JPH09257728A - Coated oil film amount measuring method - Google Patents
Coated oil film amount measuring methodInfo
- Publication number
- JPH09257728A JPH09257728A JP6437696A JP6437696A JPH09257728A JP H09257728 A JPH09257728 A JP H09257728A JP 6437696 A JP6437696 A JP 6437696A JP 6437696 A JP6437696 A JP 6437696A JP H09257728 A JPH09257728 A JP H09257728A
- Authority
- JP
- Japan
- Prior art keywords
- amount
- oil film
- oil
- measuring
- fluorescent
- Prior art date
- Legal status (The legal status is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the status listed.)
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- Investigating Or Analyzing Materials Using Thermal Means (AREA)
Abstract
Description
【０００１】[0001]
【発明の属する技術分野】本発明は、鋼板等の金属材料
の表面に塗布された油の量（以下、「油膜量」という）
の測定方法、特に、鋼板表面に極めて薄い油膜が形成さ
れた場合の油膜量の測定方法に関する。TECHNICAL FIELD The present invention relates to the amount of oil applied to the surface of a metal material such as a steel plate (hereinafter referred to as “oil film amount”).
The present invention relates to a method for measuring the amount of oil film when a very thin oil film is formed on the surface of a steel sheet.
【０００２】[0002]
【従来の技術】金属材料、例えばブリキ等の素材として
使用される極薄ブライト冷延鋼板を製造する際、焼鈍処
理を施した後に、調質度、表面肌および平坦度の改善を
図るための調質圧延が行われる。2. Description of the Related Art When manufacturing an ultra-thin bright cold-rolled steel sheet used as a material for a metal material such as tin plate, it is intended to improve the temper, surface texture and flatness after annealing treatment. Temper rolling is performed.
【０００３】この調質圧延の方法としては、調圧油を用
いないで圧延する乾式調質圧延と、調圧油をスプレーで
鋼板表面に噴射させる湿式調質圧延とがあるが、湿式調
質圧延が一般的である。これは、調圧油をスプレーする
ことによる鋼板およびロール表面の清浄化、およびワー
クロールへの異物の付着等による外観欠陥の発生防止が
期待できるとともに、調圧油が優れた防錆効果も有して
いるからである。As the temper rolling method, there are dry temper rolling in which no pressure regulating oil is used and wet temper rolling in which pressure regulating oil is sprayed onto the surface of the steel sheet. Rolling is common. This can be expected to clean the surface of the steel sheet and roll by spraying pressure-regulating oil, and to prevent appearance defects due to foreign matter adhering to the work roll, and the pressure-regulating oil also has an excellent rust prevention effect. Because they are doing it.
【０００４】しかしながら、湿式調質圧延を行うと、摩
擦係数が小さいため鋼板に過度の伸びが生じやすく、し
かも伸び率が安定せず、さらに鋼板表面の光沢も悪くな
るという欠点がある。一方、乾式調質圧延を行った場合
は、光沢度は高く、伸び率も安定するが、上記の外観欠
陥が生じやすく、また、摩擦係数が大きいため圧延荷重
が大きくなり、材質によっては所定の伸び率が得られな
いという問題がある。したがって、調圧油の供給量を制
御し、湿式と乾式の中間的な極薄油膜のもとでの圧延方
法の開発が求められている。However, when the wet temper rolling is carried out, there is a drawback that the steel sheet is likely to be excessively elongated due to its small friction coefficient, and further, the elongation rate is not stable and the gloss of the steel sheet surface is deteriorated. On the other hand, when dry temper rolling is performed, the glossiness is high and the elongation is stable, but the above-mentioned appearance defects are likely to occur, and since the friction coefficient is large, the rolling load becomes large, and depending on the material, There is a problem that the elongation cannot be obtained. Therefore, there is a demand for the development of a rolling method under the control of the amount of pressure-regulating oil supplied and an intermediate ultra-thin oil film of wet type and dry type.
【０００５】このためには、湿式調質圧延におけるより
も薄い油膜が鋼板表面に形成された場合の油膜量の測定
技術が必須となる。For this purpose, a technique for measuring the amount of oil film when a thinner oil film is formed on the surface of the steel sheet than in wet temper rolling is essential.
【０００６】油膜量の測定には、古くは、付着している
油膜を除去する前後の金属板の重量差を測定する重量法
や、油膜を金属板の表面から水面に移行させて油の単分
子膜を形成させ、その面積を測定することにより油膜量
を求めるハイドロフィルバランス法と呼ばれる方法が用
いられてきた。しかし、重量法では、通常、試料（金属
板）の重量に比べて塗布される油膜量がわずかであるた
めその重量差が小さく、試料秤量時の誤差が油膜量の測
定値に大きく影響する。また、ハイドロフィルバランス
法では、金属板の表面に付着している油を水面に移行さ
せるのに長時間を要し、さらに、水面上に移行させた油
の面積の測定は手間がかかる上、個人誤差が生じ易い等
の問題がある。[0006] For the measurement of the amount of oil film, a gravimetric method of measuring the weight difference of the metal plate before and after removing the adhering oil film, or by transferring the oil film from the surface of the metal plate to the surface of water and then measuring the oil film A method called a hydrofill balance method has been used in which a molecular film is formed and the area of the molecular film is measured to determine the amount of the oil film. However, in the gravimetric method, the amount of the oil film applied is usually small compared to the weight of the sample (metal plate), so that the difference in weight is small, and an error in weighing the sample greatly affects the measured value of the oil film amount. Further, in the hydrofill balance method, it takes a long time to transfer the oil adhering to the surface of the metal plate to the water surface, and further, the measurement of the area of the oil transferred to the water surface is troublesome, There is a problem that personal errors are likely to occur.
