CN113860857A - Alumina ceramic composite material and preparation method and application thereof - Google Patents
Alumina ceramic composite material and preparation method and application thereof Download PDFInfo
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Abstract
The invention provides an alumina ceramic composite material which is prepared from the following raw materials in percentage by mass: 72-97.9% of aluminum oxide, 0.1-5% of graphene, 1-10% of zirconium oxide, 0.5-3% of sintering aid and 0.5-10% of binder. The alumina ceramic composite material provided by the invention takes alumina as a matrix, and the content of the alumina ceramic composite material is adjusted, so that the graphene and the zirconia have a synergistic toughening effect, and the toughness of the alumina ceramic material is improved. Experimental results show that the bending strength of the alumina ceramic composite material is 648-728 MPa, and the fracture toughness is 6.0-7.6 MPa.m1/2。
Description
Technical Field
The invention relates to the technical field of ceramic materials, in particular to an alumina ceramic composite material and a preparation method and application thereof.
Background
The alumina ceramic material has the characteristics of high hardness, high temperature resistance, corrosion resistance, wear resistance and the like, is widely applied to various fields of machinery, metallurgy, chemical industry, medical treatment and the like, but has low toughness, influences the service life and limits the application range.
At present, the toughening of the alumina ceramic material is mainly to add rare earth oxide into the alumina ceramic material, for example, the influence of the rare earth oxide on the performance of the alumina ceramic is researched by yaojing of Nanjing university of industry, and the addition of the rare earth oxide is considered to not only reduce the sintering temperature of the alumina ceramic, but also improve the toughness; and for example, after the influence of the rare earth oxide on the ceramic fiber structure and the mechanical property is researched by the ministry of the university of Jia Musi and the like, the addition of the rare earth oxide has larger influence on the microstructure and the mechanical property of the material, the toughening mechanism is mainly the toughening effect brought by crack bridging, bifurcation and deflection, and the bridging of crack tips and the crystal grain pulling-out mechanism in the fracture process, and the fracture toughness of the material is greatly improved. However, as the requirements for the use environment of the alumina ceramic material become more stringent, the requirement for toughness becomes higher, and thus, providing the alumina ceramic material with high toughness becomes a problem to be solved urgently.
Disclosure of Invention
The invention aims to provide an alumina ceramic composite material, and a preparation method and application thereof. The alumina ceramic composite material provided by the invention has high toughness.
In order to achieve the above object, the present invention provides the following technical solutions:
the invention provides an alumina ceramic composite material which is prepared from the following raw materials in percentage by mass: 72-97.9% of aluminum oxide, 0.1-5% of graphene, 1-10% of zirconium oxide, 0.5-3% of sintering aid and 0.5-10% of binder.
Preferably, the material is prepared from the following raw materials in percentage by mass: 75-95% of aluminum oxide, 0.5-4% of graphene, 3.5-8% of zirconium oxide, 0.5-3% of sintering aid and 0.5-10% of binder.
Preferably, the material is prepared from the following raw materials in percentage by mass: 80-90% of aluminum oxide, 1-2% of graphene, 4.5-6% of zirconium oxide, 1-2% of sintering aid and 3.5-10% of binder.
Preferably, the particle size of the alumina is 100nm to 3 μm.
Preferably, the sintering aid comprises at least one of calcium oxide, magnesium oxide, silicon dioxide, lanthanum oxide and titanium dioxide.
Preferably, the binder comprises PVA and/or PVB.
The invention also provides a preparation method of the alumina ceramic composite material, which comprises the following steps:
(1) mixing alumina, graphene, zirconia, a sintering aid and a binder, and then carrying out ball milling to obtain a mixed material;
(2) and (2) sequentially pressing and sintering the mixed material obtained in the step (1) to obtain the alumina ceramic composite material.
Preferably, the rotation speed of ball milling in the step (1) is 400-500 r/min, and the ball milling time is 1-1.5 h.
Preferably, the sintering temperature in the step (2) is 1200-1500 ℃, and the sintering time is 30-120 min.
The invention also provides the application of the alumina ceramic composite material in the technical scheme or the alumina ceramic composite material prepared by the preparation method in the technical scheme in a ceramic filter plate.
