CN107817165A - Device for measuring stress corrosion behavior of steel in corrosion environment - Google Patents
Device for measuring stress corrosion behavior of steel in corrosion environment Download PDFInfo
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Abstract
Description
技术领域technical field
本发明具体涉及油气田材料测试领域,更具体地涉及一种用于测定钢材在腐蚀环境中应力腐蚀行为的装置。The invention specifically relates to the field of oil and gas field material testing, and more specifically relates to a device for measuring the stress corrosion behavior of steel in a corrosive environment.
背景技术Background technique
在油气田工业中,材料的服役环境变的复杂,导致材料在使用过程中,容易发生失效脆断等,而应力腐蚀开裂是众多腐蚀失效行为中的一种,因其产生的原因是材料在腐蚀环境中,在一定的拉应力的条件下,常在无明显预兆的情况下突然发生材料脆断,危害性极大,需要开展相关的实验测试进行评价。In the oil and gas field industry, the service environment of materials becomes more and more complex, which leads to the failure and brittle fracture of materials during use, and stress corrosion cracking is one of many corrosion failure behaviors, because the reason is that the material is corroded. In the environment, under certain tensile stress conditions, material brittle fracture often occurs suddenly without obvious warning, which is extremely harmful, and relevant experimental tests need to be carried out for evaluation.
慢应变拉伸作为应力腐蚀测试和评定方法,深受广大学者的认可,但因测试装置的原因,导致测试时腐蚀介质无法密封,使得其测试装置使用受限,仅仅能测试一些腐蚀介质是不挥发性的物质,且测试效果不理想,如测试氯离子应力腐蚀行为研究,对于挥发型腐蚀介质,无法进行应力腐蚀测试评定。As a stress corrosion test and evaluation method, slow strain tension is widely recognized by scholars. However, due to the reason of the test device, the corrosive medium cannot be sealed during the test, which makes the use of the test device limited. Only some corrosive media can be tested. Volatile substances, and the test results are not ideal, such as testing the stress corrosion behavior of chloride ions, for volatile corrosive media, stress corrosion test evaluation cannot be carried out.
发明内容Contents of the invention
为解决现有技术中腐蚀体系下材料的应力腐蚀评价由于腐蚀介质中有可挥发的气体,致使现使用的实验装置无法进行评价问题,本发明提供一种用于测定钢材在腐蚀环境中应力腐蚀行为的装置。In order to solve the problem that the stress corrosion evaluation of materials under the corrosion system in the prior art cannot be evaluated due to the volatile gas in the corrosion medium, the present invention provides a method for measuring the stress corrosion of steel in a corrosion environment. device of behavior.
本发明采用如下技术方案:一种用于测定钢材在腐蚀环境中应力腐蚀行为的装置,所述装置包括内壳、试样夹持装置、腐蚀介质通入系统;所述内壳为密封壳体;所述试样夹持装置包括设置在内壳底部的下部镍基合金样架、设置在内壳中部的上部镍基合金样架,该上部镍基合金样架上方固定不锈钢磁化介质;所述内壳上方依次设置压力传感器、电磁铁;所述内壳内充有腐蚀介质。The present invention adopts the following technical scheme: a device for measuring the stress corrosion behavior of steel in a corrosive environment, the device includes an inner shell, a sample holding device, and a corrosive medium feeding system; the inner shell is a sealed shell The sample clamping device includes a lower nickel-based alloy sample rack arranged at the bottom of the inner shell, an upper nickel-based alloy sample rack arranged at the middle of the inner shell, and a stainless steel magnetizing medium is fixed above the upper nickel-based alloy sample rack; A pressure sensor and an electromagnet are sequentially arranged above the inner shell; the inner shell is filled with a corrosive medium.
所述上部镍基合金样架与不锈钢磁化介质之间设置泡沫铝夹层。A foamed aluminum interlayer is set between the upper nickel-based alloy sample holder and the stainless steel magnetized medium.
