Preparation device of intermediate alloy

Abstract

The utility model relates to the technical field of intermediate alloy preparation, in particular to an intermediate alloy preparation device. Comprising a vacuum chamber, a smelting container, a heating mechanism, a rotating mechanism, an ultrasonic vibration mechanism and a cooling mechanism, the smelting container is used for containing raw materials for preparing the intermediate alloy, the bottom face is a plane, and protective atmosphere can be introduced into the smelting container. The heating mechanism is used for heating the metal raw materials to form molten metal; the rotating mechanism is in driving connection with the smelting container, so that the smelting container can rotate; the ultrasonic vibration mechanism is connected with the smelting container and used for applying ultrasonic vibration to the molten metal in the smelting container; the cooling mechanism is arranged below the smelting container in a lifting mode and used for cooling the bottom face of the smelting container. The device can provide inner and outer double-layer protection environments during metal smelting, and is also provided with a rotating mechanism and an ultrasonic vibration mechanism, so that the oxygen content in an alloy can be effectively reduced, and the uniformity of each part of the intermediate alloy is improved.

Description

Technical Field

[0001] This utility model relates to the field of intermediate alloy preparation technology, and more specifically, to an apparatus for preparing intermediate alloys. Background Technology

[0002] Master alloys can be used in the preparation of bonding wires and as contact materials for various switches, controllers, circuit breakers, etc. The properties of master alloys have a significant impact on the product. Adding master alloys during the melting and smelting of bonding wires allows for the precise addition of dopant or alloying elements. The characteristics of master alloys are: small weight per batch; high-purity preparation, preventing the introduction of impurities; and high material homogeneity requirements, with minimal compositional error across different parts. This necessitates thorough mixing of all parts and a uniform microstructure to avoid component segregation and uneven element distribution.

[0003] Currently, the preparation equipment for master alloys is typically a vacuum induction melting furnace. In this process, dopant elements and main elements are mixed according to their weight ratios and added to the furnace. Under vacuum or inert gas protection, the mixture is heated above the alloy's melting point, maintained for a period of time, and then cooled to room temperature before the ingot is removed. Traditional vacuum induction melting furnaces have only a single layer of protection, resulting in master alloys with high oxygen content and low cleanliness. Furthermore, the lack of effective homogenization devices leads to uneven composition and significant errors in compositional accuracy across different parts of the resulting master alloy.

[0004] In view of the above, this utility model is hereby proposed. Utility Model Content

[0005] The purpose of this invention is to provide a preparation apparatus for intermediate alloys, so as to solve the technical problems of low cleanliness and uneven composition of intermediate alloys prepared by existing apparatuses.

[0006] In order to achieve the above-mentioned objectives of this utility model, the following technical solution is adopted:

[0007] An apparatus for preparing an intermediate alloy includes a vacuum chamber and a melting vessel, a heating mechanism, a rotating mechanism, an ultrasonic vibration mechanism, and a cooling mechanism located within the vacuum chamber.

[0008] The melting vessel is used to hold the raw materials required for the preparation of the intermediate alloy. The bottom surface of the melting vessel is flat, and a protective atmosphere can be introduced into the interior of the melting vessel.

[0009] The heating mechanism is used to heat the raw materials in the melting vessel to form molten metal;

[0010] The rotating mechanism is driven to the melting container so that the melting container can rotate.

[0011] The ultrasonic vibration mechanism is connected to the smelting container and is used to apply ultrasonic vibration to the molten metal in the smelting container.

[0012] The cooling mechanism is vertically and vertically positioned below the melting vessel to cool the bottom surface of the melting vessel, so that the molten metal inside the melting vessel solidifies in the form of columnar crystals to form the intermediate alloy.

[0013] Preferably, the ultrasonic vibration mechanism includes an ultrasonic vibration table with an ultrasonic generator, the rotating mechanism is mounted on the ultrasonic vibration table, one end of the melting container is connected to the rotating mechanism, and the other end of the melting container is connected to a vacuum system and an inert gas source through a rotating seal.

[0014] Preferably, the heating mechanism includes an induction coil located outside the melting container, and the induction coil is controlled by an induction power supply.

[0015] Preferably, the cooling mechanism includes a cooling pool and a lift disposed at the bottom of the cooling pool, the cooling pool being used to contain a cooling medium.

[0016] Preferably, the cooling medium is a liquid medium, and the cooling pool is connected to the inlet and outlet of the cooling machine through a pipeline.

[0017] Preferably, a temperature sensor is provided inside the melting container.

[0018] Preferably, the melting container is a quartz tube, including a quartz tube body and inlet pipes located at both ends of the quartz tube body. The two inlet pipes are coaxially arranged with the quartz tube body. One of the inlet pipes is connected to the vacuum system and the inert gas source through the rotating seal, and the other inlet pipe is connected to the rotating mechanism through the seal.

[0019] Preferably, the vacuum system includes a vacuum pump, the vacuum pump's suction port is connected to the melting vessel via a suction pipe, and the suction pipe is equipped with a first valve.

[0020] Preferably, the inert gas source includes an inert gas storage tank, which is connected to the smelting vessel via a vent pipe, and the vent pipe is equipped with a second valve.