【０００７】その後、より簡易な方法として、以下の方
法ないしは装置が提案されている。例えば、特開昭６０
−１７４９３６号公報には、予熱炉、燃焼炉、炭酸ガス
量計測器および一酸化炭素量計測器を順次接続した装置
で、金属板表面に塗布されている防錆油を予熱炉で蒸発
させ、その蒸気を燃焼炉で燃焼させ、生成する炭酸ガス
および一酸化炭素の量を測定することにより油膜量を測
定する装置が開示されている。しかしながら、この装置
を用いて油膜量を求めると、油によっては、燃焼の際に
炭化するため完全には炭酸ガスや一酸化炭素に酸化され
ず、油膜量の正確な測定ができないという問題がある。After that, the following method or device has been proposed as a simpler method. For example, JP
No. 174936 discloses an apparatus in which a preheating furnace, a combustion furnace, a carbon dioxide gas amount measuring instrument and a carbon monoxide amount measuring instrument are sequentially connected, and the rust preventive oil applied to the surface of the metal plate is evaporated in the preheating oven. An apparatus is disclosed which measures the amount of oil film by burning the vapor in a combustion furnace and measuring the amounts of carbon dioxide gas and carbon monoxide produced. However, when the oil film amount is obtained using this device, some oils are carbonized during combustion and thus are not completely oxidized to carbon dioxide gas or carbon monoxide, which makes it impossible to accurately measure the oil film amount. .
【０００８】エリプソメトリーにより鋼板表面の塗布油
膜厚をオンラインで測定する方法も提案されている
（「計測自動制御学会論文集」Ｖｏｌ．２４（１９８
８）６７０〜６７７頁）。これは、偏光光学系にビーム
スプリッタと３個の固定検光子を設けた３チャンネル型
エリプソメータを用い、油膜で覆われた試料表面に単光
色の楕円偏光を入射させ、反射光の油膜による偏光状態
の変化を測定してその膜厚を求めるもので、迅速性に優
れた方法である。しかし、この方法では測定面積が小さ
くならざるを得ず、局部の油膜量の分析に対しては有効
であるが、試料全体の油膜量の測定に対しては分析値が
ばらつきやすいという欠点がある。A method for measuring the coating oil film thickness on the surface of a steel sheet online by ellipsometry has also been proposed ("Measuring and Automatic Control Society Proceedings", Vol. 24 (198).
8) 670-677). This is a three-channel ellipsometer with a beam splitter and three fixed analyzers in the polarization optical system. Single-color elliptically polarized light is made incident on the sample surface covered with an oil film, and the reflected light is polarized by the oil film. It is a method that is excellent in quickness because it measures the change in state and obtains the film thickness. However, with this method, the measurement area must be small, and although it is effective for the analysis of the amount of oil film in a local area, there is a drawback that the analysis value tends to vary for the measurement of the amount of oil film of the entire sample. .
【０００９】また、ピストン周辺部の油膜挙動を把握す
るための手段として、蛍光剤を添加したエンジンオイル
等にレーザーを照射することにより発生する蛍光の強度
から油膜厚さを求め、油膜分布を測定する方法が開発さ
れている（「自動車技術論文集」Ｖｏｌ．２４（１９９
３）１２８〜１３３頁）。この方法も迅速性に優れてい
るが、この方法を調質圧延時の油膜量の測定に適用しよ
うとすると、圧延前に、使用する油の中に蛍光剤を添加
する必要があるため、蛍光剤が調質圧延それ自体に悪影
響を与えるという問題がある。As a means for grasping the behavior of the oil film around the piston, the oil film thickness is obtained from the intensity of the fluorescence generated by irradiating the engine oil containing a fluorescent agent with a laser to measure the oil film distribution. Method has been developed (“Car Engineering Papers” Vol. 24 (199
3) 128-133). This method is also excellent in quickness, but if you try to apply this method to the measurement of the oil film amount during temper rolling, it is necessary to add a fluorescent agent to the oil used before rolling There is a problem that the agent adversely affects the temper rolling itself.
【００１０】[0010]
【発明が解決しようとする課題】本発明はこのような状
況に鑑みなされたもので、金属材料の表面に塗布された
油膜量の測定方法、特に、鋼板表面に湿式調質圧延にお
けるよりも薄い油膜が形成された場合の油膜量の測定方
法を提供することを目的としている。SUMMARY OF THE INVENTION The present invention has been made in view of such circumstances, and a method for measuring the amount of an oil film applied to the surface of a metal material, in particular, a thinner method in wet temper rolling on the surface of a steel sheet. An object of the present invention is to provide a method for measuring an oil film amount when an oil film is formed.
【００１１】[0011]
【課題を解決するための手段】本発明者らは、上記の課
題を解決するため、まず、金属材料表面に塗布されてい
る油膜を燃焼させ、生成する炭酸ガスまたは一酸化炭素
の量を測定する方法について検討を加えた。この方法
は、比較的簡易で、材料表面全体の油膜量の測定に適す
ると考えられたからである。In order to solve the above-mentioned problems, the present inventors firstly burn the oil film applied to the surface of the metal material and measure the amount of carbon dioxide gas or carbon monoxide produced. I examined how to do it. This method is considered to be relatively simple and suitable for measuring the amount of oil film on the entire surface of the material.
