CN115521151A - Discharge plasma sintering method of silicon carbide/tantalum carbide toughened ceramic - Google Patents
Discharge plasma sintering method of silicon carbide/tantalum carbide toughened ceramic Download PDFInfo
- Publication number
- CN115521151A CN115521151A CN202211191381.7A CN202211191381A CN115521151A CN 115521151 A CN115521151 A CN 115521151A CN 202211191381 A CN202211191381 A CN 202211191381A CN 115521151 A CN115521151 A CN 115521151A
- Authority
- CN
- China
- Prior art keywords
- plasma sintering
- powder
- spark plasma
- sintering method
- temperature
- Prior art date
- Legal status (The legal status is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the status listed.)
- Pending
Links
Images
Classifications
-
- C—CHEMISTRY; METALLURGY
- C04—CEMENTS; CONCRETE; ARTIFICIAL STONE; CERAMICS; REFRACTORIES
- C04B—LIME, MAGNESIA; SLAG; CEMENTS; COMPOSITIONS THEREOF, e.g. MORTARS, CONCRETE OR LIKE BUILDING MATERIALS; ARTIFICIAL STONE; CERAMICS; REFRACTORIES; TREATMENT OF NATURAL STONE
- C04B35/00—Shaped ceramic products characterised by their composition; Ceramics compositions; Processing powders of inorganic compounds preparatory to the manufacturing of ceramic products
- C04B35/515—Shaped ceramic products characterised by their composition; Ceramics compositions; Processing powders of inorganic compounds preparatory to the manufacturing of ceramic products based on non-oxide ceramics
- C04B35/56—Shaped ceramic products characterised by their composition; Ceramics compositions; Processing powders of inorganic compounds preparatory to the manufacturing of ceramic products based on non-oxide ceramics based on carbides or oxycarbides
- C04B35/565—Shaped ceramic products characterised by their composition; Ceramics compositions; Processing powders of inorganic compounds preparatory to the manufacturing of ceramic products based on non-oxide ceramics based on carbides or oxycarbides based on silicon carbide
- C04B35/575—Shaped ceramic products characterised by their composition; Ceramics compositions; Processing powders of inorganic compounds preparatory to the manufacturing of ceramic products based on non-oxide ceramics based on carbides or oxycarbides based on silicon carbide obtained by pressure sintering
-
- C—CHEMISTRY; METALLURGY
- C04—CEMENTS; CONCRETE; ARTIFICIAL STONE; CERAMICS; REFRACTORIES
- C04B—LIME, MAGNESIA; SLAG; CEMENTS; COMPOSITIONS THEREOF, e.g. MORTARS, CONCRETE OR LIKE BUILDING MATERIALS; ARTIFICIAL STONE; CERAMICS; REFRACTORIES; TREATMENT OF NATURAL STONE
- C04B2235/00—Aspects relating to ceramic starting mixtures or sintered ceramic products
- C04B2235/02—Composition of constituents of the starting material or of secondary phases of the final product
- C04B2235/30—Constituents and secondary phases not being of a fibrous nature
- C04B2235/38—Non-oxide ceramic constituents or additives
- C04B2235/3817—Carbides
- C04B2235/3839—Refractory metal carbides
-
- C—CHEMISTRY; METALLURGY
- C04—CEMENTS; CONCRETE; ARTIFICIAL STONE; CERAMICS; REFRACTORIES
- C04B—LIME, MAGNESIA; SLAG; CEMENTS; COMPOSITIONS THEREOF, e.g. MORTARS, CONCRETE OR LIKE BUILDING MATERIALS; ARTIFICIAL STONE; CERAMICS; REFRACTORIES; TREATMENT OF NATURAL STONE
- C04B2235/00—Aspects relating to ceramic starting mixtures or sintered ceramic products
- C04B2235/02—Composition of constituents of the starting material or of secondary phases of the final product
- C04B2235/50—Constituents or additives of the starting mixture chosen for their shape or used because of their shape or their physical appearance
- C04B2235/54—Particle size related information
- C04B2235/5418—Particle size related information expressed by the size of the particles or aggregates thereof
- C04B2235/5436—Particle size related information expressed by the size of the particles or aggregates thereof micrometer sized, i.e. from 1 to 100 micron
-
- C—CHEMISTRY; METALLURGY
- C04—CEMENTS; CONCRETE; ARTIFICIAL STONE; CERAMICS; REFRACTORIES
- C04B—LIME, MAGNESIA; SLAG; CEMENTS; COMPOSITIONS THEREOF, e.g. MORTARS, CONCRETE OR LIKE BUILDING MATERIALS; ARTIFICIAL STONE; CERAMICS; REFRACTORIES; TREATMENT OF NATURAL STONE
- C04B2235/00—Aspects relating to ceramic starting mixtures or sintered ceramic products
- C04B2235/02—Composition of constituents of the starting material or of secondary phases of the final product
- C04B2235/50—Constituents or additives of the starting mixture chosen for their shape or used because of their shape or their physical appearance
- C04B2235/54—Particle size related information
