JP6112617B2 - Black skin evaluation method for steel - Google Patents
Black skin evaluation method for steel Download PDFInfo
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- JP6112617B2 JP6112617B2 JP2014102023A JP2014102023A JP6112617B2 JP 6112617 B2 JP6112617 B2 JP 6112617B2 JP 2014102023 A JP2014102023 A JP 2014102023A JP 2014102023 A JP2014102023 A JP 2014102023A JP 6112617 B2 JP6112617 B2 JP 6112617B2
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- 229910000831 Steel Inorganic materials 0.000 title claims description 80
- 239000010959 steel Substances 0.000 title claims description 80
- 238000011156 evaluation Methods 0.000 title claims description 8
- 239000000463 material Substances 0.000 claims description 66
- 229910052751 metal Inorganic materials 0.000 claims description 25
- 239000002184 metal Substances 0.000 claims description 25
- 238000007747 plating Methods 0.000 claims description 16
- 239000008151 electrolyte solution Substances 0.000 description 10
- 238000002474 experimental method Methods 0.000 description 7
- QVGXLLKOCUKJST-UHFFFAOYSA-N atomic oxygen Chemical compound [O] QVGXLLKOCUKJST-UHFFFAOYSA-N 0.000 description 5
- 229910052760 oxygen Inorganic materials 0.000 description 5
- 239000001301 oxygen Substances 0.000 description 5
- HCHKCACWOHOZIP-UHFFFAOYSA-N Zinc Chemical compound [Zn] HCHKCACWOHOZIP-UHFFFAOYSA-N 0.000 description 4
- 239000007864 aqueous solution Substances 0.000 description 4
- 238000000034 method Methods 0.000 description 4
- BASFCYQUMIYNBI-UHFFFAOYSA-N platinum Chemical compound [Pt] BASFCYQUMIYNBI-UHFFFAOYSA-N 0.000 description 4
- 239000011701 zinc Substances 0.000 description 4
- 229910052725 zinc Inorganic materials 0.000 description 4
- 238000005260 corrosion Methods 0.000 description 3
- 230000007797 corrosion Effects 0.000 description 3
- 238000010586 diagram Methods 0.000 description 3
- 239000003792 electrolyte Substances 0.000 description 3
- VEXZGXHMUGYJMC-UHFFFAOYSA-M Chloride anion Chemical compound [Cl-] VEXZGXHMUGYJMC-UHFFFAOYSA-M 0.000 description 2
- UIIMBOGNXHQVGW-UHFFFAOYSA-M Sodium bicarbonate Chemical compound [Na+].OC([O-])=O UIIMBOGNXHQVGW-UHFFFAOYSA-M 0.000 description 2
- 238000011835 investigation Methods 0.000 description 2
- 238000013507 mapping Methods 0.000 description 2
- 229910021645 metal ion Inorganic materials 0.000 description 2
- 229910000975 Carbon steel Inorganic materials 0.000 description 1
- 229910000676 Si alloy Inorganic materials 0.000 description 1
- 229910021607 Silver chloride Inorganic materials 0.000 description 1
- PTFCDOFLOPIGGS-UHFFFAOYSA-N Zinc dication Chemical compound [Zn+2] PTFCDOFLOPIGGS-UHFFFAOYSA-N 0.000 description 1
- SOIFLUNRINLCBN-UHFFFAOYSA-N ammonium thiocyanate Chemical compound [NH4+].[S-]C#N SOIFLUNRINLCBN-UHFFFAOYSA-N 0.000 description 1
- 239000010962 carbon steel Substances 0.000 description 1
- GTKRFUAGOKINCA-UHFFFAOYSA-M chlorosilver;silver Chemical compound [Ag].[Ag]Cl GTKRFUAGOKINCA-UHFFFAOYSA-M 0.000 description 1
- 239000000470 constituent Substances 0.000 description 1
- 230000007423 decrease Effects 0.000 description 1
- 230000000694 effects Effects 0.000 description 1
- 238000010894 electron beam technology Methods 0.000 description 1
- 238000004299 exfoliation Methods 0.000 description 1
- 238000010438 heat treatment Methods 0.000 description 1
- 230000001678 irradiating effect Effects 0.000 description 1
- 238000005259 measurement Methods 0.000 description 1
- 238000001000 micrograph Methods 0.000 description 1
