CN111217610A - Nanocrystalline tantalum carbide reinforced silicon-boron-carbon-nitrogen composite ceramic material and preparation method thereof - Google Patents
Nanocrystalline tantalum carbide reinforced silicon-boron-carbon-nitrogen composite ceramic material and preparation method thereof Download PDFInfo
- Publication number
- CN111217610A CN111217610A CN201910532639.7A CN201910532639A CN111217610A CN 111217610 A CN111217610 A CN 111217610A CN 201910532639 A CN201910532639 A CN 201910532639A CN 111217610 A CN111217610 A CN 111217610A
- Authority
- CN
- China
- Prior art keywords
- tantalum carbide
- powder
- nanocrystalline
- ceramic material
- boron
- 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
- C04B35/58—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 borides, nitrides, i.e. nitrides, oxynitrides, carbonitrides or oxycarbonitrides or silicides
-
- 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
- C04B35/622—Forming processes; Processing powders of inorganic compounds preparatory to the manufacturing of ceramic products
- C04B35/64—Burning or sintering processes
- C04B35/645—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
- C04B2235/30—Constituents and secondary phases not being of a fibrous nature
- C04B2235/38—Non-oxide ceramic constituents or additives
- C04B2235/3852—Nitrides, e.g. oxynitrides, carbonitrides, oxycarbonitrides, lithium nitride, magnesium nitride
- C04B2235/386—Boron nitrides
-
- 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
- C04B2235/42—Non metallic elements added as constituents or additives, e.g. sulfur, phosphor, selenium or tellurium
- C04B2235/422—Carbon
- C04B2235/425—Graphite
-
- 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
- C04B2235/42—Non metallic elements added as constituents or additives, e.g. sulfur, phosphor, selenium or tellurium
- C04B2235/428—Silicon
-
- 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 provides a nanocrystalline tantalum carbide reinforced silicon-boron-carbon-nitrogen composite ceramic material and a preparation method thereof, wherein the preparation method comprises the following steps: s1: preparing nanocrystalline tantalum carbide powder; s2: mixing the nanocrystalline tantalum carbide powder, hexagonal boron nitride, cubic silicon powder and graphite according to a preset proportion, and then carrying out high-energy ball milling to obtain composite powder; s3: and carrying out hot-pressing sintering on the composite powder to obtain the nanocrystalline tantalum carbide reinforced silicon-boron-carbon-nitrogen composite ceramic material. The invention takes silicon boron carbon nitrogen ceramic as a substrate, and adds a tantalum carbide reinforced phase to prepare a nanocrystalline tantalum carbide reinforced silicon boron carbon nitrogen complex phase ceramic material, and ultra-high temperature phase tantalum carbide particles are uniformly dispersed in an amorphous silicon boron carbon nitrogen substrate in a nanocrystalline form, so that the function of pinning crack expansion can be achieved, the mechanical property of the silicon boron carbon nitrogen ceramic is improved, and meanwhile, the ultra-high temperature property of tantalum carbide reinforces the silicon boron carbon nitrogen ceramic, so that the high temperature resistance of the complex phase ceramic material is improved, and the complex phase ceramic material can be in service at higher temperature.
Description
Technical Field
The invention relates to the field of ceramics, in particular to a nanocrystalline tantalum carbide reinforced silicon-boron-carbon-nitrogen composite ceramic material and a preparation method thereof.
Background
The rapid development of aerospace technology puts more rigorous requirements on the service performance of high-temperature structural materials. In recent years, silicon-boron-carbon-nitrogen ceramic is used as a novel quaternary structure ceramic, and the covalent structure of the silicon-boron-carbon-nitrogen ceramic endows the silicon-boron-carbon-nitrogen ceramic with good thermal stability, high-temperature oxidation resistance and creep resistance; in addition, the silicon-boron-carbon-nitrogen ceramic has the advantages of low elastic modulus, good thermal shock resistance, low density and the like, so that the silicon-boron-carbon-nitrogen ceramic has a very wide application prospect in the field of aerospace.
However, the silicon boron carbon nitrogen (SiBCN) ceramic has serious thermal damage at high temperature, and the intrinsic brittleness of the silicon boron carbon nitrogen ceramic greatly limits the wide application in the field of ultrahigh temperature. Therefore, it is a research direction to introduce the ultra-high temperature phase into the silicon boron carbon nitrogen ceramic matrix to improve the high temperature resistance of the silicon boron carbon nitrogen ceramic.
The tantalum carbide (TaC) has the advantages of high melting point (3880 ℃), high hardness (20GPa), high elastic modulus (450GPa), good thermal conductivity, chemical corrosion resistance, good thermal shock resistance and the like, and when the TaC is used as an additive phase in a matrix such as C, SiC, the TaC has obvious effects on the enhancement of the mechanical property and the improvement of the high-temperature resistance of the matrix material. The tantalum carbide is introduced into the silicon-boron-carbon-nitrogen ceramic matrix to form the multiphase ceramic with the silicon-boron-carbon-nitrogen, so that no report is provided so far.
Disclosure of Invention
The invention solves the problems that: how to improve the strength, toughness and high temperature resistance of the silicon-boron-carbon-nitrogen ceramic and make the silicon-boron-carbon-nitrogen ceramic applied in more fields.
In order to solve the problems, the invention provides a preparation method of a nanocrystalline tantalum carbide reinforced silicon-boron-carbon-nitrogen composite ceramic material, which comprises the following steps:
s1: preparing nanocrystalline tantalum carbide powder;
s2: mixing the nanocrystalline tantalum carbide powder, hexagonal boron nitride, cubic silicon powder and graphite according to a preset proportion, and then carrying out high-energy ball milling to obtain composite powder;
s3: and carrying out hot-pressing sintering on the composite powder to obtain the nanocrystalline tantalum carbide reinforced silicon-boron-carbon-nitrogen composite ceramic material.
