CN115616015A - Method for identifying nitriding and nitrocarburizing heat treatment - Google Patents
Method for identifying nitriding and nitrocarburizing heat treatment Download PDFInfo
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- CN115616015A CN115616015A CN202211157880.4A CN202211157880A CN115616015A CN 115616015 A CN115616015 A CN 115616015A CN 202211157880 A CN202211157880 A CN 202211157880A CN 115616015 A CN115616015 A CN 115616015A
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Abstract
The invention discloses a method for identifying nitriding and nitrocarburizing heat treatment, which comprises the steps of carrying out carbon element surface scanning on a white bright layer region to obtain a white bright layer color brightness and white bright layer carbon concentration curve, and obtaining a sample treatment type according to the white bright layer color brightness and white bright layer carbon concentration curve to realize the identification of nitriding and nitrocarburizing heat treatment. Specifically, according to the principle of the electronic probe, on a surface scanning map of an element, the color brightness of an area is proportional to the content of the element in the area, i.e., the higher the color brightness of a position is, the higher the content of the element in the position is represented. Therefore, the heat treatment mode of the sample is judged to be nitriding or nitrocarburizing according to the color brightness difference and the carbon concentration curve of the white bright layer and the matrix: if the color brightness of the white bright layer is higher than that of the matrix and the carbon concentration curve is obviously reduced, the sample can be judged to be subjected to nitrocarburizing treatment; if the color brightness of the white bright layer is consistent with that of the matrix and the carbon concentration curve is straight and has no obvious reduction, the sample can be judged to be subjected to nitriding treatment.
Description
Technical Field
The invention belongs to the field of automobile part manufacturing, and relates to a method for identifying nitriding and nitrocarburizing heat treatment.
Background
Nitriding and nitrocarburizing are two metal material surface strengthening heat treatment processes with similar principles and processes. The parts subjected to nitriding and nitrocarburizing treatment have the characteristics of high surface hardness, wear resistance and corrosion resistance, and can greatly improve the fatigue strength of the workpiece and prolong the service life of the workpiece. Compared with two surface strengthening heat treatment processes of carburizing and carbonitriding, the workpiece treated by the nitriding process and the carbonitriding process has the advantages of small deformation, attractive appearance, good high-temperature performance and the like. Meanwhile, the nitriding and nitrocarburizing heat treatment process is also replaced by the carburizing and nitrocarburizing process due to small environmental pollution in the treatment process, and the application range of the nitriding and nitrocarburizing heat treatment process in the automobile part industry is wider and wider.
The nitriding and nitrocarburizing heat treatment process adopts surface strengthening media with similar components, and a layer of 'white and bright layer' with equivalent hardness and thickness not more than 0.05mm can be formed on the surface of a treated workpiece. The thickness, the compactness and the continuity of the white layer are important indexes for measuring the quality of nitriding and nitrocarburizing heat treatment processes, but designers need to judge the surface heat treatment process of similar products of other companies when developing and improving the products; at this time, the workpiece cannot be identified to be subjected to nitriding or nitrocarburizing heat treatment process by analyzing the 'bright layer' by using conventional detection means such as direct-reading spectroscopy, metallographic methods, hardness methods and the like.
Disclosure of Invention
The invention aims to solve the problem that the workpiece cannot be identified through analyzing a bright white layer in the prior art and is subjected to a nitriding or nitrocarburizing heat treatment process, and provides a method for identifying nitriding and nitrocarburizing heat treatment.
In order to achieve the purpose, the invention adopts the following technical scheme to realize the purpose:
the invention provides a method for identifying nitriding and nitrocarburizing heat treatment, which comprises the following steps:
acquiring a white bright layer area of the processed sample according to the processed sample;
processing the white bright layer area to obtain the color brightness of the white bright layer and the carbon concentration curve of the white bright layer;
and obtaining the sample treatment type according to the color brightness of the white bright layer and the carbon concentration curve of the white bright layer, and realizing the identification of nitriding and nitrocarburizing heat treatment.
