# US 10,767,273 B2 · Methods for enhanced electrolytic loading of hydrogen

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- Number: US 10,767,273 B2
- Document ID: US10767273B2
- Status: Granted
- Kind: B2
- Application number: 16/361,825
- Filed: 2019-03-22
- Published: 2020-08-13
- Granted: 2020-09-08
- Earliest claimed: 2019-02-13
- Assignees: IH IP Holdings Limited
- Applicants: IH IP Holdings Limited
- Inventors: Dennis Cravens
- Web page: https://patentgrep.com/patent/US10767273B2

## CPC

- C25B 15/02: Process control or regulation
- C25B 1/04: by electrolysis of water
- C25B 9/65: Means for supplying current; Electrode connections; Electric inter-cell connections
- H01M 4/242: {Hydrogen storage electrodes}
- H01M 4/26: Processes of manufacture
- G21B 3/00: Low temperature nuclear fusion reactors, e.g. alleged cold fusion reactors
- G21B 3/002: {Fusion by absorption in a matrix}
- Y02E 30/10: Nuclear fusion reactors
- Y02E 60/10: Energy storage using batteries
- Y02E 60/36: Hydrogen production from non-carbon containing sources, e.g. by water electrolysis
- C25B: ELECTROLYTIC OR ELECTROPHORETIC PROCESSES FOR THE PRODUCTION OF COMPOUNDS OR NON-METALS; APPARATUS THEREFOR (anodic or cathodic protection C23F13/00; single-crystal growth C30B)
- H01M: PROCESSES OR MEANS, e.g. BATTERIES, FOR THE DIRECT CONVERSION OF CHEMICAL ENERGY INTO ELECTRICAL ENERGY
- G21B: FUSION REACTORS (uncontrolled reactors G21J)
- Y02E: REDUCTION OF GREENHOUSE GAS [GHG] EMISSIONS, RELATED TO ENERGY GENERATION, TRANSMISSION OR DISTRIBUTION

## Abstract

An electrolytic method of loading hydrogen into a cathode includes placing the cathode and an anode in an electrochemical reaction vessel filled with a solvent, mixing a DC component and an AC component to produce an electrolytic current, and applying an electrolytic current to the cathode. The DC component includes cycling between: a first voltage applied to the cathode for a first period of time, a second voltage applied to the cathode for a second period of time, wherein the second voltage is higher than the first voltage, and wherein the second period of time is shorter than the first period of time. The AC component has a frequency between about 1 Hz and about 100 kHz. The peak sum of the voltages supplied by the DC component and AC component is higher than the dissociation voltage of the solvent.

## Claims

### Claim 1

An electrolytic method of loading hydrogen into a cathode comprising:
placing the cathode and an anode in an electrochemical reaction vessel filled with a solvent;
mixing a DC component and an AC component to produce an electrolytic current such that the electrolytic current comprises a DC biased waveform wherein an AC waveform is superimposed onto a DC waveform;
applying the electrolytic current to the cathode, wherein a first voltage and a second voltage applied to the cathode relative to the anode that load hydrogen onto the cathode are negative,
wherein the DC component includes cycling between:
the first voltage applied to the cathode for a first period of time;
the second voltage applied to the cathode for a second period time;
wherein the first voltage is more negative than the second voltage, and
wherein the second period of time is shorter than the first period of time; and
wherein the AC component has a frequency between about 1 Hz and about 100 kHz; and
wherein the peak sum of the voltages supplied by the DC component and AC component is higher than the dissociation voltage of the solvent.

### Claim 2 (depends on 1)

The method of claim 1, further comprising:
performing an initial loading comprising:
mixing an initial DC component and an initial AC component to produce an initial electrolytic current such that the initial electrolytic current comprises a DC biased waveform wherein an AC waveform is superimposed onto a DC waveform;
applying the initial electrolytic current to the cathode, wherein a third voltage and a fourth voltage applied to the cathode relative to the anode that load hydrogen onto the cathode are negative,
wherein the initial DC component includes cycling between:
the third voltage applied to the cathode for a third period of time;
the fourth voltage applied to the cathode for a fourth period time;
wherein the fourth voltage is higher than the third voltage;
wherein the third period of time and the fourth period of time are approximately the same; and
wherein the third voltage is lower than the first voltage and the fourth voltage is lower than the second voltage; and
wherein the initial AC component has a frequency between about 1 Hz and about 100 kHz.

