氢在钢中的扩散与氢渗透传感器的研究
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摘要
工业生产中产生的氢对设备的破坏非常严重，为了预防重大恶性事故的发生，研究氢渗透传感器用来监/检测腐蚀反应产生的氢含量及对钢体设备的氢腐蚀程度，采取有效的防护措施来解决腐蚀问题，指导生产实践，实现生产安全与长周期运行，意义重大。国内外有不同类型的电化学氢传感器的研究报道，但是，不同类型传感器的测量能否得到一致的结果值得深入研究。通过设计氢渗透传感器来检测设备氢渗透速率，评估设备的安全运行状态，避免产生巨大的经济损失和严重的社会后果，具有重要的社会经济效益。
本文采用Devanathan—Stachurski渗氢电池检测原子氢的渗透速率，并设计了工程中能应用的氢渗透传感器，研究了被测设备的表面催化镀层，对电流型与电势型氢渗透传感器性能的影响，研究了胶状电解质的双电解质氢渗透传感器的性能。研究结果表明：
(1)被检测的工件表面无催化镀层时，传感器对原子氢电化学氧化没有活性，通过镀镍或镀钯层来提高对氢原子的催化氧化活性。镀层的致密性直接影响其氢原子的催化活性和传感器的灵敏度。采用我们开发的镀钯和镀镍电解液，在0.333A-dm~(-2)的阴极电流密度镀钯8~10min时，或在1.00A-dm~(-2)的电流密度下镀镍5min，都能获得良好的催化镀层。催化镀层不仅能够有效地降低背景电流，同时能提高氢原子氧化的催化活性。
(2)传感器中镍镀层与钯镀层的氧化原子氢的安全电势区间分别为+0.3~+0.4V_(Ni)和+0.2~－+0.5V_(Ni)。在较低的氧化电势下，钯的催化活性比镍高，但通过提供合适的氧化电势，使镍镀层达到和钯镀层一样高的催化活性，镍镀层的最适宜氧化电势为0.35V_(Ni)。
(3)电流型氢渗透传感器和电势型氢渗透传感器都能够应用于氢渗透测量。在相同温度条件下，随着充氢电流密度增大，稳态电势相应增加，在相同的充氢电流密度时，两者测量结果相近，最小相对偏差仅为3.0%。
(4)电流型氢渗透传感器响应比电势型传感器快，灵敏度高。两种类型氢渗透传感都具有良好的重现性。
(5)采用由胶状电解质和KOH溶液组成的双电解质电流型氢传感器，检测钢体因氢腐蚀产生的氢原子渗透速率。该氢渗透传感器有适宜的粘性和较高的导电率，可以有效地防止传感器在安装时的漏液现象，同时具有良好可靠性。
(6)现场监测试验表明设计的腐蚀监测系统能够反映设备壁氢渗透的信息，能实时、在线、无损地检测设备中原子氢浓度，为设备的安全运行提供了可靠的保证。
本论文在如下方面有创新性研究成果：（i）确定了原子氢氧化的最佳催化镀层和施镀的工艺；（ii）揭示了电流型和电势型两类电化学氢渗透传感器的性能，确定了电流型氢渗透传感器更适合于氢渗透速率的检测；（iii）采用双电解质系统解决传感器安装漏液的问题，并证实了该传感器对测量信号相应的正确性。（iv）现场检测结果显示设计的氢渗透传感器组成电化学腐蚀监测系统，可以实时、在线、无损检/监测正在运行的设备中原子氢的浓度，并对氢致裂开危险性进行评估。
The steel equipment was destroyed seriously by hydrogen, which was generated inindustrial production. In order to prevent the occurrence of malignant accidents, thesensor was developed to detect/monitor hydrogen content produced by corrosionreactions and to evaluate the hydrogen corrosion degree of steel equipment. It is ofgreat significance that effective safeguard procedures are taken to solve the corrosionproblem, to guide the production practice and finally to realize safety production andlong period running. The researches about different types of electrochemicalhydrogen sensors have been reported at home and abroad. However, it was worth tostudy in-depth whether the consistent measure results were obtained or not throughthe measurement with different type sensors. It had vital socioeconomic benefits thatthe sensor was developed to monitor the hydrogen permeation rate of equipment inreal-time and nondestructively, to evaluate the safety operation state of equipment,and to prevent occurrence of enormous loss in economy and servant socialconsequence in production operation.
