A resonant vaporization synergistic alloying method for manufacturing high-performance molybdenum alloys

Abstract

This invention discloses a resonant gasification synergistic alloying method for manufacturing high-performance molybdenum alloys, relating to the field of powder metallurgy technology. The method includes the following steps: S1, preparing materials; S2, preparing a solution; S3, adding materials to a resonant gasification synergistic device; S4, homogenizing the materials to obtain mixed powder. This invention is rationally designed, using a high-temperature gasification device to rapidly gasify the solution, dispersing it throughout the mixing chamber. The molybdenum powder in the mixing chamber is also in a dispersed state, ensuring sufficient contact between the solid powder and the solution, thus greatly improving the uniformity of alloy element addition. The molybdenum alloy precursor powder is then processed through subsequent pressing, sintering, and rolling processes, resulting in a high-performance molybdenum alloy with a tensile strength greater than 1100 MPa and an elongation greater than 7%, exhibiting excellent comprehensive performance.

Description

Technical Field

[0001] This invention relates to the field of powder metallurgy technology, and more specifically to the field of resonant gasification synergistic alloying method for manufacturing high-performance molybdenum alloys. Background Technology

[0002] Molybdenum is a refractory rare metallic element with many advantages. Powder metallurgy is commonly used in the production of molybdenum alloys. The addition of alloying elements is a crucial step in a series of processes including alloying element addition, pressing, sintering, and rolling. The most critical aspect of this process is the uniformity of alloying element addition, as it directly affects the final performance of the product. With increasingly stringent requirements for material performance, the drawbacks of existing alloying element addition methods are becoming more apparent. Common solid-solid process equipment often involves adding alloying elements in trace amounts, resulting in generally poor uniformity and a tendency to introduce impurities. Existing patents disclose the following technologies:

[0003] Patent CN101956088A, entitled "A Method for Preparing a Molybdenum-Doped Alloy," discloses the following: A method for preparing a molybdenum-doped alloy, suitable for preparing binary or multi-component molybdenum alloys. The method is characterized by the following steps: The preparation process of the alloy raw materials involves mixing an aqueous solution of the dopant element's nitrate with an auxiliary solution containing glycerol, anhydrous ethanol, and deionized water to form a mixed solution; adding MoO2 powder to the mixed solution to form a suspension; drying the suspension to obtain a mixed powder of Ce(NO3)3, glycerol, anhydrous ethanol, and MoO2; ball milling, sieving, and hydrogen reduction to obtain molybdenum alloy powder containing the dopant element; and finally, cold isostatic pressing and sintering to obtain the molybdenum-doped alloy. This method effectively ensures the bonding strength and uniformity between the alloy material and the molybdenum matrix, reducing the agglomeration of the molybdenum alloy.

[0004] In the solid-liquid method for molybdenum alloys disclosed in the aforementioned patent, the mixed alloy powder is prone to agglomeration and the introduction of impurities. Furthermore, the solid powder and the solution cannot make sufficient contact, resulting in poor uniformity of alloy element addition. These drawbacks ultimately lead to uneven particle size and low sintering activity in the prepared product, making it difficult to improve the overall performance of the molybdenum alloy product. Summary of the Invention

[0005] The purpose of this invention is to solve the technical problem that the powder and solution cannot fully contact each other in the existing solid-liquid mixing process of molybdenum alloys, resulting in poor uniformity of alloy element addition. This invention provides a resonant gasification synergistic alloying method for manufacturing high-performance molybdenum alloys.

[0006] To achieve the above objectives, the present invention specifically adopts the following technical solution:

[0007] A resonant vaporization-co-alloying method for manufacturing high-performance molybdenum alloys includes the following steps:

[0008] S1. Prepare materials: Prepare molybdenum powder, alloy additives and liquid medium for later use. Alloy additives include fructose, TiH2, ZrH2, Ti(SO4)2 and Zr(NO3)4.

[0009] S2. Solution preparation: Add fructose, TiH2, ZrH2, Ti(SO4)2 and Zr(NO3)4 from step S1 to a liquid medium to prepare an alloying element solution;

[0010] S3. Adding materials to the resonant gasification co-processing device: Add the molybdenum powder from step S1 and the alloying element solution prepared in step S2 to the resonant gasification co-processing device. The molybdenum powder and the alloying element solution are added to the mixing chamber and the high-temperature gasification device of the resonant gasification co-processing device, respectively.

