CN115236110A - Precision measurement method for micro-area carbon concentration distribution of gear carburization part - Google Patents
Precision measurement method for micro-area carbon concentration distribution of gear carburization part Download PDFInfo
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- CN115236110A CN115236110A CN202210865221.XA CN202210865221A CN115236110A CN 115236110 A CN115236110 A CN 115236110A CN 202210865221 A CN202210865221 A CN 202210865221A CN 115236110 A CN115236110 A CN 115236110A
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- G—PHYSICS
- G01—MEASURING; TESTING
- G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
- G01N23/00—Investigating or analysing materials by the use of wave or particle radiation, e.g. X-rays or neutrons, not covered by groups G01N3/00 – G01N17/00, G01N21/00 or G01N22/00
- G01N23/22—Investigating or analysing materials by the use of wave or particle radiation, e.g. X-rays or neutrons, not covered by groups G01N3/00 – G01N17/00, G01N21/00 or G01N22/00 by measuring secondary emission from the material
- G01N23/225—Investigating or analysing materials by the use of wave or particle radiation, e.g. X-rays or neutrons, not covered by groups G01N3/00 – G01N17/00, G01N21/00 or G01N22/00 by measuring secondary emission from the material using electron or ion
- G01N23/2251—Investigating or analysing materials by the use of wave or particle radiation, e.g. X-rays or neutrons, not covered by groups G01N3/00 – G01N17/00, G01N21/00 or G01N22/00 by measuring secondary emission from the material using electron or ion using incident electron beams, e.g. scanning electron microscopy [SEM]
- G01N23/2252—Measuring emitted X-rays, e.g. electron probe microanalysis [EPMA]
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- G—PHYSICS
- G01—MEASURING; TESTING
- G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
- G01N23/00—Investigating or analysing materials by the use of wave or particle radiation, e.g. X-rays or neutrons, not covered by groups G01N3/00 – G01N17/00, G01N21/00 or G01N22/00
- G01N23/22—Investigating or analysing materials by the use of wave or particle radiation, e.g. X-rays or neutrons, not covered by groups G01N3/00 – G01N17/00, G01N21/00 or G01N22/00 by measuring secondary emission from the material
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Abstract
The embodiment of the invention provides a precision measurement method for micro-area carbon concentration distribution of a gear carburized part, which relates to the technical field of heat treatment. Compared with the prior art, the method can combine the tissue morphology with component analysis to analyze the line distribution and the surface distribution of elements, and accurately reflect the carburization concentration of the carburized layer.
Description
Technical Field
The invention relates to the technical field of heat treatment, in particular to a precision measurement method for micro-area carbon concentration distribution of a gear carburized part.
Background
The traditional method for measuring the carburization method comprises a chemical method (a stripping method), a metallographic method and an effective hardened layer depth method. The chemical method is one of accurate methods for measuring the total depth of a carburized layer, but the layer-by-layer analysis is required, the process is complicated, the method is not suitable for the carburized layer analysis of irregular formed parts, the carburized layer measured by the metallographic method is equivalent to the distance from an original structure to the surface, sometimes the structure boundary is not obvious, or the thickness of the carburized layer is too thick, and the metallographic method is not suitable. The effective case depth method, according to the provisions of GB/T9450-2005, the case depth is the vertical distance from the surface of the part to a point where the Vickers hardness is 550HV 1. The above 3 methods for determining the carburized layer have advantages and disadvantages, but cannot conveniently and quickly obtain the total thickness of the carburized layer and the carbon content change of the carburized layer from the surface to the center.
Disclosure of Invention
The invention aims to provide a method for precisely measuring the micro-area carbon concentration distribution of a gear carburization part, which can combine the structure morphology with component analysis to analyze the line distribution and the surface distribution of elements and accurately reflect the carburization concentration of a carburization layer.
Embodiments of the invention may be implemented as follows:
in a first aspect, the invention provides a method for precisely measuring the micro-area carbon concentration distribution of a gear carburized part, which comprises the following steps:
setting a calibration curve of the electronic probe;
pretreating a sample to be detected;
measuring the carbon concentration of a sample to be measured by using the electronic probe;
and carrying out quantitative conversion on the carbon concentration of the sample to be detected according to the calibration curve to obtain a carbon concentration distribution curve.
In an alternative embodiment, the step of pretreating the sample to be tested comprises:
preparing a sample to obtain a polished sample to be detected;
and cleaning the sample to be detected.
