CN115286381A - 3Y-TZP zirconia ceramic sintering method with removal and scale improvement of ductile domain - Google Patents
3Y-TZP zirconia ceramic sintering method with removal and scale improvement of ductile domain Download PDFInfo
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Abstract
The invention relates to a 3Y-TZP zirconia ceramic sintering method with improved ductility domain removal scale, which comprises the steps of pre-sintering a 3Y-TZP zirconia ceramic blank, then carrying out cutting processing on the blank, and after the processing is finished, carrying out secondary complete sintering on the blank to obtain the 3Y-TZP zirconia ceramic, wherein the pre-sintering junction temperature is 1100-1300 ℃. According to the invention, the 3Y-TZP zirconia ceramic blank with high cutting processability can be prepared by controlling the pre-sintering temperature to be 1100-1300 ℃, namely the 3Y-TZP zirconia ceramic blank with relatively low material hardness, stable ductile-brittle removal characteristic and large ductile domain removal scale can be prepared, and the efficient precision processing of the ceramic material can be realized.
Description
Technical Field
The invention belongs to the technical field of inorganic non-metallic material manufacturing, and relates to a 3Y-TZP zirconia ceramic sintering method with an improved ductile domain removal scale.
Background
With the development of aerospace, semiconductor and electronic engineering, more and more brittle ceramic parts need to be subjected to ultra-precise cutting. The reason why the cutting processing of the ceramic material is a difficult problem in the field of cutting processing is that the removing mechanism of the brittle fracture of the ceramic material generates a plurality of cracks in a cutting processing area, reduces the quality of a processed surface and is difficult to realize ultra-precise cutting processing.
When the cutting depth is less than the critical cutting depth of ductile-brittle transition during the ultraprecise cutting processing of the brittle material, the ductile cutting of the brittle material can be realized. Zirconia ceramics, one of the most widely used ceramic materials, has the characteristics of high hardness and high brittleness after being fully sintered, and has an extremely small ductile domain removal scale. This requires the cutting depth to be controlled to a small value during the cutting process, which not only puts a high demand on the motion accuracy of the machine tool, but also greatly reduces the machining efficiency.
The prior sintering method of zirconia ceramics comprises a step sintering method besides complete sintering. The step sintering method is to pre-sinter ceramic blank at a lower temperature, and aims to greatly reduce the hardness of the ceramic so as to realize large-allowance processing of the ceramic, and then carry out secondary complete sintering at a high temperature after the processing is finished. However, the sintering temperature of the prior presintering is usually lower than 1000 ℃, and at the sintering temperature, the ceramic material still has a porous structure, the crystallization process is not started, and the intercrystalline bonding strength is low, so that cracks of the material are easy to nucleate and expand among the grains of the cluster under the action of cutting load, and dislocation slip motion is avoided.
The microcosmic substance of ductility removal of the polycrystalline ceramic material is continuous dislocation sliding movement in the material, so that the 3Y-TZP zirconia ceramic blank after presintering cannot generate ductility removal behavior at the existing presintering temperature, and the ultra-precision processing of the ceramic material cannot be realized.
Disclosure of Invention
In order to solve the problems in the prior art, the invention provides a 3Y-TZP zirconia ceramic sintering method with improved ductility domain removal scale.
In order to achieve the purpose, the technical scheme adopted by the invention is as follows:
A3Y-TZP zirconia ceramic sintering method comprises the steps of firstly pre-sintering a 3Y-TZP zirconia ceramic blank, then cutting and processing the blank, and then performing secondary complete sintering on the blank after the processing is finished to obtain the 3Y-TZP zirconia ceramic, wherein the pre-sintering temperature is 1100-1300 ℃;
the 3Y-TZP zirconia ceramic is zirconia ceramic added with 3mol percent of yttria stabilizer;
the main difference between the invention and the prior art is the pre-sintering temperature, and the 3Y-TZP zirconia ceramic blank with high cutting processability can be prepared by controlling the pre-sintering temperature to be 1100-1300 ℃, namely the 3Y-TZP zirconia ceramic blank with relatively low material hardness, stable ductile-brittle removal characteristic and large ductile domain removal scale; when the pre-sintering temperature is lower than 1100 ℃, although the hardness of the 3Y-TZP zirconia ceramic blank is lower, the ductile-brittle removal behavior of the ceramic material is not obvious, and the ductile domain removal scale is smaller; when the pre-sintering temperature is higher than 1300 ℃, although the ceramic material of the 3Y-TZP zirconia ceramic blank has obvious ductile-brittle removal behavior and larger ductile domain removal scale, the 3Y-TZP zirconia ceramic blank has high hardness characteristic and is not suitable for direct cutting processing any more; therefore, the invention controls the pre-sintering temperature to be 1100-1300 ℃.
