Preparation method of corrosion-resistant metal material in seawater environment

Abstract

The invention relates to the technical field of metal material preparation, and in particular to a method for preparing a corrosion-resistant metal material in a seawater environment, comprising placing a base material and a sample material on different sample plates at the same height in a reaction chamber, respectively, introducing a precursor and a reducing gas into the reaction chamber, heating the base material to a preset temperature at the same time, heating the sample material in a preset heating manner, detecting the deposition area of ​​the surface of the sample material per unit time by a reflection spectrum analysis technology and determining the optimal heating temperature of the base material, controlling the sample plate corresponding to the sample material to move around the sample plate where the base material is located in the reaction chamber to determine the optimal deposition position, moving the sample plate corresponding to the base material to the optimal deposition position, and completing the deposition of a surface coating on the base material at the optimal deposition position; ensuring that the coating is deposited under optimal process conditions, so that the final coating is more uniform and dense, thereby effectively improving the corrosion resistance of the deposited coating.

Description

Technical Field

[0001] The present invention relates to the technical field of metal material preparation, and in particular to a method for preparing a corrosion-resistant metal material in a seawater environment. Background Art

[0002] Titanium metal has excellent properties such as low density, high specific strength, good high temperature mechanical properties and creep properties, and is widely used in the fields of aviation, automobiles and ships. However, in the application of the shipbuilding field, the chemical properties of titanium metal are active and its oxidation resistance is poor. The deposition of titanium alloy coatings on base materials such as stainless steel by chemical vapor deposition can effectively solve this problem.

[0003] Chinese patent application publication number CN114836753B discloses a method for depositing a metal tantalum coating on stainless steel. The charging and discharging principle of a pulse circuit is used to build up an electrode (tantalum) on a workpiece substrate (stainless steel). At the moment when the pulse width is 50-100μs, a high current generates an electric spark between the workpiece and the electrode, causing the tantalum electrode to melt and then deposit on the workpiece substrate, thereby being tightly bonded to the workpiece substrate with high strength. The process achieves metallurgical bonding between the coating and the substrate, preventing thermal deformation of the workpiece. The process is used for surface coating, which can improve the corrosion resistance of the workpiece surface and solve the problem of easy corrosion of the workpiece when serving in harsh environments. It has strong practical value.

[0004] However, the above method lacks effective measurement and control of the deposition process, and there is a risk of uneven coating deposition during the deposition process, which in turn leads to low corrosion resistance of metal materials with deposited coatings in the marine field. Summary of the invention

[0005] To this end, the present invention provides a method for preparing corrosion-resistant metal materials in a seawater environment, so as to overcome the lack of effective measurement and control of the deposition process in the prior art, the hidden danger of uneven coating deposition during the deposition process, and the problem of low corrosion resistance of metal materials with deposited coatings in the marine field.

[0006] To achieve the above object, the present invention provides a method for preparing a corrosion-resistant metal material in a seawater environment, comprising:

[0007] Step S1, placing the matrix material and the sample material on different sample plates at the same height in the reaction chamber;

[0008] Step S2, introducing a precursor and a reducing gas into the reaction chamber according to the sizes of the base material and the sample material, and heating the base material to a preset temperature and heating the sample material in a preset heating method;

[0009] Step S3, detecting the deposition area of ​​the surface of the sample material per unit time by reflectance spectrum analysis, and determining the optimal heating temperature of the base material;

[0010] Step S4, after heating the base material and the sample material to the optimal heating temperature, controlling the sample plate corresponding to the sample material to move around the sample plate where the base material is located in the reaction chamber to determine the optimal deposition position;

[0011] Step S5, moving the sample plate corresponding to the base material to the optimal deposition position, so that the base material completes the deposition of the surface coating at the optimal deposition position;

[0012] The preset heating method satisfies that the surface temperature of the sample material within a preset period of time covers a preset temperature range centered on the preset temperature.

[0013] Further, in step S3, determining the optimal heating temperature includes:

[0014] Step S31, detecting the deposition area on the surface of the sample material at every unit time within the preset time period;

[0015] Step S32, determining the temperature corresponding to the detection with the largest deposition area as the optimal heating temperature.