In an alternative embodiment, the step of preparing the sample to obtain the polished sample to be tested includes:
cutting a metallographic specimen;
and (3) thermally inlaying by using conductive inlaying powder, and obtaining a polished sample to be detected according to the gold phase sample preparation sequence.
In an alternative embodiment, the step of washing the sample to be tested includes:
and cleaning carbon pollution brought by the surface sample preparation process of the sample to be detected by using a plasma cleaning instrument.
In an alternative embodiment, the cleaning gas of the plasma cleaner is a combination of hydrogen and oxygen.
In an alternative embodiment, the step of setting a calibration curve for the electron probe comprises:
and setting the node parameters of the electronic probe according to the material components of the sample to be detected, and drawing a standard curve.
In an alternative embodiment, the sample to be tested is 20CrMnTi.
In an alternative embodiment, the node parameter selection comprises: pure iron with a carbon content of 0.003%;20CrMnTi, the carbon content of the matrix is 0.227 percent; the carbon content of the carburized surface is as follows: 0.68 percent.
In an alternative embodiment, the electron probe has an acceleration voltage of 15Kv and a beam current of 100nA.
In an optional embodiment, the sample to be measured is a gear sample of a reduction gear.
The beneficial effects of the embodiment of the invention include, for example:
the embodiment of the invention provides a precision measurement method for micro-area carbon concentration distribution of a gear carburized part, which comprises the steps of firstly setting a calibration curve of an electronic probe, then measuring a preprocessed sample to be measured through the electronic probe, and quantitatively converting the carbon concentration of the sample to be measured according to the calibration curve, thereby obtaining a distribution curve of the carbon concentration and measuring the carbon concentration distribution from the surface to the center of the sample. Compared with the prior art, the method can combine the tissue morphology with the component analysis, perform the line distribution and surface distribution analysis of elements, and accurately reflect the carburization concentration of the carburization layer.
Drawings
In order to more clearly illustrate the technical solutions of the embodiments of the present invention, the drawings needed to be used 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 for those skilled in the art, other related drawings can be obtained according to the drawings without inventive efforts.
FIG. 1 is a block diagram of the steps of the method for precisely measuring the micro-area carbon concentration distribution of a gear carburized part provided by the invention;
FIG. 2 is a schematic illustration of a calibration curve;
fig. 3 is a carbon concentration distribution diagram.
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 present invention, it should be noted that if the terms "upper", "lower", "inside", "outside", etc. indicate an orientation or a positional relationship based on that shown in the drawings or that the product of the present invention is used as it is, this is only for convenience of description and simplification of the description, and it does not indicate or imply that the device or the element referred to must have a specific orientation, be constructed in a specific orientation, and be operated, and thus should not be construed as limiting the present invention.
Furthermore, the appearances of the terms "first," "second," and the like, if any, are used solely to distinguish one from another and are not to be construed as indicating or implying relative importance.
As disclosed in the background art, the carburized concentration of a sample is generally measured by a chemical method, a metallographic method, and an effective hardened layer depth method in the prior art. The chemical method is one of accurate methods for measuring the total depth of a carburized layer, but the layer-by-layer analysis is required, the process is complicated, the method is not suitable for the carburized layer analysis of irregular formed parts, the carburized layer measured by the metallographic method is equivalent to the distance from an original structure to the surface, sometimes the structure boundary is not obvious, or the thickness of the carburized layer is too thick, and the metallographic method is not suitable. The effective case depth method, according to the provisions of GB/T9450-2005, the case depth is the vertical distance from the surface of the part to a point where the Vickers hardness is 550HV 1.
For the gear part, because the gear belongs to an irregular part, a chemical method (stripping) test cannot be carried out; the microstructure of the carburized layer is observed by a metallographic method, the surface layer is acicular martensite, the residual austenite and the granular carbide, the core part is lath martensite, when the depth of the carburized layer is measured by the metallographic method, the observation multiple is 100X, the depth of the carburized layer is not more than 1mm, and when the depth of the carburized layer is measured by the metallographic method, the error measured by the metallographic method is large, and accurate carbon concentration distribution cannot be distinguished.
In order to solve the above problems, the present invention provides a novel carburization method using an electron probe (EMPA) that can combine the morphology of the tissue with the analysis of the composition and can perform the analysis of the line distribution and the area distribution of the elements. It should be noted that the features of the embodiments of the present invention may be combined with each other without conflict.
DETAILED DESCRIPTION OF EMBODIMENT (S) OF INVENTION
Referring to fig. 1, the present embodiment provides a method for precisely measuring the micro-area carbon concentration distribution of a gear carburized part, which can combine the tissue morphology with the component analysis to perform the line distribution and surface distribution analysis of elements, and accurately reflect the carburization concentration of a carburized layer.
