KR101677384B1 - Method of Analyzing Anti-Fingerprinting Resin Coated Galvanized Steel Sheet - Google Patents
Method of Analyzing Anti-Fingerprinting Resin Coated Galvanized Steel Sheet Download PDFInfo
- Publication number
- KR101677384B1 KR101677384B1 KR1020150113084A KR20150113084A KR101677384B1 KR 101677384 B1 KR101677384 B1 KR 101677384B1 KR 1020150113084 A KR1020150113084 A KR 1020150113084A KR 20150113084 A KR20150113084 A KR 20150113084A KR 101677384 B1 KR101677384 B1 KR 101677384B1
- Authority
- KR
- South Korea
- Prior art keywords
- steel sheet
- resin layer
- zinc
- layer
- resin
- Prior art date
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- 239000011347 resin Substances 0.000 title claims abstract description 94
- 229920005989 resin Polymers 0.000 title claims abstract description 94
- 238000000034 method Methods 0.000 title claims abstract description 17
- 229910001335 Galvanized steel Inorganic materials 0.000 title claims abstract description 16
- 239000008397 galvanized steel Substances 0.000 title claims abstract description 16
- HCHKCACWOHOZIP-UHFFFAOYSA-N Zinc Chemical compound [Zn] HCHKCACWOHOZIP-UHFFFAOYSA-N 0.000 claims description 65
- 239000011701 zinc Substances 0.000 claims description 65
- 229910052725 zinc Inorganic materials 0.000 claims description 65
- VEXZGXHMUGYJMC-UHFFFAOYSA-N Hydrochloric acid Chemical compound Cl VEXZGXHMUGYJMC-UHFFFAOYSA-N 0.000 claims description 36
- 229910000831 Steel Inorganic materials 0.000 claims description 32
- 239000010959 steel Substances 0.000 claims description 32
- HEMHJVSKTPXQMS-UHFFFAOYSA-M Sodium hydroxide Chemical compound [OH-].[Na+] HEMHJVSKTPXQMS-UHFFFAOYSA-M 0.000 claims description 30
- VKYKSIONXSXAKP-UHFFFAOYSA-N hexamethylenetetramine Chemical compound C1N(C2)CN3CN1CN2C3 VKYKSIONXSXAKP-UHFFFAOYSA-N 0.000 claims description 27
- 238000007747 plating Methods 0.000 claims description 19
- 235000010299 hexamethylene tetramine Nutrition 0.000 claims description 13
- 239000004312 hexamethylene tetramine Substances 0.000 claims description 13
- 229960004011 methenamine Drugs 0.000 claims description 13
- 238000004090 dissolution Methods 0.000 claims description 10
- KCXVZYZYPLLWCC-UHFFFAOYSA-N EDTA Chemical compound OC(=O)CN(CC(O)=O)CCN(CC(O)=O)CC(O)=O KCXVZYZYPLLWCC-UHFFFAOYSA-N 0.000 claims description 6
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims description 5
- 239000002253 acid Substances 0.000 claims description 4
- 239000000126 substance Substances 0.000 claims description 4
- PIICEJLVQHRZGT-UHFFFAOYSA-N Ethylenediamine Chemical compound NCCN PIICEJLVQHRZGT-UHFFFAOYSA-N 0.000 claims description 3
- 238000007598 dipping method Methods 0.000 claims description 2
- 230000008021 deposition Effects 0.000 abstract description 7
- 239000010410 layer Substances 0.000 description 92
- XEEYBQQBJWHFJM-UHFFFAOYSA-N Iron Chemical compound [Fe] XEEYBQQBJWHFJM-UHFFFAOYSA-N 0.000 description 9
- 238000004458 analytical method Methods 0.000 description 8
- 229960001484 edetic acid Drugs 0.000 description 5
- 230000000052 comparative effect Effects 0.000 description 4
- CWYNVVGOOAEACU-UHFFFAOYSA-N Fe2+ Chemical compound [Fe+2] CWYNVVGOOAEACU-UHFFFAOYSA-N 0.000 description 3
- 229910052742 iron Inorganic materials 0.000 description 3
- UQSXHKLRYXJYBZ-UHFFFAOYSA-N Iron oxide Chemical compound [Fe]=O UQSXHKLRYXJYBZ-UHFFFAOYSA-N 0.000 description 2
- 239000000654 additive Substances 0.000 description 2
- 239000003513 alkali Substances 0.000 description 2
- 230000002950 deficient Effects 0.000 description 2
- 239000002184 metal Substances 0.000 description 2
- 229910052751 metal Inorganic materials 0.000 description 2
- 150000007513 acids Chemical class 0.000 description 1
