CN111945171A - Tellurium corrosion protection method of alloy and effect verification test method thereof - Google Patents

Tellurium corrosion protection method of alloy and effect verification test method thereof Download PDF

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CN111945171A
CN111945171A CN202010858854.9A CN202010858854A CN111945171A CN 111945171 A CN111945171 A CN 111945171A CN 202010858854 A CN202010858854 A CN 202010858854A CN 111945171 A CN111945171 A CN 111945171A
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CN111945171B (en
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蒋力
李志军
王凯
黎超文
梁建平
叶祥熙
玉昆
陈双建
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Shanghai Institute of Applied Physics of CAS
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    • C—CHEMISTRY; METALLURGY
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Abstract

The invention discloses a tellurium corrosion protection method of an alloy, which is characterized in that an active material which is easier to react with tellurium than the alloy is introduced into a tellurium-containing corrosion environment in which the alloy is positioned to serve as an adsorbent, and the adsorbent preferentially adsorbs tellurium and reacts with the tellurium, so that the activity of tellurium in the tellurium-containing corrosion environment is reduced, and the purpose of tellurium corrosion protection of the alloy is achieved. The invention also discloses an effect verification test method of the tellurium corrosion protection method. Compared with the prior art, the method can solve the problem of tellurium corrosion of the alloy component with low cost and high efficiency under the condition of not influencing the existing design of tellurium-containing corrosion environments such as a molten salt pile and the like.

Description

Tellurium corrosion protection method of alloy and effect verification test method thereof
Technical Field
The invention relates to a tellurium corrosion protection method of an alloy.
Background
The fission product tellurium element is formed in the service process of the molten salt reactor. The tellurium elements enter a nickel-based high-temperature alloy (mainly Hastelloy N alloy, GH3535 alloy and other high-temperature molten salt corrosion resistant alloys) component through crystal-following diffusion at high temperature, so that the crystal-following cracking of the surface is caused, and the service safety of a reactor is seriously threatened.
Tellurium corrosion in a reactor is mainly embodied in two aspects of surface telluride and segregation of tellurium elements in grain boundaries, wherein the latter is mainly embodied in the hazard of tellurium corrosion. After the tellurium element is subjected to segregation to the grain boundary, the bonding force of the grain boundary is weakened, so that the grain boundary is easy to crack. The diffusion depth and the segregation concentration of the tellurium element along the surface of the alloy determine the degree of the tellurium corrosion hazard. Therefore, the root of the inhibition of alloy tellurium corrosion is to prevent the diffusion of tellurium along the surface grain boundaries.
In the early days, in order to solve this problem, researchers tried means such as increasing the content of chromium element in the alloy or the formulation of fuel salt, and although the problem of tellurium corrosion could be improved, there were also obvious disadvantages. In the molten salt reactor, the alloy structural material is required to resist not only tellurium corrosion but also molten salt corrosion. When the content of the chromium element is increased, the tellurium corrosion resistance can be improved, but the molten salt corrosion resistance is deteriorated. Therefore, the requirements of two corrosion resistance properties cannot be simultaneously satisfied by adjusting the content of chromium element. On the other hand, the problem of tellurium corrosion can also be improved by increasing the proportion of trivalent uranium elements and tetravalent uranium elements in the fuel salt and adjusting the redox potential of the fuel salt, but the adjustment can increase the cost of the fuel salt and change the original mature physical design.
Recently, in order to solve this problem, researchers have proposed protective Ni — Nb coatings, alloy deformation treatments, and the like, which can significantly improve the problems of tellurium corrosion and tellurium brittleness of the alloy, but still have the problem of high cost.
Disclosure of Invention
The technical problem to be solved by the invention is to overcome the defects of the prior art, and provide a tellurium corrosion protection method for an alloy, which can be used for solving the problem of tellurium corrosion of an alloy member at low cost and high efficiency under the condition of not influencing the existing design of tellurium-containing corrosion environments such as a molten salt pile and the like.
The invention specifically adopts the following technical scheme to solve the technical problems:
the tellurium corrosion protection method of the alloy is characterized in that an active material which is easier to react with tellurium than the alloy is introduced into a tellurium-containing corrosion environment where the alloy is located to serve as an adsorbent, and the adsorbent preferentially adsorbs tellurium and reacts with the tellurium, so that the activity of tellurium in the tellurium-containing corrosion environment is reduced, and the purpose of tellurium corrosion protection of the alloy is achieved.
Preferably, the alloy is a high temperature molten salt corrosion resistant alloy.
Preferably, the tellurium-containing corrosive environment is a tellurium vapor environment or a tellurium-containing molten salt environment.
