Gram-scale rare earth metal atomization device, evaporation module and use method
By designing a split modular rare earth metal atomization device, using cover plates with different shapes and multi-layer thermal shielding layers, the problems of poor atomic beam divergence and poor thermal stability of the rare earth metal atomization device at high temperatures are solved, and efficient and stable rare earth metal evaporation is achieved.
Patent Information
- Application Number
- CN202510328241.7
- Authority / Receiving Office
- CN · China
- Patent Type
- Applications(China)
- Current Assignee / Owner
- Filing Date
- 2025-03-19
- Publication Date
- 2025-08-01
AI Technical Summary
The existing rare earth metal atomization device has poor atomic beam divergence at high temperatures, which is difficult to meet the purification or separation requirements. The high-power heating device has poor thermal stability, and the low-power heating device cannot continuously evaporate for a long time, which is relatively expensive.
A rare earth metal atomization device in the order of gram was designed, including a cover plate group, atomized crucible group and heating wire. It adopts a split modular structure. It uses cover plates of different shapes to match atomized crucible group with different evaporation areas. It combines 4 layers of heat shielding layers and water-cooled copper tubes to ensure heating uniformity and thermal stability. The evaporation rate is controlled through step-by-step heating calibration power.
The high temperature and high rate of rare earth metals are achieved for a long period of stable evaporation, which improves material utilization, reduces costs, and ensures the uniformity and thermal stability of atomic beam flow, meeting the needs of purification or separation.
Smart Images
Figure CN120393445A_ABST
Abstract
Description
Technical Field
[0001] The present invention relates to the technical field of metal evaporation and vacuum resistance heating, and in particular to a gram-scale rare earth metal atomization device, an evaporation module and a usage method thereof. Background Art
[0002] Rare earth metals and their high-abundance isotopes have extensive applications in many fields. There is an endless stream of research on the purification of rare earth metals and their advanced separation methods. In these studies, there is a physical process of converting solid metals into metal atomic beams. Therefore, it is of great significance to develop a rare earth metal atomization device. However, most rare earth metals have high melting points and are difficult to evaporate, and there is a certain requirement for the heating temperature (>1400°C) level that can be achieved by the atomization device. In addition, the raw material cost of rare earth metals is relatively high, and the issue of material utilization rate needs to be additionally concerned. At present, high-power heating devices can achieve the stable evaporation of rare earth metals, but the divergence of atomic beams at high temperatures is poor, and it is not easy to meet the subsequent purification or separation requirements. Low-power resistance heating devices have poor thermal stability and cannot perform long-term continuous evaporation. Summary of the Invention
[0003] The purpose of the present invention is to provide an evaporation module for a gram-scale rare earth metal atomization device in view of the technical defects existing in the prior art.
[0004] Another purpose of the present invention is to provide the above-mentioned gram-scale rare earth metal atomization device.
[0005] Another purpose of the present invention is to provide a usage method for the above-mentioned gram-scale rare earth metal atomization device.
[0006] The technical solution adopted to achieve the purpose of the present invention is as follows:
[0007] An evaporation module for a gram-scale rare earth metal atomization device, comprising a cover plate group, an atomization crucible group and heating wires. The cover plate group includes two cover plates provided with mounting holes. The atomization crucible group is vertically installed through the mounting holes on one cover plate and has an opening facing outward. The shapes of the mounting holes on the two cover plates are different and are used to match atomization crucible groups with different evaporation areas. The cover plates cover the device body of the rare earth metal atomization device. The heating wires are wound around the atomization crucible group to form a heating area for uniformly heating the atomization crucible group. The atomization crucible group is used to contain rare earth metals.
[0008] In the above technical solution, the two ends of the heating wire pass through the cover plate and the insulating suspension ring from bottom to top and are respectively connected to the electrodes installed on an electrode base. Each electrode base is connected to an electrode flange arranged in the vacuum cavity through an electrode wire. The electrode flange is connected to an external power supply. The electrode base is installed on the outer surface of the top of the device body through an insulating ceramic gasket, and is located on both sides above the cover plate.
