阅读说明：本技术 真空定向提纯炉及利用该炉定向凝固提纯高纯铝的方法 (Vacuum directional purification furnace and method for purifying high-purity aluminum by utilizing furnace through directional solidification ) 是由 吴建忠 于 2018-08-24 设计创作，主要内容包括：一种真空定向提纯炉,包括炉壳,炉壳的上侧部分中固定有坩埚容器,坩埚容器的外侧端面包裹固定有保温层,保温层外部置放有加热线圈,加热线圈与保温层之间布置有电磁搅拌线圈,加热线圈与电磁搅拌线圈错位分布,坩埚容器的底端平面上开设有通孔,坩埚容器的通孔中插接固定有引晶杆,坩埚容器底部外端面上套接固定有隔热环,隔热环底端平面上抵接固定有结晶器,结晶器套接固定在引晶杆的上侧部位。本发明还公开一种真空定向提纯炉定向凝固提纯高纯铝的方法。本发明的电磁搅拌线圈能保证坩埚容器内的高温液体持续保持在高温状态,减少对加热线圈的用电量,且结晶器外侧安装有炉底测温装置,可间接地测量出坩埚容器的内部温度,降低生产成本。(The utility model provides a directional purification stove in vacuum, including the stove outer covering, be fixed with the crucible container in the upside part of stove outer covering, the outside end face parcel of crucible container is fixed with the heat preservation, heating coil has been put to the heat preservation outside, electromagnetic stirring coil has been arranged between heating coil and the heat preservation, heating coil and electromagnetic stirring coil staggered distribution, the through-hole has been seted up on the bottom plane of crucible container, it draws the brilliant pole to peg graft and be fixed with in the through-hole of crucible container, cup joint on the outer terminal surface in crucible container bottom and be fixed with heat insulating ring, the butt is fixed with the crystallizer on the heat insulating ring bottom plane, cup joint and fix the upside position at drawing the brilliant pole. The invention also discloses a method for purifying high-purity aluminum by directional solidification in the vacuum directional purification furnace. The electromagnetic stirring coil can ensure that high-temperature liquid in the crucible container is continuously kept in a high-temperature state, the power consumption of the heating coil is reduced, and the furnace bottom temperature measuring device is arranged outside the crystallizer, so that the internal temperature of the crucible container can be indirectly measured, and the production cost is reduced.)

1. A vacuum directional purification furnace comprises a furnace shell (1), wherein the furnace shell (1) is divided into an upper part and a lower part, and is characterized in that a crucible container (7) is fixed in the upper side part of the furnace shell (1), a heat insulation layer (6) is wrapped and fixed on the outer side end surface of the crucible container (7), a heating coil (5) is placed outside the heat insulation layer (6), the heating coil (5) is fixedly installed in the furnace shell (1), an electromagnetic stirring coil (4) is arranged between the heating coil (5) and the heat insulation layer (6), the heating coil (5) and the electromagnetic stirring coil (4) are distributed in a staggered manner, a through hole is formed in the bottom end plane of the crucible container (7), a crystal guiding rod (10) is fixedly inserted in the through hole of the crucible container (7), a heat insulation ring (8) is fixedly sleeved on the outer end surface of the bottom of the crucible container (7), and a crystallizer (9) is fixedly abutted on the bottom end plane of the, the crystallizer (9) is sleeved and fixed at the upper side part of the crystal leading rod (10), and the lower side part of the crystal leading rod (10) is inserted and fixed in the lower side part of the furnace shell (1).

2. The vacuum directional purification furnace as claimed in claim 1, wherein a support frame is fixedly installed in the lower side portion of the furnace shell (1), a speed reducer (12) is fixedly installed on the support frame of the furnace shell (1), and one end of the speed reducer (12) is fixedly connected with a high-speed motor (13); the other end of the speed reducer is fixedly connected with a servo motor (14), the top of the speed reducer (12) is connected with a pull-down screw rod (11) in a matching mode, and the top of the pull-down screw rod (11) is inserted into the inner portion of the seeding rod (10).

