CN112142449A - Two-dimensional transition metal titanium carbide material reinforced ceramic composite material and preparation method thereof - Google Patents
Two-dimensional transition metal titanium carbide material reinforced ceramic composite material and preparation method thereof Download PDFInfo
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Abstract
The invention relates to the field of materials, in particular to the field of ceramic composite materials, and particularly relates to a preparation method of an alumina, zirconia, silicon carbide and silicon nitride ceramic composite material. The invention adopts a novel two-dimensional transition metal titanium carbide material (MXene comprises Ti3C2 and Ti 2C) as a toughening phase, and Al2O3-MXene, ZrO2-MXene, SiC-MXene and Si3N4-MXene composite ceramic are sintered by discharge plasma. First step, preparation of MXene compound: preparing a Ti3C2 or Ti2C MXene compound by corroding a prepared or purchased ternary layered compound Ti3AlC2 or Ti2AlC with hydrofluoric acid; secondly, mixing the ceramic powder (alumina, zirconia, silicon carbide or silicon nitride) with a Ti3C2 or Ti2C MXene compound according to the weight ratio of (95-60): (5-40), mixing the raw materials with a proper sintering aid by a physical mechanical method for 5-20 hours; drying the mixed powder, and then putting the dried mixed powder into a graphite die for cold press molding, wherein the applied pressure is 10-20 MPa; sintering in a discharge plasma sintering furnace at the heating rate of 10-50 ℃ per minute and the sintering temperature of 1400-1600 ℃, the sintering time of 30-120 minutes and the sintering pressure of 10-50MPa, and then cooling to room temperature along with the furnace to prepare the Al2O3-MXene, ZrO2-MXene, SiC-MXene and Si3N4-MXene composite ceramic.
Description
The invention relates to the technical field of ceramic material science, in particular to a composite ceramic material and a preparation method thereof.
Background
The composite ceramic material has the advantages of high melting point, good wear resistance, thermochemical stability, high hardness and the like, and is suitable for manufacturing cutters for processing difficult-to-process materials. With the high-speed and sustainable development of the fields of aerospace, national defense, industry and the like in China, the requirement on the comprehensive performance of the material is higher and higher. The composite ceramic can further enhance the toughness of pure ceramic, and the hardness and high-temperature performance of the ceramic are not reduced too much, so that the composite ceramic is paid extensive attention. Titanium carbide has excellent properties such as high melting point, oxidation resistance, high strength, good thermal conductivity, good chemical stability, good toughness, and chemical inertness to steel and iron metals, and is mainly used for manufacturing cermets, heat-resistant alloys, and hard alloys. Meanwhile, because titanium carbide has the good properties, the titanium carbide is widely used as a reinforcing phase of a reinforcing matrix in various composite materials. For example, in alumina composite ceramics, titanium carbide has high strength, high hardness, excellent wear resistance and chemical stability, and thus, the alumina-titanium carbide system has been widely studied and applied.
Pure alumina powder starts to creep and sinter at approximately 1750 ℃. Such high sintering temperatures can result in shortened service life of the kiln refractories, excessive energy consumption, poor material firing performance, and the like. Therefore, a sintering aid is often added in the ceramic sintering process to reduce the sintering temperature of the high-melting-point ceramic, thereby realizing the reduction of energy consumption and preparation cost. Such as titanium dioxide, magnesium oxide, yttrium oxide, and the like. Therefore, in order for the sintering aid to perform a sintering aid function, the sintering aid is required to be uniformly mixed with the main phase.
MXene is a two-dimensional inorganic compound developed in recent years, and the materials are composed of transition metal carbide, nitride or carbonitride with the thickness of several atomic layers, have the properties of the transition metal carbide, and have special properties which are not possessed by the transition metal carbide, nitride and carbonitride due to hydroxyl groups or terminal oxygen on the surface of the materials. Therefore, the performance of the ceramic composite material can be further improved by adopting the two-dimensional titanium carbide to replace the existing titanium carbide as the reinforcing phase in the ceramic composite material.