[0016] Further, in step S4, determining the optimal deposition position includes:

[0017] Step S41, controlling the sample plate where the sample material is located to move horizontally at a plurality of positions in the reaction chamber and to stay at each position for the unit time;

[0018] Step S42, respectively detecting the deposition area on the surface of the sample material after the sample plate stops at each position;

[0019] Step S43, determining a first ratio of an average deposition area of ​​the matrix material per unit time to a reaction area of ​​the matrix material, and comparing the first ratio with a second ratio of an average deposition area of ​​the sample material per unit time to a reaction area of ​​the sample material;

[0020] Step S44: if the first ratio is greater than or equal to the second ratio, the position of the base material is maintained; if the first ratio is less than the second ratio, the sample plate corresponding to the base material is moved to a position where the sample material deposition area is the largest.

[0021] Furthermore, the detection of the deposition area includes:

[0022] Step S001, detecting, by reflection spectrum analysis, a second area on the surface of the base material and the sample material where the deposition thickness is greater than a preset thickness;

[0023] Step S002: Determine the difference between the second area and the first area whose deposition thickness is greater than a preset thickness determined by the previous reflection spectrum analysis as the deposition area.

[0024] Furthermore, the matrix material and the sample material are 317L austenitic stainless steel.

[0025] Furthermore, the sample material and the matrix material are both plates, and the size of the sample material is 1 / 20 of the size of the matrix material.

[0026] Further, in step S2, the precursor includes TiCl4 gas, and the reducing gas includes H2.

[0027] Furthermore, the preset temperature is 950°C, and the preset temperature range is 900°C to 1000°C.

[0028] Furthermore, in the step S2, the ratio of the volume of the precursor introduced per unit time to the volume of the reducing gas introduced per unit time is 1:3.

[0029] Furthermore, in step S2, the introduction rate of the precursor is 50 sccm, and the introduction rate of the reducing gas is 120 sccm.

[0030] Compared with the prior art, the beneficial effect of the present invention is that by setting the matrix material and the sample material in the reaction chamber at the same time, the deposition situation on the surface of the sample material is detected in real time by using the reflection spectrum analysis technology, and the optimal heating temperature and deposition position are determined. By setting the above online monitoring and feedback control mechanism, it is ensured that the coating is deposited under the optimal process conditions, making the final coating more uniform and dense, thereby effectively improving the corrosion resistance of the deposited coating.

[0031] Furthermore, by setting up sample materials, the present invention can effectively monitor the reaction process with relatively small raw material input and determine a more optimal reaction state for the matrix material during deposition. The small size of the sample materials makes it easier to perform reflectance spectrum analysis and determine the deposition area, further improving the corrosion resistance of the deposited coating.

[0032] Furthermore, the present invention can determine the optimal heating temperature of the base material by regularly detecting the deposition area on the surface of the sample material, so that the coating deposition efficiency is the highest. The detection frequency is high, and the optimal deposition temperature of the coating on the surface of the sample material can be captured in time to avoid coating defects caused by temperature deviation. The optimal heating temperature thus determined can ensure that the coating with the best performance is deposited on the base material, further improving the corrosion resistance of the deposited coating.

[0033] Furthermore, the present invention can detect the deposition effects of the matrix material and the sample material at different positions through the horizontal movement of the sample plate in the reaction chamber, determine the optimal deposition position, and compare the deposition efficiency per unit area of ​​the matrix material and the sample material. The position of the matrix material can be adjusted in time to ensure that it is located in the area with the best deposition effect. This automatic adjustment mechanism based on deposition efficiency comparison effectively avoids the problem of local uneven deposition due to improper position, improves the overall consistency of the coating, and further improves the corrosion resistance of the deposited coating.

[0034] Furthermore, the present invention can accurately measure the coating thickness on the surface of the substrate material and the sample material through reflection spectrum analysis, avoiding the error caused by relying solely on intuitive observation, and comparing the effective deposition area of ​​the current detection with the result of the previous detection, so as to more accurately determine the actual deposition area per unit time. Compared with directly measuring the deposition area, this difference method based on thickness change can eliminate the interference caused by the change of the substrate / sample surface state, thereby improving the detection accuracy and further improving the corrosion resistance of the deposited coating.

