JPS62129748A - Measurement for plating attachment of metal material - Google Patents

Abstract

PURPOSE:To simply measure the attachment of plating film economically on line, by measuring a background intensity of X-ray diffraction of a metal material plated to determine the plating attachment using a calibration curve. CONSTITUTION:A steel plate 14 plated in a plating tank 10 is conveyed in the direction of the arrow A with a roll 12 and X rays emitted from an X-ray bulb 16 is incident into a steel plate 14 at the angle phi of incidence as parallel beam via an emanating solar slit 18. The background of X-ray diffraction generated from the steel plate 14 is detected with a detector 22 through a light receiving solar slit 20 at the position of angle (2theta) where the diffraction X rays does not appear. The detection signal is inputted into a pulse height analyzer 26 to extract a signal of X rays alone with a proper pulse height and the intensity of the background is measured with a calculating circuit 28. The measured value is inputted into a computer 30 to calculate attachment of plating film using a calibration curve. The measured value is shown on a display 32 while the plating condition of the plating tank 10 is controlled with a process computer 34.

Description

[Detailed description of the invention] [Industrial application field]

The present invention relates to a method for measuring the amount of plating on metal materials, and is particularly suitable for measuring the amount of plating film on various plated metal plates such as iron and aluminum. Concerning improvements in quantitative measurement methods.

[Conventional technology]

Various plated steel sheets with excellent corrosion resistance, workability, paintability, weldability, etc. have been developed and are widely used for automobile bodies, home appliances, building materials, canned food, etc. When producing these plated steel sheets, in order to stabilize their quality, the amount of plating film deposited must be analyzed and the process Pi! Management is essential. As a method for analyzing the deposition cfi of a plating film, there is a chemical analysis method in which only the plating film layer is dissolved and removed using electrolysis or an appropriate acid, and the plating adhesion m is determined from the removal m. It is very difficult to dissolve just the plating layer without melting the base metal 5), so it requires great skill and a long time.Moreover, it is a destructive analysis that involves taking samples from the product, and it cannot be done online. The problem was that the reflection of measurement results in process control was extremely slow. In order to solve these problems, in recent years, plated steel sheets have been irradiated with X-rays with a wide wavelength distribution to excite various elements, generating fluorescent X-rays from the elements present in the plating film. A fluorescent X-ray analysis method that measures the intensity of the generated fluorescent X-rays and analyzes the adhesion of the plating film from the predetermined detection ff1 line has been put into practical use, and its online equipment has become commercially available. It's coming.

[Problems to be solved by the invention]

However, the fluorescent X-ray analysis method is expensive because it is necessary to install a single crystal for spectroscopy, a detector, a counting circuit, etc. for each type of metal element to be plated. When analyzing an alloy-plated steel sheet containing the same metal, there was a problem in that the analysis was impossible because fluorescent X-rays from the base metal and fluorescent X-rays from within the coating could not be distinguished. In order to solve these problems, the applicant has already proposed 12 methods for measuring the adhesion amount and composition of the plating film on an alloy-plated steel sheet containing the same metal as the base metal 5 in Japanese Patent Application No. 59-209097. ing. In this method, an alloy coated steel sheet is irradiated with characteristic X-rays and white X-rays, and the composition of the alloy coating is measured from the diffraction angle of the X-rays diffracted by the alloy coating. Fluorescence X from metal
The amount of adhesion of the alloy layer II9 is determined by correcting the glandular strength with the composition of the alloy coating. However, with this measurement method, it is necessary to simultaneously measure the composition and coating of the plating film on the alloy-plated steel sheet, which contains the same metal as the base metal, and XtQ diffraction method and X-ray fluorescence analysis method are used together. In this respect, the apparatus is expensive, and therefore, there is no need to analyze the composition of the plating coverage, and it is uneconomical when only the amount of plating is desired to be measured.

[Purpose of the invention]

The present invention has been made to solve the above-mentioned conventional problems, and it is possible to easily and inexpensively measure the amount of plating film deposited on various plated metal materials, such as plated metal plates, online. The purpose of the present invention is to provide a method for measuring the amount of plating on metal materials.

