CN110987784A - Quantitative characterization method for electrochemical corrosion resistance of nickel-based alloy - Google Patents

Quantitative characterization method for electrochemical corrosion resistance of nickel-based alloy Download PDF

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CN110987784A
CN110987784A CN201911241677.3A CN201911241677A CN110987784A CN 110987784 A CN110987784 A CN 110987784A CN 201911241677 A CN201911241677 A CN 201911241677A CN 110987784 A CN110987784 A CN 110987784A
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test piece
passivation film
test
chemical substance
proportion
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温志勋
杨艳秋
赵彦超
李振威
张旭辉
岳珠峰
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Northwestern Polytechnical University
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Abstract

The disclosure provides a quantitative characterization method for electrochemical corrosion resistance of a nickel-based alloy, and relates to the technical field of material science and engineering. The characterization method comprises the following steps: preparing a test piece according to a preset size, and performing a three-electrode electrochemical corrosion test by taking the test piece as a working electrode to generate a passivation film on the surface of the test piece; testing each chemical substance contained in the passive film and the proportion of each chemical substance in the passive film, and dividing each chemical substance into a compact substance and a non-compact substance according to the compactness of each chemical substance; and determining the corrosion resistance parameters of the test piece according to the proportion of the compact substances and the non-compact substances in the passive film respectively. The characterization method disclosed by the invention can make the test result more convincing and can improve the accuracy rate of the test result.

Description

Quantitative characterization method for electrochemical corrosion resistance of nickel-based alloy
Technical Field
The disclosure relates to the technical field of material science and engineering, in particular to a quantitative characterization method for electrochemical corrosion resistance of a nickel-based alloy.
Background
The nickel-based alloy material has good fatigue resistance and creep resistance in a high-temperature environment, and is widely applied to aviation, aerospace, industrial gas turbines and marine turbines. For example, the high-temperature gas turbine blade can be applied to a turbine blade of an aircraft engine, and is continuously washed by high-temperature gas due to the fact that adverse factors such as high stress and super-strong vibration caused by high-speed rotation are continuously applied to the turbine blade in the working process of the engine, so that the turbine blade is in a severe environment with high temperature, high pressure, strong impact and severe corrosion for a long time. Particularly in marine turbine blades which are in service in marine climates, the halide salt NaCl which is rich in water vapour above the sea water enters the engine with the combustion gases and deposits on the hot end parts of the engine. When the airplane is in a daily parking state, the sediments are easy to deliquesce to form a liquid film, so that the nickel-based single crystal is subjected to electrochemical corrosion, the service life of the blade is influenced, and the research on the electrochemical corrosion resistance of the nickel-based alloy is particularly important.
At present, the electrochemical corrosion behavior of the nickel-based alloy material is mainly researched by an electrochemical characterization method, the morphological characteristics of a corrosion product are observed by adopting an optical microscope, a field emission Scanning Electron Microscope (SEM) and an Atomic Force Microscope (AFM), the type of the corrosion product is qualitatively analyzed, the test result is lack of persuasion, and the accuracy rate is low.
It is to be noted that the information disclosed in the above background section is only for enhancement of understanding of the background of the present disclosure, and thus may include information that does not constitute prior art known to those of ordinary skill in the art.
Disclosure of Invention
The present disclosure is directed to overcome the above-mentioned deficiencies in the prior art, and provides a method for quantitatively characterizing the electrochemical corrosion resistance of a nickel-based alloy, which can make the test result more convincing and improve the accuracy of the test result.
According to one aspect of the present disclosure, there is provided a method for quantitatively characterizing electrochemical corrosion resistance of a nickel-based alloy, comprising:
preparing a test piece according to a preset size, and performing a three-electrode electrochemical corrosion test by taking the test piece as a working electrode to generate a passivation film on the surface of the test piece;
testing each chemical substance contained in the passivation film and the proportion of each chemical substance in the passivation film, and classifying each chemical substance into a dense substance and a non-dense substance according to the compactness of each chemical substance;
and determining the corrosion resistance parameters of the test piece according to the proportion of the compact substances and the non-compact substances in the passive film respectively.