Optionally, the grain size range of the nanocrystalline tantalum carbide powder is less than 20 nm.
Optionally, in step S2, the mass of the nanocrystalline tantalum carbide powder accounts for 1% to 50% of the mass of the composite powder.
Optionally, in step S2, the molar ratio of the cubic silicon powder, the hexagonal boron nitride, and the graphite is Si: BN: c ═ 0.8 to 1.2: (1.5-2.5): (2.8-3.5).
Optionally, in step S1, the specific steps of preparing the nanocrystalline tantalum carbide powder include: under the protection of argon, placing tantalum carbide particles with the particle size of 1-5 microns and grinding balls in a ball mill for ball milling to prepare the nanocrystalline tantalum carbide powder; wherein, the ball milling conditions are as follows: the ball material ratio is (10-40): 1, the rotating speed of the main disc is 200-400 r/min, the rotating speed of the planetary disc is 500-1000 r/min, and the ball milling time is 10-100 h.
Optionally, in step S2, the high-energy ball milling conditions are: the ball material ratio is (10-40): 1, the rotating speed of the main disc is 200-400 r/min, the rotating speed of the planetary disc is 500-1000 r/min, and the ball milling time is 10-100 h.
Optionally, the process conditions of the hot-pressing sintering include: the sintering temperature is 1500-2300 ℃, the sintering pressure is 20-80 Mpa, the sintering time is 20-90 min, and the protective atmosphere is nitrogen or argon or vacuum.
The invention also aims to provide a nanocrystalline tantalum carbide reinforced silicon-boron-carbon-nitrogen complex-phase ceramic material which is prepared by adopting the preparation method of the nanocrystalline tantalum carbide reinforced silicon-boron-carbon-nitrogen complex-phase ceramic material.
Optionally, the composite ceramic material includes a SiBCN matrix phase, the nanocrystalline tantalum carbide is distributed in the SiBCN matrix phase, and the nanocrystalline tantalum carbide grains are separated from each other.
Optionally, the SiBCN matrix phase contains a turbulent-layered BN (C) phase, and the grain size of the nanocrystalline tantalum carbide distributed in the BN (C) phase is 3-5 nm.
Compared with the prior art, the nanocrystalline tantalum carbide reinforced silicon-boron-carbon-nitrogen composite ceramic material and the preparation method thereof have the following advantages:
(1) the invention takes silicon boron carbon nitrogen ceramic as a substrate, and adds a tantalum carbide reinforced phase to prepare a nanocrystalline tantalum carbide reinforced silicon boron carbon nitrogen complex phase ceramic material, and ultra-high temperature phase tantalum carbide particles are uniformly dispersed in an amorphous silicon boron carbon nitrogen substrate in a nanocrystalline form, so that the function of pinning crack expansion can be achieved, the mechanical property of the silicon boron carbon nitrogen ceramic is improved, and meanwhile, the ultra-high temperature property of tantalum carbide reinforces the silicon boron carbon nitrogen ceramic, so that the high temperature resistance of the complex phase ceramic material is improved, and the complex phase ceramic material can be in service at higher temperature.
(2) The nanocrystalline tantalum carbide reinforced silicon-boron-carbon-nitrogen composite ceramic material provided by the invention has a good microstructure, nanocrystalline tantalum carbide powder with the grain diameter of 10-20nm is embedded into an amorphous SiBCN matrix phase, nanocrystalline tantalum carbide powder with the grain diameter range of 3-5nm is dispersed in a BN (C) phase in the amorphous SiBCN matrix phase, and the BN (C) is wrapped around the nanocrystalline tantalum carbide, so that the nanocrystalline tantalum carbide is prevented from growing due to grain curing; the turbulent layered structure composed of BN (C) -TaC can be coated around SiC crystal grains, so that element diffusion is inhibited, abnormal growth of the SiC crystal grains is avoided, the special microstructure enables the nanocrystalline tantalum carbide reinforced silicon-boron-carbon-nitrogen composite ceramic material to keep an amorphous-nanocrystalline structure, and the composite ceramic material has high density, mechanical property and high temperature resistance.
Drawings
The accompanying drawings, which are incorporated in and constitute a part of this specification, illustrate an embodiment of the invention and, together with the description, serve to explain the invention and not to limit the invention. In the drawings:
FIG. 1 is a flow chart of the preparation of the nanocrystalline tantalum carbide reinforced silicon-boron-carbon-nitrogen composite ceramic material;
FIG. 2 is an XRD spectrum of the nano-crystalline tantalum carbide powder after ball milling in the first embodiment;
fig. 3 is an XRD spectrum of the composite powder obtained in step S2 in the first to third embodiments and the comparative example;
FIG. 4 is an XRD (X-ray diffraction) spectrum of the nanocrystalline tantalum carbide reinforced silicon-boron-carbon-nitrogen composite ceramic material prepared after hot-pressing sintering in the first embodiment, the second embodiment and the comparative example;
FIG. 5 is a TEM image of a bulk composite phase ceramic material with nanocrystalline tantalum carbide content prepared according to the second embodiment;
fig. 6 is an EDS energy spectrum of the bulk composite phase ceramic material with nanocrystalline tantalum carbide content prepared in the second embodiment;
FIG. 7 is a graph showing the mechanical properties of complex phase ceramic materials with different nanocrystalline tantalum carbide contents;
FIG. 8 is a TG-DSC curve graph of the complex phase ceramic material with different nanocrystalline tantalum carbide contents in air.
Detailed Description
In addition, the features of the embodiments of the present invention may be combined with each other without conflict. The terms "comprising," "including," "containing," and "having" are intended to be inclusive, i.e., that additional steps and other ingredients may be added without affecting the result. The above terms encompass the terms "consisting of … …" and "consisting essentially of … …". Materials, equipment and reagents are commercially available unless otherwise specified.
