US3990953A
Expired / Lapsed
US
⏱️ 0.0 years remaining
Silicon electrodeposition
Assignee: Battelle Development Corp
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Filing: 1975-11-17
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Granted: 1976-11-09
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Expires: 1995-11-17
Abstract
Abstract Elemental silicon of utility as a corrosion resistant coating, as an absorber in a solar thermal conversion system, etc. is provided by nonaqueous electrolytic deposition thereof on a cathode body through electrolytic reduction of a silicon halide or haloid silane compound as a solute in a liquid aprotic dipolar organic solvent for the compound by passing therethrough an electrolyzing current, generally at near ambient temperature and near atmospheric pressure yet under cover of an inert gas, and desirably by pulse electrolysis. The electroplating composition consists essentially of a nonaqueous solvent solution of the anhydrous liquid aprotic dipolar organic solvent, for example propylene carbonate, dimethylformamide, etc., containing the silicon solute, such as illustrated by silicon tetrachloride and trichlorosilane, in an amount providing, or providing by inclusion therewith of a dissociable electrolyte (e.g. tetrabutylammonium perchlorate), an electrical conductivity, generally greater than one m Mho, requisite to reduce the silicon solute.
Inventors
- 👤 Alfred Ells Austin
Bibliographic Details
Application Number
—
Jurisdiction
US
Data Source
google_patents
Last Synchronized
2026-10-29 09:36
CPC Classifications
C; C25; C25D; C25D3/00; C25D3/02; C25D3/54; F; F24; F24S; F24S70/00; F24S70/20; Y; Y02; Y02E; Y02E10/00; Y02E10/40
Claims Analysis
Total Claims: 22
Claim 1
Independent Claim
90 words
A method for electrodeposition of elemental silicon on an electrically conductive cathode body, which method comprises: passing an electrolyzing current from an anode to the cathode body through an electroplating composition which is a nonaqueous solvent solution of an anhydrous liquid aprotic dipolar organic solvent containing a solute which is a silicon halide or haloid silane compound in an amount providing, or providing by supplementary inclusion in the solvent therewith of a dissociatable electrolyte, an electrical conductivity requisite to reduce said compound to deposit elemental silicon on the cathode body.
Claim 2
Independent Claim
90 words
A method for electrodeposition of elemental silicon on an electrically conductive cathode body, which method comprises: passing an electrolyzing current from an anode to the cathode body through an electroplating composition which is a nonaqueous solvent solution of an anhydrous liquid aprotic dipolar organic solvent containing a solute which is a silicon halide or haloid silane compound in an amount providing, or providing by supplementary inclusion in the solvent therewith of a dissociatable electrolyte, an electrical conductivity requisite to reduce said compound to deposit elemental silicon on the cathode body.
Claim 3
Dependent Claim
24 words
The method of claim 1 in which the passing of the electrolyzing current is with the electroplating composition under cover of an inert gas.
Claim 4
Dependent Claim
85 words
The method of claim 2 employing as the solute a silicon halide of the formula. SiX 4 wherein X is Cl, Br, or I, or a mixture thereof, or a haloid silane of the formula of H n SiX 4 -n wherein n is the integer 1, 2, or 3, and X is Cl, Br, or I, or a mixture thereof, or Si n X 2n -2 wherein X is Cl, Br, or I, and n is the integer 2, 3, 4, 5, or 6.
Claim 5
Dependent Claim
19 words
The method of claim 2 employing argon as the inert gas and at a pressure greater than atmospheric pressure.
Claim 6
Dependent Claim
34 words
The method of claim 2 in which the passing of the electrolyzing current is with the electroplating composition at a temperature below the vaporization temperature of the solute and between 20° and 100° C.
Claim 7
Dependent Claim
16 words
The method of claim 2 in which the electrical conductivity is at least 1 m Mho.
Claim 8
Dependent Claim
23 words
The method of claim 6 in which the passing of the electrolyzing current is by square wave pulsing between 0.1 and 10 Hz.
Claim 9
Dependent Claim
16 words
The method of claim 7 in which cell electrical potential is between 0.6 and 6 volts.
