CN113004050A - Double-toughened shell-structure-imitated composite ceramic material and preparation method thereof - Google Patents
Double-toughened shell-structure-imitated composite ceramic material and preparation method thereof Download PDFInfo
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Abstract
The invention belongs to the technical field of composite structure ceramic materials, and particularly relates to a double-toughened shell-structure-imitated composite ceramic material and a preparation method thereof. The preparation method comprises the following steps: the first process step: placing the flaky alumina, the nano-particle zirconia, the sodium dodecyl sulfate and the polyvinylpyrrolidone into a ball milling tank, and adding deionized water for ball milling; and a second step: pouring the ball-milled slurry into a mold, pouring liquid nitrogen into the mold to freeze the slurry, and placing the frozen blank into a freeze dryer to obtain a green blank; and a third step of: and (4) carrying out heat treatment on the prepared green body at high temperature, and carrying out hot-pressing sintering after glue discharging is finished. The invention utilizes the freeze drying process to directionally form the mixed slurry of the alumina and the zirconia to obtain a green body with a brick mud structure, and then obtains the shell-like ceramic composite material consisting of pure inorganic phases after hot-pressing sintering.
Description
Technical Field
The invention belongs to the technical field of composite structure ceramic materials, and particularly relates to a double-toughened shell-structure-imitated composite ceramic material and a preparation method thereof.
Background
The information in this background section is only for enhancement of understanding of the general background of the invention and is not necessarily to be construed as an admission or any form of suggestion that this information forms the prior art that is already known to a person of ordinary skill in the art.
The shell pearl layer is a natural layered composite material, and the systematic research on the pearl shell finds that the structure of the pearl shell can be generally divided into three parts, wherein the outermost layer is a cuticle, the next is a prismatic layer, and the innermost layer is a pearl layer. The stratum corneum, which is very thin and mainly composed of proteins, serves primarily to protect the prismatic layer from attack by certain ions in the aqueous environment. The prismatic layer is composed of superfine columnar calcite crystals and organic matters, wherein the columnar calcite crystals are perpendicular to the shell surface of the shell, the small prisms are parallel to each other, and organic substrates are embedded between the columns. The nacre is formed by alternately stacking aragonite calcium carbonate small plates and interlayer organic matrix layers. From the microstructure of the shell, a plurality of fine nano-micro-convexes also exist at the interface, and the existence of the micro-convexes increases the interface bonding area between adjacent sheets, thereby influencing the performance of the shell.
Inspired by the unique structural characteristics and excellent mechanical properties of shells, various methods are proposed to prepare the shell-like structure layered material. Ekiz et alAl is prepared by hot-pressing auxiliary tape-casting technique2O3And injecting the mixed slurry with epoxy resin into a porous mould, and then preparing the shell-like composite material by hot-pressing sintering. However, the work of rupture of the final composite material is only 254J/m2Far less than the breaking performance of a shell (1240J/m)2) (ii) a Wang et al use SiC whiskers to incorporate Si3N4In a matrix, or Al2O3And Si3N4Adding into BN interlayer, and preparing into laminated composite material by extrusion rolling and hot pressing sintering, with fracture toughness (KIC) up to 28 MPa.m1/2The breaking work can reach 4000J/m2But the increase in toughness of the material comes at the expense of a decrease in strength.
In order to increase the strength and toughness of the composite material at the same time, the prior art proposes a method for preparing a ceramic-metal, ceramic-resin shell-like structure layered composite material by combining an ice template with an infiltration technology, but the inventor finds that the strength is still difficult to meet the requirement although the strength and toughness can be enhanced, and the adopted preparation method is complex, has high operation difficulty and is not beneficial to wide application.
Disclosure of Invention
In order to solve the defects of the prior art, the invention provides a double-toughened shell-like structure composite ceramic material and a preparation method thereof.
In order to achieve the above object, the first aspect of the present invention provides a method for preparing a double-toughened shell-like composite ceramic material, which comprises the following specific steps:
the first process step: placing the flaky alumina, the nano-particle zirconia, the sodium dodecyl sulfate and the polyvinylpyrrolidone into a ball milling tank, and adding deionized water for ball milling;
and a second step: pouring the ball-milled slurry into a mold, pouring liquid nitrogen into the mold to freeze the slurry, and placing the frozen blank into a freeze dryer to obtain a green blank;
and a third step of: and (4) carrying out heat treatment on the prepared green body at high temperature, and carrying out hot-pressing sintering after glue discharging is finished.
