CN112778014B - High-performance silicon carbide ceramic material and preparation method thereof - Google Patents
High-performance silicon carbide ceramic material and preparation method thereof Download PDFInfo
- Publication number
- CN112778014B CN112778014B CN202110035598.8A CN202110035598A CN112778014B CN 112778014 B CN112778014 B CN 112778014B CN 202110035598 A CN202110035598 A CN 202110035598A CN 112778014 B CN112778014 B CN 112778014B
- Authority
- CN
- China
- Prior art keywords
- silicon carbide
- sintering
- temperature
- carbide powder
- ceramic material
- 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
-
- 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
-
- 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
-
- 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
- C04B2235/3821—Boron 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
- C04B2235/3865—Aluminium 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
-
- 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
-
- 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
-
- 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
- Y02P—CLIMATE CHANGE MITIGATION TECHNOLOGIES IN THE PRODUCTION OR PROCESSING OF GOODS
- Y02P20/00—Technologies relating to chemical industry
- Y02P20/10—Process efficiency
Abstract
The invention relates to a high-performance silicon carbide ceramic material and a preparation method thereofThe preparation method comprises the following steps: the raw materials are prepared, ball-milling and mixing are carried out, spray granulation is carried out, compression molding is carried out, sintering is carried out, and the adding proportion of alpha-silicon carbide powder and beta-silicon carbide powder in the raw materials is beneficial to strengthening of grain boundaries and grain refinement, so that the toughness and hardness of the silicon carbide ceramic are improved. The proper composition of the sintering auxiliary agent can enlarge the sintering temperature range, thereby bringing convenience to process control; the sintering aid is B 4 C. C and AlN, when B 4 C. The mass ratio of C to AlN is (1-2): (1.5-3): in the case of (1-3), the sintering aid can improve the interfacial bonding strength between silicon carbide grains and promote the improvement of high-temperature strength. When the sintering temperature is 2050 ℃, the sintering density of the silicon carbide ceramic material is higher. The prepared silicon carbide ceramic material has excellent room temperature and high temperature mechanical properties.
Description
Technical Field
The invention relates to a silicon carbide ceramic material, in particular to a high-performance silicon carbide ceramic material and a preparation method thereof.
Background
With the development of science and technology, people have higher requirements on the research of new materials. In engineering materials, not only are materials required to have good mechanical properties, but also excellent physicochemical properties such as density, corrosion resistance, high temperature resistance, heat transfer property and the like are required. And the structural ceramic material can meet the requirements of various performances.
Silicon carbide ceramics are important members of structural ceramics, have excellent high-temperature strength, high hardness, high temperature resistance, corrosion resistance and the like, and can be used for a plurality of aspects such as bearings, rotors, vehicles, shipbuilding and the like. The preparation method of the silicon carbide ceramic mainly comprises reaction sintering, hot-press sintering, pressureless sintering and the like. The reaction sintering has strict requirements on raw materials, is easy to generate free silicon, has high energy consumption and poor high-temperature performance. Hot press sintering has strict requirements on the production process, is difficult to prepare parts with complex shapes, and has high production cost. The pressureless sintering preparation cost is low, the prepared silicon carbide ceramic has good overall performance, can be used for preparing parts with complex shapes, and is easy to realize industrial production. However, the silicon carbide ceramic prepared by pressureless sintering has the problems of lower toughness, low density, further improvement of strength and hardness, and the like. At present, in order to prepare compact silicon carbide ceramics with excellent performance, in patent document 1 (CN 104446493 a), two-step pressureless solid-phase sintering is adopted to prepare the silicon carbide ceramics, but the preparation process is complex, and the toughness performance is not high.
Disclosure of Invention
Aiming at the problems existing in the prior art, the invention aims to provide a high-performance silicon carbide ceramic material and a preparation method thereof, and the prepared silicon carbide ceramic material has good mechanical properties at high temperature and high temperature.
