Patent US2544799A successfully refreshed from Google Patents.
Patent US3713993A successfully refreshed from Google Patents.
US3713993A
Expired / Lapsed
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Electrodeposition of zirconium diboride
Assignee: Union Carbide Corp
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Filing: 1970-06-08
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Granted: 1973-01-30
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Expires: 1990-06-08
Abstract
Abstract Coherent coatings of zirconium diboride are deposited electrolytically from a melt containing at least one fluoride of potassium, rubidium or cesium, at least one fluoride of an element higher in the electromotive series than zirconium and boron, at least one fluoride of zirconium, and boron trioxide. The process employs an anode of zirconium or zirconium diboride, and an electrically conductive base material as a cathode. The temperature of the electrolytic melt is maintained in excess of 750*C., and the oxygen to boron molar ratio in the melt is maintained below 1.75.
Inventors
- 👤 G Mellors
- 👤 S Senderoff
Bibliographic Details
Application Number
—
Jurisdiction
US
Data Source
google_patents
Last Synchronized
2026-10-31 20:48
CPC Classifications
C; C25; C25D; C25D9/00; C25D9/04; C25D9/08; C01; C01B; C01B35/00; C01B35/02; C01B35/04
Claims Analysis
Total Claims: 15
Claim 1
Independent Claim
222 words
Process for producing coherent deposits of zirconium diboride which comprises electrolyzing, in an inert atmosphere, an electrolytic melt which consists essentially of: i. a base melt of: a. from about 10 to about 90 weight per cent of at least one fluoride of potassium, rubidium, or cesium; and b. the balance of the base melt being at least one fluoride of other elements higher in the electromotive series than zirconium and boron; ii. at least one fluoride of zirconium in an amount sufficient to provide from about 5 to about 30 weight per cent of the simple fluoride of zirconium, the percentage being based upon the weight of the electrolytic melt, wherein the zirconium is maintained solely in the tetravalent state during production of said deposit; and iii. boron trioxide in an amount of from about 3.2 weight per cent to about 12 weight per cent, based upon weight of the electrolytic melt; wherein the anode employed in said process is zirconium or zirconium diboride, wherein the cathode is an electrically conductive base material, and wherein zirconium diboride is formed on said base material as a coherent deposit; provided that the temperature of said electrolytic melt is maintained in excess of 750*C. and the oxygen to boron molar ratio in said electrolytic melt is maintained below 1.75, during production of said deposit.
Claim 2
Dependent Claim
222 words
Process for producing coherent deposits of zirconium diboride which comprises electrolyzing, in an inert atmosphere, an electrolytic melt which consists essentially of: i. a base melt of: a. from about 10 to about 90 weight per cent of at least one fluoride of potassium, rubidium, or cesium; and b. the balance of the base melt being at least one fluoride of other elements higher in the electromotive series than zirconium and boron; ii. at least one fluoride of zirconium in an amount sufficient to provide from about 5 to about 30 weight per cent of the simple fluoride of zirconium, the percentage being based upon the weight of the electrolytic melt, wherein the zirconium is maintained solely in the tetravalent state during production of said deposit; and iii. boron trioxide in an amount of from about 3.2 weight per cent to about 12 weight per cent, based upon weight of the electrolytic melt; wherein the anode employed in said process is zirconium or zirconium diboride, wherein the cathode is an electrically conductive base material, and wherein zirconium diboride is formed on said base material as a coherent deposit; provided that the temperature of said electrolytic melt is maintained in excess of 750*C. and the oxygen to boron molar ratio in said electrolytic melt is maintained below 1.75, during production of said deposit.
Claim 3
Dependent Claim
27 words
Process of claim 1 wherein the proportion of boron trioxide in the electrolytic melt is from about 5.7 weight per cent to about 12 weight per cent.
Claim 4
Dependent Claim
18 words
Process of claim 1 wherein the base melt consists essentially of the fluorides of lithium, sodium, and potassium.
Claim 5
Dependent Claim
22 words
Process of claim 1 wherein the base melt consists essentially of the eutectic mixture of the fluorides of lithium, sodium, and potassium.
Claim 6
Dependent Claim
22 words
Process of claim 1 wherein the electrolytic melt consists essentially of sodium fluoride, potassium fluoride, lithium fluoride, zirconium tetrafluoride, and boron trioxide.
Claim 7
Dependent Claim
61 words
Process of claim 5 wherein the electrolytic melt consists essentially of the eutectic mixture of the fluorides of lithium, sodium, and potassium, about 6 to 10 weight per cent of zirconium tetrafluoride, and about 10 to 12 weight per cent of boron trioxide, the balance being said eutectic mixture, and the percentages being based upon total weight of the electrolytic melt.
Claim 8
Dependent Claim
27 words
The process of claim 5 wherein the anode is zirconium and wherein the oxygen to boron ratio is maintained below 1.75 by periodic additions of boron trioxide.
Claim 9
Dependent Claim
27 words
Process of claim 1 wherein the melt is maintained at a temperature in the range of from about 800*C. to about 900*C. during production of said deposit.
Claim 10
Dependent Claim
30 words
Process of claim 1 wherein the cathode current density is maintained within the range of from about 5 to about 100 milliamperes per square centimeter during production of said deposit.
Claim 11
Dependent Claim
22 words
Process of claim 9 wherein the cathode current density is maintained below 50 milliamperes peR square centimeter during production of said deposit.
Claim 12
Dependent Claim
19 words
Process of claim 9 wherein the anode current density is not more than about 5 milliamperes per square centimeter.
Claim 13
Dependent Claim
124 words
Process of claim 1 wherein said process comprises electrolyzing an electrolytic melt consisting essentially of: i the fluorides of potassium, sodium, and lithium; ii zirconium tetrafluoride or potassium fluozirconate; and iii boron trioxide; wherein the anode is zirconium diboride and the cathode is an electrically conductive base material, to form on said base material a coherent zirconium diboride deposit, the electrolyzing being carried out such that the anode current density does not exceed about 5 milliamperes per square centimeter; provided that during the production of said deposit the temperature of the electrolytic melt is maintained at a temperature in the range of from about 800*C. to about 900*C., and the oxygen to boron molar ratio in said electrolytic melt is maintained below about 1.75.
Claim 14
Dependent Claim
15 words
The process of claim 1 wherein the cathode is copper, stainless steel, graphite, or tantalum.
Claim 15
Dependent Claim
27 words
The process of claim 1 wherein the said coherent deposit of zirconium diboride is removed from said base material, thereby producing a substantially pure zirconium diboride object.
References Cited (Backward Citations)
US3479158A
Cited
US3600284A
Cited
USPTO Annuity & Maintenance Windows
| Annuity Stage | Window Opens | Payment Deadline | Surcharge Period Until | Estimated Fee | Status |
|---|---|---|---|---|---|
| 3.5 Years (Year 4) | 1976-01-30 | 1976-07-31 | 1977-01-30 | $2000.00 | Window Closed / Lapsed |
| 7.5 Years (Year 8) | 1980-01-30 | 1980-07-31 | 1981-01-30 | $3760.00 | Window Closed / Lapsed |
| 11.5 Years (Year 12) | 1984-01-30 | 1984-07-31 | 1985-01-30 | $7700.00 | Window Closed / Lapsed |