[0011] S4. Material homogenization to obtain mixed powder: The resonant gasification synergistic device is turned on, and the molybdenum powder is dispersed in the mixing chamber under the resonance effect. The alloy element solution added in the high-temperature gasification device is atomized and added to the mixing chamber to mix with the dispersed molybdenum powder to obtain mixed powder. The heat energy of the high-temperature gasification device simultaneously dries the mixed powder quickly, thus obtaining a molybdenum alloy precursor powder with uniform alloy element addition.

[0012] Further, in step S1, the liquid medium is either water or alcohol, and the mass ratio of the liquid medium to the alloy powder is 1:2 to 1:30.

[0013] Further, in step S1, the mass percentages of chemical elements in the molybdenum powder and alloy additives are as follows: Ti: 0.01%–1.7%, Zr: 0.01%–0.50%, C: 0.01%–0.60%, La: 0.00–1.0%, Ta: 0.00–0.40%, Nb: 0.00–0.40%, Hf: 0.00–0.30%, Y: 0.00–0.20%, with the balance being molybdenum powder and unavoidable impurities, and the sum of the mass percentages of the chemical elements is 100.

[0014] Furthermore, in step S3, when the pressure inside the mixing chamber exceeds the safe value, the ventilation device of the resonant vaporization coordinating device is activated, and the ventilation device works periodically to prevent the pressure inside the mixing chamber from becoming too high.

[0015] Furthermore, the molybdenum alloy precursor powder obtained in step S5 is processed through subsequent pressing, sintering, and rolling processes to obtain a high-performance molybdenum alloy.

[0016] Furthermore, the resonant gasification coordinating device includes a mixing chamber for loading powder materials and a high-temperature gasification device for atomizing liquid materials. The mixing chamber is connected to the high-temperature gasification device, and a resonant device is provided at the bottom of the mixing chamber to allow the powder materials to diffuse inside the mixing chamber.

[0017] Specifically, a preferred structure of the resonant gasification synergistic device is disclosed. A high-temperature gasification device rapidly vaporizes the solution, dispersing it throughout the mixing chamber. The molybdenum powder in the mixing chamber is also in a dispersed state, ensuring sufficient contact between the solid powder and the solution, thus significantly improving the uniformity of alloy element addition. Simultaneously, the high-temperature gasification device, integrated within the mixing chamber, generates heat that greatly reduces agglomeration issues common in traditional methods, while also eliminating the need for a subsequent drying step.

[0018] The resonance device ensures that molybdenum powder is continuously and uniformly dispersed in the mixing chamber. The well-designed device, combined with the high-temperature gasification equipment, improves the uniformity of alloy element addition.

[0019] Furthermore, the mixing chamber includes a housing and a sealing cover disposed on the housing. The space enclosed by the housing and the sealing cover constitutes the mixing chamber. The sealing cover is also provided with an atomizing and diffused port that communicates with the high-temperature vaporization device.

[0020] Specifically, the location of the atomizing diffuser is disclosed, with the preferred method being to place it on the sealing cap. This is convenient for processing, manufacturing, and installation, requiring only an opening on the sealing cap, resulting in low manufacturing costs.

[0021] Furthermore, a sealing ring is provided between the housing and the sealing cover, and the housing and the sealing cover are locked together by multiple locking components, which are locking bolts, and the multiple locking bolts are evenly distributed around the edge of the sealing ring.

[0022] Specifically, a preferred sealing and locking method for the shell and the sealing cover is disclosed. This method has the advantages of easy disassembly, good sealing performance, prevention of the introduction of foreign impurities, and improvement of the quality of alloy element addition.

[0023] Furthermore, it also includes a ventilation device for depressurizing the inside of the mixing chamber, which is located on the sealing cover and communicates with the inside of the mixing chamber.

[0024] Specifically, this effectively avoids safety accidents caused by excessively high air pressure inside the mixing chamber.

[0025] Furthermore, the shell is a double-layer shell, which includes an inner shell and an outer shell. The inner shell and the outer shell form an insulation cavity, which is filled with an insulation layer.

[0026] Specifically, it was disclosed that the shell is a double-layer shell, and the middle of the double-layer shell is filled with an insulation layer. The design of the insulation layer can play a heat preservation role, preventing the temperature inside the mixing chamber from being transferred to the outside through the shell, thus avoiding heat loss and saving energy.

[0027] Working principle of the resonant gasification synergistic device:

[0028] The prepared solution is placed into a high-temperature vaporization device, and molybdenum powder is poured into the mixing chamber. The top cover is closed to the mixing chamber, and the resonance device is turned on. Under the resonance effect, the molybdenum powder is dispersed in the mixing chamber. At the same time, the prepared solution is vaporized by the high-temperature vaporization device and enters the mixing chamber, where it is fully mixed with the raw material molybdenum powder. The heat energy of the high-temperature vaporization device also dries the powder quickly. The ventilation device works periodically to prevent the pressure in the mixing chamber from being too high, thus obtaining a molybdenum alloy precursor powder with uniform alloying elements.

