CN115974557B - ZrSi-Ti-based alloy 3 SiC 2 High-toughness composite ceramic as well as preparation method and application thereof - Google Patents
ZrSi-Ti-based alloy 3 SiC 2 High-toughness composite ceramic as well as preparation method and application thereof Download PDFInfo
- Publication number
- CN115974557B CN115974557B CN202211231975.6A CN202211231975A CN115974557B CN 115974557 B CN115974557 B CN 115974557B CN 202211231975 A CN202211231975 A CN 202211231975A CN 115974557 B CN115974557 B CN 115974557B
- Authority
- CN
- China
- Prior art keywords
- powder
- sic
- zrsi
- ceramic
- composite ceramic
- 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.)
- Active
Links
Classifications
-
- Y—GENERAL TAGGING OF NEW TECHNOLOGICAL DEVELOPMENTS; GENERAL TAGGING OF CROSS-SECTIONAL TECHNOLOGIES SPANNING OVER SEVERAL SECTIONS OF THE IPC; TECHNICAL SUBJECTS COVERED BY FORMER USPC CROSS-REFERENCE ART COLLECTIONS [XRACs] AND DIGESTS
- Y02—TECHNOLOGIES OR APPLICATIONS FOR MITIGATION OR ADAPTATION AGAINST CLIMATE CHANGE
- Y02E—REDUCTION OF GREENHOUSE GAS [GHG] EMISSIONS, RELATED TO ENERGY GENERATION, TRANSMISSION OR DISTRIBUTION
- Y02E30/00—Energy generation of nuclear origin
- Y02E30/30—Nuclear fission reactors
Landscapes
- Ceramic Products (AREA)
Abstract
ZrSi-Ti-based alloy 3 SiC 2 High-toughness composite ceramic, and a preparation method and application thereof. The application belongs to the field of complex phase ceramic materials. The application aims to solve the technical problem that the existing titanium carbide-silicon carbide composite ceramic cannot achieve both sinterability and excellent fracture toughness. The composite ceramic of the application is made of TiC x Phase, siC phase, (Zr, ti) C x Solid solution phase ZrSi phase, ti 3 SiC 2 Phase composition. The method comprises the following steps: step 1: mixing TiC powder, si powder and ZrC powder to obtain mixed powder, adding absolute ethyl alcohol for ultrasonic treatment, ball-milling and mixing under the protection of inert gas, drying and sieving to obtain ceramic powder; step 2: hot-pressing and sintering the ceramic powder to obtain ZrSi-Ti-based ceramic powder 3 SiC 2 Is a high-toughness composite ceramic. The application relates to a ZrSi-Ti-based alloy 3 SiC 2 The high-toughness composite ceramic is used for preparing cutters, molds and aerospace materials.
Description
Technical Field
The application belongs to the field of complex phase ceramic materials, and in particular relates to a composite material based on ZrSi-Ti 3 SiC 2 High-toughness composite ceramic, and a preparation method and application thereof.
Background
Titanium carbide (TiC) has excellent comprehensive properties such as high melting point, high hardness, good chemical stability and the like, but single TiC material has insufficient wear resistance, extremely low conductivity and large thermal expansion coefficient, and cannot meet certain specific requirements (such as mechanical manufacturing industry, aerospace and the like) in industrial production. If TiC can be combined with other rigid inert particles to make up for the performance defects of TiC, the application range of TiC is widened.
TiC and SiC phase are compounded, so that the problem of insufficient performance of TiC can be solved, and complementation of performances of two materials can be realized. However, due to their covalent bonding properties and low self-diffusion coefficient, complex phase ceramics have poor sinterability and fracture toughness, and further wide use thereof in many fields such as superhard tool materials, microelectronic materials, nuclear energy storage materials, and coating materials is limited.
