JP5790592B2 - Steel type identification device - Google Patents

Description

  TECHNICAL FIELD The present invention relates to a steel type identification device for steel materials, and in particular, a high-precision inline steel type identification device that can safely apply a fluorescent X-ray analysis method and can easily perform maintenance and inspection in the final inspection, packing and shipping process of a production line. About.

  When steel materials such as steel pipes manufactured under elaborate alloy design and production condition settings to meet advanced performance requirements from users are mis-shipped, the mis-shipped steel materials can exhibit their specified performance. Otherwise, a serious accident may occur. Therefore, it is indispensable to inspect all of the steel materials different from the user specifications before shipment. Depending on the production line, steel materials of 100 types or more may flow through the same production line, and establishment of an inspection method for identifying all of these steel types with high accuracy is an urgent issue. X-ray fluorescence analysis that can measure various alloy elements in a nondestructive manner is effective for the judgment inspection of the steel type of steel.

  In the final inspection packing and shipping line, multiple processes such as length measurement, weighing, stencil, and packing of steel products are already concentrated, so the newly added steel type identification device is compact and adversely affects other processes. It is essential that

  Patent Document 1 proposes a method using a portable X-ray analyzer and an identification label reader. Patent Document 2 proposes a material analysis apparatus that measures an alloy component by pressing a fluorescent X-ray analyzer against a steel pipe. Furthermore, Patent Document 3 proposes an irradiation chamber open type X-ray analyzer that can reliably prevent accidental X-ray irradiation.

JP 2007-320746 A JP 2011-102698 A JP-A-10-212276

  The method described in Patent Document 1 has a problem that the number of processing is limited because X-ray analysis and identification label reading must be performed manually. Have difficulty. Moreover, although it is described that there is no influence on the analysis value by the oxide film covering the steel material surface, depending on the steel type, the influence of the oxide film is large, and therefore the steel type may not be accurately identified.

  In the method described in Patent Document 2, since measurement is performed by pressing a fluorescent X-ray analyzer against the outer surface or end face of a steel pipe, positioning and pressing force control become complicated, and it takes time to measure. Further, since the measurement is performed by automatically selecting an arbitrary point, the influence on the analysis value by the oxide film becomes a problem as in Patent Document 1. Furthermore, X-ray leakage is not mentioned, and a problem remains in terms of safety.

  In the method described in Patent Document 3, the safety circuit is activated when there is no sample in the irradiation window of the irradiation chamber open type X-ray analyzer, and X-ray leakage is prevented by not irradiating X-rays. However, since it is not intended for in-line measurement on the production line, it is difficult to apply it to 100% inspection of steel pipes before shipment.

  It is an object of the present invention to provide a high-precision in-line steel type identification device that can safely apply a fluorescent X-ray analysis method and can easily perform maintenance inspection in a final inspection packaging shipping process of a steel production line. To do.

  As a result of studying a steel type identification device for a long steel material such as a steel pipe, a round steel, and a steel bar, the present inventors have obtained the following knowledge.

  (A) In order to suppress leakage of X-rays as much as possible, there can be considered a method of providing a safety device that detects the presence or absence of the steel material to be analyzed and controlling so that X-rays are not irradiated unless there is a steel material. However, in this method, when the distance between the steel material and the analyzer is more than a certain distance, there is a possibility that the X-ray cannot be irradiated and the analysis is interrupted. For example, when the steel material is long and bent, the distance between the steel material and the X-ray analyzer may be increased depending on the bending direction. Further, when the safety device fails, X-rays may leak.

  (B) In order to suppress the amount of X-ray leakage to a safety standard value or less, it is desirable to prepare a cover that shields X-rays and perform analysis therein.

  (C) Depending on the steel type of the steel material, if an oxide film is present on the surface, an accurate analytical value may not be obtained due to the effect of the film. However, it takes time to polish the film with a grinder or the like, so that the number of treatments is limited.

  (D) When the steel material that is easily affected by the film is long, X-ray analysis is performed while rotating the steel material around its longitudinal axis, thereby reducing the influence of the oxide film and reducing the variation in the analysis value. Can be reduced.

