WO2014171361A1 - 金属の欠陥検出方法 - Google Patents
金属の欠陥検出方法 Download PDFInfo
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- WO2014171361A1 WO2014171361A1 PCT/JP2014/060117 JP2014060117W WO2014171361A1 WO 2014171361 A1 WO2014171361 A1 WO 2014171361A1 JP 2014060117 W JP2014060117 W JP 2014060117W WO 2014171361 A1 WO2014171361 A1 WO 2014171361A1
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- WIPO (PCT)
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- inspection surface
- etching solution
- etching
- metal
- segregation
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- G—PHYSICS
- G01—MEASURING; TESTING
- G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
- G01N21/00—Investigating or analysing materials by the use of optical means, i.e. using sub-millimetre waves, infrared, visible or ultraviolet light
- G01N21/84—Systems specially adapted for particular applications
- G01N21/88—Investigating the presence of flaws or contamination
- G01N21/91—Investigating the presence of flaws or contamination using penetration of dyes, e.g. fluorescent ink
-
- G—PHYSICS
- G01—MEASURING; TESTING
- G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
- G01N33/00—Investigating or analysing materials by specific methods not covered by groups G01N1/00 - G01N31/00
- G01N33/20—Metals
- G01N33/204—Structure thereof, e.g. crystal structure
- G01N33/2045—Defects
-
- G—PHYSICS
- G01—MEASURING; TESTING
- G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
- G01N1/00—Sampling; Preparing specimens for investigation
- G01N1/28—Preparing specimens for investigation including physical details of (bio-)chemical methods covered elsewhere, e.g. G01N33/50, C12Q
- G01N1/32—Polishing; Etching
Definitions
- the present invention relates to a metal defect detection method for detecting defects by etching an inspection surface of a metal sample to reveal defects and imaging the inspection surface with an imaging device.
- a sulfur printing method or an etch printing method has been used as a quality evaluation method inside a metal material.
- a sample is cut out from the metal material, the cross section of the metal material is polished as an inspection surface, and evaluation is performed.
- an aqueous sulfuric acid solution is immersed in a transfer printing paper containing silver bromide and attached to the inspection surface, and the segregation of sulfur in the sample appears on the printing paper.
- This sulfur printing method it is possible to evaluate the center segregation or internal crack of a slab by utilizing the property that sulfur segregates at the center segregation part or crack part of the slab.
- the sulfur printing method is used for a material having a high sulfur concentration in a metal material, but cannot be applied to an extremely low sulfur steel having a low sulfur concentration.
- the etch print method uses the property that elements are segregated at the center segregation and cracks on the inspection surface.
- the inspection surface is etched to reveal the element segregation, and the sample is coated with petroleum jelly and then re-polished. This is a technique for visualizing segregation and cracking.
- This etch printing method can also be used for materials having a low sulfur concentration.
- the inspection surface of the metal material It is preferable to etch the inspection surface of the metal material, and to directly image the inspection surface with an imaging device such as a camera and record it as an image, because defects can be detected quickly unlike the etch printing method.
- an imaging device such as a camera and record it as an image.
- the defect portion since the defect portion is deeply dug due to the progress of etching, it is necessary to detect the defect using the deeply dug defect portion as a dark portion and the other normal portion (non-defect portion) as a bright portion.
- the inspection surface is etched (macro corrosion) and the inspection surface is imaged with an imaging device, the lightness of the defective portion and the normal portion is low because the lightness of the normal portion is low when the image is picked up with natural light or light illumination. There is a problem that the contrast is small.
- Patent Document 1 the inspection surface of a metal sample is polished in one direction, and the metal sample is etched to reveal defects in the metal sample. Then, the inspection surface is irradiated from a predetermined arrangement position using a linearly continuous light source or a light source (linear light source) in which a plurality of point light sources are linearly arranged, and the inspection surface is imaged by the imaging device. Thereby, the brightness of the normal part in the inspection surface captured image is made uniform and bright, and the defective part can be detected clearly.
