CN104263969A - Furnace pipe device and method for preparing ultra-high purity aluminum - Google Patents
Furnace pipe device and method for preparing ultra-high purity aluminum Download PDFInfo
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- CN104263969A CN104263969A CN201410454924.9A CN201410454924A CN104263969A CN 104263969 A CN104263969 A CN 104263969A CN 201410454924 A CN201410454924 A CN 201410454924A CN 104263969 A CN104263969 A CN 104263969A
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Abstract
The invention belongs to the technical field of metal purification, and relates to a furnace pipe device and a method for preparing ultra-high purity aluminum. The furnace pipe device is characterized by sequentially comprising a furnace pipe outer frame, a thin-wall seal sleeve and a graphite crucible from outside to inside, wherein a hinge furnace lid is arranged at the upper part of the furnace pipe; a water inlet hole, a water outlet hole, an observation hole, an air exhaust hole, an air inlet hole, an exhaust vent, a temperature measuring hole and a pressure measuring hole are formed in the furnace lid; a rubber seal strip is arranged between the furnace lid and the furnace pipe outer frame; and the furnace lid is connected and fastened with the furnace pipe through buckles and bolts. The furnace pipe device disclosed by the invention is capable of melting aluminum one time; the crystal is 65Kg; the height of a crystal aluminum ingot can reach 90cm; the single production can be increased by 2.5 times in comparison with that of a conventional high-purity aluminum production technology; an argon protection environment is only kept in the furnace pipe; the furnace pipe device has no environmental requirements on heating and electromagnetic stirring devices, and is strong in continuous working ability; compared with a conventional production technology, the furnace pipe device and the method have the advantages that the power consumption is reduced by 2/3; and the energy consumption cost is saved by 3/5.
Description
Technical field
The invention belongs to purification of metals technical field, relate to a kind of directional freeze in argon shield prepare ultra-pure aluminum flue apparatus and method.
Technical background
Segregation method is utilized to extract ultra-pure aluminum application comparatively general in the prior art, Chinese patent literature CN101191160 describes one " device for extracting high pure aluminum ", theoretical according to segregation at this device, the method of lift in utilization, refer to a kind of flue tube structure for extracting rafifinal in that patent, this structure only has metal shell and plumbago crucible composition, flue upper cover is without any specified otherwise, there is certain shortcoming in a kind of like this structure, if metal shell is too thin, be not enough to the weight carrying crucible and aluminium ingot, easy generation crucible bursts, the danger that aluminium liquid is revealed, if metal shell is too thick, aluminium liquid solidifies from top to bottom gradually, but due to the restriction of radiating condition, aluminium liquid is still in the condition of high temperature, and heat is difficult to scatter and disappear through metal shell, and cause cooling performance poor, refining effect is poor, and the production cycle is long.
Find the patent retrieval of now having announced, Chinese patent literature CN101696472A describes one " purification method of ultra-pure aluminum ", and this technology is loaded in purification furnace by raw material refined aluminium, vacuumizes, and use gas furnace heat fused; Move in crystal growing furnace by purification furnace again, in purification furnace, the rotary motion in crystal growing furnace well heater of aluminium liquid, by the heat dissipation capacity of crystallization control stove, reaches refining effect; Refer to a kind of vacuum purification furnace in this patent, but do not illustrate the sealing method of this purification furnace and the internal structure of purification furnace, different purification furnace structures directly can affect the refining effect of rafifinal.
Further retrieval finds, Chinese patent literature CN101748281 describes one " vacuum purifying device of high-purity aluminium ", heating unit, whipping appts and adiabatic apparatus are all placed in vacuum environment by this device, and according to directional freeze principle, method growth pattern is drawn under employing, prepare rafifinal, although this invention is rational in infrastructure, but the space of vacuum oven is large, for reaching the vacuum tightness of production requirement, need use two-stage vacuum pump, required vaccum-pumping equipment power is high, and condition of high vacuum degree is also difficult to ensure, causes purification efficiency to reduce.
Summary of the invention
Technical problem to be solved by this invention is, not enough for prior art, and provide a kind of structure simple, refining effect is good, and energy-conservation, efficient, is prepared a kind of flue device of ultra-pure aluminum under argon shield by directional solidification technique.