【００１２】前記の特開昭６０−１７４９３６号公報に
この方法を用いた装置が記載されているが、この場合
は、金属板表面に塗布された防錆油をまず予熱炉で蒸発
させ、その蒸気を燃焼炉で燃焼させる方式が採られてい
る。これは、金属板、例えば鋼板に含まれる炭素と燃焼
用の酸素との化合による炭酸ガスの生成を防止するため
とされている。また、生成する炭酸ガスおよび一酸化炭
素の量から油膜量を求めるに際しては、燃焼した防錆油
の量と生成する炭酸ガスの量との間には一定の関係があ
るので、それを利用して油膜量を求めている。The apparatus using this method is described in Japanese Patent Laid-Open No. 174936/1985. In this case, the rust preventive oil applied to the surface of the metal plate is first evaporated in a preheating furnace, A method of burning steam in a combustion furnace is adopted. This is supposed to prevent the generation of carbon dioxide gas due to the combination of carbon contained in a metal plate such as a steel plate and oxygen for combustion. Also, when determining the amount of oil film from the amounts of carbon dioxide and carbon monoxide produced, there is a certain relationship between the amount of burned rust-preventing oil and the amount of carbon dioxide produced, so use that. To obtain the amount of oil film.
【００１３】しかしながら、この方法を鋼板表面に形成
された薄い調圧油の油膜量の測定に用いたところ、油膜
量の正確な測定はできなかった。これは、調圧油が炭酸
ガスや一酸化炭素に完全には酸化されず、しかも、その
種類によって酸化効率が異なることによるものと考えら
れる。また、防錆油等の場合に比べて油膜量が著しく少
ないため、誤差が大きくなることもその一因と考えられ
る。However, when this method was used to measure the oil film amount of the thin pressure-regulating oil formed on the steel plate surface, the oil film amount could not be measured accurately. It is considered that this is because the pressure-regulating oil is not completely oxidized to carbon dioxide gas or carbon monoxide, and the oxidation efficiency varies depending on the type. In addition, the amount of the oil film is significantly smaller than that in the case of rust preventive oil and the like, and it is considered that one of the reasons is that the error becomes large.
【００１４】そこで、本発明者らは、測定に供される油
毎に、あらかじめ既知量の油を塗布した試料を用意し、
それらを蒸発させることなく直接燃焼させ、生成する炭
酸ガスまたは一酸化炭素の赤外線吸収量を測定すること
により塗布油膜量と赤外線吸収量の関係を求め、この関
係に基づいて実際の試料で得られた赤外線吸収量から油
膜量を求める方式を試みた。その結果、調圧油の種類に
よらず、また油膜量がきわめてわずかであっても、測定
が可能であることを確認した。Therefore, the inventors of the present invention prepared a sample to which a known amount of oil was applied in advance for each oil used for measurement,
By directly burning them without evaporating them, and measuring the infrared absorption of the carbon dioxide or carbon monoxide that is produced, the relationship between the amount of coating oil film and the infrared absorption is obtained, and based on this relationship, it is obtained with an actual sample. We also tried to obtain the amount of oil film from the infrared absorption. As a result, it was confirmed that measurement was possible regardless of the type of pressure-regulating oil and even when the amount of oil film was extremely small.
【００１５】さらに、本発明者らは、従来から試料表面
の組成分析に用いられている蛍光Ｘ線分析法の適用につ
いても検討した。この方法は、試料表面にＸ線を照射し
たときに発生する蛍光Ｘ線を測定する方法であるが、金
属材料表面に塗布された油膜の構成元素である炭素から
発生する蛍光Ｘ線強度を測定することにより、油膜量を
測定することができると考えられる。Furthermore, the present inventors also examined the application of the fluorescent X-ray analysis method which has been conventionally used for the composition analysis of the sample surface. This method is a method of measuring fluorescent X-rays generated when the sample surface is irradiated with X-rays, but measuring the fluorescent X-ray intensity generated from carbon which is a constituent element of the oil film applied to the surface of the metal material. By doing so, it is considered that the oil film amount can be measured.
【００１６】検討の結果、塗布油膜量とＣＫα線の蛍光
Ｘ線強度との間に良好な直線関係があることを知見し
た。As a result of the study, it was found that there is a good linear relationship between the amount of the applied oil film and the fluorescent X-ray intensity of CKα rays.
【００１７】本発明は上記の検討結果に基づいてなされ
たもので、その要旨は、下記（１）および（２）の塗布
油膜量測定方法にある。The present invention has been made on the basis of the above-mentioned examination results, and its gist resides in the following coating oil film amount measuring methods (1) and (2).