- Patent Document 1 The method described in Patent Document 1 is intended to increase the contrast between the defective portion and the normal portion by increasing the lightness of the normal portion, and does not decrease the lightness of the defective portion. Therefore, the increase in contrast is naturally limited.
- the type of light source is limited to a linear light source, and further, the installation method of the light source, specifically, the relationship between the linear direction of the linear light source and the polishing direction, and the irradiation angle with respect to the polishing direction are limited. There was a need to improve the efficiency of defect detection work.
- the present invention relates to a metal defect detection method in which a defect is detected by etching an inspection surface of a metal sample to reveal a defect, and the defect is detected by imaging the inspection surface with an imaging device, thereby reducing the brightness of the defect portion.
- An object of the present invention is to provide a metal defect detection method capable of clearly detecting a defect portion without increasing the contrast between the portion and the normal portion and without limiting the light source and the polishing direction of the inspection surface.
- the gist of the present invention is as follows.
- a defect is manifested by holding an etching solution on the inspection surface such that the inspection surface of the metal sample faces upward and the entire inspection surface is covered with the etching solution.
- the thickness of the etching solution above the inspection surface is set to more than 0 mm and not more than 10 mm, and the inspection surface is imaged by the imaging device in this state.
- the metal sample may be immersed in the etching solution.
- the metal sample may be steel having a carbon concentration of 0.5% by mass or less.
- a defect is detected by etching an inspection surface of a metal sample and the inspection surface is imaged by an imaging device
- at least the entire inspection surface is covered with an etching solution on the inspection surface.
- the etching solution is held as shown, and the inspection surface is imaged by the imaging device before the etching solution is removed.
- the elution element is segregated positively in the segregation part in the metal material.
- the segregated portion 3a and the segregated portion 3b are positively segregated from the eluted element.
- the etching solution 5 is brought into contact with the inspection surface of such a metal sample 1, the etching rate is slow for the normal part 4 where the normal metal material is exposed, and the segregation part 3 (defect part) where the eluted element segregates.
- Has a high etching rate a difference occurs in the etching depth, and as shown in FIG. 1B, the defect portions such as the segregation portion 3a and the segregation portion 3b are deeply etched to form the recesses 9a and 9b.
- the defect portion has characteristics in the brightness of the eluted element or the compound of the eluted element generated by etching in addition to the difference in the etching rate.
- the eluting element or compound of the eluting element generated in the segregation part 3 has a lightness that is generally dark enough to be black. Therefore, as shown in FIG. 1B, the elution element or the compound (8a, 8b) of the elution element exists in the depression (9a, 9b) formed in the defect portion (segregation portion 3a, 3b) such as the segregation portion.
- these eluting elements or compounds of the eluting elements can remain in the defective part as they are, the lightness of the defective part will be dark, so the brightness difference (contrast) from the bright normal part will be intense, and the inspection surface was imaged by the imaging device. Sometimes the defect can be made even more pronounced. However, after the etching has progressed, the etching surface is conventionally removed and the inspection surface is cleaned, so as shown in FIG. 1C, the dark-colored elution elements or elution element compounds (8c, 8d) are also washed away. Therefore, it could not be used for defect detection. As shown in FIG.
- the etching solution is not washed and removed, and further, the etching solution is not allowed to flow on the inspection surface, and the etching product is eluted.
- the inspection surface is imaged with the imaging device while the element or the compound of the eluted element is kept in the segregation part. Specifically, as shown in FIG. 2A to FIG. 4, the etching liquid 5 is held so that the inspection surface 2 faces upward and at least the entire inspection surface is covered with the etching liquid 5 on the inspection surface.
- the inspection surface 2 is imaged by the imaging device 12. As shown in FIG.
- the segregation part 3b can be detected by imaging with the imaging device. Furthermore, cracks accompanied by segregation can also be detected.
- the required minimum amount of the etching solution that contacts the inspection surface may be present at least enough to cover the entire inspection surface with the etching solution at the time of imaging with the imaging device. Specifically, it is only necessary to maintain a state in which the entire inspection surface is wet with the etchant.
