A BCC structure, an oxidation-resistant zero-coherence scattering alloy and its preparation method

Abstract

This invention relates to the field of neutron scattering experimental materials, proposing a neutron-diffraction-resistant, oxidation-resistant, zero-coherence scattering alloy material with a single-phase BCC structure suitable for high-temperature neutron scattering experiments, and its preparation method. This alloy contains 37.07% Ti, 59.95% Ta, and 2.98% Al, with a theoretical melting point of 1867℃. It exhibits no neutron diffraction peaks and can be used to prepare sample containers and neutron beam windows. The TiTaAl alloy shows no neutron diffraction peaks in X-ray and neutron diffraction patterns, avoiding data interference and improving experimental data quality. Its theoretical melting point is higher than existing TiZr alloys, and it maintains high strength and high ductility at high temperatures, making it suitable for high-temperature experimental environments above 800℃. After oxidation for 80 hours at 1000℃ in an atmospheric environment, the oxidation weight gain is only 43 mg / cm³. 2 It exhibits excellent antioxidant properties, improving the reusability and economy of materials. This invention achieves precise composition control and efficient manufacturing by optimizing steps such as batching, smelting, alloying, homogenization, and forging, solving problems such as inaccurate composition control, low efficiency, and high cost in existing processes, thereby improving product quality and production efficiency.

Description

Technical Field

[0001] This invention relates to the field of neutron scattering experimental materials, specifically to a BCC structure, an oxidation-resistant zero-coherence scattering alloy, and its preparation method. This alloy material can be used to prepare sample containers and neutron beam windows in neutron scattering experiments to meet the material performance requirements of high-temperature in-situ experiments. Background Technology

[0002] Neutron scattering experiments, as an important tool for studying the microstructure and dynamic properties of matter, have wide applications in materials science, physics, chemistry, and many other fields. In this experiment, the test samples are diverse in form, including solids, liquids, and powders, and require a specialized sample container placed within the test neutron beam. During the experiment, the neutron beam passes through the sample-containing container and interacts with the sample, thereby acquiring neutron scattering data to analyze the sample's microstructure and dynamic properties.

[0003] However, the scattering signal from the sample container itself can greatly complicate data analysis and severely affect data quality. Meanwhile, the sample environment in neutron scattering experiments plays an increasingly important role in in-situ neutron testing, and the complex structures and metallic components within the sample environment further exacerbate the influence of external signals on neutron scattering data. To obtain high-quality neutron scattering data, neutron scattering experiments require strict control of the scattering background to avoid various background signal sources affecting the quality of the neutron scattering data.

[0004] Currently, vanadium metal, as well as TiZr and VNi alloys, are commonly used internationally as sample containers. However, existing materials have significant limitations in high-temperature experimental environments. Vanadium metal exhibits significant embrittlement at temperatures exceeding 1200°C, and undergoes rapid and catastrophic oxidation above 675°C, severely restricting its reusability and economic viability. While TiZr zero-coherence scattering alloys show some application potential, their melting point is only 1550°C, and they soften and recrystallize above 750°C, greatly limiting their application potential under high-temperature experimental conditions. Furthermore, existing VNi alloys also suffer from oxidation and embrittlement problems above 675°C, making them unsuitable for high-temperature neutron scattering experiments.

[0005] Currently, there are no suitable zero-coherence scattering alloy materials available internationally for high-temperature experimental environments above 800℃. Existing alloy manufacturing processes suffer from problems such as inaccurate composition control, low production efficiency, and high costs, making it difficult to prepare alloy materials that meet the requirements of high-temperature neutron scattering experiments. Summary of the Invention

[0006] Based on the above problems, the present invention aims to develop a high-temperature resistant, oxidation-resistant, and neutron-diffraction-free BCC structure (i.e., body-centered cubic structure) zero-coherence scattering alloy and its preparation method, which can be used to improve the data quality and experimental efficiency of neutron scattering experiments.

