CN112778014A - High-performance silicon carbide ceramic material and preparation method thereof - Google Patents

High-performance silicon carbide ceramic material and preparation method thereof Download PDF

Info

Publication number
CN112778014A
CN112778014A CN202110035598.8A CN202110035598A CN112778014A CN 112778014 A CN112778014 A CN 112778014A CN 202110035598 A CN202110035598 A CN 202110035598A CN 112778014 A CN112778014 A CN 112778014A
Authority
CN
China
Prior art keywords
silicon carbide
sintering
carbide powder
temperature
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.)
Granted
Application number
CN202110035598.8A
Other languages
Chinese (zh)
Other versions
CN112778014B (en
Inventor
不公告发明人
Current Assignee (The listed assignees may be inaccurate. Google has not performed a legal analysis and makes no representation or warranty as to the accuracy of the list.)
Dongguan Kangbai Industrial Ceramics Co ltd
Original Assignee
Individual
Priority date (The priority date 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 date listed.)
Filing date
Publication date
Application filed by Individual filed Critical Individual
Priority to CN202110035598.8A priority Critical patent/CN112778014B/en
Publication of CN112778014A publication Critical patent/CN112778014A/en
Application granted granted Critical
Publication of CN112778014B publication Critical patent/CN112778014B/en
Active legal-status Critical Current
Anticipated expiration legal-status Critical

