Vacuum high wear-resistant zirconia-based composite ceramic material and preparation method and application thereof

By introducing whiskers into zirconia ceramics and performing vacuum carburizing treatment, a high wear-resistant zirconia-based composite ceramic material was prepared, which solved the problem of insufficient wear resistance of zirconia ceramics in a vacuum environment and realized the high-performance application of the material in the aerospace field.

CN119504277BActive Publication Date: 2026-04-28XI AN JIAOTONG UNIV
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Patent Information

Authority / Receiving Office
CN · China
Patent Type
Patents(China)
Current Assignee / Owner
XI AN JIAOTONG UNIV
Filing Date
2024-11-19
Publication Date
2026-04-28

AI Technical Summary

Technical Problem

Existing zirconia ceramics exhibit poor wear resistance in vacuum or high vacuum environments, failing to meet the long-life and reliable service requirements of high-end aerospace equipment.

Method used

A vacuum high-wear-resistant zirconia-based composite ceramic material was prepared by combining whisker toughening and vacuum carburizing techniques. The tribological properties were improved by introducing a toughening phase and infiltrating carbon atoms into the zirconia matrix.

Benefits of technology

It significantly improves the tribological properties of zirconia ceramics in a vacuum environment, reduces the wear rate and increases fracture toughness, making it suitable for high-end aerospace equipment.

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Abstract

The application discloses a kind of vacuum high wear-resistant zirconia-based composite ceramic materials and preparation method and application thereof, belong to ceramic material preparation technical field.Preparation method includes: 1) zirconia powder, stabilizer and anhydrous ethanol are mixed uniformly, and mixed slurry is prepared;2) crystal whisker is added to mixed slurry, is fully stirred uniformly, then dried, sieved, and mixed powder is prepared;3) mixed powder is formed by static pressure, and composite ceramic body is prepared, then vacuum sintering and annealing treatment are carried out, and composite ceramic is prepared;4) composite ceramic is treated by high-temperature carburizing, and carburizing composite ceramic is obtained, and vacuum high wear-resistant zirconia-based composite ceramic material is prepared by surface treatment.The zirconia-based composite ceramic material proposed in the application reduces the vacuum wear rate by 1-2 orders of magnitude compared with traditional yttria-stabilized zirconia material, and provides a new type of high-wear-resistant ceramic material for precision friction drive components in the field of aerospace.
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Description

Technical Field

[0001] This invention belongs to the field of ceramic material preparation technology, specifically relating to a vacuum high wear-resistant zirconia-based composite ceramic material, its preparation method, and its application. Background Technology

[0002] Zirconia (ZrO2) ceramics have attracted widespread attention due to their combination of advantages over traditional ceramic materials, including mechanical properties, high-temperature resistance, corrosion resistance, and insulation, as well as excellent fracture toughness. Currently, zirconia-based ceramics have been successfully used in biomedicine, aerospace, and electronic information fields as wear-resistant and corrosion-resistant materials, heat insulation / heat-resistant materials, and dielectric materials. With the rapid development of aerospace technology, higher demands are being placed on the service performance of wear-resistant materials under harsh conditions such as high vacuum and high loads. However, the wear resistance of self-adapted zirconia materials significantly degrades in vacuum or high vacuum, and their high wear rate cannot meet the requirements for reliable and long-life service of high-end aerospace equipment.

[0003] Research on zirconia mainly focuses on improving its toughness through the regulation of material composition and microstructure, but research on enhancing its vacuum / high vacuum wear resistance is limited. Studies have shown that introducing suitable whiskers can enhance the toughness and mechanical properties of zirconia ceramics, but its impact on the high vacuum tribological properties of zirconia remains to be explored. Carburizing is an effective method for controlling the surface properties of materials. Related studies indicate that after carburizing, carbon mainly exists in the interstitial spaces of zirconia in atomic form, which is beneficial for reducing its coefficient of friction. Patent applications CN1108229A ("A Carburizing Method for Oxide Ceramics") and CN103724051A ("Carburizing Method for Ceramic Sliding Materials") propose methods for carburizing oxide ceramics, but do not address the vacuum tribological properties of zirconia ceramics. Furthermore, a single carburizing treatment may lead to a decrease in the fracture toughness of zirconia ceramics, which is detrimental to improving its wear resistance.