  (E) On the other hand, when a long steel material is curved, if it is rotated, it swings in the radial direction. As a result, the distance between the X-ray analyzer and the steel material greatly fluctuates, which not only affects the analysis accuracy, but also prevents the steel material from coming into contact with the analyzer and causing the device to be damaged. It is necessary to provide a mechanism for this.

  This invention is made | formed based on such knowledge, and makes a summary the steel type identification apparatus shown to following (1)-(6).

(1) A device for identifying a steel type of a columnar or cylindrical steel material,
An analysis means comprising an X-ray generator for irradiating steel with X-rays and an X-ray detector for detecting fluorescent X-rays emitted from the steel;
X-ray shielding means for containing the analysis means and having an insertion port for inserting a steel material to prevent X-rays from leaking to the outside;
Rotating means for rotating the steel material around the axis when the steel material is irradiated with X-rays;
At the time of rotation of the steel material, a vibration suppression means for suppressing the fluctuation of the distance between the steel material and the analysis means,
A steel type identification apparatus comprising: a calculation unit for identifying a steel type from the X-ray intensity obtained by the analysis unit.

  (2) The steel type identification device according to (1), wherein the shake suppression unit includes a rotating plate that rotatably supports a steel material from the opposite side of the analyzing unit.

  (3) According to the assumed steel type, further comprising a control means for controlling one or more types selected from an acceleration voltage, a measurement time, and a measurement distance between the steel material and the analysis means in the X-ray generator. The steel type identification device according to the above (1) or (2), characterized in that it is characterized.

  (4) The steel type identification device according to any one of (1) to (3), wherein the steel type is identified using a ratio of analytical values of two or more elements.

  (5) The steel type identification device according to (4), wherein the steel type is identified using a ratio of analysis values of Cr and Ni when identifying the steel type of the steel material containing Cr and Ni.

  (6) The steel type identification apparatus according to any one of (1) to (5) above, further comprising a mechanism for analyzing a standard sample prepared in advance in the X-ray shielding means.

  Note that “steel type identification” in the present invention means identifying a steel type based on the chemical composition, for example, determining which of the existing classifications according to the chemical composition corresponds to the identification target. This includes checking whether the composition of the steel material is within the design range of the assumed steel type.

  According to the steel type identification apparatus according to the present invention, it is possible to identify the steel type of the steel material in-line with high accuracy by safely applying the fluorescent X-ray analysis method in the final inspection packing and shipping process of the production line. Furthermore, since the device has a structure simplified as much as possible, the risk of failure is low and the maintenance is excellent.

It is the front view which showed roughly an example of the steel kind identification device which concerns on this invention. It is the figure which compared the dispersion | variation in the analysis value with the case where it analyzes in the state which stopped steel materials, and when rotating. It is the figure which showed roughly another example of the steel kind identification device which concerns on this invention. (A) Plan view with no steel material inserted (b) Front view with steel material inserted It is a figure which shows an example of the analysis result by a fluorescent X ray analysis. (A) Cr analysis value (b) Ni analysis value (c) Cr / Ni ratio It is a figure which shows an example of the X-ray intensity according to an acceleration voltage. (A) Acceleration voltage 35 kV (b) Acceleration voltage 30 kV

  FIG. 1 is a diagram schematically showing an example of a steel type identification device according to the present invention. The steel type identification apparatus of the present invention includes an analysis means 2 for performing fluorescent X-ray analysis of a steel material 1, an X-ray shielding means 3 including the analysis means 2 and having a steel material insertion port 11, and a rotation means 4 for rotating the steel material 1. And the vibration suppression means 5 which suppresses the fluctuation | variation of the distance of the steel materials 1 and the analysis means 2, and the calculating means which does not show in figure which identify steel types from the acquired X-ray intensity | strength are included. Details of each component will be described below.