Preferably, the method for obtaining the sample processing type according to the white light layer domain color brightness and the white light layer carbon concentration curve is as follows:
if the color brightness of the white bright layer is higher than that of the outer matrix of the white bright layer and the carbon concentration curve of the white bright layer is reduced, performing nitrocarburizing treatment on the sample;
and if the color brightness of the white bright layer is consistent with the color brightness of the outer matrix of the white bright layer and the carbon concentration curve of the white bright layer is not changed, the sample is subjected to nitriding treatment.
Preferably, the thickness of the regions of the bright white layer is less than 0.05mm.
Preferably, the white layer area is treated with an electronic probe.
Preferably, the electronic probe selects a standard sensitivity curve to perform carbon element scanning analysis, and acquires a white bright layer color brightness curve and a white bright layer carbon concentration curve.
Preferably, the acceleration voltage of the electron probe is 15kV, the electron beam current is 100nA, and the test time is 20s.
Preferably, the processed sample is obtained by the following method:
cutting the sample, cleaning and roughly grinding the cut sample, and removing the cutting mark of the cutting line; and cleaning the coarsely ground sample in absolute ethyl alcohol, and drying the sample to obtain a processed sample.
Preferably, the material of the test sample is carbon steel or low carbon steel.
Preferably, the specimen is cut using a wire cutting method.
Preferably, the coarsely ground test specimens are ultrasonically cleaned in absolute ethanol.
Compared with the prior art, the invention has the following beneficial effects:
according to the method for identifying nitriding and nitrocarburizing heat treatment, provided by the invention, the white bright layer region can be treated, the color brightness and the carbon concentration curve of the white bright layer can be obtained, the sample treatment type can be obtained according to the color brightness and the carbon concentration curve of the white bright layer, and the identification of nitriding and nitrocarburizing heat treatment can be realized. Therefore, the method can solve the problem that the nitriding process or the nitrocarburizing heat treatment process of the part cannot be accurately judged in the prior art, and provides accurate data support for new product design and improvement and promotion of product quality. And the method is not limited by the shape and size of the sample, is simple and convenient to operate, and has intuitive and reliable results.
Further, a standard sensitivity curve mode is selected, surface scanning analysis of the carbon element content is carried out, and a distribution image of the carbon element content in the test area and a concentration curve of a straight line on the graph can be obtained.
Furthermore, an electronic probe is adopted to process the white layer area, because the electronic probe can carry out accurate quantitative analysis on elements, and the analysis precision of carbon elements reaches 0.01%.
Furthermore, the acceleration voltage of the electron probe is set to be 15kV, the electron beam current is 100nA, and the test time is 20s, so that the carbon element analysis efficiency and accuracy can be optimized.
Furthermore, carbon steel or low-carbon steel is used as the sample, because the carbon content of the sample is between 0.05 and 1.0 percent, and the carbon content is distributed in a gradient manner, the analysis accuracy can be improved.
Furthermore, the absolute ethyl alcohol is adopted for cleaning so as to easily wash off fat-soluble substances which cannot be washed off by water on the surface of the sample; and the anhydrous ethanol is volatilized quickly, and the surface residue can be volatilized immediately after the cleaning.
Further, the wire cutting method is adopted to cut the sample, and any conductive or semiconductive material can be processed regardless of the hardness of the workpiece. And the cutting seam of the linear cutting can be as narrow as only 0.005mm, only the workpiece material is subjected to trepanning processing along the profile, the material utilization rate is high, and the material can be effectively saved.
Furthermore, the sample after coarse grinding is cleaned by an ultrasonic method, the cleaning speed is high, the cleaning precision is high, tiny stain particles can be cleaned powerfully, the cleanliness of the workpiece is consistent, and the surface of the workpiece is not damaged; the cleaning liquid is not needed to be contacted by hands, and deep holes, thin seams and hidden parts of workpieces are cleaned safely and reliably.
