CN115420743A - Analysis method for inclusions in steel - Google Patents
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Abstract
The invention relates to the technical field of analysis and detection of inclusions in steel materials, in particular to an analysis method of inclusions in steel, which comprises the following steps: the method comprises the following steps: preparing a sample; step two: welding; step three: and (4) observing and evaluating the inclusions. The method for analyzing the inclusions by adopting the 'floaters' of the welding molten pool not only can reflect the total amount information of the inclusions, but also has relatively simple and convenient operation and low cost, can detect samples with larger sizes, and can adjust the sizes of different welding molten pools according to welding heat input, namely the analysis volume can be flexibly adjusted. The total amount of oxide inclusions in a certain volume of a steel sample can be effectively represented.
Description
Technical Field
The invention relates to the technical field of analysis and detection of inclusions in steel materials, in particular to an analysis method of inclusions in steel.
Background
As is well known, the nonmetallic inclusion is used as an important index for measuring the quality of steel, and various state factors such as type, composition, form, content, size, distribution and the like all affect the performance of the steel, and particularly greatly harm the mechanical property, corrosion resistance and surface quality of the steel. Therefore, in the research of smelting process, the inclusion control technology is an important research content. Therefore, the technique of characterizing and detecting inclusions is also very important, and people need to accurately and rapidly detect inclusions, understand the sources and formation mechanisms of the inclusions, and then control and remove the inclusions through an effective method.
In order to evaluate the number, size, form, distribution and composition of inclusions, various detection techniques are applied in production and scientific research. There are several categories of inclusion analysis methods: there are about 30 methods, including macroscopic and microscopic methods, physical and chemical methods, qualitative and quantitative methods, direct and indirect methods, two-dimensional plane and three-dimensional space, nondestructive and destructive methods, etc., and these methods have respective characteristics.
The technical means for detecting the inclusions on the section of the steel sample comprise: metallographic microscopes, image analyzers, scanning electron microscopes, electronic probes, etc. The qualitative and quantitative analysis of inclusions by using a metallographic microscope is the most common method and is a traditional two-dimensional detection method.
The metallographic method is to cut, grind and polish a steel block sample to prepare a metallographic sample, and then study the appearance, size, quantity and distribution characteristics of inclusions on a metallographic section under an optical microscope. Because of the characteristics of simplicity, intuition, rapidness and in-situ, the appearance observation of inclusions in steel mostly adopts a metallographic grading technology. The inclusion is studied by metallographic specimen method on the premise that the inclusion must be exposed and found on the metallographic section. The distribution of the inclusions in the steel in the three-dimensional matrix is random, so that the appearance of the inclusions on the randomly polished gold phase surface has randomness, and the phenomenon of omission is easy to occur by a metallographic method. In addition, because the orientation of the inclusions in the space is different, the same inclusion may also present different shapes and sizes on the gold phase surface, so that the metallographic method is not easy to draw a comprehensive and correct conclusion.
The detection technology of the inclusions in the whole volume of the solid steel sample comprises the following steps: ultrasonic scanning method, mannesmann inclusion analysis method, X-ray CT scanning method, electrolysis method, chemical dissolution (acid dissolution method), electron Beam Melting method (Electron Beam Melting), cold crucible Melting method, and the like. Wherein, an electron beam melting method and a water-cooled crucible remelting method belong to inclusion concentration analysis methods.
Electron beam melting method (EBM): under the vacuum condition, the steel sample is melted by high-energy electron beams, and the inclusion floats to the surface of the molten steel. And the qualitative analysis of the total amount and the composition of the inclusions can be carried out by combining SEM and EDS. The advantages are as follows: the floating efficiency of the inclusions is high, the number of the inclusions on the detection surface is far larger than that of the surface before concentration, and the size of the sample is larger, so that the accuracy is higher; in addition, the impurities are less polluted, and the original state of the impurities can be maintained. The disadvantages are as follows: carbon boiling problems occur with carbon steel, resulting in a reduction in the number of oxides; the low-melting-point inclusions are easy to sinter and agglomerate in the smelting process, so that the difficulty of evaluating the sizes of the inclusions is increased; this equipment is also expensive.
Water cooled crucible remelting process (CCBM): the sample is melted on the cold crucible, and the inclusion particles with various sizes in the sample can float up to the surface of the remelted molten steel in the melting process of the sample, thereby being beneficial to SEM observation. Its advantage is: the analyzed sample can reach 100g, and the result has statistical significance; the melting process is fast; the method can be operated under the condition of argon with certain pressure, so that the problem of carbon boiling is avoided; the collection efficiency of the inclusions is almost the same as that of the electron beam melting method.
