JP6693379B2 - Different material determination method for metal materials - Google Patents

Description

  The present invention relates to a foreign material determination method for determining whether or not a metal material is a foreign material different from a planned product type.

  Conventionally, in the manufacturing process of metal pipes, etc., when the material is received or the product is shipped, whether the material or the metal material that is the product is of the planned type (steel type if the metal material is steel) A PMI (Positive Material Identification) test for determining whether or not it is being executed. The product type means a type of metal material classified according to the composition, and the range of the content of each element constituting the composition of each product type is defined by the material standard (AMS, JIS, etc.). Then, as a result of performing the PMI inspection on the determination target metal material, it is determined that the determination metal material is a metal material (different material) of a type different from the type (planned type) scheduled to be received or shipped. In such a case, the metal material to be judged, which is a different material, is excluded from the raw materials and products, the cause of the different material mixture is investigated, if necessary, and a preventive measure is taken.

  Although many methods of PMI inspection (determination of different materials) are known, in recent years, a different material determination method using a fluorescent X-ray analysis method has become mainstream. The fluorescent X-ray analysis method irradiates a metal material with X-rays from an X-ray fluorescence analyzer, detects fluorescent X-rays generated from the metal material by the irradiated X-rays, and detects the wavelength of the detected fluorescent X-rays. It is a method of analyzing the content (content rate) of each element contained in the metal material based on the strength and strength.

  In the conventional foreign material determination method, for example, by reading an identifier attached to the determined metal material by means such as sticking, engraving, or marking, the expected product type of the determined metal material associated with this identifier is recognized. The range of the content of each element constituting the composition of the planned variety is defined by the material standard, and is described in, for example, a mill sheet. Then, the content of any of the elements contained in the judged metal material analyzed by the fluorescent X-ray analysis method is the same as that of any of the above-mentioned elements constituting the composition of the planned variety of the judged metal material defined in the material standard. When the content is out of the range, it is determined that the determination target metal material is a different material. That is, in the conventional foreign material determination method, it is general to use the material standard as a criterion for determining whether or not the metal material to be determined is a different material.

  However, since the types of each element whose content range is defined in the material standard are limited, the actual metal materials of each product type contain a small amount of elements not defined in the material standard. There are cases. Therefore, when the material standard is used as the determination standard as in the conventional case, it may be erroneously determined that the metal material to be determined is not a different material (it matches the planned product type) although it is actually a different material. Specifically, for example, the analysis value of each element by the fluorescent X-ray analysis method for the judgment target metal material different from the planned product type includes the analysis value of a trace amount of the element which is not defined in the material standard of the planned product type. However, the analytical value of the trace element is not used for the determination. Therefore, even if this analysis value exceeds the content that can be assumed for the planned product type, it will be erroneously determined that the judgment target metal material is not a different material.

  In order to reduce the erroneous determination in the above-described conventional foreign material determination method, it is conceivable to use the Ladle analysis value of each element that constitutes the composition of the intended product type of the determination target metal material as the determination standard. The ladle analysis value is an analysis value obtained by actually measuring the content of each element contained in the molten metal that is the raw material of the metal material (molten steel when the metal material is steel). Therefore, even if it is a trace element that is not specified in the material specifications of the planned product type, the Ladle analysis value of this element exists, so the analysis value and the Ladle analysis value of this element by the fluorescent X-ray analysis method It becomes possible to compare and. Therefore, if the ladle analysis value is used as the determination standard, it can be expected that the number of erroneous determinations is reduced as compared with the case where the material standard is used.

  As a foreign material determination method using a ladle analysis value as a determination criterion, for example, the method described in Patent Document 1 has been proposed. However, the method described in Patent Document 1 is a method of determining a different material by comparing the analysis value obtained by a commercially available fluorescent X-ray analyzer with the determination standard using the Ladle analysis value as it is. Therefore, there is a possibility that erroneous determination cannot be sufficiently reduced due to an error in the analysis value by the fluorescent X-ray analysis device.

Japanese Patent No. 4848846

  The present invention has been made in order to solve the problems of the above-mentioned conventional techniques, and a metal material capable of determining whether or not the metal material to be determined is a different material different from the planned product type with higher accuracy than before. It is an object of the present invention to provide a method for determining different materials.

In order to solve the above problems, a method for determining a foreign material of a metal material according to the present invention includes the following steps (1) to (6).
(1) First preparatory step: The correction content for the analysis value of the content of the element obtained by the fluorescent X-ray analysis device is determined for each product type and for each element constituting the composition of each product type.
(2) Second preparatory step: For each element that constitutes the composition of the variety, the judgment standard of the analysis value after the correction based on the correction content according to the Ladle analysis value is determined.
(3) Analysis step: The fluorescent X-ray analysis device is arranged so as to be able to face the judgment target metal material with an identifier, and the content of each of the plurality of elements contained in the judgment metal material is determined by the judgment metal material. Is analyzed by the X-ray fluorescence analyzer facing the above.
(4) Recognition step: The identifier attached to the judged metal material is detected, and the expected product type of the judged metal material associated with the identifier is recognized.
(5) Correction step: The analysis value of the content of each element obtained in the analysis step is corrected using the correction content determined in the first preparation step for the planned product recognized in the recognition step.
(6) Judgment step: The Ladle analysis value of each element constituting the composition of the planned variety is referred to, and the analysis value of the content of each element after the correction obtained by the correction step and each of the referred elements are referred to. In comparison with the determination criteria of each element determined in the second preparatory step according to the Ladle analysis value, and when any of the corrected analysis values of the content of each element does not satisfy the determination criteria of each element The judged metal material is judged to be a different material different from the planned type.
The first preparation step is characterized by including the following steps (7) and (8).
(7) First step: Prepare a plurality of kinds of preparation metal materials of known kinds, and make each preparation metal material face the fluorescent X-ray analysis device, and include each of the preparation metal materials. The content of each element to be analyzed is analyzed by the X-ray fluorescence analyzer.
(8) Second step: analysis of the ladle analysis value of each element contained in each of the preparation metal materials and the content of each element contained in each of the preparation metal materials obtained in the first step Based on the deviation from the value, the correction content for the analysis value of the content of the element obtained by the X-ray fluorescence analyzer is determined for each type and for each element constituting the composition of each type.

According to the present invention, first, in the first preparation step, the correction content for the analysis value of the content of the element obtained by the fluorescent X-ray analyzer is determined in advance.
Specifically, the first preparation step includes a first step and a second step. In the first step, a plurality of kinds of preparation metal materials whose kinds are known are prepared and included in each preparation metal material. The content of each element to be analyzed is analyzed by a fluorescent X-ray analyzer. Next, in the second step, the ladle analysis value of each element contained in each preparation metal material and the analysis value of the content of each element contained in each preparation metal material obtained in the first step The correction content is determined based on the deviation.
The correction content is determined for each type and for each element constituting the composition of each type. That is, since it is determined for each element, the correction content may differ between Cr and Fe, for example. Further, since the determination is made for each product type, for example, even if the same Cr is used, the correction contents may differ between Cr that constitutes the composition of one product type and Cr that constitutes the composition of another product type.
As described above, according to the present invention, in the first preparation step, the correction content of the analysis value by the fluorescent X-ray analysis apparatus is determined based on the deviation between the analysis value before correction and the Ladle analysis value. It is possible to correct the analytical value of the line analyzer close to the Ladle analytical value. Further, since the correction content is determined for each product type and for each element constituting the composition of each product type, the analysis value of the X-ray fluorescence analyzer for a certain element contains other elements present in the same preparation metal material. Even if affected by the amount, accurate correction is possible. Therefore, in the later-described determination step, different materials can be determined more accurately than in the case where the analysis value of the fluorescent X-ray analyzer is used as it is as in the conventional case.

