CN109943740A - A kind of combined processing agent material and preparation method thereof - Google Patents
A kind of combined processing agent material and preparation method thereof Download PDFInfo
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Abstract
The present invention discloses a kind of combined processing agent material, it is grouped as by the group of following weight ratio: Sodium acetate trihydrate 13-18%, aluminium oxide 5-9%, potassium fluoroaluminate 5-8%, strontium nitrate 13-16%, potassium chloride 3-7%, cryolite 12-16%, clay composite powder 12-15%, 2~4% sodium chloride, surplus Al；Molybdic acid RE composite can change the form and size of the harmful phase of impurity element formation, and have the potential that shines, and pyrophyllite powder can be used as rotten agent carrier degasification slagging-off, promote smelting efficiency.Three step raw material addition methods are used in preparation method, it successfully combines three kinds of sodium, strontium, rare earth alterants and retains rotten active, effective refining eutectic silicon, modification effect is more stable, the scaling loss for preventing or slowing down independent alterant when high melt extends effective deteriorating time.
Description
Technical field
The present invention relates to alloy inoculant field, in particular to a kind of combined processing agent material and preparation method thereof.
Background technique
The silicon tissue of transcocrystallized Al-Si alloy is made of the starlike primary silicon of five coarse valves and long acicular Eutectic Silicon in Al-Si Cast Alloys, this
The silicon of a little forms mutually isolates Al matrix for serious, causes stress to be concentrated at the tip of Si phase and edges and corners, and alloy is easy along crystalline substance
The boundary or plate Si itself of grain crack and form crackle, so that alloy is become fragile, mechanical performance especially elongation percentage significantly drops
Low, machining function is also bad.In order to change the existence of silicon, the mechanical property of alloy is improved, generally alloy is added
Alterant refines primary silicon and Eutectic Silicon in Al-Si Cast Alloys.
More to the research of alterant both at home and abroad, common Modification Manners are individually added into a kind of element, also have addition more
Kind element and compound, both methods all have good refining effect to primary silicon and Eutectic Silicon in Al-Si Cast Alloys.Main alterant element
Including phosphorus, sodium, strontium, rare earth and calcium, these elements can be used as single alterant, can also form composite modifier, as sulphur phosphorus is compound
Alterant, rare earth phosphorus composite modifier, strontium phosphorus composite modifier, sodium phosphorus composite modifier, carbon phosphorus composite modifier and barium phosphorus are multiple
Close alterant etc..Although these single or composite modifiers have preferable primary silicon refining effect, still deposited when rotten
In obvious disadvantage.
When using red phosphorus as alterant, burning point is relatively low, and transport and preservation are difficult, and during fine degenerate, combustion
It burns acutely, causes the reduction of phosphorus absorptivity, generate poison gas, seriously pollute environment, secondly during melting, be easy to produce a large amount of
Reaction slag and compound, corrode furnace lining, increase the loss of aluminium.And when rotten with A1-P intermediate alloy, although overcoming
State defect, but A1-P intermediate alloy is due to toxic, and the more complex price of production technology is higher, therefore is unfavorable for industrial metaplasia
It produces.When sodium alterant goes bad to transcocrystallized Al-Si alloy, there is the disadvantages of absorption poisoning effect, deteriorating time is short.The main shadow of strontium
The primary silicon pattern in transcocrystallized Al-Si alloy is rung, is not apparent on the influence of the size of primary silicon.And it is rotten using strontium, by
It is reacted in strontium with chlorine, degasification cannot be refined with chlorine or double salt containing chlorine.Strontium is rotten, and there is also easily cause air-breathing, expensive etc.
Disadvantage, therefore cannot be widely applied in industrial production.Air-breathing is easily caused in calcium metamorphic process, due to requiring calcium content
Strictly, therefore technique is difficult to grasp, and modification effect is not so good as phosphorus and sodium.Thinning effect is unknown when rare earth is as single alterant
It is aobvious, it must combine and assist sodium and the agent of phosphorus iso-metamorphism can just play metamorphism.That there is also alterant elements is mutual for other composite modifiers
Mutually inhibit, production slag production gas is excessive, accurate to match the problems such as difficulty.
