Method for prefabricating oxide film on surface of metal material

Abstract

The invention discloses a method for prefabricating an oxide film on the surface of a metal material, which relates to the technical field of nuclear power energy, and comprises the following steps: cleaning particle dust on the surface of the metal material; cleaning grease on the surface of the metal material; adding the oxidation film prefabricating liquid to prefabricate the metal material, and forming an oxidation film on the surface of the metal material; the prefabrication liquid comprises depleted zinc acetate, the prefabrication temperature ranges from 250 DEG C to 320 DEG C, and the prefabrication pressure ranges from 14.0 MPa to 16.5 MPa. According to the method, dust particles, grease and the like on the surface of a metal material are removed firstly, then prefabrication liquid is used for prefabrication, depleted zinc acetate is used as the prefabrication liquid, the prefabrication temperature and prefabrication pressure are controlled, and an oxidation film is formed on the surface of the metal material, so that the prefabrication process of the oxidation film is simple, and the production efficiency is improved. And the problem that a traditional oxidation film prefabrication process is poor in prefabrication effect is effectively solved, the good anti-corrosion effect is achieved, the corrosion rate is low, and the protection effect of the oxidation film on equipment is better.

Description

Technical Field

[0001] The invention relates to the technical field of nuclear power energy, and in particular to a method for prefabricating an oxide film on the surface of a metal material. Background Art

[0002] Nuclear power plants have a long construction period and require a large one-time investment. Once built, the cost of equipment maintenance and material changes is very high, so that in many cases it is almost impossible to replace materials and equipment. In this case, it is hoped that the failure of equipment due to corrosion and high radiation during shutdown can be avoided or mitigated by adjusting water chemistry. Seeking effective measures to inhibit the corrosion of primary circuit structural materials during service is currently the focus, hot spot and difficulty of research in the field of primary circuit system material corrosion.

[0003] The prior art also discloses some technologies for forming an oxide film on the metal surface to prevent corrosion. For example, the published patent CN106381460B discloses a method for corrosion prevention of magnesium and its alloys and the application of a MgCO3 layer as an anti-corrosion layer. The CO2 gas is plasmatized to increase its reaction activity, so that it reacts with the loose and porous MgO film generated by natural oxidation of the metal magnesium surface in the air at room temperature to form a MgCO3 protective layer to improve the corrosion resistance of magnesium and its alloys.

[0004] The published patent CN112267089B discloses a method for corrosion protection of aluminum alloys with ultra-fine microstructures. The method utilizes the characteristics of aluminum alloys with uniform and fine microstructures and grain sizes below 100 nm to controllably form a dense oxide film on the surface. By controlling the process conditions of polishing, polishing, and standing, a self-passivating film is formed on the surface of the aluminum alloy, thereby playing an anti-corrosion role.

[0005] The published patent CN116516330A discloses a system and method for passivation treatment of the inner surface of the secondary loop system equipment of a nuclear power plant, the method comprising: step 1: preparing ammonia passivation liquid in ammonia metering box; step 2: restoring the condensate polishing system to full flow treatment; step 3: controlling the hydrazine concentration of the feed water by adding ammonia metering pump; step 4: completing the passivation treatment of the inner surface of the secondary loop system and equipment. The present invention can efficiently and safely perform passivation treatment on the surface of the secondary loop system pipeline and equipment by increasing the hydrazine concentration of the secondary loop, so as to repair the passivation film as soon as possible and achieve the technical effect of reducing the corrosion rate of the equipment.

[0006] In order to effectively reduce the corrosion of the primary circuit structural materials during service, a suitable oxide film prefabrication technology is also required. Before the primary circuit system is officially put into operation, a dense oxide film is formed to effectively inhibit the corrosion of the primary circuit during operation, so as to achieve the purpose of slowing down the corrosion of the primary circuit and reducing the radiation dose field outside the core. However, the metal corrosion protection methods disclosed in the prior art (such as the metal corrosion protection methods disclosed in the three patent documents cited above) all have problems such as complex process flow and poor oxide film formation effect. Summary of the invention

[0007] Based on the problems that the current process flow for preparing anti-corrosion oxide film on metal surface is relatively complicated and the oxide film forming effect is poor, the purpose of the present invention is to provide a method for prefabricating oxide film on the surface of metal material. The prefabrication method is simple to operate. By adding suitable preparatives, the oxide film is prefabricated under specific temperature and pressure conditions, which effectively simplifies the prefabrication steps. A denser oxide film is obtained through a simpler method, so that the oxide film can effectively prevent the metal material from being corroded in the subsequent high temperature and high pressure environment.