In recent years, many efforts have been made to improve sinterability of titanium carbide-silicon composite ceramics, and chinese patent publication No. CN102390999a discloses a liquid phase sintered SiC-TiC composite ceramic composed of 15 to 50wt% of titanium carbide, 40 to 80wt% of silicon carbide, 5 to 10wt% of sintering aid Al, and a method for preparing the same 2 O 3 And Y 2 O 3 The composition is obtained by proportioning, pulping, forming, drying and sintering, the normal temperature flexural strength of the SiC-TiC composite ceramic is improved to 580Mpa, and the fracture toughness is improved to 7.8 Mpa.m 1/2 However, the ceramic prepared by the method has higher sintering temperature (1850-2000 ℃) and low density, and meanwhile, the inherent performance of the material is damaged by introducing additives with different or larger performances, so that the problems of unsatisfactory microstructure and performance and the like of the sintered material are caused. Therefore, how to reduce the sintering temperature of the ceramic and ensure the ceramic to have higher density at the same time, and especially how to ensure the toughness is a problem to be solved urgently.
Disclosure of Invention
The application aims to solve the technical problem that the existing titanium carbide-silicon carbide composite ceramic cannot achieve both sinterability and excellent fracture toughness, and provides a ceramic based on ZrSi-Ti 3 SiC 2 High-toughness composite ceramic, and a preparation method and application thereof.
The application relates to a ZrSi-Ti-based alloy 3 SiC 2 Is made of TiC x Phase, siC phase, (Zr, ti) C x Solid solution phase, ti 3 SiC 2 Phase and ZrSi phase.
Further defined, the ZrSi-Ti-based alloy 3 SiC 2 The high-toughness composite ceramic (calculated by the total mole percentage content being 100%) is prepared from 40-60% of TiC powder, 20-40% of Si powder and 10-30% of ZrC powder.
Further defined, the TiC powder, si powder and ZrC powder have a particle size of 1-3 μm.
The application relates to a ZrSi-Ti-based alloy 3 SiC 2 The preparation method of the high-toughness composite ceramic comprises the following steps:
step 1: mixing TiC powder, si powder and ZrC powder to obtain mixed powder, adding absolute ethyl alcohol for ultrasonic treatment, ball-milling and mixing under the protection of inert gas, drying and sieving to obtain ceramic powder;
step 2: hot-pressing and sintering the ceramic powder to obtain ZrSi-Ti-based ceramic powder 3 SiC 2 Is a high-toughness composite ceramic.
Further defined, the volume ratio of the mass of the mixed powder to the absolute ethyl alcohol in the step 1 is 25g: (10-15) mL.
Further defined, the frequency of the ultrasound in step 1 is 30-40kHz and the time is 10-30min.
Further defined, the ball to material ratio in step 1 is (5-50): 1, the ball milling rotating speed is 200-300rpm, and the ball milling time is 5-30h.
Further limited, the drying temperature in the step 1 is 50-70 ℃ and the time is 1-5h.
Further defined, step 1 is screened through a 200 mesh screen.
Further defined, the hot press sintering process in step 2: heating to 500-700 ℃ at a heating rate of 20-40 ℃/min, heating to 1300-1600 ℃ at a heating rate of 15-25 ℃/min, preserving heat for 0.5-3h at 1300-1600 ℃, cooling to room temperature at a heating rate of 10-30 ℃/min, pressurizing to 20-60 MPa when heating to 500-700 ℃, and maintaining the pressure at the pressure until the heat preservation is finished.
The application relates to a ZrSi-Ti-based alloy 3 SiC 2 The high-toughness composite ceramic is used for preparing cutters, molds and aerospace materials.
Compared with the prior art, the application has the remarkable effects that:
the ZrC powder is introduced, the sintering temperature is obviously reduced by optimizing the proportion of the raw material powder, and meanwhile, the composite ceramic final product is ensured to have excellent mechanical properties, and the method has the following specific advantages:
1) The application aims at compounding by regulating and controlling the formula and the process of the composite ceramicFormation of ZrSi phase and Ti in composite ceramics 3 SiC 2 The two new phases are generated, the new phase structure is finer, and the ZrSi phase and the Ti phase are generated while the densification is improved 3 SiC 2 The phases are dispersed and distributed among other phases, and the thermal expansion coefficients of the phases are different, so that cracks can deflect among interfaces of different ceramic phases in the breaking process of the material, and the breaking toughness of the composite ceramic is greatly improved.