  Next, according to the present invention, in the second preparatory step, the criterion for the corrected analytical value is determined. This criterion is based on the Ladle analysis value. That is, it is a criterion that changes depending on the magnitude of the Ladle analysis value. In addition, the criterion is determined for each element that constitutes the composition of the variety. That is, it is possible to determine the same judgment criteria for the same element regardless of the product type. However, like the first preparation step, it is also possible to determine for each product type and for each composition of each product type. That is, even if the same element is used, it is possible to make the judgment criteria different between the elements constituting the composition of one kind and the elements constituting the composition of another kind.

  Next, according to the present invention, in the analysis step, the content of each of the plurality of elements contained in the metal material to be determined, which is a determination target of whether or not it is a different material, is analyzed by the fluorescent X-ray analysis device. The analysis by the fluorescent X-ray analyzer may be performed while the metal material to be judged is stopped or may be analyzed while the metal material to be judged is conveyed at a predetermined conveying speed. It should be noted that the judged metal material is provided with an identifier for recognizing the planned product type in a recognition step described later.

  Next, according to the present invention, in the recognition step, the identifier attached to the judged metal material is detected, and the planned product type (the product product scheduled to be received or shipped. If the judged metal material is not a different material, recognize the product that should be this product). If the identifier and the planned product are stored in advance in association with each other, the other planned product associated with the identifier can be easily recognized by detecting one of the identifiers. Note that, for example, when an identifier is attached in a form in which a barcode label in which a barcode as an identifier is printed is attached to a metal material to be determined, by using a barcode reading device as an identifier detection device, It is possible to easily detect (read) the identifier represented by the bar code.

  Next, according to the present invention, in the correction step, the analysis value of the content of each element obtained in the analysis step is corrected using the correction content determined in the first preparation step. At this time, as the correction content, the correction content determined for the planned product type recognized in the recognition step is used. That is, in the correction process, since it is not yet determined whether or not the judged metal material is a different material, it is assumed that the kind of the judged metal material is a planned kind (not a different material) The correction content determined for is used.

Finally, according to the present invention, in the determination step, first, the Ladle analysis value of each element constituting the composition of the planned variety is referred to. If the planned varieties and the ladle analysis values of the elements constituting the composition of the planned varieties are stored in association with each other, the planned varieties are recognized in the recognition step, so that the ladle of each element associated with this is recognized. The analytical value can be easily referred to. Next, the analysis value of the content of each element after the correction (after the correction in the correction step) and the determination criteria of each element according to the Ladle analysis value of each referenced element (the determination criteria determined in the second preparation step) Different materials are determined by comparing and.
As described above, according to the present invention, in the determination step, the corrected analysis value, which can be expected to improve the accuracy as compared with that before the correction, and the appropriate determination standard according to the Ladle analysis value are compared. Since the determination is made in step 1, it is possible to determine a different material with higher accuracy than in the past.

  Preferably, the determination criterion determined in the second preparation step includes a first determination criterion when the ladle analysis value is less than a predetermined value and a second determination criterion when the ladle analysis value is equal to or more than a predetermined value. The second preparation step is based on the Ladle analysis value and the variation in the analysis value of the content of each element contained in the preparation metal material obtained by the first step of the first preparation step. , A step of determining the first criterion, and a step of determining the second criterion based on a value obtained by multiplying the Ladle analysis value by a predetermined coefficient, the determination step including the elements referred to above. If the ladle analysis value of is less than a predetermined value and any of the analysis values of the content of each element after correction obtained by the correction step does not satisfy the first determination criterion, the determination target metal material is Different from the planned variety And the ladle analysis value of each element referred to above is a predetermined value or more, and one of the analysis values of the content of each element after correction obtained by the correction step is 2 If the determination criteria are not satisfied, the determination target metal material is determined to be a different material from the planned product type.

According to the above preferred configuration, the determination criteria determined in the second preparation step are the first determination criteria when the ladle analysis value is less than the predetermined value and the second determination criteria when the ladle analysis value is greater than or equal to the predetermined value. Composed of. That is, in the second preparation step, the first criterion used as the criterion when the Ladle analysis value is small is determined, and the second criterion used as the criterion when the Ladle analysis value is large is determined.
Specifically, according to the above preferable configuration, based on the Ladle analysis value and the variation in the analysis value of the content of each element contained in the preparation metal material obtained in the first step of the first preparation step, , Determine the first criterion. For example, when the standard deviation of the variation of the analysis value of the content of each element contained in the preparation metal material is σ, the upper limit value of the first judgment criterion = Ladle analysis value + 4σ, the lower limit value of the first judgment criterion = Ladle analysis The value is set to -4σ. Moreover, according to the above-described preferable configuration, the second determination criterion is determined based on a value obtained by multiplying the Ladle analysis value by a predetermined coefficient. For example, the upper limit value of the second determination criterion = A × Ladle analysis value (constant of A> 1), and the lower limit value of the second determination criterion = B × Ladle analysis value (constant of B <1).

  Then, according to the preferable configuration, in the determination step, the Ladle analysis value of each element referred to for the planned variety is less than a predetermined value, and the analysis value of the content of each element after correction obtained by the correction step If any of the above does not satisfy the first determination criterion (for example, exceeds the upper limit value of the above-described first determination criterion or is less than the lower limit value of the first determination criterion), the determination target metal material is a planned product type. It is determined that the material is different. On the other hand, in the judgment step, the Ladle analysis value of each element referred to for the planned variety is equal to or more than a predetermined value, and one of the corrected analysis values of the content of each element obtained in the correction step is the second judgment criterion. If the above conditions are not satisfied (for example, the upper limit value of the second judgment criterion is exceeded or the lower limit value of the second judgment criterion is exceeded), it is determined that the judgment target metal material is a different material from the intended product type. ..

As described above, according to the above preferred configuration, determination is made when the referenced ladle analysis value of each element is smaller than a predetermined value (when it is considered that the content of each element contained in the metal material to be determined is also small). As the standard, the first judgment criterion, which is determined based on the variation in the analysis value of the content of each element actually measured for the preparation metal material, is used. Therefore, based on the content of the trace element contained in the judgment metal material, Even if different materials are judged, accurate judgment can be expected.
It should be noted that the predetermined value of the ladle analysis value, which is a boundary value for selectively using the first judgment criterion and the second judgment criterion, is, for example, one of the first judgment criterion and the second judgment criterion that has a larger deviation from the ladle analysis criterion. It may be determined that the criterion is used in the determination step. Specifically, for example, when the predetermined value of the ladle analysis value is Rc, when the ladle analysis value = Rc, the upper limit value of the first determination criterion = the upper limit value of the second determination criterion, the lower limit of the first determination criterion. Value = lower limit value of the second determination criterion, and when Ladle analysis value <Rc, upper limit value of the first determination criterion> upper limit value of the second determination criterion, lower limit value of the first determination criterion <lower limit of the second determination criterion And a predetermined value such that when the ladle analysis value> Rc, the upper limit value of the first judgment criterion <the upper limit value of the second judgment criterion, the lower limit value of the first judgment criterion> the lower limit value of the second judgment criterion. Rc may be determined.

Here, according to the results examined by the present inventors, the analysis value of the content of each element by the fluorescent X-ray analysis apparatus is determined according to the distance in the facing direction between the determination target metal material and the fluorescent X-ray analysis apparatus. However, there is a case where it varies so as to affect the result of the foreign material determination of the determination target metal material. In other words, if the correction is performed using the same correction content regardless of the separation distance, the accuracy of correction of the analysis value of the content of each element may be lowered, which may result in an erroneous determination in the different material determination.
For this reason, preferably, in the first preparation step, the separation distance between each of the preparation metal materials and the fluorescent X-ray analysis device is changed, and the first step and the second step are repeatedly executed. Thus, the plurality of correction contents according to the separation distance are determined, and in the correction process, the determination target metal material when analyzed in the analysis process among the plurality of correction contents determined in the first preparation process The correction content is selected according to the distance between the X-ray fluorescence analyzer and the X-ray fluorescence analyzer, and the analysis value of the content of each element obtained in the analysis step is corrected by the selected correction content.

