Method for producing zirconia-titanium carbide / zirconia co-fired ceramic composite

Abstract

A preparation method of a zirconia-titanium carbide / zirconia co-fired ceramic composite material is carried out in the following steps: (1) preparing Y2O3 stabilized nano ZrO2 powder and micron TiC powder as raw materials; ball milling to obtain ball-milled wet material; (2) drying, grinding and crushing to prepare powder; (3) adding polyvinyl alcohol aqueous solution dropwise, stirring and mixing, and sieving; (4) after standing, the TiC / ZrO2 round blank is prepared by dry pressing into a core mold; (5) the Y2O3 stabilized nano ZrO2 powder is prepared into granulated powder by a spray granulation method; (6) the granulated powder and the TiC / ZrO2 round blank are combined by using an external mold; (7) the composite round blank is prepared by dry pressing; and (8) after drying, pressureless sintering is carried out. The ZrO2-TiC / ZrO2 co-fired ceramic composite material has good electrical and mechanical properties, can be better applied to wearable smart products, has good interface bonding strength, and meets the requirements of different parts of ceramic materials suitable for different applications.

Description

TECHNICAL FIELD

[0001] The application belongs to the technical field of materials, and particularly relates to a preparation method of a zirconia-titanium carbide / zirconia co-fired ceramic composite material. BACKGROUND

[0002] With the development of modern high-tech and emerging industries, advanced ceramics have gradually become an important part of new materials due to their excellent physical and chemical properties such as high strength, high temperature resistance, wear resistance, corrosion resistance, and are widely used in aerospace, biomedicine, national defense industry, computers and microelectronics and other high-tech fields. Due to the high brittleness, high hardness and poor machinability of ceramics, it is difficult to process ceramics into large and complex parts, thereby limiting the application of ceramics. In order to solve this problem, ceramic joining technology emerges as the times require. By connecting ceramics with different properties or properties together, different parts of the ceramic joining material can be adapted to different application requirements, further expanding the application range of ceramics.

[0003] Non-patent document 1 recorded in International Ceramics, Volume 30, Issue 6, pages 823-827, uses a mixed powder slurry composed of CePO4 and ZrO2 to connect ZrO2 ceramics and 25vol.% CePO4 / ZrO2 ceramic green bodies under pressureless conditions to realize integrated sintering. The joint is denser than the matrix, has fewer defects, cracks and pores, and the bending strength reaches 414MPa, greatly improving the performance of the ceramic.

[0004] Patent document 2 "Ceramic connecting piece and preparation method and application thereof" (publication number CN112062590A) uses Re2O3, Al2O3 and SiC (Si3N4) to prepare a connecting material to form a sandwich structure with SiC or Si3N4 ceramic, and obtain a ceramic connecting piece with good high temperature resistance and corrosion resistance. In addition, patent document 3 "Process for connecting LaCrO3 ceramic with ZrB2 composite intermediate layer" (publication number CN113563098A) uses LaCrO3 ceramic base material and ZrB2, Al powder, and polyvinyl alcohol solution to prepare an intermediate connecting layer round sheet for connection and sintering, and the obtained LaCrO3 ceramic connecting piece joint has a bending strength of 23.79MPa, and the highest Vickers hardness of the intermediate connection is 7.01GPa.

[0005] In foreign research, patent document 4 "Production method of ceramic connection member" (publication number TW201202171 (A)) provides a manufacturing method of ceramic connection member, dispersing carbon particles in organic solvent, forming particle layer after drying, introducing free silicon into particle layer to form connection layer containing at least silicon carbide, which can prevent cracks caused by thermal shrinkage of connection layer in heat treatment process.

[0006] Patent document 5 "Ceramic connection body, method of connecting the ceramic bodies, and ceramic structural body" (publication number US2004175549) proposes a ceramic connection method by forming coarse pores with an average diameter greater than the average particle diameter of the ceramic body and a size not exceeding 2000 μm in the bonding interface between one ceramic body and another ceramic body, which can be effectively used for ceramic joints in semiconductor production and the like.