- C04B2235/5418—Particle size related information expressed by the size of the particles or aggregates thereof
- C04B2235/5445—Particle size related information expressed by the size of the particles or aggregates thereof submicron sized, i.e. from 0,1 to 1 micron
-
- C—CHEMISTRY; METALLURGY
- C04—CEMENTS; CONCRETE; ARTIFICIAL STONE; CERAMICS; REFRACTORIES
- C04B—LIME, MAGNESIA; SLAG; CEMENTS; COMPOSITIONS THEREOF, e.g. MORTARS, CONCRETE OR LIKE BUILDING MATERIALS; ARTIFICIAL STONE; CERAMICS; REFRACTORIES; TREATMENT OF NATURAL STONE
- C04B2235/00—Aspects relating to ceramic starting mixtures or sintered ceramic products
- C04B2235/65—Aspects relating to heat treatments of ceramic bodies such as green ceramics or pre-sintered ceramics, e.g. burning, sintering or melting processes
- C04B2235/656—Aspects relating to heat treatments of ceramic bodies such as green ceramics or pre-sintered ceramics, e.g. burning, sintering or melting processes characterised by specific heating conditions during heat treatment
- C04B2235/6562—Heating rate
-
- C—CHEMISTRY; METALLURGY
- C04—CEMENTS; CONCRETE; ARTIFICIAL STONE; CERAMICS; REFRACTORIES
- C04B—LIME, MAGNESIA; SLAG; CEMENTS; COMPOSITIONS THEREOF, e.g. MORTARS, CONCRETE OR LIKE BUILDING MATERIALS; ARTIFICIAL STONE; CERAMICS; REFRACTORIES; TREATMENT OF NATURAL STONE
- C04B2235/00—Aspects relating to ceramic starting mixtures or sintered ceramic products
- C04B2235/65—Aspects relating to heat treatments of ceramic bodies such as green ceramics or pre-sintered ceramics, e.g. burning, sintering or melting processes
- C04B2235/656—Aspects relating to heat treatments of ceramic bodies such as green ceramics or pre-sintered ceramics, e.g. burning, sintering or melting processes characterised by specific heating conditions during heat treatment
- C04B2235/6567—Treatment time
-
- C—CHEMISTRY; METALLURGY
- C04—CEMENTS; CONCRETE; ARTIFICIAL STONE; CERAMICS; REFRACTORIES
- C04B—LIME, MAGNESIA; SLAG; CEMENTS; COMPOSITIONS THEREOF, e.g. MORTARS, CONCRETE OR LIKE BUILDING MATERIALS; ARTIFICIAL STONE; CERAMICS; REFRACTORIES; TREATMENT OF NATURAL STONE
- C04B2235/00—Aspects relating to ceramic starting mixtures or sintered ceramic products
- C04B2235/65—Aspects relating to heat treatments of ceramic bodies such as green ceramics or pre-sintered ceramics, e.g. burning, sintering or melting processes
- C04B2235/658—Atmosphere during thermal treatment
- C04B2235/6581—Total pressure below 1 atmosphere, e.g. vacuum
-
- C—CHEMISTRY; METALLURGY
- C04—CEMENTS; CONCRETE; ARTIFICIAL STONE; CERAMICS; REFRACTORIES
- C04B—LIME, MAGNESIA; SLAG; CEMENTS; COMPOSITIONS THEREOF, e.g. MORTARS, CONCRETE OR LIKE BUILDING MATERIALS; ARTIFICIAL STONE; CERAMICS; REFRACTORIES; TREATMENT OF NATURAL STONE
- C04B2235/00—Aspects relating to ceramic starting mixtures or sintered ceramic products
- C04B2235/65—Aspects relating to heat treatments of ceramic bodies such as green ceramics or pre-sintered ceramics, e.g. burning, sintering or melting processes
- C04B2235/66—Specific sintering techniques, e.g. centrifugal sintering
- C04B2235/666—Applying a current during sintering, e.g. plasma sintering [SPS], electrical resistance heating or pulse electric current sintering [PECS]
-
- C—CHEMISTRY; METALLURGY
- C04—CEMENTS; CONCRETE; ARTIFICIAL STONE; CERAMICS; REFRACTORIES
- C04B—LIME, MAGNESIA; SLAG; CEMENTS; COMPOSITIONS THEREOF, e.g. MORTARS, CONCRETE OR LIKE BUILDING MATERIALS; ARTIFICIAL STONE; CERAMICS; REFRACTORIES; TREATMENT OF NATURAL STONE
- C04B2235/00—Aspects relating to ceramic starting mixtures or sintered ceramic products
- C04B2235/70—Aspects relating to sintered or melt-casted ceramic products
- C04B2235/74—Physical characteristics
- C04B2235/77—Density
-
- C—CHEMISTRY; METALLURGY
- C04—CEMENTS; CONCRETE; ARTIFICIAL STONE; CERAMICS; REFRACTORIES
- C04B—LIME, MAGNESIA; SLAG; CEMENTS; COMPOSITIONS THEREOF, e.g. MORTARS, CONCRETE OR LIKE BUILDING MATERIALS; ARTIFICIAL STONE; CERAMICS; REFRACTORIES; TREATMENT OF NATURAL STONE
- C04B2235/00—Aspects relating to ceramic starting mixtures or sintered ceramic products
- C04B2235/70—Aspects relating to sintered or melt-casted ceramic products
- C04B2235/96—Properties of ceramic products, e.g. mechanical properties such as strength, toughness, wear resistance
Abstract
