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CN112225557B - Preparation method of zirconia ceramic with pearl effect and product prepared by preparation method - Google Patents

Preparation method of zirconia ceramic with pearl effect and product prepared by preparation method Download PDF

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CN112225557B
CN112225557B CN202011113059.3A CN202011113059A CN112225557B CN 112225557 B CN112225557 B CN 112225557B CN 202011113059 A CN202011113059 A CN 202011113059A CN 112225557 B CN112225557 B CN 112225557B
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zirconia
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flaky alumina
pearl effect
zirconia ceramic
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CN112225557A (en
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刘琪
刘志
刘凯旋
许俊
胡礼军
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De Corematrix Co ltd
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Abstract

The invention discloses a preparation method of zirconia ceramics with pearl effect, which comprises the steps of uniformly mixing zirconia powder, flaky alumina and an additive to obtain a mixture, and carrying out tape casting to obtain a ceramic blank; and sintering the ceramic blank to obtain the zirconia ceramic with the pearl effect. In addition, the product prepared by the preparation method of the zirconia ceramic with the pearl effect is also disclosed. The zirconia ceramic provided by the invention has the advantages that the good mechanical property is maintained, the appearance aesthetic effect is enhanced, the pearlescent effect is stable and durable, and the zirconia ceramic can be used for manufacturing artificial dentures, wearable consumer electronics equipment shell materials and the like; and the preparation method has simple process and easy operation, and is suitable for large-scale production.

