A nano-alloy neutron target film material and its preparation method

Abstract

This invention discloses a nano-alloy neutron target film material and its preparation method. The chemical formula of the target film material is Ti. a X b V c Al d Nb e Where X is selected from Zr or Mg, and a, b, c, d, and e represent the atomic percentages of the corresponding elements, with 5 ≤ a ≤ 40, 5 ≤ b ≤ 40, 5 ≤ c ≤ 40, 5 ≤ d ≤ 40, and 5 ≤ e ≤ 40, and a + b + c + d + e = 100. This invention, through rational composition design, coordination of multiple elements, and specific preparation methods, nanoscales high-entropy alloys, achieving a deuterium (tritium) release temperature of the neutron target exceeding 200°C, while simultaneously increasing the deuterium storage capacity H / M to over 1.8, effectively improving the temperature resistance and deuterium storage performance of the neutron target.

Description

Technical Field

[0001] This invention relates to the field of neutron target technology, and in particular to a nano-alloy neutron target film material and its preparation method. Background Technology

[0002] The target is a key component of neutron tubes and accelerators. It not only stores deuterium (tritium) atoms but also serves as the interface for nuclear reactions. Alloying can effectively improve the hydrogen embrittlement phenomenon of pure metal target films. The preparation process of alloy targets, the types of metal elements, and the proportion of elements directly affect the microstructure and performance of the target, thereby affecting neutron yield and lifetime.

[0003] The deuterium (tritium) release temperature is a critical indicator for neutron targets. If the release temperature is too low, the target will release deuterium (tritium) before reaching the ambient operating temperature, which not only reduces the target's performance but also alters the vacuum level of the device, affecting its service life. Currently, the highest deuterium (tritium) release temperature of alloy neutron target films can reach around 150℃, which is still not ideal. Summary of the Invention

[0004] The main objective of this invention is to provide a nano-alloy neutron target film material with a higher deuterium (tritium) release temperature and its preparation method.

[0005] To achieve the above objectives, this invention provides a nano-alloy neutron target film material with the chemical formula Ti. a X b V c Al d Nb e Where X is selected from Zr or Mg, and a, b, c, d, e represent the atomic percentage of the corresponding elements, 5≤a≤40, 5≤b≤40, 5≤c≤40, 5≤d≤40, 5≤e≤40, and a+b+c+d+e=100.

[0006] Furthermore, the chemical formula of the material is Ti. 20 Zr 20 V 20 Al 20 Nb 20 Or Ti 20 Mg 20 V 20 Al 20 Nb 20 .

[0007] This invention also provides a method for preparing a nano-alloy neutron target, comprising the following steps:

[0008] S1. Perform surface pretreatment on the substrate;

[0009] S2. The above-mentioned target film material is deposited on the substrate surface using magnetron sputtering to form a nano-alloy target film.

[0010] S3. The coated neutron target is transferred to a heating furnace under oxygen-free conditions for annealing.

[0011] S4. Place the annealed neutron target into the intake platform and fill it with deuterium / tritium until saturation.

[0012] Further, in step S1, the substrate is made of molybdenum, copper or their alloys; the surface pretreatment method of the substrate is as follows: first, the substrate surface is polished, and then the substrate is ultrasonically cleaned in an ethanol / acetone solution for more than 30 minutes.

[0013] Furthermore, the substrate surface is polished to a surface roughness of [value missing].

[0014] Furthermore, in step S2, the magnetron sputtering target power is 50W to 500W, and the thickness of the nano-alloy target film is 100nm to 50μm.

[0015] Furthermore, in step S3, the annealing process is carried out under vacuum or inert atmosphere at a temperature of 150℃ to 1000℃ for 30 min to 2 h.

[0016] Further, in step S4, activation is performed by repeatedly absorbing and releasing gas in deuterium / tritium 2 to 4 times, with the deuterium / tritium absorption temperature being 300℃ to 600℃ and the deuterium / tritium absorption pressure being 100Pa to 10kPa.