In an exemplary embodiment of the present disclosure, the characterization method further includes:
and covering the area outside the preset area of the test piece with denture powder, wherein the preset area is used for participating in the electrochemical corrosion test.
In an exemplary embodiment of the present disclosure, the number of the test pieces is plural; the preparation method of the test piece according to the preset size and the three-electrode electrochemical corrosion test with the test piece as the working electrode enables the passivation film to be generated on the surface of the test piece, and comprises the following steps:
preparing a plurality of reference test pieces with different crystal orientations according to preset sizes;
smoothing each reference test piece to form each test piece;
and respectively taking each test piece as a working electrode, graphite as an auxiliary electrode and a saturated calomel electrode as a reference electrode to carry out a plurality of groups of three-electrode electrochemical corrosion tests.
In an exemplary embodiment of the present disclosure, the testing each chemical substance contained in the passivation film and a proportion of each chemical substance in the passivation film, and the classifying each chemical substance into a dense species and a non-dense species according to a denseness of each chemical substance includes:
analyzing the components of the passivation film by using an X-ray photoelectron spectrum analyzer to obtain each chemical substance contained in the passivation film and the proportion of each chemical substance in the passivation film, and dividing each chemical substance into a compact substance and a non-compact substance according to the compactness of each chemical substance;
the compact substances comprise at least one of aluminum oxide, chromium oxide, tungsten dioxide or tungsten trioxide, and the non-compact substances comprise at least one of nickel hydroxide and chromium hydroxide.
In an exemplary embodiment of the disclosure, the determining the corrosion resistance parameter of the test piece according to the ratio of the dense species and the non-dense species in the passivation film respectively comprises:
determining a corrosion resistance parameter according to the ratio of the sum of the proportion of each dense species in the passivation film to the sum of the proportion of each non-dense species in the passivation film.
In an exemplary embodiment of the present disclosure, the characterization method further includes:
testing the electrochemical impedance curve of each test piece to obtain the electrochemical impedance value of the test piece;
and testing the potentiodynamic polarization curve of each test piece to obtain the self-corrosion potential and the self-corrosion current of the test piece.
In an exemplary embodiment of the present disclosure, the characterization method further includes:
and selecting a passivation potential according to the potentiodynamic polarization curve, and carrying out constant potential polarization test according to the passivation potential to obtain the passivation film.
In an exemplary embodiment of the present disclosure, the dense substance includes aluminum oxide, chromium oxide, tungsten dioxide, or tungsten trioxide, the non-dense substance includes nickel hydroxide and chromium hydroxide, the corrosion resistance parameter is determined by a correspondence relationship between the dense substance and the non-dense substance, and the correspondence relationship is:
Figure BDA0002306424520000031
wherein R iscpTo resist corrosion parameters, Q1Q is the proportion of aluminum oxide in the passivation film2Q is the ratio of chromium oxide in the passivation film3Q is the proportion of tungsten dioxide in the passivation film4Q is the proportion of tungsten trioxide in the passivation film5Q is the proportion of nickel hydroxide in the passivation film6Is the proportion of the chromium hydroxide in the passive film.
In an exemplary embodiment of the present disclosure, the number of the test pieces is 3, and the crystal orientations of the test pieces are [001] direction, [111] direction, and [011] direction, respectively.
In an exemplary embodiment of the present disclosure, the test piece is a rectangular parallelepiped, and the preset dimension is a length: 10mm, width: 10mm, high: 5 mm; the size of the preset area is as long as: 10mm, width: 10 mm.
The quantitative characterization method for the electrochemical corrosion resistance of the nickel-based alloy can be used for carrying out an electrochemical corrosion test on a test piece, so that the corrosion process of the nickel-based alloy in an actual working environment can be simulated. In the process, the content of each chemical substance in the passive film can be quantified by analyzing the components of the passive film generated on the surface of the corroded test piece and testing the content of each component in the passive film, so that the content of each chemical substance can be visually and accurately given; meanwhile, the corrosion resistance parameters can be calculated by a mathematical method according to the proportion of compact substances to non-compact substances in the chemical substances, so that the corrosion resistance of the passivation film can be reflected by the mathematical parameters in a mathematical analysis mode, the test result is more convincing, and the accuracy of the test result can be improved.