Drawings
In order to more clearly illustrate the technical solutions of the embodiments of the present invention, the drawings required in the embodiments will be briefly described below, it should be understood that the following drawings only illustrate some embodiments of the present invention, and therefore should not be considered as limiting the scope, and those skilled in the art can also obtain other related drawings based on the drawings without inventive efforts.
FIG. 1 is a flow chart of the method for discriminating nitriding and nitrocarburizing heat treatment of the present invention.
FIG. 2 is a graph showing the scanning results of the present invention ((a) BSD image of nitrided part, (b) surface distribution of nitrided C element, (C) BSD image of nitrocarburized part, (d) surface distribution of nitrocarburized C element).
FIG. 3 is a graph showing the concentration of carbon in the nitriding treatment according to the present invention.
FIG. 4 is a graph of the concentration of carbon in the nitrocarburizing treatment of the present invention.
FIG. 5 is a standard working curve for testing carbon element according to the present invention.
Detailed Description
In order to make the objects, technical solutions and advantages of the embodiments of the present invention clearer, the technical solutions in the embodiments of the present invention will be clearly and completely described below with reference to the drawings in the embodiments of the present invention, and it is obvious that the described embodiments are some, but not all, embodiments of the present invention. The components of embodiments of the present invention generally described and illustrated in the figures herein may be arranged and designed in a wide variety of different configurations.
Thus, the following detailed description of the embodiments of the present invention, presented in the figures, is not intended to limit the scope of the invention, as claimed, but is merely representative of selected embodiments of the invention. All other embodiments, which can be derived by a person skilled in the art from the embodiments given herein without making any creative effort, shall fall within the protection scope of the present invention.
It should be noted that: like reference numbers and letters refer to like items in the following figures, and thus, once an item is defined in one figure, it need not be further defined and explained in subsequent figures.
In the description of the embodiments of the present invention, it should be noted that if the terms "upper", "lower", "horizontal", "inner", etc. are used for indicating the orientation or positional relationship based on the orientation or positional relationship shown in the drawings or the orientation or positional relationship which is usually arranged when the product of the present invention is used, the description is merely for convenience and simplicity, and the indication or suggestion that the referred device or element must have a specific orientation, be constructed and operated in a specific orientation, and thus, cannot be understood as limiting the present invention. Furthermore, the terms "first," "second," and the like are used merely to distinguish one description from another, and are not to be construed as indicating or implying relative importance.
Furthermore, the term "horizontal", if present, does not mean that the component is required to be absolutely horizontal, but may be slightly inclined. For example, "horizontal" merely means that the direction is more horizontal than "vertical" and does not mean that the structure must be perfectly horizontal, but may be slightly inclined.
The invention is described in further detail below with reference to the accompanying drawings:
the invention provides a method for identifying nitriding and nitrocarburizing heat treatment, which comprises the following steps as shown in figure 1:
s1, acquiring a white bright layer area of a processed sample according to the processed sample;
the standard sample is made of carbon steel or low-carbon steel.
The treated samples were obtained as follows: cutting the sample, cleaning and roughly grinding the cut sample, and removing the cutting mark of the cutting line; and cleaning the coarsely ground sample in absolute ethyl alcohol, and drying the sample to obtain a processed sample. Wherein, the test sample is cut by adopting a linear cutting method, and the test sample after coarse grinding is cleaned by adopting an ultrasonic method in absolute ethyl alcohol.
S2, carrying out carbon element scanning analysis on the white bright layer area to obtain the color brightness and the carbon concentration curve of the white bright layer;
the method comprises the following steps of (1) processing a white bright layer area by adopting an electronic probe, specifically: and selecting a standard sensitivity curve by the electronic probe, and carrying out carbon element scanning analysis to obtain a white bright layer color brightness curve and a white bright layer carbon concentration curve. The accelerating voltage of the electron probe is 15kV, the electron beam current is 100nA, the testing time is 20s, and the thickness of the white bright layer area is less than 0.05mm.