[0004] In summary, the significant degradation of zirconia's wear resistance in vacuum or high-vacuum environments severely restricts its widespread application in the aerospace field. Therefore, proposing a vacuum-resistant high-wear-resistant zirconia-based ceramic material and its preparation method is of great significance for the long-life and reliable service of friction components in high-end aerospace equipment. Summary of the Invention

[0005] In order to overcome the shortcomings of the prior art, the present invention aims to provide a vacuum high wear-resistant zirconia-based composite ceramic material, its preparation method and application, so as to solve the technical problem that the single carburizing treatment in the prior art results in low fracture toughness and poor wear resistance of zirconia ceramics.

[0006] To achieve the above objectives, the present invention employs the following technical solution:

[0007] This invention discloses a method for preparing a vacuum high-wear-resistant zirconia-based composite ceramic material, comprising the following steps:

[0008] 1) Thoroughly mix zirconium oxide powder, stabilizer and anhydrous ethanol to obtain a mixed slurry;

[0009] 2) Add whiskers to the mixed slurry, stir thoroughly, then dry and sieve to obtain the mixed powder;

[0010] 3) The mixed powder is statically pressed to form a composite ceramic blank, which is then subjected to vacuum sintering and annealing to obtain the composite ceramic.

[0011] 4) The composite ceramic is subjected to high-temperature carburizing treatment to obtain carburized composite ceramic, and then surface treatment is performed to obtain vacuum high wear-resistant zirconia-based composite ceramic material.

[0012] Preferably, in step 1), the amount of stabilizer is 1.5% to 5% of the amount of zirconium oxide powder; the volume ratio of the total powder of zirconium oxide powder and stabilizer to anhydrous ethanol is 1 to 1.5:1.

[0013] Preferably, the stabilizer is one or more of yttrium oxide, magnesium oxide, and calcium oxide.

[0014] Preferably, high-purity zirconium oxide powder, stabilizer, and anhydrous ethanol are mixed and ball-milled, and then filtered to obtain a mixed slurry;

[0015] More preferably, the grinding jar and grinding balls used in the ball mill are both made of zirconium oxide, the ball milling speed is 150 r / min to 300 r / min, and the time is 6 h to 15 h.

[0016] Preferably, in step 2), the amount of whiskers accounts for 5% to 20% of the mass of the mixed slurry; the whiskers are one or more of silicon carbide, silicon nitride, aluminum oxide and magnesium oxide.

[0017] Preferably, the sieving in step 2) uses a 100-300 mesh sieve.

[0018] Preferably, in step 3), the static pressing pressure is 150 MPa to 300 MPa, and the holding time is 10 min to 30 min; the process parameters for vacuum sintering and annealing are: starting from room temperature, the temperature is increased to 1200℃ to 1500℃ at a rate of 3 to 10℃ / min, the holding time is 2 h to 10 h, and then the furnace is cooled to room temperature.

[0019] Preferably, in step 4), a vacuum carburizing furnace is used for high-temperature carburizing treatment. The process parameters for high-temperature carburizing treatment are as follows: the carburizing medium is one or more of methane, ethane, acetylene and ethylene, the temperature is increased from room temperature to 850 ℃ to 1450 ℃ at a temperature increase rate of 3~10 ℃ / min, the carburizing time is 8 h to 24 h, and the chamber pressure is 1~20 Kpa.

[0020] Preferably, in step 5), the surface treatment involves grinding and polishing with 600-mesh, 1200-mesh, 2000-mesh, and 3000-mesh sandpaper in sequence until the surface roughness is less than 0.1 μm.