所述装置包括温度测试系统,该系统包括电热丝、电偶室、热电偶,所述电热丝设置在内壁外侧用于加热拉伸试样所在区域的腐蚀介质;所述电偶室伸入内壳;所述热电偶插入电偶室。The device includes a temperature testing system, the system includes an electric heating wire, a galvanic couple chamber, and a thermocouple, and the electric heating wire is arranged on the outside of the inner wall for heating the corrosive medium in the area where the tensile sample is located; the galvanic couple chamber extends into the housing; the thermocouple is inserted into the couple chamber.
所述内壳外侧设置冷却管,该冷却管设置在不锈钢磁化介质和内壳顶部之间。A cooling pipe is arranged outside the inner shell, and the cooling pipe is arranged between the stainless steel magnetized medium and the top of the inner shell.
所述电热丝与冷却管外侧均设置泡沫铝。Aluminum foam is arranged on the outside of the heating wire and the cooling pipe.
所述泡沫铝外侧设置外壳。A shell is arranged on the outside of the foamed aluminum.
本发明利用电磁铁磁力进行慢应变拉伸的拉应力,使钢材在腐蚀环境中应力腐蚀行为的测试能够实现完成,尤其能够保证在慢应变拉伸过程中的高挥发性腐蚀介质密封性,充分保证了实验人员实验时的安全性,同时保证实验过程中腐蚀溶液中挥发性介质浓度的稳定性和精确性,使得测试出的实验结果精确性高。The invention utilizes the magnetic force of the electromagnet to carry out the tensile stress of the slow-strain stretching, so that the test of the stress corrosion behavior of the steel in the corrosive environment can be completed, and especially can ensure the sealing performance of the highly volatile corrosive medium in the slow-strain stretching process, fully It ensures the safety of the experimenters during the experiment, and at the same time ensures the stability and accuracy of the concentration of the volatile medium in the corrosion solution during the experiment, so that the accuracy of the experimental results is high.
附图说明Description of drawings
图1为本发明装置结构示意图。Fig. 1 is a schematic diagram of the structure of the device of the present invention.
符号说明Symbol Description
1、电磁铁;2、外壳;3、冷却水管;4、压力传感器;5、泡沫铝6、内壳;7、内壳顶部;8、腐蚀介质溶液;9、上部镍基合金样架;10、泡沫铝夹层;11、不锈钢磁化介质;12、上部样架固定螺栓;13、硫化氢通入管;14、硫化氢通入控制阀;15、热电偶室;16、热电偶;17、废液排放通道;18、废液排放控制阀;19、二氧化碳通入管;20、二氧化碳通入控制阀;21、碳酸钠溶液通入孔;22、碳酸钠溶液通入控制阀;23、下部镍基合金样架;24、下部样架固定螺栓;25、试样固定夹;26、电热丝;27、拉伸试样;28、内壳顶部固定螺栓。1. Electromagnet; 2. Shell; 3. Cooling water pipe; 4. Pressure sensor; 5. Aluminum foam 6. Inner shell; 7. Top of the inner shell; 8. Corrosion medium solution; 9. Upper nickel-based alloy sample holder; 10 1. Foamed aluminum interlayer; 11. Stainless steel magnetized medium; 12. Fixing bolts of the upper sample rack; 13. Hydrogen sulfide inlet pipe; 14. Hydrogen sulfide inlet control valve; 15. Thermocouple chamber; 16. Thermocouple; 17. Waste liquid Discharge channel; 18. Waste liquid discharge control valve; 19. Carbon dioxide inlet pipe; 20. Carbon dioxide inlet control valve; 21. Sodium carbonate solution inlet hole; 22. Sodium carbonate solution inlet control valve; 23. Lower nickel base alloy Sample rack; 24. Lower sample rack fixing bolts; 25. Sample fixing clamp; 26. Heating wire; 27. Tensile sample; 28. Fixing bolts at the top of the inner shell.