Preferably, the active materials more reactive with tellurium are: the mean gibbs free energy for forming the telluride is less than the elemental or alloy material of the alloy forming the telluride.
Preferably, the active material is disposed in the tellurium-containing corrosive environment in a form of a large specific surface area.
Further preferably, the morphology with large specific surface area is a net shape, a thread shape or a porous foam shape.
Preferably, the active material is disposed in the tellurium-containing corrosive environment without contacting the alloy, or the active material is non-isolatedly coated on the surface of the alloy contacting the tellurium-containing corrosive environment.
Further, the surface passivation film of the active material is removed prior to introducing the active material into the tellurium-containing corrosive environment.
Preferably, the active material is pure Ni or a Ni-4Cr alloy.
Based on the same inventive concept, the following technical scheme can be obtained:
in the effect verification test method of the tellurium corrosion protection method according to any one of the above aspects, the alloy and the active material are respectively processed into equal-sized sheet-shaped tensile samples, and are simultaneously placed in a tellurium-containing corrosion environment for tellurium corrosion and then subjected to tensile deformation test, the degree of tellurium corrosion is judged from the number and depth of cracks, and the effect of the tellurium corrosion protection method is judged by comparing the tensile deformation test crack condition of the alloy sheet-shaped tensile sample which is separately placed in the tellurium-containing corrosion environment for tellurium corrosion.
Compared with the prior art, the technical scheme of the invention has the following beneficial effects:
the invention firstly proposes that an active material which is easier to react with tellurium than the alloy is introduced into a tellurium-containing corrosion environment in which the alloy is positioned as an adsorbent, and the adsorbent preferentially adsorbs tellurium and reacts with the tellurium, so that the activity of tellurium in the tellurium-containing corrosion environment is reduced, and the purpose of tellurium corrosion protection of the alloy is achieved; the invention can solve the problem of tellurium corrosion of the alloy component with low cost and high efficiency under the condition of not influencing the existing design of tellurium-containing corrosion environments such as a molten salt reactor and the like.
Drawings
FIG. 1 is a schematic diagram of the corrosion protection verification scheme of the adsorbent in tellurium vapor environment in examples 1 and 2 of the present invention;
FIG. 2 is a surface crack condition of GH3535 alloy with adsorbent pure Ni and GH3535 alloy protected by it under tellurium vapor corrosion in example 1 of the present invention;
FIG. 3 shows surface cracking of GH3535 alloy with pure Ni-4Cr as an adsorbent and GH3535 alloy protected by it under tellurium vapor corrosion in example 2 of the present invention;
FIG. 4 is a schematic diagram of the corrosion protection verification scheme of the adsorbent under the tellurium-containing molten salt environment in example 3 of the present invention;
FIG. 5 shows the GH3535 alloy tube of example 3 of the invention containing molten salt, molten salt + Cr3Te4Powder and molten salt + Cr3Te4Cracking of the inner wall of the tube under three conditions of powder and pure Ni net.
Detailed Description
Aiming at the defects of the existing alloy tellurium corrosion resistance technology, the invention adopts an adsorbent mode to carry out tellurium corrosion protection on the alloy, namely, an active material which is easier to react with tellurium than the alloy is introduced into a tellurium-containing corrosion environment where the alloy is positioned as an adsorbent, and the adsorbent preferentially adsorbs tellurium and reacts with the tellurium, so that the activity of tellurium in the tellurium-containing corrosion environment is reduced, and the aim of tellurium corrosion protection of the alloy is fulfilled. The principle of the technical scheme of the invention is different from the prior technical route of changing the physicochemical characteristics of the alloy or the molten salt to improve the tellurium corrosion resistance and the technical route of completely isolating the alloy from the tellurium corrosion environment to block the tellurium corrosion.
In the technical scheme of the invention, the selection of the adsorbent directly determines the effect of tellurium corrosion protection, and in order to accurately and quickly select the active material as the adsorbent, the average Gibbs free energy is preferably adopted as a selection index, namely, a simple substance element or an alloy material is selected, wherein the average Gibbs free energy of the formed telluride is smaller than the average Gibbs free energy of the alloy formed telluride.
Specifically, calculating Gibbs free energy of a corresponding telluride formed by a simple substance element, and calculating average Gibbs free energy of the telluride formed by the alloy according to the proportion of the simple substance element in the alloy; then, the metal of a specific simple substance element or the alloy material of the simple substance element combination is selected as an adsorbent, so that the converted average Gibbs free energy is more negative than that of the alloy material to be protected (namely, the value of the average Gibbs free energy is smaller).