[0007] Although the co-fired ceramic composite material prepared by the heterogeneous ceramic connection technology has simple preparation process and low cost, it also has some defects; first, the difference in particle size and growth habit of the two ceramics is not conducive to the formation of a dense interface layer; second, the inconsistent sintering shrinkage, thermal expansion coefficient and elastic modulus will cause interface stress, which is not conducive to connection; finally, the inconsistency of sintering temperature range will limit the connection system or initial particle size, so that the prepared ceramic is difficult to achieve the expected excellent mechanical properties or electrical properties. SUMMARY

[0008] The purpose of the present application is to provide a preparation method of zirconia-titanium carbide / zirconia co-fired ceramic composite material, which has the characteristics of external insulation and central conductivity, and can meet the actual application requirements of different parts of the material having different conductivity.

[0009] The method of the present application is carried out in the following steps:

[0010] (1) Prepare Y2O3 stabilized nano-ZrO2 powder and micron TiC powder as raw materials; put the raw materials into a ball mill tank, add anhydrous ethanol as a ball milling medium, and put it into a grinding ball for ball milling to obtain a ball milling wet material;

[0011] (2) Dry the ball milling wet material to remove the ball milling medium to make dry material; grind and crush the dry material to make powder;

[0012] (3) Add polyvinyl alcohol aqueous solution to the powder, then stir and mix uniformly, and then sieve to obtain granules;

[0013] (4) The granules are placed in a central mold and then dry-pressed to form a TiC / ZrO2 round billet;

[0014] (5) The Y2O3 stabilized nano-ZrO2 powder is granulated by spray granulation to form granulated powder;

[0015] (6) The outer mold is inverted, with the upper punch at the lower part of the mold cavity and the lower punch at the upper part of the mold cavity. The lower punch is removed, and the first part of the granulated powder is placed in the mold cavity. The lower punch is placed down, and the upper surface of the granulated powder in the mold cavity is flattened. The mold cavity is raised so that the bottom of the mold cavity is outside the boss of the upper punch. A round piece with a circular hole is used for positioning, and the TiC / ZrO2 round billet is placed in the middle of the mold cavity. The TiC / ZrO2 round billet is above the first part of the granulated powder. At this time, the top surface of the TiC / ZrO2 round billet is flush with the top surface of the raised mold cavity. The second part of the granulated powder is continuously placed in the mold cavity to fill the gap between the TiC / ZrO2 round billet and the inner wall of the mold cavity. The second part of the granulated powder is scraped flat so that the top surface of the second part of the granulated powder is flush with the top surface of the TiC / ZrO2 round billet and the top surface of the raised mold cavity. The mold cavity is raised again, and at this time, the top surface of the mold cavity is higher than the top surfaces of the TiC / ZrO2 round billet and the second part of the granulated powder. The third part of the granulated powder is placed in the twice-raised mold cavity. The lower punch is covered, and the outer mold is turned over so that the upper punch is at the upper part of the mold cavity and the lower punch is at the lower part of the mold cavity;

[0016] (7) The raw materials in the outer mold are dry-pressed to form a composite round billet;

[0017] (8) The composite round billet is dried to remove moisture, and then pressureless sintering is performed to form a ZrO2-TiC / ZrO2 co-sintered ceramic composite material.

[0018] In the above steps (1) and (5), the mole percentage of Y2O3 in the Y2O3 stabilized nano-ZrO2 powder is 3%.

[0019] In the above steps (1) and (5), the particle size of the Y2O3 stabilized nano-ZrO2 powder is 30-50 nm.

[0020] In the above step (1), the particle size of the micron TiC powder is 0.5-1.0 μm.

[0021] In the above step (1), the ball milling speed is 60-80 r / min, and the ball milling time is 12-15 h.

[0022] In the above step (1), the micron TiC powder accounts for 25-40% of the total mass of the raw materials.

[0023] In the step (1), the material of the grinding ball is ZrO2; the mass ratio of the grinding ball to the raw material is 2:1; the grinding ball is a large ball with a diameter of 10 mm and a small ball with a diameter of 6 mm, and the mass ratio of the large ball to the small ball is 1:1.

[0024] In the step (1), the mass ratio of the anhydrous ethanol to the raw material is 1:1.

[0025] In the step (2), the drying temperature is 80±1℃, and the time is at least 7 h.

[0026] In the step (3), the sieving is sieving through a 60-mesh sieve.

[0027] In the step (3), the polyvinyl alcohol (PVA) aqueous solution is 8-10% of the mass of the powder.

[0028] In the step (4), the granules are placed for at least 12 h.

[0029] In the step (4), the inner diameter of the cavity of the core mold is Φ=8 mm.