具体实施方式Detailed ways
下面结合附图和具体实施方式对本发明作进一步说明。The present invention will be further described below in conjunction with the accompanying drawings and specific embodiments.
一种用于测定钢材在腐蚀环境中应力腐蚀行为的装置,所述装置包括内壳6、试样夹持装置、腐蚀介质通入系统;所述内壳为密封壳体;所述试样夹持装置包括设置在内壳6底部的下部镍基合金样架23、设置在内壳6中部的上部镍基合金样架9,该上部镍基合金样架9上方固定不锈钢磁化介质11,所述内壳6上方依次设置压力传感器4、电磁铁1;所述内壳内充有腐蚀介质。A device for measuring the stress corrosion behavior of steel in a corrosive environment, the device includes an inner shell 6, a sample holding device, and a corrosive medium feeding system; the inner shell is a sealed shell; the sample holder The holding device includes a lower nickel-based alloy sample rack 23 arranged at the bottom of the inner shell 6, an upper nickel-based alloy sample rack 9 arranged at the middle of the inner shell 6, and a stainless steel magnetizing medium 11 is fixed above the upper nickel-based alloy sample rack 9, said A pressure sensor 4 and an electromagnet 1 are sequentially arranged above the inner shell 6; the inner shell is filled with a corrosive medium.
传统对试样的测试中,由于腐蚀气体在测试过程中难以控制,常常出现泄漏问题,危及工作人员身体健康,使试样在此环境下无法完成测试。基于此,本发明创新性地采用由电磁铁1、压力传感器4和不锈钢磁化介质11三者配合使用,对试样在腐蚀环境下的测试能够实现。In the traditional test of the sample, because the corrosive gas is difficult to control during the test process, leakage problems often occur, endangering the health of the staff, and the sample cannot be tested in this environment. Based on this, the present invention innovatively uses the electromagnet 1 , the pressure sensor 4 and the stainless steel magnetized medium 11 to be used together, so that the test of the sample in a corrosive environment can be realized.
所述上部镍基合金样架9与不锈钢磁化介质11之间设置泡沫铝夹层10。所述上部、下部镍基合金样架9、23固定试样底部,进一步优选的,在上、下部镍基合金样架23上设置试样固定夹25,用两个试样固定夹25分别将试样固定在上部镍基合金样架9和下部镍基合金样架23上,在上部镍基合金样架9中装入泡沫铝夹层10,上面放不锈钢磁化介质11,用上部样架固定螺栓12将上部镍基合金样架9、泡沫铝夹层10和不锈钢磁化介质11连接起来。泡沫铝夹层10位于不锈钢外壳2和镍基合金内壳6中间,起保温隔磁作用,整个密封系统起到封装腐蚀介质的作用。A foamed aluminum interlayer 10 is arranged between the upper nickel-based alloy sample rack 9 and the stainless steel magnetized medium 11 . The upper and lower nickel-based alloy sample racks 9, 23 fix the bottom of the sample, and further preferably, sample holders 25 are set on the upper and lower nickel-based alloy sample holders 23, and the two sample holders 25 are respectively used to fix the samples. The sample is fixed on the upper nickel-based alloy sample holder 9 and the lower nickel-based alloy sample holder 23, the foamed aluminum interlayer 10 is placed in the upper nickel-based alloy sample holder 9, the stainless steel magnetization medium 11 is placed on it, and the upper sample holder is used to fix the bolts 12 Connect the upper nickel base alloy sample holder 9, the aluminum foam interlayer 10 and the stainless steel magnetized medium 11. The foamed aluminum interlayer 10 is located between the stainless steel outer shell 2 and the nickel-based alloy inner shell 6, which plays the role of heat preservation and magnetic isolation, and the entire sealing system plays the role of sealing the corrosive medium.