- 230000003287 optical effect Effects 0.000 description 1
- 229910052697 platinum Inorganic materials 0.000 description 1
- 239000011150 reinforced concrete Substances 0.000 description 1
- 230000000717 retained effect Effects 0.000 description 1
- 239000000523 sample Substances 0.000 description 1
- 238000000926 separation method Methods 0.000 description 1
- HKZLPVFGJNLROG-UHFFFAOYSA-M silver monochloride Chemical compound [Cl-].[Ag+] HKZLPVFGJNLROG-UHFFFAOYSA-M 0.000 description 1
- 229910000030 sodium bicarbonate Inorganic materials 0.000 description 1
- 235000017557 sodium bicarbonate Nutrition 0.000 description 1
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 description 1
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- Investigating And Analyzing Materials By Characteristic Methods (AREA)
Description
本発明は、鋼材の表面に形成される黒皮の評価方法に関するものである。 The present invention relates to a method for evaluating a black skin formed on the surface of a steel material.
鉄筋コンクリートなどに実際に用いられる鋼材の表面には、熱処理工程をしたときに黒皮と呼ばれる酸化膜が形成されている。この黒皮は製造者によって厚みや均一性が異なり、必ずしも制御されているわけではない（例えば、非特許文献１参照。）。黒皮と鋼材は互いに結合する強度が弱いので、黒皮が鋼材から剥離することがある。黒皮の一部または全部が剥離した鋼材表面の部分（以下、「剥離部」と言う。）から鋼材内に塩化物イオンを含む水が侵入すると、鋼材の腐食が促進する可能性があることが知られている（例えば、非特許文献２参照。）。そこで従来より、黒皮の剥離の有無を調べることが行われている。黒皮の剥離の有無は肉眼や光学顕微鏡でも調べることができるが、より正確に調べる場合には高倍率での観察が可能な電子顕微鏡が用いられている。 An oxide film called black skin is formed on the surface of a steel material actually used for reinforced concrete or the like when a heat treatment process is performed. This black skin differs in thickness and uniformity depending on the manufacturer, and is not necessarily controlled (see, for example, Non-Patent Document 1). Since the strength of the black skin and the steel material is low, the black skin may peel off from the steel material. If water containing chloride ions enters the steel from a part of the steel surface from which part or all of the skin is peeled (hereinafter referred to as “peeled part”), corrosion of the steel may be accelerated. Is known (for example, see Non-Patent Document 2). Therefore, conventionally, the presence or absence of peeling of the black skin has been examined. The presence or absence of peeling of the black skin can be examined with the naked eye or an optical microscope, but an electron microscope capable of observation at a high magnification is used for more accurate examination.
しかしながら、電子顕微鏡で鋼材を観察すると、電子顕微鏡による画像上では黒皮に覆われた部分と剥離部とでは導電性の違いによるコントラストが小さいので、剥離部を正確に識別することが困難であった。 However, when the steel material is observed with an electron microscope, it is difficult to accurately identify the peeled portion because the contrast due to the difference in conductivity between the portion covered with the black skin and the peeled portion is small on the electron microscope image. It was.
そこで、本発明は、黒皮の剥離部分をより正確に識別することができる鋼材の黒皮評価方法を提供することを目的とする。 Then, an object of this invention is to provide the black skin evaluation method of the steel material which can identify the peeling part of a black skin more correctly.
上述したような課題を解決するために、本発明に係る鋼材の黒皮評価方法は、黒皮が形成された鋼材の黒皮が剥離した部分に金属をめっきする第１のステップと、鋼材にめっきされた金属の分布を測定する第２のステップとを有することを特徴とするものである。 In order to solve the above-described problems, the steel skin black skin evaluation method according to the present invention includes a first step of plating a metal on a portion where the black skin of the steel material on which the black skin has been peeled, and the steel material. And a second step of measuring the distribution of the plated metal.