- 239000002738 chelating agent Substances 0.000 description 1
- 239000003153 chemical reaction reagent Substances 0.000 description 1
- 239000011247 coating layer Substances 0.000 description 1
- 150000001875 compounds Chemical class 0.000 description 1
- 238000007796 conventional method Methods 0.000 description 1
- 238000005260 corrosion Methods 0.000 description 1
- 230000007797 corrosion Effects 0.000 description 1
- 230000003111 delayed effect Effects 0.000 description 1
- 238000004519 manufacturing process Methods 0.000 description 1
- 239000000463 material Substances 0.000 description 1
- 238000005259 measurement Methods 0.000 description 1
- 150000002739 metals Chemical class 0.000 description 1
- 230000003647 oxidation Effects 0.000 description 1
- 238000007254 oxidation reaction Methods 0.000 description 1
- 238000007670 refining Methods 0.000 description 1
- 150000003839 salts Chemical class 0.000 description 1
- 238000001878 scanning electron micrograph Methods 0.000 description 1
- 238000000926 separation method Methods 0.000 description 1
- 238000005406 washing Methods 0.000 description 1
- 238000005303 weighing Methods 0.000 description 1
Images
Classifications
-
- G—PHYSICS
- G01—MEASURING; TESTING
- G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
- G01N5/00—Analysing materials by weighing, e.g. weighing small particles separated from a gas or liquid
-
- 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
-
- 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
-
- 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
- G01N33/44—Resins; Plastics; Rubber; Leather
- G01N33/442—Resins; Plastics
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- Chemical & Material Sciences (AREA)
- Health & Medical Sciences (AREA)
- Life Sciences & Earth Sciences (AREA)
- General Health & Medical Sciences (AREA)
- Analytical Chemistry (AREA)
- Biochemistry (AREA)
- Physics & Mathematics (AREA)
- General Physics & Mathematics (AREA)
- Immunology (AREA)
- Pathology (AREA)
- Engineering & Computer Science (AREA)
- Food Science & Technology (AREA)
- Medicinal Chemistry (AREA)
- Investigating And Analyzing Materials By Characteristic Methods (AREA)
- Sampling And Sample Adjustment (AREA)
Abstract
Description
The present invention relates to a method of analyzing the adhesion amount of an inner fingerprint resin layer and a plating layer of a zinc plated steel sheet including a resin layer and more particularly to a method of analyzing the adhesion amount of a resin layer and a plating layer of an inner fingerprint resin zinc- And the like.
Conventionally, in order to analyze the adhesion amount of the resin layer of the inner fingerprint resin galvanized steel sheet, the inner fingerprint resin galvanized steel sheet to be analyzed is immersed in an HCl solution (hydrochloric acid 1: water: 3) The separated resin layer was filtered, dried and weighed with a weighing machine to analyze the adhesion amount of the resin layer.
However, in the conventional analysis method, when the inner fingerprint resin galvanized steel sheet is immersed in the HCl solution and the resin layer of the inner fingerprint resin zinc coated steel sheet is dissolved and separated, not only the resin layer but also the zinc plating layer is dissolved. It is impossible to analyze the adhesion amounts of the resin layer and the zinc plating layer at the same time. Therefore, at least two samples are required to analyze the adhesion amount of the resin layer and the zinc plating layer of the inner fingerprint resin zinc plated steel sheet.
Also, as shown in FIG. 1, there is a disadvantage in that analysis errors are generated because the samples have different amounts of adhesion between the resin layer and the zinc plating layer.