[0008] The present invention is achieved through the following technical solutions:

[0009] The present application provides a method for prefabricating an oxide film on the surface of a metal material, comprising the following steps:

[0010] Clean the dust particles on the surface of metal materials;

[0011] Clean grease from the surface of metal materials;

[0012] Adding an oxide film prefabrication liquid to prefabricate the metal material to form an oxide film on the surface of the metal material;

[0013] The prefabrication liquid includes depleted zinc acetate, the prefabrication temperature is 250° C. to 320° C., and the prefabrication pressure is 14.0 MPa to 16.5 MPa.

[0014] The prefabrication temperature may be 250°C, 260°C, 270°C, 280°C, 290°C, 300°C, 310°C, 320°C, or any temperature value within the temperature range.

[0015] Among them, the prefabrication pressure can be 14.0MPa, 14.5MPa, 15.0MPa, 15.5MPa, 16.0MPa, 16.5MPa, and any pressure value in this pressure range.

[0016] In the present invention, depleted zinc acetate is used as a prefabricated liquid and added to the cleaned metal material to form a uniform and dense oxide film on the metal material, which can effectively protect the metal material from corrosion in the subsequent high temperature and high pressure environment.

[0017] The formation mechanism of the oxide film is mainly that the zinc in the depleted zinc acetate diffuses into the oxide lattice and competes with the Co ions for electron holes in the oxidation corrosion layer. Part of the Co undergoes structural reorganization and forms a new metal oxide layer on the surface of the equipment. Zinc can prevent more 58 Co and 60 Co is incorporated into the outer chromite spinel of the eight cores, reducing the potential corrosion rate and thus the radiation dose. Over time, this process makes the oxide film thinner and more stable, thereby effectively slowing down the growth of FWSCC and some cracks. Compared with the traditional oxide film preformulation using hydrazine and other oxide film preformulations, this oxide film is not only more uniform and dense, but also does not affect the metal matrix structure and surface brightness, and has strong corrosion resistance even in high temperature and high pressure environments. Therefore, the prefabrication method of the oxide film on the surface of the metal material of the present invention effectively solves the problem of poor prefabrication effect of the traditional oxide film prefabrication process.

[0018] Furthermore, the concentration of the prefabricated solution is 10 mg / L to 80 mg / L.

[0019] The concentration of the preformed liquid may be 10 mg / L, 20 mg / L, 30 mg / L, 40 mg / L, 50 mg / L, 60 mg / L, 70 mg / L, 80 mg / L, or any other concentration value within the concentration range.

[0020] Furthermore, the prefabrication cycle time is 450 hours to 750 hours.

[0021] The prefabrication cycle time may be 450h, 500h, 550h, 600h, 650h, 750h, or any other time value within the prefabrication cycle time range.

[0022] Furthermore, the metal material includes stainless steel and nickel-based alloy.

[0023] Furthermore, the rinsing liquid used to clean the particle dust on the surface of the metal material is deionized water.

[0024] Furthermore, when cleaning the particulate dust on the surface of the metal material, the rinsing temperature is 25°C to 40°C.

[0025] The rinsing temperature may be 25°C, 30°C, 35°C, 40°C, or any temperature value within the rinsing temperature range.

[0026] Furthermore, when cleaning the particulate dust on the surface of the metal material, the rinsing cycle time is 25 minutes to 50 minutes.

[0027] The rinse cycle time may be 25 min, 30 min, 35 min, 40 min, 45 min, 50 min, or any other time value within the rinse cycle time range.

[0028] Furthermore, the rinse liquid used to clean the grease on the surface of the metal material includes ethanol or ether.

[0029] Furthermore, when cleaning grease on the surface of metal materials, the rinsing temperature is 20°C to 45°C.

[0030] The rinsing temperature may be 20°C, 25°C, 30°C, 35°C, 40°C, 45°C, or any other rinsing temperature within the rinsing temperature range.

[0031] Furthermore, when cleaning grease on the surface of metal materials, the rinsing cycle time is 30 minutes to 60 minutes.

[0032] Among them, the rinse cycle time can be 30min, 35min, 40min, 45min, 50min, 55min, 60min, and any time value within the rinse cycle time range.

[0033] Compared with the prior art, the present invention has the following advantages and beneficial effects:

[0034] (1) The present invention adopts a method of first removing dust particles and grease on the surface of the metal material and then using a prefabrication liquid to prefabricate the metal material, and uses depleted zinc acetate as the prefabrication liquid, controls a certain prefabrication temperature and prefabrication pressure, and forms an oxide film on the surface of the metal material. This not only simplifies the prefabrication process of the oxide film, but also effectively solves the problem of poor prefabrication effect of the traditional oxide film prefabrication process. The oxide film has a good anti-corrosion effect, a low corrosion rate, and a long corrosion resistance time, so that the oxide film has a better protective effect on the equipment.

