A method for preparing a zirconium-niobium alloy ceramic composite

Abstract

The present application relates to the technical field of ceramic materials, in particular to a preparation method of zirconium-niobium alloy ceramic composite material. The present application first carries out surface pretreatment on the zirconium-niobium alloy, which is conducive to the growth of zirconium-based ceramics on the surface of the zirconium-niobium alloy. In the gas washing process, inert gas is introduced to remove impurity gases such as nitrogen, carbon dioxide and hydrogen in the furnace cavity, so that the atmosphere in the furnace cavity is clean and pollution-free, and the generation of other zirconium-based intermetallic compounds in the subsequent heating process is reduced. After completing the gas washing process, an oxygen-containing atmosphere is filled to ensure that the gas pressure in the furnace cavity is greater than the atmospheric pressure, so that the oxygen-containing atmosphere in the furnace cavity is sufficient, and the stability and reliability of the zirconium-based oxide ceramic generation are increased. The technical method of the present application is simple, low in cost and high in processing efficiency. The prepared zirconium-niobium alloy ceramic composite material has a hard surface texture, is resistant to wear and corrosion, and can be implanted in the human body for a long time.

Description

TECHNICAL FIELD

[0001] The application relates to the technical field of ceramic materials, in particular to a preparation method of a zirconium-niobium alloy ceramic composite material. BACKGROUND

[0002] Zirconium Zr and Zr alloys are widely used in the nuclear industry due to the small thermal neutron absorption cross section, only 1.8*10 -28 m 2 , high specific strength, excellent corrosion resistance, radiation resistance, low-temperature toughness and other characteristics, and are known as the "first metal in the atomic era", and play an irreplaceable role in the nuclear industry. With the continuous research and development of Zr and Zr alloys by domestic and foreign scholars, the development and application of Zr alloys gradually shift to the biomedical field. Zr alloys have the characteristics of non-toxicity, excellent biocompatibility, low density, etc. Zr-Nb zirconium-niobium alloys have high strength and excellent corrosion resistance, and the alloying element Nb belongs to the "biocompatible metal". In the in vivo animal experiment, the Zr implant shows good bone bonding, and even has a higher contact degree than the Ti alloy implant at the joint interface, which has great application potential as a biomedical implant material.

[0003] However, during the preparation of the Zr-Nb zirconium-niobium alloy, impurity gases such as nitrogen, carbon dioxide and rare gases in the furnace cavity will contaminate the atmosphere in the furnace cavity, affecting the safety and reliability of the process. The prepared zirconium-niobium alloy ceramic composite material contains other impurities, and has uneven texture, low hardness and poor surface performance.

[0004] In order to solve the above problems and make the zirconium-niobium alloy ceramic composite material more stable, dense and uniform, the application provides a preparation method of a zirconium-niobium alloy ceramic composite material. SUMMARY

[0005] The purpose of the application is to provide a preparation method of a zirconium-niobium alloy ceramic composite material to solve the problems in the background art.

[0006] In order to solve the above technical problems, the application provides the following technical scheme:

[0007] A preparation method of a zirconium-niobium alloy ceramic composite material, comprising the following steps:

[0008] S1: surface pretreatment of the zirconium-niobium alloy sample:

[0009] Take the zirconium-niobium alloy, rough turning, fine turning, polishing and polishing, and clean and dry to obtain the pretreated zirconium-niobium alloy;

[0010] S2: preparation of a zirconia ceramic layer:

[0011] The inert gas is washed in the furnace cavity, and then the oxygen-containing atmosphere is introduced, the gas pressure in the furnace cavity is controlled to be higher than the atmospheric pressure, the temperature is raised to 650-750 DEG C, the first stage of heat preservation is carried out, the oxygen-containing atmosphere is stopped, the gas pressure in the furnace cavity is controlled to be lower than the atmospheric pressure, the second stage of heat preservation is carried out, and the zirconium-niobium alloy ceramic composite blank is obtained by cooling.

