CN109336562B - Preparation method of alumina-based ceramic composite material - Google Patents
Preparation method of alumina-based ceramic composite material Download PDFInfo
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- CN109336562B CN109336562B CN201811116379.7A CN201811116379A CN109336562B CN 109336562 B CN109336562 B CN 109336562B CN 201811116379 A CN201811116379 A CN 201811116379A CN 109336562 B CN109336562 B CN 109336562B
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- alumina
- cyclodextrin
- polydimethylsiloxane
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- PNEYBMLMFCGWSK-UHFFFAOYSA-N aluminium oxide Inorganic materials [O-2].[O-2].[O-2].[Al+3].[Al+3] PNEYBMLMFCGWSK-UHFFFAOYSA-N 0.000 title claims abstract description 47
- 239000000919 ceramic Substances 0.000 title claims abstract description 45
- 239000002131 composite material Substances 0.000 title claims abstract description 24
- 238000002360 preparation method Methods 0.000 title claims abstract description 14
- 229920000858 Cyclodextrin Polymers 0.000 claims abstract description 39
- HFHDHCJBZVLPGP-UHFFFAOYSA-N schardinger α-dextrin Chemical compound O1C(C(C2O)O)C(CO)OC2OC(C(C2O)O)C(CO)OC2OC(C(C2O)O)C(CO)OC2OC(C(O)C2O)C(CO)OC2OC(C(C2O)O)C(CO)OC2OC2C(O)C(O)C1OC2CO HFHDHCJBZVLPGP-UHFFFAOYSA-N 0.000 claims abstract description 39
- 239000004205 dimethyl polysiloxane Substances 0.000 claims abstract description 37
- 229920000435 poly(dimethylsiloxane) Polymers 0.000 claims abstract description 37
- -1 polydimethylsiloxane Polymers 0.000 claims abstract description 37
- CPLXHLVBOLITMK-UHFFFAOYSA-N magnesium oxide Inorganic materials [Mg]=O CPLXHLVBOLITMK-UHFFFAOYSA-N 0.000 claims abstract description 32
- 239000002994 raw material Substances 0.000 claims abstract description 30
- IVMYJDGYRUAWML-UHFFFAOYSA-N cobalt(ii) oxide Chemical compound [Co]=O IVMYJDGYRUAWML-UHFFFAOYSA-N 0.000 claims abstract description 28
- 229910000428 cobalt oxide Inorganic materials 0.000 claims abstract description 27
- 229910000480 nickel oxide Inorganic materials 0.000 claims abstract description 27
- GNRSAWUEBMWBQH-UHFFFAOYSA-N oxonickel Chemical compound [Ni]=O GNRSAWUEBMWBQH-UHFFFAOYSA-N 0.000 claims abstract description 27
- VYPSYNLAJGMNEJ-UHFFFAOYSA-N Silicium dioxide Chemical compound O=[Si]=O VYPSYNLAJGMNEJ-UHFFFAOYSA-N 0.000 claims abstract description 24
- BRPQOXSCLDDYGP-UHFFFAOYSA-N calcium oxide Chemical compound [O-2].[Ca+2] BRPQOXSCLDDYGP-UHFFFAOYSA-N 0.000 claims abstract description 21
- 239000000292 calcium oxide Substances 0.000 claims abstract description 21
- ODINCKMPIJJUCX-UHFFFAOYSA-N calcium oxide Inorganic materials [Ca]=O ODINCKMPIJJUCX-UHFFFAOYSA-N 0.000 claims abstract description 21
- 239000000395 magnesium oxide Substances 0.000 claims abstract description 21
- 229910052814 silicon oxide Inorganic materials 0.000 claims abstract description 20
- 239000002689 soil Substances 0.000 claims abstract description 19
- 239000000203 mixture Substances 0.000 claims abstract description 13
- AXZKOIWUVFPNLO-UHFFFAOYSA-N magnesium;oxygen(2-) Chemical compound [O-2].[Mg+2] AXZKOIWUVFPNLO-UHFFFAOYSA-N 0.000 claims abstract description 10
- SIWVEOZUMHYXCS-UHFFFAOYSA-N oxo(oxoyttriooxy)yttrium Chemical compound O=[Y]O[Y]=O SIWVEOZUMHYXCS-UHFFFAOYSA-N 0.000 claims abstract description 10
- RVTZCBVAJQQJTK-UHFFFAOYSA-N oxygen(2-);zirconium(4+) Chemical compound [O-2].[O-2].[Zr+4] RVTZCBVAJQQJTK-UHFFFAOYSA-N 0.000 claims abstract description 9
- 229910001928 zirconium oxide Inorganic materials 0.000 claims abstract description 9
- PEDCQBHIVMGVHV-UHFFFAOYSA-N Glycerine Chemical compound OCC(O)CO PEDCQBHIVMGVHV-UHFFFAOYSA-N 0.000 claims description 56
- 239000000463 material Substances 0.000 claims description 44
- 238000005245 sintering Methods 0.000 claims description 36
- MCMNRKCIXSYSNV-UHFFFAOYSA-N Zirconium dioxide Chemical compound O=[Zr]=O MCMNRKCIXSYSNV-UHFFFAOYSA-N 0.000 claims description 26
- 238000001035 drying Methods 0.000 claims description 19
- 238000007873 sieving Methods 0.000 claims description 18
