CN115993434A - High-carbon steel inter-crystal oxidation detection method - Google Patents

High-carbon steel inter-crystal oxidation detection method Download PDF

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Publication number
CN115993434A
CN115993434A CN202310091883.0A CN202310091883A CN115993434A CN 115993434 A CN115993434 A CN 115993434A CN 202310091883 A CN202310091883 A CN 202310091883A CN 115993434 A CN115993434 A CN 115993434A
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China
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sample block
detection
inter
carbon steel
sample
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CN202310091883.0A
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Inventor
沈洁
杨艳龙
周志超
赵乃胜
武甲
雷娜
张敬蕊
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Beijing Shougang Co Ltd
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Beijing Shougang Co Ltd
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Priority to CN202310091883.0A priority Critical patent/CN115993434A/en
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Abstract

The application provides a high-carbon steel inter-crystal oxidation detection method, which comprises the following steps: sample selection and machining are carried out on the high-carbon steel plate to be detected, and a sample block of the high-carbon steel plate to be detected is obtained; performing mosaic treatment on the sample block, and performing polishing to obtain a detection sample block; and detecting the detection sample block by using a detection device to obtain the inter-crystal oxidation depth of the detection sample block. The method solves the problem that the detection result has larger deviation when the inter-crystal oxidation detection of the high-carbon steel plate is carried out, and the scheme provided by the method standardizes the inter-crystal oxidation detection condition, reduces the fluctuation of the detection result, improves the accuracy of the inter-crystal oxidation detection result, provides accurate and effective data support for the adjustment of the production process, and improves the quality and market competitiveness of the product.