  According to the above preferred configuration, in the first preparation step, a plurality of correction contents are determined in accordance with the separation distance between each preparation metal material and the fluorescent X-ray analysis device in the facing direction, and in the correction step, the plurality of corrections are performed. Among the contents, the correction contents are selected and corrected according to the distance in the facing direction between the determination target metal material and the fluorescent X-ray analysis device when analyzed in the analysis step. That is, the correction is performed with the correction content that matches the distance in the facing direction between the determination target metal material and the fluorescent X-ray analysis device when actually analyzed. Therefore, even if the distance between the metal to be judged and the fluorescent X-ray analyzer changes in the opposing direction, the analysis value of the content of each element can be corrected with appropriate correction content. Is.

In addition, according to the results of the study by the present inventors, the variation in the analysis value of the content of each element by the fluorescent X-ray analysis device, depending on the transport speed of the metal material to be determined during the analysis step, It may fluctuate so as to affect the result of the determination of the dissimilar material of the determination target metal material. In other words, the determination is made using the same first determination criterion (determination criterion determined based on the variation in the analysis value of the content of each element contained in the preparation metal material) regardless of the transport speed of the determination metal material. Therefore, when a different material is determined based on the content of a trace amount of element contained in the determination target metal material, an erroneous determination may occur.
For this reason, it is preferable that the transport speed of the metal material for preparation at the time of analysis by the X-ray fluorescence analyzer be changed and the first step of the first preparation step be repeatedly performed to thereby perform the second preparation. In the step, a plurality of the first determination criteria according to the transport speed of the preparation metal material is determined, and in the determination step, the analysis step among the plurality of first determination criteria determined in the second preparation step. After selecting the first criterion according to the transport speed of the metal material to be determined when analyzed in step 1, the Ladle analysis value of each of the referenced elements is less than a predetermined value, and the corrected value obtained by the correction step is When any of the analysis values of the content of each element does not satisfy the selected first determination criterion, the determination target metal material is determined to be a different material from the planned product type.

  According to the above preferred configuration, in the second preparation step, a plurality of first determination criteria corresponding to the transportation speed of the preparation metal material is determined, and in the determination step, among the plurality of first determination criteria, the analysis step is performed. The first judgment criterion corresponding to the transport speed of the judged metal material at the time of analysis is selected and judged. That is, the determination is made according to the first determination criterion that matches the transportation speed of the determination target metal material when actually analyzed. For this reason, even if the transport speed of the metal material to be judged changes, it is possible to judge a different material with an appropriate judgment criterion.

  According to the present invention, it is possible to more accurately determine whether or not a determination target metal material is a different material different from a planned product type.

It is a schematic diagram which shows the schematic structure of the different material determination apparatus for implementing the different material determination method of the metal material which concerns on one Embodiment of this invention. It is a flowchart which shows the schematic procedure of the foreign material determination method of the metal material which concerns on one Embodiment of this invention. It is a figure which shows an example of the analysis value of the content of Cr and Fe contained in the preparation metal material P1 of one kind. It is a figure which shows an example of the correlation of the peak analysis value before correction of Ni, and a Ladle analysis value. It is a figure which shows an example of the correction content determined by the 1st preparation process S1 shown in FIG. It is a figure which shows an example of the determination criteria determined by the 2nd preparatory process S2 shown in FIG. It is a figure which shows an example of the relationship between the analysis value of the content of Ni contained in the preparation metal material P1 of one kind, and the separation distance of the preparation metal material P1 and the fluorescent X-ray analysis apparatus 10 in the facing direction. .. It is a figure which shows an example of the relationship between the analysis value of the content of Ni contained in the preparation metal material P1 of one kind, and the conveyance speed of the preparation metal material P1. No. shown in FIG. 2 and No. The analysis values of the corrected content of each element, the Ladle analysis value of each element, and the different material determination method according to the embodiment of the present invention, which are obtained for the determination target metal materials P2 of 3 types, are applied. An example of the determination criteria of each element and the determination criteria of each element applied in the foreign material determination method using the material standard will be shown. No. shown in FIG. 6 and No. The analysis value of the content of each element after the correction, which is obtained for the 12 types of the judgment target metal materials P2, the Ladle analysis value of each element, and each element applied in the foreign material judgment method according to the present embodiment, An example of the determination criteria and the determination criteria of each element applied in the foreign material determination method using the material standard will be shown. No. 2, No. 3, No. 6, No. It is a figure which shows the determination result at the time of carrying out the different material determination of the to-be-determined metal material P2 which is 12 according to the determination criteria of each kind shown in FIG. 9 and FIG. No. shown in FIG. It is a figure which shows an example of the analysis value of the content of Fe contained in the metal materials P of 12 types.

Hereinafter, referring to the accompanying drawings as needed, regarding a method for determining a different material of a metal material according to an embodiment of the present invention, when determining a different material in an inspection line before shipping a metal material (steel pipe in this embodiment) as a product Will be described as an example. In the present embodiment, a steel pipe is exemplified as the metal material, but the present invention is not limited to this, and a solid cylindrical metal material (metal rod) or a hollow cylindrical metal material (metal pipe) Including metal pipes other than steel pipe), etc., can be applied to various metal materials.
FIG. 1 is a schematic diagram showing a schematic configuration of a foreign material determination apparatus for carrying out a foreign material foreign material determination method according to an embodiment of the present invention.
As shown in FIG. 1, the foreign material determination device 100 of the present embodiment includes a fluorescent X-ray analysis device 10, an identifier detection device 20, a reference device 30, and a determination device 40.

The X-ray fluorescence analyzer 10 includes a measurement head 11 and an arithmetic control unit 12.
The measurement head 11 is arranged so as to be located below the metal material P when the metal material P (preparation metal material P1, determination target metal material P2) is analyzed. The measuring head 11 of the present embodiment can be moved up and down, and thus the separation distance between the metal material P and the measuring head 11 in the facing direction (the vertical direction in the present embodiment) can be adjusted. The measurement head 11 has an X-ray source 11a and a detector 11b. The X-ray source 11a irradiates the portion of the metal material P facing the X-ray source 11a with X-rays. The detector 11b detects the fluorescent X-rays generated from the metal material P by the X-rays emitted from the X-ray source 11a, and outputs a signal according to the intensity of the detected fluorescent X-rays and the like.
The arithmetic control unit 12 controls the operation of the measuring head 11 such as the irradiation of X-rays from the X-ray source 11a and the detection of fluorescent X-rays by the detector 11b, and the metal material based on the output signal of the detector 11b. The content (content rate) of each of the plurality of elements contained in P is calculated. The calculation control unit 12 outputs the content of each element, which is the calculation result, to the determination device 40.
As the fluorescent X-ray analyzer 10, a commercially available fluorescent X-ray analyzer of energy dispersion type or wavelength dispersion type can be applied.

  The identifier detection device 20 is a device that detects an identifier attached to the metal material P. As the detection method of the identifier detection device 20, various methods such as optical, magnetic, and electrical can be adopted according to the form of the identifier to be detected. For example, when the identifier is a bar code and the bar code label BR on which the bar code is printed is affixed to the metal material P, the identifier detection device 20 is a bar code reading device that is an optical detection system. Is used. The identifier detecting device 20 of the present embodiment is not a stationary type but a portable type. Therefore, the operator visually confirms the part of the metal material P to which the identifier is attached (the part of the metal material P to which the barcode label BR is attached), and brings the identifier detecting device 20 carried by the operator close to the above-mentioned part. By this, the identifier is detected. However, the present invention is not limited to this, and if the identifier is attached to the fixed position of the metal material P, it is also possible to employ the stationary type identifier detection device 20.