In order to achieve the above purpose, the present invention adopts the following technical scheme: the preparation method of the high-performance silicon carbide ceramic material is characterized by comprising the following steps of:
(1) Preparing raw materials: the silicon carbide powder comprises 75-90% of silicon carbide powder, 5-20% of sintering aid and 5-15% of binder in percentage by mass; the sum of the mass percentages of the components in the raw materials is 100 percent; the silicon carbide powder consists of alpha-silicon carbide powder and beta-silicon carbide powder, wherein the mass percentage of the alpha-silicon carbide powder is 60-70% based on the total weight of the silicon carbide powder, and the balance is the beta-silicon carbide powder; the average grain diameter of the alpha-silicon carbide powder is 20-200nm, and the average grain diameter of the beta-silicon carbide powder is 30-230nm; the sintering aid is B 4 C. C and AlN; b in sintering aid 4 C. The mass ratio of C to AlN is (1-2): (1.5-3): (1-3); the binder is phenolic resin;
(2) Ball milling and mixing: ball-milling and mixing silicon carbide powder, a sintering aid and a binder according to the proportion to obtain a mixed material;
(3) And (3) spray granulation: spray granulating the mixture, wherein the inlet hot air temperature of the dryer is 330-360 ℃ and the outlet hot air temperature of the dryer is 100-120 ℃ during spray drying; after granulation, the bulk density of the obtained powder is 0.93-0.97g/cm 3 ；
(4) And (5) press forming: carrying out compression molding or cold isostatic pressing molding on the powder to obtain a blank; the pressure of compression molding is 120-150MPa; the pressure of cold isostatic pressing is 200-240MPa;
(5) Sintering: under the protection of inert gas, placing the green body into a sintering furnace for sintering, wherein in the sintering process, the relation between the temperature rise temperature and time is as follows: the temperature is raised to 1000 ℃ at a rate of 3-5 ℃/min; then the temperature rising rate is 6-8 ℃/min until the sintering temperature; the sintering temperature is 2010-2100 ℃; sintering time is 30-60min; and then cooling to room temperature along with the furnace to obtain the silicon carbide ceramic material.
Preferably, the silicon carbide powder is 80% by mass of the raw material.
Preferably, the α -silicon carbide powder is 66% by mass based on the total silicon carbide powder.
Preferably, the content of the sintering aid is 8% in terms of the mass percentage of the raw materials.
Preferably, B in the sintering aid 4 C. The mass ratio of C to AlN is 1:2:2.
preferably, the dryer inlet hot air temperature is 340 ℃ and the outlet temperature is 115 ℃.
Preferably, the sintering temperature is 2050 ℃.
Preferably, the sintering time is 40min.
The invention also provides the high-performance silicon carbide ceramic material prepared by the preparation method.
The addition ratio of the alpha-silicon carbide powder to the beta-silicon carbide powder is favorable for strengthening grain boundaries and refining grains, thereby improving the toughness and the hardness of the silicon carbide ceramic. When the addition amount of the alpha-silicon carbide powder is 66%, the toughness and the hardness are optimal. During sintering, when beta-silicon carbide is converted into alpha-silicon carbide, the combination among grains is more intimate, and the sintering density of the silicon carbide ceramic is improved.
The proper composition of the sintering auxiliary agent can enlarge the sintering temperature range, thereby bringing convenience to process control; the sintering aid is B 4 C. C and AlN, when B 4 C. The mass ratio of C to AlN is (1-2): (1.5-3): in the step (1-3), the sintering aid can better improve the interfacial bonding strength among silicon carbide grains and promote the improvement of high-temperature strength; when B is 4 C. The mass ratio of C to AlN is 1:2:2, the comprehensive performance is optimal.
The sintering temperature is 2010-2100 ℃, the sintering density of the silicon carbide ceramic material is increased and then decreased along with the increase of the sintering temperature, and when the sintering temperature is 2050 ℃, the sintering density of the silicon carbide ceramic material is higher.
Through testing, the bending strength of the silicon carbide ceramic material is 760-850MPa, and the fracture toughness is 10.5-13.3 MPa.m at room temperature 1/2 The sintering density is 3.17-3.20g/cm 3 The Vickers hardness is between 30.5 and 34.0 GPa. Silicon carbide ceramic at 1400 DEG CFlexural strength of porcelain material: 630-690 MPa. The silicon carbide ceramic material prepared by the preparation method has excellent toughness, hardness, high sintering density and good high-temperature strength performance.
The invention has the beneficial effects that:
1. according to the preparation method of the high-performance silicon carbide ceramic material, the silicon carbide powder, the sintering aid and the binder are mixed by ball milling according to the proportion, and the proper proportion of the alpha-silicon carbide powder and the beta-silicon carbide powder is selected, so that the improvement of the sintering density of the silicon carbide ceramic is promoted, and the toughness and the hardness of the silicon carbide ceramic are also improved.