Description

Preparation method of zirconia ceramic with pearl effect and product prepared by preparation method
Technical Field
The invention relates to the technical field of ceramic materials, in particular to a preparation method of a zirconia ceramic with a pearlescent effect, which can be used for manufacturing artificial dentures, wearable consumer electronics equipment shell materials and the like, and a product prepared by the zirconia ceramic.
Background
The zirconia ceramic can effectively improve the brittleness of the ceramic material through a special 'phase change toughening' mechanism. The zirconia ceramics have three crystal forms, namely monoclinic phase, tetragonal phase and cubic phase. Among them, the zirconia ceramics of tetragonal phase or mixture of tetragonal phase and cubic phase are widely used in many fields, especially the use on artificial denture and wearable electronic consumer product equipment shell materials is rapidly developed. When used as a denture and shell material, zirconia ceramics are required to have not only good mechanical properties but also excellent aesthetic and optical properties. Although the zirconia ceramics can improve the glossiness by surface grinding, the method increases the process and the manufacturing cost, and the polished surface has poor gloss durability and unnatural gloss.
The two-dimensional sheet material has the dual characteristics of micron powder and nanometer material due to the unique sheet structure and the unique crystal shape. Two-dimensional sheet materials such as mica sheets, titanium dioxide sheets, aluminum oxide sheets and the like have pearl-like optical characteristics, and are applied to the fields of coatings, cosmetics and the like, for example, the sheet aluminum oxide is added into paint and coated on the surface of metal, so that the appearance aesthetic effect can be enhanced. The flaky alumina with good diameter-thickness ratio is transparent, can endure high temperature up to 1600 ℃, has flat and smooth surface and high refractive index, and can ensure that the coloring luster has third dimension and is more warm, moist and soft through the pearly luster effect. If the flaky alumina is modified on the surface of the zirconia ceramic by a surface coating method such as coating, bonding and the like to obtain the zirconia ceramic with pearl effect, the pearl effect is only limited on the surface layer of the zirconia, and the surface coating is easy to fall off and has poor durability; in addition, the flake alumina coated is not easily uniformly distributed, thereby affecting the surface decoration effect.
Disclosure of Invention
The invention aims to overcome the defects of the prior art and provide a preparation method of zirconia ceramics with pearl effect, which takes zirconia powder, flaky alumina and additives as raw materials and obtains the zirconia ceramics with pearl effect, wherein the flaky alumina is uniformly dispersed in a zirconia matrix through tape casting and sintering processes, so that the zirconia ceramics can maintain excellent mechanical property, enhance the aesthetic effect of the appearance and ensure that the pearl effect is stable and durable. The invention also aims to provide a product prepared by the preparation method.
The purpose of the invention is realized by the following technical scheme:
the invention provides a preparation method of zirconia ceramic with pearl effect, which comprises the following steps:
(1) uniformly mixing zirconia powder, flaky alumina and an additive to obtain a mixture; the additive comprises a lubricant, a bonding agent and a surface modifier, wherein the lubricant is polyethylene glycol, the bonding agent is tetraethyl silicate and/or amino silicone oil, and the surface modifier is one or the combination of polydextrose, citric acid, sodium citrate, polyacrylic acid and ammonium polyacrylate; the dosage of the flaky alumina is 1.0-8.0 wt% of the zirconia powder; the dosage of the additive is 0.5-5.0 wt% of the total amount of the zirconia powder and the flaky alumina;
(2) carrying out tape casting on the mixture to obtain a ceramic blank;
(3) sintering the ceramic blank at 1400-1600 ℃ for 0.5-4 h to obtain the pearl zirconia ceramic.
The mechanical property and the optical property of the zirconia ceramics are influenced by the crystal structure of the zirconia. Tetragonal zirconia ceramics have good mechanical strength but less transparency than cubic zirconia ceramics, which have good optical transparency but less mechanical strength than tetragonal zirconia ceramics. The three-point bending strength of zirconia ceramics decreases as the cubic phase increases. In order to have good mechanical property and optical property and be suitable for manufacturing artificial dentures, wearable consumer electronics equipment shell materials and the like, the zirconia ceramic is a tetragonal phase or a mixed phase of the tetragonal phase and the cubic phase. As the type and the content of the stabilizer can also influence the crystal form of the zirconia, in order to further ensure that a required crystal form structure of the zirconia is obtained, the zirconia is the zirconia containing the stabilizer, the stabilizer comprises yttrium oxide, magnesium oxide, calcium oxide and cerium oxide, and the content of the stabilizer is 2.0-5.0 mol%.
The performance of the zirconia ceramic with the pearl effect is influenced by the radius-thickness ratio of the flaky alumina. The larger the radius-thickness ratio of the flaky alumina is, the more obvious the pearl effect is. However, as the radius-thickness ratio of the flaky alumina increases, the uniformity of material mixing decreases, and the probability of cracking of the flaky alumina during the preparation of the sintered body increases, which easily causes the decrease of the three-point bending strength of the final sintered body. Therefore, the average diameter-thickness ratio of the flaky alumina is 50 to 130, preferably 70 to 100.
In addition, the use of the aspect ratio of the tabular alumina of the present invention also affects the properties of the final ceramic product. The content of the flaky alumina is too low, and the pearl effect is not obvious; the flaky alumina content is too high, and the three-point bending strength of the sintered body is remarkably reduced. For this purpose, the amount of the flaky alumina of the present invention is preferably 2.0 to 5.0 wt% of the zirconia powder.
The performance of the zirconia ceramic with the pearl effect is influenced by the composition and the dosage of the additive. The zirconia powder and the flaky alumina can not directly generate chemical reaction, the interface bonding force is weak, and the added bonding agent can form a silicon oxide layer between the zirconia powder and the flaky alumina in the sintering process, so that the interface chemical bonding is enhanced. The added lubricant can improve the mixing uniformity of the zirconia powder and the flaky alumina. In the scheme, the additive comprises a lubricant, a bonding agent and a surface modifier according to the mass ratio of 2: 1: 0.5-3.0.
If the content of the additive is too low, the dispersion uniformity of the flaky alumina in the sintered body is reduced; the content of the additive is too high, the additive is easy to remain, and the mechanical property and the pearlescent effect of the sintered body are reduced. For this purpose, the amount of the additive of the present invention is preferably 1.0 to 4.0 wt% of the total amount of the zirconia powder and the tabular alumina.
The performance of the zirconia ceramic with the pearl effect is influenced by the sintering temperature. The sintering temperature is too low, the sintering body is difficult to densify, and the three-point bending strength of the sintering body is reduced; the sintering temperature is too high, the crystal grains grow obviously, the three-point bending strength of the sintered body is reduced, and the energy consumption is wasted. For this purpose, the sintering temperature in the step (3) of the invention is preferably 1450-1550 ℃.
The crystal form of the zirconia ceramic is a tetragonal phase or a mixed phase of the tetragonal phase and the cubic phase, and the three-point bending strength of the zirconia ceramic is not less than 600 MPa.
The invention has the following beneficial effects:
(1) the zirconia ceramic of the invention not only maintains excellent mechanical property, but also endows the zirconia ceramic with warm and moist pearl effect, and enhances the aesthetic characteristics of the zirconia ceramic. And the flaky alumina is uniformly dispersed in the zirconia matrix, the pearlescent effect is stable and durable, the pearlescent effect is still kept after the sintered body is processed, and the method can be used for manufacturing artificial dentures, wearable consumer electronics equipment shell materials and the like.
(2) The added flaky alumina is directionally dispersed in the zirconia matrix according to the same two-dimensional structural form as much as possible through the tape casting process, so that the mechanical property of the zirconia ceramic is favorably maintained, and the pearlescent effect is further improved.
(3) The preparation method has simple process and easy operation, and is suitable for large-scale production.
Drawings
The invention will now be described in further detail with reference to the following examples and the accompanying drawings:
FIG. 1 is an XRD spectrum of a zirconia ceramic product with pearlescent effect prepared by the embodiment of the invention.
Detailed Description
The embodiment of the invention provides a preparation method of zirconia ceramic with a pearlescent effect, which comprises the following steps:
(1) mixing 2.0-5.0 mol% of yttria-stabilized zirconia powder, flaky alumina with the average diameter-thickness ratio of 50-130 and an additive for 12 hours to obtain a mixture; wherein the dosage of the flaky alumina is 1.0-8.0 wt% of the zirconia powder; the dosage of the additive is 0.5-5.0 wt% of the total amount of the zirconia powder and the flaky alumina;
(2) carrying out tape casting on the mixture, wherein the tape casting parameter is 2m/min, and the temperature is 55 ℃, so as to obtain a ceramic blank;
(3) and (3) sintering the ceramic blank in a muffle furnace at the temperature of 1400-1600 ℃ for 0.5-4 h to obtain the zirconium oxide ceramic product with the pearl effect.
The amounts of raw materials and process parameters for each example are shown in table 1.
TABLE 1 amounts of raw materials and process parameters for the examples of the invention
Figure BDA0002729232130000041
The additive in each embodiment of the invention comprises a lubricant, a bonding agent and a surface modifier, wherein the lubricant is polyethylene glycol, the bonding agent is tetraethyl silicate and/or amino silicone oil, and the surface modifier is one or the combination of polydextrose, citric acid, sodium citrate, polyacrylic acid and ammonium polyacrylate. According to the mass ratio of the lubricant to the bonding agent to the surface modifier of 2: 1: 0.5-3.0. The composition and mass ratio of the additives of each example are shown in Table 2.
TABLE 2 compositions and mass ratios of additives of the examples of the invention
Figure BDA0002729232130000042
The zirconia ceramic product with pearlescent effect prepared by the embodiments of the invention adopts an X-ray diffraction method to determine the crystal structure, and the typical XRD pattern is shown in figure 1. And testing the three-point bending strength by adopting the national standard GB/T6569-2006. The results are shown in Table 3.
TABLE 3 Crystal form Structure and Performance index of zirconia ceramic products prepared according to the examples of the present invention
Figure BDA0002729232130000051

