Material stress and micro-electrochemical in-situ corrosion potential testing device and method

Abstract

The invention relates to the technical field of material testing, and discloses a material stress and micro-electrochemical in-situ corrosion potential testing device and a material stress and micro-electrochemical in-situ corrosion potential testing method. The invention provides an experimental device capable of simulating different stresses and actual test conditions and accurately evaluating the micro-area stress corrosion behavior of a material, and the stress corrosion and micro-area corrosion potential change rules of the material under different stress and electrochemical coupling effects are visually measured in situ. And a technical support is provided for revealing a stress corrosion mechanism in a metal material service environment. Meanwhile, different sample test requirements of a plurality of material product production lines are considered, high-accuracy and high-flexibility adjustment of multiple test conditions is realized, and by planning a scientific and reasonable sample test distribution strategy, the test frequency requirement of parallel task test of the multiple material product production lines and the test device switching target are met, and the test efficiency is improved. The efficiency and operation reliability of the test system are improved.

Description

Technical Field

[0001] The present invention relates to the technical field of material testing, and in particular to a device and method for testing material stress and micro-electrochemical in-situ corrosion potential. Background Art

[0002] With the widespread application of hydrogen energy, the corrosion problem of materials in hydrogen environments has become a difficult problem that urgently needs to be solved, especially in industrial environments with certain humidity, high temperature, high pressure and complex loading conditions. Many metal structures and equipment are exposed to gaseous environments during daily use, such as industrial equipment, building structures, pipelines, etc. The stress-electrochemical coupling effect in hydrogen environments causes material corrosion damage, which not only seriously affects the mechanical properties and structural integrity of the materials, but also leads to equipment failures and safety accidents.

[0003] Existing testing devices are limited to stress corrosion behavior under a specific stress state, making it impossible to use a single testing device to simulate loading conditions under multiple stresses. Furthermore, they are limited to macroscopic corrosion behavior and cannot provide a deep understanding of the corrosion mechanism of stress-electrochemical coupling in hydrogen environments (or other corrosive gas environments). Furthermore, in actual material testing applications (such as spot checks on material product production lines), materials produced on different material product production lines may have different spot check test frequencies and test condition requirements (such as different load test methods, humidity, temperature, pressure, and corrosive gas environments) due to their application in different environments and scenarios. When faced with different test condition requirements, existing testing devices are unable to efficiently and accurately achieve the coordinated adjustment of multiple test conditions. Furthermore, when multiple specimen test tasks need to be tested continuously, it is also necessary to ensure that the parameter adjustment speed of multiple test conditions meets the multi-task test execution requirements and minimizes the switching of test devices, thereby improving the efficiency and operational reliability of the test system.

[0004] Therefore, how to achieve high-accuracy and high-flexibility adjustment of multiple test conditions under multiple stress loading conditions, provide an experimental device that can simulate different stresses and actual test conditions and accurately evaluate the stress corrosion behavior of material micro-areas, and improve the efficiency and operational reliability of the test system while ensuring that the test frequency requirements and test device switching targets of parallel task testing of multi-material product production lines are met, is a technical problem that needs to be solved urgently. Summary of the Invention

[0005] The present invention provides a material stress and micro-electrochemical in-situ corrosion potential testing device and method, aiming to solve at least one of the above technical problems.

[0006] To achieve the above objectives, the present invention provides a material stress and micro-electrochemical in-situ corrosion potential testing device, comprising: Multimodal dynamic loading control system, including static load test assembly, dynamic load test assembly, displacement sensor and load sensor; The static load test assembly and the dynamic load test assembly are configured to apply a static load test tensile force and / or a dynamic load test tensile force to a fixed target test specimen according to the test item of the target test specimen; the displacement sensor and the load sensor are configured to monitor the change in the axial displacement parameter and the load parameter of the target test specimen when subjected to the tensile force; Nanoscale multi-spectral domain electrochemical topology mapping system, including a sealed test kettle and a scanning Kelvin micro-area corrosion potential test component; The sealed test kettle is configured to provide a corrosive gas environment for the target test sample fixed in the sealed test kettle according to the test items of the target test sample; the scanning Kelvin micro-area corrosion potential test assembly is configured to perform micro-area corrosion electrochemical testing on the target test sample in the corrosive gas environment according to the test items of the target test sample; A sample test condition control system, comprising a quantum micro-field humidity coupling control component, a temperature control component, and a gas control component, configured to control humidity parameters, temperature parameters, and pressure parameters in a sealed test kettle where the target test sample is located according to the test items of the target test sample; The timing control system is configured to monitor the displacement parameters, load parameters, electrochemical parameters, humidity parameters, temperature parameters and pressure parameters of the target test specimen when executing the test item, and control the test item to stop when it is detected that the target test specimen is broken.

[0007] Optionally, the static load test assembly specifically includes: The stress ring body is disposed on the base and adopts an elastic body that generates a reaction force after compression deformation and is configured to apply static tensile stress to the target test specimen; A super loading bolt is provided on the upper side of the stress ring body and applies load through a plurality of small bolts. The super loading bolt is provided with a first load sensor for collecting load parameters of the target test specimen when subjected to static tensile stress and transmitting the load parameters to the stress ring control system; The specimen jacket is configured to fix the target test specimen and is connected to the super loading bolt to apply the load provided by the super loading bolt to the target test specimen as static tensile stress.

[0008] Optionally, the sample jacket is configured to fix the target test sample directly or indirectly using at least one of a two-point bend, a three-point bend, and a four-point bend.

[0009] Optionally, the dynamic load test assembly specifically includes: A hydraulic loading frame and a hydraulic loading head, wherein the hydraulic loading head is arranged on the hydraulic loading frame and connected to the super loading bolts, and the hydraulic loading frame is fixed to the upper side of the stress ring body by fastening bolts; The micro-stepping motor drive device is configured to control a hydraulic loading head to drive a sample jacket via a super loading bolt to apply dynamic tensile stress to a target test sample. A second load sensor is provided between the hydraulic loading head and the sample jacket for collecting load parameters of the target test sample when subjected to dynamic tensile stress and transmitting the load parameters to the stress ring control system.

