JP2015169466A - hydrogen embrittlement evaluation method - Google Patents

hydrogen embrittlement evaluation method Download PDF

Info

Publication number
JP2015169466A
JP2015169466A JP2014042731A JP2014042731A JP2015169466A JP 2015169466 A JP2015169466 A JP 2015169466A JP 2014042731 A JP2014042731 A JP 2014042731A JP 2014042731 A JP2014042731 A JP 2014042731A JP 2015169466 A JP2015169466 A JP 2015169466A
Authority
JP
Japan
Prior art keywords
steel material
time
test
steel
tensile load
Prior art date
Legal status (The legal status is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the status listed.)
Granted
Application number
JP2014042731A
Other languages
Japanese (ja)
Other versions
JP5986126B2 (en
Inventor
憲宏 藤本
Norihiro Fujimoto
憲宏 藤本
齋藤 博之
Hiroyuki Saito
博之 齋藤
孝 澤田
Takashi Sawada
孝 澤田
Current Assignee (The listed assignees may be inaccurate. Google has not performed a legal analysis and makes no representation or warranty as to the accuracy of the list.)
Nippon Telegraph and Telephone Corp
Original Assignee
Nippon Telegraph and Telephone Corp
Priority date (The priority date is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the date listed.)
Filing date
Publication date
Application filed by Nippon Telegraph and Telephone Corp filed Critical Nippon Telegraph and Telephone Corp
Priority to JP2014042731A priority Critical patent/JP5986126B2/en
Publication of JP2015169466A publication Critical patent/JP2015169466A/en
Application granted granted Critical
Publication of JP5986126B2 publication Critical patent/JP5986126B2/en
Expired - Fee Related legal-status Critical Current
Anticipated expiration legal-status Critical

Links

Images

Landscapes

  • Testing Resistance To Weather, Investigating Materials By Mechanical Methods (AREA)
  • Investigating Strength Of Materials By Application Of Mechanical Stress (AREA)

Abstract

PROBLEM TO BE SOLVED: To enable the hydrogen embrittlement evaluation of a steel to be carried out in a shorter time.SOLUTION: In a step S101, a negative potential is applied to a steel to generate hydrogen on the surface of the steel, and while so doing, a tensile load of a prescribed load value is applied to the steel for the duration of a first time and a change in current density flowing in the steel with the passage of time for which the tensile load is applied is measured, the result being made a reference change (first step). Next, in a step S102, a test steel of the same composition as the steel is prepared, the same negative potential as above is applied to the test steel to generate hydrogen on the surface of the test steel, and while so doing, a tensile load of the same prescribed load value as above is applied to the test steel for the duration of a second time, and a current density flowing in the test steel to which the tensile load is being applied is measured, the result being made an evaluation object measured value (second step). A condition is that the second time is shorter than the first time.

Description

本発明は、鋼材における水素脆化を評価する水素脆化評価方法に関する。   The present invention relates to a hydrogen embrittlement evaluation method for evaluating hydrogen embrittlement in a steel material.

鋼材は、ある使用環境において水素を含むと延性が失われ、強度が著しく低下する(非特許文献1参照)。この現象は、水素脆化と呼ばれている。鋼材の水素脆化特性の評価法の1つとして、試験片に水素を吸蔵させた状態で荷重をかけ、破断する最低荷重を比較する方法がある。破断しない荷重値を確認するための試験時間として、200時間を推奨している例がある(非特許文献2参照)。水素脆化特性評価試験は、結果にばらつきがあり、ばらつきを抑えるために試験条件について議論がなされている(非特許文献2参照)。また、鋼材などに対して水素を吸蔵させる手法には、電位制御による陰極チャージ法がある(非特許文献3参照)。   When steel contains hydrogen in a certain usage environment, the ductility is lost and the strength is significantly reduced (see Non-Patent Document 1). This phenomenon is called hydrogen embrittlement. As one method for evaluating the hydrogen embrittlement characteristics of steel, there is a method in which a load is applied in a state where hydrogen is occluded in a test piece, and the minimum load at which fracture occurs is compared. There is an example in which 200 hours is recommended as a test time for confirming a load value that does not break (see Non-Patent Document 2). In the hydrogen embrittlement characteristic evaluation test, there are variations in the results, and the test conditions are discussed in order to suppress the variations (see Non-Patent Document 2). Further, as a method for storing hydrogen in a steel material or the like, there is a cathode charging method by potential control (see Non-Patent Document 3).

