Method for producing high-purity calcium

Patent metadata

Field	Value
Publication number	US-9499877-B2
Application number	US-201214353780-A
Country	US
Kind code	B2
Filing date	Nov 13, 2012
Priority date	Dec 7, 2011
Publication date	Nov 22, 2016
Grant date	Nov 22, 2016

Abstract

The present invention provides a method for producing high-purity calcium, the method being characterized by the following: performing first sublimation purification by introducing calcium starting material having a purity, excluding the gas components, of 4N or less into a crucible of a sublimation vessel, subjecting the starting material to sublimation by heating at 750° C. to 800° C., and causing the product to deposit (evaporate) onto the inside walls of the sublimation vessel; and then, once the calcium that has been subjected to first sublimation purification is recovered, performing second sublimation purification by introducing the recovered calcium again to the crucible to the sublimation vessel, heating the recovered calcium at 750° C. to 800° C., and causing the product to similarly deposit (evaporate) on the inside walls of the sublimation vessel thereby recovering calcium having a purity of 4N5 or higher It is an object of the present invention to provide a technology with which calcium that has been brought to a high-purity can be obtained with stability to be used for the production of high-purity lanthanum, as well as to be used as a reducing agent for other rare earth elements, a desulfurizing or deoxidizing agent for metals, or a getter for high-vacuum pumps.

First claim

The invention claimed is:

1. A method of producing high-purity calcium comprising:
charging calcium starting material having a purity, excluding the gas components, of 4N or less into a crucible of a sublimation vessel;
performing first sublimation purification by heating at 750° C. to 800° C. so that calcium is sublimated and deposits (evaporates) onto the inner side wall of the sublimation vessel;
recovering the calcium purified by the first sublimation purification;
charging the calcium into a crucible of a sublimation vessel again;
performing second sublimation purification by heating at 750° C. to 800° C. so that the calcium is sublimated and deposits (evaporates) onto the inner side wall of the sublimation vessel; and
recovering the calcium having a purity of 4N5 or higher.

2. The method of producing high-purity calcium according to claim 1 , wherein calcium is sublimated at a sublimation rate of 0.25 to 0.75 g/cm 2 /h.

3. The method of producing high-purity calcium according to claim 2 , wherein the sublimation vessel is kept at a vacuum of an air pressure being equal to or less than 1×10 −4 Pa during the sublimation purification.

4. The method of producing high-purity calcium according to claim 3 , wherein the yield of the calcium starting material is 80% or more.

5. The method of producing high-purity calcium according to claim 4 , wherein the recovered high-purity calcium contains less than 5 ppm of each transition metal element.

6. The method of producing high-purity calcium according claim 4 , wherein the recovered high-purity calcium contains less than 1 ppm of each transition metal element.

7. The method of producing high-purity calcium according to claim 1 , wherein the sublimation vessel is kept at a vacuum of an air pressure being equal to or less than 1×10 −4 Pa during the sublimation purification.

8. The method of producing high-purity calcium according to claim 1 , wherein yield of the calcium starting material is 80% or more.

9. The method of producing high-purity calcium according to claim 1 , wherein the recovered high-purity calcium contains less than 5 ppm of each transition metal element.

10. The method of producing high-purity calcium according claim 1 , wherein the recovered high-purity calcium contains less than 1 ppm of each transition metal element.

Assignees

• Jx Nippon Mining & Metals Corp

Inventors

• Takahata Masahiro

Classifications

• C22B9/04

  Refining by applying a vacuum · CPC title

• C22C24/00

  Alloys based on an alkali or an alkaline earth metal · CPC title

• C22B9/02 Primary

  Refining by liquating, filtering, centrifuging, distilling, or supersonic wave action {including acoustic waves; (C22B9/003, C22B9/006, C22B9/05, C22B9/22 take precedence)} · CPC title

• C22B26/20 Primary

  Obtaining alkaline earth metals or magnesium · CPC title

• B22F9/04

  starting from solid material, e.g. by crushing, grinding or milling ({C22C1/1084 takes precedence}; crushing, grinding or milling, in general, see the relevant subclasses, e.g. B02C) · CPC title