[0029] The beneficial effects of this invention are as follows:

[0030] 1. The high-performance molybdenum alloy obtained by processing the molybdenum alloy precursor powder through subsequent pressing, sintering, and rolling processes has a tensile strength greater than 1100 MPa and an elongation greater than 7%, exhibiting excellent comprehensive properties. This method is rationally designed, allows for uniform addition of alloying elements, is easy to control, and is suitable for production at various scales, thus possessing broad application prospects.

[0031] 2. This invention uniquely utilizes a high-temperature vaporization device to rapidly vaporize the solution, dispersing it throughout the mixing chamber. The molybdenum powder in the mixing chamber is also in a dispersed state, ensuring thorough contact between the solid powder and the solution, thus significantly improving the uniformity of alloy element addition. Simultaneously, the high-temperature vaporization device, built into the mixing chamber, generates heat that greatly reduces the agglomeration phenomenon associated with traditional methods, while also eliminating the need for subsequent drying steps.

[0032] 3. The invention uniquely employs a resonance device, which, through resonance, allows molybdenum powder to be continuously and uniformly dispersed in the mixing chamber. The design is reasonable, and when combined with a high-temperature gasification device, it improves the uniformity of alloy element addition.

[0033] 4. The present invention has good sealing performance, which avoids the introduction of foreign impurities and improves the quality of alloy element addition. Attached Figure Description

[0034] Figure 1 These are scanning electron microscope images of the molybdenum alloy precursor powder obtained in Example 1;

[0035] Figure 2 This is the EDS spectrum of the molybdenum alloy precursor powder obtained in Example 1;

[0036] Figure 3 This is a SEM image of the molybdenum alloy sample obtained after sintering in Example 1;

[0037] Figure 4 This is a SEM image of the fracture surface of the molybdenum alloy sample obtained after sintering in Example 1;

[0038] Figure 5 This is a metallographic image of the molybdenum alloy sample obtained after sintering in Example 1;

[0039] Figure 6 These are scanning electron microscope images of the molybdenum alloy precursor powder obtained in Example 2;

[0040] Figure 7 These are scanning electron microscope images of the molybdenum alloy precursor powder obtained in Example 3;

[0041] Figure 8 These are scanning electron microscope and energy dispersive spectroscopy images of the molybdenum alloy precursor powder obtained in Example 4;

[0042] Figure 9 These are scanning electron microscope and energy dispersive spectroscopy images of the molybdenum alloy precursor powder obtained in Example 5;

[0043] Figure 10 This is a SEM image of the fracture surface of the molybdenum alloy sample obtained after sintering in Example 5;

[0044] Appendix Figure 11 This is a schematic diagram of the resonant gasification synergistic device;

[0045] Appendix Figure 12 yes Figure 11 A top-view structural diagram;

[0046] Figure reference numerals: 1-High temperature gasification device, 2-Sealing cover, 3-Insulation layer, 4-Ventilation device, 5-Mixing chamber, 6-Resonance device. Detailed Implementation

[0047] To make the objectives, technical solutions, and advantages of the embodiments of the present invention clearer, 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. The components of the embodiments of the present invention described and shown in the accompanying drawings can generally be arranged and designed in various different configurations.

[0048] Therefore, the following detailed description of the embodiments of the invention provided in the accompanying drawings is not intended to limit the scope of the claimed invention, but merely to illustrate selected embodiments of the invention. All other embodiments obtained by those skilled in the art based on the embodiments of the invention without inventive effort are within the scope of protection of the invention.

[0049] It should be noted that similar reference numerals and letters in the following figures indicate similar items; therefore, once an item is defined in one figure, it does not need to be further defined and explained in subsequent figures. Furthermore, the terms "first," "second," etc., are used only to distinguish descriptions and should not be construed as indicating or implying relative importance.

[0050] In the description of the embodiments of the present invention, it should be noted that the terms "inner", "outer", "upper", etc., indicate the orientation or positional relationship based on the orientation or positional relationship shown in the accompanying drawings, or the orientation or positional relationship in which the product of the invention is usually placed when in use. They are only for the convenience of describing the present invention and simplifying the description, and do not indicate or imply that the device or element referred to must have a specific orientation, or be constructed and operated in a specific orientation. Therefore, they should not be construed as limiting the present invention.