[0021] The present invention also discloses a vacuum high wear-resistant zirconia-based composite ceramic material prepared by the above preparation method. The vacuum high wear-resistant zirconia-based composite ceramic material contains a carburized layer and has whiskers distributed as a toughening phase. The thickness of the carburized layer with a carbon content of more than 0.75% is greater than 10 μm. The length of the whiskers is 5 μm to 150 μm and the aspect ratio is greater than 5.

[0022] Preferably, the composite ceramic material contains 70 wt% to 90 wt% zirconium oxide, 5 wt% to 20 wt% reinforcing phase whiskers, and a stabilizer content of 2 mol% to 5 mol% of zirconium oxide.

[0023] Preferably, in a vacuum environment, the dry friction wear rate of this vacuum high wear-resistant zirconia-based composite ceramic material, whether self-paired or paired with zirconia, is 10. -7 ~10 -8 mm 3 On the order of N·m.

[0024] Preferably, the material surface has a uniform gray-black color.

[0025] This invention also discloses the application of the above-mentioned vacuum high wear-resistant zirconia-based composite ceramic material in the field of aerospace high-end equipment manufacturing.

[0026] Preferably, it is used to manufacture key components such as wear-resistant and friction-driven components;

[0027] More preferably, for example, in the manufacture of high-performance actuators.

[0028] Compared with the prior art, the present invention has the following beneficial effects:

[0029] This invention discloses a method for preparing vacuum-hardened high-wear-resistant zirconia-based composite ceramic materials. Toughened whiskers are introduced into a stable zirconia ceramic matrix, and vacuum carburizing technology is used to infiltrate carbon atoms with anti-wear properties into the ceramic surface. This synergistically improves the mechanical properties and vacuum self-lubricating properties of traditional zirconia ceramics, significantly enhancing the tribological properties of zirconia-based ceramics in a vacuum environment. This effectively solves the technical problem of low fracture toughness and poor wear resistance in zirconia ceramics caused by single carburizing treatment in existing technologies. Furthermore, this preparation method is easy to control in terms of component content, simple to operate, and has a high yield. The zirconia-based composite ceramic materials prepared by this invention have great application potential in high-end equipment in the aerospace field.

[0030] The zirconia composite ceramic material prepared by this invention exhibits certain self-lubricating properties in a vacuum environment, reducing the wear rate by 1-2 orders of magnitude compared to traditional yttrium oxide or magnesium oxide-stabilized zirconia ceramic materials, while lowering its dry friction coefficient by more than 20%. Therefore, it can be applied in the aerospace field, providing a novel high-wear-resistant composite ceramic material for high-end aerospace equipment components. Attached Figure Description

[0031] Figure 1 This is a schematic diagram of the structure of the vacuum high wear-resistant zirconia-based composite ceramic material disclosed in this invention;

[0032] Figure 2 These are physical images of Example 1 and Comparative Example 1;

[0033] Figure 3 The nano-hardness of Examples 1, 2, 3, Comparative Example 1, and Comparative Example 2 of the present invention;

[0034] Figure 4 The average wear rate of Embodiment 1, Comparative Example 1, and Comparative Example 2 in a vacuum environment is shown. Detailed Implementation

[0035] To enable those skilled in the art to better understand the present invention, the technical solutions of the present invention will be clearly and completely described below with reference to the accompanying drawings of the embodiments of the present invention. Obviously, the described embodiments are only some embodiments of the present invention, and not all embodiments. Based on the embodiments of the present invention, all other embodiments obtained by those skilled in the art without creative effort should fall within the scope of protection of the present invention.