It is typically all using the method for swimming during aluminum alloy melt casting come degasification, principle is to be passed through certain in aluminum alloy melt
Not hydrogeneous gas generates minute bubbles, takes the hydrogen of dissolution out of aluminum alloy melt in floating-upward process using these bubbles, escapes into big
Gas.Meanwhile be to guarantee good refining effect, the selection of refining temperature should be appropriate, and temperature is excessively high, the bubble generated it is larger and
It floats quickly, refining effect is made to be deteriorated.The viscosity of aluminum alloy melt is larger when temperature is too low, and the gas being unfavorable in aluminum alloy melt fills
Divide discharge, equally can also reduce refining effect.Meanwhile can also have using ultrasonic wave, chlorine or double salt containing chlorine processing aluminum alloy melt
Effect ground degasification.
For metal impurities, general being of processing method adverse factor is favorable factor.It i.e. will by alloyage process
It becomes the second beneficial phase, in favor of the performance of material property.It is to utilize difference in most cases if having to removal
Element boiling point difference carries out high-temperature low-pressure and selectively distills, to achieve the purpose that remove metal impurities.Skimming in traditional melting
Removal step is time-consuming and laborious, but impurity removing refining effect directly affect alloy degree of purity and final mechanical property.
Chinese patent CN201610732543.1 is related to a kind of method that Metamorphism treatment prepares transcocrystallized Al-Si alloy, by with
Lower step carries out: (1) crucible being preheated to 400 ± 5 DEG C, Al28Si alloy, Al50Cu alloy and Al8Ni alloy are placed in crucible
In alloy melt is made；(2) alterant is pressed into alloy melt and is stirred evenly with bell jar；(3) with bell jar by ZnCl2Indentation
Degasification in alloy melt, skims, casting；(4) 540 ± 5 DEG C of 3~5h of heat preservation, solution treatment, ageing treatment are heated to.The method
Its mechanical property of the product of preparation is better than similar hypereutectic alloy product, simple process, it is easy to accomplish industrialization, preparation cost
It is low.
Foregoing invention, as alterant, is preferably refined using copper phosphorus intermediate alloy although having to aluminium alloy as-cast structure
Metamorphism, but Cu-P intermediate alloy due to it is rotten when need in 800~850 DEG C of heat preservation 60min, such melt temperature is excessively high
So that the serious air-breathing of aluminium alloy, while the aluminium consumption under high temperature also increases, in addition, Cu-P intermediate alloy is due to biggish containing density
Copper fashionable is easy to produce segregation being added to.Refining must be individually carried out before and after Metamorphism treatment using copper phosphorus intermediate alloy to remove
Slag degasification, slagging-off degassing effect directly affects last Mechanical Properties of Aluminum Alloys, thus while slagging-off deaeration step is many and diverse, influences
Aluminium alloy production efficiency, but can not save.
Summary of the invention
The technical problems to be solved by the invention: for can not go bad simultaneously in current transcocrystallized Al-Si alloy fusion process
Processing and slagging-off degasification and the problem of common alterant is ineffective and easy scaling loss, the present invention provides a kind of composite treating agent material
Material, solves the above problems, while transcocrystallized Al-Si alloy being made to obtain weaker luminescent properties.
In order to solve the above technical problems, the present invention provides technical solution below:
A kind of combined processing agent material, is grouped as by the group of following weight ratio: Sodium acetate trihydrate 13-18%, aluminium oxide 5-
9%, potassium fluoroaluminate 5-8%, strontium nitrate 13-16%, potassium chloride 3-7%, cryolite 12-16%, clay composite powder 12-
15%, 2~4% sodium chloride, surplus Al；
The clay composite powder boron carbide containing 25-28wt%, 20-28wt% calcium oxide, 5-8wt% molybdic acid rare earth are compound
Object, 15-18wt% zinc oxide, 5-8wt% tar, surplus are pyrophyllite powder；The molybdic acid RE composite is by sodium molybdate/nitric acid
Praseodymium calcined material and pyrophyllite powder composition.
