A neutron-diffraction-peak-free high-thermal-conductivity vni alloy plate and a manufacturing method thereof

Abstract

The present application relates to the technical field of neutron scattering experiment, in particular to a kind of neutron scattering experiment with no neutron diffraction peak, high-thermal-conductivity VNi alloy plate and its manufacturing method;The plate is composed of vanadium (V) and nickel (Ni), wherein the mass percentage of vanadium is 40% to 60%, and the mass percentage of nickel is 40% to 60%, the alloy plate has no neutron diffraction peak, and the theoretical thermal conductivity at room temperature is not less than 27 W / (m*K);And it has good processing plasticity, meets the requirements of neutron scattering experiment on sample container and neutron beam window, and the demand of efficient high-low temperature in-situ experiment;The VNi plate prepared by the present application has uniform composition, no neutron diffraction peak, meets the demand of neutron scattering experiment, and has excellent thermal conductivity;The VNi plate prepared by the method has uniform composition, no neutron diffraction peak, and good tensile forming plasticity, which meets the further processing and preparation demand of finished product.

Description

TECHNICAL FIELD

[0001] The present application relates to the technical field of neutron scattering experiments, and particularly relates to a neutron scattering experiment sample container and neutron beam window material without neutron diffraction peak and a high-thermal-conductivity VNi alloy plate and a manufacturing method thereof. BACKGROUND

[0002] In a neutron scattering experiment, the selection of a sample container and a neutron beam window material has an important influence on the quality of experimental data; at present, commonly used vanadium and TiZr alloy are used as sample containers, and V or Al is used as a neutron beam window material, but these materials have certain problems; vanadium and aluminum have neutron diffraction peaks, which will seriously interfere with the sample signal and affect the acquisition of neutron diffraction data; and although the TiZr alloy does not have a neutron diffraction peak, it has poor processing plasticity, high manufacturing cost, and poor thermal conductivity, which limits the efficiency of neutron testing experiments under high and low temperature sample environments.

[0003] The existing TiZr alloy manufacturing process has the problems of low production efficiency and high cost, and because the alloy has poor thermal conductivity, the sample temperature rising and falling speed is slow under high and low temperature sample environments, which greatly limits the application of neutron testing experiments in high and low temperature environments; at present, the composition of the VNi alloy used in neutron scattering experiments has been determined, but the composition control precision of the smelting method is still a challenge, which makes it difficult to apply large-scale processing; in addition, the VNi alloy has strong oxygen affinity, which makes the traditional hot rolling process unsuitable for the processing and preparation of the alloy plate; at the same time, because the plasticity of the VNi alloy is low, the existing cold rolling preparation process is also not suitable for this new alloy. SUMMARY

[0004] In order to solve the above problems, it is urgent to develop a new alloy and a corresponding manufacturing process to meet the high requirements of neutron scattering experiments on sample containers and neutron beam windows and to improve the efficiency of neutron testing experiments under high and low temperature environments; the present application is proposed based on this demand.

[0005] The technical scheme adopted by the present application is: a high-thermal-conductivity VNi alloy plate without neutron diffraction peak, which is composed of vanadium (V) and nickel (Ni), wherein the mass percentage of vanadium is 40% to 60%, and the mass percentage of nickel is 40% to 60%; the alloy plate has no neutron diffraction peak, and the theoretical thermal conductivity at room temperature is not less than 150 W / m·K. ; and has good processing plasticity, which meets the requirements of neutron scattering experiments on sample containers and neutron beam windows and the demand for efficient high and low temperature in-situ experiments.

[0006] The plate is obtained after homogenization treatment and hot working, which ensures that the alloy has uniform internal composition and no obvious composition segregation.

[0007] The shape of the plate includes but is not limited to flat plate, round plate, square plate, and the thickness of the plate can be adjusted as needed.

[0008] A manufacturing method of a high-thermal-conductivity VNi alloy plate without neutron diffraction peaks, mainly comprising the following steps:

[0009] (1) Alloy raw material preparation: first, high-purity vanadium (V) and nickel (Ni) raw materials are prepared;

[0010] (2) Melting process: the prepared vanadium and nickel are matched according to the predetermined mass percentage, and are put into a vacuum arc melting furnace or a vacuum induction furnace for melting. After melting, an alloy billet is formed;

[0011] (3) Homogenization treatment: the alloy billet in (2) is subjected to homogenization treatment to ensure uniform distribution of alloy components;

[0012] (4) Hot working: the alloy billet after homogenization treatment is subjected to hot working, including forging, rolling and other methods, to obtain an alloy plate with desired shape and size. During the hot working process, multiple annealing-rolling cycle treatments may be required to obtain the desired plate thickness and mechanical properties.

