JP2006208013A - Measuring instrument of adhesion amount of surface-treated film on metal strip and measuring method - Google Patents

Measuring instrument of adhesion amount of surface-treated film on metal strip and measuring method Download PDF

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JP2006208013A
JP2006208013A JP2005016412A JP2005016412A JP2006208013A JP 2006208013 A JP2006208013 A JP 2006208013A JP 2005016412 A JP2005016412 A JP 2005016412A JP 2005016412 A JP2005016412 A JP 2005016412A JP 2006208013 A JP2006208013 A JP 2006208013A
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fluorescent
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metal band
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JP4736440B2 (en
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Nobutake Baba
伸壮 馬場
Takashi Ogawa
剛史 小川
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JFE Steel Corp
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Abstract

<P>PROBLEM TO BE SOLVED: To provide an adhesion amount measuring instrument capable of analyzing the adhesion amount of a light element contained in a surface-treated film on-line with respect to the surface-treated film containing the light element such as P or the like formed on the surface of a metal strip using a fluorescent X-ray analyzer, and a measuring method. <P>SOLUTION: The measuring instrument is constituted so as to measure the adhesion amount of the film on the running metal strip having the film formed on its surface and equipped with the fluorescent X-ray measuring head arranged in a close vicinity to the running metal strip and irradiating the surface of the metal strip with X rays to detect excited and radiated fluorescent X rays, a support device for supporting the fluorescent X-ray measuring head so as to reciprocate it in the width direction of the metal strip, the shape sensor arranged on the upstream side of the metal strip running direction of the fluorescent X-ray measuring head to detect the shape of the metal strip and a retraction device for retracting the fluorescent X-ray measuring head to the outside of the end part in the width direction of the metal strip or the direction separated from a plate surface when the shape of the metal strip measured by the shape sensor exceeds a threshold value. <P>COPYRIGHT: (C)2006,JPO&NCIPI

Description

本発明は、亜鉛系めっき鋼板などの金属帯に施される化成処理皮膜、有機無機複合皮膜などの表面処理皮膜付着量をオンラインで蛍光X線分析法により測定する装置及び方法に関する。より具体的には、表面処理皮膜中のCaより原子番号の小さな元素(以下、軽元素と記載する)をオンラインで蛍光X線分析法により測定する装置及び方法に関する。   The present invention relates to an apparatus and method for measuring the amount of a surface treatment coating such as a chemical conversion coating or an organic-inorganic composite coating applied to a metal strip such as a galvanized steel sheet online by fluorescent X-ray analysis. More specifically, the present invention relates to an apparatus and a method for measuring an element having an atomic number smaller than Ca (hereinafter referred to as a light element) in the surface treatment film online by fluorescent X-ray analysis.

亜鉛系めっき鋼板のクロメート処理は、亜鉛の白錆を抑制する安価な防錆処理方法として幅広く使用され、近年、さらに耐指紋性、溶接性等の特性を付与した高品質のクロメート処理も行われている。クロメート処理のクロム付着量は、めっき鋼板の耐食性、耐指紋性、溶接性等の特性に影響を与える。従って、製品の品質管理上、クロム付着量は、所要の特性を発現できるように所定の範囲内に管理される必要がある。   Chromate treatment of galvanized steel sheet is widely used as an inexpensive rust prevention treatment method that suppresses white rust of zinc, and in recent years, high-quality chromate treatment with additional characteristics such as fingerprint resistance and weldability has also been performed. ing. The chromium adhesion amount of the chromate treatment affects the properties such as corrosion resistance, fingerprint resistance and weldability of the plated steel sheet. Therefore, for the quality control of the product, the chromium adhesion amount needs to be managed within a predetermined range so that the required characteristics can be expressed.

従来、クロム付着量は、めっき鋼板から試料片を採取し、オフラインで蛍光X線分析装置を用いて皮膜中のCrの蛍光X線強度を測定したり試料片の皮膜を化学溶解してCrを化学分析したりして求められていた。しかし、この方法は、得られる付着量は鋼板全長のごく一部分を代表する値にすぎず、また、分析に長時間を要するため、操業中に、得られた測定結果をフィードバックすることができず、厳密な付着量制御ができないという問題があった。この問題を改善するため、近年、ライン内に蛍光X線分析装置を配置し、皮膜中のCr付着量はオンラインで直接求められるようになってきた(例えば、特許文献1等参照)。   Conventionally, the amount of chromium deposited is obtained by taking a sample piece from a plated steel plate and measuring the fluorescent X-ray intensity of Cr in the film using a fluorescent X-ray analyzer offline or by chemically dissolving the film on the sample piece. It was requested by chemical analysis. However, with this method, the amount of adhesion obtained is only a value that represents only a small part of the total length of the steel sheet, and the analysis takes a long time, so the obtained measurement results cannot be fed back during operation. There is a problem that the amount of adhesion cannot be strictly controlled. In order to improve this problem, in recent years, an X-ray fluorescence analyzer has been arranged in the line, and the amount of Cr deposited in the film has been directly obtained online (see, for example, Patent Document 1).

クロメート処理液は6価クロムが含まれるため、従来から環境対策として、クロメート処理時の完全クローズドシステムによる排水処理の採用や、水洗工程を必要としない塗布型クロメート処理技術の開発が行われている。また、クロメート皮膜が微量に含有する6価クロムについても、クロム溶出を防止した有機複合被覆鋼板の開発、塗布型クロメート皮膜の難溶化の検討などが行われてきた。   Since the chromate treatment solution contains hexavalent chromium, the use of wastewater treatment with a completely closed system during chromate treatment and the development of coating-type chromate treatment technology that does not require a water-washing process have been conducted as environmental measures. . In addition, regarding hexavalent chromium contained in a minute amount in the chromate film, development of an organic composite coated steel sheet that prevents elution of chromium, and examination of poor coating-type chromate film have been carried out.

一方、環境対策面から、6価クロムを使用しないクロムフリー化成処理鋼板の開発が行われ、例えば、特許文献2、特許文献3は、下層に、クロメート皮膜に代えて、酸化物を含有するリン酸及び/又はリン酸化合物皮膜を形成し、その上層に樹脂皮膜からなる有機複合被覆を形成させる有機複合被覆鋼板を提案している。   On the other hand, in view of environmental measures, a chromium-free chemical conversion treated steel sheet that does not use hexavalent chromium has been developed. For example, Patent Documents 2 and 3 describe phosphorous containing oxide in the lower layer instead of a chromate film. An organic composite coated steel sheet is proposed in which an acid and / or phosphoric acid compound film is formed, and an organic composite coating made of a resin film is formed on the upper layer.

特許文献2、特許文献3で提案する有機複合被覆鋼板の下層皮膜はリン酸及び/又はリン酸塩を含み、軽元素のP(リン)を皮膜の主要構成元素としている。この提案に係る有機複合被覆鋼板は、従来のクロメート処理鋼板に充分代替出来る特性を有している。皮膜成分分析を迅速に行うことのできる手法として蛍光X線分析法がある。しかし、Pのような軽元素の特性X線は大気中で減衰されるため、オンラインで蛍光X線分析することはこれまで行われていない。そのため、P付着量の分析はオフラインで行わざるを得ず、処理ラインでの分析用サンプル採取時期の制約及び分析結果が得られるまでに時間遅れがあり、厳密な付着量制御ができないという問題がある。
特開平5−264481号公報 特開2001−11645号公報 特開2001−11656号公報
The lower layer film of the organic composite-coated steel sheet proposed in Patent Documents 2 and 3 contains phosphoric acid and / or phosphate, and light element P (phosphorus) is used as the main constituent element of the film. The organic composite-coated steel sheet according to this proposal has characteristics that can be sufficiently substituted for conventional chromate-treated steel sheets. There is a fluorescent X-ray analysis method as a method capable of quickly performing a film component analysis. However, since characteristic X-rays of light elements such as P are attenuated in the atmosphere, fluorescent X-ray analysis has not been performed online. For this reason, analysis of the P adhesion amount is unavoidable, and there is a problem that there is a time delay until the analysis sample collection timing in the processing line and the analysis result are obtained, and strict adhesion amount control cannot be performed. is there.
Japanese Patent Laid-Open No. 5-264811 JP 2001-11645 A JP 2001-11656 A

本発明の課題は、亜鉛系めっき鋼板などの金属帯の表面に形成されるPなどの軽元素を含む表面処理皮膜について、該皮膜中に含まれる軽元素の付着量を、蛍光X線分析装置を用いてオンライン分析できる付着量測定装置および測定方法を提供することである。   An object of the present invention is to provide an X-ray fluorescence analyzer for the amount of light elements contained in a surface treatment film containing a light element such as P formed on the surface of a metal strip such as a zinc-based plated steel sheet. It is providing the adhesion amount measuring apparatus and measuring method which can be analyzed on-line using the.

