CN112573918A - Zirconia ceramic - Google Patents
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- C04B35/48—Shaped ceramic products characterised by their composition; Ceramics compositions; Processing powders of inorganic compounds preparatory to the manufacturing of ceramic products based on oxide ceramics based on zirconium or hafnium oxides, zirconates, zircon or hafnates
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Abstract
The invention discloses zirconia ceramics. The zirconia ceramic comprises a toughening agent and a stabilizing agent, wherein the toughening agent is transition metal oxide, the content of the toughening agent in the zirconia ceramic is 0.05-20 wt%, and the stabilizing agent is Y2O3And Y in the zirconia ceramic2O3The content of (B) is 3.1-7 wt%; tetragonal zirconia with a core-shell structure exists in the zirconia ceramic, and Y at the center of the tetragonal zirconia crystal with the core-shell structure2O3The content is lower than that of Y far from the central part2O3And (4) content. According to the invention, a proper amount of transition metal oxide is added into the zirconia ceramic material, so that the impact resistance of the material is greatly improved, the falling ball impact height of the prepared zirconia ceramic is improved to more than 20cm from the existing 15cm below, and the requirement of meeting the requirement of the zirconia ceramic is metThe use requirement of the outer packaging component of the existing portable electronic equipment.
Description
Technical Field
The invention relates to the field of zirconia ceramics, in particular to zirconia ceramics for an outer packaging component of portable electronic equipment.
Background
Zirconium dioxide has excellent mechanical, thermal and electrical properties, and thus has wide applications in structural materials, optical materials, oxygen sensors and fuel cells. In recent years, zirconia ceramics have become a new favorite material in the fields of decoration, electronic products and the like due to the characteristics of high refractive index, high hardness, scratch resistance, soft hand feeling like jade and the like. Ceramic materials, however, are generally more brittle than metals and plastics, resulting in poor impact and drop resistance. In particular, the outer packaging member of portable electronic devices represented by smart phones, smart wearing, and the like has a higher requirement for the impact resistance of the material, and this is also a direction of continuous improvement in the industry.
The impact resistance of the common zirconia ceramics corresponds to the falling ball impact height test method in the patent, and is generally below 15 cm. When the common zirconia ceramics are used for manufacturing outer packing components of portable electronic equipment such as mobile phones and intelligent wearable devices, the thickness needs to be more than 0.7mm, so that the shock resistance can meet the requirement, but the weight of the whole equipment is overlarge. The thickness requirement of the outer packaging part of the portable electronic equipment is generally below 0.4mm at present, which requires that the impact resistance of the zirconia ceramic used is at least doubled to meet the requirement of the impact resistance.
At present, the industry has many researches on modifying zirconia ceramics by doping, but most zirconia ceramics are improved little for obtaining zirconia ceramics with specific colors or simply reducing the sintering temperature of the ceramics. In the aspect of improving the impact resistance of the zirconia ceramic, the existing methods have two types: (1) by reducing the stabilizer (usually Y) in the zirconia ceramic2O3) The content of (a) to improve the phase-changeability of zirconia, thereby achieving an improvement in impact resistance; (2) by introducing the oxide whiskers, impact energy is dissipated through crack deflection and a whisker pulling-out mechanism when the zirconia ceramic is fractured, so that the impact resistance of the zirconia ceramic is improved. Although the impact resistance of the zirconia ceramic can be improved to some extent by reducing the content of the stabilizer, the method can also lead to the low-temperature aging resistance of the materialThe temperature drops sharply, which is not favorable for long-term use. In addition, the method for improving the impact resistance of the zirconia ceramic by introducing oxide whiskers as in CN206551610U, and Al thereof2O3The preparation process of the crystal whisker is complex, has higher cost and is not beneficial to mass production.
Disclosure of Invention
The invention aims to overcome the defects of the prior art and provide the zirconia ceramic with high impact resistance.
In order to achieve the purpose, the technical scheme adopted by the invention is as follows:
the zirconia ceramic comprises a toughening agent and a stabilizing agent, wherein the toughening agent is transition metal oxide, the content of the toughening agent in the zirconia ceramic is 0.05-20 wt%, and the stabilizing agent is Y2O3And Y in the zirconia ceramic2O3The content of (B) is 3.1-7 wt%; tetragonal zirconia with a core-shell structure exists in the zirconia ceramic, and Y at the center of the tetragonal zirconia crystal with the core-shell structure2O3The content is lower than that of Y far from the central part2O3And (4) content.