The atomic hydrogen permeation rate was detected by the Devanathan-Stachurskicell. The sensor for detecting hydrogen permeation rate was developed in thedissertation. The influence of the catalytic coatings on the measured equipment on theperformance of amperometric-type and potentiometric-type hydrogen permeationsensors was studied. The performance of the sensor composed of double electrolyteswith gelatiniform electrolyte was investigated. The results were shown as follow:
(1)The sensor could not oxidize the atom hydrogen when the detected workpiecesurface did not plate catalytic coating, but the catalytic activity of oxidizing hydrogenatoms was improved by the coating of nickel or palladium. The catalytic activity ofoxidizing hydrogen atom, or the sensor sensitivity, directly depended on thecompactness of coating. When the electroplating was conducted for8~10min by0.333A-dm~(-2)cathode current density, the compact palladium plating on the steelcould be obtained in our developed palladium electrolyte. When the cathode currentdensity of1.00A-dm~(-2)was applied to electroplate nickel for over5min, the compactnickel plating on the detected surface of equipment was obtained. Therefore, not onlythe background current could be reduced effectually via plating nickel or palladium,but also the catalytic activity for oxidizing the hydrogen atoms could be improved.
(2) The safe potential interval of hydrogen oxidation on nickel and palladiumcoating was+0.3~+0.4V_(Ni)and+0.2~+0.5V_(Ni), separately. Under the lower oxidationpotential, the catalytic activity of palladium coating was slightly higher than that ofnickel coating. We can raise the oxidization potential to reach the same catalyticactivity on palladium coating. The optimum oxidation potential on nickel coating was0.35V_(Ni).
(3) Both of the amperometric-type and potentiometric-type hydrogen permeationsensors could be applied to the detection of hydrogen permeation rate. Under the sametemperature conditions, the steady state potential was increased with the rise ofcharging current density. The nearly agreeable results were obtained on the two typesensors under the same density of charging current. The minimum relative deviationwas only3.0%between them.
(4) The response time of amperometric hydrogen permeation sensor was shorterand the sensitivity was higher relatively. The two types of the sensors had goodreproducibility.
(5) An amperometric hydrogen sensor with double electrolytes composed of agelatiniform electrolyte and KOH solution were developed to detect the permeationrate of hydrogen atoms in steel equipment. The hydrogen permeation sensor hadsuitable viscosity and high electrical conductivity, which could prevent effectively theleakage when it was fixed and it had good reliability.
(6) The field monitoring tests showed that the designed corrosion monitoringsystem could accurately display the hydrogen permeation information of the equip-ment. It was applied in the real-time, on situ and nondestructive detecting atomichydrogen concentration in the steels. It could provide the reliability for the safeoperation of the equipment.
The innovative points of our researches were shown as follows:（i）The optimumcatalytic coatings for oxidization of atomic hydrogen and plating processes wereascertained.（ii）The performances of the amperometric-type and potentiometric-typehydrogen sensors were studied and it was found out that the amperometric hydrogenpermeation sensor was more suitable to detect the hydrogen permeation rate.（iii）The leakage problem was solved using double electrolytes system when the sensorwas fixed. The correctness of measuring signal was verified by experiments.（iv）Theresult of field monitoring showed that the developed electrochemical monitoringsystem could realize the real-time, online and nondestructive detection of atomichydrogen concentration and the estimation of the susceptibility of hydrogen induced cracking.
本文采用Devanathan—Stachurski渗氢电池检测原子氢的渗透速率，并设计了工程中能应用的氢渗透传感器，研究了被测设备的表面催化镀层，对电流型与电势型氢渗透传感器性能的影响，研究了胶状电解质的双电解质氢渗透传感器的性能。研究结果表明：
(1)被检测的工件表面无催化镀层时，传感器对原子氢电化学氧化没有活性，通过镀镍或镀钯层来提高对氢原子的催化氧化活性。镀层的致密性直接影响其氢原子的催化活性和传感器的灵敏度。采用我们开发的镀钯和镀镍电解液，在0.333A-dm~(-2)的阴极电流密度镀钯8~10min时，或在1.00A-dm~(-2)的电流密度下镀镍5min，都能获得良好的催化镀层。催化镀层不仅能够有效地降低背景电流，同时能提高氢原子氧化的催化活性。
(2)传感器中镍镀层与钯镀层的氧化原子氢的安全电势区间分别为+0.3~+0.4V_(Ni)和+0.2~－+0.5V_(Ni)。在较低的氧化电势下，钯的催化活性比镍高，但通过提供合适的氧化电势，使镍镀层达到和钯镀层一样高的催化活性，镍镀层的最适宜氧化电势为0.35V_(Ni)。
(3)电流型氢渗透传感器和电势型氢渗透传感器都能够应用于氢渗透测量。在相同温度条件下，随着充氢电流密度增大，稳态电势相应增加，在相同的充氢电流密度时，两者测量结果相近，最小相对偏差仅为3.0%。
(4)电流型氢渗透传感器响应比电势型传感器快，灵敏度高。两种类型氢渗透传感都具有良好的重现性。
(5)采用由胶状电解质和KOH溶液组成的双电解质电流型氢传感器，检测钢体因氢腐蚀产生的氢原子渗透速率。该氢渗透传感器有适宜的粘性和较高的导电率，可以有效地防止传感器在安装时的漏液现象，同时具有良好可靠性。
(6)现场监测试验表明设计的腐蚀监测系统能够反映设备壁氢渗透的信息，能实时、在线、无损地检测设备中原子氢浓度，为设备的安全运行提供了可靠的保证。
本论文在如下方面有创新性研究成果：（i）确定了原子氢氧化的最佳催化镀层和施镀的工艺；（ii）揭示了电流型和电势型两类电化学氢渗透传感器的性能，确定了电流型氢渗透传感器更适合于氢渗透速率的检测；（iii）采用双电解质系统解决传感器安装漏液的问题，并证实了该传感器对测量信号相应的正确性。（iv）现场检测结果显示设计的氢渗透传感器组成电化学腐蚀监测系统，可以实时、在线、无损检/监测正在运行的设备中原子氢的浓度，并对氢致裂开危险性进行评估。