【００１８】（１）金属材料表面に塗布された油膜量の
測定方法であって、既知量の油を塗布した金属材料につ
いて、その油を燃焼させ、生成する炭酸ガスおよび／ま
たは一酸化炭素の赤外線吸収量を測定することにより塗
布油膜量と赤外線吸収量の関係を求め、次いで、未知量
の油が塗布された金属材料について、前記と同様に炭酸
ガスおよび／または一酸化炭素の赤外線吸収量を測定
し、先に求めた塗布油膜量と赤外線吸収量の関係から塗
布された油の量を求めることを特徴とする塗布油膜量測
定方法。(1) A method for measuring the amount of an oil film applied to the surface of a metal material, wherein a carbon material and / or carbon monoxide produced by burning the oil of a metal material applied with a known amount of oil is burned. The relationship between the coating oil film amount and the infrared absorption amount is obtained by measuring the infrared absorption amount, and then the infrared absorption amount of carbon dioxide gas and / or carbon monoxide is the same as described above for the metal material coated with an unknown amount of oil. Is measured, and the amount of oil applied is determined from the relationship between the amount of applied oil film and the amount of infrared absorption previously obtained, and a method for measuring the amount of applied oil film.
【００１９】（２）金属材料表面に塗布された油膜量の
測定方法であって、既知量の油を塗布した金属材料につ
いて、蛍光Ｘ線分析法を用いてＣＫα線の蛍光Ｘ線強度
を測定することにより塗布油膜量と蛍光Ｘ線強度の関係
を求め、次いで、未知量の油が塗布された金属材料につ
いて、前記と同様にＣＫα線の蛍光Ｘ線強度を測定し、
先に求めた塗布油膜量と蛍光Ｘ線強度の関係から塗布さ
れた油の量を求めることを特徴とする塗布油膜量測定方
法。(2) A method for measuring the amount of an oil film applied to the surface of a metal material, wherein the fluorescent X-ray intensity of CKα rays is measured by a fluorescent X-ray analysis method for a metal material applied with a known amount of oil. Then, the relationship between the amount of the applied oil film and the fluorescent X-ray intensity is obtained, and then the fluorescent X-ray intensity of the CKα ray is measured in the same manner as described above for the metal material to which the unknown amount of oil is applied,
A method for measuring the amount of applied oil film, characterized in that the amount of applied oil is obtained from the relationship between the amount of applied oil film and the fluorescent X-ray intensity obtained previously.
【００２０】[0020]
【発明の実施の形態】以下に、本発明の塗布油膜量測定
方法について詳細に説明する。BEST MODE FOR CARRYING OUT THE INVENTION The method for measuring the coating oil film amount of the present invention will be described in detail below.
【００２１】図１は、前記（１）の発明、すなわち燃焼
赤外線吸収法による塗布油膜量測定方法の概略工程の一
例を模式的に示す図である。FIG. 1 is a diagram schematically showing an example of the steps of the invention (1), that is, the method for measuring the amount of applied oil film by the combustion infrared absorption method.
【００２２】図１において、表面に油が塗布された金属
試料１を燃焼炉２に導入し、酸素気流中で加熱して塗布
された油を燃焼させる。このとき発生する炭酸ガスおよ
び一酸化炭素を含む蒸気を酸素とともに酸化銅等の酸化
触媒を充填した酸化炉３へ導き、加熱して一酸化炭素の
大部分を炭酸ガスに酸化する。続いて、検出器４により
炭酸ガスおよび／または一酸化炭素の赤外線吸収量を測
定し、あらかじめ作成してある塗布油膜量と赤外線吸収
量の関係に基づいて金属試料１に塗布された油膜量を求
める。In FIG. 1, a metal sample 1 whose surface is coated with oil is introduced into a combustion furnace 2 and heated in an oxygen stream to burn the coated oil. The vapor containing carbon dioxide and carbon monoxide generated at this time is introduced into an oxidation furnace 3 filled with an oxidation catalyst such as copper oxide together with oxygen and heated to oxidize most of the carbon monoxide into carbon dioxide. Then, the infrared absorption of carbon dioxide and / or carbon monoxide is measured by the detector 4, and the amount of the oil film applied to the metal sample 1 is determined based on the relationship between the amount of the applied oil film and the infrared absorption which is created in advance. Ask.
【００２３】上記の工程において、つまり（１）の油膜
量測定方法において、炭酸ガスおよび／または一酸化炭
素の赤外線吸収量を測定することとしたのは、油を燃焼
させる際の酸化効率の違いにより（換言すれば、油の種
類により）炭酸ガスと一酸化炭素の赤外線吸収の感度が
異なるからである。塗布されている油の種類に応じて感
度の良い方を選び、その赤外線吸収量を測定値として用
いる方法を採ってもよいし、あるいは、炭酸ガスと一酸
化炭素の両方の赤外線吸収量を測定し、得られる結果を
合算する方法を採ってもよい。In the above step, that is, in the oil film amount measuring method (1), the infrared absorption amount of carbon dioxide and / or carbon monoxide is measured because of the difference in oxidation efficiency when burning oil. (In other words, the carbon dioxide gas and carbon monoxide have different infrared absorption sensitivities). Depending on the type of oil applied, you can choose the one with better sensitivity and use the infrared absorption amount as the measurement value, or you can measure the infrared absorption amount of both carbon dioxide and carbon monoxide. However, a method of adding the obtained results may be adopted.
