KR102044980B1 - Steel sheet for scale analysis, method for manufacturing of the same, method for analysis scale using the same - Google Patents

Abstract

The present invention relates to a specimen for scale analysis, a preparation method thereof, and a scale analysis method using the same.
One embodiment of the present invention provides a specimen for scale analysis including a matrix layer, a scale layer, an adhesive layer, and a glass layer.

Description

Specimen for scale analysis, preparation method thereof, and scale analysis method using the same {STEEL SHEET FOR SCALE ANALYSIS, METHOD FOR MANUFACTURING OF THE SAME, METHOD FOR ANALYSIS SCALE USING THE SAME}

One embodiment of the present invention relates to a specimen for scale analysis, a preparation method thereof, and a scale analysis method using the same.

In general, the specimens may be prepared using mounting and mechanical polishing methods to analyze the plating layer thickness, composition, and bonding state of the interface of the hot-dip steel sheet. However, due to the difference in hardness between the plated layer and the base layer, when the mechanical polishing method is processed, overpolishing occurs in the plated layer, which is actually required to be observed, so that accurate analysis is difficult. Therefore, it is difficult to prepare a specimen for plating layer analysis by a conventional method.

In addition, the scale generated on the surface of the steel sheet during the post-heat treatment greatly affects the final product quality. Therefore, scale property analysis of scale thickness, crystal phase, and thickening element has emerged as a very important problem. However, the scale generated during the post-treatment is likely to drop off from the matrix by blisters or peelings. That is, they are fragile or brittle even with a very small impact. Therefore, there is a problem in securing and preparing the scale even when performing a process such as cutting and polishing in the step of preparing a specimen for analyzing physical properties. Therefore, it is impossible to analyze the thickness, the microstructure, and the crystal phase of the scale, and there is a limit in which only simple image observation or simple composition analysis in the surface state can be performed.

It is to provide a specimen for scale analysis, a method of manufacturing the same, and a scale analysis method using the same. Through this, it is easy to observe the cross section of the steel sheet including the scale by preparing a specimen for scale analysis to minimize the damage of the scale.

Specimen for scale analysis, which is an embodiment of the present invention, may include a matrix layer, a scale layer, an adhesive layer, and a glass layer.

In this case, the adhesive layer may include a first adhesive layer including a bond, and a second adhesive layer including an epoxy system.

Specifically, the first adhesive layer may be located between both the base layer and the scale layer and on both surfaces of the scale layer.

The glass layer may be located on the second adhesive layer.

The size of the specimen may be 10mm or less in width, 10mm or less in length, and 5mm or less in height.

In addition, the cross section in the depth direction of the scale analysis specimen may be a mirrored surface.

According to another aspect of the present invention, there is provided a method for preparing a scale analysis specimen, comprising: preparing a steel sheet including a scale, forming an adhesive layer on the steel sheet including the scale, and adhering glass on the adhesive layer to form a glass layer. Forming, and processing the steel sheet formed up to the glass layer may be included.

The forming of the adhesive layer on the steel sheet including the scale may include forming a first adhesive layer by applying a bond to the steel sheet including the scale, and applying an epoxy adhesive on the first adhesive layer to form a second adhesive layer. It may comprise the step of forming.

In the step of forming a first adhesive layer by applying a bond to the steel sheet including the scale, the bond may be in a liquid form.

Processing the steel sheet formed up to the glass layer may include cutting the steel sheet on which the glass layer is formed, and polishing a cut surface of the cut steel sheet.

Grinding the cut surface of the cut steel sheet may use a cross-section polisher (CP).

Specifically, the step of grinding the cut surface of the cut steel sheet, can be polished in the voltage range of 0.1 to 10kV.

It can also be polished for 30 minutes to 8 hours.

Cutting the steel sheet on which the glass layer is formed may use a fine cutter.