[0051] The process engineering of this invention requires the use of a resonant gasification synergistic device, the structure of which is as follows:

[0052] like Figures 8 to 9 As shown, the resonant gasification synergistic device includes a mixing chamber 5 for loading powder materials and a high-temperature gasification device 1 for atomizing liquid materials. The mixing chamber 5 is connected to the high-temperature gasification device 1, and a resonant device 6 is provided at the bottom of the mixing chamber 5 to allow the powder materials to diffuse inside the mixing chamber 5.

[0053] Specifically, a preferred structure of the resonant gasification synergistic device is disclosed. A high-temperature gasification device rapidly vaporizes the solution, dispersing it throughout the mixing chamber 5. The molybdenum powder in the mixing chamber 5 is also in a dispersed state, ensuring sufficient contact between the solid powder and the solution, thus significantly improving the uniformity of alloy element addition. Simultaneously, the high-temperature gasification device, built into the mixing chamber 5, greatly reduces the agglomeration phenomenon associated with traditional methods by generating heat energy, while also eliminating the need for a subsequent drying step.

[0054] The resonant device 6 ensures that the molybdenum powder is continuously and uniformly dispersed in the mixing chamber 5. The design is reasonable, and when combined with the high-temperature gasification device, it improves the uniformity of alloy element addition.

[0055] The mixing chamber 5 includes a housing and a sealing cover 2 disposed on the housing. The space enclosed by the housing and the sealing cover 2 constitutes the mixing chamber 5. The sealing cover 2 is also provided with an atomizing and diffused port that is connected to the high-temperature vaporization device 1.

[0056] Specifically, the location of the atomizing diffuser is disclosed. It is a preferred method to place it on the sealing cover 2, which is convenient for processing, manufacturing and installation. It only requires an opening on the sealing cover 2, and the manufacturing cost is low.

[0057] A sealing ring is provided between the housing and the sealing cover 2. The housing and the sealing cover 2 are locked together by multiple locking components, which are locking bolts. The multiple locking bolts are evenly distributed around the edge of the sealing ring.

[0058] Specifically, a preferred sealing and locking method for the housing and the sealing cover 2 is disclosed. This method has the advantages of easy disassembly, good sealing performance, prevention of the introduction of foreign impurities, and improvement of the quality of alloy element addition.

[0059] It also includes a ventilation device 4 for depressurizing the inside of the mixing chamber 5, which is located on the sealing cover 2 and communicates with the inside of the mixing chamber 5.

[0060] Specifically, this effectively avoids safety accidents caused by excessively high air pressure inside the mixing chamber 5.

[0061] The shell is a double shell, which includes an inner shell and an outer shell. The inner shell and the outer shell form an insulation cavity, which is filled with an insulation layer 3.

[0062] Specifically, it is disclosed that the shell is a double-layer shell, and the middle of the double-layer shell is filled with a heat insulation layer 3. The design of the heat insulation layer 3 can play a heat preservation role, preventing the temperature inside the mixing chamber 5 from being transferred to the outside through the shell, thus avoiding heat loss and saving energy.

[0063] Example 1

[0064] This embodiment provides a resonant vaporization-coordinated alloying method for manufacturing high-performance molybdenum alloys, comprising the following steps:

[0065] S1. Prepare materials: Prepare 1.200g fructose, 3.200g TiH2, 0.490g ZrH2, 15.000g Ti(SO4)2, 2.260g Zr(NO3)4, 500g molybdenum powder, and 500ml alcohol for later use;

[0066] S2. Solution preparation: Add fructose, TiH2, ZrH2, Ti(SO4)2 and Zr(NO3)4 from step S1 to a liquid medium to prepare an alloying element solution;

[0067] S3. Material addition to resonant gasification co-processing device: The molybdenum powder in step S1 and the alloying element solution prepared in step S2 are added to the resonant gasification co-processing device. The molybdenum powder and the alloying element solution are added to the mixing chamber 5 and the high-temperature gasification device 1 of the resonant gasification co-processing device, respectively.

[0068] S4. Material homogenization to obtain mixed powder: The resonant gasification synergistic device is turned on, and the molybdenum powder is dispersed in the mixing chamber 5 under the resonance effect. The alloy element solution added in the high temperature gasification device 1 is atomized and added to the mixing chamber 5 to mix with the dispersed molybdenum powder to obtain mixed powder. The resonant gasification synergistic device is turned off after working for 10 minutes. The heat energy of the high temperature gasification device 1 simultaneously dries the mixed powder quickly, thus obtaining a molybdenum alloy precursor powder with uniform alloy element addition.