[0013] (5) Quality detection: finally, the alloy plate is subjected to quality detection, including composition analysis, thermal conductivity test, processing plasticity evaluation and neutron diffraction peak detection, to ensure that the plate meets the requirements of neutron scattering experiments.

[0014] In step (1), the ratio of alloy raw materials is determined according to the required mass percentage of vanadium and nickel, so that the purity of the raw materials reaches a certain standard, wherein the purity of vanadium is better than 99.9%, and the purity of nickel is better than 99.99%, to ensure the quality of the final alloy.

[0015] In step (2), the vacuum degree needs to be controlled during the melting process. The vacuum degree is controlled to be better than 10-3 Pa during the melting process to ensure the purity of the alloy and avoid impurities entering the alloy.

[0016] Step (3) is carried out in a high-temperature furnace, wherein the homogenization treatment temperature is controlled between 800°C and 1100°C, and the treatment time is not less than 24 hours.

[0017] A high-thermal-conductivity VNi alloy plate without neutron diffraction peaks, used for manufacturing a sample container for neutron scattering experiments or a neutron beam window.

[0018] ​The VNi plate prepared by the application has uniform composition, no neutron diffraction peak, meets the demand of neutron scattering experiment, and has excellent thermal conductivity; the VNi plate prepared by the method has uniform composition, no neutron diffraction peak, and good tensile forming plasticity, and meets the further processing and preparation demand of finished products, which specifically embodies as follows: (1) excellent physical properties: through accurate proportioning and unique processing technology, the alloy plate exhibits excellent physical properties. High-purity raw materials ensure the purity of the alloy, thereby improving the overall mechanical properties and stability; (2) excellent high thermal conductivity: the alloy plate prepared by the technical scheme has excellent thermal conductivity. This property makes it have significant advantages in application scenarios that require efficient heat conduction, such as heat dissipation devices and heat exchangers; (3) no neutron diffraction peak: the technical scheme successfully eliminates the neutron diffraction peak, which means that the plate will not produce interference signals during neutron scattering experiments, thereby ensuring the accuracy and reliability of the experiments; (4) wide application prospect: the alloy plate is not only suitable for neutron scattering experiments, but also can play an important role in high-end fields such as aerospace, nuclear industry and chemical industry. Its excellent high-temperature resistance and corrosion resistance make it an ideal material for working in extreme environments; (5) high quality standard: through strict quality detection process, including component analysis and thermal conductivity test, it is ensured that each alloy plate reaches a very high quality standard. This provides reliable product guarantee for users and reduces the risk of use.

[0019] In summary, the technical scheme successfully prepares an alloy plate with excellent physical properties, high thermal conductivity and no neutron diffraction peak through unique processing technology and high-quality raw materials, providing strong material support for the application of multiple fields. BRIEF DESCRIPTION OF DRAWINGS

[0020] Figure 1 is a preparation method process flowchart of the application.

[0021] Figure 2 is a VNi alloy neutron diffraction spectrum in the application.

[0022] Figure 3 is a VNi alloy plate neutron diffraction spectrum in the application.

[0023] Figure 4 is the mechanical properties of the VNi alloy 0.2mm plate in the application. DETAILED DESCRIPTION

[0024] The specific embodiments of the application are described in detail below in conjunction with the accompanying drawings of the specification:

[0025] As Figure 1As shown, the present application provides a neutron scattering experiment with no neutron diffraction peak, high thermal conductivity VNi alloy plate and its manufacturing method, including precise alloy composition control. Through optimization of melting, alloying and cooling solidification, rolling and other steps, high precision, high efficiency, low cost and high quality alloy plate processing and manufacturing are realized, as follows:

[0026] Stage one: melting stage (vacuum suspension melting): the block element V with purity better than 99.9% and the purity of the elemental Ni better than 99.99% are configured according to the alloy ratio, and the raw materials are cleaned by 10% HCl solution to remove the surface oxide layer. Vacuum arc melting is adopted, the current is 300A during the melting process, the refining time is 7 minutes, the power is slowly reduced to the minimum, and the furnace is discharged after cooling for 1 hour. The vacuum degree during the melting process is better than Above, 200g of alloy ingot is obtained.

[0027] Stage two: the multiple small ingots of stage one are melted together for 4 times, the first melting power is 275KW, the second melting power is 280KW, the power is reduced to 230KW, the third melting power is 260KW, and the power is reduced to 220KW with slight spatter, the refining time of each melting is 7 minutes, and the cooling time is 1 hour, to prepare kilogram-level alloy ingot with uniform composition.