【００２４】また、上記の一酸化炭素を炭酸ガスに酸化
する工程は必須ではない。しかし、通常は炭酸ガスの赤
外線吸収量を測定して油膜量を求めるケースが多く、そ
の場合は、図１に示したように酸化工程を入れる方が好
ましい。なお、この酸化工程を入れて一酸化炭素の大部
分を炭酸ガスに酸化した場合は、炭酸ガスと一酸化炭素
の両方の赤外線吸収量を測定して得られる結果を合算し
てもよいが、炭酸ガスの赤外線吸収量のみから油膜量を
求める方が簡便である。The step of oxidizing carbon monoxide to carbon dioxide gas is not essential. However, usually, there are many cases in which the amount of oil film is obtained by measuring the amount of infrared absorption of carbon dioxide, and in that case, it is preferable to include an oxidation step as shown in FIG. When most of carbon monoxide is oxidized into carbon dioxide by including this oxidation step, the results obtained by measuring the infrared absorption amounts of both carbon dioxide and carbon monoxide may be summed, It is easier to determine the amount of oil film from the amount of infrared absorption of carbon dioxide.
【００２５】図２は、前記のあらかじめ作成しておく塗
布油膜量と赤外線吸収量の関係の一例を示す図で、既知
量の油（有機系調圧油）を０〜２０ｍｇ／ｃｍ2 の範囲
で段階的に塗布した鋼板（高炭素鋼、板厚０．３ｍｍ）
表面の油膜量を図１に示した工程に従い炭酸ガスの赤外
線吸収量を測定することにより求めたものである。燃焼
炉２および酸化炉３での加熱温度は、それぞれ４５０℃
および８００℃とした。なお、この例では、金属材料と
して鋼板を用いたが、実際には、測定対象の油膜が形成
された材料について塗布油膜量と赤外線吸収量の関係を
求めておく。FIG. 2 is a diagram showing an example of a previously created to keep applying oil film amount and the infrared absorption of the relationship of the range known amount of oil (organic adjusting oil) of 0~20mg / cm 2 Steel plate applied in stages (high carbon steel, plate thickness 0.3 mm)
The amount of oil film on the surface is obtained by measuring the amount of infrared absorption of carbon dioxide according to the process shown in FIG. The heating temperature in the combustion furnace 2 and the oxidation furnace 3 is 450 ° C, respectively.
And 800 ° C. Although a steel plate was used as the metal material in this example, the relationship between the applied oil film amount and the infrared absorption amount is actually obtained for the material on which the oil film to be measured is formed.
【００２６】図２から明らかなように、塗布油膜量と赤
外線吸収量の間には良好な直線関係が認められる。As is clear from FIG. 2, a good linear relationship is recognized between the coating oil film amount and the infrared absorption amount.
【００２７】燃焼炉２において、油の大部分は燃焼して
炭酸ガスや一酸化炭素になるが、油によっては、一部が
酸化（燃焼）せずに炭化した状態で装置内に残留する。
そのため、生成した炭酸ガスや一酸化炭素の量から直接
油膜量を求めると、未酸化部分は分析誤差となる。すな
わち、油を燃焼させる際の効率（酸化効率）の違いによ
る分析誤差が生じる。In the combustion furnace 2, most of the oil burns to carbon dioxide and carbon monoxide, but some of the oil remains in the apparatus in a carbonized state without being oxidized (burned).
Therefore, if the amount of oil film is directly calculated from the amount of carbon dioxide gas or carbon monoxide produced, the unoxidized portion becomes an analytical error. That is, an analysis error occurs due to a difference in efficiency (oxidation efficiency) when burning oil.
【００２８】しかし、上記（１）の方法では、前記の図
２に示したあらかじめ求めてある塗布油膜量と赤外線吸
収量の関係に基づいて実際の金属材料について検出され
た赤外線吸収量から油膜量を求めるので、前記の油を燃
焼させる際の酸化効率の違いによる分析誤差が除かれ、
すなわち補正され、塗布油膜量を正確に求めることが可
能になる。However, in the above method (1), the amount of oil film is calculated from the amount of infrared absorption detected for the actual metal material based on the relationship between the amount of coating oil film and the amount of infrared absorption which is obtained in advance as shown in FIG. Therefore, the analysis error due to the difference in the oxidation efficiency when burning the oil is removed,
That is, it is corrected and the amount of applied oil film can be accurately obtained.
【００２９】前記の特開昭６０−１７４９３６号公報に
記載された装置により油膜量を測定する際の「蒸発」の
工程を省き、油を直接燃焼させるので、上記（１）の方
法で測定される赤外線吸収量には鋼板に含まれる炭素と
燃焼用の酸素との化合により生成した炭酸ガスによる吸
収量も含まれる可能性がある。しかし、（１）の方法に
よれば、既知量の油を塗布した金属材料についても同様
の操作を行うので、この蒸発工程の省略に起因する誤差
は相殺され、除かれるので問題はない。The method described in (1) above is used because the "evaporation" step in measuring the amount of oil film is omitted and the oil is directly burned by the apparatus described in JP-A-60-174936. The infrared absorption amount may include the absorption amount of carbon dioxide gas generated by the combination of carbon contained in the steel sheet and oxygen for combustion. However, according to the method (1), since the same operation is performed on a metal material coated with a known amount of oil, the error due to the omission of the evaporation step is offset and removed, so that there is no problem.
【００３０】油の燃焼温度は、事前に燃焼温度と赤外線
吸収量の関係を求め、最も感度が高く精度の良い温度に
設定するのが望ましい。例えば前記の有機系調圧油に対
しては、通常、４００〜７００℃とすればよい。The oil combustion temperature is preferably set to the temperature with the highest sensitivity and accuracy by previously obtaining the relationship between the combustion temperature and the infrared absorption amount. For example, with respect to the above organic pressure-regulating oil, the temperature may be generally 400 to 700 ° C.