[0035] (2) The oxide film prefabrication method of the present invention makes the oxide film formed on the surface of the metal material more uniform and dense, which can effectively protect the metal material from corrosion in the subsequent high temperature and high pressure environment.

[0036] (3) Compared with the conventional oxide film preformulation using amine and the like, the oxide film of the present invention is not only more uniform and dense, but also does not affect the metal matrix structure and surface brightness. It also has strong corrosion resistance even under high temperature and high pressure environments, effectively solving the problem of poor prefabrication effect of the conventional oxide film prefabrication process. DETAILED DESCRIPTION

[0037] In order to make the purpose, technical solutions and advantages of the embodiments of the present invention clearer, the technical solutions in the embodiments of the present invention will be clearly and completely described below. Obviously, the described embodiments are only part of the embodiments of the present invention, rather than all the embodiments.

[0038] The "range" disclosed in the present application is defined in the form of a lower limit and an upper limit, and a given range is defined by selecting a lower limit and an upper limit, and the selected lower limit and upper limit define the boundaries of a particular range. The range defined in this way can include or exclude end values, and can be combined arbitrarily, that is, any lower limit can be combined with any upper limit to form a range. If there is no special explanation, the "including" and "comprising" mentioned in the present application represent open-ended or closed-ended. For example, the "including" and "comprising" can represent that other substances not listed can also be included or included, or only listed substances can be included or included.

[0039] Therefore, the following detailed description of the embodiments of the present invention is not intended to limit the scope of the invention claimed for protection, but merely represents selected embodiments of the present invention. Based on the embodiments of the present invention, all other embodiments obtained by ordinary technicians in this field without creative work are within the scope of protection of the present invention.

[0040] Example 1

[0041] This embodiment provides a method for prefabricating an oxide film on the surface of a metal material, which is performed according to the following steps:

[0042] S1. Use 30℃ deionized water to cycle and rinse the dust particles on the surface of the metal material. The cycle time is 30 minutes. After rinsing, the rinsing liquid is discharged normally.

[0043] S2. Use 30°C ethanol to rinse and clean the grease on the surface of the metal material. The cycle time is 30 minutes. After rinsing, the rinsing liquid is discharged normally.

[0044] S3. 304 stainless steel is prefabricated using 300°C and 10ppm depleted zinc acetate. During the prefabrication process, a pressure of 14.5MPa needs to be maintained. The prefabrication time is 450 hours. After the prefabrication is completed, the prefabricated liquid is discharged. At this time, a prefabricated oxide film is formed on the 304 stainless steel.

[0045] Example 2

[0046] This embodiment provides a method for prefabricating an oxide film on the surface of a metal material, which is performed according to the following steps:

[0047] S1. Use 35℃ deionized water to cycle and rinse the dust particles on the surface of the metal material. The cycle time is 30 minutes. After rinsing, the rinsing liquid is discharged normally.

[0048] S2. Use 35°C ethanol to rinse and clean the grease on the surface of the metal material in a cycle. The cycle time is 30 minutes. After rinsing, the rinsing liquid is discharged normally.

[0049] S3. Use 290°C and 50ppm depleted zinc acetate to prefabricate 304 stainless steel. During the prefabrication process, a pressure of 15.0MPa needs to be maintained. The prefabrication time is 500 hours. After the prefabrication is completed, the prefabrication liquid is discharged. At this time, a prefabricated oxide film is formed on the 304 stainless steel.

[0050] Example 3

[0051] This embodiment provides a method for prefabricating an oxide film on the surface of a metal material, which is performed according to the following steps:

[0052] S1. Use 40℃ deionized water to cycle and rinse the dust particles on the surface of the metal material. The cycle time is 30 minutes. After rinsing, the rinsing liquid is discharged normally.

[0053] S2. Use 40°C ethanol to rinse and clean the grease on the surface of the metal material. The cycle time is 30 minutes. After rinsing, the rinsing liquid is discharged normally.

[0054] S3. 304 stainless steel is prefabricated using 310°C and 70ppm depleted zinc acetate. During the prefabrication process, a pressure of 15.5MPa is maintained. The prefabrication time is 550 hours. After the prefabrication is completed, the prefabricated liquid is discharged. At this time, a prefabricated oxide film is formed on the 304 stainless steel.

[0055] Example 4

[0056] This embodiment provides a method for prefabricating an oxide film on the surface of a metal material. The difference from Embodiment 1 is that the prefabrication temperature in this embodiment is 250° C., and the other process conditions are the same as those in Embodiment 1. The method is performed according to the following steps:

[0057] S1. Use 35℃ deionized water to cycle and rinse the dust particles on the surface of the metal material. The cycle time is 30 minutes. After rinsing, the rinsing liquid is discharged normally.