- 238000000498 ball milling Methods 0.000 claims description 14
- 238000000034 method Methods 0.000 claims description 12
- RUDFQVOCFDJEEF-UHFFFAOYSA-N yttrium(III) oxide Inorganic materials [O-2].[O-2].[O-2].[Y+3].[Y+3] RUDFQVOCFDJEEF-UHFFFAOYSA-N 0.000 claims description 12
- 238000007731 hot pressing Methods 0.000 claims description 11
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims description 10
- 229910000831 Steel Inorganic materials 0.000 claims description 9
- 238000000748 compression moulding Methods 0.000 claims description 9
- 238000002156 mixing Methods 0.000 claims description 9
- 238000000465 moulding Methods 0.000 claims description 9
- 239000010959 steel Substances 0.000 claims description 9
- 238000003756 stirring Methods 0.000 claims description 9
- 238000005303 weighing Methods 0.000 claims description 9
- 239000000377 silicon dioxide Substances 0.000 claims description 2
- 235000011187 glycerol Nutrition 0.000 claims 2
- 230000000052 comparative effect Effects 0.000 description 30
- 238000010438 heat treatment Methods 0.000 description 12
- 238000007792 addition Methods 0.000 description 10
- 239000000243 solution Substances 0.000 description 10
- 229910052751 metal Inorganic materials 0.000 description 8
- 239000002184 metal Substances 0.000 description 8
- 239000002245 particle Substances 0.000 description 6
- 239000011148 porous material Substances 0.000 description 5
- 229910010293 ceramic material Inorganic materials 0.000 description 4
- 239000013078 crystal Substances 0.000 description 4
- 238000004321 preservation Methods 0.000 description 3
- 238000005979 thermal decomposition reaction Methods 0.000 description 3
- 230000009286 beneficial effect Effects 0.000 description 2
- 230000015572 biosynthetic process Effects 0.000 description 2
- 230000007797 corrosion Effects 0.000 description 2
- 238000005260 corrosion Methods 0.000 description 2
- 230000007547 defect Effects 0.000 description 2
- 239000011521 glass Substances 0.000 description 2
- 239000011159 matrix material Substances 0.000 description 2
- 239000002923 metal particle Substances 0.000 description 2
- 230000003014 reinforcing effect Effects 0.000 description 2
- 239000000126 substance Substances 0.000 description 2
- 239000000956 alloy Substances 0.000 description 1
- 229910045601 alloy Inorganic materials 0.000 description 1
- 229910052782 aluminium Inorganic materials 0.000 description 1
- XAGFODPZIPBFFR-UHFFFAOYSA-N aluminium Chemical compound [Al] XAGFODPZIPBFFR-UHFFFAOYSA-N 0.000 description 1
- 239000007864 aqueous solution Substances 0.000 description 1
- 238000005452 bending Methods 0.000 description 1
- RKTYLMNFRDHKIL-UHFFFAOYSA-N copper;5,10,15,20-tetraphenylporphyrin-22,24-diide Chemical compound [Cu+2].C1=CC(C(=C2C=CC([N-]2)=C(C=2C=CC=CC=2)C=2C=CC(N=2)=C(C=2C=CC=CC=2)C2=CC=C3[N-]2)C=2C=CC=CC=2)=NC1=C3C1=CC=CC=C1 RKTYLMNFRDHKIL-UHFFFAOYSA-N 0.000 description 1
- 238000000354 decomposition reaction Methods 0.000 description 1
- 238000011161 development Methods 0.000 description 1
- 239000006185 dispersion Substances 0.000 description 1
- 230000000694 effects Effects 0.000 description 1
- 238000010292 electrical insulation Methods 0.000 description 1
- 239000002223 garnet Substances 0.000 description 1
- 230000002401 inhibitory effect Effects 0.000 description 1
- 238000002844 melting Methods 0.000 description 1
- 230000008018 melting Effects 0.000 description 1
- 238000012986 modification Methods 0.000 description 1
- 230000004048 modification Effects 0.000 description 1
- 150000004767 nitrides Chemical class 0.000 description 1
- 230000008520 organization Effects 0.000 description 1
- 230000003647 oxidation Effects 0.000 description 1
- 238000007254 oxidation reaction Methods 0.000 description 1
- 238000011056 performance test Methods 0.000 description 1
- 239000000843 powder Substances 0.000 description 1
- 238000003825 pressing Methods 0.000 description 1
- 238000001179 sorption measurement Methods 0.000 description 1
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Abstract