2. The sintering aid composition provided by the invention can expand the sintering temperature range, and brings convenience to process control; the sintering aid is B 4 C. C and AlN, when B 4 C. The mass ratio of C to AlN is (1-2): (1.5-3): in the case of (1-3), the sintering aid can improve the interfacial bonding strength between silicon carbide grains and promote the improvement of high-temperature strength. When B is 4 C. The mass ratio of C to AlN is 1:2:2, the comprehensive performance is optimal.
3. The optimal sintering temperature is selected, and when the sintering temperature is 2050 ℃, the sintering density of the silicon carbide ceramic material is higher. The silicon carbide ceramic material prepared by the preparation method has excellent mechanical properties at room temperature and high temperature through tests.
Detailed Description
The above-described aspects of the present invention will be described in further detail with reference to the following embodiments. The detailed description is to be regarded as illustrative in nature and not as restrictive.
Embodiment 1, a method for preparing a high-performance silicon carbide ceramic material, comprising the steps of:
(1) Preparing raw materials: the silicon carbide powder comprises 75% of silicon carbide powder, 20% of sintering aid and 5% of binder in percentage by mass; in the silicon carbide powder, the silicon carbide powder consists of alpha-silicon carbide powder and beta-silicon carbide powder, based on the total amount of the silicon carbide powderThe mass percentage of the alpha-silicon carbide powder is 60 percent, and the rest is beta-silicon carbide powder; the average grain diameter of the alpha-silicon carbide powder is 20nm, and the average grain diameter of the beta-silicon carbide powder is 230nm; the sintering aid is B 4 C. C and AlN; b (B) 4 C. The mass ratio of C to AlN is 1:2:3, a step of; the binder is phenolic resin;
(2) Ball milling and mixing: ball-milling and mixing silicon carbide powder, a sintering aid and a binder according to the proportion to obtain a mixed material;
(3) And (3) spray granulation: carrying out spray granulation on the mixed material, wherein when in spray drying, the inlet hot air temperature of a dryer is 330 ℃, and the outlet temperature is 120 ℃; after granulation, the bulk density of the obtained powder was 0.93g/cm 3 ；
(4) And (5) press forming: carrying out compression molding on the powder to obtain a blank; the pressure of compression molding is 120MPa;
(5) Sintering: under the protection of inert gas, placing the green body into a sintering furnace for sintering, wherein in the sintering process, the relation between the temperature rise temperature and time is as follows: the temperature is raised to 1000 ℃ at a speed of 3 ℃/min; then the temperature rising rate is 8 ℃/min until the sintering temperature is reached; the sintering temperature is 2010 ℃; sintering time is 60min; and then cooling to room temperature along with the furnace to obtain the silicon carbide ceramic material.
Example 2, a method for preparing a high performance silicon carbide ceramic material, comprising the steps of:
(1) Preparing raw materials: the silicon carbide powder comprises, by mass, 90% of silicon carbide powder, 5% of sintering aid and 5% of binder; the silicon carbide powder consists of alpha-silicon carbide powder and beta-silicon carbide powder, wherein the mass percentage of the alpha-silicon carbide powder is 70 percent based on the total weight of the silicon carbide powder, and the balance is the beta-silicon carbide powder; the average grain diameter of the alpha-silicon carbide powder is 200nm, and the average grain diameter of the beta-silicon carbide powder is 30nm; the sintering aid is B 4 C. C and AlN; b (B) 4 C. The mass ratio of C to AlN is 1:2:1, a step of; the binder is phenolic resin;
(2) Ball milling and mixing: ball-milling and mixing silicon carbide powder, a sintering aid and a binder according to the proportion to obtain a mixed material;
(3) And (3) spray granulation: carrying out spray granulation on the mixed material, wherein when in spray drying, the inlet hot air temperature of a dryer is 360 ℃, and the outlet temperature is 100 ℃; after granulation, the bulk density of the obtained powder was 0.97g/cm 3 ；
(4) And (5) press forming: carrying out cold isostatic pressing molding on the powder to obtain a blank; the pressure of cold isostatic pressing is 240MPa;
(5) Sintering: under the protection of inert gas, placing the green body into a sintering furnace for sintering, wherein in the sintering process, the relation between the temperature rise temperature and time is as follows: the temperature is raised to 1000 ℃ at a speed of 5 ℃/min; then the temperature rising rate is 6 ℃/min until the sintering temperature; sintering temperature is 2100 ℃; sintering time is 30min; and then cooling to room temperature along with the furnace to obtain the silicon carbide ceramic material.