2) The composite ceramic prepared by the application adopts TiCx, siC, (Zr, ti) Cx solid solution and Ti 3 SiC 2 The phase, zrSi and other components effectively improve the hardness and strength of the composite ceramic through a solid solution strengthening mechanism, and the generated Ti 3 SiC 2 The phase may enhance the processability of the composite, pushing it into further wider applications.
Drawings
FIG. 1 is an XRD schematic diagram of the composite ceramic prepared in example 3;
FIG. 2 is a schematic cross-sectional SEM of a composite ceramic prepared in example 3;
FIG. 3 is a SEM schematic of crack propagation of the composite ceramic prepared in example 3.
Detailed Description
The present application will be described in further detail with reference to the following examples in order to make the objects, technical solutions and advantages of the present application more apparent. It should be understood that the specific embodiments described herein are for purposes of illustration only and are not intended to limit the scope of the application.
The experimental methods used in the following examples are conventional methods unless otherwise specified. The materials, reagents, methods and apparatus used, without any particular description, are those conventional in the art and are commercially available to those skilled in the art.
The terms "comprising," "including," "having," "containing," or any other variation thereof, as used in the following embodiments, are intended to cover a non-exclusive inclusion. For example, a composition, step, method, article, or apparatus that comprises a list of elements is not necessarily limited to only those elements but may include other elements not expressly listed or inherent to such composition, step, method, article, or apparatus.
When an equivalent, concentration, or other value or parameter is expressed as a range, preferred range, or a range bounded by a list of upper preferable values and lower preferable values, this is to be understood as specifically disclosing all ranges formed from any pair of any upper range limit or preferred value and any lower range limit or preferred value, regardless of whether ranges are separately disclosed. For example, when ranges of "1 to 5" are disclosed, the described ranges should be construed to include ranges of "1 to 4", "1 to 3", "1 to 2 and 4 to 5", "1 to 3 and 5", and the like. When a numerical range is described herein, unless otherwise indicated, the range is intended to include its endpoints and all integers and fractions within the range. In the description and claims of the application, the range limitations may be combined and/or interchanged, if not otherwise specified, including all the sub-ranges subsumed therein.
The indefinite articles "a" and "an" preceding an element or component of the application are not limited to the requirement (i.e. the number of occurrences) of the element or component. Thus, the use of "a" or "an" should be interpreted as including one or at least one, and the singular reference of an element or component includes the plural reference unless the amount clearly dictates otherwise.
Example 1: the preparation method of the high-strength high-hardness high-toughness composite ceramic comprises the following steps:
step 1: mixing 10% zirconium carbide powder (particle size of 1-3 μm), 54% titanium carbide powder (particle size of 1-3 μm) and 36% silicon powder (particle size of 1-3 μm) into a polyethylene mixing tank according to mole percentage to obtain 25g mixed powder, adding 10mL of absolute ethyl alcohol, performing ultrasonic treatment at 35kHz for 10min, and adding Si 3 N 4 Ball grinding, placing the mixing tank on a rolling ball feeder, ball milling and mixing under the protection of inert gas, wherein the ball-to-material ratio is 40:1, ball milling at the ball milling rotating speed of 250r/min for 24 hours, then rotary steaming to remove absolute ethyl alcohol, then placing the absolute ethyl alcohol in an oven to dry for 2 hours at 60 ℃, and sieving the absolute ethyl alcohol with a 200-mesh sieve to obtain ceramic powder;
step 2: and (3) carrying out hot-pressing sintering on the ceramic powder, firstly heating to 600 ℃ at a heating rate of 30 ℃/min, then heating to 1400 ℃ at a heating rate of 20 ℃/min, preserving heat for 1h at 1400 ℃, then cooling to room temperature at a heating rate of 20 ℃/min, pressurizing to 30MPa when heating to 600 ℃, and maintaining the pressure at the pressure until preserving heat to obtain the high-strength high-hardness high-toughness composite ceramic.
