MBE source aluminum bar preparation device and preparation method

Abstract

The invention discloses an MBE source aluminum bar preparation device and method, and belongs to the technical field of MBE source aluminum bar manufacturing, and the MBE source aluminum bar preparation device is a solid-phase electrolysis device and comprises an electrolytic bath capable of being vacuumized, a first electrode, a second electrode, an aluminum bar and a heater; the first electrode and the second electrode are located at the two ends of the electrolytic cell, the first electrode and the second electrode partially extend into the electrolytic cell, and the aluminum bar is located between the first electrode and the second electrode; and the heater is used for heating the aluminum bar, and the heater and the electrolytic cell can be separated from each other. The MBE source aluminum bar preparation device can directionally remove the carbon element in the aluminum bar, so that the content of the carbon element is lower than 0.2 ppmw (weight million fraction), and the requirement of MBE aluminum is met.

Description

Technical Field

[0001] The present invention relates to the technical field of MBE source aluminum rod manufacturing, and specifically relates to an MBE source aluminum rod preparation device and a preparation method. Background Art

[0002] Aluminum has the chemical formula Al, is a silver-white light metal, and at room temperature, has a density of 2.70 g / cm 3 , and a melting point of 660 °C. MBE source aluminum is mainly used in molecular beam epitaxy (MBE). In MBE applications, there are strict requirements for carbon impurities in aluminum, requiring the aluminum content to not exceed 0.2 ppmw.

[0003] Currently, the main preparation methods of MBE source aluminum are zone melting or directional solidification in an atmosphere of hydrogen, inert gas, or vacuum. The disadvantages of these methods are: the charging container uses graphite material, and the carbon impurities in ultra-high purity aluminum cannot be effectively removed during the purification process.

[0004] Patent CN113416854A discloses a high-purity aluminum purification method combining vacuum distillation and zone melting. Its disadvantages are: using graphite as the condensation material, in the product collection section, the aluminum is in a molten state, which is prone to introducing carbon impurities, and the carbon removal effect of the subsequent zone melting process is poor, and it is ultimately difficult to obtain low-carbon ultra-high purity aluminum.

[0005] In view of this, the present application is proposed. Summary of the Invention

[0006] The purpose of the present invention is to overcome the deficiencies of the prior art and provide an MBE source aluminum rod preparation device and a preparation method. The MBE source aluminum rod preparation device of the present invention can directionally remove carbon elements in the aluminum rod, making the content of carbon elements lower than 0.2 ppmw (parts per million by weight), meeting the requirements of MBE aluminum.

[0007] To achieve the above purpose, the first aspect of the present application provides an MBE source aluminum rod preparation device, which is a solid-phase electrolysis device, including an evacuable electrolytic cell, a first electrode, a second electrode, an aluminum rod, and a heater;

[0008] The first electrode and the second electrode are located at both ends of the electrolytic cell, and part of the first electrode and the second electrode extends into the interior of the electrolytic cell, and the aluminum rod is located between the first electrode and the second electrode;

[0009] The heater is used to heat the aluminum rod, and the heater and the electrolytic cell are detachably arranged.

[0010] As an embodiment of the present application, both ends of the electrolytic cell are sealed by water-cooled flanges at both ends.

[0011] As an implementation solution of the present application, a vacuum interface is provided on the electrolytic cell.

[0012] As an implementation solution of the present application, the first electrode is an oxygen-free copper electrode, and the second electrode is an oxygen-free copper electrode.

[0013] The second aspect of the present application provides a method for preparing an MBE source aluminum rod. Based on the above-mentioned MBE source aluminum rod preparation device, it includes the following steps:

[0014] Place the aluminum rod between the first electrode and the second electrode;

[0015] Vacuumize;

[0016] Apply current to the first electrode and the second electrode through an external power supply;

[0017] Heat, remove one end of the aluminum rod close to the anode end, and the removed length accounts for 15-25% of the total length of the aluminum rod to obtain an MBE source aluminum rod.

[0018] As an implementation solution of the present application, the purity of the aluminum rod is 5N-7N.

[0019] As an implementation solution of the present application, vacuumize to a vacuum degree ≤ 0.001 Pa.