- the thickness H of the etching solution covering the upper portion of the inspection surface is too thick (if the depth from the etching solution surface to the inspection surface is too deep), as shown in FIG. Is likely to occur. If the elution element or the compound 8 of the elution element flows out of the segregation part due to this flow, the brightness of the segregation part cannot be kept dark.
- the flow 7 of the etching solution may be a flow caused by the convection of the etching solution due to a temperature difference between the inspection surface temperature and the etching solution temperature, or a flow when the etching solution is poured onto the inspection surface. Both become more significant as the thickness H of the etching solution on the inspection surface increases.
- the thickness H of the etching solution on the inspection surface is preferably 7 mm or less, more preferably 5 mm or less, and further preferably 3 mm or less.
- the lower limit of the thickness H of the etching solution on the inspection surface is more than 0 mm because the entire inspection surface only needs to be covered with the etching solution. However, it is good also as 0.3 mm or more or 0.5 mm or more in order to elute a segregation part suitably.
- a method of immersing the metal sample 1 in the etching solution in the etching container 10 as shown in FIGS. 2A and 2B can be employed.
- either the method in which the metal sample 1 is put in the etching container 10 and then the etching solution 5 is poured or the method in which the etching solution 5 is put in the etching container 10 and the metal sample 1 is immersed after that is adopted. You may do it.
- an etchant outflow prevention plate 11 is installed around the inspection surface 2 of the metal sample 1, and the etchant 5 is placed in a frame formed by the inspection surface 2 and the etchant outflow prevention plate 11. You may employ
- a method for confirming that the thickness H of the etching solution on the inspection surface is 10 mm or less will be described. If the method shown in FIGS. 2A and 2B is used, a length measurement scale is installed on the side surface of the etching container 10 and the water level of the etching solution is measured using this scale. If the thickness of the metal sample 1 is known in advance, the difference between the height at which the bottom of the metal sample 1 is in contact with the etching container and the water level of the etching solution is measured, and the thickness of the metal sample 1 is subtracted from this measured value. Thus, the thickness H of the etching solution can be calculated. If the method shown in FIG. 3 is used, the thickness H of the etchant can be measured by installing a scale on the inner side surface of the etchant outflow prevention plate 11.
- an etching solution used in the etching treatment of the present invention an etching solution that is a dark color (for example, black) with a lightness of an eluted element or a compound of the eluted element generated in a segregation part is easily selected from etching liquids that are usually used.
- etching liquids that are usually used.
- an aqueous solution of ammonium persulfate or an aqueous solution of picric acid is preferably used.
- any liquid may be used as long as it is an etching liquid that produces a segregated part or a cracked part with a segregated part to produce a dark color (for example, black) eluted element or a compound of the eluted element.
- what is necessary is just to set it as the holding time normally used about the etching liquid to be used about the holding time after an inspection surface is immersed in etching liquid until it images.
- a normal part (non-defect part) is set to bright brightness
- a defect part such as a segregation part is set to dark brightness
- a defect is detected by a brightness difference (contrast difference) between the normal part and the defect part. Therefore, it is necessary to make the normal part bright.
- the lightness of the defective portion can be a dark dark color
- sufficient lightness can be ensured by making the normal portion a normal polished surface.
- polishing may be performed using a polishing means having a roughness of 1000 or less and 100 or more as specified in JIS R6252 (2006). Thereby, the roughness of an inspection surface can be made into suitable roughness.
- the direction of polishing need not be particularly limited.
- the polishing means any of polishing paper, polishing cloth, and polishing material may be used.
- the illumination that illuminates the polished surface for imaging There is no particular limitation on the illumination that illuminates the polished surface for imaging. It is only necessary to ensure the brightness necessary for imaging with the imaging device.
- the inspection surface is observed from the imaging device and it is assumed that the inspection surface is a mirror surface, it is preferable to avoid a position where the illumination light source is reflected on the inspection surface to be observed. This is because even if the inspection surface is an irregular reflection surface, the etching liquid surface on the inspection surface is a regular reflection surface, and the image of the light source is reflected on the liquid surface and reflected in the captured image.
