CN110554019B - Method for judging distribution uniformity of oxide scale layer on surface of threaded wire rod steel - Google Patents
Method for judging distribution uniformity of oxide scale layer on surface of threaded wire rod steel Download PDFInfo
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Abstract
The invention discloses a method for judging the distribution uniformity of an iron oxide scale layer on the surface of a spiral steel wire rod, which comprises the following steps: s1, cutting the sample, wherein the cutting length of the sample is 3-5 CM; s2, placing the sample into a Raman spectrum measuring device to be clamped; s3, correcting the Raman spectrometer, and measuring the surface of the sample after correction; the Raman spectrum analysis of the scale on the surface of the wire rod steel is realized, the sample preparation is not needed, the in-situ nondestructive test of the sample can be carried out, and the real state of the scale on the surface of the sample can be objectively reflected; the invention designs a novel Raman spectrum measuring device, which can better fix the wire rod steel, flatly place the wire rod steel on a sample table, can measure Raman characteristic peaks of iron scales on all surfaces of the sample by rotating the sample, can judge the uniformity of the distribution of the iron scales of the wire rod steel by counting the peak height values of the characteristic peaks, and lays a foundation for the subsequent storage of the wire rod steel or the further protection of the rust-prone part.
Description
Technical Field
The invention belongs to the technical field of detection of a spiral steel bar, and particularly relates to a method for judging the distribution uniformity of an iron oxide scale layer on the surface of the spiral steel bar.
Background
Scale refers to a layer of iron metal oxide that forms on the surface of the strip steel when heated and processed in the hot state. The typical scale structure consists of an outermost layer of thinner Fe2O3, an Fe3O4 layer as an intermediate layer, and an FeO layer on the side close to the substrate. In the hot rolling process, Fe2O3 and Fe in the iron oxide scale layer can be caused due to different hot rolling processes and surrounding environments3The difference of the proportion of O4 and FeO and the thickness of the whole iron scale cause great changes of the structure and the thickness of the iron scale on the surface of the steel. Taking plain carbon steel hot rolled plate as an example, the microstructure of the iron scale on the surface of the hot rolled plate becomes an important index for measuring the surface quality of the hot rolled plate, and the method is suitable for plain carbon steel hot rolled platesThe research on the scale on the surface of the carbon steel hot rolled plate has been the focus of the same line of attention worldwide. The components and the structure of the iron scale generated in the hot rolling process not only can cause great influence on the production processes such as acid washing and the like; meanwhile, whether the components and the structure of the iron scale are reasonable or not can directly solve the problem that the existence of the iron scale in the hot rolling production brings much inconvenience to the subsequent process and influences the surface quality of the product. Although the presence of scale greatly affects the surface quality of the product, its presence also has its benefits. For the threaded wire rod steel, the existence of the surface iron scale isolates the wire rod steel substrate from the external environment, so that harmful gas in temperature, humidity and air can not contact the steel substrate, and the wire rod steel substrate is protected from being rusted easily. However, in the actual situation, some scale on the surface of the spiral steel bar falls off or the scale is unevenly distributed during the production process or the transportation process, so that yellow rust or large-area rust appears on a certain part of the spiral steel bar. When the surface of the wire rod steel has large-area rust, the surface quality of a product is seriously influenced, complaints or quality disagreements of a user end are easily caused, and the method can also be a reference for lowering the product price required by a user.
Disclosure of Invention
The invention aims to provide a method for judging the distribution uniformity of an iron oxide scale layer on the surface of a spiral steel wire rod, so as to solve the problems in the background technology.
In order to achieve the purpose, the invention adopts the following technical scheme: a method for judging the distribution uniformity of an iron oxide scale layer on the surface of a spiral coil bar steel comprises the following steps:
s1, cutting the sample, wherein the cutting length of the sample is 3-5CM, preferably 4 CM;
s2, placing the sample into a Raman spectrum measuring device to be clamped;
s3, correcting the Raman spectrum instrument, and measuring the surface of the sample after correction to obtain a Raman spectrum of the test point;
s4 atIn the Raman spectrogram, 223, 289, 404 and 670cm are found-1Characteristic Raman peaks, wherein, 223, 289 and 404cm-1Corresponding to alpha-Fe2O3，670cm-1Corresponding to Fe3O4Measuring the peak height values of the characteristic Raman peaks by using a High pick tool in OMNIC software;
s5, comparing the peak height values of the characteristic peaks, and deducing the content of each component in the iron scale of the sample;
s6, respectively measuring N points of the sample to obtain data of N groups of characteristic Raman peaks, and counting standard deviation values of the N points;
and S7, analyzing the standard deviation values of the N points, and judging the uniformity of the iron scale distribution on the surface of the sample.
