CN112266251B - Preparation method of silicon nitride/titanium carbide ceramic material based on spark plasma sintering - Google Patents

Preparation method of silicon nitride/titanium carbide ceramic material based on spark plasma sintering Download PDF

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CN112266251B
CN112266251B CN202011180494.8A CN202011180494A CN112266251B CN 112266251 B CN112266251 B CN 112266251B CN 202011180494 A CN202011180494 A CN 202011180494A CN 112266251 B CN112266251 B CN 112266251B
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ceramic material
sintering
plasma sintering
powder
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CN112266251A (en
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肖光春
张帅
陈照强
许崇海
衣明东
张静婕
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Qilu University of Technology
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Abstract

The invention particularly relates to a preparation method of a silicon nitride/titanium carbide ceramic material based on spark plasma sintering. Silicon nitride-based ceramic materialThe material has good mechanical property and stability, and can prepare Si with high performance 3 N 4 The SiC ceramic material is expected to be widely applied in the industrial field. The invention provides Si based on spark plasma sintering 3 N 4 Preparation method of TiC ceramic material by alpha-Si 3 N 4 TiC is the reinforcing phase, al 2 O 3 And Y 2 O 3 The sintering aid is prepared by wet ball milling, mixing and drying, and then discharge plasma sintering is carried out at 1650-1750 ℃ for 20-35min. Si prepared by the invention 3 N 4 The TiC ceramic material has good sintering compactness, and the bending strength, fracture toughness and hardness of the ceramic material are not lower than 700MPa and 6.1MPa.m 1/2 ，13GPa。

Description

Preparation method of silicon nitride/titanium carbide ceramic material based on spark plasma sintering
Technical Field
The invention belongs to the technical field of ceramic material preparation, and in particular relates to a silicon nitride/titanium carbide (Si) based on spark plasma sintering 3 N 4 Preparation method of/TiC) ceramic material and Si prepared by method 3 N 4 TiC ceramic material and application thereof.
Background
The disclosure of this background section is only intended to increase the understanding of the general background of the invention and is not necessarily to be construed as an admission or any form of suggestion that this information forms the prior art already known to those of ordinary skill in the art.
As the most popular ultra-fast sintering technique at present, spark Plasma Sintering (SPS) is used to prepare nanostructured materials, amorphous materials, intermetallic compounds, metal matrices and ceramic matrix composites. Compared with the traditional sintering mode, the Spark Plasma Sintering (SPS) technology has a faster heating speed, and can achieve the same sintering effect in a shorter sintering time. The rapid heating of Spark Plasma Sintering (SPS) prepared materials is due to the skin effect of the dc and ac components of the pulsed current, and the small thermal capacity of the heating system. During sintering, most of heat is generated by the inner edge of the die, and the higher the temperature is, the higher the temperature of the powder surface is. In Spark Plasma Sintering (SPS) the powder is placed in a graphite die and an electric current is passed through the die and sample (if the latter is a conductive material) to heat the powder body while applying pressure to the powder, and if the powder is a non-conductive material, the electric current flows mainly through the die to generate heat. In addition to the fact that the nanomaterial with no significant grain growth can be successfully prepared due to the lower sintering temperature and shorter sintering time, the SPS process has the following advantages in preparing ceramic materials due to its unique heating system: can clean grain boundary, can obviously increase superplasticity, reduce grain boundary segregation, enhance bonding quality, improve thermoelectric performance and improve ductility of alloy ceramics.
The silicon nitride-based ceramic material has higher fracture toughness and strength and excellent thermal shock resistance, corrosion resistance and wear resistance, and has wide application in the industrial field. Thus, many researchers focused their light on how to prepare high performance Si using a suitable sintering process 3 N 4 A base ceramic material. The conventional sintering modes for sintering the silicon nitride ceramic material at present are as follows: pressureless sintering, reaction sintering, gas Pressure Sintering (GPS), hot isostatic pressing sintering (HIP), and Hot Pressing (HP) sintering. Chinese patent CN 109516814A discloses a kind of Si 3 N 4 SiC complex phase ceramic material and preparation method thereof, si 3 N 4 The SiC complex phase ceramic material is Si 3 N 4 And SiC as raw material powder, tm 2 O 3 And MgO as a sintering aid, and is prepared by hot-press sintering. Although the method obtains Si with high density 3 N 4 SiC ceramic material, but the sintering time is long.