The invention relates to a discharge plasma sintering method of silicon carbide/tantalum carbide toughened ceramic, which comprises the following steps: (1) Mixing beta-SiC powder and TaC powder to obtain raw material powder; (2) And putting the raw material powder into a graphite die, compacting and fixing by using a pressure head, and transferring to a spark plasma sintering furnace for spark plasma sintering to obtain the silicon carbide/tantalum carbide toughened ceramic.
Description
Technical Field
The invention relates to a method for preparing silicon carbide/tantalum carbide toughened ceramic by a discharge plasma sintering method, belonging to the technical field of preparation of complex-phase ceramic materials.
Background
Silicon carbide is a high-hardness ceramic material, and the silicon carbide ceramic has physical properties of good mechanical properties and high hardness and strength and chemical inertness. As a structural material, the silicon carbide ceramic is widely applied to mechanical transmission parts such as bearings and the like and fixing parts such as sealing and the like; the method also has wide application in the high-precision aerospace aspect. Due to the intrinsic brittleness of the silicon carbide ceramic, the doping and compounding modes are often used for improving mechanical properties of the silicon carbide ceramic, such as hardness, fracture toughness, elastic modulus and the like, so as to improve the cutting processability of the silicon carbide ceramic and overcome the intrinsic brittleness. As a second phase of the composite material, the tantalum carbide material has the intrinsic property of relatively high fracture toughness. The tantalum carbide has a cubic crystal form, and is matched with the crystal form of 3C-SiC, and the generated solid solution has solid solution strengthening and pinning effects. In the sintering process, siC can generate phase change according to the change of pressure, atmosphere and temperature conditions, and the phase change is generated under different components in cooperation with TaC, so that the whole sintered body is subjected to particle toughening and fiber toughening effects, a sliding system in the system is increased, and the mechanical properties of the material, including hardness and fracture toughness, are improved. Because the components of the composite ceramic have stronger covalency, the sintering process usually has higher requirements on the sintering temperature, atmosphere and sintering aid. Under the condition of not adding a sintering aid, the sintering densification of the complex phase ceramic is more difficult, and higher sintering temperature is needed. It is very difficult to take into account the phase change in the process of sintering and densifying the complex phase ceramic.
The Spark Plasma Sintering (SPS) technology can be applied to the sintering preparation of various materials, and comprises metal materials and ceramic materials according to the type of a sintered body; the material comprises gradient materials and composite materials according to structural division; the flash firing and flash connection of the ceramic can also be carried out by changing the reaction conditions. The SPS technology has the characteristics of quick temperature rise, quick temperature reduction and short sintering time, the sintered finished product under the condition inhibits the growth of crystal grains due to short heat preservation time, the crystal grains are finer, and the sample density is higher compared with samples in other sintering modes at the same temperature. The SPS densification mechanism comprises two parts, namely a traditional heat transfer process, wherein heat transfer is carried out on a mold through a pressure head and a cavity, and two ends are pressed to promote sintering, the mechanism is similar to hot pressing, but the SPS densification mechanism has higher heat transfer efficiency; secondly, by applying pulse current to the powder in the die, local high temperature can be generated instantaneously when discharging at the grain gap, so that the grain surface is evaporated and melted, a neck is formed at a contact point, and evaporation-condensation substance transfer is caused by rapid cooling of the neck, thereby promoting the sintering process. Therefore, compared with the traditional hot pressing and air pressure sintering technology, the SPS technology has the advantages of advancement in ceramic densification, high temperature and quick sintering, and can realize the low-temperature quick sintering densification of the ceramic. The ceramic sintered product of the technology is usually compact in structure and uniform in structure.
