Method and application for preparing surface oxidized ceramic layers of zirconium and zirconium alloy

A technology of surface oxidation and oxidizing ceramics, which is applied in the field of medical implant materials, can solve the problems of adverse effects on the performance of the surface oxide ceramic layer, loss of thickness, and difficulty in meeting the use requirements of the surface oxide ceramic layer, so as to maintain integrity and uniformity. , to ensure the effect of protective performance

Active Publication Date: 2019-05-03
SUZHOU MICROPORT ORTHORECON CO LTD
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  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

However, according to actual operating experience, the thickness of 2-5 μm will be lost in the process of polishing the generated oxide ceramic layer to the target roughness Ra=0.02 μm required by the medical implant. Polishing treatment within the thickness range, the thickness of the final remaining surface oxide ceramic layer is difficult to meet the use requirements
Conversely, if it is necessary to retain a sufficient thickness of the surface oxide ceramic layer after polishing, it is necessary to form a thicker initial surface oxide ceramic layer, which will adversely affect the performance of the surface oxide ceramic layer
[0006] At the same time, in the traditional surface oxidation process, polishing is an inevitable process: if the cooling process is completed after high-temperature oxidation, if it is cooled slowly, because zirconium and zirconium alloys are still in the oxidation medium, the thickness of the surface oxide ceramic layer will be further increased. increase, the quality of the oxide layer formed at an unsuitable temperature is poor, and needs to be removed by polishing; if it is cooled rapidly, due to the large temperature difference between the inside and outside of the workpiece, the thermal stress is likely to cause microcracks in the outermost surface area, and it is also necessary to Area Polishing Removal

Method used

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  • Method and application for preparing surface oxidized ceramic layers of zirconium and zirconium alloy
  • Method and application for preparing surface oxidized ceramic layers of zirconium and zirconium alloy
  • Method and application for preparing surface oxidized ceramic layers of zirconium and zirconium alloy

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Experimental program
Comparison scheme
Effect test

Embodiment 1

[0050] The Zr-2.5Nb alloy (zirconium alloy containing 2.5wt% Nb) is ground and polished to change the surface roughness. The surface roughness of sample 1 is reduced to Ra=0.3792 μm, and the surface roughness of sample 2 is reduced to Ra=0.0038 μm . Put sample 1 and sample 2 together in a tube furnace, heat to 550°C in the air environment, keep warm for 6 hours, exhaust the air and feed argon into the furnace, and slowly cool to 100°C at a cooling rate of 5°C / min. Take it out after it is below ℃, and measure it with a roughness meter. The roughness of sample 1 after oxidation treatment increases to Ra=0.6852 μm, and the roughness of sample 2 increases to Ra=0.0158 μm. The cross-sectional photo of sample 1 under the metallographic microscope after oxidation is as follows: figure 2 As shown, the oxide ceramic layer, the oxygen-rich diffusion layer and the metal substrate are arranged from left to right. Through grinding and polishing, the surface roughness of sample 1 is gradu...

Embodiment 2

[0054] The commercially pure zirconium was ground and polished to change the surface roughness. The surface roughness of sample 3 was reduced to Ra=0.3886 μm, and the surface roughness of sample 4 was reduced to Ra=0.0042 μm. Put sample 3 and sample 4 together in a tube furnace, heat to 600°C in the air environment, keep warm for 4 hours, exhaust the air and feed argon into the furnace, and slowly cool to 100°C at a cooling rate of 5°C / min. It was taken out after it was below ℃, and measured by a roughness meter. The roughness of sample 3 after oxidation increased to 0.7705 μm, and the roughness of sample 4 increased to 0.0158 μm. The cross-sectional photo of sample 3 under the metallographic microscope after oxidation is as follows: Figure 5 As shown, the surface roughness is gradually reduced to Ra=0.0177μm after grinding and polishing. Figure 6 shown. The surface roughness of sample 4 after oxidation has met Ra Figure 7 shown.

[0055] Such as Figure 5 As shown, the ...

Embodiment 3

[0058] The Zr-2.5Nb alloy was ground and polished to change the surface roughness. The surface roughness of sample 5 was reduced to Ra=0.0056 μm, and the surface roughness of sample 6 was reduced to Ra=0.0055 μm. Put sample 5 and sample 6 into the tube furnace respectively, heat to 600°C in the air environment, keep warm for 4 hours, after sample 5 exhausts the air and injects argon into the furnace, slowly cool at a rate of 5°C / min Take it out after cooling to below 100°C, and sample 6 is directly cooled to below 100°C in the original oxidation atmosphere at a cooling rate of 5°C / min and then taken out. Measured by the roughness meter, the roughness of the oxidized sample 5 increased to 0.0162 μm, and the roughness of the sample 6 increased to 0.0426 μm.

[0059] The cross-sectional photo of sample 5 under the metallographic microscope is as follows: Figure 8 As shown, the average thickness of the generated oxide ceramic layer is about 9.54 μm, the oxide ceramic layer has a...

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Abstract

The invention belongs to the technical field of medical implant materials, and particularly relates to a method and application for preparing surface oxidized ceramic layers of zirconium and a zirconium alloy. The method comprises the steps of reducing the roughness of a target area and oxidation treatment and gas replacement. Materials for the medical implant materials can be prepared by the method. According to the technical scheme, the surface roughness is controlled before the surface oxidation treatment is performed, so that the surface roughness after the oxidation treatment directly meets the use requirements, and the inert gas replacement after the surface oxidation treatment avoids the formation of a film layer which is poor in performance and needs to be removed in the cooling process, based on the technical scheme, the need for post-polishing treatment is completely avoided, the integrity and uniformity of the oxidized ceramic layers are maintained, and protective performance is ensured.

Description

technical field [0001] The invention belongs to the technical field of medical implant materials, in particular to a method and application for preparing an oxide ceramic layer on the surface of zirconium and zirconium alloy. Background technique [0002] Zirconium and zirconium alloys have excellent mechanical properties, corrosion resistance and biocompatibility. These properties have been confirmed by scientists many years ago. Therefore, zirconium and zirconium alloys are very good medical implants Material. For medical implant materials, the lifespan of the implant device is the most important, especially when the patients using the implant device are young groups, the ideal implant device can be used by the patient for a lifetime. [0003] However, zirconium and zirconium alloys have poor wear resistance, which limits their application in load-bearing implants such as hip joints and knee joints. Factors affecting the service life of these load-bearing implants include...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C23C8/10C23C8/02C23C8/80A61L27/04A61L27/30A61L27/50
CPCC23C8/12C23C8/02C23C8/80A61L27/04A61L27/30A61L27/50A61L2430/24A61L2400/18A61L2420/02A61L2420/08C23C8/10C22C16/00A61L27/047A61L27/306
Inventor 申宇俞天白翁资欣
Owner SUZHOU MICROPORT ORTHORECON CO LTD
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