It is to be understood that both the foregoing general description and the following detailed description are exemplary and explanatory only and are not restrictive of the disclosure.
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The accompanying drawings, which are incorporated in and constitute a part of this specification, illustrate embodiments consistent with the present disclosure and together with the description, serve to explain the principles of the disclosure. It is to be understood that the drawings in the following description are merely exemplary of the disclosure, and that other drawings may be derived from those drawings by one of ordinary skill in the art without the exercise of inventive faculty.
FIG. 1 is a flow chart of a method for quantitatively characterizing the electrochemical corrosion resistance of a nickel-based alloy in an embodiment of the present disclosure.
Fig. 2 is a flowchart of step S110 in fig. 1.
FIG. 3 is a schematic diagram of a three-electrode electrochemical corrosion test in an embodiment of the present disclosure.
FIG. 4 is an AC impedance spectrum of the crystal orientation of the test piece in the [001] direction, [011] direction and [111] direction in the embodiment of the present disclosure.
FIG. 5 is a potentiodynamic polarization curve of the crystal orientation of a test piece in the [001] direction, the [011] direction, and the [111] direction in an embodiment of the present disclosure.
Fig. 6 to 9 are X-ray photoelectron spectra of the passivation film when the crystal orientation of the test piece is the [001] direction in the embodiment of the present disclosure.
Fig. 10 to 13 are X-ray photoelectron spectra of the passivation film when the crystal orientation of the test piece is the [011] direction in the embodiment of the present disclosure.
Fig. 14 to 17 are X-ray photoelectron spectra of the passivation film when the crystal orientation of the test piece is the [111] direction in the embodiment of the present disclosure.
In the figure: 1. a working electrode; 2. a reference electrode; 3. and an auxiliary electrode.
Detailed Description
Example embodiments will now be described more fully with reference to the accompanying drawings. Example embodiments may, however, be embodied in many different forms and should not be construed as limited to the examples set forth herein; rather, these embodiments are provided so that this disclosure will be thorough and complete, and will fully convey the concept of example embodiments to those skilled in the art. The described features, structures, or characteristics may be combined in any suitable manner in one or more embodiments. In the following description, numerous specific details are provided to give a thorough understanding of embodiments of the disclosure. One skilled in the relevant art will recognize, however, that the subject matter of the present disclosure can be practiced without one or more of the specific details, or with other methods, components, devices, steps, and the like. In other instances, well-known technical solutions have not been shown or described in detail to avoid obscuring aspects of the present disclosure.
Furthermore, the drawings are merely schematic illustrations of the present disclosure and are not necessarily drawn to scale. The same reference numerals in the drawings denote the same or similar parts, and thus their repetitive description will be omitted. The terms "the" and "said" are used to indicate the presence of one or more elements/components/etc.; the term "comprising" is used in an open-ended inclusive sense and means that there may be additional elements/components/etc. other than the listed elements/components/etc.
The disclosed embodiment provides a quantitative characterization method for electrochemical corrosion resistance of a nickel-based alloy, and as shown in fig. 1, the characterization method may include the following steps:
step S110, preparing a test piece according to a preset size, and performing a three-electrode electrochemical corrosion test by taking the test piece as a working electrode to generate a passivation film on the surface of the test piece;
step S120, testing each chemical substance contained in the passivation film and the proportion of each chemical substance in the passivation film, and dividing each chemical substance into a compact substance and a non-compact substance according to the compactness of each chemical substance;
and S130, determining the corrosion resistance parameters of the test piece according to the proportion of the compact substances and the non-compact substances in the passivation film respectively.
The quantitative characterization method for the electrochemical corrosion resistance of the nickel-based alloy can be used for carrying out an electrochemical corrosion test on a test piece, so that the corrosion process of the nickel-based alloy in an actual working environment can be simulated. In the process, the content of each chemical substance in the passive film can be quantified by analyzing the components of the passive film generated on the surface of the corroded test piece and testing the content of each component in the passive film, so that the content of each chemical substance can be visually and accurately given; meanwhile, the corrosion resistance parameters can be calculated by a mathematical method according to the proportion of compact substances to non-compact substances in the chemical substances, so that the corrosion resistance of the passivation film can be reflected by the mathematical parameters in a mathematical analysis mode, the test result is more convincing, and the accuracy of the test result can be improved.