[0028] Stage three, homogenization treatment, the alloy ingot is placed in a high temperature furnace at 800-1100℃ for more than 24h for homogenization treatment.

[0029] Stage four, the rod after homogenization is forged at 700-1200℃ to obtain rod or plate of ideal size.

[0030] Stage five, the prepared block is vacuum annealed at 700-1000℃ (vacuum better than 10-3 Pa) for more than 1 hour, and then cold-rolled by two-roller rolling mill with deformation not higher than 20%, and the annealing-rolling cycle treatment is repeated until the plate of ideal thickness is obtained.

[0031] The present application adopts distributed melting to ensure that the composition deviation of the entire alloy is less than 0.1wt% in different parts of the alloy ingot, realizing high-precision preparation of alloy ingot composition control; secondly, since VNi has poor oxidation resistance and low tensile deformation capacity, the present application adopts vacuum annealing process in the cold rolling gap, and realizes the processing and preparation of VNi alloy sheet through optimization of process parameters, and the thinnest can be 50 microns.

[0032] Example one: to ensure uniform alloy composition, distributed melting method is adopted

[0033] Step one: Fine melting: The purity of more than 99.9% of bulk elemental V and the purity of more than 99.99% of elemental Ni are configured according to the alloy ratio. The raw materials are cleaned with 10% HCl solution to remove the surface oxide layer. Vacuum arc melting is adopted, the current is 300A during the melting process, the refining time is 7 minutes, the power is slowly reduced to the minimum, and the furnace is discharged after cooling for 1 hour. The vacuum degree during the melting process is better than Above, 200g of alloy ingot is obtained.

[0034] Step two: mixed melting: several small ingots of stage one are melted together for 4 times, the first melting power is 275KW, the second melting power is 280KW, and the power is reduced to 230KW, the third melting power is 260KW, and the power is reduced to 220KW with slight spatter. The refining time of each melting is 7 minutes, and the cooling time is 1 hour. The kilogram-level alloy ingot with uniform composition is prepared.

[0035] Step three, homogenization treatment, the alloy ingot is placed in a high-temperature furnace at 800-1100°C for more than 24 hours for homogenization treatment.

[0036] Step four, the homogenized rod is forged at 700-1200°C to obtain a rod or plate of desired size.

[0037] Step five, the prepared block is vacuum annealed at 700-1000°C (vacuum better than 10-3 Pa) for more than 1 hour. This step is the key to plate rolling.

[0038] Step six, then use two-roller rolling machine for cold rolling treatment, the deformation is not higher than 20%, repeat the annealing-rolling cycle treatment until the plate of desired thickness.

[0039] Example two: preparation of VNi alloy plate

[0040] Step one: alloy raw material preparation: select vanadium raw material with purity of 99.99% and nickel raw material with purity of 99.999%, accurately weigh according to the mass percentage of vanadium 60% and nickel 40%.

[0041] Step two: melting process: put the weighed vanadium and nickel raw materials into the vacuum arc melting furnace, control the vacuum degree in the furnace to reach 6.67x10^-4 Pa, and start the arc melting. Keep the current stable during the melting process to ensure uniform mixing of the alloy components.

[0042] Step three: homogenization treatment: put the melted alloy ingot into a high-temperature furnace for homogenization treatment, the treatment temperature is 1000°C, and the treatment time is 48 hours to ensure uniform internal organization of the alloy and eliminate internal stress.

[0043] Step Four: Hot Working: After homogenization treatment, the alloy ingot is subjected to forging and rolling. First, multiple passes of forging are performed to deform the alloy ingot and refine the grains. Then, hot rolling is carried out to obtain the desired thickness of the plate. The rolling temperature and speed are controlled during the process to achieve the desired plate properties.

[0044] Step Five: Quality Inspection: The prepared VNi alloy plate is subjected to quality inspection, including composition analysis, thermal conductivity testing, and processing plasticity evaluation. The composition of the plate is accurate, the thermal conductivity is high, and the processing plasticity is good, meeting the requirements of neutron scattering experiments on materials.

[0045] Example Three: Optimization of VNi Alloy Plate Preparation Process

[0046] Step One: Preparation and Optimization of Alloy Raw Materials

[0047] Higher purity vanadium raw materials (99.999%) and nickel raw materials (99.9999%) are selected, and accurate weighing is performed according to the optimized mass percentage of 55% vanadium and 45% nickel. By optimizing the purity of raw materials and the alloy ratio, the performance of the alloy plate is further improved.

