Ternary alloy preparation device and preparation method
By controlling the temperature gradient under vacuum conditions, a vertical ternary alloy preparation device was developed to solve the problem of impurity elements introduced into the alloy, enabling the preparation of high-purity ternary alloys, improving the mechanical properties and corrosion resistance of the alloys, and expanding their applications in aviation, aerospace, biology, and electronics.
Patent Information
- Application Number
- CN202510776040.3
- Authority / Receiving Office
- CN · China
- Patent Type
- Applications(China)
- Current Assignee / Owner
- Filing Date
- 2025-06-11
- Publication Date
- 2025-09-26
AI Technical Summary
When preparing ternary alloys, existing technologies easily introduce impurity elements, resulting in a decrease in the mechanical properties and corrosion resistance of the alloys. In particular, oxide inclusions in magnesium alloys become a performance bottleneck, limiting their application in aviation, aerospace, biology and electronics.
A vertical ternary alloy preparation device is used to control the evaporation temperature and temperature gradient of different metals under vacuum conditions. The temperature gradient change in the central furnace body is used to evaporate metals A, B, and C separately, condense them to form a high-purity ternary alloy, and reduce the heavy metal content.
Effectively reduce the Fe and Ni content in the alloy, increase the corrosion rate of the alloy, and enhance the mechanical properties and forming properties of the alloy to meet the application needs of high-end fields.
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Figure CN120702220A_ABST
Abstract
Description
Technical Field
[0001] The present invention relates to alloy processing technology, and in particular to a ternary alloy preparation device and preparation method. Background Art
[0002] Ternary alloys are mostly prepared by smelting alloys. During smelting, impurity elements or inclusions are often introduced, resulting in a decrease in the alloy's mechanical properties and corrosion resistance. For example, magnesium-containing ternary alloys have extensive applications in aviation, aerospace, biology, and electronics. However, the low purity of magnesium alloys has become a key bottleneck restricting their application. In particular, inclusions such as oxidation are the source of damage to mechanical and corrosion properties. High inclusion content in magnesium alloys not only limits the potential of magnesium alloys but also significantly reduces their formability and corrosion resistance. For example, when the Fe content reaches a certain level, it significantly increases the corrosion rate of the magnesium alloy. To improve the application of AZ31 magnesium alloy in high-end applications, the impurity elements in the alloy must be reduced as much as possible. Achieving a magnesium alloy with a purity of 99.99 wt.% is essential. Summary of the Invention
[0003] In view of the defects or shortcomings of the prior art, the present invention first provides a ternary alloy preparation device.
[0004] The ternary alloy of the present invention is an alloy made of metal A, metal B, and metal C; under vacuum conditions, the evaporation temperature of metal A is higher than the evaporation temperature of metal B, and the evaporation temperature of metal B is higher than the evaporation temperature of metal C; the preparation device includes a vertical central furnace body, a metal A evaporation chamber, a metal B evaporation chamber, a metal C evaporation chamber, and a condensation chamber;
[0005] The condensation chamber is located at the axial top of the central furnace body, and the condensation chamber is communicated with the central furnace body; the metal A evaporation chamber is communicated with the central furnace body through an overflow port A, and the diameter of the overflow port A is smaller than the inner diameter of the metal A evaporation chamber; the metal B evaporation chamber is communicated with the central furnace body through an overflow port B, and the diameter of the overflow port B is smaller than the inner diameter of the metal B evaporation chamber; the metal C evaporation chamber is communicated with the central furnace body through an overflow port C, and the diameter of the overflow port C is smaller than the inner diameter of the metal C evaporation chamber;
[0006] Along the axial direction, the overflow port A is located below the overflow port B and has a distance between it and the overflow port B. The overflow port B is located below the overflow port C and has a distance between it and the overflow port C. The overflow port C is located below the condensation chamber and has a distance between it and the condensation chamber.
[0007] Optionally, the mass percentage of metal element B in the ternary alloy is higher than that of metal element A, and the mass percentage of metal element A is higher than that of metal element C; the caliber of overflow port C is smaller than that of overflow port B, and the caliber of overflow port C is smaller than that of overflow port A. Furthermore, optionally, the caliber of steam overflow port A is 1 / 3-1 / 2 of the inner diameter of the metal A evaporation chamber; the caliber of overflow port B is 1 / 2 of the inner diameter of the metal B evaporation chamber; and the caliber of steam overflow port C is 1 / 4-1 / 3 of the inner diameter of the metal C evaporation chamber.