The invention provides a double-toughened shell-like structure composite ceramic material prepared by the method, and the ceramic material is an alumina-zirconia composite material and is prepared from flaky alumina (alpha-Al)2O3) Nano alumina particles and nano zirconia (3Y-ZrO)2) And (4) particle composition.
One or more embodiments of the present invention have at least the following advantageous effects:
(1) the shell-like layered brick mud structure is obtained through a freeze drying process, and meanwhile, the nano zirconia is introduced as an inorganic mineral toughening phase, so that the shell-like structure toughening and the zirconia phase change toughening are fully utilized to perform double toughening on the alumina ceramic, the mechanical property of the alumina ceramic is obviously improved, and the alumina ceramic has good bending strength and fracture toughness. Moreover, the introduction of zirconia has better high temperature resistance and corrosion resistance than polymers or metals as the second phase.
(2) The method has the advantages of simple process, environment-friendly preparation process, cheap raw materials and wide application.
Drawings
The accompanying drawings, which are incorporated in and constitute a part of this specification, are included to provide a further understanding of the invention, and are incorporated in and constitute a part of this specification, illustrate exemplary embodiments of the invention and together with the description serve to explain the invention and not to limit the invention.
Fig. 1 is an SEM image of a dual toughened seashell-like structure composite ceramic material in example 1 of the present invention.
Fig. 2 is a BSE diagram of a dual toughened seashell-like structure composite ceramic material in example 1 of the present invention.
FIG. 3 is a graph showing the flexural strength of a dual toughened seashell-like structure composite ceramic material according to comparative example 1 of the present invention.
FIG. 4 is a graph showing fracture toughness of a dual toughened seashell-like structure composite ceramic material according to comparative example 1 of the present invention.
Detailed Description
It is to be understood that the following detailed description is exemplary and is intended to provide further explanation of the invention as claimed. Unless defined otherwise, all technical and scientific terms used herein have the same meaning as commonly understood by one of ordinary skill in the art to which this invention belongs.
It is noted that the terminology used herein is for the purpose of describing particular embodiments only and is not intended to be limiting of exemplary embodiments according to the invention. As used herein, the singular forms "a", "an" and "the" are intended to include the plural forms as well, and it should be understood that when the terms "comprises" and/or "comprising" are used in this specification, they specify the presence of stated features, steps, operations, devices, components, and/or combinations thereof, unless the context clearly indicates otherwise.
As introduced in the background art, the strength of the prepared ceramic material is still difficult to meet the requirements of the existing preparation process of the shell-like structure laminated composite ceramic, and the adopted preparation method is complex, has high operation difficulty and is not beneficial to wide application.
In order to solve the technical problems, the first aspect of the invention provides a preparation method of a double-toughened shell-like structure composite ceramic material, which comprises the following specific steps:
the first process step: placing the flaky alumina, the nano-particle zirconia, the sodium dodecyl sulfate and the polyvinylpyrrolidone into a ball milling tank, and adding deionized water for ball milling;
and a second step: pouring the ball-milled slurry into a mold, pouring liquid nitrogen into the mold to freeze the slurry, and placing the frozen blank into a freeze dryer to obtain a green blank;
and a third step of: and (4) carrying out heat treatment on the prepared green body at high temperature, and carrying out hot-pressing sintering after glue discharging is finished.
The invention takes the flaky alumina, the nano-particle alumina and the nano-particle zirconia as basic raw materials, the structure of the flaky alumina is used as the basis for constructing the shell bionic structure, the layered main structure of the flaky alumina grains stacked is obtained by the characteristic that the flaky alumina grows in a different direction in the sintering process, the brick structure of the shell-like structure is formed, and a small amount of nano-alumina particles and zirconia particles are filled between layers to form the mud structure of the shell-like structure.
In the freeze drying process, the structure of the sheet alumina can be maintained, the sheet alumina is stacked to form a layered block ceramic material, and meanwhile, alumina particles and zirconia particles can be ensured to be uniformly attached to the surface of an alumina sheet structure; the hot-pressing sintering process is to form a compact ceramic block material and simultaneously realize the tight load of the alumina particles and the zirconia particles on the alumina layer-shaped structure.
According to the method, a double toughening mechanism is constructed, firstly, a shell-like layered brick mud structure is obtained through a freeze drying process, and the shell-like structure is utilized for toughening; secondly, by introducing nano zirconia as an inorganic mineral toughening phase and utilizing zirconia phase change toughening, the mechanical property of the material is obviously improved under a dual toughening mechanism, and the material has good bending strength and fracture toughness.
In one or more embodiments of the invention, in the first step, the mass ratio of the flaky alumina to the nano alumina particles to the nano zirconia particles is 12:2:1, and the formed shell-like layered brick mud has a firmer structure and better toughness.