Links

Classifications

    • CCHEMISTRY; METALLURGY
    • C04CEMENTS; CONCRETE; ARTIFICIAL STONE; CERAMICS; REFRACTORIES
    • C04BLIME, MAGNESIA; SLAG; CEMENTS; COMPOSITIONS THEREOF, e.g. MORTARS, CONCRETE OR LIKE BUILDING MATERIALS; ARTIFICIAL STONE; CERAMICS; REFRACTORIES; TREATMENT OF NATURAL STONE
    • C04B35/00Shaped ceramic products characterised by their composition; Ceramics compositions; Processing powders of inorganic compounds preparatory to the manufacturing of ceramic products
    • C04B35/515Shaped 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
    • C04B35/56Shaped 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
    • C04B35/565Shaped 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
    • CCHEMISTRY; METALLURGY
    • C04CEMENTS; CONCRETE; ARTIFICIAL STONE; CERAMICS; REFRACTORIES
    • C04BLIME, MAGNESIA; SLAG; CEMENTS; COMPOSITIONS THEREOF, e.g. MORTARS, CONCRETE OR LIKE BUILDING MATERIALS; ARTIFICIAL STONE; CERAMICS; REFRACTORIES; TREATMENT OF NATURAL STONE
    • C04B35/00Shaped ceramic products characterised by their composition; Ceramics compositions; Processing powders of inorganic compounds preparatory to the manufacturing of ceramic products
    • C04B35/622Forming processes; Processing powders of inorganic compounds preparatory to the manufacturing of ceramic products
    • C04B35/64Burning or sintering processes
    • CCHEMISTRY; METALLURGY
    • C04CEMENTS; CONCRETE; ARTIFICIAL STONE; CERAMICS; REFRACTORIES
    • C04BLIME, MAGNESIA; SLAG; CEMENTS; COMPOSITIONS THEREOF, e.g. MORTARS, CONCRETE OR LIKE BUILDING MATERIALS; ARTIFICIAL STONE; CERAMICS; REFRACTORIES; TREATMENT OF NATURAL STONE
    • C04B2235/00Aspects relating to ceramic starting mixtures or sintered ceramic products
    • C04B2235/02Composition of constituents of the starting material or of secondary phases of the final product
    • C04B2235/30Constituents and secondary phases not being of a fibrous nature
    • C04B2235/38Non-oxide ceramic constituents or additives
    • C04B2235/3817Carbides
    • C04B2235/3821Boron carbides
    • CCHEMISTRY; METALLURGY
    • C04CEMENTS; CONCRETE; ARTIFICIAL STONE; CERAMICS; REFRACTORIES
    • C04BLIME, MAGNESIA; SLAG; CEMENTS; COMPOSITIONS THEREOF, e.g. MORTARS, CONCRETE OR LIKE BUILDING MATERIALS; ARTIFICIAL STONE; CERAMICS; REFRACTORIES; TREATMENT OF NATURAL STONE
    • C04B2235/00Aspects relating to ceramic starting mixtures or sintered ceramic products
    • C04B2235/02Composition of constituents of the starting material or of secondary phases of the final product
    • C04B2235/30Constituents and secondary phases not being of a fibrous nature
    • C04B2235/38Non-oxide ceramic constituents or additives
    • C04B2235/3852Nitrides, e.g. oxynitrides, carbonitrides, oxycarbonitrides, lithium nitride, magnesium nitride
    • C04B2235/3865Aluminium nitrides
    • CCHEMISTRY; METALLURGY
    • C04CEMENTS; CONCRETE; ARTIFICIAL STONE; CERAMICS; REFRACTORIES
    • C04BLIME, MAGNESIA; SLAG; CEMENTS; COMPOSITIONS THEREOF, e.g. MORTARS, CONCRETE OR LIKE BUILDING MATERIALS; ARTIFICIAL STONE; CERAMICS; REFRACTORIES; TREATMENT OF NATURAL STONE
    • C04B2235/00Aspects relating to ceramic starting mixtures or sintered ceramic products
    • C04B2235/02Composition of constituents of the starting material or of secondary phases of the final product
    • C04B2235/30Constituents and secondary phases not being of a fibrous nature
    • C04B2235/42Non metallic elements added as constituents or additives, e.g. sulfur, phosphor, selenium or tellurium
    • C04B2235/422Carbon
    • CCHEMISTRY; METALLURGY
    • C04CEMENTS; CONCRETE; ARTIFICIAL STONE; CERAMICS; REFRACTORIES
    • C04BLIME, MAGNESIA; SLAG; CEMENTS; COMPOSITIONS THEREOF, e.g. MORTARS, CONCRETE OR LIKE BUILDING MATERIALS; ARTIFICIAL STONE; CERAMICS; REFRACTORIES; TREATMENT OF NATURAL STONE
    • C04B2235/00Aspects relating to ceramic starting mixtures or sintered ceramic products
    • C04B2235/65Aspects relating to heat treatments of ceramic bodies such as green ceramics or pre-sintered ceramics, e.g. burning, sintering or melting processes
    • C04B2235/656Aspects 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
    • C04B2235/6562Heating rate
    • CCHEMISTRY; METALLURGY
    • C04CEMENTS; CONCRETE; ARTIFICIAL STONE; CERAMICS; REFRACTORIES
    • C04BLIME, MAGNESIA; SLAG; CEMENTS; COMPOSITIONS THEREOF, e.g. MORTARS, CONCRETE OR LIKE BUILDING MATERIALS; ARTIFICIAL STONE; CERAMICS; REFRACTORIES; TREATMENT OF NATURAL STONE
    • C04B2235/00Aspects relating to ceramic starting mixtures or sintered ceramic products
    • C04B2235/65Aspects relating to heat treatments of ceramic bodies such as green ceramics or pre-sintered ceramics, e.g. burning, sintering or melting processes
    • C04B2235/656Aspects 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
    • C04B2235/6567Treatment time
    • CCHEMISTRY; METALLURGY
    • C04CEMENTS; CONCRETE; ARTIFICIAL STONE; CERAMICS; REFRACTORIES
    • C04BLIME, MAGNESIA; SLAG; CEMENTS; COMPOSITIONS THEREOF, e.g. MORTARS, CONCRETE OR LIKE BUILDING MATERIALS; ARTIFICIAL STONE; CERAMICS; REFRACTORIES; TREATMENT OF NATURAL STONE
    • C04B2235/00Aspects relating to ceramic starting mixtures or sintered ceramic products
    • C04B2235/65Aspects relating to heat treatments of ceramic bodies such as green ceramics or pre-sintered ceramics, e.g. burning, sintering or melting processes
    • C04B2235/658Atmosphere during thermal treatment
    • CCHEMISTRY; METALLURGY
    • C04CEMENTS; CONCRETE; ARTIFICIAL STONE; CERAMICS; REFRACTORIES
    • C04BLIME, MAGNESIA; SLAG; CEMENTS; COMPOSITIONS THEREOF, e.g. MORTARS, CONCRETE OR LIKE BUILDING MATERIALS; ARTIFICIAL STONE; CERAMICS; REFRACTORIES; TREATMENT OF NATURAL STONE
    • C04B2235/00Aspects relating to ceramic starting mixtures or sintered ceramic products
    • C04B2235/70Aspects relating to sintered or melt-casted ceramic products
    • C04B2235/74Physical characteristics
    • C04B2235/77Density
    • CCHEMISTRY; METALLURGY
    • C04CEMENTS; CONCRETE; ARTIFICIAL STONE; CERAMICS; REFRACTORIES
    • C04BLIME, MAGNESIA; SLAG; CEMENTS; COMPOSITIONS THEREOF, e.g. MORTARS, CONCRETE OR LIKE BUILDING MATERIALS; ARTIFICIAL STONE; CERAMICS; REFRACTORIES; TREATMENT OF NATURAL STONE
    • C04B2235/00Aspects relating to ceramic starting mixtures or sintered ceramic products
    • C04B2235/70Aspects relating to sintered or melt-casted ceramic products
    • C04B2235/96Properties of ceramic products, e.g. mechanical properties such as strength, toughness, wear resistance
    • YGENERAL 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
    • Y02TECHNOLOGIES OR APPLICATIONS FOR MITIGATION OR ADAPTATION AGAINST CLIMATE CHANGE
    • Y02PCLIMATE CHANGE MITIGATION TECHNOLOGIES IN THE PRODUCTION OR PROCESSING OF GOODS
    • Y02P20/00Technologies relating to chemical industry
    • Y02P20/10Process efficiency

