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Preparation method of titanium alloy surface passivation film transmission observation sample

A technology of titanium alloy and passivation film is applied in the field of preparation of samples for transmission observation of passivation film on the surface of titanium alloy, which can solve the problems of high cost, complicated process and low success rate, and achieves low cost, simple process and high success rate Effect

Inactive Publication Date: 2013-10-23
INST OF METAL RESEARCH - CHINESE ACAD OF SCI
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0006] The purpose of the present invention is to provide a method for preparing a sample for transmission observation of a passivation film on the surface of a titanium alloy, so as to solve the problems of high cost, complicated process, and low success rate in the existing passivation film cross-section transmission sample preparation technology.

Method used

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  • Preparation method of titanium alloy surface passivation film transmission observation sample
  • Preparation method of titanium alloy surface passivation film transmission observation sample
  • Preparation method of titanium alloy surface passivation film transmission observation sample

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preparation example Construction

[0038] The preparation method of the titanium alloy surface passivation film transmission observation sample of the present invention, the preparation process includes conventional double spray thinning treatment, cathode polarization, anode passivation and other three parts, the specific steps are as follows:

[0039] (1) Double spray thinning treatment

[0040] The thin area of ​​the alloy transmission sample is prepared by the double-jet thinning method, and the preparation equipment is the "Denmark Struers company Tenupol-5 double-jet thinning instrument".

[0041] In the present invention, the alloy transmission sample is a disc-shaped conventional plane sample with a diameter of Φ3mm. Before double jet thinning, the sample is polished step by step with 800#-2000# SiC water abrasive paper to a thickness of 40μm-50μm. Use liquid nitrogen to keep the double jet temperature in the range of -20°C to -30°C, adjust the flow rate (the flow rate ranges from 80ml / min to 100ml / min)...

Embodiment 1

[0055] A pure titanium plane transmission sample with uniform distribution of thin areas was prepared by the "double jet thinning method". After washing and drying, the figure 1 Connect as shown. A three-electrode system was adopted, the electrode connected to the planar transmission sample was connected as the working electrode, and the cathodic polarization was performed under the constant potential mode of the electrochemical workstation. Let it stand for about 1 hour to stabilize the open circuit potential, then apply a voltage of -1V for 5 minutes to remove the surface oxide film; then apply a voltage of 1.0V for anode passivation for about 2 hours; the front end of the thin area is completely passivated Transmission samples such as figure 2 shown. In this embodiment, the electrolytic solution used for cathodic polarization and anode passivation uses NaCl as the electrolyte, and the concentration of the electrolytic solution is 0.5 wt%.

[0056] In this embodiment, th...

Embodiment 2

[0058] A flat transmission sample of Ti-6Al-4V alloy with uniform distribution of thin areas was prepared by "double-jet thinning method". After washing and drying, according to figure 1 Connect as shown. A three-electrode system was adopted, the electrode connected to the planar transmission sample was connected as the working electrode, and the cathodic polarization was performed under the constant potential mode of the electrochemical workstation. Stand for about 2 hours to stabilize the open circuit potential, then apply a voltage of -0.8V for 5 minutes to remove the surface oxide film; then apply a voltage of 0.5V for anode passivation for about 4 hours; the front end of the thin area is completely passivated transmission samples, such as Figure 4 shown. In this embodiment, the electrolytic solution used for cathodic polarization and anode passivation uses NaCl as the electrolyte, and the concentration of the electrolytic solution is 1 wt%.

[0059] In this embodiment...

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Abstract

The invention relates to the field of preparation of a transmission sample, and in particular to a preparation method of a titanium alloy surface passivation film transmission observation sample. The method comprises the following steps of: (1) performing double-spray thinning treatment on a transmission sample with diameter of 3mm and thickness of 40-50 microns polished by sand paper in acid liquor at -20to -30 DEG C to prepare a transmission sample with thin region thickness of about 30nm-100nm and uniform distribution; (2) performing cathodic polarization on the transmission sample subjected to the double spray in electrolyte under the condition of -0.5V to -1.5V for about 1-10 min so as to remove an oxide film spontaneously formed on the surface of the sample in air; and (3) performing anodic passivation treatment on the alloy sample under the condition of 0 to 2V for 0.5-5 hours to fully oxidize the alloy surface so as to form a passivation film uniformly distributed at the thin region of the transmission sample. The fully passivated thin region is completely made from metal oxide and can be free from the influence of an alloy phase of a matrix, and thus the phase composition and the element distribution of the passivation film are easily observed. The preparation method is suitable for preparing of the transmission observation sample of the passivation film of titanium, titanium alloy and the like with thickness of only several nanometers.

Description

Technical field: [0001] The invention relates to the field of transmission sample preparation, in particular to a preparation method of a titanium alloy surface passivation film transmission observation sample. Background technique: [0002] When metals or alloys are placed in media such as air or solution, they will spontaneously interact with these media to form a solid product film on the surface of the material. People call this kind of protective film that can inhibit the anodic dissolution process and is insoluble in the medium itself a passivation film. The passivation film exists as an independent phase, which is basically a compound of oxidized metal. Usually, the passivation film has limited thickness, compact structure, good covering performance, and can be firmly adsorbed on the metal surface. It plays the role of completely separating the metal from the corrosive medium, preventing the metal from contacting the corrosive medium, so that the metal basically stop...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): G01N1/28G01N1/32
Inventor 李季李述军郝玉琳杨锐
Owner INST OF METAL RESEARCH - CHINESE ACAD OF SCI
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