上記課題を解決する本発明の手段は次の通りである。   Means of the present invention for solving the above problems are as follows.

第1発明は、その表面に皮膜が形成された走行中の金属帯の皮膜付着量測定装置であって、走行中の金属帯に近接して配置され、該金属帯表面にX線を照射し、励起・放射される蛍光X線を検出する蛍光X線測定ヘッドと、前記蛍光X線測定ヘッドを該金属帯幅方向に往復動可能に支持する支持装置と、前記蛍光X線測定ヘッドの該金属帯走行方向上流に配置され、該金属帯の形状を検出する形状センサと、前記形状センサで検出した金属帯の形状が閾値を超えたときに前記蛍光X線測定ヘッドを該金属帯幅方向端部外方または板面から離れる方向に退避させる退避装置と、を備えることを特徴とする付着量測定装置である。   A first invention is an apparatus for measuring a coating amount of a traveling metal strip having a film formed on the surface thereof, which is disposed in the vicinity of the traveling metal strip and irradiates the surface of the metal strip with X-rays. A fluorescent X-ray measuring head for detecting excited and emitted fluorescent X-rays, a support device for reciprocally supporting the fluorescent X-ray measuring head in the metal band width direction, and the fluorescent X-ray measuring head A shape sensor that is disposed upstream of the metal band traveling direction and detects the shape of the metal band, and when the shape of the metal band detected by the shape sensor exceeds a threshold value, the fluorescent X-ray measurement head is moved in the metal band width direction. And a retracting device that retracts in a direction away from the end or away from the plate surface.

第2発明は、第1発明において、前記形状センサは金属帯との接触を検知する接触検知センサであることを特徴する付着量測定装置である。   A second invention is the adhesion amount measuring apparatus according to the first invention, wherein the shape sensor is a contact detection sensor for detecting contact with a metal strip.

第3発明は、第1または第2発明において、前記接触検知センサの金属帯との接触検知部は、金属帯と所定間隔を設けて金属帯幅方向に張力を張って配置された線材で構成されていることを特徴する付着量測定装置である。   According to a third aspect of the present invention, in the first or second aspect of the present invention, the contact detection part of the contact detection sensor with the metal band is constituted by a wire disposed with a predetermined distance from the metal band and tensioned in the metal band width direction. It is the adhesion amount measuring device characterized by being made.

第4発明は、第1〜第3発明において、前記蛍光X線測定ヘッドは金属帯との間隔が10mm以下になるように配置することを特徴する付着量測定装置である。   A fourth invention is the adhesion amount measuring apparatus according to any one of the first to third inventions, wherein the fluorescent X-ray measurement head is arranged so that a distance from the metal band is 10 mm or less.

第5発明は、第1〜第4発明において、前記形状の閾値は、前記蛍光X線測定ヘッドと金属帯の間隔と同じ値であることを特徴とする付着量測定装置である。   A fifth invention is the adhesion amount measuring apparatus according to any one of the first to fourth inventions, wherein the threshold value of the shape is the same value as the distance between the fluorescent X-ray measurement head and the metal strip.

第6発明は、その表面に皮膜が形成された走行中の金属帯の皮膜付着量測定方法であって、走行中の金属帯に近接して、該金属帯表面にX線を照射し、励起・放射される蛍光X線を検出する蛍光X線測定ヘッドを配置して金属帯表面に形成された表面処理皮膜の元素の蛍光X線を測定するとともに、前記蛍光X線測定ヘッドの該金属帯走行方向上流に配置した形状センサで該金属帯の形状を検出し、検出した該金属帯の形状が閾値を超えたときは、前記蛍光X線測定ヘッドを該金属帯幅方向端部外方または板面から離れる方向に退避させることを特徴とする付着量測定方法である。   A sixth invention is a method for measuring the amount of coating on a traveling metal strip having a coating formed on the surface thereof, wherein the surface of the metallic strip is irradiated with X-rays in the vicinity of the traveling metal strip and excited. A fluorescent X-ray measurement head for detecting emitted fluorescent X-rays is arranged to measure the fluorescent X-rays of the elements of the surface treatment film formed on the surface of the metal band, and the metal band of the fluorescent X-ray measurement head When the shape of the metal band is detected by a shape sensor arranged upstream in the traveling direction, and the detected shape of the metal band exceeds a threshold value, the fluorescent X-ray measurement head is moved outside the end of the metal band width direction or It is an adhesion amount measuring method characterized by retracting in a direction away from the plate surface.

第7発明は、第6発明において、前記蛍光X線測定ヘッドは金属帯との間隔が10mm以下の間隔を設けて配置され、前記形状センサが走行中の金属帯に対して前記所定間隔以上の歪量を検出すると、前記蛍光X線測定ヘッドを該金属帯幅方向端部外方または板面から離れる方向に退避させることを特徴とする付着量測定方法である。   According to a seventh aspect, in the sixth aspect, the fluorescent X-ray measurement head is disposed at a distance of 10 mm or less from the metal band, and the shape sensor is at least the predetermined distance from the traveling metal band. When the amount of strain is detected, the X-ray fluorescence measurement head is retracted in a direction away from the end of the metal band width direction or away from the plate surface.

第8発明は、第6または第7発明において、前記測定元素は、Caより原子番号の小さな元素(Caを含む)であることを特徴とする付着量測定方法である。   An eighth invention is the adhesion amount measuring method according to the sixth or seventh invention, wherein the measurement element is an element (including Ca) having an atomic number smaller than Ca.

本発明によれば、P等の軽元素を含む表面処理皮膜の付着量をオンライン分析することが可能になり、得られた測定結果をフィードバックすることで、適切な付着量制御を迅速に行うことができるようになる。また金属帯全長のごく一部分でなく、長手方向の皮膜付着量ばらつき等を容易に把握することができるようになる。   According to the present invention, it becomes possible to perform on-line analysis of the adhesion amount of a surface treatment film containing a light element such as P, and appropriate adhesion amount control can be quickly performed by feeding back the obtained measurement results. Will be able to. In addition, it is possible to easily grasp not only a small part of the entire length of the metal strip but also the coating amount variation in the longitudinal direction.

蛍光X線分析装置を用いたオンライン分析は、亜鉛系めっき鋼板上に形成されたクロメート処理皮膜中のCr分析等において既に実用化されている。蛍光X線分析装置を用いた分析では、X線発生装置からX線をめっき鋼板表面に照射し、めっき表面から発生する蛍光X線を、分光結晶体を介してX線検出器で検出する。その際、空気によるX線の吸収を防ぐため、雰囲気を真空状態とする。オンライン分析では、鋼板と蛍光X線測定ヘッドの間隔は30mm程度とされる。このようなオンライン分析では、軽元素では発生した蛍光X線が大気中で減衰されるため、これまでPのような軽元素のオンライン分析は困難とされていた。   On-line analysis using a fluorescent X-ray analyzer has already been put into practical use in, for example, Cr analysis in a chromate-treated film formed on a zinc-based plated steel sheet. In the analysis using the fluorescent X-ray analyzer, the surface of the plated steel plate is irradiated with X-rays from the X-ray generator, and the fluorescent X-rays generated from the plated surface are detected by the X-ray detector through the spectral crystal. At that time, in order to prevent absorption of X-rays by air, the atmosphere is set in a vacuum state. In the on-line analysis, the distance between the steel plate and the fluorescent X-ray measurement head is about 30 mm. In such on-line analysis, since the fluorescent X-rays generated in light elements are attenuated in the atmosphere, it has been difficult to perform on-line analysis of light elements such as P so far.

