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JP2919295B2 - Method of measuring the amount of annealed separator applied to grain-oriented electrical steel sheets - Google Patents

Method of measuring the amount of annealed separator applied to grain-oriented electrical steel sheets

Info

Publication number
JP2919295B2
JP2919295B2 JP5578495A JP5578495A JP2919295B2 JP 2919295 B2 JP2919295 B2 JP 2919295B2 JP 5578495 A JP5578495 A JP 5578495A JP 5578495 A JP5578495 A JP 5578495A JP 2919295 B2 JP2919295 B2 JP 2919295B2
Authority
JP
Japan
Prior art keywords
amount
steel sheet
grain
oriented electrical
measuring
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.)
Expired - Lifetime
Application number
JP5578495A
Other languages
Japanese (ja)
Other versions
JPH08247970A (en
Inventor
伸一郎 田原
秀隆 小南
修 関口
直樹 松浦
Current Assignee (The listed assignees may be inaccurate. Google has not performed a legal analysis and makes no representation or warranty as to the accuracy of the list.)
Nippon Steel Corp
Rigaku Corp
Original Assignee
Nippon Steel Corp
Rigaku Industrial Corp
Priority date (The priority date 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 date listed.)
Filing date
Publication date
Application filed by Nippon Steel Corp, Rigaku Industrial Corp filed Critical Nippon Steel Corp
Priority to JP5578495A priority Critical patent/JP2919295B2/en
Publication of JPH08247970A publication Critical patent/JPH08247970A/en
Application granted granted Critical
Publication of JP2919295B2 publication Critical patent/JP2919295B2/en
Anticipated expiration legal-status Critical
Expired - Lifetime legal-status Critical Current

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  • Measurement Of Radiation (AREA)
  • Chemical Treatment Of Metals (AREA)
  • Analysing Materials By The Use Of Radiation (AREA)

Description

【発明の詳細な説明】DETAILED DESCRIPTION OF THE INVENTION

【0001】[0001]

【産業上の利用分野】本発明は、主としてトランスの鉄
心に利用される方向性電磁鋼板の製造に関するものであ
り、特に、脱炭焼鈍後の焼鈍分離剤塗布量の測定方法に
関するものである。
BACKGROUND OF THE INVENTION 1. Field of the Invention The present invention relates to the production of grain-oriented electrical steel sheets mainly used for transformer cores, and more particularly to a method for measuring the amount of an annealing separator applied after decarburizing annealing.

【0002】[0002]

【従来の技術】方向性電磁鋼板を製造する場合、脱炭焼
鈍後にMgOを主成分とする焼鈍分離剤を塗布する。こ
の目的は、大きく分けて次の2つである。
2. Description of the Related Art When producing grain-oriented electrical steel sheets, an annealing separator containing MgO as a main component is applied after decarburizing annealing. The purpose is roughly divided into the following two.

【0003】第1の目的は、焼付きの防止である。即
ち、脱炭焼鈍後の方向性電磁鋼板は、約1200℃もの
高温で仕上焼鈍されるが、この時に鋼板同士が直接接触
していると、焼付いてしまうので、これを防止するので
ある。
The first purpose is to prevent image sticking. That is, the grain-oriented electrical steel sheet after the decarburizing annealing is finish-annealed at a high temperature of about 1200 ° C. At this time, if the steel sheets are in direct contact with each other, they are seized, and this is prevented.

【0004】第2の目的は、絶縁皮膜の形成である。方
向性電磁鋼板は積層して使用するが、鋼板同士は絶縁さ
れていることが必要である。この絶縁皮膜形成は、脱炭
焼鈍で作られた酸化層と、脱炭焼鈍後に塗布されたMg
Oの反応によって行われる。
[0004] The second purpose is to form an insulating film. The grain-oriented electrical steel sheets are used in layers, but the steel sheets need to be insulated from each other. This insulating film is formed by an oxide layer formed by decarburizing annealing and Mg applied after decarburizing annealing.
This is performed by the reaction of O.

【0005】この絶縁皮膜は、上記絶縁効果と併せて鋼
板に張力を与えて磁気特性を改善する効果を有する。張
力を安定して付与するには、絶縁皮膜は鋼板との密着性
の良好な緻密なものとする必要がある。
[0005] This insulating film has an effect of improving magnetic properties by applying tension to the steel sheet in addition to the above-mentioned insulating effect. In order to stably apply the tension, it is necessary that the insulating film be dense with good adhesion to the steel sheet.