For adsorbent materials lacking gibbs free energy data, the following test method for validation of effects can be used for the judgment and selection.
In the effect verification test method of the tellurium corrosion protection method according to any one of the above aspects, the alloy and the active material are respectively processed into equal-sized sheet-shaped tensile samples, and are simultaneously placed in a tellurium-containing corrosion environment for tellurium corrosion and then subjected to tensile deformation test, the degree of tellurium corrosion is judged from the number and depth of cracks, and the effect of the tellurium corrosion protection method is judged by comparing the tensile deformation test crack condition of the alloy sheet-shaped tensile sample which is separately placed in the tellurium-containing corrosion environment for tellurium corrosion.
In order to exert the tellurium corrosion protection effect to the maximum extent, the adsorbent material with large specific surface area forms such as net shape, silk shape, porous foam shape and the like is preferably adopted; before the adsorbent material is introduced into a tellurium-containing corrosion environment, a surface passivation film formed in the preparation process or placed for a long time is removed by adopting methods such as grinding, acid washing and the like, so that the adsorbent material can fully play the roles of reaction and adsorption.
When the adsorbent is used for tellurium corrosion protection of the alloy, the adsorbent can be placed in a position (for example, a position which is above the liquid level of molten salt in a molten salt reactor and does not interfere the basic function of the reactor) which is not contacted with the protected alloy in a tellurium-containing corrosion environment in a large-specific-surface-area form, and tellurium steam in a covering atmosphere is adsorbed and reacted; or the alloy is coated on the surface of the alloy contacting with the tellurium-containing corrosive environment in a non-isolated way (for example, the surface of an alloy part above or below the liquid level of the molten salt in the molten salt pile is coated by a reticular, filiform or porous foam adsorbent material), and the tellurium in the atmosphere or the molten salt is adsorbed and reacted; of course, various other possible arrangements may be used.
To facilitate understanding of the public, the technical solutions of the present invention are further described in detail below by means of several specific embodiments in conjunction with the attached drawings:
example 1: and (3) verifying that pure Ni is used as an effective adsorbent in a tellurium steam corrosion environment.
Because pure Ni has good molten salt corrosion resistance, the pure Ni is selected as the adsorbent and can be directly applied below the molten salt liquid level without worrying about the molten salt corrosion problem. This example first demonstrated the effectiveness of pure Ni as an adsorbent in a tellurium vapor corrosion environment, with the target of protection being GH3535 alloy (typical compositions: 6% -8% Cr, 15% -17% Mo, < 5% Fe, < 1% Si, < 0.8% Mn, < 0.08% C, < 0.2% Co, < 0.35% Cu, < 0.5% W, < 0.35% Al + Ti, and the balance Ni and unavoidable impurity elements).
The Gibbs free energy of formation of telluride from the main elemental composition of the GH3535 alloy and the elements disclosed (Ni: -58.95, Mo: -27.82, Cr: -61.58, Fe: -26.01, units kJ/mol), expressed as the average Gibbs free energy, is-54.28 kJ/mol, greater than the corresponding value of pure nickel-58.95 kJ/mol. Therefore, pure Ni can be used as the adsorbent.
In order to verify the effective adsorption of pure Ni, pure Ni and GH3535 alloy are processed into equal-size sheet-shaped tensile samples, subjected to tellurium steam corrosion and then subjected to tensile deformation, and the tellurium corrosion degree is judged according to the number and depth of cracks. As shown in fig. 1, the main experimental details are as follows: (1) selecting a high-purity low-hydroxyl quartz tube (one end of which is closed) with the length of 35 cm, the inner diameter of 2 cm and the thickness of 2mm as a packaging material; (2) tensile samples of GH3535 alloy and pure Ni were placed near the open end of the quartz tube and the tellurium block was placed near the closed end. (3) Inserting a quartz column into one end of the opening of the quartz tube, sealing by flame ignition, and removing air to 10 deg.C by a molecular pump during sealing-4 Pa; (4) placing the sealed quartz tube in a heat treatment furnace with double temperature ends, wherein the tellurium block is at 300 ℃, the alloy material is at 700 ℃, and the heat treatment is carried out for 250 hours; (5) and taking out the sample to check the tellurium corrosion state, breaking the sample by adopting a tensile test, and observing and judging the degree of surface cracking caused by tellurium corrosion by adopting an optical microscope. For comparison, the above procedure was performed on a sample of GH3535 alloy alone.
As shown in fig. 2, the surface of the singly corroded GH3535 alloy had significant cracks, demonstrating that it was severely corroded by tellurium. The GH3535 alloy introduced with pure Ni as an adsorbent almost observes any surface crack, and proves that the GH3535 alloy is protected by adsorption, and the obvious crack on the surface of the pure Ni of the adsorbent proves that the GH3535 alloy plays an adsorption role.