Tantalum carbide (TaC) is a covalent compound, the carbon-tantalum ratio 1:1 belongs to a cubic crystal system, and the change of the carbon-tantalum ratio can cause the change of components and generate other carbides with new different crystal systems and morphologies. As a covalent compound, the material has strong covalent bond property and stable property, and is difficult to sinter and densify. The addition of tantalum carbide gives consideration to the solid solution property of the tantalum carbide and the main phase silicon carbide and the toughening effect of self phase change generated particles and whiskers, and can greatly improve the fracture toughness of the sintered body.
The improvement of fracture toughness has positive significance for further processing after the ceramic material is sintered, and the excellent performance of SiC and TaC ceramics is difficult to be fully utilized due to poor processing resistance. The strength problem of current SiC ceramics has been substantially solved, but its intrinsic brittleness has been a negative factor limiting its applications. In order to improve the brittleness of SiC ceramic and make subsequent processing difficult, the invention provides a discharge plasma sintering method of SiC/TaC toughened ceramic, which improves the toughness of the SiC ceramic and improves the cutting processing performance.
At present, in the research of preparing SiC/TaC toughened ceramic by SPS sintering, only the research of taking TaCx as a main phase is carried out, wherein the highest addition amount of SiC is only 40%, and Ta is doped into mixed powder to generate non-cubic-phase TaC for modification through in-situ reaction. In the existing research, the sintering temperature is low, so that the beta-SiC does not reach the phase transition temperature and can not be subjected to phase transition into columnar crystals, and the improvement of the overall toughness is not facilitated; and the proportion of TaC greatly increases the overall density of the material. Liu in the Master academic paper "influence of silicon carbide additives on microstructure and mechanical properties of tantalum carbide ceramicsMixing SiC with TaC powder and sintering, wherein the highest fracture toughness of the mixture is only 4.4 +/-0.5 MPa-m when the SiC content is 40vol% based on the TaC as a main phase 1/2 . In the past, there has been a binary system of SiC-TaC in which TaC is used as a main phase and SiC is added up to 40vol% as a second phase. In the system, the addition of SiC plays a role in pinning crystal boundaries, so that pores in the crystal are avoided, and the toughness is reduced after a large amount of SiC is continuously doped.
Disclosure of Invention
Therefore, the invention provides a discharge plasma sintering method of silicon carbide/tantalum carbide toughened ceramic, which comprises the following steps:
(1) Mixing beta-SiC powder and TaC powder to obtain raw material powder;
(2) And putting the raw material powder into a graphite die, compacting and fixing by using a pressure head, and transferring to a spark plasma sintering furnace for spark plasma sintering to obtain the silicon carbide/tantalum carbide toughened ceramic.
Preferably, the purity of the beta-SiC powder is more than or equal to 99.9 percent, and the granularity is 0.2-0.5 mu m; the purity of the TaC powder is more than or equal to 99.9 percent, and the granularity is 0.8-1.2 mu m.
Preferably, the mixing mode is ball milling mixing; the rotation speed of ball milling mixing is 300-500r/min, and the ball milling time is 4-8 hours.
Also, preferably, drying and sieving are carried out after ball milling and mixing; wherein the drying temperature is 60-80 ℃ and the drying time is 6-12 hours; the sieving is 200 mesh sieving.
Preferably, the grinding balls in the ball-milling mixing are silicon carbide balls, and the ball-material ratio is (1-1.2): 1, the adding amount of the alcohol is 50-100% of the mass of the powder.
Preferably, the addition amount of the TaC powder is 5-20vol% of the total amount of the beta-SiC powder and the TaC powder.
Preferably, the axial pressure applied in the spark plasma sintering is 40-80 MPa.
Preferably, the atmosphere of the spark plasma sintering is vacuum atmosphere, the temperature is 2000-2100 ℃, and the time is 10-20 minutes.
Preferably, the temperature raising system for spark plasma sintering comprises: the temperature rise rate is 300 ℃/min within the range from room temperature to 600 ℃; the temperature is 600-2000-2100 deg.C, and the heating rate is 100 deg.C/min.