Preferably, the Sodium acetate trihydrate, aluminium oxide, potassium fluoroaluminate, strontium nitrate, potassium chloride, cryolite, sodium molybdate,
Praseodymium nitrate, sodium chloride, boron carbide, calcium oxide, zinc oxide, Al purity be all larger than 99.9wt%, partial size is 150~250 mesh, institute
Stating tar is middle coalite tar；The content 55.3 of praseodymium molybdic acid sodium salt in the sodium molybdate/praseodymium nitrate calcined material~
80.9wt%.
A kind of preparation method of above-mentioned combined processing agent material includes following specific steps:
(1) molybdic acid RE composite is prepared as follows: 10-13g sodium molybdate being added in 1000mL dehydrated alcohol, sets
In the ethanol solution 1000mL on magnetic stirring apparatus, instilling the 4-8g containing praseodymium nitrate dropwise, 16-29h, solvent are stirred in 20 DEG C of constant temperature
10-12h is dried after volatilization in 60-80 DEG C of baking oven to doing, 450~550 DEG C of 1~4h of calcining obtain sodium molybdate/praseodymium nitrate calcined material,
1L dehydrated alcohol and 110-125g pyrophyllite powder are added after being cooled to room temperature, is filtered after homogenate, precipitating drying is taken to obtain molybdic acid
RE composite；
(2) preparation of clay composite powder: dilute according to 25-28wt% boron carbide, 20-28wt% calcium oxide, 5-8wt% molybdic acid
Native compound, 15-18wt% zinc oxide, 5-8wt% tar, remaining is pyrophyllite powder ingredient, by the mixture powder outside tar removing
End is placed in planetary ball mill tank ground and mixed, using vacuumize three times pour hydrogen by the way of guarantee that oxygen content is lower than in vacuum tank
1%, prevent material from aoxidizing；The troubled liquor containing alterant is obtained with the steel ball in alcohol rinse ball grinder and tank, by the liquid
Body is placed in a vacuum drying oven, and mixed powder is obtained after vaporized alcohol is complete；
(3) tar is added in mix powder while stirring, mixture after mixing evenly is put into grinding tool and is suppressed
Blocking, compression moulding pressure is 15~25MPa, is put into roaster after being embedded with graphite powder, small in 980-1150 DEG C of heat preservation 1-2
Shi Hou, cooled to room temperature, remove graphite powder after ground on grinder, until particle size 10~15 microns to get
Clay composite powder；
(4) Sodium acetate trihydrate 13-18wt%, aluminium oxide 5-9wt%, potassium fluoroaluminate 5-8wt%, strontium nitrate 13- are pressed
It is 16wt%, potassium chloride 3-7wt%, cryolite 12-16wt%, clay composite powder 12-15wt%, 2~4wt% sodium chloride, remaining
Amount is that Al weighs raw material, fine aluminium ingot is heated to 700-750 DEG C, by clay composite powder after fine aluminium ingot is completely melt as aluminium solution
It is added as first part of raw material, and 1000~3000rpm stirs 10min, removal aluminium melt surface generates after standing the 5min time
Slag；
(5) aluminum melt temperature is increased to 850-900 DEG C, while being mixed again to what aluminum melt addition strontium nitrate and aluminium oxide formed
Uniform second part of raw material is closed, 500~1000rpm is stood after stirring 3~8min, skimming, and uses CaF2Powder thoroughly removes table
Face dross, heat preservation 10min are passed through high pure nitrogen to melt simultaneously and complete slagging-off and degassing processing；
(6) after aluminium solution being added in Sodium acetate trihydrate, potassium fluoroaluminate, cryolite, potassium chloride, sodium chloride, progress 5~
The mechanical stirring of 10min carries out degasification operation with rotary degassing machine again later, and dynamic measures H2Content works as H2Content reaches
Aluminum melt is cast into the cylinder bar of 200~400mm of diameter, this at 450-550 DEG C when 0.2~0.4mL/100g Al
Cylinder bar carries out hot extrusion deformation processing, finally obtains combined processing agent material.
Preferably, the pyrophillite ingredient are as follows: Al2O326~36wt%, K2O+Na2O is 0.05~0.5wt%, Fe2O3+
TiO2It is 0.04~1.0wt%, surplus SiO for 0.1~0.8wt%, CaO+MgO2, loss on ignition≤5%, water content is less than
0.3%, the partial size of the pyrophyllite powder is 150~250 mesh, and the extrusion ratio of the hot extrusion deformation processing is 10~20:1.