Disclosure of Invention
Against the background of the above research, the inventors believe that providing a preparation method with higher sintering efficiency is advantageous for improving Si 3 N 4 The production capacity of the SiC ceramic material and the spark plasma sintering are characterized by sintering in the pressurizing process, and the pulseThe plasma generated by the current and the pressurization during sintering are beneficial to reducing the sintering temperature of the powder. Meanwhile, the characteristics of low voltage and high current can enable the powder to be sintered and compacted rapidly. The invention applies it to Si 3 N 4 Sintering of SiC ceramic material, which is successful in shortening the sintering time to half of the pressure sintering time, in addition, the Si prepared by sintering by the method provided by the invention 3 N 4 The SiC ceramic material also has excellent mechanical properties.
Based on the technical effects, the invention provides the following technical scheme:
in a first aspect of the invention, there is provided Si based on spark plasma sintering 3 N 4 A method for preparing a TiC ceramic material, the method comprising: with Si 3 N 4 TiC is the reinforcing phase, al 2 O 3 And Y 2 O 3 The sintering aid is prepared by mixing the raw materials through wet ball milling and sintering discharge plasma.
After sintering by spark plasma, the Si 3 N 4 The preparation time of the TiC ceramic material is obviously shortened, the invention provides a corresponding temperature-rising sintering program aiming at spark plasma sintering, and the detection result shows that the sintering method provided by the invention can inhibit beta-Si 3 N 4 Increasing the ratio of alpha crystalline phases in the sintered product due to overgrowth of alpha Si 3 N 4 The crystal phase has higher strength, and the ceramic material prepared by the method is more suitable for preparing cutting tools, in particular for preparing ceramic cutters. And the introduction of TiC can better improve Si 3 N 4 Is used for the electric conduction and electric spark machining.
The beneficial effects of the above technical scheme are:
the preparation process is simple, the sintering time is short, and Si can be completed in a short time 3 N 4 Sintering of TiC ceramic material. Compared with hot press sintering, the spark plasma sintering takes only 1/2 of the time of hot press sintering. And Si prepared by the invention 3 N 4 Mechanical properties of TiC ceramic materialsExcellent performance, bending strength, fracture toughness and Vickers hardness can be achieved, and meanwhile, due to the unique sintering mechanism of SPS, beta-Si is inhibited 3 N 4 Is free of large beta-Si 3 N 4 This is for Si 3 N 4 The properties of the/TiC ceramic material are beneficial.
Drawings
The accompanying drawings, which are included to provide a further understanding of the invention and are incorporated in and constitute a part of this specification, illustrate embodiments of the invention and together with the description serve to explain the invention.
FIG. 1 shows Si prepared in example 1 3 N 4 Graph of sintering temperature and displacement of upper pressure head in spark plasma sintering process when TiC ceramic material;
FIG. 2 shows Si prepared in example 1 3 N 4 XRD detection pattern of TiC ceramic material;
FIG. 3 is Si prepared in example 1 3 N 4 SEM image of fracture surface of TiC ceramic material.
Detailed Description
It should be noted that the following detailed description is illustrative and is intended to provide further explanation of the invention. Unless defined otherwise, all technical and scientific terms used herein have the same meaning as commonly understood by one of ordinary skill in the art to which this invention belongs.
It is noted that the terminology used herein is for the purpose of describing particular embodiments only and is not intended to be limiting of exemplary embodiments according to the present invention. As used herein, the singular is also intended to include the plural unless the context clearly indicates otherwise, and furthermore, it is to be understood that the terms "comprises" and/or "comprising" when used in this specification are taken to specify the presence of stated features, steps, operations, devices, components, and/or combinations thereof.