[0069] The scanning electron microscope image of the molybdenum alloy precursor powder obtained in this embodiment is as follows: Figure 1 As shown, the prepared solution, after vaporization and drying, was uniformly mixed with molybdenum powder without caking, and the powder particles were dried evenly. The EDS spectrum of the molybdenum alloy precursor powder is shown below. Figure 2 As shown, the uniform and dispersed distribution of Ti, Mo, and Zr elements can be seen, which is consistent with the scanning electron microscope image, indicating that the molybdenum alloy precursor powder obtained by the present invention has uniform alloy element addition and excellent effect.

[0070] Based on this molybdenum alloy precursor powder, the sample underwent subsequent pressing, sintering, and rolling processes. The SEM image of the sintered sample is attached. Figure 3 As shown, the second phase was observed to be uniformly distributed on the matrix. The fracture surface SEM image of the sintered sample is attached. Figure 4 As shown, the second-phase particles are uniformly distributed throughout the grains and grain boundaries. The metallographic image of the sintered sample is attached. Figure 5 As shown, uniformly distributed second-phase particles were also observed, which corroborates the results of the SEM images. Testing revealed that the molybdenum alloy sheet prepared in this invention has a tensile strength of 1183 MPa and an elongation of 8.16%. Overall, the sample with added alloying elements via resonant gasification synergistic device exhibits a uniform microstructure and excellent comprehensive performance, making it a high-performance molybdenum alloy.

[0071] Example 2

[0072] This embodiment provides a resonant vaporization-coordinated alloying method for manufacturing high-performance molybdenum alloys, comprising the following steps:

[0073] S1. Prepare materials: Prepare 1.200g fructose, 3.200g TiH2, 0.490g ZrH2, 15.000g Ti(SO4)2, 2.260g Zr(NO3)4, 1000g molybdenum powder, and 500ml alcohol for later use;

[0074] S2. Solution preparation: Add fructose, TiH2, ZrH2, Ti(SO4)2 and Zr(NO3)4 from step S1 to a liquid medium to prepare an alloying element solution;

[0075] S3. Material addition to resonant gasification co-processing device: The molybdenum powder in step S1 and the alloying element solution prepared in step S2 are added to the resonant gasification co-processing device. The molybdenum powder and the alloying element solution are added to the mixing chamber 5 and the high-temperature gasification device 1 of the resonant gasification co-processing device, respectively.

[0076] S4. Material homogenization to obtain mixed powder: The resonant gasification synergistic device is turned on, and the molybdenum powder is dispersed in the mixing chamber 5 under the resonance effect. The alloy element solution added in the high temperature gasification device 1 is atomized and added to the mixing chamber 5 to mix with the dispersed molybdenum powder to obtain mixed powder. The resonant gasification synergistic device is turned off after working for 10 minutes. The heat energy of the high temperature gasification device 1 simultaneously dries the mixed powder quickly, thus obtaining a molybdenum alloy precursor powder with uniform alloy element addition.

[0077] The scanning electron microscope image of the molybdenum alloy precursor powder obtained in this embodiment is as follows: Figure 6 As shown, the molybdenum alloy plate prepared in this embodiment has a tensile strength of 1165 MPa and an elongation of 7.96%. Overall, the sample with added alloying elements via resonant gasification synergistic device has a uniform microstructure and excellent comprehensive performance, making it a high-performance molybdenum alloy.

[0078] Tests showed that increasing the amount of molybdenum powder added under the same experimental conditions would lead to a slight decrease in the effect of alloying element addition. When the critical addition amount is reached, the uniformity of alloying element addition will be greatly reduced. Therefore, attention should be paid to the reasonable amount of raw material molybdenum powder, which should generally not exceed 700g. Using multiple devices to form a set of equipment can greatly improve work efficiency.

[0079] Example 3

[0080] This embodiment provides a resonant vaporization-coordinated alloying method for manufacturing high-performance molybdenum alloys, comprising the following steps:

[0081] S1. Prepare materials: Prepare 1.200g fructose, 3.200g TiH2, 0.490g ZrH2, 15.000g Ti(SO4)2, 2.260g Zr(NO3)4, 500g molybdenum powder, and 500ml alcohol for later use;

[0082] S2. Solution preparation: Add fructose, TiH2, ZrH2, Ti(SO4)2 and Zr(NO3)4 from step S1 to a liquid medium to prepare an alloying element solution;

[0083] S3. Material addition to resonant gasification co-processing device: The molybdenum powder in step S1 and the alloying element solution prepared in step S2 are added to the resonant gasification co-processing device. The molybdenum powder and the alloying element solution are added to the mixing chamber 5 and the high-temperature gasification device 1 of the resonant gasification co-processing device, respectively.

