WO2010061969A1

WO2010061969A1 - Method for detecting steel hardened texture

Info

Publication number: WO2010061969A1
Application number: PCT/JP2009/070355
Authority: WO
Inventors: 瀬々昌文; 福永新一; 岩崎潤哉; 平田剛毅; 西尾渉
Original assignee: 新日本製鐵株式会社
Priority date: 2008-11-27
Filing date: 2009-11-27
Publication date: 2010-06-03
Also published as: JP5033112B2; JP2010127759A

Abstract

Provided is a method for detecting a steel hardened texture wherein the cross section of a steel ingot sample (1) is polished and polished surface (2) of the sample is corroded by immersion of the polished surface to a depth of 10 mm or less in a corrosive solution (3) with the polished surface (2) facing down. Preferably the polished surface is corroded while applying ultrasonic vibration to the sample and/or corrosive solution. It is possible to expose the hardened texture of steel grades for which the hardened texture has previously been difficult to expose, particularly low-carbon steel having a carbon concentration of 0.01 mass% or less, by immersion and corrosion of only a portion of a sample having the polished surface (surface to be corroded) in the corrosive solution.

Description

Method for detecting solidification structure of steel

The present invention relates to a method for detecting a solidified structure of steel, and more particularly to a method for detecting a solidified structure of steel capable of revealing a solidified structure even in a low carbon steel having a carbon content of 0.01% by mass or less. is there.

In the steel manufacturing process, detecting the solidification structure of the cast slab, which is a steel material after casting, evaluates internal defects such as macro segregation such as crack occurrence and center segregation of the slab, and guarantees quality in the subsequent process. Important to do. In addition, it is important to judge the presence or absence of abnormalities in the casting process and casting equipment from the occurrence of these internal defects in the slab, and to correct and maintain it in an appropriate state to prevent internal defects from occurring. . Furthermore, it is important to estimate the flow state of the internal molten steel during solidification and the cooling rate of the slab from the inclination and interval of the dendritic structure called dendrites in order to optimize the operating conditions.

The solidified structure of the slab can be observed by polishing the sample cross section of the slab, bringing the polished surface into contact with a corrosive liquid, and revealing the solidified structure. The manifestation of steel structure due to corrosion is roughly divided into two in principle. The first is an electrochemical corrosion method using a potential difference caused by a solute concentration difference at each position in a sample. The second is a chemical corrosion method utilizing a chemical potential difference of crystal grains depending on phases having different chemical potentials or crystal orientations on the surface. The first electrochemical corrosion method is used, for example, to detect dendritic structures, internal cracks, and center segregation using concentration differences due to segregation of solute elements during solidification. Examples of the second chemical corrosion method include observation of a pearlite structure using a chemical potential difference between Fe ₃ C and ferrite, macro corrosion using a chemical potential difference depending on the surface orientation of coarse ferrite grains, and the like. Therefore, in order to reveal and detect the solidified structure of the slab by corrosion, it is necessary to suppress the second chemical corrosion and cause the first electrochemical corrosion.

As a method for revealing a solidified structure of a slab, a method of corroding a sample surface using a corrosive solution containing picric acid as a main component is generally implemented (Non-patent Document 1). In addition, an etch print method has been proposed as a method for recording the revealed solidified structure (Patent Documents 1 to 5). The etch print method is a method in which the polished surface of the sample is brought into contact with a corrosive solution to corrode the polished surface, and then the sample is washed and dried, and abrasive powder is embedded in the corrosive holes on the corroded polished surface, and the surface is transparent. In this method, an adhesive tape is applied, and the abrasive powder in the corrosion holes is adhered to the transparent adhesive tape, then the tape is peeled off, and then the tape is attached to a white mount. The abrasive powder embedded in the corrosion holes is transferred to the tape, and the tape is affixed on the mount, whereby a solidified structure is revealed on the mount.

