Patent US3767476A successfully refreshed from Google Patents.
US3767476A
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Method and composition for phosphatizing steel under pressure
Assignee: United States Department of the Army
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Filing: 1971-08-31
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Granted: 1973-10-23
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Expires: 1991-08-31
Abstract
Abstract The heat and corrosion resistance of manganese phosphate coatings on ferrous surfaces can be greatly improved by modifying a conventional phosphatizing solution to reduce the ferrous ion content thereof, adding a given quantity thereto of the manganese salt obtained from an acid selected from the group consisting of citric, tartaric, gluconic, and saccharic acids and then carrying out the coating process in a closed chamber under a steam pressure in excess of one pound per square inch.
Inventors
- 👤 L Wagner
- 👤 P Chamberlain
Bibliographic Details
Application Number
—
Jurisdiction
US
Data Source
google_patents
Last Synchronized
2026-10-30 10:42
CPC Classifications
C; C23; C23C; C23C22/00; C23C22/73; C23C22/05; C23C22/06; C23C22/07; C23C22/08; C23C22/18
Claims Analysis
Total Claims: 8
Claim 1
Independent Claim
199 words
A method for treating ferrous surfaces to form a manganese phosphate coating thereon characterized by the ability to withstand, subsequent to being heated to a temperature as high as 450*F, the corrosive effect of a 5% salt spray test for more than 750 hours, said method comprising the steps of, formulating a manganese phosphatizing bath wherein the ratio of total acid to free acid is between 5 to 1 and 15 to 1 and the pH ratio is in excess of 2.0, adding from 0.1 to 2.0 percent by weight of the salt obtained by reacting manganese with an organic acid selected from the carboxylic group containing 4 to 6 carbon atoms with the particular carbon atom adjacent to at least one of the carboxyl groups being replaced by a hydroxyl group, the amount of said added manganese salt being selected to maintain said acid ratio and said pH without causing the total manganese content of said bath to exceed 5.0 percent, confining said bath and the ferrous surfaces to be coated within a sealed container, and heating the interior of said container to provide a steam pressure of between 1 and 22 psig for at least 15 minutes.
Claim 2
Independent Claim
119 words
A method for treating ferrous surfaces to form a manganese phosphate coating thereon adapted to resist the corrosive effect of a standard 5% salt spray test comprising the steps of, formulating an aqueous manganese phosphatizing bath to include between 0.01 and 1.0 percent of ferrous iron, enriching the bath with from 0.1 to 2.0 percent by weight of the manganese salt of a carboxylic acid selected from the group consisting of citric, tartaric, gluconic, and saccharic acids, confining the bath and the ferrous surfaces to be coated thereby within an autoclave, and subjecting the contents to steam pressure in excess of one psig for at least 15 minutes during the formation of the phosphate coating on the ferrous surfaces.
Claim 3
Dependent Claim
128 words
An aqueous bath for coating ferrous parts with a low porosity, non-reflective metal phosphate surface, said bath consisting essentially of, a mixture of manganese and ferrous dihydrogen Phosphates providing from 0.1 to 3.0 percent by weight of manganese and from 0.01 to 1.0 percent by weight of ferrous iron, sufficient phosphoric acid to provide a total acid to free acid ratio of between 5 to 1 and 15 to 1 and a pH between 2.1 and 3.1, and a manganese salt formed from a carboxylic acid selected from the group consisting of citric, tartaric, gluconic, and saccharic acids, said salt being added to the bath in a percentage by weight which will maintain the existing acid ratio and pH without increasing the total manganese content above 5.0 percent.
Claim 4
Dependent Claim
13 words
The phosphatizing bath defined in claim 4 wherein said salt is manganese citrate.
Claim 5
Dependent Claim
13 words
The phosphatizing bath defined in claim 4 wherein said salt is manganese tartrate.
Claim 6
Dependent Claim
13 words
The phosphatizing bath defined in claim 4 wherein said salt is manganese gluconate.
Claim 7
Dependent Claim
113 words
In an aqueous manganese base phosphatizing bath for coating ferrous parts with a low porosity, non-reflective metal phosphate surface, a mixture of manganese and ferrous dihydrogen phosphates providing from 0.1 to 3.0 percent by weight of manganese and from 0.01 to 1.0 percent by weight of ferrous iron, from 10 to 14 grams per liter of manganese citrate such that the total manganese content of the bath does not exceed 5.0 percent by weight, and sufficient phosphoric acid to provide from 0.2 to 4.0 percent of phosphate while maintaining a total acid to free acid ratio of between 5 to 1 and 15 to 1 and a pH of between 2.1 and 3.1.
Claim 8
Dependent Claim
25 words
The phosphatizing bath defined in claim 8 including sufficient manganese carbonate to adjust the total acid to free acid ratio to about 7.5 to 1.
References Cited (Backward Citations)
USPTO Annuity & Maintenance Windows
| Annuity Stage | Window Opens | Payment Deadline | Surcharge Period Until | Estimated Fee | Status |
|---|---|---|---|---|---|
| 3.5 Years (Year 4) | 1976-10-22 | 1977-04-23 | 1977-10-23 | $2000.00 | Window Closed / Lapsed |
| 7.5 Years (Year 8) | 1980-10-22 | 1981-04-23 | 1981-10-23 | $3760.00 | Window Closed / Lapsed |
| 11.5 Years (Year 12) | 1984-10-22 | 1985-04-23 | 1985-10-23 | $7700.00 | Window Closed / Lapsed |