And S3, acquiring the sample treatment type according to the color brightness of the white bright layer and the carbon concentration curve of the white bright layer, and identifying nitriding and nitrocarburizing heat treatment.
The method for acquiring the sample processing type according to the white bright layer domain color brightness and the white bright layer carbon concentration curve comprises the following steps:
if the color brightness of the white bright layer is higher than that of the outer matrix of the white bright layer and the carbon concentration curve of the white bright layer is reduced, performing nitrocarburizing treatment on the sample;
and if the color brightness of the white bright layer is consistent with the color brightness of the outer matrix of the white bright layer and the carbon concentration curve of the white bright layer is not changed, the sample is subjected to nitriding treatment.
The invention utilizes 1720 type electronic probe, the device can carry out accurate quantitative analysis of element, the analysis precision of carbon element reaches 0.01%, and the requirement of the invention can be satisfied. According to the invention, a plurality of standard samples for chemical spectra are selected, proper test parameters are set by utilizing a mapping analysis mode of an electronic probe, a region containing a white layer is selected, a standard sensitivity curve mode is selected, and surface scanning analysis of carbon elements is carried out to obtain a distribution image and a concentration gradient curve of the content of the carbon elements in the test region, as shown in fig. 2 and fig. 3. According to the principle of an electronic probe, on a surface scanning image of an element, the color brightness of an area is proportional to the content of the element in the area, namely, the higher the color brightness of a position is, the higher the content of the element in the position is represented. Therefore, the heat treatment mode of the sample is judged to be nitriding or nitrocarburizing according to the color brightness difference of carbon elements in the white bright layer and the matrix.
Selecting one nitriding heat treatment sample and one nitrocarburizing heat treatment sample, cutting a section by linear cutting, and polishing a metallographic phase. Putting the sample into a beaker containing absolute ethyl alcohol, carrying out ultrasonic cleaning, removing surface dirt, then putting the sample into an electronic probe sample cabin, selecting a Mapping analysis mode, finding a white bright layer in an image observation window of the electronic probe, framing a region containing the white bright layer, selecting a standard sensitivity curve, carrying out surface scanning analysis on carbon elements, obtaining a color change surface scanning analysis result of the carbon element content in the framed region, wherein the result is shown in figure 2, (a) is a nitriding member BSD image, (b) is nitriding treatment C element surface distribution, taking an outward-inward straight line (the straight line length is about 0.05 mm) on the surface scanning analysis result, reading the carbon concentration change on the straight line, and (C) is a nitrocarburizing member BSD image in figure 2, (d) is nitrocarburizing treatment C element surface distribution, and obtaining the carbon element contents of two samples at different distances from the surface to the inside, which are shown in figures 3, 4 and table 1. Comparing fig. 2 (b) with fig. 3, and fig. 2 (d) with fig. 4, the color brightness of the white bright layer on the surface of the nitriding treatment sample is basically consistent with that of the matrix, and the carbon concentration curve is straight; the color brightness of the white and bright layer on the surface of the nitrocarburizing treatment sample is obviously higher than that of the matrix, and the carbon concentration curve is obviously reduced from the surface to the inside, which indicates that the phenomenon of obvious recarburization exists. Therefore, the method can be effectively used for identifying nitriding or nitrocarburizing heat treatment of parts.
Table 1 carbon content (mass fraction,%) of two samples at different distances from the surface
The invention provides a method for identifying nitriding and nitrocarburizing heat treatment, which comprises the following specific steps:
1) Establishing a standard working curve of carbon element
The nitriding and nitrocarburizing materials are generally medium carbon steel or low carbon steel, and the carbon content is between 0.05 and 1.0 percent. Therefore, a group of standard samples which are similar to the matrix structure and components of the sample to be detected and have gradient carbon content distribution are selected, and the analysis accuracy is improved. The standard samples for spectrum selected by the invention are GSB H40072-94 series 4 blocks and YSB S11273 b-2007GCr15, and the detailed information is shown in Table 2.