Sodium dodecyl sulfate and polyvinylpyrrolidone play a role of a binder and a dispersant in the method, but the excessive amount of the binder and the dispersant can reduce the ratio of the alumina and the zirconia active materials, influence the toughness of the final material, and easily generate excessive bubbles in the ball milling process to influence the arrangement state of the flaky alumina and the strength of a green body; if the amount of the binder is too low, good binding and nanoparticle dispersion effects cannot be achieved; in the present invention, the addition amount of sodium lauryl sulfate and polyvinylpyrrolidone is set to 1 wt%, and the effect is most excellent at the addition amount.
Furthermore, the average molecular weight of the polyvinylpyrrolidone is 10000g/mol-30000 g/mol.
In the first procedure, the ball milling process is mainly to ensure that the flaky alumina, the nano-particle zirconia, the sodium dodecyl sulfate and the polyvinylpyrrolidone are fully contacted, and finally a uniform shell-like brick mud structure is formed, and the preferred ball milling time is 3-6 hours.
In one or more embodiments of the invention, during the heat treatment in the third step, the temperature is raised to 600-1300 ℃ at a speed of 5-10 ℃/min, and the temperature is maintained for 2-3 hours; preferably, the temperature is raised to 1100 ℃ at the speed of 10 ℃/min, and the temperature is kept for 3 hours;
in one or more embodiments of the invention, during hot-pressing sintering, argon atmosphere is added, after the temperature is raised to 1100 ℃ at the speed of 5-20 ℃/min, and then raised to 1400-1600 ℃ at the speed of 5-10 ℃/min, manual pressurization is carried out to 30MPa, and the temperature is kept for 1-3 hours;
further, after the temperature is raised to 1500 ℃ at the speed of 10 ℃/min, the pressure is manually increased to 30MPa, and the temperature is kept for 1 hour.
The invention provides a double-toughened shell-like structure composite ceramic material prepared by the method, and the ceramic material is an alumina-zirconia composite material and is prepared from flaky alumina (alpha-Al)2O3) Nano alumina particles and nano zirconia (3Y-ZrO)2) Particle composition;
furthermore, the particle size of the flake alumina is 5-11 μm, the particle size of the nano alumina is 60-90nm, and the particle size of the nano zirconia is 50-80 nm.
The composite ceramic material is a shell-like layered brick mud structure, the layered structure is formed by stacking sheet-shaped alumina to form a framework of the whole ceramic material, and alumina nanoparticles and zirconia nanoparticles are filled in the layered structure.
In order to make the technical solution of the present invention more clearly understood by those skilled in the art, the technical solution of the present invention will be described in detail below with reference to specific examples and comparative examples.
Example 1
(1) Mixing materials: 33.6g of flake alumina, 5.6g of nano alumina, 2.8g of nano zirconia, 0.42g of polyvinylpyrrolidone (molecular weight: 10000g/mol) and 0.42g of sodium lauryl sulfate were put in 58g of distilled water and mixed in a ball mill pot at 400r/min for 3 hours.
(2) And (3) freeze drying: pouring the uniformly mixed slurry into a polytetrafluoroethylene mold with a heat-conducting stainless steel base, pouring liquid nitrogen into an insulation box to finish precooling so as to prevent the liquid nitrogen from settling, and freeze-drying the liquid nitrogen in a freeze dryer according to a preset program to obtain a green body.
(3) Heat treatment and sintering: taking out the green body, placing the green body in a crucible, placing the crucible in a high-temperature box type furnace, heating to 1100 ℃ at the speed of 10 ℃/min, and preserving heat for 3 hours to finish rubber discharge. And (3) putting the blank after the heat treatment into a graphite mold for hot-pressing sintering, introducing argon atmosphere, heating to 1100 ℃ at a speed of 20 ℃/min, heating to 1500 ℃ at a speed of 10 ℃/min, preserving heat for one hour, and pressurizing to 30MPa, thereby completing the sintering process to obtain the zirconium oxide-aluminum oxide double-toughened composite ceramic material with the shell-like structure.
The SEM image and the BSE image of the double-toughened shell-like structure composite ceramic material are respectively shown in figures 1 and 2, and it can be seen that the composite ceramic material takes a layered structure formed by stacking flaky alumina grains as a main structure to form a shell-like structure brick structure, and a small amount of nano alumina particles and zirconia particles are filled between layers to form a shell-like structure mud structure. The double-toughened shell-like structure composite ceramic material has excellent comprehensive mechanical property, bending strength of 583MPa and fracture toughness of 9.1 MPa.m1/2。
Example 2
(1) Mixing materials: 33.6g of plate-shaped alumina, 5.6g of nano-alumina, 2.8g of nano-zirconia, 0.42g of polyvinylpyrrolidone (molecular weight of 30000g/mol), 0.42g of sodium lauryl sulfate in 58g of distilled water were put into a ball mill pot and mixed at 400r/min for 3 hours.