A kind of aluminium alloy preparation method carries out rotten place to transcocrystallized Al-Si alloy using above-mentioned combined processing agent material
Reason, the specific steps are as follows:
(1) melting in induction furnace by transcocrystallized Al-Si alloy adjusts 740-750 DEG C of smelting temperature, smelting time
25min；The powder that combined processing agent material is ground to 20~25 μm of partial size is spare；
(2) multiple in 740-760 DEG C of investment under 400~800rpm stirring condition after transcocrystallized Al-Si alloy is completely melt
Processing agent material is closed, additional amount is 0.6~1.5wt% of transcocrystallized Al-Si alloy, and combined processing agent material is completely forced into
Solution liquid level is hereinafter, being subsequently agitated for 3~6min, stopping stirring and standing heat preservation 10-20min；Solution is carried out when standing heat preservation
Ultrasonic treatment, frequency are 30~60kHz, and the processing time is 6~10min, and melt is cooled to 725-730 DEG C, add 0.3~
0.5wt% composite treating agent material powder, is cast in casting mold after mixing evenly；
(3) it is demoulded after natural cooling, 340~400 DEG C of solid solution 30min are air-cooled, 100~130 DEG C of timeliness 20~40h, air-cooled
Up to aluminium alloy.
Preferably, the combined processing agent material is prepared using method described in claim 4.
Preferably, the transcocrystallized Al-Si alloy ingredient is Si 20-24%, Cu 1.0-2.0%, Ni by weight percentage
1.1-1.6%, Mg1.0-1.6%, impurity≤0.6%, surplus Al.
It is that the present invention obtains the utility model has the advantages that
(1) pyrophyllite powder in molybdic acid RE composite and praseodymium element can change Sodium acetate trihydrate, aluminium oxide, fluorine
Potassium aluminate, strontium nitrate, potassium chloride, cryolite, sodium chloride, boron carbide, calcium oxide, sodium molybdate, praseodymium nitrate, zinc oxide, tar,
The form and size for the harmful phase that the impurity elements such as calcium, iron, lead are formed in pyrophyllite powder and transcocrystallized Al-Si alloy, thus reduce
The harm of impurity phase, saves slug removing step；Praseodymium element can also assist improving sodium, strontium alterant to the fine degenerate of Eutectic Silicon in Al-Si Cast Alloys
Effect changes tissue morphology, improves the Metamorphism treatment efficiency for changing alloy phase material；Meanwhile praseodymium nitrate and sodium molybdate calcine shape
At praseodymium molybdic acid sodium salt there is weaker luminous power, a small amount of addition may make aluminium alloy to shine under dark surrounds, fit
For fields such as automobile and interior decorations, without brushing or install luminescent material again.
(2) praseodymium oxide can be resolved under praseodymium nitrate hydrate heat-flash, and praseodymium oxide is mixed valence steady oxide, catalysis
Activity is low, reacts praseodymium nitrate, sodium molybdate in ethanol system in the present invention and generates rare earth molybdenum acid sodium-salt, and with clay composite powder
As the carrier of rare earth molybdenum acid sodium-salt, the defect that Rare Earth Elements of Praseodymium catalytic activity reduces under high temperature can be eliminated, high temperature is significantly improved
RE composite catalysis under melting condition changes the form and size of impurity element harmful phase, improves at Aluminum alloy modification indirectly
Mechanical property after reason.
(3) pyrophyllite powder effectively can help degasification to remove the gred, ultrasonication solution also can effectively degasification, prevent hypereutectic
The material for generating stomata in aluminium alloy castings, therefore being prepared in the present invention while Metamorphism treatment can also degasification slagging-off, save
Remove the gred deaeration step, promotes smelting efficiency, contains a large amount of silica and aluminium oxide in pyrophyllite powder, silica is in melting
Shi Keyu Al reaction generates aluminum oxide and elementary silicon, and aluminum oxide is mingled with the hardness that can further promote alloy, and
The content of Eutectic Silicon in Al-Si Cast Alloys in alloy can be improved in elementary silicon, changes the composition ratio of alloy, further increases transcocrystallized Al-Si alloy
Mechanical property.