[0030] In the step (4), the TiC / ZrO2 round blank is in a cylindrical shape, and the height is 2±0.02 mm.

[0031] In the steps (4) and (7), the dry pressing forming pressure is 50-125 MPa, and the pressure maintaining time is at least 15 s.

[0032] In the step (5), the particle size of the granulated powder is 50-100 μm.

[0033] In the step (6), the first part of the granulated powder accounts for 5 / 13 of the total mass of the entire granulated powder; and the second part of the granulated powder accounts for 3 / 13 of the total mass of the entire granulated powder.

[0034] In the step (6), the inner diameter of the cavity of the outer mold is Φ=30 mm.

[0035] In the step (8), the drying temperature is 80±1℃, and the time is at least 10 h.

[0036] In the step (8), the sintering temperature of the pressureless sintering is 1700±10℃, and the holding time is 120±10 min.

[0037] The ZrO2-TiC / ZrO2 co-sintered ceramic composite material is composed of a core and an outer part to form an integrated structure, the material of the outer part is ZrO2, and the material of the core is TiC / ZrO2.

[0038] The ZrO2-TiC / ZrO2 co-sintered ceramic composite material, the resistivity of the core TiC / ZrO2 is 0.99×10 -5 ~5.38×10-5 Ω·m.

[0039] The ZrO2-TiC / ZrO2 co-fired ceramic composite material has a bending strength of 488.3-557.5 MPa and a compressive strength of 187.8-215 MPa.

[0040] The ZrO2-TiC / ZrO2 co-fired ceramic composite material has a bending strength of 488.3-557.5 MPa and a compressive strength of 187.8-215 MPa.

[0041] The ZrO2-TiC / ZrO2 co-fired ceramic composite material has a bending strength of 488.3-557.5 MPa and a compressive strength of 187.8-215 MPa. BRIEF DESCRIPTION OF DRAWINGS

[0042] Figure 1 The ZrO2-TiC / ZrO2 co-fired ceramic composite material has a bending strength of 488.3-557.5 MPa and a compressive strength of 187.8-215 MPa.

[0043] Figure 2 The ZrO2-TiC / ZrO2 co-fired ceramic composite material has a bending strength of 488.3-557.5 MPa and a compressive strength of 187.8-215 MPa.

[0044] Figure 3 The ZrO2-TiC / ZrO2 co-fired ceramic composite material has a bending strength of 488.3-557.5 MPa and a compressive strength of 187.8-215 MPa.

[0045] Figure 4 The ZrO2-TiC / ZrO2 co-fired ceramic composite material has a bending strength of 488.3-557.5 MPa and a compressive strength of 187.8-215 MPa.

[0046] Figure 5 The ZrO2-TiC / ZrO2 co-fired ceramic composite material has a bending strength of 488.3-557.5 MPa and a compressive strength of 187.8-215 MPa. DETAILED DESCRIPTION

[0047] In the embodiment of the application, when the ball-milled wet material is dried, the drying temperature is 80±1℃, and the time is at least 7h.

[0048] In the embodiment of the present application, the drying temperature of the composite round blank is 80±1℃, and the drying time is at least 10 hours.

[0049] In the embodiment of the present application, the pressureless sintering method is as follows: (a) placing the dried composite round blank in a graphite crucible, and placing the graphite crucible in a plasma sintering furnace, and closing the furnace cover; (b) vacuumizing the plasma sintering furnace to a pressure of-0.10MPa, and starting the sintering furnace; (c) manually controlling the power to heat to 600℃, and then stopping the vacuumizing, and introducing Ar gas into the plasma sintering furnace to increase the pressure in the furnace to 0.08MPa, and then stopping the gas introduction; and then automatically controlling the temperature to increase to 1700±10℃ at a rate of 200℃ / h, and keeping the temperature for 120±10min to perform the pressureless sintering; and (d) cooling the furnace to room temperature.

[0050] In the embodiment of the present application, the dry pressing is performed by using a hydraulic universal testing machine.

[0051] In the embodiment of the present application, the Vickers hardness of the ZrO2-TiC / ZrO2 co-sintered ceramic composite material is 13.5-15.1GPa, and the fracture toughness is 5.35-6.48MPa·m 1 / 2 .

[0052] In the embodiment of the present application, the ball milling tank is a polyethylene ball milling tank.

