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CN103926146A - Constant-load stress corrosion testing device of small test sample and testing method thereof - Google Patents

Constant-load stress corrosion testing device of small test sample and testing method thereof
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CN103926146A
CN103926146ACN201410147919.3ACN201410147919ACN103926146ACN 103926146 ACN103926146 ACN 103926146ACN 201410147919 ACN201410147919 ACN 201410147919ACN 103926146 ACN103926146 ACN 103926146A
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stress
corrosion
corrosion test
loading
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CN103926146B (en
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曾德智
侯铎
张智
施太和
黄黎明
谷坛
扈俊颖
邓文良
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Southwest Petroleum University
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Abstract

Translated fromChinese

本发明涉及一种小试样恒载荷应力腐蚀评价方法及装置,其要点在于能够测试薄壁管、小尺寸构件抗应力腐蚀开裂特性,设计加工小尺寸试样,准确控制加载的拉伸应力水平,在酸性环境中进行应力腐蚀实验,根据实验结果对薄壁管、小尺寸构件在酸性腐蚀环境中抗硫化物应力腐蚀性能及作用机理进行评价研究。利用该评价方法和装置可测定无法加工标准试样的薄壁管、小尺寸构件抗应力腐蚀开裂特征,根据测试结果得出构件材质的适用性,从而对薄壁管、小尺寸构件进行选材和适用性评价。

The present invention relates to a constant load stress corrosion evaluation method and device for small samples. The main point is to test the stress corrosion cracking resistance of thin-walled pipes and small-sized components, design and process small-sized samples, and accurately control the tensile stress level of loading. , stress corrosion experiments were carried out in acidic environment, and according to the experimental results, the performance and mechanism of sulfide stress corrosion resistance of thin-walled pipes and small-sized components in acidic corrosion environment were evaluated and studied. The evaluation method and device can be used to measure the stress corrosion cracking resistance characteristics of thin-walled tubes and small-sized components that cannot be processed by standard samples, and the applicability of component materials can be obtained according to the test results, so as to select materials and Applicability evaluation.

Description

Translated fromChinese
一种小试样恒载荷应力腐蚀测试装置及其测试方法A small sample constant load stress corrosion test device and test method thereof

技术领域technical field

本发明涉及一种用于油气田薄壁管、小尺寸构件等无法加工标准试样的构件进行恒载荷应力腐蚀评价的实验方法,本发明还涉及使用该方法测试薄壁管、小尺寸构件应力腐蚀特性的实验装置。The present invention relates to an experimental method for constant load stress corrosion evaluation of components such as thin-walled pipes and small-sized components in oil and gas fields that cannot be processed by standard samples. The present invention also relates to using the method to test stress corrosion of thin-walled pipes and small-sized components. characteristic experimental setup.

背景技术Background technique

在金属材料化学实验中,需要对石油工业、化学工业中用于薄壁管、小尺寸构件等无法加工标准试样的构件进行恒载荷应力腐蚀实验,从而对构件在应力状态和腐蚀环境中进行材质优选和适用性评价。目前国内外恒载荷应力腐蚀实验一般方法是按照标准NACE0177采用应力环进行A法实验,试样尺寸φ6.35×110mm,最小夹持端直径10mm;而紧凑试样为φ3.81×110mm,最小夹持端直径5mm。对于壁厚小于4mm的薄壁管、小尺寸构件无法加工以上试样,且加工过程中易对试样本身造成力学性能损伤,评价结果与现场结果相差较大,不能为实际工况环境中构件材质的优选和适用性评价提供可靠依据。因而对于这些特殊小尺寸部位目前标准实验方法,试样尺寸参数均不能满足现场要求。In the chemical experiment of metal materials, it is necessary to conduct constant load stress corrosion experiments on components that cannot be processed with standard samples such as thin-walled pipes and small-sized components in the petroleum industry and chemical industry, so as to test the components in the stress state and corrosion environment. Material selection and applicability evaluation. At present, the general method of constant load stress corrosion test at home and abroad is to use the stress ring to carry out the A method experiment according to the standard NACE0177. The sample size is φ6.35×110mm, and the minimum clamping end diameter is 10mm; The clamping end diameter is 5mm. For thin-walled pipes and small-sized components with a wall thickness of less than 4mm, the above samples cannot be processed, and the mechanical properties of the samples themselves are easy to be damaged during the processing. It provides a reliable basis for material selection and applicability evaluation. Therefore, for these special small-sized parts, the current standard experimental methods and sample size parameters cannot meet the site requirements.

在石油和化工行业中腐蚀问题日趋严重,尤其是薄壁管、小尺寸构件均在一定应力状态下,在酸性腐蚀环境中服役。目前这些特殊部位的应力腐蚀实验评价在学术上和工程技术上具有极其重要的价值,由于缺乏相应的实验方法和装置,导致相应的评价实验不能进行。常规的应力腐蚀实验通过应力环对金属材料加载,小尺寸特殊部位无法加工试样,因而无法进行小尺寸部位的应力腐蚀实验,因而这些部位的金属材料选材没有标准实验方法和适用性评价依据,导致现场选材困难,甚至出现由于选材不合理导致的应力腐蚀开裂事故。Corrosion problems are becoming more and more serious in the petroleum and chemical industries, especially thin-walled pipes and small-sized components are all under a certain stress state and serve in acidic corrosion environments. At present, the stress corrosion test evaluation of these special parts has extremely important value in academic and engineering technology. Due to the lack of corresponding experimental methods and devices, the corresponding evaluation experiments cannot be carried out. Conventional stress corrosion experiments load metal materials through stress rings, and small-sized special parts cannot process samples, so stress corrosion experiments for small-sized parts cannot be carried out. Therefore, there is no standard experimental method and applicability evaluation basis for the selection of metal materials in these parts. This leads to difficulty in material selection on site, and even stress corrosion cracking accidents caused by unreasonable material selection.