[Means to solve the problem]

The present invention is a method for measuring the amount of plating on a metal material, the gist of which is shown in FIG. in,
The background intensity generated from the pre-deposited metal material is detected, and the relationship between the plating amount and the background intensity is revealed, and the plating line is calculated in advance. 5 material plating Dr'?:t■
The above objective has been achieved by finding the following. [Operation] When measuring a sample using the X-dust diffraction method, a diffraction line due to the crystals of the sample (Tomakadake) is measured, but a considerable amount of background is also visible.
This is caused by scattering of X P2 by the sample, etc., and requires correction when performing precise analysis, which interferes with the analysis, but the inventor stubbornly accepted the t! I have found that it provides extremely useful information when measuring the thickness of a plating wave membrane. In other words, the background intensity measured at the same corner position (2θ) using the same X-ray tube becomes foggy depending on the type of the base metal bottom and the plating film metal, and moreover, for example, the background intensity measured at the same corner position (2θ) is a haze due to only the base metal 2. Is the strength due to background only due to plating metal? If the degree is weaker than i'Q, as the penetration (the thickness and amount of plating film deposited within the penetration depth of F! I used Rubanild's clear plate 1.
1 constant′f! As in 5 Song, the measured background intensity increases. This figure shows the angle vj (2θ) as 9/
The relationship between the background intensity and the adhesion of the alloy plated wave film (7n-Fe alloy) in the case of Iζ is shown in the figure. It can be seen that a good θT suspension line is obtained even though the value varies from 8 to 14% (Zn: 92 to 86%).From this, it can be seen that the It can be seen that the plating adhesion ω can be analyzed with high accuracy even if the composition is varied within a practical range, whether it is alloy plating containing metal (Zn-Fe) or alloy plating?! On the other hand, in the 19th case, for example, the background ankylosis decreases, as in Nangxian, who measured a tin-plated fl'l plate using a Cr-Get X-ray tube as shown in Figure 3. This figure shows the background intensity and adhesion m of the tin (Sn) plating film when the definition (Qm(2θ)) is set to 90°.
8! 'Ill is shown. From FIG. 3, it can be seen that a very good calibration curve can be obtained, and this lj! f
f! By using a wire, it is possible to analyze the amount of tin plating deposited on the m-plate with high precision. Therefore, if a standard sample is created for each type of plated metal plate in advance and a calibration curve is created from the relationship between the amount of plating film attached and the background intensity, the background intensity can be measured. Adhesion of target metal material m
is required. Note that the background intensity measured in this case is not the background intensity at the diffraction angle (2θ) of the diffracted X-ray determined for background correction, as shown in FIG. Current state of X-rays 4
The background intensity may be measured anywhere as long as it is measured at an unobtrusive diffraction angle (2θ). Based on the above knowledge, the present invention has been made, and by applying characteristic X-rays to the gold tomoe material that is used as a pair, and based on the X-ray diffraction method, the angle at which the diffraction lines do not appear is determined. (2θ)
Then, the background intensity generated from the metal material hs I is detected, and using the predetermined coefficient [1] based on the relationship between the plating amount and the background intensity, the Next, the adhesion M is determined. Therefore, J of fluorescence XI/11 method:
However, since it is necessary to install a spectroscopic system (single crystal for spectroscopy, detector, counting circuit, etc.) for each element of the plated metal, it is possible to apply all types of plated metal coatings using inexpensive and standard equipment. Quantity can be measured. Also, an alloy that contains the same metal as the total bending of the base, which was previously very difficult to measure! It becomes possible to non-destructively and economically determine the amount of adhesion on the -2 side. Here, we considered online implementation of the method of the present invention.
Since it is flowing at a high speed of m 2 /min, the plated gold rF5+fi fluctuates more or less, and it is easy to catch the color tube in the concentrated method, so it is effective to use the parallel beam method. [Example] Hereinafter, an example of an apparatus for measuring plating adhesion m in which the method for measuring the amount of plating adhesion of metal materials according to the present invention is adopted will be described in detail. In this embodiment, plating (n1
The plated steel plate 14 is plated with 0 and fed 1η in the direction of the arrow Ab by the roll 12.
This is an on-line quick measurement device for measuring Metsusa (・!η) which adopts the present invention. For example, a Cr target 1-shade, an appropriate wavelength characteristic
An X-ray tube 16 that generates rays, and the X-ray tube 16 that generates the X-ray! ! (a diverging solar slit 18 that converts the X-rays emitted from the tube 16 into a parallel beam; and a light-receiving solar slit 2 that converts the background generated from the tube 14 into a parallel beam.