In order to make the aforementioned objects, features and advantages of the present invention comprehensible, embodiments accompanied with figures are described in detail below.
Referring to fig. 1, a method for preparing a nanocrystalline tantalum carbide reinforced silicon-boron-carbon-nitrogen composite ceramic material comprises the following steps:
s1: preparing nanocrystalline tantalum carbide powder;
s2: mixing the nanocrystalline tantalum carbide powder, hexagonal boron nitride, cubic silicon powder and graphite according to a preset proportion, and performing high-energy ball milling to obtain composite powder;
s3: and carrying out hot-pressing sintering on the composite powder to obtain the nanocrystalline tantalum carbide reinforced silicon-boron-carbon-nitrogen composite ceramic material.
Firstly, preparing nanocrystalline tantalum carbide powder, in step S1, specifically, weighing tantalum carbide particles with the particle size of 1-5 microns in a glove box filled with argon, putting the weighed tantalum carbide particles into a ball milling tank, adding grinding balls into the ball milling tank, taking out the ball milling tank from the glove box after sealing the ball milling tank, installing the ball milling tank on a planetary high-energy ball mill for first ball milling, taking down the ball milling tank, placing the ball milling tank in the glove box, and taking out the prepared powder to obtain the nanocrystalline tantalum carbide powder.
Wherein the grinding balls are silicon nitride balls, the mass of the added silicon nitride balls is 50-800 g, and the time for the first ball milling is set to be 10-100 h. The basic parameters of the high-energy ball mill are as follows: the ball material ratio is set to (10-40): 1, the rotating speed of the main disk is 200-400 r/min, and the rotating speed of the planetary disk is 500-1000 r/min.
The grain diameter range of the prepared nanocrystalline tantalum carbide powder is less than 20 nm.
In step S2, a mechanical alloying technique is used to mix the nanocrystalline tantalum carbide powder, the hexagonal boron nitride, the cubic silicon powder and the graphite uniformly, and then the mixture is subjected to high-energy ball milling. Specifically, the nanocrystalline tantalum carbide powder prepared in the step S1, hexagonal boron nitride, cubic silicon powder and graphite are weighed in a glove box filled with argon, the weighed nanocrystalline tantalum carbide powder, hexagonal boron nitride, cubic silicon powder and graphite are placed into a ball milling tank together, grinding balls are added into the ball milling tank, the ball milling tank is sealed and then taken out of the glove box, the ball milling tank is installed on a planetary high-energy ball mill for secondary ball milling, finally the ball milling tank is placed in the glove box, the powder is taken out, and the SiBCN-TaC composite powder is obtained and is nanoscale amorphous-nanocrystalline powder.
In step S2, the mass of the nanocrystalline tantalum carbide powder accounts for 1% -50% of the total mass of the composite powder. The mol ratio of the cubic silicon powder, the hexagonal boron nitride and the graphite powder is (0.8-1.2): (1.5-2.5): (2.8-3.5), namely Si: BN: c ═ 0.8 to 1.2: (1.5-2.5): (2.8-3.5). The purity of the cubic silicon powder is 99-99.9%, and the particle size is 1-20 μm. The purity of the hexagonal nitriding agent is 99-99.9%, and the particle size is 0.5-20 μm. The purity of the graphite powder is 99-99.9%, and the particle size is 0.5-20 μm.
In step S2, the basic parameters of the high-energy ball mill are: the ball material ratio is set to (10-40): 1, the rotating speed of the main disk is 200-400 r/min, the rotating speed of the planetary disk is 500-1000 r/min, and the time for secondary ball milling is set to be 10-100 h.
And finally, filling the composite powder prepared in the step S2 into a graphite die, carrying out hot-pressing sintering in a hot-pressing furnace, and then demoulding and taking out to obtain the nanocrystalline tantalum carbide reinforced silicon-boron-carbon-nitrogen composite ceramic material. Of course, the spark plasma sintering method may be used as the method according to the actual situation.
Wherein, the technological conditions of the hot-pressing sintering comprise: the sintering temperature is 1500-2300 ℃, the sintering pressure is 20-80 Mpa, the sintering time is 20-90 min, and the protective atmosphere is nitrogen or argon or vacuum.
The invention takes silicon boron carbon nitrogen ceramic as a substrate, and adds a tantalum carbide reinforced phase to prepare a nanocrystalline tantalum carbide reinforced silicon boron carbon nitrogen complex phase ceramic material, and ultra-high temperature phase tantalum carbide particles are uniformly dispersed in an amorphous silicon boron carbon nitrogen substrate in a nanocrystalline form, so that the function of pinning crack expansion can be achieved, the mechanical property of the silicon boron carbon nitrogen ceramic is improved, and meanwhile, the ultra-high temperature property of tantalum carbide reinforces the silicon boron carbon nitrogen ceramic, so that the high temperature resistance of the complex phase ceramic material is improved, and the complex phase ceramic material can be in service at higher temperature.
The nanocrystalline tantalum carbide reinforced silicon-boron-carbon-nitrogen composite ceramic material comprises a SiBCN matrix phase, wherein nanocrystalline tantalum carbide is distributed in the SiBCN matrix phase, and crystal grains of the nanocrystalline tantalum carbide are mutually separated. The SiBCN matrix phase comprises SiC and BN (C) phases, the size of SiC crystal grains is less than 1 mu m, and the BN (C) phases are distributed around the SiC crystal grains. The SiBCN matrix phase comprises a turbulent layer-shaped BN (C) phase, the grain diameter of the nanocrystalline tantalum carbide distributed in the BN (C) phase is 3-5nm, and the nanocrystalline tantalum carbide with the grain diameter of 10-20nm is distributed in the whole SiBCN matrix phase except the BN (C) phase.