[0084] S4. Homogenization of materials to obtain mixed powder: The resonant gasification co-processing device is turned on, and the molybdenum powder is dispersed in the mixing chamber 5 under the resonance effect. The alloy element solution added in the high-temperature gasification device 1 is atomized and added to the mixing chamber 5 to mix with the dispersed molybdenum powder to obtain mixed powder. The resonant gasification co-processing device is turned off after working for 10 minutes. The frequency of the resonant gasification co-processing device is reduced when it is working (compared to Example 1). The heat energy of the high-temperature gasification device 1 simultaneously dries the mixed powder quickly, thus obtaining a molybdenum alloy precursor powder with uniform alloy element addition.

[0085] The scanning electron microscope image of the molybdenum alloy precursor powder obtained in this embodiment is as follows: Figure 7 As shown, the molybdenum alloy plate prepared in this embodiment has a tensile strength of 1123 MPa and an elongation of 7.49%. Overall, the sample with added alloying elements via resonant gasification synergistic device has a uniform microstructure and excellent comprehensive performance, making it a high-performance molybdenum alloy.

[0086] Experiments show that the operating frequency of the resonant device affects the amplitude of the raw molybdenum powder. Too low an operating frequency will cause the raw molybdenum powder to be unable to disperse in the mixing chamber and fully contact the vaporized solution, thereby reducing the uniformity of alloying element addition. A frequency of 55HZ is suitable for 500g of molybdenum powder. For a certain amount of raw molybdenum powder, the operating frequency of the resonant device can improve the uniformity of alloying element addition.

[0087] Example 4

[0088] This embodiment provides a resonant vaporization-coordinated alloying method for manufacturing high-performance molybdenum alloys, comprising the following steps:

[0089] S1. Prepare the following materials: 1.200g fructose, 3.200g TiH2, 0.490g ZrH2, 15.000g Ti(SO4)2, 2.260g Zr(NO3)4, 500g molybdenum powder, and 500ml water.

[0090] S2. Solution preparation: Add fructose, TiH2, ZrH2, Ti(SO4)2 and Zr(NO3)4 from step S1 to a liquid medium to prepare an alloying element solution;

[0091] S3. Material addition to resonant gasification co-processing device: The molybdenum powder in step S1 and the alloying element solution prepared in step S2 are added to the resonant gasification co-processing device. The molybdenum powder and the alloying element solution are added to the mixing chamber 5 and the high-temperature gasification device 1 of the resonant gasification co-processing device, respectively.

[0092] S4. Homogenization of materials to obtain mixed powder: Turn on the resonant gasification co-processing device (replace the resonant device with a high-frequency vibration device). Under the action of the high-frequency vibration device, the molybdenum powder is dispersed in the mixing chamber 5. The alloy element solution added in the high-temperature gasification device 1 is atomized and added to the mixing chamber 5 to mix with the dispersed molybdenum powder to obtain mixed powder. After the resonant gasification co-processing device works for 60 minutes, it is turned off. The heat energy of the high-temperature gasification device 1 simultaneously dries the mixed powder quickly, thus obtaining a molybdenum alloy precursor powder with uniform alloy element addition.

[0093] The scanning electron microscope and energy dispersive spectroscopy images of the molybdenum alloy precursor powder obtained in this embodiment are as follows: Figure 8 As shown, the molybdenum alloy plate prepared in this comparative example has a tensile strength of 1192 MPa and an elongation of 8.17%. Overall, the sample with added alloying elements via resonant gasification synergistic device has a uniform microstructure and excellent comprehensive performance, making it a high-performance molybdenum alloy.

[0094] Experiments show that extending the equipment working time has little impact on the uniformity of alloy element addition. The lower mixing chamber allows the raw material molybdenum powder to be quickly dispersed and distributed within it after the resonant gasification synergistic device. The raw material solution can also be quickly dispersed in the mixing chamber and fully mixed with the raw material molybdenum powder after the high-temperature gasification device. The high-temperature gasification device also assists in drying, which accelerates the bonding process. Therefore, this invention can prepare molybdenum alloy precursor powder with uniform alloy element addition very efficiently.

[0095] Example 5

[0096] This embodiment provides a resonant vaporization-coordinated alloying method for manufacturing high-performance molybdenum alloys, comprising the following steps:

[0097] S1. Prepare the following materials: 1.200g fructose, 6.400g TiH2, 0.980g ZrH2, 30.000g Ti(SO4)2, 4.520g Zr(NO3)4, 500g molybdenum powder, and 500ml water.