[0035] Furthermore, the 317L stainless steel of the present invention has excellent corrosion resistance and is very suitable for use in marine environments. Using 317L stainless steel as the base material and sample material can ensure that the final deposited coating has excellent performance in corrosion resistance, which helps to give full play to the process advantages of the present invention and further improves the corrosion resistance of the deposited coating. BRIEF DESCRIPTION OF THE DRAWINGS

[0036] Figure 1 This is a flow chart of the method for preparing corrosion-resistant metal materials in seawater environment of the present invention;

[0037] Figure 2 A flow chart for determining the optimal heating temperature for the present invention;

[0038] Figure 3 A flow chart for determining the optimal deposition location for the present invention;

[0039] Figure 4 This is a flow chart of the deposition area detection of the present invention. DETAILED DESCRIPTION

[0040] In order to make the objects and advantages of the present invention more clearly understood, the present invention is further described below in conjunction with embodiments; it should be understood that the specific embodiments described herein are only used to explain the present invention and are not used to limit the present invention.

[0041] The preferred embodiments of the present invention are described below with reference to the accompanying drawings. It should be understood by those skilled in the art that these embodiments are only used to explain the technical principles of the present invention and are not intended to limit the protection scope of the present invention.

[0042] It should be noted that, in the description of the present invention, terms such as "up", "down", "left", "right", "inside" and "outside" indicating directions or positional relationships are based on the directions or positional relationships shown in the drawings. This is merely for the convenience of description and does not indicate or imply that the device or element must have a specific orientation, be constructed and operated in a specific orientation. Therefore, it cannot be understood as a limitation on the present invention.

[0043] In addition, it should be noted that in the description of the present invention, unless otherwise clearly specified and limited, the terms "installed", "connected", and "connected" should be understood in a broad sense, for example, it can be a fixed connection, a detachable connection, or an integral connection; it can be a mechanical connection or an electrical connection; it can be a direct connection, or it can be indirectly connected through an intermediate medium, and it can be the internal communication of two components. For those skilled in the art, the specific meanings of the above terms in the present invention can be understood according to specific circumstances.

[0044] See also Figure 1 As shown, the method for preparing a corrosion-resistant metal material in a seawater environment of the present invention comprises:

[0045] Step S1, placing the matrix material and the sample material on different sample plates at the same height in the reaction chamber;

[0046] Step S2, introducing a precursor and a reducing gas into the reaction chamber according to the sizes of the base material and the sample material, and heating the base material to a preset temperature and heating the sample material in a preset heating method;

[0047] Step S3, detecting the deposition area per unit time on the surface of the sample material by reflectance spectrum analysis, and determining the optimal heating temperature of the base material;

[0048] Step S4, after heating the base material and the sample material to the optimal heating temperature, controlling the sample plate corresponding to the sample material to move around the sample plate where the base material is located in the reaction chamber to determine the optimal deposition position;

[0049] Step S5, moving the sample plate corresponding to the base material to the optimal deposition position, so that the base material completes the deposition of the surface coating at the optimal deposition position;

[0050] The preset heating method satisfies that the surface temperature of the sample material within a preset period of time covers a preset temperature range centered on the preset temperature.

[0051] In the above embodiment, by setting the base material and the sample material in the reaction chamber at the same time, the deposition situation on the surface of the sample material is detected in real time by using the reflection spectrum analysis technology, and the optimal heating temperature and deposition position are determined. By setting the above online monitoring and feedback control mechanism, it is ensured that the coating is deposited under the optimal process conditions, so that the final coating is more uniform and dense, thereby effectively improving the corrosion resistance of the deposited coating. By setting the sample material, the reaction process can be effectively monitored with a small input of raw materials and a better reaction state can be determined for the base material during deposition. The small size of the sample material makes it easier to perform reflection spectrum analysis and determine the deposition area, further improving the corrosion resistance of the deposited coating.