1. Steel Material In the present invention, the steel material to be identified by the steel type is a columnar or cylindrical steel material, and a steel pipe is particularly suitable. The steel type of the steel material to be identified is not particularly limited as long as the chemical composition is known. Moreover, although there is no restriction | limiting in particular also about the magnitude | size of a steel material, It is preferable to make the steel material whose radius is 10-250 mm and about 1-20 m in length be identification object. Note that distortion, bending, and the like that may occur in the manufacture of steel materials are allowed. The apparatus according to the present invention exhibits an excellent effect in identifying the steel type of a steel material whose surface is covered with an oxide film.

2. Analyzing means The analyzing means according to the present invention comprises an X-ray generator and an X-ray detector. A normal X-ray fluorescence analyzer (XRF) can be used. Fluorescent X-ray detectors are broadly classified into two types, an energy dispersion type and a wavelength dispersion type, and either may be adopted. Wavelength dispersive X-ray analysis has the advantages of high sensitivity and excellent energy resolution. On the other hand, energy dispersive X-ray analysis is inferior in sensitivity and energy resolution, but has an advantage that many elements can be analyzed efficiently and rapidly. Therefore, it is preferable to use an energy dispersive X-ray analyzer as the analyzing means in the present invention.

  In addition, as a method for quantifying the content of each element from the obtained X-ray intensity, a normal method such as a calibration curve method, a standard addition method, a fundamental parameter (FP) method, or the like may be used. When the FP method is used, the analysis values of all the main component elements can be obtained. However, the analysis values of all the elements may be used for identifying the steel types, or some analysis values may be selected and used. Also good.

  Although there is no restriction | limiting in particular about the acceleration voltage (tube voltage) in an X-ray generator, What is necessary is just to adjust in the range of 25-35 kV suitably. Further, if the measurement time is long, the analysis accuracy is improved, but the processing capability is lowered. In consideration of that, it may be appropriately selected within a range of about 5 to 10 s depending on the element used for identifying the steel type. Although one analysis may be performed for one steel material, it may be performed twice or more for accuracy improvement.

  If a standard sample 15 prepared in advance in the X-ray shielding means 3 described later is analyzed as appropriate, not only can the sensitivity change with time (drift) of the X-ray analyzer be corrected, but also an abnormality in the analyzer. It is preferable because it becomes possible to discover. The standard sample is not particularly limited and any standard sample may be used, but it is preferable to select one having a composition close to that of the steel material to be measured. The measurement of the standard sample is preferably performed periodically. For example, every time 10 samples of steel are analyzed, the standard sample is measured, drift correction is performed, and whether or not the analyzer is abnormal is preferably confirmed.

3. X-ray shielding means The X-ray analysis described above is performed in the X-ray shielding means 3 to prevent X-rays from leaking outside. Normally, since X-rays are irradiated with the steel material to be analyzed covering the analysis means, it is considered that there is no leakage of X-rays, but the steel material has not been inserted into the device due to troubles such as a malfunction of the device. Even if X-rays have been irradiated in the state, X-ray leakage to the outside can be prevented by the X-ray shielding means. Although there is no restriction | limiting in particular about the raw material used for an X-ray shielding means, It is preferable to use the transparent cover (thickness 12mm, lead equivalent 0.5mm) containing the lead containing lead.

  If there is a large amount of X-ray leakage, it will be necessary to make all the facilities where the X-ray analyzer is installed an X-ray management area, and work efficiency will be significantly deteriorated. There is. For this purpose, the amount of X-ray leakage to the outside of the X-ray shielding means at the time of analysis needs to be less than 2 μSv / h, which is a management condition. The actual leakage amount is preferably 0.2 μSv / h or less. If the amount of X-ray leakage is 0.2 μSv / h or less, it can be said that there is no substantial amount of leakage from the apparatus, almost equal to the amount of natural radiation.

  From the viewpoint of preventing X-ray leakage, it is preferable to analyze in a state where the steel material is completely covered. However, in the case of a long tube or the like, it is difficult to cover all of it with X-ray shielding means. The X-ray shielding means 3 has a steel material insertion port 11 and performs analysis by inserting the steel material 1 therefrom. At this time, the steel material may be moved and inserted into the apparatus, or the apparatus may be moved and the steel material may be inserted into the apparatus. Even if the steel material insertion port 11 is always in an open state, if the positional relationship with the X-ray irradiation direction is appropriately adjusted, the X-ray leakage amount can be reduced to 0.2 μSv / h or less as described above. It is better to have a configuration in which the lid is closed when the steel material is not inserted.

