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Photolytic Behavior of Silver Iodide 1 JOURNAL OF RESEARCH of the National Bureau of Standards- A. Physics and Chemistry Vol. 67A, No.4, July-August 1963 Photolytic Behavior of Silver Iodide 1 G. Burley 2 (February 24, 1963) Silver iodide exposed to high in tensity radiation in the visible li ght spectrum was found to yield a powder X-ray diffraction pattern showing marked deviations from ideali ty. It was found possible to c?rrelate these ':,ith a decrease. il! primary extinction, indicating a constant progress froD? an Ideal ~o.a mosaic type crystalhmty. Large single crystals showed ~ronounc e d astensm 111 transmiSS IOn Laue photographs under similar experimental condi­ t~ons .. SJ?all. amounts of. colloidal silver were d~t ec ted . A mechanism for this process in ~ Ilv e r I<;>dlde IS JH:oposed, 111 general ag r ec~ent wlt.h t he t heor y of t he photographic process. rhe pnma.r y. differ ence from t he other sliver halides appears to be a considerably slower rate, permitting the observatIOn of a two step process in detail. 1. Introduction filament microscope l amp through a 5 mil polyester sheet. An atmosphere of n-butyl alco hol was No detailed investigation of the mechanism of the maintained at its vapor pressure. This was chosen changes induced in silver iodide by exposure to because it accelerated the reaction only to such an light in the visible region appears to have been made extent as not to hide its essential details. The /.. pr~viously . In the. cours.e 0.£ this work, th.e photo­ sample was irradiated for a fi.;'{ed length of time and lytlC behavlOr of slI ver lOdlde has been found to an X-ray diffractometer pattern obtained immedi­ differ considerably from that of the other sillTer ately. An angular range sufficient to cover the fiT t halides. In general, polycrystalline specimens of nine line of the diffraction pattern for the hexao'onal both sihrer chloride and silver bromide darken pbase. w~s traverse.d .eacb time. For the cgpper rapidly under these conditions, du e to the formation X-rachatlOn used thIS mcluded the range from 20 to of free silver. Powder X-ray diffraction patterns 50 0 in 28, where ~ is the Bragg angle. A scanning clearly show a decrease of the pattern for the halide, rate of 0.5 0 per nunute of the angle 28 was used for a.ccompan.ied ?y a co.rresponding increase of that for maximum resolution. Approximately monochro­ slIver, wIth mcreasmg length of exposm e to a matic radiation was obtained by use of a nickel foil constant intensity light source. The behavior of filter. Cumulative exposure times to light of 200 silver iodide under similar conditions and an analysis hI' were reached in this manner. of the r esults obtained constitute the results reported In a related experiment a large hexagonal single in this paper. crystal, of approximately 5 llm diam and 1 mm thickness, prepared by slow evaporation of a 50 2. Experimental Procedure percent aqueous solution of hydriodic acid saturated with silver iodide, was exposed to light in the same . Single crystals of silver iodide were exposed to the manner. Laue transmission X-ray diffraction dia­ lIght of an arc lamp for 1 week. Initially trans­ grams were taken at t.imed intervals. :Molybdcnum parent, they slowly became opaque. Microscopic X-radiation was used to minimize absorption effects. examination showed that the initially smooth sur­ faces oTadually roughened and resembled a poly­ 3. Results crystalline aggregate. This alteration gradually progressed into the interior of the crystals. Certain The powder X -ray diffraction patterns for silver sensitizers and halogen acceptors, such as sulfur iodide showed large changes in the intensities of dioxide and n-butyl alcohol, were found to accelerate certain lines, related to the length of exposure to this process. light. The relative intensities of certain lines as a Because the action of light on silver iodide ap­ function of cumulative exposure time are shown in peared to be primarily a surface phenomenon most figure 1. The most striking feature of this graph is subsequent work was done with powder specimens. the fact that there was a rapid and immediate in­ The powder was packed into a rectangular cavity crease for the (100 ), (101 ), (102), and (103) re:flec­ and the surface smoothed. The mount was placed tions, while other reflection intensities remained in a closed container and irradiated with a bar constant. After a period of time, varying with the J light intensity and spectral characteristics of the t source, these reflections reached a plateau. After 1 This resea rch was supported by the National Scieuce Foundation uuder Grant No. 19648. this induction period the (002 ) refle ction intensity ' 'l'his work constituted a portion of a thesis submitted by the author to George­ then began to increase while the others leveled off. town University, Was hington, D .C., iu partial fulfillment of tbe reqUirements for the Ph. D. degree (1962). There was no decrease in intensity for any reflection. 