In the present invention, the transition metal oxide does not include Y2O3。
In zirconia ceramics, Y is usually added2O3As a stabilizer, the tetragonal zirconia is mainly stabilized to room temperature in the sintering and cooling process. Under the action of external stress, the tetragonal zirconia can improve the impact resistance of zirconia ceramic through phase change toughening, but only adding Y2O3In a zirconia ceramic matrix under the condition of (1)2O3The distribution is more uniform, and the phase change toughening effect which can be exerted is limited.
The experiment of the invention finds that the impact resistance of the zirconia ceramic can be further improved by adding the transition metal oxide into the zirconia ceramic material. The transition metal oxide distributed in the grain boundary can induce the stabilizer Y in the sintering densification process2O3Diffusing and enriching to grain boundary, and finallyTetragonal zirconia to form Y2O3The core-shell structure of (2) is shown in FIG. 1. In such a core-shell structure, tetragonal zirconia in the central portion has a lower Y2O3The content and the phase change trend are strong, and the phase change toughening effect can be fully exerted; while tetragonal zirconia away from the central portion has a higher Y2O3The content can effectively prevent the tetragonal zirconia in the central part from losing the phase change toughening effect due to the transformation into the monoclinic phase in the sintering and cooling processes, so the Y-containing zirconia has the above Y2O3The impact resistance of the zirconia ceramic with the core-shell structure is greatly improved.
In the technical scheme of the invention, Y is used2O3As stabilizers, mainly tetragonal zirconia remains in the tetragonal phase at room temperature, Y2O3The amount added is generally from 3.1 to 7% by weight. Y is2O3The content is too high, so that the tetragonal phase is too stable, and even the cubic phase appears, thereby reducing the phase change toughening effect; if Y is2O3The content is too low, the stability of tetragonal phase is too poor, and the low-temperature aging phenomenon of zirconia is aggravated.
Furthermore, the test results show that the content of the transition metal oxide in the zirconia ceramic should be controlled to be 0.05 to 20 wt%. When the content of the transition metal oxide is less than 0.05 wt%, the toughening effect of the toughening agent is not obvious, the effect of improving the impact resistance of the zirconia ceramic is not obvious, and when the content of the transition metal oxide is more than 20 wt%, the sintering performance of the zirconia is reduced, meanwhile, the content of tetragonal zirconia is reduced, and the impact resistance is reduced on the contrary.
Under the condition of the same content of the transition group metal oxide, the impact resistance of the zirconium oxide ceramic is improved differently by different types of transition group metal oxides, and preferably, the cation radius of the transition group metal oxide is smaller than that of Zr4+The radius of the ions, the transition metal oxide is more preferably at least one of oxides of Cu, Mn, Fe, Co and Ni, and is more beneficial to improving the impact resistance of the zirconia ceramic.
In the present invention, the transition metal oxide may be introduced in at least one of a metal salt, an oxide and a composite oxide. The metal salt may be at least one in the form of nitrate, carbonate, sulfate, etc., which is decomposed and oxidized into an oxide during sintering.
Preferably, the content of the toughening agent in the zirconia ceramic is 0.15-15 wt%, and the effect of improving the impact resistance of the zirconia ceramic is the best.
The invention also provides application of the zirconia ceramic in an outer packaging component of portable electronic equipment. The zirconia ceramic prepared by the invention has high impact resistance, and the falling ball impact height of the zirconia ceramic is improved to more than 20cm from the existing 15cm below according to the testing method of the invention, thereby meeting the use requirements of the external packaging component of the existing portable electronic equipment.
The invention also provides application of the transition metal oxide in improving the shock resistance of zirconia ceramics, wherein the zirconia ceramics comprise the transition metal oxide and a stabilizer, the content of the transition metal oxide in the zirconia ceramics is 0.05-20 wt%, and the stabilizer is Y2O3And Y in the zirconia ceramic2O3The content of (B) is 3.1-7 wt%; tetragonal zirconia with a core-shell structure exists in the zirconia ceramic, and Y at the center of the tetragonal zirconia crystal with the core-shell structure2O3The content is lower than that of Y far from the central part2O3And (4) content.
Transition metal oxides in the existing zirconia ceramics generally reduce the crystal size after sintering by reducing the growth of crystal interface, thereby achieving the purpose of reducing the cracking problem caused by phase change, or are used as color pigments or sintering aids to reduce the sintering temperature and reduce the grain size. The research of the invention finds that the transition metal oxide is stabilized by inducing the stabilizing agent Y2O3Diffusion and enrichment are carried out to the grain boundary, so that part of tetragonal zirconia in the final zirconia ceramic forms Y2O3In which the tetragonal zirconia in the central portion has a lower Y2O3Content and phase change towardsThe potential is strong, and the effect of phase change toughening can be fully exerted; while tetragonal zirconia away from the central portion has a higher Y2O3The content can effectively prevent the tetragonal zirconia in the central part from losing the phase change toughening effect due to the transformation into the monoclinic phase in the sintering and cooling processes.