The 3Y-TZP zirconia ceramic blank has relatively low material hardness at the pre-sintering temperature (1100-1300 ℃), because the hardness of the polycrystalline ceramic depends on the minimum solid phase contact area among crystal grains, the crystal grains are converted from a high specific surface area and a high surface energy state to a low specific surface area and a low surface energy state (solid-solid contact state) under the action of a sintering driving force along with the increase of the sintering temperature, obvious crystal boundaries are generated among the crystal grains after 1300 ℃, the minimum solid phase contact area among the crystal grains is remarkably increased, and thus the ceramic material is in a high hardness state;
the 3Y-TZP zirconia ceramic blank has stable extending-brittleness removal characteristics at the pre-sintering temperature (1100-1300 ℃), because the ceramic material does not crystallize before 1100 ℃, crystal grains are only close to each other under the action of sintering driving force, and the inter-crystal mass transfer behavior is not started, so that the crystal grains are separated from each other, and the loose microstructure causes irregular fracture of the material under the action of cutting load, thereby failing to present the extending-brittleness removal characteristics; after 1100 ℃, along with the increase of sintering temperature, the inter-grain mass transfer behavior is started under the action of sintering driving force, a sintering neck is formed among grains, and the sintering neck has certain bonding strength;
the 3Y-TZP zirconia ceramic blank has larger ductile domain removal scale at the presintering temperature (1100-1300 ℃) of the invention, because clear and obvious grain boundaries are formed among crystal grains after the sintering temperature exceeds 1300 ℃, the intercrystalline bonding strength is greatly enhanced, in the material removal process, cracks always expand along the direction with lowest energy consumption, and the excessive intercrystalline bonding strength causes the cracks to expand along the interior of the crystal grains, thereby generating brittle fracture rather than plastic slip motion.
As a preferable technical scheme:
the sintering method of the 3Y-TZP zirconia ceramic has the advantages that the Vickers hardness of the 3Y-TZP zirconia ceramic blank after pre-sintering is 103-1156 HV, and the ductility domain removal scale is 1.35-3.51 mu m.
The sintering method of the 3Y-TZP zirconia ceramic has the sintering temperature of 1200 ℃.
In the sintering method of the 3Y-TZP zirconia ceramic, the Vickers hardness of the pre-sintered 3Y-TZP zirconia ceramic blank is 518HV, and the ductile domain removal scale is 3.51 mu m.
According to the sintering method of the 3Y-TZP zirconia ceramic, the pre-sintering adopts an isothermal and normal pressure sintering mode, the temperature rise rate is 5 ℃/min, the heat preservation time is 1h, the temperature rise starting point is room temperature, the temperature rise rate and the heat preservation time are general parameters on the market, and can be adjusted according to actual conditions.
The sintering method of the 3Y-TZP zirconia ceramic is characterized in that after pre-sintering, the ceramic is cooled to room temperature at a cooling rate of 5 ℃/min.
In the sintering method of the 3Y-TZP zirconia ceramic, the temperature of the secondary complete sintering is 1500 ℃, and the 3Y-TZP ceramic is completely densified at the temperature to obtain the final required physical and mechanical properties.
According to the sintering method of the 3Y-TZP zirconia ceramic, the secondary complete sintering adopts an isothermal and normal pressure sintering mode, the temperature rise rate is 5 ℃/min, the heat preservation time is 1h, the temperature rise starting point is room temperature, and the temperature rise rate and the heat preservation time are general parameters on the market and can be adjusted according to actual conditions.
Advantageous effects
The method can be used for realizing the ultra-precision processing of the zirconia ceramic material, and compared with the existing two-step sintering process scheme of the zirconia ceramic, the method has the essential differences that: the pre-sintering temperature in the prior two-step sintering is mostly below the crystallization temperature, and the main purpose is to reduce the hardness of the zirconia ceramic material, so that the conventional cutter can meet the processing requirement of the zirconia ceramic material, while the pre-sintering temperature in the invention is higher than the crystallization temperature, so that the pre-sintered ceramic has enough mechanical strength intercrystalline bonding strength, thereby meeting the dislocation slip condition of the ceramic material for ductility removal, and simultaneously, the pre-sintered 3Y-TZP zirconia ceramic blank has moderate hardness and the largest ductility domain removal scale, thereby realizing the efficient precision processing of the ceramic material.