[0098] S2. Solution preparation: Add fructose, TiH2, ZrH2, Ti(SO4)2 and Zr(NO3)4 from step S1 to a liquid medium to prepare an alloying element solution;

[0099] S3. Material addition to resonant gasification co-processing device: The molybdenum powder in step S1 and the alloying element solution prepared in step S2 are added to the resonant gasification co-processing device. The molybdenum powder and the alloying element solution are added to the mixing chamber 5 and the high-temperature gasification device 1 of the resonant gasification co-processing device, respectively.

[0100] S4. Homogenization of materials to obtain mixed powder: Turn on the resonant gasification co-processing device (replace the resonant device with a high-frequency vibration device). Under the action of the high-frequency vibration device, the molybdenum powder is dispersed in the mixing chamber 5. The alloy element solution added in the high-temperature gasification device 1 is atomized and added to the mixing chamber 5 to mix with the dispersed molybdenum powder to obtain mixed powder. After the resonant gasification co-processing device works for 10 minutes, it is turned off. The heat energy of the high-temperature gasification device 1 simultaneously dries the mixed powder quickly, thus obtaining a molybdenum alloy precursor powder with uniform alloy element addition.

[0101] The molybdenum alloy sheet prepared in this comparative example has a tensile strength of 1215 MPa and an elongation of 8.03%. Overall, the sample with added alloying elements via resonant gasification synergistic device has a uniform microstructure and excellent comprehensive performance, making it a high-performance molybdenum alloy.

[0102] The scanning electron microscope and energy dispersive spectroscopy images of the molybdenum alloy precursor powder obtained in this embodiment are as follows: Figure 9 As shown, the prepared solution, after vaporization, was uniformly mixed with molybdenum powder without caking, and the powder particles were dried and uniform. Based on this molybdenum alloy precursor powder, subsequent pressing, sintering, and rolling processes were performed. The fracture surface SEM image of the resulting molybdenum alloy sample after sintering is shown in the attached figure. Figure 10 As shown, the second-phase particles are uniformly distributed at various positions within the grains and grain boundaries. Experiments indicate that different solute ratios in the raw material solution have little effect on the uniformity of alloy element addition, but do affect the final properties of the alloy. Compared to conventional alloy element addition methods, under the same solute ratio in the raw material solution, the molybdenum alloy prepared by the resonant gasification synergistic device exhibits higher tensile strength and better overall performance.

[0103] Comparative Example 1

[0104] This embodiment provides a resonant vaporization-coordinated alloying method for manufacturing high-performance molybdenum alloys, comprising the following steps:

[0105] S1. Prepare the following materials: 1.200g fructose, 3.200g TiH2, 0.490g ZrH2, 15.000g Ti(SO4)2, 2.260g Zr(NO3)4, 500g molybdenum powder, and 500ml water.

[0106] S2. Solution preparation: Add fructose, TiH2, ZrH2, Ti(SO4)2 and Zr(NO3)4 from step S1 to a liquid medium to prepare an alloying element solution;

[0107] S3. Material addition to resonant gasification co-processing device: The molybdenum powder in step S1 and the alloying element solution prepared in step S2 are added to the resonant gasification co-processing device. The molybdenum powder and the alloying element solution are added to the mixing chamber 5 and the high-temperature gasification device 1 of the resonant gasification co-processing device, respectively.

[0108] S4. Homogenization of materials to obtain mixed powder: Turn on the resonant gasification co-processing device (replace the resonant device with a high-frequency vibration device). Under the action of the high-frequency vibration device, the molybdenum powder is dispersed in the mixing chamber 5. The alloy element solution added in the high-temperature gasification device 1 is atomized and added to the mixing chamber 5 to mix with the dispersed molybdenum powder to obtain mixed powder. After the resonant gasification co-processing device works for 10 minutes, it is turned off. The heat energy of the high-temperature gasification device 1 simultaneously dries the mixed powder quickly, thus obtaining a molybdenum alloy precursor powder with uniform alloy element addition.

[0109] The molybdenum alloy plate prepared in this comparative example has a tensile strength of 863 MPa and an elongation of 5.32%. Overall, when the resonance device is replaced with a high-frequency vibration device, the microstructure of the sample after adding alloying elements is not uniform enough.

[0110] Experiments show that high-frequency vibration equipment can also vibrate molybdenum powder to a certain height and disperse the raw molybdenum powder in the mixing chamber. However, the amplitude generated by the high-frequency vibration equipment on the molybdenum powder is low and it is not easy to adjust the amplitude. Therefore, the original resonance equipment is still the better solution.

