Method for calculating corrosion weight gain of metal materials after ion irradiation

Abstract

The application discloses a kind of metal material corrosion weight gain calculation method after ion irradiation, comprising the following steps: metal material is prepared into sample, and the geometric parameter of sample is measured;Part of sample is carried out single surface ion irradiation, and the sample needing to be corroded is weighed;Unirradiated sample and irradiated sample after ion irradiation are carried out corrosion test, and sample is taken out and weighed after corrosion test ends;According to the weight gain and surface area of unirradiated sample, the corrosion weight gain under unit area is calculated;According to the weight gain of irradiated sample and the corrosion weight gain of unirradiated sample under corresponding corrosion time per unit area, the corrosion weight gain per unit area of irradiated surface under corresponding corrosion time is calculated.The calculation method of the application, by designing the corrosion experiment of ion irradiation metal material sample to calculate the corrosion weight gain of irradiated surface, can more effectively characterize the influence of irradiation effect on high temperature and high pressure corrosion of metal material, and provide theoretical method basis.

Description

TECHNICAL FIELD

[0001] The application belongs to the field of metal material oxidation corrosion detection, and particularly relates to a calculation method of corrosion weight gain of metal material caused by irradiation after ion irradiation. BACKGROUND

[0002] Safe and efficient development of nuclear power is the energy strategy of our country, and the service safety of nuclear power key materials is the core element of long-term safe and efficient operation. Nuclear power key component materials such as reactor pressure vessels, fuel cladding and in-core components are subjected to high temperature, high pressure, corrosion, irradiation and other adverse factors during service, which comprehensively leads to the decline of material performance and the damage of structural integrity, affects the service life of the corresponding materials, and increases the safety hidden danger of nuclear power. Among them, the corrosion performance research of nuclear power materials is an important part of the aging failure evaluation of nuclear power key components, such as the corrosion of fuel cladding in the primary loop environment, and the irradiation effect of neutron irradiation causes the change of material microstructure, thereby affecting the corrosion process and mechanism of the material. In order to simulate the actual working environment, the corrosion mechanism research of nuclear power key materials under irradiation conditions needs further in-depth research.

[0003] Due to the radioactivity of neutron irradiated samples, it brings many inconveniences to the research of material performance, and ion irradiation is relatively inexpensive and efficient. At present, ion irradiation is used to simulate the damage effect caused by neutron irradiation at home and abroad. On the one hand, ion irradiation experiments are often designed only on one side of the sample, and the surface of the sample is required to be high. At present, the corresponding fixture of the terminal of the main domestic irradiation platform is fixed by pasting the sample. If double-sided irradiation is carried out, the sample after irradiation needs to be turned over, pasted again and irradiated again, which will cause the irradiation surface to be contaminated due to pasting, affecting the micro corrosion behavior, and all surfaces of the sample will produce corrosion weight gain during the corrosion process. Direct measurement of the weight gain of the single-side irradiated sample cannot quantitatively characterize the corrosion weight gain of the irradiation surface. On the other hand, the existing characterization of high temperature and high pressure corrosion weight gain of metal materials after ion irradiation is mainly qualitative comparison of the difference of corrosion performance before and after irradiation, and the corrosion weight gain of the irradiation surface cannot be obtained. SUMMARY

[0004] Therefore, in order to overcome the defects of the prior art, the purpose of the present application is to provide a calculation method of corrosion weight gain of metal material caused by irradiation after ion irradiation.

[0005] In order to achieve the above purpose, the technical scheme adopted by the present application is as follows:

[0006] A calculation method of corrosion weight gain of metal material after ion irradiation, comprising the following steps:

[0007] Preparation of metal material into a sample, and measurement of the geometric parameters of the sample;

[0008] Part of the samples are ion-irradiated on one side, and the samples which need to be tested for corrosion are weighed;

[0009] The un-irradiated samples and the irradiated samples are tested for corrosion, and after the corrosion test is finished, the samples are taken out and weighed;

[0010] The corrosion weight gain per unit area of the un-irradiated sample is calculated according to the weight gain and the surface area of the un-irradiated sample;

[0011] The corrosion weight gain per unit area of the irradiated surface of the irradiated sample at the corresponding corrosion time is calculated according to the weight gain of the irradiated sample and the corrosion weight gain per unit area of the un-irradiated sample at the corresponding corrosion time.

