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CN112552031B - SiO2-BN complex phase ceramic and preparation method thereof - Google Patents

SiO2-BN complex phase ceramic and preparation method thereof Download PDF

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CN112552031B
CN112552031B CN202011454787.0A CN202011454787A CN112552031B CN 112552031 B CN112552031 B CN 112552031B CN 202011454787 A CN202011454787 A CN 202011454787A CN 112552031 B CN112552031 B CN 112552031B
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巩鹏程
王前
任学美
巩长生
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Shandong Pengcheng Ceramic New Material Technology Co ltd
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Abstract

The invention discloses a SiO2-BN complex phase ceramic material, which is prepared from the following raw materials in parts by weight: 35-45 parts of BN, SiO2 55-65 parts of, Y2O30.1-0.5 part, CaO 0.2-0.3 part and MgO 0.1-0.3 part. The invention is on SiO2BN is added, has high thermal conductivity, excellent thermal shock property, good high temperature resistance and electrical insulation property, simultaneously has excellent wave-transmitting property and is easy to machine, and Y is added2O3Sintering aids such as CaO, MgO and the like and a stabilizer are subjected to dry-setting mixing by a vibration mill and then subjected to high-temperature hot-pressing sintering under the protection of inert gas to obtain pure SiO2The ceramic material has better thermal shock resistance and high temperature resistance, and has good complex phase ceramic material which can be machined, and the volume density of the complex phase ceramic material is more than 2.55g/cm3And a hardness of greater than 660 on the Rich scale.