TABLE 2 Standard sample C content Standard value (mass fraction,%)
As shown in fig. 5, the measurement of the X-ray intensity value was performed for the standard sample group using an electronic probe. From the intensity of X-ray of K alpha ray system of standard sample and its carbon element content, an intensity-content standard working curve diagram with linear relation is drawn. By using the standard curve, the carbon element content and the distribution state of the sample can be analyzed, and an accurate analysis result can be obtained.
2) Sample preparation
Cutting a test sample by linear cutting, according to the size of an electronic probe sample cabin, requiring that the length of the test sample is less than or equal to 30mm, the width of the test sample is less than or equal to 30mm, and the height of the test sample is less than or equal to 20mm, carrying out coarse grinding on the test sample on a grinding machine after cleaning, grinding off cutting marks of the linear cutting, grinding by using 320#, 600# and 1000# abrasive paper in sequence, polishing a detection surface by using 1 mu m diamond and 0.05 mu m aluminum oxide until no obvious scratch exists, carrying out ultrasonic cleaning in absolute ethyl alcohol for 1min-3min, then carrying out blow-drying, and quickly putting the test sample into the electronic probe sample cabin for analysis and test. And after cleaning, performing coarse grinding on the sample, grinding off cutting marks of linear cutting, grinding by using 320#, 600# and 1000# abrasive paper, polishing a detection surface by using 1-micron diamond and 0.05-micron aluminum oxide, performing ultrasonic cleaning in absolute ethyl alcohol for 1-3 min, drying, and quickly putting into an electronic probe sample cabin for analysis and test.
3) Elemental carbon surface scanning
After the electronic probe is in a stable state, selecting a Mapping analysis mode, selecting a C element as an element to be detected, and setting working conditions of the electronic probe as follows: the acceleration voltage is 15kV, the electron beam current is 100nA, the beam spot min is measured, the test time is 20s, and under the condition, the carbon element analysis efficiency and accuracy are optimal. Finding a white and bright layer in an image observation window of the electronic probe, framing a region containing the white and bright layer, selecting a standard sensitivity curve, and performing surface scanning analysis on carbon elements to obtain a color change surface scanning analysis result of the content of the carbon elements in the framed region and a carbon concentration change curve of a straight line from the surface to the inside.
4) Determination of results
Judging whether the heat treatment mode of the sample is nitriding or nitrocarburizing according to the color brightness difference and the carbon concentration curve of the white bright layer and the matrix: if the color brightness of the white bright layer is higher than that of the matrix and the carbon concentration curve is obviously reduced, the sample can be judged to be subjected to nitrocarburizing treatment; if the color brightness of the white bright layer is consistent with that of the matrix, and the carbon concentration curve is straight and has no obvious reduction, the sample can be judged to be subjected to nitriding treatment.