[0020] As an implementation solution of the present application, the current is 200-400 A.

[0021] As an implementation solution of the present application, the heating temperature is 450-630 °C.

[0022] As an implementation solution of the present application, the heating time is 100-300 h.

[0023] The beneficial effect of the present invention lies in that: the MBE source aluminum rod preparation device of the present invention can directionally remove carbon elements in the aluminum rod, so that the content of carbon elements is lower than 0.2 ppmw (parts per million by weight), meeting the requirements of MBE aluminum. Description of the Drawings

[0024] Figure 1 It is a schematic diagram of the MBE source aluminum rod preparation device of the present invention. Detailed Embodiments

[0025] To make the objectives, technical solutions, and advantages of the embodiments of the present application clearer, the technical solutions in the embodiments of the present application will be clearly and completely described below. Obviously, the described embodiments are some, but not all, of the embodiments of the present application. All other embodiments obtained by those of ordinary skill in the art based on the embodiments in the present application without creative efforts shall fall within the protection scope of the present application.

[0026] In this application, among the technical features described in an open-ended manner, it includes a closed technical solution composed of the listed features, and also includes an open technical solution containing the listed features.

[0027] In this application, regarding numerical ranges, unless otherwise specified, the above numerical ranges are considered continuous, and include the minimum and maximum values of the range, as well as each value between such minimum and maximum values. Further, when the range refers to integers, it includes each integer between the minimum and maximum values of the range. In addition, when multiple ranges are provided to describe features or characteristics, the ranges can be combined. In other words, unless otherwise specified, all ranges disclosed herein should be understood to include any and all sub-ranges subsumed therein.

[0028] In this application, there is no particular limitation on the specific dispersion and stirring treatment methods.

[0029] Unless otherwise specified, the component raw materials or instruments used in each embodiment and comparative example of the present invention are all commercially available raw materials or instruments, and the component raw materials used in each parallel experiment are of the same kind.

[0030] In addition, the terms "first" and "second" are only used for descriptive purposes and cannot be understood as indicating or implying relative importance or implicitly specifying the quantity of the indicated technical features. Thus, the features defined with "first" and "second" may explicitly or implicitly include at least one such feature. In the description of the present invention, the meaning of "a plurality" is at least two, such as two, three, etc., unless otherwise specifically defined.

[0031] As Figure 1 shown, the embodiment of this application provides an MBE source aluminum rod preparation device, which is a solid-phase electrolysis device, including an electrolytic cell 1 that can be evacuated, a first electrode 2, a second electrode 3, an aluminum rod 4, and a heater 5;

[0032] The first electrode and the second electrode are located at both ends of the electrolytic cell, and part of the first electrode and the second electrode extends into the interior of the electrolytic cell, and the aluminum rod is located between the first electrode and the second electrode;

[0033] The heater is used to heat the aluminum rod, and the heater and the electrolytic cell are separably arranged.

[0034] The MBE source aluminum rod preparation device of the present invention can directionally remove carbon elements in the aluminum rod, so that the content of carbon elements is lower than 0.2 ppmw (parts per million by weight), meeting the requirements of MBE aluminum.

[0035] As an implementation scheme of this application, both ends of the electrolytic cell are sealed by water-cooled flanges at both ends.

[0036] As an implementation scheme of the present application, a vacuum interface is provided on the electrolytic cell.

[0037] As an implementation scheme of the present application, the first electrode is an oxygen-free copper electrode, and the second electrode is an oxygen-free copper electrode. In the present invention, both the first electrode and the second electrode are oxygen-free copper electrodes, which can avoid introducing carbon impurities and other impurities.

[0038] An embodiment of the present application provides a method for preparing an MBE source aluminum rod. Based on the above-mentioned MBE source aluminum rod preparation device, the method includes the following steps:

[0039] Place the aluminum rod between the first electrode and the second electrode;

[0040] Evacuate;

[0041] Apply current to the first electrode and the second electrode through an external power supply;

[0042] Heat, and remove one end of the aluminum rod close to the anode end, and the removed length accounts for 15-25% of the total length of the aluminum rod to obtain an MBE source aluminum rod.