[0017] The beneficial effects of this invention are reflected in:

[0018] This invention achieves the increase of the deuterium (tritium) release temperature of the neutron target to above 200°C and the increase of the deuterium storage capacity H / M to above 1.8 through reasonable composition design, coordination of multiple elements and preparation method to nanoscale high-entropy alloy, effectively improving the temperature resistance and deuterium storage performance of the neutron target. Attached Figure Description

[0019] Figure 1 Here is a SEM image of the nano-alloy neutron target film prepared in Example 1;

[0020] Figure 2 The figure shows the TDS outgassing test results of the nano-alloy neutron target prepared in Example 1;

[0021] Figure 3 SEM image of the nano-alloy neutron target film prepared in Example 2;

[0022] Figure 4 The figure shows the TDS outgassing test results of the nano-alloy neutron target prepared in Example 2;

[0023] Figure 5The figure shows the TDS outgassing test results of the nano-alloy neutron target prepared in control group 1.

[0024] Figure 6 The image shows the SEM image of the nano-alloy neutron target film prepared in control group 2.

[0025] Figure 7 The figure shows the TDS outgassing test results of the nano-alloy neutron target prepared in control group 2. Detailed Implementation

[0026] The present invention will be further described in a clear and detailed manner below with reference to specific embodiments.

[0027] Unless otherwise specified, all raw materials used in the embodiments of the present invention are commercially available or obtainable by those skilled in the art; unless otherwise specified, all methods used in the embodiments of the present invention are methods mastered by those skilled in the art.

[0028] Example 1

[0029] Preparation of nano-alloy neutron targets

[0030] In this embodiment, molybdenum is used as the substrate material, and Ti is used as the substrate material. 20 Zr 20 V 20 Al 20 Nb 20 Ti was used as a target film material and was melted using a vacuum melting method. 20 Zr 20 V 20 Al 20 Nb 20 The material is smelted and shaped according to the design proportions and processed into a target size suitable for magnetron sputtering equipment, with a diameter of 2 inches and a thickness of 0.2 inches. The specific preparation method includes the following steps:

[0031] S1. Polish the substrate surface until the surface roughness is [value missing]. The substrate was then ultrasonically cleaned in ethanol for 30 minutes and then dried with compressed air.

[0032] S2. Sputtering Ti in DC mode under an argon atmosphere. 20 Zr 20 V 20 Al 20 Nb 20 During the sputtering process, the magnetron sputtering power was 150W, the gas flow rate was 10ml / min, and the vacuum level was 5.5×10⁻⁶. -4 Pa, the substrate temperature was 25℃, and the time was 1.5h, to deposit a 5μm nano-alloy target film;

[0033] S3. The coated neutron target is transferred to a heating furnace under oxygen-free conditions for annealing; the annealing process is carried out at 5×10⁻⁶ ℃. -6 The experiment was conducted under vacuum conditions of Pa, at a temperature of 800℃, for 1 hour.

[0034] S4. Place the annealed neutron target sheet into a high-vacuum gas-absorbing platform and repeatedly absorb and release gas three times in deuterium to activate the film. Then, fill the film with deuterium until it is saturated. The deuterium absorption temperature is 400℃, the deuterium absorption pressure is 10000Pa, the deuterium release temperature is 195℃, and the deuterium release pressure is under vacuum.

[0035] The nano-alloy neutron target film prepared in this embodiment was scanned using a scanning electron microscope, and the SEM image is shown below. Figure 1 As shown. From Figure 1 It can be seen that a nanofilm with a uniform structure and a certain degree of surface wrinkles was obtained.

[0036] Using TDS (thermal desorption / resorption spectroscopy) at an initial pressure of 5*10 -5 Pa tests show that the deuterium uptake of the neutron target, H / M, can reach 1.8, and the initial deuterium release temperature is close to 200℃. Figure 2 As shown.

[0037] Example 2

[0038] Preparation of nano-alloy neutron targets

[0039] In this embodiment, molybdenum is used as the substrate material, and Ti is used as the substrate material. 20 Mg 20 V 20 Al 20 Nb 20 Ti was used as a target film material and was melted using a vacuum melting method. 20 Mg 20 V 20 Al 20 Nb 20 The material is smelted and shaped according to the design proportions and processed into a target size suitable for magnetron sputtering equipment, with a diameter of 2 inches and a thickness of 0.2 inches. The specific preparation method includes the following steps:

[0040] S1. Polish the substrate surface to the desired surface roughness. The substrate was then ultrasonically cleaned in acetone for 30 minutes and then dried with compressed air.