The invention belongs to the field of ceramics, and relates to a preparation method of an alumina-based ceramic composite material. The preparation raw materials of the alumina-based ceramic comprise the following components in parts by weight: alumina: 65-75 parts of zirconium oxide: 2-4 parts of yttrium oxide: 2-4 parts of magnesium oxide: 0.5-3 parts of calcium oxide: 0.5-3 parts of silicon oxide: 1-4 parts of a mixture of nickel oxide and cobalt oxide: 0.5-10 parts of cyclodextrin: 3-6 parts, 2-5 parts of polydimethylsiloxane, and Suzhou soil: 3-10 parts.
Description
Technical Field
The invention belongs to the field of ceramics, and relates to a preparation method of an alumina-based ceramic composite material.
Background
The metal ceramic composite material is a material between high-temperature alloy and ceramic, and has the characteristics of high toughness and plasticity of metal, high melting point, corrosion resistance, wear resistance and the like of ceramic. According to the difference of ceramic phase, the metal ceramic is divided into oxide system, carbide system, boride system and nitride system, among which, the oxide system has the advantages of high hardness, good wear resistance and oxidation resistance, and is widely used, especially the alumina-based metal ceramic is more extensive. The alumina-based metal ceramic is the most stable substance in an oxide system, has the characteristics of high mechanical strength, high hardness, wear resistance, high temperature resistance, corrosion resistance, high electrical insulation, low dielectric loss and the like, is a ceramic material which is relatively early in development, low in cost and most widely applied, and has attractive application prospects in the aspects of aerospace, aviation, engine wear-resistant parts, cutters and the like. However, because the alumina-based ceramic has fatal defects of high brittleness, poor uniformity and the like, and the working reliability and the use safety of ceramic parts are influenced, so that how to improve the properties of the alumina-based ceramic, such as toughness, strength and the like, has important modern significance and practical application value.
Disclosure of Invention
Aiming at the defects of the existing alumina-based metal ceramic, the invention aims to add other oxides into the ceramic material to form a second phase so as to improve the toughness of the ceramic material; and cyclodextrin and polydimethylsiloxane are adopted to form a double-layer structure on the surface of the oxidized metal particles, so that a uniform structure is formed in the sintering process, the porosity is reduced, and the comprehensive performance of the alumina-based ceramic is improved.
In order to achieve the purpose, the invention adopts the following technical scheme: the preparation method of the alumina-based ceramic composite material comprises the following raw materials in parts by weight:
alumina: 65-75 parts of zirconium oxide: 2-4 parts of yttrium oxide: 2-4 parts of magnesium oxide: 0.5-3 parts of calcium oxide: 0.5-3 parts of silicon oxide: 1-4 parts of a mixture of nickel oxide and cobalt oxide: 0.5-10 parts of cyclodextrin: 3-6 parts, 2-5 parts of polydimethylsiloxane, and Suzhou soil: 3-10 parts.
Preferably, the mass ratio of the nickel oxide to the cobalt oxide is 1: (1-3).
Preferably, the preparation method comprises the following steps:
(1) weighing the components according to the raw material ratio, mixing alumina, zirconia, yttria, magnesia, calcium oxide, silica, nickel oxide, cobalt oxide, Suzhou soil and polydimethylsiloxane, and then adding glycerol for ball milling;
(2) drying the ball-milled materials, sieving with a 50-80 mesh sieve, placing the sieved materials in a cyclodextrin water solution, stirring for 20-60min, standing for 2-5h, drying again, and sieving with a 50-80 mesh sieve;
(3) putting the mixture into a steel die for compression molding;
(4) carrying out hot-pressing sintering on the pressed blank,
preferably, the ball milling time in the step (1) is 20-60h, and the rotation speed of the ball mill is 50-500 r/min.