[0053] In the embodiment of the present application, the ball mill is a GMS1-4 horizontal ball mill.

[0054] Embodiment 1

[0055] The flow is shown in Figure 1 .

[0056] Y2O3 stabilized nano-ZrO2 powder and micron TiC powder are prepared as raw materials; the raw materials are placed in a ball milling tank, anhydrous ethanol is added as a ball milling medium, and grinding balls are placed for ball milling to obtain a ball-milled wet material; the molar percentage of Y2O3 in the Y2O3 stabilized nano-ZrO2 powder is 3%, the particle size of the Y2O3 stabilized nano-ZrO2 powder is 30-50nm, and the particle size of the micron TiC powder is 0.5-1.0μm; the ball milling speed is 60r / min, and the ball milling time is 15h; the micron TiC powder accounts for 40% of the total mass of the raw materials; the grinding balls are made of ZrO2, and the mass ratio of the grinding balls to the raw materials is 2:1; the grinding balls are large balls with a diameter of 10mm and small balls with a diameter of 6mm, and the mass ratio of the large balls to the small balls is 1:1; and the mass ratio of the anhydrous ethanol to the raw materials is 1:1.

[0057] The ball-milled wet material is dried to remove the ball milling medium to form a dry material; and the dry material is ground and crushed to form a powder.

[0058] The polyvinyl alcohol solution is added dropwise into the powder, and then the mixture is stirred and mixed uniformly, and then is passed through a 60-mesh sieve to obtain the granules; the polyvinyl alcohol (PVA) solution is 8% of the mass of the powder;

[0059] The granules are allowed to stand for at least 12 hours, and then are loaded into a core mold to be dry-pressed to form a TiC / ZrO2 round billet; the inner diameter of the mold cavity of the core mold is Φ = 8 mm; the TiC / ZrO2 round billet is cylindrical, with a height of 2 ± 0.02 mm; the dry-pressing pressure is 50 MPa, and the pressure holding time is 30 s.

[0060] The Y2O3-stabilized nano-ZrO2 powder is granulated by a spray granulation method to form a granulated powder; the molar percentage of Y2O3 in the Y2O3-stabilized nano-ZrO2 powder is 3%; the particle size of the Y2O3-stabilized nano-ZrO2 powder is 30-50 nm, and the particle size of the granulated powder is 50-100 μm;

[0061] The outer mold is inverted, with the upper punch at the lower part of the mold cavity and the lower punch at the upper part of the mold cavity; the lower punch is removed, and the first portion of the granulated powder is loaded into the mold cavity, and the lower punch is then put down to flatten the upper surface of the granulated powder in the mold cavity; the mold cavity is raised so that the bottom of the mold cavity is located outside the boss of the upper punch, and a circular sheet with a circular hole in the center is used for positioning; the TiC / ZrO2 round billet is placed in the middle of the mold cavity, with the TiC / ZrO2 round billet located above the first portion of the granulated powder, and the top surface of the TiC / ZrO2 round billet is flush with the top surface of the raised mold cavity; the second portion of the granulated powder is continuously loaded into the mold cavity to fill the gap between the TiC / ZrO2 round billet and the inner wall of the mold cavity, and the second portion of the granulated powder is scraped flat so that the top surface of the second portion of the granulated powder is flush with the top surfaces of the TiC / ZrO2 round billet and the raised mold cavity; the mold cavity is raised again, and the top surface of the mold cavity is higher than the top surfaces of the TiC / ZrO2 round billet and the second portion of the granulated powder; the third portion of the granulated powder is loaded into the twice-raised mold cavity; the lower punch is covered, and the outer mold is turned over so that the upper punch is at the upper part of the mold cavity and the lower punch is at the lower part of the mold cavity; the first portion of the granulated powder accounts for 5 / 13 (7.5 g) of the total mass of the granulated powder; the second portion of the granulated powder accounts for 3 / 13 (4.5 g) of the total mass of the granulated powder; the inner diameter of the mold cavity of the outer mold is Φ = 30 mm, and the outer mold has the appearance as shown in Figure 5 ;

[0062] The raw material in the outer mold is dry-pressed to form a composite round billet; the dry-pressing pressure is 50 MPa, and the pressure holding time is 30 s.

[0063] The composite round billet is dried to remove water, and then is subjected to pressureless sintering to form a ZrO2-TiC / ZrO2 co-sintered ceramic composite material; the sintering temperature of the pressureless sintering is 1700 ± 10 °C, and the holding time is 120 ± 10 min.