【００３１】酸化温度については、８００℃以上であれ
ば燃焼炉で発生した一酸化炭素の大部分が炭酸ガスに酸
化されるが、１０００℃程度以上になると、酸化触媒と
して通常用いられる酸化銅が融解するので、酸化銅を触
媒として用いる場合は、８００〜９００℃とするのが好
ましい。Regarding the oxidation temperature, if it is 800 ° C. or higher, most of the carbon monoxide generated in the combustion furnace is oxidized to carbon dioxide gas, but if it is about 1000 ° C. or higher, the copper oxide usually used as an oxidation catalyst is Since it melts, the temperature is preferably 800 to 900 ° C. when copper oxide is used as a catalyst.
【００３２】炭酸ガスの測定方法としては、赤外線吸収
法の他に熱伝導度や電気伝導度を測定する方法も考えら
れる。しかし、酸素気流中では炭酸ガスの熱伝導度の測
定は困難であり、電気伝導度を測定する方法では、赤外
線吸収法に比べて感度が大幅に低下する。As a method of measuring carbon dioxide gas, a method of measuring thermal conductivity or electric conductivity can be considered in addition to the infrared absorption method. However, it is difficult to measure the thermal conductivity of carbon dioxide in an oxygen stream, and the sensitivity of the method of measuring electrical conductivity is significantly lower than that of the infrared absorption method.
【００３３】上記（１）の方法が適用できる金属材料と
しては、冷延鋼板、めっき鋼板等の鋼板や、アルミニウ
ムシート等があげられる。また、これら金属材料表面に
塗布される油は、調質圧延に用いられる各種の調圧油の
他、潤滑油、防錆油等であってもよい。Examples of metal materials to which the method (1) can be applied include steel sheets such as cold rolled steel sheets and plated steel sheets, and aluminum sheets. The oil applied to the surface of these metal materials may be various pressure-regulating oils used for temper rolling, as well as lubricating oil, rust preventive oil, and the like.
【００３４】次に、前記（２）の発明である蛍光Ｘ線分
析法による塗布油膜量測定方法について述べる。Next, the method for measuring the amount of applied oil film by the fluorescent X-ray analysis method of the invention (2) will be described.
【００３５】この方法は、前述したように、試料表面に
Ｘ線を照射したときに発生する蛍光Ｘ線（塗布された油
膜の構成元素である炭素から発生するＣＫα線）を測定
する方法である。この場合も、油の種類毎に、既知量の
油を塗布した金属材料について塗布油膜量と蛍光Ｘ線強
度（ＣＫα線の強度）の関係を求めておき、実際の金属
材料について得られた蛍光Ｘ線からこの関係を用いて塗
布油膜量を求める。As described above, this method is a method of measuring fluorescent X-rays generated when the sample surface is irradiated with X-rays (CKα rays generated from carbon which is a constituent element of the applied oil film). . Also in this case, the relationship between the coating oil film amount and the fluorescent X-ray intensity (CKα-ray intensity) is obtained for the metal material coated with a known amount of oil for each type of oil, and the fluorescence obtained for the actual metal material is obtained. The amount of applied oil film is obtained from the X-ray using this relationship.
【００３６】図３は、既知量の油（有機系調圧油）を０
〜２０ｍｇ／ｃｍ2 の範囲で段階的に塗布した鋼板（高
炭素鋼、板厚０．３ｍｍ）表面の塗布油膜量とＣＫα線
の蛍光Ｘ線強度の関係の一例を示す図である。なお、こ
の例では、金属材料として鋼板を用いているが、前記
（１）の方法の場合と同様に、測定対象の油膜が形成さ
れた材料について上記の関係を求めておく。FIG. 3 shows that a known amount of oil (organic pressure regulating oil) is
It is a figure which shows an example of the relationship between the amount of coating oil films on the surface of a steel plate (high carbon steel, plate thickness 0.3 mm) and the fluorescent X-ray intensity of CKα rays which are applied stepwise in the range of ˜20 mg / cm 2 . Although a steel plate is used as the metal material in this example, the above relationship is obtained for the material on which the oil film to be measured is formed, as in the case of the method (1).
【００３７】図３から明らかなように、塗布油膜量と蛍
光Ｘ線強度の間には良好な直線関係が得られる。したが
って、あらかじめ既知量の油を塗布した鋼板等の金属材
料について蛍光Ｘ線強度を測定して得られた塗布油膜量
と蛍光Ｘ線強度の関係を求めておけば、この油を塗布し
た金属材料についてＣＫα線の蛍光Ｘ線強度を測定する
ことによって塗布油膜量を求めることができる。As is clear from FIG. 3, a good linear relationship can be obtained between the amount of applied oil film and the intensity of fluorescent X-ray. Therefore, if the relationship between the amount of the applied oil film and the fluorescent X-ray intensity obtained by measuring the fluorescent X-ray intensity of a metal material such as a steel plate to which a known amount of oil has been applied in advance, the metallic material applied with this oil is obtained. The amount of the applied oil film can be obtained by measuring the fluorescent X-ray intensity of the CKα line.
【００３８】この方法では、前記の従来技術におけるよ
うな蛍光剤の添加の必要がないので、蛍光剤による調質
圧延に対する悪影響の懸念がない。また、Ｘ線の照射面
積は広いので、この方法は材料表面全体の油膜量の測定
手段として好適な方法である。In this method, since it is not necessary to add a fluorescent agent as in the above-mentioned prior art, there is no fear of adverse effect on temper rolling by the fluorescent agent. Further, since the X-ray irradiation area is wide, this method is suitable as a means for measuring the amount of oil film on the entire material surface.