[0058] S2. Use 35°C ethanol to rinse and clean the grease on the surface of the metal material. The cycle time is 30 minutes. After rinsing, the rinsing liquid is discharged normally.

[0059] S3. Use 250°C and 50ppm depleted zinc acetate to prefabricate 304 stainless steel. During the prefabrication process, a pressure of 15.0MPa needs to be maintained. The prefabrication time is 500 hours. After the prefabrication is completed, the prefabrication liquid is discharged. At this time, a prefabricated oxide film is formed on the 304 stainless steel.

[0060] Example 5

[0061] This embodiment provides a method for prefabricating an oxide film on the surface of a metal material. The difference from Embodiment 1 is that the prefabrication temperature in this embodiment is 260° C. The other process conditions are the same as those in Embodiment 1. The method is performed according to the following steps:

[0062] S1. Use 35℃ deionized water to cycle and rinse the dust particles on the surface of the metal material. The cycle time is 30 minutes. After rinsing, the rinsing liquid is discharged normally.

[0063] S2. Use 35°C ethanol to rinse and clean the grease on the surface of the metal material. The cycle time is 30 minutes. After rinsing, the rinsing liquid is discharged normally.

[0064] S3. Use 260°C and 50ppm depleted zinc acetate to prefabricate 304 stainless steel. During the prefabrication process, a pressure of 15.0MPa needs to be maintained. The prefabrication time is 500 hours. After the prefabrication is completed, the prefabrication liquid is discharged. At this time, a prefabricated oxide film is formed on the 304 stainless steel.

[0065] Example 6

[0066] This embodiment provides a method for prefabricating an oxide film on the surface of a metal material. The difference from Embodiment 1 is that the prefabrication pressure in this embodiment is 270° C. The other process conditions are the same as those in Embodiment 1. The method is performed according to the following steps:

[0067] S1. Use 35℃ deionized water to cycle and rinse the dust particles on the surface of the metal material. The cycle time is 30 minutes. After rinsing, the rinsing liquid is discharged normally.

[0068] S2. Use 35°C ethanol to rinse and clean the grease on the surface of the metal material. The cycle time is 30 minutes. After rinsing, the rinsing liquid is discharged normally.

[0069] S3. Use 270°C and 50ppm depleted zinc acetate to prefabricate 304 stainless steel. During the prefabrication process, a pressure of 15.0MPa needs to be maintained. The prefabrication time is 500 hours. After the prefabrication is completed, the prefabrication liquid is discharged. At this time, a prefabricated oxide film is formed on the 304 stainless steel.

[0070] Example 7

[0071] This embodiment provides a method for prefabricating an oxide film on the surface of a metal material. The difference from Embodiment 1 is that the prefabrication temperature in this embodiment is 280° C. The other process conditions are the same as those in Embodiment 1. The method is performed according to the following steps:

[0072] S1. Use 35℃ deionized water to cycle and rinse the dust particles on the surface of the metal material. The cycle time is 30 minutes. After rinsing, the rinsing liquid is discharged normally.

[0073] S2. Use 35°C ethanol to rinse and clean the grease on the surface of the metal material. The cycle time is 30 minutes. After rinsing, the rinsing liquid is discharged normally.

[0074] S3. Use 280°C and 50ppm depleted zinc acetate to prefabricate 304 stainless steel. During the prefabrication process, a pressure of 15.0MPa needs to be maintained. The prefabrication time is 500 hours. After the prefabrication is completed, the prefabrication liquid is discharged. At this time, a prefabricated oxide film is formed on the 304 stainless steel.

[0075] Example 8

[0076] This embodiment provides a method for prefabricating an oxide film on the surface of a metal material. The difference from Embodiment 1 is that the prefabrication pressure in this embodiment is 14.0 MPa, and the other process conditions are the same as those in Embodiment 1. The method is performed according to the following steps:

[0077] S1. Use 35℃ deionized water to cycle and rinse the dust particles on the surface of the metal material. The cycle time is 30 minutes. After rinsing, the rinsing liquid is discharged normally.

[0078] S2. Use 35°C ethanol to rinse and clean the grease on the surface of the metal material. The cycle time is 30 minutes. After rinsing, the rinsing liquid is discharged normally.

[0079] S3. Use 300°C and 50ppm depleted zinc acetate to prefabricate 304 stainless steel. During the prefabrication process, a pressure of 14.0MPa needs to be maintained. The prefabrication time is 500 hours. After the prefabrication is completed, the prefabrication liquid is discharged. At this time, a prefabricated oxide film is formed on the 304 stainless steel.