Embodiment 3, a method for preparing a high-performance silicon carbide ceramic material, is characterized by comprising the following steps:
(1) Preparing raw materials: the silicon carbide powder comprises 75% of silicon carbide powder, 20% of sintering aid and 5% of binder in percentage by mass; the silicon carbide powder consists of alpha-silicon carbide powder and beta-silicon carbide powder, wherein the mass percentage of the alpha-silicon carbide powder is 66 percent based on the total weight of the silicon carbide powder, and the balance is the beta-silicon carbide powder; the average grain diameter of the alpha-silicon carbide powder is 20nm, and the average grain diameter of the beta-silicon carbide powder is 230nm; the sintering aid is B 4 C. C and AlN; b (B) 4 C. The mass ratio of C to AlN is 1:2:3, a step of; the binder is phenolic resin;
(2) Ball milling and mixing: ball-milling and mixing silicon carbide powder, a sintering aid and a binder according to the proportion to obtain a mixed material;
(3) And (3) spray granulation: carrying out spray granulation on the mixed material, wherein when in spray drying, the inlet hot air temperature of a dryer is 330 ℃, and the outlet temperature is 120 ℃; after granulation, the bulk density of the obtained powder was 0.93g/cm 3 ；
(4) And (5) press forming: carrying out compression molding on the powder to obtain a blank; the pressure of compression molding is 120MPa;
(5) Sintering: under the protection of inert gas, placing the green body into a sintering furnace for sintering, wherein in the sintering process, the relation between the temperature rise temperature and time is as follows: the temperature is raised to 1000 ℃ at a speed of 3 ℃/min; then the temperature rising rate is 8 ℃/min until the sintering temperature is reached; the sintering temperature is 2010 ℃; sintering time is 60min; and then cooling to room temperature along with the furnace to obtain the silicon carbide ceramic material.
Example 4, a method for preparing a high performance silicon carbide ceramic material, comprising the steps of:
(1) Preparing raw materials: the silicon carbide powder comprises 75% of silicon carbide powder, 20% of sintering aid and 5% of binder in percentage by mass; the silicon carbide powder consists of alpha-silicon carbide powder and beta-silicon carbide powder, wherein the mass percentage of the alpha-silicon carbide powder is 66 percent based on the total weight of the silicon carbide powder, and the balance is the beta-silicon carbide powder; the average grain diameter of the alpha-silicon carbide powder is 20nm, and the average grain diameter of the beta-silicon carbide powder is 230nm; the sintering aid is B 4 C. C and AlN; b (B) 4 C. The mass ratio of C to AlN is 1:2:2; the binder is phenolic resin;
(2) Ball milling and mixing: ball-milling and mixing silicon carbide powder, a sintering aid and a binder according to the proportion to obtain a mixed material;
(3) And (3) spray granulation: carrying out spray granulation on the mixed material, wherein when in spray drying, the inlet hot air temperature of a dryer is 330 ℃, and the outlet temperature is 120 ℃; after granulation, the bulk density of the obtained powder was 0.93g/cm 3 ；
(4) And (5) press forming: carrying out compression molding on the powder to obtain a blank; the pressure of compression molding is 120MPa;
(5) Sintering: under the protection of inert gas, placing the green body into a sintering furnace for sintering, wherein in the sintering process, the relation between the temperature rise temperature and time is as follows: the temperature is raised to 1000 ℃ at a speed of 3 ℃/min; then the temperature rising rate is 8 ℃/min until the sintering temperature is reached; the sintering temperature is 2010 ℃; sintering time is 60min; and then cooling to room temperature along with the furnace to obtain the silicon carbide ceramic material.