【００３９】上記（２）の方法が適用できる金属材料と
しては、（１）の方法の場合と同様で、冷延鋼板、めっ
き鋼板等の鋼板や、アルミニウムシート等があげられ
る。また、これら金属材料表面に塗布される油も、調圧
油に限らず、潤滑油、防錆油等であってもよい。The metal material to which the method (2) can be applied is the same as in the method (1), and examples thereof include cold rolled steel sheets, steel sheets such as plated steel sheets, and aluminum sheets. Further, the oil applied to the surface of these metal materials is not limited to the pressure adjusting oil, and may be lubricating oil, rust preventive oil, or the like.
【００４０】[0040]
【実施例】調圧油（有機系調圧油）を塗布した鋼板試料
（材質：高炭素鋼、寸法：２０ｍｍ×６０ｍｍ、厚さ
０．３ｍｍ）について、燃焼赤外線吸収法を用いる本発
明の（１）の方法を適用して塗布油膜量を求めた。すな
わち、前記鋼板試料を燃焼炉に入れ、燃焼温度４５０
℃、酸化温度８００℃の条件で試料表面に塗布された油
を燃焼、酸化させた。続いて、生成した炭酸ガスの赤外
線吸収量を測定し、あらかじめ同種の調圧油についてそ
の既知量を上記試料と同じ鋼板に塗布して得られた塗布
油膜量と赤外線吸収量の関係に基づいて、塗布油膜量を
求めた。なお、比較のために、同じ調圧油を塗布した鋼
板試料について、ハイドロフィルバランス法により塗布
油膜量を測定した。EXAMPLE A steel plate sample (material: high carbon steel, size: 20 mm × 60 mm, thickness: 0.3 mm) coated with a pressure-regulating oil (organic pressure-regulating oil) was tested according to the present invention using the combustion infrared absorption method. The method of 1) was applied to determine the amount of applied oil film. That is, the steel plate sample was placed in a combustion furnace and a combustion temperature of 450
The oil applied to the surface of the sample was burned and oxidized under the conditions of ℃ and oxidation temperature of 800 ℃. Then, the infrared absorption amount of the generated carbon dioxide was measured, and based on the relationship between the coating oil film amount and the infrared absorption amount obtained by applying the known amount of the same type of pressure-regulating oil to the same steel plate as the sample in advance. The amount of applied oil film was determined. For comparison, the amount of applied oil film was measured by the hydrofill balance method for steel plate samples to which the same pressure-regulating oil was applied.
【００４１】また、上記（１）の方法で用いたものと同
じ鋼板試料について、蛍光Ｘ線分析法を用いる本発明の
（２）の方法を適用してＣＫα線の蛍光Ｘ線強度を測定
し、あらかじめ同種の調圧油についてその既知量を上記
試料と同じ鋼板に塗布して得られた塗布油膜量と蛍光Ｘ
線強度の関係から、塗布油膜量を求めた。Further, with respect to the same steel plate sample as used in the above method (1), the fluorescent X-ray intensity of CKα ray was measured by applying the method (2) of the present invention using the fluorescent X-ray analysis method. , A coating oil film amount and fluorescent X obtained by previously coating a known amount of the same type of pressure regulating oil on the same steel plate as the above sample
The amount of applied oil film was determined from the relationship of the line strength.
【００４２】図４および図５は、それぞれ燃焼赤外線吸
収法を用いる（１）の方法および蛍光Ｘ線分析法を用い
る（２）の方法により得られた結果を、ハイドロフィル
バランス法により得られた結果と対比して示した図であ
る。4 and 5 show the results obtained by the method (1) using the combustion infrared absorption method and the method (2) using the fluorescent X-ray analysis method, respectively, by the hydrofill balance method. It is the figure shown in comparison with a result.
【００４３】図４および図５から明らかなように、本発
明の方法による測定値とハイドロフィルバランス法によ
る測定値はほぼ完全に一致した。また、各測定点におけ
る相対標準偏差（標準偏差を平均値で除した値）は、燃
焼赤外線吸収法については３％以下、蛍光Ｘ線分析法に
ついては４％以下で、本発明方法によって塗布油膜量を
精度良く測定できることを確認した。As is clear from FIGS. 4 and 5, the measured values by the method of the present invention and the measured values by the hydrofill balance method were almost completely in agreement. Further, the relative standard deviation (value obtained by dividing standard deviation by the average value) at each measurement point is 3% or less for the combustion infrared absorption method and 4% or less for the fluorescent X-ray analysis method. It was confirmed that the amount can be measured with high accuracy.
【００４４】[0044]
【発明の効果】薄い油膜が金属材料（例えば、鋼板）表
面に形成された場合の油膜量の測定に際し、本発明の方
法（燃焼赤外線吸収法による塗布油膜量の測定方法、ま
たは蛍光Ｘ線分析法による塗布油膜量の測定方法）を適
用すれば、材料表面全体の油膜量を正確に、かつ比較的
簡便に測定することができる。この方法は、特に、湿式
調質圧延におけるよりも薄い油膜が鋼板表面に形成され
た場合の油膜量の測定に好適である。When a thin oil film is formed on the surface of a metal material (for example, a steel plate), the method of the present invention (a method for measuring the amount of the applied oil film by the combustion infrared absorption method, or fluorescent X-ray analysis) is used. By applying the method of measuring the amount of applied oil film by the method, the amount of oil film on the entire surface of the material can be measured accurately and relatively easily. This method is particularly suitable for measuring the oil film amount when a thinner oil film is formed on the surface of the steel sheet than in wet temper rolling.