Example 2: the preparation method of the high-strength high-hardness high-toughness composite ceramic comprises the following steps:
step 1: mixing 10% zirconium carbide powder (particle size of 1-3 μm), 54% titanium carbide powder (particle size of 1-3 μm) and 36% silicon powder (particle size of 1-3 μm) into a polyethylene mixing tank according to mole percentage to obtain 25g mixed powder, adding 10mL of absolute ethyl alcohol, performing ultrasonic treatment at 35kHz for 10min, and adding Si 3 N 4 Ball grinding, placing the mixing tank on a rolling ball feeder, ball milling and mixing under the protection of inert gas, wherein the ball-to-material ratio is 40:1, ball milling at the ball milling rotating speed of 250r/min for 24 hours, then rotary steaming to remove absolute ethyl alcohol, then placing the absolute ethyl alcohol in an oven to dry for 2 hours at 60 ℃, and sieving the absolute ethyl alcohol with a 200-mesh sieve to obtain ceramic powder;
step 2: and (3) carrying out hot-pressing sintering on the ceramic powder, firstly heating to 600 ℃ at a heating rate of 30 ℃/min, then heating to 1500 ℃ at a heating rate of 20 ℃/min, preserving heat for 1h at 1500 ℃, then cooling to room temperature at a heating rate of 20 ℃/min, pressurizing to 30MPa when heating to 600 ℃, and maintaining the pressure at the pressure until preserving heat to obtain the high-strength high-hardness high-toughness composite ceramic.
Example 3: the preparation method of the high-strength high-hardness high-toughness composite ceramic comprises the following steps:
step 1: mixing 10% zirconium carbide powder (particle size of 1-3 μm), 54% titanium carbide powder (particle size of 1-3 μm) and 36% silicon powder (particle size of 1-3 μm) into a polyethylene mixing tank according to mole percentage to obtain 25g mixed powder, adding 10mL of absolute ethyl alcohol, performing ultrasonic treatment at 35kHz for 10min, and adding Si 3 N 4 Grinding balls, placing the mixing tank on a rolling ball feeder, ball milling and mixing under the protection of inert gas, wherein the ball-to-material ratio is 40:1, ball milling at the ball milling rotating speed of 250r/min for 24 hours, then rotary steaming to remove absolute ethyl alcohol, then placing the absolute ethyl alcohol in an oven to dry for 2 hours at 60 ℃, and sieving the absolute ethyl alcohol with a 200-mesh sieve to obtain ceramic powder;
step 2: and (3) carrying out hot-pressing sintering on the ceramic powder, firstly heating to 600 ℃ at a heating rate of 30 ℃/min, then heating to 1600 ℃ at a heating rate of 20 ℃/min, preserving heat for 1h at 1600 ℃, then cooling to room temperature at a heating rate of 20 ℃/min, pressurizing to 30MPa when heating to 600 ℃, and maintaining the pressure at the pressure until preserving heat to obtain the high-strength high-hardness high-toughness composite ceramic.
XRD test is carried out on the obtained high-strength high-hardness high-toughness composite ceramic, and the test result is shown in figure 1. As can be seen from FIG. 1, the sintered product is composed of TiC x Phase, siC phase, (Zr, ti) C x Solid solution phase, zrSi phase, ti 3 SiC 2 Phase composition.
SEM test is carried out on the fracture of the obtained high-strength high-hardness high-toughness composite ceramic, and the test result is shown in figure 2. As can be seen from FIG. 2, the obtained grains of each phase of the reaction sintering are fine and dispersed, the composite ceramic is sintered compactly, and the layered Ti is 3 SiC 2 Both the existence of the (C) and the crystal-through fracture mode are improved for the strength of the material.
SEM test is carried out on crack propagation of the obtained high-strength high-hardness high-strength-toughness composite ceramic, and the test result is shown in figure 3. As can be seen from fig. 3, the material has obvious bridging and deflection in the crack propagation process, and has good effect on toughening the material.