The following is a detailed description of the steps of the quantitative characterization method for electrochemical corrosion resistance of the nickel-based alloy according to the embodiment of the present disclosure:
as shown in fig. 1, in step S110, a test piece may be prepared in a predetermined size, and a three-electrode electrochemical corrosion test may be performed using the test piece as a working electrode, so that a passivation film is generated on a surface of the test piece.
The test piece may be in the form of a block, a sheet or a plate, and is not particularly limited herein. Which may be made of a nickel-based alloy material. The test piece can be prepared according to the test requirement and the preset size, and the prepared test piece can be used for electrochemical corrosion test. Specifically, the electrochemical corrosion test device can be used as a working electrode of a three-electrode electrochemical corrosion test, and the working electrode is immersed into an electrolyte to perform the electrochemical corrosion test, so that the environment state of a turbine blade taking a nickel-based alloy as a main material in practical application is simulated.
In order to calculate the current density, the area of the test piece contacting the electrolyte during the electrochemical corrosion process can be controlled, specifically, the test piece can be cast by using denture powder, so that the denture powder covers the area outside the preset area of the test piece, so that the preset area is used for participating in the electrochemical corrosion test, the preset area can be a plane or a curved surface of the test piece, and is not specially limited, and the area can be set according to the actual size and the actual needs of the test piece.
As shown in fig. 2, in an embodiment, step S110 may include:
step S1101, preparing a plurality of reference test pieces having different crystal orientations according to a predetermined size.
The reference test piece may be of a block, cylinder, sheet or plate configuration. For example, it may be a cuboid, a cube, a cylinder, a prism or a tetrahedron, but of course, it may also be other shapes, and is not limited herein; the material may be a nickel-based alloy material, for example, the material may be a nickel-based single crystal superalloy material, and of course, other materials that may be used for performing the electrochemical corrosion performance test may also be used, and are not particularly limited herein. The preset size may be a size set according to the test requirements, and is not particularly limited herein. In one embodiment, the reference test piece may have a rectangular parallelepiped shape, and the predetermined size thereof may be: 10mm long, 10mm wide and 5mm high, although other shapes or predetermined sizes are possible and are not listed here.
In order to ensure the reproducibility of the test data, a plurality of reference test pieces can be prepared simultaneously, for example, 3, 4, 5, 6, 7 or 8, but also other numbers are possible, which are not listed here. The reference test pieces may be made of the same material or different materials, and are not particularly limited herein. In one embodiment, in order to verify the accuracy of the test result, each reference test piece may have the same material and may have different crystal orientations, for example, the number of the reference test pieces may be 3, and each reference test piece may be made of a ni-based single crystal superalloy material and may have different crystal orientations, for example, each reference test piece may be made of a ni-based single crystal superalloy material having a crystal orientation in a [001] direction, a crystal orientation in a [111] direction, and a crystal orientation in a [011] direction, respectively.
Step S1102, smoothing each of the reference test pieces to form each test piece.
The surfaces of the reference test pieces can be polished by sand paper, the surface cross of the reference test pieces is eliminated, and then the test pieces are formed, so that the surfaces of the test pieces are ensured to have the same roughness, and the local serious corrosion of the test pieces caused by the unbalanced roughness is avoided.
And step S1103, performing a plurality of groups of three-electrode electrochemical corrosion tests by respectively using each test piece as a working electrode, graphite as an auxiliary electrode and a saturated calomel electrode as a reference electrode.
As shown in FIG. 3, a three-electrode electrochemical corrosion test can be performed by using a test piece as a working electrode 1, graphite as an auxiliary electrode 3, and a saturated dry pump electrode as a reference electrode 2, for example, the test piece, graphite and a saturated dry pump can be immersed in an electrolyte at the same time, and the test piece can be connected with a polarization power supply and a potential testing instrument through leads.