(2) And (3) freeze drying: pouring the uniformly mixed slurry into a polytetrafluoroethylene mold with a heat-conducting stainless steel base, pouring liquid nitrogen into an insulation box to finish precooling so as to prevent the liquid nitrogen from settling, and freeze-drying the liquid nitrogen in a freeze dryer according to a preset program to obtain a green body.
(3) Heat treatment and sintering: taking out the green body, placing the green body in a crucible, placing the crucible in a high-temperature box type furnace, heating to 1100 ℃ at the speed of 10 ℃/min, and preserving heat for 3 hours to finish rubber discharge. And (3) putting the blank after the heat treatment into a graphite mold for hot-pressing sintering, introducing argon atmosphere, heating to 1100 ℃ at a speed of 20 ℃/min, heating to 1600 ℃ at a speed of 10 ℃/min, preserving heat for one hour, and pressurizing to 30MPa to finish the sintering process, thus obtaining the zirconium oxide-aluminum oxide double-toughened composite ceramic material with the shell-like structure.
Example 3
(1) Mixing materials: 33.6g of flake alumina, 5.6g of nano alumina, 2.8g of nano zirconia, 0.42g of polyvinylpyrrolidone (molecular weight: 10000g/mol) and 0.42g of sodium lauryl sulfate were put in 58g of distilled water and mixed in a ball mill pot at 400r/min for 3 hours.
(2) And (3) freeze drying: pouring the uniformly mixed slurry into a polytetrafluoroethylene mold with a heat-conducting stainless steel base, pouring liquid nitrogen into an insulation box to finish precooling so as to prevent the liquid nitrogen from settling, and freeze-drying the liquid nitrogen in a freeze dryer according to a preset program to obtain a green body.
(3) Heat treatment and sintering: taking out the green body, placing the green body in a crucible, placing the crucible in a high-temperature box type furnace, heating to 1100 ℃ at the speed of 10 ℃/min, and preserving heat for 3 hours to finish rubber discharge. And (3) putting the blank after the heat treatment into a graphite mold for hot-pressing sintering, introducing argon atmosphere, heating to 1100 ℃ at a speed of 20 ℃/min, heating to 1400 ℃ at a speed of 5 ℃/min, preserving heat for one hour, and pressurizing to 30MPa, thereby completing the sintering process to obtain the zirconium oxide-aluminum oxide double-toughened composite ceramic material with the shell-like structure.
Comparative example 1
(1) Mixing materials: 33.6g of flake alumina, 2.8g of nano alumina, 5.6g of nano zirconia, 0.42g of polyvinylpyrrolidone (molecular weight: 10000g/mol) and 0.42g of sodium dodecyl sulfate were put in 58g of distilled water and mixed in a ball mill pot at 300r/min for 3 hours.
(2) And (3) freeze drying: pouring the uniformly mixed slurry into a tetrafluoroethylene mold with a heat-conducting stainless steel base, pouring liquid nitrogen into an insulation box to finish precooling so as to prevent the liquid nitrogen from settling, and freeze-drying the liquid nitrogen in a freeze dryer according to a preset program to obtain a green body.
(3) Heat treatment and sintering: taking out the green body, placing the green body in a crucible, placing the crucible in a high-temperature box type furnace, heating to 1300 ℃ at the speed of 5 ℃/min, and preserving heat for 3 hours to finish rubber discharge. And (3) putting the blank after the heat treatment into a graphite mold for hot-pressing sintering, introducing argon atmosphere, heating to 1100 ℃ at a speed of 20 ℃/min, heating to 1500 ℃ at a speed of 10 ℃/min, preserving heat for one hour, and pressurizing to 30MPa, thereby completing the sintering process to obtain the zirconium oxide-aluminum oxide double-toughened composite ceramic material with the shell-like structure.
The mass ratio of the flaky alumina to the nano alumina particles to the nano zirconia particles in the double-toughened shell-structure-imitated composite ceramic material is 12:1:2, the mass ratio of the nano zirconia particles is about 7%, and the composite ceramic material has poor comprehensive mechanical properties. As can be seen from the bending strength graph (fig. 3), the composite ceramic material of comparative example 1 has a slightly higher bending strength; however, as can be seen from FIG. 4, the fracture toughness of the composite ceramic material is only 6.2MPa · m1/2The decrease is about 30%.