Another embodiment of the present invention, a scale analysis method using a scale analysis specimen, may include preparing the above-described scale analysis specimen, and analyzing the cut surface of the specimen.

At this time, the step of analyzing the cut surface of the specimen may be to analyze by SEM, EDS, EPMA or a combination thereof.

According to one embodiment of the present invention, a specimen for scale analysis may be provided. Specifically, a specimen for scale analysis may be provided for cross-sectional analysis of a steel sheet including a soft material that is brittle, such as scale. In this case, the scale analysis specimen may include an adhesive layer and a glass layer to protect the scale.

Accordingly, even when the polishing process using the cut surface polishing machine CP is performed for the cross-sectional analysis, loss of scale can be prevented. In addition, the cross-sectional analysis of the steel sheet including the scale to minimize the processing damage may be excellent.

1 is a flow chart briefly illustrating a method for preparing a specimen for scale analysis according to an embodiment of the present invention.
2 illustrates a specimen for scale analysis according to an embodiment of the present invention.
Figure 3 shows a sample for scale analysis according to Example 1.
Figure 4 illustrates a micro cutter and a processing method using the same for manufacturing a specimen for scale analysis according to an embodiment of the present invention.
FIG. 5 illustrates a cross-section polisher (CP) for manufacturing a specimen for scale analysis according to an embodiment of the present invention.
FIG. 6 is a cross-sectional view of a specimen for scale analysis of Example 1 by SEM. FIG.
7 is a result of analyzing the composition of the entire cross section of the specimen for scale analysis according to Example 1 by SEM-BEI and EDS.
8 is a result of analyzing the composition of a portion of the enlarged cross-section of the specimen for scale analysis according to Example 1 by SEM-BEI and EDS.
9 is a result of analyzing the scale layer of the specimen for scale analysis according to Example 1 by EPMA.
10 is a result of analyzing the matrix layer interface of the sample for scale analysis according to Example 1 by EPMA.

Advantages and features of the present invention and methods for achieving them will be apparent with reference to the embodiments described below in detail with the accompanying drawings. However, the present invention is not limited to the embodiments disclosed below, but may be embodied in various different forms, and the present embodiments merely make the disclosure of the present invention complete, and are common in the art to which the present invention pertains. It is provided to fully inform those skilled in the art of the scope of the invention, which is to be defined only by the scope of the claims. Like reference numerals refer to like elements throughout.

Thus, in some embodiments, well known techniques are not described in detail in order to avoid obscuring the present invention. Unless otherwise defined, all terms used in the present specification (including technical and scientific terms) may be used as meanings that can be commonly understood by those skilled in the art. When any part of the specification is to "include" any component, this means that it may further include other components, except to exclude other components unless otherwise stated. In addition, singular forms also include the plural unless specifically stated otherwise in the text.

Specimen for scale analysis, which is an embodiment of the present invention, may include a matrix layer 10, a scale layer 20, an adhesive layer 30, and a glass layer 40.

Specifically, the adhesive layer 30 may include a first adhesive layer 31 including a bond and a second adhesive layer 32 including an epoxy system.

In addition, the first adhesive layer 31 may be positioned between the base layer 10 and the scale layer 20 and on the surface of the scale layer 20.

As a result, the base layer 10 and the scale layer 20 may be adhered to each other by the first adhesive layer 31. Therefore, when analyzing using the scale analysis specimen, the scale layer 20 may be easily removed without falling off from the base layer 10.

The glass layer 40 may be located on the second adhesive layer 32.

Thus, the glass layer 40 may be bonded to the second adhesive layer 32. By further including the glass layer 40 as described above, the scale layer 20 can be protected.

In this case, the thickness of the glass layer 40 may be 1 to 2mm. However, it is not limited thereto.

The specimen may have a size of 10 mm or less, 10 mm or less, and 5 mm or less in height. When the size of the specimen is as described above, the cutting surface of the specimen can be polished in the processing step described later. Specifically, when the size of the specimen as described above, it can be inserted into the cutting surface grinding machine (CP) equipment for processing.

