CN110627499B - Preparation method of high-toughness ceramic composite - Google Patents
Preparation method of high-toughness ceramic composite Download PDFInfo
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Abstract
The invention relates to the technical field of ceramic processes, in particular to a preparation method of a high-toughness ceramic composite body. The characteristics of small hardness and high toughness of the Y1 layer and the Y2 layer and large hardness and low toughness of the X layer are fully utilized, the Y1 layer and the Y2 layer are respectively arranged at the upper end and the lower end of the X layer, and the surface layer of the ceramic composite body formed by processing has stronger toughness performance, so that the ceramic composite body has stronger capacity of absorbing deformation force when the ceramic composite body is deformed, the phenomenon of brittle fracture is reduced, and meanwhile, the middle layer has certain impact resistance capacity and provides certain structural strength for the ceramic composite body.
Description
Technical Field
The invention relates to the technical field of ceramic processes, in particular to a preparation method of a high-toughness ceramic composite.
Background
The stable zirconia ceramics has the characteristics of high strength, high hardness, wear resistance, corrosion resistance, self lubrication, high temperature resistance, high temperature conductivity, thermal expansion coefficient close to that of metals, large phase change volume effect of the stable zirconia ceramics and the like, and is widely applied to various fields such as cutters, molds, valves, advanced refractory materials, oxygen sensors, solid fuel cells, high temperature electrodes, high temperature thermosensitive ceramics, inorganic pigments, high temperature ceramic glaze and the like. In addition to the above properties, the stabilized zirconia ceramics are also popular as housing materials for exterior applications because of their high quality and their mild color.
At present, the stable zirconia ceramic products on the market are mostly made of a single material, namely, the stable zirconia ceramic products are of a single-layer structure, and the stable zirconia ceramic products made of the stable zirconia materials with different mole ratios have different performances.
Disclosure of Invention
The invention aims to provide a preparation method of a high-toughness ceramic composite with strong toughness.
In order to solve the technical problems, the invention adopts the following technical scheme: the preparation method of the high-toughness ceramic composite comprises the following process steps:
the method comprises the following steps: preparing an X layer with the thickness of 0.2 to 0.6mm by molding and processing the stabilized zirconia with the mole ratio of 2.5 to 4 percent;
step two: preparing a Y1 layer with the thickness of 0.2 to 0.6mm by molding and processing the stabilized zirconia with the mole ratio of 1 to 2.5 percent;
step three: preparing a Y2 layer with the thickness of 0.2 to 0.6mm by molding and processing the stabilized zirconia with the mole ratio of 1 to 2.5 percent;
step four: sequentially laminating the Y1 layer, the X layer and the Y2 layer from top to bottom to form a green body;
step five: packaging the green body after the step four;
step six: transferring the green body subjected to the fifth step into isostatic pressing equipment for isostatic pressing;
step seven: transferring the green body subjected to the step six into glue discharging equipment for glue discharging treatment;
step eight: transferring the green body obtained in the step seven into sintering equipment for sintering treatment to obtain a ceramic composite; the change of the processing temperature of the sintering equipment is as follows:
a: the temperature in the sintering equipment is raised to T1, the required time is 15 to 60 minutes, and the temperature of T1 is 10 to 50 ℃;
b: the temperature in the sintering equipment is raised to T1+70 ℃ to T1+120 ℃, and the required time is 90-140 minutes;
c: the temperature in the sintering equipment is raised to T1+550 ℃ to T1+600 ℃, and the required time is 300-400 minutes;
d: the temperature in the sintering equipment is raised to T1+1000 ℃ to T1+1050 ℃, and the required time is 240-350 minutes;
e: the temperature in the sintering equipment is increased from T1+1370 ℃ to T1+1440 ℃ for 120-200 minutes;
f: the temperature within the sintering apparatus was maintained to T1+1370 to T1+1440 degrees celsius for 180 to 260 minutes.
Preferably, the step eight: transferring the green body obtained in the step seven into sintering equipment for sintering treatment to obtain a ceramic composite; the change of the processing temperature of the sintering equipment is as follows:
a: the temperature in the sintering equipment is raised to T1, the required time is 20 to 50 minutes, and the temperature of T1 is 15 to 40 ℃;
b: the temperature in the sintering equipment is raised to T1+70 ℃ to T1+100 ℃, and the required time is 100-140 minutes;
c: the temperature in the sintering equipment is increased to T1+550 ℃ to T1+580 ℃, and the required time is 320-400 minutes;
d: the temperature in the sintering equipment is raised to T1+1000 ℃ to T1+1040 ℃, and the required time is 260-340 minutes;
e: the temperature in the sintering equipment is increased from T1+1370 ℃ to T1+1420 ℃, and the required time is 150-200 minutes;
f: the temperature within the sintering apparatus is maintained to T1+1370 degrees celsius to T1+1420 degrees celsius for a duration of 200 to 260 minutes.