[0012] S3: the surface post-treatment is carried out on the zirconium-niobium alloy ceramic composite blank:

[0013] The zirconium-niobium alloy ceramic composite blank is polished and polished, washed and dried, and the zirconium-niobium alloy ceramic composite material is prepared.

[0014] More preferably, the oxygen-containing atmosphere is oxygen-argon mixed gas, the flow rate of the oxygen-containing atmosphere is 1-3 L / min, and after the oxygen-containing atmosphere is introduced, the oxygen content in the furnace cavity is 20% oxygen partial pressure.

[0015] More preferably, during the first stage of heat preservation, the heat preservation time is 90-120 min; at this time, the gas pressure in the furnace cavity is higher than the atmospheric pressure, and the gas pressure in the furnace cavity is 0.005-0.01 MPa.

[0016] More preferably, during the second stage of heat preservation, the heat preservation time is 90-120 min; at this time, the gas pressure in the furnace cavity is less than the atmospheric pressure, and the gas pressure in the furnace cavity is (-0.03)-(-0.02) MPa.

[0017] More preferably, the washing step is specifically: argon is introduced, the argon fills the furnace cavity, when the gas pressure in the furnace cavity is 0.05 MPa, the introduction is stopped, the vacuum is extracted to-0.1 MPa, and the washing is repeated several times to complete the washing.

[0018] More preferably, the zirconium-niobium alloy is Zr-xNb, χ=0.5 or 1 or 2.5.

[0019] More preferably, during the heating process, the heating rate is 5-10 DEG C / min.

[0020] More preferably, the roughness of the zirconium-niobium alloy after the pretreatment in S1 is 0.02 μm; in S3, the surface roughness of the zirconium-niobium alloy ceramic composite material is 0.02 μm.

[0021] More preferably, in S1 and S3, the W2.5-8000 mesh polishing paste is used during polishing.

[0022] Compared with the prior art, the beneficial effects achieved by the present application are:

[0023] (1) The present application first carries out surface pretreatment on the Zr-xNb alloy, which is conducive to the growth of zirconium-based ceramics on the surface of the zirconium-niobium alloy, so that the zirconium-niobium alloy ceramic composite material is more stable, dense and uniform. The present application relates to a process suitable for Zr-xNb alloy, wherein x=0.5, 1, 2.5.

[0024] During the gas washing process, nitrogen is introduced to remove impurity gases such as nitrogen, carbon dioxide and rare gases in the furnace chamber, so that the atmosphere in the furnace chamber is clean and pollution-free, and the generation of other zirconium-based intermetallic compounds during the subsequent heating process is reduced.

[0025] After the gas washing process is completed, the furnace chamber is in a low vacuum environment. At this time, an oxygen-containing atmosphere is filled, and the air inlet valve and the air outlet valve are controlled so that the air inlet amount of the air inlet valve is greater than the air exhaust amount of the air outlet valve, so that the air pressure in the furnace chamber is greater than the atmospheric pressure, and the air pressure gauge reading is maintained at 0.005-0.01 MPa, so that the oxygen-containing atmosphere in the furnace chamber is supplied sufficiently, and the stability and reliability of the zirconium-based oxide ceramic generation are increased.

[0026] Since the zirconium-niobium alloy has the property of absorbing oxygen, it is easy to react with oxygen at high temperature. The pressurized oxygen supply process can ensure sufficient oxygen supply in the furnace chamber. The heating process is carried out in an atmosphere with an oxygen content of 20-25% oxygen partial pressure. The oxygen-containing atmosphere is introduced before the heating starts, and the flow rate of the atmosphere is 1-3 L / min, and the heating starts at the same time. The heating rate is 5-10℃ / min, and the temperature is raised to the highest temperature and held for 90-120 minutes. After the first stage of holding, the oxygen-containing atmosphere is stopped. The heating rate of the first stage of holding is set to 5-10℃ / min, and the heating temperature is set to 650-750℃. At this time, the temperature span range is relatively narrow, and this temperature interval is suitable for the nucleation and growth of zirconium-based oxide ceramics, which is conducive to the growth of the surface ceramic layer.