目前,常规的恒载荷应力腐蚀实验方法存在以下不足:At present, the conventional constant load stress corrosion test method has the following deficiencies:

(A)试样尺寸较大,不适用于薄壁管、小尺寸构件抗应力腐蚀性能测试;(A) The size of the sample is large, which is not suitable for the stress corrosion resistance test of thin-walled pipes and small-sized components;

(B)小尺寸部位强制加工为标准试样造成力学性能损伤,实验结果可靠性和现场参考价值降低;(B) Forced processing of small-sized parts into standard samples causes damage to mechanical properties, reducing the reliability of experimental results and the value of on-site reference;

(C)检测装置不适用于小尺寸试样的测试,载荷量程过大造成载荷的不准确,实验过程中无法实时监控试样载荷大小。(C) The detection device is not suitable for the test of small-sized samples, and the load range is too large to cause inaccurate loads, and it is impossible to monitor the sample load in real time during the experiment.

为解决常规恒载荷应力腐蚀实验不能进行小尺寸试样应力腐蚀实验的问题,本发明借助应力环,提出了小试样恒载荷应力腐蚀评价方法,设计小尺寸应力腐蚀实验的试样夹持、加载装置,形成适用于小尺寸试样恒载荷应力腐蚀新型实验方法,能够很好的解决上述问题。In order to solve the problem that the conventional constant load stress corrosion test cannot carry out the small size sample stress corrosion test, the present invention proposes a small sample constant load stress corrosion evaluation method with the help of the stress ring, and designs the sample clamping, The loading device forms a new experimental method suitable for constant load stress corrosion of small-sized samples, which can well solve the above problems.

发明内容Contents of the invention

本发明要解决的技术问题是针对现有技术的不足,提供一种能够较真实反映现场工况、用于测定薄壁管、小尺寸构件恒载荷应力腐蚀实验的方法。The technical problem to be solved by the present invention is to provide a method for measuring constant load stress corrosion tests of thin-walled pipes and small-sized components that can truly reflect on-site working conditions for the deficiencies of the prior art.

本发明要解决的另一技术问题是提供一种结构简单、易于操作、安全可靠、能够方便地进行多组平行实验、用于模拟小尺寸试样恒载荷应力腐蚀实验所用的夹持装置。Another technical problem to be solved by the present invention is to provide a clamping device that is simple in structure, easy to operate, safe and reliable, can conveniently carry out multiple parallel experiments, and is used for simulating small-sized sample constant load stress corrosion experiments.

本发明是通过如下技术方案实现:The present invention is realized through the following technical solutions:

一种小试样恒载荷应力腐蚀测试装置,其特征在于该装置包括以下部件:位移传感器(1)、加载螺杆(2)、固定螺杆(3)、底座(4)、应力环(7)、应力测定试样(9)、腐蚀试验腔(12)、试样(16)和实验介质(17);A small sample constant load stress corrosion test device, characterized in that the device includes the following components: displacement sensor (1), loading screw (2), fixing screw (3), base (4), stress ring (7), Stress measurement sample (9), corrosion test chamber (12), sample (16) and experimental medium (17);

所述应力环(7)通过固定螺杆(3)由固定螺母(5)固定在底座(4)上,该应力环(7)内部具有腐蚀试验腔(12),该腐蚀试验腔(12)装有实验介质(17)和试样(16),所述固定螺杆(3)的U型夹具端穿过腐蚀试验腔(12)的底部并固定试样(16)的下部,所述固定螺杆(3)和腐蚀试验腔(12)之间具有下密封环(18)。The stress ring (7) is fixed on the base (4) by the fixing nut (5) through the fixing screw (3). The stress ring (7) has a corrosion test chamber (12) inside, and the corrosion test chamber (12) is equipped with There is an experimental medium (17) and a sample (16), the U-shaped clamp end of the fixing screw (3) passes through the bottom of the corrosion test chamber (12) and fixes the lower part of the sample (16), the fixing screw ( 3) There is a lower sealing ring (18) between the corrosion test chamber (12).

所述加载螺杆(2)通过加载螺母(6)穿过应力环(7)的上部和应力测定试样(9)的一端连接,该应力测定试样(9)的另一端为U型夹具端,所述应力测定试样(9)的U型夹具端穿过腐蚀试验腔(12)的上部并固定试样(16)的上部,所述加载螺杆(2)和腐蚀试验腔(12)之间具有上密封环(11),所述应力测定试样(9)的尺寸与试样(16)相同,并在该应力测定试样(9)的中部安装应变片(10)。The loading screw (2) passes through the upper part of the stress ring (7) through the loading nut (6) and is connected to one end of the stress measurement sample (9), and the other end of the stress measurement sample (9) is a U-shaped clamp end , the U-shaped clamp end of the stress measurement sample (9) passes through the upper part of the corrosion test chamber (12) and fixes the upper part of the sample (16), the loading screw (2) and the corrosion test chamber (12) There is an upper sealing ring (11) between them, the size of the stress measurement sample (9) is the same as that of the sample (16), and a strain gauge (10) is installed in the middle of the stress measurement sample (9).

所述底座(4)具有一支架,该支架上安装有位移传感器(1),该位移传感器(1)位于应力环(7)的上部。The base (4) has a bracket on which a displacement sensor (1) is installed, and the displacement sensor (1) is located on the upper part of the stress ring (7).

所述上密封环(11)和下密封环(18)与腐蚀试验腔(12)间安装密封圈(13);所述应力测定试样(9)的U型夹具端和固定螺杆(3)的U型夹具端通过销钉(20)固定试样(16)。A sealing ring (13) is installed between the upper sealing ring (11) and the lower sealing ring (18) and the corrosion test chamber (12); the U-shaped clamp end of the stress measurement sample (9) and the fixing screw (3) The end of the U-shaped clamp fixes the sample (16) through a pin (20).