Preferably, the step eight: transferring the green body obtained in the step seven into sintering equipment for sintering treatment to obtain a ceramic composite; the change of the processing temperature of the sintering equipment is as follows:
a: the temperature in the sintering equipment is raised to T1, the required time is 20 to 40 minutes, and the temperature of T1 is 25 to 40 ℃;
b: the temperature in the sintering equipment is raised to T1+80 ℃ to T1+95 ℃, and the required time is 100-130 minutes;
c: the temperature in the sintering equipment is increased to T1+550 ℃ to T1+580 ℃, and the required time is 340-370 minutes;
d: the temperature in the sintering equipment is increased to T1+1000 ℃ to T1+1030 ℃, and the required time is 260-310 minutes;
e: the temperature in the sintering equipment is increased from T1+1370 ℃ to T1+1400 ℃, and the required time is 160-200 minutes;
f: the temperature within the sintering apparatus was maintained to T1+1370 degrees celsius to T1+1400 degrees celsius for a duration of 220 to 260 minutes.
Preferably, the forming process in the step one is any one of dry pressing, casting, gelling, injection molding, film rolling, dry bag type isostatic pressing, spraying and screen printing; the molding processing in the second step is any one of dry pressing, tape casting, gelling, injection molding, film rolling, dry bag type isostatic pressing, spraying and screen printing; and the forming in the third step is any one of dry pressing, tape casting, gelling, injection molding, film rolling, dry bag type isostatic pressing, spraying and screen printing.
Preferably, the encapsulation treatment in the fifth step is to place the green body after the fourth step into an encapsulation bag for vacuum encapsulation.
Preferably, the processing parameters of the isostatic pressing treatment in the step six are as follows: the pressure is 130 to 170 MPa, the pressure maintaining time is 10 to 30 minutes, and the water temperature is 48 to 70 ℃.
Preferably, the isostatic pressing in the sixth step is cold isostatic pressing or warm isostatic pressing.
Preferably, the thickness of the ceramic composite body to which the step eight is performed is 0.4 to 1.5 mm.
Preferably, the method further comprises the step nine: and (5) performing cutting treatment, grinding treatment, polishing treatment and film coating treatment on the ceramic composite body subjected to the step eight.
Preferably, at least one transition layer is arranged between the Y1 layer and the X layer and between the Y2 layer and the X layer.
Preferably, the mole ratio of the Y1 layer is less than that of the transition layer, and the mole ratio of the transition layer between the Y1 layer and the X layer is less than that of the X layer; the mole ratio of the Y2 layer is less than that of the transition layer, and the mole ratio of the transition layer between the Y1 layer and the X layer is less than that of the X layer.
The invention has the beneficial effects that: the invention provides a preparation method of a high-toughness ceramic composite, which fully utilizes the characteristics of small hardness and high toughness of a Y1 layer and a Y2 layer and large hardness and low toughness of an X layer, and arranges a Y1 layer and a Y2 layer at the upper end and the lower end of the X layer respectively, so that the surface layer of the ceramic composite formed by processing has stronger toughness, thereby having stronger capacity of absorbing deformation force when the ceramic composite is deformed, reducing the occurrence of brittle fracture, and simultaneously the middle layer has certain impact resistance capacity and providing certain structural strength for the ceramic composite.
Drawings
FIG. 1 is a schematic structural view of a high toughness ceramic composite of the present invention.
FIG. 2 is a graph showing the variation of the processing temperature of the sintering equipment in the high toughness ceramic composite of the present invention.
Detailed Description
The present invention will be further described with reference to the following examples, which are not intended to limit the scope of the present invention.