The cross section in the depth direction of the scale analysis specimen may be a mirrored surface.

As will be described later, a cross section in the depth direction of the specimen may be processed in the step S400 of processing the steel sheet formed up to the glass layer. Thus, the cross section of the specimen for scale analysis may be in a mirrored state. Therefore, scale analysis of the specimen may be easy.

In another embodiment of the present invention, a method for preparing a specimen for analysis of scale, preparing a steel sheet including a scale (S100), forming an adhesive layer on the steel sheet including the scale (S200), and glass on the adhesive layer It may include the step of forming a glass layer by adhering (S300), and processing the steel sheet formed up to the glass layer (S400).

First, a step (S100) of preparing a steel sheet including a scale may be performed.

Specifically, in the step (S100), the steel sheet may be any steel sheet including a scale.

More specifically, a steel sheet in which blisters are generated on a scale after a high temperature in-situ XRD experiment may be prepared on the heat treated specimen. However, it is not limited thereto.

Therefore, in this specification, the steel sheet including the scale means a steel sheet including the scale layer on the surface of the matrix layer.

Thereafter, forming an adhesive layer on the steel sheet including the scale (S200) may be performed.

Specifically, the step 200 is a step of forming a first adhesive layer by applying a bond to the steel sheet including the scale (S210), and by applying an epoxy-based adhesive on the first adhesive layer to form a second adhesive layer Step S220 may be included.

First, in step 210, the bond may be applied to the surface of the scale layer of the steel sheet prepared in the previous step 100.

Specifically, in step 210, the bond may be a liquid phase.

More specifically, when the bond is a liquid phase, it may penetrate between the scale layers to improve the adhesion between the steel sheet (base layer) and the scale layer. In addition, the bonding time can be reduced because the bond hardens quickly when in the liquid form.

More specifically, the bond may be applied to the surface of the scale layer so as to protrude convexly. In addition, it is possible to sufficiently bond the bond between the base layer and the scale layer.

Thus, the first adhesive layer including the bond may be positioned between the scale layer surface and the matrix layer and the scale layer through the step 210.

By applying the bond so that the scale layer and the base layer adhere as described above, loss of scale can be prevented. Thus, cross-sectional analysis of the specimen including the scale may be easy.

In addition, the step (S210) may be dried at room temperature for several seconds to 36 hours to form a first adhesive layer. However, it is not limited thereto.

Thereafter, in step S220, an epoxy-based adhesive may be applied onto the first adhesive layer to form a second adhesive layer.

The epoxy adhesive serves to bond the glass in the step described later.

Thereafter, the glass may be bonded to the second adhesive layer to form a glass layer (S300).

The glass layer formed in the step (S300) is located on the scale layer, it is possible to protect the surface of the specimen during the cross-sectional analysis after using the specimen.

Finally, the step (S400) of processing the steel sheet formed to the glass layer can be performed.

In detail, the processing of the steel sheet formed up to the glass layer may include cutting the steel sheet on which the glass layer is formed (S410) and polishing a cut surface of the cut steel sheet (S420).

More specifically, in the step (S410) it can be cut using a fine cutter to cut the steel sheet glass layer is formed. At this time, the cutting wheel of the fine cutter can be fixed by cutting to face the glass portion of the specimen.

More specifically, a device called a fine cutter can be equipped with a weight to process the specimen. More specifically, the specimen may be processed using the weight of the mounted weight, the weight of the specimen, and the load of gravity.

When cutting using a fine cutter as described above, it is possible to reduce the damage by reducing the stress generated in the first direct contact with the specimen surface.

In addition, in step S410 it may be cut in the length or width direction of the steel sheet.

The size of the specimen delivered by the step (S410) may be 10mm or less in width, 10mm or less in length, and 5mm or less in height. Specifically, cutting to a size in the above range may be possible after the polishing process.