Disclosure of Invention
The invention aims to overcome the defects of the prior art and provides a preparation method of ceramic-MXene titanium carbide (Ti 3C2 or Ti 2C) composite ceramic, wherein MXene titanium carbide (Ti 3C2 or Ti 2C) two-dimensional transition metal carbide is used as a reinforcing phase, and the sintering uniformity of ceramic powder at a lower temperature and powder sintering is improved, so that the high-hardness and high-toughness ceramic-MXene titanium carbide (Ti 3C2 or Ti 2C) composite ceramic is prepared.
Drawings
FIG. 1 is a process flow diagram of a two-dimensional transition metal carbide MXene titanium carbide (Ti 3C2 or Ti 2C) reinforced composite ceramic of the present invention;
FIG. 2 is a scanning electron micrograph of MXene-Ti3C2 obtained by preparation;
FIG. 3 is a scanning electron micrograph of the composite ceramic obtained in example 5;
FIG. 4 is a Vickers hardness indentation diagram of the composite ceramic prepared in example 5.
Detailed Description
The following detailed description of the present disclosure will be made with reference to specific examples, but not to limit the scope of the present disclosure as claimed.
MXene-two-dimensional transition metal carbide (Ti 3C2 and Ti 2C) preparation:
the invention adopts the known method to prepare MXene-two-dimensional transition metal carbide (Ti 3C2 and Ti 2C), slowly adding 3 g of prepared or purchased Ti3AlC2 or Ti2AlC powder into 50% hydrofluoric acid solution, stirring for 24 hours at normal temperature, washing with deionized water to be neutral, and vacuum drying to obtain the Ti3C2 or Ti2C powder.
Example 1
Mixing the MXene-Ti3C2 and the alumina powder according to the weight ratio of 5: mixing materials accurately according to a weight ratio of 95, ball-milling the materials for 5 hours by using absolute ethyl alcohol as a ball-milling medium, drying slurry, and preparing powder; putting the ball-milled powder into a graphite die, forming under the pressure of 10MPa, and then putting the graphite die into a discharge plasma sintering furnace for vacuum sintering, wherein the sintering temperature is as follows: 1600 ℃, heating rate: 10 ℃ per min and 50MPa pressure; and (3) preserving the heat for 120 minutes, cooling and reducing the pressure after the heat preservation is finished, and successfully preparing the alumina-titanium oxycarbide composite ceramic with the Vickers hardness of 18 GPa.
Example 2
Mixing the MXene-Ti 2C and the alumina powder according to the weight ratio of 40: mixing materials accurately at a weight ratio of 60, ball-milling the materials for 20 hours by using absolute ethyl alcohol as a ball-milling medium, drying the slurry, and preparing powder; putting the ball-milled powder into a graphite die, forming under the pressure of 20MPa, and then putting the graphite die into a discharge plasma sintering furnace for vacuum sintering, wherein the sintering temperature is as follows: 1400 ℃, heating rate: 50 ℃ per min and 10MPa pressure; and (3) preserving the heat for 60 minutes, cooling and reducing the pressure after the heat preservation is finished, and successfully preparing the alumina-titanium oxycarbide composite ceramic with the Vickers hardness of 15 GPa.
Example 3
Mixing the MXene-Ti3C2 and the alumina powder according to the weight ratio of 20: mixing materials accurately in a weight ratio of 80, ball-milling the materials for 10 hours by using absolute ethyl alcohol as a ball-milling medium, drying the slurry, and preparing powder; putting the ball-milled powder into a graphite die, forming under the pressure of 20MPa, and then putting the graphite die into a discharge plasma sintering furnace for vacuum sintering, wherein the sintering temperature is as follows: 1500 ℃, heating rate: 20 ℃ per min and the pressure of 20 MPa; and (3) preserving heat for 30 minutes, cooling and reducing pressure after the heat preservation is finished, and successfully preparing the alumina-titanium oxycarbide composite ceramic with the Vickers hardness of 17 GPa.
