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CN-121977489-A - Titanium alloy nanoscale oxide film thickness measuring method and device

CN121977489ACN 121977489 ACN121977489 ACN 121977489ACN-121977489-A

Abstract

The application discloses a method and a device for measuring the thickness of a titanium alloy nanoscale oxide film, which belong to the technical field of oxide film thickness measurement, wherein the measuring method comprises the steps of obtaining the content of metal elements in the titanium alloy to be measured, and calculating the mass ratio of inherent components of Ti and Al; intercepting and cleaning a sample from the titanium alloy to be tested, carrying out layer-by-layer etching on the cleaned sample, collecting metal element content data of each etching layer, calculating the mass ratio of Ti to Al corresponding to each etching layer, judging that the etching depth reaches the boundary etching time corresponding to the boundary of the oxide film and the substrate, and calculating the thickness of the oxide film by utilizing the boundary etching time and the etching rate. According to the oxide film thickness measuring method, the boundary is defined from the essence of the components by the difference of the mass ratio of Ti/Al and the mass ratio of the inherent components of the matrix in the layer-by-layer etching process, the influence of manual operation is small, and the accurate quantitative measurement of the nano oxide film thickness can be realized.

Inventors

  • WANG YANING
  • Gao Xuanzhi
  • WANG ZIHAO
  • WANG YUEHAN
  • TIAN YUEMING
  • GAO SONG
  • YANG CHUNCHENG

Assignees

  • 中国航发北京航空材料研究院

Dates

Publication Date
20260505
Application Date
20260211

Claims (10)

  1. 1. A method for measuring the thickness of a titanium alloy nano-scale oxide film is characterized by comprising the following steps: Obtaining the content of metal elements in the titanium alloy to be detected, and calculating the inherent component mass ratio R 0 of Ti and Al; Intercepting a sample from a titanium alloy to be detected and cleaning the surface of the sample to obtain a cleaned sample; carrying out layer-by-layer etching on the cleaned sample, and collecting metal element content data of each etching layer; Calculating the mass ratio R of Ti and Al corresponding to each etching layer; Judging that the etching depth reaches the boundary etching time T corresponding to the boundary of the oxide film and the substrate based on the deviation coefficient R of R and R 0 ; And calculating the thickness d of the oxide film by using the boundary etching time T and the etching rate v.
  2. 2. The method for measuring the thickness of the nano-scale oxide film of the titanium alloy according to claim 1, wherein the step of obtaining the content of the metal element in the titanium alloy to be measured comprises the step of measuring the content of the metal element in the titanium alloy to be measured by adopting an X-ray fluorescence spectrometer or an inductively coupled plasma atomic emission spectrometer.
  3. 3. The method for measuring the thickness of the titanium alloy nano-scale oxide film according to claim 1, wherein dust-free cloth is adopted for cleaning the surface, and gasoline, acetone, deionized water and absolute ethyl alcohol are respectively dipped in the dust-free cloth for cleaning and then are purged and dried.
  4. 4. The method for measuring the thickness of a titanium alloy nano-scale oxide film according to claim 1, wherein the step of etching the cleaned sample layer by layer to collect metal element content data of each etched layer comprises the steps of: And carrying out layer-by-layer etching on the cleaned sample by adopting Ar + as etching ions, and collecting metal element content data of a corresponding etching layer by utilizing an XPS instrument after each etching.
  5. 5. The method for measuring the thickness of a titanium alloy nano-scale oxide film according to claim 4, wherein the etching rate of each layer is constant, the etching time of each layer is 10-50s, and the etching depth of each layer is 2-10nm.
  6. 6. The method for measuring the thickness of a titanium alloy nano-scale oxide film according to claim 4, wherein the number of etching layers in the layer-by-layer etching is 5-200.
  7. 7. The method for measuring the thickness of a titanium alloy nano-scale oxide film according to claim 4, wherein the XPS instrument is vacuumized to be less than or equal to 1X 10 -9 Pa.
  8. 8. The method for measuring a thickness of a titanium alloy nano-scale oxide film according to claim 1, wherein determining that an etching depth reaches an accumulated etching time T corresponding to a boundary between the oxide film and a substrate based on a deviation coefficient R of R and R 0 , comprises: And drawing a distribution curve of R of each etching layer and accumulated etching time T reaching the corresponding etching layer, taking a deviation coefficient R of R and R 0 as a boundary judgment parameter, taking R which is less than or equal to 15.0% for n times continuously as a boundary judgment condition, and taking the first T meeting the boundary judgment condition as the boundary etching time T.
  9. 9. The method for measuring the thickness of a titanium alloy nano-scale oxide film according to claim 8, wherein n is not less than 5.
  10. 10. A titanium alloy nanoscale oxide film thickness measuring device is characterized by comprising: the sample preparation unit is used for intercepting a sample from the titanium alloy to be detected and cleaning the surface of the sample to obtain a cleaned sample; An inherent component measuring unit for measuring the content of metal elements in the cleaned sample and calculating an inherent component mass ratio R 0 of Ti and Al; The etching collection unit is used for carrying out layer-by-layer etching on the cleaned sample and collecting the metal element content data of each etching layer; The etching layer calculating unit is used for calculating the mass ratio R of Ti and Al corresponding to each etching layer; the judging unit is used for judging that the etching depth reaches the boundary etching time T corresponding to the boundary of the oxide film and the substrate based on the deviation coefficient R of R and R 0 ; and a thickness calculating unit for calculating the thickness d of the oxide film by using the boundary etching time T and the etching rate v.