(4) present invention prepares sodium, strontium, RE multiple modification using raw material melting once, and raw material adds in three times when melting
Enter, due to the more resistance to scaling loss of rare earth element, thus is firstly added clay composite powder, second of addition strontium nitrate and aluminium oxide, nitre
Sour strontium and fine aluminium form Al-Sr intermediate alloy as strontium alterant, without additional preparation Al-Sr intermediate alloy as raw material, oxygen
Changing aluminium is then used as dispersed phase to be present in combined processing agent material, improves the hardness of transcocrystallized Al-Si alloy；Due to sodium alterant
Intolerant to scaling loss, therefore it is eventually adding Sodium acetate trihydrate, potassium fluoroaluminate, cryolite, potassium chloride, sodium chloride.In the order described above
Raw material is added, the rotten activity of raw material can be retained to greatest extent, and the characteristic of three kinds of alterants is superimposed, reach rotten place
Manage effect stability, and it is long and without preclinical effect to handle effective time, the mechanical property of the alloy after processing have compared with
To significantly improve.
(5) sodium alterant itself has an excellent modification effect, but there are deteriorating time is short and poisoning effect, praseodymium sheet
Body modification effect is unobvious, but sodium and strontium alterant can be assisted to improve modification effect, and strontium alterant itself has air-breathing, price high
Expensive disadvantage, but deteriorating time is long, modification effect is good, and pyrophillite as carrier can degasification, overcome the defect of strontium alterant,
Coarse primary silicon and α-Al phase can be effectively refined after triplicity, overcome number of drawbacks existing for single alterant, have
Go bad rapid-action, the incubation time is short, and effective deteriorating time range is big, dissolves rapidly, modification effect stablizes excellent feature, through locating
Crystalline silicon phase in later transcocrystallized Al-Si alloy to be managed mutually obviously to refine with α-Al, crystal phase partial size can be down to 20 μm or so, so that
The mechanical property of alloy is significantly improved.
Specific embodiment
Below by the description to embodiment, specific embodiments of the present invention will be described in further detail, with side
Those skilled in the art is helped to have more complete, accurate and deep understanding to inventive concept of the invention, technical solution.
Embodiment 1: it is prepared as follows combined processing agent material:
One, the preparation of raw material:
Sodium acetate trihydrate, aluminium oxide, potassium fluoroaluminate, strontium nitrate, potassium chloride, cryolite, sodium molybdate, praseodymium nitrate, chlorination
Sodium, boron carbide, calcium oxide, zinc oxide, Al purity be all larger than 99.9wt%, partial size is 150 mesh, and the tar is middle low temperature coal
Tar.
Pyrophillite ingredient are as follows: Al2O326wt%, K2O+Na2O is 0.05wt%, Fe2O3+TiO2For 0.1wt%, CaO+
MgO is 0.04wt%, surplus SiO2, loss on ignition≤5%, for water content less than 0.3%, the partial size of pyrophyllite powder is 150 mesh.
Transcocrystallized Al-Si alloy ingredient is Si 20% by weight percentage, Cu 1.0%, Ni 1.1%, Mg1.0%, miscellaneous
Matter≤0.6%, surplus Al.
