CN-122016738-A - Method for in-situ observation of Ti alloy sample by high-temperature laser confocal microscope

Abstract

The invention belongs to the technical field of in-situ observation sample preparation, and in particular relates to a method for in-situ observation of a Ti alloy sample by a high-temperature laser confocal microscope, which comprises the following steps of S1, grinding, polishing and ultrasonic cleaning treatment of the Ti alloy; S2, carrying out plasma spraying treatment on the alumina crucible, spraying a layer of yttrium oxide powder on the surface of the alumina crucible, S3, suspending a pure titanium sheet in a hearth of a high-temperature laser confocal microscope, S4, placing the Ti alloy sample pretreated in the step S1 into the crucible, and carrying out in-situ observation through the high-temperature laser confocal microscope. The method is simple to operate, solves the problems that the Ti alloy is easy to oxidize at high temperature and is not suitable for observing the crucible, and can be used for in-situ observation of microstructure evolution of the Ti alloy under a high-temperature laser confocal microscope and real-time observation of the tissue evolution process of the Ti alloy so as to facilitate subsequent research of growth mechanism analysis and growth dynamics quantification.

Inventors

• LIU CHAO
• YUAN XIAOBO
• DING LIANLI
• TIAN LEI
• Yu Rongzhou

Assignees

• 宁波职业技术大学

Dates

Publication Date

20260512

Application Date

20260320

Claims (10)

1. 1. A method for in-situ observation of a Ti alloy sample by a high temperature laser confocal microscope, the method being applied to a Ti alloy having a Ti content of 53at.% or more, characterized by comprising the steps of: S1, preprocessing Ti alloy, namely grinding, polishing and ultrasonic cleaning the Ti alloy; S2, carrying out plasma spraying treatment on the alumina crucible, and spraying a layer of yttrium oxide powder on the surface of the alumina crucible; S3, hanging a pure titanium sheet in a hearth of the high-temperature laser confocal microscope; s4, placing the Ti alloy sample pretreated in the step S1 into the crucible treated in the step S2, and observing the Ti alloy sample in situ by a high-temperature laser confocal microscope.
2. 2. The method for in-situ observation of a Ti alloy sample by a high temperature laser confocal microscope according to claim 1, wherein the Ti content in the Ti alloy is 53at.% to 80at.%.
3. 3. The method for in-situ observation of a Ti alloy specimen by a high temperature laser confocal microscope according to claim 1, wherein in step S1, polishing is performed until the surface roughness is less than 3 μm.
4. 4. The method for in-situ observation of a Ti alloy sample by a high temperature laser confocal microscope according to claim 1, wherein in step S1, polishing treatment is performed using a diamond polishing paste of 0.25 μm to 1.0 μm.
5. 5. The method for in-situ observation of a Ti alloy sample by a high temperature laser confocal microscope according to claim 1, wherein in step S2, the yttrium oxide powder is spherical yttrium oxide powder with a particle size of 35 μm to 50 μm.
6. 6. The method for in-situ observation of a Ti alloy sample by a high temperature laser confocal microscope according to claim 1, wherein in step S2, the powder feeding rate of the plasma spraying treatment is 30g/min to 60g/min, and the process comprises: the first layer is sprayed with working current of 500-600A, working voltage of 35-45V and spraying of 30-50 μm; The second layer, in which the working current is 650A-700A, the working voltage is 50V-75V, and the spraying is 50 mu m-70 mu m; And the third layer, wherein the working current is 500-600A, the working voltage is 35-45V, and the spraying is 30-60 mu m.
7. 7. The method for in-situ observation of a Ti alloy sample by a high temperature laser confocal microscope according to claim 1, wherein in step S2, the plasma arc moving speed of the plasma spraying treatment is 70 mm/S-90 mm/S, and the working distance is 90 mm-110 mm.
8. 8. The method for in-situ observation of a Ti alloy sample by a high temperature laser confocal microscope according to claim 1, wherein in step S2, the spray thickness is 130 μm to 180 μm.
9. 9. The method for in-situ observation of a Ti alloy specimen by a high temperature laser confocal microscope according to claim 1, wherein in step S3, the pure titanium foil is analytically 99.99%.
10. 10. The method for in-situ observation of a Ti alloy sample by a high temperature laser confocal microscope according to claim 1, wherein in step S4, the flow rate of the inert gas is 100mL/min to 150mL/min during observation.