[0010] Optionally, the hydraulic loading head is configured to adopt a ball screw, and a grating sensor is provided between the ball screw and the hydraulic loading frame, and the ball screw and the grating sensor jointly drive the sample jacket to apply dynamic tensile stress of the target strain rate to the target test sample.

[0011] Optionally, the displacement sensor specifically includes: a non-contact laser extensometer, which is installed outside the observation window of the sealed test kettle and is configured to monitor the change in axial displacement parameters of the target test specimen when it is subjected to tensile force.

[0012] Optionally, the sealed test kettle specifically includes: A sealed cavity, wherein the sealed cavity is provided with a detachable sealing cover, a sample mounting hole is provided at the center of the detachable sealing cover, and the target test sample is arranged in the sealed cavity and extends through the sample mounting hole to be fixed through the sample jacket; The sealed cavity is provided with a humidity regulating port connected to a quantum micro-field humidity coupling control component. The quantum micro-field humidity coupling control component includes an ultrasonic humidifier arranged on the outside and a humidity transmitter arranged inside the sealed test kettle, and is configured to control the humidity parameters in the sealed test kettle where the target test sample is located according to the test items of the target test sample; The sealed cavity is provided with an exhaust port and an air inlet connected to a gas control assembly. The gas control assembly includes a gas distributor, a gas cylinder assembly, and a pressure sensor disposed inside the sealed test kettle. The gas control assembly is configured to inject corrosive gas into the sealed cavity according to the test items of the target test specimen, thereby controlling the pressure parameters inside the sealed test kettle where the target test specimen is located. A temperature control component is provided in the sealed cavity, and the temperature control component includes a temperature sensor and a heating tube, and is configured to control the temperature parameters in the sealed test kettle where the target test sample is located according to the test items of the target test sample.

[0013] Optionally, the scanning Kelvin micro-area corrosion potential test assembly specifically includes: A driving arm and a scanning probe, wherein the scanning probe is connected to an external lock-in amplifier via a bias source fixed to the driving arm; In which, the scanning probe is configured to contact the surface of the target test sample, the bias source is configured to transfer charge to the probe through the driving arm to form a potential difference, and the phase-locked amplifier is configured to detect the weak signal of the potential difference and compare it with the reference signal to realize micro-area corrosion electrochemical testing of the target test sample in a corrosive gas environment.

[0014] In addition, to achieve the above-mentioned object, the present invention also provides a material stress and micro-electrochemical in-situ corrosion potential testing method, which is used in a material stress and micro-electrochemical in-situ corrosion potential testing system. The material stress and micro-electrochemical in-situ corrosion potential testing system includes a test planning terminal and a plurality of material stress and micro-electrochemical in-situ corrosion potential testing devices as described in any one of the above. The method includes: S1: Obtain a set of sample test requirements for several material product production lines during a target test period; wherein the sample test task set includes the sample attributes and sample test frequency of each material product production line; S2: matching a sample test condition set for each material product production line based on the sample test characteristics in the sample attributes, and generating a sample test task list for a target test period based on the sample test condition set and the sample test frequency; wherein the sample test condition set includes a load test mode, a corrosive gas type, a test temperature, a test humidity, and a test pressure; S3: querying the initial sample test condition set of each material stress and micro-electrochemical in-situ corrosion potential testing device at the initial moment of the target test period, sequentially selecting the sample test tasks and the test period of each sample test task that are assigned to each material stress and micro-electrochemical in-situ corrosion potential testing device and are sequentially executed during the target test period from the sample test task list, using an optimization algorithm to solve the sample test tasks and the test period of each sample test task that are sequentially executed by each material stress and micro-electrochemical in-situ corrosion potential testing device during the target test period, and generating a sample test allocation strategy; S4: According to the sample test allocation strategy, generate a set of sample test conditions for each material stress and micro-electrochemical in-situ corrosion potential testing device at different times during the target test period, and perform sample tests on several material product production lines during the target test period based on the sample test condition sets at different times.

[0015] Optionally, the sample test tasks assigned to each material stress and micro-electrochemical in-situ corrosion potential testing device and executed sequentially during the target test period and the test period of each sample test task are sequentially selected from the sample test task list, and an optimization algorithm is used to solve the sample test tasks sequentially executed by each material stress and micro-electrochemical in-situ corrosion potential testing device during the target test period and the test period of each sample test task to generate a sample test allocation strategy, specifically including: S31: Selecting, from the sample test task list, the sample test tasks that are assigned to each material stress and micro-electrochemical in-situ corrosion potential test device and are sequentially executed during the target test period and the test period of each sample test task to solve the sample test allocation strategy; S32: The first constraint condition is to make the interval time between two adjacent sample test tasks of each material product production line when being executed by the material stress and micro-electrochemical in-situ corrosion potential testing device shorter than the interval time corresponding to the sample test frequency of the material product line; the second constraint condition is to make the sample test condition adjustment time of adjusting the sample test condition set of the previous sample test task to the sample test condition set of the next sample test task when each material stress and micro-electrochemical in-situ corrosion potential testing device executes two adjacent sample test tasks shorter than the interval time between the test periods of the previous sample test task and the next sample test task; and the optimization goal is to minimize the number of times two adjacent sample test tasks of each material product production line are executed by different material stress and micro-electrochemical in-situ corrosion potential testing devices; S33: An optimization algorithm is used to solve the sample test tasks and the test period of each sample test task that are sequentially performed by each material stress and micro-electrochemical in-situ corrosion potential test device during the target test period, and a sample test allocation strategy is generated.

