# US 11,306,030 B2 · Method for preparing graphene-CCTO based ceramic composite dielectric material

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- Number: US 11,306,030 B2
- Document ID: US11306030B2
- Status: Granted
- Kind: B2
- Application number: 16/910,781
- Filed: 2020-06-24
- Published: 2021-02-04
- Granted: 2022-04-19
- Earliest claimed: 2019-07-30
- Assignees: Chongqing Institute of East China Normal University; East China Normal University
- Applicants: Chongqing Institute of East China Normal University; East China Normal University
- Inventors: Heping Zeng; Yanwei Huang; Jiayang He
- Web page: https://patentgrep.com/patent/US11306030B2

## CPC

- C04B 35/462: based on titanates
- C01G 23/003: {Titanates (C01G23/001 takes precedence)}
- C04B 35/6264: {Mixing media, e.g. organic solvents}
- C04B 35/62645: {Thermal treatment of powders or mixtures thereof other than sintering}
- C04B 35/62655: {Drying, e.g. freeze-drying, spray-drying, microwave or supercritical drying}
- C04B 35/63416: {Polyvinylalcohols [PVA]; Polyvinylacetates}
- C04B 2235/3208: Calcium oxide or oxide-forming salts thereof, e.g. lime
- C04B 2235/3224: Rare earth oxide or oxide forming salts thereof, e.g. scandium oxide
- C04B 2235/3225: Yttrium oxide or oxide-forming salts thereof
- C04B 2235/3232: Titanium oxides or titanates, e.g. rutile or anatase
- C04B 2235/3244: Zirconium oxides, zirconates, hafnium oxides, hafnates, or oxide-forming salts thereof
- C04B 2235/3251: Niobium oxides, niobates, tantalum oxides, tantalates, or oxide-forming salts thereof
- C04B 2235/3281: Copper oxides, cuprates or oxide-forming salts thereof, e.g. CuO or Cu2O
- C04B 2235/3284: Zinc oxides, zincates, cadmium oxides, cadmiates, mercury oxides, mercurates or oxide forming salts thereof
- C04B 2235/3293: Tin oxides, stannates or oxide forming salts thereof, e.g. indium tin oxide [ITO]
- C04B 2235/401: Alkaline earth metals
- C04B 2235/407: Copper
- C04B 2235/422: Carbon
- C04B 2235/425: Graphite
- C04B 2235/441: Alkoxides, e.g. methoxide, tert-butoxide
- C04B 2235/449: Organic acids, e.g. EDTA, citrate, acetate, oxalate
- C04B 2235/604: Pressing at temperatures other than sintering temperatures
- C04B 2235/665: Local sintering, e.g. laser sintering
- C04B: LIME, MAGNESIA; SLAG; CEMENTS; COMPOSITIONS THEREOF, e.g. MORTARS, CONCRETE OR LIKE BUILDING MATERIALS; ARTIFICIAL STONE {(roofing granules E04D7/005)}; CERAMICS (devitrified glass-ceramics C03C10/00); REFRACTORIES; TREATMENT OF NATURAL STONE
- C01G: COMPOUNDS CONTAINING METALS NOT COVERED BY SUBCLASSES C01D OR C01F (metal hydrides {monoborane, diborane or addition complexes thereof} C01B6/00; salts of oxyacids of halogens C01B11/00; peroxides, salts or peroxyacids C01B15/00; thiosulfates, dithionites, polythionates C01B17/64; compounds containing selenium, or tellurium C01B19/00; binary compounds of nitrogen with metals C01B21/06; azides C01B21/08; {compounds containing nitrogen, other non-metals and metal C01B21/082}; metal amides C01B21/092; nitrites C01B21/50; {compounds of noble gases C01B23/0005}; phosphides C01B25/08; salts of oxyacids of phosphorus C01B25/16; carbides C01B32/90; compounds containing silicon C01B33/00; compounds containing boron C01B35/00; compounds having molecular sieve properties but not having base-exchange properties C01B37/00; compounds having molecular sieve and base-exchange properties, e.g. crystalline zeolites, C01B39/00; cyanides C01C3/08; salts of cyanamide C01C3/16; thiocyanates C01C3/20)

## Abstract

Provided is a method for preparing a graphene-copper calcium titanate CCTO based ceramic composite dielectric material, which includes: dissolving metal ion sources in respective solvents to obtain respective solutions, and mixing the solutions evenly to obtain a precursor collosol of the CCTO based ceramic; allowing the precursor collosol of the CCTO based ceramic to stand for aging, followed by adding a graphene oxide dispersion to mix with the precursor collosol evenly, drying the resulting mixture to obtain dry precursor powders of the graphene-CCTO based ceramic, which are then grinded into fine powders, followed by irradiating by a low-power laser to obtain graphene-CCTO based ceramic composite powders; and compacting and molding the graphene-CCTO based ceramic composite powders, followed by catalytic synthesis with a high-power laser to obtain the graphene-CCTO based ceramic composite dielectric material.

## Claims

### Claim 1

A method for preparing a graphene-copper calcium titanate CCTO based ceramic composite dielectric material, comprising:
dissolving a titanium ion source, a copper ion source and a calcium ion source in respective solvents to obtain respective solutions, and mixing the solutions evenly to obtain a precursor collosol of the CCTO based ceramic;
allowing the precursor collosol of the CCTO based ceramic to stand for aging, followed by adding a graphene oxide dispersion in a mass ratio of graphene to the CCTO based ceramic in a range of 1:3 to 1:100 to mix with the precursor collosol evenly, drying the resulting mixture to obtain dry precursor powders of the graphene-CCTO based ceramic, which are then ground into fine powders, followed by irradiating by a low-power laser having a power of lower than 50 W to obtain graphene-CCTO based ceramic composite powders; and
compacting and molding the graphene-CCTO based ceramic composite powders, followed by catalytic synthesis with a high-power laser having a power in a range of higher than 50 W to obtain the graphene-CCTO based ceramic composite dielectric material.

### Claim 2 (depends on 1)

The method according to claim 1, wherein the CCTO based ceramic comprises copper calcium titanate or copper calcium titanate doped with a metal oxide.

### Claim 3 (depends on 2)

The method according to claim 2, wherein the metal oxide comprises at least one selected from yttrium oxide, ytterbium oxide, zinc oxide, tin oxide, tantalum oxide, hafnium oxide, gadolinium oxide, and zirconium oxide.

### Claim 4 (depends on 1)

The method according to claim 1, wherein the drying is performed at a temperature in a range of 100 to 180° C.

### Claim 5 (depends on 1)

The method according to claim 1, wherein the graphene-CCTO based ceramic composite powders are compacted and molded by oil press, cold isostatic pressing or pressing with PVA granulation.

### Claim 6 (depends on 1)

The method according to claim 1, wherein the low-power laser has a power in a range of 15 to 25 W.

### Claim 7 (depends on 1)

The method according to claim 1, wherein the high-power laser has a power in a range of 78 to 300 W.