[0043] In the present invention, by placing the aluminum rod between two electrodes and applying current to make the current flow through the aluminum rod, under the action of specific temperature and current, carbon elements are promoted to enrich towards the anode end directionally. Finally, one end of the aluminum rod close to the anode end is removed, so as to effectively remove the carbon elements in the aluminum rod and obtain an MBE source aluminum rod that meets the requirements.

[0044] It should be noted that when connecting to the external power supply, both the first electrode and the second electrode can be connected to the positive and / or negative poles of the power supply. When the first electrode is connected to the positive pole, the first electrode is the anode; when the second electrode is connected to the positive pole, the second electrode is the anode.

[0045] In one of the embodiments, the purity of the aluminum rod is 5N-7N, for example, it can be 5N, 5.5N, 6N, 6.5N, 7N or the range composed of any two of them.

[0046] In one of the embodiments, evacuate to a vacuum degree ≤ 0.001 Pa.

[0047] In one of the embodiments, the current is 200-400 A, for example, it can be 200 A, 250 A, 300 A, 350 A, 400 A or the range composed of any two of them.

[0048] In one of the embodiments, the heating temperature is 450-630 °C, for example, it can be 450 °C, 500 °C, 550 °C, 600 °C, 630 °C or the range composed of any two of them.

[0049] In one of the embodiments, the heating time is 100 to 300 h, and for example, it can be 100 h, 120 h, 150 h, 180 h, 200 h, 250 h, 300 h, or the range composed of any two of them.

[0050] The following examples are provided to facilitate the understanding of the present invention. These examples are provided not to limit the scope of the claims.

[0051] Example 1

[0052] An MBE source aluminum rod preparation device, which is a solid-phase electrolysis device, includes an electrolytic cell 1 that can be evacuated, a first oxygen-free copper electrode 2, a second oxygen-free copper electrode 2, an aluminum rod 4, and a heater 5;

[0053] The first electrode and the second electrode are located at both ends of the electrolytic cell, and part of the first electrode and the second electrode extends into the interior of the electrolytic cell, and the aluminum rod is located between the first electrode and the second electrode;

[0054] The heater is used to heat the aluminum rod, and the heater and the electrolytic cell are detachably arranged.

[0055] Both ends of the electrolytic cell are sealed by water-cooled flanges 6 at both ends.

[0056] A vacuum interface 7 is provided on the electrolytic cell.

[0057] Example 2

[0058] An MBE source aluminum rod preparation method, based on the MBE source aluminum rod preparation device described in Example 1, includes the following steps:

[0059] (1) Place a 6N5 purity aluminum rod (carbon content is 2.1 ppmw) with a length of 20 cm and a diameter of 10 mm between the first oxygen-free copper electrode and the second oxygen-free copper electrode;

[0060] (2) Evacuate to a vacuum degree of 0.001 Pa;

[0061] (3) Apply a current of 200 A to the first oxygen-free copper electrode and the second oxygen-free copper electrode through an external power supply; where the positive pole of the external power supply is connected to the first oxygen-free copper electrode (which is the anode);

[0062] (4) Heat to 500 °C through the heater and maintain for 280 h;

[0063] (5) Take out the aluminum rod, remove one end of the aluminum rod close to the anode end, and the removed length is 4 cm to obtain an MBE source aluminum rod.

[0064] Example 3

[0065] A method for preparing an MBE source aluminum rod, based on the MBE source aluminum rod preparation device described in Example 1, includes the following steps:

[0066] (1) Place a 6N5 purity aluminum rod with a length of 20 cm and a diameter of 10 mm (carbon content is 2.1 ppmw) between the first oxygen-free copper electrode and the second oxygen-free copper electrode;

[0067] (2) Evacuate to a vacuum degree of 0.001 Pa;

[0068] (3) Apply a current of 400 A to the first oxygen-free copper electrode and the second oxygen-free copper electrode through an external power supply; the positive pole of the external power supply is connected to the first oxygen-free copper electrode (which is the anode);

[0069] (4) Heat to 600 °C through a heater and maintain for 120 h;

[0070] (5) Take out the aluminum rod and remove one end of the aluminum rod close to the anode end, with a removal length of 4 cm, to obtain the MBE source aluminum rod.