[0048] Step Two: Melting and Refining Process

[0049] The weighed vanadium and nickel raw materials are placed in a vacuum induction furnace for melting, and the vacuum degree in the furnace is controlled to reach a higher value of 6.67×10 -5 Pa. During the melting process, refining agents are added to further remove impurities and gases in the alloy, improving the purity of the alloy.

[0050] Step Three: Homogenization Treatment and Heat Treatment

[0051] After the alloy liquid is cast into an ingot, homogenization treatment and heat treatment are performed. The homogenization treatment temperature is 1100°C, and the treatment time is 72 hours to ensure that the alloy composition is more uniform. Heat treatment includes solid solution treatment and aging treatment to improve the strength and hardness of the alloy.

[0052] Step Four: Precision Hot Working

[0053] The alloy ingot after heat treatment is subjected to precision forging and rolling. By controlling the forging temperature and deformation, as well as the rolling speed and rolling passes, the grains are further refined and the density of the plate is improved. Finally, the alloy plate with more uniform thickness and smoother surface is obtained.

[0054] Step Five: Comprehensive Quality Inspection and Evaluation

[0055] The prepared optimized VNi alloy plate is comprehensively detected and evaluated. In addition to the conventional component analysis, thermal conductivity test and processing plasticity evaluation, neutron diffraction peak detection, corrosion resistance test and the like are added. It is ensured that the plate not only meets the requirements of neutron scattering experiment, but also has more excellent corrosion resistance and longer service life.

[0056] It should be noted that, according to the basic properties of vanadium (V) and nickel (Ni) alloy and its application in material science, especially the related characteristics of neutron diffraction, high thermal conductivity and processing plasticity, the content of vanadium and nickel in the alloy has a significant influence on the performance of the alloy (such as thermal conductivity, processing plasticity, etc.), so the mass percentage of vanadium (V) and nickel (Ni) in the embodiment of the present application is the result of multiple experiments according to the material properties.

Claims

1. A non-neutron-diffraction-peak, high-thermal-conductivity VNi alloy plate material, characterized by: The plate is composed of vanadium (V) and nickel (Ni), wherein the mass percentage of vanadium is 40% to 60%, and the mass percentage of nickel is 40% to 60%; the alloy plate has no neutron diffraction peak, and the theoretical thermal conductivity at room temperature is not less than ; and has good processing plasticity, meets the requirements of neutron scattering experiments on sample containers and neutron beam windows, and meets the requirements of efficient high and low temperature in-situ experiments. The manufacturing method of the non-neutron diffraction peak, high thermal conductivity VNi alloy plate material includes the following steps: (1) Alloy raw material preparation: select vanadium raw material with purity better than 99.9% and nickel raw material with purity better than 99.99%, accurately weigh according to the mass percentage of vanadium 40% to 60% and nickel 40% to 60%; (2) Melting process: the weighed vanadium and nickel raw materials are put into a vacuum arc melting furnace, the vacuum degree in the furnace is controlled to be better than , and the alloy blank is obtained by melting. (3) Homogenization treatment: the melted alloy blank is subjected to homogenization treatment, the treatment temperature is 800-1100℃, and the treatment time is not less than 24 hours; (4) Hot working: the alloy blank after homogenization treatment is subjected to hot working, including forging and rolling, and multiple annealing-rolling cycle treatment is carried out during hot working, the rolling in multiple annealing-rolling cycle treatment is cold rolling, to obtain the alloy plate material with required shape and size, until the ideal thickness and mechanical properties are obtained; (5) Quality detection: the prepared alloy plate material is subjected to quality detection, including composition analysis, thermal conductivity test, processing plasticity evaluation and neutron diffraction peak detection, to ensure that the plate material meets the requirements of neutron scattering experiment.

2. The VNi alloy plate without neutron diffraction peak and high thermal conductivity according to claim 1, characterized in that: The shape of the plate material includes but is not limited to round plate and square plate, and the thickness of the plate material is adjusted according to the requirement.

3. The method of manufacturing a high thermal conductivity VNi alloy plate without neutron diffraction peaks according to claim 1, characterized in that: Step (3) is carried out in a high temperature furnace, wherein the temperature and time of homogenization treatment are controlled within the range that ensures uniform distribution of alloy internal components.

4. The non-peaked, high thermal conductivity VNi alloy sheet of any one of claims 1-3, wherein: It is used for manufacturing sample holding container or neutron beam window for neutron scattering experiment.

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