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US4108690A
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Method for producing an amorphous, light weight calcium phosphate coating on ferrous metal surfaces
Assignee: Henkel Corp
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Filing: 1977-01-31
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Granted: 1978-08-22
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Expires: 1997-01-31
Abstract
Abstract A method is disclosed for producing a non-crystalline, light weight tightly adherent coating of calcium phosphate on ferrous metal surfaces. In this method, the ferrous metal surface is treated with a coating solution containing calcium phosphate together with an oxidizing agent at a pH which closely approaches but does not exceed the saturation point of the calcium phosphate in solution. In practicing the method of this invention, the calcium phosphate content of the coating bath is preselected from the range of from about 0.01 to about 1.0 moles per liter as measured by the Ca ++ cation. Next, a bath temperature of from about 50° F. to about 160° F. is selected. The pH of the bath is raised to a pH approaching but not exceeding the saturation point of calcium phosphate at the selected temperature and the bath is brought to the selected temperature. Coating of the ferrous metal with the calcium phosphate solution is accomplished by conventional dip or spray methods. The resultant coating, though amorphous and with very low coating weight, provides the same superior bonding characteristics associated with heavier and crystalline prior art phosphate coating materials.
Inventors
- 👤 Ferdinand P. Heller
Bibliographic Details
Application Number
—
Jurisdiction
US
Data Source
google_patents
Last Synchronized
2026-10-25 23:40
CPC Classifications
C; C23; C23C; C23C22/00; C23C22/05; C23C22/06; C23C22/07; C23C22/08; C23C22/22
Claims Analysis
Total Claims: 16
Claim 1
Independent Claim
122 words
A method of producing an amorphous, light weight, tightly adherent calcium phosphate coating on a ferrous metal surface comprising applying, at a temperature of from about 50° F to about 160° F., to a metal surface a coating from an aqueous coating solution consisting of an aqueous solution of calcium phosphate and an oxidizing agent, in which the calcium phosphate is present in an amount of from about 0.01 to about 1.0 moles per liter as measured by the Ca++ cation and in which the pH of the solution is between about 3.0 and about 4.2 and said pH is as close as possible to, but does not exceed, the saturation pH of the calcium phosphate at said concentration and said temperature.
Claim 2
Independent Claim
122 words
A method of producing an amorphous, light weight, tightly adherent calcium phosphate coating on a ferrous metal surface comprising applying, at a temperature of from about 50° F to about 160° F., to a metal surface a coating from an aqueous coating solution consisting of an aqueous solution of calcium phosphate and an oxidizing agent, in which the calcium phosphate is present in an amount of from about 0.01 to about 1.0 moles per liter as measured by the Ca++ cation and in which the pH of the solution is between about 3.0 and about 4.2 and said pH is as close as possible to, but does not exceed, the saturation pH of the calcium phosphate at said concentration and said temperature.
Claim 3
Dependent Claim
23 words
A method according to claim 1 in which the calcium cation of the calcium phosphate is supplied in the form of calcium carbonate.
Claim 4
Dependent Claim
25 words
The method according to claim 1 wherein the phosphate anion of the calcium phosphate is supplied in the form of an aqueous phosphoric acid solution.
Claim 5
Dependent Claim
34 words
The method according to claim 1 in which the temperature is between about 90° F to about 120° F. and the pH of the aqueous coating solution is between about 3.7 and about 3.8.
Claim 6
Dependent Claim
25 words
The method according to claim 1 in which the oxidizing agent is selected from the group consisting of alkali metal nitrites and alkali metal chlorates.
Claim 7
Dependent Claim
25 words
The method according to claim 5 wherein said oxidizing agent is an alkali metal nitrite present in an amount of less than about 200 ppm.
Claim 8
Dependent Claim
30 words
The method according to claim 6 wherein said alkali metal nitrite is sodium nitrite and wherein said amount of sodium nitrite present is between about 30 to about 80 ppm.
Claim 9
Dependent Claim
26 words
The method according to claim 1 in which the aqueous coating solution is applied to the metal surface by spraying said solution on said metal surface.
Claim 10
Dependent Claim
25 words
The method according to claim 1 in which said aqueous solution is applied to the metal surface by immersing said metal surface into said solution.
Claim 11
Dependent Claim
25 words
The method according to claim 1 wherein said calcium phosphate coating is applied to a thickness of less than about 50 milligrams per square foot.
Claim 12
Dependent Claim
43 words
The method according to claim 1 in which said aqueous coating solution of calcium phosphate is derived from a concentrate in which the calcium phosphate is present in the concentrate in a ratio of about 1 calcium cation for every 3 phosphate anions.
Claim 13
Dependent Claim
33 words
The method of claim 1 in which the aqueous coating solution is derived from a concentrate comprising: from about 5% to about 20% calcium carbonate from about 10% to about 60% phosphoric acid.
Claim 14
Dependent Claim
21 words
The method of claim 12 in which the concentrate contains by weight about 9% calcium carbonate and about 30% phosphoric acid.
Claim 15
Independent Claim
144 words
A method of producing an amorphous, light weight, tightly adherent calcium phosphate coating on a ferrous metal surface comprising: (A) providing an aqueous solution consisting of from about 1.0 to about 5.0 grams/liter of calcium carbonate, from about 3 to about 15 grams/liter phosphoric acid, and from about 0.05 to about 0.30 grams/liter sodium nitrite, wherein the pH of said aqueous solution is between about 3.0 and about 4.2 and is as close as possible to, but does not exceed, the saturation pH of calcium phosphate at the solution temperature of (B); (b) heating said solution to from about 90° F to about 120° F.; (c) applying said solution to said ferrous metal surface for a time sufficient to deposit thereon a noncrystalline, bonded coating of calcium phosphate to a coating thickness of less than about 50 milligrams per square foot of metal surface.
Claim 16
Independent Claim
144 words
A method of producing an amorphous, light weight, tightly adherent calcium phosphate coating on a ferrous metal surface comprising: (A) providing an aqueous solution consisting of from about 1.0 to about 5.0 grams/liter of calcium carbonate, from about 3 to about 15 grams/liter phosphoric acid, and from about 0.05 to about 0.30 grams/liter sodium nitrite, wherein the pH of said aqueous solution is between about 3.0 and about 4.2 and is as close as possible to, but does not exceed, the saturation pH of calcium phosphate at the solution temperature of (B); (b) heating said solution to from about 90° F to about 120° F.; (c) applying said solution to said ferrous metal surface for a time sufficient to deposit thereon a noncrystalline, bonded coating of calcium phosphate to a coating thickness of less than about 50 milligrams per square foot of metal surface.
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) | 1981-08-21 | 1982-02-20 | 1982-08-22 | $2000.00 | Window Closed / Lapsed |
| 7.5 Years (Year 8) | 1985-08-21 | 1986-02-20 | 1986-08-22 | $3760.00 | Window Closed / Lapsed |
| 11.5 Years (Year 12) | 1989-08-21 | 1990-02-20 | 1990-08-22 | $7700.00 | Window Closed / Lapsed |