Thereafter, in step S420, the cut surface of the cut steel sheet may be polished using a cross-section polisher (CP).

Specifically, a device called a cross-section polisher (CP) is a device for processing a section of a specimen using Ar ions. When the cut surface is polished using the cut surface grinding machine, a large area can be processed in a short time. In addition, it can be finely polished to the processing cross section at a weak voltage.

Thus, the polished specimen as described above can also be analyzed by EBSD.

Specifically, the step (S420) may be polished to a voltage range of 0.1 to 10kV. More specifically, it can be polished for 30 minutes to 8 hours.

In this way, the cross-sectional area of the specimen may be finely polished to process the surface state to the level of mirroring. In addition, the back-scattered electrons (e.g., back-scattered electrons) from the surface may be easily detected, and thus crystal orientation analysis and texture analysis may be easy.

Hereinafter, the embodiment will be described in detail. However, the following examples are merely to illustrate the invention, but the content of the present invention is not limited by the following examples.

Production Example

First, after the in-situ high temperature XRD experiment of the 22MnB5 post-heat treated specimen, a steel sheet having a scale layer was prepared.

Then, it was applied to the scale layer surface by varying the type of adhesive disclosed in Table 1 below. And dried for 24 hours at room temperature to form a first adhesive layer.

Thereafter, an epoxy-based adhesive was applied on the first adhesive layer to form a second adhesive layer.

Thereafter, glass was adhered to the second adhesive layer to form a glass layer.

And the steel plate formed to the glass layer was cut | disconnected in the longitudinal direction using the fine cutter. At this time, the cutting wheel of the fine cutter was fixed by cutting to face the glass portion of the specimen.

At this time, the used fine cutter is also disclosed in FIG.

Figure 4 illustrates a micro cutter and a processing method using the same for manufacturing a specimen for scale analysis according to an embodiment of the present invention.

Finally, the cut surface of the steel sheet cut at 8 kV, 2.8 Ma for 2 hours using a cut surface grinding machine (CP). The cut surface grinding machine CP used at this time is also shown in FIG.

FIG. 5 illustrates a cross-section polisher (CP) for manufacturing a specimen for scale analysis according to an embodiment of the present invention.

Specifically, the cut surface grinding machine is equipped with a total of three ion guns. Thus, there is typically an advantage that can process a large area at a much faster speed than a grinder equipped with one or two ion guns.

Comparative Example 1 Comparative Example 2 Example 1 Type of glue Paste Carbon-tape Super Bond Adhesion failure failure success

The results of manufacturing different kinds of first adhesive layers are as described in Table 1 above.

Specifically, Comparative Example 1 used a paste as a first adhesive layer, and Comparative Example 2 used a carbon tape (Carbon-tape) as a first adhesive layer. As a result, it can be seen that Example 1 was successfully bonded with the base layer and the scale layer using the super strong bond.

This is because the pastes and the carbon tapes of Comparative Examples 1 and 2, due to the viscosity of the introduction, caused the scale to fall off from the base layer when applied to the scale layer surface.

On the other hand, in the case of the super strong bond used in Example 1, it was a commercially available product in the general liquid type with little viscosity. As a result of using the super bond, it was confirmed that the base layer and the scale layer completely adhered after sufficient drying.

Experimental Example

Using the scale analysis specimen prepared in Example 1, the cross section of the specimen was analyzed.

The result is as shown in the figure.

6 is an image showing a cross section of the specimen for scale analysis of Example 1;

As shown in Figure 6, the cross section of the specimen for scale analysis of Example 1 is about 2mm in width, and the processed depth can be visually confirmed that the level of about 500㎛. The processing width and depth of the cross section can be controlled in proportion to the voltage and time. That is, the voltage and time of the polishing machine can be controlled and used according to the analysis purpose.

In addition, the average thickness of the scale confirmed through the cutting surface grinding machine (CP) processing is confirmed to be about 100㎛ level.