南雲 道彦 他、「鋼の力学的挙動に及ぼす水素の影響」、鉄と鋼、第9巻、第10号、2004年。Michihiko Nagumo et al., “Effect of Hydrogen on Mechanical Behavior of Steel”, Iron and Steel, Vol. 9, No. 10, 2004. 20%チオシアン酸アンモニウム溶液中でのPC鋼材の水素脆化試験方法、社団法人 腐食防食協会、JSCE S 1201、2012年。Test method for hydrogen embrittlement of PC steel in 20% ammonium thiocyanate solution, Japan Corrosion Protection Association, JSCE S 1201, 2012. Y. HAGIHARA, "Evaluation of Delayed Fracture Characteristics of High-strength Bolt Steels by CSRT", ISIJ International, Vol. 2, No.2, pp.292-297, 2012.Y. HAGIHARA, "Evaluation of Delayed Fracture Characteristics of High-strength Bolt Steels by CSRT", ISIJ International, Vol. 2, No.2, pp.292-297, 2012. P. Ghods et al. , "Microscopic investigation of mill scale and its proposed effect on the variability of chloride-induced depassivation of carbon steel rebar", Corrosion Science, vol.53, pp.946-954, 2011.P. Ghods et al., "Microscopic investigation of mill scale and its proposed effect on the variability of chloride-induced depassivation of carbon steel rebar", Corrosion Science, vol.53, pp.946-954, 2011. P. Ghods et al. , "Electrochemical investigation of chloride-induced depassivation of black steel rebar under simulated service conditions", Corrosion Science, vol.52, pp.1649-1659, 2010.P. Ghods et al., "Electrochemical investigation of chloride-induced depassivation of black steel rebar under simulated service conditions", Corrosion Science, vol.52, pp.1649-1659, 2010.

しかしながら、上述した鋼材の水素脆化評価では、評価に多大な時間を要すると言う問題があった。上述した水素脆化試験の結果にはばらつきが出るため、6回試験することが推奨されている。このため、破断しない荷重を確認するなどの評価を実施するためには、200時間×6=1200時間を必要とすることになる。   However, in the above-described evaluation of hydrogen embrittlement of steel materials, there is a problem that a long time is required for the evaluation. Since the results of the hydrogen embrittlement test described above vary, it is recommended that the test be performed six times. For this reason, 200 hours × 6 = 1200 hours are required to perform an evaluation such as confirming a load that does not break.

本発明は、以上のような問題点を解消するためになされたものであり、より短時間で、鋼材の水素脆化評価が実施できるようにすることを目的とする。   The present invention has been made to solve the above-described problems, and an object thereof is to enable hydrogen embrittlement evaluation of steel materials in a shorter time.

本発明に係る水素脆化評価方法は、鋼材を電解質水溶液に浸漬し、鋼材が腐食しない電気化学条件で、電解質水溶液に浸漬している鋼材に負電位を印加して鋼材の表面に水素を発生させた状態で、鋼材に所定の荷重値の引っ張り荷重を第1の時間加え、引っ張り荷重を加えている時間の経過において鋼材に流れる電流密度の変化を測定して基準変化とする第1ステップと、鋼材と同じ組成の試験鋼材を電解質水溶液に浸漬し、電気化学条件で、電解質水溶液に浸漬している試験鋼材に負電位を印加して試験鋼材の表面に水素を発生させた状態で、試験鋼材に所定の荷重値の引っ張り荷重を、第1の時間より短い第2の時間加え、引っ張り荷重を加えている試験鋼材に流れる電流密度を測定して評価対象測定値とする第2ステップと、基準変化の第2の時間における値と評価対象測定値との比較により、試験鋼材の水素脆化を評価する第3ステップとを備え、第1の時間は、鋼材に負電位を印加して鋼材の表面に水素を発生させながら鋼材に所定の荷重値の引っ張り荷重を加えた状態で、鋼材が破断しない範囲の時間とする。   In the hydrogen embrittlement evaluation method according to the present invention, a steel material is immersed in an aqueous electrolyte solution. Under electrochemical conditions in which the steel material does not corrode, a negative potential is applied to the steel material immersed in the aqueous electrolyte solution to generate hydrogen on the surface of the steel material. In this state, a tensile load having a predetermined load value is applied to the steel material for a first time, and a change in the current density flowing in the steel material is measured over the course of the time during which the tensile load is applied. The test steel material having the same composition as the steel material is immersed in an aqueous electrolyte solution, and under electrochemical conditions, a negative potential is applied to the test steel material immersed in the aqueous electrolyte solution to generate hydrogen on the surface of the test steel material. A second step in which a tensile load having a predetermined load value is applied to the steel material for a second time shorter than the first time, and the current density flowing in the test steel material to which the tensile load is applied is measured to obtain an evaluation object measurement value; Standard change A third step of evaluating hydrogen embrittlement of the test steel material by comparing the value at the second time with the measurement value to be evaluated, and applying a negative potential to the steel material during the first time on the surface of the steel material In a state where a tensile load of a predetermined load value is applied to the steel material while generating hydrogen, the time is set so that the steel material does not break.

上記水素脆化評価方法において、電解質水溶液はアルカリ水溶液であればよい。   In the hydrogen embrittlement evaluation method, the aqueous electrolyte solution may be an alkaline aqueous solution.