[0012] According to some preferred embodiments of the present application, the corrosion weight gain per unit area of the un-irradiated sample is calculated by the following formula:

[0013]

[0014] In the formula, W 0,unirr. is the weight of the un-irradiated sample before corrosion, W t,unirr. is the weight of the un-irradiated sample after corrosion, S 抛光面,unirr. is the surface area of the un-irradiated sample.

[0015] According to some preferred embodiments of the present application, the surface area S 抛光面,unirr. of the un-irradiated sample is calculated by the following formula:

[0016] S 抛光面,unirr. = 2·a unirr. ·b unirr. + 2(a unirr. +b unirr. )·h unirr.

[0017] In the formula, a unirr. is the length of the un-irradiated sample, b unirr. is the width of the un-irradiated sample, and h unirr. is the thickness of the un-irradiated sample.

[0018] According to some preferred embodiments of the present application, the corrosion weight gain per unit area of the irradiated surface of the irradiated sample at the corresponding corrosion time is calculated by the following formula:

[0019]

[0020] In the formula, W 0,irr. is the weight of the irradiated sample before corrosion, W t,irr. is the weight of the irradiated sample after corrosion, S 抛光面,irr. is the surface area of the irradiated sample after removing the irradiated surface, and X t抛光面S represents the corrosion weight gain per unit area of ​​the unirradiated sample at the corresponding corrosion time. 辐照面,irr. This represents the irradiated surface area of ​​the irradiated sample.

[0021] According to some preferred embodiments of the invention, the unirradiated surface area S on the irradiated sample 抛光面,irr. It is calculated using the following formula:

[0022] S 抛光面,irr. =a irr. ·b irr. +2(a irr. +b irr. )·h irr.

[0023] In the formula, a irr. b is the length of the irradiated sample. irr. h is the width of the irradiated sample. irr. The thickness of the irradiated sample.

[0024] According to some preferred embodiments of the invention, the irradiated surface area S on the irradiated sample 辐照面,irr. It is calculated using the following formula:

[0025] S 辐照面,irr. =a irr. ·b irr.

[0026] According to some preferred embodiments of the present invention, when preparing a sample, the metal material is cut into a cuboid sheet, and a through hole is made in the cuboid sheet that extends through its thickness direction, and then the cuboid sheet is surface treated.

[0027] According to some preferred embodiments of the present invention, the length and width of the cuboid sheet are both greater than or equal to 10 mm, and the thickness is less than or equal to 1.5 mm.

[0028] According to some preferred embodiments of the invention, the inner diameter of the through hole is less than or equal to 1 mm.

[0029] According to some preferred embodiments of the present invention, the surface treatment is one or more of grinding, cleaning, and polishing on the surface of the cuboid sheet.

[0030] Due to the adoption of the above technical solutions, the advantages of this invention compared with the prior art are as follows: The method for calculating the corrosion weight gain of metal materials after ion irradiation of this invention calculates the corrosion weight gain of the irradiated surface by designing corrosion experiments of ion-irradiated metal material samples; it overcomes the problem that it is difficult to accurately measure the corrosion weight gain caused by irradiation in high-temperature corrosion experiments of metal samples irradiated on one side in traditional methods, and can more effectively characterize the influence of irradiation on the high-temperature and high-pressure corrosion of metal materials, and provides a theoretical and methodological basis. Attached Figure Description

[0031] To more clearly illustrate the technical solutions in the embodiments of the present invention, the accompanying drawings used in the description of the embodiments will be briefly introduced below. Obviously, the accompanying drawings described below are only some embodiments of the present invention. For those skilled in the art, other drawings can be obtained based on these drawings without creative effort.