Further preferred is: in S2, the Raman spectrum measuring device is a cuboid 5-10cm long and 2-4cm wide, a U-shaped groove is arranged in the middle of the cuboid, the left fixed end of the U-shaped groove is connected with a base into a whole, the whole base is in a flat state, the left fixed end is 2-4cm high, 2-4cm wide and 0.5-2cm long, the base is 8cm long and 3cm wide, a groove 1-2cm wide is arranged in the middle of the base and used for placing a right movable end, the groove is 1-2cm deep, the right upright end is 2-4cm high, 2-4cm wide and 0.5-2cm thick, the bottom of the right movable end is connected with a base groove slide way, the movable end slides in the groove according to the diameter of a sample, the movable end is connected with the fixed end of the sample through a spring in the slide way, and the left end and the right end of the U-shaped groove are consistent in size.
Further preferred is: and a sponge clamp with the thickness of 5-10mm is arranged at the contact part of the Raman measurement device and the sample.
Further preferably: in S5, comparing the peak height values of the characteristic peaks, and when the content of each component in the iron scale of the sample is deduced, determining that the larger the peak height value of the characteristic Raman peak is, the higher the content of the corresponding substance is; .
Further preferred is: the lower the peak of the characteristic raman peak is measured, the lower the corresponding species content.
Further preferably: in S6, N points of the sample are measured to obtain N sets of data of characteristic raman peaks, and the standard deviation values of the N points are counted, where N is equal to or greater than five.
Further preferred is: in S7, when the uniformity of the iron scale distribution on the surface of the sample is judged, the standard deviation values of the N points are checked, and the larger the standard deviation value is, the larger the difference among the points in the sample is; the smaller the standard deviation value, the smaller the difference between the individual points within the sample.
Further preferred is: the larger the difference between each point in the sample is, the worse the uniformity of the iron scale distribution on the surface of the sample is; the smaller the difference between the points inside the sample is, the better the uniformity of the iron scale distribution on the surface of the sample is.
Further preferred is: after cutting the sample, soaking the sample in absolute ethyl alcohol for ultrasonic cleaning for 1-5 min.
Further preferred is: when the Raman spectrum measuring device is used for measurement, a 780nm or 532nm light source is selected as an excitation light source, the power of the light source is set to be 10-23mW, and the measurement is carried out for 2-128 times.
The invention has the technical effects and advantages that: compared with the prior art, the method for judging the distribution uniformity of the oxide scale layer on the surface of the spiral steel rod has the following advantages:
1. the Raman spectrum analysis of the scale on the surface of the wire rod steel is realized, the sample preparation is not needed, the in-situ nondestructive test of the sample can be carried out, and the real state of the scale on the surface of the sample can be objectively reflected;
2. the invention designs a novel Raman spectrum measuring device, which can better fix the wire rod steel, flatly place the wire rod steel on a sample table, can measure Raman characteristic peaks of iron scales on all surfaces of the sample by rotating the sample, can judge the uniformity of the distribution of the iron scales of the wire rod steel by counting the peak height values of the characteristic peaks, and lays a foundation for the subsequent storage of the wire rod steel or the further protection of the rust-prone part.