The invention provides an alumina ceramic composite material which is prepared from the following raw materials in percentage by mass: 72-97.9% of aluminum oxide, 0.1-5% of graphene, 1-10% of zirconium oxide, 0.5-3% of sintering aid and 0.5-10% of binder. The alumina ceramic composite material provided by the invention takes alumina as a matrix, and the content of the alumina ceramic composite material is adjusted, so that the graphene and the zirconia have a synergistic toughening effect, and the toughness of the alumina ceramic material is improved. Experimental results show that the bending strength of the alumina ceramic composite material is 648-728 MPa, and the fracture toughness is 6.0-7.6 MPa.m1/2。
Detailed Description
The invention provides an alumina ceramic composite material which is prepared from the following raw materials in percentage by mass: 72-97.9% of aluminum oxide, 0.1-5% of graphene, 1-10% of zirconium oxide, 0.5-3% of sintering aid and 0.5-10% of binder.
The raw materials of the alumina ceramic composite material comprise, by mass, 72-97.9% of alumina, preferably 75-95%, more preferably 80-90%, and even more preferably 85%. In the present invention, the particle size of the alumina is preferably 100nm to 3 μm, and more preferably 1 to 2 μm. The source of the alumina is not particularly limited in the present invention, and commercially available products known to those skilled in the art may be used. In the present invention, the alumina is a matrix of the composite material.
The raw materials of the alumina ceramic composite material provided by the invention also comprise 0.1-5% of graphene by mass percentage, preferably 0.5-4%, further preferably 1-2%, and more preferably 1.5%. In the invention, the thickness of the graphene is preferably 1-5 nm; the diameter of the graphene is preferably 5-10 mu m. The source of the graphene is not particularly limited in the present invention, and commercially available products known to those skilled in the art may be used. In the invention, the graphene and the zirconia can be used for synergistically toughening, so that the toughness of the alumina ceramic composite material is improved.
The raw materials of the alumina ceramic composite material provided by the invention also comprise 1-10% of zirconia by mass percentage, preferably 3.5-8%, further preferably 4.5-6%, and more preferably 5-5.5%. In the present invention, the particle size of the zirconia is preferably 80nm to 1 μm. The source of the zirconia in the present invention is not particularly limited, and commercially available products known to those skilled in the art may be used. In the invention, the aluminum oxide and the graphene can be synergistically toughened, so that the toughness of the aluminum oxide ceramic composite material is improved.
The raw materials of the alumina ceramic composite material also comprise 0.5-3% of sintering aid by mass percentage, preferably 1-2%, more preferably 1.5%. In the present invention, the sintering aid preferably includes at least one of calcium oxide, magnesium oxide, silicon dioxide, lanthanum oxide, and titanium dioxide, more preferably lanthanum oxide; the particle size of the sintering aid is preferably larger than 600 mesh. The source of the sintering aid is not particularly limited in the present invention, and commercially available products known to those skilled in the art may be used. In the invention, the sintering aid can not only reduce the sintering temperature, but also further improve the toughness of the alumina ceramic composite material.
The raw materials of the alumina ceramic composite material also comprise 0.5-10% of binder by mass percentage, preferably 3.5-10%, and more preferably 5-8%. In the present invention, the binder preferably comprises PVA and/or PVB. The source of the binder is not particularly limited in the present invention, and commercially available products known to those skilled in the art may be used. In the present invention, the binder plays a role of binding.
The alumina ceramic composite material provided by the invention takes alumina as a matrix, and the content of the alumina ceramic composite material is adjusted, so that the graphene and the zirconia have a synergistic toughening effect, and the toughness of the alumina ceramic material is improved.
The invention also provides a preparation method of the alumina ceramic composite material, which comprises the following steps:
(1) mixing alumina, graphene, zirconia, a sintering aid and a binder, and then carrying out ball milling to obtain a mixed material;
(2) and (2) sequentially pressing and sintering the mixed material obtained in the step (1) to obtain the alumina ceramic composite material.
The method comprises the steps of mixing alumina, graphene, zirconia, a sintering aid and a binder, and then carrying out ball milling to obtain a mixed material.