[0036] It should be noted that the terms "first," "second," etc., in the specification, claims, and accompanying drawings of this invention are used to distinguish similar objects and are not necessarily used to describe a specific order or sequence. It should be understood that such data can be interchanged where appropriate so that the embodiments of the invention described herein can be implemented in orders other than those illustrated or described herein. Furthermore, the terms "comprising" and "having," and any variations thereof, are intended to cover a non-exclusive inclusion; for example, a process, method, system, product, or apparatus that comprises a series of steps or units is not necessarily limited to those steps or units explicitly listed, but may include other steps or units not explicitly listed or inherent to such processes, methods, products, or apparatus.

[0037] The present invention will now be described in further detail with reference to the accompanying drawings:

[0038] Example 1

[0039] In this embodiment, yttrium oxide is used as a stabilizer, silicon carbide whiskers, and vacuum carburizing to prepare zirconia-based composite ceramics, with the total mass of the powder (total mass of stabilizer, whiskers, zirconia, and binder) as the basis. The specific implementation includes the following steps:

[0040] 1) Yttrium oxide stabilized zirconia slurry

[0041] 80 wt% of zirconium oxide powder, yttrium oxide stabilizer, and anhydrous ethanol were added to a zirconium oxide ball mill jar. The amount of yttrium oxide added was 3 mol% of zirconium oxide, the volume ratio of anhydrous ethanol to powder was 1~1.5, the ball mill speed was 200 r / min, and the ball milling time was 10 h. The grinding balls were filtered out to obtain a mixed slurry.

[0042] 2) Preparation of composite powder

[0043] Add 10 wt% silicon carbide whiskers and 0.75 wt% binder (PVB) to the mixed slurry and mix for 90 min; then dry and sieve (200 mesh) the mixed slurry to obtain silicon carbide whisker reinforced zirconia composite powder;

[0044] 3) Composite ceramic blank

[0045] The composite powder was placed in a mold and held under static pressure of 300 MPa for 20 min to obtain a composite ceramic green body.

[0046] 4) Composite ceramic firing

[0047] The composite ceramic blank was placed in a vacuum sintering furnace, and the furnace temperature was increased to 1450 ℃ at a rate of 5 ℃ / min. After holding at this temperature for 2.5 h, it was naturally cooled to room temperature to obtain the composite ceramic.

[0048] 5) Carburizing

[0049] The composite ceramic was placed in a vacuum carburizing furnace and heated to 900 ℃ at a rate of 5 ℃ / min. Acetylene gas was introduced and the vacuum degree was 2 kPa. After maintaining the temperature for 20 h, it was naturally cooled to room temperature to obtain the carburized composite ceramic.

[0050] 6) Grinding and polishing treatment

[0051] The carburized composite ceramic was successively ground with 600-grit, 1200-grit, 2000-grit, and 3000-grit sandpaper to remove the surface carbon layer. Finally, it was polished until the surface roughness was less than 0.1 μm, thus completing the material preparation.

[0052] Example 2

[0053] In this embodiment, yttrium oxide is used as a stabilizer, silicon nitride whiskers, and vacuum carburizing to prepare zirconia-based composite ceramics, with the total mass of the powder as the basis. The specific implementation includes the following steps:

[0054] 1) Yttrium oxide stabilized zirconia slurry

[0055] 75 wt% zirconium oxide powder, yttrium oxide stabilizer, and anhydrous ethanol were added to a zirconium oxide ball mill jar. The amount of yttrium oxide added was 4 mol% of zirconium oxide, the volume ratio of anhydrous ethanol to powder was 1~1.5, the ball mill speed was 150 r / min, and the ball milling time was 12 h. The grinding balls were filtered out to obtain a mixed slurry.

[0056] 2) Preparation of composite powder

[0057] Add 12 wt% silicon nitride whiskers to the mixed slurry and mix for 120 min; then dry and sieve (200 mesh) the mixed slurry to obtain silicon nitride whisker reinforced zirconium oxide composite powder;

[0058] 3) Composite ceramic blank

[0059] The composite powder was placed in a mold and held under static pressure of 200 MPa for 25 min to obtain a composite ceramic green body; (the binder used for granulation was polyethylene glycol and polyvinyl alcohol).