[0027] After the first stage of holding is completed, the furnace chamber is closed and the air pressure in the furnace chamber is reduced to less than atmospheric pressure, which improves the safety and stability of the process technology at high temperature.

[0028] During the preparation of the zirconium-niobium alloy sample, there is a holding process without oxygen-containing atmosphere in the preparation of the surface zirconia ceramic, which is conducive to the stability of the zirconium-based oxide ceramic, and the zirconium-niobium alloy ceramic composite material is further stabilized, densified and homogenized.

[0029] During the preparation of the zirconium-niobium alloy ceramic composite material, only oxygen element is introduced and zirconia is formed, and there is no other element harmful to human body, and the material has good biocompatibility.

[0030] The priority exhaust valve re-closes the intake valve, and then the furnace cavity is controlled at an air pressure of -0.02 to -0.03 MPa by using a vacuum pump, which ensures that the atmosphere in the furnace cavity is not polluted, and the safe and stable operation of the equipment in a high-temperature environment is ensured by reducing the air pressure in the closed furnace cavity, thereby avoiding the rupture of the furnace cavity caused by the expansion of the gas heated.

[0031] The surface post-treatment of the material improves the surface finish, so that the zirconium-niobium alloy ceramic composite material has more excellent surface performance after being made into an implant product.

[0032] In the heat preservation process, the zirconium-niobium alloy is oxidized with the oxygen-containing atmosphere in the furnace cavity to generate zirconium-based oxide ceramic on the surface of the zirconium-niobium alloy, and the two form a zirconium-niobium alloy ceramic composite material together.

[0033] (2) The technical method is simple, low in cost and high in processing efficiency. The zirconium-niobium alloy ceramic composite material prepared has a hard and wear-resistant surface and is corrosion-resistant. The zirconium element, niobium element and zirconium-based oxide ceramic ZrO2 in the zirconium-niobium alloy are all bio-friendly materials, have good bio-affinity, and are suitable for being used as the material of artificial joints or other human implant products. Compared with other technologies, the technology involved in the present application has a cleaner preparation environment, a safer and more reliable process, no other impurities in the zirconium-niobium alloy ceramic composite material prepared, and the material is uniform and dense, wear-resistant and corrosion-resistant. Compared with the zirconium alloy, the surface performance of the zirconium-niobium alloy ceramic composite material is greatly improved, and the material can be implanted in the human body for a long time. BRIEF DESCRIPTION OF DRAWINGS

[0034] The accompanying drawings are included to provide a further understanding of the present application, and constitute a part of the specification, illustrate the present application together with the embodiments thereof, and explain the present application, but do not limit the present application. In the drawings:

[0035] Figure 1 is a cross-sectional view of a zirconium-niobium alloy ceramic composite blank of Example 1 of the present application;

[0036] Figure 2 is a sample image of a zirconium-niobium alloy ceramic composite material of Example 1 of the present application;

[0037] Figure 3 is a cross-sectional element distribution diagram of a zirconium-niobium alloy ceramic composite blank of Example 2 of the present application. DETAILED DESCRIPTION

[0038] The technical solutions in the embodiments of the present application will be clearly and completely described below. Obviously, the described embodiments are only part of the embodiments of the present application, rather than all the embodiments. Based on the embodiments in the present application, all other embodiments obtained by those of ordinary skill in the art without creative work fall within the protection scope of the present application.

[0039] Embodiment 1

[0040] S1: surface pre-treatment of the zirconium-niobium alloy sample:

[0041] The Zr-0.5Nb alloy was selected as the base material, and the Zr-0.5Nb alloy sample was subjected to surface pre-treatment.

[0042] The Zr-0.5Nb alloy was processed into a circular sheet of by rough turning and finish turning processes, and was polished on a polishing disc using 100#, 300#, 800#, 1500# and 3000# water sandpaper, and W2.5-8000 mesh polishing paste, until the surface roughness Ra was 0.02 μm. Ultrasonic cleaning was performed in acetone solution and anhydrous ethanol solution for 15 min, respectively, and the surface was air-dried after cleaning to obtain the pre-treated zirconium-niobium alloy.