3. The vacuum directional purification furnace as claimed in claim 1, wherein a furnace bottom temperature measuring device is installed at the outer side of the crystallizer (9).

4. The vacuum directional purification furnace according to claim 1, wherein the furnace wall of the furnace shell (1) has a double-layer structure, the outer layer furnace wall and the inner layer furnace wall of the furnace shell (1) are fixed to form an integral structure, and a gap is reserved between the outer layer furnace wall and the inner layer furnace wall.

5. The vacuum directional purification furnace according to claim 4, characterized in that the furnace shell (1) is fixedly provided with a furnace door opening mechanism (2) on the top, and one end frame of the furnace door opening mechanism (2) is hinged on the top frame of the furnace shell (1); the other end is fastened and fixed on the other side frame at the top of the furnace shell (1).

6. The vacuum directional purification furnace as claimed in claim 5, wherein the furnace door opening mechanism (2) is fixedly provided with a viewing hole (3) on the outer end surface.

7. A method for purifying high-purity aluminum by utilizing the directional solidification of the vacuum directional purification furnace as claimed in any one of claims 1 to 6, which is characterized by comprising the following steps of, firstly, selecting materials; selecting an aluminum raw material with the purity of 4N-4N 5, and physically cleaning the surface of the aluminum raw material; secondly, smelting; putting the prepared aluminum raw material in the first step into a crucible container (7), heating the aluminum raw material to 670-730 ℃, and completely melting the aluminum raw material to obtain aluminum liquid; thirdly, solidifying and purifying; standing the aluminum liquid obtained in the second step at 670-730 ℃ for 7-80 minutes; then cooling the bottom of the crucible container (7) to control the temperature of the aluminum liquid from the crystallization surface to the top within the range of 660-700 ℃ from low to high, crystallizing the aluminum liquid from the crystallizer (9), and obtaining a crystalline ingot after 1-8 hours; fourthly, obtaining a finished product; according to different purity requirements, a part of 15 to 70 percent of the thickness is removed from the tail part of the crystallization ingot, and 5N to 5N5 high-purity aluminum can be obtained.

Technical Field

The invention relates to a vacuum directional purification furnace and a method for purifying high-purity aluminum by utilizing the vacuum directional purification furnace through directional solidification.

Background

In the field of electronics industry, in particular in the high-tech fields of optoelectronic storage media, semiconductor devices, superconducting cables and the like, 5 to 6N of high-purity aluminum is required. The purity of high-purity aluminum is expressed by two methods, one is that the content of aluminum or the industry standard mark, such as 99.95%, 99.99%, AL99.993A%, etc., is directly written; one is represented by the "number + N" or "number + N + number", e.g., 4N for 99.99%, 4N6 for 99.996%, etc. Generally, when specific detection elements are not described, the aluminum content is subject to the regulation in the "refined aluminum ingot for remelting YS/T665-2009" standard in the non-ferrous metal industry of china.

At present, three-layer liquid electrolytic refining method, segregation principle purification method, organic solution electrolytic method and the like are mostly adopted in all countries in the world to prepare high-purity or high-purity aluminum with various purities. The purity of the aluminum extracted by the advanced three-layer liquid electrolysis method is basically between 4N and 4N8, but the power consumption is generally more than 13000kwh/t and is about 4 to 5 times of that of the segregation method, the cost is difficult to reduce, and harmful gases such as hydrogen fluoride, carbon monoxide, sulfur dioxide and the like and waste electrolyte are generated in the electrolysis process to seriously pollute the environment; the organic solution electrolysis method is generally used for preparing a small amount of ultra-pure aluminum with purity of more than 7N due to high energy consumption, low yield and complex process, and is not suitable for industrial production. The segregation principle purification method belongs to a physical purification method, can be used for preparing high-purity aluminum with the purity of 3N 5-6N% according to different raw materials, processes and equipment, and has the advantages of low energy consumption, low labor intensity, no chemical reaction pollution and wider application. The segregation principle purification method of aluminum has various realization modes, and at present, a distributed crystallization method, a zone melting method and a directional solidification method are mainly adopted. The distributed crystallization method is industrially used in a large amount abroad, the purification effect depends on the purity of the primary aluminum, generally 99.5 to 99.95 percent of aluminum raw material is used for purification to obtain 3N5 to 4N5 high-purity aluminum, but the production efficiency is low, the purified aluminum is polluted by residual aluminum liquid, the process and equipment are complex, and the purification effect is limited; the zone melting method can obtain 5N 5-6N high-purity aluminum, is mainly used for further purifying the high-purity aluminum by a three-layer liquid method or other segregation methods, has complex equipment, low efficiency and higher energy consumption, and is not suitable for industrial production.