本発明者らは、前述の特許文献2、特許文献3に記載される有機複合被覆鋼板のP(リン)を皮膜の主要構成元素とする皮膜について、蛍光X線分析装置を用いて、P付着量のオンライン分析の可否、分析精度等を調査した。その結果、蛍光X線分析装置として、蛍光X線測定ヘッド内に、めっき鋼板にX線を入射するX線発生装置および前記めっき鋼板側から出てくるL系列およびK系列の蛍光X線強度を測定する半導体検出器を有する光学系とを設けて、前記蛍光X線測定ヘッド内を含む光学系のX線入・出射光路の一部または全部をX線吸収の小さいガスで満たすとともに、さらに蛍光X線測定ヘッドはめっき鋼板との間隔が10mm以下の所定間隔を設けて近接配置することで、実操業において操業管理に使用するに十分な分析精度でP付着量のオンライン分析が可能になることを見出した。本発明はこの知見に基きなされたものである。   The present inventors use a fluorescent X-ray analyzer to attach P to a film having P (phosphorus) of the organic composite coated steel sheet described in Patent Document 2 and Patent Document 3 described above as a main constituent element of the film. We investigated the possibility of online analysis of quantity and the accuracy of analysis. As a result, as an X-ray fluorescence analyzer, an X-ray generator for injecting X-rays into the plated steel sheet and the L-series and K-series fluorescence X-ray intensities coming out from the plated steel sheet side in the fluorescent X-ray measuring head. An optical system having a semiconductor detector to be measured, and filling part or all of the X-ray incident / exit optical path of the optical system including the inside of the fluorescent X-ray measurement head with a gas having a small X-ray absorption, The fluorescent X-ray measurement head is placed close to the plated steel plate with a predetermined distance of 10 mm or less, so that on-line analysis of the P deposition amount can be performed with sufficient analysis accuracy to be used for operation management in actual operation. I found out. The present invention is based on this finding.

以下、本発明の実施の形態について詳しく説明する。なお、以下の本発明の実施の形態は、金属帯は亜鉛系めっき鋼板を念頭において説明する。   Hereinafter, embodiments of the present invention will be described in detail. In the following embodiments of the present invention, the metal strip will be described with a galvanized steel sheet in mind.

図1は本発明の実施の形態に係る付着量測定装置を備える鋼板の連続電気めっきラインの要部を示す概略側面図である。本実施の形態では、形状センサは接触式センサが設置され、形状測定ヘッドは鋼板幅方向端部外方に退避させる。   FIG. 1 is a schematic side view showing a main part of a continuous electroplating line for steel sheets provided with an adhesion amount measuring apparatus according to an embodiment of the present invention. In the present embodiment, a contact sensor is installed as the shape sensor, and the shape measuring head is retracted outward from the end portion in the steel plate width direction.

図1において、1は鋼板、2は巻き戻し装置、3は入側ルーパ、4は電気めっきセクション、5は塗装セクション、6は形状検出部(形状センサ)、7は付着量測定部、8は出側ルーパ、9は巻き取り装置である。   In FIG. 1, 1 is a steel plate, 2 is a rewinding device, 3 is an entry side looper, 4 is an electroplating section, 5 is a coating section, 6 is a shape detection unit (shape sensor), 7 is an adhesion amount measurement unit, and 8 is An exit side looper 9 is a winding device.

電気めっきセクション4は、アルカリ脱脂後酸洗処理を行う前処理部と電気亜鉛めっきを行うめっき部と後処理を行う後処理部を備える。塗装セクション5は、第1塗装部5aと第2塗装部5bを備える。第1塗装部5aは、鋼板1の表裏面の各々に塗布液を塗布する3ロールタイプのロールコータ21a、22a及び塗布した塗布液を加熱乾燥し、しかる後冷却するオーブン23aを備える。第2塗装部5bは、鋼板1の表裏面の各々に塗布液を塗布する2ロールタイプのロールコータ21b、22b及び塗布した塗布液を加熱乾燥し、しかる後冷却するオーブン23bを備える。   The electroplating section 4 includes a pretreatment portion that performs pickling after alkali degreasing, a plating portion that performs electrogalvanization, and a posttreatment portion that performs posttreatment. The painting section 5 includes a first painting part 5a and a second painting part 5b. The 1st coating part 5a is equipped with the oven 23a which heat-drys the apply | coating application liquid, and then cools it after 3 roll type roll coaters 21a and 22a which apply | coat an application liquid to each of the front and back of the steel plate 1. FIG. The second coating unit 5b includes two-roll type roll coaters 21b and 22b that apply the coating liquid to the front and back surfaces of the steel sheet 1, and an oven 23b that heats and drys the applied coating liquid and then cools it.

付着量測定部7は、鋼板通板方向に対して、第2塗装部5bの下流に配置され、形状検出部6は、第1塗装部5aと第2塗装部5bの間に配置されている。   The adhesion amount measuring unit 7 is disposed downstream of the second coating unit 5b with respect to the sheet passing direction, and the shape detection unit 6 is disposed between the first coating unit 5a and the second coating unit 5b. .

図2、図3は、付着量測定部7の要部を示す図で、図2は概略側面図、図3は図2のA−A矢視図である。   2 and 3 are diagrams showing a main part of the adhesion amount measuring unit 7, FIG. 2 is a schematic side view, and FIG. 3 is a view taken along arrow AA in FIG.

図2に示すように、デフレクターロール31、32間の鋼板1を挟む反対側に、サポートロール33a、33bが、鋼板1をパスラインより前方に押し込むように配置されている。サポートロール33a、33bの押し込み量は、当該ロールで鋼板のC反りを防止できる適宜の押し込み量とされる。蛍光X線測定ヘッド(以下、測定ヘッド)34a、34bは、各々サポートロール33a、33bに対して鋼板1を挟んだ反対側に該鋼板1に近接して所定間隔を開けて配置されている。めっき表面に形成された表面処理皮膜中の軽元素から放射される蛍光X線検出精度を確保する観点から、測定ヘッド34a、34bは鋼板との間隔が10mm以下の所定間隔を設けて近接配置される。前記所定間隔は7mm以下とすることがより好ましい。   As shown in FIG. 2, support rolls 33 a and 33 b are arranged on the opposite side of the steel plate 1 between the deflector rolls 31 and 32 so as to push the steel plate 1 forward from the pass line. The pressing amount of the support rolls 33a and 33b is set to an appropriate pressing amount that can prevent C warpage of the steel sheet with the roll. Fluorescent X-ray measurement heads (hereinafter referred to as measurement heads) 34a and 34b are arranged on the opposite side of the support rolls 33a and 33b with the steel plate 1 sandwiched between them and at a predetermined interval. From the viewpoint of ensuring the detection accuracy of fluorescent X-rays radiated from light elements in the surface treatment film formed on the plating surface, the measurement heads 34a and 34b are arranged close to each other with a predetermined interval of 10 mm or less from the steel plate. The The predetermined interval is more preferably 7 mm or less.

