Method for flux growth of KTiOPO.sub.4 and its analogues
AssigneeE. I. Du Pont de Nemours and Company
InventorThurman E. Gier
Life of this patent
Estimating the term…
Abstract
A process for the manufacture of single crystals of MTiOXO.sub.4, wherein M is K, Rb or Tl and X is P or As, of optical quality and of sufficient size for use in nonlinear optical devices. In the process, starting ingredients chosen to be within the region of the ternary phase diagram in which the desired crystal MTiOXO.sub.4 product is the only stable solid phase, are heated to produce MTiOXO.sub.4 and then controllably cooled to crystallize the desired product. In a preferred method the ingredients are placed in a temperature gradient in which the hot zone ranges from about 800.degree.-1000.degree. C. and the cold zone about 10.degree.-135.degree. C. cooler, maintaining the temperature gradient for about 3 days to about 3 weeks, cooling, and recovering MTiOXO.sub.4 crystals.
Claims9
In an improved process for producing a single crystal of MTiOXO.sub.4 by combining and heating starting materials comprising MTiOXO.sub.4 and a nonaqueous flux M/X/O, or their precursors, where M is selected from the group consisting of K, Rb and Tl and X is selected from the group consisting of P and As, said process being carried out either by (a) heating the combined starting materials, in such amounts that the ratio of MTiOXO.sub.4 to flux at the highest heating temperature is greater than the saturation value, in a temperature gradient wherein the hot zone is within the range about 800.degree. C. to about 1000.degree. C. and the cold zone is within the range about 10.degree. C. to about 135.degree. C. cooler than the hot zone so as to produce a nonaqueous melt;
- maintaining the temperature gradient for about 3 days to about 3 weeks to allow crystal growth;
- and cooling and recovering crystalline MTiOXO.sub.4, or (b) uniformly heating the combined starting materials, in such amounts that the ratio of MTiOXO.sub.4 to flux at the highest heating temperature is less than the saturation value, to a temperature within the range about 700.degree. C. to about 1100.degree. C. until a clear nonaqueous solution is produced;
- slowly cooling the solution at a rate no greater than 5.degree. C. per hour to effect crystallization of MTiOXO.sub.4 ;
- and recovering crystalline MTiOXO.sub.4, the improvement characterized in that the composition of the combined starting materials is within the trigonal regions ABC, DEF, GHI, JKL, MNO, PQR or STU of FIGS. 1 to 7, respectively, wherein the Pna2.sub.1 -type MTiOXO.sub.4 is the only stable solid phase in equilibrium with the molten flux.
Dependencies are inferred from the claim text.