Disclosure of Invention

Aiming at the defects of the prior art, the invention provides the vacuum directional purification furnace capable of solving the problems.

In order to solve the technical problem, the invention is solved by the following technical scheme:

the utility model provides a directional purification stove in vacuum, includes the stove outer covering, the stove outer covering is divided into two parts from top to bottom, be fixed with the crucible container in the upside part of stove outer covering, the outside terminal surface of crucible container wraps up in and is fixed with the heat preservation, heating coil has been place to the outside of heat preservation, heating coil fixed mounting has arranged electromagnetic stirring coil between heating coil and the heat preservation, heating coil and electromagnetic stirring coil dislocation distribution, the through-hole has been seted up on the bottom plane of crucible container, the grafting is fixed with draws the brilliant pole in the through-hole of crucible container, cup joint on the bottom outer terminal surface of crucible container and be fixed with the heat insulating ring, the butt is fixed with the crystallizer on the bottom plane of heat insulating ring, the crystallizer cup joints and fixes the upside position at drawing the brilliant pole, the downside position grafting of drawing the brilliant pole is fixed.

In the technical scheme, a support frame is fixedly arranged in the lower side part of the furnace shell, a speed reducer is fixedly arranged on the support frame of the furnace shell, and one end of the speed reducer is fixedly connected with a high-speed motor; the other end of the speed reducer is fixedly connected with a servo motor, the top of the speed reducer is connected with a pull-down screw rod in a matching mode, and the top of the pull-down screw rod is inserted into the inner portion of the seeding rod.

In the technical scheme, a furnace bottom temperature measuring device is arranged on the outer side of the crystallizer.

In the technical scheme, the furnace wall of the furnace shell is of a double-layer structure, the outer layer furnace wall and the inner layer furnace wall of the furnace shell are fixedly integrated into a whole, and a space is reserved between the outer layer furnace wall and the inner layer furnace wall.

In the technical scheme, the top of the furnace shell is fixedly provided with a furnace door opening mechanism, and a frame at one end of the furnace door opening mechanism is hinged on a frame at the top of the furnace shell; the other end is fastened and fixed on the other side frame at the top of the furnace shell.

In the technical scheme, the observation hole 3 is fixedly arranged on the end face of the outer side of the furnace door opening mechanism.

The invention also discloses a method for purifying high-purity aluminum by utilizing the vacuum directional purification furnace through directional solidification, which comprises the following steps:

the method comprises the following steps of firstly, selecting materials; selecting an aluminum raw material with the purity of 4N-4N 5, and physically cleaning the surface of the aluminum raw material; secondly, smelting; putting the prepared aluminum raw material in the first step into a crucible container, heating the aluminum raw material to 670-730 ℃, and completely melting the aluminum raw material to obtain aluminum liquid; thirdly, solidifying and purifying; standing the aluminum liquid obtained in the second step at 670-730 ℃ for 7-80 minutes; cooling the bottom of the crucible container to control the temperature of the aluminum liquid from the crystallization surface to the top within the range of 660-700 ℃, crystallizing the aluminum liquid from a crystallizer, and obtaining a crystalline ingot after 1-8 hours; fourthly, obtaining a finished product; according to different purity requirements, a part of 15 to 70 percent of the thickness is removed from the tail part of the crystallization ingot, and 5N to 5N5 high-purity aluminum can be obtained.