Description

High-carbon steel inter-crystal oxidation detection method
Technical Field
The application relates to the technical field of steel rolling, in particular to a high-carbon steel inter-crystal oxidation detection method.
Background
Grain boundaries in metals and alloys are derived from regions of irregular arrangement and increased number of crystal defects (vacancies and dislocations), oxygen atoms diffuse faster along the grain boundaries and combine with certain alloying elements to form oxide particles, a phenomenon known as intergranular oxidation, which falls within the category of internal oxidation. The inter-crystal oxidation occurs in the range of tens micrometers on the surface layer of the material, so that the strength and plasticity of the material are greatly reduced, the early failure phenomenon occurs in the use process, and the subsequent processing and forming of the material are directly influenced, so that the inter-crystal oxidation phenomenon in the material production process is strictly controlled, the product quality is ensured, and the customer requirements are met.
At present, the inter-crystal oxidation is not in accordance with the national standard or industry standard, the understanding of the inter-crystal oxidation by each laboratory and the measurement method of the inter-crystal oxidation sample by the detection personnel are different, so that the detection data of each laboratory is not comparable, and the detection result is generally in larger deviation. In order to meet the requirements of high-carbon steel production and subsequent deep processing and use, a set of inter-crystal oxidation detection method needs to be established, inter-crystal oxidation detection conditions are standardized, fluctuation of detection results is reduced, production is guided better, and accurate and effective data support is provided for production process adjustment.
Based on the method, how to adopt an effective method to detect the inter-crystal oxidation of the high-carbon steel plate and ensure the accuracy of detection results and the quality of the high-carbon steel plate is a technical problem to be solved urgently.
Disclosure of Invention
The utility model provides a high carbon steel intergranular oxidation detection method, this application has solved the problem that there is great deviation in the testing result when carrying out high carbon steel sheet intergranular oxidation detection, and the scheme that this application proposed has standardized the intergranular oxidation detection condition, has reduced the fluctuation of testing result, has improved the accuracy of intergranular oxidation testing result, provides accurate effective data support for production technology adjustment, has improved the quality and the market competition of product.
Specifically, the application adopts the following technical scheme:
the embodiment of the application provides a high-carbon steel inter-crystal oxidation detection method, which comprises the following steps: sample selection and machining are carried out on the high-carbon steel plate to be detected, and a sample block of the high-carbon steel plate to be detected is obtained; performing mosaic treatment on the sample block, and performing polishing to obtain a detection sample block; and detecting the detection sample block by using a detection device to obtain the inter-crystal oxidation depth of the detection sample block.
In some embodiments of the present application, based on the foregoing, the method further comprises, prior to subjecting the sample block to the mosaic treatment: and removing a heat affected zone and a cold shearing zone on the sample block.
In some embodiments of the present application, based on the foregoing solution, the performing mosaic treatment on the sample block, and then polishing includes: embedding the sample block by adopting a thermal embedding method or a cold embedding method; and polishing the inlaid sample block according to the principle that the surface of the sample block is free from deformation, scratch, water stain and dirt.
In some embodiments of the present application, based on the foregoing solution, the polishing the sample block after the mosaic treatment includes: and (3) sequentially carrying out coarse grinding, fine grinding and polishing on the sample block by adopting coarse sand paper to fine sand paper.
In some embodiments of the present application, the sample block is polished mechanically based on the foregoing protocol.
In some embodiments of the present application, based on the foregoing solution, the time for polishing the sample block after the mosaic treatment is 2min to 5min.
In some embodiments of the present application, based on the foregoing, the detecting the detection sample block using a detection device includes: and observing the whole side part of one side of the detection sample block by using a detection device, selecting the most severe view field for detection, calculating the average value of the measured values obtained in the most severe place, and taking the average value as the inter-crystal oxidation depth of the detection sample block.
In some embodiments of the present application, based on the foregoing solution, the using a detection device observes the whole of one side edge of the detection sample block, and selects the most severe field of view for detection, where the number of times of detection of the most severe field of view is at least 5.
In some embodiments of the present application, based on the foregoing solution, the deeper the inter-crystal oxidation depth of the detection sample block, the poorer the quality of the high carbon steel plate corresponding to the detection sample block.
In some embodiments of the present application, based on the foregoing solution, after performing mosaic processing on the sample block and polishing, the method further includes: and observing the detection sample block, and judging whether the detection sample block meets the standard of inter-crystal oxidation detection.
According to the technical scheme, the application has at least the following advantages and positive effects:
by adopting the scheme provided by the application, the problem that the detection result has larger deviation when the inter-crystal oxidation detection of the high-carbon steel plate is carried out can be solved.
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For a clearer description of the technical solutions of the present application, the drawings that are needed in the description of the embodiments will be briefly described below, it being obvious that the drawings in the description below are some embodiments of the present invention, and that other drawings may be obtained according to these drawings without inventive effort for a person skilled in the art.
FIG. 1 shows a flow chart of a method for detecting intergranular oxidation of high carbon steel in one embodiment of the present application.
Detailed Description
Example embodiments will now be described more fully with reference to the accompanying drawings. However, the exemplary embodiments may be embodied in many 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 the example embodiments to those skilled in the art.
Furthermore, 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 present application. One skilled in the relevant art will recognize, however, that the aspects of the application can be practiced without one or more of the specific details, or with other methods, components, devices, steps, etc. In other instances, well-known methods, devices, implementations, or operations are not shown or described in detail to avoid obscuring aspects of the application.
The flow diagrams depicted in the figures are exemplary only, and do not necessarily include all of the elements and operations/steps, nor must they be performed in the order described. For example, some operations/steps may be decomposed, and some operations/steps may be combined or partially combined, so that the order of actual execution may be changed according to actual situations.
