, the in tersections of the boundary p la ne with the ba al planes of both grains were nearly parallel to w . T he direction of a line defect, as described a bove, will b e expressed in terms of the a ngle 0 between w a nd the line of the defect. 0 for the line defects of I - I ' and 2- 2' in Figure I a re roughly 35° and 0° respectively. T he line defects 2- 2' in Figure I (c) did not a ppear on the topogra ph Figure I (b) which was ta ken with a [ 10 I 0]

g-vector. Since the line defects run parallel to the rota tion axis w , or [ IOI O], this is well understood from the extinction condition g . U = 0, if the displacement field vector U is assumed to be perpendicular to the line of the defect.

Lattice dislocation configurations inside the crystal did no t change apprecia bly with light deformations as can be seen if Figure 1 (b) is compared with F igure 1 (a). However, boundary defects were generated by such a ligh t deforma tion. Therefore, these grain-boundary defects are not the d efects genera ted by the absorption of la ttice dislocations. T he fact that the sam e images appeared again after successive lig h t deformations m ay imply tha t these defects ar e closely related to the grain-boundary structure itself and this presumption is confirmed by a set of observations shown in Figure 2.

Figure 2 (a) is an X-ray topograph of a gra in boundary of the same kind as before (8 = 34°) which was disposed in a specimen in the way shown in F igure 2(b). The boundary bent several degrees a t A, B, and c, and bent a good deal a t D . R egions of AB, BC, CD, and the upper­part above A were macroscopically fi a t, but the lower part below D was curved . Strong images at b ends A, B, C, a nd D and the other line images in F igure 2(a) appeared just after a light compressive deforma tion in the direction (J on Figure 2 (b) . T wo kinds of fine, parallel line images in the region B C correspond to those shown in F igure I (c) . T he a ngle 0 between the line defects and w = [IOIO] was roug hly 35° and 0° for grains 1 and 2 in F igure 2 res­pectively. Many strong images with differen t directions existed in the region AB as indicated by the numera ls 3 to 7. T he crystallogra phic orientations of regions AB and BC were not

(a)

L lmm L-...J

( b) (c) Fig. 3. Change of images rif grain-boundary difects during ageing at - 20°C. Allto/Jographs were taken w ith (1 lOO) diffracting

plane.

(a) A topograph taken jllst after a light diformatioll shear stress of 2.2 X IOS Pa (2.2 kg/cm2 ) was ap/)lied on the boundary for 30 s.

(b) A topograph taken after ageing for 4 h. (c) A topograp!Z taken after ageing for I d.

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J OU R NA L OF O L AC IOL OOY

symmetrical, but made almost the same deviation from symmetry as is shown in Figure 2(C). The line of the bend B is not parallel to the rota tion axis w , although the line defect 2 is parallel to w. Even though the misorienta tion angle f) is a pproximately 35° both for AB and BO, such a small cha nge in the orienta tion of the boundary pla ne introduced a large difference in the a ppearance of the boundary defects. Complex stra in fields can be recognized in the lower r egion below D , in which the bounda ry plane was considerably devia ted from a sym­metric disposition .

The images in Figures I (b) and (c) disappeared within a few hours of the end of the first deforma tion, but further d eformations intensified those images and they then took a few days

A A

B

(a)

( b)

(c)

Fig. 4. D ifects on the [IOIOJ/47° tilt grain boundary. All topographs were taken with ( IOi'O) diffracting planes.

(a) T opographs before deformation. (b) T opographs after the first deformation, shear stress of 5.4 X 10' Pa (0.55 kg /cm2 ) was applied on the bOUlldary fo r I h. (c) A topograph after the second deformation. (d ) A schematic illustration of the specimen. Rotatioll axis w was not on the boulldary plane exactly but its deviatioll was small .

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OBSERVATIONS OF I CE G RAI N BOUNDARIES

to disappear by ageing processes (Fig. I (d )) . A typical disappearance of line defects at the boundary is shown in Figure 3. Weak images such as I - I ' a nd 2- 2' in Figure 3 (a) completely disappeared in four hours and the strong ones gradually broa dened (Fig. 3 (b )) and became fainter a fter a day (Fig. 3 (C)) . After ageing for a few days, no boundary defec ts were recog­nized in the region BC in Figure 2, bu t the defects such as 3, 5 , a nd 6 in the region AB were still visible a nd complex stra in fields existed in the lower part below D.

Lattice dislocations on the basal plane seem to be generated from points where grain­bounda ry defects meet the specimen surface as can be seen in Figure 3(a) . Therefore, lines of intersec tion of the boundary and the specimen surface would a ppear to be the m ost favourable sources for lattice disloca tions during deformation.

3. 2 . Specimen wilh e = 47°

The dislocation density in the 4t specimen was high (Fig. 4), so that fa int images could not have been distinguished even if they ha d ex isted at the boundary. All of the topographs in Figure 4 were taken with (1010) diffracting planes in both grains I a nd 2.