[0080] Example 9

[0081] This embodiment provides a method for prefabricating an oxide film on the surface of a metal material. The difference from Embodiment 1 is that the prefabrication pressure in this embodiment is 16.0 MPa, and the other process conditions are the same as those in Embodiment 1. The method is performed according to the following steps:

[0082] S1. Use 35℃ deionized water to cycle and rinse the dust particles on the surface of the metal material. The cycle time is 30 minutes. After rinsing, the rinsing liquid is discharged normally.

[0083] S2. Use 35°C ethanol to rinse and clean the grease on the surface of the metal material. The cycle time is 30 minutes. After rinsing, the rinsing liquid is discharged normally.

[0084] S3. Use 300°C and 50ppm depleted zinc acetate to prefabricate 304 stainless steel. During the prefabrication process, a pressure of 16.0MPa needs to be maintained. The prefabrication time is 500 hours. After the prefabrication is completed, the prefabrication liquid is discharged. At this time, a prefabricated oxide film is formed on the 304 stainless steel.

[0085] Example 10

[0086] This embodiment provides a method for prefabricating an oxide film on the surface of a metal material. The difference from Embodiment 1 is that the prefabrication pressure in this embodiment is 16.5 MPa, and the other process conditions are the same as those in Embodiment 1. The method is performed according to the following steps:

[0087] S1. Use 35℃ deionized water to cycle and rinse the dust particles on the surface of the metal material. The cycle time is 30 minutes. After rinsing, the rinsing liquid is discharged normally.

[0088] S2. Use 35°C ethanol to rinse and clean the grease on the surface of the metal material. The cycle time is 30 minutes. After rinsing, the rinsing liquid is discharged normally.

[0089] S3. Use 300°C and 50ppm depleted zinc acetate to prefabricate 304 stainless steel. During the prefabrication process, a pressure of 16.5MPa needs to be maintained. The prefabrication time is 500 hours. After the prefabrication is completed, the prefabrication liquid is discharged. At this time, a prefabricated oxide film is formed on the 304 stainless steel.

[0090] Embodiment 11

[0091] This embodiment provides a method for prefabricating an oxide film on the surface of a metal material. The difference from Embodiment 1 is that the concentration of the prefabricated liquid in this embodiment is 20 ppm, and the other process conditions are the same as those in Embodiment 1. The method is performed according to the following steps:

[0092] S1. Use 30℃ deionized water to cycle and rinse the dust particles on the surface of the metal material. The cycle time is 30 minutes. After rinsing, the rinsing liquid is discharged normally.

[0093] S2. Use 30°C ethanol to rinse and clean the grease on the surface of the metal material. The cycle time is 30 minutes. After rinsing, the rinsing liquid is discharged normally.

[0094] S3. 304 stainless steel is prefabricated using 300°C and 20ppm depleted zinc acetate. During the prefabrication process, a pressure of 14.5MPa needs to be maintained. The prefabrication time is 450 hours. After the prefabrication is completed, the prefabricated liquid is discharged. At this time, a prefabricated oxide film is formed on the 304 stainless steel.

[0095] Example 12

[0096] This embodiment provides a method for prefabricating an oxide film on the surface of a metal material. The difference from Embodiment 1 is that the concentration of the prefabricated liquid in this embodiment is 30 ppm, and the other process conditions are the same as those in Embodiment 1. The method is performed according to the following steps:

[0097] S1. Use 30℃ deionized water to cycle and rinse the dust particles on the surface of the metal material. The cycle time is 30 minutes. After rinsing, the rinsing liquid is discharged normally.

[0098] S2. Use 30°C ethanol to rinse and clean the grease on the surface of the metal material. The cycle time is 30 minutes. After rinsing, the rinsing liquid is discharged normally.

[0099] S3. 304 stainless steel is prefabricated using 300°C and 30ppm depleted zinc acetate. During the prefabrication process, a pressure of 14.5MPa needs to be maintained. The prefabrication time is 450 hours. After the prefabrication is completed, the prefabricated liquid is discharged. At this time, a prefabricated oxide film is formed on the 304 stainless steel.

[0100] Example 13

[0101] This embodiment provides a method for prefabricating an oxide film on the surface of a metal material. The difference from Embodiment 1 is that the concentration of the prefabricated liquid in this embodiment is 40 ppm, and the other process conditions are the same as those in Embodiment 1. The method is performed according to the following steps:

[0102] S1. Use 30℃ deionized water to cycle and rinse the dust particles on the surface of the metal material. The cycle time is 30 minutes. After rinsing, the rinsing liquid is discharged normally.

[0103] S2. Use 30°C ethanol to rinse and clean the grease on the surface of the metal material. The cycle time is 30 minutes. After rinsing, the rinsing liquid is discharged normally.

[0104] S3. Use 300°C and 40ppm depleted zinc acetate to prefabricate 304 stainless steel. During the prefabrication process, a pressure of 14.5MPa needs to be maintained. The prefabrication time is 450 hours. After the prefabrication is completed, the prefabrication liquid is discharged. At this time, a prefabricated oxide film is formed on the 304 stainless steel.