所述应力测定试样(9)的U型夹具端和固定螺杆(3)的U型夹具端与试样(16)之间具有绝缘垫片(19),该绝缘垫片(19)为聚四氟乙烯材质;所述加载螺杆(2)、固定螺杆(3)、固定螺母(5)、加载螺母(6)、应力环(7)和销钉(20)是由耐腐蚀性能的哈氏合金加工而成。There is an insulating gasket (19) between the U-shaped clamp end of the stress measurement sample (9) and the U-shaped clamp end of the fixing screw (3) and the sample (16), and the insulating gasket (19) is poly Tetrafluoroethylene material; the loading screw (2), fixing screw (3), fixing nut (5), loading nut (6), stress ring (7) and pin (20) are made of corrosion-resistant Hastelloy processed.

所述加载螺母(6)和应力环(7)之间具有旋转垫片(8),该旋转垫片(8)由耐腐蚀性能的哈氏合金加工而成。There is a rotating washer (8) between the loading nut (6) and the stress ring (7), and the rotating washer (8) is processed from corrosion-resistant Hastelloy alloy.

所述腐蚀试验腔(12)还具有进气口(14)和出气口(15)。The corrosion test chamber (12) also has an air inlet (14) and an air outlet (15).

所其试样(16)为扁平矩形试样,其厚度为0.9mm~2mm,宽度为3mm~5mm。The sample (16) is a flat rectangular sample with a thickness of 0.9 mm to 2 mm and a width of 3 mm to 5 mm.

所述实验介质(17)为腐蚀介质。The experimental medium (17) is a corrosive medium.

一种采用如前所述的小试样恒载荷应力腐蚀测试装置进行腐蚀测试的方法,其特征在于包括以下步骤:A kind of method that adopts small sample constant load stress corrosion testing device as mentioned above to carry out corrosion test is characterized in that comprising the following steps:

步骤一,根据所需模拟现场工况条件设计实验腐蚀介质、试样加载载荷大小;Step 1, design the experimental corrosion medium and the load size of the sample according to the required simulated on-site working conditions;

步骤二,安装试样(16),通过加载螺杆(2)加载应力,通过位移传感器(1)和应变片(10)确定载荷;Step 2, install the sample (16), load the stress through the loading screw (2), and determine the load through the displacement sensor (1) and the strain gauge (10);

步骤三,将腐蚀介质加入腐蚀实验腔(12)中,将进气口(14)、出气口(15)分别连接至H2S、CO2或N2气瓶和废气处理系统;Step 3, adding the corrosive medium into the corrosion test chamber (12), connecting the gas inlet (14) and the gas outlet (15) to theH2S ,CO2 orN2 gas cylinder and the waste gas treatment system respectively;

步骤四,腐蚀实验腔(12)中腐蚀介质进行充分除氧后,通入H2S或CO2等腐蚀性气体,记录时间开始实验,所述试验时间为720h;Step 4: After the corrosive medium in the corrosion test chamber (12) is fully deoxidized, the corrosive gas such as H2 S or CO2 is introduced, and the test is started after recording the time, and the test time is 720 hours;

步骤五,实验结束后,进行充分除氧,将试样(16)卸下,观察试样是否断裂并进行裂纹检测、试样表面腐蚀形貌和腐蚀产物分析。Step 5, after the experiment, fully deoxidize, remove the sample (16), observe whether the sample is broken, and perform crack detection, sample surface corrosion morphology and corrosion product analysis.

有益效果:Beneficial effect:

(A)试样尺寸小,便于加工;(A) The sample size is small and easy to process;

(B)能够同时利用应变片和位移传感器检测载荷,保障加载载荷的精确性。(B) The strain gauge and the displacement sensor can be used to detect the load at the same time, so as to ensure the accuracy of the loaded load.

(C)实验过程中可实时监控试样是否发生形变以及位移随时间变化的关系曲线。(C) During the experiment, it is possible to monitor in real time whether the sample is deformed and the relationship curve of the displacement with time.

附图说明Description of drawings

下面结合附图及实施方式对本发明作进一步详细的说明:Below in conjunction with accompanying drawing and embodiment the present invention is described in further detail:

图1是实现本发明的主要装置结构示意图。Fig. 1 is a structural schematic diagram of the main device for realizing the present invention.

图2是实现本发明的试样夹持部位示意图。Fig. 2 is a schematic diagram of the sample clamping part for realizing the present invention.

图3是实现本发明的小试样加工尺寸图。Fig. 3 is a processing dimension diagram of a small sample of the present invention.

图4是本发明加载载荷与常规方法载荷大小对比图。Fig. 4 is a comparison chart of the loading load of the present invention and that of the conventional method.

具体实施方式Detailed ways

下面结合具体实施例,进一步阐述本发明。Below in conjunction with specific embodiment, further illustrate the present invention.