以上説明したことにより、本発明によれば、より短時間で、鋼材の水素脆化評価が実施できるようになるという優れた効果が得られる。   As described above, according to the present invention, it is possible to obtain an excellent effect that hydrogen embrittlement evaluation of a steel material can be performed in a shorter time.

図1は、本発明の実施の形態における水素脆化評価方法を説明するためのフローチャートである。FIG. 1 is a flowchart for explaining a hydrogen embrittlement evaluation method in an embodiment of the present invention. 図2は、本発明の水素脆化評価方法を実施するために用いる装置の構成を示す断面図である。FIG. 2 is a cross-sectional view showing the configuration of an apparatus used for carrying out the hydrogen embrittlement evaluation method of the present invention. 図3は、定電位制御により鋼材に対して水素を吸蔵させながら引っ張り荷重を加えた状態における鋼材に流れる電流の時間変化を示す特性図である。FIG. 3 is a characteristic diagram showing the change over time of the current flowing in the steel material in a state where a tensile load is applied while hydrogen is occluded in the steel material by constant potential control. 図4は、本発明の実施例における引っ張り試験とともに実施している電流測定で測定された電流変化を示す特性図である。FIG. 4 is a characteristic diagram showing a current change measured by a current measurement performed together with a tensile test in the example of the present invention.

以下、本発明の実施の形態について図を参照して説明する。図1は、本発明の実施の形態における水素脆化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 with reference to the drawings. FIG. 1 is a flowchart for explaining a hydrogen embrittlement evaluation method in an embodiment of the present invention.

まず、ステップS101で、鋼材に負電位を印加して鋼材の表面に水素を発生させながら鋼材に所定の荷重値の引っ張り荷重を第1の時間加え、引っ張り荷重を加えている時間の経過において鋼材に流れる電流密度の変化を測定して基準変化とする(第1ステップ)。鋼材を電解質水溶液に浸漬し、鋼材が腐食しない電気化学条件で、電解質水溶液に浸漬している鋼材に負電位を印加して鋼材の表面に水素を発生させる。引っ張り荷重を加えてから上記水素の発生をさせてもよく、水素を発生させた状態としてから、引っ張り荷重を加えるようにしてもよい。   First, in step S101, a tensile load having a predetermined load value is applied to the steel material for a first time while applying a negative potential to the steel material to generate hydrogen on the surface of the steel material. The change in the current density flowing through is measured and used as a reference change (first step). A steel material is immersed in an aqueous electrolyte solution, and a negative potential is applied to the steel material immersed in the aqueous electrolyte solution under electrochemical conditions in which the steel material does not corrode to generate hydrogen on the surface of the steel material. The hydrogen may be generated after the tensile load is applied, or the tensile load may be applied after the hydrogen is generated.

ここで、上述した負電位を印加して引っ張り荷重を加えている第1の時間は、鋼材に負電位を印加して鋼材の表面に水素を発生させながら鋼材に所定の荷重値の引っ張り荷重を加えた状態で、鋼材が破断しない範囲の時間とするとよい。また、加える引っ張り荷重は、対象とする鋼材の弾性領域応力範囲(降伏応力以下)とするとよい。   Here, in the first time during which the negative potential is applied and the tensile load is applied, the tensile load having a predetermined load value is applied to the steel material while applying a negative potential to the steel material to generate hydrogen on the surface of the steel material. It is good to set it as the time of the range which does not fracture | rupture steel materials in the added state. Moreover, it is good for the tensile load to add to the elastic region stress range (below yield stress) of the steel material made into object.

次に、ステップS102で、鋼材と同じ組成の試験鋼材を用意し、試験鋼材に上述と同じ負電位を印加して試験鋼材の表面に水素を発生させながら試験鋼材に上述と同じ所定の荷重値の引っ張り荷重を第2の時間加え、引っ張り荷重を加えている試験鋼材に流れる電流密度を測定して評価対象測定値とする(第2ステップ)。第2の時間が経過した時点で電流密度の測定を実施して評価対象測定値を得る。前述同様に、試験鋼材を電解質水溶液に浸漬し、試験鋼材が腐食しない電気化学条件で、電解質水溶液に浸漬している鋼材に負電位を印加して試験鋼材の表面に水素を発生させる。引っ張り荷重を加えてから上記水素の発生をさせてもよく、水素を発生させた状態としてから、引っ張り荷重を加えるようにしてもよい。例えば、鋼材(試験鋼材)の破壊荷重の0.9倍の荷重とした定荷重試験とすればよい。ここで、第2の時間は、第1の時間より短い条件とする。   Next, in step S102, a test steel material having the same composition as that of the steel material is prepared, and the same negative load as described above is applied to the test steel material while applying the same negative potential to the test steel material to generate hydrogen on the surface of the test steel material. The tensile load is applied for a second time, and the current density flowing through the test steel material to which the tensile load is applied is measured to obtain a measurement value for evaluation (second step). When the second time elapses, the current density is measured to obtain an evaluation target measurement value. As described above, the test steel material is immersed in an aqueous electrolyte solution, and a negative potential is applied to the steel material immersed in the aqueous electrolyte solution under electrochemical conditions in which the test steel material does not corrode to generate hydrogen on the surface of the test steel material. The hydrogen may be generated after the tensile load is applied, or the tensile load may be applied after the hydrogen is generated. For example, a constant load test may be used in which the load is 0.9 times the fracture load of the steel material (test steel material). Here, the second time is set to be shorter than the first time.