[0021] Preferably, the rotating mechanism includes a motor, which is connected to the melting container via a reducer or a linkage mechanism;

[0022] Alternatively, the rotating mechanism may include a rocking cylinder.

[0023] Compared with the prior art, the beneficial effects of this utility model are as follows:

[0024] (1) The device provided by this utility model can provide a double-layer protective environment for metal smelting, which can effectively prevent the intermediate alloy from being oxidized, reduce the oxygen content in the alloy, and ensure the cleanliness of the intermediate alloy.

[0025] (2) This utility model is equipped with a rotating mechanism and an ultrasonic vibration mechanism. During the melting process, the molten metal can be fully mixed by swinging and ultrasonic vibration. Ultrasonic vibration can also completely remove the gas in the molten metal and make the molten metal flow completely to the bottom surface of the melting container, so that the depth of the molten metal is uniform in all places. It also eliminates shrinkage porosity during the solidification process. The cooling mechanism located below the melting container can cool the bottom surface of the melting container to form a vertical temperature field. During the solidification process, the crystal grows from the low temperature zone to the high temperature zone into uniform columnar crystals. The intermediate alloy prepared by the device provided by this utility model has higher uniformity. Attached Figure Description

[0026] To more clearly illustrate the specific embodiments of this utility model or the technical solutions in the prior art, the drawings used in the description of the specific embodiments or the prior art will be briefly introduced below. Obviously, the drawings described below are some embodiments of this utility model. For those skilled in the art, other drawings can be obtained from these drawings without creative effort.

[0027] Figure 1 A schematic diagram of the melting state of the intermediate alloy preparation apparatus provided in this embodiment of the utility model;

[0028] Figure 2 A schematic diagram of the cooling state of the intermediate alloy preparation apparatus provided in this embodiment of the utility model;

[0029] Figure 3 This is a schematic diagram of the structure of a quartz tube as a melting container provided in an embodiment of the present invention;

[0030] Figure 4 This is a schematic diagram of columnar crystal growth during the preparation of intermediate alloys using the apparatus of this invention.

[0031] Figure label:

[0032] 1-Induction power supply; 2-Induction coil; 3-Melting container; 4-Seal; 5-Rotating mechanism; 6-Ultrasonic vibration table; 7-Vacuum chamber; 8-Cooling pool; 9-Cooling medium; 10-Elevator; 11-Cooler; 12-Molten metal; 13-Vacuum system; 14-Rotating seal; 15-Temperature sensor; 16-Inert gas source. Detailed Implementation

[0033] The technical solution of this utility model will be clearly and completely described below with reference to the accompanying drawings and specific embodiments. However, those skilled in the art will understand that the embodiments described below are only some embodiments of this utility model, not all embodiments, and are only used to illustrate this utility model, and should not be regarded as limiting the scope of this utility model. Based on the embodiments of this utility model, all other embodiments obtained by those skilled in the art without creative effort are within the protection scope of this utility model. Where specific conditions are not specified in the embodiments, conventional conditions or conditions recommended by the manufacturer shall be followed. Where the manufacturers of reagents or instruments are not specified, they are all conventional products that can be purchased commercially.

[0034] In the description of this utility model, it should be noted that the terms "center," "upper," "lower," "left," "right," "vertical," "horizontal," "inner," and "outer," etc., indicating the orientation or positional relationship, are based on the orientation or positional relationship shown in the accompanying drawings and are only for the convenience of describing this utility model 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, and therefore should not be construed as a limitation of this utility model. Furthermore, the terms "first," "second," and "third" are used for descriptive purposes only and should not be construed as indicating or implying relative importance.

[0035] In the description of this utility model, it should be noted that, unless otherwise explicitly specified and limited, the terms "installation," "connection," and "joining" should be interpreted broadly. For example, they can refer to a fixed connection, a detachable connection, or an integral connection; they can refer to a mechanical connection or an electrical connection; they can refer to a direct connection or an indirect connection through an intermediate medium; and they can refer to the internal connection of two components. Those skilled in the art can understand the specific meaning of the above terms in this utility model based on the specific circumstances.

[0036] like Figure 1 As shown, this utility model provides an apparatus for preparing an intermediate alloy, including a vacuum chamber 7 and a melting container 3 located in the vacuum chamber 7, a heating mechanism, a rotating mechanism 5, an ultrasonic vibration mechanism, and a cooling mechanism.

[0037] The melting container 3 is used to hold the raw materials required for the preparation of intermediate alloys. The bottom surface of the melting container 3 is flat, which is to ensure that the thickness of the molten metal is uniform throughout. During the operation, the interior of the melting container 3 can be isolated from the vacuum chamber 7, and a protective atmosphere can be introduced into its interior. The melting container 3 and the vacuum chamber 7 can provide a double-layer protective environment for the metal melting process.

[0038] The heating mechanism is used to heat the raw materials in the melting container 3 to form molten metal;

[0039] The rotating mechanism 5 is driven to the melting container 3 so that the melting container 3 can rotate to mix the molten metal;

[0040] The ultrasonic vibration mechanism is connected to the melting container 3 and is used to apply ultrasonic vibration to the molten metal in the melting container 3. The ultrasonic vibration makes the molten metal fully mixed and at the same time completely removes the gas inside the molten metal. During cooling, the ultrasonic vibration can also eliminate shrinkage porosity.