4). Rotating means As described above, when an oxide film is present on the surface of a steel material, there are steel types for which an accurate analytical value cannot be obtained due to the influence of the film. In addition, depending on the degree of bending of the steel material, the measurement distance between the steel material and the analysis means may be increased, which may hinder measurement of elements having a low content. In such a case, the X-ray analysis by the analysis means 2 is performed while rotating the steel material around the longitudinal axis of the steel material.

  FIG. 2 compares the variation of the analysis value between the case where the steel material is analyzed in a stationary state and the case where the steel material is analyzed while being rotated. The horizontal line shows the true analytical value of steel. As a result, in the analysis in a stationary state, the variation was very large, and the value of the relative standard deviation (RSD) was 20.2%. On the other hand, when the analysis was performed while rotating, the RSD was 6.1%. It is considered that there is no problem in the identification of the steel type if the variation is this level.

  There is no restriction | limiting in particular about a rotational speed, What is necessary is just to adjust suitably in balance with measurement time. The rotation speed is preferably adjusted so as to make one or more rounds within the measurement time. However, when the steel material is bent, accurate measurement is possible when the steel material approaches the analysis means. Therefore, if the rotational speed is too high, the measurement becomes difficult. Therefore, it is preferable to set so as to make about two rounds within a measurement time of 5 to 6 s.

  If the steel material is rotated about the axis at the same time as it is moved in the axial direction, an average of a wider range of analysis values can be obtained.

  Depending on the steel type, it is difficult to form an oxide film, and analysis is possible even when the measurement distance is long, and therefore rotation during measurement may be unnecessary. In such a case, analysis may be performed with the rotating means stopped. Further, the first analysis may be performed in a state where the rotating means is stopped. As a result, if it is determined that the steel type is different from the assumed steel type, the second analysis may be performed in the rotated state.

5. Vibration control means In particular, in the case of a long steel material, distortion, bending, and the like that cannot be avoided in production can occur. For example, in the case of a steel material having a length of 10 m or more, bending of about 5 mm may occur at the pipe end. Then, as the steel material 1 swings in the radial direction with the rotation and the distance to the analysis means 2 fluctuates, the analysis accuracy is adversely affected, possibly contacting the analysis means and causing failure of the apparatus. There is. Therefore, it is necessary to suppress fluctuations in the distance between the steel material 1 and the analysis means 2. In addition, the fluctuation | variation of the distance of steel materials here and an analysis means means the distance in the X-ray irradiation position. Moreover, suppressing the fluctuation | variation of the distance of steel materials and an analysis means does not necessarily need to keep the distance of steel materials and an analysis means completely constant, What is necessary is just to be able to suppress in the range which does not hinder analysis.

  Although there is no restriction | limiting in particular about the structure for suppressing a vibration, The rotation board 5a as shown in FIG. 1 is provided in the upper part which is the other side of the analysis means 2, and it restrict | limits the upward vibration of steel materials. Is good. By using the rotating plate, it is possible to suppress the shake while reducing the contact resistance with the steel material. The rotating plate 5a is not necessarily in contact with the steel material, and may be separated from the steel material, for example, when there is little deflection of the steel material.

  FIG. 3 is a diagram schematically showing another example of the steel type identification device according to the present invention. Fig.3 (a) is a top view of the apparatus based on this invention in the state which has not inserted the steel material 1, FIG.3 (b) moved the apparatus to the steel material side, and the state which inserted the steel material 1 It is a front view of the apparatus which concerns on this invention. As shown in FIG. 3, the rotating plate 5 a which is the shake suppression means 5 serves as a lid for the steel material insertion port 11 in a state where the steel material 1 is not inserted into the X-ray shielding means 3. be able to. Further, by using the cylinder 12, the lid of the steel material insertion port 11 may be automatically opened and closed according to the entry and exit of the steel material 1 in the X-ray shielding means 3. If it is said structure, even if a cylinder does not open and close automatically by failure, when a steel material is inserted in an apparatus, it is possible to push open a cover smoothly.