参阅图1所示,本发明中一种小试样恒载荷应力腐蚀实验装置,主要包括位移传感器(1)、加载螺杆(2)、固定螺杆(3)、底座(4)、固定螺母(5)、加载螺母(6)、应力环(7)、旋转垫片(8)、应力测定试样(9)、应变片(10)、上密封环(11)、腐蚀实验腔(12)、密封圈(13)、进气口(14)、出气口(15)、试样(16)、实验介质(17)、下密封环(18)、绝缘垫片(19)、销钉(20);所述的应力环(7)上、下部分别设有内螺纹,下部通过固定螺杆(3)、固定螺母(5)牢牢固定在底座(4)上,上部通过应力测定试样(9)、加载螺母(6)、旋转垫片(8)进行加载;所述的加载螺杆(2)下端设有应力测定试样(9),大小、尺寸与试样(16)相同,平行部位设置有应变片(10),从而实时监测加载应力的大小;所述的应力环(7)加载挠度通过位移传感器(1)测定并实时记录;所述的试样(16)设置在腐蚀实验腔(12)中,被实验介质(17)完全浸没,通过加载螺杆(2)、固定螺杆(3)连接并进行加载,通过上密封环(11)、下密封环(18)以及密封圈(13)密封,形成封闭系统;所述的腐蚀实验腔(12)上设置有进气口(14)和出气口(15),可持续通入腐蚀性气体;所述的试样(16)上端与加载螺杆(2)通过销钉(20)连接,下端与固定螺杆(3)通过销钉(20)连接,试样(16)与加载螺杆(2)、固定螺杆(3)之间设置有绝缘垫片(19),从而避免电偶因素造成的实验误差,使实验结果准确可靠。Referring to shown in Fig. 1, a kind of small sample constant load stress corrosion test device among the present invention mainly comprises displacement sensor (1), loading screw rod (2), fixed screw rod (3), base (4), fixed nut (5 ), loading nut (6), stress ring (7), rotating washer (8), stress measurement sample (9), strain gauge (10), upper sealing ring (11), corrosion test chamber (12), sealing ring (13), air inlet (14), air outlet (15), sample (16), test medium (17), lower sealing ring (18), insulating gasket (19), pin (20); The upper and lower parts of the stress ring (7) are respectively provided with internal threads, the lower part is firmly fixed on the base (4) by the fixing screw (3) and the fixing nut (5), and the upper part is fixed by the stress measurement sample (9), loading The nut (6) and the rotating washer (8) are loaded; the lower end of the loading screw (2) is provided with a stress measurement sample (9), which is the same size and dimension as the sample (16), and the parallel part is provided with a strain gauge (10), so as to monitor the size of the loading stress in real time; the loading deflection of the stress ring (7) is measured and recorded in real time by the displacement sensor (1); the sample (16) is arranged in the corrosion test cavity (12) , is completely submerged by the experimental medium (17), connected and loaded by the loading screw (2) and the fixed screw (3), and sealed by the upper sealing ring (11), the lower sealing ring (18) and the sealing ring (13), forming Closed system; said corrosion test chamber (12) is provided with an air inlet (14) and an air outlet (15), which can be continuously fed into corrosive gas; the upper end of said sample (16) is connected with the loading screw (2 ) is connected by a pin (20), the lower end is connected with the fixed screw (3) by a pin (20), and an insulating gasket (19) is arranged between the sample (16) and the loading screw (2) and the fixed screw (3), In this way, experimental errors caused by galvanic factors are avoided, and the experimental results are accurate and reliable.

本发明中一种小试样恒载荷应力腐蚀评价方法如下。A small sample constant load stress corrosion evaluation method in the present invention is as follows.

(A)现场工况条件模拟化,具体方法如下:(A) Simulation of on-site working conditions, the specific method is as follows:

(a)根据现场工况条件确定气相、液相组分,通过腐蚀实验腔(12)容积计算液相组分的配制,以及通入H2S、CO2等腐蚀性气体的速度;(a) Determine the gas phase and liquid phase components according to the on-site working conditions, calculate the preparation of the liquid phase components according to the volume of the corrosion test chamber (12), and the speed of introducing corrosive gases such as H2 S and CO2 ;

(b)按照现场构件受力条件,根据其所受应力或应变大小选择加载载荷大小。(b) According to the force conditions of the components on site, select the load size according to the stress or strain.

(B)安装夹具及加载过程,具体方法如下:(B) Installation fixture and loading process, the specific method is as follows:

(a)将试样(16)上端于应力测定试样(9)下端通过销钉(20)连接,用绝缘垫片(19)将试样(16)与应力测定试样(9)绝缘,试样(16)下端于固定螺杆(3)通过销钉(20)连接,同样用绝缘垫片(19)进行绝缘,然后将密封圈(13)和上密封环(11)、下密封环(18)分别安装在应力测定试样(9)下端和固定螺杆(3)上端,整体放入腐蚀实验腔(12)中并拧紧上密封环(11)和下密封环(18)以保证密封,使用固定螺母(5)将固定螺杆(3)、应力环(7)固定于底座(4)上,使用加载螺杆(2)和加载螺母(6)将应力测定试样(9)上端固定,将应变片(10)贴在应力测定试样(9)平行段,安装位移传感器(1)按照实验设计应力开始加载,记录相关数据,同时观察位移传感器(1)和应变片(10)的读数以确保试样(16)加载载荷的准确性;(a) Connect the upper end of the sample (16) to the lower end of the stress measurement sample (9) through a pin (20), and use an insulating gasket (19) to insulate the sample (16) from the stress measurement sample (9). The lower end of the sample (16) is connected to the fixed screw rod (3) through a pin (20), and is also insulated with an insulating gasket (19), and then the sealing ring (13), the upper sealing ring (11), and the lower sealing ring (18) They are respectively installed on the lower end of the stress measurement sample (9) and the upper end of the fixed screw (3), put them into the corrosion test chamber (12) as a whole and tighten the upper sealing ring (11) and the lower sealing ring (18) to ensure the sealing. The nut (5) fixes the fixing screw (3) and the stress ring (7) on the base (4), uses the loading screw (2) and the loading nut (6) to fix the upper end of the stress measurement sample (9), and the strain gauge (10) Stick it on the parallel section of the stress measurement sample (9), install the displacement sensor (1) start loading according to the experimental design stress, record the relevant data, and observe the readings of the displacement sensor (1) and the strain gauge (10) at the same time to ensure that the test Sample (16) load accuracy;

(b)将腐蚀介质加入腐蚀实验腔(12)中,将进气口(14)、出气口(15)分别连接在H2S、CO2或N2气瓶和废气处理系统;(b) Add the corrosive medium to the corrosion test chamber (12), and connect the gas inlet (14) and the gas outlet (15) to theH2S ,CO2 orN2 gas cylinder and the exhaust gas treatment system respectively;

(C)腐蚀实验腔(12)中腐蚀介质进行充分除氧后,通入H2S或CO2等腐蚀性气体,记录时间开始实验。(C) After the corrosive medium in the corrosion test chamber (12) is fully deoxidized, the corrosive gas such as H2 S or CO2 is introduced, and the test is started after recording the time.