【0006】従って、このような良好な品質の絶縁性皮
膜を得るためには、脱炭焼鈍で形成される酸化層の質量
を適正なものとするとともに、MgOの諸特性及び塗布
量を厳密に管理する必要がある。
[0006] Therefore, in order to obtain such a good quality insulating film, the mass of the oxide layer formed by decarburization annealing is made appropriate, and the various properties and coating amount of MgO are strictly controlled. Need to be managed.

【0007】鋼板の表面の金属の鍍金量あるいは金属、
非金属の塗布量の測定には放射線を応用した測定法が一
般に知られている(特開昭53−42762号公報)。
これは、図4に示すように、放射線源1より発せられた
放射線が鋼板地金表面(Fe)に当たり、その結果、表
面から放射されるFeの特性X線を検出するが、その際
に表面付着物により特性X線の強度が減衰するため、こ
の減衰量から付着量の厚みを計測することを基本原理と
する。
The amount of metal plating on the surface of the steel sheet or the metal,
For measuring the amount of nonmetal applied, a measuring method using radiation is generally known (JP-A-53-42762).
This is because, as shown in FIG. 4, the radiation emitted from the radiation source 1 hits the steel sheet metal surface (Fe), and as a result, characteristic X-rays of Fe emitted from the surface are detected. Since the intensity of the characteristic X-ray is attenuated by the attached matter, the basic principle is to measure the thickness of the attached amount from the amount of attenuation.

【0008】放射線源1より一定強度で発せられた放射
線は、鋼板地金表面からFeの特性X線が発せられる。
この特性X線量は検出器2で検出され、変換器3で電気
信号に変換される。鋼板と検出器2の位置関係が一定の
場合は、表面に一様な付着物があるとその物質の特性に
より特性X線量が減衰されるため、電気信号と表面の付
着量は図2のような関数関係を持つ。すなわち電気信号
の検出によって表面の付着量が検出できる。
Radiation emitted from the radiation source 1 at a constant intensity emits characteristic X-rays of Fe from the surface of the steel sheet metal.
This characteristic X-ray amount is detected by the detector 2 and converted into an electric signal by the converter 3. When the positional relationship between the steel plate and the detector 2 is constant, if there is a uniform deposit on the surface, the characteristic X-ray dose is attenuated by the characteristics of the substance, so that the electric signal and the amount of deposit on the surface are as shown in FIG. Functional relationship. That is, the amount of adhesion on the surface can be detected by detecting the electric signal.

【0009】[0009]

【発明が解決しようとする課題】しかし、前記の検出方
法では、鋼板と検出器の位置関係が変化すると、この関
数関係も変化する。特に図4の平面図に垂直な直線を中
心にした回転方向の鋼板傾きに対しては、検出量が大き
く変化する。この特性X線検出量の変化は主に、鋼板表
面から放射される特性X線の、検出器2に到達するまで
の間に通過する付着物の厚みの変化によって生じ、特性
X線検出量は鋼板傾きΔθによって式1のように表され
る。
However, in the above detection method, when the positional relationship between the steel plate and the detector changes, this functional relationship also changes. In particular, the detection amount greatly changes with respect to the steel plate inclination in the rotation direction about a straight line perpendicular to the plan view of FIG. This change in the characteristic X-ray detection amount is mainly caused by a change in the thickness of the deposit of the characteristic X-ray radiated from the surface of the steel sheet before reaching the detector 2. It is expressed as Expression 1 by the steel plate inclination Δθ.

【0010】[0010]

【数1】 但し、I0 :鋼板傾き0のときの特性X線検出量 I :鋼板傾きΔθのときの特性X線検出量 μ1 :放射線源の付着物質吸収係数(定数項) μ2 :検出対象の特性X線の付着物質吸収係数(定数
項) α :鋼板表面の鉛直線に対する、検出器と鋼板上の検
出点とを結ぶ線の間の角度
(Equation 1) Here, I 0 : the characteristic X-ray detection amount when the steel plate inclination is 0 I: the characteristic X-ray detection amount when the steel plate inclination is Δθ μ 1 : the absorption coefficient of the attached substance of the radiation source (constant term) μ 2 : the characteristic of the detection target Absorption coefficient of X-ray adhering substances (constant term) α: Angle between the line connecting the detector and the detection point on the steel sheet with respect to the vertical line on the steel sheet surface

【0011】この特性X線検出量の変化は、例えば焼鈍
分離剤が付着した鋼板を測定する際にΔθ=3°の変化
があると、焼鈍分離剤による特性X線減衰量の20%程
度まで達し、正確な検出は望めない。
[0011] The change in the characteristic X-ray detection amount may be, for example, up to about 20% of the characteristic X-ray attenuation by the annealing separator when there is a change of Δθ = 3 ° when measuring the steel sheet to which the annealing separator is attached. And accurate detection cannot be expected.