[0007] The technical solution adopted by the present invention to solve the technical problem is: a BCC structure, oxidation-resistant zero-coherence scattering alloy, wherein the chemical composition of the alloy by weight percentage is: Ti 37.07%, Ta 59.95%, Al 2.98%, the remainder being unavoidable impurities, and the theoretical melting point of the alloy is 1867℃, with no neutron diffraction peaks.

[0008] The alloy showed no significant weight gain after oxidation at 1000℃ for 2 hours in an atmospheric environment; after 80 hours of oxidation, the weight gain was only 43 mg / cm³. 2 It exhibits excellent antioxidant properties.

[0009] The raw materials for preparing the alloy include bulk elemental Ti with a purity of better than 99.99%, elemental Ta with a purity of better than 99.99%, and elemental Al with a purity of better than 99.999%.

[0010] The alloy raw materials need to be cleaned with a 10% HCl solution before being mixed to remove the surface oxide layer.

[0011] A method for preparing an oxidation-resistant zero-coherence scattering alloy with no diffraction peaks for high-temperature neutron scattering includes the following steps:

[0012] Step 1, Proportioning: Prepare alloy raw materials by mixing bulk elemental Ti with a purity of better than 99.99%, elemental Ta with a purity of better than 99.99%, and elemental Al with a purity of better than 99.999% in a ratio of 37.07Ti:59.95Ta:2.98Al (wt%), and remove the surface oxide layer by cleaning with 10% HCl solution;

[0013] Step 2, Smelting: Vacuum suspension smelting is adopted. First, Ti / Ta is placed in the furnace for pre-smelting. The smelting power is 209kW, and the smelting time is 5 minutes. The power is slowly reduced to the minimum, and the furnace is cooled for 1 hour to obtain TiTa alloy ingots.

[0014] Step 3, Alloying: The TiTa alloy ingots refined in Step 2 and pure aluminum ingredients are put into the furnace for melting. The melting power is 235kW, 220kW and 200kW respectively. The melting and refining time for each melting and refining is 10 minutes and the cooling time is 1 hour. Kilogram-level alloy ingots with uniform composition are prepared.

[0015] Step 4, Homogenization treatment: Place the alloy ingot in a high-temperature furnace and perform vacuum annealing treatment (vacuum degree better than 5*10-3Pa) at 1000℃-1400℃ for more than 24 hours or annealing treatment under Ar gas protection to homogenize it.

[0016] Step 5: Forging: The homogenized bar stock is forged at a temperature above 1000℃ to obtain bars or plates of the ideal size.

[0017] In step two, the vacuum level during the smelting process is better than 5*10-3 Pa.

[0018] In step three, a cooling process is performed after each melting, with a cooling time of 1 hour.

[0019] In step four, the homogenization process is performed by vacuum annealing or annealing under Ar gas protection.

[0020] The alloy exhibits excellent high strength and high plasticity at high temperatures.

[0021] The aforementioned zero-coherence diffraction peak-free oxidation-resistant alloy for high-temperature neutron scattering, or its preparation method, is applicable to the manufacture of sample containers and neutron beam windows in neutron scattering experiments, and can effectively improve the data quality and experimental efficiency of neutron scattering experiments.

[0022] The beneficial effects of this invention are as follows: The TiTaAl alloy of this invention has no neutron diffraction peaks in the neutron diffraction pattern, which can effectively avoid interference with neutron scattering data, significantly improve the data quality of neutron scattering experiments, and provide a reliable guarantee for accurate analysis of sample microstructure and dynamic characteristics; the alloy of this invention has a theoretical melting point of 1867℃, which is significantly improved compared with the existing TiZr alloy (melting point 1550℃), and can still maintain high strength and high plasticity at high temperatures, and can be used stably in high-temperature experimental environments above 800℃, meeting the mechanical performance requirements of sample container and neutron beam window in high-temperature neutron scattering experiments; after oxidation at 1000℃ for 80 hours, the oxidation weight gain of the TiTaAl alloy is only 43mg / cm³. 2 Under these conditions, V and VNi alloys will undergo severe oxidation. The alloy of this invention exhibits excellent oxidation resistance, improves the reusability and economy of the material, and reduces experimental costs. By optimizing steps such as batching, smelting, alloying, homogenization, and forging, this invention achieves precise control of alloy composition and an efficient manufacturing process, improving product quality and production efficiency, and solving the problems of inaccurate composition control, low production efficiency, and high cost in existing alloy manufacturing processes. Attached Figure Description