(D)实验结束后,进行充分除氧,将试样(16)卸下,观察试样是否断裂并进行裂纹检测、试样表面腐蚀形貌和腐蚀产物分析,具体方法如下:(D) After the experiment is over, fully deoxidize, the sample (16) is unloaded, observe whether the sample is broken and carry out crack detection, sample surface corrosion morphology and corrosion product analysis, the specific methods are as follows:

(a)若试样(16)断裂,清洗断口进行断口形貌观察及作用机理分析得出实验报告;(a) If the sample (16) breaks, clean the fracture, observe the fracture morphology and analyze the mechanism of action to obtain an experiment report;

(b)若试样(16)没有断裂,首先进行试样表面腐蚀形貌、腐蚀产物膜分析;然后清洗腐蚀产物,观察试样基体腐蚀状态,分析总结得出实验报告。(b) If the sample (16) is not broken, first analyze the corrosion morphology and corrosion product film on the surface of the sample; then clean the corrosion product, observe the corrosion state of the sample substrate, analyze and summarize the test report.

实例1采用小试样进行常规应力腐蚀测试Example 1 uses a small sample for conventional stress corrosion testing

对某金属复合管抗应力腐蚀性能进行测试,首先按照图3尺寸加工试样6件,试样厚度可根据复合管壁厚进行相应调整,将其安装于应力腐蚀实验装置,具体加载数据如表1。To test the stress corrosion resistance of a certain metal composite pipe, first process 6 samples according to the size shown in Figure 3. The thickness of the sample can be adjusted accordingly according to the wall thickness of the composite pipe, and it is installed in the stress corrosion test device. The specific loading data is shown in the table 1.

实验720小时后,清洗试样进行形貌观察与显微分析发现,6个试样均未发生断裂,但不同部位出现一定程度损伤,其中试件1和试件2宏观表面无损伤,试件4有明显开裂的宏观裂纹,试件6表面出现鱼鳞状损伤,试件3和试件5表面有不规则宏观损伤,通过试样损伤程度可判定材料在该环境下抵抗应力腐蚀的性能。After 720 hours of the experiment, the samples were cleaned for morphology observation and microscopic analysis. It was found that none of the six samples were broken, but a certain degree of damage occurred in different parts. Among them, there was no damage on the macroscopic surface of specimen 1 and specimen 2. 4 has obvious cracking macroscopic cracks, fish scale damage appears on the surface of specimen 6, irregular macroscopic damage occurs on the surface of specimen 3 and specimen 5, and the stress corrosion resistance performance of the material in this environment can be determined by the damage degree of the specimen.

实例2本发明进行小试样应力腐蚀测试Example 2 The present invention carries out small sample stress corrosion test

同样加工试样6件,按照本发明将试样装配于应力腐蚀试样装置上,对载荷进行测试时暂不安装腐蚀实验腔(12),将应变片(10)贴于应力测定试样(9)平行段,根据力的相互作用原理,只需对应力测定试样(9)进行应力应变测试,即可准确测得试样(16)受到的拉应力,从而进一步验证应力环加载载荷的准确性。6 samples are processed equally, and the sample is assembled on the stress corrosion sample device according to the present invention, and the corrosion experiment cavity (12) is not installed temporarily when the load is tested, and the strain gauge (10) is attached to the stress measurement sample ( 9) In the parallel section, according to the principle of force interaction, the tensile stress of the sample (16) can be accurately measured only by performing a stress-strain test on the stress measurement sample (9), thereby further verifying the stability of the stress ring loading load. accuracy.

为验证该装置加载的准确性和可靠性,分别将应变片(10)贴于应力测定试样(9)和试样(16)的平行段,分别记为A1、A3,然后对试样进行加载,并实时记录应变片数据,测得A1与A3部位应力、应变大小相一致,说明试样(16)和应力测定试样(9)所受载荷大小一致,符合本装置设计结果。将其数据与常规应力环加载数据对比发现,运用应力环标定曲线所得计算载荷较实际载荷小,即利用常规应力环标定曲线所加载在试样(16)上的实际载荷远大于理论设计载荷,常规应力环加载与本发明装置加载对比如图4,说明有必要使用该装置进行加载以及对常规应力环加载方法进行验证。In order to verify the accuracy and reliability of the loading of the device, the strain gauges (10) were respectively attached to the parallel sections of the stress measurement sample (9) and the sample (16), which were respectively marked as A1 and A3, and then the samples were Loading, and real-time recording of the strain gauge data, the measured stress and strain at A1 and A3 are consistent, indicating that the loads on the sample (16) and the stress measurement sample (9) are consistent, which is consistent with the design results of this device. Comparing its data with the conventional stress ring loading data, it is found that the calculated load obtained by using the stress ring calibration curve is smaller than the actual load, that is, the actual load loaded on the sample (16) by using the conventional stress ring calibration curve is much greater than the theoretical design load, The comparison between conventional stress ring loading and the loading of the device of the present invention is shown in Fig. 4, which shows that it is necessary to use the device for loading and to verify the conventional stress ring loading method.