Typically, when processing the specimen using argon (Ar) or gallium (Ga) gas, damage such as curtain effect (curtain effect) may occur on the surface of the specimen.

In contrast, in the case of Example 1 according to the present invention, it can be seen that the cross section of the specimen is well processed without a series of damage. In addition, it was found that the scale to be analyzed is also well adhered without falling off from the base layer.

EDS and EPMA analysis is also possible using the specimen for scale analysis of Example 1 according to the present invention. Specifically, the type, form, thickening element, and the like of the crystal phase with respect to the thickness direction of the interface (base layer) on the scale surface can be analyzed.

This can also be confirmed through FIGS. 7 to 9.

7 is a result of analyzing the composition of the entire cross section of the specimen for scale analysis according to Example 1 by SEM-BEI and EDS.

8 is a result of analyzing the composition of a portion of the enlarged cross-section of the specimen for scale analysis according to Example 1 by SEM-BEI and EDS.

Specifically, comparing the content values of oxygen (O) and iron (Fe) derived from EDS in atomic% (at%), it is possible to know a kind of rough scale.

This is as disclosed in Table 2 below.

Ingredient (at%) FeO Fe ₃ O ₄ Fe ₂ O ₃ Fe 50 43 40 O 50 57 60

Table 2 discloses the types of scales depending on the ratio of iron and oxygen.

This allows scale analysis of the points disclosed in FIGS. 7 and 8.

First, the results of EDS analysis of FIG. 7 are shown in Table 3 below.

At% Point 1 Point 2 Point 3 Point 4 Point 5 Point 6 Point 7 O 57.09 50.81 55.80 50.87 55.51 58.19 52.64 Mn - 0.73 - 0.79 - - 0.93 Fe 42.91 48.46 44.20 48.34 44.49 41.81 46.44 Phase Fe ₂ O ₃ FeO Fe ₃ O ₄ FeO Fe ₃ O ₄ Fe ₂ O ₃ FeO

Specifically, it can be seen that the type of scale formed at Points 1 and 6, which are the surfaces of the specimen, is Fe ₂ O ₃ (Hematite). It can be seen that FeO (Wustite) and Fe ₃ O ₄ (Magnetite) are formed at Point 2, 4, 5, and 7 below.

The type of scale can also be distinguished in SEM-BEI (Back-scattered Electron Image) mode.

This can be confirmed in more detail in FIG. 8 where the composition of the enlarged cross-section is analyzed by EDS.

First, the EDS analysis results of FIG. 8 are shown in Table 4 below.

At% Point 1 Point 2 Point 3 Point 4 Point 5 Point 6 Point 7 Point 8 Point 9 Point 10 O 56.21 56.34 51.82 55.57 55.32 51.51 55.04 56.66 56.74 57.30 Mn - - 0.96 0.62 - 0.80 - - 0.84 - Fe 43.79 43.66 47.23 43.81 44.68 47.69 44.96 43.34 42.42 42.70 Phase Fe ₂ O ₃ Fe ₂ O ₃ FeO Fe ₃ O ₄ Fe ₃ O ₄ FeO Fe ₃ O ₄ Fe ₃ O ₄ Fe ₃ O ₄ Fe ₃ O ₄

Specifically, it can be confirmed that the magnetite (Fe ₃ O ₄ ) formed in the granule form under the barometer, hematite (Fe ₂ O ₃ ) shown in Figure 8 and Table 4 and Wustite (FeO) having a bright contrast. .

And it can be seen that the content ratio of oxygen and iron confirmed through the EDS composition analysis is almost consistent with the contents of Table 2.

In addition, the results of the enrichment element analysis using the specimen for scale analysis are as disclosed in FIGS. 9 and 10.

9 is a result of analyzing the scale layer of the sample for scale analysis according to Example 1 by EPMA.

10 is a result of analyzing the matrix layer interface of the sample for scale analysis according to Example 1 by EPMA.