The operation of mixing the alumina, the graphene, the zirconia, the sintering aid and the binder is not particularly limited, and the technical scheme for preparing the mixed material, which is well known to those skilled in the art, is adopted.
In the invention, the ball milling is preferably carried out in a ball mill, and the rotating speed of the ball milling is preferably 400-500 r/min; the ball milling time is preferably 1-1.5 h, and more preferably 1.2-1.3 h. The ball mill of the present invention is not particularly limited in its type, and a ball mill known to those skilled in the art may be used. The invention can realize the uniform dispersion of the raw materials by controlling the rotation speed and time of the ball milling.
After the mixed material is obtained, the mixed material is sequentially pressed and sintered to obtain the alumina ceramic composite material.
In the present invention, the pressing preferably includes one of roll forming, isostatic pressing, and axial pressing; the pressing pressure is preferably 100-500 MPa, and more preferably 200-300 MPa; the pressing time is preferably 1-5 min, and more preferably 2-3 min.
In the invention, the sintering temperature is preferably 1200-1500 ℃, and more preferably 1300-1400 ℃; the sintering time is preferably 30-120 min, more preferably 60-100 min, and even more preferably 80-90 min. In the invention, the sintering can improve the density of the compact body, thereby improving the mechanical property of the composite material.
In the present invention, the sintering is preferably vacuum sintering; the degree of vacuum of the vacuum sintering is preferably not higher than 3X 10-1Pa。
The preparation method provided by the invention is simple in process and suitable for industrial production.
The invention also provides the application of the alumina ceramic composite material in the technical scheme or the alumina ceramic composite material prepared by the preparation method in the technical scheme in a ceramic filter plate. The application operation of the alumina ceramic composite material in the ceramic filter plate is not particularly limited, and the application operation known by the technicians in the field can be adopted.
The technical solution of the present invention will be clearly and completely described below with reference to the embodiments of the present invention. It is to be understood that the described embodiments are merely exemplary of the invention, and not restrictive of the full scope of the invention. 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 alumina ceramic composite material is prepared from the following raw materials in percentage by mass: 97.9% of alumina, 0.1% of graphene, 1% of zirconia, 0.5% of sintering aid and 0.5% of binder;
wherein the particle size of the alumina is 1-2 μm; the thickness of the graphene is 1-5 nm, and the diameter of the graphene is 5-10 mu m; the particle size of the zirconia is 80 nm; the sintering aid is lanthanum oxide with the granularity of 1000 meshes; the adhesive is PVB;
the preparation method of the alumina ceramic composite material comprises the following steps:
(1) mixing alumina, graphene, zirconia, a sintering aid and a binder, and then carrying out ball milling to obtain a mixed material; wherein the rotation speed of the ball milling is 400r/min, and the time is 1.5 h;
(2) sequentially pressing and vacuum sintering the mixed material obtained in the step (1) to obtain an alumina ceramic composite material; wherein the pressing is isostatic pressing, the pressure is 200MPa, and the time is 5 min; sintering at 1200 deg.C for 100 min; the vacuum degree of vacuum sintering is 3 multiplied by 10-1Pa。
Example 2
The alumina ceramic composite material is prepared from the following raw materials in percentage by mass: 95% of alumina, 0.5% of graphene, 3.5% of zirconia, 0.5% of sintering aid and 0.5% of binder;
wherein the particle size of the alumina is 1-2 μm; the thickness of the graphene is 1-5 nm, and the diameter of the graphene is 5-10 mu m; the particle size of the zirconia is 80 nm; the sintering aid is lanthanum oxide with the granularity of 1000 meshes; the adhesive is PVB;
the preparation method of the alumina ceramic composite material comprises the following steps:
(1) mixing alumina, graphene, zirconia, a sintering aid and a binder, and then carrying out ball milling to obtain a mixed material; wherein the rotation speed of the ball milling is 400r/min, and the time is 1.5 h;
(2) sequentially pressing and vacuum sintering the mixed material obtained in the step (1) to obtain an alumina ceramic composite material; wherein the pressing is isostatic pressing, the pressure is 200MPa, and the time is 5 min; sintering at 1200 deg.C for 100 min; the vacuum degree of vacuum sintering is 3 multiplied by 10-1Pa。
Example 3