As shown in fig. 1 to 2, the preparation method of the ceramic composite with high toughness comprises the following process steps:
the method comprises the following steps: preparing an X layer with the thickness of 0.2 to 0.6mm by molding and processing the stabilized zirconia with the mole ratio of 2.5 to 4 percent;
step two: preparing a Y1 layer with the thickness of 0.2 to 0.6mm by molding and processing the stabilized zirconia with the mole ratio of 1 to 2.5 percent;
step three: preparing a Y2 layer with the thickness of 0.2 to 0.6mm by molding and processing the stabilized zirconia with the mole ratio of 1 to 2.5 percent;
step four: sequentially laminating the Y1 layer, the X layer and the Y2 layer from top to bottom to form a green body;
step five: packaging the green body after the step four;
step six: transferring the green body subjected to the fifth step into isostatic pressing equipment for isostatic pressing;
step seven: transferring the green body subjected to the step six into glue discharging equipment for glue discharging treatment;
step eight: transferring the green body obtained in the step seven into sintering equipment for sintering treatment to obtain a ceramic composite; the change of the processing temperature of the sintering equipment is as follows:
a: the temperature in the sintering equipment is raised to T1, the required time is 15 to 60 minutes, and the temperature of T1 is 10 to 50 ℃;
b: the temperature in the sintering equipment is raised to T1+70 ℃ to T1+120 ℃, and the required time is 90-140 minutes;
c: the temperature in the sintering equipment is raised to T1+550 ℃ to T1+600 ℃, and the required time is 300-400 minutes;
d: the temperature in the sintering equipment is raised to T1+1000 ℃ to T1+1050 ℃, and the required time is 240-350 minutes;
e: the temperature in the sintering equipment is increased from T1+1370 ℃ to T1+1440 ℃ for 120-200 minutes;
f: the temperature within the sintering apparatus was maintained to T1+1370 to T1+1440 degrees celsius for 180 to 260 minutes.
Preferably, the step eight: transferring the green body obtained in the step seven into sintering equipment for sintering treatment to obtain a ceramic composite; the change of the processing temperature of the sintering equipment is as follows:
a: the temperature in the sintering equipment is raised to T1, the required time is 20 to 50 minutes, and the temperature of T1 is 15 to 40 ℃;
b: the temperature in the sintering equipment is raised to T1+70 ℃ to T1+100 ℃, and the required time is 100-140 minutes;
c: the temperature in the sintering equipment is increased to T1+550 ℃ to T1+580 ℃, and the required time is 320-400 minutes;
d: the temperature in the sintering equipment is raised to T1+1000 ℃ to T1+1040 ℃, and the required time is 260-340 minutes;
e: the temperature in the sintering equipment is increased from T1+1370 ℃ to T1+1420 ℃, and the required time is 150-200 minutes;
f: the temperature within the sintering equipment was maintained to T1+1370 degrees celsius to T1+1420 degrees celsius for a duration of 200 to 260 minutes.
Preferably, the Y1 layer and the Y2 layer can be prepared by molding process (any one of dry pressing, casting, gel molding, injection molding, film rolling, dry bag type isostatic pressing, spraying and screen printing) separately in advance, or the Y1 layer and the Y2 layer can be directly processed on the X layer, namely the Y1 layer and the Y2 layer are prepared by molding process (any one of dry pressing, casting, gel molding, injection molding, film rolling, dry bag type isostatic pressing, spraying and screen printing) directly on the upper and lower end surfaces of the X layer.
In a general ceramic composite body manufactured by the present invention, the X layer accounts for 2% to 95% of the total thickness of the ceramic composite body, and when the ceramic composite body is applied to a mobile phone back plate, the X layer accounts for 60% to 80% of the total thickness of the ceramic composite body, although the ceramic composite body of the present invention may be applied to other products according to actual requirements.
Preferably, the glue discharging equipment is a glue discharging furnace, the sintering equipment is a sintering furnace, and in addition, the glue discharging treatment and the sintering treatment can be processed through a tunnel furnace integrating the glue discharging treatment and the sintering treatment.
Preferably, the stabilizing agent used in preparing the stabilized zirconia material can be any one or more of yttrium oxide, cerium oxide, calcium oxide and magnesium oxide; if yttria-stabilized zirconia is used to prepare the ceramic composite, the yttria-stabilized zirconia is black yttria-stabilized zirconia.
In this embodiment, the molding process in the first step is any one of dry pressing, tape casting, gelling, injection molding, film rolling, dry bag isostatic pressing, spraying, and screen printing; the molding processing in the second step is any one of dry pressing, tape casting, gelling, injection molding, film rolling, dry bag type isostatic pressing, spraying and screen printing; and the forming in the third step is any one of dry pressing, tape casting, gelling, injection molding, film rolling, dry bag type isostatic pressing, spraying and screen printing.
In this embodiment, the encapsulation treatment in the fifth step is to place the green body after the fourth step into an encapsulation bag for vacuum encapsulation.
In this embodiment, the processing parameters of the isostatic pressing in the sixth step are as follows: the pressure is 130 to 170 MPa, the pressure maintaining time is 10 to 30 minutes, and the water temperature is 48 to 70 ℃.
In this embodiment, the isostatic pressing in the sixth step is cold isostatic pressing or warm isostatic pressing.
In this example, the thickness of the ceramic composite body to which the step eight is performed is 0.4 to 1.5 mm.