[0008] An optional solution is that the central furnace body is divided into a bottom area, a middle area, an upper area and a top area from the axial bottom to the top, the metal A evaporation chamber is arranged in the bottom area of the central furnace body, the metal B evaporation chamber is arranged on the side of the middle area, the metal C evaporation chamber is arranged on the side of the upper area, and the condensation chamber is arranged in the top area of the central furnace body.
[0009] Another optional solution is that the metal B evaporation chamber and the metal C evaporation chamber are respectively located on both sides of the central furnace body.
[0010] An optional solution is that the outer walls of the central furnace body, metal A evaporation chamber, metal B evaporation chamber and metal C evaporation chamber are all made of carbon steel and the inner lining is made of refractory material, and electric heating rods are provided between the outer walls and the inner lining of the metal A evaporation chamber, metal B evaporation chamber and metal C evaporation chamber.
[0011] An optional solution is that the outer wall of the condensation chamber is made of carbon steel, the inner lining is made of refractory material, and electric heating rods are provided between the outer wall and the inner lining of the condensation chamber.
[0012] The device of the present invention has a vertical structure, which makes good use of the temperature gradient change from bottom to top, reduces the mutual interference of the temperatures of different evaporation chambers, and can effectively utilize the heat of the system.
[0013] The present invention also provides a method for preparing a ternary alloy using the above-mentioned device, the method comprising:
[0014] (1) Place the formulated amounts of metals A, B, and C into the corresponding evaporation chambers, and then evacuate the chamber;
[0015] (2) The temperature in the evaporation chamber of metal A is heated to the evaporation temperature of metal A, and the temperature is kept at the evaporation temperature of metal A; then the temperature in the evaporation chamber of metal B is heated to the evaporation temperature of metal B, and the temperature is kept at the evaporation temperature of metal B; then the temperature in the evaporation chamber of metal C is heated to the evaporation temperature of metal C, and the temperature is kept at the evaporation temperature of metal C; during the process, the temperature in the condensation chamber is raised from room temperature to the condensation temperature and the temperature is kept at the condensation temperature, and the condensation temperature is lower than the evaporation temperature of metal C;
[0016] (3) Each evaporation chamber and condensation chamber continue to keep warm;
[0017] (4) Under the condition that the condensation chamber continues to be kept warm: first stop the heating and heat preservation of the evaporation chamber of metal A, then stop the heating and heat preservation of the evaporation chamber of metal B, and finally stop the heating and heat preservation of the evaporation chamber of metal C;
[0018] (5) Cool the inside of the device until the temperature in the condensation chamber drops to room temperature, stop vacuuming, and collect the ternary alloy in the condensation chamber.
[0019] Optionally, the vacuum condition is 1-10Pa.
[0020] Optionally, under vacuum conditions, the evaporation temperature of metal A is 300-700°C higher than that of metal B; the evaporation temperature of metal B is 250-450°C higher than that of metal C; and the condensation temperature is 50-100°C lower than the evaporation temperature of metal C.
[0021] A further solution also includes: processing the collected ternary alloy under hot pressing conditions to densify its structure.
[0022] Optionally, the metal A is aluminum, the metal B is magnesium, and the metal C is zinc; and the evaporation temperature of metal A is 1300-1500°C, the evaporation temperature of metal B is 800-1000°C, and the evaporation temperature of metal C is 450-550°C; after heating three times in step (2), the temperature of the condensation chamber rises from room temperature to 400-450°C.
[0023] The present invention achieves the purpose of preparing a high-purity ternary alloy by evaporating, mixing and condensing three elements at a rate according to the composition ratio of the ternary alloy (for example, Mg:Al:Zn=200:4-5:1-2) in the same vacuum system through device improvements and temperature control of different evaporation chambers.
[0024] The present invention can reduce the content of heavy metals, Fe, and Ni, in the alloy, thereby reducing the corrosion rate of the ternary alloy. This is particularly true for AZ31 alloy, as it addresses the difficulty in ensuring the proper Al composition in AZ31, which is caused by the low Al vapor pressure and slow evaporation rate. This ternary vapor phase synthesis system solves the problem of Al evaporation difficulties. BRIEF DESCRIPTION OF THE DRAWINGS
[0025] Figure 1 It is a structural drawing of the device of the present invention.
[0026] Figure 2 The XRD pattern of the product prepared in Example 1 is shown in FIG.