For solving the problems of the technologies described above, flue device ecto-entad of the present invention is followed successively by flue outside framework, thin-walled seal cartridge, plumbago crucible; Flue device top is hinge type bell, and bell is provided with prosopyle, posticum, vision slit, aspirating hole, air inlet port, venting hole, thermometer hole and pressure tap; The rubber weather strip that width is 1 ~ 3cm is installed between bell and flue outside framework.
Flue outside framework is made up of three parts from top to bottom, and top is step-like sidewall seal ring set, and middle part to be formed by connecting inversed taper platform shape by radial steel plate by 4 blocks of longitudinal steel plates, forms bottom the flue of lower end with same steel plate and longitudinal Plate Welding; Flue outside framework material is high temperature steel, and thickness is 0.3cm ~ 0.8cm, and sidewall seal ring set diameter is 25cm ~ 40cm, and length is 0.1m ~ 0.4m, and mid diameter is 20cm ~ 32cm, and length is 0.5m ~ 1.3m, and base diameter is equal with longitudinal steel plate lower end diameter; Flue outside framework mainly plays carrying effect, load-bearing 150Kg ~ 300Kg; Thin-walled seal cartridge is at flue housing internal layer, and top is connected with the sidewall seal ring set of flue housing by seamless welding, makes flue inside become sealed environment; Thin-walled seal cartridge material is high temperature steel, and thickness is 0.06cm ~ 0.15cm, and length is 0.5m ~ 1.4m; Innermost layer is high purity graphite crucible, and crucible is close to inside thin-walled seal cartridge, and plumbago crucible top is furnished with the graphite cover of middle with hole, and the purity of plumbago crucible reaches 99.9wt% ~ 99.999wt%, crucible wall thickness 2cm ~ 3cm, internal diameter 15cm ~ 23cm, external diameter 19cm ~ 29cm.
The hinge type bell on flue top is two-layer up and down, edge seal, and centre is empty hollow bell, prosopyle is connected with die cavity in bell with posticum, and object is when solidifying Purification of Aluminum, forms directed cooling environment at flue top, reduce temperature of aluminum liquid, improve purification efficiency; Vision slit is communicated to flue inside, and pass through metal clip at vision slit end rubber sheet gasketing and transparent glass fastening, play sealing function, vision slit diameter is 1.5cm ~ 4cm; Aspirating hole is communicated to flue inside, and outside is connected with vacuum pump, and effect vacuumized flue inside before fusing aluminium ingot; Pressure tap, air inlet port and venting hole share a passage, are communicated to flue inside, install four-way interface in passage outer end, air inlet and exhaust control respectively, inlet mouth outer end is connected with argon bottle, and the object of inlet mouth is after flue inside is evacuated, and passes into argon shield; Venting port object is that flue internal gas expands when aluminium liquid melts, and release gas decompression, prevents flue dilatational strain; The external tensimeter of pressure tap, measures flue air pressure inside value in real time, ensures aluminium liquid purification quality; Thermometer hole is communicated to flue inside, installs thermopair, measures flue internal temperature in real time, ensures purification efficiency.
Between flue housing and bell, rubber seal is installed, and both connect by buckle bolt fastening, ensure the sealing effectiveness of flue.
The operation steps of purification flue:
(1) feed, require: in crucible, aluminium material the end of from up, fill intensive, aluminium material can't be made to be stuck in plumbago crucible and to make aluminium material not arrive crucible bottom.
(2) cover graphite cover, at sidewall seal ring set surface mounting rubber weather strip, then cover bell, guarantee the stopping property of boiler clothing inside.
(3) close vent valve and argon gas cut-in valve, open vacuum pump and take out valve.
(4) open vacuum pump, after 8 ~ 15 minutes, make pressure gauge registration be 0.001MPa ~ 0.01MPa.
(5) open argon gas cut-in valve, close vacuum pump and take out valve, open argon gas and pass into switch until weather gage registration is 0.1MPa ~ 0.15MPa.
(6) close argon gas cut-in valve, then start to add hot melt aluminium.
(7), after aluminium ingot fusing, open water intaking valve and outlet valve, lift is started to flue, purifies.