In this embodiment, the method further includes the ninth step: and C, performing cutting treatment, grinding treatment, polishing treatment and film coating treatment on the ceramic composite body subjected to the step eight.
In this embodiment, at least one transition layer is disposed between the Y1 layer and the X layer and between the Y2 layer and the X layer.
In the embodiment, the mole ratio of the Y1 layer is less than that of the transition layer, and the mole ratio of the transition layer between the Y1 layer and the X layer is less than that of the X layer; the mole ratio of the Y2 layer is less than that of the transition layer, and the mole ratio of the transition layer between the Y1 layer and the X layer is less than that of the X layer.
The characteristics of small hardness and high toughness of the Y1 layer and the Y2 layer and large hardness and low toughness of the X layer are fully utilized, the Y1 layer and the Y2 layer are respectively arranged at the upper end and the lower end of the X layer, and the surface layer of the ceramic composite body formed by processing has stronger toughness performance, so that the ceramic composite body has stronger capacity of absorbing deformation force when the ceramic composite body is deformed, the phenomenon of brittle fracture is reduced, and meanwhile, the middle layer has certain impact resistance capacity and provides certain structural strength for the ceramic composite body.
The first embodiment is as follows: the preparation method of the high-toughness ceramic composite comprises the following process steps:
the method comprises the following steps: preparing an X layer with the thickness of 0.2mm by molding and processing the stabilized zirconia with the mole ratio of 2.5;
step two: forming the stabilized zirconia with the mole ratio of 1% to obtain a Y1 layer with the thickness of 0.2 mm;
step three: forming the stabilized zirconia with the mole ratio of 1% to obtain a Y2 layer with the thickness of 0.2 mm;
step four: sequentially laminating the Y1 layer, the X layer and the Y2 layer from top to bottom to form a green body;
step five: packaging the green body after the step four;
step six: and D, moving the green body which is subjected to the step five into isostatic pressing equipment for isostatic pressing treatment, wherein the processing parameters of the isostatic pressing treatment are as follows: the pressure is 130 MPa, the pressure maintaining time is 10 minutes, and the water temperature is 48 ℃;
step seven: transferring the green body subjected to the step six into glue discharging equipment for glue discharging treatment;
step eight: transferring the green body obtained in the step seven into sintering equipment for sintering treatment to obtain a ceramic composite body, wherein the thickness of the ceramic composite body is 0.4 mm; the change of the processing temperature of the sintering equipment is as follows:
a: the temperature in the sintering equipment is raised to 10 ℃, and the required time is 15 minutes;
b: the temperature in the sintering equipment is raised to 80 ℃, and the required time is 90 minutes;
c: the temperature in the sintering equipment is increased to 560 ℃, and the required time is 300 minutes;
d: the temperature in the sintering equipment is increased to 1010 ℃, and the required time is 240 minutes;
e: the temperature in the sintering equipment is raised to 1380 ℃ and the required time is 120 minutes;
f: the temperature in the sintering equipment was maintained to 1380 ℃ for 180 minutes.
Example two: the preparation method of the high-toughness ceramic composite comprises the following process steps:
the method comprises the following steps: preparing an X layer with the thickness of 0.3mm by molding and processing the stabilized zirconia with the mole ratio of 2.8%;
step two: preparing a Y1 layer with the thickness of 0.27mm by molding and processing the stabilized zirconia with the mole ratio of 1.5%;
step three: preparing a Y2 layer with the thickness of 0.33mm by molding and processing the stabilized zirconia with the mole ratio of 1.7%;
step four: sequentially laminating the Y1 layer, the X layer and the Y2 layer from top to bottom to form a green body;
step five: packaging the green body after the step four;
step six: and D, moving the green body which is subjected to the step five into isostatic pressing equipment for isostatic pressing treatment, wherein the processing parameters of the isostatic pressing treatment are as follows: the pressure is 138 MPa, the pressure maintaining time is 13 minutes, and the water temperature is 55 ℃;
step seven: transferring the green body subjected to the step six into glue discharging equipment for glue discharging treatment;
step eight: transferring the green body obtained in the step seven into sintering equipment for sintering treatment to obtain a ceramic composite body, wherein the thickness of the ceramic composite body is 0.7 mm; the change of the processing temperature of the sintering equipment is as follows:
a: the temperature in the sintering equipment is raised to 20 ℃, and the required time is 23 minutes;
b: the temperature in the sintering equipment is raised to 100 ℃, and the required time is 101 minutes;
c: the temperature in the sintering equipment is raised to 583 ℃, and the required time is 330 minutes;
d: the temperature in the sintering equipment is increased to 1040 ℃, and the required time is 270 minutes;
e: the temperature in the sintering equipment is increased to 1410 ℃, and the required time is 130 minutes;
f: the temperature in the sintering equipment was maintained to 1410 degrees celsius for 200 minutes.