As described in the background art, for the prior art Si with high density 3 N 4 And the SiC ceramic material has longer sintering time and low production efficiency. In order to solve the technical problemsThe invention provides Si based on spark plasma sintering 3 N 4 The preparation method of the TiC ceramic material shortens the hot-press sintering time by 1/2 compared with the prior method, and Si prepared by the method 3 N 4 The TiC ceramic has good mechanical properties.
In a first aspect of the invention, there is provided Si based on spark plasma sintering 3 N 4 A method for preparing a TiC ceramic material, the method comprising: with Si 3 N 4 TiC is the reinforcing phase, al 2 O 3 And Y 2 O 3 The sintering aid is prepared by mixing the raw materials through wet ball milling and sintering discharge plasma.
Preferably, in the preparation method, the volume percentage of the raw materials is as follows: alpha-Si 3 N 4 70-85％，TiC 5-15％，Al 2 O 3 1-6％，Y 2 O 3 3-7％。
Further, the volume percentage of TiC is 7-10%, or the Al 2 O 3 Is 2-4% by volume, or Y 2 O 3 The volume percentage of the raw materials is 4-6%, the raw materials are adjusted within the volume percentage range, and the sum of the other components is 100%.
In some embodiments of the above preferred technical solutions, the volume percentages of the raw materials are as follows: alpha-Si 3 N 4 80％，TiC 10％，Al 2 O 3 4％，Y 2 O 3 6％。
In some embodiments of the above preferred technical solutions, the volume percentages of the raw materials are as follows: alpha-Si 3 N 4 82％，TiC 10％，Al 2 O 3 3％，Y 2 O 3 5％。
In some embodiments of the above preferred technical solutions, the volume percentages of the raw materials are as follows: alpha-Si 3 N 4 75％，TiC 15％，Al 2 O 3 4％，Y 2 O 3 6％。
Preferably, the alpha-Si 3 N 4 The average particle size of the powder is 0.5-1 μm.
Preferably, the TiC powder has an average particle size of 0.5-1 μm.
Preferably, the Al 2 O 3 The average particle size of the powder is 0.5-2 μm.
Preferably, said Y 2 O 3 The average particle size of the powder is 0.1-0.5 μm.
Preferably, the preparation method specifically comprises the following steps:
(1) By reacting alpha-Si 3 N 4 TiC powder is respectively added into the dispersion medium to be uniformly dispersed to obtain alpha-Si 3 N 4 Mixing the suspension and TiC suspension to obtain a complex phase suspension;
(2) Weighing alpha-Si 3 N 4 Dispersing agent 1-5wt%, adding into dispersing medium to dissolve, adding dispersing agent solution into the above-mentioned complex phase suspension, adding Al 2 O 3 And Y 2 O 3 The powder is uniformly dispersed to obtain a mixed system;
(3) Transferring the mixed system obtained in the step (2) into a ball milling tank for ball milling; drying the ball milling liquid after finishing, and sieving to obtain mixed powder;
(4) And (3) filling the mixed powder in the step (3) into a mould for molding, and then performing spark plasma sintering.
Further, in the step (1) or (2), the dispersion medium may include, but is not limited to, absolute ethanol or absolute methanol.
Further, in the step (2), the dispersing agent includes, but is not limited to, polyethylene glycol, specifically polyethylene glycol 6000.
Further, in the step (3), ball milling balls are added according to the ball material weight ratio of 10:0.5-1.5, and ball milling is carried out for 40-50 hours under the protection atmosphere; specifically, the protective atmosphere is nitrogen.
Further, in the step (3), the ball grinding balls are cemented carbide balls YG6 or YG8.
Further, in the step (3), the ball milling solution is dried by one of, but not limited to, normal pressure drying, vacuum drying, spray drying or freeze drying.
In a specific embodiment, the drying is vacuum drying, and the drying is performed at 80-120 ℃ for 12-24 hours.
Further, in the step (3), the ball milling liquid is dried and then sieved by a 100-120 mesh sieve, so as to obtain mixed powder.
Further, in the step (4), the spark plasma sintering parameter is as follows: rate of temperature rise: before 1300 ℃,90-110 ℃/min, which is higher than 1300 ℃,30-50 ℃/min; sintering temperature is 1650-1750 ℃; the heat preservation time is 20-35min, and the heat preservation is 10-17min after the temperature reaches 1600 ℃ and the sintering temperature respectively; the axial pressure is 25-35MPa.