【0012】このような鋼板の傾きによる誤差を解消す
るため、焼鈍分離剤が付着した鋼板では、接触式ロール
を使用したり、測定部の鋼板にテンションをかける方法
が考えられるが、MgO等の焼鈍分離剤が剥離するため
この方法は採用できない。
In order to eliminate such an error due to the inclination of the steel sheet, for a steel sheet to which an annealing separating agent has adhered, a method of using a contact roll or applying a tension to the steel sheet of the measuring unit is considered. This method cannot be adopted because the annealing separating agent peels off.

【0013】鋼板上の2点(複数点)での塗布量の測定
量と2点間の鋼板の傾きから、付着量を求める方法も知
られているが、鋼板の傾斜は必ずしも一様ではなく、こ
れによる誤差を伴うこととなる。
[0013] A method is also known in which the amount of adhesion is determined from the measured amount of coating at two points (plural points) on the steel sheet and the inclination of the steel sheet between the two points, but the inclination of the steel sheet is not always uniform. , Resulting in an error.

【0014】したがって、現在は、鋼板単位面積当たり
の塗布量を、切り出しサンプルによる重量法で測定して
おり、オンラインでの正確な測定はできなかった。
Therefore, at present, the amount of coating per unit area of a steel sheet is measured by a gravimetric method using cut samples, and accurate on-line measurement cannot be performed.

【0015】本発明が解決すべき課題は、鋼板が多少傾
いても、高精度の焼鈍分離剤付着量の測定を行うことの
できる方法を提供することにある。
The problem to be solved by the present invention is to provide a method capable of measuring the amount of annealed separating agent with high accuracy even when the steel sheet is slightly inclined.

【0016】[0016]

【課題を解決するための手段】前記課題を解決するた
め、本発明の方向性電磁鋼板の焼鈍分離剤塗布量の測定
方法は、脱炭焼鈍済みの方向性電磁鋼板への焼鈍分離剤
塗布量を、放射線源からの放射線を鋼板表面に照射し、
鋼板から発生する特性X線を検出器で検出することによ
って求めるに際し、2つの検出器を放射線源に対して対
称な位置に配置し、前記2つの検出器で検出したX線強
度の相加平均値を基に焼鈍分離剤塗布量を求めるもので
ある。
In order to solve the above-mentioned problems, a method for measuring the amount of an annealing separator applied to a grain-oriented electrical steel sheet according to the present invention is as follows. Irradiates the surface of the steel sheet with radiation from a radiation source,
When detecting characteristic X-rays generated from a steel sheet by detecting them with a detector, the two detectors are arranged at symmetrical positions with respect to the radiation source, and the intensity of the X-rays detected by the two detectors is determined.
The application amount of the annealing separating agent is determined based on the arithmetic mean value of the degrees .

【0017】[0017]

【作用】鋼板傾きΔθと、Δθ=0の場合の検量線によ
って得られた鋼板表面付着量測定値の真値からの誤差と
の関係は、鋼板傾きの小さな範囲では、ほぼ原点対称で
かつ直線的となる。そこで、2つの検出器を放射線照射
面に対して線対称な位置に配し、両者の付着量検出結果
の平均を取ることによって、鋼板傾きΔθによる誤差を
排除できる。これによって、接触ロールによってパスラ
インの安定化のできない焼鈍分離剤のような対象物に対
しても、オンラインで正確な付着量検出ができる。
The relationship between the inclination of the steel sheet Δθ and the error from the true value of the measured value of the amount of adhesion of the steel sheet surface obtained by the calibration curve when Δθ = 0 is almost symmetrical and linear in the range of small inclination of the steel sheet. Become a target. Therefore, by arranging the two detectors at positions symmetrical with respect to the radiation irradiation surface and averaging the detection results of the adhesion amounts of the two detectors, it is possible to eliminate an error due to the steel plate inclination Δθ. As a result, even for an object such as an annealing separator in which the pass line cannot be stabilized by the contact roll, it is possible to detect the attached amount accurately online.