Drawings
FIG. 1 is a graph showing the relative density and grain size variation of pre-sintered 3Y-TZP zirconia ceramic blank at different pre-sintering temperatures;
FIG. 2 is a scanning electron microscope image of a pre-sintered 3Y-TZP zirconia ceramic blank at different pre-sintering temperatures; wherein (a) is a scanning electron micrograph at 1000 ℃; (b) is a scanning electron micrograph at 1200 ℃; (c) is a scanning electron micrograph at 1300 ℃; (d) is a scanning electron micrograph at 1500 ℃;
FIG. 3 is a graph showing the Vickers hardness of pre-sintered 3Y-TZP zirconia ceramic blank at different pre-sintering temperatures;
FIG. 4 is a force signal fluctuation variance diagram in the scribing process of the pre-sintered 3Y-TZP zirconia ceramic blank at different pre-sintering temperatures;
FIG. 5 is a scale evolution diagram of the ductile region and transition region removal of the pre-sintered 3Y-TZP zirconia ceramic blank at different pre-sintering temperatures.
Detailed Description
The invention will be further illustrated with reference to specific embodiments. It should be understood that these examples are for illustrative purposes only and are not intended to limit the scope of the present invention. Further, it should be understood that various changes or modifications of the present invention can be made by those skilled in the art after reading the teaching of the present invention, and these equivalents also fall within the scope of the claims appended to the present application.
Example 1
A sintering method of 3Y-TZP zirconia ceramics comprises the following specific steps:
(1) The 3Y-TZP ceramic powder was dry-pressed at a pressure of 90MPa and subsequently hot isostatically pressed at 300 ℃ at a pressure of 240MPa to obtain a density of 3.24g/cm 3 The 3Y-TZP zirconia ceramic blank;
(2) Pre-sintering the 3Y-TZP zirconia ceramic blank at 1200 ℃, wherein the sintering adopts an isothermal and normal pressure sintering mode, the temperature rise rate is 5 ℃/min, the heat preservation time is 1h, and the pre-sintered 3Y-TZP zirconia ceramic blank is obtained after being cooled to the room temperature at the cooling rate of 5 ℃/min;
the Vickers hardness of the prepared pre-sintered 3Y-TZP zirconia ceramic blank is 518HV, and the ductile domain removal scale is 3.51 mu m;
(3) Cutting the pre-sintered 3Y-TZP zirconia ceramic blank in the step (2);
(4) And (3) performing secondary complete sintering on the product obtained in the step (3) at 1500 ℃ to obtain the 3Y-TZP zirconia ceramic, wherein the secondary complete sintering adopts an isothermal normal pressure sintering mode, the temperature rise rate is 5 ℃/min, and the heat preservation time is 1h.
Example 2
A sintering method of 3Y-TZP zirconia ceramics comprises the following specific steps:
(1) The 3Y-TZP ceramic powder was dry-pressed at a pressure of 90MPa and subsequently hot isostatically pressed at 300 ℃ at a pressure of 240MPa to obtain a density of 3.24g/cm 3 The ceramic green body of (1);
(2) Pre-sintering the 3Y-TZP zirconia ceramic blank at 1100 ℃, wherein the sintering adopts an isothermal and normal pressure sintering mode, the temperature rise rate is 5 ℃/min, the heat preservation time is 1h, and the pre-sintered 3Y-TZP zirconia ceramic blank is obtained after being cooled to the room temperature at the cooling rate of 5 ℃/min;
the Vickers hardness of the prepared pre-sintered 3Y-TZP zirconia ceramic blank is 103HV, and the ductile domain removal scale is 1.35 mu m;
(3) Cutting the pre-sintered 3Y-TZP zirconia ceramic blank in the step (2);
(4) And (3) performing secondary complete sintering on the product obtained in the step (3) at 1500 ℃ to obtain the 3Y-TZP zirconia ceramic, wherein the secondary complete sintering adopts an isothermal normal pressure sintering mode, the temperature rise rate is 5 ℃/min, and the heat preservation time is 1h.