In a specific embodiment of the foregoing preferred technical solution, the preparation method includes the following steps:
(1) Weighing alpha-Si according to a proportion 3 N 4 Respectively adding proper amount of absolute ethyl alcohol as dispersion medium into TiC powder, performing ultrasonic dispersion, and mechanically stirring for 10-20min to obtain alpha-Si 3 N 4 Mixing the suspension and TiC suspension to obtain a complex-phase suspension;
(2) Weighing alpha-Si 3 N 4 1-5wt% of polyethylene glycol 6000 is dissolved in absolute ethanol and added into the complex phase suspension, and then Al is added according to the proportion 2 O 3 And Y 2 O 3 Dispersing the powder by ultrasonic and mechanically stirring for 30-50min;
(3) Pouring the final suspension obtained in the step (2) into a ball milling tank, adding ball milling balls according to the weight ratio of ball materials of 10:1, performing ball milling for 48 hours under a protective atmosphere, drying the ball milling liquid at 80-120 ℃ for 12-24 hours in a vacuum drying oven, sieving through a 100-120 mesh sieve to obtain mixed powder, and sealing and preserving for later use;
(4) And (3) filling the mixed powder obtained in the step (3) into a graphite mold, cold-pressing and molding, and then putting into a discharge plasma sintering furnace for sintering.
In a second aspect of the invention, there is provided Si based on spark plasma sintering as described in the first aspect 3 N 4 Si prepared by preparation method of TiC ceramic material 3 N 4 TiC ceramicPorcelain material.
In a third aspect of the present invention, there is provided Si as described in the first aspect 3 N 4 The TiC ceramic material is applied to the fields of cutting tools, wear-resistant parts, inserts, aviation industry products and the like.
In order to make the technical solution of the present invention more clearly known to those skilled in the art, the technical solution of the present invention will be described in detail with reference to specific examples, and the raw materials involved in the following examples are all commercially available products.
Example 1
Si based on Spark Plasma Sintering (SPS) 3 N 4 Preparation method of TiC ceramic material, the volume percentage of the raw material components is alpha-Si 3 N 4 82％，TiC 10％，Al 2 O 3 3％，Y 2 O 3 5％。
Weighing alpha-Si according to a proportion 3 N 4 Respectively adding proper amount of absolute ethyl alcohol as a dispersion medium into TiC powder, performing ultrasonic dispersion and mechanical stirring for 15min to obtain alpha-Si 3 N 4 A suspension, tiC suspension; mixing the two suspensions to obtain a complex phase suspension. Weighing Si 3 N 4 Polyethylene glycol 6000 accounting for 3 weight percent of the powder is dissolved by absolute ethyl alcohol and added into the complex phase suspension, and then Al is added according to the proportion 2 O 3 And Y 2 O 3 Dispersing the powder by ultrasonic and mechanically stirring for 45min; and pouring the obtained final suspension into a ball milling tank, adding ball milling balls according to the ball weight ratio of 10:1, and performing ball milling for 48 hours in a nitrogen atmosphere.
Drying the obtained ball milling liquid for 12 hours at 110 ℃ in a vacuum drying oven, sieving through a 100-mesh sieve to obtain mixed powder, filling the obtained mixed powder into a graphite mold, and placing the graphite mold into a discharge plasma sintering furnace for hot-press sintering after cold press molding; spark plasma sintering parameters: 100 ℃/min before 1300 ℃; 1300-1450 ℃ 50 ℃/min; 30 ℃/min at 1450-1600 ℃; preserving heat at 1600 ℃ for 15min; 30 ℃/min at 1600 ℃ to 1700 ℃; preserving heat at 1700 ℃ for 10min; the pressure is 30MPa.
