# US 12,191,078 B2 · Ternary composite material, supercapacitor, and related methods

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- Number: US 12,191,078 B2
- Document ID: US12191078B2
- Status: Granted
- Kind: B2
- Application number: 18/063,998
- Filed: 2022-12-09
- Published: 2023-06-15
- Granted: 2025-01-07
- Earliest claimed: 2021-12-13
- Assignees: Purdue Research Foundation
- Applicants: Purdue Research Foundation
- Inventors: Jong Hyun Choi; Duncan Neal Houpt; Jaehoon Ji
- Web page: https://patentgrep.com/patent/US12191078B2

## CPC

- H01G 11/36: Nanostructures, e.g. nanofibres, nanotubes or fullerenes
- C01B 32/16: Preparation
- C01B 32/174: Derivatisation; Solubilisation; Dispersion in solvents
- H01G 11/02: using combined reduction-oxidation reactions, e.g. redox arrangement or solion
- H01G 11/26: characterised by their structure, e.g. multi-layered, porosity or surface features
- H01G 11/30: characterised by their material
- H01G 11/32: Carbon-based
- H01G 11/46: Metal oxides
- H01G 11/48: Conductive polymers
- H01G 11/86: specially adapted for electrodes (carbonisation or activation of carbon for the manufacture of electrodes H01G11/34)
- Y02E 60/13: Energy storage using capacitors
- H01G: CAPACITORS; CAPACITORS, RECTIFIERS, DETECTORS, SWITCHING DEVICES, LIGHT-SENSITIVE OR TEMPERATURE-SENSITIVE DEVICES OF THE ELECTROLYTIC TYPE (selection of specified materials as dielectric H01B3/00; capacitors having potential barriers H10D1/62, H10K10/10)
- C01B: NON-METALLIC ELEMENTS; COMPOUNDS THEREOF; {METALLOIDS OR COMPOUNDS THEREOF NOT COVERED BY SUBCLASS C01C}
- Y02E: REDUCTION OF GREENHOUSE GAS [GHG] EMISSIONS, RELATED TO ENERGY GENERATION, TRANSMISSION OR DISTRIBUTION

## Abstract

Ternary composite material, electrode, supercapacitor, and related methods. A ternary composite material includes a scaffold formed of carbon nanotubes (CNT), a first layer of zeolitic imidazolate 8 (ZIF-8) crystals formed on the scaffold of the CNT, and a second layer of molybdenum disulfide (MoS2) flakes formed on the first layer of the ZIF-8 crystals. An electrode can be formed with the ternary composite. A supercapacitor may include one or more electrodes that are at least partly formed of the ternary composite material. Methods of producing the ternary composite material and the electrodes are also disclosed.

## Claims

### Claim 1

A ternary composite material comprising:
a scaffold formed of carbon nanotubes (CNT);
a first layer of zeolitic imidazolate 8 (ZIF-8) crystals formed on the scaffold of the CNT; and
a second layer of molybdenum disulfide (MoS2) flakes formed on the first layer of the ZIF-8 crystals,
wherein the ZIF-8 crystals are thiolated, and
wherein sulfur vacancies of the MoS2 flakes are bound to thiol group binding sites of the ZIF-8 crystals.

### Claim 2 (depends on 1)

A supercapacitor comprising an electrode at least partly formed of the ternary composite material of claim 1.

### Claim 3 (depends on 2)

The supercapacitor of claim 2, wherein the electrode has a specific capacitance of about 262 F/g.

### Claim 4 (depends on 3)

The supercapacitor of claim 3, wherein the electrode retains at least 90 percent of the specific capacitance over 50,000 cycles.

### Claim 5 (depends on 2)

The supercapacitor of claim 2, wherein the electrode has an energy density of about 52.4 Wh/kg measured at a scan rate of 20 mV/s.

### Claim 6 (depends on 2)

The supercapacitor of claim 2, wherein the electrode has a power density of about 3680 W/kg under 100 mV/s.

### Claim 7 (depends on 2)

The supercapacitor of claim 2, wherein the electrode has energy storage mechanisms comprising a surface-controlled capacitive process and a diffusion-controlled redox process with nearly equal contributions at a scan rate of 100 mV/s.

### Claim 8 (depends on 2)

A method of producing an electrode of the supercapacitor of claim 2, the method comprising:
producing a thin film of the ternary composite material;
depositing the thin film on a substrate with a conductive epoxy thereon; and
curing the conductive epoxy, thereby securing the thin film on the substrate.

### Claim 9 (depends on 8)

The method of claim 8, wherein producing the thin film comprises:
vacuum-filtrating a solution comprising the ternary composite material on a porous polytetrafluoroethylene (PTFE) membrane such that the solution diffuses through the membrane while the ternary composite material remains on the membrane and forms the thin film.

### Claim 10 (depends on 9)

The method of claim 9, further comprising:
washing the thin film with ethanol and water; and
heating the thin film for a period of time sufficient to remove impurities therefrom.

### Claim 11 (depends on 8)

The method of claim 8, wherein the ternary composite material is produced by a method comprising:
providing the CNT;
synthesizing the first layer of the ZIF-8 crystals on the CNT to form a binary composite material; and
reacting the binary composite material with the MoS2 flakes to form the ternary composite material.

### Claim 12 (depends on 11)

The method of claim 11, wherein the CNT are prepared by a high-pressure, gas-phase decomposition of CO (HiPco) process.

### Claim 13 (depends on 11)

The method of claim 11, wherein providing the CNT comprises reacting the CNT and dopamine hydrochloride to form CNT-dopamine complexes.

### Claim 14 (depends on 13)

The method of claim 13, wherein the synthesizing the first layer of the ZIF-8 crystals on the CNT comprises:
combining the CNT-dopamine complexes, dimethylformamide (DMF), zinc chloride, and 1h-1,2,4-triazole-3-thiol in a mixture; and
heating the mixture for a time sufficient to form the first layer of the ZIF-8 crystals on the CNT.

### Claim 15 (depends on 11)

The method of claim 11, wherein the MoS2 flakes are produced by sonicating bulk MoS2 crystals in DMF.

### Claim 16 (depends on 1)

A method of producing the ternary composite material of claim 1, the method comprising:
providing the CNT;
synthesizing the first layer of the ZIF-8 crystals on the CNT to form a binary composite material; and
reacting the binary composite material with the MoS2 flakes to form the ternary composite material.

### Claim 17 (depends on 16)

The method of claim 16, wherein the CNT are prepared by a high-pressure, gas-phase decomposition of CO (HiPco) process.

### Claim 18 (depends on 16)

The method of claim 16, wherein providing the CNT comprises reacting the CNT and dopamine hydrochloride to form CNT-dopamine complexes.

### Claim 19 (depends on 18)

The method of claim 18, wherein the synthesizing the first layer of the ZIF-8 crystals on the CNT comprises:
combining the CNT-dopamine complexes, dimethylformamide (DMF), zinc chloride, and 1h-1,2,4-triazole-3-thiol in a mixture; and
heating the mixture for a time sufficient to form the first layer of the ZIF-8 crystals on the CNT.

### Claim 20 (depends on 16)

The method of claim 16, wherein the MoS2 flakes are produced by sonicating bulk MoS2 crystals in DMF.