Example 2: and (3) verification that the Ni-4Cr alloy is used as an effective adsorbent in a tellurium steam corrosion environment.
In this example, the effectiveness of a Ni-4Cr binary alloy (Cr content of 4 wt.%) as an adsorbent in a tellurium vapor etching environment was verified, and the protected target was GH3535 alloy (typical compositions: 6% -8% Cr, 15% -17% Mo, < 5% Fe, < 1% Si, < 0.8% Mn, < 0.08% C, < 0.2% Co, < 0.35% Cu, < 0.5% W, < 0.35% Al + Ti, and the balance Ni and unavoidable impurity elements).
The Gibbs free energy of formation of telluride from the main elemental composition of GH3535 alloy and the elements disclosed (Ni: -58.95, Mo: -27.82, Cr: -61.58, Fe: -26.01, units kJ/mol), expressed as the average Gibbs free energy, is-54.28 kJ/mol, with a corresponding value of-59.07 kJ/mol for the Ni-4Cr binary alloy. Therefore, pure Ni-4Cr can be used as the adsorbent.
In order to verify the effective adsorbability of the Ni-4Cr binary alloy, the Ni-4Cr binary alloy and the GH3535 alloy are processed into equal-size sheet-shaped tensile samples, and then tensile deformation is carried out after tellurium steam corrosion, and the tellurium corrosion degree is judged according to the number and depth of cracks. As shown in fig. 1, the main experimental details are as follows: (1) selecting a high-purity low-hydroxyl quartz tube (one end of which is closed) with the length of 35 cm, the inner diameter of 2 cm and the thickness of 2mm as a packaging material; (2) tensile samples of GH3535 alloy and Ni-4Cr binary alloy were placed near the open end of the quartz tube, and a tellurium block was placed near the closed end. (3) Inserting a quartz column into one end of the opening of the quartz tube, sealing by flame ignition, and removing air to 10 deg.C by a molecular pump during sealing-4Pa; (4) placing the sealed quartz tube in a heat treatment furnace with double temperature ends, wherein the tellurium block is at 300 ℃, the alloy material is at 700 ℃, and the heat treatment is carried out for 250 hours; (5) and taking out the sample to check the tellurium corrosion state, breaking the sample by adopting a tensile test, and observing and judging the degree of surface cracking caused by tellurium corrosion by adopting an optical microscope. For comparison, the above procedure was performed on a sample of GH3535 alloy alone.
As shown in fig. 3, the surface of the singly corroded GH3535 alloy had significant cracks, demonstrating that it was severely corroded by tellurium. The GH3535 alloy introduced with the Ni-4Cr binary alloy as the adsorbent almost observes any surface crack, proves that the GH3535 alloy is protected by adsorption, and simultaneously, the obvious crack on the surface of the adsorbent Ni-4Cr binary alloy proves that the GH3535 alloy plays an adsorption role.
Example 3: and (3) verifying that pure Ni is used as an effective adsorbent in a tellurium-containing molten salt corrosion environment.
Because pure Ni has good molten salt corrosion resistance, the pure Ni is selected as the adsorbent and can be directly applied below the molten salt liquid level without worrying about the molten salt corrosion problem. In the example, the effectiveness of pure Ni as an adsorbent in a tellurium-containing molten salt corrosion environment is verified, and the protected objects are GH3535 alloy (typical components are 6-8% of Cr, 15-17% of Mo, less than or equal to 5% of Fe, less than or equal to 1% of Si, less than or equal to 0.8% of Mn, less than or equal to 0.08% of C, less than or equal to 0.2% of Co, less than or equal to 0.35% of Cu, less than or equal to 0.5% of W, less than or equal to 0.35% of Al + Ti, and the balance of Ni and inevitable impurity elements).
The Gibbs free energy of formation of telluride from the main elemental composition of the GH3535 alloy and the elements disclosed (Ni: -58.95, Mo: -27.82, Cr: -61.58, Fe: -26.01, units kJ/mol), expressed as the average Gibbs free energy, is-54.28 kJ/mol, greater than the corresponding value of pure nickel-58.95 kJ/mol. Therefore, pure Ni can be used as the adsorbent.