Japanese Patent Publication No. 64-2212 JP 61-170581 A Japanese Patent Laid-Open No. 1-227943 JP-A-7-198565 JP-A-6-213786

Regarding the method for revealing the solidification structure of the slab using the corrosive liquid mainly composed of picric acid described in Non-Patent Document 1, if the solute element concentration in the steel is not so low, solidification is in progress. Since the concentration difference due to segregation of solute elements is not small, a clear solidified structure can be revealed. On the other hand, the low solute element concentration in the steel, especially in the low carbon steel with a carbon concentration of 0.01% by mass or less, the concentration difference due to segregation of the solute element during solidification is small, so that the solidified structure is clearly revealed. It turned out to be difficult.

The present invention has a low solute element concentration in steel, and it has been difficult to detect a clear solidified structure by conventional steel types, particularly low carbon steel having a carbon concentration of 0.01% by mass or less. It is an object of the present invention to provide a method of revealing a solidified structure by means of this and thereby detecting the solidified structure of steel.

Conventionally, when a polished surface of a sample is corroded to reveal a solidified structure, the entire sample has been immersed in a corrosive liquid. On the other hand, by immersing only a part of the sample including the polished surface (corrosive surface) of the sample in a corrosive liquid and performing corrosion, the steel type, in particular, the carbon concentration, which has conventionally been difficult to reveal the solidified structure, is reduced. It has been clarified that a solidified structure can be revealed even in a low carbon steel of 0.01% by mass or less. In this case, it will be immersed in a corrosive liquid with the corroded surface down.

This invention is made | formed based on the said knowledge, The place made into the summary is as follows.
(1) It is characterized by polishing a cross section of a sample of steel slab, with the polished surface of the sample facing downward, and by immersing the polished surface of the sample in a corrosive solution within 10 mm, and corroding the polished surface. A solidified structure detection method for steel.
(2) The method for detecting a solidified structure of steel as described in (1) above, wherein the polished surface is corroded while ultrasonically vibrating one or both of the sample and the corrosive liquid.
(3) After contacting the polishing surface of the sample with a corrosive liquid to corrode the polishing surface, the sample is washed and dried, and polishing powder is embedded in the corrosive holes of the corroded polishing surface, and a transparent adhesive tape is applied to the polishing surface. The solidified structure of steel according to (1) or (2) above, wherein the abrasive powder in the corrosion holes is adhered to the transparent adhesive tape, then the tape is peeled off, and then the tape is attached to the mount. Detection method.
(4) The method for detecting a solidified structure of steel according to any one of (1) to (3) above, wherein the carbon content of the steel slab is 0.01% by mass or less.
(5) The size of the sample is 200 to 500 mm in length, 300 to 2100 mm in width, and 50 to 200 mm in thickness on the corroded surface, according to any one of (1) to (4) above A method for detecting the solidification structure of steel.

The present invention polishes a cross section of a sample of a steel slab, corrodes the polished surface with the polished surface of the sample facing downward, and the immersion depth of the polished surface of the sample in the corrosive liquid is within 10 mm. In the past, it was difficult to detect a clear solidified structure, especially low carbon steel with a carbon concentration of 0.01% by mass or less, and the solidified structure was revealed by corrosion, thereby solidifying the steel. It becomes possible to detect the tissue.

It is a figure which shows the immersion condition of the sample in a corrosive liquid, (a) is an example in which only a part of the sample is immersed with the polishing surface facing downward, (b) is an example in which an ultrasonic transducer is further contacted, (C) is an example in which the entire sample is immersed with the polishing surface facing downward, and (d) is an example in which the entire sample is immersed with the polishing surface facing up.

As shown in FIG. 1, the corrosive liquid tank 4 is filled with the corrosive liquid 3. The polished surface 2 of the sample 1 is immersed in the corrosive liquid 3. In either case, the polishing surface 2 is disposed below the liquid surface 5 of the corrosive liquid.

For example, an aqueous solution containing 20 g / liter of picric acid, 5 g / liter of cupric chloride, and 20 g / liter of a surfactant can be used as a corrosive solution that reveals a solidified structure of steel. As the surfactant, for example, a commercially available product under the trade name Rypon F can be used.