The identifier detected by the identifier detecting device 20 is input to the reference device 30. On the other hand, the upper process computer (hereinafter, referred to as “upper process computer”) 200 for controlling the inspection line melts the molten metal which is the raw material of the metal material P associated with the identifier attached to the metal material P. The metal number and the product type associated with the molten metal number and the ladle analysis value of each element constituting the composition of the product type are stored. The ladle analysis value is measured in advance in the molten metal component adjusting step (steel making step when the metal material is steel) and stored in the host computer 200. That is, the host computer 200 stores the type of the metal material P associated with the identifier and the Ladle analysis value of each element forming the composition of the type.
The reference device 30 outputs the identifier input from the identifier detection device 20 to the host computer 200. As a result, the host computer 200 outputs, to the reference device 30, the type of the metal material P associated with the input identifier and the Ladle analysis value of each element that constitutes the composition of the type. The reference device 30 outputs the information input from the host computer 200 to the determination device 40.
Note that the reference device 30 can be configured by, for example, a personal computer in which a program for executing the above operation is installed.

The determination device 40 receives the analysis values of the contents of each of the plurality of elements contained in the metal material P analyzed by the fluorescent X-ray analysis device 10 (calculated by the calculation control unit 12). In addition, the reference device 30 inputs the type of the metal material P associated with the identifier attached to the metal material P and the ladle analysis value of each element constituting the composition of the type to the determination device 40. .. The determination device 40 corrects the analysis value by the fluorescent X-ray analysis device 10 based on these input information, and compares the corrected analysis value with the determination criterion according to the Ladle analysis value, thereby determining the metal material. It is determined whether P is a different material.
The determination device 40 can be composed of, for example, a personal computer in which a program for executing the above operation is installed.

  In the schematic configuration described above, the different material determination device 100 includes the identifier detection device 20 and the example in which the identifier detected by the identifier detection device 20 is input to the reference device 30 has been described, but the present invention is not limited to this. Not a thing. For example, the operator can visually confirm the identifier and manually input it to the reference device 30.

Hereinafter, a foreign material determination method using the foreign material determination device 100 having the above-described schematic configuration will be described.
FIG. 2 is a flow chart showing a schematic procedure of a foreign material determination method for a metal material according to an embodiment of the present invention. As shown in FIG. 2, the dissimilar material determination method according to this embodiment includes a first preparation step S1, a second preparation step S2, an analysis step S3, a recognition step S4, a correction step S5, and a determination step S6. including. Hereinafter, the respective steps S1 to S6 will be sequentially described with reference to FIG. 2 and other drawings as appropriate.

<First preparation step S1>
In the first preparation step S1, the correction content for the analysis value of the content of the element obtained by the fluorescent X-ray analysis apparatus 10 is determined for each type and for each element constituting the composition of each type.
Specifically, the first preparation step S1 includes a first step S11 and a second step S12.

(First step S11)
In the first step S11, a plurality of types of preparation metal materials (steel pipes in the present embodiment) P1 of known types are prepared. The preparation metal material P1 is preferably prepared for all types that can be conveyed to the inspection line in which the foreign material determination device 100 is installed.
Next, in the first step S11, one type of preparation metal material P1 is conveyed to a position facing the fluorescent X-ray analysis apparatus 10. Specifically, in the inspection line in which the X-ray fluorescence analyzer 100 is installed, a transfer mechanism (not shown in FIG. 1) including a transfer roller that transfers the metal material P in the longitudinal direction is installed. By driving the transport mechanism, the preparatory metal material P1 is transported, and a predetermined portion of the preparatory metal material P1 reaches a position facing the measurement head 11 of the X-ray fluorescence analyzer 10.
Next, in the first step S11, the content of each element contained in the preparation metal material P1 is analyzed by the fluorescent X-ray analysis device 10. That is, a predetermined portion of the preparation metal material P1 facing the measurement head 11 is irradiated with X-rays from the X-ray source 11a, fluorescent X-rays are detected by the detector 11b, and the calculation control unit 12 prepares the preparation metal material. The content of each element contained in P1 is calculated.
Containing each element contained in each preparatory metal material P1 by sequentially repeating the transportation of the preparatory metal material P1 and the analysis by the fluorescent X-ray analysis device 10 for all prepared preparatory metal materials P1. The amount will be analyzed. In addition, it is preferable to prepare a plurality of preparatory metal materials P1 of the same type and repeatedly analyze the preparatory metal materials P1 of the same type a plurality of times.

The analysis by the fluorescent X-ray analysis apparatus 10 may be performed while the preparation metal material P1 is stopped, or when the preparation metal material P1 is conveyed at a predetermined conveyance speed. good.
When analyzing a plurality of parts in a state in which the preparation metal material P1 is stopped, by performing intermittent conveyance in which the preparation metal material P1 is conveyed and stopped repeatedly, a plurality of pieces are prepared in the longitudinal direction of the preparation metal material P1. It is possible to perform analysis of different sites. Further, in the case where the transport mechanism is configured to be able to rotate the preparation metal material P1 in the circumferential direction, the preparation metal material P1 is rotated and stopped repeatedly, so that the preparation metal material P1 is rotated in the circumferential direction. It is also possible to analyze multiple different sites.
Further, when analyzing a plurality of parts in a state where the preparation metal material P1 is conveyed at a predetermined conveyance speed, based on the fluorescent X-ray generated by the X-ray irradiated for a predetermined time (for example, about 10 seconds). The preparation is performed by analyzing one part of the preparation metal material P1 and analyzing the other part of the preparation metal material P1 based on the fluorescent X-rays generated by the X-rays irradiated for the next predetermined time. It is possible to analyze a plurality of different parts in the longitudinal direction of the working metal material P1.

(Second step S12)
In the second step S12, first, the Ladle analysis value of each element contained in the preparation metal material P1 is referred to. It is possible to refer to the preparatory metal material P1 because its kind is known and the Laddle analysis value of each element constituting the composition of the kind is stored in the high-order process control computer 200.
Next, in the second step S12, fluorescence is detected based on the deviation between the referenced Ladle analysis value of each element and the analysis value of the content of each element contained in the preparation metal material P1 obtained in the first step S11. The correction content for the analysis value of the content of the element obtained by the X-ray analysis apparatus 10 is determined.

FIG. 3 is a diagram showing an example of analysis values of the contents of Cr and Fe contained in the preparation metal material P1 of one type. FIG. 3A shows the analytical value of the Cr content, and FIG. 3B shows the analytical value of the Fe content. The vertical axis of FIG. 3 is the analysis value by the fluorescent X-ray analyzer 10, and the horizontal axis is the frequency. Specifically, FIG. 3 shows that the content of Cr and Fe is repeated about 100 times for one kind of preparation metal material P1 (for different parts of the same preparation metal material P1 or different preparation metal material P1). It is a figure which shows the frequency distribution of the analysis value at the time of analyzing. More specifically, in the data shown in FIG. 3, the preparatory metal material P1 and the fluorescent X-ray analyzer 10 (measuring head 11) are set to a separation distance of 5 mm in the facing direction, and the preparatory metal material P1 is conveyed. It is the result of analysis while making the irradiation time of X-rays per time 10 seconds while transporting at a speed of 22 m / min.
In the example shown in FIG. 3A, a deviation occurs between the Ladle analysis value of Cr and the analysis value of the Cr content which are referred to for the preparation metal material P1 of one type. Further, in the example shown in FIG. 3B, a deviation occurs between the Ladle analysis value of Fe referred to for the preparation metal material P1 of one type and the analysis value of the Fe content. Therefore, as described above, in the second step S12, the correction content for the analysis value of the content of the element obtained by the fluorescent X-ray analysis apparatus 10 is determined based on this deviation.

Specifically, for example, a deviation (Ladle analysis) between a referenced Ladle analysis value and an analysis value having a peak frequency in the frequency distribution of the analysis values as shown in FIG. 3 (hereinafter appropriately referred to as “peak analysis value”) It is possible to calculate (value-peak analysis value) and determine the correction content to add the calculated deviation. That is, assuming that the analysis value before correction obtained by the fluorescent X-ray analysis apparatus 10 is X, the calculated deviation is B, and the analysis value after correction is Y, the correction content is expressed by the following formula (1), for example. Be done.
Y = X + B (1)
By performing the correction represented by the above formula (1), the corrected analysis value Y can be brought close to the Ladle analysis value.