[0016] The beneficial effects of the present invention are: a material stress and micro-electrochemical in-situ corrosion potential testing device and method are proposed, which includes a multi-modal dynamic loading control system, a nano-scale multi-spectral domain electrochemical topological mapping system, a sample test condition control system and a timing control system. By simulating the corrosive gas environment under different humidity, temperature, pressure, different stress and load conditions, an experimental device is provided that can simulate different stresses and actual test conditions and accurately evaluate the stress corrosion behavior of the material micro-area. The stress corrosion and micro-area corrosion potential change law of the material under different stress and electrochemical coupling is visually determined in situ, providing technical support for revealing the stress corrosion mechanism of metal materials in the service environment. At the same time, considering the different sample testing requirements of several material product production lines, high-accuracy and high-flexibility adjustment of multiple test conditions is achieved. By planning a scientific and reasonable sample test allocation strategy, while ensuring that the test frequency requirements and test device switching targets of the parallel task testing of multiple material product production lines are met, the efficiency and operational reliability of the test system are improved. BRIEF DESCRIPTION OF THE DRAWINGS

[0017] Figure 1 Schematic diagram of the structure of the material stress and micro-electrochemical in-situ corrosion potential testing device of the present invention; Figure 2 Schematic diagram of the structure of the dynamic load test assembly of the present invention; Figure 3Schematic diagram of the structure of the static load test assembly of the present invention; Figure 4 Schematic diagram of the process of the material stress and micro-electrochemical in-situ corrosion potential testing method of the present invention.

[0018] Description of reference numerals: 1-stress ring body; 2-super loading bolt; 3-load sensor; 4-sample jacket; 5-base; 6-support long rod; 7-positioning instrument; 8-stress ring control system; 9-cavity; 10-detachable sealing cover; 11-phase-locked amplifier; 12-driving arm; 13-bias source; 14-scanning probe; 15-heating tube; 16-temperature sensor; 17-ultrasonic humidifier; 18-humidity transmitter; 19-liquid inlet; 20-water vapor outlet; 21-air inlet; 22-exhaust outlet; 23-pressure sensor; 24-hydraulic loading head; 25-hydraulic loading frame; 26-micro-stepping motor drive device; 27-fastening bolt; 28-four-point bending mold. DETAILED DESCRIPTION

[0019] In order to make the purpose, technical solutions and advantages of the present invention more clearly understood, the present invention will be further described in detail below with reference to the accompanying drawings and embodiments. It should be understood that the specific embodiments described herein are only used to explain the present invention and are not intended to limit the present invention.

[0020] The embodiment of the present invention provides a material stress and micro-electrochemical in-situ corrosion potential testing device, referring to Figure 1-Figure 3 shown.

[0021] In this embodiment, a material stress and micro-electrochemical in-situ corrosion potential testing device includes: A multi-modal dynamic loading control system, comprising a static load test assembly, a dynamic load test assembly, a displacement sensor, and a load sensor 3; The static load test assembly and the dynamic load test assembly are configured to apply a static load test tensile force and / or a dynamic load test tensile force to a fixed target test specimen according to the test item of the target test specimen; the displacement sensor and the load sensor 3 are configured to monitor the axial displacement parameter change and the load parameter change of the target test specimen when subjected to the tensile force; Nanoscale multi-spectral domain electrochemical topology mapping system, including a sealed test kettle and a scanning Kelvin micro-area corrosion potential test component; The sealed test kettle is configured to provide a corrosive gas environment for the target test sample fixed in the sealed test kettle according to the test items of the target test sample; the scanning Kelvin micro-area corrosion potential test assembly is configured to perform micro-area corrosion electrochemical testing on the target test sample in the corrosive gas environment according to the test items of the target test sample; A sample test condition control system, comprising a quantum micro-field humidity coupling control component, a temperature control component, and a gas control component, configured to control humidity parameters, temperature parameters, and pressure parameters in a sealed test kettle where the target test sample is located according to the test items of the target test sample; The timing control system is configured to monitor the displacement parameters, load parameters, electrochemical parameters, humidity parameters, temperature parameters and pressure parameters of the target test specimen when executing the test item, and control the test item to stop when it is detected that the target test specimen is broken.

[0022] It should be noted that existing testing devices are limited to stress corrosion behavior under a specific stress state, making it impossible to use a single testing device to measure loading conditions under multiple stresses. Furthermore, they are limited to macroscopic corrosion behavior and cannot provide a deep understanding of the corrosion mechanism of stress-electrochemical coupling in hydrogen environments (or other corrosive gas environments). To address these issues, this embodiment simulates corrosive gas environments under different humidity, temperature, pressure, stress, and load conditions, providing an experimental device capable of simulating different stresses and actual testing conditions and accurately evaluating the stress corrosion behavior of materials in micro-areas. This device allows for in-situ visualization of the changes in stress corrosion and micro-area corrosion potential of materials under different stresses and electrochemical coupling, providing technical support for revealing the stress corrosion mechanism of metal materials in service environments.

[0023] In a preferred embodiment, the static load test assembly specifically includes: The stress ring body 1 is provided on the base 5 and is an elastic body that generates a reaction force after compression deformation and is configured to apply static tensile stress to the target test specimen; A super loading bolt 2 is provided on the upper side of the stress ring body 1 and applies load through a plurality of small bolts. The super loading bolt 2 is provided with a first load sensor for collecting load parameters of the target test specimen when subjected to static tensile stress and transmitting the load parameters to the stress ring control system 8; The sample jacket 4 is configured to fix the target test sample and is connected to the super loading bolt 2 to apply the load provided by the super loading bolt 2 to the target test sample as static tensile stress.

[0024] Furthermore, the sample jacket 4 is configured to fix the target test sample directly or indirectly by using at least one of two-point bending, three-point bending and four-point bending molds, such as Figure 3 FIG. 2 is a schematic diagram showing the installation of the four-point bending die 28 .

[0025] In actual application, the static load test assembly includes the stress ring body 1, super loading bolts 2, sample jacket 4, a positioner 7, a support rod 6 and a base 5. The static load test assembly is manufactured according to NACE TM0177-05 Method A; the ring body is the main part of the stress ring, and is composed of an elastic body that can generate a reaction force after being compressed and deformed, so as to apply tensile stress to the sample; a super loading bolt 2 protruding toward the center of the stress ring is provided on the upper side of the ring body; the super loading bolt 2 is loaded by eight small bolts; the super loading bolt 2 is connected to a load sensor 3, which displays the load force in real time; the load sensor 3 is connected to the stress ring control system 8; the super loading bolt 2 is connected to the sample jacket 4; the sample jacket 4 is used to fix the sample; a base 5 is provided at the bottom of the stress ring body 1; the base 5 is provided with a support rod 6; the support rod 6 is provided with a positioner 7; the positioner 7 can indirectly display the size of the loading force, and is used in conjunction with the load sensor 3 to ensure the accuracy and stability of the load force.