Claims (8)

1. A preparation method of zirconia ceramics with pearl effect is characterized by comprising the following steps:
(1) uniformly mixing zirconia powder, flaky alumina and an additive to obtain a mixture; the additive comprises a lubricant, a bonding agent and a surface modifier, wherein the lubricant is polyethylene glycol, the bonding agent is tetraethyl silicate and/or amino silicone oil, and the surface modifier is one or the combination of polydextrose, citric acid, sodium citrate, polyacrylic acid and ammonium polyacrylate; the average diameter-thickness ratio of the flaky alumina is 50-130, and the dosage of the flaky alumina is 1.0-8.0 wt% of the zirconia powder; the dosage of the additive is 0.5-5.0 wt% of the total amount of the zirconia powder and the flaky alumina, and the mass ratio of the lubricant to the binder to the surface modifier in the additive is 2: 1: 0.5-3.0;
(2) carrying out tape casting on the mixture to obtain a ceramic blank;
(3) and sintering the ceramic blank at 1400-1600 ℃ for 0.5-4 h to obtain the zirconia ceramic with the pearlescent effect, wherein the flaky alumina is uniformly dispersed in the zirconia matrix.
2. The method for preparing a zirconia ceramic having a pearl effect according to claim 1, characterized in that: the zirconia is zirconia containing a stabilizer, the stabilizer comprises yttrium oxide, magnesium oxide, calcium oxide or cerium oxide, and the content of the stabilizer is 2.0-5.0 mol%.
3. The method for preparing a zirconia ceramic having a pearl effect according to claim 1, characterized in that: the average diameter-thickness ratio of the flaky alumina is 70-100.
4. The method for preparing a zirconia ceramic having a pearl effect according to claim 1, characterized in that: the dosage of the flaky alumina is 2.0-5.0 wt% of the zirconia powder.
5. The method for preparing a zirconia ceramic having a pearl effect according to claim 1, characterized in that: the dosage of the additive is 1.0-4.0 wt% of the total amount of the zirconia powder and the flaky alumina.
6. The method for preparing a zirconia ceramic having a pearl effect according to claim 1, characterized in that: and (3) the sintering temperature in the step (3) is 1450-1550 ℃.
7. A product obtained by the method for producing a zirconia ceramic having a pearl effect according to any one of claims 1 to 6.
8. The product obtained by the method for preparing zirconia ceramics with pearlescent effect according to claim 7 is characterized in that: the crystal form of the zirconia ceramic is a tetragonal phase or a mixed phase of the tetragonal phase and the cubic phase, and the three-point bending strength is more than or equal to 600 MPa.
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