Example 5, a method for preparing a high performance silicon carbide ceramic material, comprising the steps of:
(1) Preparing raw materials: the silicon carbide powder comprises 75% of silicon carbide powder, 20% of sintering aid and 5% of binder in percentage by mass; the silicon carbide powder consists of alpha-silicon carbide powder and beta-silicon carbide powder, wherein the mass percentage of the alpha-silicon carbide powder is 66 percent based on the total weight of the silicon carbide powder, and the balance is the beta-silicon carbide powder; the average grain diameter of the alpha-silicon carbide powder is 20nm, and the average grain diameter of the beta-silicon carbide powder is 230nm; the sintering aid is B 4 C. C and AlN; b (B) 4 C. The mass ratio of C to AlN is 1:2:2; the binder is phenolic resin;
(2) Ball milling and mixing: ball-milling and mixing silicon carbide powder, a sintering aid and a binder according to the proportion to obtain a mixed material;
(3) And (3) spray granulation: carrying out spray granulation on the mixed material, wherein when in spray drying, the inlet hot air temperature of a dryer is 330 ℃, and the outlet temperature is 120 ℃; after granulation, the bulk density of the obtained powder was 0.93g/cm 3 ；
(4) And (5) press forming: carrying out compression molding on the powder to obtain a blank; the pressure of compression molding is 120MPa;
(5) Sintering: under the protection of inert gas, placing the green body into a sintering furnace for sintering, wherein in the sintering process, the relation between the temperature rise temperature and time is as follows: the temperature is raised to 1000 ℃ at a speed of 3 ℃/min; then the temperature rising rate is 8 ℃/min until the sintering temperature is reached; the sintering temperature is 2050 ℃; sintering time is 60min; and then cooling to room temperature along with the furnace to obtain the silicon carbide ceramic material.
Comparative example 1, a method for preparing a high performance silicon carbide ceramic material, comprising the steps of:
(1) Preparing raw materials: the silicon carbide powder comprises 75% of silicon carbide powder, 20% of sintering aid and 5% of binder in percentage by mass; in the silicon carbide powder, the silicon carbide powder is composed of alpha-silicon carbide powder and beta-silicon carbide powder composition, based on the total silicon carbide powder, of 60% by mass of alpha-silicon carbide powder and the balance beta-silicon carbide powder; the average grain diameter of the alpha-silicon carbide powder is 20nm, and the average grain diameter of the beta-silicon carbide powder is 230nm; the sintering aid is B 4 C, performing operation; the binder is phenolic resin;
(2) Ball milling and mixing: ball-milling and mixing silicon carbide powder, a sintering aid and a binder according to the proportion to obtain a mixed material;
(3) And (3) spray granulation: carrying out spray granulation on the mixed material, wherein when in spray drying, the inlet hot air temperature of a dryer is 330 ℃, and the outlet temperature is 120 ℃; after granulation, the bulk density of the obtained powder was 0.93g/cm 3 ；
(4) And (5) press forming: carrying out compression molding on the powder to obtain a blank; the pressure of compression molding is 120MPa;
(5) Sintering: under the protection of inert gas, placing the green body into a sintering furnace for sintering, wherein in the sintering process, the relation between the temperature rise temperature and time is as follows: the temperature is raised to 1000 ℃ at a speed of 3 ℃/min; then the temperature rising rate is 8 ℃/min until the sintering temperature is reached; the sintering temperature is 2010 ℃; sintering time is 60min; and then cooling to room temperature along with the furnace to obtain the silicon carbide ceramic material.
Comparative example 2, a method for preparing a high performance silicon carbide ceramic material, comprising the steps of:
(1) Preparing raw materials: the silicon carbide powder comprises 75% of silicon carbide powder, 20% of sintering aid and 5% of binder in percentage by mass; the silicon carbide powder consists of alpha-silicon carbide powder and beta-silicon carbide powder, wherein the mass percentage of the alpha-silicon carbide powder is 60 percent based on the total weight of the silicon carbide powder, and the balance is the beta-silicon carbide powder; the average grain diameter of the alpha-silicon carbide powder is 20nm, and the average grain diameter of the beta-silicon carbide powder is 230nm; the sintering aid is B 4 C. C and AlN; b (B) 4 C. The mass ratio of C to AlN is 1:2:5, a step of; the binder is phenolic resin;
(2) Ball milling and mixing: ball-milling and mixing silicon carbide powder, a sintering aid and a binder according to the proportion to obtain a mixed material;
(3) And (3) spray granulation: carrying out spray granulation on the mixed material, wherein when in spray drying, the inlet hot air temperature of a dryer is 330 ℃, and the outlet temperature is 120 ℃; after granulation, the bulk density of the obtained powder was 0.93g/cm 3 ；
(4) And (5) press forming: carrying out compression molding on the powder to obtain a blank; the pressure of compression molding is 120MPa;
(5) Sintering: under the protection of inert gas, placing the green body into a sintering furnace for sintering, wherein in the sintering process, the relation between the temperature rise temperature and time is as follows: the temperature is raised to 1000 ℃ at a speed of 3 ℃/min; then the temperature rising rate is 8 ℃/min until the sintering temperature is reached; the sintering temperature is 2010 ℃; sintering time is 60min; and then cooling to room temperature along with the furnace to obtain the silicon carbide ceramic material.