The ceramic material prepared in this example was cut into pieces of 3 mm. Times.4 mm. Times.35 mmStandard strip samples, then the bars were subjected to rough grinding, lapping, chamfering, and polishing. The mechanical property test shows that the flexural strength of the material is 959MPa, the hardness is 15.21GPa, and the fracture toughness is 8.61 MPa.M 1/2 . From FIG. 1, it can be seen that spark plasma sintering Si 3 N 4 Densification and crystal growth of ceramic materials. Before 1200 ℃, the powder is heated and expanded, the lower pressing head moves downwards, and the Z-axis displacement is reduced. Densification occurs after 1200 c, at which point the hold-down head is moved up and the Z-axis displacement is increased. When the temperature reaches 1700 ℃, the crystal starts to grow, the ceramic material starts to expand, and the Z-axis displacement is reduced. From FIG. 2, it can be found that Si after sintering 3 N 4 The phase composition of the TiC ceramic material is beta-Si 3 N 4 、TiC 0.3 N 0.7 And a small amount of alpha-Si 3 N 4 Wherein TiC0.3N0.7 is mainly due to Si during sintering 3 N 4 And TiC. And it can be found from fig. 2 that the crystallinity of each of the ceramic materials is good. FIG. 3 shows Si 3 N 4 SEM image of fracture surface of TiC ceramic material shows homogeneous crystal grain and no larger beta-Si 3 N 4 And the compactness is good, no obvious air holes are found, and the ceramic material has excellent mechanical properties.
Example 2
Si based on Spark Plasma Sintering (SPS) 3 N 4 Preparation method of TiC ceramic material, the volume percentage of the raw material components is alpha-Si 3 N 4 82％，TiC 10％，Al 2 O 3 3％，Y 2 O 3 5％。
Weighing alpha-Si according to a proportion 3 N 4 TiC powder is respectively added with proper amount of absolute ethyl alcohol as a dispersion medium, and is subjected to ultrasonic dispersion and mechanical stirring for 15min to prepare alpha-Si 3 N 4 A suspension, tiC suspension; mixing the three suspensions to obtain a complex phase suspension. Weighing Si 3 N 4 Dispersing agent with 3wt% of powder weight, dissolving with absolute ethyl alcohol, adding into complex phase suspension, and proportionally adding Al 2 O 3 And Y 2 O 3 Dispersing the powder by ultrasonic and mechanically stirring for 45min; and pouring the obtained final suspension into a ball milling tank, adding ball milling balls according to the ball weight ratio of 10:1, and performing ball milling for 48 hours in a nitrogen atmosphere.
Drying the obtained ball milling liquid for 12 hours at 110 ℃ in a vacuum drying oven, sieving through a 100-mesh sieve to obtain mixed powder, filling the obtained mixed powder into a graphite mold, and placing the graphite mold into a discharge plasma sintering furnace for hot-press sintering after cold press molding; spark plasma sintering parameters: 100 ℃/min before 1300 ℃; 1300-1450 ℃ 50 ℃/min; 30 ℃/min at 1450-1600 ℃; preserving heat at 1600 ℃ for 15min; 30 ℃/min at 1600 ℃ to 1650 ℃; preserving heat at 1650 ℃ for 10min; the pressure is 30MPa.
The ceramic material prepared in this example was cut into standard strip-like test pieces of 3mm×4mm×35mm, and then the bars were subjected to rough grinding, lapping, chamfering, and polishing. The mechanical property test is carried out on the material, and the result shows that the bending strength of the material is 768MPa, the hardness is 15.81GPa, and the fracture toughness is 6.19 MPa.M 1/2 . And the introduction of TiC can better improve Si 3 N 4 Is used for the electric conduction and electric spark machining.
Example 3
Si based on Spark Plasma Sintering (SPS) 3 N 4 Preparation method of TiC ceramic material, the volume percentage of the raw material components is alpha-Si 3 N 4 82％，TiC 10％，Al 2 O 3 3％，Y 2 O 3 5％。
Weighing alpha-Si according to a proportion 3 N 4 TiC powder is respectively added with proper amount of absolute ethyl alcohol as a dispersion medium, and is subjected to ultrasonic dispersion and mechanical stirring for 15min to prepare alpha-Si 3 N 4 A suspension, tiC suspension; mixing the three suspensions to obtain a complex phase suspension. Weighing Si 3 N 4 Dispersing agent with 3wt% of powder weight, dissolving with absolute ethyl alcohol, adding into complex phase suspension, and proportionally adding Al 2 O 3 And Y 2 O 3 Dispersing the powder by ultrasonic and mechanically stirring for 45min; pouring the obtained final suspension into a ball milling tank, adding ball milling balls according to the ball weight ratio of 10:1, and adding nitrogenBall milling is carried out for 48 hours under the gas atmosphere.