Even if the same kind is used, since the content of the element varies over a wide range, the deviation B in the above formula (1) may be set to a constant value regardless of the uncorrected analysis value X. There are elements (for example, Ni) that cannot be corrected with sufficient accuracy. For such an element, for example, the deviation B in the above equation (1) may be represented by a linear function (α · X + β) of the analysis value X before correction. By substituting B = (α · X + β) into the above equation (1), the following equation (2) is obtained.
Y = X + (α · X + β) (2)
In the above formula (2), if a = (1 + α) and b = β, the following formula (3) is obtained.
Y = a · X + b (3)
As for the slope a and the intercept b of the linear function represented by the above equation (3), the peak analysis value before correction is substituted into X of the equation (3), and the Ladle analysis value is substituted into Y of the equation (3). Then, it can be calculated by performing an approximate calculation such as the least square method.
Since the above formula (1) can be considered to correspond to the case where a = 1 in the formula (3), it does not matter whether the element content varies over a wide range within the same product type. Alternatively, it is also possible to apply the correction contents represented by the equation (3).

FIG. 4 is a diagram showing an example of the correlation between the peak analysis value of Ni before correction and the Ladle analysis value. The vertical axis (Y axis) in FIG. 4 is the Ladle analysis value, and the horizontal axis (X axis) is the peak analysis value before correction. As shown in FIG. 4, when both are approximated by a linear function by the method of least squares, the linear function (approximation line) is Y = 0.98 · X + 0.23. That is, it means that a = 0.98 and b = 0.23 in the above equation (3).
By performing the correction represented by the above formula (3), it is possible to bring the analysis value Y after correction close to the Ladle analysis value.

  The determination of the correction content described above is sequentially repeated for the prepared metal materials P1 of all the prepared products, so that in the second step S12, the fluorescence X is obtained for each product and for each element constituting the composition of each product. The correction content for the analysis value of the content of the element obtained by the line analysis device 1 is determined.

FIG. 5 is a diagram showing an example of the correction contents determined in the first preparation step S1. In the example shown in FIG. 1-No. The correction contents (including the case of a = 1) represented by the above equation (3) are determined for each of 16 types up to 16. Furthermore, the correction content represented by the above-mentioned formula (3) is determined for each of the 10 elements of Mn, Cu, Ni, Cr, Mo, Co, Ti, Nb, Fe, and W that compose the composition of each product type. ing. However, in the example shown in FIG. 5, the correction contents are the same for all types except Cr and Fe.
The correction content as shown in FIG. 5 determined in the first preparation step S1 is stored in the determination device 40.

  In the present embodiment, as described above, the correction content is determined based on the deviation between the ladle analysis value and the peak analysis value, but the present invention is not limited to this, and for example, the ladle analysis value and the analysis can be performed. It is also possible to determine the correction content based on the deviation from the average value.

<Second preparation step S2>
In the second preparatory step S2, a judgment criterion corresponding to the ladle analysis value (a judgment criterion of the analytical value after correction based on the correction content in the first preparation step S1) is determined for each element constituting the composition of the variety.
FIG. 6 is a diagram showing an example of the determination criteria determined in the second preparation step S2. FIG. 6A is an explanatory diagram showing the content of the determination standard, and FIG. 6B is a diagram showing an example of the values of the parameters A to D shown in FIG. 6A.
As shown in FIG. 6A, the determination criteria determined in the second preparation step S2 of the present embodiment are the first determination criteria when the ladle analysis value R is less than the predetermined value Rc and the ladle analysis value R is predetermined. It is composed of a second determination criterion when the value is Rc or more.

  The first criterion is determined based on the ladle analysis value R and the variation in the analysis value of the content of each element contained in the preparatory metal material P1 obtained in the first step S11 of the first preparatory step S1. It In the present embodiment, as shown in FIG. 6A, the upper limit value of the first determination criterion is the ladle analysis value R + A and the lower limit value is the ladle analysis value R + B. That is, when the corrected analysis value Y is R + B ≦ Y ≦ R + A, the first determination criterion is satisfied. In FIG. 6A, the data plotted as “◯” in the region of the first determination criterion satisfies the first determination criterion, and the data plotted as “x” does not satisfy the first determination criterion. become. For example, when the standard deviation of the variation of the analysis value of the content of each element contained in the preparatory metal material P1 as illustrated for Cr and Fe in FIG. 3 is σ, the above parameter A = + 4σ and the parameter B = − It is determined to be 4σ. The values of the parameters A and B of each element shown in FIG. 6B are the values of + 4σ and -4σ obtained in the first step S11 of the first preparation step S1.

  The second criterion is determined based on the value obtained by multiplying the Ladle analysis value R by a predetermined coefficient. In the present embodiment, as shown in FIG. 6A, the upper limit value of the second criterion is C · R and the lower limit value is D · R. That is, when the corrected analysis value Y is D · R ≦ Y ≦ C · R, the second determination criterion is satisfied. In FIG. 6A, the data plotted with “◯” in the area of the second judgment criterion satisfies the second judgment criterion, and the data plotted with “x” does not satisfy the second judgment criterion. become. In the example shown in FIG. 6B, each element has C = 1.1 and D = 0.9.

It should be noted that the predetermined value Rc of the Ladle analysis value R, which is a boundary value for selectively using the first determination criterion and the second determination criterion, does not need to be a common value for each element, and may be set to a different value for each element. good. The predetermined value Rc may be determined, for example, so that one of the first determination criterion and the second determination criterion that has a larger deviation from the Ladle analysis value R is used in the determination step S6.
Specifically, when the ladle analysis value R = Rc, the upper limit value R + A of the first judgment criterion = the upper limit value CR of the second judgment criterion, the lower limit value R + B of the first judgment criterion = the lower limit value of the second judgment criterion. When the ladle analysis value R <Rc, the upper limit value R + A of the first determination criterion, the upper limit value C · R of the second determination criterion, and the lower limit value R + B of the first determination criterion of the second determination criterion When the lower limit value D · R is reached and the ladle analysis value R> Rc, the upper limit value R + A of the first determination criterion <the upper limit value C · R of the second determination criterion, the lower limit value R + B of the first determination criterion> the second determination criterion The predetermined value Rc may be determined so as to be the lower limit value D · R.

As described above, the determination criteria determined in the second preparation step S2 of the present embodiment are the elements actually measured for the preparation metal material P1 as the determination criteria when the ladle analysis value R is smaller than the predetermined value Rc. When a different material is determined based on the content of a trace amount of element contained in the determination target metal material P2 in the determination step S6, which will be described later, since the first determination criterion determined based on the variation σ of the analysis value of the content of However, accurate determination can be expected.
The determination criteria as shown in FIG. 6 determined in the second preparation step S2 are stored in the determination device 40.

<Analysis step S3>
In the analysis step S3, the determination target metal material P2, which is a determination target of whether or not it is a different material, is transported to a position facing the fluorescent X-ray analysis device 10, similarly to the preparation metal material P1. For example, a bar code label BR having a bar code printed thereon is attached to the judged metal material P2, so that the judged metal material P2 has an identifier represented by a bar code. Then, similar to the preparation metal material P1, the content of each of the plurality of elements (for example, 10 kinds of elements shown in FIG. 5) contained in the determination metal material P2 is analyzed by the fluorescent X-ray analysis device 10.
The analysis value of the content of each element analyzed in the analysis step S3 is input from the fluorescent X-ray analysis device 10 to the determination device 40.

<Recognition step S4>
In the recognition step S4, the identifier attached to the determination target metal material P2 is detected, and the planned type of the determination target metal material P2 associated with the identifier (for example, No. 1 to No. 16 shown in FIG. Recognize one of 16 types).
Specifically, the identifier detection device 20 detects the identifier attached to the determination target metal material P2, and the detected identifier is input to the reference device 30. The reference device 30 outputs the identifier input from the identifier detection device 20 to the host computer 200. As a result, the host computer 200 configures the planned product type (product type scheduled to be transported on the inspection line) of the judgment target metal material P2 associated with the input identifier and the composition of each of the planned product types. The Ladle analysis value of the element is output to the reference device 30. The planned type of the judgment target metal material P2 and the Ladle analysis value of each element constituting the composition of the planned type are input from the reference device 30 to the judgment device 40.