Preferably, the glycerol added in the step (1) is respectively 1-1.5 times of the mass of the material.
Preferably, the concentration of the cyclodextrin aqueous solution is 10-50%.
Preferably, the molding pressure is 200-400MPa, and the dwell time is 5-10 min.
Preferably, in the hot-pressing sintering, the sintering temperature is 1200-1400 ℃, the heat preservation time is 1-4h, and the sintering pressure is 5-30 MPa.
Further preferably, in the hot-pressing sintering, the temperature is raised to 600-800 ℃ at the speed of 5-10 ℃/min, and then the temperature is heated to 1200-1400 ℃ at the speed of more than or equal to 50 ℃/min.
Compared with the prior art, the invention has the beneficial effects that:
on the basis of taking alumina as a main component, the ceramic composite material is added with zirconia, yttria, magnesia, calcium oxide, silicon oxide, nickel oxide and cobalt oxide, and the toughness of the ceramic material is improved through the formation of a second phase; and a double-layer structure of cyclodextrin and polydimethylsiloxane is formed on the surfaces of the oxidized metal particles, and the sintered pores are reduced and the density is improved by utilizing the adhesion effect of the two substances and the difference of thermal decomposition temperature. The finally obtained composite material has good isotropy, structural uniformity and high-temperature creep resistance, and simultaneously, the strength, the toughness and the like are improved.
Detailed Description
The technical solution of the present invention is further described below by means of specific examples. The raw materials used in the examples of the present invention are those commonly used in the art, and the methods used in the examples are those conventional in the art, unless otherwise specified.
In one embodiment of the invention, the preparation raw materials of the alumina-based ceramic comprise the following components in parts by weight: alumina: 65-75 parts of zirconium oxide: 2-4 parts of yttrium oxide: 2-4 parts of magnesium oxide: 0.5-3 parts of calcium oxide: 0.5-3 parts of silicon oxide: 1-4 parts of a mixture of nickel oxide and cobalt oxide: 0.5-10 parts of cyclodextrin: 3-6 parts, 2-5 parts of polydimethylsiloxane, and Suzhou soil: 3-10 parts. Wherein the mass ratio of nickel oxide to cobalt oxide is 1: (1-3).
In the alumina-based ceramic matrix material, alumina is used as a main component, a small amount of zirconia, yttria, magnesia, calcium oxide, silicon oxide, nickel oxide and cobalt oxide are doped as reinforcing components, a second phase formed by the reinforcing components is distributed on the grain boundary of the alumina-based matrix, the increase of alumina grains is inhibited, microcracks are generated at the tips of cracks, stress concentration is relieved, and ductile crack bridges formed on the upper and lower surfaces of the cracks can obviously improve the fracture toughness of the material. More specifically, the silicon oxide can reduce the sintering temperature, increase the intermolecular tension, increase the glass phase and inhibit the oversize of alumina grains; the yttrium oxide forms second-phase aluminum garnet at the grain boundary, thereby inhibiting the growth of crystal grains, reducing the generation of closed air holes and increasing the compactness of the ceramic; in the ceramic forming process, the zirconia is beneficial to the formation of a glass phase, the bonding strength of a second phase is increased, the porosity is reduced, when the ceramic is acted by an external force, the cobalt oxide forms tetragonal crystals to be monoclinic crystals, the volume is rapidly expanded, further, the expansion of the existing micro cracks in the ceramic can be prevented, and the ceramic fracture is relieved; the simultaneous addition of nickel oxide and cobalt oxide can play a toughening role better than the single addition, and when the simultaneous addition is carried out, the mass ratio of nickel oxide to cobalt oxide is controlled to be 1: (1-3).
In one embodiment of the present invention, a method for preparing an alumina-based ceramic includes the steps of:
(1) weighing the components according to the raw material ratio, mixing alumina, zirconia, yttria, magnesia, calcium oxide, silicon oxide, nickel oxide, cobalt oxide, Suzhou soil and polydimethylsiloxane, adding glycerol, and carrying out ball milling for 20-60h, wherein the mass of the glycerol is 1-1.5 times that of the materials, and the rotating speed of a ball mill is 50-500 r/min.