Example three: the preparation method of the high-toughness ceramic composite comprises the following process steps:
the method comprises the following steps: preparing an X layer with the thickness of 0.4mm by molding and processing the stabilized zirconia with the mole ratio of 3%;
step two: preparing a Y1 layer with the thickness of 0.38mm by molding and processing the stabilized zirconia with the mole ratio of 1.9%;
step three: preparing a Y2 layer with the thickness of 0.45mm by molding and processing the stabilized zirconia with the mole ratio of 2.1 percent;
step four: sequentially laminating the Y1 layer, the X layer and the Y2 layer from top to bottom to form a green body;
step five: packaging the green body after the step four;
step six: and D, moving the green body which is subjected to the step five into isostatic pressing equipment for isostatic pressing treatment, wherein the processing parameters of the isostatic pressing treatment are as follows: the pressure is 143 MPa, the pressure maintaining time is 20 minutes, and the water temperature is 63 ℃;
step seven: transferring the green body subjected to the step six into glue discharging equipment for glue discharging treatment;
step eight: transferring the green body obtained in the step seven into sintering equipment for sintering treatment to obtain a ceramic composite body, wherein the thickness of the ceramic composite body is 1 mm; the change of the processing temperature of the sintering equipment is as follows:
a: the temperature in the sintering equipment is raised to 30 ℃, and the required time is 35 minutes;
b: the temperature in the sintering equipment is raised to 120 ℃, and the required time is 118 minutes;
c: the temperature in the sintering equipment is raised to 600 ℃, and the required time is 360 minutes;
d: the temperature in the sintering equipment is increased to 1060 ℃, and the required time is 310 minutes;
e: the temperature in the sintering equipment is increased to 1430 ℃ and the required time is 160 minutes;
f: the temperature in the sintering equipment was maintained to 1430 ℃ for 240 minutes.
Example four: the preparation method of the high-toughness ceramic composite comprises the following process steps:
the method comprises the following steps: preparing an X layer with the thickness of 0.5mm by molding and processing the stabilized zirconia with the mole ratio of 3.5;
step two: preparing a Y1 layer with the thickness of 0.51mm by molding and processing the stabilized zirconia with the mole ratio of 2.3 percent;
step three: preparing a Y2 layer with the thickness of 0.54mm by molding and processing the stabilized zirconia with the mole ratio of 2.2 percent;
step four: sequentially laminating the Y1 layer, the X layer and the Y2 layer from top to bottom to form a green body;
step five: packaging the green body after the step four;
step six: and D, moving the green body which is subjected to the step five into isostatic pressing equipment for isostatic pressing treatment, wherein the processing parameters of the isostatic pressing treatment are as follows: the pressure is 159 MPa, the pressure maintaining time is 24 minutes, and the water temperature is 67 ℃;
step seven: transferring the green body subjected to the step six into glue discharging equipment for glue discharging treatment;
step eight: transferring the green body obtained in the step seven into sintering equipment for sintering treatment to obtain a ceramic composite body, wherein the thickness of the ceramic composite body is 1.2 mm; the change of the processing temperature of the sintering equipment is as follows:
a: the temperature in the sintering equipment is raised to 40 ℃, and the required time is 50 minutes;
b: the temperature in the sintering equipment is raised to 140 ℃, and the required time is 129 minutes;
c: the temperature in the sintering equipment is raised to 631 ℃, and the required time is 380 minutes;
d: the temperature in the sintering equipment is raised to 1080 ℃, and the required time is 340 minutes;
e: the temperature in the sintering equipment is increased to 1460 ℃, and the required time is 180 minutes;
f: the temperature in the sintering equipment was maintained to 1460 degrees celsius for 250 minutes.
