CN104831079B - Segregation method refined aluminium effectively removes the method for vanadium in purifying - Google Patents
Segregation method refined aluminium effectively removes the method for vanadium in purifying Download PDFInfo
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- CN104831079B CN104831079B CN201510242133.4A CN201510242133A CN104831079B CN 104831079 B CN104831079 B CN 104831079B CN 201510242133 A CN201510242133 A CN 201510242133A CN 104831079 B CN104831079 B CN 104831079B
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Abstract
The segregation method refined aluminium of a kind of metal material and field of metallurgy effectively removes the method for vanadium in purifying, Al Fe Si Ni intermediate alloy and primary aluminum to be purified by preparing carry out mixed smelting, aluminium liquid after mixed smelting is oriented solidification purification processes, i.e. removes the v element in primary aluminum.Use cost of the present invention is low, technique is simple, easily operated, the present invention is capable of the segregation coefficient of vanadium and changes into 0.1 0.3 from 5.8, become the element being enriched with in the liquid phase, solidifying segregation process is utilized the highest elemental vanadium by 90% to remove, such that it is able to obtain the 4N5 refined aluminium that purity is up to state standards on a large scale.
Description
Technical field
The present invention relates to the technology of a kind of metal material and field of metallurgy, specifically a kind of segregation method refined aluminium effectively goes in purifying
Method except vanadium.
Background technology
Generally purity (aluminium content) more than 99.99% fine aluminium be called rafifinal.Rafifinal is mainly for the preparation of magnetron sputtering
Target, shielding material, bonding line, high purity aluminium oxide and vacuum evaporation material etc., navigate in scientific research, chemical industry, electronics industry and aviation
It etc. field have purposes widely.
Segregation method is the important method that rafifinal purifies, and has energy consumption technical characterstic low, free of contamination, the most progressively substitutes three-layer-liquid
Electrolysis.Segregation method is to utilize solute element gold of this physical phenomenon of different solubility invention in liquid phase and solid phase in process of setting
Belong to method of purification.The removal efficiency of each impurity element is determined by its segregation coefficient in aluminium, generally carries out table with its segregation coefficient K
Levy.Segregation coefficient K refers at a certain temperature, impurity element concentration C in solid phasesWith the concentration in the liquid phase balanced each other with it
ClRatio, i.e. K=Cs/Cl.The impurity element of K < 1 is enriched with in the liquid phase, it is easy to separate with segregation method.The impurity element of K > 1 exists
Solid phase is enriched with, it is difficult to separate with segregation method.In the 99 kinds of elements being capable of detecting when in aluminum current, the most very difficult segregation method carries
The pure segregation coefficient element more than 1 only has 9 kinds, and in these 9 kinds of elements, vanadium content in aluminium is the highest.Existing rafifinal carries
Pure technology there is no and be specifically designed for the effective ways that impurity vanadium is removed.
Therefore, for removing the special process method of the segregation coefficients such as Ti, V element more than 1, (China is specially in such as boron process
Profit document number CN102031406A open (bulletin) day 2011.04.27, in disclosed aluminium alloy, impurity elements of ferrum, titanium and vanadium goes
Except method) etc. method be developed, but owing to needs add other flux, it is dirty that the impurity element being mixed into from flux creates secondary
Dye, adds purification difficulty and cost.Therefore select the high pure element that segregation coefficient is little to carry out trace interpolation, thus reach to change mesh
The method of mark element segregation coefficient, becomes the revolutionary process changing tradition segregation method.
Summary of the invention
The problem that the present invention is directed to the impurity element vanadium that existing rafifinal segregation purification technique cannot be removed, proposes a kind of segregation method essence
Aluminium effectively removes the method for vanadium in purifying, use cost is low, and technique is simple, it is easy to operation, has wide industrial applications prospect.
The present invention is achieved by the following technical solutions:
The present invention relates to a kind of aluminium alloy removing removal of impurity vanadium in refined aluminium purifies, specially Al Fe Si Ni intermediate alloy.
In described Al Fe Si Ni intermediate alloy: the percentage by weight sum of iron and silicon is less than 2000ppm, the weight hundred of nickel
Proportion by subtraction is less than 300ppm.
The purity of described iron, silicon and nickel in Al Fe Si Ni intermediate alloy is both needed to more than 5N.
Mixing, by the Al Fe Si Ni intermediate alloy prepared in advance and primary aluminum to be purified are carried out mixed smelting, is melted by the present invention
Aluminium liquid after refining is oriented solidification purification processes, i.e. removes the v element in primary aluminum.
Described Al Fe Si Ni intermediate alloy with aluminium liquid to be purified, the quality of the aluminium liquid obtained after melting sources the most to be purified
Ratio is 1:500 1:1500.
Described melting, uses inert gas shielding vacuum environment, removes residual sprue in smelting furnace, and raffinal melting is complete
Rear removing surface scale, carries out mixed smelting by the Al Fe Si Ni intermediate alloy prepared with needing the primary aluminum carrying out purifying, molten
Refining temperature is 700 850 DEG C, is incubated 30min to Wen Houxu.
In described directional solidification purification processes, liquid phase region temperature need to control on fine aluminium fusing point 660 DEG C, and solid liquid interface advances
Speed need to control at 30 μm/s.
Technique effect
Compared with prior art, the present invention adds a certain proportion of trace iron, silicon and nickel element in raffinal liquid, changes vanadium
Element segregation behavior in aluminium, makes the segregation coefficient of vanadium change into 0.1 0.3 from 5.8, becomes the element being enriched with in the liquid phase, profit
Can the highest elemental vanadium by 90% remove, such that it is able to obtain the 4N5 that purity is up to state standards on a large scale by solidifying segregation process
Refined aluminium.