[0060] 4) Composite ceramic firing

[0061] The composite ceramic blank was placed in a vacuum sintering furnace, and the furnace temperature was increased to 1400 ℃ at a rate of 5 ℃ / min. After holding at that temperature for 5 h, it was naturally cooled to room temperature to obtain the composite ceramic.

[0062] 5) Carburizing

[0063] The composite ceramic was placed in a vacuum carburizing furnace and heated to 900 ℃ at a rate of 5 ℃ / min. Methane gas was introduced and the vacuum degree was 3 kPa. After maintaining the temperature for 16 h, the temperature was naturally cooled to room temperature to obtain the carburized composite ceramic.

[0064] 6) Grinding and polishing treatment

[0065] The carburized composite ceramic was successively ground with 600-grit, 1200-grit, 2000-grit, and 3000-grit sandpaper to remove the surface carbon layer. Finally, it was polished until the surface roughness was less than 0.1 μm, thus completing the material preparation.

[0066] Example 3

[0067] In this embodiment, zirconia-based composite ceramics are prepared using magnesium oxide as a stabilizer, alumina whiskers, and vacuum carburizing, with the total mass of the powder as the basis. The specific implementation includes the following steps:

[0068] 1) Yttrium oxide stabilized zirconia slurry

[0069] 85 wt% of zirconium oxide powder, magnesium oxide stabilizer, and anhydrous ethanol were added to a zirconium oxide ball mill jar. The amount of magnesium oxide added was 3 mol% of zirconium oxide, the volume ratio of anhydrous ethanol to powder was 1~1.5, the ball mill speed was 200 r / min, and the ball milling time was 10 h. The grinding balls were filtered out to obtain a mixed slurry.

[0070] 2) Preparation of composite powder

[0071] Add 10 wt% alumina whiskers to the mixed slurry and mix for 90 min; then dry and sieve (200 mesh) the mixed slurry to obtain silicon carbide whisker reinforced zirconium oxide composite powder;

[0072] 3) Composite ceramic blank

[0073] The composite powder was placed in a mold and held under static pressure of 300 MPa for 20 min to obtain a composite ceramic green body.

[0074] 4) Composite ceramic firing

[0075] The composite ceramic blank was placed in a vacuum sintering furnace, and the furnace temperature was increased to 1450 ℃ at a rate of 5 ℃ / min. After holding at that temperature for 5 h, it was naturally cooled to room temperature to obtain the composite ceramic.

[0076] 5) Carburizing

[0077] The composite ceramic was placed in a vacuum carburizing furnace and heated to 950 ℃ at a rate of 5 ℃ / min. Ethylene gas was introduced and the vacuum degree was 1.5 KPa. After maintaining the temperature for 24 h, the temperature was naturally cooled to room temperature to obtain the carburized composite ceramic.

[0078] 6) Grinding and polishing treatment

[0079] The carburized composite ceramic was successively ground with 600-grit, 1200-grit, 2000-grit, and 3000-grit sandpaper to remove the surface carbon layer. Finally, it was polished until the surface roughness was less than 0.1 μm, thus completing the material preparation.

[0080] Comparative Example 1

[0081] The comparative example is yttrium oxide-stabilized zirconia ceramic, based on the total mass of the powder. Unlike the previous embodiments, whiskers were not added as a toughening phase, and carburizing treatment was not performed. The specific implementation includes the following steps:

[0082] 1) Yttrium oxide stabilized zirconia slurry

[0083] 80 wt% of zirconium oxide powder, yttrium oxide stabilizer, and anhydrous ethanol were added to a zirconium oxide ball mill jar. The amount of yttrium oxide added was 3 mol% of zirconium oxide, the volume ratio of anhydrous ethanol to powder was 1~1.5, the ball mill speed was 200 r / min, and the ball milling time was 10 h. The grinding balls were filtered out to obtain a mixed slurry.