It should be noted that three electrodes can form two loops: one is a polarization loop; the second is a potential measuring circuit. The polarization loop is provided with a polarization current, so that the control and measurement of the magnitude of the polarization current can be carried out in the circuit. The potential of the working electrode 1 with respect to the reference electrode 2 can be measured or controlled using a potentiometric or control instrument in a potential measurement circuit in which almost no current flows. Therefore, through the three-electrode electrochemical corrosion test, current can pass through the interface of the working electrode 1, the stability of the potential of the reference electrode 2 is not influenced, and the current and the potential passing through the working electrode 1 can be measured simultaneously, so that the polarization curve of the working electrode 1 can be obtained. Thus, the potential of the working electrode 1 can be measured by the reference electrode 2. The reference electrode 2 may have a known, stable electrode potential and no polarization occurs during the measurement. The auxiliary electrode 3 can be used to pass current to achieve polarization of the working electrode 1.
The test piece with crystal orientation in the [001] direction, the test piece with crystal orientation in the [111] direction and the test piece with crystal orientation in the [011] direction can be used as the working electrode 1 respectively to perform three groups of electrochemical corrosion tests simultaneously, of course, the test piece with other crystal orientations or the test piece with other materials can also be used as the working electrode 1 to perform electrochemical corrosion resistance tests, and are not listed.
During the test, the electrochemical impedance curves of the test pieces can be tested by using a CorrTest electrochemical workstation (model CS300H), and the electrochemical impedance values of the test pieces can be obtained, and the test results are shown in FIG. 4. Meanwhile, the potentiodynamic polarization curve of each test piece can be tested, the self-corrosion potential and the self-corrosion current of each test piece can be obtained, the test result is shown in figure 5, wherein the abscissa is the self-corrosion current, the ordinate is the self-corrosion voltage, and each curve in figure 5 can be fitted to obtain the crystal orientation of [001]]The self-corrosion current of the test piece in the direction is 2.7697 mu A/cm2The self-corrosion voltage is-1.0876V; crystal orientation of [0101 ]]The self-corrosion current of the test piece in the direction is 10.937 mu A/cm2The self-corrosion voltage is-1.1532V; crystal orientation of [111]]The self-corrosion current of the test piece in the direction is 4.4781 mu A/cm2The self-etching voltage is-1.0298V. The self-corrosion potential is a potential at which the surface of the test piece reaches a stable corrosion state in the absence of an applied current. The current density corresponding to the self-corrosion potential is the self-corrosion current, and the self-corrosion current can be used for judging the possibility of electrochemical corrosion of the test piece.
And selecting the potential capable of generating the passivation film as the passivation potential according to the potentiodynamic polarization curve, and performing constant potential polarization test on each test piece, so that the passivation film is generated in the preset area where each test piece participates in electrochemical corrosion.
As shown in fig. 1, in step S120, each chemical substance and the proportion of each chemical substance in the passivation film may be tested, and each chemical substance may be classified into a dense substance and a non-dense substance according to the compactness of each chemical substance.
The passivation film may be a chemical substance generated by the reaction of the surface material of the test piece and the electrolyte, and the type of the chemical substance may vary with the type of the electrolyte, for example, it may be an oxide or a hydroxide, and of course, other substances may be also included, which are not listed here. The components of the passivation film can be analyzed by an X-ray photoelectron spectrum analyzer, so that various chemical substances contained in the passivation film and the content of the chemical substances in the passivation film are obtained, the proportion of the chemical substances in the passivation film is calculated, and the chemical substances can be divided into compact substances and non-compact substances according to the compactness of the chemical substances. The passivation film may include one dense species or a plurality of dense species, and accordingly, it may include one non-dense species or a plurality of non-dense species, which is not particularly limited herein.