Example 4: the preparation method of the high-strength high-hardness high-toughness composite ceramic comprises the following steps:
step 1: mixing 30% zirconium carbide powder (particle size of 1-3 μm), 42% titanium carbide powder (particle size of 1-3 μm) and 28% silicon powder (particle size of 1-3 μm) into a polyethylene mixing tank according to mole percentage to obtain 25g mixed powder, adding 10mL of absolute ethyl alcohol, performing ultrasonic treatment at 35kHz for 10min, and adding Si 3 N 4 Ball grinding, placing the mixing tank on a rolling ball feeder, ball milling and mixing under the protection of inert gas, wherein the ball-to-material ratio is 40:1, ball milling at a ball milling rotation speed of 250r/min for 24 hours, and then spin steaming to remove anhydrousEthanol, drying in an oven at 60 ℃ for 2 hours, and sieving with a 200-mesh sieve to obtain ceramic powder;
step 2: and (3) carrying out hot-pressing sintering on the ceramic powder, firstly heating to 600 ℃ at a heating rate of 30 ℃/min, then heating to 1400 ℃ at a heating rate of 20 ℃/min, preserving heat for 1h at 1400 ℃, then cooling to room temperature at a heating rate of 20 ℃/min, pressurizing to 30MPa when heating to 600 ℃, and maintaining the pressure at the pressure until preserving heat to obtain the high-strength high-hardness high-toughness composite ceramic.
Example 5: the preparation method of the high-strength high-hardness high-toughness composite ceramic comprises the following steps:
step 1: mixing 30% zirconium carbide powder (particle size of 1-3 μm), 42% titanium carbide powder (particle size of 1-3 μm) and 28% silicon powder (particle size of 1-3 μm) into a polyethylene mixing tank according to mole percentage to obtain 25g mixed powder, adding 10mL of absolute ethyl alcohol, performing ultrasonic treatment at 35kHz for 10min, and adding Si 3 N 4 Ball grinding, placing the mixing tank on a rolling ball feeder, ball milling and mixing under the protection of inert gas, wherein the ball-to-material ratio is 40:1, ball milling at the ball milling rotating speed of 250r/min for 24 hours, then rotary steaming to remove absolute ethyl alcohol, then placing the absolute ethyl alcohol in an oven to dry for 2 hours at 60 ℃, and sieving the absolute ethyl alcohol with a 200-mesh sieve to obtain ceramic powder;
step 2: and (3) carrying out hot-pressing sintering on the ceramic powder, firstly heating to 600 ℃ at a heating rate of 30 ℃/min, then heating to 1500 ℃ at a heating rate of 20 ℃/min, preserving heat for 1h at 1500 ℃, then cooling to room temperature at a heating rate of 20 ℃/min, pressurizing to 30MPa when heating to 600 ℃, and maintaining the pressure at the pressure until preserving heat to obtain the high-strength high-hardness high-toughness composite ceramic.
Example 6: the preparation method of the high-strength high-hardness high-toughness composite ceramic comprises the following steps:
step 1: mixing 30% zirconium carbide powder (particle size of 1-3 μm), 42% titanium carbide powder (particle size of 1-3 μm) and 28% silicon powder (particle size of 1-3 μm) into a polyethylene mixing tank according to mole percentage to obtain 25g mixed powder, adding 10mL of absolute ethyl alcohol, performing ultrasonic treatment at 35kHz for 10min, and adding Si 3 N 4 Ball grinding, placing the mixing tank on a rolling ball feeder, ball milling and mixing under the protection of inert gas, wherein the ball-to-material ratio is 40:1, ball milling at the ball milling rotating speed of 250r/min for 24 hours, then rotary steaming to remove absolute ethyl alcohol, then placing the absolute ethyl alcohol in an oven to dry for 2 hours at 60 ℃, and sieving the absolute ethyl alcohol with a 200-mesh sieve to obtain ceramic powder;
step 2: and (3) carrying out hot-pressing sintering on the ceramic powder, firstly heating to 600 ℃ at a heating rate of 30 ℃/min, then heating to 1600 ℃ at a heating rate of 20 ℃/min, preserving heat for 1h at 1600 ℃, then cooling to room temperature at a heating rate of 20 ℃/min, pressurizing to 30MPa when heating to 600 ℃, and maintaining the pressure at the pressure until preserving heat to obtain the high-strength high-hardness high-toughness composite ceramic.