【図１】燃焼赤外線吸収法による塗布油膜量測定方法の
概略工程を模式的に示す図である。FIG. 1 is a diagram schematically showing a schematic process of a method for measuring a coating oil film amount by a combustion infrared absorption method.
【図２】塗布油膜量と赤外線吸収量の関係の一例を示す
図である。FIG. 2 is a diagram showing an example of a relationship between a coating oil film amount and an infrared absorption amount.
【図３】塗布油膜量と蛍光Ｘ線強度の関係の一例を示す
図である。FIG. 3 is a diagram showing an example of the relationship between the amount of applied oil film and the intensity of fluorescent X-rays.
【図４】ハイドロフィルバランス法と燃焼赤外線吸収法
による塗布油膜量の測定値の関係を示す図である。FIG. 4 is a diagram showing a relationship between measured values of an amount of applied oil film by a hydrofill balance method and a combustion infrared absorption method.
【図５】ハイドロフィルバランス法と蛍光Ｘ線分析法に
よる塗布油膜量の測定値の関係を示す図である。FIG. 5 is a diagram showing a relationship between measured values of a coating oil film amount by a hydrofill balance method and a fluorescent X-ray analysis method.
１：金属試料 ２：燃焼炉 ３：酸化炉 ４：検出器 1: Metal sample 2: Combustion furnace 3: Oxidation furnace 4: Detector
Claims (2)
法であって、既知量の油を塗布した金属材料について、
その油を燃焼させ、生成する炭酸ガスおよび／または一
酸化炭素の赤外線吸収量を測定することにより塗布油膜
量と赤外線吸収量の関係を求め、次いで、未知量の油が
塗布された金属材料について、前記と同様に炭酸ガスお
よび／または一酸化炭素の赤外線吸収量を測定し、先に
求めた塗布油膜量と赤外線吸収量の関係から塗布された
油の量を求めることを特徴とする塗布油膜量測定方法。1. A method for measuring the amount of an oil film applied to the surface of a metal material, the method comprising:
By burning the oil and measuring the infrared absorption of the carbon dioxide gas and / or carbon monoxide that is produced, the relationship between the coating oil film amount and the infrared absorption is obtained, and then the metal material coated with an unknown amount of oil The coating oil film is characterized in that the infrared absorption of carbon dioxide and / or carbon monoxide is measured in the same manner as described above, and the amount of the applied oil is determined from the relationship between the previously determined coating oil film amount and the infrared absorption amount. Quantity measurement method.
法であって、既知量の油を塗布した金属材料について、
蛍光Ｘ線分析法を用いてＣＫα線の蛍光Ｘ線強度を測定
することにより塗布油膜量と蛍光Ｘ線強度の関係を求
め、次いで、未知量の油が塗布された金属材料につい
て、前記と同様にＣＫα線の蛍光Ｘ線強度を測定し、先
に求めた塗布油膜量と蛍光Ｘ線強度の関係から塗布され
た油の量を求めることを特徴とする塗布油膜量測定方
法。2. A method for measuring the amount of oil film applied to the surface of a metal material, the method comprising:
The relationship between the amount of the applied oil film and the fluorescent X-ray intensity is obtained by measuring the fluorescent X-ray intensity of CKα rays using the fluorescent X-ray analysis method, and then the metallic material coated with an unknown amount of oil is the same as above. The method for measuring the amount of applied oil film is characterized in that the fluorescent X-ray intensity of CKα ray is measured, and the amount of applied oil is obtained from the relationship between the previously obtained amount of applied oil film and the fluorescent X-ray intensity.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| JP6437696A JPH09257728A (en) | 1996-03-21 | 1996-03-21 | Coated oil film amount measuring method |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| JP6437696A JPH09257728A (en) | 1996-03-21 | 1996-03-21 | Coated oil film amount measuring method |
Publications (1)
| Publication Number | Publication Date |
|---|---|
| JPH09257728A true JPH09257728A (en) | 1997-10-03 |
Family
ID=13256530
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| JP6437696A Pending JPH09257728A (en) | 1996-03-21 | 1996-03-21 | Coated oil film amount measuring method |
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| Country | Link |
|---|---|
| JP (1) | JPH09257728A (en) |
Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| JP2008521673A (en) * | 2004-11-29 | 2008-06-26 | ヴァレオ システム デシュヤージュ | How to apply anti-friction coating to wiper blade rubber profile and control its quality |
| CN114280216A (en) * | 2021-12-24 | 2022-04-05 | 中国石油大学(北京) | Oil sand oil content determination method |
-
1996
- 1996-03-21 JP JP6437696A patent/JPH09257728A/en active Pending
Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| JP2008521673A (en) * | 2004-11-29 | 2008-06-26 | ヴァレオ システム デシュヤージュ | How to apply anti-friction coating to wiper blade rubber profile and control its quality |
| CN114280216A (en) * | 2021-12-24 | 2022-04-05 | 中国石油大学(北京) | Oil sand oil content determination method |
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