The method for precisely measuring the micro-area carbon concentration distribution of the gear carburized part is used for measuring the carburized concentration distribution of a gear of a speed reducer. Of course, the speed reducer gear is merely described here as an example, and does not serve a limiting function.
The method for precisely measuring the micro-area carbon concentration distribution of the gear carburized part comprises the following steps of:
s1: a calibration curve for the electron probe is set.
Specifically, it is necessary to set an electron probe, and since the electron probe is an apparatus for analyzing the composition of a micro-area by using a characteristic X-ray generated after a sample is acted on by an electron beam, qualitative and quantitative analysis can Be performed on the electron probe except for a few light elements such as H, he, li, be, etc., and also for elements after U element. It can only analyze chemical composition by itself and cannot directly determine the carbon concentration distribution. The electron probe works far away from the point that an extremely narrow electron beam which is accelerated and focused is used as a probe to excite a certain micro area in a sample to emit characteristic X rays, and the wavelength and the intensity of the X rays are measured, so that the elements in the micro area can be qualitatively analyzed. Conventional line analysis of the electronic probe belongs to the category of qualitative analysis, content change of element distribution cannot be intuitively obtained, and quantitative conversion of line analysis can be performed by using a calibration curve in the embodiment, so that the content of the element distribution can be intuitively read.
When a calibration curve is actually set, node parameters of the electronic probe need to be set according to material components of a sample to be measured, and a standard curve is drawn. Specifically, the sample that awaits measuring is the gear tooth sample of speed reducer, and the sample material that awaits measuring in this embodiment is 20CrMnTi, and node parameter selection includes: pure iron with a carbon content of 0.003%;20CrMnTi, the carbon content of the matrix is 0.227 percent; the carbon content of the carburized surface is as follows: the calibration curve for 0.68% carbon is shown in FIG. 2.
In this example, the acceleration voltage of the electron probe is 15Kv, and the beam current is 100nA.
It should be noted that, in order to eliminate the interference of the matrix components, a calibration curve may be prepared according to the gear material components, and the calibration curve is drawn by using pure iron (C: 0.003%), 20CrMnTi (matrix C: 0.227%), and the C content of the carburized surface (C: 0.68%), and the parameters of the electronic probe are as follows: the accelerating voltage is 15Kv, and the beam current is 100nA.
S2: and (4) pretreating a sample to be detected.
Specifically, a sample to be measured in a polished state is first prepared, and then the sample to be measured is cleaned. In actual operation, firstly, a carburized metallographic specimen is cut, then, conductive embedding powder is used for hot embedding, and a polished sample to be detected is obtained according to the gold phase sample preparation sequence. The carbon pollution brought by the surface sample preparation process of the sample to be detected can be cleaned by using the plasma cleaning instrument, and the cleaning gas of the plasma cleaning instrument is the combination of hydrogen and oxygen.
It should be noted that in this embodiment, the chemical component 20CrMnTi of the speed reducer gear is carburized, then the metallographic sample of the tooth portion is cut, and is hot-inlaid with conductive inlaying powder, and the sample to be measured in a polished state is obtained according to the conventional metallographic sample preparation sequence. Cleaning carbon pollution brought by sample preparation process on sample surface by using plasma cleaning instrument, and selecting gas H 2 /O 2 And (4) combining.
S3: and measuring the carbon concentration of the sample to be measured by using an electronic probe, and quantitatively converting the carbon concentration of the sample to be measured according to the calibration curve to obtain a carbon concentration distribution curve.
Specifically, the electronic probe is subjected to quantitative conversion through a calibration curve, so that the carbon concentration distribution from the surface of the gear to the core of the gear is measured. The calibration curve is reasonably set according to different materials, and the carbon content/carbon concentration corresponding to the thickness can be intuitively obtained by utilizing the quantitative conversion of the calibration curve, as shown in fig. 3.
It is worth noting that in the actual measurement, the line scan is carried out from the carburized part surface to the substrate until the curve is relatively flat and tends to be stable, and finally the results of the line analysis are quantified through special transformation. The thickness of the carburized layer and the change of the carbon content of the carburized layer from the surface to the center can be directly obtained from curve data, and the result can be used as a proper basis for measuring the carburization process.