Drying the obtained ball milling liquid for 12 hours at 110 ℃ in a vacuum drying oven, sieving through a 100-mesh sieve to obtain mixed powder, filling the obtained mixed powder into a graphite mold, and placing the graphite mold into a discharge plasma sintering furnace for hot-press sintering after cold press molding; spark plasma sintering parameters: 100 ℃/min before 1300 ℃; 1300-1450 ℃ 50 ℃/min; 30 ℃/min at 1450-1600 ℃; preserving heat at 1600 ℃ for 15min; 30 ℃/min at 1600 ℃ to 1700 ℃; preserving heat at 1700 ℃ for 15min; the pressure is 30MPa.
The ceramic material prepared in this example was cut into standard strip-like test pieces of 3mm×4mm×35mm, and then the bars were subjected to rough grinding, lapping, chamfering, and polishing. The mechanical property test is carried out on the material, and the result shows that the flexural strength of the material is 886MPa, the hardness is 13.73GPa, and the fracture toughness is 7.85 MPa.M 1/2 。
Example 4
Si based on Spark Plasma Sintering (SPS) 3 N 4 Preparation method of TiC ceramic material, the volume percentage of the raw material components is alpha-Si 3 N 4 82％，TiC 10％，Al 2 O 3 4％，Y 2 O 3 6％。
Weighing alpha-Si according to a proportion 3 N 4 TiC powder is respectively added with proper amount of absolute ethyl alcohol as a dispersion medium, and is subjected to ultrasonic dispersion and mechanical stirring for 15min to prepare alpha-Si 3 N 4 A suspension, tiC suspension; mixing the three suspensions to obtain a complex phase suspension. Weighing Si 3 N 4 Dispersing agent with 3wt% of powder weight, dissolving with absolute ethyl alcohol, adding into complex phase suspension, and proportionally adding Al 2 O 3 And Y 2 O 3 Dispersing the powder by ultrasonic and mechanically stirring for 45min; pouring the obtained final suspension into a ball milling tank, adding ball milling balls according to the ball material weight ratio of 10:1, and performing ball milling for 48 hours in a nitrogen atmosphere;
drying the obtained ball milling liquid for 12 hours at 110 ℃ in a vacuum drying oven, sieving through a 100-mesh sieve to obtain mixed powder, filling the obtained mixed powder into a graphite mold, and placing the graphite mold into a discharge plasma sintering furnace for hot-press sintering after cold press molding; spark plasma sintering parameters: 100 ℃/min before 1300 ℃; 1300-1450 ℃ 50 ℃/min; 30 ℃/min at 1450-1600 ℃; preserving heat at 1600 ℃ for 15min; 30 ℃/min at 1600 ℃ to 1700 ℃; preserving heat at 1700 ℃ for 10min; the pressure is 30MPa.
The ceramic material prepared in this example was cut into standard strip-like test pieces of 3mm×4mm×35mm, and then the bars were subjected to rough grinding, lapping, chamfering, and polishing. The mechanical property test is carried out on the material, and the result shows that the bending strength of the material is 891MPa, the hardness is 13.21GPa, and the fracture toughness is 8.37 MPa.M 1/2 。
Example 5
Si based on Spark Plasma Sintering (SPS) 3 N 4 Preparation method of TiC ceramic material, the volume percentage of the raw material components is alpha-Si 3 N 4 82％，TiC 10％，Al 2 O 3 3％，Y 2 O 3 5％。
Weighing alpha-Si according to a proportion 3 N 4 TiC powder is respectively added with proper amount of absolute ethyl alcohol as a dispersion medium, and is subjected to ultrasonic dispersion and mechanical stirring for 15min to prepare alpha-Si 3 N 4 A suspension, tiC suspension; mixing the three suspensions to obtain a complex phase suspension. Weighing Si 3 N 4 Dispersing agent with 3wt% of powder weight, dissolving with absolute ethyl alcohol, adding into complex phase suspension, and proportionally adding Al 2 O 3 And Y 2 O 3 Dispersing the powder by ultrasonic and mechanically stirring for 45min; and pouring the obtained final suspension into a ball milling tank, adding ball milling balls according to the ball weight ratio of 10:1, and performing ball milling for 48 hours in a nitrogen atmosphere.