[0027] Figure 3 This is the EDS result of the product prepared in the example. Figure 3 (a) is the microstructure photograph of the ternary alloy. Figure 3 (b) Figure 3(a) Spectrum of electron spectroscopy analysis. DETAILED DESCRIPTION
[0028] Unless otherwise specified, the scientific and technical terms used herein are understood according to the knowledge of ordinary technicians in the relevant fields.
[0029] The three metal raw materials used in the ternary alloy feedstock of the present invention have different evaporation temperatures under vacuum conditions (e.g., 1-10 MPa). To achieve vaporization of each metal within the device and create a temperature gradient within the central furnace body that is beneficial for ternary alloy synthesis, specific solutions can adjust the axial distance between the overflow ports of each metal evaporation chamber and the size relationship between the inner diameter of each metal evaporation chamber and the corresponding overflow port diameter to achieve a suitable temperature gradient within the central furnace body, based on the evaporation temperatures of the three metals. In other specific solutions, the evaporation rate of each metal can be adjusted by adjusting the size of the corresponding overflow port diameter, thereby meeting the different content requirements of the three metal elements in the target ternary alloy.
[0030] The following examples further illustrate the present invention by taking the processing of AZ31 alloy as an example.
[0031] Example:
[0032] This embodiment is a specific device for preparing ternary alloy materials. Figure 1 As shown, the device is provided with a central furnace body 1, the bottom area of the central furnace body is provided with a metal A evaporation chamber 2, the middle area of the central furnace body bulges outward to the side to form a metal B evaporation chamber 3, the upper area bulges outward to the other side to form a metal C evaporation chamber 4, the top area is a condensation chamber 5, and the top of the condensation chamber is provided with a vacuum port 9; the metal A evaporation chamber is connected to the central furnace body through an overflow port A6; the metal B evaporation chamber is connected to the central furnace body through an overflow port B7; and the metal C evaporation chamber is connected to the central furnace body through an overflow port C8;
[0033] In this embodiment, see Figure 1 As shown, the structure inside the condensing chamber adopts the existing crystallizer structure; the central furnace body and the outer walls of each evaporation chamber are made of carbon steel, the lining insulation structure adopts insulation material, and resistance rods are provided between the outer wall and the inner lining of each evaporation chamber for heating; in addition, in order to prevent the instability of the condensing chamber temperature, resistance rods are also provided inside the condensing chamber furnace wall of this embodiment for heating.
[0034] Among them, the axial dimension of the central furnace body 1 is: 1.2 meters, and the central furnace body diameter is 150mm; the axial height of the metal A evaporation chamber is: 150mm, the inner diameter is 300mm, and the overflow port A6 diameter is 120mm; the inner diameter and inner length (length along the radial direction of the central furnace body) of the metal B evaporation chamber are 180mm and 330mm respectively, and the overflow port B7 diameter is 90mm; the diameter and inner length of the metal C evaporation chamber are: 120mm and 240mm respectively, and the overflow port C8 diameter is 30mm; the axial height of the condensation chamber is: 240mm;
[0035] The axial distance between the top and the bottom of the metal B evaporation chamber is 180 mm; the axial distance between the top of the metal B evaporation chamber and the bottom of the metal C evaporation chamber is 150 mm; the axial distance between the top of the metal C evaporation chamber and the bottom of the condensation chamber is 80 mm.
[0036] The above-mentioned device is used to prepare AZ31 ternary magnesium alloy material. The specific preparation method is as follows:
[0037] Step 1: Magnesium, aluminum, and zinc are placed in three evaporation chambers according to the ratio of the elements in the AZ31 alloy: 96: (3-6): 1 (mass fraction). In the metal A evaporation chamber, i.e., the Al evaporation chamber, as much aluminum as possible is placed, and the surface area of the aluminum is as large as possible. The entire system is then evacuated to 0.1-1 Pa.
[0038] Step 2: First, heat the aluminum evaporation chamber to a temperature of 1300-1500°C at a heating rate of 5-10°C / min. The temperature of the entire system is raised. Due to heat conduction and temperature gradients, when the aluminum evaporation chamber reaches 1300-1500°C, the temperature of the metal B evaporation chamber (i.e., the magnesium evaporation chamber) is approximately 100-200°C, and the temperature of the metal C evaporation chamber (i.e., the zinc evaporation chamber) is approximately 50-100°C. In this case, the temperature is insufficient to evaporate the magnesium and zinc. The condensation chamber is kept at approximately room temperature.