  The shake suppression unit 5 may further include one or more protective members for protecting the steel material 1 from contacting the analysis unit 2. For example, as shown in FIG. 3, a protective roller 5b, a protective spherical three-point roller 5c, and a protective stainless case 5d can be provided as protective members. By providing these protective members, the analysis means 2 can be prevented from being damaged even if the steel material 1 approaches the analysis means 2 due to vibration.

6). Calculation means The steel type is identified from the analysis result obtained by the analysis means 2 by a calculation means (not shown). A normal PC or the like may be used as the calculation means. In the calculation means, threshold values of each component determined for each steel material are registered, and it is confirmed whether or not the analysis value of the steel material to be inspected is within the threshold value. Then, if the registered steel type and the analysis result match, an instruction is given to transfer to the shipping process, and if it does not match, the analysis condition is changed and an instruction is given to perform the analysis again. be able to. If it does not match the registered steel type even after reinspection, it can be transported to another storage without shipping.

  For the identification of the steel type, an analysis value of one or more specific elements may be used, or a ratio of analysis values of two or more elements may be used. The analysis value of the element can be influenced by the oxide film, but the effect of the oxide film can be canceled out by looking at the ratio of elements having a similar degree of influence. Therefore, in order to more accurately identify the steel type, it is preferable to use the ratio of analysis values between elements. At this time, when the result of the steel type identification based on the analysis value of the specific element is different from the result of the steel type identification based on the ratio of the analysis value between the elements, the result based on the more reliable analysis value ratio may be prioritized. However, since it cannot be identified, it may be re-inspected.

  The above steel type identification has an excellent effect when using a ratio of analytical values of Cr and Ni, particularly in a steel material containing Cr and Ni. FIG. 4 shows, as an example, analytical values of Cr and Ni and Cr / Ni ratios in various steel pipes containing 11.90% Cr and 4.50% Ni in mass%. The solid line shows the true analytical value of steel. In addition, the one-dot chain line L in the figure indicates that the steel type of the analyzed steel material is steel type A containing 11.90% of Cr and 4.50% of Ni, or 18.00% of Cr and Ni. It is a reference line for judging whether it is steel type B containing 9.00%. As a result, it can be seen that, in both the analysis values of Cr and Ni, the steel line A is identified by the reference line L. However, the variation in analysis values of Cr and Ni is large. On the other hand, it can be seen that the variation in the Cr / Ni ratio is very small. Thus, the use of the ratio of the analysis values of two or more elements, particularly the ratio of the analysis values of Cr and Ni, is extremely effective when performing high-precision steel type identification.

7). Control means In the present invention, one or more selected from (i) the acceleration voltage in the X-ray generator, (ii) the measurement time, and (iii) the measurement distance between the steel material and the analysis means, depending on the assumed steel type. It is preferable to further comprise a control means for controlling. As the control means, a normal PC or the like may be used, and the control means may be performed by the same PC as the calculation means. Hereinafter, each of (i) to (iii) will be described using an example.

(I) Acceleration voltage (tube voltage)
FIG. 5 shows an example of X-ray measurement intensities of Ti, Cr, Fe, Ni and Mo when the acceleration voltage in the X-ray generator is 35 kV and 30 kV, respectively. When the acceleration voltage is large, the X-ray intensity of Mo (atomic weight 95.94), which is a heavy element, is observed to be relatively large. On the other hand, when the acceleration voltage is small, light element Ti (atomic weight 47.87), It can be seen that the X-ray intensities of Cr (atomic weight 52.00), Fe (atomic weight 55.85) and Ni (atomic weight 58.69) are observed to be relatively large. That is, it is preferable to adjust the acceleration voltage in the X-ray generator according to the measurement target element.