The invention mainly aims to find a simple and quick analysis method for inclusions in steel, and can quickly and qualitatively evaluate the overall level of the inclusions in the steel.
Disclosure of Invention
The present invention has been made in view of the above problems, and an object of the present invention is to provide a method for analyzing inclusions in steel.
The purpose of the invention is realized as follows: a method for analyzing inclusions in steel comprises the following steps: the method comprises the following steps: sample preparation: cutting a steel sample to be analyzed into a strip sample with the thickness of 1-10 mm; step two: welding implementation: performing welding operation by adopting a tungsten electrode argon arc welding method; argon with the flow rate of 8-15L/min is adopted for protection; selecting welding current of 80-120A and welding speed of 200-550mm/min by using a welding machine to perform a welding test to form a welding seam; step three: observation and evaluation of inclusions: after the welding test is finished, firstly, macroscopically observing the amount of floating objects on the surface of a welding seam by naked eyes, macroscopically and qualitatively evaluating the total amount of inclusions in steel,
and cutting a welding seam sample containing 'floating objects', observing the aggregation form and distribution of the inclusions under a scanning electron microscope, and analyzing the components of the inclusions by using an X-ray energy spectrometer.
In the first step, a test sample needs to have a flat surface, if the test sample is a plate sample, the test sample is directly cut, and if the test sample is a section bar, a bar material or a pipe material sample, a flat surface needs to be processed to be used as a surface for implementing a welding test; the surface can not have oxidized skin and oil stain, if the oxidized skin exists, the acid cleaning treatment is needed; if the surface is greasy, the sample needs to be cleaned by absolute ethyl alcohol.
And the argon protection in the step two adopts a welding gun gas supply mode or a protection mode that the welding gun does not supply gas and double rows of gas blow are carried out on two sides of the welding seam.
The invention has the beneficial effects that: although the conventional metallographic analysis method for the inclusions in the steel has the characteristics of simplicity, intuition, rapidness and in-situ analysis, the method has the defect that the inclusion is analyzed randomly and has a limited detection field by a two-dimensional surface detection method, only one cross section is detected, and the total amount information of the inclusions cannot be reflected.
The electron beam melting method can reflect the total amount information of the inclusions, but the equipment is expensive, and the detection cost is high.
The method for analyzing the inclusions by adopting the 'floaters' of the welding molten pool not only can reflect the total amount information of the inclusions, but also has relatively simple and convenient operation and low cost, can detect samples with larger sizes, and can adjust the sizes of different welding molten pools according to welding heat input, namely the analysis volume can be flexibly adjusted. The total amount of oxide inclusions in a certain volume of a steel sample can be effectively represented.
Drawings
The invention is further described below with reference to the accompanying drawings.
FIG. 1 is an SEM of macroscopic "floaters" on the weld of a smelter weld coupon (1).
FIG. 2 is an SEM of macroscopic "floaters" on the weld of the A smelter weld coupon (2).
FIG. 3 is a typical spectrum plot of macroscopic "floaters" on the weld of a smelter weld coupon.
FIG. 4 is an SEM of microscopic "floaters" on the weld of a B smelter weld coupon (1).
FIG. 5 is an SEM of microscopic "floaters" on the weld of a B smelter weld coupon (2).
FIG. 6 is a typical spectral plot of microscopic "floaters" on the weld of a B smelter weld coupon.
Fig. 7 is a photograph of nitride inclusions in "floats" on the weld bead (1).
Fig. 8 is a photograph of nitride inclusions in "floats" on the weld bead (2).
Fig. 9 is a plot of the energy spectrum of nitride inclusions in the "float" on the weld bead.
FIG. 10 is a topographical view of "floaters" inclusions (1).
FIG. 11 is a topographical view of "floaters" inclusions (2).
FIG. 12 is a topographical view of "floaters" inclusions (3).
Figure 13 is a graph of typical composition of "float" inclusions.
FIG. 14 is a topographical view of 430 weld surface "floats" (1).
FIG. 15 is a topographical view of 430 weld surface "floats" (2).
FIG. 16 is a topographical view of the weld surface "float" 430 (FIG. 3).
FIG. 17 is a graph of typical composition of 430 weld surface "floaters".
Detailed Description
The technology is a technology for detecting inclusions in the whole volume of a solid steel sample, and is a method for concentrating and analyzing the inclusions in steel.