确定加载载荷大小后,重新使用本发明装置对某金属复合管进行抗应力腐蚀实验,分别加载80%σs、100%σs两种应力等级,具体加载参数如表2,经过720小时腐蚀实验后,试样均未发生断裂,也没有裂纹以及表面损伤,试样无明显塑性变形的痕迹,说明经本发明修改后的加载方法是合理的,也说明实例1中试样之所以出现明显沿晶裂纹及损伤,原因在于常规应力环加载应力过大造成,出现较大实验误差,而采用本发明装置所得实验结果准确、可靠。After determining the size of the loaded load, re-use the device of the present invention to carry out a stress corrosion test on a metal composite pipe, and load two stress levels of 80% σs and 100% σs respectively. The specific loading parameters are shown in Table 2. After 720 hours of corrosion experiments, No fracture occurred in the samples, no cracks and surface damage, and the samples had no obvious traces of plastic deformation, which shows that the loading method modified by the present invention is reasonable, and also shows that the sample in Example 1 has obvious intergranular cracks And damage, the reason is that the conventional stress ring loading stress is too large, resulting in large experimental errors, but the experimental results obtained by the device of the present invention are accurate and reliable.

表1Table 1

表2Table 2

应理解,这些实施例仅用于说明本发明而不用于限制本发明的范围。此外应理解,在阅读了本发明讲授的内容之后,本领域技术人员可以对本发明作各种改动或修改,这些等价形式同样落于本申请所附权利要求书所限定的范围。It should be understood that these examples are only used to illustrate the present invention and are not intended to limit the scope of the present invention. In addition, it should be understood that after reading the teachings of the present invention, those skilled in the art can make various changes or modifications to the present invention, and these equivalent forms also fall within the scope defined by the appended claims of the present application.

Claims (8)