[0023] Figure 1 This is a Pandat phase diagram showing the relationship between the calculated and theoretical melting points of the TiTaAl alloy of this invention;

[0024] Figure 2 This is the X-ray diffraction pattern of the TiTaAl alloy of this invention, which exhibits a typical BCC structure;

[0025] Figure 3 This is the neutron diffraction pattern of the TiTaAl alloy with no neutron diffraction peaks according to the present invention;

[0026] Figure 4 These are the test results of the oxidation properties of the TiTaAl alloy of this invention;

[0027] Figure 5 This is a comparison chart of the mechanical properties of the TiTaAl alloy in the embodiments of the present invention and current zero-coherence scattering alloys;

[0028] Figure 6 This is a schematic diagram showing the high-temperature mechanical properties of the TiTaAl alloy compared to the TiZr alloy in this embodiment of the invention. Detailed Implementation

[0029] The specific embodiments of the present invention will be described in detail below with reference to the accompanying drawings:

[0030] like Figure 1-6 As shown, a zero-coherence, oxidation-resistant alloy with no diffraction peaks is used for high-temperature neutron scattering. It is suitable for manufacturing sample containers and neutron beam windows in neutron scattering experiments, and can effectively improve the data quality and experimental efficiency of neutron scattering experiments. It exhibits excellent high strength and high plasticity at high temperatures. The chemical composition of the alloy, by weight percentage, is: Ti 37.07%, Ta 59.95%, Al 2.98%, with the remainder being unavoidable impurities. The theoretical melting point of the alloy is 1867℃, and it has no neutron diffraction peaks.

[0031] The alloy showed no significant weight gain after oxidation at 1000℃ for 2 hours in an atmospheric environment; after 80 hours of oxidation, the weight gain was only 43 mg / cm³. 2 It exhibits excellent antioxidant properties.

[0032] The raw materials for preparing the alloy include bulk elemental Ti with a purity of better than 99.99%, elemental Ta with a purity of better than 99.99%, and elemental Al with a purity of better than 99.999%.

[0033] The alloy raw materials need to be cleaned with a 10% HCl solution before being mixed to remove the surface oxide layer.

[0034] A method for preparing an oxidation-resistant zero-coherence scattering alloy with no diffraction peaks for high-temperature neutron scattering includes the following steps:

[0035] Step 1, Proportioning: Prepare alloy raw materials by mixing bulk elemental Ti with a purity of better than 99.99%, elemental Ta with a purity of better than 99.99%, and elemental Al with a purity of better than 99.999% in a ratio of 37.07Ti:59.95Ta:2.98Al (wt%), and remove the surface oxide layer by cleaning with 10% HCl solution;

[0036] Step 2, Smelting: Vacuum suspension smelting is adopted. First, Ti / Ta is placed in the furnace for pre-smelting. The smelting power is 209kW, and the smelting time is 5 minutes. The power is slowly reduced to the minimum, and the furnace is cooled for 1 hour to obtain TiTa alloy ingots.

[0037] Step 3, Alloying: The TiTa alloy ingots refined in Step 2 and pure aluminum ingredients are put into the furnace for melting. The melting power is 235kW, 220kW and 200kW respectively. The melting and refining time for each melting and refining is 10 minutes and the cooling time is 1 hour. Kilogram-level alloy ingots with uniform composition are prepared.

[0038] Step 4, Homogenization treatment: Place the alloy ingot in a high-temperature furnace and perform vacuum annealing treatment (vacuum degree better than 5*10-3Pa) at 1000℃-1400℃ for more than 24 hours or annealing treatment under Ar gas protection to homogenize it.

[0039] Step 5: Forging: The homogenized bar stock is forged at a temperature above 1000℃ to obtain bars or plates of the ideal size.

[0040] In step two, the vacuum level during the smelting process is better than 5*10-3 Pa.

