Metal corrosion test device and test method for HF atmosphere

Abstract

The invention relates to the technical field of metal corrosion test, and discloses a metal corrosion test device and test method for HF atmosphere, the metal corrosion test device comprises a furnace body, a to-be-tested metal sample is arranged in the furnace body, and a mixed gas inlet and a mixed gas outlet are respectively arranged at two ends of the furnace body; the atmosphere supply system is communicated with the mixed gas inlet through a first pipeline, and the atmosphere supply system is used for preparing HF gas and conveying the HF gas to the furnace body; the temperature control system is arranged on the furnace body and is used for controlling the temperature in the furnace body; the gas adjusting system is arranged on the furnace body and is used for controlling the gas flow rate of the mixed gas inlet; and the monitoring system is arranged on the furnace body and is used for monitoring the change of the metal sample to be detected. According to the invention, a stable HF atmosphere environment and accurate temperature control can be provided, and the gas fluidity can be ensured, so that the corrosion behavior of metal under real working conditions can be better simulated, and support and reference are provided for related fields.

Description

Technical Field

[0001] The present invention relates to the technical field of metal corrosion testing, in particular to a metal corrosion testing device and a testing method for HF atmosphere. Background Art

[0002] With the rapid development of the photovoltaic industry, the recycling of a large number of waste photovoltaic modules has become increasingly problematic. Pyrolysis, a key recycling method for photovoltaic modules, effectively separates high-value materials from them. However, the thermal decomposition of photovoltaic backsheets during the pyrolysis process releases large amounts of fluorine-containing gases, particularly hydrofluoric acid (HF), which can severely corrode the furnace material and shorten the equipment's service life.

[0003] Laser cladding is a material surface modification technology that uses a high-energy-density laser beam as a heat source to deposit a layer of alloy material on the surface of the material, achieving metallurgical bonding between the cladding material and the underlying material. The molten pool formed by the high-energy laser beam can generate a dense coating structure during rapid cooling. The corrosion-resistant elements (such as Cr, Ni, Mo, etc.) added to the cladding coating can form a stable protective oxide layer or passivation film, further enhancing corrosion resistance. The formation of a uniform, dense cladding layer on the surface of 316L stainless steel can effectively prevent contact between the corrosive medium and the base material, reducing the occurrence of corrosion reactions. This effectively improves the service life and reliability of the material in corrosive environments.

[0004] The existing technology still lacks test equipment for HF environment corrosion resistance testing, which cannot provide a basis for the selection of pyrolysis furnace materials and life extension during the recycling of photovoltaic modules, and cannot provide a reference for solving the corrosion problem of metal materials in fluorine-containing environments.

[0005] Therefore, there is an urgent need for a metal corrosion test device and test method for HF atmosphere to solve the above problems. Summary of the Invention

[0006] The object of the present invention is to provide a metal corrosion test device and test method for HF atmosphere to solve the problems existing in the above-mentioned prior art.

[0007] To achieve the above object, the present invention provides the following solution: The present invention provides a metal corrosion test device for HF atmosphere, comprising:

[0008] A furnace body, wherein a metal sample to be tested is arranged inside, and a mixed gas inlet and a mixed gas outlet are respectively provided at both ends of the furnace body;

[0009] an atmosphere supply system, connected to the mixed gas inlet through a first pipe, the atmosphere supply system being used to prepare HF gas and deliver the HF gas to the furnace body;

[0010] a temperature control system, disposed on the furnace body, for controlling the temperature inside the furnace body;

[0011] a gas regulating system, provided on the furnace body, for controlling the gas flow rate of the mixed gas inlet;

[0012] The monitoring system is arranged on the furnace body and is used to monitor changes in the metal sample to be tested.

[0013] According to a metal corrosion testing device for HF atmosphere provided by the present invention, the atmosphere supply system includes a nitrogen gas source and an HF generator, the nitrogen gas source and the HF generator are respectively connected to an atmosphere mixing tank through pipelines, and the atmosphere mixing tank is connected to the first pipeline.

[0014] According to a metal corrosion testing device for HF atmosphere provided by the present invention, the temperature control module includes a temperature sensing module, a heating module, and a temperature control module. The temperature sensing module is used to monitor the temperature, the heating module is used to heat the metal sample to be tested, and the temperature control module is used to adjust the temperature in the furnace body.

[0015] According to a metal corrosion testing device for HF atmosphere provided by the present invention, the gas regulating module includes a gas circulation module and a gas flow rate control module, and the gas flow rate control module is used to adjust the flow rate and distribution of the gas.