[0052] See also Figure 2 As shown, the determination of the optimal heating temperature includes:

[0053] Step S31, detecting the deposition area on the surface of the sample material every unit time within a preset period of time;

[0054] Step S32, determining the temperature corresponding to the detection of the largest deposition area as the optimal heating temperature.

[0055] In the above embodiment, by regularly detecting the deposition area on the surface of the sample material, the optimal heating temperature of the base material can be determined, so that the coating deposition efficiency is the highest. The detection frequency is high, and the optimal deposition temperature of the coating on the surface of the sample material can be captured in time to avoid coating defects caused by temperature deviation. The optimal heating temperature thus determined can ensure that the coating with the best performance is deposited on the base material, further improving the corrosion resistance of the deposited coating.

[0056] See also Figure 3 As shown, the determination of the optimal deposition position includes:

[0057] Step S41, controlling the sample plate where the sample material is located to move horizontally at several positions in the reaction chamber and to stay at each position for a unit time;

[0058] Step S42, respectively detecting the deposition area on the surface of the sample material after the sample plate stops at each position;

[0059] Step S43, determining a first ratio of an average deposition area of ​​the matrix material per unit time to a reaction area of ​​the matrix material, and comparing the first ratio with a second ratio of an average deposition area of ​​the sample material per unit time to a reaction area of ​​the sample material;

[0060] Step S44: if the first ratio is greater than or equal to the second ratio, the position of the base material is maintained; if the first ratio is less than the second ratio, the sample plate corresponding to the base material is moved to a position where the sample material deposition area is the largest.

[0061] In the above embodiment, by horizontally moving the sample plate in the reaction chamber, the deposition effects of the matrix material and the sample material at different positions can be detected, the optimal deposition position can be determined, and the deposition efficiency per unit area of ​​the matrix material and the sample material can be compared. The position of the matrix material can be adjusted in time to ensure that it is located in the area with the best deposition effect. This automatic adjustment mechanism based on comparison of deposition efficiency effectively avoids the problem of local uneven deposition due to improper positioning, improves the overall consistency of the coating, and further improves the corrosion resistance of the deposited coating.

[0062] See also Figure 4 As shown, the detection of the deposition area includes:

[0063] Step S001, detecting, by reflection spectrum analysis, a second area on the surface of the base material and the sample material where the deposition thickness is greater than a preset thickness;

[0064] Step S002: Determine the difference between the second area and the first area whose deposition thickness is greater than the preset thickness determined by the previous reflection spectrum analysis as the deposition area.

[0065] In the above embodiment, the coating thickness on the surface of the substrate material and the sample material can be accurately measured through reflection spectrum analysis, avoiding errors caused by relying solely on intuitive observation. By comparing the effective deposition area of ​​the current detection with the result of the previous detection, the actual deposition area per unit time can be more accurately determined. Compared with directly measuring the deposition area, this difference method based on thickness change can eliminate interference caused by changes in the substrate / sample surface state, thereby improving detection accuracy and further improving the corrosion resistance of the deposited coating.

[0066] Specifically, the base material and the sample material are 317L austenitic stainless steel.

[0067] Specifically, both the sample material and the matrix material are plates, and the size of the sample material is 1 / 20 of the size of the matrix material.

[0068] Specifically, in step S2, the precursor includes TiCl4 gas, and the reducing gas includes H2.

[0069] Specifically, the preset temperature is 950°C, and the preset temperature range is 900°C to 1000°C.

[0070] Specifically, in step S2, the ratio of the volume of the precursor introduced to the volume of the reducing gas introduced per unit time is 1:3.

[0071] Specifically, in step S2, the introduction rate of the precursor is 50 sccm, and the introduction rate of the reducing gas is 120 sccm.

[0072] In the above embodiment, 317L stainless steel has excellent corrosion resistance and is very suitable for use in marine environments. Using 317L stainless steel as the base material and sample material can ensure that the final deposited coating has excellent performance in corrosion resistance, which helps to give full play to the process advantages of the present invention and further improves the corrosion resistance of the deposited coating.