[0043] S2: preparation of the zirconia ceramic layer:

[0044] The furnace cavity was subjected to three gas washing treatments, and inert gas argon was introduced to fill the furnace cavity. When the gas pressure gauge reading was 0.05 MPa, the argon valve was closed, and the furnace cavity was pumped to a vacuum degree of -0.1 MPa. This step was repeated three times. After the gas washing treatment was completed, the furnace cavity was in a low vacuum environment. At this time, an oxygen-containing atmosphere was filled, and the inlet and outlet valves were controlled so that the inlet gas flow rate was greater than the outlet gas flow rate, ensuring that the gas pressure in the furnace cavity was greater than the atmospheric pressure, and the gas pressure gauge reading was maintained at 0.005 MPa. The pre-treated Zr-0.5Nb alloy sample was placed in the atmosphere heat treatment furnace, and an atmosphere with an oxygen partial pressure of 20% was introduced at a flow rate of 1 L / min. The heating rate was set to 5 ℃ / min, and the heating temperature was set to 650 ℃. The first stage of heat preservation lasted for 90 min. After the first stage of heat preservation was completed, the oxygen supply was stopped, the exhaust valve was closed first, and then the inlet valve was closed. Subsequently, the vacuum pump was used to control the gas pressure in the furnace cavity to -0.03 MPa. The sample continued to be heat preserved in the closed furnace cavity at a pressure less than atmospheric pressure for 120 min. After the heat preservation was completed, it was cooled to 25 ℃, and a zirconium-niobium alloy ceramic composite blank was obtained.

[0045] S3: surface post-treatment of the zirconium-niobium alloy ceramic composite blank:

[0046] Polishing is performed on the polishing disc using W2.5-8000 mesh polishing paste until the surface roughness Ra is 0.02 μm. Ultrasonic cleaning is performed in acetone solution and anhydrous ethanol solution respectively for 15 min, and the surface is air-dried after cleaning to obtain the zirconium-niobium alloy ceramic composite material.

[0047] Example 2

[0048] S1: Surface pre-treatment of the zirconium-niobium alloy sample:

[0049] The Zr-1Nb alloy is selected as the base material, and the surface of the Zr-1Nb alloy sample is pre-treated.

[0050] The Zr-1Nb alloy is processed into a circular sheet of 100#, 300#, 800#, 1500# and 3000# water sandpaper are used for grinding, and W2.5-8000 mesh polishing paste is used for polishing on the polishing disc until the surface roughness Ra is 0.02 μm. Ultrasonic cleaning is performed in acetone solution and anhydrous ethanol solution respectively for 18 min, and the surface is air-dried after cleaning to obtain the pre-treated zirconium-niobium alloy.

[0051] S2: Preparation of the zirconia ceramic layer:

[0052] The furnace cavity is subjected to three times of gas washing treatment, and inert gas argon is introduced to fill the furnace cavity. When the gas pressure indicator is 0.05 MPa, the argon valve is closed, the furnace cavity is pumped to a vacuum degree of -0.1 MPa, and the step is repeated three times. After the gas washing treatment is completed, the furnace cavity is in a low vacuum environment, at which time an oxygen-containing atmosphere is filled, and the inlet and outlet valves are controlled so that the inlet gas volume is greater than the outlet gas volume, ensuring that the gas pressure in the furnace cavity is greater than the atmospheric pressure, and the gas pressure gauge indicator is maintained at 0.008 MPa. The pre-treated Zr-1Nb alloy sample is placed in the atmosphere heat treatment furnace, an atmosphere with an oxygen partial pressure of 20% is introduced, the gas flow rate is 2 L / min, the heating rate is set to 8 ℃ / min, the heating temperature is set to 700 ℃, and the first stage holding time is 100 min. After the first stage holding is completed, the oxygen is stopped, the inlet valve is closed after the exhaust valve is closed, and then the vacuum pump is used to control the gas pressure in the furnace cavity to -0.025 MPa. The sample continues to be held in the closed furnace cavity at a pressure less than atmospheric pressure for 100 min, and then cools to 30 ℃ to obtain the zirconium-niobium alloy ceramic composite blank.