[0084] 2) Powder preparation

[0085] Polyvinyl alcohol was added to the mixed slurry for granulation, drying, and sieving (200 mesh) to obtain yttrium oxide stabilized zirconia powder;

[0086] 3) Ceramic blank

[0087] The composite powder was placed in a mold and held under static pressure of 300 MPa for 20 min to obtain a zirconia ceramic green body.

[0088] 4) Ceramic firing

[0089] Zirconia ceramic blanks were placed in a vacuum sintering furnace, and the furnace temperature was increased to 1450 ℃ at a rate of 5 ℃ / min. After holding at this temperature for 2 h, the blanks were naturally cooled to room temperature to obtain yttrium-stabilized zirconia ceramics.

[0090] 5) Grinding and polishing treatment

[0091] Zirconia ceramics are ground and polished until the surface roughness is less than 0.1 μm, thus completing the material preparation.

[0092] Comparative Example 2

[0093] The comparative example is a silicon carbide whisker-toughened zirconia-based composite ceramic, with the total mass of the powder as the baseline. The specific implementation includes the following steps:

[0094] 1) Yttrium oxide stabilized zirconia slurry

[0095] 80 wt% of zirconium oxide powder, yttrium oxide stabilizer, and anhydrous ethanol were added to a zirconium oxide ball mill jar. The amount of yttrium oxide added was 3 mol% of zirconium oxide, the volume ratio of anhydrous ethanol to powder was 1~1.5, the ball mill speed was 200 r / min, and the ball milling time was 10 h. The grinding balls were filtered out to obtain a mixed slurry.

[0096] 2) Preparation of composite powder

[0097] Add 10 wt% silicon carbide whiskers and 0.75 wt% binder (PVB) to the mixed slurry and mix for 90 min; then dry and sieve (200 mesh) the mixed slurry to obtain silicon carbide whisker reinforced zirconia composite powder;

[0098] 3) Composite ceramic blank

[0099] The composite powder was placed in a mold and held under static pressure of 300 MPa for 20 min to obtain a composite ceramic green body.

[0100] 4) Composite ceramic firing

[0101] The composite ceramic blank was placed in a vacuum sintering furnace, and the furnace temperature was increased to 1450 ℃ at a rate of 5 ℃ / min. After holding at this temperature for 2.5 h, it was naturally cooled to room temperature to obtain the composite ceramic blank.

[0102] 5) Grinding and polishing treatment

[0103] The composite ceramic blank was successively ground with 600-grit, 1200-grit, 2000-grit, and 3000-grit sandpaper, and finally polished until the surface roughness was less than 0.1 μm, thus completing the material preparation.

[0104] Comparative Example 3

[0105] This comparative example is a carburized yttrium oxide-stabilized zirconia ceramic, based on the total mass of the powder. Unlike the previous embodiments, whiskers were not added as a toughening phase. The specific implementation includes the following steps:

[0106] 1) Yttrium oxide stabilized zirconia slurry

[0107] 80 wt% of zirconium oxide powder, yttrium oxide stabilizer, and anhydrous ethanol were added to a zirconium oxide ball mill jar. The amount of yttrium oxide added was 3 mol% of zirconium oxide, the volume ratio of anhydrous ethanol to powder was 1~1.5, the ball mill speed was 200 r / min, and the ball milling time was 10 h. The grinding balls were filtered out to obtain a mixed slurry.

[0108] 2) Powder preparation

[0109] Polyvinyl alcohol was added to the mixed slurry for granulation, drying, and sieving (200 mesh) to obtain yttrium oxide stabilized zirconia powder;

[0110] 3) Ceramic blank

[0111] Yttrium-stabilized zirconia was placed in a mold and held under a static pressure of 300 MPa for 20 min to obtain a yttrium-stabilized zirconia ceramic green body.