Two, the preparation of combined processing agent material
(1) molybdic acid RE composite is prepared as follows: 10g sodium molybdate being added in 1000mL dehydrated alcohol, is placed in
On magnetic stirring apparatus, the ethanol solution 1000mL of the 4g containing praseodymium nitrate is instilled dropwise, 16h is stirred in 20 DEG C of constant temperature, after solvent volatilization
10h to dry, 450 DEG C of calcining 1h is dried in 60 DEG C of baking ovens, obtains sodium molybdate/praseodymium nitrate calcined material, the sodium molybdate/praseodymium nitrate calcining
1L dehydrated alcohol and 110g pyrophyllite powder is added in the content 55.3wt% of praseodymium molybdic acid sodium salt in object after being cooled to room temperature, even
It is filtered after slurry, precipitating drying is taken to obtain molybdic acid RE composite；
(2) preparation of clay composite powder: compound according to 25wt% boron carbide, 20wt% calcium oxide, 5wt% molybdic acid rare earth
Object, 15wt% zinc oxide, 5wt% tar, remaining is pyrophyllite powder ingredient, and the mix powder outside tar removing is placed in planet ball
Grinding jar ground and mixed, using vacuumize three times pour hydrogen by the way of guarantee in vacuum tank that oxygen content is lower than 1%, prevent material
Oxidation；The troubled liquor containing alterant is obtained with the steel ball in alcohol rinse ball grinder and tank, which is placed in vacuum and is done
In dry case, mixed powder is obtained after vaporized alcohol is complete；
(3) tar is added in mix powder while stirring, mixture after mixing evenly is put into grinding tool and is suppressed
Blocking, compression moulding pressure is 15MPa, is put into roaster after being embedded with graphite powder, naturally cold after 980 DEG C keep the temperature 1 hour
But to room temperature, ground on grinder after removing graphite powder, until particle size at 10 microns to get clay composite powder；
(4) Sodium acetate trihydrate 13wt%, aluminium oxide 5wt%, potassium fluoroaluminate 5wt%, strontium nitrate 13wt%, potassium chloride are pressed
3wt%, cryolite 12wt%, clay composite powder 12wt%, sodium chloride 2wt%, surplus are that Al weighs raw material, and fine aluminium ingot is added
Heat is added after fine aluminium ingot is completely melt as aluminium solution using clay composite powder as first part of raw material to 700 DEG C, and 1000rpm
10min is stirred, the slag that removal aluminium melt surface generates after standing the 5min time；
(5) aluminum melt temperature is increased to 850 DEG C, while the mixing that strontium nitrate and aluminium oxide composition is added to aluminum melt again is equal
Second part of even raw material, 500rpm are stood after stirring 3min, skimming, and use CaF2Powder thoroughly removes surface scum, heat preservation
10min is passed through high pure nitrogen to melt simultaneously and completes slagging-off and degassing processing；
(6) after aluminium solution being added in Sodium acetate trihydrate, potassium fluoroaluminate, cryolite, potassium chloride, sodium chloride, 5min is carried out
Mechanical stirring, carry out degasification operation with rotary degassing machine again later, and dynamic measures H2Content works as H2Content reaches 0.2mL/
Aluminum melt is cast into the cylinder bar of diameter 200mm when 100g Al, the cylinder bar is carried out hot extrusion buckling at 450 DEG C
Shape processing, extrusion ratio 10:1 finally obtain combined processing agent material.
Metamorphism treatment is carried out to transcocrystallized Al-Si alloy using above-mentioned combined processing agent material, the specific steps are as follows:
(1) melting in induction furnace by transcocrystallized Al-Si alloy adjusts 740 DEG C of smelting temperature, smelting time 25min；It will
The powder that combined processing agent material is ground to 20 μm of partial size is spare；
(2) after transcocrystallized Al-Si alloy is completely melt, under 400rpm stirring condition, in 740 DEG C of investment composite treating agents
Material, additional amount are the 0.6wt% of transcocrystallized Al-Si alloy, and combined processing agent material is completely forced into solution liquid level hereinafter,
It is subsequently agitated for 3min, stops stirring and standing heat preservation 10min；Solution is ultrasonically treated when standing heat preservation, frequency is
30kHz, processing time are 6min, and melt is cooled to 725 DEG C, adds 0.3wt% composite treating agent material powder to fill out
Rotten scaling loss amount is mended, is cast in casting mold after mixing evenly；
(3) it is demoulded after natural cooling, 340 DEG C of solid solution 30min are air-cooled, 100 DEG C of timeliness 20h, air-cooled up to aluminium alloy.
Embodiment 2: it is prepared as follows combined processing agent material:
One, the preparation of raw material:
Sodium acetate trihydrate, aluminium oxide, potassium fluoroaluminate, strontium nitrate, potassium chloride, cryolite, sodium molybdate, praseodymium nitrate, chlorination
Sodium, boron carbide, calcium oxide, zinc oxide, Al purity be all larger than 99.9wt%, partial size is 250 mesh, and the tar is high temperature coal tar
Oil.