[0053] S3: Surface post-treatment of the zirconium-niobium alloy ceramic composite blank:

[0054] Polishing was performed on the polishing disc using W2.5-8000 mesh polishing paste until the surface roughness Ra was 0.02 μm. Ultrasonic cleaning was performed in acetone solution and anhydrous ethanol solution for 18 min, respectively, and the surface was air-dried after cleaning to obtain the zirconium-niobium alloy ceramic composite material.

[0055] Example 3

[0056] S1: Surface pre-treatment of the zirconium-niobium alloy sample:

[0057] The Zr-2.5Nb alloy was selected as the base material, and the Zr-2.5Nb alloy sample was subjected to surface pre-treatment.

[0058] The Zr-2.5Nb alloy was processed into a circular sheet of 100#, 300#, 800#, 1500#, and 3000# water sandpaper, respectively, and polishing was performed on the polishing disc using W2.5-8000 mesh polishing paste until the surface roughness Ra was 0.02 μm. Ultrasonic cleaning was performed in acetone solution and anhydrous ethanol solution for 20 min, respectively, and the surface was air-dried after cleaning to obtain the pre-treated zirconium-niobium alloy.

[0059] S2: Preparation of the zirconia ceramic layer:

[0060] The furnace cavity was subjected to three gas washing treatments, and inert gas argon was introduced to fill the furnace cavity. When the gas pressure gauge reading was 0.05 MPa, the argon valve was closed, and the furnace cavity was pumped to a vacuum degree of -0.1 MPa. This step was repeated three times. After completing the gas washing treatment, the furnace cavity was in a low vacuum environment. At this time, an oxygen-containing atmosphere was filled, and the gas inlet valve and outlet valve were controlled so that the gas inlet amount of the inlet valve was greater than the gas exhaust amount of the outlet valve, ensuring that the gas pressure in the furnace cavity was greater than the atmospheric pressure, and the gas pressure gauge reading was maintained at 0.01 MPa. The pre-treated Zr-2.5Nb alloy sample was placed in the atmosphere heat treatment furnace, and an atmosphere with an oxygen partial pressure of 20% was introduced at a flow rate of 3 L / min. The heating rate was set to 10 ℃ / min, and the heating temperature was set to 750 ℃. The first stage of heat preservation lasted for 120 min. After the first stage of heat preservation was completed, the oxygen supply was stopped, the exhaust valve was closed first, and then the inlet valve was closed. Subsequently, the vacuum pump was used to control the gas pressure in the furnace cavity to -0.02 MPa. The sample continued to be heat preserved in the closed furnace cavity at a pressure less than atmospheric pressure for 90 min. After the heat preservation was completed, it was cooled to 25 ℃ to obtain a zirconium-niobium alloy ceramic composite blank.

[0061] S3: Surface post-treatment of the zirconium-niobium alloy ceramic composite blank:

[0062] Polishing is performed on the polishing disc using W2.5-8000 mesh polishing paste until the surface roughness Ra is 0.02 μm. Ultrasonic cleaning is performed in acetone solution and anhydrous ethanol solution respectively for 20 min, and the surface is air-dried after cleaning to obtain the zirconium-niobium alloy ceramic composite material.

[0063] Comparative Example 1:

[0064] S1: Surface pre-treatment is performed on the zirconium-niobium alloy sample:

[0065] The Zr-2.5Nb alloy is selected as the base material, and surface pre-treatment is performed on the Zr-2.5Nb alloy sample.