The adoption of the glycerol wet ball milling can not only uniformly disperse the powder, but also refine the particle size to obtain a uniform dispersion system with refined grains, and the particle size after ball milling is controlled to be 0.1-2 mu m.
(2) Drying the ball-milled materials, sieving with a 50-80 mesh sieve, placing the sieved materials in 10-50% cyclodextrin water solution, stirring for 20-60min, standing for 2-5h, drying again, and sieving with a 50-80 mesh sieve.
(3) And putting the mixture into a steel die for compression molding, wherein the molding pressure is 200-400MPa, and the pressure maintaining time is 5-10 min.
(4) And carrying out hot-pressing sintering on the pressed blank, wherein the sintering temperature is 1200-1400 ℃, the heat preservation time is 1-4h, and the sintering pressure is 5-30 MPa.
And (3) drying the ball-milled materials for the first time, solidifying the polydimethylsiloxane adsorbed on the surfaces of the particles, and then placing the solidified polydimethylsiloxane into a thick cyclodextrin water solution, wherein the polydimethylsiloxane has stronger adsorption capacity to the cyclodextrin, and the cyclodextrin is deposited on the surfaces of the particles solidified with the polydimethylsiloxane, so that oxide particles form a double-layer structure of a polydimethylsiloxane layer and a cyclodextrin layer from inside to outside. The cyclodextrin has strong adsorbability between layers, and in the pressing process, the cyclodextrin tightly adheres oxide particles, so that the sintering density is improved. The thermal decomposition speed of the cyclodextrin layer is lower than that of polydimethylsiloxane, the cyclodextrin layer is firstly thermally decomposed and volatilized in the sintering process, formed pores are filled with the polydimethylsiloxane, then the polydimethylsiloxane is thermally decomposed, the pores are decomposed layer by layer to reduce the generation of sintering pores, and crystal grains are refined to form a uniform organization structure.
The sintering process can be carried out by heating to 1200-1400 ℃ at a conventional speed and carrying out heat preservation sintering. The temperature can be further optimized and selected, the temperature is firstly increased to 600 ℃ at the speed of 5-10 ℃/min, and then the temperature is heated to 1200-1400 ℃ at the speed of more than or equal to 50 ℃/min. The slow temperature rise can prolong the thermal decomposition interval time of the cyclodextrin layer and the polydimethylsiloxane, so that the polydimethylsiloxane layer has enough time to fill the pores left by the decomposition of the cyclodextrin layer, and the tissue structure can be refined.
Example 1
The alumina-based ceramic composite material of the embodiment is prepared from the following raw materials in parts by weight: alumina: 70 parts of zirconium oxide: 3 parts, yttrium oxide: 3 parts of magnesium oxide: 2 parts, calcium oxide: 1 part, silicon oxide: 2 parts, nickel oxide: 2 parts, cobalt oxide: 5 parts, cyclodextrin: 4 parts, 3 parts of polydimethylsiloxane, and Suzhou soil: 5 parts of the raw materials.
Weighing the components according to the proportion of the raw materials, mixing alumina, zirconia, yttria, magnesia, calcium oxide, silicon oxide, nickel oxide, cobalt oxide, Suzhou soil and polydimethylsiloxane, adding glycerol, and carrying out ball milling for 40 hours, wherein the rotating speed of the ball mill is 200 revolutions per minute, and the addition amount of the glycerol is 1.2 times of that of the materials; drying the ball-milled materials, sieving the ball-milled materials by a 60-mesh sieve, then placing the sieved materials in a 30% cyclodextrin water solution, stirring for 40min, standing for 3h, drying again and sieving the materials by the 60-mesh sieve; putting the mixture dried again into a steel mould for compression molding, wherein the molding pressure is 300MPa, and the pressure maintaining time is 8 min; and (3) carrying out hot-pressing sintering on the pressed blank, conventionally heating the blank to 1300 ℃ in a vacuum furnace, keeping the temperature and sintering for 3h, and sintering under the applied pressure of 20 MPa.
Example 2
The alumina-based ceramic composite material of the embodiment is prepared from the following raw materials in parts by weight: alumina: 70 parts of zirconium oxide: 3 parts, yttrium oxide: 3 parts of magnesium oxide: 2 parts, calcium oxide: 1 part, silicon oxide: 2 parts, nickel oxide: 2 parts, cobalt oxide: 5 parts, cyclodextrin: 4 parts, 3 parts of polydimethylsiloxane, and Suzhou soil: 5 parts of the raw materials.