Example five: the preparation method of the high-toughness ceramic composite comprises the following process steps:
the method comprises the following steps: forming and processing the stable zirconia with the mole ratio of 4% to obtain an X layer with the thickness of 0.6 mm;
step two: preparing a Y1 layer with the thickness of 0.6mm by molding and processing the stabilized zirconia with the mole ratio of 2.5%;
step three: forming the stabilized zirconia with the mole ratio of 2.5% to obtain a Y2 layer with the thickness of 0.6 mm;
step four: sequentially laminating the Y1 layer, the X layer and the Y2 layer from top to bottom to form a green body;
step five: packaging the green body after the step four;
step six: and D, moving the green body which is subjected to the step five into isostatic pressing equipment for isostatic pressing treatment, wherein the processing parameters of the isostatic pressing treatment are as follows: the pressure is 170 MPa, the pressure maintaining time is 30 minutes, and the water temperature is 70 ℃;
step seven: transferring the green body subjected to the step six into glue discharging equipment for glue discharging treatment;
step eight: transferring the green body obtained in the step seven into sintering equipment for sintering treatment to obtain a ceramic composite body, wherein the thickness of the ceramic composite body is 1.5 mm; the change of the processing temperature of the sintering equipment is as follows:
a: the temperature in the sintering equipment is raised to 50 ℃, and the required time is 60 minutes;
b: the temperature in the sintering equipment is raised to 170 ℃, and the required time is 140 minutes;
c: the temperature in the sintering equipment is raised to 650 ℃, and the required time is 400 minutes;
d: the temperature in the sintering equipment is raised to 1100 ℃, and the required time is 350 minutes;
e: the temperature in the sintering equipment is increased to 1490 ℃, and the required time is 200 minutes;
f: the temperature in the sintering equipment was maintained to 1490 degrees celsius for a duration of 260 minutes.
Comparative example 1: the preparation method of the high-toughness ceramic composite comprises the following process steps:
the method comprises the following steps: preparing an X layer with the thickness of 0.1mm by molding and processing the stabilized zirconia with the mole ratio of 1%;
step two: forming the stabilized zirconia with the mole ratio of 0.5% to obtain a Y1 layer with the thickness of 0.1 mm;
step three: forming the stabilized zirconia with the mole ratio of 0.3% to obtain a Y2 layer with the thickness of 0.1 mm;
step four: sequentially laminating the Y1 layer, the X layer and the Y2 layer from top to bottom to form a green body;
step five: packaging the green body after the step four;
step six: and D, moving the green body which is subjected to the step five into isostatic pressing equipment for isostatic pressing treatment, wherein the processing parameters of the isostatic pressing treatment are as follows: the pressure is 110 MPa, the pressure maintaining time is 3 minutes, and the water temperature is 33 ℃;
step seven: transferring the green body subjected to the step six into glue discharging equipment for glue discharging treatment;
step eight: transferring the green body obtained in the seventh step into sintering equipment for sintering treatment to obtain a ceramic composite body, wherein the thickness of the ceramic composite body is 0.1 mm; the change of the processing temperature of the sintering equipment is as follows:
a: the temperature in the sintering equipment is raised to 5 ℃, and the required time is 6 minutes;
b: the temperature in the sintering equipment is increased to 65 ℃, and the required time is 73 minutes;
c: the temperature in the sintering equipment is raised to 520 ℃, and the required time is 240 minutes;
d: the temperature in the sintering equipment is raised to 950 ℃, and the required time is 180 minutes;
e: the temperature in the sintering equipment is increased to 1300 ℃, and the required time is 85 minutes;
f: the temperature in the sintering equipment is maintained to 1300 ℃ for 120 minutes.
Comparative example 2: the preparation method of the high-toughness ceramic composite comprises the following process steps:
the method comprises the following steps: preparing an X layer with the thickness of 1.3mm by molding and processing the stabilized zirconia with the mole ratio of 6 percent;
step two: preparing a Y1 layer with the thickness of 1.4mm by molding and processing the stabilized zirconia with the mole ratio of 4 percent;
step three: preparing a Y2 layer with the thickness of 1.5mm by molding and processing the stabilized zirconia with the mole ratio of 3.7 percent;
step four: sequentially laminating the Y1 layer, the X layer and the Y2 layer from top to bottom to form a green body;
step five: packaging the green body after the step four;
step six: and D, moving the green body which is subjected to the step five into isostatic pressing equipment for isostatic pressing treatment, wherein the processing parameters of the isostatic pressing treatment are as follows: the pressure is 200 MPa, the pressure maintaining time is 42 minutes, and the water temperature is 80 ℃;
step seven: transferring the green body subjected to the step six into glue discharging equipment for glue discharging treatment;
step eight: transferring the green body obtained in the step seven into sintering equipment for sintering treatment to obtain a ceramic composite body, wherein the thickness of the ceramic composite body is 2 mm; the change of the processing temperature of the sintering equipment is as follows:
a: the temperature in the sintering equipment is raised to 62 ℃, and the required time is 80 minutes;
b: the temperature in the sintering equipment is raised to 200 ℃, and the required time is 170 minutes;
c: the temperature in the sintering equipment is raised to 700 ℃, and the required time is 470 minutes;
d: the temperature in the sintering equipment is raised to 1180 ℃, and the required time is 450 minutes;
e: the temperature in the sintering equipment is raised to 1600 ℃, and the required time is 280 minutes;
f: the temperature in the sintering equipment was maintained to 1600 ℃ for 350 minutes.