【0018】[0018]

【実施例】以下、本発明を実施例を参照しながら具体的
に説明する。図1は本発明の実施例の構成を示す概略図
である。同図において、1は放射線源、2A,2BはX
線検出器、3A,3Bは検出量を電気信号に変換する信
号変換器、4A,4BはX線検出量を鋼板表面の付着量
に変換する検量線の入った付着量変換器、5は付着量変
換器4A,4Bによって変換された付着量の情報を平均
化する演算器、6は表示・記録装置を示す。
DESCRIPTION OF THE PREFERRED EMBODIMENTS The present invention will be specifically described below with reference to embodiments. FIG. 1 is a schematic diagram showing a configuration of an embodiment of the present invention. In the figure, 1 is a radiation source, 2A and 2B are X
Line detectors, 3A and 3B are signal converters for converting the detected amount into electric signals, 4A and 4B are adhesion amount converters containing a calibration curve for converting the X-ray detection amount to the adhesion amount on the steel sheet surface, and 5 is the adhesion amount converter. An arithmetic unit 6 for averaging the information of the adhesion amounts converted by the amount converters 4A and 4B, and 6 denotes a display / recording device.

【0019】鋼板傾きΔθと、Δθ=0の場合の検量線
によって得られた鋼板表面付着量測定値の真値からの誤
差との関係は、図3のようになる。鋼板傾きの小さな範
囲、例えば|Δθ|≦3°の範囲では、ほぼ原点対称と
なる。すなわち、図1のように検出器2A,2Bを放射
線照射面に対して線対称な位置に配する。式(1)によ
り、検出器2A,2Bの検出出力は次のようになる。
FIG. 3 shows the relationship between the steel sheet inclination Δθ and the error from the true value of the measured value of the steel sheet surface adhesion amount obtained from the calibration curve when Δθ = 0. In a small range of the steel plate inclination, for example, in the range of | Δθ | ≦ 3 °, the origin is almost symmetric. That is, as shown in FIG. 1, the detectors 2A and 2B are arranged at positions that are line-symmetric with respect to the radiation irradiation surface. According to equation (1), the detection outputs of the detectors 2A and 2B are as follows.

【0020】通常検出器として構成する場合、式(1)
においてμ1 <<μ2 となる波長を選択する。このた
め、式(1)の第1項は無視してもよい。すなわち、一
方の検出器による検出量は式(2)で表される。
When the detector is configured as a normal detector, equation (1)
In the above, a wavelength satisfying μ 1 << μ 2 is selected. Therefore, the first term of equation (1) may be ignored. That is, the amount detected by one of the detectors is expressed by equation (2).

【数2】 但し、I1 :鋼板傾きΔθのときの特性X線検出量(Equation 2) Here, I 1 is the characteristic X-ray detection amount when the steel plate inclination is Δθ.

【0021】図1のように線源をはさんで反対側に検出
器を設置した場合、その検出器での検出量は、傾きΔθ
が正負反対に作用するため、式(3)で表される。
When a detector is installed on the opposite side across the radiation source as shown in FIG. 1, the amount of detection by the detector has a slope Δθ
Acts in the opposite direction, and is therefore expressed by equation (3).

【数3】 但し、I2 :鋼板傾きΔθのときの特性X線検出量(Equation 3) Here, I 2 is the characteristic X-ray detection amount when the steel plate inclination is Δθ.

【0022】I1,I2の平均をとると、Δθ<<αの条
件の下では、式(4)が成立する。
Taking the average of I 1 and I 2 , equation (4) holds under the condition of Δθ << α.

【数4】 (Equation 4)

【0023】式(4)はΔθに影響を受けない。すなわ
ち、Δθが変動しても検出量は一定となる。
Equation (4) is not affected by Δθ. That is, the detected amount is constant even if Δθ fluctuates.

【0024】このように、両者の付着量検出結果の平均
を取ることによって、鋼板傾きΔθによる誤差を排除で
きる。これによって、接触ロールによってパスラインの
安定化のできない焼鈍分離剤のような対象物に対して
も、オンラインで正確な付着量検出ができる。
As described above, by taking the average of the detection results of the adhesion amounts of the two, an error due to the steel plate inclination Δθ can be eliminated. As a result, even for an object such as an annealing separator in which the pass line cannot be stabilized by the contact roll, it is possible to detect the attached amount accurately online.

【0025】[0025]

【発明の効果】上述したように、本発明によれば、2つ
の検出器をX線源に対して対称な位置に配置し、鋼板表
面からの特性X線を検出してそれらの平均をとること
で、鋼板傾きに起因する誤差が相殺され、高精度の焼鈍
分離剤塗布量が求められる。したがって、従来ではオン
ラインでは困難であった高精度の測定が可能となる。
As described above, according to the present invention, two detectors are arranged symmetrically with respect to the X-ray source, and characteristic X-rays from the surface of the steel sheet are detected and averaged. As a result, the error caused by the inclination of the steel sheet is offset, and a high-precision amount of the applied annealed separating agent is obtained. Therefore, high-precision measurement, which was conventionally difficult online, can be performed.