Compared with prior art, advantage of the present invention is: the present invention adopts flue outside framework to carry flue and aluminium liquid weight, reduces the load metamorphism of thin-walled sealing boiler clothing, uses thin-walled sealing boiler clothing flue can be made to form good sealed environment on the one hand; Can effectively prevent inner crucible to be oxidized on the other hand, extend pot life; In addition, when flue pulls out from induction stirring process furnace, use thin-walled sealing boiler clothing can accelerate the cooling performance having gone out oven body part, improve the purification efficiency of aluminium ingot; Two-layer up and down, edge seal, centre is empty hollow bell, water-in is connected with die cavity in bell with water outlet, stores cooling circulating water at bell inner chamber, forms directed cooling environment, reduce temperature of aluminum liquid, improve purification efficiency, flue upper operating room temps can be reduced, for operator provides safe Working environment simultaneously; The present invention is for vacuumizing, and the melting purifying plant of logical argon shield, relative to traditional vacuum oven, in this invention, flue space is little, and required vaccum-pumping equipment power is low, and argon gas intake is few, easy and simple to handle, and reach energy-saving effect, greatly reduce production cost, pass into argon gas and can dilute air remaining in flue, reduce oxygen concentration, in addition, the flue being connected with argon gas can prevent boiler clothing distortion at high temperature, extends the work-ing life of purification flue; The present invention designs disposable molten aluminium, crystallization is 65Kg, and crystallization aluminium ingot height reaches 90cm, and relative to conventional rafifinal production technology, single output can improve 2.5 times; Current conventional ultra-pure aluminum production technology, smelting apparatus, whipping appts and crystallization apparatus all under vacuum conditions, continuous seepage ability, vacuum environment is easily destroyed; Only allow in flue and keep argon shield environment, do not have environmental requirement to heating and electromagnetic mixing apparatus, non-stop run ability is strong, with conventional manufacturing techniques ratio, reduces power consumption 2/3, energy efficient cost 3/5.
attached body explanation
Fig. 1, Fig. 2 are the flue tube structure schematic diagram that the present invention extracts ultra-pure aluminum; Fig. 3 is the flue pictorial diagram that the present invention extracts ultra-pure aluminum.
1. bell; 2. rubber weather strip; 3. high purity graphite packing; 4. seamless welding interface; 5. flue outside framework;
6. thin-walled seal cartridge; 7. plumbago crucible; 8. graphite cover; 9. prosopyle; 10. posticum; Aspirating hole; Air inlet port; Pressure tap; Venting hole; Thermometer hole; Vision slit.
Embodiment
The purification flue of 60Kg capacity is all adopted in following examples.
The flue tube structure preparing ultra-pure aluminum adopted in following examples is as shown in Figure 1: flue device ecto-entad be followed successively by flue outside framework 5., thin-walled seal cartridge 6., plumbago crucible 7.; Flue top be hinge type bell 1., 9. bell is provided with prosopyle, posticum 10., vision slit, aspirating hole, air inlet port, venting hole, thermometer hole, pressure tap form; Rubber weather strip is installed 2. between bell and flue outside framework, and both connect by buckle bolt fastening; 5. flue outside framework is made up of three parts from top to bottom, and top is step-like sidewall seal ring set, and middle part to be formed by connecting inversed taper platform shape by radial steel plate by 4 blocks of longitudinal steel plates, forms bottom the flue of lower end with same steel plate and longitudinal Plate Welding; Thin-walled seal cartridge is 6. at flue outside framework 5. internal layer, and 4. top be connected with flue outside framework sidewall seal ring set 5. by seamless welding, makes flue inside become sealed environment; Innermost layer be high purity graphite crucible 7., plumbago crucible be 7. close to thin-walled seal cartridge 6. inner side, 8. plumbago crucible top be furnished with the graphite cover of middle with hole; 1. the hinge type bell on flue top is two-layer up and down, edge seal, and centre is empty hollow bell, prosopyle 9. with posticum 10. with bell 1. in die cavity be connected; Vision slit is communicated to flue inside, passes through metal clip fastening at vision slit end rubber sheet gasketing and transparent glass; Aspirating hole is communicated to flue inside, and outside is connected with vacuum pump; Pressure tap, air inlet port and venting hole share a passage, are communicated to flue inside, install four-way interface in passage outer end, and air inlet and exhaust control respectively, and inlet mouth outer end is connected with argon bottle, the external tensimeter of pressure tap; Thermometer hole is communicated to flue inside, installs thermopair.