[0071] Example 4

[0072] A method for preparing an MBE source aluminum rod, based on the MBE source aluminum rod preparation device described in Example 1, includes the following steps:

[0073] (1) Place a 6N5 purity aluminum rod with a length of 20 cm and a diameter of 10 mm (carbon content is 2.1 ppmw) between the first oxygen-free copper electrode and the second oxygen-free copper electrode;

[0074] (2) Evacuate to a vacuum degree of 0.001 Pa;

[0075] (3) Apply a current of 300 A to the first oxygen-free copper electrode and the second oxygen-free copper electrode through an external power supply; the positive pole of the external power supply is connected to the first oxygen-free copper electrode (which is the anode);

[0076] (4) Heat to 550 °C through a heater and maintain for 200 h;

[0077] (5) Take out the aluminum rod and remove one end of the aluminum rod close to the anode end, with a removal length of 4 cm, to obtain the MBE source aluminum rod.

[0078] Comparative Example 1

[0079] A method for preparing an MBE source aluminum rod, based on the MBE source aluminum rod preparation device described in Example 1, includes the following steps:

[0080] (1) Place a 6N5 purity aluminum rod with a length of 20 cm and a diameter of 10 mm (carbon content is 2.1 ppmw) between the first oxygen-free copper electrode and the second oxygen-free copper electrode;

[0081] (2) Evacuate to a vacuum degree of 0.001 Pa;

[0082] (3) Apply a current of 100 A to the first oxygen-free copper electrode and the second oxygen-free copper electrode through an external power supply; the positive pole of the external power supply is connected to the first oxygen-free copper electrode (which is the anode);

[0083] (4) Heat to 550 °C through a heater and maintain for 200 h;

[0084] (5) Take out the aluminum rod, remove one end of the aluminum rod close to the anode end, and the removal length is 4 cm to obtain the MBE source aluminum rod.

[0085] Comparative Example 2

[0086] A method for preparing an MBE source aluminum rod, based on the MBE source aluminum rod preparation device described in Example 1, includes the following steps:

[0087] (1) Place a 6N5 purity aluminum rod (carbon content is 2.1 ppmw) with a length of 20 cm and a diameter of 10 mm between the first oxygen-free copper electrode and the second oxygen-free copper electrode;

[0088] (2) Evacuate to a vacuum degree of 0.001 Pa;

[0089] (3) Apply a current of 500 A to the first oxygen-free copper electrode and the second oxygen-free copper electrode through an external power supply; the positive pole of the external power supply is connected to the first oxygen-free copper electrode (which is the anode);

[0090] (4) Heat to 550 °C through a heater and maintain for 200 h;

[0091] (5) Take out the aluminum rod, remove one end of the aluminum rod close to the anode end, and the removal length is 4 cm to obtain the MBE source aluminum rod.

[0092] Comparative Example 3

[0093] A method for preparing an MBE source aluminum rod, based on the MBE source aluminum rod preparation device described in Example 1, includes the following steps:

[0094] (1) Place a 6N5 purity aluminum rod (carbon content is 2.1 ppmw) with a length of 20 cm and a diameter of 10 mm between the first oxygen-free copper electrode and the second oxygen-free copper electrode;

[0095] (2) Evacuate to a vacuum degree of 0.001 Pa;

[0096] (3) Apply a current of 300 A to the first oxygen-free copper electrode and the second oxygen-free copper electrode through an external power supply; the positive pole of the external power supply is connected to the first oxygen-free copper electrode (which is the anode);

[0097] (4) Heat it to 650 °C through a heater and maintain for 200 h;

[0098] (5) Take out the aluminum rod, remove one end of the aluminum rod close to the positive electrode end, with a removal length of 4 cm, to obtain the MBE source aluminum rod.