Has the advantages that:
the invention provides an efficient preparation method of high-performance silicon carbide/tantalum carbide toughened ceramic, which adopts SPS technology to sinter SiC/TaC toughened ceramic, and no sintering aid is added in the sintering process; the sintering mode has rapid temperature rise and fall, short heat preservation time, energy conservation and environmental protection; the crystal structure and the phase change characteristic of different components are comprehensively considered in component selection, the comprehensive performance of a finished product is enhanced, the fracture toughness of the SiC ceramic material is greatly improved, and the cutting processing resistance is improved.
Drawings
FIG. 1 is an SEM image of a ceramic sample prepared in example 3;
FIG. 2 is an XRD pattern of a ceramic sample made in accordance with example 3;
FIG. 3 is an SEM image of a ceramic sample prepared in example 1;
figure 4 is an XRD pattern of the ceramic sample prepared in example 2.
Detailed Description
The present invention is further illustrated by the following examples, which are to be understood as merely illustrative and not restrictive.
The following exemplary method for spark plasma sintering of silicon carbide/tantalum carbide toughened ceramic is described.
Mixing 99.9% purity beta-SiC powder with particle size of 0.2-0.5 μm and 99.9% purity TaC powder with particle size of 0.8-1.2 μm, adding alcohol and dispersant, grinding in ball mill, oven drying, and sieving.
Wherein the grain diameter of the SiC powder is 0.2-0.5 μm. The particle diameter of the TaC powder is 0.8-1.2 μm. The adding amount of the TaC powder is 5-20vol% of the total powder. The grinding balls are silicon carbide balls, and the ball material ratio is 1-1.2:1. the ball milling speed is 300-500r/min. The drying (drying) temperature is 60-80 ℃, and the drying time is 6-12h. The dispersant comprises at least one of tetramethylammonium hydroxide (TMAH), polyethyleneimine (PEI) and polyacrylic acid (PAA). Wherein, the addition amount of the dispersant (such as TMAH) is 0.5 to 1wt percent of the total mass of the powder. The adding amount of the alcohol is 50-100% of the total mass of the powder.
Putting the dried and sieved powder into a graphite die, compacting and fixing by using a pressure head, and transferring to a discharge plasma sintering furnace; vacuumizing, adjusting the pressure applied on the graphite mold to a target value, and then heating; the temperature is within the range from room temperature to 600 ℃, and the heating rate is 300 ℃/min; heating at 600-1900-2100 deg.c at 100 deg.c/min, and maintaining for 10-20min to obtain the toughened SiC/TaC ceramic.
As an example of the preparation method of the silicon carbide/tantalum carbide toughened ceramic spark plasma sintering method, the method comprises the following steps: beta-SiC powder with purity of 99.9 percent and granularity of 0.2-0.5 mu m and TaC powder with purity of 99.9 percent and granularity of 0.8-1.2 mu m are used as raw materials, are placed in a high-strength graphite die to be compacted and are placed between an upper electrode and a lower electrode of a discharge plasma sintering (SPS) device. Before sintering, vacuumizing to below 5Pa, increasing the axial pressure to 5-10MPa, heating, pressurizing to 40-80MPa in the heating process, keeping the pressure, and preserving the heat for 10-20min to obtain the SiC-TaC complex phase ceramic without the sintering aid.
According to the invention, taC is added into beta-SiC as a second phase, and the solid solution strengthening principle and the toughening property of the second phase with multiple slip planes are utilized. Simultaneously, the SPS technology is adopted for densification, partial phase transformation of the beta-SiC is carried out by controlling the pressure and the heat preservation time, partial alpha-SiC particles are generated in situ, and the particle toughening is realized. No sintering aid is needed to be added in the sintering process, the process time is short, the temperature is low, and the method is energy-saving and environment-friendly.
The present invention will be described in further detail with reference to examples. It is also to be understood that the following examples are illustrative of the present invention and are not to be construed as limiting the scope of the invention, and that certain insubstantial modifications and adaptations of the invention by those skilled in the art may be made in light of the above teachings. The specific process parameters and the like of the following examples are also only one example of suitable ranges, i.e., those skilled in the art can select the appropriate ranges through the description herein, and are not limited to the specific values exemplified below.