Embodiment 1: select purity to be the refined aluminium of 4N3,
(1) feed, require: in crucible, aluminium material the end of from up, fill intensive, aluminium material can't be made to be stuck in plumbago crucible and to make aluminium material not arrive crucible bottom.
(2) cover graphite cover, at sidewall seal ring set surface mounting rubber weather strip, then cover bell, guarantee the stopping property of boiler clothing inside.
(3) close vent valve and argon gas cut-in valve, open vacuum pump and take out valve.
(4) open vacuum pump, after 10 minutes, make pressure gauge registration be 0.0015Mpa.
(5) open argon gas cut-in valve, close vacuum pump and take out valve, open argon gas and pass into switch until weather gage registration is 0.1Mpa.
(6) close argon gas cut-in valve, then start to add hot melt aluminium.
(7), after aluminium ingot fusing, open water intaking valve and outlet valve, lift is started to flue, purifies.
Can obtain the ultra-pure aluminum of more than 5N, Inorganic Material Analysis test center of Shanghai silicate institute of attached Chinese Academy of Sciences analytical test report is as following table one.
Embodiment 2: select purity to be the refined aluminium of 4N6,
(1) feed, require: in crucible, aluminium material the end of from up, fill intensive, aluminium material can't be made to be stuck in plumbago crucible and to make aluminium material not arrive crucible bottom.
(2) cover graphite cover, at sidewall seal ring set surface mounting rubber weather strip, then cover bell, guarantee the stopping property of boiler clothing inside.
(3) close vent valve and argon gas cut-in valve, open vacuum pump and take out valve.
(4) open vacuum pump, after 12 minutes, make pressure gauge registration be 0.001Mpa.
(5) open argon gas cut-in valve, close vacuum pump and take out valve, open argon gas and pass into switch until weather gage registration is 0.15Mpa.
(6) close argon gas cut-in valve, then start to add hot melt aluminium.
(7), after aluminium ingot fusing, open water intaking valve and outlet valve, lift is started to flue, purifies.
Can obtain the ultra-pure aluminum of more than 5N5, Inorganic Material Analysis test center of Shanghai silicate institute of attached Chinese Academy of Sciences analytical test report is as following table two.
table one GDMS analysis report list
unit: ppm
table two GDMS analysis report list?
unit: ppm
Claims (7)
1. for the preparation of a flue device for ultra-pure aluminum, it is characterized in that, flue device ecto-entad is followed successively by flue outside framework, thin-walled seal cartridge and plumbago crucible; Flue top is hinge type bell.
2. a kind of flue device for the preparation of ultra-pure aluminum according to claim 1, it is characterized in that: flue outside framework is made up of three parts from top to bottom, top is step-like sidewall seal ring set, middle part to be formed by connecting inversed taper platform shape by radial steel plate by 4 blocks of longitudinal steel plates, forms bottom the flue of lower end with same steel plate and longitudinal Plate Welding; Flue outside framework material is high temperature steel, and thickness is 0.3cm ~ 0.8cm, and sidewall seal ring set diameter is 25cm ~ 40cm, and length is 0.1m ~ 0.4m, and mid diameter is 20cm ~ 32cm, and length is 0.5m ~ 1.3m, and base diameter is equal with longitudinal steel plate lower end diameter; Flue outside framework mainly plays carrying effect, load-bearing 150Kg ~ 300Kg.
3. a kind of flue device for the preparation of ultra-pure aluminum according to claim 1, is characterized in that: thin-walled seal cartridge is at flue housing internal layer, and top is connected with the sidewall seal ring set of flue housing by seamless welding, makes flue inside become sealed environment; Thin-walled seal cartridge material is high temperature steel, and thickness is 0.06cm ~ 0.15cm, and length is 0.5m ~ 1.4m.
4. a kind of flue device for the preparation of ultra-pure aluminum according to claim 1, it is characterized in that: innermost layer is high purity graphite crucible, crucible is close to inside thin-walled seal cartridge, plumbago crucible top is furnished with the graphite cover of middle with hole, the purity of plumbago crucible reaches 99.9wt% ~ 99.999wt%, crucible wall thickness 2cm ~ 3cm, internal diameter 15cm ~ 23cm, external diameter 19cm ~ 29cm.