In the test pieces with different crystal orientations, the content of the passivation film may have a slight difference, and the content of each chemical substance in the passivation film of each test piece may be quantitatively detected by X-ray photoelectron spectroscopy, as shown in fig. 6 to 9, which is an X-ray photoelectron spectroscopy of a passivation film with a crystal orientation of [001] direction, in which the abscissa is binding energy and the ordinate is relative intensity. The types of the substances contained in the passivation film can be uniquely and correspondingly determined according to the peak positions of the curves and the corresponding relation between the peak positions and the binding energy in the abscissa. The ratio of the oxidation state to the metal state of each metal in the figure can be calculated, and it can be seen that the ratio of nickel oxide to metallic nickel is 2.338, the ratio of chromium oxide to metallic chromium is 6.306, the ratio of tungsten oxide to metallic tungsten is 5.707, and the ratio of aluminum oxide to metallic aluminum is 7.424 in the [001] direction of the crystal orientation. As shown in fig. 10 to 13, the X-ray photoelectron spectrum of the passivation film having the crystal orientation in the [011] direction is shown, in which the abscissa is the binding energy and the ordinate is the relative intensity. The types of the substances contained in the passivation film can be uniquely and correspondingly determined according to the peak positions of the curves and the corresponding relation between the peak positions and the binding energy in the abscissa. The ratio of the oxidation state to the metal state of each metal in the figure can be calculated, and it can be seen that the ratio of nickel oxide to metallic nickel is 3.381, the ratio of chromium oxide to metallic chromium is 5.993, the ratio of tungsten oxide to metallic tungsten is 5.772, and the ratio of metallic aluminum to aluminum oxide is 5.924 in the direction of [011] crystal orientation. As shown in fig. 14 to 17, the X-ray photoelectron spectrum of the passivation film having the crystal orientation of [111] direction is shown, in which the abscissa is the binding energy and the ordinate is the relative intensity. The types of the substances contained in the passivation film can be uniquely and correspondingly determined according to the peak positions of the curves and the corresponding relation between the peak positions and the binding energy in the abscissa. The ratio of the oxidation state to the metal state of each metal in the figure can be calculated, and it can be seen that the ratio of nickel oxide to metallic nickel is 2.410, the ratio of chromium oxide to metallic chromium is 6.124, the ratio of tungsten oxide to metallic tungsten is 5.836, and the ratio of aluminum oxide to metallic aluminum is 6.302 in the direction of [111 ].
The dense substance may be a substance having high corrosion resistance, and the non-dense substance may be a substance having low corrosion resistance. For example, the dense substance may include at least one of aluminum oxide, chromium oxide, tungsten dioxide, or tungsten trioxide, and the non-dense substance may include at least one of nickel hydroxide and chromium hydroxide, but of course, the dense substance may also be other substances with stronger corrosion resistance, and the non-dense substance may also be other substances with weaker corrosion resistance, which are not listed here.
As shown in fig. 1, in step S130, the corrosion resistance parameter of the test piece is determined according to the ratio of the dense species and the non-dense species in the passivation film.
In one embodiment, the dense species may include a plurality of chemical species, and the non-dense species may also include a plurality of chemical species, and the content ratio of each chemical species in the passivation film may be calculated respectively, and the content of each of the plurality of dense species and the content of each of the plurality of non-dense species may be summed in a classified manner to obtain the proportion of the dense species and the proportion of the non-dense species. The various chemical substances can be classified and summed through a computer program or software, and of course, the calculation can also be carried out through manual calculation, and the calculation mode is not particularly limited.
The corrosion resistance parameter can be determined according to the ratio of the sum of the proportion of each compact substance in the passive film to the sum of the proportion of each non-compact substance in the passive film, the corrosion resistance of the test piece can be intuitively reflected through the mathematical parameter, and the larger the corrosion resistance parameter is, the better the corrosion resistance of the test piece is.
For example, the dense species may include aluminum oxide, chromium oxide, tungsten dioxide, or tungsten trioxide, the non-dense species includes nickel hydroxide and chromium hydroxide, and the corrosion resistance parameter is determined by a correspondence between the dense species and the non-dense species, which may be:
Figure BDA0002306424520000101
wherein R iscpTo resist corrosion parameters, Q1Q is the proportion of aluminum oxide in the passivation film2Q is the ratio of chromium oxide in the passivation film3Q is the proportion of tungsten dioxide in the passivation film4Q is the proportion of tungsten trioxide in the passivation film5Q is the proportion of nickel hydroxide in the passivation film6Is the proportion of the chromium hydroxide in the passive film.
