CN110823938A - Method for statistical analysis of TiN and TiC inclusions in steel material - Google Patents
Method for statistical analysis of TiN and TiC inclusions in steel material Download PDFInfo
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- 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
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- G01N23/2252—Measuring emitted X-rays, e.g. electron probe microanalysis [EPMA]
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- G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
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Abstract
The invention discloses a method for statistically analyzing TiN and TiC inclusions in steel materials, which comprises the steps of accurately defining the peak position of N elements and the accurate content of the N elements in the TiN inclusions by using a spectrometer in EPMA (enhanced particle emission spectrometry), establishing a database so as to separate TiN and TiC, applying the established database to automatic inclusion detection and analysis, rapidly defining and analyzing the TiN and TiC inclusions in the steel materials by using the AFA characteristic analysis function in Explorer, statistically analyzing the size and the number of the inclusions, and analyzing the result in combination with the material organization, the performance, the components and the process, thereby providing effective theoretical support for optimizing the components and improving the process. The method is simple and easy to implement, has no influence of human factors, solves the problems of inaccurate detection result and interference by external factors in the prior art, quickly optimizes the process for producing the steel materials, improves the production efficiency and can save a large amount of cost for companies.
Description
Technical Field
The invention relates to a detection and analysis method for accurately defining and statistically analyzing TiN and TiC inclusions, and belongs to the field of equipment detection and analysis.
Background
Ti is added into the steel material to separate out fine and dispersed TiC particles, the strength of the steel is improved by increasing the number of the fine TiC particles and utilizing the precipitation strengthening effect of the fine TiC particles, and the TiC particles in the wear-resistant steel are combined with Mo element to form (TiMo) C particles which are hard and can increase the wear resistance of the wear-resistant steel. However, Ti has strong chemical activity in molten steel, and is easy to form large-size nitride inclusions with elements such as N, and premature precipitation of TiN has a tendency of aggregation and growth, so that TiN inclusions with large particles and edges and corners are formed in the molten steel, which not only cannot play a role in refining grains, but also can become a fatigue crack source and is unfavorable for wear resistance, so that the formation and the amount of the TiN inclusions need to be controlled, and the harm to steel is reduced. Therefore, accurate statistical analysis of the number, size and distribution of TiN and (TiMo) C particles is very important for wear resistant steels. However, when a sample is analyzed, the surface of the sample is easily carbonized under the action of high voltage, so that the content of C is high, the content of C element in an energy spectrum result is inaccurate, C and N belong to light elements, and the large error of energy spectrum analysis is always a great trouble in industrial analysis, so that the accurate definition and statistics of the quantity, size and form distribution of TiC and TiN particles have great significance for the improvement of wear-resistant steel technology and material performance.
Disclosure of Invention
In view of the problems in the prior art, the present invention provides a method for statistical analysis of TiN and TiC inclusions by using EPMA (electron probe micro-analyzer) and an automatic inclusion analyzer (Explorer4), which can accurately count the types, amounts, sizes and morphological distributions of inclusions, so as to improve and adjust the process according to the inclusion formation rules, and ensure that the material structure and properties meet the requirements. The method has the advantages of no influence of human factors, high statistical analysis speed and accurate and reliable result, can be used as a method for statistical analysis of inclusions in steel materials, and provides technical indexes for adjustment of production processes.
The invention specifically adopts the following technical scheme:
a method for statistical analysis of TiN and TiC inclusions in steel materials by using an electronic probe analyzer and an inclusion automatic analyzer is characterized by comprising the following steps:
step 1: sample preparation
Preparing a sample according to the sample preparation requirement, wherein the sample is in a polished state and does not need to be corroded;
step 2: detection test
2-1, defining relevant parameters of TiN by using a TiN standard sample configured by an electronic probe analyzer, wherein the relevant parameters comprise acceleration voltage, beam spot and the peak position and content of N element, establishing a database, and using the database as a standard for detecting TiN inclusions by using an inclusion automatic analyzer;
2-2, grinding and polishing the sample according to the requirement of an inclusion automatic analyzer, selecting the database established in the step 2-1 to define TiN and TiC inclusions during detection and analysis, and classifying, defining and scanning the Ti-containing inclusions by using a classification rule file;
and step 3: data analysis
And (3) analyzing and processing the data detected and scanned in the step (2), calculating the size, the quantity and the proportion of the TiN inclusions and the (TiMo) C inclusions, combining the result with the material composition process, analyzing the influence of the result on the material structure and the performance, and comparing the optimal composition process.