[0009] In the above technical solution, the atomization crucible group is a boat-shaped material tube or a single-row material tube, and the single-row material tube includes a plurality of material tubes arranged at intervals in sequence.
[0010] Another aspect of the present invention further includes a gram-scale rare earth metal atomization device, including the evaporation module, the heat preservation module and the device body described above. The evaporation module is covered on the device body through a cover plate. The heat preservation module includes a heat shield container and a heat preservation cover plate. The atomization crucible group and the heating wire located below the cover plate are arranged in the heat shield container. The heat shield container is installed in the device body. The heat preservation cover plate is covered on the cover plate. After the rare earth metal in the atomization crucible group is heated and evaporated, the atomic beam deposits on the heat preservation cover plate.
[0011] In the above technical solution, the heat shield container is lapped on the support structure, and the support structure is installed on the device body.
[0012] In the above technical solution, the container wall of the heat shield container is 4 layers of heat shield layers arranged at intervals, and the inner and outer surfaces of each layer of heat shield layer are polished.
[0013] In the above technical solution, the 4 layers of heat shield layers arranged at intervals include 3 layers of tungsten metal heat shield layers arranged inside and a layer of ceramic heat shield layer wrapped outside.
[0014] In the above technical solution, the heat preservation cover plate includes two baffle plates arranged at intervals and a current limiting baffle located between the two baffle plates. The current limiting baffle is aligned with the cover plate up and down to restrict the atomic beam evaporated from the outlet of the atomization crucible group.
[0015] In the above technical solution, each baffle plate is a multi-layer metal baffle plate arranged at intervals.
[0016] In the above technical solution, a water-cooled copper tube is wound around the outer surface of the device body by vacuum brazing.
[0017] Another aspect of the present invention further includes a method for using the gram-scale rare earth metal atomization device described above, including the following steps:
[0018] Step 1, Power Calibration: Load rare earth metal into a certain tube of the single-row feeder tubes in the atomization crucible group. The external power supply supplies power to the heating wire, and stepwise heating is adopted to heat the tube filled with rare earth metal. During the heating process, the temperature around the heating wire is measured by a thermocouple, and the metal evaporation rate at the outlet of the tube is measured by a film thickness gauge probe. Record the evaporation rate at different heating powers, determine the change of the metal evaporation rate in the tube, and calibrate the power of a single tube to reduce the usage amount of metal materials while obtaining its evaporation characteristic parameters, greatly saving the experimental cost;
[0019] Step 2, Control of the Divergence of the Evaporation Beam of the Single-Row Feeder Tube: After power calibration, add the rare earth metal from Step 1 into all the tubes of the single-row feeder tube, and adopt the method in Step 1 for stepwise heating to carry out metal evaporation, so as to multiply the evaporation rate, and record the mass of each tube before and after the experiment, and calculate its average evaporation rate through the difference value. Confirm the heating uniformity in the heating area of the heating wire by comparing the evaporation parameters between the tubes.
[0020] Step 3, Long-Time High-Speed Evaporation of the Boat-Shaped Tube: After the heating uniformity is confirmed, replace the single-row feeder tube with a boat-shaped tube to expand the evaporation area and increase the metal evaporation rate. Adjust the heating power of the heating wire and monitor the temperature change situation to make parameters such as the metal evaporation rate and evaporation amount meet the actual requirements, and carry out long-time high-speed evaporation while ensuring the thermal stability of the whole device, and finally obtain an evaporation beam that meets the requirements.
[0021] Compared with the prior art, the beneficial effects of the present invention are as follows:
[0022] 1. By using a cover plate provided with mounting holes of different shapes, the present invention can match feeder tubes with different arrangement modes for experiments, realize the high-temperature, high-speed and long-time stable evaporation of rare earth metals, obtain the target beam while ensuring the material utilization rate, and save costs.