Further, in the conventional analysis method, since only the resin layer is not dissolved and the zinc plating layer is dissolved, it is difficult to analyze the foreign substance contained in the zinc plating layer.
A preferred aspect of the present invention is to provide a method of analyzing the adhesion amount of the resin layer and the coating layer deposition amount of the inner fingerprint resin zinc-plated steel sheet as one sample.
Another aspect of the present invention is to provide a method for analyzing the adhesion amount of the resin layer, the deposition amount of the plating layer, and the foreign substance in the plating layer of the inner fingerprint resin zinc-plated steel sheet as one sample.
According to a preferred aspect of the present invention, there is provided a method of manufacturing a zinc fingerprint zinc plated steel sheet, comprising: preparing an inner fingerprint zinc plated steel sheet including a resin layer and a zinc plated layer;
The above fingerprint resin galvanized steel sheet was immersed in a solution of a resin layer in which 5 to 30 ppm of Ethylene Diamine Tertraacetic Acid and 20 to 100 ppm of hexamethylene tetramine were mixed in a NaOH solution Dissolving and removing the resin layer of the inner fingerprint resin zinc-coated steel sheet;
Measuring the weight of the galvanized steel sheet from which the resin layer has been removed;
Obtaining an adhesion amount of the resin layer using the weight of the zinc-plated steel sheet before and after the removal of the resin layer;
Dipping the zinc plated steel sheet from which the resin layer has been removed as described above into a hydrochloric acid solution to dissolve and remove the zinc plated layer;
Measuring the weight of the steel sheet from which the zinc plated layer has been removed as described above;
And a step of obtaining an adhesion amount of the zinc plated layer by using the weight of the zinc plated steel sheet before the removal of the zinc plated layer and the weight of the steel sheet from which the zinc plated layer has been removed.
The present invention further relates to a method of analyzing an inner fingerprint resin galvanized steel sheet, which further comprises the step of analyzing a foreign substance contained in the zinc plating layer prior to the step of dissolving and removing the zinc plating layer.
According to a preferred aspect of the present invention, since only the resin layer is dissolved, the adhesion amount of the resin layer can be analyzed precisely and accurately, and furthermore, the foreign matter component in the plating layer below the resin layer can be accurately analyzed, , The analysis time can be shortened.
BRIEF DESCRIPTION OF DRAWINGS FIG. 1 is a cross-sectional photograph of an example of two zinc fingerprinted resin-coated steel sheet samples including a resin layer and a zinc plated layer.
According to a preferred aspect of the present invention, the adhesion amount of the resin layer and the zinc plating layer of the inner fingerprint resin zinc-plated steel sheet including the resin layer and the zinc plating layer can be analyzed as one sample.
An example of two inner fingerprint resin galvanized steel sheet samples including a resin layer and a zinc plated layer is shown in Fig.
As shown in FIG. 1, the adhesion amounts of the resin layer and the zinc plated layer are different from each other in the two samples. Therefore, according to the conventional method, at least two samples must be used, resulting in an analysis error.
In the present invention, since one sample is used, the analysis error described above can not be generated.
In the present invention, the inner fingerprint resin galvanized steel sheet is immersed in a resin layer dissolving solution to dissolve and remove the resin layer of the inner fingerprint resin zinc coated steel sheet.
The resin layer dissolving solution used herein is preferably a resin layer dissolving solution in which 5 to 30 ppm of ethylene diamine tetraacetic acid and 10 to 100 ppm of hexamethylene tetramine are mixed in an NaOH solution .
The NaOH is a component for dissolving the fingerprint resin layer, and it is preferable to use a 3 to 10% NaOH solution, more preferably a 4 to 6% NaOH solution, more preferably a 5% NaOH solution .
Ethylene Diamine Tertraacetic Acid is a component which forms a metal salt (chelator compound) to protect metals from acids and alkali. When the content is less than 5 ppm, there is a fear that the zinc adhered amount is peeled off If the concentration exceeds 30 ppm, washing may not be performed well and the consumption of the reagent may be large, resulting in an increase in cost. The amount of the ethylenediaminetetraacetic acid to be added is preferably 5 to 20 ppm in consideration of separation of the zinc adhered amount and cost.