測定ヘッド34aは、その下部に駆動装置35aを有する台車36aが設置され、駆動装置35aを駆動させることで、鋼板幅方向に設置されたレール37a上を移動自在である。同様に測定ヘッド34bは、その下部に駆動装置35bを有する台車36bが設置され、駆動装置35bを駆動させることで、鋼板幅方向に設置されたレール37b上を移動自在である。38a、38bはガス供給管及び制御配線用のコンベアであり、その内部にX線発生器への信号、X線検出器からの信号を送信・受信するための配線、駆動機構35a、35bを駆動させるための配線等が配置されている。図3中、二点差線で示される34a′、34a″及び34b′、34b″は各々測定ヘッド34a、34bの前進限の位置、後退限の位置を示している。   The measurement head 34a is provided with a carriage 36a having a driving device 35a in the lower portion thereof, and is movable on a rail 37a installed in the steel plate width direction by driving the driving device 35a. Similarly, the measurement head 34b is provided with a carriage 36b having a driving device 35b in the lower portion thereof, and is movable on a rail 37b installed in the steel plate width direction by driving the driving device 35b. Reference numerals 38a and 38b denote gas supply pipes and control wiring conveyors, which drive signals to the X-ray generator and wiring for transmitting / receiving signals from the X-ray detector, and drive mechanisms 35a and 35b. Wiring and the like are arranged for this purpose. In FIG. 3, 34 a ′, 34 a ″ and 34 b ′, 34 b ″ indicated by a two-dot difference line indicate the forward limit position and the backward limit position of the measurement heads 34 a, 34 b, respectively.

図4は、前記付着量検出部7の要部を説明する概略図である。蛍光X線測定ヘッド11はめっき鋼板1と所要間隔を設けて配置され、該測定ヘッド11には、ガス供給装置17から当該ヘッド11内にヘリウムガスを供給する配管が接続されている。ヘリウムガスは、L系列蛍光X線に対して吸収が小さく、光路中のX線の減衰が小さい。なお、光路中のX線の減衰が小さいものであれば、他のガスであってもよく、例えば窒素ガスであってもよい。   FIG. 4 is a schematic diagram for explaining a main part of the adhesion amount detection unit 7. The fluorescent X-ray measurement head 11 is arranged at a required distance from the plated steel plate 1, and a pipe for supplying helium gas from the gas supply device 17 into the head 11 is connected to the measurement head 11. Helium gas has little absorption with respect to L-series fluorescent X-rays, and X-ray attenuation in the optical path is small. In addition, as long as attenuation | damping of the X-ray in an optical path is small, other gas may be sufficient, for example, nitrogen gas may be sufficient.

この蛍光X線測定ヘッド11は、箱状に形成され、X線の入射光路およびめっき鋼板1側からの蛍光X線出射光路となる部分に開口部が形成されている。   The fluorescent X-ray measurement head 11 is formed in a box shape, and an opening is formed in a portion that becomes an X-ray incident optical path and a fluorescent X-ray emission optical path from the plated steel sheet 1 side.

前記蛍光X線測定ヘッド11内には光学系12が配置されている。該光学系12は、X線発生器13および半導体検出器14を有し、さらにX線発生器13から発生するX線の入射光路およびこのX線の入射によってめっき鋼板側から出てくるX線の出射光路の一部または全部をヘリウムガスで満たすようなガス通路15および16が設けられ、めっき皮膜2からのL系列蛍光X線およびK系列蛍光X線を半導体検出器14で測定する。   An optical system 12 is disposed in the fluorescent X-ray measurement head 11. The optical system 12 includes an X-ray generator 13 and a semiconductor detector 14, and an X-ray incident optical path generated from the X-ray generator 13 and an X-ray emitted from the plated steel plate side by the incidence of the X-ray. Gas passages 15 and 16 are provided so that a part or all of the emission optical path of the gas is filled with helium gas, and L-series fluorescent X-rays and K-series fluorescent X-rays from the plating film 2 are measured by the semiconductor detector 14.

半導体検出器14により測定されたL系列蛍光X線強度およびK系列蛍光X線強度はそれぞれ付着量処理演算部53に送出される。   The L-series fluorescence X-ray intensity and the K-series fluorescence X-ray intensity measured by the semiconductor detector 14 are sent to the adhesion amount processing calculation unit 53, respectively.

この付着量処理演算部53は、L系列蛍光X線強度およびK系列蛍光X線強度を取り込み、検量線法に基づいて皮膜付着量を求める。ここで、検量線法とは、予め測定条件とされる所定の入射角でX線を入射し、このX線入射によって得られる同じく測定条件とされる所定の測定角で測定される分析目的元素のL系列の蛍光X線強度の検量線を、既知のめっき鋼板における皮膜付着量をパラメータとして求めて記憶しておく。K系列の蛍光X線強度の検量線についても、同様に測定条件の下に皮膜付着量をパラメータとして求めて記憶しておく。   The adhesion amount processing calculation unit 53 takes in the L-series fluorescence X-ray intensity and the K-series fluorescence X-ray intensity, and obtains the film adhesion amount based on the calibration curve method. Here, the calibration curve method means that an X-ray is incident at a predetermined incident angle that is set in advance as a measurement condition, and an analysis target element that is obtained by this X-ray incidence and is measured at a predetermined measurement angle that is also set as the measurement condition. A calibration curve for the fluorescent X-ray intensity of the L series is obtained and stored with the coating amount on a known plated steel sheet as a parameter. Similarly, a calibration curve of K-series fluorescence X-ray intensity is obtained and stored as a parameter of the coating amount under the measurement conditions.

この状態において半導体検出器14からのL系列蛍光X線強度およびK系列蛍光X線強度を取り込み、取り込んだX線強度と前記検量線に基き、被測定対象の皮膜中の軽元素の付着量を求める。   In this state, the L-series fluorescence X-ray intensity and the K-series fluorescence X-ray intensity from the semiconductor detector 14 are taken in, and the amount of light elements attached to the film to be measured is determined based on the taken-in X-ray intensity and the calibration curve. Ask.

図5は、図4の分析装置を用いて、めっき表面にリン酸含有皮膜を有する亜鉛めっき鋼板について、該分析装置がオンラインで使用されるのと同じ条件で、実施例1で皮膜形成するリン酸含有皮膜のP付着量とPの蛍光X線強度(L系列)の関係を調査した結果を示す。蛍光X線測定ヘッドとめっき鋼板の間隔は5mmである。P付着量とP強度との間によい相関関係が認められる。P付着量をx(mn/m2)、半導体検出装置で検出するPの蛍光X線強度をy(kcps)とすると、両者の関係式は、y=0.009x+0.2785で表される。この関係を用いて、オンラインでP強度を測定してP付着量を求めることができる。 FIG. 5 is a graph showing the phosphorous formed in Example 1 on the same condition as the analyzer is used on-line for a galvanized steel sheet having a phosphoric acid-containing film on the plating surface. The result of investigating the relationship between the P adhesion amount of the acid-containing film and the fluorescent X-ray intensity (L series) of P is shown. The interval between the fluorescent X-ray measurement head and the plated steel sheet is 5 mm. A good correlation is observed between the P adhesion amount and the P intensity. Assuming that the P adhesion amount is x (mn / m 2 ) and the fluorescent X-ray intensity of P detected by the semiconductor detection device is y (kcps), the relational expression between them is expressed as y = 0.000x + 0.2785. Using this relationship, the P adhesion amount can be obtained by measuring the P intensity online.

図6は、図4の分析装置を用いて、前記と同様にして、めっき表面にSi含有皮膜を形成した亜鉛めっき鋼板について、Si付着量とSiの蛍光X線強度(L系列)の関係を調査した結果を示す。Si付着量とSi強度の間にもよい相関関係が認められる。Si付着量x(mg/m2)、半導体検出装置で検出するSiの蛍光X線強度をy(kcps)とすると、両者の関係式は、y=0.2607x+0.0212で表される。この関係を用いて、オンラインでSi強度を測定してSi付着量を求めることができる。 FIG. 6 shows the relationship between the Si adhesion amount and the X-ray fluorescence intensity (L series) of Si in a galvanized steel sheet having a Si-containing coating formed on the plating surface in the same manner as described above, using the analyzer of FIG. The survey results are shown. A good correlation is also observed between the Si adhesion amount and the Si strength. Assuming that the Si adhesion amount x (mg / m 2 ) and the fluorescence X-ray intensity of Si detected by the semiconductor detection device are y (kcps), the relational expression between them is expressed as y = 0.2607x + 0.0212. Using this relationship, the Si adhesion amount can be obtained by measuring the Si intensity online.