Landscapes

  • Chemical & Material Sciences (AREA)
  • Engineering & Computer Science (AREA)
  • Ceramic Engineering (AREA)
  • Manufacturing & Machinery (AREA)
  • Materials Engineering (AREA)
  • Structural Engineering (AREA)
  • Organic Chemistry (AREA)
  • Inorganic Chemistry (AREA)
  • Ceramic Products (AREA)

Abstract

The invention relates to a high-performance silicon carbide ceramic material and a preparation method thereof, wherein the preparation method comprises the following steps: the preparation method comprises the steps of preparing raw materials, ball-milling and mixing, spraying and granulating, pressing and molding, and sintering, wherein the alpha-silicon carbide powder and the beta-silicon carbide powder in the raw materials are added and proportioned, so that the grain boundary strengthening and grain refining are facilitated, and the toughness and hardness of the silicon carbide ceramic are improved. The proper composition of the sintering aid can enlarge the sintering temperature range and bring convenience to process control; the sintering aid is B4C. C and AlN, when B4C. The mass ratio of C to AlN is (1-2): (1.5-3): (1-3), the sintering aid can improve the interface bonding strength between silicon carbide crystal grains and promote the improvement of the 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

High-performance silicon carbide ceramic material and preparation method thereof
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 the field of engineering materials, not only are good mechanical properties required, but also excellent physicochemical properties, such as density, corrosion resistance, high temperature resistance, heat transfer property, etc., are required. And the structural ceramic material can meet the requirements of various properties.
Silicon carbide ceramics are an important member of structural ceramics, have excellent properties such as high-temperature strength, high hardness, high-temperature resistance, corrosion resistance and the like, and can be used in many aspects such as bearings, rotors, vehicles, shipbuilding and the like. The preparation method of the silicon carbide ceramic mainly comprises reaction sintering, hot-pressing sintering, pressureless sintering and the like. The reaction sintering has strict requirements on raw materials, is easy to generate free silicon, and has high energy consumption and poor high-temperature performance. The hot-pressing 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, parts with complex shapes can be prepared, and the industrialized production is easy to realize. However, the silicon carbide ceramic prepared by pressureless sintering still has the problems of lower toughness, low density, strength and hardness which need to be further improved, and the like. At present, in order to prepare a compact silicon carbide ceramic with excellent performance, patent document 1(CN104446493A) adopts two-step pressureless solid-phase sintering to prepare the silicon carbide ceramic, but the preparation process is complex and the toughness is not high.
Disclosure of Invention
Aiming at the problems 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 room temperature and high temperature.
In order to achieve the purpose, the 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: according to the mass percentage, in the raw materials, the content of the silicon carbide powder is 75-90%, the content of the sintering aid is 5-20%, and the content of the binder is 5-15%; the sum of the mass percentages of the components in the raw materials is 100 percent; in the silicon carbide powder, the silicon carbide powder consists of alpha-silicon carbide powder and beta-silicon carbide powder, wherein the mass percent of the alpha-silicon carbide powder is 60-70 percent, and the balance is 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 30-230 nm; the sintering aid is composed of B4C. C and AlN; b in the sintering aid4C. 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 the silicon carbide powder, the sintering aid and the binder according to the proportion to obtain a mixed material;
(3) spray granulation: carrying out spray granulation on the mixed material, wherein when spray drying is carried out, the hot air temperature at the inlet of the dryer is 330-360 ℃, and the temperature at the outlet of the dryer is 100-120 ℃; after granulation, the bulk density of the obtained powder is 0.93-0.97g/cm3
(4) And (3) pressing and forming: carrying out compression molding or cold isostatic pressing on the powder to obtain a blank; the pressure for compression molding is 120-150 MPa; the pressure of the cold isostatic pressing is 200-240 MPa;
(5) and (3) sintering: and under the protection of inert gas, putting the blank into a sintering furnace for sintering, wherein in the sintering process, the relationship between the temperature rise and the time is as follows: the temperature is between room temperature and 1000 ℃, and the heating rate is 3-5 ℃/min; then the heating rate is 6-8 ℃/min until the sintering temperature is reached; the sintering temperature is 2010-2100 ℃; the sintering time is 30-60 min; and then cooling to room temperature along with the furnace to obtain the silicon carbide ceramic material.
Preferably, the content of the silicon carbide powder is 80% by mass of the raw material.
Preferably, the mass percentage of the α -silicon carbide powder is 66% based on the total amount of the silicon carbide powder.
Preferably, the content of the sintering aid is 8% by mass of the raw materials.
Preferably, B in the sintering aid4C. 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 40 min.
The invention also provides a high-performance silicon carbide ceramic material prepared by the preparation method.
The addition proportion of the alpha-silicon carbide powder and the beta-silicon carbide powder is beneficial to strengthening of crystal boundary and grain refinement, thereby improving the toughness and hardness of the silicon carbide ceramic. When the addition amount of the alpha-silicon carbide powder is 66%, the toughness and the hardness of the alpha-silicon carbide powder are optimal. During the sintering process, when the beta-silicon carbide is converted into the alpha-silicon carbide, the combination among crystal grains is more close, and the sintering density of the silicon carbide ceramic is improved.