Figure 4 (a) shows topographs taken just after the specimen was prepared. The images xy were generated by plane-bla de scratches on the surface a nd they disappeared during ageing as shown in Figure 4 (b ) . The boundary plane was bent at AB and, less severely, at CD. The images AB a nd CD were similar to those occurring along bends of the boundary as shown in Figure 2. Most characteristic defects begin at intersections of the boundary with the specimen surface and extend furth er into the interior a long the boundary pla ne as deforma tion increases (e.g. EF a nd GH ) . S for EF was approximately 65°. These images disappeared in a few days during ageing at - 20°C as with the e = 34° specimens. The a ngle S between the rotation axis wand those parallel line images which a re just visible a long IJ in Figures 4 (b) and (c) were roughly 20°. These line images a re simila r to the line defects I - I ' in Figure I , they a re stra ig h t a nd inclined to the rotation axis with angle S. However, other images were very different from those obtained with the specimens with 8 = 34°.

4. DISCUSSION

The fine, parall el line defects observed on the grain boundary of a 34° specimen indicate that the gra in boundary h a a n ordered structure. Coinciden ce site lattice (CSL ) construction is useful in a n examination of the periodicity of gra in boundaries (see, for example, Brandon a nd others, (964). A CSL is constructed from the coincident sites of two crystal lattices set at arbitra ry misorienta tions. Although in genera l, the unit cell of a CSL is la rger than that of the origina l grains, it becom es comparatively small when the disposition of the two gra ins satisfi es certa in special misorientation relationships. It is difficult to consider the CSL for the ice structure, so, for an a pproximation , we consider the simple hexagonal lattice with cia = ,';8 /3. Figure 5 (a) shows the unit ce ll of the CSL formed for a 34.05° rotation around the [1010] ax is. Since 35 lattice points of each grain (open a nd closed dots) are included in a layer OPQ,R of the unit cell as shown in Figure 5(a), the r eciprocal density ~ of CSL points is 35 . The same atomic a rra ngement is made on an adjacent layer shifted I. 7a to the direction [1216]. A three-dimensiona l unit cell of the CSL is shown in Figure 5(b) . The value of~ in this CSL is not small , but the density of CSL points in the pla ne O PTS (12 1 I ) is very high . T herefore, it is expected that the boundary has an ordered structure if the boundary plane lies on, or nearly parallel to, the (i 2 1 I) pla ne in a bicrystal with this misorientation.

The CSL theory predic ts two kinds of line defects: structural gra in-bounda ry dislocations, which compensate for deviations from exact CSL misorienta tion, and steps, which are generated by breaking the boundary into low-energy facets when the average boundary plane does not lie parallel to a high-density CSL plane. Structural grain-boundary dislocations

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JOURNAL OF GLACIOLOGY

p ~ " ~I'. ,--O---O--------~~O--O-----------'O'--O----------~'

• 0 0 0 • 0

o o o

0 0

0

0

o o o ~.1c} : ~\V~-----------D--~--------~O~~------------~"R

o • 0

o • o

o • 0

o o o

(0 )

( b)

Fig. 5. Coincidence site lattice for the case of 8 = 34.05°.

(a) Arrangement of both lattice points on a layer perpmdicular to the rotation axis [1010] in a unit cell of CSL. Open dols are lattice points of grain 2 and closed dots are those of grain I.

(b) A unit cell of the CSL, the roiation axis is OS. OS ~ I .7a, 0 W ~ I.9a, OP:::; 3.40, and OR ~ 16.7a, where a is Ihe leT/glh of a-axis of ice. The plane OPTS coincides with (1 21 I ) bowzdary plane.

have been observed in metals by electron microscopy (for example, Ishida and others, 1969; Balluffi and others, 1972) and it has been confirmed that they can exist on the boundary in an equilibrium state. Since the line defects observed on the grain boundary in ice disappear after annealing, they cannot be stable grain-boundary dislocations of this type.

Faceting of grain boundaries has also been observed in metals by many investigators, and it has been well explained by the CSL theory (Wagner and others, 1974) . In a previous study which we have made into the boundary migration of ice bicrystals, * macroscopic faceting of grain boundaries was observed, the facet planes being approximately parallel to the os, OT, and ps directions in Figure 5, all of which were close-packed directions of the appropriate CSL. Steps thus generated by faceting are probably strain-free in the equilibrium state. However, when the specimen is subjected to stress, and grains slide past each other on the boundary plane between the steps, new strain fields should be generated around the steps due to a concentration of plastic deformation there. Images of type 2-2' in Figure I (c) and of type 2 on the BC plane in Figure 2(a) appeared after deformation of the specimens and are well-understood to be steps around which strong strain fields were generated by the process described above. The fact that the displacement vector U of the 2-2' line defects in Figure I (C) is perpendicular to the line as described in Section 3.1 supports this concept.

Clear, straight, parallel images of I-I' type in Figure I and of type I in Figure 2 may also be interpreted as a stepped structure of the grain boundary, although their direction (0 = 35 0

) is not parallel to any high-density row of CSL points on the (1211 ) plane. The disappearance of the images after specimen annealing is similar to the behaviour of type 2-2'

* Paper by T. Hondoh and A. Higashi entitled "Anisotropic migration and faceting of large-angle grain boundaries in ice bicrystals", in preparation.