[0016] According to a metal corrosion test device for HF atmosphere provided by the present invention, the monitoring system includes a monitoring module and an alarm module, the monitoring module is used to monitor changes in the metal sample to be tested, and the alarm module is used to issue an alarm.

[0017] According to the present invention, a metal corrosion test device for HF atmosphere further includes a tail gas recovery tank, which is connected to the mixed gas outlet through a second pipeline.

[0018] According to the present invention, a metal corrosion test device for HF atmosphere is provided. In the HF generating device, fluorite and sulfuric acid are used as reaction raw materials, and a lead can is used as a reaction container to generate HF gas.

[0019] According to the metal corrosion test device for HF atmosphere provided by the present invention, the metal sample to be tested is one of a stainless steel plate, a nickel-based alloy plate or a laser cladding coating plate.

[0020] According to the metal corrosion testing device for HF atmosphere provided by the present invention, the furnace body is a tubular furnace.

[0021] A metal corrosion test method for HF atmosphere comprises the following steps:

[0022] The metal sample to be tested is cleaned, weighed, and then installed in the furnace body;

[0023] After preheating the furnace body, the HF atmosphere is delivered into the furnace body through the atmosphere supply system, and the HF concentration is 10%-40%;

[0024] The temperature in the furnace is adjusted by the temperature control system, and the temperature is raised to three groups of 25°C, 60°C, and 90°C at a heating rate of 10°C / min, and then kept warm;

[0025] After the test is completed, the metal sample to be tested is taken out, cleaned, and weighed again, and the corrosion rate is calculated using the weight loss method.

[0026] Compared with the prior art, the present invention has the following advantages and technical effects:

[0027] The present invention provides a metal corrosion testing device and method for an HF atmosphere. A metal sample to be tested is placed within a furnace via a bracket. An atmosphere supply system injects atmosphere into the furnace. A temperature control system regulates the temperature during the test. A gas regulation system ensures stable gas delivery. A monitoring system collects test data. This application provides a stable HF atmosphere, precise temperature control, and guaranteed gas flow to better simulate the corrosion behavior of metals under real-world operating conditions, providing support and reference for related fields. BRIEF DESCRIPTION OF THE DRAWINGS

[0028] In order to more clearly illustrate the embodiments of the present invention or the technical solutions in the prior art, the following briefly introduces the drawings required for use in the embodiments. Obviously, the drawings described below are only some embodiments of the present invention. Those skilled in the art can also derive other drawings based on these drawings without inventive work.

[0029] Figure 1 It is a schematic diagram of the overall structure of the present invention;

[0030] Figure 2 This is the macroscopic morphology of the 316L stainless steel after corrosion in hydrofluoric acid atmosphere under different conditions of the present invention;

[0031] Figure 3 The corrosion rate of 316L stainless steel in a hydrofluoric acid atmosphere varies with the concentration of hydrofluoric acid.

[0032] Figure 4 This is the macroscopic morphology of the Inconel625 nickel-based alloy after corrosion in HF atmosphere;

[0033] Figure 5 The corrosion rate of the nickel-based alloy Inconel 625 in an HF atmosphere varies with the concentration of hydrofluoric acid.

[0034] Figure 6 This is a macroscopic morphology of the cladding coating of the present invention after corrosion in HF atmosphere;

[0035] Figure 7 This is the element distribution result diagram of the laser cladding coating of the present invention;

[0036] Figure 8 This is a comparison chart of the corrosion rates of the laser cladding coatings of the present invention;

[0037] Among them, 1. furnace body; 2. metal sample to be tested; 3. mixed gas inlet; 4. mixed gas outlet; 5. first pipeline; 6. nitrogen gas source; 7. HF generator; 8. atmosphere mixing tank; 9. tail gas recovery tank; 10. second pipeline. DETAILED DESCRIPTION

[0038] The following will clearly and completely describe the technical solutions in the embodiments of the present invention in conjunction with the accompanying drawings. Obviously, the described embodiments are only part of the embodiments of the present invention, not all of the embodiments. Based on the embodiments of the present invention, all other embodiments obtained by ordinary technicians in this field without making creative efforts are within the scope of protection of the present invention.

[0039] In order to make the above-mentioned objects, features and advantages of the present invention more obvious and easy to understand, the present invention is further described in detail below with reference to the accompanying drawings and specific embodiments.