[0023] 2. The overall size of the rare earth metal atomization device of the present invention is relatively small. Under the action of the water-cooled copper tubes wound around the device body, the thermal stability of the device is effectively guaranteed. Metal evaporation can be realized by connecting the heating wire to the external power supply for power-on heating, and the operation is simple and convenient. The rare earth metal atomization device can realize stable heating above 1600°C. Taking the evaporation experiment result of gadolinium metal as an example, the average evaporation rate ≥ 1 g / h at a heating power of 3170 W, and the atomic density in the beam ≥ 1×1011 cm -3 , realizing the evaporation of refractory rare earth metals in gram scale.
[0024] 3. The rare earth metal atomization device of the present invention adopts a split-type modular design. The atomization crucible group, heating wire, insulation module, device body, and cover plate can all be installed and maintained independently, significantly improving operability while reducing unnecessary waste generation. BRIEF DESCRIPTION OF THE DRAWINGS
[0025] Figure 1 It is a structural diagram of the cover plate, atomization crucible group, and heating wire of the present invention;
[0026] Figure 2 It is a schematic diagram of two replaceable material tubes and the cover plate of the present invention;
[0027] Figure 3 It is a sectional view of the atomization crucible group of the present invention;
[0028] Figure 4 It is a structural diagram of the heat insulation cover plate of the present invention;
[0029] Figure 5 It is a schematic diagram of the external structure of the present invention.
[0030] Among them, 1: atomization crucible group, 2: cover plate, 3: heating wire, 4: insulating suspension ring, 5: thermal shielding container, 6: support structure, 7: device body, 8: water-cooled copper tube, 9: heat insulation cover plate, 10: current-limiting baffle, 11: electrode base, 12: insulating ceramic gasket, 13: electrode wire, 14: single-row material tube, 15: boat-shaped material tube. DETAILED DESCRIPTION OF THE EMBODIMENTS
[0031] The present invention will be further described in detail below in conjunction with specific embodiments. It should be understood that the specific embodiments described herein are only used to explain the present invention and are not used to limit the present invention.
[0032] Embodiment 1
[0033] As Figures 1-2 shown, an evaporation module of a gram-scale rare earth metal atomization device includes a cover plate group, an atomization crucible group 1, and a heating wire 3. The cover plate group includes two cover plates 2 provided with mounting holes. The two cover plates 2 are used alternately to cover the device body 7 of the rare earth metal atomization device. The shapes of the mounting holes on the two cover plates 2 are different and are used to match the atomization crucible group 1 with different evaporation areas. The atomization crucible group 1 is vertically inserted through a mounting hole on one cover plate 2 and has an opening facing outward. The heating wire 3 is wound around the atomization crucible group 1 to form a heating area for uniformly heating the atomization crucible group 1. The atomization crucible group 1 is used to contain rare earth metal, and the heating wire 3 is used to heat the rare earth metal in the atomization crucible group 1. The atomization crucible group 1 is two replaceable material tube groups with different evaporation port areas. By replacing different cover plates 2, the two material tubes can be inserted.
[0034] Further, after the heating wire 3 winds around the atomization crucible group 1, its two ends pass through the cover plate 2 and the insulating suspension ring 4 from bottom to top and are respectively connected to the electrodes installed on an electrode base 11. Each electrode base 11 is connected to an electrode flange arranged in a vacuum chamber (the gram-scale rare earth metal atomization device in this embodiment needs to be placed and used in a vacuum environment) through an electrode wire 13. The electrode flange is connected to an external power supply. The electrode base 11 is installed on the outer surface of the top of the device body 7 through an insulating ceramic gasket 12. The insulating suspension ring 4 is provided to achieve insulation between the heating wire 3 and the cover plate 2, improve the deformation condition of the heating wire 3, and enhance the thermal stability of the entire device. Specifically, the heating wire 3 is a tungsten metal fine wire with a diameter of 2 mm and a length of about 600 mm, and is energized by being connected to the electrodes through copper wires.