[0026] It should be noted that the super loading bolt 2 replaces the uniaxial loading bolt of the traditional stress ring, has higher strength, better corrosion resistance and more reliable fastening effect, and can ensure that the sample is subjected to stable stress loading during the test under extreme conditions. The super loading bolt 2 provided in the device of the present invention also monitors parameters such as stress, strain or corrosion rate through the built-in load sensor 3. Accurately understanding the load resistance of the material under different load forces provides a scientific basis for the study of various professional materials and special metal materials. The stress ring control system 8 can display the load force and is provided with a temperature control component that can display the temperature and adjust the temperature.

[0027] In a preferred embodiment, the dynamic load test assembly specifically includes: A hydraulic loading frame 25 and a hydraulic loading head 24, wherein the hydraulic loading head 24 is arranged on the hydraulic loading frame 25 and connected to the super loading bolt 2, and the hydraulic loading frame 25 is fixed to the upper side of the stress ring body 1 by fastening bolts 27; The micro-stepping motor drive device 26 is configured to control the hydraulic loading head 24 to drive the sample jacket 4 through the super loading bolt 2 to apply dynamic tensile stress to the target test sample. A second load sensor is provided between the hydraulic loading head 24 and the sample jacket 4 for collecting the load parameters of the target test sample when subjected to dynamic tensile stress and transmitting them to the stress ring control system 8.

[0028] Furthermore, the hydraulic loading head 24 is configured to use a ball screw, and a grating sensor is provided between the ball screw and the hydraulic loading frame 25. The ball screw and the grating sensor jointly drive the sample jacket 4 to apply dynamic tensile stress of the target strain rate to the target test sample.

[0029] In actual application, the dynamic load test assembly includes a micro-stepping motor drive device 26, a hydraulic loading frame 25, a hydraulic loading head 24 and a fastening bolt 27; the hydraulic loading head 24 is configured to use a ball screw, and a grating sensor is provided between the ball screw and the hydraulic loading frame 25 to ensure that the stretching rate is within 10 -3 ~10 -8 The load sensor 3 is precisely adjustable within the range of mm / s. The load sensor 3 is arranged between the hydraulic loading head 24 and the sample jacket 4. The load sensor 3 integrates DCPD (Direct Current Potential Drop) technology to measure the crack initiation and propagation rate online and realize crack propagation monitoring. The hydraulic loading head 24 is connected to the super loading bolt 2 by bolts.

[0030] It should be noted that the static load test assembly and the dynamic load test assembly can be used separately or in combination. If the dynamic load test assembly needs to be used alone, it is only necessary to unload the super loading bolt 2; if the static load test assembly needs to be used alone, the high-performance micro-stepping motor drive system does not need to be turned on; if the two need to be used in combination, the specimen can be pre-loaded by the super loading bolt 2, and then stretched at a slow strain rate at a certain strain rate to simulate the production operation of the material under actual complex working conditions.

[0031] In a preferred embodiment, the displacement sensor specifically includes: a non-contact laser extensometer, installed outside the observation window of the sealed test kettle, and configured to monitor the change in axial displacement parameters of the target test specimen when subjected to a tensile force.

[0032] In a preferred embodiment, the sealed test kettle specifically comprises: A sealed cavity 9 is provided with a detachable sealing cover 10, a sample mounting hole is provided at the center of the detachable sealing cover 10, and the target test sample is arranged in the sealed cavity 9 and extends through the sample mounting hole to be fixed through the sample jacket 4; The sealed cavity 9 is provided with a humidity regulating port connected to a quantum micro-field humidity coupling control assembly. The quantum micro-field humidity coupling control assembly includes an ultrasonic humidifier 17 disposed externally and a humidity transmitter 18 (including a quantized humidity probe and a signal conversion module) disposed inside the sealed test kettle. The humidity transmitter 18 is configured to control the humidity parameters in the sealed test kettle where the target test sample is located according to the test items of the target test sample. The sealed cavity 9 is provided with an exhaust port 22 and an air inlet 21 connected to a gas control assembly. The gas control assembly includes a gas distributor, a gas cylinder assembly, and a pressure sensor 23 disposed inside the sealed test kettle. The gas is configured to inject corrosive gas into the sealed cavity 9 according to the test items of the target test sample, thereby controlling the pressure parameters inside the sealed test kettle where the target test sample is located. The sealed cavity 9 is provided with a temperature control component, which includes a temperature sensor 16 and a heating tube 15 and is configured to control the temperature parameters in the sealed test kettle where the target test sample is located according to the test items of the target test sample.

[0033] In actual application, the test kettle includes a cavity 9 and a removable sealing cover 10; the test kettle structure is C-276 Hastelloy-liquid level glass plate, and the operator can observe the status of the internal medium and the sample through the wall of the liquid level gauge glass container. The pressure resistance range of the liquid level gauge glass plate is usually between 1~20MPa, and the heat resistance stability is ΔT 250℃~ΔT 1200℃, which can meet the temperature and pressure required for the experiment; a sample mounting hole is provided in the center of the removable sealing cover 10; the cavity 9 and the removable sealing cover 10 of the test kettle are sealed and connected with O-rings and bolts, which can completely prevent gas leakage.

[0034] In a specific embodiment, a heating tube 15 (eg, a Hastelloy heating tube) is provided inside the test kettle cavity 9 , and the heating tube 15 is connected to a temperature sensor 16 ; the temperature sensor 16 and the heating tube 15 form a temperature control assembly.