以上のようにして基準変化および評価対象測定値が得られたら、ステップS103で、基準変化の第2の時間における値と評価対象測定値との比較により、試験鋼材の水素脆化を評価する(第3ステップ)。この評価では、第2の時間における評価対象測定値が、第2の時間における基準変化の電流密度より低い範囲となっていれば、試験鋼材は、基準変化の測定条件において、第1の時間が経過した後でも、水素脆化による破断が発生しないと判断する。   When the reference change and the evaluation target measurement value are obtained as described above, hydrogen embrittlement of the test steel material is evaluated in step S103 by comparing the value of the reference change at the second time with the evaluation target measurement value ( (3rd step). In this evaluation, if the measurement value to be evaluated in the second time is in a range lower than the current density of the reference change in the second time, the test steel material has the first time in the measurement condition of the reference change. Even after the lapse of time, it is determined that the fracture due to hydrogen embrittlement does not occur.

従来の評価においては、200時間を推奨している例もあり(非特許文献2参照)、第1の時間を少なくとも100時間とすることが必要とされている。このため、試験鋼材を評価する場合、試験鋼材毎に最低でも100時間の試験時間を必要としていた。例えば、2つの試験鋼材を評価する場合、100×2時間=200時間が必要となっていた。   In the conventional evaluation, there is an example in which 200 hours are recommended (see Non-Patent Document 2), and the first time is required to be at least 100 hours. For this reason, when test steel materials are evaluated, a test time of at least 100 hours is required for each test steel material. For example, when two test steel materials are evaluated, 100 × 2 hours = 200 hours are required.

これに対し、本発明によれば、試験鋼材の測定においては、第1の時間より短い第2の時間をかければよく、第2の時間は、10時間程度で十分である。このため、例えば2つの試験鋼材を評価する場合、基準変化を求める時間を含め、100時間+10×2時間=120時間であればよく、より短時間で鋼材の水素脆化評価が実施できるようになる。   On the other hand, according to the present invention, in the measurement of the test steel material, a second time shorter than the first time may be used, and about 10 hours is sufficient for the second time. For this reason, for example, when two test steel materials are evaluated, it is sufficient that 100 hours + 10 × 2 hours = 120 hours including the time for obtaining the reference change so that the hydrogen embrittlement evaluation of the steel materials can be performed in a shorter time. Become.

ここで、上述した測定は、例えば、図2に示す装置を用いて実施すればよい。この装置は、アクリル樹脂などから構成された容器201と、同様にアクリル樹脂から構成された蓋202と、容器201に収容された電解質溶液203とを備える。電解質溶液203は、例えば1%チオシアン酸アンモニウムを添加した0.1Mの水酸化ナトリウム水溶液である。電解質溶液203は、アルカリ水溶液であればよい。また、この装置は、電解質溶液203中に配置された参照極204,対極205を備える。参照極204は、Ag/AgCl(銀塩化銀)電極であり、対極205は、Pt電極である。また、対象となる鋼材206は、容器201の底部から蓋202を貫通して電解質溶液203に接触する状態とされている。   Here, the above-described measurement may be performed using, for example, the apparatus shown in FIG. The apparatus includes a container 201 made of acrylic resin or the like, a lid 202 similarly made of acrylic resin, and an electrolyte solution 203 accommodated in the container 201. The electrolyte solution 203 is, for example, a 0.1 M sodium hydroxide aqueous solution to which 1% ammonium thiocyanate is added. The electrolyte solution 203 may be an alkaline aqueous solution. This apparatus also includes a reference electrode 204 and a counter electrode 205 disposed in the electrolyte solution 203. The reference electrode 204 is an Ag / AgCl (silver silver chloride) electrode, and the counter electrode 205 is a Pt electrode. In addition, the target steel material 206 is in a state of penetrating the lid 202 from the bottom of the container 201 and contacting the electrolyte solution 203.

鋼材206は、直径9mm、長さ450mmの棒状とし、容器201の底部の貫通部では、シリコーンゴムによる栓207により電解質溶液203が漏れないようにシールされている。また、参照極204は、蓋202を貫通して先端部が電解質溶液203に接触する状態としており、蓋202に栓208で固定されている。   The steel material 206 has a rod shape with a diameter of 9 mm and a length of 450 mm, and is sealed so that the electrolyte solution 203 does not leak through a stopper 207 made of silicone rubber at the bottom through portion of the container 201. Further, the reference electrode 204 is in a state of penetrating the lid 202 and having a tip portion in contact with the electrolyte solution 203, and is fixed to the lid 202 with a plug 208.

