# US 12,759,944 B2 · Max phases by reactive flash sintering and a method for ultrafast synthesis thereof

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- Number: US 12,759,944 B2
- Document ID: US12759944B2
- Status: Granted
- Kind: B2
- Application number: 18/566,610
- Filed: 2022-05-27
- Published: 2024-08-08
- Granted: 2026-10-13
- Earliest claimed: 2021-06-02
- Assignees: Council of Scientific and Industrial Research
- Applicants: Council of Scientific and Industrial Research
- Inventors: Laxmidhar Besra; Nuwula Usha Kiran; Bishnu Choudhary; Sriparna Chatterjee
- Web page: https://patentgrep.com/patent/US12759944B2

## CPC

- C04B 35/5615: {based on titanium silicon carbides}
- C04B 35/6261: {Milling}
- C04B 35/62625: {Wet mixtures}
- C04B 35/62655: {Drying, e.g. freeze-drying, spray-drying, microwave or supercritical drying}
- C04B 35/6268: {characterised by the applied pressure or type of atmosphere, e.g. in vacuum, hydrogen or a specific oxygen pressure}
- C04B 35/651: {Thermite type sintering, e.g. combustion sintering}
- C04B 2235/404: Refractory metals
- C04B 2235/422: Carbon
- C04B 2235/428: Silicon
- C04B 2235/6567: Treatment time
- C04B 2235/666: Applying a current during sintering, e.g. plasma sintering [SPS], electrical resistance heating or pulse electric current sintering [PECS]
- C04B 2235/80: Phases present in the sintered or melt-cast ceramic products other than the main phase
- 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

## Abstract

The present invention discloses a novel flash sintering process for synthesis of MAX phases, namely, but not limited to Ti2SnC and Ti3SiC2 in an extremely short time. The process is a combustion synthesis where a relatively low voltage in a range of 20-60 V/cm is applied using a DC/AC power source across the compact precursor material prior to ignition. The flash event is observed with a quick rise in current flow in a range of 100-300 mA/mm2 followed by measured temperature range of 1200-1400° C. in a green compact body of different MAX phase compositions. The process of the present invention enables the synthesis of MAX phases in air by suppressing oxidation of the material because of the very short residence time of the flashing event. In addition, the present invention focuses on synthesis of MAX phase in bulk to serve as the starting material for the development of two-dimensional MXenes.

## Claims

### Claim 1

A process for synthesis of a dense and pure MAX phase, comprising the following steps:
a) forming a mixture of a transition metal (M), a post-transition metal (A) and a non-metal (X) in a certain stoichiometric ratio, wherein the transition metal is titanium, wherein the post-transition metal is selected from tin and silicon, wherein the non-metal is carbon;
b) wet-milling the mixture in a solvent followed by vacuum drying to form a compact disc;
c) igniting exothermally the compact disc sandwiched between two flat graphite electrodes, to initiate combustion on an application of current having an electric field in a range of 20-60 V/cm, thereby promoting propagation of the combustion in an extremely short time;
d) terminating the application of current to obtain the MAX phase;
wherein the MAX phase is a three-dimensional (3D) layered transition metal carbides or nitrides or carbonitrides.

### Claim 2 (depends on 1)

The process as claimed in claim 1, wherein the mixture has a M:A:X molar ratio of about 2:0.2-1.0:1 for synthesis of Ti2SnC as MAX phase.

### Claim 3 (depends on 1)

The process as claimed in claim 1, wherein the mixture has a M:A:X molar ratio of about 3:1.0-1.8:2 for synthesis of Ti3SiC2 as MAX phase.

### Claim 4 (depends on 1)

The process as claimed in claim 1, wherein a pressure of about 5 MPa to 30 MPa is employed onto the mixture to form a compact disc.

### Claim 5 (depends on 1)

The process as claimed in claim 1, wherein pre-heating of the compacted disc is done in a range of 200-400° C.

### Claim 6 (depends on 1)

The process as claimed in claim 1, wherein the application of current is in a continuous mode and is in an optimized range of 100-300 mA/mm2.

### Claim 7 (depends on 1)

The process as claimed in claim 1, wherein temperature of the compact disc during flash event is about 1200-1400° C. and duration of the flash sintering process is less than 10 seconds.

### Claim 8 (depends on 1)

The process as claimed in claim 1, wherein the process is conducted in vacuum, or in an atmosphere of an inert gas.

### Claim 9 (depends on 1)

The process as claimed in claim 1, wherein the process is conducted in air without oxidation of the transition metal, the post-transition metal and the non-metal.

### Claim 10 (depends on 1)

The process as claimed in claim 1, wherein the MAX phase formed is grey in colour and is easily pulverizable.