[0041] The cooling mechanism is vertically and vertically positioned below the melting vessel 3 to cool the bottom surface of the melting vessel 3, so that the molten metal inside the melting vessel 3 solidifies into an intermediate alloy in a uniform columnar crystal form.

[0042] In some specific embodiments of this utility model, the ultrasonic vibration mechanism includes an ultrasonic vibration table 6 with an ultrasonic generator, a rotating mechanism 5 mounted on the ultrasonic vibration table 6, one end of the melting container 3 connected to the rotating mechanism 5, and the other end of the melting container 3 connected to the vacuum system 13 and the inert gas source 16 through a rotating seal 14. The vacuum system 13 and the inert gas source 16 are used to provide a first protective atmosphere inside the melting container 3, and the vacuum chamber 7 is used to provide a second protective atmosphere outside the melting container, thereby providing double protection for the molten metal and improving the cleanliness of the intermediate alloy.

[0043] In some specific embodiments of this utility model, the working process of the above-mentioned preparation device is as follows: The melting container 3 containing the raw materials and the rotating mechanism 5 are installed. The melting container 3 is connected to the vacuum system 13 and the inert gas source 16 by rotating the sealing element 14. The vacuum chamber 7 can be connected to the vacuum system 13 through pipes and valves, or it can be evacuated separately using another vacuum system (not shown in the figure). Then, the air in the melting container 3 and the vacuum chamber 7 is extracted, and inert gas is introduced into the melting container 3. This utility model places the melting mechanism in the vacuum chamber 7, providing a double-layer protective environment for melting and preventing damage. The alloy is oxidized to ensure its cleanliness. Then, the heating mechanism is turned on to heat and melt the raw materials to obtain molten metal 12. The rotating mechanism 5 is started to drive the melting container 3 to rotate and swing back and forth, so that the molten metal 12 is fully mixed. After the rotation and swinging mixing has been completed for a period of time, the rotating mechanism 5 is stopped and the ultrasonic vibration is turned on, so that the molten metal in the melting container 3 is under ultrasonic vibration, the gas in the molten metal 12 is completely discharged, and the molten metal 12 flows completely to the bottom surface of the melting container 3, and the depth of the molten metal is uniform everywhere. The heating is stopped and the cooling mechanism is started to cool the bottom surface of the melting container 3, and the molten metal solidifies to form columnar crystals.

[0044] In some specific embodiments of this utility model, the heating mechanism includes an induction coil 2 located outside the melting container 3, and the induction coil 2 is controlled by an induction power supply 1.

[0045] In some specific embodiments of this utility model, the cooling mechanism includes a cooling pool 8 and a lift 10 disposed at the bottom of the cooling pool 8. The cooling pool 8 is used to contain the cooling medium 9 for cooling the molten metal 12.

[0046] In some specific embodiments of this utility model, the cooling medium 9 is a liquid medium, and the cooling pool 8 is connected to the inlet and outlet of the cooling machine 11 through a pipe, so that the cooling medium 9 can circulate in and out of the cooling machine 11 for cooling, thereby ensuring the cooling temperature of the cooling medium 9. As an example, the cooling medium 9 used can be cooling water.

[0047] like Figure 2 As shown, after the melting is completed, heating is stopped, the induction coil 2 is moved aside, the elevator 10 is started, the cooling pool 8 is raised, and the bottom surface of the melting container 3 is immersed in the cooling medium 9. The molten metal is in a uniform temperature field with a vertical distribution of hot at the top and cold at the bottom, and forms a uniform columnar crystal structure that grows upward in ultrasonic vibration.

[0048] In some specific embodiments of this utility model, a temperature sensor 15 is provided inside the melting container 3 to detect the temperature of the molten metal 12.

[0049] In some specific embodiments of this utility model, the bottom surface of the melting container is rectangular. In other embodiments, it can also be other shapes, such as circular, elliptical, etc.

[0050] like Figure 3 As shown, in some specific embodiments of this utility model, the melting container 3 is a quartz tube, including a quartz tube body and inlet pipes located at both ends of the quartz tube body. The two inlet pipes are coaxially arranged with the quartz tube body. The inlet pipe located at one end of the quartz tube body is connected to the vacuum system 13 and the inert gas source 16 through a rotating seal 14, and the inlet pipe located at the other end of the quartz tube body is connected to the rotating mechanism 5 through a seal 4. In other embodiments, the melting container 3 can also be a container made of other high-temperature resistant materials.

[0051] like Figure 1 and Figure 2 As shown, in some specific embodiments of this utility model, the vacuum system 13 includes a vacuum pump. The vacuum pump's suction port is connected to the melting container 3 through a suction pipe. A first valve is provided on the suction pipe. When it is necessary to evacuate the melting container, the first valve is opened, the vacuum pump is started, and when the required pressure is reached, the evacuation is stopped and the first valve is closed.