The proper composition of the sintering aid can enlarge the sintering temperature range and bring convenience to process control; the sintering aid is B4C. C and AlN, when B4C. Mass of C and AlNThe proportion is (1-2): (1.5-3): (1-3), the sintering aid can better improve the interface bonding strength among silicon carbide crystal grains and promote the improvement of high-temperature strength; when B is present4C. The mass ratio of C to AlN is 1: 2: 2, the overall performance is best.
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.
Tests show that the bending strength of the silicon carbide ceramic material is between 760 and 850MPa and the fracture toughness is between 10.5 and 13.3 MPa.m at room temperature1/2The sintered density is 3.17-3.20g/cm3The Vickers hardness is between 30.5 and 34.0 GPa. The bending strength of the silicon carbide ceramic material at the high temperature of 1400 ℃ is as follows: between 630 and 690 MPa. The silicon carbide ceramic material obtained by the preparation method has excellent strength and 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, provided by the invention, the silicon carbide powder, the sintering aid and the binder are subjected to ball milling and mixing 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 bring convenience to process control; the sintering aid is B4C. C and AlN, when B4C. The mass ratio of C to AlN is (1-2): (1.5-3): (1-3), the sintering aid can improve the interface bonding strength between silicon carbide crystal grains and promote the improvement of the high-temperature strength. When B is present4C. The mass ratio of C to AlN is 1: 2: 2, the overall performance is best.
3. And selecting the optimal sintering temperature, wherein the sintering density of the silicon carbide ceramic material is higher when the sintering temperature is 2050 ℃. Tests show that the silicon carbide ceramic material prepared by the preparation method has excellent mechanical properties at room temperature and high temperature.
Detailed Description
The present invention will be described in further detail with reference to the following examples. The specific embodiments are to be considered as illustrative and not restrictive in character.
Embodiment 1, a method for preparing a high-performance silicon carbide ceramic material, comprising the steps of:
(1) preparing raw materials: according to the mass percentage, in the raw materials, the content of the silicon carbide powder is 75 percent, the content of the sintering aid is 20 percent, and the content of the binder is 5 percent; in the silicon carbide powder, the silicon carbide powder consists of alpha-silicon carbide powder and beta-silicon carbide powder, wherein the mass percent of the alpha-silicon carbide powder is 60 percent, 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 230 nm; the sintering aid is composed of B4C. C and AlN; b is4C. The mass ratio of C to AlN is 1: 2: 3; the binder is phenolic resin;
(2) ball milling and mixing: ball-milling and mixing the silicon carbide powder, the sintering aid and the binder according to the proportion to obtain a mixed material;
(3) spray granulation: carrying out spray granulation on the mixed material, wherein during spray drying, the hot air temperature at the inlet of a dryer is 330 ℃, and the outlet temperature is 120 ℃; after granulation, the bulk density of the obtained powder was 0.93g/cm3
(4) And (3) pressing and forming: carrying out compression molding on the powder to obtain a blank; the pressure for compression molding is 120 MPa;
(5) and (3) sintering: and under the protection of inert gas, putting the blank into a sintering furnace for sintering, wherein in the sintering process, the relationship between the temperature rise and the time is as follows: the temperature is between room temperature and 1000 ℃, and the heating rate is 3 ℃/min; then the heating rate is 8 ℃/min until the sintering temperature is reached; the sintering temperature is 2010 ℃; the sintering time is 60 min; and then cooling to room temperature along with the furnace to obtain the silicon carbide ceramic material.
Embodiment 2, a method for preparing a high-performance silicon carbide ceramic material, comprising the steps of:
(1) preparing raw materials: according to the mass percentage, in the raw materials, the content of the silicon carbide powder is 90%, the content of the sintering aid is 5%, and the content of the binder is 5%; in the silicon carbide powder, the silicon carbide powder consists of alpha-silicon carbide powder and beta-silicon carbide powder, wherein the mass percent of the alpha-silicon carbide powder is 70 percent, 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 30 nm; the sintering aid is composed of B4C. C and AlN; b is4C. The mass ratio of C to AlN is 1: 2: 1; the binder is phenolic resin;
(2) ball milling and mixing: ball-milling and mixing the silicon carbide powder, the sintering aid and the binder according to the proportion to obtain a mixed material;
(3) spray granulation: carrying out spray granulation on the mixed material, wherein when spray drying is carried out, the hot air temperature at the inlet of a dryer is 360 ℃, and the outlet temperature is 100 ℃; after granulation, the bulk density of the obtained powder was 0.97g/cm3
(4) And (3) pressing and forming: carrying out cold isostatic pressing on the powder to obtain a blank; the pressure of cold isostatic pressing is 240 MPa;
(5) and (3) sintering: and under the protection of inert gas, putting the blank into a sintering furnace for sintering, wherein in the sintering process, the relationship between the temperature rise and the time is as follows: the temperature is between room temperature and 1000 ℃, and the heating rate is 5 ℃/min; then the heating rate is 6 ℃/min until the sintering temperature is reached; the sintering temperature is 2100 ℃; the sintering time is 30 min; 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, comprising the steps of:
(1) preparing raw materials: according to the mass percentage, in the raw materials, the content of the silicon carbide powder is 75 percent, the content of the sintering aid is 20 percent, and the content of the binder is 5 percent; in the silicon carbide powder, the silicon carbide powder consists of alpha-silicon carbide powder and beta-silicon carbide powder, the mass percent of the alpha-silicon carbide powder is 66 percent based on the total weight of the silicon carbide powder, and the rest isIs 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 230 nm; the sintering aid is composed of B4C. C and AlN; b is4C. The mass ratio of C to AlN is 1: 2: 3; the binder is phenolic resin;
(2) ball milling and mixing: ball-milling and mixing the silicon carbide powder, the sintering aid and the binder according to the proportion to obtain a mixed material;
(3) spray granulation: carrying out spray granulation on the mixed material, wherein during spray drying, the hot air temperature at the inlet of a dryer is 330 ℃, and the outlet temperature is 120 ℃; after granulation, the bulk density of the obtained powder was 0.93g/cm3
(4) And (3) pressing and forming: carrying out compression molding on the powder to obtain a blank; the pressure for compression molding is 120 MPa;
(5) and (3) sintering: and under the protection of inert gas, putting the blank into a sintering furnace for sintering, wherein in the sintering process, the relationship between the temperature rise and the time is as follows: the temperature is between room temperature and 1000 ℃, and the heating rate is 3 ℃/min; then the heating rate is 8 ℃/min until the sintering temperature is reached; the sintering temperature is 2010 ℃; the sintering time is 60 min; and then cooling to room temperature along with the furnace to obtain the silicon carbide ceramic material.
Embodiment 4, a method for preparing a high-performance silicon carbide ceramic material, comprising the steps of:
(1) preparing raw materials: according to the mass percentage, in the raw materials, the content of the silicon carbide powder is 75 percent, the content of the sintering aid is 20 percent, and the content of the binder is 5 percent; in the silicon carbide powder, the silicon carbide powder consists of alpha-silicon carbide powder and beta-silicon carbide powder, wherein the mass percent of the alpha-silicon carbide powder is 66 percent, 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 230 nm; the sintering aid is composed of B4C. C and AlN; b is4C. 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 the silicon carbide powder, the sintering aid and the binder according to the proportion to obtain a mixed material;
(3) spray granulation: carrying out spray granulation on the mixed material, wherein during spray drying, the hot air temperature at the inlet of a dryer is 330 ℃, and the outlet temperature is 120 ℃; after granulation, the bulk density of the obtained powder was 0.93g/cm3
(4) And (3) pressing and forming: carrying out compression molding on the powder to obtain a blank; the pressure for compression molding is 120 MPa;
(5) and (3) sintering: and under the protection of inert gas, putting the blank into a sintering furnace for sintering, wherein in the sintering process, the relationship between the temperature rise and the time is as follows: the temperature is between room temperature and 1000 ℃, and the heating rate is 3 ℃/min; then the heating rate is 8 ℃/min until the sintering temperature is reached; the sintering temperature is 2010 ℃; the sintering time is 60 min; and then cooling to room temperature along with the furnace to obtain the silicon carbide ceramic material.
Embodiment 5, a method for preparing a high-performance silicon carbide ceramic material, comprising the steps of:
(1) preparing raw materials: according to the mass percentage, in the raw materials, the content of the silicon carbide powder is 75 percent, the content of the sintering aid is 20 percent, and the content of the binder is 5 percent; in the silicon carbide powder, the silicon carbide powder consists of alpha-silicon carbide powder and beta-silicon carbide powder, wherein the mass percent of the alpha-silicon carbide powder is 66 percent, 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 230 nm; the sintering aid is composed of B4C. C and AlN; b is4C. 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 the silicon carbide powder, the sintering aid and the binder according to the proportion to obtain a mixed material;
(3) spray granulation: carrying out spray granulation on the mixed material, wherein during spray drying, the hot air temperature at the inlet of a dryer is 330 ℃, and the outlet temperature is 120 ℃; after granulation, the bulk density of the obtained powder was 0.93g/cm3
(4) And (3) pressing and forming: carrying out compression molding on the powder to obtain a blank; the pressure for compression molding is 120 MPa;
(5) and (3) sintering: and under the protection of inert gas, putting the blank into a sintering furnace for sintering, wherein in the sintering process, the relationship between the temperature rise and the time is as follows: the temperature is between room temperature and 1000 ℃, and the heating rate is 3 ℃/min; then the heating rate is 8 ℃/min until the sintering temperature is reached; the sintering temperature is 2050 ℃; the sintering time is 60 min; 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, characterized by comprising the steps of:
(1) preparing raw materials: according to the mass percentage, in the raw materials, the content of the silicon carbide powder is 75 percent, the content of the sintering aid is 20 percent, and the content of the binder is 5 percent; in the silicon carbide powder, the silicon carbide powder consists of alpha-silicon carbide powder and beta-silicon carbide powder, wherein the mass percent of the alpha-silicon carbide powder is 60 percent, 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 230 nm; the sintering aid is B4C; the binder is phenolic resin;
(2) ball milling and mixing: ball-milling and mixing the silicon carbide powder, the sintering aid and the binder according to the proportion to obtain a mixed material;