The alumina ceramic composite material is prepared from the following raw materials in percentage by mass: 90% of alumina, 1% of graphene, 4.5% of zirconia, 1% of sintering aid and 3.5% of binder;
wherein the particle size of the alumina is 1-2 μm; the thickness of the graphene is 1-5 nm, and the diameter of the graphene is 5-10 mu m; the particle size of the zirconia is 80 nm; the sintering aid is lanthanum oxide with the granularity of 1000 meshes; the adhesive is PVB;
the preparation method of the alumina ceramic composite material comprises the following steps:
(1) mixing alumina, graphene, zirconia, a sintering aid and a binder, and then carrying out ball milling to obtain a mixed material; wherein the rotation speed of the ball milling is 400r/min, and the time is 1.5 h;
(2) sequentially pressing and vacuum sintering the mixed material obtained in the step (1) to obtain an alumina ceramic composite material; wherein the pressing is isostatic pressing, the pressure is 200MPa, and the time is 5 min; sintering at 1200 deg.C for 100 min; the vacuum degree of vacuum sintering is 3 multiplied by 10-1Pa。
Example 4
The alumina ceramic composite material is prepared from the following raw materials in percentage by mass: 80% of alumina, 2% of graphene, 6% of zirconia, 2% of sintering aid and 10% of binder;
wherein the particle size of the alumina is 1-2 μm; the thickness of the graphene is 1-5 nm, and the diameter of the graphene is 5-10 mu m; the particle size of the zirconia is 80 nm; the sintering aid is lanthanum oxide with the granularity of 1000 meshes; the adhesive is PVB;
the preparation method of the alumina ceramic composite material comprises the following steps:
(1) mixing alumina, graphene, zirconia, a sintering aid and a binder, and then carrying out ball milling to obtain a mixed material; wherein the rotation speed of the ball milling is 400r/min, and the time is 1.5 h;
(2) sequentially pressing and vacuum sintering the mixed material obtained in the step (1) to obtain an alumina ceramic composite material; wherein the pressing is isostatic pressing, the pressure is 200MPa, and the time is 5 min; sintering at 1200 deg.C for 100 min; the vacuum degree of vacuum sintering is 3 multiplied by 10-1Pa。
Example 5
The alumina ceramic composite material is prepared from the following raw materials in percentage by mass: 75% of aluminum oxide, 4% of graphene, 8% of zirconium oxide, 3% of sintering aid and 10% of binder;
wherein the particle size of the alumina is 1-2 μm; the thickness of the graphene is 1-5 nm, and the diameter of the graphene is 5-10 mu m; the particle size of the zirconia is 80 nm; the sintering aid is lanthanum oxide with the granularity of 1000 meshes; the adhesive is PVB;
the preparation method of the alumina ceramic composite material comprises the following steps:
(1) mixing alumina, graphene, zirconia, a sintering aid and a binder, and then carrying out ball milling to obtain a mixed material; wherein the rotation speed of the ball milling is 400r/min, and the time is 1.5 h;
(2) sequentially pressing and vacuum sintering the mixed material obtained in the step (1) to obtain an alumina ceramic composite material; wherein the pressing is isostatic pressing, the pressure is 200MPa, and the time is 5 min; sintering at 1200 deg.C for 100 min; the vacuum degree of vacuum sintering is 3 multiplied by 10-1Pa
Example 6
The alumina ceramic composite material is prepared from the following raw materials in percentage by mass: 72% of aluminum oxide, 5% of graphene, 10% of zirconium oxide, 3% of sintering aid and 10% of binder;
wherein the particle size of the alumina is 1-2 μm; the thickness of the graphene is 1-5 nm, and the diameter of the graphene is 5-10 mu m; the particle size of the zirconia is 80 nm; the sintering aid is lanthanum oxide with the granularity of 1000 meshes; the adhesive is PVB;
the preparation method of the alumina ceramic composite material comprises the following steps:
(1) mixing alumina, graphene, zirconia, a sintering aid and a binder, and then carrying out ball milling to obtain a mixed material; wherein the rotation speed of the ball milling is 400r/min, and the time is 1.5 h;
(2) sequentially pressing and vacuum sintering the mixed material obtained in the step (1) to obtain an alumina ceramic composite material; wherein the pressing is isostatic pressing, the pressure is 200MPa, and the time is 5 min; sintering at 1200 deg.C for 100 min; the vacuum degree of vacuum sintering is 3 multiplied by 10-1Pa。
Comparative example 1
Changing the raw material composition of the alumina ceramic composite material on the basis of the embodiment 1, and obtaining the alumina ceramic composite material under the unchanged other conditions; the alumina ceramic composite material is prepared from the following raw materials in percentage by mass: 97.9% of alumina, 1.1% of graphene, 0.5% of sintering aid and 0.5% of binder.