Example 4
Mixing the MXene-Ti3C2 and the alumina powder according to the weight ratio of 30: mixing materials accurately according to the weight ratio of 70, ball-milling the materials for 10 hours by using absolute ethyl alcohol as a ball-milling medium, drying slurry, and preparing powder; putting the ball-milled powder into a graphite die, forming under the pressure of 20MPa, and then putting the graphite die into a discharge plasma sintering furnace for vacuum sintering, wherein the sintering temperature is as follows: 1500 ℃, heating rate: 20 ℃ per min and 30 MPa; and (3) preserving the heat for 60 minutes, cooling and reducing the pressure after the heat preservation is finished, and successfully preparing the alumina-titanium oxycarbide composite ceramic with the Vickers hardness of 17 GPa.
Example 5
Mixing the MXene-Ti3C2 and zirconia powder according to the weight ratio of 30: mixing materials accurately according to the weight ratio of 70, ball-milling the materials for 10 hours by using absolute ethyl alcohol as a ball-milling medium, drying slurry, and preparing powder; putting the ball-milled powder into a graphite die, forming under the pressure of 20MPa, and then putting the graphite die into a discharge plasma sintering furnace for vacuum sintering, wherein the sintering temperature is as follows: 1500 ℃, heating rate: 20 ℃ per min and 30 MPa; and (3) preserving the heat for 60 minutes, cooling and reducing the pressure after the heat preservation is finished, and successfully preparing the alumina-titanium oxycarbide composite ceramic with the Vickers hardness of 18 GPa.
Example 6
Mixing the MXene-Ti3C2 and the silicon carbide powder according to the weight ratio of 30: mixing materials accurately according to the weight ratio of 70, ball-milling the materials for 10 hours by using absolute ethyl alcohol as a ball-milling medium, drying slurry, and preparing powder; putting the ball-milled powder into a graphite die, forming under the pressure of 20MPa, and then putting the graphite die into a discharge plasma sintering furnace for vacuum sintering, wherein the sintering temperature is as follows: 1500 ℃, heating rate: 20 ℃ per min and 30 MPa; and (3) preserving the heat for 60 minutes, cooling and reducing the pressure after the heat preservation is finished, and successfully preparing the alumina-titanium oxycarbide composite ceramic with the Vickers hardness of 17 GPa.
Example 7
Mixing the prepared MXene-Ti3C2 and silicon nitride powder according to the weight ratio of 30: mixing materials accurately according to the weight ratio of 70, ball-milling the materials for 10 hours by using absolute ethyl alcohol as a ball-milling medium, drying slurry, and preparing powder; putting the ball-milled powder into a graphite die, forming under the pressure of 20MPa, and then putting the graphite die into a discharge plasma sintering furnace for vacuum sintering, wherein the sintering temperature is as follows: 1500 ℃, heating rate: 20 ℃ per min and 30 MPa; and (3) preserving the heat for 60 minutes, cooling and reducing the pressure after the heat preservation is finished, and successfully preparing the alumina-titanium oxycarbide composite ceramic with the Vickers hardness of 19 GPa.
Claims (4)
1. The ceramic composite material and the preparation method thereof are characterized in that: the composite ceramic comprises the following components in percentage by weight:
60 to 95 percent of ceramic powder
40-5% of MXene compound.
2. The ceramic composite material and the method for preparing the same according to claim 1, wherein: the ceramic is alumina, zirconia, silicon carbide or silicon nitride.
3. The ceramic composite material and the method for preparing the same according to claim 1, wherein: the MXene compound is Ti3C2 or Ti 2C.
4. The process steps of the ceramic composite material of claim 1 are:
1) the ceramic powder and the MXene compound prepared by the method in claim 3 are Ti3C2 or Ti2C powder, and the weight ratio is 95: 5-60: 40, taking absolute ethyl alcohol as a ball milling medium, carrying out ball milling for 5-20 hours, drying slurry, and preparing powder;
2) putting the ball-milled powder into a graphite die, forming under the pressure of 10-20MPa, and then putting the graphite die into a discharge plasma sintering furnace for vacuum sintering, wherein the sintering temperature is as follows: 1400 ℃ and 1600 ℃, the heating rate is as follows: 10-50 ℃ per min, 10-50MPa and 30-120 minutes of heat preservation.