この状態で、ポテンショスタット(不図示)を用い、鋼材206を作用極とし、参照極204および対極205を用いた3極構成で、鋼材206に、参照極204に対して負の電位を印加する。この電位印加により、電解質溶液203に触れている鋼材206の表面には、水素が発生する。印加する電位は、電解質溶液203に触れている鋼材206の表面が、腐食しない電気化学条件の電位とすればよい。また、このように電位を印加している状態で、対極205と鋼材206との間に流れる電流を測定し、鋼材206の寸法などにより、電流密度を得る。   In this state, a potentiostat (not shown) is used, the steel material 206 is used as a working electrode, and a negative potential is applied to the steel material 206 with respect to the reference electrode 204 in a three-pole configuration using the reference electrode 204 and the counter electrode 205. . By this potential application, hydrogen is generated on the surface of the steel material 206 that is in contact with the electrolyte solution 203. The potential to be applied may be a potential under electrochemical conditions in which the surface of the steel material 206 in contact with the electrolyte solution 203 does not corrode. Further, the current flowing between the counter electrode 205 and the steel material 206 is measured in a state where the potential is applied as described above, and the current density is obtained based on the dimensions of the steel material 206 and the like.

本発明は、定電位制御により鋼材に対して水素を吸蔵させながら引っ張り荷重を加え、図3に示すように、予め決めた測定時間(t0)の電流値(i0)を読み取ることで、実施した試験条件で予め決めた試験時間内に破断するかどうかを早期に判断し、試験時間を飛躍的に短縮するようにしたものである。 The present invention applies a tensile load while absorbing hydrogen into the steel material by constant potential control, and reads the current value (i 0 ) of a predetermined measurement time (t 0 ) as shown in FIG. Whether or not to break within a predetermined test time under the test conditions carried out is judged at an early stage, and the test time is drastically shortened.

以下、本発明の実施例について説明する。以下では、実施例として、引っ張り強度σB1450MPa、φ9mmの一般的な高強度鋼(Fe−0.25%Si)を対象の鋼材として、本発明の水素脆化評価方法を実施した評価結果について説明する。   Examples of the present invention will be described below. Below, the evaluation result which implemented the hydrogen embrittlement evaluation method of this invention is made into the steel material made into general high strength steel (Fe-0.25% Si) of tensile strength (sigma) B1450MPa and (phi) 9mm as an Example. .

まず、1wt%チオシアン酸アンモニウムを添加した1MのNaHCO3水溶液を電解質水溶液として用いた。また、参照極として銀塩化銀電極、対極として白金線を用い、前述したように、鋼材(試験片)は作用極とした。これらの電極構成で、−1000mVvs.SSEに電位を制御した。陰極チャージすることで試験片表面に水素を発生させる。これにより、試験片に水素が吸蔵(吸収)する状態となる。定荷重による引っ張り試験で加える荷重は、0.90σB、0.88σBとし、各々の条件で3回ずつ測定を実施した。 First, a 1M NaHCO 3 aqueous solution to which 1 wt% ammonium thiocyanate was added was used as an aqueous electrolyte solution. In addition, a silver / silver chloride electrode was used as the reference electrode and a platinum wire was used as the counter electrode, and as described above, the steel material (test piece) was the working electrode. With these electrode configurations, -1000 mVvs. The potential was controlled to SSE. Hydrogen is generated on the surface of the test piece by cathodic charging. Thereby, it will be in the state which hydrogen occludes (absorbs) to a test piece. The load applied in the tensile test with a constant load was 0.90σB and 0.88σB, and measurement was performed three times under each condition.

以下の表1に、引っ張り試験の結果を示す。   Table 1 below shows the results of the tensile test.

Figure 2015169466
Figure 2015169466

表1に示すように、測定時間内に破断したのは、0.90σBでは3回中3回、0.88σBでは3回中1回であった。破断時間は、上記荷重条件の差により倍以上の差があることもあった。   As shown in Table 1, the breakage within the measurement time was 3 times in 3 times for 0.90σB and 1 time in 3 times for 0.88σB. The rupture time may be more than double due to the difference in the load conditions.

次に、上述した引っ張り試験とともに実施している電流測定で測定された電流変化について図4に示す。いずれの試験片においても、測定時間とともに電流値が低下しているが、電流値は、試験片によって異なった。また、0.90σBの測定では、電流値が大きいほど定荷重測定の破断時間が短い。また、0.88σBの測定では、唯一破断したときの電流値は、3回の測定で最大であった。   Next, FIG. 4 shows the current change measured by the current measurement performed together with the tensile test described above. In any test piece, the current value decreased with the measurement time, but the current value varied depending on the test piece. Further, in the measurement of 0.90σB, the breaking time of the constant load measurement is shorter as the current value is larger. Moreover, in the measurement of 0.88σB, the current value at the time of the only breakage was the maximum in three measurements.