Comparative example 2
Changing the raw material composition of the alumina ceramic composite material on the basis of the embodiment 1, and obtaining the alumina ceramic composite material under the unchanged other conditions; the alumina ceramic composite material is prepared from the following raw materials in percentage by mass: 97.9 percent of alumina, 1.1 percent of zirconia, 0.5 percent of sintering aid and 0.5 percent of binder.
The alumina ceramic composite materials prepared in examples 1 to 6 and comparative examples 1 to 2 were subjected to performance tests, and the results are shown in table 1.
TABLE 1 Performance data for alumina ceramic composites prepared in examples 1-6 and comparative examples 1-2
As can be seen from example 1 and comparative examples 1 and 2 of table 1, graphene and zirconia in the present invention can synergistically improve toughness of the alumina ceramic composite material.
As can also be seen from table 1, the toughness of the alumina ceramic composite gradually increases as the contents of graphene and zirconia increase.
As can be seen from the above examples and comparative examples, the alumina ceramic composite material provided by the present invention has high toughness.
The foregoing is only a preferred embodiment of the present invention, and it should be noted that, for those skilled in the art, various modifications and decorations can be made without departing from the principle of the present invention, and these modifications and decorations should also be regarded as the protection scope of the present invention.
Claims (10)
1. An alumina ceramic composite material is prepared from the following raw materials in percentage by mass: 72-97.9% of aluminum oxide, 0.1-5% of graphene, 1-10% of zirconium oxide, 0.5-3% of sintering aid and 0.5-10% of binder.
2. The alumina ceramic composite material according to claim 1, which is prepared from the following raw materials in percentage by mass: 75-95% of aluminum oxide, 0.5-4% of graphene, 3.5-8% of zirconium oxide, 0.5-3% of sintering aid and 0.5-10% of binder.
3. The alumina ceramic composite material according to claim 2, which is prepared from the following raw materials in percentage by mass: 80-90% of aluminum oxide, 1-2% of graphene, 4.5-6% of zirconium oxide, 1-2% of sintering aid and 3.5-10% of binder.
4. The alumina ceramic composite according to any one of claims 1 to 3, wherein the particle size of the alumina is 100nm to 3 μm.
5. The alumina ceramic composite material according to any one of claims 1 to 3, wherein the sintering aid comprises at least one of calcium oxide, magnesium oxide, silica, lanthanum oxide, and titanium dioxide.
6. The alumina ceramic composite of any one of claims 1 to 3, wherein the binder comprises PVA and/or PVB.
7. A method for preparing the alumina ceramic composite material of any one of claims 1 to 6, comprising the steps of:
(1) mixing alumina, graphene, zirconia, a sintering aid and a binder, and then carrying out ball milling to obtain a mixed material;
(2) and (2) sequentially pressing and sintering the mixed material obtained in the step (1) to obtain the alumina ceramic composite material.
8. The preparation method of claim 7, wherein the rotation speed of the ball milling in the step (1) is 400-500 r/min, and the ball milling time is 1-1.5 h.
9. The preparation method according to claim 7, wherein the sintering temperature in the step (2) is 1200-1500 ℃, and the sintering time is 30-120 min.
10. Use of the alumina ceramic composite material according to any one of claims 1 to 6 or the alumina ceramic composite material prepared by the preparation method according to any one of claims 7 to 9 in a ceramic filter plate.
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