Comparative example 1: the preparation method of the composite ceramic comprises the following steps:
step 1: mixing 60% titanium carbide powder (particle size of 1-3 μm) and 40% silicon powder (particle size of 1-3 μm) into polyethylene mixing tank according to mole percentage to obtain 25g mixed powder, adding 10mL absolute ethanol, ultrasonic treating at 35kHz for 10min, and adding Si 3 N 4 Ball grinding, placing the mixing tank on a rolling ball feeder, ball milling and mixing under the protection of inert gas, wherein the ball-to-material ratio is 40:1, ball milling at the ball milling rotating speed of 250r/min for 24 hours, then rotary steaming to remove absolute ethyl alcohol, then placing the absolute ethyl alcohol in an oven to dry for 2 hours at 60 ℃, and sieving the absolute ethyl alcohol with a 200-mesh sieve to obtain ceramic powder;
step 2: and (3) carrying out hot-pressing sintering on the ceramic powder, firstly heating to 600 ℃ at a heating rate of 30 ℃/min, then heating to 1400 ℃ at a heating rate of 20 ℃/min, preserving heat for 1h at 1400 ℃, then cooling to room temperature at a heating rate of 20 ℃/min, pressurizing to 30MPa when heating to 600 ℃, and maintaining the pressure at the pressure until the heat preservation is finished to obtain the titanium carbide-silicon carbide ceramic.
Comparative example 2: the preparation method of the composite ceramic comprises the following steps:
step 1: mixing 60% titanium carbide powder (particle size of 1-3 μm) and 40% zirconium carbide powder (particle size of 1-3 μm) into polyethylene mixing tank to obtain 25g mixed powder, adding 10mL absolute ethanol, and standing at 35kHzSonicating for 10min, then adding Si 3 N 4 Ball grinding, placing the mixing tank on a rolling ball feeder, ball milling and mixing under the protection of inert gas, wherein the ball-to-material ratio is 40:1, ball milling at the ball milling rotating speed of 250r/min for 24 hours, then rotary steaming to remove absolute ethyl alcohol, then placing the absolute ethyl alcohol in an oven to dry for 2 hours at 60 ℃, and sieving the absolute ethyl alcohol with a 200-mesh sieve to obtain ceramic powder;
step 2: and (3) carrying out hot-pressing sintering on the ceramic powder, firstly heating to 600 ℃ at a heating rate of 30 ℃/min, then heating to 1400 ℃ at a heating rate of 20 ℃/min, preserving heat for 1h at 1400 ℃, then cooling to room temperature at a heating rate of 20 ℃/min, pressurizing to 30MPa when heating to 600 ℃, and maintaining the pressure at the pressure until the heat preservation is finished to obtain the titanium carbide-zirconium carbide ceramic.
Detection test:
mechanical test analysis of the composite ceramics of examples 1 to 6 and the ceramics of comparative examples 1 to 2 was performed using a ceramic having a size of 2X 4X 25mm 3 The bending strength was measured by a three-point bending test on an Instron-1186 machine with a span of 20mm and a ram speed of 0.5mm/min, and the results are shown in Table 1.
(II) hardness tests were conducted on the composite ceramics of examples 1 to 6 and the ceramics of comparative examples 1 to 2, and the Vickers hardness was measured under an external load of 9.8N using the Vickers indentation test, with a residence time of 10s. The results are shown in Table 1.
TABLE 1 sample Performance test data for examples 1-6, comparative examples 1-2
| Flexural Strength (MPa) | Vickers hardness (GPa) | Fracture toughness (MPa.m) 1/2 ) | |
| Example 1 | 606±8 | 17.6±1.3 | 6.4±0.2 |
| Example 2 | 580±34 | 20.2±1.2 | 6.7±0.3 |
| Example 3 | 548±38 | 25.7±1.5 | 5.5±0.5 |
| Example 4 | 500±45 | 20.6±1.7 | 4.6±0.5 |
| Example 5 | 540±44 | 24.4±0.8 | 5.6±0.4 |
| Example 6 | 577±34 | 23.8±1.2 | 5.1±0.2 |
| Comparative example 1 | 501±63 | 13.9±0.8 | 4.0±0.8 |
| Comparative example 2 | 313±21 | 16.1±0.9 | 3.5±0.8 |
In the foregoing, the present application is merely preferred embodiments, which are based on different implementations of the overall concept of the application, and the protection scope of the application is not limited thereto, and any changes or substitutions easily come within the technical scope of the present application as those skilled in the art should not fall within the protection scope of the present application. Therefore, the protection scope of the present application should be subject to the protection scope of the claims.