Example 3
A sintering method of 3Y-TZP zirconia ceramics comprises the following specific steps:
(1) The 3Y-TZP ceramic powder was dry-pressed at a pressure of 90MPa and subsequently hot isostatically pressed at 300 ℃ at a pressure of 240MPa to obtain a density of 3.24g/cm 3 The ceramic green body of (1);
(2) Pre-sintering the 3Y-TZP zirconia ceramic blank at 1300 ℃, wherein the sintering adopts an isothermal and normal pressure sintering mode, the temperature rise rate is 5 ℃/min, the heat preservation time is 1h, and the pre-sintered 3Y-TZP zirconia ceramic blank is obtained after being cooled to the room temperature at the cooling rate of 5 ℃/min;
the Vickers hardness of the prepared pre-sintered 3Y-TZP zirconia ceramic blank is 1156HV, and the ductile domain removal scale is 2.1 mu m;
(3) Cutting the pre-sintered 3Y-TZP zirconia ceramic blank in the step (2);
(4) And (3) performing secondary complete sintering on the product obtained in the step (3) at 1500 ℃ to obtain the 3Y-TZP zirconia ceramic, wherein the secondary complete sintering adopts an isothermal normal pressure sintering mode, the temperature rise rate is 5 ℃/min, and the heat preservation time is 1h.
The properties of microscopic materials of the zirconia ceramics at different sintering temperatures are different, the macroscopic cutting response of the zirconia ceramics is also different, and the presintering temperature of the zirconia ceramics is explored in order to improve the removal scale of the ductile domain; wherein the microscopic material properties include grain size, intergranular bonding mode, material density, material hardness, material removal behavior, and ductile domain removal scale.
The invention discloses a process for exploring the presintering temperature, which comprises the following specific steps:
the 3Y-TZP ceramic powder was dry-pressed at a pressure of 90MPa and subsequently hot isostatically pressed at 300 ℃ at a pressure of 240MPa to obtain a density of 3.24g/cm 3 The ceramic green body of (2);
the ceramic blank is placed in a normal pressure sintering furnace, the temperature rise rate is respectively increased to 800-1500 ℃ at the speed of 5 ℃/min, the temperature is preserved for one hour at each appointed presintering temperature (the appointed temperature is 800 ℃, 900 ℃, 1000 ℃, 1100 ℃,1200 ℃, 1300 ℃, 1400 ℃ and 1500 ℃), and then the ceramic blank is cooled to the room temperature at the cooling rate of 5 ℃/min, thus obtaining the presintering 3Y-TZP zirconia ceramic blank.
When the density of the material is measured by an Archimedes method, the density of the material at 800-1500 ℃ is shown as a dotted line in figure 1, and the densification state of the ceramic is obviously changed before and after 1200 ℃, wherein the relative density of the ceramic before 1200 ℃ is less than 70%, the material is in a porous state, and the relative density of the ceramic after 1200 ℃ is more than 85%, and the material already presents the densification state.
The average grain size and the intercrystalline bonding mode of the material are measured by adopting an electron microscope observation method, the grain size of the material at 800-1500 ℃ is shown as a solid line in figure 1, the grain growth behavior is obviously changed before and after 1200 ℃, the grain size is 89.53-115.15 nm before, the grain growth rate is slow, after the temperature, the grain growth rate is rapidly increased, and the grain size is 151.66-522.65 nm.
As shown in fig. 2, which is a microstructure morphology diagram of a pre-sintered 3Y-TZP zirconia ceramic blank under a scanning electron microscope and at different pre-sintering temperatures, it can be known that at 1000 ℃, the size of crystal grains is relatively small, and the crystal grains are clustered under the action of a sintering driving force, but a sintering neck is not formed yet; at 1200 ℃, sintering necks are formed among crystal grains, and crystal grains are accumulated, so that substance transmission exists among the crystal grains, and the bonding strength among the crystal grains is gradually improved; at 1300 ℃, the internal pores of the pre-sintered 3Y-TZP zirconia ceramic blank are gradually isolated and closed, an obvious crystal boundary is formed, and the intercrystalline bonding strength is obviously improved; the material is completely densified at 1500 ℃, the internal pores of the material are eliminated, the intercrystalline solid phase bonding area is the largest, and the bonding strength is also the highest.