<Correction step S5>
In the correction step S5, the analysis value of the content of each element obtained in the analysis step S3 is corrected using the correction content determined in the first preparation step S1 for the planned type recognized in the recognition step S4.
Specifically, as described above, the determination device 40 receives the analysis values of the contents of the respective elements contained in the determination target metal material P2 analyzed by the fluorescent X-ray analysis device 10. Further, the reference device 30 inputs to the determination device 40 the planned product type of the determination target metal material P2 associated with the identifier attached to the determination target metal material P2. The determination device 40 corresponds to the planned product type input from the reference device 30 among the correction contents (see FIG. 5) determined and stored for each product type and for each element constituting the composition of each product type as described above. Select the correction details. For example, the planned variety is No. In the case of No. 6, No. 6 shown in FIG. The correction contents of 6 types will be selected. Then, the determination device 40 corrects the analysis value of the content of each of the plurality of elements analyzed by the fluorescent X-ray analysis device 10 using the selected correction content.

<Judgment step S6>
In the determination step S6, the Ladle analysis value of each element constituting the composition of the planned product type is referred to. That is, as described above, the Ladle analysis value of each element constituting the composition of the planned variety is input from the reference device 30 to the determination device 40. Then, the determination device 40 determines the determination standard of each element determined in the second preparation step according to the analysis value of the content of each element after correction obtained in the correction step S5 and the Ladle analysis value of each element referred to. Contrast with. If any of the corrected analysis values of the content of each element does not satisfy the determination criterion of each element, the determination device 40 determines that the determination target metal material P2 is a different material from the planned product type. On the other hand, the determination device 40 determines that the determination target metal material P2 is not a different material (a metal material that matches the planned product type) when all of the corrected analysis values of the content of each element satisfy the determination criteria of each element. ) Is determined.
Specifically, in the determination step S6 of the present embodiment, the determination device 40 determines that the Ladle analysis value R of each referenced element is less than the predetermined value Rc, and the corrected element of each element obtained in the correction step S5. When any of the analysis values Y of the content does not satisfy the first determination criterion, it is determined that the determination target metal material P2 is a different material from the planned product type. On the other hand, the determination device 40 determines that the to-be-determined metal material P2 is not a different material when all of the corrected analysis values Y of the content of each element satisfy the first determination criterion. Further, the determination device 40 determines that the ladle analysis value R of each element referred to is equal to or larger than the predetermined value Rc, and any one of the analysis values Y of the corrected content of each element obtained in the correction step S5 is the second value. When the determination criteria are not satisfied, the determination target metal material P2 is determined to be a different material from the planned product type. On the other hand, the determination device 40 determines that the determination target metal material P2 is not a different material when all the analysis values Y of the corrected content of each element satisfy the second determination criterion.

  By including the steps S1 to S6 described above, the dissimilar material determination method according to the present embodiment can more accurately determine whether or not the determination target metal material P2 is different from the planned product type. ..

  Here, according to the result of examination by the present inventors, according to the separation distance of the determination target metal material P2 and the fluorescent X-ray analysis apparatus 10 (measurement head 11) in the facing direction (the vertical direction in the present embodiment). The analysis value of the content of each element by the fluorescent X-ray analysis apparatus 10 may vary so as to affect the result of the foreign material determination of the determination target metal material P2. In other words, in the correction step S5, if the same correction content is used regardless of the separation distance, the accuracy of correction of the analysis value of the content of each element is lowered, and thus an erroneous determination is made in the different material determination. May get.

FIG. 7 shows an example of the relationship between the analysis value of the content of Ni contained in the preparation metal material P1 of one type and the distance in the facing direction between the preparation metal material P1 and the X-ray fluorescence analyzer 10. FIG. The vertical axis of FIG. 7 is the ratio of the analysis value by the X-ray fluorescence analyzer 10 and the Ladle analysis value, and the horizontal axis is the facing direction of the preparation metal material P1 and the X-ray fluorescence analyzer 10 (measurement head 11). The separation distance. In the figure, the data plotted with “◯” indicate peak analysis values, and the bars extending vertically from “◯” indicate variations in analysis values. Specifically, FIG. 7 shows that for one kind of preparation metal material P1 (for different parts of the same preparation metal material P1 or for different preparation metal material P1), each separation distance is repeated about 100 times. It is a figure which shows the analysis value when analyzing the content of Ni. More specifically, the data shown in FIG. 7 is the result of analysis with the preparatory metal material P1 stopped (conveyance speed 0 m / min) with the irradiation time of X-rays per time set to 5 seconds. ..
As shown in FIG. 7, the peak analysis value of the Ni content varies by about 10% depending on the separation distance.

  Therefore, in order to reduce the influence of the separation distance, in the first preparation step S1, the separation distance in the facing direction between each preparation metal material P1 and the X-ray fluorescence spectrometer 10 is changed to change the first step S11 and the first step S11. It is preferable to determine the plurality of correction contents according to the separation distance by repeatedly performing the two steps S12. That is, in the first preparation step, it is preferable that a plurality of correction contents as shown in FIG. 5 are determined according to the separation distance and stored in the determination device 40. Then, in the correction step S5, the determination device 40 opposes the determination target metal material P2 and the fluorescent X-ray analysis device 10 in the analysis process S3 among the plurality of correction contents determined in the first preparation process S1. It is preferable that the correction content is selected according to the distance in the direction and the analysis value of the content of each element obtained in the analysis step S3 is corrected by the selected correction content.

According to the above-described preferable configuration, for example, the distance between the determination target metal material P2 and the fluorescent X-ray analysis device 10 in the facing direction is changed such that the transport position of the determination target metal material P2 is changed due to the change of the specification of the inspection line or the like. Even under changing conditions, it is possible to correct the analysis value of the content of each element with appropriate correction content.
The distance between the determination target metal material P2 and the X-ray fluorescence analyzer 10 in the facing direction can be measured by installing a distance meter such as a laser distance meter in the inspection line. By inputting this measurement result to the determination device 40, the determination device 40 can automatically select the correction content according to the separation distance. However, the present invention is not limited to this, and the separation distance is calculated based on the initial position of the measurement head 11 of the X-ray fluorescence analyzer 10 and the command value of the amount of elevation of the measurement head 11, and this calculation is performed. It is also possible to input the result to the determination device 40.

  Further, according to the results of the examination by the present inventors, the analysis value of the content of each element by the fluorescent X-ray analysis apparatus 10 is determined according to the transport speed of the determination target metal material P2 at the time of analysis in the analysis step S3. The variation may vary so as to affect the result of the foreign material determination of the determination target metal material P2. In other words, the same first determination criterion (determination criterion determined based on the variation in the analysis value of the content of each element contained in the preparatory metal material P1) is used regardless of the transport speed of the determination metal material P2. If the different material is determined based on the content of the trace amount of element contained in the determination target metal material P2, there is a possibility that an erroneous determination may occur.

FIG. 8: is a figure which shows an example of the relationship between the analysis value of the content of Ni contained in the preparation metal material P1 of one kind, and the conveyance speed of the preparation metal material P1. The vertical axis of FIG. 8 is the ratio of the analysis value by the fluorescent X-ray analysis apparatus 10 and the ladle analysis value, and the horizontal axis is the transport speed of the preparation metal material P1. In the figure, the data plotted with “◯” indicate peak analysis values, and the bars extending vertically from “◯” indicate variations in analysis values. Specifically, FIG. 8 shows that for one kind of preparation metal material P1 (for different parts of the same preparation metal material P1 or for different preparation metal material P1), it is repeated about 100 times at each conveying speed. It is a figure which shows the analysis value when analyzing the content of Ni. More specifically, in the data shown in FIG. 8, the separation distance in the facing direction between the preparation metal material P1 and the fluorescent X-ray analysis apparatus 10 (measurement head 11) is set to 7 mm, and the X-ray per It is the result of analysis with irradiation time of 5 seconds.
As shown in FIG. 8, the peak analysis value of the Ni content does not change much depending on the transport speed of the preparatory metal material P1. However, the variation in the analysis value of the Ni content is larger when the transport speed of the preparatory metal material P1 is higher than when the preparatory metal material P1 is stopped.

