CN114591084B - Method for rapidly preparing compact TiC ceramic at low temperature - Google Patents
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Abstract
The invention discloses a method for preparing compact TiC ceramics at a low temperature, which comprises the following steps: the chemical precipitation method is adopted to introduce alumina nano particles on the surfaces of TiC matrix particles, and the SPS technology is adopted to prepare almost completely compact TiC ceramics at 1500 ℃ and 1400 ℃ by adopting the one-step and two-step rapid sintering technology, so that the fracture toughness is obviously improved compared with the pure TiC ceramics with the same density.
Description
Technical Field
The invention relates to the technical field of ceramic materials, in particular to a method for rapidly preparing compact TiC ceramic at low temperature.
Background
TiC ceramic has the characteristics of high melting point, high strength, high hardness, good high-temperature stability and the like, and is a high-temperature or ultrahigh-temperature ceramic material with great potential. Has wide application prospect in the fields of high-speed machining, metallurgy, chemical industry, aerospace and the like. In recent years, tiC ceramics are closely focused by researchers in the field of nuclear industry as inert matrix fuel (GenIV-IMF) or nuclear fuel dilution materials for fourth generation nuclear reactors due to the characteristics of small sub-absorption interface, radiation resistance, good heat conduction, electric conduction and the like, and a great deal of research work is carried out on the TiC ceramics.
TiC is mainly a ceramic material formed by covalent bonds, which determines that TiC cannot consume elastic strain energy to relieve stress concentration under the action of certain external load like a metal material, so that TiC is brittleThe sex becomes a fatal weakness restricting the application thereof. For decades, researchers have made a great deal of research effort in improving the fracture toughness of TiC ceramics. Metals (e.g., ni, fe, co) and alloys (e.g., ni-Mo-Al, ni-Cr and Ni-Co-Cr) were the earliest additives for TiC ceramic toughening. Although the metal or alloy additives can improve the fracture toughness of TiC ceramics to a certain extent, the inherent high hardness, abrasion resistance, corrosion resistance and high temperature mechanical properties are sacrificed. Middle and late 90 th century, ni 3 Intermetallic compounds such as Al, feAl and FeSi are used as additives for improving the high temperature and high temperature performance of TiC ceramics. However, the addition of a large amount of intermetallic compounds with lower melting points to the matrix toughens the inherent performance advantages of TiC ceramic matrix such as high melting point, high hardness, chemical stability and high temperature stability. In order to eliminate hidden trouble caused by additives such as metals, alloys or intermetallic compounds, the urgent need is to find a toughening mode which can improve the fracture toughness of TiC ceramics and keep the inherent excellent performance of TiC ceramics.
Disclosure of Invention
The invention aims to provide a method for preparing compact TiC ceramic at a low temperature.
In order to achieve the above purpose, the present invention adopts the following technical scheme:
a method for preparing compact TiC ceramics at a low temperature rapidly comprises the following steps:
(1) Weighing a certain amount of analytically pure aluminum nitrate powder, pouring the powder into a beaker filled with deionized water, and uniformly dispersing the powder by ultrasonic waves;
(2) Weighing TiC powder, pouring the TiC powder into another beaker containing deionized water, and uniformly dispersing by ultrasonic waves;
(3) Then, slowly pouring the aluminum nitrate solution into the TiC suspension and continuously stirring;
(4) Finally, ammonia water is slowly added into the TiC suspension in a spray manner, and the pH value of the TiC suspension is regulated to be 9.0-10.0; continuing stirring for a period of time to fully perform precipitation reaction;
(5) Vacuum rotary drying the suspension with complete precipitation;
(6) Sieving the dried powder, weighing a certain amount of the powder, putting the powder into a graphite grinding tool, and performing densification sintering by using a discharge plasma sintering technology;
(7) The sintering temperature in the step (6) is 1400-1600 ℃, and the heating mode comprises the following steps: a) A one-step sintering method: heating from room temperature to 1000 ℃ with 30MPa pressure, gradually increasing to 50MPa, and preserving heat at the highest temperature for 5min;
or, b) a two-step sintering process: heating from room temperature to 1000 ℃ by adopting 30MPa pressure, gradually increasing to 50MPa, quickly cooling to 100 ℃ after the sintering temperature is raised to the highest temperature, and then preserving heat for 5min.