In the preparation process, the nanocrystalline tantalum carbide powder with smaller size is dispersed in a BN (C) phase in an amorphous SiBCN matrix phase, and the BN (C) is wrapped around the nanocrystalline tantalum carbide, so that the nanocrystalline tantalum carbide is prevented from growing up due to grain curing; the turbulent layered structure composed of BN (C) -TaC can be coated on the surface of the SiC crystal grain, so that element diffusion is inhibited, abnormal growth of the SiC crystal grain is avoided, the nanocrystalline tantalum carbide reinforced silicon-boron-carbon-nitrogen composite ceramic material keeps a nanocrystalline-amorphous structure in the special distribution form, and the composite ceramic material has high density, mechanical property and high temperature resistance.
It will be appreciated that, according to the hallpitch relationship, δ is δ ═ δ0+kd-1/2Wherein d is a crystal grain diameter, δ0δ is the yield point for the frictional force acting on the dislocation. Increasing as d decreases, the delta yield point increases, i.e., the smaller the grain size, the higher the strength of the material. Therefore, the introduction of the nanocrystalline tantalum carbide has a good strengthening effect on the system.
The density of the multiphase ceramic material is 2.6-2.79 g/cm3The bending strength is 350-400 MPa, and the fracture toughness is 4-4.4 MPa.m1/2The elastic modulus is 145 to 167GPa, and the Vickers hardness is 5 to 7.4 GPa. Compared with the common silicon-boron-carbon-nitrogen ceramic material, the density and the mechanical property are increased to different degrees.
The technical solutions of the present invention will be further described below with reference to several exemplary embodiments (not all embodiments), so as to clarify the objects and advantages of the present invention.
Implementation mode one
The preparation method of the nanocrystalline tantalum carbide reinforced silicon-boron-carbon-nitrogen composite ceramic material is carried out according to the following steps:
s1: in a glove box filled with argon, 17g of tantalum carbide particles with the particle size of 1-5 microns are weighed, the weighed tantalum carbide particles are placed into a ball milling tank, 340g of grinding balls are added into the ball milling tank, the ball milling tank is sealed and then taken out of the glove box, the ball milling tank is mounted on a planetary high-energy ball mill for ball milling, and the ball-to-material ratio is set to be 20: 1, the rotating speed of the main disc is 350r/min, the rotating speed of the planetary disc is 800r/min, and the ball milling time is 30 hours, so that the nanocrystalline tantalum carbide powder is obtained.
S2: weighing nanocrystalline tantalum carbide powder, hexagonal boron nitride, cubic silicon powder and graphite powder (the total mass of the powder is 17g) in a glove box filled with argon, and putting the nanocrystalline tantalum carbide powder, the hexagonal boron nitride, the cubic silicon powder and the graphite powder into a ball milling tank, wherein the nanocrystalline tantalum carbide powder accounts for 5% of the total mass of the composite powder, and the molar ratio of the cubic silicon powder to the hexagonal boron nitride to the graphite powder is 2:1: 3; 340g of grinding balls are put into the ball milling tank; then the ball milling tank is taken out from the glove box after being sealed, and then the ball milling tank is arranged on a planetary high-energy ball mill for ball milling, the ball-material ratio is set to be 20: 1, setting the rotation speed of a main disc at 350r/min, setting the rotation speed of a planetary disc at 600r/min, ball milling for 20 hours, and finally placing a ball milling tank in a glove box, and taking out to obtain powder, namely the SiBCN-TaC composite powder.
S3: and (4) putting the composite powder obtained in the step (S3) into a vacuum hot-pressing sintering furnace for hot-pressing sintering, wherein the sintering temperature is 1900 ℃, the sintering pressure is 60Mpa, the sintering time is 60min, and the nano-crystal tantalum carbide reinforced silicon-boron-carbon-nitrogen composite ceramic material is obtained in vacuum.
Referring to fig. 2, fig. 2 is an X-ray diffraction (XRD) pattern of the nano-crystalline tantalum carbide powder after ball milling, from fig. 2, it can be observed that TaC diffraction peaks remarkably broadened at the bottom part, and it is described that the nano-crystalline tantalum carbide powder with smaller crystal grains is obtained by the preparation method of the present embodiment.
The present embodiment will be describedMachining the finally obtained nanocrystalline tantalum carbide reinforced silicon-boron-carbon-nitrogen composite ceramic material to obtain a standard sample, testing the density and testing the mechanical property on a universal mechanical testing machine, wherein the test result is as follows: the material density of the complex phase ceramic material is 2.61g/cm3Bending strength of 351.3 +/-5.5 MPa and fracture toughness of 4.04 +/-0.15 MPa.m1/2The elastic modulus is 141.4 +/-3.8 GPa, and the Vickers hardness is 5 +/-0.1 GPa.
Second embodiment
The present embodiment is different from the first embodiment in that: in step S2 of the method for preparing a nanocrystalline tantalum carbide-reinforced silicon-boron-carbon-nitrogen composite ceramic material according to the embodiment, the added nanocrystalline tantalum carbide powder accounts for 10% of the total mass of the composite powder.
The nanocrystalline tantalum carbide reinforced silicon-boron-carbon-nitrogen complex phase ceramic material finally obtained in the embodiment is machined to obtain a standard sample, then the density is tested, and the mechanical property is tested on a universal mechanical testing machine, wherein the test result is as follows: the material density of the complex phase ceramic material is 2.79g/cm3The bending strength is 399.5 +/-10.3 MPa, and the fracture toughness is 4.26 +/-0.14 MPa.m1/2The elastic modulus is 164.1 +/-3.1 GPa, and the Vickers hardness is 7.2 +/-0.2 GPa.