Preferably, in the above application, the cation radius of the transition group metal oxide is smaller than Zr4+The radius of the ion.
Preferably, in the above application, the transition metal oxide is at least one of oxides of Cu, Mn, Fe, Co, Ni.
Preferably, in the above application, the content of the transition metal oxide in the zirconia ceramic is 0.15 to 15 wt%, which can further improve the impact resistance of the zirconia ceramic.
Compared with the prior art, the invention has the beneficial effects that:
according to the invention, the transition metal oxide is added into the zirconia ceramic material, so that the impact resistance of the material is greatly improved, the falling ball impact height of the prepared zirconia ceramic is improved to more than 20cm from the existing 15cm, and the use requirement of the external packaging component of the existing portable electronic equipment is met.
Compared with the traditional oxide whisker toughened zirconia ceramic, the zirconia ceramic of the invention can achieve the purpose of improving the shock resistance only by adding a small amount of transition metal oxide, has low cost and simple preparation method, and can be suitable for industrialized batch production.
Drawings
Fig. 1 shows an HAADF image (a) and a Y-element distribution diagram (b) of the zirconia ceramic prepared in example 1, the original image of the Y-element distribution diagram being a color image.
Detailed Description
To better illustrate the objects, aspects and advantages of the present invention, the present invention will be further described with reference to specific examples. It will be understood by those skilled in the art that the specific embodiments described herein are merely illustrative of the invention and are not intended to limit the invention.
The zirconia ceramics of examples and comparative examples were prepared by the following method: introducing a transition metal oxide into a zirconia ceramic material, carrying out ball milling, slurry mixing to obtain slurry, carrying out spray granulation to obtain granulated materials, forming and sintering the granulated materials to obtain a sintered body, and carrying out subsequent machining on the sintered body to obtain the zirconia ceramic. The kinds of transition metal oxides, specific contents thereof, and contents of stabilizers in the zirconia ceramics of examples and comparative examples are shown in table 1.
The zirconia ceramics of the above examples and comparative examples were subjected to an impact resistance test by the following method:
processing the zirconia ceramic sintered body into a thin square piece with the thickness of 55mm x 0.4mm, polishing two sides, placing on an acrylic clamp, and hollowing out the middle of the sample with the thickness of 55mm x 55 mm; then, a steel ball with the weight of 32g is freely dropped to hit the center point of the sample, the initial height of the steel ball is 15cm, the steel ball is lifted by 5cm each time until the sample is damaged, at least 20 samples are tested, and the average falling ball impact height is counted.
The results are shown in Table 1.
TABLE 1
From the results shown in table 1, it can be seen that when the content of the transition metal oxide is less than 0.05 wt%, the toughening effect of the toughening agent is not significant, and the impact resistance is not significantly improved, and when the content of the transition metal oxide is more than 20 wt%, the sintering property of zirconia is reduced, and at the same time, the tetragonal zirconia content is reduced, and the impact resistance is rather reduced, so that in order to ensure that the zirconia ceramic has high impact resistance and meet the use requirement of the external packaging component of the existing portable electronic device, the content of the transition metal oxide in the zirconia ceramic in the present invention should be controlled to be 0.05-20 wt%, preferably 0.15-15 wt%. In addition, under the condition of the same content of the toughening agent, the impact resistance of the zirconia ceramic is improved differently by different types of transition metal oxides, preferably the transition metal oxidesMnO、Fe2O3At least one of NiO, CuO and CoO, and the prepared zirconia ceramic has better impact resistance.
As is clear from the results of comparative examples 3 to 4, example 20 and examples 30 to 31, Y2O3The content affects the impact resistance of the zirconia ceramic. Using more than 7 wt% of Y2O3When the content is higher than the content, the tetragonal phase of the zirconia ceramic is too stable, and even a cubic phase appears, so that the phase change toughening effect is reduced, and the impact resistance is obviously reduced. Using less than 3.1 wt% of Y2O3When the content is higher, the stability of the tetragonal phase of the zirconia ceramic is too poor, the content of the monoclinic phase is higher, the phase change toughening effect is reduced, and the impact strength is reduced. Adopting 3.1-7 wt% of Y2O3At this content, the zirconia ceramics have the best impact resistance. Therefore, the present invention preferably employs 3.1 to 7 wt% of Y2O3And (4) content.