[0041] S2. Sputtering Ti in DC mode under an argon atmosphere. 20 Mg 20 V 20 Al 20 Nb 20During the sputtering process, the magnetron sputtering power was 100W, the gas flow rate was 10ml / min, and the vacuum level was 5.5×10⁻⁶. -4 Pa, the substrate temperature is 25℃, the time is 1h, and a 1μm nano alloy target film is deposited.

[0042] S3. The coated neutron target is transferred to a heating furnace under oxygen-free conditions for annealing. The annealing is carried out under an inert atmosphere at a temperature of 200°C for 2 hours.

[0043] S4. Place the annealed neutron target sheet into a high-vacuum gas-absorbing platform and repeatedly absorb and vent it in deuterium four times to activate the film. Then, fill it with deuterium until it is saturated. The deuterium absorption temperature is 400℃, the deuterium absorption pressure is 10000Pa, the deuterium release temperature is 195℃, and the deuterium release pressure is under vacuum.

[0044] The nano-alloy neutron target film prepared in this embodiment was scanned using a scanning electron microscope, and the SEM image is shown below. Figure 3 As shown. From Figure 3 It can be seen that the obtained nanofilm is composed of bulk particles with a particle size of about 100 nm.

[0045] TDS testing showed that the neutron target's deuterium uptake (H / M) reached 1.95, and the initial deuterium release temperature was as high as 200℃. Figure 4 As shown.

[0046] Example 3

[0047] The effect of V on the deuterium release temperature of the neutron target

[0048] Based on Example 2, V in the target film material was omitted, and other steps and conditions were the same as in Example 2, serving as control group 1.

[0049] TDS testing was performed on the nano-alloy neutron target prepared in control group 1, and the results showed that the initial deuterium release temperature dropped to around 130℃. Figure 5 As shown.

[0050] Example 4

[0051] The effect of Al on neutron target performance

[0052] Based on Example 2, Al in the target film material was omitted, and other steps and conditions were the same as in Example 2, serving as control group 2.

[0053] Electron microscopy was performed on the nano-alloy neutron target film prepared in control group 2, as shown in... Figure 6 As shown, the grain size reaches over 100 nanometers, and through TDS testing, its deuterium absorption is significantly reduced, with an H / M ratio of only 1.2, and the initial deuterium release temperature is also as low as around 120℃. Figure 7 As shown.

[0054] The above description is only a preferred embodiment of the present invention and is not intended to limit the present invention. Any modifications, equivalent substitutions, improvements, etc., made within the spirit and principles of the present invention should be included within the protection scope of the present invention.

Claims

1. A nano-alloy neutron target film material, characterized in that: The chemical formula is Ti 20 Mg 20 V 20 Al 20 Nb 20 .

2. A method for preparing a nano-alloy neutron target, characterized in that, Includes the following steps: S1. Perform surface pretreatment on the substrate; S2. A nano-alloy target film is formed by depositing the target film material as described in claim 1 onto the substrate surface using a magnetron sputtering method. S3. The coated neutron target is transferred to a heating furnace under oxygen-free conditions for annealing. S4. Activate the annealed neutron target and then fill it with deuterium / tritium until saturation.

3. The method for preparing the nano-alloy neutron target as described in claim 2, characterized in that, In step S1, the substrate is made of molybdenum, copper or their alloys; the surface pretreatment method of the substrate is as follows: first, the substrate surface is polished, and then the substrate is ultrasonically cleaned in an ethanol / acetone solution for more than 30 minutes.

4. The method for preparing the nano-alloy neutron target as described in claim 2, characterized in that, In step S2, the magnetron sputtering target power is 50W to 500W, and the thickness of the nano-alloy target film is 100nm to 50μm.

5. The method for preparing the nano-alloy neutron target as described in claim 2, characterized in that, In step S3, the annealing process is carried out under vacuum or inert atmosphere at a temperature of 150℃ to 1000℃ for 30 min to 2 h.

6. The method for preparing the nano-alloy neutron target as described in claim 2, characterized in that, In step S4, activation is performed by repeatedly absorbing and releasing gas in deuterium / tritium 2 to 4 times, with the deuterium / tritium absorption temperature being 300℃ to 600℃ and the deuterium / tritium absorption pressure being 100Pa to 10kPa.

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