上記鋼材の黒皮評価方法において、第１のステップは、鋼材に定電流を流し、鋼材の電位が黒皮が還元される電位に達する前に終了するようにしてもよい。 In the steel skin black skin evaluation method, the first step may be performed before a constant current is passed through the steel material and before the potential of the steel material reaches a potential at which the black skin is reduced.
本発明によれば、黒皮が形成された鋼材の黒皮が剥離した部分に金属をめっきすることにより、めっきした金属と黒皮とは正確に識別できるので、剥離部分をより正確に識別することができる。 According to the present invention, the plated metal and the black skin can be accurately identified by plating the metal on the portion where the black skin of the steel material on which the black skin is formed is peeled off, so that the peeled portion is more accurately identified. be able to.
以下、図面を参照して本発明の実施の形態について詳細に説明する。図１は、本発明の実施の形態に係る鋼材の黒皮評価方法を説明するためのフローチャートである。 Hereinafter, embodiments of the present invention will be described in detail with reference to the drawings. FIG. 1 is a flowchart for explaining a black skin evaluation method for a steel material according to an embodiment of the present invention.
［鋼材の黒皮評価方法］
まず、黒皮が形成された鋼材（以下、単に「鋼材」と言う。）の黒皮が剥離した部分に金属をめっきする（ステップＳ１）。このめっきを行うときの装置構成の一例を図２に示す。この図２に示すように、鋼材にめっきを行うときには、電解液を貯留しためっき槽１と、このめっき槽１に浸漬した鋼材２、電極３および参照極４と、これらの電極に電気的に接続され、それぞれに電力を供給する制御装置５とを用意する。そして、制御装置５により、鋼材２を陰極、電極３を陽極としてこれらの間に定電流を所定の時間流す。これにより、黒皮が一部または全部剥離した鋼材１表面の剥離部に選択的に金属がめっきされる。このように剥離部に金属がめっきされる原理について、図３を参照して以下に説明する。
[Evaluation method for steel skin]
First, a metal is plated on a portion where a black skin of a steel material (hereinafter simply referred to as “steel material”) on which the black skin is formed is peeled off (step S1). An example of the apparatus configuration when performing this plating is shown in FIG. As shown in FIG. 2, when the steel material is plated, the plating tank 1 storing the electrolytic solution, the steel material 2, the electrode 3 and the reference electrode 4 immersed in the plating tank 1, and the electrodes are electrically connected. A control device 5 that is connected and supplies power to each is prepared. Then, the control device 5 uses the steel material 2 as a cathode and the electrode 3 as an anode, and a constant current flows between them for a predetermined time. Thereby, a metal is selectively plated on the peeled portion on the surface of the steel material 1 where the black skin is partially or entirely peeled off. The principle of plating the metal on the peeling portion in this way will be described below with reference to FIG.
＜剥離部に金属がめっきされる原理＞
電解液中に鋼材と電極を浸漬し、鋼材に定電流が流れるように電流制御を行ったとき、図３に示すように、電解液側から鋼材１１に流れる定電流Ｉは、鋼材１１の表面に形成された黒皮１２から鋼材１１に流れる電流Ｉscaleと、剥離部１３によって電解液中に露出した部分の鋼材１１に流れるＩmetalの和で表すことができる。なお、図３に示す矢印は、鋼材表面の電流密度分布を模式的に示すものであり、矢印が大きいほど大きな電流が流れることを意味している。
<Principle that metal is plated on the peeling part>
When current control is performed so that a constant current flows in the steel material by immersing the steel material and the electrode in the electrolytic solution, the constant current I flowing from the electrolyte side to the steel material 11 is the surface of the steel material 11 as shown in FIG. The current I scale flowing from the black skin 12 to the steel material 11 and the I metal flowing in the steel material 11 in the portion exposed to the electrolytic solution by the peeling portion 13 can be expressed as In addition, the arrow shown in FIG. 3 shows the current density distribution on the steel material surface schematically, and means that a larger current flows as the arrow becomes larger.