Example 1:
(1) Preparing materials: siC powder was prepared so that the SiC content was 95% vol. Charging 95% vol β -SiC powder, 5% vol TaC powder, the corresponding alcohol and grinding balls into a ball mill at a rotation speed of 300r/min, taking out the slurry after 4 hours, putting into an oven, drying at 60 ℃ for 12 hours, and sieving with a 200-mesh sieve;
(2) Firing: and (3) placing a proper amount of sieved powder into a graphite die with the inner diameter of 20mm, compacting, placing the compacted powder between an upper electrode and a lower electrode of an SPS device, vacuumizing, starting to electrify and heat, heating to 600 ℃ at the speed of 300 ℃/min, heating to 2100 ℃ at the sintering temperature at the speed of 100 ℃/min, keeping the axial pressure at 40MPa for 10 minutes, cooling, and taking out a sample.
The relative density of the sample obtained in example 1 was measured to be 95.4%, the hardness was measured to be 17.70. + -. 0.42GPa, and the fracture toughness (indentation method) was measured to be 2.59. + -. 0.14 MPa-m 1/2 。
Example 2:
(1) Preparing materials: preparing SiC powder with TaC content of 80 vol%. Charging 80% vol β -SiC powder, 20vol% TaC powder, corresponding alcohol and grinding balls into a ball mill at a rotation speed of 300r/min, taking out the slurry after 8 hours, putting into an oven, drying at 70 ℃ for 12 hours, and sieving by a 200-mesh sieve;
(2) Firing: and (3) placing a proper amount of sieved powder into a graphite die with the inner diameter of 40mm, compacting, placing the powder between an upper electrode and a lower electrode of an SPS device, vacuumizing, starting to electrify and heat, heating to 600 ℃ at the speed of 300 ℃/min, heating to the sintering temperature of 2000 ℃ at the speed of 100 ℃/min, keeping the axial pressure at 40MPa, keeping the temperature for 10 minutes, and cooling to take out a sample.
The sample obtained in example 2 was measured to have a relative density of 97.9%, a hardness of 20.62. + -. 1.01GPa, and a fracture toughness (SENB) of 5.13. + -. 0.66MPa · m 1/2 。
Example 3:
(1) Preparing materials: preparing SiC powder with TaC content of 80 vol%. Putting 80 percent vol beta-SiC powder, 20 percent vol TaC powder, corresponding alcohol and grinding balls into a ball mill at the rotating speed of 300r/min, taking out slurry after 6 hours, putting the slurry into an oven, drying the slurry for 6 hours at the temperature of 80 ℃, and sieving the slurry by a 200-mesh sieve;
(2) Firing: and (3) placing a proper amount of sieved powder into a graphite die with the inner diameter of 40mm, compacting, placing the powder between an upper electrode and a lower electrode of an SPS device, vacuumizing, starting to electrify and heat, heating to 600 ℃ at the speed of 300 ℃/min, heating to 2100 ℃ at the speed of 100 ℃/min, keeping the axial pressure at 40MPa, preserving the temperature for 20 minutes, and cooling and taking out the sample.
The relative density of the sample obtained in example 3 was measured to be 99.2%, the hardness was 21.64. + -. 0.46GPa, and the fracture toughness was 8.34. + -. 0.79 MPa. M 1/2 。
Comparative example 1
(1) Preparing materials: preparing pure beta-SiC powder. Putting beta-SiC powder, corresponding alcohol and grinding balls into a ball mill at the rotating speed of 300r/min, taking out slurry after 6 hours, putting the slurry into an oven, drying for 12 hours at 70 ℃, and sieving by a 200-mesh sieve;
(2) And (3) firing: and (3) placing a proper amount of sieved powder into a graphite die with the inner diameter of 20mm, compacting, placing the compacted powder between an upper electrode and a lower electrode of an SPS device, vacuumizing, starting to electrify and heat, heating to 600 ℃ at the speed of 300 ℃/min, heating to the sintering temperature of 2000 ℃ at the speed of 100 ℃/min, keeping the axial pressure at 40MPa for 10 minutes, cooling, and taking out a sample.
The relative density of the sample obtained in comparative example 1 was determined to be less than 65%, the hardness was determined to be less than 8GPa, and the fracture toughness was determined to be less than 1MPa m 1/2 。
The key point of the invention is that TaC is added into beta-SiC as a second phase, and the solid solution strengthening principle and the property of the second phase for increasing the slip surface are utilized. And meanwhile, the SPS technology is used for sintering, partial phase change of beta-SiC occurs by controlling the heat preservation time and the pressure, the phase change does not occur in the system at the SiC phase change temperature of below 1900 ℃, columnar crystals cannot be generated to play a toughening role, and the overall performance is lower because the sample is not densified. Sintering densification can be promoted and the phase change process of beta-SiC can be promoted by increasing the sintering temperature, so that the improvement of fracture toughness is facilitated, partial alpha-SiC particles are formed in situ, and the grain toughening is realized.