[0035] In a specific embodiment, the removable sealing cover 10 of the test kettle is connected to an ultrasonic humidifier 17; a humidity transmitter 18 is provided inside the test kettle and is connected to the ultrasonic humidifier 17; the ultrasonic humidifier 17 is provided with a liquid inlet 19 and a water vapor outlet 20; the ultrasonic humidifier 17 has a display and a humidity controller, which can accurately display and adjust the humidity inside the test kettle; It should be noted that the ultrasonic humidifier 17 can generate uniform water mist, making the moisture distribution in the kettle more uniform, and by using humidity-sensitive and gas-sensitive material testing technology with high precision and high stability, it can achieve high-precision and high-efficiency gas concentration and humidity control.

[0036] In a specific embodiment, the test kettle is provided with an air inlet 21 and an exhaust port 22, and the air inlet 21 is connected to a gas control component; the gas control component includes a gas cylinder group and a gas distributor; a pressure sensor 23 is provided inside the test kettle for controlling the pressure inside the test kettle.

[0037] It should be noted that the gas distributor has multiple channels, so the gas cylinder group can add or delete gas cylinders according to needs.

[0038] In a preferred embodiment, the scanning Kelvin micro-area corrosion potential test assembly specifically includes: A driving arm 12 and a scanning probe 14 , wherein the scanning probe 14 is connected to an external lock-in amplifier 11 via a bias source 13 fixed to the driving arm 12 ; Among them, the scanning probe 14 is configured to contact the surface of the target test sample, the bias source 13 is configured to transfer charge to the probe through the driving arm 12 to form a potential difference, and the phase-locked amplifier 11 is configured to detect the weak signal of the potential difference and compare it with the reference signal to realize micro-area corrosion electrochemical testing of the target test sample in a corrosive gas environment.

[0039] In practical applications, the scanning Kelvin micro-area corrosion potential test assembly includes a phase-locked amplifier 11, a driving arm 12, a bias source 13 and a scanning probe 14, which can perform nanoscale micro-area corrosion electrochemical tests such as micro-area corrosion potential and EIS; the driving arm 12 is controlled by a VC driver, supports parallel multi-probe operation, and supports operation of probes of different diameters; the driving arm 12 is connected to the scanning probe 14, and is used to control the movement of the scanning probe 14 relative to the sample to be tested; the upper end of the scanning probe 14 is connected to the bias source 13; the bias source 13 is fixed to the driving arm 12 and connected to the phase-locked amplifier 11; when the scanning probe 14 contacts the surface of the sample to be tested, the bias source 13 transfers charge to the probe through the driving arm 12, forming a small potential difference; the phase-locked amplifier 11 is used for weak signal detection, and improves the signal-to-noise ratio of the signal by accurately comparing the phase of the input signal with the reference signal and providing high-gain amplification, making the output signal more stable and reliable.

[0040] It should be noted that the lock-in amplifier 11 is directly installed in the electrochemical workstation. Furthermore, if stress corrosion testing is not required, the electrochemical testing system can be used alone to study micro-corrosion testing, such as pitting detection on metal surfaces and localized corrosion sensitivity in atmospheric environments. Furthermore, the scanning probe 14 can be replaced with a tungsten wire probe, as needed, to measure surface cleanliness, defects, damage, and uniformity of small areas of semiconductor materials in different atmospheres.

[0041] In a specific embodiment, the material stress and micro-electrochemical in-situ corrosion potential testing device is provided with a timing control system; the timing control system includes a timing control unit and a fracture sensor; the timing control unit adopts a PLC industrial programmable controller as a control unit to record the stress ring experimental parameters; the fracture sensor can sense and automatically alarm after the experiment is completed.

[0042] In this embodiment, the testing principle of the material stress and micro-electrochemical in-situ corrosion potential testing device specifically adopts the following operating steps: Step 1: Prepare a standard stress corrosion specimen. Pass the standard specimen through the center hole of the test kettle cover and install it in the specimen jacket 4 of the stress ring. Ensure good contact between the specimen and the specimen jacket 4 to avoid slipping or loosening. The specimen jacket 4 described in the present invention is a replaceable mold that can meet the needs of stress corrosion specimens of different sizes and shapes, not limited to the standard specimen sizes and shapes described in NACE TM0177-05 Method A.

[0043] Step 2: Secure the captive bolts on the test kettle lid and test the kettle's sealing performance. Use the gas control assembly to fill the test kettle with nitrogen. Transmit the pressure data inside the kettle to the stress ring control system via pressure sensor 23, and observe whether the pressure changes over time. If the pressure does not change, indicating that the test kettle is airtight, the gas control assembly is used to release the pressure and reintroduce the required gas and pressure. Add deionized water to the liquid inlet 19 of the ultrasonic humidifier 17, and adjust the desired humidity inside the kettle using the ultrasonic humidifier's control panel.

[0044] It should be noted that, in addition to N2 and H2, the device of the present invention can also introduce gases such as CO2, O2 and H2S, as well as various corrosive gas media required for the test.

[0045] Step 3: Adjust the tip of the scanning probe 14 to the sample surface by adjusting the driving arm 12; It should be noted that when the tip of the scanning probe 14 contacts the sample surface, the bias source 13 transfers charge to the probe via the drive arm 12, creating a tiny potential difference. This tiny signal is amplified and processed by the lock-in amplifier 11, ultimately outputting an image reflecting the potential distribution on the sample surface. The scanning Kelvin probe system described in the present invention is capable of measuring the micro-region properties of materials under varying atmospheric humidity, and even other gaseous environments, and their environmental variations. Its principles are based on existing technology and will not be further elaborated upon here.

[0046] Step 4: Adjust the small bolt on the super-loading bolt 2 and tighten the top bolt to generate a thrust force (axial). The thrust bolt has a small friction diameter, achieving high thrust with relatively low torque, accurately achieving different uniaxial loading stresses. If heating is required, adjust the temperature control assembly to transfer heat through the Hastelloy heating pipe in the test kettle. A temperature sensor 16 is installed inside the test kettle to monitor the temperature inside the test kettle at all times.

[0047] It should be noted that earlier stress rings used a single nut to apply load, making it difficult to accurately and repeatedly provide unidirectional tensile loads. The present invention's device, utilizing the super-load bolt 2, avoids these drawbacks of traditional stress rings. Furthermore, the stress ring's load monitoring unit measures the load value online. If the load changes during the test, adjustments can be made by adjusting the small bolt on the super-load bolt 2.