ここで、黒皮１２の電気抵抗は、鋼材１１の電気抵抗よりも大きい。
このため、剥離部１３によって電解液中に露出した鋼材１１には、図３中の大きな矢印で示すように、大きな電流が流れる。一方、黒皮１２は、図３中の小さな矢印で示すように、小さな電流しか流れない。
また、剥離部１３によって電解液中に露出した部分の鋼材１１と電解液との界面には、黒皮１２の部分と比較して、相対的に大きな電位差が生じる。
したがって、めっきする金属イオンが溶解した電解液中に鋼材と電極を浸漬し、鋼材に定電流が流れるように電流制御すると、剥離部によって電解液中に露出した部分の鋼材には、大きな電流が流れ、かつ、電解液との界面の電位差が大きいので、金属が選択的にめっきされることとなる。
Here, the electric resistance of the black skin 12 is larger than the electric resistance of the steel material 11.
For this reason, a large current flows through the steel material 11 exposed in the electrolytic solution by the peeling portion 13 as indicated by a large arrow in FIG. On the other hand, the black skin 12 flows only a small current as indicated by a small arrow in FIG.
In addition, a relatively large potential difference is generated at the interface between the steel material 11 and the electrolytic solution at a portion exposed in the electrolytic solution by the peeling portion 13 as compared with the portion of the black skin 12.
Therefore, if the steel material and the electrode are immersed in an electrolytic solution in which the metal ions to be plated are dissolved, and the current is controlled so that a constant current flows through the steel material, a large current is applied to the steel material exposed to the electrolytic solution by the peeling portion. Since the potential difference between the flow and the interface with the electrolytic solution is large, the metal is selectively plated.
鋼材にめっきする金属は、例えば亜鉛など、黒皮の還元電位よりも低い電位で還元される金属からなる。なお、亜鉛を鋼材の剥離部にめっきする場合には、亜鉛イオンが溶解した電解液中に鋼材と白金からなる電極を浸漬し、これらの間に定電流を所定の時間流せばよい。このとき、電解質中に鋼材と亜鉛からなる電極とを浸漬して、これらの間に定電流を所定の時間流すことにより鋼材の剥離部に亜鉛をめっきするようにしてもよいことは言うまでもない。 The metal plated on the steel material is a metal that is reduced at a potential lower than the reduction potential of the black skin, such as zinc. In addition, when plating zinc on the peeling part of steel materials, the electrode which consists of steel materials and platinum may be immersed in the electrolyte solution which zinc ion melt | dissolved, and a constant current should just flow through these for the predetermined time. At this time, it goes without saying that the steel material and the electrode made of zinc may be immersed in the electrolyte, and zinc may be plated on the peeled portion of the steel material by flowing a constant current between them for a predetermined time.
鋼材にめっきするときに鋼材に流す定電流の値および電流を流す時間は、適宜自由に設定することができる。
なお、鋼材にめっきをし続けると、黒皮表面にも金属がめっきされるので、黒皮と剥離部とが識別できなくなるのを防ぐために、黒皮表面に金属がめっきされる前にめっきを終了することが望ましい。黒皮表面に金属がめっきされないようにするには、例えば、鋼材にめっきするときに流す電流の値および電流を流す時間を、黒皮が保持される値、すなわち黒皮が還元されない値に設定することにより実現することができる。この値は、めっきするときに実際に流す定電流を鋼材に流して黒皮を還元させる実験を行って、黒皮が還元されずに保持される電位を予め求めておき、この求めた電位に基づいて設定すればよい。その実験の一例を以下に説明する。
The value of the constant current that flows through the steel material when the steel material is plated and the time during which the current flows can be set as appropriate.
If the steel is continuously plated, metal is also plated on the black skin surface, so in order to prevent the black skin and the peeled portion from being indistinguishable, plating must be performed before the metal is plated on the black skin surface. It is desirable to end. In order to prevent metal from being plated on the black skin surface, for example, the current value and the current flow time when plating on steel are set to values at which the black skin is retained, that is, the black skin is not reduced. This can be realized. This value is obtained by conducting an experiment to reduce the black skin by flowing a constant current that is actually passed through the steel material when plating, and obtaining a potential at which the black skin is held without being reduced beforehand. It may be set based on. An example of the experiment will be described below.