The steel equipment was destroyed seriously by hydrogen, which was generated inindustrial production. In order to prevent the occurrence of malignant accidents, thesensor was developed to detect/monitor hydrogen content produced by corrosionreactions and to evaluate the hydrogen corrosion degree of steel equipment. It is ofgreat significance that effective safeguard procedures are taken to solve the corrosionproblem, to guide the production practice and finally to realize safety production andlong period running. The researches about different types of electrochemicalhydrogen sensors have been reported at home and abroad. However, it was worth tostudy in-depth whether the consistent measure results were obtained or not throughthe measurement with different type sensors. It had vital socioeconomic benefits thatthe sensor was developed to monitor the hydrogen permeation rate of equipment inreal-time and nondestructively, to evaluate the safety operation state of equipment,and to prevent occurrence of enormous loss in economy and servant socialconsequence in production operation.
The atomic hydrogen permeation rate was detected by the Devanathan-Stachurskicell. The sensor for detecting hydrogen permeation rate was developed in thedissertation. The influence of the catalytic coatings on the measured equipment on theperformance of amperometric-type and potentiometric-type hydrogen permeationsensors was studied. The performance of the sensor composed of double electrolyteswith gelatiniform electrolyte was investigated. The results were shown as follow:
(1)The sensor could not oxidize the atom hydrogen when the detected workpiecesurface did not plate catalytic coating, but the catalytic activity of oxidizing hydrogenatoms was improved by the coating of nickel or palladium. The catalytic activity ofoxidizing hydrogen atom, or the sensor sensitivity, directly depended on thecompactness of coating. When the electroplating was conducted for8~10min by0.333A-dm~(-2)cathode current density, the compact palladium plating on the steelcould be obtained in our developed palladium electrolyte. When the cathode currentdensity of1.00A-dm~(-2)was applied to electroplate nickel for over5min, the compactnickel plating on the detected surface of equipment was obtained. Therefore, not onlythe background current could be reduced effectually via plating nickel or palladium,but also the catalytic activity for oxidizing the hydrogen atoms could be improved.
(2) The safe potential interval of hydrogen oxidation on nickel and palladiumcoating was+0.3~+0.4V_(Ni)and+0.2~+0.5V_(Ni), separately. Under the lower oxidationpotential, the catalytic activity of palladium coating was slightly higher than that ofnickel coating. We can raise the oxidization potential to reach the same catalyticactivity on palladium coating. The optimum oxidation potential on nickel coating was0.35V_(Ni).
(3) Both of the amperometric-type and potentiometric-type hydrogen permeationsensors could be applied to the detection of hydrogen permeation rate. Under the sametemperature conditions, the steady state potential was increased with the rise ofcharging current density. The nearly agreeable results were obtained on the two typesensors under the same density of charging current. The minimum relative deviationwas only3.0%between them.
(4) The response time of amperometric hydrogen permeation sensor was shorterand the sensitivity was higher relatively. The two types of the sensors had goodreproducibility.
(5) An amperometric hydrogen sensor with double electrolytes composed of agelatiniform electrolyte and KOH solution were developed to detect the permeationrate of hydrogen atoms in steel equipment. The hydrogen permeation sensor hadsuitable viscosity and high electrical conductivity, which could prevent effectively theleakage when it was fixed and it had good reliability.
(6) The field monitoring tests showed that the designed corrosion monitoringsystem could accurately display the hydrogen permeation information of the equip-ment. It was applied in the real-time, on situ and nondestructive detecting atomichydrogen concentration in the steels. It could provide the reliability for the safeoperation of the equipment.
The innovative points of our researches were shown as follows:（i）The optimumcatalytic coatings for oxidization of atomic hydrogen and plating processes wereascertained.（ii）The performances of the amperometric-type and potentiometric-typehydrogen sensors were studied and it was found out that the amperometric hydrogenpermeation sensor was more suitable to detect the hydrogen permeation rate.（iii）The leakage problem was solved using double electrolytes system when the sensorwas fixed. The correctness of measuring signal was verified by experiments.（iv）Theresult of field monitoring showed that the developed electrochemical monitoringsystem could realize the real-time, online and nondestructive detection of atomichydrogen concentration and the estimation of the susceptibility of hydrogen induced cracking.
引文
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