Weighing the components according to the proportion of the raw materials, mixing alumina, zirconia, yttria, magnesia, calcium oxide, silicon oxide, nickel oxide, cobalt oxide, Suzhou soil and polydimethylsiloxane, adding glycerol, and carrying out ball milling for 40 hours, wherein the rotating speed of the ball mill is 200 revolutions per minute, and the addition amount of the glycerol is 1.2 times of that of the materials; drying the ball-milled materials, sieving the ball-milled materials by a 60-mesh sieve, then placing the sieved materials in a 30% cyclodextrin water solution, stirring for 40min, standing for 3h, drying again and sieving the materials by the 60-mesh sieve; putting the mixture dried again into a steel mould for compression molding, wherein the molding pressure is 300MPa, and the pressure maintaining time is 8 min; and (3) carrying out hot-pressing sintering on the pressed blank, heating the blank to 700 ℃ in a vacuum furnace at the speed of 8 ℃/min, then heating the blank to 1300 ℃ at the speed of 60 ℃/min, keeping the temperature and sintering for 3h, and applying the sintering pressure of 20 MPa.
Example 3
The alumina-based ceramic composite material of the embodiment is prepared from the following raw materials in parts by weight: alumina: 70 parts of zirconium oxide: 3 parts, yttrium oxide: 3 parts of magnesium oxide: 2 parts, calcium oxide: 1 part, silicon oxide: 2 parts, nickel oxide: 5 parts, cobalt oxide: 2 parts, cyclodextrin: 4 parts, 3 parts of polydimethylsiloxane, and Suzhou soil: 5 parts of the raw materials.
Weighing the components according to the proportion of the raw materials, mixing alumina, zirconia, yttria, magnesia, calcium oxide, silicon oxide, nickel oxide, cobalt oxide, Suzhou soil and polydimethylsiloxane, adding glycerol, and carrying out ball milling for 40 hours, wherein the rotating speed of the ball mill is 200 revolutions per minute, and the addition amount of the glycerol is 1.2 times of that of the materials; drying the ball-milled materials, sieving the ball-milled materials by a 60-mesh sieve, then placing the sieved materials in a 30% cyclodextrin water solution, stirring for 40min, standing for 3h, drying again and sieving the materials by the 60-mesh sieve; putting the mixture dried again into a steel mould for compression molding, wherein the molding pressure is 300MPa, and the pressure maintaining time is 8 min; and (3) carrying out hot-pressing sintering on the pressed blank, heating the blank to 700 ℃ in a vacuum furnace at the speed of 8 ℃/min, then heating the blank to 1300 ℃ at the speed of 60 ℃/min, keeping the temperature and sintering for 3h, and applying the sintering pressure of 20 MPa.
Example 4
The alumina-based ceramic composite material of the embodiment is prepared from the following raw materials in parts by weight: alumina: 70 parts of zirconium oxide: 3 parts, yttrium oxide: 3 parts of magnesium oxide: 2 parts, calcium oxide: 1 part, silicon oxide: 2 parts, nickel oxide: 2 parts, cobalt oxide: 5 parts, cyclodextrin: 4 parts, 3 parts of polydimethylsiloxane, and Suzhou soil: 5 parts of the raw materials.
Weighing the components according to the proportion of the raw materials, mixing alumina, zirconia, yttria, magnesia, calcium oxide, silicon oxide, nickel oxide, cobalt oxide, Suzhou soil and polydimethylsiloxane, adding glycerol, and carrying out ball milling for 40 hours, wherein the rotating speed of the ball mill is 200 revolutions per minute, and the addition amount of the glycerol is 1.2 times of that of the materials; drying the ball-milled materials, sieving the ball-milled materials with a 60-mesh sieve, then placing the sieved materials in a 5% cyclodextrin water solution, stirring for 40min, standing for 3h, drying again and sieving with the 60-mesh sieve; putting the mixture dried again into a steel mould for compression molding, wherein the molding pressure is 300MPa, and the pressure maintaining time is 8 min; and (3) carrying out hot-pressing sintering on the pressed blank, heating the blank to 700 ℃ in a vacuum furnace at the speed of 8 ℃/min, then heating the blank to 1300 ℃ at the speed of 60 ℃/min, keeping the temperature and sintering for 3h, and applying the sintering pressure of 20 MPa.