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Cited By (8)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN113337145A (en) * | 2021-06-03 | 2021-09-03 | 苏州大学 | MXene reinforced silicate adhesive ceramic coating and preparation method thereof |
| CN113480313A (en) * | 2021-08-06 | 2021-10-08 | 航天特种材料及工艺技术研究所 | MXene toughened ultrahigh-temperature ceramic composite material and preparation method thereof |
| CN114057505A (en) * | 2021-12-13 | 2022-02-18 | 西安邮电大学 | Preparation method of porous flaky alumina framework |
| CN115259874A (en) * | 2021-04-29 | 2022-11-01 | 中国科学院福建物质结构研究所 | Toughened and conductive MXene-zirconia composite ceramic and preparation method thereof |
| CN115340384A (en) * | 2022-08-02 | 2022-11-15 | 浙江东新新材料科技有限公司 | Two-dimensional transition metal carbide reinforced silicon carbide ceramic and preparation method thereof |
| CN116553937A (en) * | 2023-03-20 | 2023-08-08 | 衡阳凯新特种材料科技有限公司 | Silicon nitride composite ceramic material for sealing ring and preparation method thereof |
| CN116854452A (en) * | 2023-07-04 | 2023-10-10 | 天目山实验室 | Preparation method of two-dimensional ceramic material toughened alumina ceramic |
| CN116553937B (en) * | 2023-03-20 | 2024-07-26 | 衡阳凯新特种材料科技有限公司 | Silicon nitride composite ceramic material for sealing ring and preparation method thereof |
-
2020
- 2020-09-12 CN CN202010956858.0A patent/CN112142449A/en not_active Withdrawn
Cited By (11)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN115259874A (en) * | 2021-04-29 | 2022-11-01 | 中国科学院福建物质结构研究所 | Toughened and conductive MXene-zirconia composite ceramic and preparation method thereof |
| CN115259874B (en) * | 2021-04-29 | 2023-11-17 | 中国科学院福建物质结构研究所 | Toughened and conductive MXene-zirconia composite ceramic and preparation method thereof |
| CN113337145A (en) * | 2021-06-03 | 2021-09-03 | 苏州大学 | MXene reinforced silicate adhesive ceramic coating and preparation method thereof |
| CN113337145B (en) * | 2021-06-03 | 2022-03-01 | 苏州大学 | MXene reinforced silicate adhesive ceramic coating and preparation method thereof |
| CN113480313A (en) * | 2021-08-06 | 2021-10-08 | 航天特种材料及工艺技术研究所 | MXene toughened ultrahigh-temperature ceramic composite material and preparation method thereof |
| CN113480313B (en) * | 2021-08-06 | 2022-06-10 | 航天特种材料及工艺技术研究所 | MXene toughened ultrahigh-temperature ceramic composite material and preparation method thereof |
| CN114057505A (en) * | 2021-12-13 | 2022-02-18 | 西安邮电大学 | Preparation method of porous flaky alumina framework |
| CN115340384A (en) * | 2022-08-02 | 2022-11-15 | 浙江东新新材料科技有限公司 | Two-dimensional transition metal carbide reinforced silicon carbide ceramic and preparation method thereof |
| CN116553937A (en) * | 2023-03-20 | 2023-08-08 | 衡阳凯新特种材料科技有限公司 | Silicon nitride composite ceramic material for sealing ring and preparation method thereof |
| CN116553937B (en) * | 2023-03-20 | 2024-07-26 | 衡阳凯新特种材料科技有限公司 | Silicon nitride composite ceramic material for sealing ring and preparation method thereof |
| CN116854452A (en) * | 2023-07-04 | 2023-10-10 | 天目山实验室 | Preparation method of two-dimensional ceramic material toughened alumina ceramic |
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