所述装置包括温度测试系统,该系统包括电热丝26、电偶室15、热电偶16,所述电热丝26设置在内壁外侧用于加热拉伸试样所在区域的腐蚀介质;所述电偶室15伸入内壳;所述热电偶16插入电偶室15,通过通过温度反馈控制电热丝26,使得测试温度均衡。Described device comprises temperature test system, and this system comprises heating wire 26, galvanic couple chamber 15, thermocouple 16, and described heating wire 26 is arranged on the outside of inner wall and is used for heating the corrosive medium in the area where tensile sample is located; The chamber 15 protrudes into the inner shell; the thermocouple 16 is inserted into the thermocouple chamber 15, and the heating wire 26 is controlled through temperature feedback to make the test temperature equalize.
所述内壳外侧设置冷却管3,该冷却管3设置在不锈钢磁化介质11和内壳顶部7之间,冷却水管3保持内壳上部温度在室温状态。使内壳上部温度在室温状态是为了保证上部的电磁铁和不锈钢导磁之间的磁场和电磁力是受温度影响的,温度太高会导致电磁力下降,会造成拉伸力不足的状态。A cooling pipe 3 is arranged on the outside of the inner shell, and the cooling pipe 3 is arranged between the stainless steel magnetized medium 11 and the top 7 of the inner shell, and the cooling water pipe 3 keeps the temperature of the upper part of the inner shell at room temperature. Keeping the temperature of the upper part of the inner shell at room temperature is to ensure that the magnetic field and electromagnetic force between the upper electromagnet and the stainless steel magnetic conductor are affected by temperature. If the temperature is too high, the electromagnetic force will decrease and the tensile force will be insufficient.
所述电热丝26与冷却管3外侧均设置泡沫铝5。利用泡沫铝的隔磁性和保温性,可保证实验人员电磁辐射,并可保证试样所处环境的温度的保持稳定。Aluminum foam 5 is provided on the outside of the heating wire 26 and the cooling pipe 3 . Utilizing the magnetic isolation and thermal insulation properties of foamed aluminum, it can ensure the electromagnetic radiation of the experimenters, and can ensure the stability of the temperature of the environment where the sample is located.
所述泡沫铝5外侧设置外壳2。The shell 2 is arranged on the outside of the foamed aluminum 5 .
工作过程:打开内壳顶部7,将拉伸试样27用试样固定夹25固定在下部镍基合金样架上,倒入含氯化钠的溶液于镍基合金内壳6中,再用试样固定夹25将拉伸试样27固定在上部镍基合金样架9上,在上部镍基合金样架9中装入泡沫铝夹层10,上面放不锈钢磁化介质11,用上部样架固定螺栓12将上部镍基合金样架9、泡沫铝夹层10和不锈钢磁化介质11连接起来;再倒入含氯化钠的溶液,盖上内壳顶部7,用内壳顶部7固定螺栓密封紧密;内壳顶部7上放压力传感器4,压力传感器4上放电磁铁1。Working process: open the top 7 of the inner shell, fix the tensile sample 27 on the lower nickel-based alloy sample holder with the sample fixing clip 25, pour the solution containing sodium chloride into the nickel-based alloy inner shell 6, and then use The sample fixing clamp 25 fixes the tensile sample 27 on the upper nickel-based alloy sample holder 9, puts the foamed aluminum interlayer 10 in the upper nickel-based alloy sample holder 9, puts the stainless steel magnetizing medium 11 on it, and fixes it with the upper sample holder The bolt 12 connects the upper nickel-based alloy sample holder 9, the foamed aluminum interlayer 10 and the stainless steel magnetized medium 11; then pour the solution containing sodium chloride, cover the top 7 of the inner shell, and seal it tightly with the fixing bolts on the top 7 of the inner shell; A pressure sensor 4 is placed on the top 7 of the inner shell, and a magnet 1 is placed on the pressure sensor 4 .