Pyrophillite ingredient are as follows: Al2O336wt%, K2O+Na2O is 0.5wt%, Fe2O3+TiO2For 0.8wt%, CaO+MgO
For 1.0wt%, surplus SiO2, loss on ignition≤5%, for water content less than 0.3%, the partial size of pyrophyllite powder is 250 mesh.
Transcocrystallized Al-Si alloy ingredient is Si 24% by weight percentage, Cu 2.0%, Ni 1.6%, Mg1.6%, miscellaneous
Matter≤0.6%, surplus Al.
Two, the preparation of combined processing agent material:
(1) molybdic acid RE composite is prepared as follows: 13g sodium molybdate being added in 1000mL dehydrated alcohol, is placed in
On magnetic stirring apparatus, the ethanol solution 1000mL of the 8g containing praseodymium nitrate is instilled dropwise, 29h is stirred in 20 DEG C of constant temperature, after solvent volatilization
12h to dry, 550 DEG C of calcining 4h is dried in 80 DEG C of baking ovens, obtains sodium molybdate/praseodymium nitrate calcined material, the sodium molybdate/praseodymium nitrate calcining
1L dehydrated alcohol and 125g pyrophyllite powder is added in the content 80.9wt% of praseodymium molybdic acid sodium salt in object after being cooled to room temperature, even
It is filtered after slurry, precipitating drying is taken to obtain molybdic acid RE composite；
(2) preparation of clay composite powder: compound according to 28wt% boron carbide, 28wt% calcium oxide, 8wt% molybdic acid rare earth
Object, 18wt% zinc oxide, 8wt% tar, remaining is pyrophyllite powder ingredient, and the mix powder outside tar removing is placed in planet ball
Grinding jar ground and mixed, using vacuumize three times pour hydrogen by the way of guarantee in vacuum tank that oxygen content is lower than 1%, prevent material
Oxidation；The troubled liquor containing alterant is obtained with the steel ball in alcohol rinse ball grinder and tank, which is placed in vacuum and is done
In dry case, mixed powder is obtained after vaporized alcohol is complete；
(3) tar is added in mix powder while stirring, mixture after mixing evenly is put into grinding tool and is suppressed
Blocking, compression moulding pressure is 25MPa, is put into roaster after being embedded with graphite powder, natural after 1150 DEG C keep the temperature 2 hours
Be cooled to room temperature, remove graphite powder after ground on grinder, until particle size at 15 microns to get clay composite powder；
(4) Sodium acetate trihydrate 18wt%, aluminium oxide 9wt%, potassium fluoroaluminate 8wt%, strontium nitrate 16wt%, potassium chloride are pressed
7wt%, cryolite 16wt%, clay composite powder 15wt%, sodium chloride 4wt%, surplus are that Al weighs raw material, and fine aluminium ingot is added
Heat is added after fine aluminium ingot is completely melt as aluminium solution using clay composite powder as first part of raw material to 750 DEG C, and 3000rpm
10min is stirred, the slag that removal aluminium melt surface generates after standing the 5min time；
(5) aluminum melt temperature is increased to 900 DEG C, while the mixing that strontium nitrate and aluminium oxide composition is added to aluminum melt again is equal
Second part of even raw material, 1000rpm are stood after stirring 8min, skimming, and use CaF2Powder thoroughly removes surface scum, heat preservation
10min is passed through high pure nitrogen to melt simultaneously and completes slagging-off and degassing processing；
(6) after aluminium solution being added in Sodium acetate trihydrate, potassium fluoroaluminate, cryolite, potassium chloride, sodium chloride, 10min is carried out
Mechanical stirring, carry out degasification operation with rotary degassing machine again later, and dynamic measures H2Content works as H2Content reaches 0.4mL/
Aluminum melt is cast into the cylinder bar of diameter 400mm when 100g Al, the cylinder bar is carried out hot extrusion buckling at 550 DEG C
Shape processing, extrusion ratio 20:1 finally obtain combined processing agent material.
