Institute of Metals Division - Dislocations in Ruby Laser Crystals

As part of a program to establish the effect of crystal imperfections on laser output, a detailed study was made of the dislocation structure of ruby crystals obtained from varioius sources. Using KHSO4 as an etchant, a detailed mapping of the dislocation structure on the (0001) and the (1150) planes was carried out. A less extensive study was made of the rhombohedral planes. The average dislocation density on the basal plane was 1.5 to 3 x 106 cm&apos;2 and on the (1120) planes -5 x 10&apos; cm-2. Howe7!er, considerable variation existed between areas on a given plane. The subboundaries in the basal plane tended to lie along [1100] type directions while those on the (1120) plane tended to lie: a) parallel to the basal plane, b) along truces of the (1101) plane, and c) along normals to the traces of the (0001) planes. The orientations suggest that mang of the dislocations lie on the (0001), (1701), and (1150) planes A Laue back-rellection nnalysis Of c-axis wander in one crystal revealed a gradual increase in misorientation from me end of the crystal to the other, with a maximum variation of 1°35&apos;. Slight etching of a mechanically polished crystal revealed mumerous polishing scratches, suggesting the existence of a plastic flow layer. It is recognized that chromium concentration, lineage, and other crystalline imperfections play a role in the efficiency of ruby lasers.&apos; Consequently, it is desirable to establish in detail the imperfection structure of ruby crystals to be used as lasers. Some exploratory work along this line had already been done by Barnes&apos; and Dils and Martin.&apos;" How- referred to as the morphological system, as described by Kronberg.4 The Miller indices given in the present paper will be based on this morphological system. In this system, the three common growth planes are the (0001), the {1120}, and the {1101}.5 Since these planes are of high stability, it is expected that they are most suitable for study by the etch-pit technique. In the present investigation, a detailed mapping of the dislocation structure was carried out for the (0001) and the (1130) planes. A less extensive study was made of the etch-pit structure on rhombohedra1 planes. An analysis of dislocations in sapphire (the ruby host) was first made by kronberg,4 who postulated that slip on the (0001) plane occurred by motion of dislocations with Burgers vector 1/3 <1150> and that these dislocations might dissociate into quarter partials. An etch-pit technique using boiling phosphoric acid was developed by Scheuplein and Gibbs6, 7 for identifying dislocations intersecting the (0001) planes and the planes near (2021) in sapphire. Al-ford and Stephens8 were able to reveal dislocations on the (0001) and {1120} planes in sapphire and ruby by etching in fused potassium bisulfate (KHS04) at 675°C. The termini of basal dislocations [(000l), <1120>] were revealed by Palmour and Kriegel9 on {1120} and {1010} by thermally etching sapphire. Bond and Harvey10 were able to decorate dislocations in sapphire by adding 1 pet by weight of ZrO2 to the Al2O3 powder used in the growth of the crystals by the Verneuil technique and then heating the grown crystals for 4 hr at 1500°C. They found, using optical transmission microscopy, that many dislocations had straight segments which were parallel to one of the six [1120] directions in the basal plane. Single dislocation lines curved smoothly from one alignment to the other, turning through angles of 60 to 120 deg. Also observed were isolated hexagonal loops, approximately 10 µ in diameter, the sides of which lay along the same directions as did the longer dislocations. MATERIAL AND ETCHING PROCEDURE The ruby specimens used in this study (all containing approximately 0.04 pet Cr) had been obtained from four different sources: Linde Co., Meller Co., Valpey Crystal Corp., and those grown at Aerospace Corp.* For the initial phase of this study, several specimens were cut from the slab shown schematically in Fig. 1 which had previously been cut from a disk boule obtained from the Linde