[0112] 4) Ceramic firing

[0113] Zirconia ceramic blanks were placed in a vacuum sintering furnace, and the furnace temperature was increased to 1450 ℃ at a rate of 5 ℃ / min. After holding at this temperature for 2 h, the blanks were naturally cooled to room temperature to obtain yttrium-stabilized zirconia ceramics.

[0114] 5) Carburizing

[0115] The composite ceramic was placed in a vacuum carburizing furnace and heated to 900 ℃ at a rate of 5 ℃ / min. Acetylene gas was introduced and the vacuum degree was 2 kPa. After maintaining the temperature for 20 h, it was naturally cooled to room temperature to obtain a carburized yttrium-stabilized zirconia ceramic blank.

[0116] 6) Grinding and polishing treatment

[0117] The carburized yttrium oxide stabilized zirconia ceramic was successively ground with 600-grit, 1200-grit, 2000-grit, and 3000-grit sandpaper to remove the surface carbon layer. Finally, it was polished until the surface roughness was less than 0.1 μm, thus completing the material preparation.

[0118] Figure 1 The diagram shows the structure of the vacuum high wear-resistant zirconia-based composite ceramic material of the present invention.

[0119] Figure 2 The images show a comparison of physical samples from Example 1, Comparative Example 1, Comparative Example 2, and Comparative Example 3. It can be seen that the composite ceramic material prepared by the method of the present invention is grayish-black, Comparative Example 1 and Comparative Example 2 are white, and Comparative Example 3 is dark grayish-black.

[0120] Figure 3 The fracture toughness test results of the ceramic materials prepared in the examples and comparative examples are shown. Vickers microhardness tester and optical microscopy were used, with a consistent test load of 49 N. The results show that the fracture toughness of Example 1, Comparative Example 1, Comparative Example 2, and Comparative Example 3 are 11.4 MPa·m. 1 / 2 10.6 MPa·m 1 / 2 11.75 MPa·m 1 / 2 and 7.85 MPa·m 1 / 2 As can be seen, Example 1 and Comparative Example 2 have similar high fracture toughness, while carburizing alone leads to a decrease in fracture toughness of about 20%-30%.

[0121] Figure 4 As shown, the average friction coefficient and wear rate are compared between the examples and comparative examples under the same pairings and test parameters. The results show that at 5 × 10⁻⁶... -4 Under Pa environment, zirconia pair (Ø6 mm), and 4 N normal load conditions, the wear rate in Example 1 was 3.0 × 10⁻⁶. -7 mm 3 / N·m, the average wear rate of Comparative Example 1 is 9.9×10 -6 mm 3 / N·m, the average wear rate of Comparative Example 2 is 8.45×10 -6 mm 3 / N·m, the average wear rate of Comparative Example 3 is 2.12×10 -6 mm 3 / N·m. The wear rate of Example 1 was approximately 1 / 33, 1 / 27, and 1 / 7 of that of Comparative Examples 1, 2, and 3, respectively, indicating that simple whisker toughening cannot significantly improve the wear resistance of zirconia ceramics in a vacuum, while Example 1 clearly has superior vacuum wear resistance.

[0122] In summary, the method disclosed in this invention utilizes a combination of whisker toughening and carburizing to prepare a zirconia-based composite ceramic material with excellent vacuum wear resistance. This material mainly consists of zirconia, a stabilizer, toughening whiskers, and a carburized layer to improve tribological properties. The stabilizer is one or more of yttrium oxide, magnesium oxide, and calcium oxide; the toughening whiskers are one or more of high-temperature resistant silicon carbide, silicon nitride, alumina, and magnesium oxide; and the carburized layer is formed using vacuum high-temperature carburizing treatment. This invention proposes that its vacuum wear resistance is 1-2 orders of magnitude higher than that of traditional yttrium oxide or magnesium oxide-stabilized zirconia materials, providing a novel high-wear-resistant composite ceramic material for high-end equipment components in the aerospace field.