[0039] After the temperature of the aluminum evaporation chamber reaches 1300-1500℃, heat the magnesium evaporation chamber to 800-1000℃ at a heating rate of 5-10 degrees / min. When the temperature of the magnesium evaporation chamber reaches 800-1000℃, the temperature of the condensation chamber can reach about 200℃.
[0040] After the magnesium evaporation chamber temperature reaches 800-1000℃, heat the zinc evaporation temperature to between 450-550℃ at a heating rate of 5-10 degrees / min; when the zinc evaporation chamber temperature reaches 450-550℃, the condensation chamber temperature can reach about 400℃;
[0041] Step 3: After the temperatures of the three heating chambers are constant, keep them warm for 2.5 hours. The specific time is based on the complete evaporation of metallic magnesium. Allow aluminum, magnesium, and zinc to evaporate continuously. The temperature of the aluminum evaporation chamber is 1300-1500°C, the temperature of the magnesium evaporation chamber is 800-1000°C, and the temperature of the zinc evaporation chamber is 450-550°C. Under heat conduction and temperature gradient, the temperature of the condensation chamber can be guaranteed to be between 400-450°C.
[0042] Step 4: Stop heating. The order of stopping heating is to stop heating the aluminum evaporation chamber first, then stop heating the magnesium evaporation chamber, and finally stop heating the zinc evaporation chamber to ensure the temperature gradient of the entire system and ensure that the three metal vapors of aluminum, magnesium and zinc do not crystallize on the non-condenser wall before reaching the condenser;
[0043] Step 5: Stop vacuuming and allow the device to cool naturally until the condenser slowly cools down to room temperature, and take out the collected ternary magnesium alloy from the condenser crystallizer;
[0044] Step 6: The magnesium alloy collected in step 5 can be hot pressed (300-350° C., pressure 40 MPa) to obtain a dense ternary magnesium alloy.
[0045] The XRD pattern of the product obtained in this embodiment is as follows Figure 2 The energy spectrum (EDS) analysis results are shown in Figure 3 As shown in Table 2, the energy spectrum (EDS) analysis of the obtained product shows that (1) the main chemical composition is: Mg: 92.38wt.%; Al: 5.78wt.%; Zn: 1.7wt.%. (2) the mechanical properties of the obtained product are: tensile strength 260-280MPa, elongation 3-10%; (3) the corrosion rate of the obtained product in simulated body fluid is <0.15mg / (cm 2 .day). Corrosion rates of the solution components of simulated body fluids (see Table 1 below):
[0046] Table 1 Solution composition of simulated body fluids
[0047] Serial number chemical composition g / L 1 NaCl 8 2 KCl 0.4 3 <![CDATA[CaCl2]]> 0.14 4 <![CDATA[NaHCO3]]> 0.35 5 <![CDATA[MgCl2.6H2O]]> 0.1 6 <![CDATA[C6H6O6]]> 1 7 <![CDATA[MgSO47H2O]]> 0.06 8 <![CDATA[KH2PO4]]> 0.06 9 <![CDATA[Na2HPO412H2O]]> 0.06
[0048] Table 2 is Figure 3 (b)-corresponding spectrum value
[0049]
[0050]
Claims
1. A device for preparing a ternary alloy, wherein the ternary alloy is an alloy of metal A, metal B, and metal C; under vacuum conditions, the evaporation temperature of metal A is higher than the evaporation temperature of metal B, and the evaporation temperature of metal B is higher than the evaporation temperature of metal C; characterized in that: The preparation device includes a vertical central furnace body, a metal A evaporation chamber, a metal B evaporation chamber, a metal C evaporation chamber and a condensation chamber; The condensation chamber is located at the axial top of the central furnace body, and the condensation chamber is communicated with the central furnace body; the metal A evaporation chamber is communicated with the central furnace body through an overflow port A, and the diameter of the overflow port A is smaller than the inner diameter of the metal A evaporation chamber; the metal B evaporation chamber is communicated with the central furnace body through an overflow port B, and the diameter of the overflow port B is smaller than the inner diameter of the metal B evaporation chamber; the metal C evaporation chamber is communicated with the central furnace body through an overflow port C, and the diameter of the overflow port C is smaller than the inner diameter of the metal C evaporation chamber; Along the axial direction, the overflow port A is located below the overflow port B and has a distance between it and the overflow port B. The overflow port B is located below the overflow port C and has a distance between it and the overflow port C. The overflow port C is located below the condensation chamber and has a distance between it and the condensation chamber.