これらのことから、同じ測定条件であれば、予め決めた測定時間において検出された電流値を、予め実施してある測定の電流値(基準値)と比較することで、以下の表2に示すように、より長い測定時間の後で破断するかしないかを判断することができると推察される。   From these, under the same measurement conditions, the current value detected at a predetermined measurement time is compared with the current value (reference value) of the measurement that has been performed in advance, as shown in Table 2 below. Thus, it is assumed that it can be determined whether or not the fracture occurs after a longer measurement time.

Figure 2015169466
Figure 2015169466

結果が未破断になる測定は、従来では測定を最低100時間継続しなければならないが、本発明により、測定中に読み取った電流値(電流密度)より、これまで未破断であったときの電流値の方が大きい場合に即座に未破断と判定し、測定を終了させることができ、飛躍的に測定時間を短縮することができる。電流値を読み取る測定時間については、予め決めることができるが、黒皮が形成されたままの試験片では、電位印加により黒皮がほとんど還元されるチャージ開始6時間後の電流値を読むとよい。   In the measurement in which the result is unbroken, conventionally, the measurement has to be continued for at least 100 hours. However, according to the present invention, the current when unruptured has been obtained from the current value (current density) read during the measurement. When the value is larger, it is immediately determined that the sample has not broken, and the measurement can be terminated, and the measurement time can be dramatically shortened. The measurement time for reading the current value can be determined in advance. However, in the test piece with the black skin formed, it is better to read the current value 6 hours after the start of the charge when the black skin is almost reduced by the potential application. .

ここで、鉄筋コンクリートなど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、鋼材の化学組成が同一であっても、製造者によって厚さや均一性が異なり、必ずしも制御されているわけではない(非特許文献4参照)。このような状態の黒皮であるが、黒皮を研磨することにより、塩化物イオンに対する感受性が低下し、さらに評価結果も安定するとの報告がある(非特許文献5参照)。しかしながら、黒皮が形成されたままの試験片では従来技術に記載したとおり測定結果の変動が多く、条件によっては測定回数をさらに増やす必要があり、さらに測定時間が長期化する。これに対し、本発明によれば、測定時間の長期化が防げるようになる。   Here, an oxide film called black skin is formed on the surface of a steel material used for reinforced concrete or the like when a heat treatment process is performed. Even if the chemical composition of the steel material is the same, the thickness and uniformity of the black skin differ depending on the manufacturer, and are not necessarily controlled (see Non-Patent Document 4). Although it is a black skin of such a state, there exists a report that the sensitivity with respect to a chloride ion falls by polishing a black skin, and also the evaluation result is stabilized (refer nonpatent literature 5). However, as described in the prior art, a test piece with a black skin still formed has many fluctuations in measurement results, and depending on the conditions, it is necessary to further increase the number of measurements, which further increases the measurement time. On the other hand, according to the present invention, the measurement time can be prevented from being prolonged.

以上に説明したように、本発明によれば、水素を吸蔵させている状態で引っ張り試験を行う測定において、より短い測定時間の結果を、同じ測定時間における基準変化と比較するようにしたので、対象となる鋼材(試験鋼材)の評価を、より短い測定時間の結果で行えるようになる。このように、本発明によれば、より短時間で、鋼材の水素脆化評価が実施できるようになる。   As described above, according to the present invention, in the measurement in which the tensile test is performed in a state where hydrogen is occluded, the result of the shorter measurement time is compared with the reference change in the same measurement time. The target steel material (test steel material) can be evaluated with a shorter measurement time. Thus, according to the present invention, it becomes possible to perform hydrogen embrittlement evaluation of a steel material in a shorter time.

なお、本発明は以上に説明した実施の形態に限定されるものではなく、本発明の技術的思想内で、当分野において通常の知識を有する者により、多くの変形および組み合わせが実施可能であることは明白である。例えば、第2の時間が経過した時点の電流密度に限るものではなく、第2の時間の間の電流密度の変化を評価対象測定値として用いるようにしてもよい。   The present invention is not limited to the embodiment described above, and many modifications and combinations can be implemented by those having ordinary knowledge in the art within the technical idea of the present invention. It is obvious. For example, it is not limited to the current density at the time when the second time has elapsed, and a change in current density during the second time may be used as the measurement value to be evaluated.

201…容器、202…蓋、203…電解質溶液、204…参照極、205…対極、206…鋼材、207…栓、208…栓。   201 ... container, 202 ... lid, 203 ... electrolyte solution, 204 ... reference electrode, 205 ... counter electrode, 206 ... steel material, 207 ... stopper, 208 ... stopper.