[0041] In step three, a cooling process is performed after each melting, with a cooling time of 1 hour.

[0042] In step four, the homogenization process is performed by vacuum annealing or annealing under Ar gas protection.

[0043] Example 1

[0044] Step 1: Ingredients

[0045] Using a ratio of 37.07Ti:59.95Ta:2.98Al (wt%), bulk elemental Ti with a purity better than 99.99%, elemental Ta with a purity better than 99.99%, and elemental Al with a purity better than 99.999% were selected as raw materials. The raw materials were washed in a 10% HCl solution to remove the surface oxide layer and ensure the purity of the raw materials.

[0046] Step 2: Melting

[0047] Using vacuum suspension melting technology, Ti and Ta were first placed in a melting furnace for pre-melting. The melting power was set to 209 kW, and the melting time was 5 minutes. Then, the power was slowly reduced to the minimum, maintaining a vacuum level better than 5 × 10⁻³ Pa. After cooling for 1 hour, the TiTa alloy ingot was obtained.

[0048] Step 3: Alloying

[0049] The TiTa alloy ingots obtained in step two were placed together with pure aluminum feedstock into a melting furnace for three melting processes. The first melting power was 235kW, the second was 220kW, and the third was reduced to 200kW. Each melting and refining process took 10 minutes, and the cooling time was 1 hour to ensure uniform alloy composition, ultimately producing kilogram-sized TiTaAl alloy ingots.

[0050] Step 4: Homogenization

[0051] The alloy ingot is placed in a high-temperature furnace and subjected to vacuum annealing at 1000℃-1400℃ for more than 24 hours (vacuum degree better than 5×10-3Pa), or annealed under Ar gas protection, in order to achieve the homogenization of the alloy.

[0052] Step 5: Forging

[0053] The homogenized alloy bars are forged at temperatures above 1000℃, and bars or plates of ideal dimensions are obtained by controlling the forging process parameters.

[0054] Compared with existing TiZr alloys, the TiTaAl alloy prepared in this embodiment showed no significant weight gain after oxidation at 1000℃ for 2 hours in an atmospheric environment; after oxidation for 80 hours, the weight gain was only 43 mg / cm³. 2 It exhibits excellent oxidation resistance. At the same time, the theoretical melting point of TiTaAl alloy is 1867℃, which is significantly higher than that of TiZr alloy (1550℃), and it can still maintain high strength and high plasticity at high temperatures.

[0055] Example 2

[0056] Step 1: Ingredients

[0057] Similar to Example 1, raw materials were selected in the ratio of 37.07Ti:59.95Ta:2.98Al (wt%) and then cleaned.

[0058] Steps two through five: smelting, alloying, homogenization, and forging.

[0059] Steps two through five are exactly the same as in Example 1, using precise melting, alloying, homogenization and forging processes to prepare high-quality TiTaAl alloy bars or plates.

[0060] The TiTaAl alloy prepared in this embodiment exhibits excellent mechanical properties. Its yield strength is significantly higher than that of the TiZr alloy across a temperature range from room temperature to 800°C. Particularly at 800°C, the yield strength of the TiTaAl alloy remains at a high level, while the yield strength of the TiZr alloy decreases significantly due to softening. Furthermore, the TiTaAl alloy also possesses good plasticity, meeting the stringent requirements for sample containers and neutron beam windows in high-temperature neutron scattering experiments.

[0061] In this embodiment, TiZr alloy and VNi alloy from the prior art were selected as comparative examples. Under the same high-temperature neutron scattering experimental conditions, TiZr alloy softened and underwent recrystallization at temperatures exceeding 750°C, severely affecting its high-temperature mechanical properties. VNi alloy, on the other hand, experienced a rapid and catastrophic oxidation reaction at temperatures above 675°C, leading to a sharp decline in material properties. In contrast, the TiTaAl alloy of this invention maintains excellent mechanical properties and oxidation resistance even under high-temperature experimental conditions above 800°C, demonstrating significant technical advantages.