[0064] The ZrO2-TiC / ZrO2 co-fired ceramic composite material consists of a core and an outer layer forming a single integrated structure. (See attached image.) Figure 4 As shown, the outer material is ZrO2 (insulating), and the core material is TiC / ZrO2 (conductive); the resistivity of the core is 0.99 × 10⁻⁶. -5 Ω·m; Interface microstructure such as Figure 2 As shown in (a), the conductive inner TiC / ZrO2 region is composed of dark gray ZrO2 phase and bright white TiC phase, with a small number of pores observed. There are no macroscopic cracks at the interface junction, and the interface remains intact throughout the mechanical grinding process. EDS energy dispersive spectroscopy analysis of the interface shows that the concentration of Zr element near the ZrO2-TiC / ZrO2 interface is almost uniform. Ti element is mainly distributed in the TiC portion of the inner TiC / ZrO2 ceramic, and no significant diffusion into the outer ZrO2 was observed.

[0065] Interface fracture morphology as follows Figure 3 As shown in (a), the left side of the interface is a TiC / ZrO2 ceramic part, and the right side of the interface is a ZrO2 ceramic part. The two are directly connected without an intermediate transition layer. Even if fracture occurs, the interface part remains relatively intact without cracks. However, the density of the ZrO2 ceramic structure near the right side of the interface is low, and there are relatively many pores that have not been eliminated.

[0066] The flexural strength of the ZrO2-TiC / ZrO2 co-fired ceramic composite material is 488.3 MPa; the compressive strength is 187.8 MPa; the ZrO2-TiC / ZrO2 co-fired ceramic composite material obtained meets the expectations.

[0067] Example 2

[0068] The method is the same as in Example 1, except that:

[0069] (1) The ball milling speed is 70 r / min, the ball milling time is 14 h, and the micron TiC powder accounts for 35% of the total mass of the raw materials;

[0070] (2) The polyvinyl alcohol aqueous solution is 9% of the powder mass;

[0071] (3) When dry pressing to form TiC / ZrO2 round blanks, the pressure of dry pressing is 75MPa and the holding time is 25s;

[0072] (4) When the composite round blank is formed by dry pressing, the pressure is 75MPa and the holding time is 25s;

[0073] (5) The resistivity of the core of the ZrO2-TiC / ZrO2 co-fired ceramic composite material is 1.31 × 10⁻⁶. -5 Ω·m; Interface microstructure such as Figure 2(b) shown; interface fracture morphology as shown in Figure 3 (b) shown;

[0074] (6) The bending strength of the ZrO2-TiC / ZrO2 co-fired ceramic composite material is 537.5 MPa, and the compressive strength is 196.6 MPa.

[0075] Example 3

[0076] The method is the same as in Example 1, except that:

[0077] (1) The ball milling speed is 75 r / min, the ball milling time is 13 h, and the micron TiC powder accounts for 30% of the total mass of the raw materials;

[0078] (2) The polyvinyl alcohol aqueous solution is 10% of the mass of the powder;

[0079] (3) When the TiC / ZrO2 round billet is made by dry pressing, the dry pressing pressure is 100 MPa, and the pressure holding time is 20 s;

[0080] (4) When the composite round billet is made by dry pressing, the pressure is 100 MPa, and the pressure holding time is 20 s;

[0081] (5) The resistivity of the core of the ZrO2-TiC / ZrO2 co-fired ceramic composite material is 2.14 x 10 -5 Ω·m; the interface microstructure is as shown in Figure 2 (c) shown; the interface fracture morphology is as shown in Figure 3 (c) shown;

[0082] (6) The bending strength of the ZrO2-TiC / ZrO2 co-fired ceramic composite material is 545.0 MPa, and the compressive strength is 207.3 MPa.