打开碳酸钠溶液通入控制阀22、在碳酸钠溶液通入孔21处通入氮气,清除腐蚀介质中的氧;关闭控制阀22打开硫化氢通入控制阀14,在硫化氢通入入口13上通入硫化氢;打开二氧化碳通入控制阀20,在二氧化碳通入孔19上通入二氧化碳。保持硫化氢的压力和二氧化碳压力,形成三元腐蚀体系。Open the sodium carbonate solution and feed the control valve 22, feed nitrogen at the sodium carbonate solution feed hole 21, remove the oxygen in the corrosive medium; close the control valve 22 and open the hydrogen sulfide feed control valve 14, and feed the hydrogen sulfide into the inlet 13 Pass into hydrogen sulfide; Open the carbon dioxide feed control valve 20, feed carbon dioxide on the carbon dioxide feed hole 19. Maintain the pressure of hydrogen sulfide and carbon dioxide to form a ternary corrosion system.
在热电偶室15中插入热电偶16,电热丝26通电流加热,通过温度反馈控制电热丝26,使得测试温度达到实验要求,同时开冷却水管3保持上部温度在室温状态。Insert a thermocouple 16 into the thermocouple chamber 15, heat the heating wire 26 with current, control the heating wire 26 through temperature feedback, so that the test temperature meets the experimental requirements, and at the same time open the cooling water pipe 3 to keep the upper temperature at room temperature.
电磁铁1通电,磁化不锈钢磁化介质11,吸引不锈钢磁化介质11,进而带动上部镍基合金样架9拉动拉伸试样27,使其受到拉应力,在腐蚀介质中受到应力腐蚀,通过力传感器4反馈调节电磁铁1的电流进而控制电磁铁的吸力;并设置力值和记录力值。The electromagnet 1 is energized to magnetize the stainless steel magnetized medium 11, attract the stainless steel magnetized medium 11, and then drive the upper nickel-based alloy sample holder 9 to pull the tensile sample 27, so that it is subjected to tensile stress and subjected to stress corrosion in the corrosive medium, through the force sensor 4 Feedback to adjust the current of the electromagnet 1 to control the suction force of the electromagnet; and set and record the force value.
拉伸试样27拉断后,关闭硫化氢通入控制阀14和二氧化碳通入控制阀20,打开废液排放控制阀18,用废液排放孔17将腐蚀废液排至碳酸钠溶液中或氢氧化钠溶液中;待容器内的腐蚀介质快排完时,打开碳酸钠溶液通入控制阀22,对装置中通入少量的碳酸钠溶液,再通过废液排放孔17排除废液,这样5-6次后,可开装置,去除拉伸试样27,进行断口分析。After the tensile sample 27 is broken, close the hydrogen sulfide feed control valve 14 and the carbon dioxide feed control valve 20, open the waste liquid discharge control valve 18, and use the waste liquid discharge hole 17 to discharge the corrosion waste liquid into the sodium carbonate solution or hydrogen In the sodium oxide solution; when the corrosive medium in the container is almost exhausted, open the sodium carbonate solution and feed the control valve 22, feed a small amount of sodium carbonate solution into the device, and then get rid of the waste liquid through the waste liquid discharge hole 17, so that 5 After -6 times, the device can be opened to remove the tensile sample 27 for fracture analysis.