### Claim 3 (depends on 1)

The method of claim 1, further comprising sealing the electrochemical reaction vessel.

### Claim 4 (depends on 3)

The method of claim 3, further comprising flushing the electrochemical reaction vessel with a reductive gas prior to sealing the electrochemical vessel.

### Claim 5 (depends on 1)

The method of claim 1, further comprising applying a magnetic field to the electrochemical reaction vessel.

### Claim 6 (depends on 1)

The method of claim 1, wherein the frequency of the AC component is dynamically adjusted.

### Claim 7 (depends on 1)

The method of claim 1, wherein the DC component and AC component of the electrolytic current is mixed with a DC bias.

### Claim 8 (depends on 1)

The method of claim 1, wherein the cathode is comprised of at least one of palladium or a palladium alloy.

### Claim 9 (depends on 1)

The method of claim 1, wherein the cathode has a hydrogen diffusion rate greater than about 0.1 cm3/cm2/s.

### Claim 10 (depends on 1)

The method of claim 1, wherein the cathode has a hydrogen diffusion rate greater than about 1.4 cm3/cm2/s.

### Claim 11 (depends on 1)

The method of claim 1, wherein the solvent is a solution containing LiOH.

### Claim 12 (depends on 1)

The method of claim 1, wherein the solvent is a solution containing LiOD.

### Claim 13

A system for electrolytic loading of hydrogen into a cathode comprising:
an electrochemical reaction vessel filled with a solvent;
a cathode and an anode disposed within the electrochemical reaction vessel;
an electrolytic current source connected to the cathode, wherein the electrolytic current source is programmed to apply an electrolytic current to the cathode, wherein a first voltage and a second voltage applied to the cathode relative to the anode that load hydrogen onto the cathode are negative, and wherein the electrolytic current comprises:
a DC component, wherein the DC component cycles between:
the first voltage applied to the cathode for a first period of time;
the second voltage applied to the cathode for a second period time;
wherein the first voltage is more negative than the second voltage, and
wherein the second period of time is shorter than the first period of time; and
a AC component with a frequency between about 1 Hz and about 100 kHz;
wherein the peak sum of the voltages supplied by the DC component and AC component is higher than the dissociation voltage of the solvent and
wherein the DC component and the AC component are mixed such that the electrolytic current comprises a DC biased waveform wherein an AC waveform is superimposed onto a DC waveform.

### Claim 14 (depends on 13)

The system of claim 13, wherein the electrochemical reaction vessel is sealed.

### Claim 15 (depends on 14)

The system of claim 14, wherein the electrochemical reaction vessel is flushed with a reductive gas prior to sealing.

### Claim 16 (depends on 13)

The system of claim 13, further comprising a magnetic field applied to the electro chemical reaction vessel.

### Claim 17 (depends on 13)

The system of claim 13, wherein the frequency of the AC component is dynamically adjusted.

### Claim 18 (depends on 13)

The system of claim 13, further comprising a mixer, wherein the mixer mixes the DC component and AC component of the electrolytic current with a DC bias.

### Claim 19 (depends on 13)

The system of claim 13, wherein the cathode is comprised of at least one of palladium or a palladium alloy.

### Claim 20 (depends on 13)

The system of claim 13, wherein the cathode has a hydrogen diffusion rate greater than about 0.1 cm3/cm2/s.

### Claim 21 (depends on 13)

The system of claim 13, wherein the cathode has a hydrogen diffusion rate greater than about 1.4 cm3/cm2/s.

### Claim 22 (depends on 13)

The system of claim 13, wherein the solvent is a solution containing LiOH.

### Claim 23 (depends on 13)

The system of claim 13, wherein the solvent is a solution containing LiOD.