[0099] Comparative Example 4

[0100] A method for preparing an MBE source aluminum rod, based on the MBE source aluminum rod preparation device described in Example 1, includes the following steps:

[0101] (1) Place a 6N5 purity aluminum rod (with a carbon content of 2.1 ppmw) with a length of 20 cm and a diameter of 10 mm between the first oxygen-free copper electrode and the second oxygen-free copper electrode;

[0102] (2) Evacuate to a vacuum degree of 0.001 Pa;

[0103] (3) Apply a current of 300 A to the first oxygen-free copper electrode and the second oxygen-free copper electrode through an external power supply; where the positive electrode of the external power supply is connected to the first oxygen-free copper electrode (which is the anode);

[0104] (4) Heat it to 360 °C through a heater and maintain for 200 h;

[0105] (5) Take out the aluminum rod, remove one end of the aluminum rod close to the positive electrode end, with a removal length of 4 cm, to obtain the MBE source aluminum rod.

[0106] Among them, the carbon content in the aluminum rods of Examples 2-4 and Comparative Examples 1-4 is shown in Table 1.

[0107] Table 1

[0108]

[0109]

[0110] It can be seen from Table 1 that the MBE source aluminum rod preparation device described in the present invention can directionally remove carbon elements in the aluminum rod, making the carbon element content lower than 0.2 ppmw (parts per million by weight), meeting the requirements of MBE aluminum.

[0111] Comparing Example 1 with Comparative Examples 1-2, it can be seen that the current is the key parameter of the present invention. Controlling the current to be 200-400 A effectively reduces the carbon element in the aluminum rod. When the current deviates from the range of the present invention, the carbon element cannot be removed.

[0112] Comparing Example 1 with Comparative Examples 3 to 4, it can be seen that the heating temperature is a key parameter of the present invention. The heating temperature is 450 to 630 °C, which effectively reduces the carbon element in the aluminum rod. When the heating temperature deviates from the scope of the present invention, the carbon element cannot be removed.

[0113] Finally, it should be noted that the above embodiments are only used to illustrate the technical solutions of the present invention rather than to limit the protection scope of the present invention. Although the present invention has been described in detail with reference to the preferred embodiments, those of ordinary skill in the art should understand that the technical solutions of the present invention can be modified or equivalently replaced without departing from the essence and scope of the technical solutions of the present invention.

Claims

1. An MBE source aluminum rod preparation device, which is a solid phase electrolysis device, characterized in that: The invention comprises a vacuum electrolytic cell, a first electrode, a second electrode, an aluminum rod and a heater; The first electrode and the second electrode are located at two ends of the electrolytic cell, and parts of the first electrode and the second electrode extend into the interior of the electrolytic cell, and the aluminum rod is located between the first electrode and the second electrode; The heater is used to heat the aluminum rod, and the heater and the electrolytic cell can be arranged separately from each other.

2. The MBE source aluminum rod preparation device according to claim 1, characterized in that: Both ends of the electrolytic cell are sealed by water-cooling flanges at both ends.

3. The MBE source aluminum rod preparation device according to claim 1, characterized in that: The electrolytic cell is provided with a vacuum interface.

4. The MBE source aluminum rod preparation device according to claim 1, characterized in that: The first electrode is an oxygen-free copper electrode, and the second electrode is an oxygen-free copper electrode.

5. A method for preparing an MBE source aluminum rod, characterized in that: The MBE source aluminum rod preparation device according to any one of claims 1 to 4 comprises the following steps: placing an aluminum rod between the first electrode and the second electrode; Vacuuming; Applying current to the first electrode and the second electrode through an external power supply; The aluminum rod is heated and one end close to the anode end is removed, wherein the removed length accounts for 15-25% of the total length of the aluminum rod, thereby obtaining an MBE source aluminum rod.

6. The method for preparing an MBE source aluminum rod according to claim 5, characterized in that: The purity of the aluminum rod is 5N-7N.

7. The method for preparing an MBE source aluminum rod according to claim 5, characterized in that: Evacuate to a vacuum degree of ≤0.001Pa.

8. The method for preparing an MBE source aluminum rod according to claim 5, characterized in that: The current is 200-400A.

9. The method for preparing an MBE source aluminum rod according to claim 5, characterized in that: The heating temperature is 450-630°C.

10. The method for preparing an MBE source aluminum rod according to claim 5, characterized in that: The heating time is 100 to 300 hours.

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