Under the condition of argon protection, a welding tester is utilized to locally melt the steel sample on the surface of the steel sample by adopting a welding principle to form a welding molten pool, and according to a metallurgical principle, nonmetallic inclusions in the volume of the molten pool float and gather on the surface to form 'floaters' on the surface of the welding molten pool. The amount of these "floaters" is directly related to the total amount of inclusions in the steel, the more such "floaters" and, conversely, the less "floaters". When the steel contains more inclusions, the 'floating objects' on the surface of the welding molten pool can be seen by naked eyes, and if the purity of the steel is higher, the 'floating objects' on the surface of the welding molten pool are not obvious and need to be observed and evaluated by a Scanning Electron Microscope (SEM).
If the 'floating objects' on the surface of the welding molten pool are visible by naked eyes, the severity of the non-metallic inclusions in the steel can be evaluated macroscopically and qualitatively through eye observation, then the welding sample is cut into a proper size, and the qualitative analysis of the quantity and the composition of the inclusions is carried out by utilizing a Scanning Electron Microscope (SEM) and an X-ray energy spectrometer (EDS).
During welding, argon protection is needed to prevent the oxidation of alloy elements in steel, otherwise the number of floating objects on the surface of a welding pool is increased, the components are changed, and the level of inclusions in the steel cannot be truly reflected.
If the quantity of the inclusions in different steel samples is to be evaluated in a comparative way, the welding process parameters are required to be kept constant, and the volume of the formed welding pool is basically consistent.
The technology is very effective in analyzing oxide inclusions in steel, and has limitation on analysis of sulfides (such as MnS) and nitrides because the temperature of a welding pool is very high (generally more than 1500 ℃), mnS and nitrides in the steel can be partially or completely dissolved in the welding melting process, and only a small part of residues can float together with the oxide inclusions to form 'floaters'. Most of oxide inclusions have high melting points and exist in a solid phase in a welding melting pool all the time, and the oxide inclusions are gathered and float up to the surface of a weld bead to form floating objects because the density of the oxide inclusions is less than that of molten steel.
The method utilizes a Tungsten Inert Gas (TIG) welding method to form a welding pool with a certain volume on the surface of a steel sample, impurities in steel can automatically gather and float to the surface of the welding pool according to a metallurgical principle, then naked eye macroscopic observation and scanning electron microscope microscopic observation are combined, the total amount of the impurities is qualitatively evaluated and analyzed, the scanning electron microscope and an X-ray energy spectrometer are utilized to analyze the components of the impurities, and thus the qualitative analysis of the total amount and the components of the impurities in the steel is realized.
The specific implementation operation process can be divided into the following three steps:
1. sample preparation
The steel sample to be analyzed is cut into a piece of sample of suitable dimensions.
In order to facilitate the implementation of a welding test, the sample needs to have a flat surface, if the sample is a plate sample, the sample can be directly cut, and if the sample is a section bar, a bar material or a pipe sample, a flat surface needs to be processed to be used as a welding implementation surface.
The welding surface must not have oxide scale and greasy dirt. If there is an oxide scale, an acid pickling treatment is required. If the surface is greasy, the sample needs to be cleaned by absolute ethyl alcohol.
2. Welding practice
And performing welding operation by adopting a Tungsten Inert Gas (TIG) method.
Argon gas with the flow rate of 8-15L/min is adopted for protection, and the protection mode can adopt a welding gun gas supply mode or a welding gun gas non-supply mode and a protection mode of double-row gas blowing at two sides of a welding line.
And (3) selecting a welding current of 80-120A and a welding speed of 200-550mm/min by using a qualified welding machine to perform a welding test, and forming a welding seam with a certain length. It should be noted that if the thickness of the sample is thin, the welding parameters are selected to ensure that the sample is not welded through, otherwise, the back of the sample is protected by argon.
It should be noted that the thickness of the sample is 1-10mm, if the thickness of the sample is thin (for example, less than 1 mm), the welding current may be less than 80A, and it is ensured that the sample is not welded through, otherwise, the back of the sample is protected by argon.
3. Observation and evaluation of inclusions
After the welding test is finished, the amount of floating objects on the surface of the welding seam is macroscopically observed by naked eyes, and the macroscopic qualitative evaluation is carried out on the total amount of inclusions in the steel.
A weld sample containing 'floating objects' is cut, the aggregation form and distribution of inclusions are observed under a Scanning Electron Microscope (SEM), and the composition analysis of the inclusions is carried out by an X-ray energy spectrometer (EDS).