Comparative example 3, a method for preparing a high performance silicon carbide ceramic material, comprising the steps of:
(1) Preparing raw materials: the silicon carbide powder comprises, by mass, 65% of silicon carbide powder, 15% of a sintering aid and 20% of a binder; the silicon carbide powder consists of alpha-silicon carbide powder and beta-silicon carbide powder, wherein the mass percentage of the alpha-silicon carbide powder is 80 percent based on the total weight of the silicon carbide powder, and the balance is the beta-silicon carbide powder; the average grain diameter of the alpha-silicon carbide powder is 20nm, and the average grain diameter of the beta-silicon carbide powder is 230nm; the sintering aid is B 4 C. C and AlN; b (B) 4 C. The mass ratio of C to AlN is 1:2:3, a step of; the binder is phenolic resin;
(2) Ball milling and mixing: ball-milling and mixing silicon carbide powder, a sintering aid and a binder according to the proportion to obtain a mixed material;
(3) And (3) spray granulation: carrying out spray granulation on the mixed material, wherein when in spray drying, the inlet hot air temperature of a dryer is 330 ℃, and the outlet temperature is 120 ℃; after granulation, the bulk density of the obtained powder was 0.93g/cm 3 ；
(4) And (5) press forming: carrying out compression molding on the powder to obtain a blank; the pressure of compression molding is 120MPa;
(5) Sintering: under the protection of inert gas, placing the green body into a sintering furnace for sintering, wherein in the sintering process, the relation between the temperature rise temperature and time is as follows: the temperature is raised to 1000 ℃ at a speed of 3 ℃/min; then the temperature rising rate is 8 ℃/min until the sintering temperature is reached; sintering temperature is 2300 ℃; sintering time is 60min; and then cooling to room temperature along with the furnace to obtain the silicon carbide ceramic material.
The performance of the finished products of examples 1-5 and comparative examples 1-3 was tested according to the present invention, and the test results are shown in Table 1.
TABLE 1 test Performance of silicon carbide ceramic materials
As can be seen from table 1: the addition ratio of the alpha-silicon carbide powder to the beta-silicon carbide powder is favorable for improving the toughness and the hardness of the silicon carbide ceramic, and the sintering density is also improved. When the addition amount of the alpha-silicon carbide powder is 66%, the toughness and the hardness are optimal. The proper composition of the sintering auxiliary agent can enlarge the sintering temperature range, thereby bringing convenience to process control; the proper proportion of the sintering auxiliary agent is determined, so that the interface bonding strength among silicon carbide grains can be better improved, and the high-temperature strength can be improved. When the sintering temperature is 2050 ℃, the sintering density of the silicon carbide ceramic material is higher.
The bending strength of the silicon carbide ceramic material prepared by the invention is 760-850MPa, and the fracture toughness is 10.5-13.3 MPa.m at room temperature 1/2 The sintering density is 3.17-3.20g/cm 3 The Vickers hardness is between 30.5 and 34.0 GPa. Flexural strength of silicon carbide ceramic material at 1400 ℃ high temperature: 630-690MPa, and excellent mechanical properties at room temperature and high temperature.
The foregoing examples are set forth in order to provide a more thorough explanation of the present invention, and are not intended to limit the scope of the present invention, in which modifications and adaptations should and are intended to be within the scope of the present invention.
