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Platinum Metals Review PLATINUM METALS REVIEW A quurterly survey of research on the platinum metuls and of dwelopments in their applications in industry ~~ VOL. 14 OCTOBER 1970 NO. 4 Contents Platinum Containers for the Growth of Single Crystal Oxides 118 Platinum Inclusions in Laser Glasses 122 Rhodium Plated Langmuir Probes for Sounding Rockets 123 Platinum and the Refractory Oxides 124 Combined Catalysts for Ammonia Oxidation 130 Absorption of Hydrogen by Palladium Alloys 131 Platinum-Carbon Catalysts with Molecular Sieve Properties 133 Platinum Metal Coatings for Stereoscan Specimens 139 The History of Matthey Bishop 140 Abstracts 147 New Patents 156 Index to Volume 14 159 Communications should be addressed to The Editor, Platinum Metals Review Johnson, Matthey & Co Limited, Hatton Garden, London ECl P 1 AE Platinum Containers for the Growth of Single Crystal Oxides By L. G. Van Uitert Bell Telephone Laboratories Incorporated, Murray Hill, Kew Jersey The growth of single crystal oxides for optical and magnetic purposes is commonly carried out using platinum containers. ilIodijications to container design have been important factors in improving growth conditions. A new composite three-layer crucible has been fabricated in platinum and iridium for growing crystals of sodium barium niobate, and a platinum container which can be drained of jlux has been de- veloped for growing rare earth iron garnets. Single crystals are of basic importance as taker design. A melt (or fused mixture of the integral parts of semiconductor devices, components of a crystal) can conveniently be oscillators, transducers, detectors, delay lines contained in a platinum crucible-susceptor and power limiters. There is also an interest that is heated by radio frequency induction. in nearly perfect optical crystals for coherent In Fig. z a boule of lead molybdate (PbMoO,), light sources (lasers), non- linear optical applications (se- cond harmonic generators and parametric oscillators) and as light beam modulators, de- flectors and phase shifters. Further, there are a number of uses for large, uniform, single crystals of yttrium or rare earth iron garnets having con- trolled magnetic properties. The emphasis placed on size and uniformity has moti- vated a search for ways to improve crystal growth. One important part of this effort has been to modify the con- Fig. 1 The furnace in which single crystal garnets are grown in a platinum crucible. The operator is preparing to drain 08the $ux by puncturing the seal in the container bottom PZutinumMetuZsRev., 1970, 14, (4), 118-121 118 Fig. 2 A single crystal of lead molybdate being pulled from the melt. The platinum crucible susceptor is heated by a radio frequency induction coil, the top turn of which is visible here which is particularly useful for acousto-optic applica- tions, is shown being pulled from a melt contained in a platinum crucible that is 3 inches in diameter and 3 inches high (I). The crucible is embedded in zirconia granules that are contained by a quartz liner that is closely fitted by a multi-turn r.f. coil (only the top turn is evident). Little difficulty is encountered with the been used to grow NaBa,Nb,O,, crystals for crucible in growing PbMoO, (melting point about 50 hours. This crucible has expanded 1065°C). However, when growing sodium to nearly twice its original volume. The third barium niobate (NaBa,Nb,O,,, an important (C) is a new, composite, three-layer crucible. material for non-linear optical applications) It was constructed by close fitting a 0.040 the platinum crucible expands extensively inch wall platinum crucible inside a 0.040 over the several hours required to complete inch wall iridium crucible which in turn was the growth run (2). This shortens the useful close fitted inside a 0.020 inch wall platinum lifetime of the crucible and increases the crucible. The inner and outer platinum difficulty of maintaining uniform crystal crucibles were joined at the top. The growth conditions. The melting point of fourth crucible (D) is such a container after NaBa,Nb,O,, is near 145o"C, about 285°C 20 hours of use. The outer wall expanded due closer than that of PbMoO, to the melting to internal gas pressure and subsequently point of platinum at 1773°C. It is essential burned through. The fifth crucible (E) was to use platinum in contact with the also constructed in the same manner as NaBa,Nb,O,, melt, rather than the higher crucible C. However, several tiny vent melting point noble metals (such as rhodium holes were drilled through the outer platinurn or iridium) to avoid contamination by oxides layer to permit entrapped gas to escape of the latter that colour the crystal. For- during heating. The crucible shown (E) has tunately, the surface stability of platinum can been