[0052] like Figure 1 and Figure 2As shown, in some specific embodiments of this utility model, the inert gas source 16 includes an inert gas storage tank, which is connected to the melting container 3 through a vent pipe. A second valve is provided on the vent pipe. After the melting container 3 is evacuated, the second valve is opened to introduce inert protective gas into the melting container 3. After the gas is introduced to the required pressure, the second valve is closed and melting begins.

[0053] In some specific embodiments of this utility model, the rotating mechanism 5 includes a motor, which is connected to the melting container 3 through a reducer or a linkage mechanism. The motor drives the melting container 3 to swing back and forth through the reducer or linkage mechanism. In other embodiments, the rotating mechanism 5 can also be a swing cylinder, which directly drives the melting container 3 to swing, thereby mixing the molten metal in the melting container 3.

[0054] In some specific embodiments, the method for preparing intermediate alloys using the preparation apparatus provided by this utility model includes the following steps:

[0055] S1. Ingredient preparation: Prepare ingredients according to the ingredient ratio;

[0056] S2. Melting: The prepared raw materials are placed in a melting container. The interior of the melting container is under a first protective atmosphere, and the container is placed under a second protective atmosphere. Heating is used to melt the raw materials into molten metal. The molten metal is then repeatedly agitated and mixed to ensure thorough mixing. After agitation and mixing, ultrasonic vibration is applied to completely remove any gas from the molten metal and to ensure that the molten metal flows completely to the bottom surface of the melting container, resulting in uniform molten metal depth throughout. The bottom surface of the melting container is flat, and within the melting container, the thickness H of the molten metal and the bottom surface area S (inner surface area) of the melting container satisfy the following relationship: The unit for H is mm, and the unit for S is mm. 2 r is the coefficient relating the bottom area to the thickness of the molten metal;

[0057] S3. Cooling: After melting is completed, heating is stopped, and the bottom surface of the melting container is cooled under ultrasonic vibration. This places the molten metal in a vertically distributed temperature field with the upper part heated and the lower part cooled, forming an upward-growing columnar crystal structure. Ultrasonic waves can eliminate shrinkage porosity during solidification. After the molten metal has completely solidified, the intermediate alloy is obtained.

[0058] The internal space of the smelting container of this invention is a protective atmosphere, and the smelting container itself is also in an external environment containing a protective atmosphere. This double-layer protection further reduces the oxygen content in the intermediate alloy and improves its cleanliness. Furthermore, the homogenization methods of reciprocating rocking mixing and ultrasonic vibration during the smelting process ensure thorough mixing of the components in the molten metal, improving the uniformity of the intermediate alloy's microstructure. Ultrasonic vibration after rocking mixing completely removes gases from the molten metal and ensures the molten metal flows completely to the bottom surface of the smelting container, resulting in uniform molten depth throughout. Ultrasonic vibration also eliminates shrinkage porosity during solidification. By rationally controlling the relationship between the bottom surface area S of the smelting container and the thickness H of the molten metal, the molten metal can be approximated as an infinitely large plane. The solidification stability field can then be approximated as a vertical gradient temperature field on an infinitely large plane. During solidification, crystals grow from the low-temperature region (i.e., the lower part of the molten metal) to the high-temperature region (i.e., the upper part of the molten metal) into uniform columnar crystals (such as...). Figure 4 (As shown); The intermediate alloy prepared by this device and method is in the shape of a sheet with uniform thickness, high cleanliness and good uniformity.

[0059] In some specific embodiments, step S3 is followed by a cutting and inspection step; wherein, the cutting method involves placing the intermediate alloy sheet obtained in step S3 horizontally and cutting it into small pieces along the vertical direction. Because the microstructure of the intermediate alloy sheet is uniform in all horizontal directions, the intermediate alloy blocks cut by this method have a high degree of compositional uniformity.

[0060] In some specific embodiments, the prepared intermediate alloy can be any one of silver-copper intermediate alloy, gold-beryllium intermediate alloy, and copper-palladium intermediate alloy, but is not limited to these few types and can also be other types of intermediate alloys.

[0061] In some specific embodiments, in step S1, the purity of the metal raw materials used is ≥99.99%, such as the purity of silver, copper, and palladium. Using high-purity raw materials can improve the cleanliness of the intermediate alloy product.

[0062] In some specific embodiments, in step S1, the total mass of the raw materials is 50-500g. For example, it can be any one value or a range of any two values ​​among 50g, 100g, 200g, 300g, 400g, and 500g.

[0063] In some specific embodiments, in step S2, the first protective atmosphere and the second protective atmosphere are independently selected from a vacuum atmosphere or an inert gas atmosphere.

[0064] In some specific embodiments, the first protective atmosphere is an inert gas atmosphere. Before melting, the air inside the melting vessel is extracted to bring its absolute pressure to 10. -4 -10-2 Pa, and then fill it with inert gas to atmospheric pressure; the second protective atmosphere is a vacuum atmosphere with an absolute pressure of 10 Pa. -1 -10Pa.

[0065] In some specific embodiments, in step S2, the thickness H of the molten metal is 0.5-10 mm. For example, it can be any one value or a range of any two values ​​from 0.5 mm, 1.3 mm, 2.3 mm, 3 mm, 4 mm, 5.2 mm, 6 mm, 7 mm, 8 mm, 9 mm, and 10 mm.