Example one
Comparative analysis of inclusions in 441 ferritic stainless steel plates produced by different smelters
1. Sample preparation
A. And B, the thickness of the 441 ferrite stainless steel cold-rolled plate produced by two different smelters is 2.3mm, each steel plate with the thickness of 500mm x 100mm is cut, and the surface of the steel plate is cleaned by absolute ethyl alcohol.
2. Welding test
The welding method comprises the following steps: tungsten argon arc welding (TIG)
The type of the welding machine is as follows: under-pine TC-400TX4
Welding parameters are as follows: the welding current is 100A, the welding speed is 500mm/min, and the argon flow is 8L/min.
3. Evaluation of inclusions
The method is characterized in that firstly, the welding seams of two steel plates are straight through naked eyes, the grayish white spots on the welding seams of the A smelting plant can be seen, and the welding seams of the B smelting plant have no macroscopic floating objects, which shows that the total amount of impurities in the steel plates of the B smelting plant is obviously less than that of the A smelting plant, and the purity of the 441 stainless steel produced by the B smelting plant is better.
A plurality of samples containing macroscopic 'floating objects' are cut out and observed and analyzed by a Zeiss EVO18 scanning electron microscope and an Oxford energy spectrometer. FIGS. 1, 2, and 3 are typical SEM photographs and typical energy spectrum curves of macroscopic "floaters" on the weld of the welded samples of the A smelter. The diameters of a plurality of macroscopic 'floaters' on the sample welding bead of the A smelting plant are all more than 1mm, and the purity of the A smelting plant is poor. Typical spectral curves are seen to be mainly oxides of Al, ca, ti.
No macroscopic "floating objects" were found on the weld beads of the B smelter welded specimens, but many "floating objects" were found in the scanning electron microscope observation (see FIG. 4), the number and size of which were much smaller and much smaller than those of the A smelter welded specimens, and the inclusion components were also oxides mainly containing Al, ca and Ti.
Further careful observation and analysis of the "floating objects" on the welding sample weld bead by a scanning electron microscope and an energy spectrometer are carried out, a small amount of nitride impurities with regular shapes are found in the "floating objects" besides a large amount of oxide impurities, the energy spectrum analysis shows that the composite nitride (Ti, nb) N mainly comprises TiN, and the images and the typical energy spectrum curves of the back scattering electron components of the nitride in the welding sample weld bead "floating objects" of the A smelting plant are shown in the figures 7, 8 and 9.
From the observation of the whole welding seam, the quantity of the oxide inclusions is far larger than that of the nitrides, which is mainly because most of the nitrides are dissolved in the welding melting process, ti, nb and N elements are re-dissolved in the welding seam metal, and only part of large-particle nitrides have no time to dissolve and float on the surface of the welding seam to be mixed with oxide floating materials.
Example two
Inclusion analysis of T330TCG enamel steel.
1. Sample preparation
A500mm by 100mm steel plate was cut out from a hot-rolled plate of T330TCG enamel steel 5mm thick, and the surface was cleaned with absolute ethanol.
2. Welding test
The welding method comprises the following steps: argon tungsten arc welding (TIG)
The type of the welding machine is as follows: WS-500 model full digital argon arc welding machine of Beijing times company
Welding parameters are as follows: the welding current is 110A, the welding speed is 300mm/min, and the argon flow is 10L/min.
3. Observation and evaluation of inclusions
More 'floating objects' can be seen on the welding bead observed by naked eyes, which indicates that the purity of the steel plate is poor. A plurality of samples are cut and observed and analyzed by a Zeiss EVO18 scanning electron microscope and an Oxford energy spectrometer. FIGS. 10, 11, 12 and 13 are the appearance and composition curves of "floating" inclusions, and it can be seen that a large number of inclusions, typically Al2O3-CaO composite oxides, are floating on the surface of the weld bead.
EXAMPLE III
430 ferritic stainless steel.
1. Sample preparation
A500mm by 100mm steel plate was cut out from a hot-rolled plate of 430 ferritic stainless steel 4mm thick, and the surface was cleaned with absolute ethanol.
2. Welding test
The welding method comprises the following steps: tungsten argon arc welding (TIG)
The type of the welding machine is as follows: WS-500 model full digital argon arc welding machine of Beijing times company
Welding parameters are as follows: the welding current is 110A, the welding speed is 400mm/min, and the argon flow is 8.5L/min.