The indentation method is adopted to measure the hardness of the material, the Vickers hardness of the ceramic is shown in figure 3 at 800-1500 ℃, the vickers hardness of the ceramic is shown in the range of 800-1000 ℃, the material has extremely low hardness (19-32 HV) due to low bonding strength between crystal grains, the crystallization process starts at 1100 ℃, the hardness of the ceramic slightly rises to reach 103HV, the hardness of the ceramic reaches 518HV along with the increase of the crystallinity at 1200 ℃, and the ceramic has high hardness (1156-1295 HV) due to the formation of crystal boundaries and the enlargement of the minimum solid phase contact area after 1300 ℃, so that the ceramic is not suitable for direct cutting processing any more.
Testing the removal behavior of the pre-sintered 3Y-TZP zirconia ceramic blank at different pre-sintering temperatures by adopting a variable-cutting-depth micron scratching experiment, and performing variance analysis on a force signal in the scratching process, wherein the result shows that as shown in FIG. 4, the fluctuation variance of the force signal is smaller in the whole scratching process before 1000 ℃, namely the material has no ceramic material extending-brittleness removal behavior; after 1100 ℃, the fluctuation variance of the force signal presents obvious segmentation characteristics, and the material removal presents typical ceramic material ductile-brittle removal behavior, so that the ceramic high-quality processing can be realized by utilizing ductile removal.
The scratch morphology is combined to measure the ductile domain and transition domain removal scale of the 3Y-TZP ceramic in the range of 1100-1500 ℃, and the result is shown in figure 5, it can be found that at 1100 ℃, the crystallization process of the ceramic is just started, the microstructure in the material is transformed from a porous state to a densified state and is in an unstable transition state, and therefore, the ductile domain removal scale is small. After 1200 ℃, the ductility domain and transition domain size of the pre-sintered 3Y-TZP zirconia ceramic blank are gradually reduced along with the increase of the pre-sintering temperature, and the maximum ductility domain and transition size of the pre-sintered 3Y-TZP zirconia ceramic blank sintered at 1200 ℃ are respectively 3.51 μm and 7.47 μm. Compared with the fully sintered alloy, the expansion is respectively 1.89 times and 2.08 times.
According to the research process, the low-hardness, ductile-brittle removal characteristic and the maximum ductile domain removal scale are taken as constraint conditions, the optimum temperature of the pre-sintering temperature is finally obtained through optimization and is 1200 ℃, the hardness of the material is 518HV at the moment, the material is still within the cutting and processing capacity range of a conventional cutter, the intercrystalline bonding strength is improved along with the starting of the crystallization process, the ductile-brittle removal characteristic of the material is achieved, and the large-scale crushing of the low-strength ceramic material is avoided. And the method has the largest ductile domain removal scale, and can realize the ultra-precise cutting processing of the ceramic material.
Claims (8)
1. A sintering method of 3Y-TZP zirconia ceramics is characterized in that pre-sintering is carried out on a 3Y-TZP zirconia ceramic blank, then cutting processing is carried out on the blank, and after the processing is finished, secondary complete sintering is carried out on the blank to obtain the 3Y-TZP zirconia ceramics, wherein the pre-sintering temperature is 1100-1300 ℃.
2. The sintering method of 3Y-TZP zirconia ceramic according to claim 1, wherein the Vickers hardness of the pre-sintered 3Y-TZP zirconia ceramic blank is 103 to 1156HV, and the ductile domain removal scale is 1.35 to 3.51 μm.
3. The sintering method of 3Y-TZP zirconia ceramic according to claim 2, characterized in that the pre-sintering temperature is 1200 ℃.
4. The sintering method of 3Y-TZP zirconia ceramic according to claim 3, wherein the Vickers hardness of the pre-sintered 3Y-TZP zirconia ceramic blank is 518HV, and the ductile domain removal scale is 3.51 μm.
5. The sintering method of 3Y-TZP zirconia ceramic according to claim 1, characterized in that the presintering adopts isothermal and normal pressure sintering, the temperature rise rate is 5 ℃/min, and the holding time is 1h.
6. The method of claim 1, wherein the pre-sintered body is cooled to room temperature at a cooling rate of 5 ℃/min.
7. The sintering method of 3Y-TZP zirconia ceramic according to claim 1, characterized in that the temperature of the second sintering is 1500 ℃.
8. The sintering method of 3Y-TZP zirconia ceramic according to claim 7, characterized in that the secondary complete sintering adopts isothermal and normal pressure sintering, the temperature rise rate is 5 ℃/min, and the holding time is 1h.
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