KR100325341B1 - Method for measuring thickness of coated layer in non-directional electric steel - Google Patents

Method for measuring thickness of coated layer in non-directional electric steel Download PDF

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KR100325341B1
KR100325341B1 KR1019970030173A KR19970030173A KR100325341B1 KR 100325341 B1 KR100325341 B1 KR 100325341B1 KR 1019970030173 A KR1019970030173 A KR 1019970030173A KR 19970030173 A KR19970030173 A KR 19970030173A KR 100325341 B1 KR100325341 B1 KR 100325341B1
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thickness
convergence time
peak
measured
steel sheet
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KR1019970030173A
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KR19990005951A (en
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조남웅
손병관
정진호
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포항종합제철 주식회사
재단법인 포항산업과학연구원
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    • GPHYSICS
    • G01MEASURING; TESTING
    • G01BMEASURING LENGTH, THICKNESS OR SIMILAR LINEAR DIMENSIONS; MEASURING ANGLES; MEASURING AREAS; MEASURING IRREGULARITIES OF SURFACES OR CONTOURS
    • G01B11/00Measuring arrangements characterised by the use of optical techniques
    • G01B11/02Measuring arrangements characterised by the use of optical techniques for measuring length, width or thickness
    • G01B11/06Measuring arrangements characterised by the use of optical techniques for measuring length, width or thickness for measuring thickness ; e.g. of sheet material
    • G01B11/0616Measuring arrangements characterised by the use of optical techniques for measuring length, width or thickness for measuring thickness ; e.g. of sheet material of coating
    • GPHYSICS
    • G01MEASURING; TESTING
    • G01BMEASURING LENGTH, THICKNESS OR SIMILAR LINEAR DIMENSIONS; MEASURING ANGLES; MEASURING AREAS; MEASURING IRREGULARITIES OF SURFACES OR CONTOURS
    • G01B9/00Measuring instruments characterised by the use of optical techniques
    • G01B9/04Measuring microscopes
    • GPHYSICS
    • G01MEASURING; TESTING
    • G01BMEASURING LENGTH, THICKNESS OR SIMILAR LINEAR DIMENSIONS; MEASURING ANGLES; MEASURING AREAS; MEASURING IRREGULARITIES OF SURFACES OR CONTOURS
    • G01B9/00Measuring instruments characterised by the use of optical techniques
    • G01B9/02Interferometers
    • G01B9/02041Interferometers characterised by particular imaging or detection techniques
    • G01B9/02044Imaging in the frequency domain, e.g. by using a spectrometer

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  • Measurement Of Length, Angles, Or The Like Using Electric Or Magnetic Means (AREA)

Abstract

PURPOSE: A measuring method of a thickness of a coated layer in a non-directional electric steel is provided to measure the thickness of insulated film layer by easily measuring a Fe peak convergence time of a GDS(Glow Discharge Spectrometer). CONSTITUTION: A Fe peak convergence time is measured by a GDS. The thickness of a standard sample is measured with using a scanning microscope by producing the standard sample according to the composition of resin. An inclination is measured by plotting the measured thickness and the Fe peak convergence time. The thickness of a coated layer is calculated by multiplying the inclination by the Fe peak convergence time. Thereby, the Fe peak convergence time is measured easily, quickly and exactly.

Description

무방향성 전기강판의 코팅층 두께 측정방법Coating layer thickness measurement method of non-oriented electrical steel sheet

본 발명은 무방향성 전기강판의 양표면에 코팅되는 절연코팅층의 두께를 측정하는 방법에 관한 것이다.The present invention relates to a method for measuring the thickness of an insulating coating layer coated on both surfaces of a non-oriented electrical steel sheet.

일반적으로 무방향성 전기강판은 절연성, 내식성, 가공성 등의 특성을 필요로하기 때문에 전기강판의 표면에 무기 혹은 유 ·무기계의 코팅액을 도포한다.In general, since non-oriented electrical steel sheet requires characteristics such as insulation, corrosion resistance, and workability, inorganic or non-machined coating liquid is applied to the surface of electrical steel sheet.