Description

SiO (silicon dioxide)2-BN complex phase ceramic and preparation method thereof
Technical Field
The invention belongs to the technical field of ceramic materials, and particularly relates to SiO2-BN complex phase ceramic and a preparation method thereof.
Background
Ceramic materials are generally produced by molding, sintering and other processes under strictly controlled conditions using artificially synthesized high-purity inorganic compounds as raw materials to produce inorganic materials having a fine crystalline structure. It has a series of excellent physical, chemical and biological properties, and the new-type ceramic material has its unique superiority in performance. In the aspects of thermal and mechanical properties, the material has the advantages of high temperature resistance, heat insulation, high hardness, abrasion resistance and the like; electrical properties such as insulation, piezoelectricity, semiconductivity, and magnetism; has the functions of catalysis, corrosion resistance, adsorption and the like in the chemical aspect; in the biological aspect, the material has certain biocompatibility and can be used as a biological structure material and the like. Ceramic materials are divided into two main categories according to chemical components: one type is pure oxide ceramics, such as Al2O3、ZrO2、MgO、CaO、BeO、ThO2Etc.; the other is non-oxide ceramics such as carbide, boride, nitride, silicide, etc. The performance and feature classification can be divided into: high temperature ceramics, ultra hard ceramics, high toughness ceramics, semiconductor ceramics. Electrolyte ceramics, magnetic ceramics, conductive ceramics, and the like. With the continuous improvement of components, structures and processes, new ceramics have appeared in many varieties.
The silicon dioxide has the advantages of excellent chemical stability and thermal stability, high strength, oxidation resistance, corrosion resistance, excellent dielectric property and the like, is one of the advanced ceramic materials with the best comprehensive performance at present, is the most ideal wave-transmitting material and armor material for the aircraft radome, but has high strength, high hardness and brittleness, is difficult to machine, increases the processing cost, has low yield and limits the wide application of the silicon dioxide.
Therefore, the research and development of a silica complex phase ceramic which has better thermal shock resistance and high temperature resistance and good machinability is a problem to be solved by the technical personnel in the field.
Disclosure of Invention
In view of the above, the present invention provides a SiO2-BN complex phase ceramic and a preparation method thereof.
In order to achieve the purpose, the invention adopts the following technical scheme:
SiO (silicon dioxide)2-BN complex phase ceramic material, which is prepared from the following raw materials in parts by weight:
35-45 parts of BN, SiO255-65 parts of, Y2O30.1-0.5 part of CaO, 0.2-0.3 part of CaO and 0.1-0.3 part of MgO.
The invention has the beneficial effects that: the invention is on SiO2BN is added, has high thermal conductivity, excellent thermal shock property, good high temperature resistance and electrical insulation property, simultaneously has excellent wave-transmitting property and is easy to machine, and Y is added2O3CaO, MgO sintering aid and stabilizer are mixed by vibration grinding and drying, and then are sintered by high temperature hot pressing under the protection of inert gas, thus obtaining pure SiO2The ceramic material has better thermal shock resistance and high temperature resistance, and has good complex phase ceramic material which can be mechanically processed, and the volume density of the complex phase ceramic material is more than 2.55g/cm3And a hardness of greater than 660 on the Rich scale.
The invention also provides SiO2-BN composite ceramic material preparation method, including the following steps:
(1) according to one kind of SiO2Weighing the raw materials of the BN complex phase ceramic material according to the parts by weight;
(2) mixing the raw materials, ball-milling to obtain powder, and pulverizingCold-pressing and granulating the powder to obtain granules, filling the granules into a mould for hot-pressing sintering and forming, and demoulding to obtain SiO2-BN composite ceramic material.
The invention has the beneficial effects that: the preparation method of the SiO2-BN complex phase ceramic material has simple process and convenient operation, and is suitable for large-scale production and application.
Further, in the step (2), the step of hot-pressing sintering molding comprises:
1) loading the granules into a mold, transferring into a vacuum furnace, vacuumizing to-0.1 Mpa, heating to 1400 deg.C at 15 deg.C/min, and introducing N into the vacuum furnace2And pressurizing to-0.05 Mpa;
2) heating to 1500 deg.C at 10 deg.C/min, heating to 1550 deg.C at 8 deg.C/min, heating to 1600 deg.C at 5 deg.C/min, pressurizing to 5MPa, and maintaining the temperature and pressure for 30 min;
3) heating to 1850 ℃ at the speed of 3 ℃/min, pressurizing to 30MPa, keeping the temperature and the pressure for 60min, then releasing the pressure, naturally cooling to room temperature, and demolding to obtain the SiO2-BN complex phase ceramic material.
The beneficial effects of the further technical scheme are that: after nitrogen is filled, the product is protected, and trace metal oxides and N existing in the raw materials can be ensured2Reacting to produce new nitride and raise the purity of the final product, owing to SiO2And BN are extremely difficult to sinter, and the heat preservation and pressure maintaining operation can ensure that the materials are completely sintered so as to be subjected to hot pressing at the back.
Further, in the step (2), ball milling is carried out until the particle size of the powder is 6-8 microns.
Further, in the step (2), the mold is a carbon fiber mold.
Detailed Description
The technical solutions in the embodiments of the present invention will be clearly and completely described below, and it is obvious that the described embodiments are only a part of the embodiments of the present invention, and not all embodiments. All other embodiments, which can be derived by a person skilled in the art from the embodiments given herein without making any creative effort, shall fall within the protection scope of the present invention.
Example 1
The preparation method of the SiO2-BN complex phase ceramic material comprises the following steps:
(1) weighing 35 g of BN and SiO255-65 g, Y2O30.1 g, CaO 0.2 g and MgO 0.1 g;
(2) mixing and ball-milling the raw materials to obtain powder with the particle size of 6 microns, then carrying out cold pressing granulation on the powder to obtain particles, and then filling the particles into a carbon fiber mold for hot-pressing sintering molding, wherein the hot-pressing sintering molding comprises the following specific steps:
1) loading the granules into a mold, transferring into a vacuum furnace, vacuumizing to-0.1 Mpa, heating to 1400 deg.C at 15 deg.C/min, and introducing N into the vacuum furnace2And pressurizing to-0.05 Mpa;
2) heating to 1500 deg.C at 10 deg.C/min, heating to 1550 deg.C at 8 deg.C/min, heating to 1600 deg.C at 5 deg.C/min, pressurizing to 5MPa, and maintaining the temperature and pressure for 30 min;
3) heating to 1850 deg.C at 3 deg.C/min, pressurizing to 30MPa, maintaining the temperature and pressure for 60min, then releasing the pressure, naturally cooling to room temperature, demolding to obtain the SiO2-BN composite ceramic material, testing the SiO2-BN composite ceramic material of example 1, wherein the density is 2.60g/cm3The resulting steel sheet had a hardness of 692 measured by a Leeb hardness tester, a bending strength of 165MPa measured by a three-point bending method, and a thermal expansion coefficient of 3.6X 10-6and/K, good thermal shock resistance, and no cracking after being heated to 1000 ℃ from room temperature and cooled for 40 times.
Example 2
The preparation method of the SiO2-BN complex phase ceramic material comprises the following steps:
(1) weighing BN 40 g and SiO259 g, Y2O30.5 g, CaO 0.3 g and MgO 0.2 g;
(2) mixing and ball-milling the raw materials to obtain powder with the particle size of 7 microns, then carrying out cold pressing granulation on the powder to obtain particles, and then filling the particles into a carbon fiber mold for hot-pressing sintering molding, wherein the hot-pressing sintering molding comprises the following specific steps:
1) loading the granules into a mould and transferring into a vacuum furnaceVacuumizing the vacuum furnace to-0.1 Mpa, heating the vacuum furnace from room temperature to 1400 deg.C at 15 deg.C/min, and introducing N into the vacuum furnace2And pressurizing to-0.05 Mpa;
2) heating to 1500 deg.C at 10 deg.C/min, heating to 1550 deg.C at 8 deg.C/min, heating to 1600 deg.C at 5 deg.C/min, pressurizing to 5MPa, and maintaining the temperature and pressure for 30 min;
3) heating to 1850 deg.C at 3 deg.C/min, pressurizing to 30MPa, maintaining the temperature and pressure for 60min, releasing pressure, naturally cooling to room temperature, and demolding to obtain the above SiO2-BN composite ceramic material. For example 2SiO2-BN composite ceramic material having a density of 2.58g/cm3690 in terms of the Leeb hardness measured by a Leeb hardness meter, 163MPa in terms of the bending strength measured by a three-point bending method, and 3.55X 10 in terms of the thermal expansion coefficient-6and/K, good thermal shock resistance, and no cracking after heating from room temperature to 1000 ℃ and water cooling for 38 times.
Example 3
The preparation method of the SiO2-BN complex phase ceramic material comprises the following steps:
(1) weighing BN45 g, SiO265g, Y2O30.3 g, CaO 0.2 g and MgO 0.2 g;
(2) mixing and ball-milling the raw materials to obtain powder with the particle size of 8 microns, then carrying out cold pressing granulation on the powder to obtain particles, then filling the particles into a carbon fiber mould to carry out hot pressing sintering molding, wherein the hot pressing sintering molding comprises the following specific steps:
1) loading the granules into a mold, transferring into a vacuum furnace, vacuumizing to-0.1 Mpa, heating to 1400 deg.C at 15 deg.C/min, and introducing N into the vacuum furnace2And pressurizing to-0.05 Mpa;
2) heating to 1500 deg.C at 10 deg.C/min, heating to 1550 deg.C at 8 deg.C/min, heating to 1600 deg.C at 5 deg.C/min, pressurizing to 5MPa, and maintaining the temperature and pressure for 30 min;
3) heating to 1850 deg.C at 3 deg.C/min, pressurizing to 30MPa, maintaining the temperature and pressure for 60min, releasing pressure, naturally cooling to room temperature, and demolding to obtain the SiO2-BN composite ceramic material. The example 3SiO2-BN composite ceramic material was tested,the density of the powder is 2.65g/cm3694 Leeb hardness measured by a Leeb hardness meter, 168MPa bending strength measured by a three-point bending method, and 3.67X 10 thermal expansion coefficient-6and/K, good thermal shock resistance, and no cracking after being heated to 1000 ℃ from room temperature and cooled for 41 times by water.
The description of the disclosed embodiments is provided to enable any person skilled in the art to make or use the present invention. Various modifications to these embodiments will be readily apparent to those skilled in the art, and the generic principles defined herein may be applied to other embodiments without departing from the spirit or scope of the invention. Thus, the present invention is not intended to be limited to the embodiments shown herein but is to be accorded the widest scope consistent with the principles and novel features disclosed herein.