[0032] Figure 1 This is a schematic diagram of the geometric parameters of the sample prepared in a preferred embodiment of the present invention;

[0033] Figure 2 This is a corrosion weight gain curve of a zirconium alloy sample before and after irradiation in an embodiment of the present invention. Detailed Implementation

[0034] To enable those skilled in the art to better understand the technical solutions of the present invention, the technical solutions of the embodiments of the present invention will be clearly and completely described below with reference to the accompanying drawings. Obviously, the described embodiments are only some embodiments of the present invention, and not all embodiments. Based on the embodiments of the present invention, all other embodiments obtained by those skilled in the art without creative effort should fall within the scope of protection of the present invention.

[0035] This invention provides a method for calculating the corrosion weight gain of metallic materials after ion irradiation, comprising the following steps:

[0036] Step 1) Sample preparation

[0037] The initial metal material is wire-cut into a thin sheet with a rectangular geometric shape, with a length of A, a width of B, and a thickness of H, wherein the length A and the width B are both not less than 10 mm, and the thickness H is not greater than 1.5 mm.

[0038] For samples of rectangular thin plates, 10% of the sum of the front and back surface areas must be greater than the surface area of ​​the four sides, i.e., 10% × 2A × B > 2(A + B) × H.

[0039] A through-hole, penetrating the thickness of the sample, is made to facilitate suspension during corrosion experiments. The inner diameter of the through-hole is no greater than 1 mm, and the weight gain due to corrosion on the hole wall surface can be neglected in the calculation.

[0040] Step 2) Sample processing

[0041] The surfaces of the samples, including the front and back surfaces and the four side surfaces, are polished with 400-mesh, 800-mesh and 1200-mesh sandpaper in sequence, and each sandpaper is polished until the scratches are uniform and cover the polishing traces of the previous sandpaper. Then, according to different materials, the surfaces are cleaned or pickled to remove the surface oxide film, and the cleaned samples are polished and the geometric parameters a, b and h of the samples after surface treatment are measured, as shown in Figure 1 .

[0042] Step 3), obtaining the irradiated sample and the non-irradiated sample and obtaining the initial weight

[0043] One of the polished surfaces is selected for ion irradiation with a corresponding dose to obtain a single-side irradiated sample under a specific condition. The irradiated sample and the non-irradiated sample after irradiation are weighed to obtain the initial weight before corrosion, which are denoted as W 0,irr. and W 0,unirr. , respectively.

[0044] Step 4), performing a corrosion experiment and obtaining the weight after corrosion

[0045] The non-irradiated sample and the irradiated sample after ion irradiation are placed in the same autoclave for oxidation corrosion experiment. The corrosion conditions can be different according to different experimental designs. After a corresponding time t of corrosion, the samples are taken out and dried, and then weighed. The weight of the non-irradiated sample after corrosion is denoted as W t,unirr , and the weight of the irradiated sample after corrosion is denoted as W t,irr. .

[0046] Step 5), calculating the corrosion weight gain per unit area of the non-irradiated polished surface

[0047] The corrosion weight gain ΔW t,unirr. of the non-irradiated sample is calculated as follows:

[0048] ΔW t,unirr. = W t,nuirr. -W 0,unirr. = X t抛光面 · S 抛光面,unirr.

[0049] In the formula, X t抛光面 is the corrosion weight gain per unit area of the polished surface of the non-irradiated sample under the corrosion time t, and S 抛光面,unirr. is the area of the polished surface of the non-irradiated sample, which is calculated by the following formula:

[0050] S 抛光面,unirr. = 2·a unirr. ·b unirr. + 2(a unirr. +b unirr. )·h unirr.

[0051] The corrosion weight gain per unit area X on the polished surface of the unirradiated sample at corrosion time t is calculated t抛光面 may be expressed as

[0052]

[0053] Step 6), the corrosion weight gain per unit area of the irradiated surface of the irradiated sample at the corresponding corrosion time is calculated

[0054] For the single-side irradiated sample, the unit area corrosion increment caused by the polished but unirradiated surface of the sample on the four sides is approximately equal to X of the unirradiated sample t抛光面 Therefore, the corrosion weight gain X caused by irradiation in the single-side irradiated sample is t辐照面 may be expressed by the following calculation formula, and thus the law of the difference in corrosion weight gain between the irradiated and unirradiated conditions of the sample is obtained.

[0055] ΔW t,irr. = ΔW 辐照 + ΔW 未辐照

[0056] S 辐照面,irr. = a irr. · b irr.