(Ii) Measurement time When a sample containing V having a content of 0.1% or less and Mo having a content of 0.2% or more was analyzed by measuring each of V and Mo as measurement times 4, 6 and 10 s, With V having a low content, measurement was possible for all samples at 10 s. However, the sample was about 1/3 at 4 s, and measurement was impossible because the measurement time was too short. At 6 s, measurement was impossible with about 1/6 sample. On the other hand, with Mo having a relatively high content, measurement of all samples was possible in all of 4, 6, and 10 s. Such data is accumulated, and the optimum measurement time can be determined based on the accumulated data. In particular, when the content of an element important for identifying the steel type is low, it is preferable to adjust the measurement time to be long.

(Iii) Measurement distance Samples containing Nb with a content of about 0.1% and V with a content of about 0.2% were analyzed with the measurement distances of Nb and V being 5, 6 and 9 mm, respectively. With Nb having a low content, measurement was impossible because the measurement distance was too long for a sample of about 1/3 at 9 mm, and measurement was impossible for one sample even at 6 mm. If it was 5 mm, it was possible to measure all samples. On the other hand, at V having a relatively high content, all samples could be measured regardless of the measurement distance. As described above, the measurement distance is an important factor in the measurement of an element having a low content. Note that the measurement distance between the steel material and the analysis means can be adjusted by moving the entire analyzer up and down relative to the steel material.

  As described above, one analysis may be performed for one steel material, but it may be performed twice or more for accuracy improvement. However, if it is determined by the first analysis that the steel type is different from the assumed steel type, It may be controlled to change the conditions (i) to (iii) to perform the second analysis.

8). Ensuring Safety In addition to the above, the steel type identification device according to the present invention may be provided with means for ensuring safety as necessary. As shown in FIG. 3, it is preferable to confirm the presence of the steel pipe by one or more material detection sensors 13. Moreover, the stopper 14 for preventing that steel materials collide accidentally in the back of an apparatus can also be provided. The standard sample 15 described above can be installed in the X-ray shielding means 3. Furthermore, it is desirable to improve safety by attaching a plurality of X-ray leakage prevention confirmation sensors (not shown).

  According to the steel type identification apparatus according to the present invention, the steel type can be identified with high accuracy in-line by safely applying the fluorescent X-ray analysis method in the final inspection packing and shipping process of the production line of the steel material. Furthermore, since the device has a simplified structure as much as possible, the risk of failure is low and the maintenance is excellent.

1. 1. Steel material Analysis means 3. X-ray shielding means4. Rotating means 5. Shaking suppression means 5a. Rotating plate 5b. Protective roller 5c. Protective spherical 3-point roller 5d. 10. Stainless steel case for protection Steel insertion slot 12. Cylinder 13. Material detection sensor 14. Stopper 15. Standard sample

Claims (6)

A device for identifying a steel grade of a cylindrical or cylindrical steel material,
An analysis means comprising an X-ray generator for irradiating steel with X-rays and an X-ray detector for detecting fluorescent X-rays emitted from the steel;
X-ray shielding means for containing the analysis means and having an insertion port for inserting a steel material to prevent X-rays from leaking to the outside;
Rotating means for rotating the steel material around the axis when the steel material is irradiated with X-rays;
At the time of rotation of the steel material, a vibration suppression means for suppressing the fluctuation of the distance between the steel material and the analysis means,
A steel type identification apparatus comprising: a calculation unit for identifying a steel type from the X-ray intensity obtained by the analysis unit.   The steel type identification device according to claim 1, wherein the shake suppressing unit includes a rotating plate that rotatably supports a steel material from the opposite side of the analyzing unit.   According to the assumed steel type, it is further provided with a control means for controlling one or more types selected from the acceleration voltage in the X-ray generator, the measurement time, and the measurement distance between the steel material and the analysis means. The steel type identification device according to claim 1 or 2.   The steel type identification device according to any one of claims 1 to 3, wherein a steel type is identified using a ratio of analysis values of two or more elements.   5. The steel type identification device according to claim 4, wherein when identifying a steel type of a steel material containing Cr and Ni, the steel type is identified using a ratio of analysis values of Cr and Ni.   The steel type identification device according to any one of claims 1 to 5, further comprising a mechanism for analyzing a standard sample prepared in advance in the X-ray shielding means.