The foregoing has described the general principles, principal features, and advantages of the invention. It will be understood by those skilled in the art that the present invention is not limited to the embodiments described above, which are given by way of illustration of the principles of the present invention, and that various changes and modifications may be made without departing from the spirit and scope of the invention as defined by the appended claims. The scope of the invention is defined by the appended claims and equivalents thereof.
Claims (8)
1. A discharge plasma sintering method of silicon carbide/tantalum carbide toughened ceramic is characterized by comprising the following steps:
(1) Mixing beta-SiC powder and TaC powder to obtain raw material powder;
(2) And putting the raw material powder into a graphite die, compacting and fixing by using a pressure head, and transferring to a spark plasma sintering furnace for spark plasma sintering to obtain the silicon carbide/tantalum carbide toughened ceramic.
2. The spark plasma sintering method of claim 1 wherein the beta-SiC powder has a purity of 99.9% or more and a particle size of 0.2 to 0.5 μm; the purity of the TaC powder is more than or equal to 99.9 percent, and the granularity is 0.8-1.2 mu m.
3. The spark plasma sintering method according to claim 1 or 2, wherein the mixing manner is ball milling; the rotation speed of ball milling mixing is 300-500r/min, and the ball milling time is 4-8 hours;
preferably, drying and sieving are carried out after ball milling and mixing; wherein the drying temperature is 60-80 ℃, and the drying time is 6-12 hours; the sieving is 200 mesh sieving.
4. The spark plasma sintering method of claim 3, wherein the milling balls in the ball milling and mixing are silicon carbide balls, and the ball-to-material ratio is (1-1.2): 1, the adding amount of the alcohol is 50-100% of the mass of the powder.
5. The spark plasma sintering method as claimed in any one of claims 1 to 4, wherein the TaC powder is added in an amount of 5 to 20vol% based on the total amount of the β -SiC powder and the TaC powder.
6. The spark plasma sintering method according to any one of claims 1 to 5, wherein the axial pressure applied in the spark plasma sintering is 40 to 80MPa.
7. The spark plasma sintering method according to any one of claims 1 to 6, wherein the atmosphere of the spark plasma sintering is a vacuum atmosphere, the temperature is 2000 to 2100 ℃, and the time is 10 to 20 minutes.
8. The spark plasma sintering method according to claim 7, wherein the temperature raising system of the spark plasma sintering includes: the temperature rise rate is 300 ℃/min within the range from room temperature to 600 ℃; the temperature is 600-2000-2100 deg.C, and the heating rate is 100 deg.C/min.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN202211191381.7A CN115521151A (en) | 2022-09-28 | 2022-09-28 | Discharge plasma sintering method of silicon carbide/tantalum carbide toughened ceramic |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN202211191381.7A CN115521151A (en) | 2022-09-28 | 2022-09-28 | Discharge plasma sintering method of silicon carbide/tantalum carbide toughened ceramic |
Publications (1)
| Publication Number | Publication Date |
|---|---|
| CN115521151A true CN115521151A (en) | 2022-12-27 |
Family
ID=84699450
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| CN202211191381.7A Pending CN115521151A (en) | 2022-09-28 | 2022-09-28 | Discharge plasma sintering method of silicon carbide/tantalum carbide toughened ceramic |
Country Status (1)
| Country | Link |
|---|---|
| CN (1) | CN115521151A (en) |
Citations (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101417878A (en) * | 2007-10-24 | 2009-04-29 | 中国科学院金属研究所 | TaC-SiC ceramic composite material synthesized by hot pressing at in-situ reaction and synthetic method thereof |
| US8409491B1 (en) * | 2007-09-28 | 2013-04-02 | The United States of America as represented by the Administrator of the National Aeronautics & Space Administration (NASA) | In-situ formation of reinforcement phases in ultra high temperature ceramic composites |
| US20180311729A1 (en) * | 2015-11-04 | 2018-11-01 | Commissariat A L'energie Atomique Et Aux Energies Alternatives | Die and piston of an sps apparatus, sps apparatus comprising same, and method of sintering, densification or assembly in an oxidising atmosphere using said apparatus |
| CN111217610A (en) * | 2019-06-19 | 2020-06-02 | 哈尔滨工业大学 | Nanocrystalline tantalum carbide reinforced silicon-boron-carbon-nitrogen composite ceramic material and preparation method thereof |
-
2022