Specimen is cut out from the slab to detect the solidified structure. Next, polishing is performed on the cross section of the sample where the solidified structure is to be detected. The polishing conditions are preferably a finished surface of about # 240 to # 1000 after flattening and rough polishing the cross section to be polished. The size of the sample is preferably such that the surface to be polished and corroded (corroded surface) has a vertical width of 200 to 500 mm, a horizontal width of 300 to 2100 mm, and a thickness of 50 to 200 mm. By setting it as such a size, it is possible to reveal the solidified structure within a range in which the sample can be easily handled and using a wide surface as a corroded surface.

In the present invention, after the cross section of the steel slab sample is polished, as shown in FIG. 1 (a), the polishing surface 2 of the sample 1 faces downward and the corrosive liquid 3 on the polishing surface 2 of the sample 1 is placed. The dipping depth d is set to 10 mm or less, and the polished surface 2 is corroded. A portion of the sample 1 that is more than 10 mm away from the polishing surface 2 is not attacked by the corrosive liquid 3 and is exposed on the corrosive liquid bath. This makes it possible to reveal the solidified structure by corrosion even in the case of steel types that have conventionally been difficult to detect a clear solidified structure, particularly low-carbon steel having a carbon concentration of 0.01% by mass or less. The coagulated tissue can be detected.

In addition to forming a current loop in preference to the corroded surface 2 by corroding the polished surface 2 (corroded surface) downward and the immersion depth d in the corrosive liquid 3 within 10 mm as described above. It is considered that waste products generated on the corroded surface due to corrosion are easily removed, and a corrosive liquid having a high corrosive ability is supplied to the corroded surface, thereby improving the clarity of the solidified structure. On the other hand, as for the immersion depth d in the corrosive liquid 3, according to the experiment results of the present inventors, when the immersion depth d in the corrosive liquid exceeds 10 mm, the clarity of the solidified structure starts to decrease. The reason for this is presumed that the contribution of the current loop formed between the corroded surface facing downward increases and the clarity of the solidified structure of the corroded surface deteriorates.

In the method for detecting a solidified structure of steel targeted by the present invention, electrochemical corrosion utilizing a potential difference due to a solute concentration difference at each position in a sample is efficiently promoted. The reason is that the electrochemical corrosion effective for detecting the solidified structure is a corrosion using a potential difference due to a difference in solute concentration at each position in the sample, and a current loop is formed at a portion where the solute concentration is high and a portion where the solute concentration is low. When a local battery reaction occurs, a solid and solid solidified structure is revealed.

At this time, when the entire sample is immersed in a corrosive solution as in the prior art (FIGS. 1 (c) and (d)), if the surface other than the surface on which the solidified structure is to be exposed (corrosion surface) is in a conductive state, corrosion occurs. Since the current flows in addition to the surface, the density of the solidified structure is blurred on the important corroded surface.
On the other hand, in the method for detecting a solidified structure of steel according to the present invention, only the surface where the solidified structure is to be exposed is immersed in a corrosive liquid, and the local cell reaction, that is, the electrochemical reaction only on the surface where the solidified structure is to be exposed. In order to accelerate corrosion efficiently, it is difficult to reveal the solidification structure of conventional steel types, such as steel types that have a relatively small concentration difference due to segregation of solute elements during solidification, especially low carbon steel with a carbon concentration of 0.01% by mass or less. This makes it possible to reveal a clear solidified structure even with the steel type.

In the above-described method for detecting a solidified structure of steel according to the present invention, it is more preferable that the polished surface is corroded while ultrasonically vibrating one or both of the sample and the corrosive liquid. The example shown in FIG. 1B is an example in which the sample 1 is ultrasonically vibrated by bringing the ultrasonic vibrator 6 into contact with the sample 1. In the present invention, since the polishing surface 2 of the sample is faced downward and immersed in the corrosive liquid, by applying ultrasonic vibration to one or both of the sample and the corrosive liquid, It is considered that the removal is further promoted, the corrosion easily proceeds, and the clarity of the solidified structure is further improved. Since the purpose of vibrating the sample is to promote the removal of waste products caused by corrosion as described above, the same effect can be obtained by a similar method without being limited to ultrasonic vibration. It is also effective to promote the removal of waste products generated on the corroded surface by vibrating the corrosive liquid itself, or in combination with the vibration of the sample. The composition of the corrosive liquid in the case of applying ultrasonic vibration is not limited to the above composition, and any corrosive liquid that acts as an electrochemical corrosive liquid using a potential difference due to a solute concentration difference at each position in the sample may be used. The same effect can be obtained.