(3) spray granulation: carrying out spray granulation on the mixed material, wherein during spray drying, the hot air temperature at the inlet of a dryer is 330 ℃, and the outlet temperature is 120 ℃; after granulation, the bulk density of the obtained powder was 0.93g/cm3
(4) And (3) pressing and forming: carrying out compression molding on the powder to obtain a blank; the pressure for compression molding is 120 MPa;
(5) and (3) sintering: and under the protection of inert gas, putting the blank into a sintering furnace for sintering, wherein in the sintering process, the relationship between the temperature rise and the time is as follows: the temperature is between room temperature and 1000 ℃, and the heating rate is 3 ℃/min; then the heating rate is 8 ℃/min until the sintering temperature is reached; the sintering temperature is 2010 ℃; the sintering time is 60 min; 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, characterized by comprising the steps of:
(1) preparing raw materials: according to the mass percentage, in the raw materials, the content of the silicon carbide powder is 75 percent, the content of the sintering aid is 20 percent, and the content of the binder is 5 percent; in the silicon carbide powder, the silicon carbide powder consists of alpha-silicon carbide powder and beta-silicon carbide powder, wherein the mass percent of the alpha-silicon carbide powder is 60 percent, 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 230 nm; the sintering aid is composed of B4C. C and AlN; b is4C. The mass ratio of C to AlN is 1: 2: 5; the binder is phenolic resin;
(2) ball milling and mixing: ball-milling and mixing the silicon carbide powder, the sintering aid and the binder according to the proportion to obtain a mixed material;
(3) spray granulation: carrying out spray granulation on the mixed material, wherein during spray drying, the hot air temperature at the inlet of a dryer is 330 ℃, and the outlet temperature is 120 ℃; after granulation, the bulk density of the obtained powder was 0.93g/cm3
(4) And (3) pressing and forming: carrying out compression molding on the powder to obtain a blank; the pressure for compression molding is 120 MPa;
(5) and (3) sintering: and under the protection of inert gas, putting the blank into a sintering furnace for sintering, wherein in the sintering process, the relationship between the temperature rise and the time is as follows: the temperature is between room temperature and 1000 ℃, and the heating rate is 3 ℃/min; then the heating rate is 8 ℃/min until the sintering temperature is reached; the sintering temperature is 2010 ℃; the sintering time is 60 min; 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, characterized by comprising the steps of:
(1) preparing raw materials: according to the mass percentage, in the raw materials, the content of the silicon carbide powder is 65%, the content of the sintering aid is 15%, and the content of the binder is 20%; in the silicon carbide powder, the silicon carbide powder consists of alpha-silicon carbide powder and beta-silicon carbide powder, wherein the mass percent of the alpha-silicon carbide powder is 80 percent, and the balance is the beta-silicon carbide powder; alpha-The average grain diameter of the silicon carbide powder is 20nm, and the average grain diameter of the beta-silicon carbide powder is 230 nm; the sintering aid is composed of B4C. C and AlN; b is4C. The mass ratio of C to AlN is 1: 2: 3; the binder is phenolic resin;
(2) ball milling and mixing: ball-milling and mixing the silicon carbide powder, the sintering aid and the binder according to the proportion to obtain a mixed material;
(3) spray granulation: carrying out spray granulation on the mixed material, wherein during spray drying, the hot air temperature at the inlet of a dryer is 330 ℃, and the outlet temperature is 120 ℃; after granulation, the bulk density of the obtained powder was 0.93g/cm3
(4) And (3) pressing and forming: carrying out compression molding on the powder to obtain a blank; the pressure for compression molding is 120 MPa;
(5) and (3) sintering: and under the protection of inert gas, putting the blank into a sintering furnace for sintering, wherein in the sintering process, the relationship between the temperature rise and the time is as follows: the temperature is between room temperature and 1000 ℃, and the heating rate is 3 ℃/min; then the heating rate is 8 ℃/min until the sintering temperature is reached; the sintering temperature is 2300 ℃; the sintering time is 60 min; and then cooling to room temperature along with the furnace to obtain the silicon carbide ceramic material.
The invention performs a performance test on the finished products of examples 1-5 and comparative examples 1-3, and the test results are shown in Table 1.
TABLE 1 test Properties of silicon carbide ceramic materials
Figure BDA0002893135310000081
From table 1, it can be seen that: the addition proportion of the alpha-silicon carbide powder and 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 of the alpha-silicon carbide powder are optimal. The proper composition of the sintering aid can enlarge the sintering temperature range and bring convenience to process control; the interface bonding strength among silicon carbide crystal grains can be better improved by determining the proper proportion of the sintering aid, and the improvement of the high-temperature strength is promoted. 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 invention has the bending strength of 760-850MPa and the fracture toughness of 10.5-13.3 MPa-m at room temperature1/2The sintered density is 3.17-3.20g/cm3The Vickers hardness is between 30.5 and 34.0 GPa. The bending strength of the silicon carbide ceramic material at the high temperature of 1400 ℃ is as follows: between 630 and 690MPa, excellent room temperature and high temperature mechanical properties.
The foregoing examples are set forth to illustrate the present invention more clearly and should not be construed as limiting the scope of the present invention, which is intended to be limited thereby, and all such changes and modifications that can be made without departing from the scope of the present invention are intended to be within the scope of the present invention.