[0105] Embodiment 14

[0106] This embodiment provides a method for prefabricating an oxide film on the surface of a metal material. The difference from Embodiment 1 is that the concentration of the prefabricated liquid in this embodiment is 60 ppm, and the other process conditions are the same as those in Embodiment 1. The method is performed according to the following steps:

[0107] S1. Use 30℃ deionized water to cycle and rinse the dust particles on the surface of the metal material. The cycle time is 30 minutes. After rinsing, the rinsing liquid is discharged normally.

[0108] S2. Use 30°C ethanol to rinse and clean the grease on the surface of the metal material. The cycle time is 30 minutes. After rinsing, the rinsing liquid is discharged normally.

[0109] S3. Use 300°C and 60ppm depleted zinc acetate to prefabricate 304 stainless steel. During the prefabrication process, a pressure of 14.5MPa needs to be maintained. The prefabrication time is 450 hours. After the prefabrication is completed, the prefabrication liquid is discharged. At this time, a prefabricated oxide film is formed on the 304 stainless steel.

[0110] Embodiment 15

[0111] This embodiment provides a method for prefabricating an oxide film on the surface of a metal material. The difference from Embodiment 1 is that the concentration of the prefabricated liquid in this embodiment is 80 ppm, and the other process conditions are the same as those in Embodiment 1. The method is performed according to the following steps:

[0112] S1. Use 30℃ deionized water to cycle and rinse the dust particles on the surface of the metal material. The cycle time is 30 minutes. After rinsing, the rinsing liquid is discharged normally.

[0113] S2. Use 30°C ethanol to rinse and clean the grease on the surface of the metal material. The cycle time is 30 minutes. After rinsing, the rinsing liquid is discharged normally.

[0114] S3. 304 stainless steel is prefabricated using 300°C and 80ppm depleted zinc acetate. During the prefabrication process, a pressure of 14.5MPa needs to be maintained. The prefabrication time is 450 hours. After the prefabrication is completed, the prefabricated liquid is discharged. At this time, a prefabricated oxide film is formed on the 304 stainless steel.

[0115] Example 16

[0116] This embodiment provides a method for prefabricating an oxide film on the surface of a metal material. The difference from Embodiment 1 is that the metal material in this embodiment is a nickel-based alloy, and the other process conditions are the same as those in Embodiment 1. The method is performed according to the following steps:

[0117] S1. Use 30℃ deionized water to cycle and rinse the dust particles on the surface of the metal material. The cycle time is 30 minutes. After rinsing, the rinsing liquid is discharged normally.

[0118] S2. Use 30°C ethanol to rinse and clean the grease on the surface of the metal material. The cycle time is 30 minutes. After rinsing, the rinsing liquid is discharged normally.

[0119] S3. The nickel-based alloy is prefabricated using 300°C and 10ppm depleted zinc acetate. During the prefabrication process, a pressure of 14.5MPa needs to be maintained. The prefabrication time is 450 hours. After the prefabrication is completed, the prefabricated liquid is discharged. At this time, a prefabricated oxide film is formed on the nickel-based alloy.

[0120] Comparative Example 1

[0121] This comparative example provides a method for prefabricating an oxide film on the surface of a metal material. The difference from Example 1 is that the prefabrication temperature in this comparative example is 230° C., and the other process conditions are the same as those in Example 1. The method is carried out according to the following steps:

[0122] S1. Use 35℃ deionized water to cycle and rinse the dust particles on the surface of the metal material. The cycle time is 30 minutes. After rinsing, the rinsing liquid is discharged normally.

[0123] S2. Use 35°C ethanol to rinse and clean the grease on the surface of the metal material. The cycle time is 30 minutes. After rinsing, the rinsing liquid is discharged normally.

[0124] S3. Use 230°C and 50ppm depleted zinc acetate to prefabricate 304 stainless steel. During the prefabrication process, a pressure of 15.0MPa needs to be maintained. The prefabrication time is 500 hours. After the prefabrication is completed, the prefabrication liquid is discharged. At this time, a prefabricated oxide film is formed on the 304 stainless steel.

[0125] Comparative Example 2

[0126] This comparative example provides a method for prefabricating an oxide film on the surface of a metal material. The difference from Example 1 is that the prefabrication temperature in this comparative example is 330° C., and the other process conditions are the same as those in Example 1. The method is carried out according to the following steps:

[0127] S1. Use 35℃ deionized water to cycle and rinse the dust particles on the surface of the metal material. The cycle time is 30 minutes. After rinsing, the rinsing liquid is discharged normally.