皮膜が複層構造皮膜で、その1の層の付着量分析を行うときは、複層構造皮膜の鋼板において、その1の層について分析対象元素について前記のような関係を求めればよい。   When the film is a multi-layer structure film and the amount of adhesion of the first layer is analyzed, the relationship as described above may be obtained for the element to be analyzed for the one layer in the steel sheet of the multi-layer structure film.

本発明では、測定ヘッド11を鋼板1との間隔が10mm以下、より好ましくは7mm以下となる所定間隔を設けて近接配置する。走行中の鋼板形状は常時安定して平坦とは云えず、局部的に、中伸び、耳波等の鋼板形状の値が前記所定間隔以上となる場合がある。このような形状の劣る鋼板が付着量検出部7を通過すると、測定ヘッド11と接触して損傷させる恐れがある。従って、鋼板形状が劣る部分があるときは、該部分が付着量検出部を通過する前に測定ヘッド11を鋼板通板部分の外に確実に退避させて装置の損傷を防止することが不可欠である。本発明では、係る観点から、付着量検出部7の上流に鋼板形状を検出する形状センサと、測定ヘッド11を鋼板通板部分の外側に退避させる退避手段を備える。形状センサは鋼板形状が予め定めた閾値以上であることを検知すると、退避手段で測定ヘッド11を鋼板通板部分の外側に退避させる。このような装置を備えることで、初めて軽元素のオンライン分析を安定して行うことができる。   In the present invention, the measuring head 11 is arranged close to the steel plate 1 with a predetermined interval of 10 mm or less, more preferably 7 mm or less. The steel plate shape during traveling cannot always be said to be stable and flat, and locally, the values of the steel plate shape such as medium elongation and ear waves may be equal to or greater than the predetermined interval. When such a steel plate having an inferior shape passes through the adhesion amount detection unit 7, there is a risk of contact with the measuring head 11 and damage. Therefore, when there is a portion with a poor steel plate shape, it is indispensable to prevent the apparatus from being damaged by reliably retracting the measuring head 11 outside the steel plate passage portion before the portion passes through the adhesion amount detection unit. is there. In the present invention, from such a viewpoint, a shape sensor that detects the shape of the steel sheet is provided upstream of the adhesion amount detection unit 7 and a retracting means that retracts the measuring head 11 to the outside of the steel plate passage portion. When the shape sensor detects that the steel plate shape is equal to or greater than a predetermined threshold, the retraction means retracts the measuring head 11 to the outside of the steel plate passage portion. By providing such an apparatus, online analysis of light elements can be stably performed for the first time.

鋼板形状を検出する形状センサは、センサと鋼板とを非接触で鋼板形状を検知する非接触式形状センサ、センサと鋼板を接触させて鋼板形状を検知する接触式形状センサを採用することができる。形状センサは鋼板幅方向の形状の最大値(最大歪)を検出できるものが好ましい。   As the shape sensor for detecting the steel plate shape, a non-contact type sensor for detecting the steel plate shape without contact between the sensor and the steel plate, or a contact type sensor for detecting the steel plate shape by bringing the sensor into contact with the steel plate can be adopted. . The shape sensor is preferably one that can detect the maximum value (maximum strain) of the shape in the width direction of the steel sheet.

本実施の形態では、図1には、鋼板幅方向の歪の最大値を検知できる非接触式形状センサが設置されている。図7は、形状検出部(接触式形状センサ)6の要部を示す概略図である。形状センサは、めっき鋼板1がデフレクターロール41に巻きかけられている位置で、該デフレクターロール41の軸方向に延在し、鋼板面と平行で、該鋼板面と所定間隔をあけて、めっき鋼板の一方の端部外側から他方の端部外側に張られて配置されたワイヤ43と、該ワイヤ43に通電する電源装置44と、該ワイヤ43に流れる電流を計測する電流計45とを備える。ワイヤ43とめっき鋼板1の間隔は、測定ヘッド34a、34bとめっき鋼板1の間隔と同じ間隔にされている。ワイヤ43とめっき鋼板1が接触すると、電流計45で検出する電流値が変化する。電流の変化量がある閾値以上になると鋼板形状不良と判断する。   In the present embodiment, a non-contact shape sensor capable of detecting the maximum value of strain in the steel plate width direction is installed in FIG. FIG. 7 is a schematic view showing a main part of the shape detection unit (contact type shape sensor) 6. The shape sensor is a position where the plated steel sheet 1 is wound around the deflector roll 41, extends in the axial direction of the deflector roll 41, is parallel to the steel sheet surface, and is spaced apart from the steel sheet surface by a predetermined distance. A wire 43 extending from the outer side of one end to the outer side of the other end, a power supply device 44 for energizing the wire 43, and an ammeter 45 for measuring the current flowing through the wire 43. The distance between the wire 43 and the plated steel sheet 1 is the same as the distance between the measurement heads 34 a and 34 b and the plated steel sheet 1. When the wire 43 and the plated steel plate 1 come into contact with each other, the current value detected by the ammeter 45 changes. If the amount of change in current is greater than or equal to a certain threshold value, it is determined that the shape of the steel sheet is defective.

図8は、本発明の実施の形態に係る付着量測定装置の制御系統を説明するフロー図である。図8中、51は形状演算部、52は駆動装置制御部、53は付着量処理演算部、54は集中制御盤、55は警報装置である。   FIG. 8 is a flowchart for explaining a control system of the adhesion amount measuring apparatus according to the embodiment of the present invention. In FIG. 8, 51 is a shape calculation unit, 52 is a drive device control unit, 53 is an adhesion amount processing calculation unit, 54 is a centralized control panel, and 55 is an alarm device.

付着量処理演算部53には、第1塗装部で塗布形成する表面処理皮膜について、予め調査して求めた測定対象の軽元素の蛍光X線強度と皮膜付着量との関係、例えば、測定対象の軽元素がPである場合、図5に示すごときPの強度と付着量の関係が入力されて記憶されている。また、必要に応じて付着量の上限又は下限の閾値が設定されている。測定ヘッド34a、34bでは、X線発生器13からX線をめっき鋼板に照射し、発生した蛍光X線強度を半導体検出器14で検出する。検出したX線強度を付着量処理演算部53に送る。   In the adhesion amount processing calculation unit 53, the relationship between the fluorescent X-ray intensity of the light element to be measured and the amount of film adhesion, which has been obtained by examining the surface treatment film applied and formed in the first coating part, for example, the measurement object When the light element is P, the relationship between the strength of P and the adhesion amount as shown in FIG. 5 is inputted and stored. Further, an upper limit or a lower limit threshold of the adhesion amount is set as necessary. In the measurement heads 34 a and 34 b, the plated steel plate is irradiated with X-rays from the X-ray generator 13, and the generated fluorescent X-ray intensity is detected by the semiconductor detector 14. The detected X-ray intensity is sent to the adhesion amount processing calculation unit 53.