  Therefore, in order to reduce the influence of the transport speed, the transport speed of the preparatory metal material P1 at the time of analysis by the fluorescent X-ray analyzer 10 is changed and the first step S11 of the first preparatory step S1 is repeatedly executed. Therefore, in the second preparation step S2, it is preferable to determine a plurality of first determination criteria according to the transportation speed of the preparation metal material P1. That is, in the second preparation step S2, it is preferable to determine a plurality of first determination criteria as shown in FIG. 6 according to the transport speed and store them in the determination device 40. Then, in the determination step S6, the determination device 40 determines, among the plurality of first determination criteria determined in the second preparation step S2, the first determination criterion corresponding to the transport speed of the determination target metal material P2 when the analysis is performed in the analysis step S3. A first criterion selected by selecting a criterion and the ladle analysis value R of each element referred to is less than a predetermined value Rc, and one of the analysis values of the content of each element after correction obtained in the correction step S5 is selected. If the judgment criteria are not satisfied, the judgment target metal material P2 is judged to be a different material from the planned product type (if all the analysis values of the content of each element after correction satisfy the selected first judgment criteria, It is preferable to determine that the determination metal material P2 is not a different material).

According to the above-described preferable configuration, for example, even in a situation in which the transport speed of the determination target metal material P2 changes due to a change in the operating condition of the inspection line, it is possible to determine a different material with an appropriate determination standard. is there.
The transport speed of the determination target metal material P2 can be measured using, for example, a speedometer generally installed in the inspection line. By inputting this measurement result to the determination device 40, the determination device 40 can automatically select the first determination criterion according to the transport speed.

Hereinafter, an example of the result of the foreign material determination performed by the foreign material determination method using the ladle analysis value according to the present embodiment will be described. In addition, in order to compare with the foreign material determination method according to the present embodiment, a foreign material determination method using a material standard was performed for the same determination target metal material P2. However, also in the foreign material determination method using the material standard, the correction of the analysis value of the content was performed in the same manner as the foreign material determination method according to the present embodiment.
9 is the same as No. 1 shown in FIG. 2 and No. The analysis value of the content of each element after correction obtained for the judgment target metal material P2 of 3 types, the Ladle analysis value of each element, and each element applied in the foreign material judgment method according to the present embodiment. An example of the determination criteria and the determination criteria of each element applied in the foreign material determination method using the material standard will be shown. 9 (a) shows No. 9 (b) shows the results obtained for the judgment target metal material P2 of the type 2. The results obtained for the judged metal materials P2 of 3 types are shown. Similarly, in FIG. 6 and No. The analysis value of the content of each element after the correction, which is obtained for the 12 types of the judgment target metal materials P2, the Ladle analysis value of each element, and each element applied in the foreign material judgment method according to the present embodiment, An example of the determination criteria and the determination criteria of each element applied in the foreign material determination method using the material standard will be shown. 10 (a) shows No. 10 (b) shows the results obtained for the judged metal material P2 of the product type No. 6 shown in FIG. The result obtained about 12 types of to-be-determined metal materials P2 is shown.
In FIG. 9 and FIG. 10, the “determination criterion upper limit value (present invention)” is the upper limit value of the determination criterion (first determination criterion or second determination criterion) of each element applied in the foreign material determination method according to the present embodiment. Means The “determination criterion lower limit value (present invention)” means the lower limit value of the determination criterion (first determination criterion or second determination criterion) of each element applied in the foreign material determination method according to the present embodiment. “Judgment standard upper limit value (material standard)” means the upper limit value of the judgment standard of each element applied in the different material judging method using the material standard. The “determination criterion lower limit value (material standard)” means the lower limit value of the determination criterion of each element applied in the foreign material determination method using the material standard. "-" Shown in each criterion column means that the element corresponding to each column is not used for different material determination.

For example, No. 1 shown in FIG. In the case of the 2 varieties, the ladle analysis value of Mn is 1.50 [%]. As shown in FIG. 6 described above, in the present embodiment, the upper limit value of the first determination criterion of Mn is the ladle analysis value R + 0.35 [%], and the upper limit value of the second determination criterion of Mn is the ladle analysis value R. Since it is × 1.1 [%], Rc for Mn is 3.50 [%] from Rc + 0.35 = Rc × 1.1. Since the ladle analysis value of Mn shown in FIG. 9A is 1.50 [%] as described above and is less than Rc, the first judgment criterion is applied to Mn in the judgment step S6. become. Therefore, the upper limit of the Mn determination criterion applied in the foreign material determination method according to the present embodiment is 1.50 + 0.35 = 1.85 [%], as shown in FIG. 9A. Similarly, the lower limit of the Mn determination standard is 1.50-0.35 = 1.15 [%].
On the other hand, No. 1 shown in FIG. In the case of the 2 types, the Ladle analysis value of Cr is 17.60 [%]. As shown in FIG. 6 described above, in the present embodiment, the upper limit value of the first determination criterion of Cr is the ladle analysis value R + 1.00 [%], and the upper limit value of the second determination criterion of Cr is the ladle analysis value R. Since it is × 1.1 [%], Rc + 1.00 = Rc × 1.1, and thus Rc = 10.00 [%] for Cr. As described above, the Ladle analysis value of Cr shown in FIG. 9A is 17.60 [%] and is Rc or more. Therefore, in the determination step S6, the second determination criterion is applied to Cr. become. Therefore, the upper limit value of the Cr determination criterion applied in the foreign material determination method according to the present embodiment is 17.60 × 1.1 = 19.36 [%], as shown in FIG. 9A. Similarly, the lower limit of the Cr determination standard is 17.60 × 0.9 = 15.84 [%].
Regarding the judgment criteria of each element of each kind shown in FIGS. 9 and 10, the upper limit value and the lower limit value of the applicable judgment criteria are determined in the same manner as above.

FIG. 11 shows that the type is No. 2, No. 3, No. 6, No. It is a figure which shows the determination result at the time of carrying out the different material determination of the to-be-determined metal material P2 which is 12 according to the determination criteria of each kind shown in FIG. 9 and FIG. FIG. 11A shows the result of judgment using the judgment standard applied in the foreign material judgment method according to the present embodiment, and FIG. 11B shows the result judged in the foreign material judgment method using the material standard. The result of the judgment is shown. The vertical axis of FIG. 11 shows the actual product type of the judged metal material P2, and the horizontal axis shows the judgment standard of the planned product type of the judged metal material P2. “O” shown in FIG. 11 indicates a case where it is determined that the material is not different, and “x” indicates a case where the material is determined to be different.
As shown in FIG. 11A, according to the foreign material determination method according to the present embodiment, when the actual product type of the determination target metal material P2 is different from the planned product type, all are different materials (plotted with “×”). ) Is correctly determined. On the other hand, when the actual product type of the metal material P2 to be judged is the same as the planned product type, it is correctly determined that all the materials are not different materials (plotted with “◯”).
On the other hand, as shown in FIG. 11B, according to the foreign material determination method using the material standard, the actual product type of the determination target metal material P2 is No. 2 and the planned variety is No. Even in the case of 3, it is erroneously determined that it is not a different material (plotted with “◯”). The actual product type of the judged metal material P2 is No. 3 and the planned variety is No. Even in the case of 2, it is erroneously determined that it is not a different material (plotted with "○").