[0035] Further, the two material tube groups are respectively a boat-shaped material tube 15 and a single-row material tube 14. The single-row material tube 14 includes a plurality of material tubes arranged at intervals in sequence along the length direction of the cover plate 2. Arranging a plurality of material tubes in sequence can, on the one hand, multiply the evaporation rate, and on the other hand, record the mass of each material tube before and after the experiment, and calculate its average evaporation rate through the difference value. The heating uniformity in the heating body wrapping area is confirmed by comparing the evaporation parameters between the material tubes. Compared with the boat-shaped material tube 15, the number of collisions between the metal atoms ejected from the outlet of each material tube in the single-row material tube and the metal atoms evaporated from the adjacent material tubes is less, and the overall divergence of the beam current is better than that of the boat-shaped material tube 15 under the same power. When the boat-shaped material tube 15 replaces the single-row material tube 14, the evaporation area can be expanded, and the metal evaporation rate can be further increased. The boat-shaped material tube 15 directly faces the actual requirements of metal evaporation. To meet the parameter requirements such as the metal evaporation rate and evaporation volume, the heating power is adjusted and the temperature change of the key parts is monitored, and long-term high-rate evaporation is carried out while ensuring thermal stability, and finally an evaporation beam current that meets the requirements is obtained.
[0036] Further, the size of each material tube of the single-row material tube is about φ5×55 mm. By fusion welding of standard tungsten tubes, it is ensured that there are no gaps and no leakage at the bottom of the material tube. Relying on the high melting point and corrosion resistance of tungsten metal, the metal material tube can maintain a stable state during the continuous high-temperature evaporation process.
[0037] Embodiment 2
[0038] As Figures 3-5As shown in the figure, this embodiment provides a gram-scale rare earth metal atomization device described in Embodiment 1, including the evaporation module, heat preservation module, and device body 7 described in Embodiment 1. The evaporation module is covered on the device body 7 through a cover plate 2. The heat preservation module includes a heat shield container 5 and a heat preservation cover plate 9. The atomization crucible group 1 and heating wire 3 located below the cover plate 2 are arranged in the heat shield container 5. The heat shield container 5 is installed in the device body 7. The heat preservation cover plate 9 covers the cover plate 2. After the rare earth metal in the atomization crucible group 1 is heated and evaporated, the atomic beam deposits on the heat preservation cover plate 9.
[0039] Furthermore, the heat shield container 5 is lapped on a support structure 6. The support structure 6 is installed on the device body 7 through screws. The container wall of the heat shield container 5 is 4 layers of heat shield layers arranged at intervals. The inner and outer surfaces of each layer of heat shield layer are polished to reduce the surface roughness, increase the number of specular reflections, and effectively reduce the heat dissipation in the heating area. The heat shield layers are arranged at intervals so that the heat escaping upward from the outlet of the atomization crucible group 1 is reflected between the heat shield layers, and part of the heat can flow back into the heat shield container 5, which can not only improve the heating efficiency but also reduce the cavity temperature and extend the evaporation time of rare earth metals. Furthermore, the 4 layers of heat shield layers arranged at intervals include 3 layers of tungsten metal heat shield layers arranged inside and a layer of ceramic heat shield layer wrapped outside.
[0040] Furthermore, the heat preservation cover plate 9 includes two baffle plates arranged at intervals and a flow-limiting baffle 10 located between the two baffle plates. The flow-limiting baffle 10 is aligned with the cover plate 2 up and down to restrict the atomic beam evaporated from the outlet of the atomization crucible group 1 to obtain an ideal beam shape. Each baffle plate is a multi-layer metal baffle arranged at intervals so that the heat radiating upward is reflected multiple times between the multi-layer metal baffles, thereby reducing the radiative heat transfer to the external environment.