코팅액은 일반적으로 콜로이달 실리카, Ca- 혹은 Mg-크로메이트(Chromate), 수지 등의 성분을 함유한다. 이들 조성에 따라서 용액의 안정성, 도포성, 색상 등의 여러 가지 특성이 변화한다. 롤 코터(Roll coater)를 사용하여 도포작업후 건조를 실시하면 고상의 절연피막을 형성한다.The coating solution generally contains components such as colloidal silica, Ca- or Mg-Chromate, resin, and the like. According to these compositions, various characteristics, such as stability of a solution, applicability | paintability, and a color, change. Drying is performed after the application using a roll coater to form a solid insulating film.

이렇게 형성된 절연피막의 두께는 절연성, 내식성, 표면외관 및 가공후 용접성에 커다란 영향을 미친다. 전기강판의 실제 제품에서 요구되는 이들 특성을 제어하기 위해서 절연피막의 두께를 조절하여야 하고, 작업공정후의 피막층의 두께를 정확히 평가할 필요가 발생한다.The thickness of the insulating film thus formed has a great influence on insulation, corrosion resistance, surface appearance and weldability after processing. In order to control these properties required in the actual product of electrical steel sheet, the thickness of the insulating film should be adjusted, and there is a need to accurately evaluate the thickness of the coating layer after the working process.

실제품의 무방향성 전기강판의 절연피막층 두께는 일반적으로 0.3-0.8μm의 범위 값의 매우 얇은 피막으로 이들의 값을 정확히 측정하는 것이 용이하지 못하고, 작업공정의 두께조절은 작업자의 경험에 의존하고 있다.The thickness of insulation coating layer of non-oriented electrical steel sheet of real product is generally very thin film in the range of 0.3-0.8μm, and it is not easy to measure these values accurately, and the thickness control of the work process depends on the operator's experience. .

종래에 사용한 피막측정에 있어서는 접촉식 도막측정법으로 이것은 침상의 프로브(probe)를 피막층에 접촉시키어 피막층의 전기전도도의 차이를 검출하여 산출되는 방식이다.In the conventional coating measurement, the contact coating method is a method which is calculated by contacting a needle-shaped probe with a coating layer to detect a difference in electrical conductivity of the coating layer.

그러나 전기강판에 있어서는 일부조성의 불균일 석출, 피막형상의 불균일, 소지 강판의 표면조도 영향등으로 인하여 측정부위별 오차가 크게 나타난다. 피박두께를 정확하게 측정하기 위해서는 전기강판의 단면을 몰딩하여, 주사현미경(SEM) 장비로 관찰하는 것이 보다 정확하다고 하겠다.However, in the electrical steel sheet, errors due to the measurement site appear largely due to uneven deposition of some compositions, uneven film formation, and the influence of surface roughness of the steel sheet. In order to accurately measure the thickness, it is more accurate to mold the cross section of the electrical steel sheet and observe it with a scanning microscope (SEM) device.

그러나 주사현미경 측정을 위해서는 시편준비 및 관찰 단면가공 등이 필요하며 장시간이 소요되는 문제점이 있다.However, in order to measure the scanning microscope, specimen preparation and observation cross-section processing are required, and a long time is required.

본발명은 절연피막처리된 표준시편을 제작한후 표준시편의 Fe 피크(peak) 수렴 시간을 측정하고 이들 시편을 주사현미경 올 사용하여 두께를 측정한다음 분광분석기에서 Fe 피크의 수렴시간과 주사현미경의 피막두께 관계식을 규정함으로서, 종래의 접촉식 측정법보다 신속, 정확하며, 용이하게 분광분석기의 Fe 피크 수렴시간을 측정하여 규정식의하여 절연피막층의 두께를 측정할 수 있도록한 무방향성 전기강판의 코팅 두께 측정방법을 제공함에 그 목적이 있는 것이다.According to the present invention, after preparing an insulating coated standard specimens, the Fe peak convergence time of the standard specimens was measured, and the thicknesses of the specimens were measured using a scanning microscope. The convergence time and scanning microscope of the Fe peaks in a spectrometer were measured. Coating of non-oriented electrical steel sheet by defining the film thickness relation of the film thickness, which is faster, more accurate, and easier to measure the Fe peak convergence time of the spectrometer, and the thickness of the insulating film layer can be measured by the formula. The purpose is to provide a thickness measurement method.