Drawings
FIG. 1 is a schematic diagram of the surface components and contents of the sample No. 1-1 in the present invention:
FIG. 2 is a schematic diagram of the surface composition and content of the sample No. 1-2 in the present invention;
FIG. 3 is a schematic diagram of the surface components and contents of samples No. 1-3 in the present invention;
FIG. 4 is a schematic diagram of the surface components and contents of the samples No. 1-4 in the present invention;
FIG. 5 is a schematic diagram of the surface composition and content of samples No. 1-5 in the present invention;
FIG. 6 is a schematic diagram of the surface composition and content of samples No. 1-6 in the present invention;
FIG. 7 is a schematic diagram of the surface composition and content of the sample No. 2-1 in the present invention;
FIG. 8 is a schematic diagram of the surface composition and content of the sample No. 2-2 in the present invention;
FIG. 9 is a schematic diagram of the surface composition and content of the sample No. 2-3 in the present invention;
FIG. 10 is a schematic diagram of the surface composition and content of the sample No. 2-4 in the present invention;
FIG. 11 is a schematic diagram of the surface composition and content of the sample No. 2-5 in the present invention;
FIG. 12 is a schematic diagram of the surface composition and content of the sample No. 2-6 in the present invention;
FIG. 13 is a schematic diagram of the surface composition and content of the sample No. 3-1 in the present invention;
FIG. 14 is a schematic diagram of the surface composition and content of sample No. 4-1 in the present invention;
fig. 15 is a schematic structural view of a raman spectrum measuring device of the present invention.
Detailed Description
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 only a part of the embodiments of the present invention, and not all of the embodiments. The specific embodiments described herein are merely illustrative of the invention and do not delimit 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.
Example one
The invention provides a method for judging the distribution uniformity of an iron scale layer on the surface of a spiral steel wire rod, which comprises the following steps:
s1, cutting the sample, wherein the cutting length of the sample is 3-50M;
s2, placing the sample into a Raman spectrum measuring device to be clamped;
s3, correcting the Raman spectrum instrument, measuring the surface of the sample under the condition of more than 500 times of amplification after correction, and obtaining a Raman spectrum chart of the test point:
s4, finding 223, 289, 404 and 670cm in the Raman spectrogram-1Characteristic Raman peaks, wherein, 223, 289 and 404cm-1Corresponding to alpha-Fe2O3，670cm-1Corresponding to Fe3O4Measuring the peak height values of the characteristic Raman peaks by using a High pick tool in OMNIC software;
s5, comparing the peak height values of the characteristic peaks, and deducing the content of each component in the iron scale of the sample;
s6, respectively measuring N points of the sample to obtain data of N groups of characteristic Raman peaks, and counting standard deviation values of the N points;
and S7, analyzing the standard deviation values of the N points, and judging the uniformity of the iron scale distribution on the surface of the sample.
The invention specifically comprises the following steps: in S2, the Raman spectrum measuring device is a cuboid 8cm long and 3cm wide, a U-shaped groove is arranged in the middle of the cuboid, the left fixed end of the U-shaped groove is connected with the base to form a whole, the whole base is in a flat state, the left fixed end is 3cm high, 3cm wide, 1cm long, 8cm long and 3cm wide, a groove 1cm wide is arranged in the middle of the base and used for placing a right movable end, the groove is 1cm deep, the right upright end is 2cm high, 3cm wide and 1cm thick, the bottom of the right movable end is connected with a base groove slide way, the movable end and the sample fixed end slide in the groove according to the diameter of a sample, and the movable end and the sample fixed end are connected through a spring in the slide way.
By adopting the scheme, the diameter of the sample can be flexibly adjusted according to the diameter of the sample.
The invention specifically comprises the following steps: and a sponge interlayer with the thickness of 5mm is arranged at the contact part of the Raman measurement device and the sample.
By adopting the scheme, the situation that the test sample is directly contacted with the measuring device and the iron scale on the surface of the test sample is worn or falls off can be avoided.
The invention specifically comprises the following steps: in S5, comparing the peak height values of the characteristic peaks, and when the content of each component in the iron scale of the sample is deduced, determining that the larger the peak height value of the characteristic Raman peak is, the higher the content of the corresponding substance is; .
The invention specifically comprises the following steps: the lower the peak of the characteristic raman peak measured, the lower the corresponding species content.
By adopting the scheme, the peak value of the characteristic Raman peak can be analyzed, so that the content of the corresponding substance can be analyzed.
The invention specifically comprises the following steps: in S6, N points of the sample are measured to obtain N sets of data of characteristic raman peaks, and the standard deviation values of the N points are counted, where N is equal to or greater than five.
By adopting the scheme, the numerical value of the sample can be determined.