[0066] The thickness of the molten metal can be calculated using the following formula:

[0067]

[0068] Where H is in mm; m is the weight of the master alloy in g; and ρ is the density of the master alloy in g / cm³. 3 S is the area of ​​the base, in mm. 2 .

[0069] The thickness H of the molten metal can be expressed as the mass m of each metal component. i and density ρ i Calculate the thickness of each individual liquid metal, and then sum them to obtain the total thickness of the liquid metal.

[0070] As can be seen from the above formula, H and S are inversely proportional. If H is too small, the bottom area of ​​the melting container required for melting will be too large, increasing the cost. For melting containers made of certain materials (such as quartz tubes), it is difficult to guarantee the strength. If H is too large, columnar crystal growth will be difficult to penetrate the entire thickness, reducing the uniformity of the material. Therefore, it is necessary to reasonably control the thickness H of the molten metal.

[0071] In some specific embodiments, in step S2, the oscillation angle of the reciprocating rocking mixing is not less than 10°, for example, it can be any one value or a range of any two values ​​among ±12°, ±15°, ±20°, ±25°, and ±30°; the maximum oscillation angle is determined to ensure that the detection head of the temperature sensor does not leave the liquid surface; the reciprocating rocking mixing time is 5-20 minutes, for example, it can be any one value or a range of any two values ​​among 5 minutes, 8 minutes, 10 minutes, 12 minutes, 15 minutes, 18 minutes, and 20 minutes; the reciprocating rocking speed is 10-300 rpm, for example, it can be any one value or a range of any two values ​​among 10 rpm, 15 rpm, 30 rpm, 60 rpm, 100 rpm, 150 rpm, 200 rpm, and 300 rpm; the reciprocating rocking can fully mix the molten metal and improve the uniformity of the intermediate alloy.

[0072] In some specific embodiments, in steps S2 and S3, the frequency f of the ultrasonic vibration satisfies the following relationship:

[0073]

[0074] Where f is in Hz; l 晶 is the unit cell parameter of the metal, in mm; R is the continuous crystal growth rate, in mm / s; μ1 is a constant related to the diffusion coefficient and latent heat of crystallization, in mm / (s·K), taken as 100; ΔT k It is the kinetic undercooling at the interface front, measured in K, and is set to 10. -4 K; n is the number of ultrasonic vibrations during the solidification of each unit cell in the crystal, n≥1.

[0075] If it can be ensured that the molten metal vibrates at least once during the solidification process of each unit cell, the molten metal can fill the gaps caused by solidification shrinkage, preventing shrinkage porosity on the upper surface of the intermediate alloy and resulting in a very uniform microstructure throughout the intermediate alloy. When n is 1, the calculated frequency is the minimum frequency. When the frequency is lower than this value, shrinkage cavities will form on the upper part of the metal during solidification, and the distribution will be uneven along the planar direction.

[0076] In some specific embodiments, in steps S2 and S3, the power P of the ultrasonic vibration satisfies the following relationship:

[0077]

[0078] Where P is in kW; M is the total weight of the ultrasonic vibration table in kg; and A is the ultrasonic amplitude in m, typically 10. -6 m; f is the ultrasonic frequency, and the unit is Hz.

[0079] When the ultrasonic power is lower than this value, the metal does not vibrate sufficiently during solidification, which will increase the deviation and inhomogeneity of the intermediate alloy composition.

[0080] In some specific embodiments, the ultrasonic vibration time in step S2 is 1-20 minutes, for example, it can be any value or a range of any two values ​​from 1 minute, 3 minutes, 5 minutes, 8 minutes, 10 minutes, 12 minutes, 15 minutes, 18 minutes, to 20 minutes. This ultrasonic vibration not only ensures uniform mixing of the molten metal but also removes gases from the molten metal, allowing the molten metal to flow onto the bottom surface of the melting vessel to form a molten liquid of uniform thickness.

[0081] In some specific embodiments, in step S3, the cooling temperature is 5-30°C. For example, it can be any one value or a range of any two values ​​among 5°C, 10°C, 15°C, 20°C, 25°C, and 30°C.

[0082] The following describes the solution with reference to specific application examples. Unless otherwise specified, the raw materials used in the examples can be purchased commercially. The following examples are all implemented using the device provided by this utility model.

[0083] Example 1

[0084] S1. Ingredients: Weigh out 49g of silver granules with a purity of 99.999% (M Ag ) and 1g of copper granules with a purity of 99.99% (M) Cu ), to obtain raw materials;

[0085] S2. Melting: The prepared raw materials are loaded into a quartz tube. After the quartz tube is installed and reliably sealed, the air in the quartz tube and the vacuum chamber is extracted, so that the absolute pressure in the quartz tube reaches 1×10⁻⁶. -3 Pa, the absolute pressure inside the vacuum chamber is 1×10 Pa. -1 Pa, then fill the quartz tube with argon gas to atmospheric pressure, turn on the induction power supply, use the induction coil to heat, melt the raw materials to obtain molten metal, start the rotating mechanism to reciprocate and mix, the swing angle is ±12°, the swing speed is 30 rpm, swing and mix for 20 minutes, then stop the rotating mechanism, turn on the ultrasonic vibration, expel the gas in the molten metal, so that the molten metal flows completely to the bottom surface of the quartz tube and the molten metal depth is uniform in all places, stop heating after ultrasonic vibration for 10 minutes;