And (3) testing the bending strength: the bending strength of the first to fifth examples and the first and second comparative examples was tested by a three-point bending tester; and (3) testing fracture toughness: the fracture toughness of the first to fifth examples and the first and second comparative examples is tested by an indentation method; vickers hardness test: and pressing a diamond pyramid pressure head with an included angle of 136 degrees between opposite surfaces into the surface of the sample to be tested under the action of a specified load F, removing the load after keeping the time, measuring the length d of a diagonal line of the indentation, further calculating the surface area of the indentation, and finally calculating the average pressure on the surface area of the indentation, namely the Vickers hardness value of the metal. The test results are shown in Table I.
Table one: bending strength, fracture toughness, vickers hardness contrast:
a second table: the ceramic composite of the present invention was compared to fracture toughness for 2% stabilized zirconia and 3% stabilized zirconia:
the test data of the table I and the table II are combined to obtain that the ceramic composite prepared by the invention has higher improvement on fracture toughness compared with the stable zirconia of the comparative example 1, the comparative example 2 and the stable zirconia of the 3 percent, the ceramic composite can be applied to the fields of mobile phone back plates, ceramic knives, watch shells and the like, when products such as the mobile phone back plates, the ceramic knives, the watch shells and the like are deformed under pressure, the higher fracture toughness can absorb the deformation force, the phenomenon that the ceramic composite is deformed to cause fracture is reduced, and the table I shows that if the molar ratio of the stable zirconia is reduced, the Vickers hardness of the ceramic composite is reduced, namely the impact resistance is reduced, the prepared finished product cannot be used by consumers without worry, and the larger time expenditure and the cost are greatly improved in the preparation process, are not paid.
If the terms "first" and "second" are used for descriptive purposes only and not for indicating or implying relative importance or implicitly indicating the number of technical features. Thus, a definition of "a first" or "a second" feature may explicitly or implicitly include one or more of the features, and in the description of the invention, "a number" means two or more unless explicitly defined otherwise.
The above-mentioned embodiments only express a plurality of embodiments of the present invention, and the description thereof is more specific and detailed, but not to be construed as limiting the scope of the present invention. It should be noted that, for a person skilled in the art, several variations and modifications can be made without departing from the inventive concept, which falls within the scope of the present invention. Therefore, the protection scope of the present patent shall be subject to the appended claims.
Claims (8)
1. The preparation method of the high-toughness ceramic composite comprises the following process steps: the method comprises the following steps: preparing an X layer with the thickness of 0.2 to 0.6mm by molding yttria-stabilized zirconia with the mole ratio of 2.5 to 4 percent; step two: preparing Y1 layer with thickness of 0.2-0.6 mm by molding yttria-stabilized zirconia with mole ratio of 1-2.5%; step three: preparing Y2 layer with thickness of 0.2-0.6 mm by molding yttria-stabilized zirconia with mole ratio of 1-2.5%; step four: sequentially stacking the Y1 layer, the X layer and the Y2 layer from top to bottom to form a green body, wherein at least one transition layer is arranged between the Y1 layer and the X layer and between the Y2 layer and the X layer; step five: packaging the green body after the step four; step six: transferring the green body subjected to the fifth step into isostatic pressing equipment for isostatic pressing treatment; step seven: transferring the green body subjected to the step six into glue discharging equipment for glue discharging treatment; step eight: transferring the green body obtained in the step seven into sintering equipment for sintering treatment to obtain a ceramic composite; the change of the processing temperature of the sintering equipment is as follows: a: the temperature in the sintering equipment is raised to T1, the required time is 15 to 60 minutes, and the temperature of T1 is 10 to 50 ℃; b: the temperature in the sintering equipment is raised to T1+70 ℃ to T1+120 ℃, and the required time is 90-140 minutes; c: the temperature in the sintering equipment is raised to T1+550 ℃ to T1+600 ℃, and the required time is 300-400 minutes; d: the temperature in the sintering equipment is raised to T1+1000 ℃ to T1+1050 ℃, and the required time is 240-350 minutes; e: the temperature in the sintering equipment is increased from T1+1370 ℃ to T1+1440 ℃ for 120-200 minutes; f: the temperature within the sintering apparatus was maintained to T1+1370 to T1+1440 degrees celsius for 180 to 260 minutes.