Example 5
The alumina-based ceramic composite material of the embodiment is prepared from the following raw materials in parts by weight: alumina: 65 parts, zirconia: 4 parts, yttrium oxide: 4 parts, magnesium oxide: 0.5 part, calcium oxide: 0.5 part, silicon oxide: 1 part, nickel oxide: 3 parts of cobalt oxide: 5 parts, cyclodextrin: 6 parts, 5 parts of polydimethylsiloxane, and Suzhou soil: 6 parts.
Weighing the components according to the proportion of the raw materials, mixing alumina, zirconia, yttria, magnesia, calcium oxide, silicon oxide, nickel oxide, cobalt oxide, Suzhou soil and polydimethylsiloxane, adding glycerol, and carrying out ball milling for 30 hours, wherein the rotating speed of the ball mill is 100 revolutions per minute, and the addition of the glycerol is 1.0 time of that of the materials; drying the ball-milled materials, sieving the ball-milled materials with a 50-mesh sieve, then placing the sieved materials in a cyclodextrin water solution with the concentration of 20%, stirring for 30min, standing for 4h, and drying again and sieving the ball-milled materials with the 50-mesh sieve; putting the mixture dried again into a steel mould for compression molding, wherein the molding pressure is 200MPa, and the pressure maintaining time is 10 min; and (3) carrying out hot-pressing sintering on the pressed blank, heating the blank to 600 ℃ in a vacuum furnace at the speed of 10 ℃/min, then heating the blank to 1200 ℃ at the speed of 70 ℃/min, keeping the temperature for sintering for 2h, and applying the sintering pressure of 30 MPa.
Example 6
The alumina-based ceramic composite material of the embodiment is prepared from the following raw materials in parts by weight: alumina: 75 parts of zirconium oxide: 2 parts, yttrium oxide: 2 parts, magnesium oxide: 3 parts, calcium oxide: 3 parts, silicon oxide: 1 part, nickel oxide: 1 part, cobalt oxide: 3 parts, cyclodextrin: 4 parts, 3 parts of polydimethylsiloxane, and Suzhou soil: 5 parts of the raw materials.
Weighing the components according to the proportion of the raw materials, mixing alumina, zirconia, yttria, magnesia, calcium oxide, silicon oxide, nickel oxide, cobalt oxide, Suzhou soil and polydimethylsiloxane, adding glycerol, and carrying out ball milling for 40 hours, wherein the rotating speed of the ball mill is 300 revolutions per minute, and the addition amount of the glycerol is 1.5 times of that of the materials; drying the ball-milled materials, sieving the ball-milled materials with an 80-mesh sieve, then placing the sieved materials in a 40% cyclodextrin water solution, stirring for 50min, standing for 3h, drying again and sieving the materials with an 80-mesh sieve; putting the mixture dried again into a steel mould for compression molding, wherein the molding pressure is 300MPa, and the pressure maintaining time is 5 min; and (3) carrying out hot-pressing sintering on the pressed blank, heating the blank to 800 ℃ in a vacuum furnace at the speed of 5 ℃/min, then heating the blank to 1400 ℃ at the speed of 80 ℃/min, keeping the temperature for sintering for 3h, and applying the sintering pressure of 10 MPa.
Comparative example 1
The difference between the comparative example 1 and the example 2 is that cyclodextrin is not included in the raw materials for preparing the ceramic composite material of the comparative example 1, and the ball-milled materials are directly pressed and formed after being dried and sieved by a 60-mesh sieve. The rest is the same as in example 2.
Comparative example 2
Comparative example 2 is different from example 2 in that polydimethylsiloxane is not included in the ceramic composite material preparation raw material of comparative example 2, and the rest is the same as example 2.
Comparative example 3
The difference between the comparative example 3 and the example 2 is that the raw materials for preparing the ceramic composite material of the comparative example 3 do not contain cyclodextrin and polydimethylsiloxane, and the ball-milled materials are dried, sieved by a 60-mesh sieve and then directly pressed and molded. The rest is the same as in example 2.
Comparative example 4
The difference between the comparative example 4 and the example 2 is that in the preparation method of the ceramic composite material of the comparative example 4, cyclodextrin and polydimethylsiloxane are mixed with oxide in a ball milling mode, and the ball-milled material is directly pressed and formed after being dried and sieved by a 60-mesh sieve. The rest is the same as in example 2.
Comparative example 5
Comparative example 5 is different from example 2 in that nickel oxide is not included in the ceramic composite raw material of comparative example 5, and the rest is the same as example 2.
Comparative example 6
Comparative example 6 is different from example 2 in that cobalt oxide is not included in the ceramic composite raw material of comparative example 6, and the rest is the same as example 2.