The invention discloses a method for statistical analysis of TiN and TiC inclusions in steel materials by utilizing an EPMA and inclusion automatic analyzer, which is used for statistical analysis of Ti-containing inclusions in the steel materials. In the prior art, in the process of analyzing inclusions by using an energy spectrum, C and N elements are easily polluted by charges to cause a difference between a result and an actual value, so that the result is difficult to distinguish carbide or nitride, the proportion of the two inclusions in a steel material is difficult to statistically analyze, and the analysis result cannot be used as an accurate reference value to be combined with material components and a process. Aiming at the phenomenon, the method accurately defines the peak position of the N element and the accurate content of the N element in the TiN inclusions by using a spectrometer in the EPMA, establishes a database so as to separate the TiN and the TiC, then applies the established database to the automatic analysis of the inclusions, quickly defines and analyzes the TiN and the TiC inclusions in the steel material by using the AFA characteristic analysis function in an automatic inclusion analyzer, performs statistical analysis on the size and the quantity of the inclusions, combines and analyzes the result with the material organization, the performance, the components and the process, and provides effective theoretical support for optimizing the components and improving the process. The method is simple and easy to implement, has no influence of human factors, solves the problems of inaccurate detection result and interference by external factors in the prior art, quickly optimizes the process for producing the steel materials, improves the production efficiency and can save a large amount of cost for companies.
Drawings
FIG. 1 statistics of the number of inclusion particle sizes;
FIG. 2 inclusion particle composition;
figure 3 ternary phase diagram distribution of inclusion particles.
Detailed Description
The technical solution of the present invention is further described in detail below.
The invention discloses a method for statistically analyzing TiN and TiC inclusions in a steel material by using an electronic probe analyzer (EPMA-1720) and an automatic inclusion analyzer (Explorer4), which is a method for defining and distinguishing TiN and TiC and counting the size, quantity, distribution and other characteristics of the TiN and TiC, and sequentially comprises a sample preparation step, a detection and test step, a data processing and calculation step and a comparative analysis step.
First, sample preparation step
Preparing samples according to the sample preparation requirement of GB/T4930, wherein the flatness and the smoothness of the samples are in accordance with the sample preparation requirement, and the samples are polished and do not need to be corroded;
second, testing the test
1. The N element peak position and the content of TiN in the steel sample are defined by using a standard sample of an EPMA device, the accelerating voltage (the accelerating voltage is set to be 20kV), the beam spot and the like of the EPMA analysis are set, a database is established, and the database is used as a standard for detecting TiN inclusions by using an inclusion automatic analyzer. The database refers to the relevant information of TiN particles defined according to requirements, including N element peak positions and contents, and serves as the basis for TiN definition and statistics in inclusion analysis.
The relevant parameters for establishing TiN are defined according to the TiN content in a standard sample, the peak position and the content of the N element are defined according to the standard sample, because the TiN and the TiC in the test steel are not single TiN and TiC, the TiN particles can also contain a certain amount of C element, and the (TiMo) C particles can also contain a small amount of N element, the content of the N element in the TiN needs to be defined, for example, the content of the N element can be defined as TiN inclusion, and the N content is lower than the content of the N element and is not TiN. Since the C element is easily affected by high charges during analysis in the (TiMo) C particles, it is not recommended to define the content of the C element, but by the contents of Ti and Mo elements. The acceleration voltage, beam spot, etc. are set according to the sample and the analysis requirements.
2. And (3) grinding and polishing the sample according to the requirements of an inclusion automatic analyzer, wherein the sample is required to be flat and clean, TiN inclusions are defined by selecting the database established in the step 1 during detection and analysis, and meanwhile, Ti-containing inclusions in the material are classified, defined and scanned by selecting a proper classification rule file. The classification rule means: TiN: ti is more than 50, N is more than or equal to 10, and (Ti + N) is more than or equal to 90and Mo is less than 8; (TiMo) C: ti 65and N20 and Mo 5and (Ti + Mo) > 80; { unclasified }: counts < 100; { unclasified }: si is more than or equal to 75; the other identified points are Unlasified; wherein the content of each element is mass percent. And scanning the inclusion components by using an energy spectrometer in the inclusion scanning process, classifying the inclusions according to the scanning result and classification rules, and classifying the inclusions into TiN, (TiMo) C and other undefined particles. Because the content of the C element is easy to increase along with charge deposition, and the carbide in the test material contains the Mo element, the (TiMo) C particles in the test material are calculated by replacing the content of the Ti and Mo elements with detection. The statistics of the number and size of TiN and (TiMo) C particles in the super wear-resistant steel in the test are shown in figure 1, the component content is shown in figure 2, and the distribution in a ternary phase diagram is shown in figure 3.