[0086] In this embodiment, the quartz tube used has the following dimensions: height 50mm, bottom length L = 50mm, bottom width W = 50mm, wall thickness d = 2mm, and inlet diameter 10mm; the thickness of the molten metal is calculated as follows:

[0087]

[0088] Compared to molten metal, the bottom surface of a quartz tube can be considered as an infinitely large plane;

[0089] The ultrasonic frequency is calculated as follows:

[0090]

[0091] In this embodiment, the ultrasonic frequency is selected as 28kHz;

[0092] The rotating mechanism uses a motor and a reducer, weighing 500g; the quartz tube weighs 100g; the seal weighs 100g; the molten metal weighs 50g; and the total weight M on the ultrasonic vibration table is 0.75kg.

[0093] Calculate the ultrasonic frequency:

[0094]

[0095] In this embodiment, the ultrasonic power is selected as 4.5kW;

[0096] S3. Cooling: Move the heating coil aside, raise the cooling pool, immerse the bottom of the quartz tube in the cooling water, and place the molten metal in a uniform temperature field with a vertical distribution of hot at the top and cold at the bottom, and form a uniform columnar crystal structure that grows upward during ultrasonic vibration.

[0097] S4. Break the quartz tube to remove the alloy sheet and cut it into pieces. Place the middle alloy sheet horizontally and cut it into small pieces along the vertical direction.

[0098] S5. Randomly select 5 pieces from the cut blocks, use ICP to detect the Cu content in the intermediate alloy, and test its oxygen content. The test results are shown in Table 1.

[0099] Example 2

[0100] S1. Ingredients: Weigh 99g of gold flakes with a purity of 99.999% (M Au ) and 1g of beryllium particles with a purity of 99.99% (M Be ), to obtain raw materials;

[0101] S2. Melting: The prepared raw materials are loaded into a quartz tube. After the quartz tube is installed and reliably sealed, the air in the quartz tube and the vacuum chamber is extracted, so that the absolute pressure in the quartz tube reaches 1×10⁻⁶. -2 The absolute pressure in the vacuum chamber is 10 Pa. Argon gas is then introduced into the quartz tube to atmospheric pressure. The induction power supply is turned on, and the induction coil is used for heating to melt the raw materials and obtain molten metal. The rotating mechanism is started to perform reciprocating oscillation mixing with an oscillation angle of ±15° and an oscillation speed of 60 rpm. After oscillation mixing for 10 minutes, the rotating mechanism is stopped, and ultrasonic vibration is turned on to expel the gas in the molten metal, so that the molten metal flows completely to the bottom surface of the quartz tube and the molten metal depth is uniform in all places. Heating is stopped after ultrasonic vibration for 10 minutes.

[0102] In this embodiment, the quartz tube used has the following dimensions: height 50mm, bottom length L = 70mm, bottom width W = 70mm, wall thickness d = 2mm, and inlet diameter 15mm; the thickness of the molten metal is calculated as follows:

[0103]

[0104] Compared to molten metal, the bottom surface of a quartz tube can be considered as an infinitely large plane;

[0105] The ultrasonic frequency is calculated as follows:

[0106]

[0107] In this embodiment, the ultrasonic frequency is selected as 25kHz;

[0108] The rotating mechanism uses a swing cylinder, weighing 270g; the quartz tube weighs 120g; the seal weighs 150g; the molten metal weighs 100g; and the total weight M on the ultrasonic vibration table is 0.64kg.

[0109] Calculate the ultrasonic frequency:

[0110]

[0111] In this embodiment, the ultrasonic power is selected as 2.5kW;

[0112] S3. Cooling: Move the heating coil aside, raise the cooling pool, immerse the bottom of the quartz tube in the cooling water, and place the molten metal in a uniform temperature field with a vertical distribution of hot at the top and cold at the bottom, and form a uniform columnar crystal structure that grows upward during ultrasonic vibration.

[0113] S4. Break the quartz tube to remove the alloy sheet and cut it into pieces. Place the middle alloy sheet horizontally and cut it into small pieces along the vertical direction.

[0114] S5. Randomly select 5 pieces from the cut blocks, use ICP to detect the Be content in the master alloy, and test its oxygen content. The test results are shown in Table 2.

[0115] Example 3

[0116] S1. Ingredients: Weigh 490g of copper ingots with a purity of 99.999% (M Cu ) and 10g of palladium powder with a purity of 99.99% (M) Pd The copper ingots are broken into small copper pieces to obtain the raw materials;

[0117] S2. Melting: The prepared raw materials are loaded into a quartz tube. After the quartz tube is installed and reliably sealed, the air in the quartz tube and the vacuum chamber is extracted, so that the absolute pressure in the quartz tube reaches 8 × 10⁻⁶. -3Pa, the absolute pressure in the vacuum chamber is 5Pa, then argon gas is filled into the quartz tube to atmospheric pressure, the induction power supply is turned on, and the induction coil is used for heating to melt the raw materials to obtain molten metal. The rotating mechanism is started to perform reciprocating oscillation mixing, with an oscillation angle of ±20° and an oscillation speed of 15rpm. After oscillation mixing for 5min, the rotating mechanism is stopped, and ultrasonic vibration is turned on to expel the gas in the molten metal, so that the molten metal flows completely to the bottom surface of the quartz tube and the molten metal depth is uniform in all places. After ultrasonic vibration for 10min, heating is stopped.