[0057] S 抛光面,irr. = a irr. · b irr. + 2(a irr. + b irr. )· h irr.

[0058] ΔW t,irr. = X t辐照面 · S 辐照面,irr. + X t抛光面 · S 抛光面,irr.

[0059]

[0060] In the above formula, unirr. means unirradiated, and irr. means irradiated.

[0061] Implementation case:

[0062] In this embodiment, a zirconium alloy (Zr-1 Nb) is subjected to corrosion for 3, 7 and 14 days under the conditions of high temperature and high pressure water in a simulated reactor primary loop environment at 360℃ and 18.6 MPa after ion irradiation, and then irradiation oxidation weight gain characterization measurement is performed, the steps are as follows:

[0063] 1) The initial zirconium alloy sample was wire-cut to a thin sheet with a geometry of about 15x15x0.7mm, a surface area satisfying 10% x 2 x 15 x 15 > 2(15+15) x 0.7, and a through hole with a diameter of 0.8mm was punched at a position above the surface of the sample to facilitate corrosion suspension of the grid.

[0064] 2) The surface of the sample was polished with 400 mesh, 800 mesh, and 1200 mesh sandpaper in sequence, and each sandpaper polishing was unified in the direction of scratches and covered the polishing marks of the previous sandpaper. Since the material is a zirconium niobium alloy, the surface was pickled with mixed acid according to the YS / T1308-2019 standard, and the pickled sample was electrochemically polished. After polishing, the geometric parameters a, b, h of the sample were measured, and the data are shown in Table 1.

[0065] 3) One of the polished surfaces was selected for single-sided ion irradiation with a corresponding dose (Xe ion irradiation to 0.2dpa). The irradiated sample and the unirradiated sample were weighed to obtain the initial weight before high-pressure autoclave corrosion, denoted as W0, and the data are shown in Table 1.

[0066] 4) The unirradiated zirconium alloy sample and the ion-irradiated zirconium alloy sample were placed in the same high-pressure autoclave for oxidation corrosion experiment. The corrosion conditions were 360°C, 18.6MPa, and 0.01mol / L LiOH solution. After corrosion for a corresponding time t (t=3, 7, 14), the sample was taken out, dried, and weighed, denoted as W t , and the data are shown in Table 1.

[0067] Table 1 Size parameters and weighing data of corrosion samples

[0068]

[0069] 5) For the unirradiated sample, the corrosion weight gain X on the polished surface of the unirradiated sample at time t was calculated using the following formula t抛光面 , and the actual data are shown in Table 2.

[0070] ΔW t,unirr. = W t,unirr. - W 0,unirr. = X t抛光面 · S 抛光面,unirr.

[0071] S 抛光面 = 2a unirr. b unirr. + 2(a unirr. + b unirr. )h unirr.

[0072]

[0073] 6) For single-sided irradiated samples, the side surface around the sample is approximated to the increase in corrosion per unit area caused by the polished but unirradiated surface of the sample X t抛光面 and the increase in weight due to irradiation in the single-sided irradiated sample is calculated using the following formula X t辐照面 .

[0074] ΔW t,irr. = ΔW 辐照 + ΔW 未辐照

[0075] S 辐照面,irr. = a irr. · b irr.

[0076] S 抛光面,irr. = a irr. · b irr. + 2(a irr. + b irr. )· h irr.

[0077] ΔW t,irr. = X t辐照面 · S 辐照面,irr. + X t抛光面 · S 抛光面,irr.

[0078]

[0079] The specific calculation data are shown in Table 2, and the corrosion weight gain curves before and after irradiation are shown in Figure 2 , thereby obtaining the difference in corrosion weight gain of Zr-1 Nb material after unirradiation and ion irradiation for 3, 7, and 14 days under high temperature and high pressure corrosion.