After exposing the solidified structure to the corroded surface, record the solidified structure. It is good also as taking a direct photograph of the corroded surface which revealed the solidification structure | tissue by corrosion. More preferably, an etch print method can be used. In this method, the polished surface of the sample is brought into contact with a corrosive liquid to corrode the polished surface, then the sample is washed and dried, and abrasive powder is embedded in the corroded holes on the corroded polished surface, and the transparent adhesive tape is applied to the polished surface. Is applied, and the abrasive powder in the corrosion holes is adhered to the transparent adhesive tape, and then the tape is peeled off, and then the tape is attached to a white mount. The abrasive powder embedded in the corrosion holes is transferred to the tape, and the tape is affixed on the mount, so that the density of the abrasive powder transferred to the tape corresponds to the solidified structure. It is revealed in

The steel solidification structure detection method of the present invention can be applied to a wide range of steel components to reveal the solidification structure. In particular, it is also possible to detect a solidified structure by using the present invention for a component system in which it is difficult to reveal a solidified structure by a conventional method, that is, a low carbon steel having a carbon content of 0.01% by mass or less. This is preferable.

The present invention was applied using an ultra-low carbon steel for automobiles having a carbon concentration of 0.001 mass%, a low-carbon steel sheet for cold rolling of 0.01 mass%, and a medium carbon steel sheet for thick plates of 0.1 mass%. The size of the sample cut out from the slab was the full height in the slab, the half width in the width direction, and the thickness was 50 mm or 100 mm. As a result, the corroded surface was in the range of 250 mm in length and 500 to 700 mm in width.

As the corrosive solution, an aqueous solution containing 20 g / liter of picric acid, 5 g / liter of cupric chloride and 20 g / liter of surfactant was used. As the surfactant, a commercial product under the trade name Raipon F was used. The temperature of the corrosive liquid was 25 ° C., and the corrosion time was 60 minutes.

Etch printing was used as a method for recording the solidified structure after corrosion. In this method, the polished surface of the sample is brought into contact with a corrosive liquid to corrode the polished surface, and then the sample is washed and dried, and polishing powder is embedded in the corrosive holes of the corroded polished surface, and the transparent adhesive tape is applied to the polished surface. Is applied, and the abrasive powder in the corrosion holes is adhered to the transparent adhesive tape, and then the tape is peeled off, and then the tape is attached to a white mount.

Table 1 shows the test conditions and evaluation results.

When the polishing surface 2 of the sample 1 is brought into contact with the corrosive liquid 3, as shown in FIG. 1 (a), the polishing surface 2 of the sample 1 faces downward and the polishing surface 2 of the sample 1 is used. The polishing surface 2 was corroded by setting the immersion depth d to 5 mm or 10 mm. For the comparative example, as shown in FIGS. 1C and 1D, the entire sample 1 is immersed in the corrosive liquid 3, or the immersion depth d of the polished surface 2 of the sample in the corrosive liquid 3 is 15 to 50 mm. did. The direction of the polished surface of the sample in the comparative example was both upward and downward.

As shown in FIG. 1B, the ultrasonic vibrator 6 having a frequency of 40 kHz and 100 W was brought into contact with the upper surface of the corroded sample 1 to vibrate the sample 1 ultrasonically.

When detecting the solidified structure, center segregation, internal cracking, and dendritic structure were detected. ◎: Extremely clear, ◯: Clear, Δ: Existence could be confirmed but unclear, x: Existence itself could not be identified. The degree of detection of the solidified structure becomes difficult in the order of center segregation → internal crack → dendritic structure.