[0118] In this embodiment, the quartz tube used has the following dimensions: height 50mm, bottom length L = 120mm, bottom width W = 100mm, wall thickness d = 3mm, and inlet diameter 20mm; the thickness of the molten metal is calculated as follows:

[0119]

[0120] Compared to molten metal, the bottom surface of a quartz tube can be considered as an infinitely large plane;

[0121] The ultrasonic frequency is calculated as follows:

[0122]

[0123] In this embodiment, the ultrasonic frequency is selected as 28kHz;

[0124] The rotating mechanism uses a motor and linkage mechanism, weighing 1000g; the quartz tube weighs 350g; the seal weighs 200g; the molten metal weighs 500g; and the total weight M on the ultrasonic vibration table is 2.05kg.

[0125] Calculate the ultrasonic frequency:

[0126]

[0127] In this embodiment, the ultrasonic power is selected as 12kW;

[0128] S3. Cooling: Move the heating coil aside, raise the cooling pool, immerse the bottom of the quartz tube in the cooling water, and place the molten metal in a uniform temperature field with a vertical distribution of hot at the top and cold at the bottom, and form a uniform columnar crystal structure that grows upward during ultrasonic vibration.

[0129] S4. Break the quartz tube to remove the alloy sheet and cut it into pieces. Place the middle alloy sheet horizontally and cut it into small pieces along the vertical direction.

[0130] S5. Randomly select 5 pieces from the cut blocks, use ICP to detect the Pd content in the intermediate alloy, and test its oxygen content. The test results are shown in Table 3.

[0131] Comparative Example 1

[0132] S1. Ingredients: Weigh out 49g of silver granules with a purity of 99.999% (M Ag ) and 1g of copper granules with a purity of 99.99% (M) Cu ), to obtain raw materials;

[0133] S2. Melting: The raw materials are placed in a high-purity graphite crucible, which is then placed in a vacuum induction melting furnace for melting. The air in the melting furnace is extracted to achieve an absolute pressure of 3 × 10⁻⁶. -3 Pa, argon gas is introduced for protection, and melting is carried out. During the melting process, electromagnetic stirring is added at a frequency of 15 Hz for 10 minutes.

[0134] S3. Testing: Materials were taken from five different parts of the refined intermediate alloy ingot, and the copper content in the intermediate alloy was tested using ICP. The oxygen content was also tested. The test results are shown in Table 1.

[0135] Comparative Example 2

[0136] Comparative Example 2 is similar to Example 1, except that the ultrasonic frequency is 15 kHz, and all other conditions are the same as in Example 1. The composition and oxygen content of the intermediate alloy were measured, and the results are shown in Table 1.

[0137] Comparative Example 3

[0138] Comparative Example 3 is similar to Example 2, except that the ultrasonic power is 1kW and all other conditions are the same as in Example 2. The composition and oxygen content of the intermediate alloy were measured, and the results are shown in Table 2.

[0139] Comparative Example 4

[0140] Comparative Example 4 is similar to Example 3, except that the bottom length of the quartz tube is L = 70 mm, the bottom width is W = 70 mm, the height is 50 mm, the wall thickness is d = 3 mm, the calculated metal liquid thickness is H = 13.6 mm, and r = 4.7. All other conditions are the same as in Example 3. The composition and oxygen content of the intermediate alloy were measured, and the results are shown in Table 3.

[0141] Test case

[0142] (1) The copper and oxygen contents of different cuts or positions of the intermediate alloys obtained in Example 1, Comparative Example 1 and Comparative Example 2 were tested respectively, and the results are shown in Table 1.

[0143] (2) The beryllium content and oxygen content of the intermediate alloys obtained in Example 2 and Comparative Example 3 at different cuts or positions were tested respectively, and the results are shown in Table 2.

[0144] (3) The palladium content and oxygen content of the intermediate alloys obtained in Example 3 and Comparative Example 4 at different cuts or positions were tested respectively, and the results are shown in Table 3;

[0145] In the experimental example, the component deviation was calculated using the root mean square error method; the inhomogeneity was calculated using the formula: (maximum value - minimum value) / theoretical value.

[0146] Table 1

[0147]

[0148] Comparing Example 1 and Comparative Example 1, it can be seen that the compositional deviation and inhomogeneity of the intermediate alloy obtained using a conventional vacuum melting apparatus are greater than those of the intermediate alloy obtained using the apparatus of this invention. Furthermore, because Comparative Example 1 only used a single vacuum system, although the vacuum melting furnace was evacuated to an absolute pressure of 3 × 10⁻⁶, the compositional deviation and inhomogeneity were significantly reduced. -3 However, because there is no outer vacuum system for protection, the vacuum system is closed during the melting process, and oxygen in the air will gradually and slowly permeate into the furnace. Therefore, the oxygen content of the intermediate alloy obtained is higher than that of the intermediate alloy obtained in this embodiment of the present invention.