Specifically, the actual product type of the judged metal material P2 is No. 2 and the planned variety is No. In the case of 3, the analysis value of the content of each element after correction is as shown in FIG. The result shown in FIG. This is the result of correction as No. 2, but as shown in FIG. 2 varieties and No. Since the correction content is the same as that of the product of No. 3, the planned product is No. The correction result is the same as when the correction is made as 3. No. 1 shown in FIG. No. 2 shown in FIG. Comparing with the criteria of 3 types (the criteria of using the material standard), the criteria of all the elements of Mn, Ni and Cr are satisfied. Therefore, as described above, the actual product type of the judged metal material P2 is No. 2 and the planned variety is No. Even in the case of 3, it is erroneously determined that it is not a different material (plotted with “◯”).
On the other hand, No. 1 shown in FIG. No. 2 shown in FIG. Comparing the determination criteria of the present embodiment of the three types, the corrected analysis value of Ti shown in FIG. 9A is 0.54 [%], whereas the Ti shown in FIG. Since the upper limit value of the judgment standard of No. 3 is 0.35 [%] and the lower limit value is 0.00 [%], the judgment standard is not satisfied. Therefore, as described above, the actual product type of the judged metal material P2 is No. 2 and the planned variety is No. In the case of 3, it is correctly determined that the material is different (plotted with "x").
The actual product type of the judged metal material P2 is No. No. 3 and the planned variety is No. The same applies when the number is 2.
As described above, according to the foreign material determination method according to the present embodiment, it is possible to accurately determine whether or not the determination target metal material P2 is a foreign material different from the planned product type, as compared with the foreign material determination method using the material standard. It is possible.

  Further, according to the foreign material determination method according to the present embodiment, since the analysis value of the fluorescent X-ray analysis apparatus 10 analyzed in the analysis step S3 is corrected in the correction step S5, the analysis value of the fluorescent X-ray analysis apparatus 10 is used as it is. Different materials can be determined more accurately than in the case. Hereinafter, this point will be described with a specific example.

12 is the same as that shown in FIG. It is a figure which shows an example of the analysis value of the content of Fe contained in the metal materials P of 12 types. 12A shows the analysis value before correction, and FIG. 12B shows the analysis value after correction. The vertical axis of FIG. 12 is the analysis value, and the horizontal axis is the frequency. Specifically, FIG. It is a figure which shows the frequency distribution of the analysis value when the content of Fe is repeatedly analyzed about 100 times about the metal materials P of 12 types. Note that FIG. 12A has the same data as the above-described FIG. 3B.
As shown in FIG. The correction contents of Fe for the 12 types are Y = X−0.80. Therefore, the corrected analysis value shown in FIG. 12B is 0.80 [%] smaller than the uncorrected analysis value shown in FIG. 12A. The planned product type of the metal material P shown in FIG. In the case of 12, the ladle analysis value of the metal material P is 4.0 [%], and therefore the first determination criterion is applied as the determination criterion for the different material determination, and as shown in FIG. Has an upper limit value of 5.0 [%] and a lower limit value of 3.0 [%].
Among the analysis values of the Fe content before correction shown in FIG. 12 (a), there is data that does not satisfy the above-mentioned determination criteria. That is, there is a possibility that it may be erroneously determined to be a different material although it is not actually a different material. On the other hand, all the analysis values of the corrected Fe content shown in FIG. 12 (b) satisfy the above determination criteria, so that it is correctly determined that they are not different materials.
As described above, according to the foreign material determination method according to the present embodiment, the analysis value of the fluorescent X-ray analysis apparatus 10 analyzed in the analysis step S3 is corrected in the correction step S5, so that the foreign material can be accurately determined.

10 ... Fluorescent X-ray analysis device 11 ... Measuring head 12 ... Calculation control unit 20 ... Identifier detection device 30 ... Reference device 40 ... Judgment device 100 ... Dissimilar material judgment device BR. ..Bar code label P ... Metal material P1 ... Preparation metal material P2 ... Measured metal material

Claims (4)

A first preparatory step for deciding the correction content for the analysis value of the content of the element obtained by the fluorescent X-ray analysis device, for each kind and for each element constituting the composition of each kind;
A second preparatory step for determining a criterion for the corrected analytical value based on the correction content according to the Ladle analysis value for each element constituting the composition of the variety;
The fluorescent X-ray analysis device is arranged so as to be able to face the judgment target metal material with an identifier, and the content of each of the plurality of elements contained in the judgment metal material is the fluorescent X facing the judgment metal material. An analysis step of analyzing with a line analyzer,
A recognition step of detecting an identifier attached to the judged metal material, and recognizing a planned product type of the judged metal material associated with the identifier,
A correction step of correcting the analysis value of the content of each element obtained by the analysis step, using the correction content determined in the first preparation step for the planned type recognized in the recognition step,
Depending on the Ladle analysis value of each element constituting the composition of the planned variety, the analysis value of the content of each element after the correction obtained by the correction step and the Ladle analysis value of each of the referenced elements When the determination criteria of each element determined in the second preparation step are compared and any of the corrected analysis values of the content of each element does not satisfy the determination criteria of each element, the determination target metal material Includes a determination step of determining that the material is different from the planned product,
The first preparation step is
Prepare a plurality of types of preparation metal materials of known types, make each preparation metal material face the fluorescent X-ray analysis device, and determine the content of each element contained in each of the preparation metal materials. A first step of analyzing by the fluorescent X-ray analyzer,
Based on the difference between the ladle analysis value of each element contained in each of the preparation metal materials and the analysis value of the content of each element contained in each of the preparation metal materials obtained by the first step, A second step of determining correction contents for the analysis value of the content of the element obtained by the fluorescent X-ray analysis device, for each element and for each element constituting the composition of each element,
A method for determining a foreign material of a metal material, comprising: The determination criterion determined in the second preparation step includes a first determination criterion when the Ladle analysis value is less than a predetermined value and a second determination criterion when the Ladle analysis value is a predetermined value or more,
In the second preparation step,
The first criterion is determined based on the ladle analysis value and the variation in the analysis value of the content of each element contained in the preparation metal material obtained in the first step of the first preparation step. Process,
Determining the second criterion based on a value obtained by multiplying the Ladle analysis value by a predetermined coefficient,
The determination step is
When the Ladle analysis value of each element referred to is less than a predetermined value and any of the analysis values of the content of each element after correction obtained by the correction step does not satisfy the first determination criterion, A step of determining that the judgment target metal material is a different material different from the planned product type,
When the ladle analysis value of each of the referenced elements is equal to or more than a predetermined value and any of the corrected analysis values of the content of each element obtained in the correcting step does not satisfy the second determination criterion, A step of determining that the judgment target metal material is a different material different from the planned product type,
The method for determining a foreign material of a metal material according to claim 1, comprising: In the first preparation step, the separation distance is changed by changing the separation distance between the preparation metal material and the fluorescent X-ray analysis device in the facing direction, and repeating the first step and the second step. Decides a plurality of correction contents according to
In the correction step, among the plurality of correction contents determined in the first preparation step, correction according to the distance in the facing direction between the determination target metal material and the fluorescent X-ray analysis device when analyzed in the analysis step Select the content, and correct the analysis value of the content of each element obtained by the analysis step by the selected correction content,
The method for determining a dissimilar material of a metal material according to claim 1 or 2, characterized in that. In the second preparation step, the preparation step is performed by changing the transport speed of the preparation metal material when performing analysis with the X-ray fluorescence analyzer and repeatedly executing the first step of the first preparation step. Determining a plurality of the first determination criteria according to the transport speed of the metal material,
In the determination step, among the plurality of first determination criteria determined in the second preparation step, the first determination criteria corresponding to the transport speed of the determination target metal material when analyzed in the analysis step is selected, and the reference is made. If the Ladle analysis value of each element is less than a predetermined value and any of the analysis values of the content of each element after the correction obtained by the correction step does not satisfy the selected first determination criterion, The judged metal material is judged to be a different material from the above-mentioned planned product type,
The method for determining a foreign material of a metal material according to claim 2 or 3, characterized in that.

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