The hexamethylenetetramine is a component for preventing the oxidation or corrosion of the ferrous iron. When the content of the hexamethylenetetraamine is less than 20 ppm, it is difficult to protect the ferrous iron from the alkali iron or hydrochloric acid. When the content exceeds 100 ppm, It is preferable to limit the content to 20 ~ 100ppm because it may be difficult to clean the surface of iron or zinc.
The mixing amount of the hexamethylene tetramine is more preferably limited to 40 to 90 ppm in consideration of the refining iron and the cost.
The temperature of the resin layer dissolving solution is preferably, for example, 25 to 60 ° C, and more preferably, the temperature of the resin layer dissolving solution is 40 to 60 ° C.
If the temperature of the resin layer dissolving solution is too low, the peeling may be delayed. If the temperature is too high, peeling may occur too quickly, and the workability may deteriorate.
The resin layer dissolution time may vary depending on the adhesion amount of the resin layer to be analyzed. For example, when the resin adhesion amount is less than 2600 mg, the resin layer dissolution time may be less than 1.5 minutes. In terms of efficiency, desirable.
The weight of the galvanized steel sheet from which the resin layer has been removed as described above is measured.
Preferably, the galvanized steel sheet from which the resin layer has been removed as described above is washed and dried, and the weight is measured.
The adhesion amount of the resin layer can be analyzed by calculating the adhesion amount of the resin layer using the weight of the zinc-plated steel sheet before and after the removal of the resin layer.
The adhesion amount of the resin layer analyzed as described above may be, for example, 2600 mg or less.
In the present invention, it is also possible to analyze a trace amount of adhesion of resin layer of 100 mg or less (excluding 0).
In the present invention, since only the resin layer can be dissolved and removed, when the weight can be measured in units of not more than 100 mg, even the adhesion amount of not more than 100 mg can be analyzed.
The zinc plated steel sheet from which the resin layer has been removed as described above is immersed in a hydrochloric acid solution to dissolve and remove the zinc plated layer.
As the hydrochloric acid solution, a hydrochloric acid solution having a ratio of hydrochloric acid: water of 1: 1 to 3 is preferably used. A more preferable hydrochloric acid solution is 1 + 3 HCl (hydrochloric acid 1: water: 3) solution.
To the hydrochloric acid solution, 20 to 100 ppm of hexamethylene tetramine is preferably added to protect the iron oxide.
The weight of the steel sheet from which the zinc plated layer has been removed as described above is measured.
Preferably, the steel sheet from which the zinc-plated layer has been removed as described above is washed and dried, and then its weight is measured.
The adhesion amount of the resin layer can be analyzed by calculating the adhesion amount of the zinc plated layer using the weight of the zinc-plated steel sheet before the removal of the zinc-plated layer and the weight of the steel sheet from which the zinc-plated layer has been removed.
According to a preferred aspect of the present invention, foreign matters contained in the zinc plated layer may be analyzed prior to the step of dissolving and removing the zinc plated layer.
The foreign matter analysis can be performed by SEM image measurement, component analysis, microscopic observation, and the like.
By analyzing the foreign material, it becomes possible to identify the cause of the defective sample, and it becomes possible to identify the cause of many defective products.
Hereinafter, one aspect of the present invention will be described in more detail by way of examples.
(Example)
A resin layer dissolution solution was prepared by mixing 60 ppm of hexamethylene tetramine in 0.5% NaOH solution and mixing ethylene diamine tetraacetic acid (EDTA) as shown in Table 1 below.
A zinc fingerprinted zinc plated steel plate containing a resin layer and a zinc plated layer was immersed in the resin layer dissolving solution to dissolve the resin layer for the period of time shown in the following Table 1 and then the zinc dissolution amount of the zinc plated layer was measured And the results are shown in Table 1 below.