The HAADF image (a) and the Y element distribution map (b) of the zirconia ceramic of example 1 are shown in FIG. 1, and Y in the zirconia ceramic prepared by the present invention2O3Enriched at the grain boundary to finally form Y2O3Has a core-shell structure, the tetragonal zirconia in the central part of the crystal has a lower Y2O3The content and the phase change trend are strong, and the phase change toughening effect can be fully exerted; while tetragonal zirconia away from the central portion has a higher Y2O3The content can effectively prevent the tetragonal zirconia in the central part from losing the phase change toughening effect due to the transformation into the monoclinic phase in the sintering and cooling processes.
Finally, it should be noted that the above embodiments are only used for illustrating the technical solutions of the present invention and not for limiting the protection scope of the present invention, and although the present invention is described in detail with reference to the preferred embodiments, it should be understood by those skilled in the art that modifications or equivalent substitutions can be made on the technical solutions of the present invention without departing from the spirit and scope of the technical solutions of the present invention.
Claims (9)
1. The zirconia ceramic is characterized by being prepared from zirconia ceramicThe porcelain comprises a toughening agent and a stabilizing agent, wherein the toughening agent is transition metal oxide, the content of the toughening agent in the zirconia ceramic is 0.05-20 wt%, and the stabilizing agent is Y2O3And Y in the zirconia ceramic2O3The content of (B) is 3.1-7 wt%; tetragonal zirconia with a core-shell structure exists in the zirconia ceramic, and Y at the center of the tetragonal zirconia crystal with the core-shell structure2O3The content is lower than that of Y far from the central part2O3And (4) content.
2. The zirconia ceramic of claim 1 wherein the cation radius of the transition group metal oxide is less than Zr4+The radius of the ion.
3. The zirconia ceramic of claim 1 or 2 wherein the transition group metal oxide is at least one of Cu, Mn, Fe, Co, Ni oxides.
4. The zirconia ceramic of claim 3 wherein the amount of toughening agent in the zirconia ceramic is from 0.15 to 15 wt%.
5. Use of the zirconia ceramic of any one of claims 1 to 4 in an outer packaging component for a portable electronic device.
6. The application of the transition metal oxide in improving the shock resistance of the zirconia ceramic is characterized in that the zirconia ceramic comprises the transition metal oxide and a stabilizer, wherein the content of the transition metal oxide in the zirconia ceramic is 0.05-20 wt%, and the stabilizer is Y2O3And Y in the zirconia ceramic2O3The content of (B) is 3.1-7 wt%; tetragonal zirconia with a core-shell structure exists in the zirconia ceramic, and Y at the center of the tetragonal zirconia crystal with the core-shell structure2O3The content is lower than that of Y far from the central part2O3And (4) content.
7. Use according to claim 6, wherein the transition group metal oxide has a cation radius of less than Zr4+The radius of the ion.
8. Use according to claim 6 or 7, wherein the transition group metal oxide is at least one of the oxides of Cu, Mn, Fe, Co, Ni.
9. Use according to claim 8, wherein the zirconia ceramic has a content of transition metal oxides of 0.15 to 15 wt%.
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Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN113788674A (en) * | 2021-08-30 | 2021-12-14 | 潮州三环（集团）股份有限公司 | Conductive ceramic and preparation method thereof |
| CN117945747A (en) * | 2022-10-19 | 2024-04-30 | 比亚迪股份有限公司 | Zirconia composite ceramic and preparation method and application thereof |
Citations (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN105669191A (en) * | 2016-04-22 | 2016-06-15 | 潮州三环（集团）股份有限公司 | Black zirconia ceramic and preparation method thereof |
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Patent Citations (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN105669191A (en) * | 2016-04-22 | 2016-06-15 | 潮州三环（集团）股份有限公司 | Black zirconia ceramic and preparation method thereof |
Non-Patent Citations (1)
| Title |
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| 王迎军主编: "《新型材料科学与技术 无机材料卷 下》", 31 October 2016, 华南理工大学出版社 * |
Cited By (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN113788674A (en) * | 2021-08-30 | 2021-12-14 | 潮州三环（集团）股份有限公司 | Conductive ceramic and preparation method thereof |
| CN113788674B (en) * | 2021-08-30 | 2022-05-13 | 潮州三环（集团）股份有限公司 | Conductive ceramic and preparation method thereof |
| CN117945747A (en) * | 2022-10-19 | 2024-04-30 | 比亚迪股份有限公司 | Zirconia composite ceramic and preparation method and application thereof |
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