[0149] The ultrasonic frequency of Comparative Example 2 is lower than that of Example 1, n < 1, and the metal does not vibrate sufficiently during solidification. It cannot meet the requirement that the molten metal vibrates at least once when each cell solidifies. The compositional deviation and inhomogeneity of the prepared intermediate alloy are higher than those of Example 1, but it is still better than the intermediate alloy produced by a conventional vacuum melting furnace.

[0150] Table 2

[0151]

[0152]

[0153] Comparative Example 3 has a lower ultrasonic power than Example 2. The metal was not vibrated sufficiently during solidification, resulting in higher compositional deviations and inhomogeneities in the prepared intermediate alloy compared to Example 2.

[0154] Table 3

[0155]

[0156] Compared with Example 3, the bottom area of ​​the quartz tube in Comparative Example 4 is smaller. The bottom surface of the solidified molten metal cannot be regarded as an infinitely large plane. The metal liquid level is higher, and it cannot grow into uniform columnar crystals. After solidification, the structure of each part is uneven. The composition deviation and inhomogeneity of the prepared intermediate alloy are higher than those of Example 3.

[0157] Although the present invention has been illustrated and described with specific embodiments, it should be understood that the above embodiments are only used to illustrate the technical solutions of the present invention and not to limit it; those skilled in the art should understand that modifications can be made to the technical solutions described in the foregoing embodiments, or equivalent substitutions can be made to some or all of the technical features therein, without departing from the spirit and scope of the present invention; and these modifications or substitutions do not cause the essence of the corresponding technical solutions to deviate from the scope of the technical solutions of the embodiments of the present invention; therefore, this means that all such substitutions and modifications that fall within the scope of the present invention are included in the appended claims.

Claims

1. An apparatus for preparing an intermediate alloy, characterized in that, It includes a vacuum chamber and a melting vessel located inside the vacuum chamber, a heating mechanism, a rotating mechanism, an ultrasonic vibration mechanism, and a cooling mechanism; The melting vessel is used to hold the raw materials required for the preparation of the intermediate alloy. The bottom surface of the melting vessel is flat, and a protective atmosphere can be introduced into the interior of the melting vessel. The heating mechanism is used to heat the raw materials in the melting vessel to form molten metal; The rotating mechanism is driven to the melting container so that the melting container can rotate. The ultrasonic vibration mechanism is connected to the smelting container and is used to apply ultrasonic vibration to the molten metal in the smelting container. The cooling mechanism is vertically and vertically positioned below the melting vessel to cool the bottom surface of the melting vessel, so that the molten metal inside the melting vessel solidifies in the form of columnar crystals to form the intermediate alloy.

2. The apparatus for preparing the intermediate alloy according to claim 1, characterized in that, The ultrasonic vibration mechanism includes an ultrasonic vibration table with an ultrasonic generator, a rotating mechanism mounted on the ultrasonic vibration table, one end of the melting container connected to the rotating mechanism, and the other end of the melting container connected to a vacuum system and an inert gas source via a rotating seal.

3. The apparatus for preparing the intermediate alloy according to claim 1, characterized in that, The heating mechanism includes an induction coil located outside the melting vessel, and the induction coil is controlled by an induction power source.

4. The apparatus for preparing the intermediate alloy according to claim 1, characterized in that, The cooling mechanism includes a cooling pool and a lift located at the bottom of the cooling pool, the cooling pool being used to contain the cooling medium.

5. The apparatus for preparing the intermediate alloy according to claim 4, characterized in that, The cooling medium is a liquid medium, and the cooling pool is connected to the inlet and outlet of the cooling machine through pipes.

6. The apparatus for preparing the intermediate alloy according to claim 1, characterized in that, The melting vessel is equipped with a temperature sensor.

7. The apparatus for preparing the intermediate alloy according to claim 2, characterized in that, The melting container is a quartz tube, including a quartz tube body and inlet pipes located at both ends of the quartz tube body. The two inlet pipes are coaxially arranged with the quartz tube body. One of the inlet pipes is connected to the vacuum system and the inert gas source through the rotating seal, and the other inlet pipe is connected to the rotating mechanism through the seal.

8. The apparatus for preparing the intermediate alloy according to claim 2, characterized in that, The vacuum system includes a vacuum pump, the vacuum pump's suction port is connected to the melting vessel via a suction pipe, and the suction pipe is equipped with a first valve.

9. The apparatus for preparing the intermediate alloy according to claim 2, characterized in that, The inert gas source includes an inert gas storage tank, which is connected to the smelting vessel via a vent pipe, and the vent pipe is equipped with a second valve.

10. The apparatus for preparing the intermediate alloy according to claim 1, characterized in that, The rotating mechanism includes a motor, which is connected to the melting container via a reducer or a linkage mechanism. Alternatively, the rotating mechanism may include a rocking cylinder.

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