301 180 160 140 150 0/ 0 Ie 120 (101) 100 (103) ,., II 00) 'in 80 c: Q) c: / 60 ~,_,-, /" . / ' • 10~ ..... .. .· ·········· ··· ..... .......... ...... \ ', 40 ..... •..... 110 20 .-. - . - .: .::::c ~=~ .= . ~ . (002) 1102) _ ...7"',<,~ . - , _ "' _ ._,, _ __ . - .. - ._ .- . _ ._" - " - . _._.I,,?,C2. ._._. _._._ "- '- . ( . /:(j~~==~=~~.g~02i --------------~ .50 .54 ,58 ,62 ,66 ,70 ,74 Z Ie for Silver ~/ o F I G1:RE 2. Calculated i ntens~tie s .for several r-efiections of i hexagonal stiver lOdlde, as a j unetlOn of the uariable zlc posi­ o 10 20 30 4 0 50 60 70 80 90 ttOnal parameter for the silver ato m , TI ME I hr FIGURE 1. Relative 1:ntensities of several low angle powder X-ray' dl:Oraehon lmes Jor silver iodide, as a function of lTradwtlOn tl 1nC by ltght m the Vls! vle region (CuKa radiat-ion) . atom. TJ~e vari l1;tion of the amplitude of the structure factors fo r the observed diffraction lines I was calculated over a fairly hU'o'e 1'ano'e of values for +- ' Secondly, the number and angular positions of t he the silver z parameter. The '=' result is shown in X-ray powder difl'raction lines were found to remain gr aphical form in fin'me 2. It is obvious that no atomic shift is poss ible which will increase all inten­ essentially il: var~3:nt during the entire procedure. No systematIc shIft was detectfible. sities simultaneo usly. Another possibili ty which had to be considered . Th.irdly, t.he pO~'7der diffraction patterns of ligh t­ lITachated sIlver IOdIde were re-examined for the was the existence of stacking faul ts. This refers to pyesence of metallic silver. The (110) reflection of random . de,:iati?ns of layers from the required sLI ver hl1;s the largest intensity and appears at a 28 progresslOn for eIther t he hexagonal or face-centered cubic lattice which are ABAB , , . and ABCABC a.ngle ?f .38. 11 0 . On the difl'raction patterns of sLI ver IOdId e samples irradiated for 50 hI' a very . :' respectively. D eviations may be introduced small and broad peak was located at this position. by eIther growth or deformation faulting. The peak increased slightly in height with successive The experimental details for this behavior have exposures to light. This clearly establi shed the pres­ been reported in the closely analogous case of cobalt ence of fin ely divided silver in amounts laro'e enouo'h metal [1 ].3 The general theory for mistakes in t? b detected by the X-ray method afteI~ expo s u~' e layer structures was published at the same time by tImes longer than 50 hr. Wilson [2 , 3]. Th~ difhacti?n pattern for a layer t:y~e s.tr u ct~r e wIth stackll1g faults has sharp 4. Intensity Changes dlflractIOn lInes when (h- k )/3 h as in teo'er values (whe1:e hand k are Miller indices ); in all ~th er cases f./ the hnes are broadened. This behavior was not The problems to be solved included findino' an observed for silver iodide, }., explanation for t he anomalous intensity cha~lO'es Thelines with integer values of (h- k )/3, indexed observed and correlating this with the theory of the m ~he hexagonal syst.em , are, however, the only ones photographic process, wluch occur also for the zincblende-type cubic The efl'ect of varying the positional parameters of polymo~ ' ph. ~rh es~ were the only difl'raction lines the at.oms on the magnitude of the intensities was whose mt en s ~ ty ~Jd r:ot change during the initial InvestIgated first. Sil ver iodide can exist in both a phase .of th.e lllul11ll1a.tIOn. The implications of this cubic zinchlende and a hexagonal wurtzite form at behaYlor WIll be con sIdered later. room temperature. No distortion of the structure An explanation in terms of a defect structure fo!, the cubic. zin cblen de-type phase is possible ~ppears equally unlikely since the line widths and wltho~t destroYll1g the symmetry. In the hexagonal mcoherent backgroynd ,scattering did not change wurtzlte-type structure the x and y parameters of markedly. Annealmg of a defect structure does in­ both atoms are fixed and only the z parameters can crease t he peak heights of the diffraction diagram, var~. In addition, the origin may be chosen arbi­ but the area under the peak profiles remains constant. trarily .and can be placed at the iodine position for conv~men? e .
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