used to grow NaBa,Nb,O,, crystals for be combined with the rigidity of iridium by more than zoo hours without expanding or using composite crucibles. suffering distortion beyond that experienced Several crucibles are shown in Fig. 3. The using iridium alone as the crucible material. first (A) is a new 1.5 inch diameter x 1.5 inch Crystals that do not grow well from the height x 0.060 inch wall platinum crucible. melt are often best prepared by growth from The second (B) is a similar crucible that has a solvent or flux. The yttrium or rare earth Platinum Metals Rev., 1970, 14, (4) 119 Fig. 3 Platinum and composite platinum-iridium-platinum trilayer crucibles compared. A New platinum crucible B Platinum crucible after 50 hours growing sodium barium niobate crystals C New composite crucible D Composite crucible after 20 hours use E Composite crucible with vent holes to permit escape of entrapped gas during heating. Afier 200 hours use it was distorted no more than one made of iridium Fig. 4 A platinum container used for the jlux growth of large garnet crystals has been designed to permit draining at high temperatures Platinum Metals Rev., 1970, 14, (4) 120 Fig. 5 Garnets grown by the technique which includes draining of thejux are used in microwave devices, delay lines, tunable lasers and bubhle domain devices. Demand for them is increasing steadily iron garnets (e.g. Y,Fe,O,,) are such crucible is mounted on a hollow pedestal in a materials. These crystals are grown by vertical muffle resistance furnace during slowly exsolving the crystal components from crystal growth. The operator shown in Fig. I a PbO.PbF,*B,O, flux by cooling at about is preparing to drain the flu by puncturing 15°C per day from 1300OC to 950°C (3). the seal in the bottom of the container. The Below the lower temperature the garnets flux drains quietly into the catch tray. After tend to redissolve and therefore they should the flux is drained the furnace is shut down be separated from the flux. However, large and allowed to cool to room temperature. crystals will crack if they are subjected to Garnets that have been grown under these thermal shock. This can be avoided by re- conditions are shown in Fig. 5. The crystals moving the flux at 95OUcwhile the crystals have found use in microwave devices, delay remain in the furnace. lines, tunable lasers and bubble domain A platinum container that has been de- devices. signed to permit draining at high tempera- References tures is shown in Fig. 4. The 8 inch diameter I D. A. Pinnow, L. G. Van Uitert, A. W. x8 inch height xo.060 inch wall container Warner and W. A. Bonner, Appl. Phys. Letterx, 1969,15, 83-86 weighs about pounds. The hole in the 15 2 L. G. Van Uitert, J. J. Rubin and W. A. centre leads into a 4 inch long stand-off that can Bonner, IEEE Trans., 1968, QE-4, 622-627 be fitted with a welded-in insert. The insert is 3 W. H. Grodkiewicz, E. F. Dearbom and L. G. Van Uitert, 3. Phyr. Chem. Solids, 1967, punctured to drain off the flux. The covered 441-444 Platinum Metals Rev., 1970, 14, (4) 121 Platinum Inclusions in Laser Glasses THEIR ORIGIN AND PREVENTION For some years it has been known that a platinum crucibles, platinum heating elements few particles of platinum may be found in all or thermocouples, and are conveyed as vapour optical glasses which have been melted in to the molten glass. The evidence for this is systems containing platinum. These have that platinum particles were not found in never been observed to affect the performance glasses which had been melted in platinum of even the most critical of lenses but in 1963 in an atmosphere of pure nitrogen, even after it was discovered at the American Optical they had been kept molten for 90 hours at Corporation that in laser rods operated at high 2,45O0C. Moreover, in an experiment in peak powers they may absorb so much which a stream of oxygen was passed through energy as to cause explosive fracture. a horizontal tube furnace over a sheet of The particles, as described by Richard F. platinum and then over a ceramic crucible Woodcock in a report (I) of investigations in containing molten glass, both side by side, the Central Research Laboratory of the particles of platinum were found in the glass. American Optical Corporation at South- The investigators, however, were not able to bridge, Massachusetts, are generally lacy and establish the mechanism by which the lacy irregular in shape with rounded globular particles of metallic platinum were formed in contours. They may be so small as only just the molten glass from the gaseous oxide in the to be resolved by the optical microscope- atmosphere above. On the other hand, they about 2 pm across-and exceptionally they showed that satisfactory laser glass, free from may be as large as 500 pm.
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