[0066] The Zr-2.5Nb alloy is processed into a circular sheet of through rough turning and finish turning processes, and is polished using W2.5-8000 mesh polishing paste on a polishing disc until the surface roughness Ra is 0.02 μm, to obtain the pre-treated zirconium-niobium alloy.

[0067] S2: Zirconium oxide ceramic layer preparation:

[0068] Inert gas argon is introduced to fill the furnace cavity, and when the gas pressure reading is 0.05 MPa, the argon valve is closed, and the furnace cavity is pumped to a vacuum degree of -0.1 MPa. The pre-treated Zr-2.5Nb alloy sample is placed in the atmosphere heat treatment furnace, and an atmosphere with an oxygen partial pressure of 20% is introduced at a flow rate of 3 L / min, the heating rate is set to 10 ℃ / min, the heating temperature is set to 750 ℃, and the first stage holding time is 120 min. After the first stage holding is completed, the oxygen supply is stopped, the priority exhaust valve is closed, and then the furnace cavity is controlled to a gas pressure of -0.02 MPa using a vacuum pump, and the sample continues to be held in the closed furnace cavity at less than atmospheric pressure for a second stage holding time of 90 min. After the holding is completed, it is cooled to 25 ℃ to obtain a zirconium-niobium alloy ceramic composite blank.

[0069] S3: Surface post-treatment is performed on the zirconium-niobium alloy ceramic composite blank:

[0070] Polishing is performed on the polishing disc using W2.5-8000 mesh polishing paste until the surface roughness Ra is 0.02 μm. Ultrasonic cleaning is performed in acetone solution and anhydrous ethanol solution respectively for 20 min, and the surface is air-dried after cleaning to obtain the zirconium-niobium alloy ceramic composite material.

[0071] Parameter changes of Example 1 to Example 3 and Comparative Example 1:

[0072] Example 1 Example 2 Example 3 Comparative Example 1 Zirconium niobium alloy composition Zr-0.5Nb Zr-1Nb Zr-2.5Nb Zr-2.5Nb Pre-treatment cleaning time min 15 18 20 0 First stage furnace atmosphere pressure MPa 0.005 0.008 0.01 0 Heating temperature °C 650 700 750 750 Heating rate °C / min 5 8 10 10 Gas flow rate L / min 1 2 3 3 First stage holding time min 90 100 120 120 Second stage furnace atmosphere pressure MPa -0.03 -0.025 -0.02 -0.02 Second stage holding time min 120 100 90 90 Post-treatment cleaning time min 15 18 20 20

[0073] Experiment

[0074] The zirconium-niobium alloy ceramic composite materials prepared in Example 1 to Example 3 and Comparative Example 1 were subjected to performance testing. The Vickers hardness of the zirconium-niobium alloy ceramic composite material was measured by using an HV-1000 microhardness tester, and the applied load was 100 g, and the pressure holding time was 5 s. Five points on the surface of the sample were measured for hardness, and the average value was taken as the test value. The zirconium-niobium alloy ceramic composite material was subjected to continuous loading and unloading by using a nanoindentation tester at a load of 1000 μN, and the surface nanoindentation hardness of the zirconium-niobium alloy ceramic composite material was obtained.

[0075] The obtained data are shown in the following table:

[0076] Vickers hardness / HV Surface nanoindentation hardness / GPa Example 1 670 13.8 Example 2 640 13.6 Example 3 560 12.8 Comparative Example 1 507 11.7

[0077] Conclusion: The experimental results show that the Vickers hardness of the surface of the zirconium-niobium alloy ceramic composite material samples prepared in Example 1 to Example 3 is 560-670 HV, and the surface nanoindentation hardness is 12.8 GPa-13.8 GPa. In Comparative Example 1, the first stage furnace cavity gas pressure is 0 MPa, and the Vickers hardness of the zirconium-niobium alloy ceramic composite material prepared is reduced to only 507 HV, and the surface nanoindentation hardness is 11.7 GPa, which is significantly reduced. After the gas washing treatment in step S2 of Example 1 to Example 3 is completed, the gas inlet valve is controlled to have a gas inlet amount greater than the gas outlet valve, so as to ensure that the gas pressure in the furnace cavity is greater than the atmospheric pressure, and the gas pressure table display value is maintained at 0.005-0.01 MPa. At this time, the oxygen-containing atmosphere supply in the furnace cavity is sufficient, the stability and reliability of the zirconium-based oxide ceramic generation are increased, and the hardness is increased.