- any film camera or digital camera can be used as long as the imaging device can image the inspection surface. It is preferable to use an imaging device using a semiconductor imaging device or the like because captured image data can be taken into an image processing device and image analysis of a defective portion can be performed.
- FIG. 4 it is preferable to arrange the imaging device 12 vertically above the geometric center C of the inspection surface 2. In this case, under the condition that the height of the light source is the same as the height of the imaging device, an area 14 having a width and length twice that of the inspection surface 2 is assumed as the arrangement position of the light source 13. If the light source 13 is arranged outside the region 14 with the geometric center of the image pickup device 12, the light directly reflected by the light source is not reflected on the inspection surface portion in the picked-up image.
- the metal sample 1 is washed to remove the etching solution from the inspection surface 2.
- the element normally contained in the metal during the etching behaves as an eluting element.
- An elemental compound is generated and acts to darken the brightness of the normal part. If the brightness of the normal part becomes too dark, it becomes difficult to recognize a brightness difference from a defect part such as a segregation part.
- the metal sample is carbon steel, when the carbon concentration in the steel is 0.5% by mass or less, the brightness of the normal part is not so dark, and the present invention can be suitably used.
- the present invention was applied to three types of carbon steel having the components shown in Table 1 as three levels of carbon steel having different carbon concentrations.
- Continuous cast slabs (width: 1200 mm, thickness: 250 mm, length: 5000 mm) of each steel type are cut perpendicularly in the length direction (casting direction) to cut out a metal sample having a length direction of 50 mm and further divided into two in the width direction.
- a metal sample 1 of 600 mm ⁇ 250 mm ⁇ 50 mm was cut out, and a vertical cross section with respect to the length direction of the continuous cast slab was set as an inspection surface 2 (size: 600 mm ⁇ 250 mm).
- the inspection surface 2 was polished using No. 300 polishing paper defined in JIS R6252. Polishing was performed in a random direction without being aware of the polishing direction.
- FIG. 2A and FIG. 2B As a method of holding the etching solution on the upper surface of the inspection surface, mainly using a method of immersing a metal sample in the etching solution in the etching container 10 as shown in FIGS. 2A and 2B, as shown in FIG.
- An etching solution outflow prevention plate 11 is installed around the inspection surface 2 of the metal sample 1 and only one example is adopted in which the etching solution 5 is poured into a frame formed by the inspection surface 2 and the etching solution outflow prevention plate 11.
- An etching solution was supplied after using a 10% aqueous solution of ammonium persulfate as the etching solution 5 and placing the metal sample 1 in the etching container 10. In the method shown in FIG. 2A and FIG.
- a scale is installed on the inner side surface of the etching container 10 to measure the thickness of the etching solution in a portion where the metal sample 1 is not present in the etching container, and the measurement is performed in advance.
- the thickness H of the etching solution at the upper part of the inspection surface was evaluated by subtracting the metal sample thickness. No measured value was obtained for the thickness H when the inspection surface was not wet.
- a digital single-lens reflex camera (imaging screen size: 22.3 mm ⁇ 14.9 mm, effective pixels: about 15.1 million pixels, lens: focal length 28 mm), as shown in FIG. It was installed at a position 1.5 m above the geometric center C). Further, as a light source 13 for illumination, as shown in FIG. 7, a bulb with a rated power consumption of 500 W is formed at four corners of a square (1.5 m ⁇ 1.5 m) parallel to the inspection surface 2 with the position of the imaging device 12 as the center of gravity. Four were arranged.
- the region 14 which is not preferable as the arrangement position of the light source 13 is in a range of 1.2 m ⁇ 0.5 m, all the light sources 13 are arranged outside the range of the region 14, and the region of the inspection surface of the captured image is The reflected image of the light source is not reflected.
- Table 2 shows processing conditions and evaluation results.