It should be noted that the terms "first," "second," and the like in the description and claims of the present application and in the above-described figures are used for distinguishing between similar objects and not necessarily for describing a particular sequential or chronological order. It is to be understood that the objects so used may be interchanged where appropriate such that the embodiments of the present application described herein may be implemented in sequences other than those illustrated or described.
In this application, a brief description of the intergranular oxidation of high carbon steel will be given. The inter-crystal oxidation of high carbon steel means: at high temperature, oxygen atoms diffuse from the edges of the material into the steel and form grey-black oxide species distributed along grain boundaries in the range of tens of microns on the surface of the high carbon steel material. The high-carbon steel plate has an intergranular oxidation structure, and the binding force at the grain boundary is very weak, so that the surface of the steel plate is cracked during rolling or post-processing treatment, and the like, and potential safety hazards exist during use. In order to avoid the problems of unqualified quality and the like of the high-carbon steel plate in subsequent use, the rolled high-carbon steel plate needs to be sampled and detected to detect whether the high-carbon steel plate has an inter-crystal oxidation defect or not and whether the quality requirement of the subsequent use is met, and the application provides a high-carbon steel inter-crystal oxidation detection method which can solve the problems.
The implementation details of the technical solutions of the embodiments of the present application are described in detail below:
according to an exemplary embodiment of the present application, there is provided a method for detecting intergranular oxidation of high carbon steel, the method including the steps S1 to S3 as follows:
and S1, selecting and machining a sample of the high-carbon steel plate to be detected to obtain a sample block of the high-carbon steel plate to be detected.
In this application, after the rolling of the high carbon steel sheet is completed, in order to detect whether the high carbon steel sheet has an inter-grain oxidation defect and whether the defect of the high carbon steel sheet satisfies the subsequent use, it is necessary to perform inter-grain oxidation detection on the high carbon steel sheet. Firstly, sample selection and machining are required to be carried out on a high-carbon steel plate to be detected to obtain a sample block of the high-carbon steel plate to be detected, wherein the sample selection can be carried out according to a technical protocol and the requirements of customers to select the position capable of representing the material characteristics, different customers have different quality requirements on the high-carbon steel plate, if the customers possibly have special quality requirements on a certain position of the steel plate, and the steel plate at the corresponding position is selected to be used as the sample block of the high-carbon steel plate to be detected when the sample is sampled.
And S2, performing mosaic treatment on the sample block, and performing polishing to obtain a detection sample block.
In this application, after obtaining the sample block, it is still required to inlay the processing and polish the sample block, because the sample block cut directly on the high-carbon steel plate still can not satisfy the condition of inter-crystal oxidation detection, because inter-crystal oxidation is in the range of tens micrometers on the high-carbon steel plate surface layer, the requirement on the shape of the side portion and the quality of the side portion of the sample is higher, therefore, it is required to inlay the sample block with a protection sample, after inlay the processing, polish the sample block to obtain the detection sample block, and the detection sample block at this time can satisfy the condition of inter-crystal oxidation detection.
And step S3, detecting the detection sample block by using a detection device to obtain the inter-crystal oxidation depth of the detection sample block.
In this application, use detection device to detect after obtaining detect sample piece, detection device can include the microscope, when carrying out the inter-granular oxidation degree of depth that detects the sample piece, carry out inter-granular oxidation degree of depth measurement by corresponding measuring software, use the microscope in detect sample piece's one side limit portion carries out careful observation, when detect sample piece surface begins to appear along the continuous or intermittent different colours of grain boundary coarsening structure of grain boundary and is inter-granular oxidation, and the inter-granular oxidation degree of depth is measured (inter-granular oxidation degree of depth is the vertical distance that disappears from high carbon steel sheet surface to the grain boundary coarsening structure) through inter-granular oxidation degree of depth detection device, can select the most serious visual field to carry out a lot of measurements for guaranteeing measuring result's accuracy.
In one embodiment of the present application, before the sample block is subjected to the mosaic treatment, the method further comprises: and removing a heat affected zone and a cold shearing zone on the sample block.
In this application, before will the sample piece is inlay the processing, still need get rid of heat affected zone and cold shearing district on the sample piece, in order to guarantee the accuracy of follow-up inter-grain oxidation degree of depth testing result and be convenient for high-carbon steel sheet more conveniently detect, can use equipment such as plate shearing machine, sawing machine, milling machine or wire cut lathe to cut into size (length x width) 20mm (can also cut into other sizes, this application does not do special limit to this, can adjust according to actual conditions) the cubic that will wait for the high-carbon steel sheet to be detected, can leave heat affected zone or cold shearing district in the cutting place of sample piece when cutting, if not get rid of, will influence the smooth going on of follow-up detection and the accuracy of testing result.
In one embodiment of the present application, the embedding treatment and polishing of the sample block include:
and inlaying the sample block by adopting a thermal inlaying method or a cold inlaying method.
And polishing the inlaid sample block according to the principle that the surface of the sample block is free from deformation, scratch, water stain and dirt.
In the application, embedding is an important link in the preparation process of metallographic samples, and is an indispensable procedure especially for some samples which are tiny, irregular in shape, need to protect edges and need to be polished automatically. According to the technical scheme, the sample block can be subjected to mosaic treatment by a hot mosaic method or a cold mosaic method according to customer requirements and material requirements and laboratory specific conditions. After the sample block is inlaid, polishing the sample block, so that the surface of the polished sample block has the effects of no deformation, no scratch, no water stain and no dirt.
In one embodiment of the present application, the polishing the sample block after the mosaic treatment includes: and (3) sequentially carrying out coarse grinding, fine grinding and polishing on the sample block by adopting coarse sand paper to fine sand paper.
In one embodiment of the present application, the sample block is polished mechanically.
In one embodiment of the present application, the time for polishing the sample block after the mosaic treatment is 2min to 5min.