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OBSERVATIONS OF ICE GRAIN BOUNDARIES

images (Fig. 3) and indicates that the strain fields relaxed in a bout one day. R eappearance or these line images at the sam e sites on the boundary after furth er deformation a lso supports this idea.

It seems to be difficult to interpret the other, more complex images (from 3 to 7 on the plane AB in Figure 2(a)) in terms of the CSL concept alone. The plane AB deviates from BC by 6.3° as indicated in Figure 2 (b ) . However, on the microscopic scale, AB and BC make the a ngles with the basal planes of two grains in the bicrystal shown in Figure 2(C) . Devia tions from symmetry a re the same for both AB and BC, but defect structures on the boundary are quite different. H artt and others ( 1974) observed similar curved grain boundaries in zinc and discu sed a corrugated boundary structure which could explain the deviation of the mis­orientation from the exact CSL value. Further experimenta l studies are needed before such an idea can be applied to ice.

Complex strain fields are observed on the boundary as shown in Figure 4 a nd, as stated in Section 3.2 for the case of e = 47 °, the a ng le deviates appl'eciably from a n exact CSL misorientation relation (Higashi, 1978). These are more difficult to explain qua ntitatively. However, since the defects desig nated EF on Figure 4 extended during deforma tion and reappeared during repeated d eformations even a fter they had disappeared during ageing, it can be said tha t the grain boundary of such a disordered structure has different types of structure and that these change regularly with straining along the boundary.

REFERE CES

Balluffi , R. W. , and others. 1972. E lectron microscope studies of gra in bounda ry dislocat ion behavior, [by] R . W. Ba lluffi, Y. K omem and T. Schober. Surface Science, Vol. 3 1, p. 68- 103 .

Bishop, G. H ., and others. 1971. Grain boundary faceting of <10(0) tilt boundaries in zinc, [by] G . H. Bishop, "V. H . H artt and G . A. Bruggeman . Acta M etallurgica, Vol. 19, No. I , p. 37- 47.

Bra ndon, D. G., and others. 1964. A field ion microscope stud y of atom ic configura tion at grain boundaries, [by] D. G. Brandon, B. R alph, S. R anganathan and M. S. Wald. Acta M etallllrgica, Vol. 12, No. 7, p. 813- 2 1.

H artt, W. H. , alld others. 1974. Grain boundary faceting o f < 10( 0) tilt boundar ies in zinc. II , [by] W. H. H a rtt, G. H . Bishop a nd G. A. Bruggeman. Acta M etallllrgica, Vol. 22, No. 8, p. 97 1- 83.

Higashi , A. 1978. Structure a nd beha viour of grain boundaries in polycrystalline ice. J ouT1Ial of Glaci% gy, Vol. 21, No. 85, p. 589- 605.

I shida, Y. , and others. 1969. Grain-boundary fine structure in an iron a ll oy, [by] Y. lshida, 1. H asegawa and F. Nagata . J ournal of Applied Physics, Vol. 40, No. 5, p . 2 182- 86.

Loberg, B. , and Norden, H . 1976. High resolution microscopy of grain boundary structure. (Ill C hadwick, G. A. , and Smith, D . A. , ed. Grain boundary stl'llctllre and properties. London, Acade mic Press, p . 1- 43.)

""agner, W. R ., alld others. 1974. Faceting of high-a ngl e grain boundaries in the coincidence la tti ce, by W. R . Wagner, T. Y. Van and R. W . Ba lluffi . Philosophical Maga z.ine, Eighth Se!'. , Vol. 29, No. 4, p. 895- 904.

DIS C USSIO N

W . B. KAMB: Whatis the evidence on the basis of which you interpret the line defects seen in your grain boundaries as steps in the boundary surface? Why are the steps so straight and parallel, and yet not uniformly spaced?

T. HONDOH: The fact that the line-defect images appeared only after the deformation and reappeared at som e sites after successive light deformation implies that some line structures exist on the boundary to generate the strain fields around them a fter the deformation . Possible structures are microscopic stepped structures or corrugated structures generated by decom­posing of a macros cope boundary plane to low-energy facets. We do not have any sufficient explanations about the directions of defect lines and spacing of them .

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JOURNAL OF GLAC10LOGY

D. R. HOMER: Yesterday, I presented (Homer and Glen, 1978, p. 436) some observations we have made of the deformation of bicrystals in which we suppress macroscopic grain-boundary sliding (we can, of course, say nothing about microscopic sliding) . One of our observations was that cracks appear close to the grain boundary when specimens are deformed through a strain of perhaps 0.2. This is in some ways similar to your observations here. An explanation of such cracks can follow directly from your mechanism of grain-boundary steps. If the grains separate in the opposite sense to that in your diagram then a void, and possibly a crack, can form.

HONDOR: Thank you for your comments. I have observed the macroscopic displacement along the boundary accompanied with grain-boundary migration during long-period shear deformation. I think this implies that migration of microscopic steps brings the macroscopic grain-boundary migration and the displacement along boundary.

REFERENCE Homer, D. R ., and Glen, J. \!\'. 1978. The creep activation energies of ice. J ournal of Glaciology, Vo!. 21 , No. 85,

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