Has the advantages that: compared with the prior art, the invention has the following beneficial effects:

the heating coils and the electromagnetic stirring coils of the vacuum directional purification furnace are distributed in a staggered manner, the electromagnetic stirring coils generate an alternating magnetic field after being electrified, the alternating magnetic field can generate eddy currents when acting on high-temperature liquid in the crucible container, the high-temperature liquid in the crucible container is continuously kept in a high-temperature state, the temperature is uniform, the power consumption of the heating coils is reduced, meanwhile, a furnace bottom temperature measuring device is installed on the outer side of the crystallizer, the internal temperature of the crucible container can be indirectly measured, the internal temperature of the crucible container is ensured to be within a set temperature range, and the production cost is reduced.

Drawings

FIG. 1 is a front view of a vacuum directional purification furnace.

Detailed Description

Referring to fig. 1, a vacuum directional purification furnace comprises a furnace shell 1, wherein the furnace wall of the furnace shell 1 is of a double-layer structure, an outer layer furnace wall and an inner layer furnace wall of the furnace shell 1 are fixedly formed into an integral structure, a gap is reserved between the outer layer furnace wall and the inner layer furnace wall, cooling water is filled in the gap, the temperature of the furnace wall of the furnace shell 1 can be reduced through flowing cooling water, the furnace shell 1 cannot be burnt for a long time at high temperature to collapse in shape, a furnace door opening mechanism 2 is fixedly installed on the top of the furnace shell 1, and one end frame of the furnace door opening mechanism 2 is hinged to the top frame of the furnace shell 1; the other end is fastened and fixed on the other side frame at the top of the furnace shell 1, an observation hole 3 is fixedly installed on the outer end face of the furnace door opening mechanism 2, the observation hole 3 is used for observing the working condition in the furnace shell 1 in real time, and a countermeasure can be timely made when a sudden situation occurs, the furnace shell 1 is divided into an upper part and a lower part, a crucible container 7 is fixed in the upper part of the furnace shell 1, a through hole is arranged on the bottom end plane of the crucible container 7, a crystal guiding rod 10 is inserted and fixed in the through hole of the crucible container 7, a heat insulation ring 8 is sleeved and fixed on the outer end face of the bottom of the crucible container 7, a crystallizer 9 is abutted and fixed on the bottom end plane of the heat insulation ring 8, the crystallizer 9 is sleeved and fixed at the upper part of the crystal guiding rod 10, the lower part of the crystal guiding rod 10 is inserted and fixed in the lower part of the furnace shell 1, a support frame (not shown in the figure) is, one end of the speed reducer 12 is fixedly connected with a high-speed motor 13; the other end of the lower end of the speed reducer 12 is fixedly connected with a servo motor 14, the top of the speed reducer 12 is connected with a lower pull screw rod 11 in a matching mode, the top of the lower pull screw rod 11 is inserted into the seeding rod 10, the speed reducer 12 can complete power output through a high-speed motor 13, then the speed reducer 12 conveys torque to the lower pull screw rod 11, the lower pull screw rod 11 can move up and down in the seeding rod 10 in a reciprocating mode along the axial direction, and crystalline aluminum ingots inside the seeding rod 10 are scraped off by the lower pull screw rod 11 and then fall to the bottom of the furnace shell 1 and collected.