Claims (9)
1. ZrSi-Ti-based alloy 3 SiC 2 Is characterized in that the high-toughness composite ceramic consists of TiC x Phase, siC phase, (Zr, ti) C x Solid solution phase, zrSi phase, ti 3 SiC 2 The phase composition is prepared from 54% of TiC powder, 36% of Si powder and 10% of ZrC powder by mol content.
2. A ZrSi-Ti based alloy according to claim 1 3 SiC 2 The high-toughness composite ceramic is characterized in that the granularity of TiC powder, si powder and ZrC powder is 1-3 mu m.
3. ZrSi-Ti based according to any one of claims 1-2 3 SiC 2 The preparation method of the high-toughness composite ceramic is characterized by comprising the following steps:
step 1: mixing TiC powder, si powder and ZrC powder to obtain mixed powder, adding absolute ethyl alcohol for ultrasonic treatment, ball-milling and mixing under the protection of inert gas, drying and sieving to obtain ceramic powder;
step 2: hot-pressing and sintering the ceramic powder to obtain a baseIn ZrSi-Ti 3 SiC 2 Is a high-toughness composite ceramic.
4. The method according to claim 3, wherein the volume ratio of the mass of the mixed powder to the absolute ethanol in the step 1 is 25g: (10-15) mL.
5. A method according to claim 3, wherein the ultrasound in step 1 has a frequency of 30-40kHz for a period of 10-30min.
6. A method according to claim 3, wherein the ball to material ratio in step 1 is (5-50): 1, the ball milling rotating speed is 200-300rpm, and the ball milling time is 5-30h.
7. A method according to claim 3, wherein in step 1 the drying temperature is 50-70 ℃ and the time is 1-5h, and the drying is carried out by sieving with a 200 mesh sieve.
8. A method according to claim 3, characterized in that the hot-press sintering process in step 2: heating to 500-700 ℃ at a heating rate of 20-40 ℃/min, heating to 1300-1600 ℃ at a heating rate of 15-25 ℃/min, preserving heat at 1300-1600 ℃ for 0.5-3h, cooling to room temperature at a heating rate of 10-30 ℃/min, pressurizing to 20-60 MPa when heating to 500-700 ℃, and maintaining the pressure at the pressure until the heat preservation is finished.
9. ZrSi-Ti based according to any one of claims 1-2 3 SiC 2 The high-toughness composite ceramic is used for preparing cutters, molds and aerospace materials.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN202211231975.6A CN115974557B (en) | 2022-10-10 | 2022-10-10 | ZrSi-Ti-based alloy 3 SiC 2 High-toughness composite ceramic as well as preparation method and application thereof |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN202211231975.6A CN115974557B (en) | 2022-10-10 | 2022-10-10 | ZrSi-Ti-based alloy 3 SiC 2 High-toughness composite ceramic as well as preparation method and application thereof |
Publications (2)
| Publication Number | Publication Date |
|---|---|
| CN115974557A CN115974557A (en) | 2023-04-18 |
| CN115974557B true CN115974557B (en) | 2023-08-15 |
Family
ID=85974684
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| CN202211231975.6A Active CN115974557B (en) | 2022-10-10 | 2022-10-10 | ZrSi-Ti-based alloy 3 SiC 2 High-toughness composite ceramic as well as preparation method and application thereof |
Country Status (1)
| Country | Link |
|---|---|
| CN (1) | CN115974557B (en) |
Citations (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101343183A (en) * | 2007-07-13 | 2009-01-14 | 中国科学院金属研究所 | Zirconium titanium carbide particle reinforced silicon aluminum titanium carbide zirconium based composite material and preparation thereof |
| JP2009107909A (en) * | 2007-10-31 | 2009-05-21 | National Institute Of Advanced Industrial & Technology | Method for producing fine crystal particle titanium silicon carbide ceramic |
| CN109868475A (en) * | 2019-01-23 | 2019-06-11 | 中国科学院宁波材料技术与工程研究所 | Cladding nuclear fuels and preparation method thereof, nuclear fuel assembly |
| CN113480313A (en) * | 2021-08-06 | 2021-10-08 | 航天特种材料及工艺技术研究所 | MXene toughened ultrahigh-temperature ceramic composite material and preparation method thereof |
-