3. Evaluation of inclusions
The floating objects can be seen on the welding bead by naked eyes, which indicates that the purity of the steel plate is poor. A plurality of samples are cut and observed and analyzed by a Zeiss EVO18 scanning electron microscope and an Oxford energy spectrometer. FIGS. 14, 15, 16 and 17 are the shape and composition curves of "floating" inclusions, and it can be seen that a large amount of inclusions are accumulated on the surface of the weld bead in a floating manner, and the typical composition is MgO-Al2O3-SiO2-CaO composite silicate inclusions.
The patent provides an analysis method for qualitatively evaluating inclusions in steel simply, conveniently and rapidly. The method is a technology for detecting the inclusions in the whole volume of a solid steel sample, and is a method for concentrating and analyzing the inclusions in the steel. A welding molten pool with a certain volume is formed on the surface of a steel sample by utilizing a Tungsten Inert Gas (TIG) welding method, impurities in steel can automatically gather and float to the surface of the welding molten pool according to a metallurgical principle to form 'floaters' on the surface of a welding line, and qualitative evaluation and analysis on the total amount and the composition of the impurities in the steel are realized through macroscopic observation of the 'floaters', scanning electron microscope microscopic observation and X-ray energy spectrometer component analysis.
The theoretical basis of the method is that a steel sample is locally melted by utilizing the principle of argon tungsten-arc welding, and nonmetallic inclusions in the volume of a molten pool float upwards and gather on the surface according to the metallurgical principle to form 'floaters' on the surface of a welding seam. The amount of these "floaters" is directly related to the total amount of inclusions in the steel. The qualitative evaluation and analysis of the total amount and the composition of inclusions in the steel are realized by macroscopic observation and scanning electron microscope microscopic observation of the floaters and the component analysis of an X-ray energy spectrometer. The method allows rapid and efficient qualitative characterization of the number and composition of non-metallic inclusions in steel by practice of a number of examples.
The above description is only an embodiment of the present invention, but the structural features of the present invention are not limited thereto, and any changes or modifications within the scope of the present invention by those skilled in the art are covered by the present invention.
Claims (3)
1. A method for analyzing inclusions in steel, which is characterized by comprising the following steps: the method comprises the following steps:
the method comprises the following steps: sample preparation: cutting a steel sample to be analyzed into a strip sample with the thickness of 1-10 mm;
step two: and (3) welding implementation: performing welding operation by adopting a tungsten electrode argon arc welding method; argon with the flow rate of 8-15L/min is adopted for protection; selecting welding current of 80-120A and welding speed of 200-550mm/min by using a welding machine to perform a welding test to form a welding seam;
step three: observation and evaluation of inclusions: after the welding test is finished, firstly, macroscopically observing the amount of 'floating objects' on the surface of a welding seam by naked eyes, carrying out macroscopic qualitative evaluation on the total amount of inclusions in steel,
a welding line sample containing 'floating objects' is cut, the aggregation form and distribution of the inclusions are observed under a scanning electron microscope, and the inclusions are analyzed by an X-ray energy spectrometer.
2. The method of analyzing inclusions in steel according to claim 1, wherein: in the first step, a test sample needs to have a flat surface, if the test sample is a plate sample, the test sample is directly cut, and if the test sample is a section bar, a bar material or a pipe material sample, a flat surface needs to be processed to be used as a surface for implementing a welding test; the surface can not have oxidized skin and oil stain, if the oxidized skin exists, the acid cleaning treatment is needed; if the surface is greasy, the sample needs to be cleaned by absolute ethyl alcohol.
3. The method for analyzing inclusions in steel according to claim 1, wherein: and the argon protection in the step two adopts a welding gun gas supply mode or a protection mode that the welding gun does not supply gas and double rows of gas blow are carried out on two sides of the welding seam.
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CN115856004A (en) * | 2023-01-30 | 2023-03-28 | 中航久远科技(北京)有限公司 | Method for predicting deformation capacity of inclusions in 430 ferritic stainless steel in hot rolling process |
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CN115856004A (en) * | 2023-01-30 | 2023-03-28 | 中航久远科技(北京)有限公司 | Method for predicting deformation capacity of inclusions in 430 ferritic stainless steel in hot rolling process |
CN115856004B (en) * | 2023-01-30 | 2023-05-05 | 中航久远科技(北京)有限公司 | Method for predicting 430 deformation capability of inclusion in ferrite stainless steel in hot rolling process |
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