[0123] The above content is only for illustrating the technical concept of the present invention and should not be construed as limiting the scope of protection of the present invention. Any modifications made to the technical solution based on the technical concept proposed in this invention shall fall within the scope of protection of the claims of this invention.

Claims

1. A method for preparing a vacuum high-wear-resistant zirconia-based composite ceramic material, characterized in that, Includes the following steps: 1) Mix zirconium oxide powder, stabilizer and anhydrous ethanol thoroughly to obtain a mixed slurry; the amount of stabilizer is 1.5% to 5% of the molar amount of zirconium oxide powder; the volume ratio of the total powder of zirconium oxide powder and stabilizer to anhydrous ethanol is 1 to 1.5:

1. 2) Add whiskers to the mixed slurry, stir thoroughly until homogeneous, then dry and sieve to obtain the mixed powder; the amount of whiskers should be 5% to 20% of the mass of the mixed slurry. 3) The mixed powder is statically pressed to form a composite ceramic blank, which is then subjected to vacuum sintering and annealing to obtain the composite ceramic. The static pressing pressure is 150 MPa~300 MPa, and the holding time is 10 min~30 min. The process parameters for vacuum sintering and annealing are: starting from room temperature, the temperature is increased to 1200 ℃-1500 ℃ at a temperature increase rate of 3~10 ℃ / min, and the holding time is 2h~10 h, and then the temperature is cooled to room temperature in the furnace. 4) The composite ceramic is subjected to high-temperature carburizing treatment to obtain carburized composite ceramic, followed by surface treatment to obtain a vacuum high-wear-resistant zirconia-based composite ceramic material. In a vacuum environment, the dry friction wear rate of this vacuum high-wear-resistant zirconia-based composite ceramic material, whether self-paired or paired with zirconia, is 10. -7 ~10 -8 mm 3 On the order of N·m.

2. The method for preparing vacuum high wear-resistant zirconia-based composite ceramic material according to claim 1, characterized in that, The stabilizer is one or more of yttrium oxide, magnesium oxide and calcium oxide.

3. The method for preparing vacuum high wear-resistant zirconia-based composite ceramic material according to claim 1, characterized in that, In step 2), the whiskers are one or more of silicon carbide, silicon nitride, aluminum oxide and magnesium oxide.

4. The method for preparing vacuum high wear-resistant zirconia-based composite ceramic material according to claim 1, characterized in that, In step 4), the process parameters for high-temperature carburizing are as follows: the carburizing medium is one or more of methane, ethane, acetylene and ethylene, the temperature is increased from room temperature to 850 ℃~1450 ℃ at a rate of 3~10 ℃ / min, the carburizing time is 8 h~24 h, and the chamber pressure is 1~20 KPa.

5. The method for preparing vacuum high wear-resistant zirconia-based composite ceramic material according to claim 1, characterized in that, In step 4), the surface is treated by grinding and polishing with 600-grit, 1200-grit, 2000-grit and 3000-grit sandpaper in sequence until the surface roughness is less than 0.1 μm.

6. A vacuum high-wear-resistant zirconia-based composite ceramic material prepared by the preparation method according to any one of claims 1 to 5, characterized in that, This vacuum high wear-resistant zirconia-based composite ceramic material contains a carburized layer and whiskers distributed as a toughening phase.

7. The vacuum high-wear-resistant zirconia-based composite ceramic material according to claim 6, characterized in that, The thickness of the carburized layer with a carbon content higher than 0.75% is greater than 10 μm; the length of the whiskers is 5 μm to 150 μm, and the aspect ratio is greater than 5. In a vacuum environment, the dry friction wear rate of this high-wear-resistant zirconia-based composite ceramic material, whether self-paired or paired with zirconia, is 10. -7 ~10 -8 mm 3 On the order of N·m.

8. The application of the vacuum high wear-resistant zirconia-based composite ceramic material as described in claim 6 or 7 in the field of aerospace high-end equipment manufacturing.

Citation Information

Patent Citations

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