- 2022-09-28 CN CN202211191381.7A patent/CN115521151A/en active Pending
Patent Citations (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US8409491B1 (en) * | 2007-09-28 | 2013-04-02 | The United States of America as represented by the Administrator of the National Aeronautics & Space Administration (NASA) | In-situ formation of reinforcement phases in ultra high temperature ceramic composites |
| CN101417878A (en) * | 2007-10-24 | 2009-04-29 | 中国科学院金属研究所 | TaC-SiC ceramic composite material synthesized by hot pressing at in-situ reaction and synthetic method thereof |
| US20180311729A1 (en) * | 2015-11-04 | 2018-11-01 | Commissariat A L'energie Atomique Et Aux Energies Alternatives | Die and piston of an sps apparatus, sps apparatus comprising same, and method of sintering, densification or assembly in an oxidising atmosphere using said apparatus |
| CN111217610A (en) * | 2019-06-19 | 2020-06-02 | 哈尔滨工业大学 | Nanocrystalline tantalum carbide reinforced silicon-boron-carbon-nitrogen composite ceramic material and preparation method thereof |
Non-Patent Citations (3)
| Title |
|---|
| SANDAN KUMAR SHARMA等: "Erosive wear behavior of spark plasma-sintered SiC–TaC composites", 《APPLIED CERAMIC TECHNOLOGY》 * |
| 刘晗: "碳化硅添加剂对碳化钽陶瓷显微组织及力学性能的影响", 《中国优秀硕士学位论文全文数据库（工程科技Ⅰ辑）》 * |
| 陈忠明等: "原位增强SiC陶瓷", 《无机材料学报》 * |
Similar Documents
| Publication | Publication Date | Title |
|---|---|---|
| CN109987941B (en) | High-entropy ceramic composite material with oxidation resistance and preparation method and application thereof | |
| US7166550B2 (en) | Ceramic composite body of silicon carbide/boron nitride/carbon | |
| CN106904977B (en) | Preparation of surface hard and core tough Si by two-step sintering method3N4Method for producing ceramic material | |
| CN111825471B (en) | Method for preparing continuous carbon fiber toughened ultrahigh-temperature ceramic matrix composite material through electrophoretic deposition | |
| CN113636842B (en) | High-entropy diboride-boron carbide complex phase ceramic, preparation method and application thereof | |
| CN111004034B (en) | Silicon carbide ceramic, method for producing same, and semiconductor component | |
| CN109320251B (en) | Preparation method of high-performance pressureless sintering silicon carbide composite ceramic | |
| CN112830798B (en) | Preparation method of boron carbide granulation powder for pressureless sintering | |
| CN112125653A (en) | Graphene ceramic composite material prepared based on 3D printing and preparation method thereof | |
| CN104045350A (en) | Method for preparing silicon nitride /silicon carbide ceramic composite by use of reaction sintering process | |
| CN107937792B (en) | Gradient composite ceramic cutter material and preparation method thereof | |
| CN113121237A (en) | Boron carbide-based composite ceramic and preparation process thereof | |
| CN113416076A (en) | Preparation method of self-reinforced silicon carbide ceramic material | |
| CN101734920B (en) | Titanium nitride porous ceramics and preparation method thereof | |
| CN113416077B (en) | High-temperature ceramic cutter material with double composite structure and preparation method and application thereof | |
| CN115536403A (en) | High-toughness silicon nitride ceramic material and preparation method thereof | |
| KR20190048811A (en) | Method for manufacturing silicon carbide dense bodies having excellent thermal conductivity and thermal durability | |
| CN109467442B (en) | Silicon nitride ceramic and preparation method thereof | |
| CN116217233B (en) | Complex-phase ceramic of SiC whisker and high-entropy boride hardened and toughened high-entropy carbide, and preparation method and application thereof | |
| CN115557793B (en) | High-entropy ceramic with fine grains, high hardness and high toughness, and preparation method and application thereof | |
| CN110963812A (en) | Preparation method of carbon nano tube toughened silicon carbide ceramic | |
| CN115521151A (en) | Discharge plasma sintering method of silicon carbide/tantalum carbide toughened ceramic | |
| CN114516756B (en) | Silicon carbide composite ceramic material and preparation method and application thereof | |
| CN109851329A (en) | A kind of fine grain Al2O3/ SiC composite ceramic tool material and preparation process | |
| CN108503370A (en) | A kind of single-phase silicon nitride ceramics and its SPS preparation processes |
Legal Events
| Date | Code | Title | Description |
|---|---|---|---|
| PB01 | Publication | ||
| PB01 | Publication | ||
| SE01 | Entry into force of request for substantive examination | ||
| SE01 | Entry into force of request for substantive examination |