A solution prepared by mixing hexamethylenetetramine (Hexamethylene Tetramine) in a solution of 1 + 3 HCl (hydrochloric acid 1: water: 3) as shown in the following Table 2 was prepared. To this solution, a galvanized steel sheet And the zinc plating layer was dissolved and removed for the time shown in Table 2 below. Then, the dissolution amount of iron (Fe) was measured for each dissolution time, and the results are shown in Table 2 below.
Honor
As shown in Tables 1 and 2, in the case of Inventive Example (1-4) in accordance with the present invention, the zinc dissolution amount of the zinc plated layer and the dissolution amount of ferrous iron (Fe) (1-2). ≪ / RTI > From these results, it can be seen that according to the present invention, the adhesion of the resin layer and the zinc plating layer can be more precisely analyzed with one test piece.
Claims (9)
To the NaOH solution, 5 to 30 ppm of ethylenediamine tetraacetic acid and 20 to 100 ppm of hexamethylenetetramine (
Hexamethylene Tetramine) to dissolve and remove the resin layer of the inner fingerprint resin zinc plated steel sheet by immersing the inner fingerprint resin zinc plated steel sheet in the resin layer dissolving solution.
Measuring the weight of the galvanized steel sheet from which the resin layer has been removed;
Obtaining an adhesion amount of the resin layer using the weight of the zinc-plated steel sheet before and after the removal of the resin layer;
Dipping the zinc plated steel sheet from which the resin layer has been removed as described above into a hydrochloric acid solution to dissolve and remove the zinc plated layer;
Measuring the weight of the steel sheet from which the zinc plated layer has been removed as described above;
A method of analyzing a zinc fingerprinted zinc plated steel sheet comprising the steps of: determining the adhesion amount of the zinc plated layer by using the weight of the zinc plated steel sheet before removal of the zinc plated layer and the weight of the steel sheet from which the zinc plated layer has been removed.
Priority Applications (1)
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KR1020150113084A KR101677384B1 (en) | 2015-08-11 | 2015-08-11 | Method of Analyzing Anti-Fingerprinting Resin Coated Galvanized Steel Sheet |
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KR1020150113084A KR101677384B1 (en) | 2015-08-11 | 2015-08-11 | Method of Analyzing Anti-Fingerprinting Resin Coated Galvanized Steel Sheet |
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Citations (4)
Publication number | Priority date | Publication date | Assignee | Title |
---|---|---|---|---|
KR910004112B1 (en) * | 1988-12-28 | 1991-06-22 | 포항종합제철 주식회사 | Measuring method for the impurities layer of finger marks in the zinc galvanizing |
JPH10267918A (en) * | 1997-03-27 | 1998-10-09 | Nippon Steel Corp | Solution for chemical analysis of zinc-iron alloy group 2-layer plated steel board, and chemical analysis method using it |
JP2000146776A (en) * | 1998-11-04 | 2000-05-26 | Toray Ind Inc | Method for measuring adhesion amount of silicone-based oil agent |
KR20150007467A (en) * | 2013-07-11 | 2015-01-21 | 주식회사 포스코 | System and method for analyzing elementary in coating plate using lazer |
-
2015
- 2015-08-11 KR KR1020150113084A patent/KR101677384B1/en active IP Right Grant
Patent Citations (4)
Publication number | Priority date | Publication date | Assignee | Title |
---|---|---|---|---|
KR910004112B1 (en) * | 1988-12-28 | 1991-06-22 | 포항종합제철 주식회사 | Measuring method for the impurities layer of finger marks in the zinc galvanizing |
JPH10267918A (en) * | 1997-03-27 | 1998-10-09 | Nippon Steel Corp | Solution for chemical analysis of zinc-iron alloy group 2-layer plated steel board, and chemical analysis method using it |
JP2000146776A (en) * | 1998-11-04 | 2000-05-26 | Toray Ind Inc | Method for measuring adhesion amount of silicone-based oil agent |
KR20150007467A (en) * | 2013-07-11 | 2015-01-21 | 주식회사 포스코 | System and method for analyzing elementary in coating plate using lazer |
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