Translated fromChinese
1.一种小试样恒载荷应力腐蚀测试装置,其特征在于该装置包括以下部件:位移传感器(1)、加载螺杆(2)、固定螺杆(3)、底座(4)、应力环(7)、应力测定试样(9)、腐蚀试验腔(12)、试样(16)和实验介质(17);1. A small sample constant load stress corrosion test device is characterized in that the device includes the following components: displacement sensor (1), loading screw (2), fixing screw (3), base (4), stress ring (7 ), stress measurement sample (9), corrosion test chamber (12), sample (16) and experimental medium (17);所述应力环(7)通过固定螺杆(3)由固定螺母(5)固定在底座(4)上,该应力环(7)内部具有腐蚀试验腔(12),该腐蚀试验腔(12)装有实验介质(17)和试样(16),所述固定螺杆(3)的U型夹具端穿过腐蚀试验腔(12)的底部并固定试样(16)的下部,所述固定螺杆(3)和腐蚀试验腔(12)之间具有下密封环(18);The stress ring (7) is fixed on the base (4) by the fixing nut (5) through the fixing screw (3). The stress ring (7) has a corrosion test chamber (12) inside, and the corrosion test chamber (12) is equipped with There is an experimental medium (17) and a sample (16), the U-shaped clamp end of the fixing screw (3) passes through the bottom of the corrosion test chamber (12) and fixes the lower part of the sample (16), the fixing screw ( 3) There is a lower sealing ring (18) between the corrosion test chamber (12);所述加载螺杆(2)通过加载螺母(6)穿过应力环(7)的上部和应力测定试样(9)的一端连接,该应力测定试样(9)的另一端为U型夹具端,所述应力测定试样(9)的U型夹具端穿过腐蚀试验腔(12)的上部并固定试样(16)的上部,所述加载螺杆(2)和腐蚀试验腔(12)之间具有上密封环(11),所述应力测定试样(9)的尺寸与试样(16)相同,并在该应力测定试样(9)的中部安装应变片(10);The loading screw (2) passes through the upper part of the stress ring (7) through the loading nut (6) and is connected to one end of the stress measurement sample (9), and the other end of the stress measurement sample (9) is a U-shaped clamp end , the U-shaped clamp end of the stress measurement sample (9) passes through the upper part of the corrosion test chamber (12) and fixes the upper part of the sample (16), the loading screw (2) and the corrosion test chamber (12) There is an upper sealing ring (11) between them, the size of the stress measurement sample (9) is the same as that of the sample (16), and a strain gauge (10) is installed in the middle of the stress measurement sample (9);所述底座(4)具有一支架,该支架上安装有位移传感器(1),该位移传感器(1)位于应力环(7)的上部。The base (4) has a bracket on which a displacement sensor (1) is installed, and the displacement sensor (1) is located on the upper part of the stress ring (7).2.如权利要求1所述的一种小试样恒载荷应力腐蚀测试装置,其特征在于所述上密封环(11)和下密封环(18)与腐蚀试验腔(12)间安装密封圈(13);所述应力测定试样(9)的U型夹具端和固定螺杆(3)的U型夹具端通过销钉(20)固定试样(16)。2. A small sample constant load stress corrosion test device according to claim 1, characterized in that a sealing ring is installed between the upper sealing ring (11) and the lower sealing ring (18) and the corrosion test chamber (12) (13); the U-shaped clamp end of the stress measurement sample (9) and the U-shaped clamp end of the fixing screw (3) fix the sample (16) through the pin (20).3.如权利要求2所述的一种小试样恒载荷应力腐蚀测试装置,其特征在于所述应力测定试样(9)的U型夹具端和固定螺杆(3)的U型夹具端与试样(16)之间具有绝缘垫片(19),该绝缘垫片(19)为聚四氟乙烯材质;所述加载螺杆(2)、固定螺杆(3)、固定螺母(5)、加载螺母(6)、应力环(7)和销钉(20)是由耐腐蚀性能的哈氏合金加工而成。3. A small sample constant load stress corrosion test device as claimed in claim 2, characterized in that the U-shaped clamp end of the stress measurement sample (9) and the U-shaped clamp end of the fixing screw (3) are in contact with There is an insulating gasket (19) between the samples (16), and the insulating gasket (19) is made of polytetrafluoroethylene; the loading screw (2), fixing screw (3), fixing nut (5), loading The nut (6), the stress ring (7) and the pin (20) are processed by corrosion-resistant Hastelloy.4.如权利要求1所述的一种小试样恒载荷应力腐蚀测试装置,其特征在于所述加载螺母(6)和应力环(7)之间具有旋转垫片(8),该旋转垫片(8)由耐腐蚀性能的哈氏合金加工而成。4. A small sample constant load stress corrosion test device according to claim 1, characterized in that there is a rotating washer (8) between the loading nut (6) and the stress ring (7), the rotating washer Sheet (8) is processed by corrosion-resistant Hastelloy.5.如权利要求1所述的一种小试样恒载荷应力腐蚀测试装置,其特征在于所述腐蚀试验腔(12)还具有进气口(14)和出气口(15)。5. A small sample constant load stress corrosion test device according to claim 1, characterized in that the corrosion test chamber (12) also has an air inlet (14) and an air outlet (15).6.如权利要求1所述的一种小试样恒载荷应力腐蚀测试装置,其特征在于所其试样(16)为扁平矩形试样,其厚度为0.9mm~2mm,宽度为3mm~5mm。6. A kind of small sample constant load stress corrosion test device as claimed in claim 1, it is characterized in that its sample (16) is a flat rectangular sample, its thickness is 0.9mm~2mm, and width is 3mm~5mm .7.如权利要求1所述的一种小试样恒载荷应力腐蚀测试装置,其特征在于所述实验介质(17)为腐蚀介质。7. A small sample constant load stress corrosion test device as claimed in claim 1, characterized in that said test medium (17) is a corrosive medium.8.一种采用如权利要求1-7所述的小试样恒载荷应力腐蚀测试装置进行腐蚀测试的方法,其特征在于包括以下步骤:8. A method for carrying out corrosion testing using the small sample constant load stress corrosion testing device as claimed in claim 1-7, is characterized in that comprising the following steps:步骤一,根据所需模拟现场工况条件设计实验腐蚀介质、试样加载载荷大小;Step 1, design the experimental corrosion medium and the load size of the sample according to the required simulated on-site working conditions;步骤二,安装试样(16),通过加载螺杆(2)加载应力,通过位移传感器(1)和应变片(10)确定载荷;Step 2, install the sample (16), load the stress through the loading screw (2), and determine the load through the displacement sensor (1) and the strain gauge (10);步骤三,将腐蚀介质加入腐蚀实验腔(12)中,将进气口(14)、出气口(15)分别连接至H2S、CO2或N2气瓶和废气处理系统;Step 3, adding the corrosive medium into the corrosion test chamber (12), connecting the gas inlet (14) and the gas outlet (15) to theH2S ,CO2 orN2 gas cylinder and the waste gas treatment system respectively;步骤四,腐蚀实验腔(12)中腐蚀介质进行充分除氧后,通入H2S或CO2等腐蚀性气体,记录时间开始实验,所述试验时间为720h;Step 4: After the corrosive medium in the corrosion test chamber (12) is fully deoxidized, corrosive gases such as H2 S or CO2 are introduced, and the test is started after recording the time, and the test time is 720 hours;步骤五,实验结束后,进行充分除氧,将试样(16)卸下,观察试样是否断裂并进行裂纹检测、试样表面腐蚀形貌和腐蚀产物分析。Step 5, after the experiment, fully deoxidize, remove the sample (16), observe whether the sample is broken, and perform crack detection, sample surface corrosion morphology and corrosion product analysis.
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CN111141612A (en)*2020-01-212020-05-12鞍钢股份有限公司 A device and method for testing the resistance to hydrogen sulfide stress corrosion of oil well pipes
CN111426572A (en)*2020-03-132020-07-17天津大学 A constant load stress corrosion online observation test device in hydrofluoric acid environment
CN111721617A (en)*2020-07-302020-09-29中冶建筑研究总院(深圳)有限公司 Axial tensile test device and test method for specimen under constant temperature erosion environment
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CN112268854A (en)*2020-10-292021-01-26中国石油天然气集团有限公司Pipe corrosion resistance evaluation device, installation method and evaluation method in corrosive environment
CN112393970A (en)*2020-11-132021-02-23中国石油天然气集团有限公司Method and device for evaluating stress corrosion cracking sensitivity of pipe
CN112730208A (en)*2020-12-162021-04-30贵州电网有限责任公司Weather-resistant steel tower welding connection part test device and test method thereof
CN112730207A (en)*2020-12-162021-04-30贵州电网有限责任公司Weather-resistant steel iron tower bolt connection part test device and test method thereof
CN112834332A (en)*2020-12-292021-05-25江苏容大材料腐蚀检验有限公司Loading detection method and monitoring system for sulfide stress corrosion uniaxial tensile test
CN112924368A (en)*2021-01-252021-06-08西南石油大学Metal material corrosion resistance testing device and testing method thereof
CN113049386A (en)*2021-03-292021-06-29三峡国际能源投资集团有限公司High-ductility cement-based composite material displacement control load holding device and method
CN113588420A (en)*2021-07-272021-11-02中铝材料应用研究院有限公司Constant load stress testing device and method for bar and rod test sample applied to corrosive environment
CN114441306A (en)*2021-12-242022-05-06中国特种设备检测研究院 Test method and device for metal protective coating in stress corrosion environment
CN114544340A (en)*2022-02-102022-05-27武汉钢铁有限公司Metal material strain fatigue testing device and method based on corrosion environment
CN114659889A (en)*2022-03-092022-06-24中铁隆昌铁路器材有限公司High-strength steel sample delayed fracture test device and method
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CN116539512A (en)*2023-05-122023-08-04北京科技大学 A kind of stress corrosion simulation experiment equipment