【図面の簡単な説明】[Brief description of the drawings]

【図1】 本発明の実施例の構成を示す概略図である。FIG. 1 is a schematic diagram showing a configuration of an embodiment of the present invention.

【図2】 特性X線検出量と表面付着量の関係を示すグ
ラフである。
FIG. 2 is a graph showing a relationship between a characteristic X-ray detection amount and a surface adhesion amount.

【図3】 鋼板傾きと付着量検出の誤差の関係を示すグ
ラフである。
FIG. 3 is a graph showing the relationship between the inclination of a steel sheet and an error in detection of the amount of adhesion.

【図4】 X線による付着物量検出方法の原理の説明図
である。
FIG. 4 is an explanatory diagram of the principle of a method for detecting the amount of attached matter using X-rays.

【図5】 鋼板の傾斜角と検出X線量変動特性を示すグ
ラフである。
FIG. 5 is a graph showing a tilt angle of a steel sheet and a variation characteristic of a detected X-ray dose.

【符号の説明】[Explanation of symbols]

1 放射線源、2A,2B X線検出器、3A,3B
信号変換器、4A,4B付着量変換器、5 演算器、6
表示・記録装置
1 radiation source, 2A, 2B X-ray detector, 3A, 3B
Signal converter, 4A, 4B adhesion amount converter, 5 arithmetic unit, 6
Display and recording device

───────────────────────────────────────────────────── フロントページの続き (72)発明者 関口 修 北九州市戸畑区飛幡町1−1 新日本製 鐵株式会社八幡製鐵所内 (72)発明者 松浦 直樹 大阪府高槻市赤大路町14番8号 理学電 機工業株式会社内 (56)参考文献 特開 平1−242908(JP,A) 特開 昭59−222586(JP,A) 特開 平2−250980(JP,A) 特開 昭60−133308(JP,A) 特開 昭64−59044(JP,A) 特開 昭53−42762(JP,A) (58)調査した分野(Int.Cl.6,DB名) G01N 23/22 - 23/227 C23C 22/00 JICSTファイル(JOIS)──────────────────────────────────────────────────続 き Continuing from the front page (72) Osamu Sekiguchi 1-1, Hibata-cho, Tobata-ku, Kitakyushu-shi Nippon Steel Corporation Yawata Works (72) Inventor Naoki Matsuura 14-8 Akaoji-cho, Takatsuki-shi, Osaka No. Rika Denki Kogyo Co., Ltd. (56) References JP-A-1-242908 (JP, A) JP-A-59-222586 (JP, A) JP-A-2-250980 (JP, A) JP-A-60 -133308 (JP, A) JP-A-64-59044 (JP, A) JP-A-53-42762 (JP, A) (58) Fields investigated (Int. Cl. 6 , DB name) G01N 23/22- 23/227 C23C 22/00 JICST file (JOIS)

Claims (1)

(57)【特許請求の範囲】(57) [Claims] 【請求項1】 脱炭焼鈍済みの方向性電磁鋼板への焼鈍
分離剤塗布量を、放射線源からの放射線を鋼板表面に照
射し、鋼板から発生する特性X線を検出器で検出するこ
とによって求めるに際し、2つの検出器を放射線源に対
して対称な位置に配置し、前記2つの検出器で検出した
X線強度の相加平均値を基に焼鈍分離剤塗布量を求める
ことを特徴とする方向性電磁鋼板の焼鈍分離剤塗布量の
測定方法。
1. The amount of an annealing separator applied to a decarburized annealed grain-oriented electrical steel sheet is determined by irradiating radiation from a radiation source onto the steel sheet surface and detecting characteristic X-rays generated from the steel sheet by a detector. In the calculation, two detectors were arranged at symmetrical positions with respect to the radiation source, and detected by the two detectors.
A method for measuring the amount of an annealing separator applied to a grain-oriented electrical steel sheet, wherein the amount of an annealing separator applied is determined based on an arithmetic mean value of X-ray intensities .
JP5578495A 1995-03-15 1995-03-15 Method of measuring the amount of annealed separator applied to grain-oriented electrical steel sheets Expired - Lifetime JP2919295B2 (en)

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JP5043387B2 (en) * 2006-08-29 2012-10-10 日本電子株式会社 Film analysis method and apparatus by fluorescent X-ray analysis
CN104198513A (en) * 2014-09-12 2014-12-10 江苏天瑞仪器股份有限公司 Quick determination method for cadmium element in grains with X-ray fluorescent spectrometry
CN104181182A (en) * 2014-09-12 2014-12-03 江苏天瑞仪器股份有限公司 Method for rapidly measuring arsenic element in grain by X fluorescent spectrometry

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