In this application, when carrying out the mill and throw to the sample piece, can adopt by coarse sand paper to fine sand paper to carry out the coarse grinding in proper order, fine grinding and polishing to the sample piece for the sample piece surface after the mill throws reaches the effect that does not have deformation, no mar, no water stain, no filth. Because the edge quality of the sample block is required to be high in the grinding and polishing process, mechanical polishing is adopted when the sample block is polished to ensure the analysis effect, and the time can be controlled to be within 2-5 min when the sample block is ground and polished.
In one embodiment of the present application, the detecting the detection sample block using the detection device includes:
and observing the whole side part of one side of the detection sample block by using a detection device, selecting the most severe view field for detection, calculating the average value of the measured values obtained in the most severe place, and taking the average value as the inter-crystal oxidation depth of the detection sample block.
In one embodiment of the present application, the detecting device is used to observe the whole of one side edge of the detected sample block, and the most severe field of view is selected for detection, where the number of times of detection of the most severe field of view is at least 5.
In this application, when the detection device is used to perform random detection on the detection sample, the microscope may be used to observe the whole morphology of the detection sample block at 100 times of the microscope, determine that the morphology of the edge of the detection sample block is not deformed, is not scratched, is not water-stained, is not polluted, and is gradually amplified from low power to high power to 500 times or 1000 times, carefully observe the edge of one side of the detection sample block, when the surface of the detection sample block starts to appear grain boundary coarsening structures with different colors continuously or intermittently along the grain boundary, that is, inter-grain oxidation, the most severe field of view is selected for detection, then the inter-grain oxidation depth of the most severe field of view is measured by inter-grain oxidation measurement software (i.e. the vertical distance from the surface of the high-carbon steel plate to the coarsening structure), calculate the average value of the measured value obtained by the detection, take the average value as the inter-grain oxidation depth of the detection sample block, measure the accuracy of the measured result at random, the number of times is generally at least 5, and for the measurement result pursued more accurately, the number of times of measurement can be calculated, and the number of times of measurement can be increased more accurately, and the measurement result is obtained more and the number of times is calculated.
In the application, for a part of critical materials or a product with strict requirements on inter-crystal oxidation, it is necessary to measure the depth of inter-crystal oxidation at the deepest part of the deepest part, because different materials have different tolerance on inter-crystal oxidation defects, and for a part of critical materials or a product with strict requirements on inter-crystal oxidation, customers have different product quality requirements, it is necessary to measure the depth of inter-crystal oxidation at the deepest part of the product, so as to determine whether the depth of inter-crystal oxidation at the deepest part of the product meets the quality requirements of the critical materials or the product with strict requirements on inter-crystal oxidation, and avoid products which do not meet market requirements from flowing into the market.
In the method, the oxide morphology at the grain boundary can be accurately observed by selecting and amplifying 500-5000 multiplying power according to customer demands or product demands, the depth of an inter-crystal oxide layer is measured, and the inter-crystal oxidation is subjected to micro-region component analysis by an energy spectrometer to determine whether the defect is caused by the inter-crystal oxidation.
In one embodiment of the present application, the deeper the inter-crystal oxidation depth of the test sample block, the poorer the quality of the high carbon steel sheet corresponding to the test sample block.
In one embodiment of the present application, after the sample block is subjected to mosaic treatment and then polished to obtain a detection sample block, the method further includes: and observing the detection sample block, and judging whether the detection sample block meets the standard of inter-crystal oxidation detection.
In this application, after the sample block is inlaid and polished, after the sample block is obtained, the sample block is detected, and then the sample block is observed, so as to determine whether the sample block meets the standard of inter-crystal oxidation detection, the whole morphology of the sample block can be observed in a microscope 100 times earlier by using a microscope, it is determined that the edge morphology of the sample block is free from deformation, scratch, water stain, dirt and the like, and if the sample block is found not to meet the standard of inter-crystal oxidation detection, the sample block is required to be sampled again, inlaid and polished.
According to the technical scheme, the application has at least the following advantages and positive effects:
firstly, adopt the scheme that this application provided, can solve the problem that there is great deviation in the testing result when carrying out high-carbon steel sheet intergranular oxidation detection, the scheme that this application provided standardizes the intergranular oxidation detection condition, has reduced the fluctuation of testing result, has improved the accuracy of intergranular oxidation testing result, provides accurate effectual data support for the production technology adjustment, has improved the quality and the market competition of product.
Secondly, by adopting the scheme provided by the application, the detection conditions of the inter-crystal oxidation are standardized, the inter-crystal oxidation sample measurement method of laboratory inspectors is unified, the difference of the inspection results is reduced, the consistency of the detection results is ensured, the product quality is further improved, the production is effectively guided, accurate and effective data support is provided for product process adjustment and scientific research product research and development, and further the requirements of customers on the subsequent deep processing molding and use of materials are met.
Thirdly, adopt the scheme that this application provided, through carrying out high carbon steel sheet intergranular oxidation detection to the accurate judgement of high carbon steel sheet quality has avoided not meeting the product inflow market of market demand, has improved the quality and the market competition of product.
Fourth, by adopting the scheme provided by the application, a tester can select different methods to measure the inter-crystal oxidation depth of the material according to actual conditions so as to obtain more accurate and stable measurement results.
While the present application has been described with reference to several exemplary embodiments, it is understood that the terminology used is intended to be in the nature of words of description and illustration rather than of limitation. As the present application may be embodied in several forms without departing from the spirit or essential attributes thereof, it should be understood that the above-described embodiments are not limited by any of the details of the foregoing description, but rather should be construed broadly within its spirit and scope as defined in the appended claims, and therefore all changes and modifications that fall within the metes and bounds of the claims, or equivalence of such metes and bounds are therefore intended to be embraced by the appended claims.