[0073] So far, the technical solutions of the present invention have been described in conjunction with the preferred embodiments shown in the accompanying drawings. However, it is easy for those skilled in the art to understand that the protection scope of the present invention is obviously not limited to these specific embodiments. Without departing from the principle of the present invention, those skilled in the art can make equivalent changes or substitutions to the relevant technical features, and the technical solutions after these changes or substitutions will fall within the protection scope of the present invention.

[0074] The above are only preferred embodiments of the present invention and are not intended to limit the present invention. For those skilled in the art, the present invention can be modified and varied in various ways. Any modification, equivalent replacement, improvement, etc. made within the spirit and principle of the present invention shall be included in the protection scope of the present invention.

Claims

1. A method for preparing a corrosion-resistant metal material in a seawater environment, characterized in that: include: Step S1, placing the matrix material and the sample material on different sample plates at the same height in the reaction chamber; Step S2, introducing a precursor and a reducing gas into the reaction chamber according to the sizes of the base material and the sample material, and heating the base material to a preset temperature and heating the sample material in a preset heating method; Step S3, detecting the deposition area of ​​the surface of the sample material per unit time by using a reflection spectrum analysis technique, and determining the optimal heating temperature of the base material; Step S4, after heating the base material and the sample material to the optimal heating temperature, controlling the sample plate corresponding to the sample material to move around the sample plate where the base material is located in the reaction chamber to determine the optimal deposition position; Step S5, moving the sample plate corresponding to the base material to the optimal deposition position, so that the base material completes the deposition of the surface coating at the optimal deposition position; Wherein, the preset heating mode satisfies that the surface temperature of the sample material in the preset time period covers a preset temperature range centered on the preset temperature; In step S3, determining the optimal heating temperature includes: Step S31, detecting the deposition area on the surface of the sample material at every unit time within the preset time period; Step S32, determining the temperature corresponding to the detection with the largest deposition area as the optimal heating temperature In step S4, determining the optimal deposition position includes: Step S41, controlling the sample plate where the sample material is located to move horizontally at a plurality of positions in the reaction chamber and to stay at each position for the unit time; Step S42, respectively detecting the deposition area on the surface of the sample material after the sample plate stops at each position; Step S43, determining a first ratio of an average deposition area of ​​the matrix material per unit time to a reaction area of ​​the matrix material, and comparing the first ratio with a second ratio of an average deposition area of ​​the sample material per unit time to a reaction area of ​​the sample material; Step S44, if the first ratio is greater than or equal to the second ratio, the position of the base material is maintained; if the first ratio is less than the second ratio, the sample plate corresponding to the base material is moved to a position where the sample material deposition area is the largest; The detection of the deposition area includes: Step S001, detecting, by reflection spectrum analysis, a second area on the surface of the base material and the sample material where the deposition thickness is greater than a preset thickness; Step S002: Determine the difference between the second area and the first area whose deposition thickness is greater than a preset thickness determined by the previous reflection spectrum analysis as the deposition area.

2. The method for preparing corrosion-resistant metal materials in seawater environment according to claim 1, characterized in that: The matrix material and the sample material are 317L austenitic stainless steel.

3. The method for preparing corrosion-resistant metal materials in seawater environment according to claim 1, characterized in that: The sample material and the base material are both plates, and the size of the sample material is 1 / 20 of the size of the base material.

4. The method for preparing corrosion-resistant metal materials in seawater environment according to claim 1, characterized in that: In the step S2, the precursor includes TiCl4 gas, and the reducing gas includes H2.

5. The method for preparing corrosion-resistant metal materials in seawater environment according to claim 1, characterized in that: The preset temperature is 950°C, and the preset temperature range is 900°C~1000°C.

6. The method for preparing corrosion-resistant metal materials in seawater environment according to claim 1, characterized in that: In the step S2, the ratio of the volume of the precursor introduced per unit time to the volume of the reducing gas introduced per unit time is 1:

3.

7. The method for preparing corrosion-resistant metal materials in seawater environment according to claim 1, characterized in that: In the step S2, the introduction rate of the precursor is 50 sccm, and the introduction rate of the reducing gas is 120 sccm.

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