Description

Method for in-situ observation of Ti alloy sample by high-temperature laser confocal microscope Technical Field The invention particularly relates to a method for in-situ observation of a Ti alloy sample by a high-temperature laser confocal microscope, and belongs to the technical field of in-situ observation sample preparation. Background Since the discovery, titanium has become an important structural metal material due to its low density, high specific strength and good corrosion resistance. Pure titanium can quickly form a stable and compact oxide film in air, so that the pure titanium still maintains excellent chemical stability in high-temperature, humid and chlorine-containing environments. Through reasonable alloying and hot working processes, different types of titanium alloys can have high strength, good toughness and corrosion resistance at the same time, so that the titanium alloy is widely applied in the engineering field. The crossover of material science and biomedical engineering has driven the development of new implant materials over the past decades. Titanium and its alloys are rapidly becoming clinically widely accepted medical metallic materials by virtue of their good biocompatibility, suitable modulus of elasticity, and unique osseointegration capabilities. The characteristic of stable combination with bone tissue is established directly, which lays a foundation for the development of modern oral implants and orthopedic implants. Titanium alloys have been used in large scale in orthopedic joint prostheses, spinal fixation devices, intra-traumatic fixation devices, dental implants, and related devices. In addition to structural members that are subjected to cyclic loading, titanium alloys are also used in cardiovascular implant devices, such as stents, prosthetic heart valves, cardiac pacemaker housings, and chronically implanted sensors, where reliability requirements for long-term service are more stringent. The patent application with publication number of CN119555459A discloses a preparation method of a metallographic specimen of a high-temperature titanium alloy, which greatly improves the preparation efficiency of the metallographic specimen of the high-temperature titanium alloy, but after the method is adopted for the alloy with high Ti content, the microstructure of the Ti alloy cannot be observed in a visual field during high-temperature observation. Ti alloy is easy to oxidize under high-temperature environment and has complex tissue evolution, so that research on the high-temperature tissue evolution rule of the Ti alloy faces a certain difficulty. The laser confocal microscope has the capability of high-temperature heating and real-time observation of microstructure, and is an important means for researching the evolution of the high-temperature microstructure of the metal material. However, the oxidation sensitivity and surface morphology change of the high Ti content alloy under high temperature conditions make the preparation of in situ observation samples more challenging, such as the surface being prone to thick oxide layer formation, the sample edge being prone to warpage or deformation, thereby affecting imaging quality and experimental reliability. In addition, the traditional alumina crucible can react with Ti to cause alloy to adhere to the crucible when the temperature is raised, so that microstructure of the Ti alloy can not be observed in a visual field, and the yttrium oxide crucible has poor thermal shock property and is easy to crack in the process of raising the temperature. In summary, the prior art has obvious defects, so that the development of a sample preparation method for high-Ti alloy and suitable for a high-temperature laser confocal microscope has important significance for obtaining clear and stable in-situ observation images and accurately analyzing high-temperature phase transition and tissue evolution behaviors of the high-Ti alloy, and provides key technical support for deeply understanding service mechanisms of the high-Ti alloy in aerospace, biomedical and high-corrosion environments. Disclosure of Invention Aiming at the defects existing in the prior art, the invention provides a method for in-situ observation of a Ti alloy sample by a high-temperature laser confocal microscope, which is simple to operate, solves the problems that the Ti alloy is easy to oxidize at high temperature and is not suitable for an observation crucible, and can observe the microstructure evolution of the Ti alloy in situ and observe the tissue evolution process of the Ti alloy in real time under the high-temperature laser confocal microscope so as to facilitate the subsequent study of growth mechanism analysis and growth dynamics quantification. The technical scheme for solving the technical problems is that the method for in-situ observation of the Ti alloy sample by the high-temperature laser confocal microscope is applied to Ti alloy with the Ti content of mo