- Examples 1 to 6 and Comparative Examples 1 to 5 are cases where the method shown in FIGS. 2A and 2B is used, and Example 7 is a case where the method shown in FIG. 3 is used. Conditions that deviate from the scope of the present invention are underlined.
- the temperature of the etching solution and the metal sample was room temperature.
- the captured image captured by the imaging device was subjected to image analysis, the brightness threshold value was set, the image was binarized, and the black portion after binarization was determined to be a defect.
- the number of defects on the inspection surface 2 was counted.
- the number of defects evaluated was normalized with the number of defects evaluated in Comparative Example 1, and for Example 5 and Comparative Example 4, the evaluated number of defects was compared with Comparative Example 4.
- the number of defects evaluated was normalized with the number of defects evaluated in Comparative Example 5 for Example 6 and Comparative Example 5, and the number of defects NNL in each condition was calculated. From this NNL, the inspection status was evaluated according to the following criteria and entered in Table 2.
- Example 1 and Comparative Example 1 are obtained by changing the imaging timing of the inspection surface 2 on the basis of Comparative Example 1. Comparative Example 1 imaged after removing the etching solution had a result of “inferior”, but Example 1 imaged before removing the etching solution had a result of “pretty good”.
- Examples 1 to 4 and Comparative Examples 2 and 3 were obtained by changing the wetness of the inspection surface and the etching solution and the thickness of the etching solution held on the inspection surface with reference to Example 1. If the inspection surface is wetted with the etching solution and the thickness H of the etching solution is 10 mm or less, a good evaluation result can be obtained. Also, good results could be obtained for Example 7 using the method shown in FIG.
- Comparative Examples 1, 4, and 5 are the same as Comparative Example 1 as the standard, and the steel types are changed.
- Example 1 is the same as the standard, and the steel type is changed.
- the carbon content in the metal material exceeds 0.50%, the evaluation result decreases to “good but slightly inferior”.
- the present invention is not limited to the embodiments specifically described in the above-described embodiments and examples, and can be modified within the scope defined in the claims.
- the present invention is also applicable to the case of configuring a method for detecting a defective portion in a metal of the present invention, in particular, a steel piece, with high accuracy and speed by combining one or all of the above embodiments, examples and modifications. Is included in the scope of rights.
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Abstract
Description
本願は、2013年4月17日に、日本に出願された特願2013-086496号に基づき優先権を主張し、その内容をここに援用する。
(1)本発明の第一の態様は、金属試料の検査面を上向きにして、前記検査面の全面がエッチング液で覆われるように前記検査面の上部にエッチング液を保持して欠陥を現出させ、前記検査面の上部の前記エッチング液の厚みを0mm超10mm以下とし、この状態で撮像装置によって前記検査面を撮像する金属の欠陥検出方法である。
(2)上記(1)に記載の金属の欠陥検出方法では、前記エッチング液の中に前記金属試料を浸漬させてもよい。
(3)上記(1)又は(2)に記載の金属の欠陥検出方法では、前記金属試料が、炭素濃度が0.5質量%以下の鋼であってもよい。