Claims (2)

鋼材を電解質水溶液に浸漬し、前記鋼材が腐食しない電気化学条件で、前記電解質水溶液に浸漬している前記鋼材に負電位を印加して前記鋼材の表面に水素を発生させた状態で、前記鋼材に所定の荷重値の引っ張り荷重を第1の時間加え、引っ張り荷重を加えている時間の経過において前記鋼材に流れる電流密度の変化を測定して基準変化とする第1ステップと、
前記鋼材と同じ組成の試験鋼材を前記電解質水溶液に浸漬し、前記電気化学条件で、前記電解質水溶液に浸漬している前記試験鋼材に負電位を印加して前記試験鋼材の表面に水素を発生させた状態で、前記試験鋼材に前記所定の荷重値の引っ張り荷重を、前記第1の時間より短い第2の時間加え、引っ張り荷重を加えている前記試験鋼材に流れる電流密度を測定して評価対象測定値とする第2ステップと、
前記基準変化の前記第2の時間における値と前記評価対象測定値との比較により、前記試験鋼材の水素脆化を評価する第3ステップと
を備え、
前記第1の時間は、前記鋼材に前記負電位を印加して前記鋼材の表面に水素を発生させながら前記鋼材に前記所定の荷重値の引っ張り荷重を加えた状態で、前記鋼材が破断しない範囲の時間とする
ことを特徴とする水素脆化評価方法。
In the state in which the steel material is immersed in an aqueous electrolyte solution, and a negative potential is applied to the steel material immersed in the aqueous electrolyte solution under electrochemical conditions in which the steel material is not corroded to generate hydrogen on the surface of the steel material. A first step of applying a tensile load of a predetermined load value to the first time, measuring a change in current density flowing through the steel material in the lapse of time when the tensile load is applied, and a first step as a reference change;
A test steel material having the same composition as the steel material is immersed in the electrolyte aqueous solution, and under the electrochemical conditions, a negative potential is applied to the test steel material immersed in the electrolyte aqueous solution to generate hydrogen on the surface of the test steel material. In this state, a tensile load having the predetermined load value is applied to the test steel material for a second time shorter than the first time, and a current density flowing through the test steel material to which the tensile load is applied is measured for evaluation. A second step of measuring values;
A third step of evaluating hydrogen embrittlement of the test steel material by comparing the value at the second time of the reference change with the measurement value to be evaluated, and
The first time is a range in which the steel material is not broken in a state where a tensile load of the predetermined load value is applied to the steel material while applying a negative potential to the steel material to generate hydrogen on the surface of the steel material. A method for evaluating hydrogen embrittlement, characterized by:
請求項1記載の水素脆化評価方法において、
前記電解質水溶液はアルカリ水溶液であることを特徴とする水素脆化評価方法。
In the hydrogen embrittlement evaluation method according to claim 1,
The method for evaluating hydrogen embrittlement, wherein the aqueous electrolyte solution is an alkaline aqueous solution.
JP2014042731A 2014-03-05 2014-03-05 Hydrogen embrittlement evaluation method Expired - Fee Related JP5986126B2 (en)

Priority Applications (1)

Application Number Priority Date Filing Date Title
JP2014042731A JP5986126B2 (en) 2014-03-05 2014-03-05 Hydrogen embrittlement evaluation method

Applications Claiming Priority (1)

Application Number Priority Date Filing Date Title
JP2014042731A JP5986126B2 (en) 2014-03-05 2014-03-05 Hydrogen embrittlement evaluation method

Publications (2)

Publication Number Publication Date
JP2015169466A true JP2015169466A (en) 2015-09-28
JP5986126B2 JP5986126B2 (en) 2016-09-06

Family

ID=54202335

Family Applications (1)

Application Number Title Priority Date Filing Date
JP2014042731A Expired - Fee Related JP5986126B2 (en) 2014-03-05 2014-03-05 Hydrogen embrittlement evaluation method

Country Status (1)

Country Link
JP (1) JP5986126B2 (en)

Cited By (2)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
JP2019211328A (en) * 2018-06-05 2019-12-12 日本電信電話株式会社 Crack occurrence detection method, crack occurrence detection device, and crack occurrence detection program
WO2023058086A1 (en) * 2021-10-04 2023-04-13 日本電信電話株式会社 Hydrogen embrittlement risk assessment method and device therefor

Citations (5)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
JP2000329726A (en) * 1999-05-19 2000-11-30 Nippon Steel Corp Evaluation method for hydrogen embrittlement susceptibility of steel product
JP2004309197A (en) * 2003-04-03 2004-11-04 Sumitomo Metal Ind Ltd Method for evaluating resistance to delayed fracture
JP2010054494A (en) * 2008-07-28 2010-03-11 Kobe Steel Ltd Method for evaluating hydrogen cracking resistivity of steel products
JP2012184992A (en) * 2011-03-04 2012-09-27 Japan Steel Works Ltd:The Determination method for fatigue crack life under high pressure hydrogen atmosphere
JP2013057612A (en) * 2011-09-09 2013-03-28 Nippon Telegr & Teleph Corp <Ntt> Hydrogen occlusion method