Description

Titanium alloy nanoscale oxide film thickness measuring method and device Technical Field The application belongs to the technical field of oxide film thickness measurement, and particularly relates to a method and a device for measuring the thickness of a titanium alloy nanoscale oxide film. Background The titanium alloy is widely applied to the key fields of aerospace and the like due to high strength, strong corrosion resistance and light weight. Under the natural environment or low-temperature oxidation condition, the titanium alloy is easy to form an ultrathin oxide film of multi-element oxides such as TiO 2、Al2O3, the thickness is usually 1-100nm, the thickness of the oxide film can reach 100-500nm after high-temperature short-time oxidation, and the titanium alloy still belongs to the nanoscale category. The thickness of the oxide film directly influences the core performances such as corrosion resistance, fatigue life and the like of the material. The difficulty in measuring the thickness of the nano oxide film is that the boundary between the oxide film and the substrate is accurately defined, the thickness is quantized, and meanwhile, the operation convenience, the result repeatability and the measurement accuracy are considered. The current methods for measuring the thickness of the alloy oxide film are mainly optical microscope section method and Scanning Electron Microscope (SEM) measurement method. The method comprises the steps of cutting, embedding, grinding and polishing alloy samples, observing a cross section interface by an optical microscope, measuring the thickness by means of a scale, wherein the operation is relatively simple, the method is suitable for medium-thickness oxide films with the thickness of more than or equal to 0.5 mu m, the resolution is lower, the method cannot measure nano-scale ultrathin films, the sample of the SEM measuring method needs additional fine ion polishing after cutting, embedding and rough grinding, the thickness is measured by using an electron beam scanning imaging method and software, the thickness of all the oxide films with the thickness of more than or equal to 1nm can be theoretically measured, the resolution can reach 1-10nm, the sample preparation is complex, the problems of sample preparation damage and cross section interface blurring are solved, and the actual measurement error of the nano-scale thin films is large. At present, the thickness of an alloy oxide film is directly measured by preparing a cross-section sample of the alloy, but the method is limited by sample preparation, resolution and interface recognition capability, so that the accurate detection requirement of a nanoscale ultrathin oxide film is difficult to meet, and a more reliable method and device for measuring the nanoscale oxide film thickness on the surface of the titanium alloy are needed. Disclosure of Invention In order to solve the above problems, the present application provides a method for measuring a thickness of a titanium alloy nano-scale oxide film, comprising: Obtaining the content of metal elements in the titanium alloy to be detected, and calculating the inherent component mass ratio R 0 of Ti and Al; Intercepting a sample from a titanium alloy to be detected and cleaning the surface of the sample to obtain a cleaned sample; carrying out layer-by-layer etching on the cleaned sample, and collecting metal element content data of each etching layer; Calculating the mass ratio R of Ti and Al corresponding to each etching layer; Judging that the etching depth reaches the accumulated etching time T corresponding to the boundary of the oxide film and the substrate based on the deviation coefficient R of R and R 0; And calculating the thickness d of the oxide film by using the accumulated etching time T and the etching rate v. Further, obtaining the metal element content in the titanium alloy to be measured comprises measuring the metal element content in the titanium alloy to be measured by adopting an X-ray fluorescence spectrometer or an inductively coupled plasma atomic emission spectrometer. Further, cleaning the surface, namely dipping gasoline, acetone, deionized water and absolute ethyl alcohol into dust-free cloth respectively, sequentially wiping the surface of a sample, and finally blowing and drying by using low-pressure compressed air. Further, the cleaned sample is etched layer by layer, and metal element content data of each etching layer is collected, including: Ar + is used as etching ions to carry out layer-by-layer etching on the cleaned sample, and after each etching, the XPS instrument is used for collecting metal element content data of the corresponding etching layer. Further, the etching rate of the layer-by-layer etching is constant, the etching time of each layer is 10-50s, and the depth of each layer etching is 2-10nm. Further, the number of etching layers of the layer-by-layer etching is 5-200. Further, the XPS instrument is vacuumized