[0040] Reference Figures 1-8 The present invention provides a metal corrosion test device for HF atmosphere, comprising:

[0041] A furnace body 1 is provided with a metal sample 2 to be tested, and a mixed gas inlet 3 and a mixed gas outlet 4 are provided at both ends of the furnace body 1;

[0042] An atmosphere supply system is connected to the mixed gas inlet 3 through a first pipe 5, and the atmosphere supply system is used to prepare HF gas and deliver the HF gas to the furnace body 1;

[0043] A temperature control system is provided on the furnace body 1 and is used to control the temperature inside the furnace body 1;

[0044] A gas regulating system is provided on the furnace body 1 and is used to control the gas flow rate of the mixed gas inlet 3;

[0045] The monitoring system is arranged on the furnace body 1 and is used to monitor the changes of the metal sample 2 to be tested.

[0046] In one embodiment of the present invention, the metal sample 2 to be tested is placed in the furnace body 1 through a bracket, the atmosphere is injected into the furnace body 1 through a set atmosphere supply system, the temperature during the test is adjusted by a set temperature control system, the stable delivery of the gas is ensured by a set gas regulation system, and the test data is collected by a set monitoring system.

[0047] As an optional embodiment, the atmosphere supply system includes a nitrogen source 6 and an HF generator 7 , the nitrogen source 6 and the HF generator 7 are respectively connected to an atmosphere mixing tank 8 through pipelines, and the atmosphere mixing tank 8 is connected to the first pipeline 5 .

[0048] In one embodiment of the present invention, the required atmosphere is produced by an atmosphere mixing tank 8 and transported into the furnace body 1 .

[0049] As an optional embodiment, the temperature control module includes a temperature sensing module, a heating module, and a temperature control module. The temperature sensing module is used to monitor the temperature, the heating module is used to heat the metal sample 2 to be tested, and the temperature control module is used to adjust the temperature inside the furnace body 1.

[0050] In one embodiment of the present invention, the temperature inside the furnace body 1 is monitored by a temperature sensing module, electric heating is performed by a heating module, and the temperature inside the furnace body 1 is controlled by a temperature control module.

[0051] Specifically, the temperature control module includes a K-type thermocouple for temperature sensing, a 900°C tube furnace module selected from Hefei Kejing OTF-400X-IDH-ZM for heating, and temperature control directly using the SR93 on the island power supply, ±0.01°C, and Modbus RTU.

[0052] As an optional implementation, the gas regulation module includes a gas circulation module and a gas flow rate control module, and the gas flow rate control module is used to adjust the flow rate and distribution of the gas.

[0053] In one embodiment of the present invention, the flow of gas is achieved by a gas circulation module, and the flow rate and distribution of gas are controlled by a gas flow rate control module.

[0054] As an optional implementation, the monitoring system includes a monitoring module and an alarm module. The monitoring module is used to monitor changes in the metal sample 2 to be tested, and the alarm module is used to issue an alarm.

[0055] In one embodiment of the present invention, a monitoring module is provided to monitor changes in the metal sample 2 to be tested and collect image data, and an alarm module is provided to provide audio and visual warnings for temperature, gas leakage, etc. during the test.

[0056] As an optional embodiment, the system further includes a tail gas recovery tank 9 , which is connected to the mixed gas outlet 4 through a second pipe 10 .

[0057] In one embodiment of the present invention, the tail gas recovery tank 9 is provided to recover the generated tail gas to avoid environmental pollution.

[0058] As an optional embodiment, the HF generating device 7 uses fluorite and sulfuric acid as reaction raw materials and a lead can as a reaction container to generate HF gas.

[0059] In one embodiment of the present invention, fluorite and sulfuric acid are used as reaction raw materials to continuously and stably generate HF gas.

[0060] As an optional embodiment, the metal sample 2 to be tested is one of a stainless steel plate, a nickel-based alloy plate or a laser cladding coating plate.

[0061] In one embodiment of the present invention, the metal sample 2 to be tested is one of 316L stainless steel plate, Inconel625 nickel-based alloy plate and laser cladding Inconel625 coating plate, and a control test is performed.

[0062] As an optional embodiment, the furnace body 1 is a tubular furnace.

[0063] In one embodiment of the present invention, the furnace body 1 is preferably a tubular furnace.

[0064] A metal corrosion test method for HF atmosphere comprises the following steps:

[0065] The metal sample 2 to be tested is cleaned, weighed, and then installed in the furnace body 1;

[0066] After preheating the furnace body 1, an HF atmosphere is supplied into the furnace body 1 through the atmosphere supply system, and the HF concentration is 10%-40%;

[0067] The temperature in the furnace body 1 is adjusted by a temperature control system, and the temperature is raised to three sets of temperatures of 25°C, 60°C, and 90°C at a heating rate of 10°C / min, and then kept warm;

[0068] After the test is completed, the metal sample 2 to be tested is taken out, cleaned and weighed again, and the corrosion rate is calculated using the weight loss method.