2. The method of preparing a high toughness ceramic composite of claim 1 wherein: the eighth step: transferring the green body obtained in the step seven into sintering equipment for sintering treatment to obtain a ceramic composite; the change of the processing temperature of the sintering equipment is as follows: a: the temperature in the sintering equipment is raised to T1, the required time is 20 to 50 minutes, and the temperature of T1 is 15 to 40 ℃; b: the temperature in the sintering equipment is raised to T1+70 ℃ to T1+100 ℃, and the required time is 100-140 minutes; c: the temperature in the sintering equipment is increased to T1+550 ℃ to T1+580 ℃, and the required time is 320-400 minutes; d: the temperature in the sintering equipment is raised to T1+1000 ℃ to T1+1040 ℃, and the required time is 260-340 minutes; e: the temperature in the sintering equipment is increased from T1+1370 ℃ to T1+1420 ℃, and the required time is 150-200 minutes; f: the temperature within the sintering apparatus is maintained to T1+1370 degrees celsius to T1+1420 degrees celsius for a duration of 200 to 260 minutes.
3. The method of preparing a high toughness ceramic composite of claim 1, wherein: the eighth step: transferring the green body obtained in the step seven into sintering equipment for sintering treatment to obtain a ceramic composite; the change of the processing temperature of the sintering equipment is as follows: a: the temperature in the sintering equipment is raised to T1, the required time is 20 to 40 minutes, and the temperature of T1 is 25 to 40 ℃; b: the temperature in the sintering equipment is raised to T1+80 ℃ to T1+95 ℃, and the required time is 100-130 minutes; c: the temperature in the sintering equipment is increased to T1+550 ℃ to T1+580 ℃, and the required time is 340-370 minutes; d: the temperature in the sintering equipment is increased to T1+1000 ℃ to T1+1030 ℃, and the required time is 260-310 minutes; e: the temperature in the sintering equipment is increased from T1+1370 ℃ to T1+1400 ℃, and the required time is 160-200 minutes; f: the temperature within the sintering apparatus was maintained to T1+1370 degrees celsius to T1+1400 degrees celsius for a duration of 220 to 260 minutes.
4. The method of preparing a high-toughness ceramic composite body according to any one of claims 1 to 3, wherein: the forming processing in the step one is any one of dry pressing, tape casting, gelling, injection molding, film rolling, dry bag type isostatic pressing, spraying and screen printing; the forming processing in the second step is any one of dry pressing, tape casting, gelling, injection molding, film rolling, dry bag type isostatic pressing, spraying and screen printing; the forming process in the third step is any one of dry pressing, tape casting, gelling, injection molding, film rolling, dry bag type isostatic pressing, spraying and screen printing.
5. The method of preparing a high-toughness ceramic composite body according to any one of claims 1 to 3, wherein: the processing parameters of the isostatic pressing treatment in the sixth step are as follows: the pressure is 130 to 170 MPa, the pressure maintaining time is 10 to 30 minutes, and the water temperature is 48 to 70 ℃.
6. The method of preparing a high-toughness ceramic composite body according to any one of claims 1 to 3, wherein: and the isostatic pressing treatment in the sixth step is cold isostatic pressing treatment or warm isostatic pressing treatment.
7. The method of preparing a high-toughness ceramic composite body according to any one of claims 1 to 3, wherein: the thickness of the ceramic composite body completing the step eight is 0.4 to 1.5 mm.
8. The method of preparing a high-toughness ceramic composite body according to any one of claims 1 to 3, wherein: the method also comprises the ninth step: and C, performing cutting treatment, grinding treatment, polishing treatment and film coating treatment on the ceramic composite body subjected to the step eight.
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| CN203401768U (en) * | 2013-05-29 | 2014-01-22 | 苏州衡业新材料科技有限公司 | Toughened zirconium oxide ceramic with combined structure |
| CN107337450A (en) * | 2017-06-30 | 2017-11-10 | 广东新秀新材料股份有限公司 | High tenacity ceramics, its preparation method and application |
| CN107445612A (en) * | 2017-06-28 | 2017-12-08 | 瑞声科技(新加坡)有限公司 | Zirconia ceramics and preparation method thereof |
| CN207108835U (en) * | 2017-06-14 | 2018-03-16 | 东莞华晶粉末冶金有限公司 | A kind of layered composite ceramic plate and mobile terminal device |
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| CN203401768U (en) * | 2013-05-29 | 2014-01-22 | 苏州衡业新材料科技有限公司 | Toughened zirconium oxide ceramic with combined structure |
| CN207108835U (en) * | 2017-06-14 | 2018-03-16 | 东莞华晶粉末冶金有限公司 | A kind of layered composite ceramic plate and mobile terminal device |
| CN107445612A (en) * | 2017-06-28 | 2017-12-08 | 瑞声科技(新加坡)有限公司 | Zirconia ceramics and preparation method thereof |
| CN107337450A (en) * | 2017-06-30 | 2017-11-10 | 广东新秀新材料股份有限公司 | High tenacity ceramics, its preparation method and application |
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