[0128] S2. Use 35°C ethanol to rinse and clean the grease on the surface of the metal material. The cycle time is 30 minutes. After rinsing, the rinsing liquid is discharged normally.

[0129] S3. 304 stainless steel is prefabricated using 330°C and 50ppm depleted zinc acetate. During the prefabrication process, a pressure of 15.0MPa is maintained. The prefabrication time is 500 hours. After the prefabrication is completed, the prefabricated liquid is discharged. At this time, a prefabricated oxide film is formed on the 304 stainless steel.

[0130] Comparative Example 3

[0131] This comparative example provides a method for prefabricating an oxide film on the surface of a metal material. The difference from Example 1 is that the prefabrication pressure in this comparative example is 13.0 MPa, and the other process conditions are the same as those in Example 1. The method is carried out according to the following steps:

[0132] S1. Use 35℃ deionized water to cycle and rinse the dust particles on the surface of the metal material. The cycle time is 30 minutes. After rinsing, the rinsing liquid is discharged normally.

[0133] S2. Use 35°C ethanol to rinse and clean the grease on the surface of the metal material. The cycle time is 30 minutes. After rinsing, the rinsing liquid is discharged normally.

[0134] S3. Use 300°C and 50ppm depleted zinc acetate to prefabricate 304 stainless steel. During the prefabrication process, a pressure of 13.0MPa needs to be maintained. The prefabrication time is 500 hours. After the prefabrication is completed, the prefabrication liquid is discharged. At this time, a prefabricated oxide film is formed on the 304 stainless steel.

[0135] Comparative Example 4

[0136] This comparative example provides a method for prefabricating an oxide film on the surface of a metal material. The difference from Example 1 is that the prefabrication pressure in this comparative example is 17.0 MPa, and the other process conditions are the same as those in Example 1. The method is carried out according to the following steps:

[0137] S1. Use 35℃ deionized water to cycle and rinse the dust particles on the surface of the metal material. The cycle time is 30 minutes. After rinsing, the rinsing liquid is discharged normally.

[0138] S2. Use 35°C ethanol to rinse and clean the grease on the surface of the metal material. The cycle time is 30 minutes. After rinsing, the rinsing liquid is discharged normally.

[0139] S3. Use 300°C and 50ppm depleted zinc acetate to prefabricate 304 stainless steel. During the prefabrication process, a pressure of 17.0MPa needs to be maintained. The prefabrication time is 500 hours. After the prefabrication is completed, the prefabrication liquid is discharged. At this time, a prefabricated oxide film is formed on the 304 stainless steel.

[0140] Comparative Example 5

[0141] This comparative example provides a method for prefabricating an oxide film on the surface of a metal material. The difference from Example 1 is that the concentration of the prefabricated liquid in this comparative example is 8 ppm, and the other process conditions are the same as those in Example 1. The method is carried out according to the following steps:

[0142] S1. Use 35℃ deionized water to cycle and rinse the dust particles on the surface of the metal material. The cycle time is 30 minutes. After rinsing, the rinsing liquid is discharged normally.

[0143] S2. Use 35°C ethanol to rinse and clean the grease on the surface of the metal material. The cycle time is 30 minutes. After rinsing, the rinsing liquid is discharged normally.

[0144] S3. Use 300°C and 8ppm depleted zinc acetate to prefabricate 304 stainless steel. During the prefabrication process, a pressure of 14.5MPa needs to be maintained. The prefabrication time is 500 hours. After the prefabrication is completed, the prefabrication liquid is discharged. At this time, a prefabricated oxide film is formed on the 304 stainless steel.

[0145] Comparative Example 6

[0146] This comparative example provides a method for prefabricating an oxide film on the surface of a metal material. The difference from Example 1 is that the concentration of the prefabricated liquid in this comparative example is 85 ppm, and the other process conditions are the same as those in Example 1. The steps are as follows:

[0147] S1. Use 35℃ deionized water to cycle and rinse the dust particles on the surface of the metal material. The cycle time is 30 minutes. After rinsing, the rinsing liquid is discharged normally.

[0148] S2. Use 35°C ethanol to rinse and clean the grease on the surface of the metal material. The cycle time is 30 minutes. After rinsing, the rinsing liquid is discharged normally.

[0149] S3. Use 300°C and 85ppm depleted zinc acetate to prefabricate 304 stainless steel. During the prefabrication process, a pressure of 14.5MPa needs to be maintained. The prefabrication time is 500 hours. After the prefabrication is completed, the prefabrication liquid is discharged. At this time, a prefabricated oxide film is formed on the 304 stainless steel.