이와같은 목적을 갖는 본발명은 분광분석기로 Fe 피크(peak) 수렴시간을 측정하는 단계와, 수지의 조성에 따른 표준시편을 제조하여 주사현미경을 이용 표준시편의 두께를 측정하는 단계와, 상기 측정된 두께와 Fe 피크 수렴시간을 플롯(plot)하여 기울기를 측정하는 단계와 상기 코팅층의 두께는 기울기 x Fe 피크 수렴시간으로 구하는 단계로 구성됨을 특징으로 한다.The present invention having the above object is to measure the Fe peak (peak) convergence time with a spectrophotometer, to prepare a standard specimen according to the composition of the resin to measure the thickness of the standard specimen using a scanning microscope, and the measurement Plotting the measured thickness and Fe peak convergence time (plot) to measure the slope and the thickness of the coating layer is characterized by consisting of the step of obtaining the slope x Fe peak convergence time.

도1(가)-(마)는 본 발명에서 측정된 분광분석기에 의한 절연피막 두께에 따른 성분변화를 나타낸 그래프Figure 1 (a)-(e) is a graph showing the component changes according to the thickness of the insulating film by the spectrometer measured in the present invention

도2는 본 발명에 실시한 절연피막두께 변화에 따른 분광분석기 Fe 피크의 수렴 시간을 나타낸 그래프2 is a graph showing the convergence time of the Fe peak of the spectrometer according to the change in the thickness of the insulating film according to the present invention

본발명은 무방향성 전기강판의 절연피막 두께를 측정함에 있어서, 분광분석기로 Fe 피크(peak) 수렴시간을 측정하는 단계와, 수지의 조성에 따른 표준시편을 제조하여 주사현미경을 이용 표준시편의 두께를 측정하는 단계와, 상기 측정된 두께와 Fe 피드 수렴시간을 플롯(plot)하여 기울기를 측정하는 단계와, 상기 코팅층의 두께는 기울기 x Fe피크 수렴시간으로 구하는 단계로 구성하여서 된것이다.The present invention is to measure the thickness of the Fe peak convergence time with a spectrophotometer in measuring the insulation film thickness of the non-oriented electrical steel sheet, and to prepare a standard specimen according to the composition of the resin to the thickness of the standard specimen using a scanning microscope Measuring the step, and plotting the measured thickness and the Fe feed convergence time (plot) to measure the slope, and the thickness of the coating layer is composed of the step of obtaining the slope x Fe peak convergence time.

이와같이 구성된 본발명의 작용을 설명하면 다음과 같다The operation of the present invention configured as described above is as follows.

본 발명에서는 깊이를 프로파일(profile)할 수 있는 분광분석기인 GDS(Glow Disharge Spectrometer)를 사용하였다.In the present invention, a GDS (Glow Disharge Spectrometer), which is a spectrometer capable of profile depth, was used.

우선 콜로이달 실리카, Mg-chromate,수지등의 특정조성으로 혼합, 합성된 코팅액으로 절연피막처리된 표준시편을 제작하였다. 표준 시편은 특정조성의 절연 코팅액을 전기강판위에 0회, 2회, 4회, 6회, 8회 코팅처리하여 650℃근처에서 15초간 건조시키어 절연피막을 전기강판위에 형성시켜 제작하였다.First, standard specimens prepared with an insulating coating were prepared using a coating solution mixed and synthesized in a specific composition such as colloidal silica, Mg-chromate, and resin. Standard specimens were prepared by coating a specific composition of insulating coating solution on an electrical steel sheet 0 times, 2 times, 4 times, 6 times, 8 times, and drying it for 15 seconds at around 650 ° C to form an insulating film on the electrical steel sheet.

