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Method and apparatus for processing metals, and the metals so produced

A metal and equipment technology, applied in chemical instruments and methods, metal material coating technology, ion exchange column/bed method, etc., can solve problems such as semiconductor component failure

Inactive Publication Date: 2003-10-15
HONEYWELL INT INC
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

Finally, the presence of radioactive elements such as U and Th in cobalt is undesirable because they emit alpha-rays, which can lead to failure of semiconductor components

Method used

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  • Method and apparatus for processing metals, and the metals so produced
  • Method and apparatus for processing metals, and the metals so produced
  • Method and apparatus for processing metals, and the metals so produced

Examples

Experimental program
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Effect test

example 1

[0054] Electrolytic formation of cobalt

[0055] CoSO 4 ·7H 2A 1472 lb sample of O was dissolved in 370 gallons of water while stirring. While stirring again, the pH of the cobalt sulfate solution was adjusted to 2 by adding 2.44 gallons of 98% sulfuric acid, ACS grade. The solution was added to a separate electrolytic cell and heated to 122°F. Circulation was initiated to an ion exchange tank containing 5 cubic feet of resin with a flow rate of 0.5 GPM through the tank. The cobalt sulfate solution was analyzed and found to contain 80-90 g / L Co, 3-4 mg / L Fe, 1-2 mg / L Ni, and a pH of 2. The electrolysis was performed at a constant current of 300 A, and a voltage drop from 9 V to 5 V was observed after 216 hours of operation. Cathode is 99.95% Co plate at 18A / ft 2 work at current densities. Approximately 116 lbs of cobalt were obtained, which corresponds to a cathode current efficiency of 74%. The analysis results of the deposited layer are shown in Table 1 as "High Puri...

Embodiment 2

[0058] CoCl 2 system

[0059] Cobalt powder with a purity of 3N8 (99.98%), powder A, and 2N7 (99.7%), powder B were dissolved in HCl (35-38% by weight in water). The solution was then heated to about 80°C with stirring for about 10 hours. Add 2 L of deionized water to dissolve the solid CoCl 2 ·6H 2 O was dissolved and stirred at about 50°C for about 8 hours. More deionized water was then added to obtain a final solution volume of about 5 liters.

[0060] A plastic tube with an inner diameter of 0.953 cm and a length of 120 cm was connected to one end of the pressure reducer and used as an ion exchange column. Glass wool is used as the screen material. The tube was filled with approximately 42.6 ml of Dowex M-4195 anion exchange resin having an average size of 20-50 mesh. Prior to loading, it was conditioned by passing 2 bed volumes (BV) of HCl solution through the resin at a flow rate of approximately 15 BV / Hr. The pH of the HCl solution is the same as the pH of the d...

Embodiment 3

[0070] Fe removal

[0071] Fe is the main impurity element in cobalt. Like Ni, it affects the breakthrough flux of the cobalt sputtering target and is therefore preferably minimized. Although the resin employed in the present invention has the ability to absorb a certain amount of Fe, an additional Fe removal step is required when the Fe content in the raw cobalt is high. Fe can be removed in different ways: 1) Fe(OH) 3 precipitation; 2) solvent extraction; 3) additional selective ion exchange; and so on. In particular instances, this method has successfully converted Fe(OH) 3 The precipitation of Fe is incorporated in the cobalt refining process to deal with excess Fe impurities.

[0072] For Fe(OH) 3 For precipitation, blow air or oxygen into the impure CoSO during stirring 4 or CoCl 2 solution for a certain period of time, so that the Fe 2+ Ions are oxidized to Fe 3+ ion. Then add NaOH to CoSO 4 or CoCl 2 solution to change its pH to about 4. Due to Fe(OH) 3 L...

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Abstract

The invention encompasses a method and apparatus for producing high-purita metals (such as, for example, high-purity cobalt), and also encompasses the high-purity metals so produced. The method an comprise a combination of electrolysis and ion exchange followed by melting to produce cobalt of a desired purity. The method can result in the production of high-purity cobalt comprising total metallic impurities of less than 50 ppm. Individual elemental impurities of the produced cobalt can be follows: Na and K less than 0.5 ppm each, Fe less than 10 ppm, Ni less than 5 ppm, Cr less than 1 ppm, Ti less than 3 ppm and O less than 450 ppm.

Description

field of invention [0001] The invention described herein relates to methods and apparatus for producing metals, and to metals produced thereby. In a particular aspect, the process of the invention is used to produce cobalt, including CoCl 2 and / or CoSO 4 Dissolution and purification of the solution, followed by further refining and deposition by electrolysis. Vacuum smelting can be performed after electrolysis to further produce refined cobalt. The cobalt produced is preferably "high purity" cobalt, excluding gaseous impurities, which is defined according to this invention as having a total metal purity of 99.99% (4N) or greater. The resulting high-purity cobalt is suitable for use in sputtering targets and related microelectronics applications. The cobalt material can also be a lower purity cobalt, for example, a cobalt material that is about 99.9% cobalt. Background of the invention [0002] High purity metals are required for many modern processes, eg, as solders, sp...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): B01J47/02B01J47/12C22B23/06C23C14/14C23C14/34C25C1/00C25C1/08C25C7/00C25C7/06
CPCC25C1/08C22B23/06C25C1/00
Inventor G·王D·M·海多克J·勒曼
Owner HONEYWELL INT INC
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