Drying the obtained ball milling liquid for 12 hours at 110 ℃ in a vacuum drying oven, sieving through a 100-mesh sieve to obtain mixed powder, filling the obtained mixed powder into a graphite mold, and placing the graphite mold into a discharge plasma sintering furnace for hot-press sintering after cold press molding; spark plasma sintering parameters: 100 ℃/min before 1300 ℃; 1300-1450 ℃ 50 ℃/min; 30 ℃/min at 1450-1600 ℃; preserving heat at 1600 ℃ for 15min; 30 ℃/min at 1600 ℃ to 1700 ℃; preserving heat at 1700 ℃ for 10min; the pressure is 40MPa.
Will implement the present embodimentThe ceramic material prepared in the example was cut into standard bar-shaped test pieces of 3mm×4mm×35mm, and then the bars were subjected to rough grinding, chamfering, and polishing. The mechanical property test is carried out on the material, and the result shows that the flexural strength of the material is 801MPa, the hardness is 14.63GPa, and the fracture toughness is 7.26 MPa.M 1/2 。
The above description is only of the preferred embodiments of the present invention and is not intended to limit the present invention, but various modifications and variations can be made to the present invention by those skilled in the art. Any modification, equivalent replacement, improvement, etc. made within the spirit and principle of the present invention should be included in the protection scope of the present invention.

Claims (3)

1. Si based on spark plasma sintering 3 N 4 The preparation method of the TiC ceramic material is characterized by comprising the following steps: with Si 3 N 4 TiC is the reinforcing phase, al 2 O 3 And Y 2 O 3 The volume percentage of raw materials used as sintering auxiliary agent is as follows: alpha-Si 3 N 4 82%，TiC 10%，Al 2 O 3 3%，Y 2 O 3 5%；
The preparation method specifically comprises the following steps:
weighing alpha-Si according to a proportion 3 N 4 Respectively adding proper amount of absolute ethyl alcohol as a dispersion medium into TiC powder, performing ultrasonic dispersion and mechanical stirring for 15min to obtain alpha-Si 3 N 4 A suspension, tiC suspension; mixing the two suspensions to obtain a complex phase suspension; weighing Si 3 N 4 Polyethylene glycol 6000 accounting for 3 weight percent of the powder is dissolved by absolute ethyl alcohol and added into the complex phase suspension, and then Al is added according to the proportion 2 O 3 And Y 2 O 3 Dispersing the powder by ultrasonic and mechanically stirring for 45min; pouring the obtained final suspension into a ball milling tank, adding ball milling balls according to the ball material weight ratio of 10:1, and performing ball milling for 48 hours in a nitrogen atmosphere;
drying the obtained ball milling liquid for 12 hours at 110 ℃ in a vacuum drying oven, sieving through a 100-mesh sieve to obtain mixed powder, filling the obtained mixed powder into a graphite mold, and placing the graphite mold into a discharge plasma sintering furnace for hot-press sintering after cold press molding; spark plasma sintering parameters: 100 ℃/min before 1300 ℃; 1300-1450 ℃ 50 ℃/min; 30 ℃/min at 1450-1600 ℃; preserving heat at 1600 ℃ for 15min; 30 ℃/min at 1600 ℃ to 1700 ℃; preserving heat at 1700 ℃ for 10min; the pressure is 30MPa.
2. Si based on spark plasma sintering as claimed in claim 1 3 N 4 Si prepared by preparation method of TiC ceramic material 3 N 4 TiC ceramic material.
3. Si according to claim 2 3 N 4 The TiC ceramic material is applied to the fields of production of cutting tools, wear-resistant parts, inserts and products for aviation industry.
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