The invention specifically comprises the following steps: in S7, when the uniformity of the iron scale distribution on the surface of the sample is judged, the standard deviation values of the N points are checked, and the larger the standard deviation value is, the larger the difference among the points in the sample is; the smaller the standard deviation value, the smaller the difference between the individual points within the sample.
The invention specifically comprises the following steps: the larger the difference between each point in the sample is, the worse the uniformity of the iron scale distribution on the surface of the sample is; the smaller the difference between the points inside the sample is, the better the uniformity of the iron scale distribution on the surface of the sample is.
By adopting the scheme, the uniformity of the distribution of the iron scale on the surface of the sample can be judged.
The invention specifically comprises the following steps: after cutting the sample, the sample is soaked in absolute ethyl alcohol for ultrasonic cleaning for 1 min.
The invention specifically comprises the following steps: when the Raman spectrum measuring device is used for measurement, 780nm is selected as an excitation light source, the power of the light source is set to be 20mW, and the measurement is carried out for 32 times.
The working principle is as follows: firstly, cutting a sample, then correcting a Raman spectrum instrument,after correction, under the condition of more than 500 times of amplification, the surface of the sample is measured to obtain a Raman spectrogram of the test point, and then 223, 289, 404 and 670cm are found in the Raman spectrogram-1Characteristic Raman peaks, wherein, 223, 289 and 404cm-1Corresponding to alpha-Fe2O3，670cm-1Corresponding to Fe3O4Measuring the peak height values of the characteristic Raman peaks by using a Highpick tool in OMNIC software, comparing the peak height values of the characteristic peaks, deducing the content of each component in the iron scale of the sample, then respectively measuring N points of the sample to obtain the data of N groups of characteristic Raman peaks, counting the standard deviation values of the N points, finally analyzing the standard deviation values of the N points, and judging the uniformity of the iron scale distribution on the surface of the sample; the Raman spectrum analysis of the scale on the surface of the wire rod steel is realized, the sample preparation is not needed, the in-situ nondestructive test of the sample can be carried out, and the real state of the scale on the surface of the sample can be objectively reflected; the uniformity of the iron scale distribution on the surface of the steel wire rod directly influences the rust resistance of the steel wire rod, and no better direct and quick analysis method is available at present for judging the uniformity of the iron scale distribution on the surface of the steel wire rod. Aiming at the problem, the invention designs a novel Raman spectrum measuring device which can better fix the wire rod steel, flatly place the wire rod steel on a sample table, measure Raman characteristic peaks of iron scales on all surfaces of the sample by rotating the sample, judge the uniformity of the distribution of the iron scales of the wire rod steel by counting the peak height value of the characteristic peaks and lay a foundation for the storage of the subsequent wire rod steel or the further protection of the easy-to-rust part.
Example two
The invention also provides a method for judging the distribution uniformity of the scale layer on the surface of the spiral steel bar as shown in figures 1-15, which is different from the first embodiment in that:
the diameter of a sample of the threaded coil steel is 10mm, the difference of surface iron oxide scale of the threaded coil steel is considered, the spinning temperature of a is 925 ℃, the fan is started for 100 percent, the spinning temperature of b is 925 ℃ and the fan is started for 30 percent, the distribution uniformity of the surface iron oxide scale layer is judged after production is finished, the threaded coil steel produced by the process a is marked as No. 1, and the threaded coil steel produced by the process b is marked as No. 2.
The test steps for measuring the surface components and the contents of the No. 1 and No. 2 samples by the Raman spectrum are as follows:
1) cutting the sample into 4 cm;
2) soaking the sample in absolute ethyl alcohol, and ultrasonically cleaning for 1 min;
3) clamping by using a Raman spectrum measuring device, placing on an objective table, and measuring under the condition of amplifying by more than 500 times;
4) 780nm is selected as an excitation light source, the power of the light source is set to be 20mW, the measurement is carried out for 32 times, and data are collected;
5) the characteristic Raman spectrum is obtained as follows, and 293 and 410cm can be known by comparing with the standard spectrum-1The corresponding substance is alpha-Fe2O3，670cm-1Corresponding substance is Fe3O4(ii) a 293, 410 and 670cm by Omnic software-1The peak height of the characteristic raman peak was calculated as shown in table 1.