Third embodiment
The present embodiment is different from the first embodiment in that: in step S2 of the method for preparing a nanocrystalline tantalum carbide-reinforced silicon-boron-carbon-nitrogen composite ceramic material according to the embodiment, the added nanocrystalline tantalum carbide powder accounts for 15% of the total mass of the composite powder.
Embodiment IV
The difference between the embodiment and the above embodiment is that the preparation method of the nanocrystalline tantalum carbide reinforced silicon-boron-carbon-nitrogen composite ceramic material is carried out according to the following steps:
s1: in the glove box filled with argon, 12g of tantalum carbide particles with the particle size of 1-5 microns are weighed, the weighed tantalum carbide particles are placed into a ball milling tank, 420g of grinding balls are added into the ball milling tank, the ball milling tank is sealed and then taken out of the glove box, the ball milling tank is mounted on a planetary high-energy ball mill for ball milling, and the ball-to-material ratio is set to be 25: 1, the rotating speed of the main disc is 300r/min, the rotating speed of the planetary disc is 800r/min, and the ball milling time is 30 hours, so that the nanocrystalline tantalum carbide powder is obtained.
S2: weighing nanocrystalline tantalum carbide powder, hexagonal boron nitride, cubic silicon powder and graphite powder (the total mass of the powder is 17g) in a glove box filled with argon, and putting the nanocrystalline tantalum carbide powder, the hexagonal boron nitride, the cubic silicon powder and the graphite powder into a ball milling tank, wherein the nanocrystalline tantalum carbide powder accounts for 5% of the total mass of the composite powder, and the molar ratio of the cubic silicon powder to the hexagonal boron nitride to the graphite powder is 0.8:1: 2.8; then 500g of grinding balls are put into the ball milling tank; then the ball milling tank is taken out from the glove box after being sealed, and then the ball milling tank is arranged on a planetary high-energy ball mill for ball milling, the ball-material ratio is set to be 20: 1, setting the rotation speed of a main disc at 300r/min, setting the rotation speed of a planetary disc at 800r/min, ball milling for 30 hours, finally placing a ball milling tank in a glove box, and taking out to obtain powder, namely the SiBCN-TaC composite powder.
S3: and (4) putting the composite powder obtained in the step (S3) into a vacuum hot-pressing sintering furnace for hot-pressing sintering, wherein the sintering temperature is 1900 ℃, the sintering pressure is 50Mpa, the sintering time is 60min, and the nano-crystal tantalum carbide reinforced silicon-boron-carbon-nitrogen composite ceramic material is obtained in vacuum.
Fifth embodiment
The preparation method of the nanocrystalline tantalum carbide reinforced silicon-boron-carbon-nitrogen composite ceramic material is carried out according to the following steps:
s1: in a glove box filled with argon, 5g of tantalum carbide particles with the particle size of 1-5 microns are weighed, the weighed tantalum carbide particles are placed into a ball milling tank, 50g of grinding balls are added into the ball milling tank, the ball milling tank is sealed and then taken out of the glove box, the ball milling tank is mounted on a planetary high-energy ball mill for ball milling, and the ball-to-material ratio is set to be 10: 1, the rotating speed of the main disc is 200r/min, the rotating speed of the planetary disc is 500r/min, and the ball milling time is 10 hours, so that the nanocrystalline tantalum carbide powder is obtained.
S2: weighing nanocrystalline tantalum carbide powder, hexagonal boron nitride, cubic silicon powder and graphite powder in a glove box filled with argon, and putting the nanocrystalline tantalum carbide powder, the hexagonal boron nitride, the cubic silicon powder and the graphite powder into a ball milling tank (the total mass of the powder is 17g), wherein the nanocrystalline tantalum carbide powder accounts for 10% of the total mass of the composite powder, and the molar ratio of the cubic silicon powder to the hexagonal boron nitride to the graphite powder is 1:2: 3; then 500g of grinding balls are put into the ball milling tank; then the ball milling tank is taken out from the glove box after being sealed, and then the ball milling tank is arranged on a planetary high-energy ball mill for ball milling, wherein the ball-material ratio is set to be 25: 1, setting the rotation speed of a main disc at 300r/min, setting the rotation speed of a planetary disc at 800r/min, ball milling for 30 hours, finally placing a ball milling tank in a glove box, and taking out to obtain powder, namely the SiBCN-TaC composite powder.
S3: and (5) putting the composite powder obtained in the step (S3) into a vacuum hot-pressing sintering furnace for hot-pressing sintering, wherein the sintering temperature is 1900 ℃, the sintering pressure is 50Mpa, the sintering time is 60min, and the protective atmosphere is argon, so that the nanocrystalline tantalum carbide reinforced silicon-boron-carbon-nitrogen composite ceramic material is prepared.
Comparative example:
to further illustrate the reinforcing effect of the nanocrystalline tantalum carbide on the silicon-boron-carbon-nitrogen ceramic, a pair of proportions is set as follows:
the comparative example differs from the first embodiment in that no tantalum carbide reinforcing phase is introduced into the silicon boron carbon nitride ceramic. The preparation method of the silicon-boron-carbon-nitrogen ceramic material is carried out according to the following steps:
weighing hexagonal boron nitride, cubic silicon powder and graphite powder (the total mass of the powder is 17g) in a glove box filled with argon, putting the powder into a ball milling tank, wherein the molar ratio of the cubic silicon powder to the hexagonal boron nitride to the graphite powder is 2:1:3, and then putting 340g of milling balls; then the ball milling tank is taken out from the glove box after being sealed, and then the ball milling tank is arranged on a planetary high-energy ball mill for ball milling, the ball-material ratio is set to be 20: 1, setting the main disc rotating speed at 350r/min, the planetary disc rotating speed at 600r/min, ball milling for 20h, finally placing the ball milling tank in a glove box, taking out the powder, putting the powder into a vacuum hot-pressing sintering furnace for hot-pressing sintering, wherein the sintering temperature is 1900 ℃, the sintering pressure is 60Mpa, the sintering time is 60min, and carrying out vacuum treatment to obtain the silicon-boron-carbon-nitrogen ceramic.