＜黒皮が還元される電位を求める実験＞
この実験では、１ｗｔ％のチオシアン酸アンモニウム（ＮＨ4ＳＣＮ）を添加した１Ｍ（モル）の炭酸水素ナトリウム（ＮａＨＣＯ3）水溶液を脱気した溶液中に、作用極として直径φが９ｍｍの一般的な高強度鋼（Ｆｅ−０．２５％Ｓｉ合金など）からなる鋼材、参照極としてとして銀−塩化銀（Ａｇ／ＡｇＣｌ）電極、対極として白金線（Ｐｔ）を挿入し、鋼材に１０［μＡ／ｃｍ2］の電流密度の定電流が流れるようにした。このときに得られた鋼材の電位の時間変化を図４に示す。
<Experiment to find potential to reduce black skin>
In this experiment, a 1M (mol) aqueous solution of sodium bicarbonate (NaHCO 3 ) added with 1 wt% ammonium thiocyanate (NH 4 SCN) was degassed, and a general diameter of 9 mm as a working electrode was used. A steel material made of high-strength steel (Fe-0.25% Si alloy, etc.), a silver-silver chloride (Ag / AgCl) electrode as a reference electrode, and a platinum wire (Pt) as a counter electrode, and 10 [μA / A constant current with a current density of cm 2 ] was allowed to flow. FIG. 4 shows the time change of the electric potential of the steel material obtained at this time.
図４に示す実線は、鋼材の電位の時間変化を示す。この実線から分かるように、鋼材の電位は、鋼材に電流を流し始めてから一定の時間（図４では１８０分）まではほぼ一定の値であり、その後に低下して、この低下した値でほぼ一定に保持されている。これは、上述した水溶液中の鋼材に電流を流すと、初めに水溶液中の溶存酸素が還元され、続いて黒皮が還元されるからである。したがって、開始から１８０分までの電位は電解液中の溶存酸素が還元されているときの値であり、１８０分以降の電位は黒皮が還元されているときの値であることがわかる。そこで、この黒皮が還元されているときの電位を予め求めておく。そして、鋼材にめっきするときには、鋼材の電位を観測しながら、その実験のときと同じ定電流を鋼材に流す。そして、鋼材の電位が予め求めた黒皮が還元される電位に達する前に、鋼材に電流を流すことを停止する。これにより、黒皮の表面にめっきされるのを防ぐことができる、すなわち剥離部のみにめっきすることができる。 The solid line shown in FIG. 4 shows the time change of the potential of the steel material. As can be seen from this solid line, the electric potential of the steel material is a substantially constant value until a certain time (180 minutes in FIG. 4) after the current starts to flow through the steel material, and then decreases. Is held constant. This is because when an electric current is passed through the steel material in the aqueous solution described above, the dissolved oxygen in the aqueous solution is first reduced and then the black skin is reduced. Therefore, it can be seen that the potential from the start to 180 minutes is a value when the dissolved oxygen in the electrolyte is reduced, and the potential after 180 minutes is a value when the black skin is being reduced. Therefore, the potential when the black skin is being reduced is obtained in advance. When plating the steel material, the same constant current as in the experiment is passed through the steel material while observing the potential of the steel material. And before the electric potential of steel materials reaches the electric potential by which the black skin calculated | required previously is reduced, it stops flowing an electric current through steel materials. Thereby, it can prevent plating on the surface of a black skin, ie, it can plate only to a peeling part.