[0048] Step 5: Start the stress ring to conduct stress corrosion testing and the scanning Kelvin probe system to conduct micro-corrosion potential testing. During the experiment, the deformation and stress of the sample can be monitored in real time through the timing control system. When the sample surface breaks, the fracture sensor transmits the fracture signal to the timing control system, which issues an alarm.

[0049] If a stress corrosion test under slow strain rate tension (dynamic load) is to be performed, the only change in step 1 is to unload the small bolt on the super-loaded bolt 2 and input the required strain rate through the stress ring control system. If a combination of the two is required, it can be achieved by simply inputting the required strain rate through the stress ring control system after performing step 1 above. In summary, the present invention, based on the stress ring test system, incorporates a slow strain rate tensile test system and the scanning Kelvin probe system to non-destructively study the micro-corrosion potential changes during stress corrosion of test specimens. This allows for more accurate investigation of the causes of stress corrosion cracking in materials under complex operating conditions and loading conditions, and reveals the mechanisms of stress corrosion. This represents a significant improvement over existing technologies.

[0050] Reference Figure 4 The embodiment of the present invention provides a material stress and micro-electrochemical in-situ corrosion potential testing method, which is used in a material stress and micro-electrochemical in-situ corrosion potential testing system. The material stress and micro-electrochemical in-situ corrosion potential testing system includes a test planning terminal and a plurality of material stress and micro-electrochemical in-situ corrosion potential testing devices as described in any one of the above. The method includes: S1: Obtain a set of sample test requirements for several material product production lines during a target test period; wherein the sample test task set includes the sample attributes and sample test frequency of each material product production line; S2: matching a sample test condition set for each material product production line based on the sample test characteristics in the sample attributes, and generating a sample test task list for a target test period based on the sample test condition set and the sample test frequency; wherein the sample test condition set includes a load test mode, a corrosive gas type, a test temperature, a test humidity, and a test pressure; S3: querying the initial sample test condition set of each material stress and micro-electrochemical in-situ corrosion potential testing device at the initial moment of the target test period, sequentially selecting the sample test tasks and the test period of each sample test task that are assigned to each material stress and micro-electrochemical in-situ corrosion potential testing device and are sequentially executed during the target test period from the sample test task list, using an optimization algorithm to solve the sample test tasks and the test period of each sample test task that are sequentially executed by each material stress and micro-electrochemical in-situ corrosion potential testing device during the target test period, and generating a sample test allocation strategy; S4: According to the sample test allocation strategy, generate a set of sample test conditions for each material stress and micro-electrochemical in-situ corrosion potential testing device at different times during the target test period, and perform sample tests on several material product production lines during the target test period based on the sample test condition sets at different times.

[0051] It should be noted that in the actual application scenarios of material testing (such as random inspections of material product production lines), material products produced by different material product production lines may have different random inspection test frequencies and test condition requirements (such as different load testing methods, humidity, temperature, pressure, and corrosive gas environments, etc.) due to their applications in different environments and scenarios. When faced with different test condition requirements, existing testing devices are unable to efficiently and accurately achieve the joint adjustment of multiple test conditions. When continuous testing of multiple sample test tasks is required, it is also necessary to ensure that the parameter adjustment speed of multiple test conditions meets the multi-task test execution conditions and the switching of test devices is minimized to improve the efficiency and operational reliability of the test system. In order to solve the above problems, this embodiment takes into account the different sample testing requirements of several material product production lines in the target test period, and realizes high-accuracy and high-flexibility adjustment of multiple test conditions under multiple stress loads. The optimization algorithm is used to solve the sample testing tasks and the test period of each sample testing task that are performed in sequence by each material stress and micro-electrochemical in-situ corrosion potential testing device in the target test period, and a scientific and reasonable sample testing allocation strategy is generated. While ensuring that the test frequency requirements and test device switching targets of parallel task testing of multiple material product production lines are met, the efficiency and operational reliability of the test system are improved.

[0052] Furthermore, the sample test tasks and the test period of each sample test task that are assigned to each material stress and micro-electrochemical in-situ corrosion potential test device and are sequentially executed during the target test period are selected from the sample test task list. An optimization algorithm is used to solve the sample test tasks and the test period of each sample test task that are sequentially executed during the target test period by each material stress and micro-electrochemical in-situ corrosion potential test device, and generate a sample test allocation strategy step, which specifically includes: S31: Selecting, from the sample test task list, the sample test tasks that are assigned to each material stress and micro-electrochemical in-situ corrosion potential test device and are sequentially executed during the target test period and the test period of each sample test task to solve the sample test allocation strategy; S32: The first constraint condition is to make the interval time between two adjacent sample test tasks of each material product production line when being executed by the material stress and micro-electrochemical in-situ corrosion potential testing device shorter than the interval time corresponding to the sample test frequency of the material product line; the second constraint condition is to make the sample test condition adjustment time of adjusting the sample test condition set of the previous sample test task to the sample test condition set of the next sample test task when each material stress and micro-electrochemical in-situ corrosion potential testing device executes two adjacent sample test tasks shorter than the interval time between the test periods of the previous sample test task and the next sample test task; and the optimization goal is to minimize the number of times two adjacent sample test tasks of each material product production line are executed by different material stress and micro-electrochemical in-situ corrosion potential testing devices; S33: An optimization algorithm is used to solve the sample test tasks and the test period of each sample test task that are sequentially performed by each material stress and micro-electrochemical in-situ corrosion potential test device during the target test period, and a sample test allocation strategy is generated.