Machining the silicon-boron-carbon-nitrogen ceramic finally obtained in the comparative example to obtain a standard sample, then testing the density and the mechanical property on a universal mechanical testing machine, wherein the test result is as follows: the material density of the silicon-boron-carbon-nitrogen ceramic is 2.24g/cm3Bending strength of 127.9 +/-19.7 MPa and fracture toughness of 1.82 +/-0.23 MPa.m1/2Elasticity ofThe modulus is 70.6 +/-4.7 GPa, and the Vickers hardness is 2.2 +/-0.1 GPa.
For convenience of description, and mainly comparing the performance of the composite phase ceramic after introducing nanocrystalline tantalum carbide in different proportions, the example in which nanocrystalline tantalum carbide powder accounts for 5% of the total mass of the composite powder is represented by ST5, the example in which nanocrystalline tantalum carbide powder accounts for 10% of the total mass of the composite powder is represented by ST10, the example in which nanocrystalline tantalum carbide powder accounts for 15% of the total mass of the composite powder is represented by ST15, and the example in which nanocrystalline tantalum carbide powder is not added is represented by ST0, according to the difference that nanocrystalline tantalum carbide powder accounts for the total mass of the composite powder.
The effects of the nanocrystalline tantalum carbide reinforced silicon-boron-carbon-nitrogen composite ceramic material and the silicon-boron-carbon-nitrogen ceramic prepared by the embodiments are verified by the following test comparison:
referring to fig. 3, the composite powder obtained in step S2 in the first to third embodiments and the comparative example was examined with an X-ray diffractometer to obtain an XRD pattern. As can be seen from the figure, after ball milling, the lattice structures of Si, BN and C are damaged to form an amorphous structure; the diffraction peak of TaC exists in the XRD pattern and is wider, so that TaC is distributed in amorphous SiBCN in the form of nano-crystals.
And (3) combining with the graph shown in fig. 4, adopting an X-ray diffractometer to obtain XRD patterns of the nanocrystalline tantalum carbide reinforced silicon-boron-carbon-nitrogen complex-phase ceramic material prepared after hot-pressing sintering in the first embodiment, the second embodiment and the comparative embodiment. As can be seen from the figure, after the thermal sintering, the XRD pattern of the nanocrystalline tantalum carbide reinforced silicon-boron-carbon-nitrogen composite ceramic material prepared by the hot-press sintering has obvious BN (C), SiC and TaC diffraction peaks, which shows that the composite powder has obvious crystallization in the sintering process, and the broadening phenomenon at the bottom of the individual diffraction peak can also be found in the figure, which shows that the prepared composite ceramic material has amorphous or nanocrystalline.
With reference to fig. 5 and 6, scanning the bulk composite ceramic material prepared by ST10 with a transmission electron microscope and an energy spectrometer to obtain a TEM image and an EDS energy spectrum. As can be seen from the two figures, nanocrystalline tantalum carbide exists in the prepared complex phase ceramic material in two sizes, wherein nanocrystalline tantalum carbide with a relatively large size is uniformly distributed in the whole ceramic matrix, and nanocrystalline tantalum carbide with a relatively small size is distributed in the turbulent layered BN (C) phase. Wherein the grain size distributed in the BN (C) phase is in the range of 3 to 5 nm. BN (C) is wrapped around the nanocrystalline tantalum carbide. The growth of nanocrystalline tantalum carbide due to grain curing is avoided; and a turbulent layer structure consisting of BN (C) -TaC is coated on the surface of the SiC to inhibit element diffusion and avoid abnormal growth of SiC grains.
And (3) performing mechanical detection on the complex-phase ceramic materials prepared by ST0, ST5 and ST10 to obtain a bending strength comparison graph by combining with the graph shown in FIG. 7. As can be seen from the figure, the bending strength is gradually enhanced along with the increase of the mass fraction of the nanocrystalline tantalum carbide, which shows that the nanocrystalline tantalum carbide can be used as a reinforcing phase to improve the strength of the silicon-boron-carbon-nitrogen ceramic.
Referring to fig. 8, thermogravimetric analysis and differential scanning calorimetry were used to detect the complex phase ceramic material with different nanocrystalline tantalum carbide content in air atmosphere, and a TG-DSC curve graph was obtained.
FIG. 8 is a TG-DSC curve graph of the complex phase ceramic material with different nanocrystalline tantalum carbide contents in air. As can be seen from the figure, between 600 ℃ and 850 ℃. The nanocrystalline tantalum carbide enhances the oxidation of carbon in the silicon-boron-carbon-nitrogen composite ceramic material, and the mass of the composite ceramic material is weightless. The BN (C) phase is oxidized at 850-1000 ℃, and the mass is increased. Generated B2O3The oxide film is spread on the surface of the ceramic material to avoid the continuous oxidation, so that the quality of the complex phase ceramic material at 1000-1400 ℃ is constant. Along with the increase of the content of the nanocrystalline tantalum carbide, the weight loss rate of the complex phase ceramic material at 600-850 ℃ is gradually reduced, and the introduction of the nanocrystalline tantalum carbide is beneficial to improving the oxidation performance of the complex phase ceramic material at the stage of 600-1400 ℃.
As can be seen from the above, after the nanocrystalline tantalum carbide is introduced into the silicon-boron-carbon-nitrogen ceramic matrix, the material density of the prepared complex-phase ceramic material is 2.6-2.79 g/cm3The bending strength is 350 to 400MPa, and the fracture toughness is 4 to 4.4 MPa.m1/2An elastic modulus of 145 to 167GPa and a Vickers hardness of 5 to 7.4GPa, in comparison with the aboveThe density and the mechanical property are increased to different degrees in the common silicon-boron-carbon-nitrogen ceramic material. Namely, the prepared complex phase ceramic material shows good mechanical property and high temperature resistance, and is suitable for manufacturing core components for aerospace heat protection.