Claims (3)

1. SiO (silicon dioxide)2The BN complex phase ceramic material is characterized by being prepared from the following raw materials in parts by weight:
35-45 parts of BN, SiO255-65 parts of, Y2O3 0.1-0.5 part of CaO, 0.2-0.3 part of CaO and 0.1-0.3 part of MgO;
the SiO2-BN composite ceramic material preparation method, including the following steps:
(1) according to one kind of SiO2Weighing the raw materials of the BN complex phase ceramic material according to the parts by weight;
(2) mixing and ball-milling the raw materials to obtain powder, then carrying out cold pressing granulation on the powder to obtain particles, then filling the particles into a die for hot pressing sintering molding, and demoulding to obtain SiO2-BN composite ceramic material;
the hot-pressing sintering molding method comprises the following steps:
1) loading the granules into a mold, transferring into a vacuum furnace, vacuumizing to-0.1 MPa, heating to 1400 deg.C at 15 deg.C/min, and charging N2And pressurizing to-0.05 MPa;
2) heating to 1500 deg.C at 10 deg.C/min, heating to 1550 deg.C at 8 deg.C/min, heating to 1600 deg.C at 5 deg.C/min, pressurizing to 5MPa, and maintaining the temperature and pressure for 30 min;
3) heating to 1850 deg.C at 3 deg.C/min, pressurizing to 30MPa, maintaining the temperature and pressure for 60min, releasing pressure, naturally cooling to room temperature, and demolding to obtain the SiO2-BN composite ceramic material.
2. SiO as claimed in claim 12-BN complex phase ceramic material, characterized in that in the step (2), the powder is ball milled until the grain diameter of the powder is 6-8 microns.
3. SiO according to claim 12-BN composite ceramic material, characterized in that in step (2) the mould is a carbon fibre mould.
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