The method for identifying nitriding and nitrocarburizing heat treatment provided by the invention can solve the problem that the nitriding of parts or the nitrocarburizing heat treatment process cannot be accurately judged, and provides accurate data support for new product design and improvement and promotion of product quality. The method has the advantages that: the method is not limited by the shape and size of the sample, the test can be performed after the metallographic phase of the cross section is polished and dedusted, the sample does not need to be corroded, the operation is simple and convenient, and the result is visual and reliable. Nitriding and nitrocarburizing are two metal material surface strengthening heat treatment processes with similar principles and processes, and both adopt surface strengthening media with similar components. The surface of the component subjected to nitriding and nitrocarburizing treatment can form a layer of white bright layer with equivalent hardness and thickness not more than 0.05mm. Only nitrogen element is permeated into the white bright layer on the surface of the workpiece after nitriding heat treatment, and the carbon element content of the white bright layer and the matrix is not different; the nitrocarburizing heat treatment not only has the infiltration of nitrogen element, but also has the infiltration of carbon element, and the carbon content of the surface white and bright layer is obviously higher than that of the matrix. Based on the difference, the invention judges the heat treatment process of the sample by detecting the difference between the surface white and bright layer and the matrix carbon element. According to the principle of an electronic probe, on a surface scanning image of an element, the color brightness of an area is proportional to the content of the element in the area, namely, the higher the color brightness of a position is, the higher the content of the element in the position is represented. Therefore, the heat treatment mode of the sample is judged to be nitriding or nitrocarburizing according to the color brightness difference and the carbon concentration curve of the white bright layer and the matrix: if the color brightness of the white bright layer is basically consistent with that of the matrix and the carbon concentration curve is straight and has no obvious reduction, the sample can be judged to be subjected to nitriding treatment; if the color brightness of the white bright layer is higher than that of the matrix, and the carbon concentration curve is obviously reduced, the sample can be judged to be subjected to nitrocarburizing treatment.
The above is only a preferred embodiment of the present invention, and is not intended to limit the present invention, and various modifications and changes will occur to those skilled in the art. Any modification, equivalent replacement, or improvement made within the spirit and principle of the present invention should be included in the protection scope of the present invention.
Claims (10)
1. A method for identifying nitriding and nitrocarburizing heat treatment is characterized by comprising the following steps:
acquiring a white bright layer area of the processed sample according to the processed sample;
processing the white bright layer area to obtain the color brightness of the white bright layer and the carbon concentration curve of the white bright layer;
and obtaining the sample treatment type according to the color brightness of the white bright layer and the carbon concentration curve of the white bright layer, and realizing the identification of nitriding and nitrocarburizing heat treatment.
2. The method for discriminating nitriding and nitrocarburizing heat treatment according to claim 1, wherein the method for obtaining the type of sample treatment based on the brightfield color brightness and brightfield carbon concentration curve is as follows:
if the color brightness of the white bright layer is higher than that of the outer matrix of the white bright layer and the carbon concentration curve of the white bright layer is reduced, performing nitrocarburizing treatment on the sample;
and if the color brightness of the white bright layer is consistent with the color brightness of the outer matrix of the white bright layer and the carbon concentration curve of the white bright layer is not changed, the sample is subjected to nitriding treatment.
3. The method for discriminating nitriding and nitrocarburizing heat treatment according to claim 1, wherein the thickness of the albedo region is less than 0.05mm.
4. The method for discriminating nitriding and nitrocarburizing heat treatment according to claim 1, wherein the bright layer region is treated with an electronic probe.
5. The method for discriminating nitriding and nitrocarburizing heat treatment according to claim 4, wherein an electronic probe selects a standard sensitivity curve to perform carbon element scanning analysis, and a curve of white bright layer color brightness and white bright layer carbon concentration is obtained.
6. The method for discriminating nitriding and nitrocarburizing heat treatment according to claim 4, wherein the acceleration voltage of the electron probe is 15kV, the electron beam current is 100nA, and the test time is 20s.
7. Method for the discrimination of nitriding and nitrocarburizing heat treatment according to claim 1, characterized in that the treated sample is obtained by the following method:
cutting the sample, cleaning and roughly grinding the cut sample, and removing the cutting mark of the cutting line; and cleaning the coarsely ground sample in absolute ethyl alcohol, and drying the sample to obtain a processed sample.
8. The method for discriminating nitriding and nitrocarburizing heat treatment according to claim 7, wherein the material of the specimen is carbon steel or low carbon steel.
9. The method for discriminating nitriding and nitrocarburizing heat treatment according to claim 7, wherein the sample is cut by a wire cutting method.
10. The method for discriminating nitriding and nitrocarburizing heat treatment according to claim 7, wherein the rough-ground test piece is cleaned by an ultrasonic method in absolute ethanol.
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