[0069] In one embodiment of the present invention, when in use:

[0070] Sample preparation: Corrosion experiments were conducted using 316L stainless steel plates, Inconel625 nickel-based alloy plates, and laser-clad Inconel625 coatings. HF solution was used as the corrosion reagent, and the plates were cut into 25mm×25mm×3mm thin plates using a wire cutter. A hole was punched at one end of the sample for easy hanging. The hole size was 3mm. Before the experiment began, the surface was cleaned, polished with 400-2000# sandpaper, polished with 1μm diamond polishing paste, and then ultrasonically cleaned in alcohol. The experiment was then conducted using a polytetrafluoroethylene tank, and the samples were subjected to corrosion experiments using a hanging plate method. The metal sample 2 to be tested was weighed and placed on a dedicated bracket in the experimental device to ensure sample stability.

[0071] Furnace preheating: Open the nitrogen source 6, introduce nitrogen into the furnace 1, and heat the furnace 1 to 100°C and keep it warm for 10 minutes.

[0072] Atmosphere adjustment: After opening the tail gas recovery tank 9, start the HF generator 7 and adjust the atmosphere mixing ratio so that the furnace body 1 forms the required HF atmosphere with an HF concentration of 10%-40%.

[0073] Temperature setting: The target temperature of the furnace body 1 is set by the temperature control system, and the temperature is increased to three groups of 25°C, 60°C, and 90°C at a heating rate of 10°C / min, and then kept warm.

[0074] Experimental process: The holding time at the required experimental temperature shall not exceed 240 h, and the temperature and HF gas concentration in the furnace body 1 shall be closely monitored.

[0075] After the experiment, turn off the HF generator 7 and continue to introduce nitrogen into the furnace 1. Stop the nitrogen introduction after the residual HF in the furnace 1 is completely exhausted. Finally, close the tail gas recovery tank 9. Then, cool the metal sample 2 in air. After cooling, remove the surface corrosion products and weigh the sample. Clean the sample surface, rinse and dry it, and weigh it again. Record the sample mass and calculate the corrosion rate using the weight loss method. To ensure the accuracy of the results, perform three replicates for each test condition and calculate the average value.

[0076] In one embodiment of the present invention, 316L stainless steel sample with a size of 40 mm × 20 mm × 3 mm was corroded at 25°C, 60°C, and 90°C for 240 h in an atmosphere with HF concentrations of 10%, 24%, and 40%, and the corrosion resistance of the atmosphere was tested.

[0077] Reference Figure 2Macromorphology of 316L stainless steel after corrosion in hydrofluoric acid atmosphere under different conditions: (a) 10% HF / 25℃; (b) 24% HF / 25℃; (c) 40% HF / 25℃; (d) 10% HF / 60℃; (e) 24% HF / 60℃; (f) 40% HF / 60℃; (g) 10% HF / 90℃; (h) 24% HF / 90℃; (i) 40% HF / 90℃.

[0078] In one embodiment of the present invention, a sample of Inconel 625 nickel-based alloy with a size of 40 mm × 20 mm × 3 mm was corroded at 25°C, 60°C, and 90°C for 240 h in an atmosphere with HF concentrations of 10%, 24%, and 40%.

[0079] Reference Figure 4 Macromorphology of Inconel625 nickel-based alloy after corrosion in HF atmosphere (a) 10% HF / 25℃; (b) 24% HF / 25℃; (c) 40% HF / 25℃; (d) 10% HF / 60℃; (e) 24% HF / 60℃; (f) 40% HF / 60℃; (g) 10% HF / 90℃; (h) 24% HF / 90℃; (i) 40% HF / 90℃.

[0080] In one embodiment of the present invention, the optimal process parameters for preparing Inconel625 coating on the surface of 316L stainless steel using a laser cladding method are: a powder feeding rate of 9.6 g / min, a laser power of 2000 W, and a scanning speed of 4 mm / s to prepare an anti-corrosion coating.

[0081] Reference Figure 6 The corrosion results show clear corrosion marks on the coating surface, with corrosion products accumulating on the sample surface, large dark-gray areas, and increased roughness. This indicates that the Inconel 625 coating experienced severe corrosion in the HF atmosphere. The coating exhibited a striped structure after corrosion, which may be due to the microstructure of the cladding layer.

[0082] Reference Figure 7 It can be found that the substrate and the nickel-based alloy coating have good bonding, there is a clear boundary between the cladding layer and the substrate, and the microstructure is mainly composed of dendrites and columnar crystals.