測定ヘッド34a、34bは鋼板幅方向に走行自在である。通常、測定ヘッド34a、34bを鋼板幅方向の全幅に渡り一定速度で横行を繰り返し、鋼板幅方向の付着量を測定する方法、測定ヘッド34a、34bを横行させて鋼板幅方向の3箇所(中央部及び各々の端部近傍部分)で所定時間停止して当該3箇所の付着量を測定する方法、測定ヘッド34a、34bを鋼板幅方向中央に配置して当該位置の付着量を測定する方法のいずれかの測定を行う。   The measuring heads 34a and 34b can run in the width direction of the steel plate. Usually, the measuring heads 34a and 34b are repeatedly traversed at a constant speed over the entire width in the steel sheet width direction, and the amount of adhesion in the steel sheet width direction is measured. The measuring heads 34a and 34b are traversed in three positions in the steel sheet width direction (center And a method of measuring the amount of adhesion at the position by placing the measuring heads 34a and 34b at the center in the width direction of the steel sheet. Take one of the measurements.

付着量処理演算部53は、測定ヘッド34a、34bから送られてきたX線強度信号を処理し、記憶されているX線強度と付着量との関係に基き、皮膜付着量を演算して求める。求めた付着量は、集中制御盤54に出力して表示する。また、求めた付着量が上限閾値又は下限閾値を外れた場合は警報装置55に信号を送り、付着量が閾値範囲を外れたことを音声及び/又は表示灯で操作員に知らしめる。   The adhesion amount processing calculation unit 53 processes the X-ray intensity signal sent from the measurement heads 34a and 34b, and calculates and obtains the film adhesion amount based on the relationship between the stored X-ray intensity and the adhesion amount. . The obtained adhesion amount is output to the centralized control panel 54 and displayed. Further, when the determined adhesion amount is out of the upper threshold value or the lower threshold value, a signal is sent to the alarm device 55 to notify the operator by voice and / or an indicator lamp that the adhesion amount is out of the threshold range.

形状センサ6の電流計45で計測した電流値は形状演算部51に送られる。形状演算部51は、電流値が予め定めた閾値以上であるか否かを判定し、電流値が閾値を下回るとワイヤ43と鋼板1が接触したと判定し、判定結果を駆動装置制御部52に出力する。駆動装置制御部52は駆動装置35a、35bを駆動させて測定ヘッド34a、34bを鋼板端部外方の後退限34a″、34b″まで移動させる。測定ヘッド34a、34bを退避させる鋼板形状の閾値は、鋼板と測定ヘッドの間隔と同じ値に設定する。また、警報装置55に信号を送り、測定ヘッド34a、34bの退避限への退避を音声及び/又は表示灯で操作員に知らしめる。形状センサと鋼板が接触していないことを確認したら捜査員が付着量測定を再開する。   The current value measured by the ammeter 45 of the shape sensor 6 is sent to the shape calculation unit 51. The shape calculation unit 51 determines whether or not the current value is equal to or greater than a predetermined threshold value. When the current value falls below the threshold value, the shape calculation unit 51 determines that the wire 43 and the steel plate 1 are in contact with each other, and the determination result is determined by the drive device control unit 52. Output to. The driving device controller 52 drives the driving devices 35a and 35b to move the measuring heads 34a and 34b to the retreating limits 34a "and 34b" outside the steel plate ends. The steel plate shape threshold for retracting the measuring heads 34a, 34b is set to the same value as the distance between the steel plate and the measuring head. Further, a signal is sent to the alarm device 55 to notify the operator of the retracting of the measuring heads 34a, 34b to the retracting limit by voice and / or an indicator lamp. When it is confirmed that the shape sensor and the steel plate are not in contact, the investigator restarts the adhesion amount measurement.

なお、形状センサ6と付着量測定部7の鋼板通板方向の間隔は、駆動装置35a、35bが測定ヘッド34a、34bを各々の退避限34a″、34b″まで移動させるのに要する応答時間と、鋼板走行速度とを考慮して、形状センサ6で検知した形状不良部位が付着量測定部7に到達する前に、測定ヘッド34a、34bが退避限34a″、34b″に移動可能な適宜間隔に設定される。鋼板走行速度はめっきセクションの処理能力、塗装セクションの処理能力に対応して変化するので、形状不良部位の走行位置のトラッキングを行い、そのトラッキング情報に基づき測定ヘッド34a、34bを退避させるタイミングを決定することが有利である。上記条件が満たされ、また、形状検出部6通過後に鋼板形状不良を発生させることがなれば、形状検出部6の配置場所は特に限定されない。前述の実施の形態では、形状センサ6は第2塗装部の上流に設けたが、第2塗装部の下流に設けてもよい。   The distance between the shape sensor 6 and the adhesion amount measuring unit 7 in the sheet passing direction is the response time required for the driving devices 35a, 35b to move the measuring heads 34a, 34b to the respective retraction limits 34a ", 34b". In consideration of the traveling speed of the steel plate, the measurement heads 34a, 34b can be moved to the retraction limits 34a ", 34b" before the defective shape portion detected by the shape sensor 6 reaches the adhesion amount measuring unit 7. Set to Since the steel plate traveling speed changes corresponding to the processing capability of the plating section and the processing capability of the coating section, tracking of the traveling position of the defective shape portion is performed, and the timing for retracting the measuring heads 34a and 34b is determined based on the tracking information. It is advantageous to do so. If the above conditions are satisfied and a steel plate shape defect is generated after passing through the shape detection unit 6, the arrangement location of the shape detection unit 6 is not particularly limited. In the above-described embodiment, the shape sensor 6 is provided upstream of the second coating portion, but may be provided downstream of the second coating portion.

以上説明した発明の実施の形態では、形状センサは接触式センサであったが、形状センサは非接触式センサであってもよい。非接触式形状センサとしては、鋼板がデフレクターロールに巻きかけられている位置で、鋼板の一方の端部外側に、鋼板に近接させて鋼板面に平行に鋼板の他方の端部側に向かってレーザ光を照射する投光器と、鋼板の他方の端部外側にレーザ光を受光するCCDカメラを用いた受光器とを配置し、受光器で受光する受光量に基き、鋼板形状(基準パスラインからの鋼板の変位量)を計測することができる。   In the embodiment of the invention described above, the shape sensor is a contact sensor, but the shape sensor may be a non-contact sensor. As a non-contact type sensor, at the position where the steel plate is wound around the deflector roll, toward the other end side of the steel plate in parallel with the steel plate surface, close to the steel plate, outside one end portion of the steel plate A projector that irradiates laser light and a light receiver using a CCD camera that receives the laser light are arranged outside the other end of the steel plate. Based on the amount of light received by the light receiver, the shape of the steel plate (from the reference pass line) The amount of displacement of the steel plate) can be measured.

また、測定ヘッドは鋼板幅方向端部の外側に退避させたが、測定ヘッドを、鋼板面と直角方向、または鋼板面に対して鋼板走行方向の斜め上方、または斜め下方に、板面から離れる方向に移動させる退避方式であってもよい。   In addition, the measuring head was retracted to the outside of the end in the width direction of the steel plate, but the measuring head was separated from the plate surface in a direction perpendicular to the steel plate surface, or diagonally above or diagonally below the steel plate running direction with respect to the steel plate surface. A retraction method of moving in the direction may be used.