[0053] In this embodiment, the first constraint condition is that the interval between any two times that the sample of each material product production line is subjected to the material stress and micro-electrochemical in-situ corrosion potential testing device satisfies the sample test frequency (ensuring that the sample test frequency of each material product production line meets the requirements), and the second constraint condition is that the interval between any two adjacent sample test tasks performed by each material stress and micro-electrochemical in-situ corrosion potential testing device is longer than the sample test condition adjustment time taken for the sample test condition set of the previous sample test task to be adjusted to the sample test condition set of the next sample test task (ensuring that the switching adjustment speed of the sample test condition set of each material stress and micro-electrochemical in-situ corrosion potential testing device meets the requirements ), with the minimum sum of the switching frequencies of the sample test tasks of each material product production line in the material stress and micro-electrochemical in-situ corrosion potential testing device as the optimization goal (minimizing the number of switching times of the task execution device allocation, reducing the overall error rate of the material product production line test tasks, and improving reliability), an optimization algorithm (such as a genetic algorithm) is used to solve the most suitable sample test tasks and the most suitable test time period for each sample test task to be executed in sequence by each material stress and micro-electrochemical in-situ corrosion potential testing device during the target test period. While ensuring that the test frequency requirements and test device switching targets of the parallel task testing of multiple material product production lines are met, the test system efficiency and operational reliability are improved.

[0054] It should be noted that each material stress and micro-electrochemical in-situ corrosion potential testing device is adjusted from the sample test condition set of the previous sample test task to the sample test condition set of the next sample test task. The sample test conditions that need to be switched and adjusted include the load test mode (for example, switching from a single static load test to a single dynamic load test), the type of corrosion gas (for example, switching from H2 to CO2), the test temperature (for example, switching from 40°C to 80°C), the test humidity (for example, switching from 30% to 50%) and the test pressure (0.5MPa to 0.3MPa). The estimation of the time consumption for adjusting the sample test conditions can be matched in the pre-stored test mapping relationship table of the switching adjustment parameter values ​​of different sample test condition sets and the corresponding adjustment time consumption. After obtaining the sample test condition adjustment time consumption, the sample test allocation strategy planning and solution considering the second constraint condition is performed.

[0055] Other embodiments or specific implementations of the material stress and micro-electrochemical in-situ corrosion potential testing method of the present invention can refer to the above-mentioned device embodiments and will not be repeated here.

[0056] It should be understood that, in the description of this specification, reference to terms such as "one embodiment," "another embodiment," "other embodiments," or "first to Nth embodiments" means that the specific features, structures, materials, or characteristics described in conjunction with that embodiment or example are included in at least one embodiment or example of the present invention. In this specification, the schematic representation of the above terms does not necessarily refer to the same embodiment or example. Moreover, the specific features, structures, materials, or characteristics described may be combined in any appropriate manner in any one or more embodiments or examples.

[0057] It should be noted that, in this document, the terms "comprises," "includes," or any other variations thereof are intended to encompass non-exclusive inclusion, such that a process, method, article, or system comprising a series of elements includes not only those elements but also other elements not explicitly listed, or elements inherent to such process, method, article, or system. In the absence of further limitations, an element defined by the phrase "comprising a ..." does not exclude the presence of other identical elements in the process, method, article, or system comprising the element.

[0058] The above are only preferred embodiments of the present invention and are not intended to limit the patent scope of the present invention. Any equivalent structure or equivalent process transformation made using the contents of the present invention description and drawings, or directly or indirectly applied in other related technical fields, are also included in the patent protection scope of the present invention.

Claims

1. A material stress and micro-electrochemical in-situ corrosion potential testing device, characterized in that: include: Multimodal dynamic loading control system, including static load test assembly, dynamic load test assembly, displacement sensor and load sensor; The static load test assembly and the dynamic load test assembly are configured to apply a static load test tensile force and / or a dynamic load test tensile force to a fixed target test specimen according to the test item of the target test specimen; the displacement sensor and the load sensor are configured to monitor the change in the axial displacement parameter and the load parameter of the target test specimen when subjected to the tensile force; Nanoscale multi-spectral domain electrochemical topology mapping system, including a sealed test kettle and a scanning Kelvin micro-area corrosion potential test component; The sealed test kettle is configured to provide a corrosive gas environment for the target test sample fixed in the sealed test kettle according to the test items of the target test sample; the scanning Kelvin micro-area corrosion potential test assembly is configured to perform micro-area corrosion electrochemical testing on the target test sample in the corrosive gas environment according to the test items of the target test sample; A sample test condition control system, comprising a quantum micro-field humidity coupling control component, a temperature control component, and a gas control component, configured to control humidity parameters, temperature parameters, and pressure parameters in a sealed test kettle where the target test sample is located according to the test items of the target test sample; The timing control system is configured to monitor the displacement parameters, load parameters, electrochemical parameters, humidity parameters, temperature parameters and pressure parameters of the target test specimen when executing the test item, and control the test item to stop when it is detected that the target test specimen is broken.

2. The material stress and micro-electrochemical in-situ corrosion potential testing device according to claim 1, characterized in that: The static load test assembly specifically includes: The stress ring body is disposed on the base and adopts an elastic body that generates a reaction force after compression deformation and is configured to apply static tensile stress to the target test specimen; A super loading bolt is provided on the upper side of the stress ring body and applies load through a plurality of small bolts. The super loading bolt is provided with a first load sensor for collecting load parameters of the target test specimen when subjected to static tensile stress and transmitting the load parameters to the stress ring control system; The specimen jacket is configured to fix the target test specimen and is connected to the super loading bolt to apply the load provided by the super loading bolt to the target test specimen as static tensile stress.

3. The material stress and micro-electrochemical in-situ corrosion potential testing device according to claim 2, characterized in that: The sample jacket is configured to fix the target test sample directly or indirectly by using at least one of two-point bending, three-point bending and four-point bending molds.

4. The material stress and micro-electrochemical in-situ corrosion potential testing device according to claim 1, characterized in that: The dynamic load test assembly specifically includes: A hydraulic loading frame and a hydraulic loading head, wherein the hydraulic loading head is arranged on the hydraulic loading frame and connected to the super loading bolts, and the hydraulic loading frame is fixed to the upper side of the stress ring body by fastening bolts; The micro-stepping motor drive device is configured to control a hydraulic loading head to drive a sample jacket via a super loading bolt to apply dynamic tensile stress to a target test sample. A second load sensor is provided between the hydraulic loading head and the sample jacket for collecting load parameters of the target test sample when subjected to dynamic tensile stress and transmitting the load parameters to the stress ring control system.

