Apparatus for maintaining peroxide concentration

• US 4,477,329 A
• Filed: 08/20/1982
• Issued: 10/16/1984
• Est. Priority Date: 02/05/1982
• Status: Expired due to Fees

• Current Assignee: Lockheed Martin Corporation (Martin Marietta Corporation)
• Original Assignee: Lockheed Martin Corporation (Martin Marietta Corporation)
• Inventors: Weber, Kenneth E., Rogers, Alisa K.
• Primary Examiner(s): Tung, T.
• Application Number:
  US06/410,183
• Time in Patent Office: 788 Days
• Field of Search: 204/1 T, 204/195 R, 204/195 P, 204/195 B, 148/6.14 R, 423/272, 423/273
• US Class Current: 137/93
• CPC Class Codes: C23C 22/64 Treatment of refractory metals or alloys based thereon
• CPC Class Codes: C23C 22/77 Controlling or regulating of the coating process
• CPC Class Codes: G01N 27/4166 measuring a particular property of an electrolyte
• CPC Class Codes: Y10T 137/2509 By optical or chemical property

Abstract

A modified alkaline peroxide pre-bond process for the surface treatment of titanium is useful as a practical production process. In this modified process, an exceptionally wide range of allowable peroxide concentration, namely, from 0.001 molar to 0.2 molar (and preferably 0.001 molar to 0.01 molar) may be tolerated and a novel real-time peroxide monitoring and control technique is employed. The process is further improved by means of the use of stabilizers such as precipitated magnesium silicate which greatly increases bath life-time and reduces the overall operating cost of the process. Solution operating conditions have been defined which permit titanium adherends to be processed satisfactorily over a wide range of hydrogen peroxide concentration. In particular, the acceptable temperature range is 125° F.-165° F. (51.7° C.-73.8° C.); the treatment period is 15 to 25 minutes and the hydroxide concentration is 0.3 to 0.9 molar. The preferred values are approximately 145° F. (62.7° C.); 20 minutes, and 0.5 molar, respectively. An electrochemical method has been established utilizing a magnesium electrode (114) which provides a stable potential characteristic that is dependent only on the concentration of the peroxide. The resultant capability to reliably monitor the peroxide concentration in real time in turn permits an automated feed system to be effectively utilized for sustaining the peroxide concentration within the desired limits.

Claims

1. An automated system for maintaining the concentration of hydrogen peroxide within an alkaline peroxide treatment solution at a value in excess of a predetermined lower limit, said system comprising:

a treatment tank;

a treatment solution contained within said treatment tank;

means for agitating said solution within said treatment tank so as to ensure that said solution is relatively homogeneous both with respect to chemical composition and with respect to physical properties;

a first electrode;

a second electrode consisting essentially of pure magnesium metal, said first and second electrodes both being at least partially immersed into said treatment solution within said treatment tank;

a reservoir containing concentrated hydrogen peroxide solution;

a remotely controllable valve operatively interposed between said reservoir and said treatment tank so as to control the flow of said concentrated hydrogen peroxide solution from said reservoir to said tank; and

circuit means for monitoring the voltage across said first and second electrodes and for generating a control pulse to open said valve as said voltage decreases to a predetermined lower threshold voltage.

2. The automated system of claim 1, wherein said first electrode is a saturated calomel electrode.

3. The automated system of claim 1, wherein said lower threshold voltage corresponds to a hydrogen peroxide concentration of less than approximately 0.002 molar.