[0062] In summary, the TiTaAl alloy of this invention achieves a perfect combination of high strength, high plasticity, and excellent oxidation resistance through precise control of alloy composition and efficient manufacturing process, providing an ideal sample container and neutron beam window material for high-temperature neutron scattering experiments.

Claims

1. A BCC structure, oxidation-resistant zero-coherence scattering alloy, characterized in that: The chemical composition of the alloy, by weight percentage, is: Ti 36.5~37.5%, Ta 59.5~60.5%, Al 2.7~3.1%, with the remainder being unavoidable impurities. The alloy has a theoretical melting point of 1867℃, a single-phase BCC structure, and no neutron diffraction peaks.

2. The BCC structure, oxidation-resistant zero-coherence scattering alloy according to claim 1, characterized in that: The alloy showed no significant weight gain after oxidation for 2 hours at 1000℃ in an atmospheric environment; after 80 hours of oxidation, the weight gain was only 43 mg / cm², demonstrating excellent oxidation resistance.

3. A BCC structure, oxidation-resistant zero-coherence scattering alloy according to claim 1 or 2, characterized in that: The raw materials for preparing the alloy include bulk elemental Ti with a purity higher than 99.99%, elemental Ta with a purity higher than 99.99%, and elemental Al with a purity higher than 99.999%.

4. The BCC structure, oxidation-resistant zero-coherence scattering alloy according to claim 3, characterized in that: The raw materials for the preparation of the alloy need to be cleaned with a 10% HCl solution before batching to remove the surface oxide layer.

5. A method for preparing a BCC structure, oxidation-resistant zero-coherence scattering alloy, characterized in that: Includes the following steps: Step 1, Proportioning: Mix elemental Ti with a purity higher than 99.99%, elemental Ta with a purity higher than 99.99%, and elemental Al with a purity higher than 99.999% in a ratio of 37.07Ti:59.95Ta:2.98Al (wt%) to prepare alloy raw materials, and clean them with 10% HCl solution to remove the surface oxide layer; Step 2, Smelting: Vacuum suspension smelting is adopted. First, Ti / Ta is placed in the furnace for pre-smelting. The smelting power is 209kW, and the smelting time is 5 minutes. The power is slowly reduced to the minimum, and the furnace is cooled for 1 hour to obtain TiTa alloy ingots. Step 3, Alloying: The TiTa alloy ingots refined in Step 2 and pure aluminum ingredients are put into the furnace for melting. The melting power is 235kW, 220kW and 200kW respectively. The melting and refining time for each melting and refining is 10 minutes and the cooling time is 1 hour. Kilogram-level alloy ingots with uniform composition are prepared. Step 4: Homogenization treatment: Place the alloy ingot in a high-temperature furnace and perform vacuum annealing at 1000℃-1400℃ for more than 24 hours, with a vacuum degree higher than 5×10⁻⁶. -3 Annealing under Pa or Ar gas protection for homogenization; Step 5: Forging: The homogenized alloy ingot is forged at a temperature above 1000℃ to obtain bars or plates of ideal size.

6. The method for preparing a BCC structure, oxidation-resistant zero-coherence scattering alloy according to claim 5, characterized in that: In step two, the vacuum degree during the melting process is 5×10⁻⁶. -3 Pa or above.

7. The method for preparing a BCC structure, oxidation-resistant zero-coherence scattering alloy according to claim 5, characterized in that: In step three, a cooling process is performed after each melting, with a cooling time of 1 hour.

8. The method for preparing a BCC structure, oxidation-resistant zero-coherence scattering alloy according to claim 5, characterized in that: In step four, the homogenization process is performed by vacuum annealing or annealing under Ar gas protection.

9. The method for preparing a BCC structure, oxidation-resistant zero-coherence scattering alloy according to claim 5, characterized in that: The alloy exhibits excellent high strength and high plasticity at high temperatures.

10. The application of a BCC structure, oxidation-resistant zero-coherence scattering alloy according to any one of claims 1-4, characterized in that: The alloy is suitable for manufacturing sample containers and neutron beam windows in neutron scattering experiments, and can effectively improve the data quality and experimental efficiency of neutron scattering experiments.

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