TABLE 1
As is clear from the results in Table 1, the compositions of the iron oxide scale layers on the surfaces of the samples No. 1 and No. 2 were the same and both of them were alpha-Fe2O3And Fe3O4By comparison of 293, 670cm-1The peak heights of the Raman peaks are shown, the average values of the two are found to be relatively close, which indicates that the contents of all components in the scale are relatively close, and the SD value of the sample No. 1 is smaller than that of the sample No. 2 in terms of SD standard deviation, which indicates that the contents of the components between all points on the surface of the sample No. 1 are closer, and the distribution of the scale is more uniform.
Example three.
The invention also provides a method for judging the distribution uniformity of the scale layer on the surface of the spiral steel bar as shown in figures 1-15, which is different from the first embodiment in that:
under two technologies, the uniformity of the distribution of the iron oxide scale layer on the surface of the spiral steel rod is inspected. The 3# sample is an old process, and the 4# sample increases the spinning temperature and reduces the cooling speed. According to the steps of the test scheme, the iron oxide scale layers of 5 different parts on the surface of the sample are subjected to Raman spectrum measurement, the measured Raman spectrum is as follows, one Raman chart of the 3# sample and one Raman chart of the 4# sample are respectively listed as representatives, other Raman spectrums are similar to the Raman spectrums, and the measured test data are shown in a table 2.
The Raman spectrum measurement 3# and 4# sample surface scale components comprise the following steps:
1) cutting the sample into 4 cm;
2) soaking the sample in absolute ethyl alcohol, and ultrasonically cleaning for 1 min;
3) clamping by using a Raman spectrum measuring device, placing on an objective table, and measuring under the condition of more than 500 times of magnification;
4) 780nm is selected as an excitation light source, the power of the light source is set to be 20mW, the measurement is carried out for 32 times, and data are collected;
5) the characteristic Raman spectrum is obtained as follows, and 293 and 410cm can be known by comparing with the standard spectrum-1The corresponding substance is alpha-Fe2O3，670cm-1The corresponding substance is Fe3O4(ii) a 293, 410 and 670cm by Omnic software-1The peak height of the characteristic raman peak was calculated as shown in table 2.
Raman characteristic peak height values of iron scale on surface of samples in Table 23 # and 4#
| Wave number/cm-1 | 3#-1 | 3#-2 | 3#-3 | 3#-4 | 3#-6 | Mean value of | SD |
| 293 | 4.845 | 19.354 | 6.485 | 1.071 | 5.960 | 7.28 | 45.39 |
| 670 | 4.551 | 4.944 | 1.051 | 1.496 | 1.08 | 2.25 | 4.44 |
| Wave number/cm-1 | 4#-1 | 4#-2 | 4#-3 | 4#-4 | 4#-6 | Mean value of | SD |
| 293 | 10.02 | 15.21 | 12.465 | 9.182 | 13.58 | 11.79 | 27.70 |
| 670 | 4.356 | 4.057 | 5.075 | 4.078 | 5.23 | 4.55 | 2.27 |
As is clear from the results in Table 2, the compositions of the iron oxide scale layers on the surfaces of samples No. 3 and No. 4 were the same and both of them were alpha-Fe2O3And Fe3O4By comparison of 293, 670cm-1The peak heights of the Raman peaks are shown, the average values of the two are found to be greatly different, the average value of the 3# sample is obviously smaller than that of the 4# sample, and the fact that the alpha-Fe in the scale of the 3# sample is proved2O3And Fe3O4The content of the alpha-Fe is lower than that of the alpha-Fe in the iron oxide skin layer of the No. 4 sample2O3And Fe3O4The content of (A); 293cm in the 1# sample as seen from SD standard deviation-1Has an SD much larger than 293cm of a 4# sample-1This indicates that alpha-Fe is present between the points on the surface of the No. 1 sample2O3The content difference is large, 670cm in 3# sample-1The SD value of (D) is also larger than 670cm in the sample No. 4-1The SD value of (1) is large, and Ee between each point in the scale on the surface of the 3# sample is also shown3O4Content difference of (2) to Fe between points on the surface of sample No. 43O4The content difference is large, which shows that the uniformity of the oxide scales on the surface of the twisted steel produced by the old process is poorer than that of the oxide scales on the surface of the twisted steel produced by the new process, and the distribution is more uneven, so the production process of the 4# sample is recommended.