5. a kind of flue device for the preparation of ultra-pure aluminum according to claim 1 is characterized in that: described bell is provided with prosopyle, posticum, vision slit, aspirating hole, air inlet port, venting hole, thermometer hole, pressure tap; Bell is two-layer up and down, edge seal, and centre is empty hollow bell, and prosopyle is connected with die cavity in bell with posticum, and object is when solidifying Purification of Aluminum, forms directed cooling environment at flue top, reduces temperature of aluminum liquid, improves purification efficiency; Vision slit is communicated to flue inside, and pass through metal clip at vision slit end rubber sheet gasketing and transparent glass fastening, play sealing function, vision slit diameter is 1.5cm ~ 4cm; Aspirating hole is communicated to flue inside, and outside is connected with vacuum pump, and effect vacuumized flue inside before fusing aluminium ingot; Pressure tap, air inlet port and venting hole share a passage, are communicated to flue inside, install four-way interface in passage outer end, air inlet and exhaust control respectively, air inlet port outer end is connected with argon bottle, and the object of air inlet port is after flue inside is evacuated, and passes into argon shield; Venting hole object is that flue internal gas expands when aluminium liquid melts, and release gas decompression, prevents flue dilatational strain; The external tensimeter of pressure tap, measures flue air pressure inside value in real time, ensures aluminium liquid purification quality; Thermometer hole is communicated to flue inside, installs thermopair, measures flue internal temperature in real time, ensures purification efficiency.
6. a kind of flue device for the preparation of ultra-pure aluminum according to claim 1 is characterized in that: between flue outside framework and bell, install the rubber seal that width is 1 ~ 3cm, and both connect fastening by buckle bolt.
7. use flue device as claimed in claim 1 to prepare the method for ultra-pure aluminum, it is characterized in that step is as follows:
(1) feed, require: in crucible, aluminium material the end of from up, fill intensive, aluminium material can't be made to be stuck in plumbago crucible and to make aluminium material can not arrive crucible bottom;
(2) cover graphite cover, at the sidewall seal ring set surface mounting rubber weather strip of flue outside framework, then cover bell, guarantee the stopping property of boiler clothing inside;
(3) close vent valve and argon gas cut-in valve, open vacuum pump and take out valve;
(4) open vacuum pump, after 8 ~ 15 minutes, make pressure gauge registration be 0.001Mpa ~ 0.01Mpa;
(5) open argon gas cut-in valve, close vacuum pump and take out valve, open argon gas and pass into switch until weather gage registration is 0.1Mpa ~ 0.15MPa;
(6) close argon gas cut-in valve, then start to add hot melt aluminium;
(7), after aluminium ingot fusing, open water intaking valve and outlet valve, lift is started to flue, purifies.
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Cited By (4)
| Publication number | Priority date | Publication date | Assignee | Title |
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| WO2017151288A1 (en) * | 2016-02-29 | 2017-09-08 | Asml Netherlands B.V. | Method and apparatus for purifying target material for euv light source |
| CN108251658A (en) * | 2018-02-05 | 2018-07-06 | 江苏金海铝业有限公司 | A kind of method of directional solidification extraction ultra-pure aluminum under electromagnetic agitation |
| CN112708778A (en) * | 2020-12-04 | 2021-04-27 | 宁波锦越新材料有限公司 | Electron-grade ultra-high-purity aluminum crystallization device |
| CN114525387A (en) * | 2022-04-08 | 2022-05-24 | 佛山市明富兴金属材料有限公司 | Magnetic core vacuum heat treatment device and process |
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Cited By (6)
| Publication number | Priority date | Publication date | Assignee | Title |
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| WO2017151288A1 (en) * | 2016-02-29 | 2017-09-08 | Asml Netherlands B.V. | Method and apparatus for purifying target material for euv light source |
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| CN114525387A (en) * | 2022-04-08 | 2022-05-24 | 佛山市明富兴金属材料有限公司 | Magnetic core vacuum heat treatment device and process |
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Effective date of registration: 20180205 Address after: Zhenjiang City, Jiangsu province 212009 District No. 42 Dingmao pan Zong Lu Patentee after: Jiangsu Jinhai Aluminum Industry Co., Ltd. Address before: Zhenjiang City, Jiangsu Province, 212013 Jingkou District Road No. 301 Patentee before: Jiangsu University |
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