Claims (9)

1. The preparation method of the high-performance silicon carbide ceramic material is characterized by comprising the following steps of:
(1) preparing raw materials: according to the mass percentage, in the raw materials, the content of the silicon carbide powder is 75-90%, the content of the sintering aid is 5-20%, and the content of the binder is 5-15%; the sum of the mass percentages of the components in the raw materials is 100 percent; in the silicon carbide powder, the silicon carbide powder consists of alpha-silicon carbide powder and beta-silicon carbide powder, wherein the mass percent of the alpha-silicon carbide powder is 60-70 percent, and the balance is 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 30-230 nm; the sintering aid is composed of B4C. C and AlN; b in the sintering aid4C. 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 the silicon carbide powder, the sintering aid and the binder according to the proportion to obtain a mixed material;
(3) spray granulation: carrying out spray granulation on the mixed material, wherein when spray drying is carried out, the hot air temperature at the inlet of the dryer is 330-360 ℃, and the temperature at the outlet of the dryer is 100-120 ℃; after granulation, the bulk density of the obtained powder is 0.93-0.97g/cm3
(4) And (3) pressing and forming: carrying out compression molding or cold isostatic pressing on the powder to obtain a blank; the pressure for compression molding is 120-150 MPa; the pressure of the cold isostatic pressing is 200-240 MPa;
(5) and (3) sintering: and under the protection of inert gas, putting the blank into a sintering furnace for sintering, wherein in the sintering process, the relationship between the temperature rise and the time is as follows: the temperature is between room temperature and 1000 ℃, and the heating rate is 3-5 ℃/min; then the heating rate is 6-8 ℃/min until the sintering temperature is reached; the sintering temperature is 2010-2100 ℃; the sintering time is 30-60 min; and then cooling to room temperature along with the furnace to obtain the silicon carbide ceramic material.
2. The method for preparing a high-performance silicon carbide ceramic material according to claim 1, wherein the content of the silicon carbide powder is 80% by mass of the raw material.
3. The method for preparing a high-performance silicon carbide ceramic material according to claim 1 or 2, wherein the α -silicon carbide powder is 66% by mass based on the total amount of the silicon carbide powder.
4. The method for preparing a high-performance silicon carbide ceramic material according to claim 1 or 2, wherein the content of the sintering aid is 8% by mass of the raw materials.
5. The method for preparing high-performance silicon carbide ceramic material according to claim 2 after 1, wherein B is the sintering aid4C. The mass ratio of C to AlN is 1: 2: 2.
6. the method for preparing high-performance silicon carbide ceramic material according to claim 1 or 2, wherein the temperature of hot air at the inlet of the dryer is 340 ℃ and the temperature at the outlet of the dryer is 115 ℃.
7. The process for the preparation of high performance silicon carbide ceramic material according to any of claims 1-6, wherein the sintering temperature is 2050 ℃.
8. The method for preparing a high performance silicon carbide ceramic material according to any one of claims 1 to 7, wherein the sintering time is 40 min.
9. A high-performance silicon carbide ceramic material, which is prepared by the method for preparing the high-performance silicon carbide ceramic material according to any one of claims 1 to 8.
CN202110035598.8A 2021-01-12 2021-01-12 High-performance silicon carbide ceramic material and preparation method thereof Active CN112778014B (en)