Claims (5)
1. The preparation method of the high-performance silicon carbide ceramic material is characterized by comprising the following steps of:
(1) Preparing raw materials: the silicon carbide powder comprises 75% of silicon carbide powder, 20% of sintering aid and 5% of binder in percentage by mass; the sum of the mass percentages of the components in the raw materials is 100 percent; the silicon carbide powder consists of alpha-silicon carbide powder and beta-silicon carbide powder, wherein the mass percentage of the alpha-silicon carbide powder is 66 percent based on the total weight of the silicon carbide powder, and the balance is the beta-silicon carbide powder; the average grain diameter of the alpha-silicon carbide powder is 20-200nm, and the average grain diameter of the beta-silicon carbide powder is 30-230nm; the sintering aid is B 4 C. C and AlN; b in the sintering aid 4 C. The mass ratio of C to AlN is 1:2:2; the binder is phenolic resin;
(2) Ball milling and mixing: ball-milling and mixing silicon carbide powder, a sintering aid and a binder according to the proportion to obtain a mixed material;
(3) And (3) spray granulation: spray granulating the mixture, wherein the inlet hot air temperature of the dryer is 330-360 ℃ and the outlet hot air temperature of the dryer is 100-120 ℃ during spray drying; after granulation, the bulk density of the obtained powder is 0.93-0.97g/cm 3 ；
(4) And (5) press forming: carrying out compression molding or cold isostatic pressing molding on the powder to obtain a blank; the pressure of compression molding is 120-150MPa; the pressure of cold isostatic pressing is 200-240MPa;
(5) Sintering: under the protection of inert gas, placing the green body into a sintering furnace for sintering, wherein in the sintering process, the relation between the temperature rise temperature and time is as follows: the temperature is raised to 1000 ℃ at a rate of 3-5 ℃/min; then the temperature rising rate is 6-8 ℃/min until the sintering temperature; the sintering temperature is 2010-2100 ℃; sintering time is 30-60min; and then cooling to room temperature along with the furnace to obtain the silicon carbide ceramic material.
2. The method for preparing high-performance silicon carbide ceramic material according to claim 1, wherein the inlet hot air temperature of the dryer is 340 ℃ and the outlet temperature is 115 ℃.
3. The method of producing high performance silicon carbide ceramic material according to any of claims 1 to 2, wherein the sintering temperature is 2050 ℃.
4. The method of producing a high performance silicon carbide ceramic material according to any of claims 1 to 2, wherein said sintering time is 40 minutes.
5. A high performance silicon carbide ceramic material, characterized in that it is prepared according to the method for preparing a high performance silicon carbide ceramic material according to any one of claims 1 to 4.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN202110035598.8A CN112778014B (en) | 2021-01-12 | 2021-01-12 | High-performance silicon carbide ceramic material and preparation method thereof |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN202110035598.8A CN112778014B (en) | 2021-01-12 | 2021-01-12 | High-performance silicon carbide ceramic material and preparation method thereof |
Publications (2)
| Publication Number | Publication Date |
|---|---|
| CN112778014A CN112778014A (en) | 2021-05-11 |
| CN112778014B true CN112778014B (en) | 2023-06-13 |
Family
ID=75757054
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| CN202110035598.8A Active CN112778014B (en) | 2021-01-12 | 2021-01-12 | High-performance silicon carbide ceramic material and preparation method thereof |
Country Status (1)
| Country | Link |
|---|---|
| CN (1) | CN112778014B (en) |
Families Citing this family (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN113072383A (en) * | 2021-05-20 | 2021-07-06 | 郑州海赛高技术陶瓷有限责任公司 | Preparation method and application of corrosion-resistant silicon carbide ceramic |
| CN113416076A (en) * | 2021-08-16 | 2021-09-21 | 东北大学 | Preparation method of self-reinforced silicon carbide ceramic material |
| CN113929489B (en) * | 2021-10-22 | 2023-05-12 | 湘潭大学 | Ceramic and preparation method thereof |
| CN114249595B (en) * | 2021-12-30 | 2022-11-22 | 扬州北方三山工业陶瓷有限公司 | Silicon carbide ceramic material for optical system, reflector, preparation method and sintering aid |
Citations (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| JP2000226264A (en) * | 1999-02-02 | 2000-08-15 | Mitsubishi Chemicals Corp | Production of carbon-ceramic composite molded form |
| WO2016186365A1 (en) * | 2015-05-18 | 2016-11-24 | 주식회사 원익큐엔씨 | Low-resistance silicon carbide ceramic material using atmospheric sintering scheme and method for manufacturing same |
Family Cites Families (7)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US5656218A (en) * | 1995-05-19 | 1997-08-12 | Industrial Technology Research Institute | Method for making high performance self-reinforced silicon carbide using a pressureless sintering process |