0, a background detector 22 for detecting the intensity of the background that has passed through the light-receiving solar slit 20, and a goniometer 24 for installing the light-receiving solar slit 20 and the background detector 22 at arbitrary angular positions; A pulse height selector 26 that extracts X-rays with an appropriate wave height (wavelength), a counting circuit 28 that measures the intensity of the X-rays extracted by the wave height (wavelength) type separator 26, and a computer that determines the amount of plating film deposited. 30 and a display 32 that displays the calculation results of the computer 30 in the form of a current line, etc., and outputs a signal to a processing computer 34 that controls the plating conditions, etc. of the plating (coupling 10). The operation of the embodiment will be explained below. .At that time, X
The X-rays emitted from the ray tube 16 are made into a parallel beam via the diverging solar slit 18, and the plating m
The beam is irradiated toward the tentative point 14 at an incident angle φ. Then, back brown diffraction lines are generated from the plated steel plate 14. The background intensity of the generated X-rays is controlled by a light-receiving solar slit 2 at an appropriate angle (2θ) where diffraction lines from the plating film and the base layer of the plated steel plate 14 do not appear.
0 through the background detector 22. The background intensity detected by the background detector 22 is determined by the wave height). Only the X-rays with an appropriate wave height (wavelength) are extracted by the separate device 2G, and the background intensity is measured by the counting circuit 28. The measurement of the background intensity (in) measured by the counting circuit 28 is manually inputted to the calculator 30, and the background intensity measured by the plated material 11 is calculated based on the measured line determined in advance for each type of plating scale.
9 (=I ff fi is performed. The result is displayed on the display 32 on the field line, and is also input to the process computer 34, and analyzed (lrr determines the plating line ('1) of plating ff1lo. etc. Here, if the light receiving solar slit 20 and the background detector 22 are installed on the goniometer 24,
Since the background intensity can be measured at any angle (2θ), it is possible to measure various types of plated steel sheets, which is very effective. If the measurement positions δ(20) can be selected, they may be fixed. Further, the wave height separator 26 may be used, for example, for input QJ 'I',
By extracting only the wavelength of the characteristic X-rays, the elements contained in the plating film and the base steel sheet caused by the white color generated simultaneously with the characteristic X-rays from the X-ray tube 16 are extracted. It is important to remove fluorescent XI. Furthermore, the opening angles of the solar slit 18 of the source 11 and the solar slit 2o of the light receiving device are determined according to the method for measuring the degree of alloying of galvanealed crystals (Japanese Unexamined Patent Publication No. 59-9-1989), which has already been filed by the applicant of the present application.
As shown in 13/13), 1 to 4 degrees is optimal, and in this way, there is a wide range in which the 1t color tube will not be affected by the fluttering of the plated steel plate 14 to be measured, so it is easy to go online. become. Furthermore, in the method for measuring the degree of alloying described above, the X-ray diffraction intensity and background intensity of the target crystal lattice plane are simultaneously measured to determine the degree of alloying after background correction, but the method of the present invention By using +Jl, it is possible to measure not only the degree of alloying but also the thickness and amount of plating film applied. It can be seen that 17 effective methods are provided. In addition, in the above-mentioned embodiment, a plated metal (a) was given as an example of a plated metal material, but the metal material is not limited to this, and metal materials such as iron, aluminum, etc. All metals (including metal materials) [Effects of the invention] As explained above, according to the present invention, the spectroscopic system (spectroscopic It is possible to measure the adhesion amount of all kinds of plated metal films using a safe and simple device, without the need to install any equipment (such as metal oxide crystals, detectors, counting circuits, etc.). It is now possible to measure the alloy film containing the same metal as the oligometal in a non-bursting, cost-effective manner.In addition, online measurement and analysis is now possible. 1. Since the floor information can be immediately fed back to the line, it greatly contributes to stable operation and quality improvement in production lines for all types of plated metals.

[Brief explanation of drawings]

FIG. 1 is a flowchart showing the gist of the present invention;
Figure 3 shows an example of the relationship between the amount of alloy (Zn-Fe) plating on a galvanized plate and the background strength for detailed explanation of the present invention. FIG. 11, a diagram showing an example of the relationship between the field plating amount and the background intensity, similarly shows the relationship between the diffraction angle (2
FIG. 5 is a diagram showing an example of the relationship between the X-ray intensity and showing the depiction,
FIG. 2 is a block diagram showing a partial layout. 10... Plating (a, 1/l... Plated steel (reverse), 16... X-ray tube, 18... Diverging solar slit, 20... Receiving solar slit, 22... Background Detector, 26... Wave height divider, 28... Counting circuit,
30... Computer, ψ... X-ray incident angle,
2θ...Background measurement angle.

Claims (1)

[Claims] (1) A coated metal material is irradiated with characteristic X-rays, and the background intensity generated from the metal material is detected at an angular position where no diffraction X-rays appear, and the relationship between the amount of plating and the background intensity is determined. A method for measuring the amount of plating on a metal material, characterized in that the amount of plating on the metal material is determined from the detected background intensity using a calibration curve determined in advance based on.