여기서 코팅처리된 4종의 전기강판을 1x1cm로 절취하고, 주사현미경 관찰을 위하여 아크릴수지로 단면이 관찰방향이 되도록 몰딩하였다. 주사현미경에 의한 피막단면의 두께측정값은 하기 표1에 나타내었다.Here, the four coated steel sheets were cut to 1 × 1 cm and molded with acrylic resin so that the cross section was in the direction of observation for scanning microscope observation. The measured thickness of the film cross section by the scanning microscope is shown in Table 1 below.

분광분석기 측정에 있어서는 소지강판과 코팅된 4층의 시편을 온도, 진공도, 전류, 전압, 측정면적(φ4mm) 등의 일정한 조건하에서 측정하였다.In the spectrophotometer measurement, the steel sheet and the coated four-layer specimens were measured under constant conditions such as temperature, vacuum degree, current, voltage, and measurement area (φ4 mm).

각 원소의 검출강도 기여도를 결과 그래프에서 용이하게 분별할 수 있도록 규정하여 표준측정조건으로 하였다. 이러한 조건하에서 표준시편의 분광분석기 결과를 도 1에 나타내었다.The detection intensity contribution of each element was defined as a standard measurement condition so that it could be easily distinguished from the result graph. The spectroscopy results of the standard specimens under these conditions are shown in FIG. 1.

상기 도1의(가)에서 알수 있듯이 코팅처리 되지 않은 소지강판에 있어서는 Fe 피크의 시간변화는 처음부터 급격히 상승하여 일정의 강도를 갖는 것을 알 수 있다.As can be seen in Figure 1 (a) it can be seen that in the non-coated base steel sheet, the time change of the Fe peak increases rapidly from the beginning and has a certain strength.

도1의 (나)는 2회 코팅처리된 것으로 19초의 측정시간후 Fe 피크의 수렴이 시작되고 Si, Cr, Mg, O, C등의 피크는 소지강판이 나타남에 따라 감소되는 것이 관찰된다.1 (b) is coated twice, the convergence of Fe peaks starts after the measurement time of 19 seconds and the peaks of Si, Cr, Mg, O, C, etc. are observed to decrease as the steel sheet appears.

도1의 (다)에 있어서 원소검출의 피크 양상은 도1의 (나)와 유사하나 Fe의 피크를 수렴하는데 걸리는 시간은 도1의 (나)보다 길어짐을 알 수 있다.In Fig. 1 (c), the peak pattern of element detection is similar to that of Fig. 1 (b), but the time taken to converge the Fe peak is longer than that of Fig. 1 (b).

도1의 (라)와 도1 (마)의 Fe피크 수렴시간은 순서대로 점점 길어짐을 알 수 있다. 이와같이 코팅의 횟수 즉 코팅층의 두께가 늘어남에 따라서 Fe 피크의 수렴에 걸리는 시간은 길어져 비례관계가 있음을 알 수 있었다.It can be seen that the Fe peak convergence time of FIGS. 1 (d) and 1 (e) becomes longer in order. As described above, as the number of coatings, that is, the thickness of the coating layer increases, the time taken for convergence of the Fe peak becomes long, and it is found that there is a proportional relationship.

5종 표준시편의 주사현미경서 관찰된 절연피막층 두께와 분관분석기의 측정에서 Fe 피크의 수렴시간 관계를 도2에 나타내었다.Fig. 2 shows the relationship between the thickness of the insulation film observed on the scanning microscopes of five standard specimens and the convergence time of the Fe peaks in the analytical analyzer.

상기 도2에서 알수 있듯이 코팅층의 두께(T/μm)=0.0199 x Fe 피크의 수렴시간 (t/sec)--------식(1)As can be seen in Figure 2 the thickness of the coating layer (T / μm) = 0.0199 x Fe peak convergence time (t / sec) -------- Formula (1)

의 관계가 있음을 알 수 있었다. 코팅액을 사용하여 도포처리하는 전기강판의 피막두께에 있어서 피막의 표준시편을 제작하여 주사현미경에 의해 두께를 측정한후 분관분석기로 시간을 측정하면 두께와 시간의 관계식을 결정할 수 있다.It was found that there is a relationship. In the coating thickness of the coated steel sheet coated with a coating solution, a standard specimen of the coating was prepared, the thickness thereof was measured by a scanning microscope, and time was measured using an analytical analyzer to determine the relationship between thickness and time.