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 true CN112778014A (en) 2021-05-11
CN112778014B 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)

Cited By (4)

* Cited by examiner, † Cited by third party
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
CN113929489A (en) * 2021-10-22 2022-01-14 湘潭大学 Ceramic and preparation method thereof
CN114249595A (en) * 2021-12-30 2022-03-29 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 (9)

* Cited by examiner, † Cited by third party
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
JPH11130538A (en) * 1997-10-30 1999-05-18 Nippon Steel Corp Silicon carbide-based sintered compact and its production
JP2000226264A (en) * 1999-02-02 2000-08-15 Mitsubishi Chemicals Corp Production of carbon-ceramic composite molded form
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
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
US20190249059A1 (en) * 2016-06-13 2019-08-15 Teijin Limited Silicon carbide production method and silicon carbide composite material
CN112159233A (en) * 2020-09-11 2021-01-01 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

Patent Citations (9)

* Cited by examiner, † Cited by third party
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
JPH11130538A (en) * 1997-10-30 1999-05-18 Nippon Steel Corp Silicon carbide-based sintered compact and its production
JP2000226264A (en) * 1999-02-02 2000-08-15 Mitsubishi Chemicals Corp Production of carbon-ceramic composite molded form
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
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
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
CN112159233A (en) * 2020-09-11 2021-01-01 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

Non-Patent Citations (1)

* Cited by examiner, † Cited by third party
Title
MALIK R ET AL.: "Effect of AlN addition on the electrical resistivity of pressureless sintered SiC ceramics with B4C and C", 《JOURNAL OF THE AMERICAN CERAMIC SOCIETY》 *

Cited By (4)

* Cited by examiner, † Cited by third party
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
CN113929489A (en) * 2021-10-22 2022-01-14 湘潭大学 Ceramic and preparation method thereof
CN114249595A (en) * 2021-12-30 2022-03-29 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

Also Published As

Publication number Publication date
CN112778014B (en) 2023-06-13

Similar Documents

Publication Publication Date Title
CN112778014A (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
CN108706973B (en) Preparation method of high-strength high-thermal-conductivity graphite material
CN110818428B (en) Preparation method of eutectic reinforced toughened silicon nitride ceramic
CN1326801C (en) Method for preparing composite material combined with corundum based on bauxite beta-Sialon
CN110590377A (en) High beta-phase compact silicon nitride ceramic and low-temperature preparation method
CN111517806B (en) High-toughness silicon nitride ceramic and preparation method thereof
CN101734925B (en) Silicon nitride porous ceramics with controllable porosity and preparation method thereof
CN111908923A (en) High-hardness silicon nitride ceramic and preparation method thereof
CN114318038A (en) Boride modified Mo2FeB2Base cermet and method for preparing same
CN101734920B (en) Titanium nitride porous ceramics and preparation method thereof
CN110627504A (en) Pressureless sintering preparation method of boron carbide composite material
CN113416077B (en) High-temperature ceramic cutter material with double composite structure and preparation method and application thereof
CN105859297B (en) A kind of silicon carbide composite fireproof materials and preparation method thereof
CN107963891A (en) A kind of single-phase silicon nitride ceramic material and its microwave sintering preparation process
CN113880557A (en) AL2O3-cBN-based ceramic cutting tool material and method for producing the same
CN106747433B (en) Zirconia-based nano ceramic tool and die material and preparation method thereof
CN102731098A (en) Silicon boron oxygen nitrogen fiber/silicon nitride ceramic composite material and preparation method thereof
CN111517798A (en) Carbide-based ceramic material, preparation method and application thereof
CN110877980A (en) High-strength silicon carbide/silicon nitride composite ceramic and preparation method thereof
CN108145618B (en) Microwave preparation method of nano ceramic bond CBN grinding tool
CN109400176A (en) A kind of high-performance silicon nitride ceramics and its preparation method and application
CN112573932B (en) Homogeneous body re-sintered fused zirconia mullite brick and preparation method thereof
CN112341202B (en) Granulation powder for improving performance of reaction sintered silicon carbide and preparation method thereof
CN110937903B (en) High-strength and high-thermal-conductivity silicon nitride ceramic material and preparation method thereof

Legal Events

Date Code Title Description
PB01 Publication
PB01 Publication
SE01 Entry into force of request for substantive examination
SE01 Entry into force of request for substantive examination
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