図9は、測定ヘッド11を、鋼板面に対して直角方向に退避させる装置の構成例である。台車36上に、測定ヘッド11を鋼板面と直角方向にスライド可能に保持する摺動部材61と、測定ヘッド11を鋼板面と直角方向に前進または後退させるモータとギア機構を内蔵する駆動装置62が配置されている。測定ヘッド11の前進位置は、皮膜分析を行うための所定位置である。測定ヘッド11の後退位置は、鋼板の形状不良の際に測定ヘッド11と鋼板との接触を回避できる適宜の位置である。皮膜付着量分析の際は、測定ヘッド11は前進位置に配置され、形状センサ6が鋼板の形状不良を検知すると、駆動装置制御部からの指令に基き、駆動装置62を駆動して、測定ヘッド11に連結されている軸63を後退させ、測定ヘッド11を後退位置に移動する。本装置では、測定ヘッド11を退避させる時間、または退避させ測定ヘッド11を測定位置に復帰させるための時間を短縮でき、したがって、皮膜付着量分析を行えない鋼板長を短くできる利点がある。必要に応じて、測定ヘッドを該めっき鋼板幅方向端部外方に対比させる方式と板面から離れる方向に退避させる方式を併用してよい。   FIG. 9 is a configuration example of an apparatus for retracting the measuring head 11 in a direction perpendicular to the steel plate surface. On the carriage 36, a sliding member 61 that holds the measuring head 11 so as to be slidable in a direction perpendicular to the steel plate surface, a driving device 62 that incorporates a motor and a gear mechanism for moving the measuring head 11 forward or backward in a direction perpendicular to the steel plate surface. Is arranged. The advance position of the measuring head 11 is a predetermined position for performing film analysis. The retracted position of the measuring head 11 is an appropriate position at which contact between the measuring head 11 and the steel plate can be avoided when the shape of the steel plate is poor. At the time of film adhesion amount analysis, the measuring head 11 is disposed at the forward position, and when the shape sensor 6 detects a shape failure of the steel sheet, the driving device 62 is driven based on a command from the driving device control unit to measure the measuring head. 11, the shaft 63 connected to 11 is retracted, and the measuring head 11 is moved to the retracted position. In this apparatus, the time for retracting the measuring head 11 or the time for retracting and returning the measuring head 11 to the measurement position can be shortened, and therefore, there is an advantage that the length of the steel plate that cannot perform the coating amount analysis can be shortened. If necessary, a method of comparing the measuring head to the outside of the end portion in the width direction of the plated steel plate and a method of retracting in the direction away from the plate surface may be used in combination.

本発明によれば、P、Siなどの軽元素を含む皮膜の付着量を、蛍光X線分析装置を用いてオンライン分析が可能になる。鋼板を走行させながら付着量測定を迅速に行うことができ、測定結果を塗装工程にフィードバックすることで、従来に比べて厳密かつ迅速な付着量制御が可能になる。   According to the present invention, it is possible to perform on-line analysis of the amount of coating containing a light element such as P and Si using a fluorescent X-ray analyzer. The amount of adhesion can be measured quickly while the steel plate is running, and the amount of adhesion can be controlled more strictly and quickly than in the past by feeding back the measurement result to the painting process.

塗装速度を高めると付着量ばらつきが大きくなる傾向がある。そのため、これまで、付着量範囲外れの発生を防止する観点から塗装速度は低めに設定して操業していたが、本発明によれば、厳密な付着量制御が可能になるので、塗装速度を高めることが可能になり、生産性の向上にも寄与する。   Increasing the coating speed tends to increase the amount of adhesion. Therefore, until now, from the viewpoint of preventing the occurrence of out of the adhesion amount range, the coating speed has been set to be low, but according to the present invention, it is possible to strictly control the adhesion amount. It can be increased and contributes to the improvement of productivity.

本発明の実施例について説明する。図1の電気亜鉛めっきラインで、厚さ0.4〜2.3mm×幅910〜1880mmの範囲内にある鋼板に電気亜鉛めっきを施し、次いで第1塗装部で、第一リン酸:0.01mol/l、コロイダルシリカ:0.01mol/l、及びMg:0.01mol/lを含有する、pH3の処理液を塗布し、しかる後に焼き付け処理を行い、P付着量の目標範囲が45〜65mg/m2であるリン酸含有皮膜を有する表面処理鋼板を製造し、オフラインの蛍光X線分析装置で形成された皮膜のP付着量を測定した。 Examples of the present invention will be described. In the electrogalvanizing line of FIG. 1, electrogalvanizing was performed on a steel sheet having a thickness of 0.4 to 2.3 mm × width of 910 to 1880 mm, and then, in the first coating portion, the first phosphoric acid: 0.0. A treatment liquid of pH 3 containing 01 mol / l, colloidal silica: 0.01 mol / l, and Mg: 0.01 mol / l was applied, followed by baking treatment, and the target range of P adhesion amount was 45 to 65 mg. A surface-treated steel sheet having a phosphoric acid-containing film of / m 2 was produced, and the P adhesion amount of the film formed by an off-line fluorescent X-ray analyzer was measured.

本発明法では、オンライン分析装置の測定ヘッド11、形状センサ6のワイヤ43は、各々最大装入厚さの鋼板(板厚2.3mm)に対する間隔が5mmとなる位置に配置し、ライン内に配置された分析装置で検出されるP付着量に基き、該P付着量が45〜65mg/m2の範囲内となるように各ロールの回転数、塗液濃度等の塗布条件を調整した。Pの蛍光X線強度とP付着量の関係は、図1に示した関係を用いた。 In the method of the present invention, the measuring head 11 of the on-line analyzer and the wire 43 of the shape sensor 6 are arranged at positions where the distance to the steel sheet having a maximum charging thickness (plate thickness 2.3 mm) is 5 mm, and within the line. Based on the P adhesion amount detected by the arranged analyzer, the application conditions such as the rotation speed of each roll and the coating liquid concentration were adjusted so that the P adhesion amount was in the range of 45 to 65 mg / m 2 . The relationship shown in FIG. 1 was used for the relationship between the fluorescent X-ray intensity of P and the adhesion amount of P.

オフラインの蛍光X線分析装置でのP付着量の測定結果に基きP付着量を調整した従来法ではP付着量の目標範囲外れの発生割合は0.5%であったが、本発明法ではP付着量の目標範囲外れは発生しなかった。また、本発明法では、鋼板の形状不良部分があっても、形状センサ6が鋼板の形状不良を検知し、測定ヘッド11を鋼板端部の外側に退避させたので測定ヘッド11損傷のトラブルは発生しなかった。   In the conventional method in which the P deposition amount is adjusted based on the measurement result of the P deposition amount with an offline X-ray fluorescence spectrometer, the occurrence rate of the P deposition amount outside the target range was 0.5%. The P adhesion amount did not deviate from the target range. Further, in the method of the present invention, even if there is a defective shape portion of the steel plate, the shape sensor 6 detects the defective shape of the steel plate and retracts the measuring head 11 to the outside of the end portion of the steel plate. Did not occur.

本発明は、P、Siなどの軽元素を含む皮膜の付着量を、蛍光X線分析装置を用いてオンライン分析するための装置、オンライン分析する方法として利用することができる。   INDUSTRIAL APPLICABILITY The present invention can be used as an apparatus for online analysis of a coating amount containing a light element such as P and Si, and a method for online analysis using a fluorescent X-ray analyzer.

本発明の実施の形態に係る付着量測定装置を備える鋼板の連続電気めっきラインの要部を示す概略側面図である。It is a schematic side view which shows the principal part of the continuous electroplating line of the steel plate provided with the adhesion amount measuring apparatus which concerns on embodiment of this invention. 付着量測定部の要部を概略側面図である。It is a schematic side view of the principal part of an adhesion amount measurement part. 図2のA−A矢視図である。It is an AA arrow line view of FIG. 本発明の実施の形態に係る付着量測定装置の付着量検出部7の要部を説明する概略図である。It is the schematic explaining the principal part of the adhesion amount detection part 7 of the adhesion amount measuring apparatus which concerns on embodiment of this invention. 本発明の実施の形態に係る蛍光X線分析装置の蛍光X線測定ヘッドとめっき鋼板の間隔を5mmとしたときのP付着量と蛍光X線強度の関係を示す図である。It is a figure which shows the relationship between the amount of P adhesion, and a fluorescent X ray intensity when the space | interval of the fluorescent X ray measuring head and plated steel plate of the fluorescent X ray analyzer which concerns on embodiment of this invention is 5 mm. 本発明の実施の形態に係る蛍光X線分析装置の蛍光X線測定ヘッドとめっき鋼板の間隔を5mmとしたときのSi付着量と蛍光X線強度の関係を示す図である。It is a figure which shows the relationship between the amount of Si adhesion, and fluorescent X-ray intensity when the space | interval of the fluorescent X-ray measuring head of the fluorescent X-ray analyzer which concerns on embodiment of this invention and a plated steel plate is 5 mm. 形状検出部の要部を示す概略図である。It is the schematic which shows the principal part of a shape detection part. 本発明の実施の形態に係る付着量測定装置の制御方法を説明するフロー図である。It is a flowchart explaining the control method of the adhesion amount measuring apparatus which concerns on embodiment of this invention. 測定ヘッドを、鋼板面の直角方向に退避させる装置の要部構成例を示す概略平面図である。It is a schematic plan view which shows the example of a principal part structure of the apparatus which retracts a measurement head to the orthogonal | vertical direction of a steel plate surface.