[0083] Example 4

[0084] The method is the same as in Example 1, except that:

[0085] (1) The ball milling speed is 80 r / min, the ball milling time is 12 h, and the micron TiC powder accounts for 25% of the total mass of the raw materials;

[0086] (2) The polyvinyl alcohol aqueous solution is 10% of the mass of the powder;

[0087] (3) When the TiC / ZrO2 round billet is made by dry pressing, the dry pressing pressure is 125 MPa, and the pressure holding time is 15 s;

[0088] (4) When the composite round billet is made by dry pressing, the pressure is 125 MPa, and the pressure holding time is 15 s;

[0089] (5) The resistivity of the ZrO2-TiC / ZrO2 co-fired ceramic composite in the core is 5.38 x 10 -5 Ω·m; the interface microstructure is as shown in Figure 2 (d); the interface fracture morphology is as shown in Figure 3 (d); the interface fracture morphology is as shown in

[0090] (6) The bending strength of the ZrO2-TiC / ZrO2 co-fired ceramic composite is 557.5 MPa, and the compressive strength is 215.0 MPa.

[0091] Example 5

[0092] The method is the same as in Example 1, except that:

[0093] (1) The ball milling speed is 70 r / min, the ball milling time is 13 h, and the micron TiC powder accounts for 30% of the total mass of the raw materials;

[0094] (2) The polyvinyl alcohol aqueous solution is 9% of the mass of the powder;

[0095] (3) When the TiC / ZrO2 round billet is made by dry pressing, the dry pressing pressure is 75 MPa, and the pressure holding time is 25 s;

[0096] (4) When the composite round billet is made by dry pressing, the pressure is 75 MPa, and the pressure holding time is 25 s;

[0097] (5) The resistivity of the ZrO2-TiC / ZrO2 co-fired ceramic composite in the core is 1.96 x 10 -5 Ω·m;

[0098] (6) The bending strength of the ZrO2-TiC / ZrO2 co-fired ceramic composite is 532.4 MPa, and the compressive strength is 190.2 MPa.

[0099] Example 6

[0100] The method is the same as in Example 1, except that:

[0101] (1) The ball milling speed is 70 r / min, the ball milling time is 15 h, and the micron TiC powder accounts for 40% of the total mass of the raw materials;

[0102] (2) The polyvinyl alcohol aqueous solution is 10% of the mass of the powder;

[0103] (3) When the TiC / ZrO2 round billet is made by dry pressing, the dry pressing pressure is 75 MPa, and the pressure holding time is 30 s;

[0104] (4) When the composite round billet is made by dry pressing, the pressure is 75 MPa, and the pressure holding time is 30 s;

[0105] (5) The resistivity of the ZrO2-TiC / ZrO2 co-fired ceramic composite in the core is 1.26 x 10 -5 Ω m.

[0106] (6) The bending strength of the ZrO2-TiC / ZrO2 co-fired ceramic composite is 528.6 MPa, and the compressive strength is 187.3 MPa.

[0107] Example 7

[0108] The method is the same as that in Example 1, except that:

[0109] (1) The ball milling speed is 70 r / min, the ball milling time is 12 h, and the micron TiC powder accounts for 30% of the total mass of the raw materials;

[0110] (2) The polyvinyl alcohol aqueous solution is 9% of the mass of the powder;

[0111] (3) When the TiC / ZrO2 round billet is made by dry pressing, the dry pressing pressure is 75 MPa, and the pressure holding time is 20 s;

[0112] (4) When the composite round billet is made by dry pressing, the pressure is 75 MPa, and the pressure holding time is 20 s;

[0113] (5) The resistivity of the ZrO2-TiC / ZrO2 co-fired ceramic composite in the core is 1.17 x 10 -5 Ω m.

[0114] (6) The bending strength of the ZrO2-TiC / ZrO2 co-fired ceramic composite is 526.4 MPa, and the compressive strength is 190.6 MPa.

[0115] Example 8

[0116] The method is the same as that in Example 1, except that:

[0117] (1) The ball milling speed is 70 r / min, the ball milling time is 14 h, and the micron TiC powder accounts for 40% of the total mass of the raw materials;

[0118] (2) The polyvinyl alcohol aqueous solution is 10% of the mass of the powder;

[0119] (3) When the TiC / ZrO2 round billet is made by dry pressing, the dry pressing pressure is 75 MPa, and the pressure holding time is 40 s;

[0120] (4) When the composite round billet is made by dry pressing, the pressure is 75 MPa, and the pressure holding time is 40 s;

[0121] (5) The resistivity of the ZrO2-TiC / ZrO2 co-fired ceramic composite in the core is 1.28 x 10 -5 Ω m.

[0122] (6) The bending strength of the ZrO2-TiC / ZrO2 co-fired ceramic composite material is 523.2 MPa, and the compressive strength is 191.5 MPa.