Although the present disclosure has been described above, the scope of the present disclosure is not limited thereto. Those skilled in the art can make various changes and modifications without departing from the spirit and scope of the present disclosure, and such changes and modifications will fall within the scope of the present invention.
Claims (10)
1. A preparation method of a nanocrystalline tantalum carbide reinforced silicon-boron-carbon-nitrogen composite ceramic material is characterized by comprising the following steps:
s1: preparing nanocrystalline tantalum carbide powder;
s2: mixing the nanocrystalline tantalum carbide powder, hexagonal boron nitride, cubic silicon powder and graphite according to a preset proportion, and then carrying out high-energy ball milling to obtain composite powder;
s3: and carrying out hot-pressing sintering on the composite powder to obtain the nanocrystalline tantalum carbide reinforced silicon-boron-carbon-nitrogen composite ceramic material.
2. The method according to claim 1, wherein the nanocrystalline tantalum carbide powder has a particle size range of less than 20 nm.
3. The method according to claim 1, wherein in step S2, the mass of the nanocrystalline tantalum carbide powder accounts for 1-50% of the mass of the composite powder.
4. The preparation method according to claim 1, wherein in step S2, the molar ratio of the cubic silicon powder, the hexagonal boron nitride, and the graphite is Si: BN: c ═ 0.8 to 1.2: (1.5-2.5): (2.8-3.5).
5. The preparation method according to any one of claims 1 to 4, wherein in step S1, the specific steps of preparing the nanocrystalline tantalum carbide powder comprise:
under the protection of argon, placing tantalum carbide particles with the particle size of 1-5 microns and grinding balls in a ball mill for ball milling to prepare the nanocrystalline tantalum carbide powder;
wherein, the ball milling conditions are as follows: the ball material ratio is (10-40): 1, the rotating speed of the main disc is 200-400 r/min, the rotating speed of the planetary disc is 500-1000 r/min, and the ball milling time is 10-100 h.
6. The preparation method according to any one of claims 1 to 4, wherein in step S2, the high-energy ball milling conditions are: the ball material ratio is (10-40): 1, the rotating speed of the main disc is 200-400 r/min, the rotating speed of the planetary disc is 500-1000 r/min, and the ball milling time is 10-100 h.
7. The production method according to any one of claims 1 to 4, wherein the process conditions of the hot press sintering include: the sintering temperature is 1500-2300 ℃, the sintering pressure is 20-80 Mpa, the sintering time is 20-90 min, and the protective atmosphere is nitrogen or argon or vacuum.
8. A nanocrystalline tantalum carbide reinforced silicon-boron-carbon-nitrogen complex-phase ceramic material is characterized by being prepared by the preparation method of the nanocrystalline tantalum carbide reinforced silicon-boron-carbon-nitrogen complex-phase ceramic material according to any one of claims 1-7.
9. The composite phase ceramic material according to claim 8, wherein the composite phase ceramic material comprises a SiBCN matrix phase, wherein nanocrystalline tantalum carbide is distributed in the SiBCN matrix phase, and wherein individual grains of nanocrystalline tantalum carbide are separated from one another.
10. The composite phase ceramic material according to claim 9, wherein the SiBCN matrix phase comprises a turbulent layered BN (C) phase, and the nanocrystalline tantalum carbide distributed within the BN (C) phase has a grain size of 3-5 nm.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201910532639.7A CN111217610A (en) | 2019-06-19 | 2019-06-19 | Nanocrystalline tantalum carbide reinforced silicon-boron-carbon-nitrogen composite ceramic material and preparation method thereof |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201910532639.7A CN111217610A (en) | 2019-06-19 | 2019-06-19 | Nanocrystalline tantalum carbide reinforced silicon-boron-carbon-nitrogen composite ceramic material and preparation method thereof |
Publications (1)
| Publication Number | Publication Date |
|---|---|
| CN111217610A true CN111217610A (en) | 2020-06-02 |
Family
ID=70810821
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| CN201910532639.7A Pending CN111217610A (en) | 2019-06-19 | 2019-06-19 | Nanocrystalline tantalum carbide reinforced silicon-boron-carbon-nitrogen composite ceramic material and preparation method thereof |
Country Status (1)
| Country | Link |
|---|---|
| CN (1) | CN111217610A (en) |
Cited By (6)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN114538905A (en) * | 2022-03-24 | 2022-05-27 | 朱艳 | Ceramic material with nanocrystalline structure and preparation method thereof |
| CN114907125A (en) * | 2022-06-20 | 2022-08-16 | 北方民族大学 | Preparation method of tantalum carbide ceramic composite material |
| CN115521151A (en) * | 2022-09-28 | 2022-12-27 | 中国科学院上海硅酸盐研究所 | Discharge plasma sintering method of silicon carbide/tantalum carbide toughened ceramic |
| CN116143526A (en) * | 2022-12-30 | 2023-05-23 | 新化县顺达电子陶瓷有限公司 | Ceramic material for high-heat-conductivity 5G signal base station |
| CN116477952A (en) * | 2023-05-09 | 2023-07-25 | 哈尔滨工业大学 | Preparation method of tantalum hafnium carbide-silicon boron carbon nitrogen ceramic diffusion couple |