2022
- 2022-10-10 CN CN202211231975.6A patent/CN115974557B/en active Active
Patent Citations (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101343183A (en) * | 2007-07-13 | 2009-01-14 | 中国科学院金属研究所 | Zirconium titanium carbide particle reinforced silicon aluminum titanium carbide zirconium based composite material and preparation thereof |
| JP2009107909A (en) * | 2007-10-31 | 2009-05-21 | National Institute Of Advanced Industrial & Technology | Method for producing fine crystal particle titanium silicon carbide ceramic |
| CN109868475A (en) * | 2019-01-23 | 2019-06-11 | 中国科学院宁波材料技术与工程研究所 | Cladding nuclear fuels and preparation method thereof, nuclear fuel assembly |
| CN113480313A (en) * | 2021-08-06 | 2021-10-08 | 航天特种材料及工艺技术研究所 | MXene toughened ultrahigh-temperature ceramic composite material and preparation method thereof |
Non-Patent Citations (1)
| Title |
|---|
| 李良 ; 周爱国 ; .Ti_3SiC_2复合材料的研究进展.硅酸盐通报.2011,(05),第1114-1117、1141页. * |
Also Published As
| Publication number | Publication date |
|---|---|
| CN115974557A (en) | 2023-04-18 |
Similar Documents
| Publication | Publication Date | Title |
|---|---|---|
| CN110483085B (en) | Whisker reinforced alumina composite ceramic and preparation method and application thereof | |
| US11634364B2 (en) | Boron carbide composite and production method therefor | |
| EP0414910B1 (en) | Alumina ceramic, production thereof, and throwaway tip made therefrom | |
| CN108624772B (en) | Ultra-fine grain tungsten carbide-based hard alloy material and preparation method thereof | |
| CN110655407A (en) | Preparation method of silicon carbide ceramic with controllable resistance | |
| KR102533534B1 (en) | Tungsten carbide-based cemented carbide and manufacturing method thereof | |
| CN111646801B (en) | Boron carbide-tungsten carbide composite ceramic gradient material for cutter and preparation method and application thereof | |
| CN107523710A (en) | A kind of whisker modified Ti (C, N) based composite metal ceramic preparation of resistance to high temperature oxidation | |
| CN113416077B (en) | High-temperature ceramic cutter material with double composite structure and preparation method and application thereof | |
| CN105645963A (en) | Recrystallized silicon carbide product and preparation method thereof | |
| CN112500167A (en) | Preparation method of densified titanium carbide composite ceramic | |
| CN109811177A (en) | A kind of preparation method of highly conductive high-intensitive silver-graphene composite material | |
| US4425141A (en) | Composite ceramic cutting tool | |
| CN109354504B (en) | Boron carbide-based composite ceramic sintering aid and sintering process | |
| CN115974557B (en) | ZrSi-Ti-based alloy 3 SiC 2 High-toughness composite ceramic as well as preparation method and application thereof | |
| CN113929463B (en) | Method for preparing titanium secondary group carbonitride solid solution multiphase ceramic material by sintering method | |
| CN109650922B (en) | SU-304L metal reinforced silicon carbide-based composite ceramic material and preparation method of master batch thereof | |
| CN109851329A (en) | A kind of fine grain Al2O3/ SiC composite ceramic tool material and preparation process | |
| JPS61146762A (en) | Antiabrasive silicon nitride base product | |
| CA1285582C (en) | Ceramic based composites with improved fracture toughness | |
| CN105903972B (en) | A kind of diamond compact and preparation method thereof | |
| CN118326191B (en) | Alumina ceramic grinding ball with adjustable specific gravity and preparation method thereof | |
| EP0095129B1 (en) | Composite ceramic cutting tool and process for making same | |
| CN115321988A (en) | Fiber-reinforced silicon nitride ceramic composite material and preparation method thereof | |
| CN115386759B (en) | Ti (C) 7 ,N 3 )/TiB 2 WC micro-nano composite metal ceramic cutter material and preparation method thereof |
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 | ||
| GR01 | Patent grant | ||
| GR01 | Patent grant |