[0111] The table below compares the performance of Examples 1-5 and Comparative Example 1. The molybdenum alloy mixture obtained using this method, after subsequent pressing, sintering, and rolling processes, produces a high-strength, high-toughness molybdenum alloy with a tensile strength greater than 1100 MPa and an elongation greater than 7%, exhibiting excellent comprehensive performance. This method is rationally designed, produces uniform and easily controlled mixtures, and is suitable for various production scales, thus possessing broad application prospects.

[0112]

Claims

1. A resonant vaporization-coordinated alloying method for manufacturing high-performance molybdenum alloys, characterized in that, Includes the following steps: S1. Prepare materials: Prepare molybdenum powder, alloy additives and liquid medium for later use. Alloy additives include fructose, TiH2, ZrH2, Ti(SO4)2 and Zr(NO3)4. The liquid medium is either water or alcohol, and the mass ratio of the liquid medium to the alloy powder is 1:2 to 1:

30. The mass percentages of chemical elements in the molybdenum powder and alloy additives are as follows: Ti: 0.01%–1.7%, Zr: 0.01%–0.50%, C: 0.01%–0.60%, La: 0.00–1.0%, Ta: 0.00–0.40%, Nb: 0.00–0.40%, Hf: 0.00–0.30%, Y: 0.00–0.20%, with the balance being molybdenum powder and unavoidable impurities. The sum of the mass percentages of the chemical elements is 100. S2. Solution preparation: Add fructose, TiH2, ZrH2, Ti(SO4)2 and Zr(NO3)4 from step S1 to a liquid medium to prepare an alloying element solution; S3. Material addition to resonant gasification co-processing device: The molybdenum powder in step S1 and the alloying element solution prepared in step S2 are added to the resonant gasification co-processing device. The molybdenum powder and the alloying element solution are added to the mixing chamber (5) and the high-temperature gasification device (1) of the resonant gasification co-processing device, respectively. The resonant gasification coordinating device includes a mixing chamber (5) for loading powder materials and a high-temperature gasification device (1) for atomizing liquid materials. The mixing chamber (5) is connected to the high-temperature gasification device (1). A resonant device (6) is provided at the bottom of the mixing chamber (5) to allow the powder materials to diffuse inside the mixing chamber (5). The mixing chamber (5) includes a housing and a sealing cover (2) disposed on the housing. The space enclosed by the housing and the sealing cover (2) constitutes the mixing chamber (5). The sealing cover (2) is also provided with an atomizing diffuser that communicates with the high-temperature vaporization device (1). S4. Material homogenization to obtain mixed powder: The resonant gasification synergistic device is turned on, and the molybdenum powder is dispersed in the mixing chamber (5) under the resonance effect. The alloy element solution added in the high temperature gasification device (1) is atomized and added to the mixing chamber (5) to mix with the dispersed molybdenum powder to obtain mixed powder. The heat energy of the high temperature gasification device (1) simultaneously dries the mixed powder quickly, thus obtaining a molybdenum alloy precursor powder with uniform alloy element addition. It also includes a ventilation device (4) for depressurizing the inside of the mixing chamber (5), the ventilation device (4) being located on the sealing cover (2) and communicating with the inside of the mixing chamber (5).

2. The resonant vaporization synergistic alloying method for manufacturing high-performance molybdenum alloys according to claim 1, characterized in that, In step S3, when the pressure in the mixing chamber (5) exceeds the safe value, the gas exchange device (4) of the resonant gasification synergistic device is turned on, and the gas exchange device (4) works periodically to prevent the pressure in the mixing chamber (5) from being too high.

3. The resonant vaporization synergistic alloying method for manufacturing high-performance molybdenum alloys according to claim 1, characterized in that, The molybdenum alloy precursor powder obtained in step S5 is processed by subsequent pressing, sintering, and rolling processes to obtain a high-performance molybdenum alloy.

4. The resonant vaporization synergistic alloying method for manufacturing high-performance molybdenum alloys according to claim 1, characterized in that, A sealing ring is provided between the housing and the sealing cover (2). The housing and the sealing cover (2) are locked together by multiple locking components, which are locking bolts. The multiple locking bolts are evenly distributed around the edge of the sealing ring.

5. The resonant vaporization synergistic alloying method for manufacturing high-performance molybdenum alloys according to claim 1, characterized in that, The shell is a double-layer shell, which includes an inner shell and an outer shell. The inner shell and the outer shell form a heat-insulating cavity, and the heat-insulating cavity is filled with a heat-insulating layer (3).

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