Claims

1. A method for producing a zirconia-titanium carbide / zirconia co-fired ceramic composite material, characterized by The following steps are taken: (1) Prepare Y2O3 stabilized nano ZrO2 powder and micron TiC powder as raw materials, with the micron TiC powder accounting for 25-40% of the total mass of the raw materials; put the raw materials into a ball mill tank, add anhydrous ethanol as a ball milling medium, and put in grinding balls for ball milling to obtain a ball-milled wet material; (2) Dry the ball-milled wet material to remove the ball milling medium, and prepare a dry material; grind and crush the dry material to prepare a powder; (3) Add polyvinyl alcohol aqueous solution to the powder, then stir and mix uniformly, and sieve to obtain granules; (4) Place the granules in a center mold, and dry-press to form a TiC / ZrO2 round billet; (5) Spray granulate the Y2O3 stabilized nano ZrO2 powder to prepare a granulated powder; (6) Invert the outer mold so that the upper press head is at the lower part of the mold cavity and the lower press head is at the upper part of the mold cavity; remove the lower press head, place the first part of the granulated powder in the mold cavity, and press the upper surface of the granulated powder in the mold cavity flat; raise the mold cavity so that the bottom of the mold cavity is outside the boss of the upper press head, position with a round plate with a circular hole, place the TiC / ZrO2 round billet in the middle of the mold cavity, and the TiC / ZrO2 round billet is above the first part of the granulated powder, at this time the top surface of the TiC / ZrO2 round billet is flush with the top surface of the raised mold cavity; continue to place the second part of the granulated powder in the mold cavity to fill the gap between the TiC / ZrO2 round billet and the inner wall of the mold cavity, and scrape the second part of the granulated powder flat so that the top surface of the second part of the granulated powder is flush with the top surface of the TiC / ZrO2 round billet and the top surface of the raised mold cavity; raise the mold cavity again, at this time the top surface of the mold cavity is higher than the top surfaces of the TiC / ZrO2 round billet and the second part of the granulated powder; place the third part of the granulated powder in the twice-raised mold cavity; cover the lower press head, and turn the outer mold so that the upper press head is at the upper part of the mold cavity and the lower press head is at the lower part of the mold cavity; (7) Dry-press the raw materials in the outer mold to form a composite round billet; (8) Dry the composite round billet to remove moisture, then perform pressureless sintering at a sintering temperature of 1700±10℃ for a holding time of 120±10 min to prepare a ZrO2-TiC / ZrO2 co-sintered ceramic composite material; The ZrO2-TiC / ZrO2 co-fired ceramic composite material is composed of a core and an outer part, the outer part is made of ZrO2, the core is made of TiC / ZrO2, the resistivity of the core TiC / ZrO2 is 0.99×10 -5 ~5.38×10 -5 Ω·m; the bending strength of the ZrO2-TiC / ZrO2 co-fired ceramic composite material is 488.3~557.5MPa, and the compressive strength is 187.8~215MPa.

2. The method of producing a zirconia-titanium carbide / zirconia co-fired ceramic composite according to claim 1, characterized in that In steps (1) and (5), the mole percentage of Y2O3 in the Y2O3 stabilized nano ZrO2 powder is 3%.

3. The method of making a zirconia-titanium carbide / zirconia co-fired ceramic composite of claim 1, wherein In steps (1) and (5), the particle size of the Y2O3 stabilized nano ZrO2 powder is 30-50 nm.

4. The method of making a zirconia-titanium carbide / zirconia co-fired ceramic composite of claim 1, wherein In step (1), the particle size of the micron TiC powder is 0.5-1.0 μm.

5. The method of making a zirconia-titanium carbide / zirconia co-fired ceramic composite of claim 1, wherein In step (3), the sieving is through a 60-mesh sieve.

6. The method of making a zirconia-titanium carbide / zirconia co-fired ceramic composite of claim 1, wherein In step (3), the polyvinyl alcohol aqueous solution is 8-10% of the mass of the powder.

7. The method of making a zirconia-titanium carbide / zirconia co-fired ceramic composite of claim 1, wherein In steps (4) and (7), the dry-pressing pressure is 50-125 MPa, and the pressure holding time is at least 15 s.

8. The method of making a zirconia-titanium carbide / zirconia co-fired ceramic composite of claim 1, wherein In step (5), the particle size of the granulated powder is 50-100 μm.

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