The crucible container 7 is made of a graphite crucible, the outer side end surface of the crucible container 7 is wrapped and fixed with a heat insulation layer 6, the heat insulation layer 6 is made of high-temperature resistant cotton, the heat insulation layer 6 can increase the heat insulation performance of the crucible container 7, the cooling time of high-temperature liquid is prolonged, a heating coil 5 is placed outside the heat insulation layer 6, the heating coil 5 is fixedly installed in the furnace shell 1, an electromagnetic stirring coil 4 is arranged between the heating coil 5 and the heat insulation layer 6, the heating coil 5 and the electromagnetic stirring coil 4 are distributed in a staggered mode, molten liquid in the crucible container 7 is stirred through vortex completed by the electromagnetic stirring coil 4, an alternating magnetic field is generated after the electromagnetic stirring coil 4 is electrified, the alternating magnetic field acts on the high-temperature liquid in the crucible container 7 and can generate vortex, the high-temperature liquid in the crucible container 7 is continuously kept in a high-temperature state, the temperature is uniform, the energy consumption is reduced.

A furnace bottom temperature measuring device (not shown) is arranged outside the crystallizer 9, the internal temperature of the crucible container 7 can be indirectly measured through the furnace bottom temperature measuring device, the internal temperature of the crucible container 7 is ensured to be within a set temperature range, the energization amount of the heating coil 5 is reduced, and the production cost is reduced.

The method for purifying high-purity aluminum by directional solidification comprises the following steps of firstly, selecting materials; selecting an aluminum raw material with the purity of 4N-4N 5, and physically cleaning the surface of the aluminum raw material; secondly, smelting; putting the prepared aluminum raw material in the first step into a crucible container 7, heating the aluminum raw material to 670-730 ℃, and completely melting the aluminum raw material to obtain aluminum liquid; thirdly, solidifying and purifying; standing the aluminum liquid obtained in the second step at 670-730 ℃ for 7-80 minutes; then cooling the bottom of the crucible container 7 to control the temperature of the aluminum liquid from the crystallization surface to the top within the range of 660-700 ℃ from low to high, crystallizing the aluminum liquid from a crystallizer 9, and obtaining a crystalline ingot after 1-8 hours; fourthly, obtaining a finished product; according to different purity requirements, a part of 15 to 70 percent of the thickness is removed from the tail part of the crystallization ingot, and 5N to 5N5 high-purity aluminum can be obtained.

The second embodiment, the method for purifying high-purity aluminum by directional solidification is carried out according to the following steps, namely, the first step, material selection; selecting an aluminum raw material with the purity of 4N 5-5N, and physically cleaning the surface of the aluminum raw material; secondly, smelting; putting the prepared aluminum raw material in the first step into a crucible container 7, heating the aluminum raw material to 670 ℃ or 730 ℃, and completely melting the aluminum raw material to obtain aluminum liquid; thirdly, solidifying and purifying; standing the aluminum liquid obtained in the second step at 670 ℃ or 730 ℃ for 7 minutes or 80 minutes; then cooling the bottom of the crucible container 7 to control the temperature of the aluminum liquid from low to high from the crystallization surface to 660 ℃ or 700 ℃, crystallizing the aluminum liquid from the crystallizer 9, and obtaining a crystalline ingot after 1 hour or 8 hours; fourthly, obtaining a finished product; according to the difference of purity requirements, a 15% or 70% part of the thickness is removed from the tail part of the crystallization ingot, and 5N5 or 6N high-purity aluminum can be obtained.

Heating coils 5 and electromagnetic stirring coils 4 of the vacuum directional purification furnace are distributed in a staggered mode, the electromagnetic stirring coils 4 generate alternating magnetic fields after being electrified, the alternating magnetic fields act on high-temperature liquid in the crucible container 7 to generate eddy currents, the high-temperature liquid in the crucible container 7 is continuously kept in a high-temperature state, the temperature is uniform, the power consumption of the heating coils 5 is reduced, meanwhile, a furnace bottom temperature measuring device is installed on the outer side of a crystallizer 9, the internal temperature of the crucible container 7 can be indirectly measured, the internal temperature of the crucible container 7 is guaranteed to be within a set temperature range, and the production cost is reduced.

The above-described embodiments are merely illustrative of the preferred embodiments of the present invention and do not limit the spirit and scope of the present invention. Various modifications and improvements of the technical solutions of the present invention may be made by those skilled in the art without departing from the design concept of the present invention, and the technical contents of the present invention are all described in the claims.