2. The ternary alloy preparation device according to claim 1, characterized in that: The mass percentage content of metal element B in the ternary alloy is higher than that of metal element A, and the mass percentage content of metal element A is higher than that of metal element C; the diameter of overflow port C is smaller than that of overflow port B, and the diameter of overflow port C is smaller than that of overflow port A.
3. The ternary alloy preparation device according to claim 1, characterized in that: The diameter of the steam overflow port A is 1 / 3-1 / 2 of the inner diameter of the metal A evaporation chamber; the diameter of the overflow port B is 1 / 2 of the inner diameter of the metal B evaporation chamber; the diameter of the steam overflow port C is 1 / 4-1 / 3 of the inner diameter of the metal C evaporation chamber.
4. The ternary alloy preparation device according to claim 1, characterized in that: From the axial bottom to the top, the central furnace body is divided into the bottom area, the middle area, the upper area and the top area respectively. The metal A evaporation chamber is located in the bottom area of the central furnace body, the metal B evaporation chamber is located on the side of the middle area, the metal C evaporation chamber is located on the side of the upper area, and the condensation chamber is located in the top area of the central furnace body.
5. The ternary alloy preparation device according to claim 4, characterized in that: The metal B evaporation chamber and the metal C evaporation chamber are respectively located on both sides of the central furnace body.
6. The ternary alloy preparation device according to claim 1, characterized in that: The outer walls of the central furnace body, metal A evaporation chamber, metal B evaporation chamber and metal C evaporation chamber are all made of carbon steel and the inner lining is made of refractory material, and electric heating rods are provided between the outer walls and the inner lining of the metal A evaporation chamber, metal B evaporation chamber and metal C evaporation chamber.
7. The ternary alloy preparation device according to claim 5, characterized in that: The outer wall of the condensation chamber is made of carbon steel, the inner lining is made of refractory material, and electric heating rods are provided between the outer wall and the inner lining of the condensation chamber.
8. A method for preparing a ternary alloy, characterized in that: The method adopts the device according to any one of claims 1 to 6, and the preparation method comprises: (1) Place the formulated amounts of metals A, B, and C into the corresponding evaporation chambers, and then evacuate the chamber; (2) The temperature in the evaporation chamber of metal A is heated to the evaporation temperature of metal A, and the temperature is kept at the evaporation temperature of metal A; then the temperature in the evaporation chamber of metal B is heated to the evaporation temperature of metal B, and the temperature is kept at the evaporation temperature of metal B; then the temperature in the evaporation chamber of metal C is heated to the evaporation temperature of metal C, and the temperature is kept at the evaporation temperature of metal C; during the process, the temperature in the condensation chamber is raised from room temperature to the condensation temperature and the temperature is kept at the condensation temperature, and the condensation temperature is lower than the evaporation temperature of metal C; (3) Each evaporation chamber and condensation chamber continue to keep warm; (4) Under the condition that the condensation chamber continues to be kept warm: first stop the heating and heat preservation of the evaporation chamber of metal A, then stop the heating and heat preservation of the evaporation chamber of metal B, and finally stop the heating and heat preservation of the evaporation chamber of metal C; (5) Cool the inside of the device until the temperature in the condensation chamber drops to room temperature, stop vacuuming, and collect the ternary alloy in the condensation chamber.
9. The method for preparing a ternary alloy according to claim 8, characterized in that: The vacuum condition is 1-10Pa.
10. The method for preparing a ternary alloy according to claim 8, characterized in that: Under vacuum conditions, the evaporation temperature of metal A is 300-700℃ higher than that of metal B; the evaporation temperature of metal B is 250-450℃ higher than that of metal C; and the condensation temperature is 50-100℃ lower than the evaporation temperature of metal C.
11. The method for preparing a ternary alloy according to claim 7, wherein: Also includes: The collected ternary alloy was processed under hot pressing conditions to densify its structure.
12. The method for preparing a ternary alloy according to claim 7, wherein: The metal A is aluminum, the metal B is magnesium, and the metal C is zinc; the evaporation temperature of the metal A is 1300-1500°C, the evaporation temperature of the metal B is 800-1000°C, and the evaporation temperature of the metal C is 450-550°C; after the three heatings in step (2), the temperature of the condensation chamber rises from room temperature to 400-450°C.