[0041] Furthermore, a water-cooled copper tube 8 is wound around the outer surface of the device body 7 by vacuum brazing to further reduce the radiative heat transfer to the external environment.
[0042] Furthermore, a film thickness gauge probe is arranged at the outlet of the atomization crucible group 1 to measure the metal evaporation rate, record the evaporation rate under different heating powers, and determine the change of the evaporation rate of a certain metal.
[0043] Embodiment 3
[0044] This embodiment provides a method for using the gram-scale rare earth metal atomization device described in Embodiment 2, including the following steps:
[0045] Step 1, Power Calibration: A single-row material tube 14 in the atomization crucible group 1 is installed on a matching cover plate 2, and the cover plate 2 covers the device body. Rare earth metal is loaded into a certain material tube. The external power supply supplies power to the heating wire 3, and stepwise heating is adopted to heat the material tube containing rare earth metal. During the heating process, the temperature around the heating wire 3 is measured by a thermocouple, and the metal evaporation rate at the outlet of the material tube is measured by a film thickness gauge probe. The evaporation rate at different heating powers is recorded to determine the change in the evaporation rate of the metal in the material tube, and power calibration is performed on a single material tube to reduce the usage amount of metal materials while obtaining its evaporation characteristic parameters, greatly saving the experimental cost;
[0046] Step 2, Control of the Divergence of the Evaporation Beam of the Single-Row Material Tube 14: After power calibration, the rare earth metal from Step 1 is added to all the material tubes of the single-row material tube 14, and stepwise heating is carried out in the same way as in Step 1 for metal evaporation to multiply the evaporation rate, and the mass of each material tube before and after the experiment is recorded, and its average evaporation rate is calculated by the difference. The heating uniformity in the heating area of the heating wire 3 is confirmed by comparing the evaporation parameters between the material tubes.
[0047] Step 3, Long-Time High-Rate Evaporation of the Boat-Shaped Material Tube 15: After the heating uniformity is confirmed, the single-row material tube 14 is replaced with the boat-shaped material tube 15 to expand the evaporation area and increase the metal evaporation rate, and the cover plate 2 matching the boat-shaped material tube is replaced. The heating power of the heating wire 3 is adjusted and the temperature change is monitored to make parameters such as the metal evaporation rate and evaporation amount meet the actual requirements, and long-time high-rate evaporation is carried out while ensuring the thermal stability of the entire device, and finally an evaporation beam meeting the requirements is obtained.
[0048] It should be noted that the gram-scale rare earth metal atomization device in this embodiment needs to be placed in a high-vacuum environment (vacuum container) for operation.
[0049] The above are only the preferred embodiments of the present invention. It should be pointed out that for those of ordinary skill in the art, without departing from the principle of the present invention, several improvements and refinements can be made, and these improvements and refinements should also be regarded as the protection scope of the present invention.
Claims
1. An evaporation module of a gram-scale rare earth metal atomization device, characterized in that It includes a cover plate group, an atomization crucible group and heating wires. The cover plate group includes two cover plates provided with mounting holes. The atomization crucible group is vertically installed on one cover plate through the mounting holes. The shapes of the mounting holes on the two cover plates are different and are used to match atomization crucible groups with different evaporation areas. One of the cover plates covers the device body of the rare earth metal atomization device. The heating wires surround the atomization crucible group to form a heating area for uniformly heating the atomization crucible group. The atomization crucible group is used to hold rare earth metals.
2. The evaporation module of the gram-scale rare earth metal atomization device according to claim 1, characterized in that, The two ends of the heating wires pass through the cover plate and the insulating hanging rings from bottom to top and are respectively connected to electrodes installed on an electrode base. Each electrode base is connected to an electrode flange arranged in a vacuum cavity through an electrode wire. The electrode flange is connected to an external power supply. The electrode base is installed on the outer surface of the top of the device body through an insulating ceramic gasket and is located on both sides above the cover plate.