In order to facilitate the effectiveness of pure Ni as an adsorbent in a tellurium-containing molten salt corrosion environment, in this embodiment, a GH3535 alloy to be protected is prepared into a tubular shape, the adsorbent pure Ni is designed into a mesh shape and is attached to the inner wall of a GH3535 tube for adsorption protection, and a corrosion medium is added with Cr for adsorption protection3Te4Powdered FliNaK molten salt. And cutting a part of the GH3535 alloy pipe, which is in contact with the tellurium-containing molten salt, into an annular sample, and observing the condition of cracks after performing a tensile test to evaluate the degree of tellurium corrosion. As shown in fig. 4, the main experimental details are as follows: (1) selecting a GH3535 alloy pipe as an experimental container, wherein the outer diameter of the experimental container is 13.72mm, the thickness of the experimental container is 1.65mm, the length of the experimental container is 15cm, and a 150-mesh high-purity Ni net is attached to the inner wall of the pipe; (2) 10mg of FLiNaK fused salt and a proper amount of tellurium source Cr3Te4Fully mixing the powder, filling the powder into a tube, and welding and sealing two ends in a vacuum glove box by adopting homogeneous GH3535 alloy original sheets; (3) placing the sealed GH3535 alloy pipe at 700 ℃ and preserving heat for 1000 hours; (4) and after the heat preservation is finished, cooling the GH3535 alloy pipe, taking out the molten salt, cutting the position of the lower end of the pipe completely soaked in the molten salt to form an annular sample, stretching, and observing and judging the degree of surface cracking caused by tellurium corrosion by using an optical microscope. For comparison, two control experiments were designed, namely (1) adding molten salt without Cr3Te4Powder and (2) molten salt and Cr3Te4Powder but without a pure nickel mesh as adsorbent.
As shown in figure 5 of the drawings,when only molten salt exists in the GH3535 alloy pipe, the ring cut from the pipe has no surface crack after tensile fracture; when GH3535 alloy pipe contains molten salt and Cr3Te4During powder forming, the ring cut from the tube has significant surface cracks after tensile fracture, which proves the occurrence of tellurium corrosion; when GH3535 alloy pipe contains molten salt and Cr3Te4When the powder has the adsorption protection of the pure nickel net, the ring piece cut from the pipe has no surface crack after tensile fracture, and the pure nickel net is proved to play the adsorption protection role.

Claims (10)

1. The tellurium corrosion protection method of the alloy is characterized in that an active material which is easier to react with tellurium than the alloy is introduced into a tellurium-containing corrosion environment in which the alloy is positioned to serve as an adsorbent, and the adsorbent preferentially adsorbs and reacts with tellurium, so that the activity of tellurium in the tellurium-containing corrosion environment is reduced, and the purpose of tellurium corrosion protection of the alloy is achieved.
2. A method of tellurium corrosion protection of the alloy of claim 1, wherein said alloy is a high temperature molten salt corrosion resistant alloy.
3. A method of tellurium corrosion protection of the alloy of claim 1, wherein said tellurium-containing corrosion environment is a tellurium vapor environment or a tellurium-containing molten salt environment.
4. A method for tellurium corrosion protection of an alloy as claimed in claim 1, wherein said active materials more reactive with tellurium are: the mean gibbs free energy for forming the telluride is less than the elemental or alloy material of the alloy forming the telluride.
5. A method for tellurium corrosion protection of an alloy as claimed in claim 1, wherein said active material is disposed in said tellurium-containing corrosive environment in a high surface area configuration.
6. A method of tellurium corrosion protection of an alloy as claimed in claim 5, wherein said high specific surface area morphology is reticulated, filamentous or porous foam.
7. A method for tellurium corrosion protection of an alloy as claimed in claim 1, wherein said active material is disposed in said tellurium-containing corrosive environment without contacting said alloy, or wherein said active material is non-isolatedly coated on a surface of said alloy contacting said tellurium-containing corrosive environment.
8. A method for tellurium corrosion protection of an alloy as claimed in claim 1, wherein the surface passivation film of said active material is removed prior to introducing said active material into a tellurium containing corrosion environment.
9. A method for tellurium corrosion protection of an alloy as claimed in claim 1, wherein said active material is pure Ni or a Ni-4Cr alloy.
10. The method for testing the effectiveness of the tellurium corrosion prevention method according to any one of claims 1 to 9, wherein the alloy and the active material are processed into sheet-like elongated samples having the same size, and the sheet-like elongated samples are subjected to tellurium corrosion in a tellurium-containing corrosion environment and then subjected to a tensile deformation test, and the degree of tellurium corrosion is determined from the number and depth of cracks, and the effectiveness of the tellurium corrosion prevention method is determined by comparing the tensile deformation test crack condition with that of an alloy sheet-like elongated sample subjected to tellurium corrosion in a tellurium-containing corrosion environment alone.
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