Preferably, the ultrasonic dispersion time in step (1) is 20 minutes.
Preferably, the ultrasonic dispersion time in step (2) is 20 minutes.
Preferably, the concentration of the ammonia water in the step (4) is: 0.01mol/L.
Preferably, stirring is continued in step (4) for 2 hours.
Preferably, in step (6), a 60 mesh screen is passed.
The invention adopts a chemical precipitation mode to introduce Al into TiC matrix 2 O 3 And (3) rapidly preparing the TiC high-temperature ceramic with high density at low temperature by a Spark Plasma Sintering (SPS) technology.
Drawings
FIG. 1 shows TiC-Al of the present invention 2 O 3 Schematic diagram of the process flow of preparing the mixed powder;
FIG. 2 shows SPS sintering apparatus (a) TiC particles (b) and TiC-Al obtained by chemical precipitation 2 O 3 A microstructure schematic diagram of the mixed powder (c) in the sintering process;
FIG. 3 shows the TiC-Al powder particles (a) and TiC-Al particles treated by chemical precipitation 2 O 3 Transmission electron microscope photograph of powder particle (b), (c) TiC-Al 2 O 3 An energy spectrum analysis chart of the particle surface layer;
FIG. 4 shows pure TiC and TiC-10wt% Al after sintering at 1500 ℃ 2 O 3 A section morphology comparison graph of the ceramic;
FIG. 5 shows pure TiC and TiC-10wt% Al after sintering at 1500 ℃ 2 O 3 Fracture toughness comparison chart of ceramics;
FIG. 6 is TiC-10wt% Al 2 O 3 A relative density comparison graph of ceramics after different heating modes;
FIG. 7 is TiC-10wt% Al 2 O 3 Fracture toughness comparison graph of ceramics after different heating modes.
Detailed Description
The technical solutions in the embodiments of the present invention will be clearly and completely described below with reference to the drawings in the embodiments of the present invention, but the scope of protection of the present invention is not limited.
Referring to fig. 1 and 2, the invention provides a method for preparing compact TiC ceramics at a low temperature, which mainly comprises the following steps:
1, 1wt%, 2wt%, 3wt%, 5wt% and 10wt% Al in terms of the weight are weighed first 2 O 3 Pouring the pure aluminum nitrate powder into a beaker containing deionized water, and uniformly performing ultrasonic dispersion for 20min; in order to ensure better sintering performance, the addition amount of the alumina which does not affect the inherent performance of TiC cannot be higher than 15wt%;
2, weighing 10g of TiC powder, pouring the powder into another beaker containing deionized water, and uniformly performing ultrasonic dispersion for 20min;
3, slowly pouring the aluminum nitrate solution into the TiC suspension and continuing magnetic stirring;
4, finally, slowly adding ammonia water (0.01 mol/L) into the TiC suspension in a spray manner, and regulating and controlling the pH value to be about 9.0;
5, continuously magnetically stirring the suspension with the pH value adjusted for 2 hours to ensure that the precipitation reaction is fully carried out;
6, finally, vacuum rotary drying the suspension with the completely precipitated;
and 7, sieving the dried powder with a 60-mesh sieve, weighing 2g of the powder, putting the powder into a graphite grinding tool with the diameter of 20mm, and performing densification sintering by utilizing an SPS technology.
8, sintering temperature is 1400-1600 ℃, and two heating modes are adopted: a) A one-step sintering method, namely, heating from room temperature to 1000 ℃ and adopting 30MPa pressure, gradually increasing to 50MPa (or 80 MPa), and preserving heat for 5min at the highest temperature;
b) The two-step sintering process includes raising the temperature from room temperature to 1000 deg.c under 30MPa, raising the temperature to 50MPa, raising the sintering temperature to highest temperature, fast cooling to 100 deg.c and maintaining for 5min.