3. The evaporation module of the gram-scale rare earth metal atomization device according to claim 1, characterized in that, The atomization crucible group is a boat-shaped material tube or a single-row material tube. The single-row material tube includes a plurality of material tubes arranged at intervals in sequence.
4. A gram-scale rare earth metal atomization device, characterized in that, It includes the evaporation module, the heat preservation module, the device body and the cover plate covering the device body according to any one of claims 1 to 3. The heat preservation module includes a heat shield container and a heat preservation cover plate. The atomization crucible group and the heating wires located below the cover plate are arranged in the heat shield container. The heat shield container is installed in the device body. The heat preservation cover plate covers the cover plate. After the rare earth metal in the atomization crucible group is heated and evaporated, the atomic beam deposits on the heat preservation cover plate.
5. The gram-scale rare earth metal atomization device according to claim 4, wherein The heat shield container is lapped on a support structure, and the support structure is installed on the device body.
6. The gram-scale rare earth metal atomization device according to claim 4, characterized in that, The container wall of the heat shield container is 4 layers of heat shield layers arranged at intervals, and the inner and outer surfaces of each layer of heat shield layer are polished.
7. The gram-scale rare earth metal atomization device according to claim 4, wherein The 4 layers of heat shield layers arranged at intervals include 3 layers of tungsten metal heat shield layers arranged inside and one layer of ceramic heat shield layer wrapped outside.
8. The gram-scale rare earth metal atomization device according to claim 4, characterized in that, The heat preservation cover plate includes two baffle plates arranged at intervals and a current-limiting baffle located between the two baffle plates. The current-limiting baffle is aligned with the cover plate up and down to restrict the atomic beam evaporated from the outlet of the atomization crucible group.
9. The gram-scale rare earth metal atomization device according to claim 4, characterized in that, Each baffle plate is a multi-layer metal baffle arranged at intervals.
10. The gram-scale rare earth metal atomization device according to claim 4, wherein, Water-cooled copper tubes are wound around the outer surface of the device body by vacuum brazing.
11. The method of using the gram-scale rare earth metal atomization device according to any one of claims 4 to 10, characterized in that, It includes the following steps: Step 1, power calibration: The single-row material tube in the atomization crucible group is installed on a cover plate that matches it. The cover plate covers the device body. Rare earth metal is loaded into a certain material tube. The external power supply supplies power to the heating wires and uses a stepped temperature increase to heat the material tube containing the rare earth metal. During the heating process, the temperature around the heating wires is measured by a thermocouple, and the metal evaporation rate at the outlet of the material tube is measured by a film thickness gauge probe. The evaporation rate values under different heating powers are recorded to determine the change in the evaporation rate of the metal in the material tube, and power calibration is performed on a single material tube to reduce the usage amount of metal materials and obtain its evaporation characteristic parameters at the same time; Step 2, Control of the divergence of the evaporation beam of the single-row material tube: After power calibration, add the rare earth metal from Step 1 to all the material tubes of the single-row material tube, and perform stepwise heating in the manner of Step 1 to carry out metal evaporation, so as to multiply the evaporation rate, and record the mass of each material tube before and after the experiment, and calculate its average evaporation rate through the difference value. Confirm the heating uniformity in the heating area of the heating wire by comparing the evaporation parameters between the material tubes; Step 3, High-rate evaporation of the boat-shaped material tube for a long time: After the heating uniformity is confirmed, replace the single-row material tube with a boat-shaped material tube to expand the evaporation area and increase the metal evaporation rate, and replace it with a cover plate matching the boat-shaped material tube, adjust the heating power of the heating wire and monitor the temperature change, so that the metal evaporation rate and evaporation amount meet the actual requirements, and perform high-rate evaporation while ensuring the thermal stability of the entire device, and finally obtain an evaporation beam meeting the requirements.