# US 5,705,048 A · Apparatus and a process for regenerating a CUCl.sub.2 etchant

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- Number: US 5,705,048 A
- Document ID: US5705048A
- Status: Granted
- Kind: A
- Application number: 08/624,825
- Filed: 1996-03-27
- Granted: 1998-01-06
- Earliest claimed: 1996-03-27
- Assignees: Oxley Research, Inc.
- Inventors: James E. Oxley; Raymond J. Smialek; Ronald A. Putt
- Web page: https://patentgrep.com/patent/US5705048A

## CPC

- C23F 1/46: Regeneration of etching compositions
- C23F: NON-MECHANICAL REMOVAL OF METALLIC MATERIAL FROM SURFACE (working metal by laser beams B23K26/00; desurfacing by applying flames B23K7/00; working of metal by electro-erosion B23H; producing decorative effects by removing surface material, e.g. by engraving, by etching, B44C1/22; electrolytic etching or polishing C25F); INHIBITING CORROSION OF METALLIC MATERIAL OR INCRUSTATION IN GENERAL; MULTI-STEP PROCESSES FOR SURFACE TREATMENT OF METALLIC MATERIAL INVOLVING AT LEAST ONE PROCESS PROVIDED FOR IN CLASS C23 AND AT LEAST ONE PROCESS COVERED BY SUBCLASS C21D OR C22F OR CLASS C25

## Abstract

The present invention relates to an apparatus and a process for regenerating a used etchant solution, which solution contains a metal in divalent form. The apparatus includes a tank which is originally supplied with the etchant solution; a first electrolytic cell for converting solution from the tank to a solution containing a high fraction of a monovalent form of the metal; and a second electrolytic tank for plating metal from the solution containing a high fraction of the monovalent form of the metal. The details of the process of the present invention are set forth in the disclosure.

## Claims

### Claim 1

An apparatus for regenerating a used etchant solution in a sump, said used etchant solution containing a metal in divalent form, said apparatus comprising:
means for supplying said used etchant solution to a control tank;
first electrolytic means connected to said control tank for receiving solution containing said metal in said divalent form from said control tank and for converting said solution with said divalent form of said metal into a solution containing a high fraction of a monovalent form of said metal;
means for returning said solution containing a high fraction of said monovalent form of said metal to said control tank;
means for returning overflow of solution from said control tank to said sump; and
second electrolytic means communicating with said control tank for receiving said solution containing a high fraction of said monovalent form of said metal and for converting said monovalent form of said metal to said metal.

### Claim 2 (depends on 1)

The apparatus of claim 1 further comprising means for feeding said used etchant solution to said first and second electrolytic means as an anolyte.

### Claim 3 (depends on 1)

The apparatus of claim 1 wherein said metal in said divalent form comprises cupric copper and said first electrolytic means converts cupric copper to cuprous copper and said second electrolytic means converts cuprous copper to copper metal.

### Claim 4 (depends on 1)

The apparatus of claim 1 wherein:
said first electrolytic means comprises an electrochemical cell having an anode chamber and a cathode chamber;
said anode chamber has a flow through anode therein; and
said cathode chamber has a flow through cathode therein.

### Claim 5 (depends on 4)

The apparatus of claim 4 wherein said flow through anode and said flow through cathode are each formed by a flow-through electrode formed from graphite or carbon felt.

### Claim 6 (depends on 5)

The apparatus of claim 5 wherein said etchant solution is supplied to said anode chamber and said solution containing a high fraction of the monovalent form of said metal is supplied to said cathode chamber.

### Claim 7 (depends on 1)

The apparatus of claim 1 wherein:
said second electrolytic means comprises a plating cell having a cathode chamber and an anode chamber;
said cathode chamber having a flow-by cathode; and
said anode chamber having a flow through anode.

### Claim 8 (depends on 7)

The apparatus of claim 7 wherein said flow-by cathode comprises a flow-through graphite or carbon felt anode and said cathode comprises a flow-by graphite plate cathode.

### Claim 9

A process for regenerating a solution of used etchant in a sump, said used etchant solution containing a concentration of a metal in divalent form, said process comprising the steps of:
supplying a quantity of said etchant solution containing said metal in divalent form to a control tank;
forcing an overflow of solution from said control tank to said sump;
supplying solution from said control tank to a first electrolytic cell;
electrolytically converting said solution with said divalent form of said metal in said first electrolytic cell to a solution containing a high fraction of a monovalent form of said metal;
returning said solution containing a high fraction of said monovalent form of said metal to said control tank;
supplying said solution containing a high fraction of said monovalent form of said metal from said control tank to a second electrolytic cell; and
electrolytically converting said monovalent form of said metal in said solution to said metal in said second electrolytic cell.

### Claim 10 (depends on 9)

The process of claim 9 further comprising feeding said used etchant solution as an anolyte to said first and second electrolytic cells.

### Claim 11 (depends on 9)

The process of claim 9 wherein:
said metal in said divalent form in said etchant comprises cupric copper;
said first electrolytic converting step comprises converting said cupric copper to cuprous copper in said first electrolytic cell; and
said second electrolytic converting step comprises converting said cuprous copper to copper in said second electrolytic cell.

### Claim 12 (depends on 11)

The process of claim 11 further comprising maintaining a solution in said tank having a concentration of said cupric copper in the range of from about 0.3 g/l to about 2.5 g/l.