이후 실제품의 코팅층 두께관리는 분관분석기 측정으로 Fe 피크의 수렴시간을 측정하므로서 신속, 정확하고 용이하게 두께의 측정이 가능하다.Since the coating layer thickness management of the actual product can be measured quickly, precisely and easily by measuring the convergence time of the Fe peak by analytical analyzer measurement.

(표 1) 표준시편의 주사현미경에 의한 두께 및 분관분석기에 의한 Fe 피크 수렴시간TABLE 1Thickness by Scanning Microscope of Standard Specimen and Fe Peak Convergence Time by Specimen Analyzer

Figure pat00001
Figure pat00001

실시예Example

본 발명에서 규정한 식 (1)을 사용하여 작업공정후의 실제품의 두께를 측정하여 였다. 표준시편과 제품에 사용한 코팅액의 조성은 동일하다. 표준시편 분광분석기 측정시의 조건을 사용하여 제품의 Fe 피크 수렴시간을 측정하였다. 측정된 시간을 식(1)을 사용하여 제품의 절연피막층의 두께를 하기 표 2와 같이 용이하게 규정할 수 있었다.The thickness of the actual product after a work process was measured using Formula (1) prescribed | regulated by this invention. The composition of the standard solution and the coating solution used in the product are identical. Fe peak convergence time of the product was measured using the conditions of the standard specimen spectrometer measurement. Using the formula (1), the measured time was able to easily define the thickness of the insulating film layer of the product as shown in Table 2 below.

[표 2]TABLE 2

Figure pat00002
Figure pat00002

이상과같은 본발명은 절연피막처리된 표준시편을 제작한후 표준시편의 Fe 피크 이 수렴시간을 측정하고 이들 시편을 주사현미경을 사용하여 두께를 측정한다음. 분광분석기에서 Fe 피크의 수렴시간과 주사현미경의 피막두께 관계식을 규정함으로서, 종래의 접촉식 측정법보다 신속, 정확하며, 용이하게 분광분석기의 Fe 피크 수렴시간을 측정하여 규정식의하여 절연피막층의 두께를 측정할 수 있는 효과가 있다.The present invention as described above is to measure the convergence time of the Fe peak of the standard specimen after preparing the insulating specimen treated standard specimens and then measure the thickness of these specimens using a scanning microscope. By defining the relationship between the Fe peak convergence time and the film thickness of the scanning microscope in the spectrometer, the Fe peak convergence time of the spectrometer can be measured more quickly, accurately and easily than the conventional contact measurement method. There is a measurable effect.

Claims (1)

무방향성 전기강판의 절연피막 두께를 측정함에 있어서, 분광분석기(GDS)로 Fe 피크 수렴시간을 측정하는 단계와.In measuring the insulating film thickness of the non-oriented electrical steel sheet, measuring the peak peak convergence time with a spectrometer (GDS). 수지의 조성에 따른 표준시편을 제조하여 주사현미경을 이용 표준시편의 두께를 측정하는 단계와.Preparing a standard specimen according to the composition of the resin and measuring the thickness of the standard specimen using a scanning microscope. 상기 측정된 두께와 Fe 피크 수렴시간을 플롯(plot)하여 기울기를 측정하는 단계와.Plotting the measured thickness and Fe peak convergence time to measure a slope; 상기 코팅층의 두께는 기울기 x Fe 피크 수렴시간으로 구하는 단계를 포함하여 구성됨을 특징으로하는 무방향성 전기강판의 코팅두께 측정방법.The thickness of the coating layer is a coating thickness measurement method of a non-oriented electrical steel sheet, characterized in that it comprises a step of obtaining by the slope x Fe peak convergence time.
KR1019970030173A 1997-06-30 1997-06-30 Method for measuring thickness of coated layer in non-directional electric steel KR100325341B1 (en)

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