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CN104880367A (en)*2015-05-262015-09-02中国特种设备检测研究院Constant load tensile test method and test device for sample in stress sensitive environment
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CN105136651B (en)*2015-08-182017-12-01重庆硕奥科技有限公司 An automatic detection method for heat and humidity resistance based on metal plates
CN105158093A (en)*2015-08-312015-12-16武汉钢铁(集团)公司Testing device for fatigue crack growth rate under seawater corrosive environment and measuring method for testing device
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CN105388101B (en)*2015-12-022019-01-18中国石油天然气集团公司A kind of Combined Loading stress corrosion testing device and method
CN105973793A (en)*2016-05-302016-09-28中国科学院金属研究所Downhole stress corrosion testing method and device
CN105973793B (en)*2016-05-302019-01-18中国科学院金属研究所A kind of underground stress corrosion test method and device
CN106442282A (en)*2016-08-312017-02-22西安摩尔石油工程实验室股份有限公司Constant load stress corrosion test device with load sensor
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CN106546529B (en)*2016-10-142019-03-26天津大学Marine structure stress corrosion testing device under alternation of wetting and drying
CN106546529A (en)*2016-10-142017-03-29天津大学Marine structure stress corrosion testing device under alternation of wetting and drying
CN107817165A (en)*2017-11-282018-03-20嘉峪关天源新材料有限责任公司Device for measuring stress corrosion behavior of steel in corrosion environment
CN109100217A (en)*2018-09-262018-12-28中国石油天然气集团有限公司A kind of 4 points of curved test fixtures of anti-H 2 S stress corrosion
CN109443920A (en)*2018-12-032019-03-08中国电子产品可靠性与环境试验研究所((工业和信息化部电子第五研究所)(中国赛宝实验室))Environment-pulling force coupling test devices, systems, and methods
CN109443921A (en)*2018-12-032019-03-08中国电子产品可靠性与环境试验研究所((工业和信息化部电子第五研究所)(中国赛宝实验室))Environment-pulling force coupling test device and system
CN109443921B (en)*2018-12-032024-05-28中国电子产品可靠性与环境试验研究所((工业和信息化部电子第五研究所)(中国赛宝实验室))Environment-tensile coupling test device and system
CN109916737A (en)*2019-03-042019-06-21鞍钢股份有限公司Method for testing stress corrosion resistance of oil well pipe
CN110095350A (en)*2019-04-302019-08-06北京航天发射技术研究所Evaluate the constant load testing stand and test method of transmitting station substrate corrosion susceptibility
CN110231218A (en)*2019-07-262019-09-13西南石油大学The constant strain stress corrosion testing device and its test method of a kind of analog scene corrosive environment
CN111141612A (en)*2020-01-212020-05-12鞍钢股份有限公司 A device and method for testing the resistance to hydrogen sulfide stress corrosion of oil well pipes
CN111141612B (en)*2020-01-212022-05-13鞍钢股份有限公司Device and method for testing hydrogen sulfide stress corrosion resistance of oil well pipe
CN111426572A (en)*2020-03-132020-07-17天津大学 A constant load stress corrosion online observation test device in hydrofluoric acid environment
CN111721617A (en)*2020-07-302020-09-29中冶建筑研究总院(深圳)有限公司 Axial tensile test device and test method for specimen under constant temperature erosion environment
CN112098206B (en)*2020-09-012022-07-08合肥通用机械研究院有限公司 A bolt stress corrosion test device and a test method using the same
CN112240851A (en)*2020-10-142021-01-19衡阳华菱钢管有限公司Loading auxiliary device
CN112268854A (en)*2020-10-292021-01-26中国石油天然气集团有限公司Pipe corrosion resistance evaluation device, installation method and evaluation method in corrosive environment
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CN112393970A (en)*2020-11-132021-02-23中国石油天然气集团有限公司Method and device for evaluating stress corrosion cracking sensitivity of pipe
CN112730207A (en)*2020-12-162021-04-30贵州电网有限责任公司Weather-resistant steel iron tower bolt connection part test device and test method thereof
CN112730208A (en)*2020-12-162021-04-30贵州电网有限责任公司Weather-resistant steel tower welding connection part test device and test method thereof
CN112730208B (en)*2020-12-162024-08-02贵州电网有限责任公司Device and method for testing welding connection part of weathering steel tower
CN112730207B (en)*2020-12-162024-05-17贵州电网有限责任公司Test device and test method for bolt connection part of weathering steel tower
CN112834332A (en)*2020-12-292021-05-25江苏容大材料腐蚀检验有限公司Loading detection method and monitoring system for sulfide stress corrosion uniaxial tensile test
CN112924368A (en)*2021-01-252021-06-08西南石油大学Metal material corrosion resistance testing device and testing method thereof
CN113049386A (en)*2021-03-292021-06-29三峡国际能源投资集团有限公司High-ductility cement-based composite material displacement control load holding device and method
CN113049386B (en)*2021-03-292023-01-31三峡国际能源投资集团有限公司High-ductility cement-based composite material displacement control load holding device and method
CN113588420A (en)*2021-07-272021-11-02中铝材料应用研究院有限公司Constant load stress testing device and method for bar and rod test sample applied to corrosive environment
CN114441306A (en)*2021-12-242022-05-06中国特种设备检测研究院 Test method and device for metal protective coating in stress corrosion environment
CN114544340A (en)*2022-02-102022-05-27武汉钢铁有限公司Metal material strain fatigue testing device and method based on corrosion environment
CN114659889A (en)*2022-03-092022-06-24中铁隆昌铁路器材有限公司High-strength steel sample delayed fracture test device and method
CN116429575A (en)*2023-04-172023-07-14新余钢铁股份有限公司 A kind of tensile performance testing method
CN116539512B (en)*2023-05-122023-12-22北京科技大学Stress corrosion simulation experiment equipment
CN116539512A (en)*2023-05-122023-08-04北京科技大学 A kind of stress corrosion simulation experiment equipment

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