| CN116477952B (en) * | 2023-05-09 | 2024-05-17 | 哈尔滨工业大学 | Preparation method of tantalum hafnium carbide-silicon boron carbon nitrogen ceramic diffusion couple |
Citations (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101870586A (en) * | 2010-07-07 | 2010-10-27 | 哈尔滨工业大学 | Amorphous and nanocrystalline Si-B-C-N ceramic composite material and preparation method thereof |
-
2019
- 2019-06-19 CN CN201910532639.7A patent/CN111217610A/en active Pending
Patent Citations (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101870586A (en) * | 2010-07-07 | 2010-10-27 | 哈尔滨工业大学 | Amorphous and nanocrystalline Si-B-C-N ceramic composite material and preparation method thereof |
Non-Patent Citations (2)
| Title |
|---|
| 徐甲强等: "《材料合成化学与合成实例》", 28 February 2015, 哈尔滨工业大学出版社 * |
| 李贺军等: "《先进材料复合学》", 30 December 2016, 西北工业大学出版社 * |
Cited By (8)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN114538905A (en) * | 2022-03-24 | 2022-05-27 | 朱艳 | Ceramic material with nanocrystalline structure and preparation method thereof |
| CN114538905B (en) * | 2022-03-24 | 2023-08-01 | 潮州市潮安区雅莱尔陶瓷有限公司 | Ceramic material with nanocrystalline structure and preparation method thereof |
| CN114907125A (en) * | 2022-06-20 | 2022-08-16 | 北方民族大学 | Preparation method of tantalum carbide ceramic composite material |
| CN115521151A (en) * | 2022-09-28 | 2022-12-27 | 中国科学院上海硅酸盐研究所 | Discharge plasma sintering method of silicon carbide/tantalum carbide toughened ceramic |
| CN116143526A (en) * | 2022-12-30 | 2023-05-23 | 新化县顺达电子陶瓷有限公司 | Ceramic material for high-heat-conductivity 5G signal base station |
| CN116143526B (en) * | 2022-12-30 | 2023-12-08 | 新化县顺达电子陶瓷有限公司 | Ceramic material for high-heat-conductivity 5G signal base station |
| CN116477952A (en) * | 2023-05-09 | 2023-07-25 | 哈尔滨工业大学 | Preparation method of tantalum hafnium carbide-silicon boron carbon nitrogen ceramic diffusion couple |
| CN116477952B (en) * | 2023-05-09 | 2024-05-17 | 哈尔滨工业大学 | Preparation method of tantalum hafnium carbide-silicon boron carbon nitrogen ceramic diffusion couple |
Similar Documents
| Publication | Publication Date | Title |
|---|---|---|
| CN111217610A (en) | Nanocrystalline tantalum carbide reinforced silicon-boron-carbon-nitrogen composite ceramic material and preparation method thereof | |
| Jia et al. | Metastable Si-BCN ceramics and their matrix composites developed by inorganic route based on mechanical alloying: Fabrication, microstructures, properties and their relevant basic scientific issues | |
| Yin et al. | Spark plasma sintering of B4C-TiB2-SiC composite ceramics using B4C, Ti3SiC2 and Si as starting materials | |
| CN105132742A (en) | Graphene reinforced titanium-based composite and preparation method thereof | |
| Torosyan et al. | Reactive, nonreactive, and flash spark plasma sintering of Al2O3/SiC composites—A comparative study | |
| WO2014098370A1 (en) | Method for manufacturing cemented carbide including carbon nanotube, cemented carbide manufactured thereby, and cemented carbide cutting tool including cemented carbide | |
| US5372978A (en) | Monolithic, fully dense silicon carbide material, method of manufacturing and end uses | |
| Zhang et al. | Improvement of densification and microstructure of HfB2 ceramics by Ta/Ti substitution for Hf | |
| Geng et al. | Microstructure and mechanical properties of TaC ceramics with 1–7.5 mol% Si as sintering aid | |
| Xia et al. | Effect of boron doping on fracture behavior of carbon fiber reinforced lithium aluminosilicate glass ceramics matrix composites | |
| Liao et al. | Strengthening and toughening effects of MWCNTs on Si2BC3N ceramics sintered by SPS technique | |
| Lv et al. | Tunable strength of SiCf/β-Yb2Si2O7 interface for different requirements in SiCf/SiC CMC: Inspiration from model composite investigation | |
| WO2023029080A1 (en) | Boron nitride nanotube/nanosheet-boron carbide ceramic composite material and preparation method therefor | |
| Neuman et al. | Microstructure and mechanical properties of reaction‐hot‐pressed zirconium diboride based ceramics | |
| Wan et al. | Highly creep‐resistant silicon nitride/silicon carbide nano–nano composites | |
| Qiu et al. | Microstructural evolution and mechanical properties of h-BN composite ceramics with Y 2 O 3–AlN addition by liquid-phase sintering | |
| Feng et al. | Medium‐temperature sintering efficiency of ZrB2 ceramics using polymer‐derived SiBCN as a sintering aid | |
| Guo et al. | High hardness (TiZr) C ceramic with dislocation networks | |
| Liang et al. | Catalytic Preparation of Si 3 N 4-Bonded SiC Refractories and Their High-Temperature Properties | |
| Xiang et al. | Microstructures and mechanical properties of CVD-SiC coated PIP-C/SiC composites under high temperature | |
| Dash et al. | Compressive creep of SiC whisker/Ti3SiC2 composites at high temperature in air | |
| JPH03242375A (en) | Silicon carbide body body having high toughness and destruction resistance and manufacture thereof | |
| Malik et al. | Mechanical properties of silicon carbide—in situ zirconium carbonitride composites | |
| JP2010070421A (en) | METHOD FOR MANUFACTURING SiC FIBER-REINFORCED SiC COMPOSITE MATERIAL | |
| Zhu et al. | Effects of Zr and chopped C fiber on microstructure and mechanical properties of SiBCN ceramics |
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 | ||
| RJ01 | Rejection of invention patent application after publication |
Application publication date: 20200602 |
|
| RJ01 | Rejection of invention patent application after publication |