According to the precise measurement method for the micro-area carbon concentration distribution of the gear carburized part, line scanning is carried out on a matrix from a carburized surface through an electronic probe line analysis function until a curve is relatively flat and tends to be stable. According to the material characteristics, in order to reduce the interference of trace elements, a standard curve is prepared, and finally, the results of line analysis are quantified through special transformation. The thickness of the carburized layer and the carbon content change of the carburized layer from the surface to the center can be directly obtained from curve data, and the result can be used as a basis for judging whether the carburization process is proper or not. Meanwhile, the method is rapid, convenient and accurate, each 1um step is scanned, and the detection period of the distance from the surface to the core (0-1.4 mm) is only 18 minutes.
In summary, the embodiment of the present invention provides a method for precisely measuring the micro-area carbon concentration distribution of a gear carburized part, which includes setting a calibration curve of an electronic probe, measuring a pre-processed sample to be measured by the electronic probe, and quantitatively converting the carbon concentration of the sample to be measured according to the calibration curve, thereby obtaining a carbon concentration distribution curve and measuring the carbon concentration distribution from the surface to the center of the sample. Compared with the prior art, the method can combine the tissue morphology with the component analysis, perform the line distribution and surface distribution analysis of elements, and accurately reflect the carburization concentration of the carburization layer.
The above description is only for the specific embodiment of the present invention, but the scope of the present invention is not limited thereto, and any changes or substitutions that can be easily conceived by those skilled in the art within the technical scope of the present invention are included in the scope of the present invention. Therefore, the protection scope of the present invention shall be subject to the protection scope of the claims.
Claims (10)
1. A method for precisely measuring the micro-area carbon concentration distribution of a gear carburized part is characterized by comprising the following steps of:
setting a calibration curve of the electronic probe;
pretreating a sample to be detected;
and determining a sample to be detected by using the electronic probe, and quantitatively converting the carbon concentration of the sample to be detected according to the calibration curve to obtain a carbon concentration distribution curve.
2. The method for precisely measuring the micro-area carbon concentration distribution of the gear carburized part according to claim 1, characterized in that the step of pretreating a sample to be measured comprises:
preparing a sample to obtain a polished sample to be detected;
and cleaning the sample to be detected.
3. The method for precisely measuring the micro-area carbon concentration distribution of the gear carburized part according to claim 2, characterized in that the step of preparing a sample to obtain a polished sample to be measured comprises:
cutting a metallographic specimen;
and (3) carrying out hot inlaying by using conductive inlaying powder, and obtaining a polished sample to be detected according to the gold phase sample preparation sequence.
4. The method for precisely measuring the micro-area carbon concentration distribution of the gear carburized part according to claim 2, characterized in that the step of cleaning the sample to be measured comprises:
and cleaning carbon pollution brought by the surface sample preparation process of the sample to be detected by using a plasma cleaning instrument.
5. The method for precisely measuring the micro-zone carbon concentration distribution in the gear carburized part according to claim 4, characterized in that the cleaning gas of the plasma cleaning apparatus is a combination of hydrogen and oxygen.
6. The method of precisely measuring the micro-zone carbon concentration distribution of a gear carburized part according to claim 1, characterized in that the step of setting a calibration curve of an electronic probe comprises:
and setting the node parameters of the electronic probe according to the material components of the sample to be detected, and drawing a standard curve.
7. The method for precisely measuring the micro-area carbon concentration distribution of the gear carburized part according to claim 6, characterized in that the sample to be measured is 20CrMnTi.
8. The method of precisely measuring the micro-zone carbon concentration distribution of a gear carburized part according to claim 7, characterized in that the nodal parameters comprise: pure iron with a carbon content of 0.003%;20CrMnTi, the carbon content of the matrix is 0.227 percent; the carbon content of the carburized surface is as follows: 0.68 percent.
9. The method for precisely measuring the micro-area carbon concentration distribution in the gear carburized part according to claim 7, characterized in that the acceleration voltage of the electronic probe is 15Kv and the beam current is 100nA.
10. The method for precisely measuring the micro-area carbon concentration distribution of the gear carburized part according to claim 1, characterized in that the sample to be measured is a tooth sample of a carburized reduction gear.
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Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
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| CN116306059A (en) * | 2023-05-25 | 2023-06-23 | 中国机械总院集团北京机电研究所有限公司 | Method for rapidly calculating carbon concentration distribution in pulse carburizing process |
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Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
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| CN116306059A (en) * | 2023-05-25 | 2023-06-23 | 中国机械总院集团北京机电研究所有限公司 | Method for rapidly calculating carbon concentration distribution in pulse carburizing process |
| CN116306059B (en) * | 2023-05-25 | 2023-08-29 | 中国机械总院集团北京机电研究所有限公司 | Method for rapidly calculating carbon concentration distribution in pulse carburizing process |
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