Example 1
TiC-1wt％Al 2 O 3 The preparation of the ceramic comprises the following specific preparation processes:
1, 1 weight percent Al after conversion is firstly weighed 2 O 3 Pouring the pure aluminum nitrate powder into a beaker containing deionized water, and uniformly performing ultrasonic dispersion for 20min;
2, weighing 10g of TiC powder, pouring the powder into another beaker containing deionized water, and uniformly performing ultrasonic dispersion for 20min;
3, slowly pouring the aluminum nitrate solution into the TiC suspension and continuing magnetic stirring;
4, finally, slowly adding ammonia water (0.01 mol/L) into the TiC suspension in a spray manner, and regulating and controlling the pH value to be about 9.0;
5, continuously magnetically stirring the suspension with the pH value adjusted for 2 hours to ensure that the precipitation reaction is fully carried out;
6, finally, vacuum rotary drying the suspension with the completely precipitated;
and 7, sieving the dried powder with a 60-mesh sieve, weighing 2g of the powder, putting the powder into a graphite grinding tool with the diameter of 20mm, and performing densification sintering by utilizing an SPS technology.
8, adopting a one-step sintering method heating mode, heating from room temperature to 1000 ℃ and adopting 30MPa pressure, then gradually increasing to 50MPa, and preserving heat for 5min at the highest temperature of 1600 ℃.
Example 2
TiC-5wt％Al 2 O 3 The preparation of the ceramic comprises the following specific preparation processes:
1, firstly weighing 5wt% of Al after conversion 2 O 3 Pouring the pure aluminum nitrate powder into a beaker containing deionized water, and uniformly performing ultrasonic dispersion for 20min;
2, weighing 10g of TiC powder, pouring the powder into another beaker containing deionized water, and uniformly performing ultrasonic dispersion for 20min;
3, slowly pouring the aluminum nitrate solution into the TiC suspension and continuing magnetic stirring;
4, finally, slowly adding ammonia water (0.01 mol/L) into the TiC suspension in a spray manner, and regulating and controlling the pH value to be about 9.0;
5, continuously magnetically stirring the suspension with the pH value adjusted for 2 hours to ensure that the precipitation reaction is fully carried out;
6, finally, vacuum rotary drying the suspension with the completely precipitated;
and 7, sieving the dried powder with a 60-mesh sieve, weighing 2g of the powder, putting the powder into a graphite grinding tool with the diameter of 20mm, and performing densification sintering by utilizing an SPS technology.
8, heating from room temperature to 1000 ℃ by adopting a one-step sintering method heating mode, adopting 30MPa pressure, gradually increasing to 50MPa, and preserving heat for 5min at the highest temperature of 1600 ℃;
example 3
TiC-10wt％Al 2 O 3 Preparation of ceramics, specific preparation process and parameters
1, firstly weighing 10wt% of Al after conversion 2 O 3 Pouring the pure aluminum nitrate powder into a beaker containing deionized water, and uniformly performing ultrasonic dispersion for 20min;
2, weighing 10g of TiC powder, pouring the powder into another beaker containing deionized water, and uniformly performing ultrasonic dispersion for 20min;
3, slowly pouring the aluminum nitrate solution into the TiC suspension and continuing magnetic stirring;
4, finally, slowly adding ammonia water (0.01 mol/L) into the TiC suspension in a spray manner, and regulating and controlling the pH value to be about 9.0;
5, continuously magnetically stirring the suspension with the pH value adjusted for 2 hours to ensure that the precipitation reaction is fully carried out;
6, finally, vacuum rotary drying the suspension with the completely precipitated;
and 7, sieving the dried powder with a 60-mesh sieve, weighing 2g of the powder, putting the powder into a graphite grinding tool with the diameter of 20mm, and performing densification sintering by utilizing an SPS technology.
8, (a) adopting a one-step sintering method heating mode, heating from room temperature to 1000 ℃ and adopting 30MPa pressure, then gradually increasing to 50MPa, and preserving heat for 5min at the highest temperature of 1500 ℃;
(b) Adopting a one-step sintering method heating mode, heating from room temperature to 1000 ℃ by adopting 50MPa pressure, gradually increasing to 80MPa, and preserving heat for 5min at the highest temperature of 1500 ℃ and 1600 ℃;
(c) The two-step sintering method is adopted to raise the temperature from room temperature to 1000 ℃ by adopting 30MPa pressure, then gradually increasing the temperature to 50MPa, quickly reducing the temperature to 1400 ℃ after the sintering temperature is raised to the highest temperature of 1500 ℃, and then preserving the heat for 5min.