Specifically, in order to determine the elements concentrated at the matrix and the scale interface, the analysis was performed using an Electron Probe X-ray Micro Analyzer (EPMA) element mapping method.

More specifically, FIG. 9 shows an image of the content of elements concentrated at the bottom interface of the scale. 10 is an image showing the content of elements concentrated in the interface of the upper end of the base layer.

9 and 10, it can be seen that Si, Mo, and Cr are concentrated in both the scale layer and the matrix layer. More specifically, in the case of the scale layer, it is possible to check a portion where the image comes out lightly according to the concentration distribution of oxygen. This means that as can be seen from the above-described EDS analysis, the fact that the type of scale varies according to the amount of oxygen can also be confirmed in the EPMA results.

Although the embodiments of the present invention have been described above with reference to the accompanying drawings, those skilled in the art to which the present invention pertains may implement the present invention in other specific forms without changing the technical spirit or essential features thereof. I can understand that.

Therefore, it should be understood that the embodiments described above are exemplary in all respects and not restrictive. The scope of the present invention is shown by the following claims rather than the detailed description, and all changes or modifications derived from the meaning and scope of the claims and their equivalents should be construed as being included in the scope of the present invention. .

10: base layer
20: scale layer
30: adhesive layer
31: first adhesive layer
32: second adhesive layer
40: glass layer

Claims (16)

Base layer;
Scale layer;
Adhesive layer; And
Including a glass layer,
The adhesive layer may include a first adhesive layer including a bond; And a second adhesive layer comprising an epoxy-based,
The first adhesive layer is located between the base layer and the scale layer and on the surface of the scale layer,
The second adhesive layer is located between the first adhesive layer and the glass layer,
The glass layer is located on the second adhesive layer, the specimen for scale analysis.
delete delete delete In claim 1,
The size of the specimen is a scale analysis specimens of size less than 10mm, less than 10mm, and less than 5mm in height.
In claim 5,
A cross section in the depth direction of the scale analysis specimen is mirror-scaled specimen.
Preparing a steel sheet including a scale;
Forming an adhesive layer on the steel sheet including the scale;
Adhering glass on the adhesive layer to form a glass layer; And
Process for producing a specimen for scale analysis comprising the step of processing the steel sheet formed to the glass layer.
In claim 7,
Forming an adhesive layer on the steel sheet including the scale,
Applying a bond to the steel sheet including the scale to form a first adhesive layer; And
A method for manufacturing a specimen for scale analysis comprising applying an epoxy-based adhesive on the first adhesive layer to form a second adhesive layer.
In claim 8,
In the step of forming a first adhesive layer by applying a bond to the steel sheet including the scale,
The bond is a method for producing a specimen for scale analysis in liquid form.
In claim 7,
The step of processing the steel sheet formed up to the glass layer,
Cutting the steel sheet on which the glass layer is formed; And
Method for producing a scale analysis specimen comprising the step of polishing the cut surface of the cut steel sheet.
In claim 10,
Polishing the cut surface of the cut steel sheet,
A method for preparing a specimen for scale analysis using a cross-section polisher (CP).
In claim 11,
Polishing the cut surface of the cut steel sheet,
Method for producing a specimen for scale analysis polished to a voltage range of 0.1 to 10kV.
In claim 12,
Polishing the cut surface of the cut steel sheet,
Method for preparing a scale analysis specimens to be polished for 30 minutes to 8 hours.
In claim 10,
Cutting the steel sheet on which the glass layer is formed,
Method for producing a specimen for scale analysis using a fine cutter.
Preparing a specimen according to any one of claims 1, 5 and 6; And
Scale analysis method using a specimen for scale analysis comprising the step of analyzing the cut surface of the specimen.
The method of claim 15,
Analyzing the cut surface of the specimen,
Scale analysis method using a specimen for scale analysis analyzed by SEM, EDS, EPMA or a combination thereof.

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