5. The material stress and micro-electrochemical in-situ corrosion potential testing device according to claim 4, characterized in that: The hydraulic loading head is configured to use a ball screw, and a grating sensor is provided between the ball screw and the hydraulic loading frame. The ball screw and the grating sensor jointly drive the sample jacket to apply dynamic tensile stress of a target strain rate to the target test sample.

6. The material stress and micro-electrochemical in-situ corrosion potential testing device according to claim 1, characterized in that: The displacement sensor specifically includes a non-contact laser extensometer, which is installed outside the observation window of the sealed test kettle and is configured to monitor the change in axial displacement parameters of the target test sample when it is subjected to a tensile force.

7. The material stress and micro-electrochemical in-situ corrosion potential testing device according to claim 1, characterized in that: The sealed test kettle specifically comprises: A sealed cavity, wherein the sealed cavity is provided with a detachable sealing cover, a sample mounting hole is provided at the center of the detachable sealing cover, and the target test sample is arranged in the sealed cavity and extends through the sample mounting hole to be fixed through the sample jacket; The sealed cavity is provided with a humidity regulating port connected to a quantum micro-field humidity coupling control component. The quantum micro-field humidity coupling control component includes an ultrasonic humidifier arranged on the outside and a humidity transmitter arranged inside the sealed test kettle, and is configured to control the humidity parameters in the sealed test kettle where the target test sample is located according to the test items of the target test sample; The sealed cavity is provided with an exhaust port and an air inlet connected to a gas control assembly. The gas control assembly includes a gas distributor, a gas cylinder assembly, and a pressure sensor disposed inside the sealed test kettle. The gas control assembly is configured to inject corrosive gas into the sealed cavity according to the test items of the target test specimen, thereby controlling the pressure parameters inside the sealed test kettle where the target test specimen is located. A temperature control component is provided in the sealed cavity, and the temperature control component includes a temperature sensor and a heating tube, and is configured to control the temperature parameters in the sealed test kettle where the target test sample is located according to the test items of the target test sample.

8. The material stress and micro-electrochemical in-situ corrosion potential testing device according to claim 1, characterized in that: The scanning Kelvin micro-area corrosion potential test assembly specifically includes: A driving arm and a scanning probe, wherein the scanning probe is connected to an external lock-in amplifier via a bias source fixed to the driving arm; In which, the scanning probe is configured to contact the surface of the target test sample, the bias source is configured to transfer charge to the probe through the driving arm to form a potential difference, and the phase-locked amplifier is configured to detect the weak signal of the potential difference and compare it with the reference signal to realize micro-area corrosion electrochemical testing of the target test sample in a corrosive gas environment.

9. A material stress and micro-electrochemical in-situ corrosion potential testing method, characterized in that: A material stress and micro-electrochemical in-situ corrosion potential testing system is used, wherein the material stress and micro-electrochemical in-situ corrosion potential testing system comprises a test planning terminal and a plurality of material stress and micro-electrochemical in-situ corrosion potential testing devices according to any one of claims 1 to 8. The method comprises: S1: Obtain a set of sample test requirements for several material product production lines during a target test period; wherein the sample test task set includes the sample attributes and sample test frequency of each material product production line; S2: matching a sample test condition set for each material product production line based on the sample test characteristics in the sample attributes, and generating a sample test task list for a target test period based on the sample test condition set and the sample test frequency; wherein the sample test condition set includes a load test mode, a corrosive gas type, a test temperature, a test humidity, and a test pressure; S3: querying the initial sample test condition set of each material stress and micro-electrochemical in-situ corrosion potential testing device at the initial moment of the target test period, sequentially selecting the sample test tasks and the test period of each sample test task that are assigned to each material stress and micro-electrochemical in-situ corrosion potential testing device and are sequentially executed during the target test period from the sample test task list, using an optimization algorithm to solve the sample test tasks and the test period of each sample test task that are sequentially executed by each material stress and micro-electrochemical in-situ corrosion potential testing device during the target test period, and generating a sample test allocation strategy; S4: According to the sample test allocation strategy, generate a set of sample test conditions for each material stress and micro-electrochemical in-situ corrosion potential testing device at different times during the target test period, and perform sample tests on several material product production lines during the target test period based on the sample test condition sets at different times.

10. The material stress and micro-electrochemical in-situ corrosion potential testing method according to claim 9, characterized in that: The sample test tasks and the test period of each sample test task that are sequentially assigned to each material stress and micro-electrochemical in-situ corrosion potential test device and executed sequentially during the target test period are sequentially selected from the sample test task list. The sample test tasks and the test period of each sample test task that are sequentially executed by each material stress and micro-electrochemical in-situ corrosion potential test device during the target test period are solved using an optimization algorithm to generate a sample test allocation strategy, specifically including: S31: Selecting, from the sample test task list, the sample test tasks that are assigned to each material stress and micro-electrochemical in-situ corrosion potential test device and are sequentially executed during the target test period and the test period of each sample test task to solve the sample test allocation strategy; S32: The first constraint condition is to make the interval time between two adjacent sample test tasks of each material product production line when being executed by the material stress and micro-electrochemical in-situ corrosion potential testing device shorter than the interval time corresponding to the sample test frequency of the material product line; the second constraint condition is to make the sample test condition adjustment time of adjusting the sample test condition set of the previous sample test task to the sample test condition set of the next sample test task when each material stress and micro-electrochemical in-situ corrosion potential testing device executes two adjacent sample test tasks shorter than the interval time between the test periods of the previous sample test task and the next sample test task; and the optimization goal is to minimize the number of times two adjacent sample test tasks of each material product production line are executed by different material stress and micro-electrochemical in-situ corrosion potential testing devices; S33: An optimization algorithm is used to solve the sample test tasks and the test period of each sample test task that are sequentially performed by each material stress and micro-electrochemical in-situ corrosion potential test device during the target test period, and a sample test allocation strategy is generated.

Images