Claims (10)

1. A method for detecting the intergranular oxidation of high-carbon steel, which is characterized by comprising the following steps:
sample selection and machining are carried out on the high-carbon steel plate to be detected, and a sample block of the high-carbon steel plate to be detected is obtained;
performing mosaic treatment on the sample block, and performing polishing to obtain a detection sample block;
and detecting the detection sample block by using a detection device to obtain the inter-crystal oxidation depth of the detection sample block.
2. The method of claim 1, wherein prior to subjecting the sample block to the tessellation process, the method further comprises:
and removing a heat affected zone and a cold shearing zone on the sample block.
3. The method of claim 2, wherein the subjecting the sample block to a mosaic treatment followed by polishing comprises:
embedding the sample block by adopting a thermal embedding method or a cold embedding method;
and polishing the inlaid sample block according to the principle that the surface of the sample block is free from deformation, scratch, water stain and dirt.
4. A method according to claim 3, wherein said polishing of said mosaic-treated sample mass comprises:
and (3) sequentially carrying out coarse grinding, fine grinding and polishing on the sample block by adopting coarse sand paper to fine sand paper.
5. The method of claim 4, wherein the sample block is polished mechanically.
6. The method of claim 5, wherein the polishing time for the mosaic treatment of the sample block is 2min to 5min.
7. The method of claim 6, wherein detecting the test sample block using a detection device comprises:
and observing the whole side part of one side of the detection sample block by using a detection device, selecting the most severe view field for detection, calculating the average value of the measured values obtained in the most severe place, and taking the average value as the inter-crystal oxidation depth of the detection sample block.
8. The method of claim 7, wherein the detecting means is used to observe the whole of a side portion of the sample block, and the most severe field of view is selected for detection, and the number of times of detection of the most severe field of view is at least 5.
9. The method of claim 8, wherein the deeper the inter-crystal oxidation depth of the test sample pieces, the poorer the quality of the high carbon steel sheet corresponding to the test sample pieces.
10. The method of claim 1, wherein after the sample block is subjected to a mosaic treatment and then polished to obtain a test sample block, the method further comprises:
and observing the detection sample block, and judging whether the detection sample block meets the standard of inter-crystal oxidation detection.
CN202310091883.0A 2023-01-28 2023-01-28 High-carbon steel inter-crystal oxidation detection method Pending CN115993434A (en)

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Application Number Priority Date Filing Date Title
CN202310091883.0A CN115993434A (en) 2023-01-28 2023-01-28 High-carbon steel inter-crystal oxidation detection method

Applications Claiming Priority (1)

Application Number Priority Date Filing Date Title
CN202310091883.0A CN115993434A (en) 2023-01-28 2023-01-28 High-carbon steel inter-crystal oxidation detection method

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Publication Number Publication Date
CN115993434A true CN115993434A (en) 2023-04-21

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Application Number Title Priority Date Filing Date
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