The quantitative characterization method for the electrochemical corrosion resistance of the nickel-based alloy can be used for carrying out electrochemical corrosion tests on a test piece. In the process, the surface of the test piece can be polished, so that the influence of roughness on the surface of the test piece is avoided; the denture powder casting sample can be adopted, the area of the test piece participating in electrochemical corrosion is controlled, and the current density collection is facilitated; the trend of the electrochemical corrosion resistance of different test pieces can be analyzed through the shaping of an electrochemical impedance curve and a potentiodynamic polarization curve, the components of a passive film generated on the surface of the test piece and the content of each component in the passive film can be tested on the basis of qualitative analysis, and the content of each chemical substance in the passive film can be quantified, so that the content of each chemical substance can be visually and accurately given; meanwhile, the corrosion resistance parameters can be calculated by a mathematical method according to the proportion of compact substances to non-compact substances in the chemical substances, so that the corrosion resistance of the passivation film can be reflected by the mathematical parameters in a mathematical analysis mode, the test result is more convincing, and the accuracy of the test result can be improved.
Other embodiments of the disclosure will be apparent to those skilled in the art from consideration of the specification and practice of the disclosure disclosed herein. This application is intended to cover any variations, uses, or adaptations of the disclosure following, in general, the principles of the disclosure and including such departures from the present disclosure as come within known or customary practice within the art to which the disclosure pertains. It is intended that the specification and examples be considered as exemplary only, with a true scope and spirit of the disclosure being indicated by the following claims.

Claims (10)

1. A quantitative characterization method for electrochemical corrosion resistance of a nickel-based alloy is characterized by comprising the following steps:
preparing a test piece according to a preset size, and performing a three-electrode electrochemical corrosion test by taking the test piece as a working electrode to generate a passivation film on the surface of the test piece;
testing each chemical substance contained in the passivation film and the proportion of each chemical substance in the passivation film, and classifying each chemical substance into a dense substance and a non-dense substance according to the compactness of each chemical substance;
and determining the corrosion resistance parameters of the test piece according to the proportion of the compact substances and the non-compact substances in the passive film respectively.
2. The characterization method according to claim 1, further comprising:
and covering the area outside the preset area of the test piece with denture powder, wherein the preset area is used for participating in the electrochemical corrosion test.
3. The characterization method according to claim 1, wherein the number of the test pieces is plural; the preparation method of the test piece according to the preset size and the three-electrode electrochemical corrosion test with the test piece as the working electrode enables the passivation film to be generated on the surface of the test piece, and comprises the following steps:
preparing a plurality of reference test pieces with different crystal orientations according to preset sizes;
smoothing each reference test piece to form each test piece;
and respectively taking each test piece as a working electrode, graphite as an auxiliary electrode and a saturated calomel electrode as a reference electrode to carry out a plurality of groups of three-electrode electrochemical corrosion tests.
4. The characterization method according to claim 1, wherein the testing each chemical substance contained in the passivation film and a proportion of each chemical substance in the passivation film, and the classifying each chemical substance into a dense species and a non-dense species according to a denseness of each chemical substance comprises:
analyzing the components of the passivation film by using an X-ray photoelectron spectrum analyzer to obtain each chemical substance contained in the passivation film and the proportion of each chemical substance in the passivation film, and dividing each chemical substance into a compact substance and a non-compact substance according to the compactness of each chemical substance;
the compact substances comprise at least one of aluminum oxide, chromium oxide, tungsten dioxide or tungsten trioxide, and the non-compact substances comprise at least one of nickel hydroxide and chromium hydroxide.
5. The characterization method according to claim 1, wherein the determining the corrosion resistance parameter of the test piece according to the ratio of the dense species and the non-dense species in the passivation film comprises:
determining a corrosion resistance parameter according to the ratio of the sum of the proportion of each dense species in the passivation film to the sum of the proportion of each non-dense species in the passivation film.
6. The characterization method according to claim 3, further comprising:
testing the electrochemical impedance curve of each test piece to obtain the electrochemical impedance value of the test piece;
and testing the potentiodynamic polarization curve of each test piece to obtain the self-corrosion potential and the self-corrosion current of the test piece.
7. The characterization method of claim 6, further comprising:
and selecting a passivation potential according to the potentiodynamic polarization curve, and carrying out constant potential polarization test according to the passivation potential to obtain the passivation film.