[0083] Reference Figure 8 The average corrosion rate of the laser cladding coating at 90°C and an HF concentration of 40% is 6.25 mm / y. The results show that the laser cladding method can be used to prepare Inconel625 coating on the surface of 316L stainless steel to improve the corrosion resistance of stainless steel against hydrofluoric acid.

[0084] In the description of the present invention, it should be understood that the terms "longitudinal", "transverse", "up", "down", "front", "back", "left", "right", "vertical", "horizontal", "top", "bottom", "inside", "outside", etc., indicating the orientation or position relationship, are based on the orientation or position relationship shown in the accompanying drawings, and are only for the convenience of describing the present invention, rather than indicating or implying that the device or element referred to must have a specific orientation, be constructed and operated in a specific orientation, and therefore cannot be understood as a limitation on the present invention.

[0085] The embodiments described above are merely descriptions of preferred embodiments of the present invention and are not intended to limit the scope of the present invention. Without departing from the spirit of the present invention, various modifications and improvements made to the technical solutions of the present invention by persons skilled in the art should fall within the scope of protection defined by the claims of the present invention.

Claims

1. A metal corrosion test device for HF atmosphere, characterized in that: include: A furnace body (1) is provided with a metal sample (2) to be tested therein, and a mixed gas inlet (3) and a mixed gas outlet (4) are provided at both ends of the furnace body (1); an atmosphere supply system, connected to the mixed gas inlet (3) via a first pipe (5), the atmosphere supply system being used to prepare HF gas and deliver the HF gas to the furnace body (1); A temperature control system, arranged on the furnace body (1), for controlling the temperature inside the furnace body (1); a gas regulating system, arranged on the furnace body (1) and used for controlling the gas flow rate of the mixed gas inlet (3); A monitoring system is provided on the furnace body (1) and is used to monitor changes in the metal sample (2) to be tested.

2. The metal corrosion test device for HF atmosphere according to claim 1, characterized in that: The atmosphere supply system comprises a nitrogen gas source (6) and an HF generator (7), wherein the nitrogen gas source (6) and the HF generator (7) are respectively connected to an atmosphere mixing tank (8) through pipelines, and the atmosphere mixing tank (8) is connected to the first pipeline (5).

3. The metal corrosion test device for HF atmosphere according to claim 1, characterized in that: The temperature control module comprises a temperature sensing module, a heating module and a temperature control module. The temperature sensing module is used to monitor the temperature. The heating module is used to heat the metal sample (2) to be tested. The temperature control module is used to adjust the temperature in the furnace body (1).

4. The metal corrosion testing device for HF atmosphere according to claim 1, characterized in that: The gas regulating module includes a gas circulation module and a gas flow rate control module, and the gas flow rate control module is used to adjust the flow rate and distribution of the gas.

5. The metal corrosion testing device for HF atmosphere according to claim 1, characterized in that: The monitoring system comprises a monitoring module and an alarm module, wherein the monitoring module is used to monitor changes in the metal sample (2) to be tested, and the alarm module is used to issue an alarm.

6. The metal corrosion testing device for HF atmosphere according to claim 1, characterized in that: It also includes a tail gas recovery tank (9), which is connected to the mixed gas outlet (4) through a second pipe (10).

7. The metal corrosion testing device for HF atmosphere according to claim 1, characterized in that: In the HF generating device (7), fluorite and sulfuric acid are used as reaction raw materials, and a lead tank is used as a reaction container to generate HF gas.

8. The metal corrosion testing device for HF atmosphere according to claim 1, characterized in that: The metal sample (2) to be tested is one of a stainless steel plate, a nickel-based alloy plate or a laser cladding coating plate.

9. The metal corrosion testing device for HF atmosphere according to claim 1, characterized in that: The furnace body (1) is a tubular furnace.

10. A metal corrosion test method for HF atmosphere, applicable to the metal corrosion test device for HF atmosphere according to claim 1, characterized in that: The following steps are involved: The metal sample (2) to be tested is cleaned and weighed, and then installed in the furnace body (1); After preheating the furnace body (1), HF atmosphere is delivered into the furnace body (1) through the atmosphere supply system, with the HF concentration being 10%-40%; The temperature inside the furnace (1) is adjusted by the temperature control system, and the temperature is raised to three sets of temperatures of 25°C, 60°C, and 90°C at a heating rate of 10°C / min, and then kept warm; After the test is completed, the metal sample (2) to be tested is taken out, cleaned and weighed again, and the corrosion rate is calculated using the weight loss method.

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