1.6<NNL ・・・かなり良い
1.3<NNL≦1.6 ・・・良い
1.0<NNL≦1.3 ・・・良いが少し劣る
0.7<NNL≦1.0 ・・・劣る
NNL≦0.7 ・・・かなり劣る
2 検査面
3 偏析部
4 正常部
5 エッチング液
7 エッチング液の流れ
8 溶出元素もしくは溶出元素の化合物
9 窪み
10 エッチング用容器
11 エッチング液流出防止板
12 撮像装置
13 光源
14 領域
Claims (3)
- 金属試料の検査面を上向きにして、前記検査面の全面がエッチング液で覆われるように前記検査面の上部にエッチング液を保持して欠陥を現出させ、前記検査面の上部の前記エッチング液の厚みを0mm超10mm以下とし、この状態で撮像装置によって前記検査面を撮像する
ことを特徴とする金属の欠陥検出方法。 - 前記エッチング液の中に前記金属試料を浸漬させる
ことを特徴とする請求項1に記載の金属の欠陥検出方法。 - 前記金属試料が、炭素濃度が0.5質量%以下の鋼である
ことを特徴とする請求項1又は2に記載の金属の欠陥検出方法。
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JP2015512450A JP5904304B2 (ja) | 2013-04-17 | 2014-04-07 | 金属の欠陥検出方法 |
BR112015025556-6A BR112015025556B1 (pt) | 2013-04-17 | 2014-04-07 | Método de inspeção de defeito de metal |
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JP2013-086496 | 2013-04-17 | ||
JP2013086496 | 2013-04-17 |
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Cited By (4)
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KR20190006800A (ko) * | 2017-07-11 | 2019-01-21 | 현대자동차주식회사 | 차체의 변형 검증시스템, 및 그 제어방법 |
JP2019066189A (ja) * | 2017-09-28 | 2019-04-25 | 新日鐵住金株式会社 | 鋳片分析装置、鋳片分析方法及びプログラム |
CN112147142A (zh) * | 2020-09-23 | 2020-12-29 | 中国航发贵州黎阳航空动力有限公司 | 一种用检测液提高零件衬度的检测方法及检测液制备方法 |
JP2021085536A (ja) * | 2019-11-25 | 2021-06-03 | リンナイ株式会社 | キッチンシステム及びその設置方法 |
Families Citing this family (1)
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CN113406294B (zh) * | 2021-06-30 | 2022-02-18 | 江苏汉诺威铸业有限公司 | 一种金属铸造件表面检测装备 |
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JP2011220810A (ja) * | 2010-04-08 | 2011-11-04 | Nippon Steel Corp | 金属の欠陥検出方法及び欠陥検出装置 |
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- 2014-04-07 JP JP2015512450A patent/JP5904304B2/ja active Active
- 2014-04-07 WO PCT/JP2014/060117 patent/WO2014171361A1/ja active Application Filing
- 2014-04-07 BR BR112015025556-6A patent/BR112015025556B1/pt active IP Right Grant
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JPH0560743A (ja) * | 1991-09-04 | 1993-03-12 | Mitsubishi Heavy Ind Ltd | 鉄鋼材料の疲労損傷検出方法 |
JP2008210947A (ja) * | 2007-02-26 | 2008-09-11 | Japan Aerospace Exploration Agency | 半導体基板の評価方法 |
JP2011220810A (ja) * | 2010-04-08 | 2011-11-04 | Nippon Steel Corp | 金属の欠陥検出方法及び欠陥検出装置 |
Cited By (7)
Publication number | Priority date | Publication date | Assignee | Title |
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KR20190006800A (ko) * | 2017-07-11 | 2019-01-21 | 현대자동차주식회사 | 차체의 변형 검증시스템, 및 그 제어방법 |
KR102310422B1 (ko) | 2017-07-11 | 2021-10-07 | 현대자동차 주식회사 | 차체의 변형 검증시스템, 및 그 제어방법 |
JP2019066189A (ja) * | 2017-09-28 | 2019-04-25 | 新日鐵住金株式会社 | 鋳片分析装置、鋳片分析方法及びプログラム |
JP2021085536A (ja) * | 2019-11-25 | 2021-06-03 | リンナイ株式会社 | キッチンシステム及びその設置方法 |
JP7417406B2 (ja) | 2019-11-25 | 2024-01-18 | リンナイ株式会社 | キッチンシステムの設置方法 |
CN112147142A (zh) * | 2020-09-23 | 2020-12-29 | 中国航发贵州黎阳航空动力有限公司 | 一种用检测液提高零件衬度的检测方法及检测液制备方法 |
CN112147142B (zh) * | 2020-09-23 | 2023-10-27 | 中国航发贵州黎阳航空动力有限公司 | 一种用检测液提高零件衬度的检测方法及检测液制备方法 |
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JPWO2014171361A1 (ja) | 2017-02-23 |
BR112015025556A2 (pt) | 2017-07-18 |
JP5904304B2 (ja) | 2016-04-13 |
BR112015025556B1 (pt) | 2021-12-14 |
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