8. The characterization method according to claim 4, wherein the dense species comprises aluminum oxide, chromium oxide, tungsten dioxide or tungsten trioxide, the non-dense species comprises nickel hydroxide and chromium hydroxide, the corrosion resistance parameter is determined by a correspondence relationship between the dense species and the non-dense species, the correspondence relationship is as follows:
Figure FDA0002306424510000021
wherein R iscpTo resist corrosion parameters, Q1Q is the proportion of aluminum oxide in the passivation film2Q is the ratio of chromium oxide in the passivation film3Q is the proportion of tungsten dioxide in the passivation film4Q is the proportion of tungsten trioxide in the passivation film5Q is the proportion of nickel hydroxide in the passivation film6Is the proportion of the chromium hydroxide in the passive film.
9. The characterization method according to claim 3, wherein the number of the test pieces is 3, and the crystal orientations of the test pieces are [001] direction, [111] direction and [011] direction, respectively.
10. The characterization method according to claim 2, wherein the test piece is a rectangular parallelepiped, and the predetermined dimension is a length: 10mm, width: 10mm, high: 5 mm; the size of the preset area is as long as: 10mm, width: 10 mm.
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Cited By (1)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN113418762A (en) * 2021-06-12 2021-09-21 西北工业大学 Preparation method of transmission electron microscope sample for observing nano structure of passivation film

Citations (6)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN101762454A (en) * 2010-02-03 2010-06-30 海洋王照明科技股份有限公司 Dual-ring electrochemical dynamic potential reactivating evaluating method for diphase stainless steel intercrystalline corrosion sensitivity
CN103014814A (en) * 2012-12-03 2013-04-03 中国科学院金属研究所 Electrochemical treatment method of increasing corrosion resistance of medical beta-type titanium alloy surface
CN104880399A (en) * 2014-10-23 2015-09-02 中国石油化工股份有限公司 Film pre-formation-after corrosion passive film performance detection method
CN105466844A (en) * 2015-11-26 2016-04-06 中国航空工业集团公司沈阳飞机设计研究所 Aluminum lithium alloy corrosion resistance evaluation method
CN108344679A (en) * 2018-01-18 2018-07-31 北京科技大学 A method of characterization cast austenitic-ferritic stainless steel pitting corrosion
CN110261291A (en) * 2019-07-12 2019-09-20 安泰科技股份有限公司 The corrosion proof method of rapid evaluation metal protective film

Patent Citations (6)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN101762454A (en) * 2010-02-03 2010-06-30 海洋王照明科技股份有限公司 Dual-ring electrochemical dynamic potential reactivating evaluating method for diphase stainless steel intercrystalline corrosion sensitivity
CN103014814A (en) * 2012-12-03 2013-04-03 中国科学院金属研究所 Electrochemical treatment method of increasing corrosion resistance of medical beta-type titanium alloy surface
CN104880399A (en) * 2014-10-23 2015-09-02 中国石油化工股份有限公司 Film pre-formation-after corrosion passive film performance detection method
CN105466844A (en) * 2015-11-26 2016-04-06 中国航空工业集团公司沈阳飞机设计研究所 Aluminum lithium alloy corrosion resistance evaluation method
CN108344679A (en) * 2018-01-18 2018-07-31 北京科技大学 A method of characterization cast austenitic-ferritic stainless steel pitting corrosion
CN110261291A (en) * 2019-07-12 2019-09-20 安泰科技股份有限公司 The corrosion proof method of rapid evaluation metal protective film

Non-Patent Citations (4)

* Cited by examiner, † Cited by third party
Title
刘莉等: "均匀化退火及挤压对Mg-Hg-Ga合金显微组织和耐腐蚀性能的影响", 《中国有色金属学报》 *
司瑞雪等: "Ti和Ta对单晶镍基合金在水溶液中腐蚀行为的影响", 《辽宁化工》 *
张瑜: "在硝酸溶液中不锈钢表面钝化膜的电化学特性", 《腐蚀与防护》 *
王乃光等: "合金化及热处理对镁合金阳极材料组织及性能的影响", 《中国有色金属学报》 *

Cited By (1)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN113418762A (en) * 2021-06-12 2021-09-21 西北工业大学 Preparation method of transmission electron microscope sample for observing nano structure of passivation film

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