Detailed description of the invention
Elaborating embodiments of the invention below, the present embodiment is implemented under premised on technical solution of the present invention,
Give detailed embodiment and concrete operating process, but protection scope of the present invention is not limited to following embodiment.
Embodiment 1
During the present embodiment realizes preparing rafifinal based on segregation method purification by following steps, the effective of vanadium removes:
Step one, in proportion configuration Al Fe Si Ni intermediate alloy.Wherein the percentage by weight sum of iron and silicon is 600ppm,
The percentage by weight of nickel is 50ppm.The purity of the iron added, silicon and nickel is both needed to more than 5N.
Step 2, clears up smelting furnace, crucible for smelting, thermocouple.
Step 3, carries out melting by the intermediate alloy configured and primary aluminum at 900 DEG C, and intermediate alloy is mixed into aluminium liquid to be purified
Ratio is 1:500, is incubated 20min after temperature.
Step 4, is oriented melted material solidification and processes, and liquid phase region temperature controls at 700 DEG C, and solid liquid interface advances
Speeds control is 15 μm/s.
Implementation result: the present embodiment prepares rafifinal sample, shows through GDMS sample analysis, vanadium during directional solidification
Segregation coefficient be reduced to 0.2 by 5.8, segregation effect is obvious, and the purification efficiency of vanadium is greatly improved.
Embodiment 2
During the present embodiment realizes preparing rafifinal based on segregation method purification by following steps, the effective of vanadium removes:
Step one, in proportion configuration Al Fe Si Ni intermediate alloy.Wherein the percentage by weight of iron is 800ppm, the weight of silicon
Percentage 700ppm, the percentage by weight of nickel is 100ppm.The purity of the iron added, silicon and nickel is both needed to more than 4N.
Step 2, clears up smelting furnace, crucible for smelting, thermocouple.
Step 3, carries out melting, intermediate alloy and aluminium to be purified at 850 DEG C by the intermediate alloy configured in proportion and primary aluminum
It is 1:1500 that liquid is mixed into ratio, is incubated 25min after temperature.
Step 4, is oriented melted material solidification and processes, and liquid phase region temperature controls at 700 DEG C, and solid liquid interface advances
Speeds control is 15 μm/s.
Implementation result: the present embodiment prepares rafifinal sample；Show through GDMS sample analysis, vanadium during directional solidification
Segregation coefficient be reduced to 0.3 by 5.8, segregation effect is obvious, and the purification efficiency of vanadium is greatly improved.
Embodiment 3
During the present embodiment realizes preparing rafifinal based on segregation method purification by following steps, the effective of vanadium removes:
Step one, in proportion configuration Al Fe Si Ni intermediate alloy.Wherein the percentage by weight sum of iron and silicon is 1000ppm,
The percentage by weight of nickel is 1500ppm.The purity of the iron added, silicon and nickel is both needed to more than 4N.
Step 2, clears up smelting furnace, crucible for smelting, thermocouple.
Step 3, carries out melting, intermediate alloy and aluminium to be purified at 900 DEG C by the intermediate alloy configured in proportion and primary aluminum
It is 1:1000 that liquid is mixed into ratio, is incubated 20min after temperature.
Step 4, is oriented melted material solidification and processes, and liquid phase region temperature controls at 700 DEG C, and solid liquid interface advances
Speeds control is 15 μm/s.
Implementation result: the present embodiment prepares rafifinal sample；Show through GDMS sample analysis, vanadium during directional solidification
Segregation coefficient be reduced to 0.1 by 5.8, segregation effect is obvious, and the purification efficiency of vanadium is greatly improved.
Claims (6)
1. the aluminium alloy removing removal of impurity vanadium in refined aluminium purifies, it is characterised in that this aluminium alloy is in the middle of Al-Fe-Si-Ni
Alloy, wherein: the percentage by weight sum of iron and silicon is less than 2000ppm, the percentage by weight of nickel is less than 300ppm.
In refined aluminium purifies, remove the aluminium alloy of removal of impurity vanadium the most according to claim 1, it is characterized in that, described Al-Fe-Si-Ni
The purity of iron, silicon and nickel in intermediate alloy is both needed to more than 5N.
3. the method effectively removing vanadium during a segregation method refined aluminium purifies, it is characterised in that by by prepare in advance as above-mentioned
Al-Fe-Si-Ni intermediate alloy described in any claim and primary aluminum to be purified carry out mixed smelting, are entered by the aluminium liquid after mixed smelting
Row directional solidification purification processes, i.e. removes the v element in primary aluminum.
Method the most according to claim 3, is characterized in that, described Al-Fe-Si-Ni intermediate alloy and aluminium liquid to be purified
Mass ratio is 1:500 1:1500.
Method the most according to claim 3, is characterized in that, described melting, uses inert gas shielding vacuum environment,
Remove residual sprue in smelting furnace, remove surface scale after raffinal melting, close in the middle of the Al-Fe-Si-Ni that will prepare
Gold carries out mixed smelting with needing the primary aluminum carrying out purifying, and smelting temperature is 700-850 DEG C, is incubated 30min to Wen Houxu.
Method the most according to claim 3, is characterized in that, in described directional solidification purification processes, liquid phase region temperature needs
Controlling on fine aluminium fusing point 660 DEG C, solid liquid interface fltting speed need to control at 30 μm/s.
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| CN101514416A (en) * | 2009-01-09 | 2009-08-26 | 毕祥玉 | Allumel intermediate alloy and preparation method thereof |
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