TiC-10wt% Al prepared in example 3 below 2 O 3 Ceramic as an example for performance characterization
As shown in FIG. 3, FIG. 3 shows the TiC-Al powder particles (a) and TiC-Al powder particles treated by chemical precipitation 2 O 3 Transmission electron microscope photograph of powder particle (b), (c) TiC-Al 2 O 3 An energy spectrum analysis chart of the particle surface layer; as can be seen from fig. 3, the surface of the TiC powder treated by the chemical precipitation method is covered with an aluminum-containing oxide layer, and the oxide layer is sintered at high temperature to form nano Al in situ 2 O 3 The particles not only promote the sintering of the TiC matrix, but also improve the fracture toughness of the matrix.
Referring to FIG. 4, FIG. 4 shows pure TiC and TiC-10wt% Al after sintering at 1500 ℃ 2 O 3 The cross-sectional morphology of the ceramic; as can be seen, tiC-10wt% Al 2 O 3 The density of the ceramic is obviously higher than that of pure TiC ceramic at the sintering temperature of 1500 ℃.
Referring to FIG. 5, FIG. 5 shows pure TiC and TiC-10wt% Al after sintering at 1500 ℃ 2 O 3 As can be seen from FIG. 3, tiC-10wt% Al 2 O 3 The ceramic has higher fracture toughness than the pure TiC ceramic prepared under the same condition at the sintering temperature of 1500 ℃.
TiC-10wt％Al 2 O 3 Density and fracture toughness of ceramics at different temperature rise modes:
as shown in FIG. 6, tiC-10wt% Al 2 O 3 As can be seen from FIG. 6, the two-step sintering method can significantly reduce TiC-10wt% Al 2 O 3 The sintering temperature of the ceramic is equivalent to 1600 ℃ in a one-step sintering method, and the sintering temperature is reduced by 200 ℃ when the relative density is obtained at 1400 ℃.
FIG. 7 is TiC-10wt% Al 2 O 3 As can be seen from FIG. 7, tiC-10wt% Al prepared by the two-step sintering method at 1400 ℃ is shown by comparing fracture toughness of ceramics after different heating modes 2 O 3 The ceramic has higher fracture toughness, the value of which is about 5.5MP.m1/2, which is obviously higher than that of a sample prepared at 1600 ℃ in a one-step sintering method.
The method for preparing TiC ceramics at low temperature rapidly comprises the following steps: alumina nano particles are introduced on the surfaces of TiC matrix particles by adopting a chemical precipitation method, and almost completely compact TiC ceramics can be prepared at 1500 ℃ and 1400 ℃ by adopting SPS one-step and two-step rapid sintering technology, so that the fracture toughness of the prepared ceramics is obviously improved compared with that of pure TiC ceramics with the same density.
While the foregoing is directed to the preferred embodiments of the present invention, it will be appreciated by those skilled in the art that changes and modifications may be made without departing from the principles of the invention, such changes and modifications are also intended to be within the scope of the invention.
Claims (8)
1. The method for preparing the compact TiC ceramic at a low temperature rapidly is characterized by comprising the following steps of:
(1) Weighing a certain amount of analytically pure aluminum nitrate powder, pouring the powder into a beaker filled with deionized water, and uniformly dispersing the powder by ultrasonic waves;
(2) Weighing TiC powder, pouring the TiC powder into another beaker containing deionized water, and uniformly dispersing by ultrasonic waves;
(3) Slowly pouring the aluminum nitrate solution into the TiC suspension and continuously stirring;
(4) Finally, ammonia water is slowly added into the TiC suspension in a spray manner, and the pH value of the TiC suspension is regulated to be 9.0-10.0; continuing stirring for a period of time to fully perform precipitation reaction;
(5) Vacuum rotary drying the suspension with complete precipitation;
(6) Sieving the dried powder, weighing a certain amount of the powder, putting the powder into a graphite grinding tool, and performing densification sintering by using a discharge plasma sintering technology;
(7) The sintering temperature in the step (6) is 1400-1600 ℃, and the heating mode is a two-step sintering method: heating from room temperature to 1000 ℃ by adopting 30MPa pressure, gradually increasing to 50MPa, quickly cooling to 100 ℃ after the sintering temperature is raised to the highest temperature, and then preserving heat for 5min.