[0150] Comparative Example 7

[0151] This comparative example adopts the method disclosed in the prior art (patent CN116516330A) to form a passivation film on the surface of 304 stainless steel. The specific method is:

[0152] Step 1: Prepare hydrazine passivation solution in the hydrazine metering box;

[0153] Step 2: Restore the condensate polishing system to full flow processing;

[0154] Step 3: Control the hydrazine concentration of the feed water to 10ppm by adding a hydrazine metering pump;

[0155] Step 4: Use the hydrazine solution to prefabricate 304 stainless steel. During the prefabrication process, a pressure of 14.5 MPa needs to be maintained. The prefabrication time is 450 hours. After the prefabrication is completed, the prefabrication liquid is discharged. At this time, a prefabricated oxide film is formed on the 304 stainless steel.

[0156] The corrosion resistance of the oxide film prefabricated on the surface of the metal material using the prefabrication methods of Examples 1 to 16 and Comparative Examples 1 to 7 was tested by the uniform corrosion full immersion test method (JB / T7901-2001), and the test results are shown in Table 1 below.

[0157] Table 1 Corrosion resistance test data of oxide film prefabricated by different methods

[0158]

[0159]

[0160] It can be seen from the test data in the table that after 96 hours of testing by the uniform corrosion full immersion test method (JB / T7901-2001), the corrosion resistance of the oxide film prefabricated by the method of the embodiment of the present invention is significantly higher than that of the oxide film prefabricated by the method in the comparative example. Moreover, by comparison, it is found that the concentration of the prefabricated liquid, the temperature during prefabrication and the pressure during prefabrication will affect the corrosion resistance of the oxide film, and the corrosion resistance of the oxide film prefabricated by the prefabricated liquid concentration, the temperature during prefabrication and the pressure during prefabrication defined in the present invention is higher than that of the comparative example, proving that the oxide film prefabricated on the surface by the prefabrication method of the present application has a better corrosion resistance effect, and the prefabrication process is simple, which effectively solves the problem of poor prefabrication effect of the traditional oxide film prefabrication process, so that the oxide film has a better protective effect on the equipment. At the same time, the oxide film prepared by the prefabrication method of the present application is not only more uniform and dense than the traditional oxide film prefabrication using hydrazine and other oxide film prefabricants, but also does not affect the metal matrix structure and surface brightness, and has strong corrosion resistance even in high temperature and high pressure environments.

[0161] The above description shows and describes the preferred embodiments of the present invention. As mentioned above, it should be understood that the present invention is not limited to the form disclosed herein, and should not be regarded as excluding other embodiments, but can be used in various other combinations, modifications and environments, and can be modified within the scope of the invention concept described herein through the above teachings or the technology or knowledge of the relevant field. The changes and modifications made by those skilled in the art do not depart from the spirit and scope of the present invention, and should be within the scope of protection of the claims attached to the present invention.

Claims

1. A method for prefabricating an oxide film on the surface of a metal material, characterized in that: The following steps are involved: Clean the dust particles on the surface of metal materials; Clean grease from the surface of metal materials; Adding an oxide film prefabrication liquid to prefabricate the metal material to form an oxide film on the surface of the metal material; The prefabrication liquid includes depleted zinc acetate, the prefabrication temperature is 250° C. to 320° C., and the prefabrication pressure is 14.0 MPa to 16.5 MPa.

2. The method for prefabricating an oxide film on the surface of a metal material according to claim 1, characterized in that: The concentration of the prefabricated solution is 10 mg / L to 80 mg / L.

3. The method for prefabricating an oxide film on the surface of a metal material according to claim 1, characterized in that: The prefabrication cycle time is 450h~750h.

4. The method for prefabricating an oxide film on the surface of a metal material according to claim 1, characterized in that: The metal material includes stainless steel and nickel-based alloy.

5. The method for prefabricating an oxide film on the surface of a metal material according to claim 1, characterized in that: The rinsing liquid used to clean the particulate dust on the surface of metal materials is deionized water.

6. The method for prefabricating an oxide film on the surface of a metal material according to claim 5, characterized in that: When cleaning particulate dust on the surface of metal materials, the rinsing temperature is 25℃~40℃.

7. A method for prefabricating an oxide film on the surface of a metal material according to claim 5 or 6, characterized in that: When cleaning particulate dust on the surface of metal materials, the rinsing cycle time is 25 minutes to 50 minutes.

8. The method for prefabricating an oxide film on the surface of a metal material according to claim 1, characterized in that: Rinsing fluids used to clean grease from metal surfaces include ethanol or ether.

9. The method for prefabricating an oxide film on the surface of a metal material according to claim 8, characterized in that: When cleaning grease on the surface of metal materials, the rinsing temperature is 20℃~45℃.

10. A method for prefabricating an oxide film on the surface of a metal material according to claim 8 or 9, characterized in that: When cleaning grease on the surface of metal materials, the rinsing cycle time is 30 minutes to 60 minutes.

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