Third step, data analysis step
And analyzing and processing the data detected and scanned in the second step, and calculating the size, the number, the occupied proportion and the like of the TiN inclusions and the (TiMo) C inclusions by utilizing the inclusion classification rules. Wherein, the size of the inclusion measures the distance between two pixel points of the scanned inclusion; the quantity is that the detected impurities of the equipment accord with the classification rule, and the impurities are counted as one impurity if the detected impurities accord with the condition; the ratio of the area occupied is the area of the scanned inclusions to the area of the scanned area. And the data of the quantity, the size, the components and the like of the inclusions obtained according to the analysis result are linked with the precipitation nucleation and the growth behavior of the inclusions, the precipitation and growth processes of the inclusions are analyzed, and the precipitation and growth processes are combined with the influence of the inclusions on the organization and the performance, so that an optimal production scheme meeting the requirements of customers is made.
The size and quantity proportion errors of the TiN and (TiMo) C inclusions detected, calculated and analyzed by the method are small, errors caused by artificial observation factors are avoided, the result is accurate and reliable, the efficiency is high, and a new analysis means and a new analysis method are provided for detecting and analyzing the TiN and (TiMo) C inclusions in the ultrahigh Ti-containing alloy.
In addition to the above embodiments, the present invention may have other embodiments. All technical solutions formed by adopting equivalent substitutions or equivalent transformations fall within the protection scope of the claims of the present invention.
Claims (5)
1. A method for statistical analysis of TiN and TiC inclusions in steel materials by using an electronic probe analyzer and an inclusion automatic analyzer is characterized by comprising the following steps:
step 1: sample preparation
Preparing a sample according to the sample preparation requirement, wherein the sample is in a polished state and does not need to be corroded;
step 2: detection test
2-1, defining relevant parameters of TiN by using a TiN standard sample configured by an electronic probe analyzer, wherein the relevant parameters comprise acceleration voltage, beam spot and the peak position and content of N element, establishing a database, and using the database as a standard for detecting TiN inclusions by using an inclusion automatic analyzer;
2-2, grinding and polishing the sample according to the requirement of an inclusion automatic analyzer, selecting the database established in the step 2-1 to define TiN and TiC inclusions during detection and analysis, and classifying, defining and scanning the Ti-containing inclusions by using a classification rule file;
and step 3: data analysis
And (3) analyzing and processing the data detected and scanned in the step (2), calculating the size, the quantity and the proportion of the TiN inclusions and the (TiMo) C inclusions, combining the result with the material composition process, analyzing the influence of the result on the material structure and the performance, and comparing the optimal composition process.
2. The method for the statistical analysis of TiN and TiC inclusions in steel and iron materials using an electron probe analyzer and an inclusion autoanalyzer according to claim 1, wherein the acceleration voltage is 20 kV.
3. The method for the statistical analysis of TiN and TiC inclusions in steel and iron materials using an electron probe analyzer and an automatic inclusion analyzer as claimed in claim 1, wherein TiC is calculated by substituting the contents of Ti and Mo elements for the test.
4. The method for statistical analysis of TiN and TiC inclusions in steel materials using an electron probe analyzer and an inclusion automatic analyzer as set forth in claim 1, wherein the classification rule file: TiN: ti is more than 50, N is more than or equal to 10, Ti + N is more than or equal to 90, and Mo is less than 8; (TiMo) C: ti 65and N20 and Mo 5and (Ti + Mo) > 80; { unclasified }: counts < 100; { unclasified }: si is more than or equal to 75; the other identified points are Unlasified; wherein the content of each element is mass percent.
5. The method for statistical analysis of TiN and TiC inclusions in steel materials using an electronic probe analyzer and an inclusion automatic analyzer as claimed in claim 1, wherein the step 1 is performed according to the sample preparation requirement of GB/T4930.
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