| JP3970394B2 (en) * | 1997-10-30 | 2007-09-05 | 新日鉄マテリアルズ株式会社 | Method for manufacturing silicon carbide sintered body |
| JP2004043241A (en) * | 2002-07-11 | 2004-02-12 | Mamoru Omori | High purity silicon carbide sintered compact and its forming method |
| CN101591169A (en) * | 2009-05-22 | 2009-12-02 | 浙江东新密封有限公司 | A kind of silicon carbide carbonized complex phase ceramic sealing material and preparation method thereof |
| CN106064946A (en) * | 2016-05-31 | 2016-11-02 | 台州东新密封有限公司 | Mechanical seal SiC/ graphite diphase ceramic material and preparation method thereof |
| US20190249059A1 (en) * | 2016-06-13 | 2019-08-15 | Teijin Limited | Silicon carbide production method and silicon carbide composite material |
| CN112159233B (en) * | 2020-09-11 | 2022-03-08 | 中国科学院上海硅酸盐研究所 | Silicon carbide-based composite ceramic material with high electric field strength resistance and preparation method thereof |
-
2021
- 2021-01-12 CN CN202110035598.8A patent/CN112778014B/en active Active
Patent Citations (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| JP2000226264A (en) * | 1999-02-02 | 2000-08-15 | Mitsubishi Chemicals Corp | Production of carbon-ceramic composite molded form |
| WO2016186365A1 (en) * | 2015-05-18 | 2016-11-24 | 주식회사 원익큐엔씨 | Low-resistance silicon carbide ceramic material using atmospheric sintering scheme and method for manufacturing same |
Also Published As
| Publication number | Publication date |
|---|---|
| CN112778014A (en) | 2021-05-11 |
Similar Documents
| Publication | Publication Date | Title |
|---|---|---|
| CN112778014B (en) | High-performance silicon carbide ceramic material and preparation method thereof | |
| CN101555156B (en) | Boron nitride crystal whisker/silicon nitride ceramic composite material and preparation method thereof | |
| CN110818428B (en) | Preparation method of eutectic reinforced toughened silicon nitride ceramic | |
| CN110590377A (en) | High beta-phase compact silicon nitride ceramic and low-temperature preparation method | |
| CN1326801C (en) | Method for preparing composite material combined with corundum based on bauxite beta-Sialon | |
| CN113321494A (en) | Oxidation-resistant long-life heat absorption and storage integrated corundum-mullite ceramic and preparation method thereof | |
| CN113929466B (en) | Preparation method of aluminum-boron carbide composite material | |
| CN101734925B (en) | Silicon nitride porous ceramics with controllable porosity and preparation method thereof | |
| CN110627504A (en) | Pressureless sintering preparation method of boron carbide composite material | |
| CN112062574B (en) | High-performance nano silicon carbide ceramic and preparation method and application thereof | |
| CN114318038A (en) | Boride modified Mo2FeB2Base cermet and method for preparing same | |
| CN113880557A (en) | AL2O3-cBN-based ceramic cutting tool material and method for producing the same | |
| CN111515404B (en) | Preparation method of cBN/Al composite material | |
| CN111517798A (en) | Carbide-based ceramic material, preparation method and application thereof | |
| CN111499386A (en) | Composite ceramic material and preparation method thereof | |
| CN112341202B (en) | Granulation powder for improving performance of reaction sintered silicon carbide and preparation method thereof | |
| CN113321513B (en) | High-strength silicon nitride ceramic material and preparation method thereof | |
| CN109400176A (en) | A kind of high-performance silicon nitride ceramics and its preparation method and application | |
| CN114380606A (en) | Preparation process of machined high-strength refractory material | |
| CN107619290A (en) | A kind of preparation method of CNT enhancing zirconium diboride ceramics based composites | |
| CN108821774B (en) | Preparation method of porous silicon nitride-silicon carbide composite ceramic | |
| CN1179919C (en) | Prepn process of sand blasting ceramic nozzle | |
| CN114315364A (en) | Method for preparing clean SiC ceramic by adding nano Si powder into precursor | |
| CN111410539A (en) | Y-Al-Si-O multi-element glass phase reinforced hexagonal boron nitride-based multiphase ceramic and preparation method thereof | |
| CN116143523B (en) | Pressureless sintered silicon carbide blank intermediate, silicon carbide ceramic and preparation method |
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 | ||
| TA01 | Transfer of patent application right | ||
| TA01 | Transfer of patent application right |
Effective date of registration: 20230516 Address after: 523000 workshop 6, danshuiao Industrial Zone, Qiaoli village, Changping Town, Dongguan City, Guangdong Province Applicant after: Dongguan Kangbai Industrial Ceramics Co.,Ltd. Address before: 718100 No.1, South Street, Yinzhou Town, Mizhi County, Yulin City, Shaanxi Province Applicant before: Luo Huanhuan |
|
| GR01 | Patent grant | ||
| GR01 | Patent grant |