[0080] Table 2 Corrosion weight gain of the corrosion sample

[0081]

[0082] The present application provides a method for calculating the corrosion weight gain of the irradiated surface of a sheet-shaped metal material after single-sided ion irradiation by designing a corrosion experiment of an ion irradiated metal material sample. The method overcomes the problem that it is difficult to accurately measure the corrosion weight gain caused by irradiation in a high temperature corrosion experiment of a conventional single-sided ion irradiated metal sample. Based on the method, the influence of irradiation on the corrosion performance of some metal materials can be further studied, the corrosion weight gain data can be more effectively measured, the influence of irradiation effects on high temperature and high pressure corrosion of metal materials can be more effectively characterized, and theoretical method basis is provided.

[0083] The above examples are only for illustrating the technical concept and characteristics of the present application, and the purpose is to enable those skilled in the art to understand the content of the present application and to implement it, and cannot limit the protection scope of the present application. Any equivalent changes or modifications made according to the spirit and essence of the present application shall be covered within the protection scope of the present application.

Claims

1. A method for calculating the corrosion weight gain of metallic materials after ion irradiation, characterized in that, Includes the following steps: The metallic material is prepared into a sample, and the geometric parameters of the sample are measured; Some samples were subjected to single-sided ion irradiation, and the samples that needed to be subjected to corrosion tests were weighed. Corrosion tests were conducted on unirradiated samples and irradiated samples after ion irradiation. After the corrosion tests were completed, the samples were removed and weighed. The corrosion weight gain per unit area is calculated based on the weight gain and surface area of ​​the unirradiated sample; Based on the weight gain of the irradiated sample and the corrosion weight gain per unit area of ​​the unirradiated sample at the corresponding corrosion time, the corrosion weight gain per unit area of ​​the irradiated surface of the irradiated sample at the corresponding corrosion time is calculated. The corrosion weight gain per unit area of ​​the irradiated surface of the irradiated sample at the corresponding corrosion time (X) t辐照面 The following formula is used to calculate: In the formula, W 0,irr. W is the weight of the irradiated sample before corrosion. t,irr. S is the weight of the irradiated sample after corrosion. 抛光面,irr. X represents the surface area of ​​the irradiated sample after removing the irradiated surface. t抛光面 S represents the corrosion weight gain per unit area of ​​the unirradiated sample at the corresponding corrosion time. 辐照面,irr. This represents the irradiated surface area of ​​the irradiated sample.

2. The calculation method according to claim 1, characterized in that, The corrosion weight gain per unit area of ​​the unirradiated sample was calculated using the following formula: In the formula, W 0,unirr. W represents the weight of the unirradiated sample before corrosion. t,unirr. S represents the weight of the unirradiated sample after corrosion. 抛光面,unirr. This represents the surface area of ​​the unirradiated sample.

3. The calculation method according to claim 1, characterized in that, Surface area S of the unirradiated sample 抛光面,unirr. It is calculated using the following formula: S 抛光面,unirr. =2·a unirr. ·b unirr. +2(a unirr. +b unirr. )·h unirr. In the formula, a unirr. b is the length of the unirradiated sample. unirr. h represents the width of the unirradiated sample. unirr. The thickness of the unirradiated sample.

4. The calculation method according to claim 1, characterized in that, The unirradiated surface area S on the irradiated sample 抛光面,irr. It is calculated using the following formula: S 抛光面,irr. =a irr. ·b irr. +2(a irr. +b irr. )·h irr. In the formula, a irr. b is the length of the irradiated sample. irr. h is the width of the irradiated sample. irr. The thickness of the irradiated sample.

5. The calculation method according to claim 1, characterized in that, The irradiated surface area S on the irradiated sample 辐照面,irr. It is calculated using the following formula: S 辐照面,irr. =a irr. ·b irr.

6. The calculation method according to claim 1, characterized in that... When preparing the sample, the metal material is cut into a cuboid sheet and a through hole is made in the cuboid sheet to penetrate its thickness direction. Then the cuboid sheet is surface treated.

7. The calculation method according to claim 6, characterized in that, The length and width of the cuboid sheet are both greater than or equal to 10 mm, and the thickness is less than or equal to 1.5 mm.

8. The calculation method according to claim 6, characterized in that, The inner diameter of the through hole is less than or equal to 1 mm.

9. The calculation method according to claim 6, characterized in that, The surface treatment is one or more of the following: grinding, cleaning, and polishing of the surface of the rectangular thin sheet.

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