System and Method for Monolithic Crystal Growth

Abstract

A monolithic crystal having the atomic formula W n X m Y p Z r , with at least one dimension greater than about 10 mm. A method for top seed, solution growth of a monolithic crystal, wherein the method includes the steps of: preparing a precursor, forming a seed crystal, and forming the monolithic crystal. Some configurations of the method include the differential control of the crystal flux temperature in a furnace and the rotational frequency of a seed crystal in the crystal flux.

1 . A monolithic crystal comprising the atomic formula W n X m Y p Z r , and having at least one dimension greater than 10 mm. 
     
     
         2 . The composition of  claim 1  wherein W comprises at least one element chose from the group consisting of Li, Na, K, Rb, Cs, Mg, Ca, Sr, and Ba. 
     
     
         3 . The composition of  claim 1  wherein X comprises at least one element chosen from the group consisting of Fe, Ti, V, Cr, Mn, Co, Ni, Cu, Zn, Zr, Nb, Mo, Pd, Ag, Cd, Hf, Ta, W, Pt, Au, and Hg. 
     
     
         4 . The composition of  claim 1  wherein Y comprises at least one element chosen from the group consisting of P, Al, Si, S, Ga, Ge, As, Se, In, Sn, Sb, Te, I, Tl, Pb, or Bi. 
     
     
         5 . The composition of  claim 1  wherein Z comprises at least one element chosen from the group consisting of O, F, Cl, or Br 
     
     
         6 . The composition of  claim 1 , wherein n, m, p, and r comprise an integer or zero. 
     
     
         7 . The composition of  claim 6 , wherein r comprises a multiple of 7. 
     
     
         8 . A method of producing a monolithic crystal comprising:
 fanning a crystal flux;   forming a seed crystal; and   forming a monolithic crystal by inserting the seed crystal into the crystal flux in a temperature controlled furnace.   
     
     
         9 . The method of  claim 8 , wherein forming a crystal flux further comprises:
 preparing a mixture of solid precursors; and   heating the precursors.   
     
     
         10 . The method of  claim 9 , further comprising:
 mechanically reducing the solid precursors; and   analyzing the purity of the solid precursors.   
     
     
         11 . The method of  claim 9 , wherein heating the precursors comprises controlling the temperature with respect to a critical temperature of the precursors to maintain a liquid crystal flux. 
     
     
         12 . The method of  claim 11 , further comprising mixing the precursors with other materials in a stoichiometric ratio. 
     
     
         13 . The method of  claim 8 , wherein forming a seed crystal comprises:
 cooling the temperature of the crystal flux;   seeding initial crystals;   collecting the initial crystals; and   faulting primary seed crystals.   
     
     
         14 . The method of  claim 13 , wherein cooling the temperature of the crystal flux further comprises controlling the temperature with respect to a critical temperature of the crystal flux. 
     
     
         15 . The method of  claim 13 , wherein seeding and collecting the initial crystals comprises
 inserting a seed material into the crystal flux;   controlling the temperature of the crystal flux in order to permit the formation of initial crystals; and   withdrawing the seed material from the crystal flux,
 wherein the seed material comprises a Group VIII transition metal wire. 
   
     
     
         16 . The method of  claim 13 , wherein forming primary seed crystals further comprises
 physically altering the initial crystal;   re-seeding the initial crystal into the crystal flux under controlled temperatures;   growing the initial crystal until at least one dimension is at least 5 mm;   withdrawing the initial crystal; and   physically altering the initial crystal to have at least one predetermined property chosen from the group consisting of faces, edges, crystal planes, and size.   
     
     
         17 . The method of  claim 8 , wherein forming the monolithic crystal further comprises:
 seeding the initial crystal into a temperature controlled crystal flux;   rotating the initial crystal in the crystal flux to faun a primary crystal;   collecting the primary crystal from the crystal flux; and   processing the primary crystal to form a monolithic crystal.   
     
     
         18 . The method of  claim 17 , wherein seeding the initial crystal further comprises coupling the initial crystal to a seed material. 
     
     
         19 . The method of  claim 17 , wherein rotating the initial crystal comprises controlling the rotational frequency of the initial crystal in the crystal flux to control the shape of the primary crystal. 
     
     
         20 . The method of  claim 8 , wherein controlling the temperature of the furnace further comprises controlling the temperature around the melting temperature of the crystal or the saturation temperature of the crystal. 
     
     
         21 . A method for producing metallic monolithic crystal comprising:
 preparing a liquid crystal flux comprising an inorganic salt of a metal;   forming seed crystals in the liquid crystal flux;   altering the seed crystals to comprise predetermined properties;   inserting and rotating the seed crystals in the liquid crystal flux to control morphology of crystal formation thereon; and   controlling the temperature of the liquid crystal flux to form a monolithic crystal having at least one dimension greater than 10 mm.   
     
     
         22 . The method of  claim 21 , wherein the metal comprises at least one chosen from the group consisting of Li, Na, K, Rb, Cs, Mg, Ca, Sr, and Ba. 
     
     
         23 . The method of  claim 21 , wherein forming seed crystals and inserting the seed crystals in the liquid crystal flux comprises a top-seeded solution growth in a furnace. 
     
     
         24 . The method of  claim 21 , wherein altering the seed crystals to comprise predetermined properties further comprises cutting the seed crystals to form predetemined faces, edges, and crystal planes of the desired monolithic crystal. 
     
     
         25 . The method of  claim 21  wherein the monolithic crystal comprises LiFeP 2 O 7  or K 3 V 5 O 14 .