Finally, it should also be noted that the terms "comprises," "comprising," or any other variation thereof, are intended to cover a non-exclusive inclusion, such that a process, method, article, or apparatus that comprises a list of elements does not include only those elements but may include other elements not expressly listed or inherent to such process, method, article, or apparatus.
While preferred embodiments of the present invention have been described, additional variations and modifications in those embodiments may occur to those skilled in the art once they learn of the basic inventive concepts. Therefore, it is intended that the appended claims be interpreted as including preferred embodiments and all such alterations and modifications as fall within the scope of the invention.
It will be apparent to those skilled in the art that various changes and modifications may be made in the present invention without departing from the spirit and scope of the invention. Thus, if such modifications and variations of the present invention fall within the scope of the claims of the present invention and their equivalents, the present invention is also intended to include such modifications and variations.
Claims (5)
1. A method for judging the distribution uniformity of an iron oxide scale layer on the surface of a spiral coil bar steel is characterized by comprising the following steps:
s1, cutting the sample, wherein the cutting length of the sample is 3-5 CM;
s2, placing a sample into a Raman spectrum measuring device to be clamped, wherein the Raman spectrum measuring device is in a cuboid shape, a U-shaped groove is formed in the middle of the Raman spectrum measuring device, a sample fixing end on the left side of the U-shaped groove is connected with a base into a whole, the whole base is in a flat state, a base groove is formed in the middle of the base and used for placing a movable end, the bottom of the movable end is connected with a slide way of the base groove in a sliding mode, the movable end and the sample fixing end are connected in the slide way through a spring, the sample fixing end and the movable end at two ends of the U-shaped groove are identical in size, and a sponge interlayer with the thickness of 5-10mm is arranged at a position, in contact with the sample, in the U-shaped groove;
s3, correcting the Raman spectrum instrument, and measuring the surface of the sample after correction to obtain a Raman spectrum of the test point;
S4、in the Raman spectrogram, 223, 289, 404 and 670cm are found-1Characteristic Raman peaks, wherein, 223, 289 and 404cm-1Corresponding to alpha-Fe2O3，670cm-1Corresponding to Fe3O4Measuring the peak height values of the characteristic Raman peaks by using a High pick tool in OMNIC software;
s5, comparing the peak height values of the characteristic peaks, and deducing the content of each component in the iron scale of the sample;
s6, respectively measuring N points of the sample to obtain data of N groups of characteristic Raman peaks, and counting standard deviation values of the N points, wherein the numerical value of N is more than or equal to five;
s7, analyzing the standard deviation values of the N points, and judging the uniformity of the iron scale distribution on the surface of the sample, wherein the larger the standard deviation value is, the larger the difference among the points in the sample is, and the worse the uniformity of the iron scale distribution on the surface of the sample is; the smaller the standard deviation value, the smaller the difference between the respective points inside the sample, and the better the uniformity of the oxide scale distribution on the surface of the sample.
2. The method for determining the distribution uniformity of the scale layer on the surface of the spiral wound rod steel as claimed in claim 1, wherein: in S5, when the peak heights of the characteristic peaks are compared and the levels of the components in the iron scale of the sample are estimated, the higher the peak height of the characteristic raman peak is, the higher the content of the corresponding substance is.
3. The method for determining the distribution uniformity of the scale layer on the surface of the spiral wound rod steel as claimed in claim 1, wherein: the lower the peak of the characteristic raman peak is measured, the lower the corresponding species content.
4. The method for determining the distribution uniformity of the scale layer on the surface of the spiral wound rod steel as claimed in claim 1, wherein: after cutting the sample, soaking the sample in absolute ethyl alcohol for ultrasonic cleaning for 1-5min, and ultrasonic cleaning for 2-3 times.
5. The method for determining the distribution uniformity of the scale layer on the surface of the spiral wound rod steel as claimed in claim 1, wherein: when the Raman spectrum measuring device is used for measurement, a 780nm or 532nm light source is selected as an excitation light source, the power of the light source is set to be 10-23mW, and the measurement is carried out for 2-128 times.
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