Patent Citations (5)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
JP2000329726A (en) * 1999-05-19 2000-11-30 Nippon Steel Corp Evaluation method for hydrogen embrittlement susceptibility of steel product
JP2004309197A (en) * 2003-04-03 2004-11-04 Sumitomo Metal Ind Ltd Method for evaluating resistance to delayed fracture
JP2010054494A (en) * 2008-07-28 2010-03-11 Kobe Steel Ltd Method for evaluating hydrogen cracking resistivity of steel products
JP2012184992A (en) * 2011-03-04 2012-09-27 Japan Steel Works Ltd:The Determination method for fatigue crack life under high pressure hydrogen atmosphere
JP2013057612A (en) * 2011-09-09 2013-03-28 Nippon Telegr & Teleph Corp <Ntt> Hydrogen occlusion method

Cited By (6)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
JP2019211328A (en) * 2018-06-05 2019-12-12 日本電信電話株式会社 Crack occurrence detection method, crack occurrence detection device, and crack occurrence detection program
WO2019235303A1 (en) * 2018-06-05 2019-12-12 日本電信電話株式会社 Method for detecting occurrence of cracks and the like, device for detecting occurrence of cracks and the like, and program for detecting occurrence of cracks and the like
US20210231596A1 (en) * 2018-06-05 2021-07-29 Nippon Telegraph And Telephone Corporation Method for Detecting Occurrence of Cracks and the Like, Device for Detecting Occurrence of Cracks and the Like, And Program for Detecting Occurrence of Cracks and the Like
JP7029061B2 (en) 2018-06-05 2022-03-03 日本電信電話株式会社 Rhagades occurrence detection method, crack occurrence detection device and crack occurrence detection program
US11913895B2 (en) 2018-06-05 2024-02-27 Nippon Telegraph And Telephone Corporation Method for detecting occurrence of cracks and the like, device for detecting occurrence of cracks and the like, and program for detecting occurrence of cracks and the like
WO2023058086A1 (en) * 2021-10-04 2023-04-13 日本電信電話株式会社 Hydrogen embrittlement risk assessment method and device therefor

Also Published As

Publication number Publication date
JP5986126B2 (en) 2016-09-06

Similar Documents

Publication Publication Date Title
JP6163433B2 (en) Crevice corrosion test method and crevice corrosion test equipment
JP2018204949A (en) Evaluation method for hydrogen embrittlement resistance characteristic of steel material
JP6354476B2 (en) Characterization method for hydrogen embrittlement of steel
JP2014041073A (en) Steel material evaluation method
JP5986126B2 (en) Hydrogen embrittlement evaluation method
JP6470716B2 (en) Method for calculating test piece area and test cell size in hydrogen embrittlement property evaluation test
JP2015031554A (en) Hydrogen penetration potential prediction method
JP6740176B2 (en) Hydrogen permeation test device
JP6342783B2 (en) Hydrogen penetration evaluation method
CN115931538B (en) Method for measuring influence degree of hydrogen in acidic environment on metal stress corrosion cracking
JP6973193B2 (en) Hydrogen embrittlement resistance evaluation method
JP6278839B2 (en) Crevice corrosion test equipment and crevice corrosion test method
JP6724761B2 (en) Hydrogen embrittlement evaluation apparatus, hydrogen embrittlement evaluation method, and test piece used therein
JP6309826B2 (en) Fracture stress estimation method and fracture stress estimation device for oxide film fracture
JP2000329726A (en) Evaluation method for hydrogen embrittlement susceptibility of steel product
JP7029061B2 (en) Rhagades occurrence detection method, crack occurrence detection device and crack occurrence detection program
JP2020030187A (en) Hydrogen filling method and hydrogen embrittlement characteristics evaluation method
JP6001581B2 (en) Hydrogen embrittlement characteristics evaluation method
JP6042772B2 (en) Method of evaluating hydrogen penetration characteristics for metal members
JP2015135302A (en) Hydrogen occlusion method
JP6112617B2 (en) Black skin evaluation method for steel
JP2010281687A (en) Method for predicting amount of corrosion of metal material in contact state of different metal
JP2016130638A (en) Method for evaluating hydrogen embrittlement characteristics
JP2019196918A (en) Method, device, and program for estimating fracture starting point in steel material
JP2019039794A (en) Measurement method of hydrogen embrittlement resistance characteristic value

Legal Events

Date Code Title Description
A621 Written request for application examination

Free format text: JAPANESE INTERMEDIATE CODE: A621

Effective date: 20151117

A977 Report on retrieval

Free format text: JAPANESE INTERMEDIATE CODE: A971007

Effective date: 20160719

TRDD Decision of grant or rejection written
A01 Written decision to grant a patent or to grant a registration (utility model)

Free format text: JAPANESE INTERMEDIATE CODE: A01

Effective date: 20160802

A61 First payment of annual fees (during grant procedure)

Free format text: JAPANESE INTERMEDIATE CODE: A61

Effective date: 20160804

R150 Certificate of patent or registration of utility model

Ref document number: 5986126

Country of ref document: JP

Free format text: JAPANESE INTERMEDIATE CODE: R150

LAPS Cancellation because of no payment of annual fees