なお、上述した黒皮の還元電位を求めるための実験の際には、極力酸素を除去した水溶液を用いることが望ましい。これにより、還元される溶存酸素の量が少なくなるので、黒皮の還元が早く始まるとともに、黒皮の還元の際に溶存酸素が影響を及ぼすことを防ぐことができる。この結果、実験時間を短縮したり、電位の時間変化をより明確に検出したりすることができる。
また、測定される電位は、黒皮と剥離部の混成電位を示しているため、予め決めた金属イオン種が含まれていれば測定した電位が高くても電流を制御している間は剥離部にめっきされることとなる。
In the above-described experiment for determining the reduction potential of the black skin, it is desirable to use an aqueous solution from which oxygen is removed as much as possible. As a result, the amount of dissolved oxygen to be reduced is reduced, so that the reduction of the black skin starts early, and it is possible to prevent the dissolved oxygen from affecting the reduction of the black skin. As a result, the experiment time can be shortened, and the potential change with time can be detected more clearly.
In addition, since the measured potential indicates the mixed potential of the black skin and the peeled portion, if a predetermined metal ion species is included, the peeled off while controlling the current even if the measured potential is high. The part will be plated.
＜金属の分布の測定＞
ステップＳ１により鋼材の剥離部に金属がめっきされると、鋼材にめっきされた金属の分布を測定する（ステップＳ２）。
めっきされた金属の分布の測定には、元素マッピングの各種方法を用いることができる。例えば、電子線を対象物に照射する事により発生する特性Ｘ線の波長と強度から構成元素を分析するＥＰＭＡ（電子線マイクロアナライザ:Electron Probe MicroAnalyser）を用いることができる。
<Measurement of metal distribution>
When metal is plated on the peeled portion of the steel material in step S1, the distribution of the metal plated on the steel material is measured (step S2).
Various methods of element mapping can be used to measure the distribution of the plated metal. For example, EPMA (Electron Probe MicroAnalyser) that analyzes constituent elements from the wavelength and intensity of characteristic X-rays generated by irradiating an object with an electron beam can be used.
ステップＳ１によりめっきされた鋼材の表面は、黒皮と剥離部にめっきされた金属とから構成されている。黒皮とめっきされた金属は、黒皮と鋼材本体と比較して、導電性が大きく異なる。したがって、めっきされた鋼材に対して元素マッピングを行うと、めっきされた箇所とめっきされていない箇所との間に明確なコントラストを付けることが可能となるので、結果として、剥離部を正確に判別することができる。 The surface of the steel material plated in step S1 is composed of a black skin and a metal plated on the peeling portion. Compared with the black skin and the steel body, the conductivity is significantly different between the black skin and the plated metal. Therefore, when elemental mapping is applied to plated steel, it is possible to provide a clear contrast between the plated and unplated locations, and as a result, the separation is accurately identified. can do.
以上説明したように、本実施の形態によれば、黒皮が形成された鋼材の黒皮が剥離した部分に金属をめっきすることにより、めっきした金属と黒皮とは正確に識別できるので、結果として、剥離部分をより正確に識別することができる。 As described above, according to the present embodiment, by plating the metal on the part where the black skin of the steel material on which the black skin has been peeled, the plated metal and the black skin can be accurately identified. As a result, the peeled portion can be more accurately identified.
本発明は、黒皮が形成された鋼材を用いる各種方法に適用することができる。 The present invention can be applied to various methods using a steel material on which a black skin is formed.
１…めっき槽、２…鋼材、３…電極、４…作用極、５…制御装置、１１…鋼材、１２…黒皮、１３…剥離部。 DESCRIPTION OF SYMBOLS 1 ... Plating tank, 2 ... Steel material, 3 ... Electrode, 4 ... Working electrode, 5 ... Control apparatus, 11 ... Steel material, 12 ... Black skin, 13 ... Exfoliation part.
Claims (2)
前記鋼材にめっきされた前記金属の分布を測定する第２のステップと
を有することを特徴とする鋼材の黒皮評価方法。 A first step of plating a metal on a portion of the steel material on which the black skin has been peeled;
And a second step of measuring a distribution of the metal plated on the steel material.
前記第１のステップは、前記鋼材に定電流を流し、前記鋼材の電位が前記黒皮が還元される電位に達する前に終了する
ことを特徴とする鋼材の黒皮評価方法。 In the black skin evaluation method of the steel material according to claim 1,
The first step is to apply a constant current to the steel material and finish before the potential of the steel material reaches a potential at which the black skin is reduced.
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