The ceramic composite materials of examples 1 to 6 and comparative examples 1 to 6 were subjected to performance tests, and the results are shown in table 1.
TABLE 1
| Examples | Density g/cm3 | Porosity% | Bending strength MPa | Fracture toughness Mpa m1/2 |
| Example 1 | 3.30 | 1.6 | 775 | 13.9 |
| Example 2 | 3.35 | 0.6 | 820 | 14.8 |
| Example 3 | 3.26 | 2.3 | 680 | 12.5 |
| Example 4 | 3.25 | 2.7 | 700 | 13.1 |
| Example 5 | 3.32 | 0.9 | 800 | 14.5 |
| Example 6 | 3.33 | 0.8 | 810 | 14.6 |
| Comparative example 1 | 3.12 | 4.5 | 545 | 10.7 |
| Comparative example 2 | 3.13 | 4.3 | 580 | 10.5 |
| Comparative example 3 | 3.10 | 5.2 | 500 | 9.9 |
| Comparative example 4 | 3.12 | 4.2 | 530 | 10.2 |
| Comparative example 5 | 3.18 | 2.9 | 620 | 12.1 |
| Comparative example 6 | 3.19 | 2.8 | 610 | 11.9 |
As can be seen from table 1, the density, porosity and toughness of comparative examples 1 to 6 are lower than those of the ceramic composite materials of examples 1 to 6, particularly comparative examples 1 to 3, and poor performance is exhibited because cyclodextrin and polydimethylsiloxane are respectively absent in the composite materials of comparative examples 1 to 2, and cyclodextrin and polydimethylsiloxane are simultaneously absent in comparative example 3, while comparative example 4, which contains cyclodextrin and polydimethylsiloxane but are added together with the oxidized metal, hardly forms a double-layer structure on the oxidized metal surface and also exhibits poor performance. And the embodiment 2 adopts the better parameters of the embodiment of the invention, and has better performance compared with the embodiments 1, 3-6.
The specific embodiments described herein are merely illustrative of the spirit of the invention. Various modifications or additions may be made to the described embodiments or alternatives may be employed by those skilled in the art without departing from the spirit or ambit of the invention as defined in the appended claims.
Claims (8)
1. The preparation method of the alumina-based ceramic composite material is characterized in that the alumina-based ceramic is prepared from the following raw materials in parts by weight:
alumina: 65-75 parts of zirconium oxide: 2-4 parts of yttrium oxide: 2-4 parts of magnesium oxide: 0.5-3 parts of calcium oxide: 0.5-3 parts of silicon oxide: 1-4 parts of a mixture of nickel oxide and cobalt oxide: 0.5-10 parts of cyclodextrin: 3-6 parts, 2-5 parts of polydimethylsiloxane, and Suzhou soil: 3-10 parts;
the preparation method comprises the following steps:
(1) weighing the components according to the proportion of the raw materials, mixing alumina, zirconia, yttria, magnesia, calcium oxide, silica, nickel oxide, cobalt oxide, Suzhou soil and polydimethylsiloxane, and then adding glycerol for ball milling;
(2) drying the ball-milled materials, sieving with a 50-80 mesh sieve, placing the sieved materials in a cyclodextrin water solution, stirring for 20-60min, standing for 2-5h, drying again, and sieving with a 50-80 mesh sieve;
(3) putting the mixture into a steel die for compression molding;
(4) and carrying out hot-pressing sintering on the pressed blank.
2. The method according to claim 1, wherein the mass ratio of the nickel oxide to the cobalt oxide is 1: (1-3).
3. The preparation method according to claim 1, wherein the ball milling time in the step (1) is 20-60h, and the rotation speed of the ball mill is 50-500 rpm.
4. The method according to claim 1, wherein the glycerin is added in an amount of 1 to 1.5 times by mass based on the material in the step (1).
5. The method according to claim 1, wherein the concentration of the aqueous cyclodextrin solution is 10 to 50%.
6. The preparation method according to claim 1, wherein the molding pressure is 200-400MPa, and the dwell time is 5-10 min.
7. The method as claimed in claim 1, wherein the sintering temperature is 1200-1400 ℃, the holding time is 1-4h, and the sintering pressure is 5-30 MPa.
8. The method as claimed in claim 7, wherein the temperature is raised to 800 ℃ at a rate of 5-10 ℃/min, and then to 1400 ℃ at a rate of 50 ℃/min.
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