Comparative example 2
(1) Mixing materials: 33.6g of plate-shaped alumina, 5.6g of nano-alumina, 2.8g of nano-zirconia, 0.84g of polyvinylpyrrolidone (molecular weight: 10000g/mol) and 0.84g of sodium dodecyl sulfate were put in 58g of distilled water and mixed in a ball mill pot at 400r/min for 3 hours.
(2) And (3) freeze drying: pouring the uniformly mixed slurry into a polytetrafluoroethylene mold with a heat-conducting stainless steel base, pouring liquid nitrogen into an insulation box to finish precooling so as to prevent the liquid nitrogen from settling, and freeze-drying the liquid nitrogen in a freeze dryer according to a preset program to obtain a green body.
(3) Heat treatment and sintering: taking out the green body, placing the green body in a crucible, placing the crucible in a high-temperature box type furnace, heating to 1100 ℃ at the speed of 10 ℃/min, and preserving heat for 3 hours to finish rubber discharge. Putting the blank after the heat treatment into a graphite mold for hot-pressing sintering, introducing argon atmosphere, heating to 1100 ℃ at 20 ℃/min, heating to 1500 ℃ at 10 ℃/min, preserving heat for one hour, pressurizing to 30MPa, and finishing the sintering process to obtain the zirconium oxide-oxidized material with the shell-like structureAn aluminum double-toughened composite ceramic material. Wherein, the polyvinylpyrrolidone and the sodium dodecyl sulfate are used as a dispersant and a binder, after the addition amount is increased, a large amount of bubbles are generated in the mixing stage, the viscosity and the fluidity of the slurry are influenced, the oriented arrangement effect of the flaky alumina is poor finally, the green strength after freeze drying is reduced, the fracture toughness of the sintered composite ceramic material is poor, and the fracture toughness is 4-5 MPa.m1/2In the meantime.
The above description is only a preferred embodiment of the present invention and is not intended to limit the present invention, and various modifications and changes may be made by those skilled in the art. Any modification, equivalent replacement, or improvement made within the spirit and principle of the present invention should be included in the protection scope of the present invention.
Claims (10)
1. A preparation method of a double-toughened shell-like structure composite ceramic material is characterized by comprising the following specific steps:
the first process step: placing the flaky alumina, the nano-particle zirconia, the sodium dodecyl sulfate and the polyvinylpyrrolidone into a ball milling tank, and adding deionized water for ball milling;
and a second step: pouring the ball-milled slurry into a mold, pouring liquid nitrogen into the mold to freeze the slurry, and placing the frozen blank into a freeze dryer to obtain a green blank;
and a third step of: and (4) carrying out heat treatment on the prepared green body at high temperature, and carrying out hot-pressing sintering after glue discharging is finished.
2. The method of claim 1, wherein: the mass ratio of the flaky alumina to the nano alumina particles to the nano zirconia particles is 12:2: 1.
3. The method of claim 1, wherein: sodium lauryl sulfate and polyvinylpyrrolidone were added in an amount of 1 wt%.
4. The method of claim 1, wherein: the average molecular weight of the polyvinylpyrrolidone is 10000g/mol-30000 g/mol.
5. The method of claim 1, wherein: in the first procedure, the ball milling time is 3-6 hours.
6. The method of claim 1, wherein: during heat treatment, the temperature is raised to 600-1300 ℃ at the speed of 5-10 ℃/min, and the temperature is kept for 2-3 hours;
preferably, the temperature is raised to 1100 ℃ at a speed of 10 ℃/min, and the temperature is maintained for 3 hours.
7. The method of claim 1, wherein: in the third step, during hot-pressing sintering, argon is added, the temperature is raised to 1100 ℃ at the speed of 5-20 ℃/min, then the temperature is raised to 1400-1600 ℃ at the speed of 5-10 ℃/min, then manual pressurization is carried out to 30MPa, and the temperature is kept for 1-3 hours.
8. The method of claim 7, wherein: heating to 1500 deg.C at 10 deg.C/min, manually pressurizing to 30MPa, and holding for 1 hr.
9. The double-toughened shell-like structure composite ceramic material obtained by the preparation method of any one of claims 1 to 8, which consists of flaky alumina, nano alumina particles and nano zirconia particles.
10. The double toughened seashell-like structural composite ceramic material of claim 9, wherein: the particle size of the flake alumina is 5-11 μm, the particle size of the nano alumina is 60-90nm, and the particle size of the nano zirconia is 50-80 nm.
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