Method for fabricating apatite crystals and ceramics
AssigneeLawrence Livermore National Security, LLC
InventorsThomas F. Soules, Kathleen I. Schaffers, John B. Tassano, Jr., Joel P. Hollingsworth
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Abstract
The present invention provides a method of crystallizing Yb:C-FAP [Yb3+:Ca5(PO4)3F], by dissolving the Yb:C-FAP in an acidic solution, following by neutralizing the solution. The present invention also provides a method of forming crystalline Yb:C-FAP by dissolving the component ingredients in an acidic solution, followed by forming a supersaturated solution.
Claims17
A method of preparing a crystalline form of a compound of formula I:
- (A1−nYn)5(PO4)3X (I)
- wherein
- A is selected from the group consisting of Ca, Sr and Ba,
- Y is a dopant selected from the group consisting of Yb, Nd, Ce, Cr, Tm, Ho, Er, and Sm,
- subscript n is from 0 to about 0.1, and
- X is selected from the group consisting of F, Cl and OH,
- the method comprising:
- dissolving the compound of formula I in an aqueous solution comprising an acid, wherein the solution is at a temperature of from about 0 to about 100° C.;
- and
- forming a supersaturated solution of the compound of formula I, thereby preparing the crystalline form of the compound of formula I.
A crystalline form of a compound of formula Ib:
- (Ca1−nYbn)5(PO4)3F (Ib)
- wherein subscript n is about 0.01, and
- wherein the X-ray crystal structure of the compound has the following 2-theta peaks:
- 25.978, 31.780, 32.319, 32.779, 34.082 and 49.520,
- the compound prepared by the process comprising:
- dissolving Ca5(PO4)3F in an aqueous solution comprising concentrated hydrochloric acid and ytterbium, wherein the solution is at a temperature of from about 0 to about 100° C.;
- and
- adding concentrated ammonium hydroxide to the solution to neutralize the solution, thereby preparing the crystalline form of (Ca1−n Ybn)5(PO4)3F, where subscript n is about 0.01, thereby preparing the crystalline form of the compound of formula Ib.
A method of preparing a crystalline form of a compound of formula I:
- (A1−nYn)5(PO4)3X (I)
- wherein
- A is selected from the group consisting of Ca, Sr and Ba,
- Y is a dopant selected from the group consisting of Yb, Nd, Ce, Cr, Tm, Ho, Er, and Sm,
- subscript n is from about 0.001 to about 0.1, and
- X is selected from the group consisting of F, Cl and OH,
- the method comprising:
- dissolving an alkaline earth fluoride, an alkaline earth phosphate, an alkaline earth carbonate and a salt of the dopant Y in an aqueous solution comprising an acid, wherein the solution is at a temperature of from about 0 to about 100° C.;
- and
- forming a supersaturated solution of the compound of formula I, thereby preparing a crystalline form of the compound of formula I.
Dependencies are inferred from the claim text.