由于油气田腐蚀环境较为复杂,常常伴有多类腐蚀介质,相互影响,对材料的应力腐蚀评价提出了更高的要求,而H2S、CO2、Cl-腐蚀作为作为主要的几种腐蚀环境,其组成的腐蚀介质体系H2S-CO2-Cl-三元腐蚀体系下材料的应力腐蚀评价由于腐蚀介质中有可挥发的H2S和CO2气体,无法密封,致使现使用的实验装置无法进行评价,致使H2S-CO2-Cl-三元腐蚀体系下的材料选择变的困难,本发明尤其适用于H2S-CO2-Cl-三元腐蚀体系。Due to the complex corrosion environment of oil and gas fields, often accompanied by multiple types of corrosion media, which interact with each other, higher requirements are put forward for the evaluation of stress corrosion of materials, and H 2 S, CO 2 , Cl - corrosion are the main corrosion environments , the stress corrosion evaluation of materials under the corrosive medium system H 2 S-CO 2 -Cl - ternary corrosion system. Because there are volatile H 2 S and CO 2 gases in the corrosive medium, they cannot be sealed, so the current experiment The device cannot be evaluated, which makes it difficult to select materials under the H 2 S-CO 2 -Cl - ternary corrosion system. The present invention is especially suitable for the H 2 S-CO 2 -Cl - ternary corrosion system.
当腐蚀介质是H2S-CO2-Cl-三元腐蚀体系时,所述腐蚀介质通过腐蚀介质通入系统进入内壳6。所述腐蚀介质通入系统包括二氧化碳通入管20、废液排放通道17、硫化氢通入管13、碳酸钠溶液通入管21,所述腐蚀介质通入系统设置在上部镍基合金样架9与下部镍基合金样架23之间;所述二氧化碳通入管20上设置二氧化碳通入控制阀20;硫化氢通入管13上设置硫化氢通入控制阀14;碳酸钠溶液通入管21上设置碳酸钠溶液通入控制阀22;废液排放通道17上设置废液排放控制阀18。When the corrosive medium is H 2 S—CO 2 —Cl — ternary corrosion system, the corrosive medium enters the inner shell 6 through the corrosive medium feeding system. The corrosive medium feeding system includes a carbon dioxide feeding pipe 20, a waste liquid discharge channel 17, a hydrogen sulfide feeding pipe 13, and a sodium carbonate solution feeding pipe 21. The corrosive medium feeding system is arranged on the upper nickel base alloy sample rack 9 and the lower Between nickel-based alloy sample racks 23; carbon dioxide inlet control valve 20 is set on the carbon dioxide inlet pipe 20; hydrogen sulfide inlet control valve 14 is arranged on the hydrogen sulfide inlet pipe 13; sodium carbonate solution is arranged on the sodium carbonate solution inlet pipe 21 Lead into the control valve 22; the waste liquid discharge control valve 18 is set on the waste liquid discharge channel 17.
本发明利用电磁铁磁力进行慢应变拉伸的拉应力,可保证在慢应变拉伸过程中的高挥发性腐蚀介质密封性,充分保证了实验人员实验时的安全性,同时保证实验过程中腐蚀溶液中挥发性介质浓度的稳定性和精确性,使得测试出的实验结果具有精确性;利用泡沫铝的隔磁性和保温性,可保证实验人员电磁辐射,并可保证试样所处环境的温度的保持稳定;本发明可进行材料在不同温度、不同浓度条件下载H2S-CO2-Cl-三元腐蚀体系的应力腐蚀测试及评定,克服了其他设备无法进行不同温度、不同浓度条件复杂的多元含硫化氢应力腐蚀测试,适应性广。The invention utilizes the magnetic force of the electromagnet to carry out the tensile stress of the slow-strain stretching, which can ensure the sealing performance of the highly volatile corrosive medium during the slow-strain stretching process, fully guarantee the safety of the experimenters during the experiment, and at the same time ensure the corrosion during the experiment process The stability and accuracy of the concentration of the volatile medium in the solution makes the experimental results accurate; the use of the foamed aluminum's magnetic isolation and thermal insulation can ensure the electromagnetic radiation of the experimenters and the temperature of the environment where the sample is located. stable; the present invention can carry out the stress corrosion test and evaluation of the H 2 S-CO 2 -Cl - ternary corrosion system of materials under different temperature and different concentration conditions, which overcomes the complicated conditions of different temperatures and different concentrations that cannot be performed by other equipment The multi-component hydrogen sulfide-containing stress corrosion test has wide adaptability.
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