2. A method for preparing dense TiC ceramics at a fast low temperature as defined in claim 1, wherein: the ultrasonic dispersion time in the step (1) is 20min.
3. A method for preparing dense TiC ceramics at a fast low temperature as defined in claim 1, wherein: the ultrasonic dispersion time in the step (2) is 20min.
4. A method for preparing dense TiC ceramics at a fast low temperature as defined in claim 1, wherein: the concentration of the ammonia water in the step (4) is as follows: 0.01mol/L.
5. A method for preparing dense TiC ceramics at a fast low temperature as defined in claim 1, wherein: and (4) continuing stirring for 2 hours.
6. A method for preparing dense TiC ceramics at a fast low temperature as defined in claim 1, wherein: in the step (6), the mixture is sieved by a 60-mesh sieve.
7. A method for preparing dense TiC ceramics at a fast low temperature as defined in claim 1, wherein: in the step (1), 1 to 15wt% of Al is weighed after conversion 2 O 3 Is prepared from aluminum nitrate powder.
8. The method for preparing dense TiC ceramic at a rapid low temperature according to claim 1, comprising the steps of:
(1) Firstly, 10wt% of Al after conversion is weighed 2 O 3 Pouring the pure aluminum nitrate powder into a beaker containing deionized water, and uniformly performing ultrasonic dispersion for 20min;
(2) Weighing 10g of TiC powder, pouring the powder into another beaker containing deionized water, and uniformly performing ultrasonic dispersion for 20min;
(3) Then, slowly pouring the aluminum nitrate solution into the TiC suspension and continuing magnetic stirring;
(4) Finally, ammonia water is slowly added into the TiC suspension in a spray manner, and the pH value of the TiC suspension is regulated and controlled to be about 9.0;
(5) Continuously magnetically stirring the suspension with the pH value adjusted for 2 hours to ensure the full progress of precipitation reaction;
(6) Finally, the suspension liquid with complete precipitation is dried in a vacuum rotary mode;
(7) Sieving the dried powder with a 60-mesh sieve, weighing 2g of the powder, putting the powder into a graphite grinding tool with the diameter of 20mm, and performing densification sintering by utilizing an SPS technology;
(8) The two-step sintering method is adopted to raise the temperature from room temperature to 1000 ℃ by adopting 30MPa pressure, then gradually increasing the temperature to 50MPa, quickly reducing the temperature to 1400 ℃ after the sintering temperature is raised to the highest temperature of 1500 ℃, and then preserving the heat for 5min.
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| CN1377852A (en) * | 2001-03-30 | 2002-11-06 | 中国科学院化工冶金研究所 | Al2O3-titanium carbide base nano composite ceramic and its preparing method |
| CN103820695A (en) * | 2014-03-19 | 2014-05-28 | 成都理工大学 | Method for preparing Al2O3/TiC coating hard alloy based on liquid phase sintering process |
| CN112111664A (en) * | 2020-09-16 | 2020-12-22 | 西安建筑科技大学 | Two-step sintering method for preparing chemically modified titanium-based composite material and preparation method thereof |
| FR3099154A1 (en) * | 2019-07-26 | 2021-01-29 | Industries Micromecaniques Internationales (Imi) | Dense part in ternary ceramic-ceramic composite material and its manufacturing process |
| CN114591084A (en) * | 2022-02-17 | 2022-06-07 | 惠州学院 | Method for preparing compact TiC ceramic at low temperature rapidly |
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| CN1377852A (en) * | 2001-03-30 | 2002-11-06 | 中国科学院化工冶金研究所 | Al2O3-titanium carbide base nano composite ceramic and its preparing method |
| CN103820695A (en) * | 2014-03-19 | 2014-05-28 | 成都理工大学 | Method for preparing Al2O3/TiC coating hard alloy based on liquid phase sintering process |
| FR3099154A1 (en) * | 2019-07-26 | 2021-01-29 | Industries Micromecaniques Internationales (Imi) | Dense part in ternary ceramic-ceramic composite material and its manufacturing process |
| CN112111664A (en) * | 2020-09-16 | 2020-12-22 | 西安建筑科技大学 | Two-step sintering method for preparing chemically modified titanium-based composite material and preparation method thereof |
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