Claim 10
Dependent Claim
31 words
The method of claim 2 employing the anhydrous liquid aprotic dipolar organic solvent selected from the group consisting of propylene carbonate, tetrahydrofuran, acetonitrile, dimethyl sulfite, tetramethylenesulfone, ethylene carbonate, N,N-dimethylacetamide, and dimethylformamide.
Claim 11
Dependent Claim
23 words
The method of claim 2 employing the anhydrous liquid aprotic dipolar organic solvent of propylene carbonate and the solute which is silicon tetrachloride.
Claim 12
Dependent Claim
22 words
The method of claim 2 employing the anhydrous liquid aprotic dipolar organic solvent of propylene carbonate and the solute which is trichlorosilane.
Claim 13
Dependent Claim
24 words
The method of claim 2 employing the anhydrous liquid aprotic dipolar organic solvent of dimethylformamide and the inert dissociatable electrolyte which is tetrabutylammonium perchlorate.
Claim 14
Dependent Claim
76 words
An electroplating composition for electrolytic deposition of elemental silicon therefrom on a cathode body, which composition consists essentially of: a nonaqueous solvent solution of an anhydrous liquid aprotic dipolar organic solvent containing a solute of a silicon halide of haloid silane compound in an amount adapted to provide, or adapted to provide by a dissociatable electrolyte included in the solvent, an electrical conductivity requisite to reduce said compound upon passing an electrolyzing current through said composition.
Claim 15
Dependent Claim
76 words
An electroplating composition for electrolytic deposition of elemental silicon therefrom on a cathode body, which composition consists essentially of: a nonaqueous solvent solution of an anhydrous liquid aprotic dipolar organic solvent containing a solute of a silicon halide of haloid silane compound in an amount adapted to provide, or adapted to provide by a dissociatable electrolyte included in the solvent, an electrical conductivity requisite to reduce said compound upon passing an electrolyzing current through said composition.
Claim 16
Dependent Claim
84 words
The composition of claim 13 in which the solute is a silicon halide of the formula SiX 4 wherein X is Cl, Br, I or a mixture thereof or a haloid silane of the formula of H n SiX 4 -n wherein n is the integer 1, 2, or 3, and X is Cl, Br, I, or a mixture thereof, or Si n X 2n +2 wherein X is Cl, Br, or I, and n is the integer 2, 3, 4, 5, or 6.
Claim 17
Dependent Claim
21 words
The composition of claim 13 containing the solute in the amount providing an electrical conductivity of at least 1 m Mho.
Claim 18
Dependent Claim
33 words
The composition of claim 13 i which the anhydrous liquid aprotic dipolar organic solvent is selected from the group consisting of propylene carbonate, tetrahydrofuran, acetonitrile, dimethyl sulfite, tetramethylenesulfone, ethylene carbonate, N,N-dimethylacetamide, and dimethylformamide.
Claim 19
Dependent Claim
27 words
The composition of claim 13 containing the solute in the amount constituting between a 0.005 M solution and a saturated solution in the anhydrous liquid aprotic solvent.
Claim 20
Dependent Claim
23 words
The composition of claim 17 in which the anhydrous liquid aprotic dipolar organic solvent is propylene carbonate and the solute is silicon tetrachloride.
Claim 21
Dependent Claim
22 words
The composition of claim 17 in which the anhydrous liquid aprotic dipolar organic solvent is propylene carbonate and the solute is trichlorosilane.
Claim 22
Dependent Claim
24 words
The composition of claim 17 in which the anhydrous liquid aprotic dipolar organic solvent is dimethylformamide and the inert dissociatable electrolyte is tetrabutylammonium perchlorate.
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) | 1979-11-09 | 1980-05-10 | 1980-11-09 | $2000.00 | Window Closed / Lapsed |
| 7.5 Years (Year 8) | 1983-11-09 | 1984-05-10 | 1984-11-09 | $3760.00 | Window Closed / Lapsed |
| 11.5 Years (Year 12) | 1987-11-09 | 1988-05-10 | 1988-11-09 | $7700.00 | Window Closed / Lapsed |