As shown in FIG. 1 (d), Comparative Examples 1 to 3 in which the entire corroded surface is faced upward and immersed in the corrosive liquid, and Comparative Examples in which the corroded surface is faced downward and immersed in the corrosive liquid have an immersion depth of more than 10 mm. In Comparative Examples 10 to 12 (FIG. 1C) in which 4 to 9 and the entire sample were immersed in a corrosive solution, the solidified structure after corrosion was unclear. Originally, when the carbon concentration was relatively large due to solidification segregation and the carbon concentration was 0.1% by mass, center segregation could be detected to some extent clearly, but in Comparative Examples 3, 9, and 12, the internal cracks and the inclination of the dendritic structure Although the interval was confirmed, it was unclear. However, in Comparative Example 6 where the immersion depth was 15 mm, although a slight improvement tendency was recognized, it was not sufficient. Further, when the carbon concentration having a relatively small solute concentration difference due to solidification segregation is 0.01% by mass or 0.001% by mass, Comparative Examples 4 and 5 in which the immersion depth is 15 mm as in the case of 0.1% by mass. However, as shown in Comparative Examples 1, 2, 7, 8, 10, and 11, the existence itself cannot be identified from the inclination and interval of the dendritic structure, internal cracks, and center segregation. It was.

On the other hand, as shown in FIG. 1A, in the inventive examples 1 to 12 in which the corroded surface 2 faces downward and the immersion depth d in the corrosive liquid 3 is 10 mm or less, the solute concentration difference due to solidification segregation is relatively small. Even when the carbon concentration was 0.01% by mass or 0.001% by mass, the dendritic structure was improved to a level higher than the level at which the inclination and interval of the dendritic structure, internal cracks, and center segregation could be confirmed. In particular, as shown in FIG. 1B, in Examples 7 and 8 of the present invention in which ultrasonic vibration was applied with an immersion depth of 5 mm, the internal cracks and the center segregation were improved to a level that could be clearly discriminated. In addition, when the carbon concentration was originally 0.1% by mass with a relatively large difference in solute concentration due to solidification segregation, it was improved in the same manner. It is now possible to discriminate very clearly from the gaps, internal cracks, and center segregation.

The present invention is not limited to the above-described embodiment, and can be changed without changing the gist of the present invention. For example, some or all of the above-described embodiments and modifications are possible. The method of detecting the solidification structure of steel of the present invention by combining the above is also included in the scope of the right of the present invention.

As described above, the present invention is a steel type in which the concentration difference due to segregation of solute elements during solidification, in which the solidification structure is difficult to detect by a simple process, in particular, the carbon concentration is 0.01% by mass or less. Since the solidification structure of low carbon steel can be detected clearly, it is extremely useful in industry.

1 Sample 2 Polished surface (corrosion surface)
3 Corrosion liquid 4 Corrosion liquid tank 5 Liquid level 6 Ultrasonic vibrator d Immersion depth

Claims

A steel characterized in that a cross section of a sample of a steel slab is polished, the polished surface of the sample is faced down, and the polished surface is corroded by setting the immersion depth of the polished surface of the sample to a corrosive liquid within 10 mm. Coagulation tissue detection method.
The method for detecting a solidified structure of steel according to claim 1, wherein the polished surface is corroded while ultrasonically vibrating one or both of the sample and the corrosive liquid.
After contacting the polishing surface of the sample with a corrosive liquid to corrode the polishing surface, the sample is washed and dried, and then the polishing powder is embedded in the corrosion holes on the corroded polishing surface, and a transparent adhesive tape is applied to the surface of the polishing surface. The method for detecting a solidified structure of steel according to claim 1 or 2, wherein after the abrasive powder in the corrosion holes is adhered to the adhesive tape, the tape is peeled off, and then the tape is attached to the mount.
The method for detecting a solidified structure of steel according to any one of claims 1 to 3, wherein the carbon content of the steel slab is 0.01 mass% or less.
The method for detecting a solidified structure of steel according to any one of claims 1 to 4, wherein the size of the sample is 200 to 500 mm in length, 300 to 2100 mm in width, and 50 to 200 mm in thickness on the corroded surface. .