[0078] Finally, it should be noted that the above only describes the preferred embodiments of the present application and is not intended to limit the present application. Although the present application has been described in detail with reference to the foregoing embodiments, those skilled in the art can still modify the technical solutions described in the foregoing embodiments or make equivalent replacements to some technical features. Any modification, equivalent replacement, improvement, etc. made within the spirit and principles of the present application shall be included in the protection scope of the present application.

Claims

1. A method of making a zirconium-niobium alloy ceramic composite material, characterized by: The method comprises the following steps: S1: surface pre-treatment of the zirconium-niobium alloy sample: Take the zirconium-niobium alloy, rough turn, finish turn, polish, clean and dry to obtain the pre-treated zirconium-niobium alloy; S2: zirconia ceramic layer preparation: wash the furnace cavity with inert gas, then introduce the oxygen-containing atmosphere, control the gas pressure in the furnace cavity to be higher than the atmospheric pressure, heat to 650-750℃, carry out the first stage of heat preservation, stop introducing the oxygen-containing atmosphere, control the gas pressure in the furnace cavity to be lower than the atmospheric pressure, carry out the second stage of heat preservation, cool, and obtain the zirconium-niobium alloy ceramic composite blank; S3: surface post-treatment of the zirconium-niobium alloy ceramic composite blank: polish, clean and dry the zirconium-niobium alloy ceramic composite blank to obtain the zirconium-niobium alloy ceramic composite material; The oxygen-containing atmosphere is oxygen-argon mixed gas, the flow rate of the oxygen-containing atmosphere is 1-3L / min, and after the oxygen-containing atmosphere is introduced, the oxygen content in the furnace cavity is 20% oxygen partial pressure.

2. The method of claim 1, wherein the zirconium-niobium alloy ceramic composite is prepared by the steps of: During the first stage of heat preservation, the heat preservation time is 90-120min; at this time, the gas pressure in the furnace cavity is higher than the atmospheric pressure, and the gas pressure in the furnace cavity is 0.005-0.01MPa. ​ 3. The method of claim 1, wherein the zirconium-niobium alloy ceramic composite is prepared by the steps of: During the second stage of heat preservation, the heat preservation temperature is 650-750℃, and the heat preservation time is 90-120min; at this time, the gas pressure in the furnace cavity is lower than the atmospheric pressure, and the gas pressure in the furnace cavity is (-0.03)-(-0.02)MPa. ​ 4. The method of claim 1, wherein the zirconium-niobium alloy ceramic composite is prepared by the steps of: The washing step specifically comprises: introducing argon to fill the furnace cavity with argon, stopping the introduction when the gas pressure in the furnace cavity is 0.05MPa, vacuumizing, and repeating the process several times to complete the washing. ​ 5. The method of claim 1, wherein the zirconium-niobium alloy ceramic composite is prepared by the steps of: The zirconium-niobium alloy is Zr-xNb, x=0.5 or 1 or 2.

5. ​ 6. The method of claim 1, wherein the zirconium-niobium alloy ceramic composite is prepared by the steps of: During the heating process, the heating rate is 5-10℃ / min. ​ 7. The method of claim 1, wherein the zirconium-niobium alloy ceramic composite is prepared by the steps of: The roughness of the pre-treated zirconium-niobium alloy in S1 is 0.02μm; in S3, the surface roughness of the zirconium-niobium alloy ceramic composite material is 0.02μm. ​ 8. The method of claim 1, wherein the zirconium-niobium alloy ceramic composite is prepared by the steps of: In S1 and S3, W2.5-8000 mesh polishing paste is used for polishing. ​

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