符号の説明Explanation of symbols

1 鋼板(めっき鋼板)
2 巻き戻し装置
3 入側ルーパ
4 電気めっき部
5 塗装部
6 形状検出部(形状センサ)
7 付着量測定部
8 出側ルーパ
9 巻き取り装置
11 蛍光X線測定ヘッド(測定ヘッド)
12 光学系
13 X線発生器
14 半導体検出器
15、16 ガス通路
17 ガス供給装置
31、32 デフレクターロール
33a、33b サポートロール
34a、34b 蛍光X線測定ヘッド
35a、35b 駆動装置
36a、36b 台車
37a、37b レール
38a、38b コンベア
41 デフレクターロール
42 支持装置
43 ワイヤ
44 電源装置
45 電流計
46 線材の固定装置
51 形状演算
52 駆動装置制御部
53 付着量処理演算部(信号処理・解析装置)
54 集中制御盤
55 警報装置
61 摺動部材
62 駆動装置
63 軸
1 Steel plate (plated steel plate)
2 Rewinding device 3 Incoming looper 4 Electroplating unit 5 Coating unit 6 Shape detection unit (shape sensor)
7 Adhering Amount Measurement Unit 8 Outlet Looper 9 Winding Device 11 Fluorescent X-ray Measurement Head (Measurement Head)
DESCRIPTION OF SYMBOLS 12 Optical system 13 X-ray generator 14 Semiconductor detector 15, 16 Gas passage 17 Gas supply device 31, 32 Deflector roll 33a, 33b Support roll 34a, 34b Fluorescence X-ray measuring head 35a, 35b Drive device 36a, 36b Cart 37a, 37b Rails 38a, 38b Conveyor 41 Deflector roll 42 Support device 43 Wire 44 Power supply device 45 Ammeter 46 Wire rod fixing device 51 Shape calculation 52 Drive device control unit 53 Adhesion amount processing calculation unit (signal processing / analysis device)
54 Central control panel 55 Alarm device 61 Sliding member 62 Drive device 63 Axis

Claims (8)

その表面に皮膜が形成された走行中の金属帯の皮膜付着量測定装置であって、走行中の金属帯に近接して配置され、該金属帯表面にX線を照射し、励起・放射される蛍光X線を検出する蛍光X線測定ヘッドと、前記蛍光X線測定ヘッドを該金属帯幅方向に往復動可能に支持する支持装置と、前記蛍光X線測定ヘッドの該金属帯走行方向上流に配置され、該金属帯の形状を検出する形状センサと、前記形状センサで検出した金属帯の形状が閾値を超えたときに前記蛍光X線測定ヘッドを該金属帯幅方向端部外方または板面から離れる方向に退避させる退避装置と、を備えることを特徴とする付着量測定装置。   A device for measuring the amount of coating on a traveling metal strip with a coating formed on its surface, which is disposed in the vicinity of the traveling metal strip, and irradiates the surface of the metallic strip with X-rays to be excited and emitted. A fluorescent X-ray measuring head for detecting the fluorescent X-ray, a support device for supporting the fluorescent X-ray measuring head so as to reciprocate in the metal band width direction, and an upstream of the fluorescent X-ray measuring head in the traveling direction of the metal band. And a shape sensor for detecting the shape of the metal band, and when the shape of the metal band detected by the shape sensor exceeds a threshold, the fluorescent X-ray measurement head is moved outward of the end of the metal band width direction or And a retracting device for retracting in a direction away from the plate surface. 前記形状センサは金属帯との接触を検知する接触検知センサであることを特徴する請求項1記載の付着量測定装置。   The adhesion amount measuring apparatus according to claim 1, wherein the shape sensor is a contact detection sensor that detects contact with a metal strip. 前記接触検知センサの金属帯との接触検知部は、金属帯と所定間隔を設けて金属帯幅方向に張力を張って配置された線材で構成されていることを特徴する請求項1または請求項2記載の付着量測定装置。   The contact detection part with the metal band of the said contact detection sensor is comprised with the metal rod which has arrange | positioned tension | tensile_strength in the metal band width direction and provided the predetermined space | interval with a metal band. The adhesion amount measuring apparatus according to 2. 請求項1〜請求項3において、前記蛍光X線測定ヘッドは金属帯との間隔が10mm以下になるように配置することを特徴する付着量測定装置。   4. The adhesion amount measuring apparatus according to claim 1, wherein the fluorescent X-ray measurement head is arranged so that a distance from the metal band is 10 mm or less. 前記形状の閾値は、前記蛍光X線測定ヘッドと金属帯の間隔と同じ値であることを特徴とする請求項1〜請求項4のいずれかの項記載の付着量測定装置。   The adhesion amount measuring apparatus according to any one of claims 1 to 4, wherein the threshold value of the shape is the same value as an interval between the fluorescent X-ray measurement head and the metal strip. その表面に皮膜が形成された走行中の金属帯の皮膜付着量測定方法であって、走行中の金属帯に近接して、該金属帯表面にX線を照射し、励起・放射される蛍光X線を検出する蛍光X線測定ヘッドを配置して金属帯表面に形成された表面処理皮膜の元素の蛍光X線を測定するとともに、前記蛍光X線測定ヘッドの該金属帯走行方向上流に配置した形状センサで該金属帯の形状を検出し、検出した該金属帯の形状が閾値を超えたときは、前記蛍光X線測定ヘッドを該金属帯幅方向端部外方または板面から離れる方向に退避させることを特徴とする付着量測定方法。   A method for measuring the amount of coating on a traveling metal band having a film formed on the surface thereof, wherein the fluorescent light is excited and emitted by irradiating the surface of the metallic band with X-rays in the vicinity of the traveling metal band. A fluorescent X-ray measuring head for detecting X-rays is arranged to measure the fluorescent X-rays of the element of the surface treatment film formed on the surface of the metal band, and arranged upstream of the fluorescent X-ray measuring head in the traveling direction of the metal band. The shape sensor detects the shape of the metal band, and when the detected shape of the metal band exceeds a threshold value, the fluorescent X-ray measuring head is moved away from the end of the metal band width direction or away from the plate surface. A method for measuring the amount of adhesion, characterized in that it is evacuated. 請求項6において、前記蛍光X線測定ヘッドは金属帯との間隔が10mm以下の間隔を設けて配置され、前記形状センサが走行中の金属帯に対して前記所定間隔以上の歪量を検出すると、前記蛍光X線測定ヘッドを該金属帯幅方向端部外方または板面から離れる方向に退避させることを特徴とする付着量測定方法。   The fluorescent X-ray measurement head according to claim 6, wherein the fluorescent X-ray measurement head is arranged with an interval of 10 mm or less from the metal band, and the shape sensor detects a strain amount greater than the predetermined interval with respect to the traveling metal band. The method for measuring the amount of adhesion, characterized in that the fluorescent X-ray measurement head is retracted in the direction away from the end of the metal band width direction or away from the plate surface. 前記測定元素は、Caより原子番号の小さな元素(Caを含む)であることを特徴とする請求項6または請求項7記載の付着量測定方法。   The adhesion amount measuring method according to claim 6 or 7, wherein the measurement element is an element (including Ca) having an atomic number smaller than Ca.
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