Metamorphism treatment is carried out to transcocrystallized Al-Si alloy using above-mentioned combined processing agent material, the specific steps are as follows:
(1) melting in induction furnace by transcocrystallized Al-Si alloy adjusts 750 DEG C of smelting temperature, smelting time 25min；It will
The powder that combined processing agent material is ground to 25 μm of partial size is spare；
(2) after transcocrystallized Al-Si alloy is completely melt, under 800rpm stirring condition, in 760 DEG C of investment composite treating agents
Material, additional amount are the 1.5wt% of transcocrystallized Al-Si alloy, and combined processing agent material is completely forced into solution liquid level hereinafter,
It is subsequently agitated for 6min, stops stirring and standing heat preservation 20min；Solution is ultrasonically treated when standing heat preservation, frequency is
60kHz, processing time are 10min, and melt is cooled to 730 DEG C, adds 0.5wt% composite treating agent material powder to fill out
Rotten scaling loss amount is mended, is cast in casting mold after mixing evenly；
(3) it is demoulded after natural cooling, 400 DEG C of solid solution 30min are air-cooled, 130 DEG C of timeliness 40h, air-cooled up to aluminium alloy.
Embodiment 3: it is prepared as follows combined processing agent material:
One, the preparation of raw material:
Sodium acetate trihydrate, aluminium oxide, potassium fluoroaluminate, strontium nitrate, potassium chloride, cryolite, sodium molybdate, praseodymium nitrate, chlorination
Sodium, boron carbide, calcium oxide, zinc oxide, Al purity be all larger than 99.9wt%, partial size is 200 mesh, and the tar is middle low temperature coal
Tar.
Pyrophillite ingredient are as follows: Al2O331wt%, K2O+Na2O is 0.275wt%, Fe2O3+TiO2For 0.45wt%, CaO+
MgO is 0.55wt%, surplus SiO2, loss on ignition≤5%, for water content less than 0.3%, the partial size of pyrophyllite powder is 200 mesh.
Transcocrystallized Al-Si alloy ingredient is Si 22% by weight percentage, Cu 1.5%, Ni 1.35%, Mg1.3%, miscellaneous
Matter≤0.6%, surplus Al.
Two, the preparation of combined processing agent material
(1) molybdic acid RE composite is prepared as follows: 11.5g sodium molybdate being added in 1000mL dehydrated alcohol, sets
In the ethanol solution 1000mL on magnetic stirring apparatus, instilling the 6g containing praseodymium nitrate dropwise, 22h, solvent volatilization are stirred in 20 DEG C of constant temperature
11h is dried in 70 DEG C of baking ovens afterwards to doing, 500 DEG C of calcining 2.5h obtain sodium molybdate/praseodymium nitrate calcined material, the sodium molybdate/praseodymium nitrate
1L dehydrated alcohol and 118g pyrophillite is added in the content 62.6wt% of praseodymium molybdic acid sodium salt in calcined material after being cooled to room temperature
Powder filters after homogenate, and precipitating drying is taken to obtain molybdic acid RE composite；
(2) preparation of clay composite powder: multiple according to 26.5wt% boron carbide, 24wt% calcium oxide, 6.5wt% molybdic acid rare earth
Object, 16.5wt% zinc oxide are closed, 6.5wt% tar, remaining is pyrophyllite powder ingredient, and the mix powder outside tar removing is placed in
Planetary ball mill tank ground and mixed, using vacuumize three times pour hydrogen by the way of guarantee in vacuum tank that oxygen content is lower than 1%, prevent
Only material aoxidizes；The troubled liquor containing alterant is obtained with the steel ball in alcohol rinse ball grinder and tank, which is placed in
In vacuum oven, mixed powder is obtained after vaporized alcohol is complete；
(3) tar is added in mix powder while stirring, mixture after mixing evenly is put into grinding tool and is suppressed
Blocking, compression moulding pressure is 20MPa, is put into roaster after being embedded with graphite powder, after 1060 DEG C keep the temperature 1.5 hours, from
So be cooled to room temperature, remove graphite powder after ground on grinder, until particle size at 13 microns to get clay composite powder；
(4) Sodium acetate trihydrate 15.5wt%, aluminium oxide 7wt%, potassium fluoroaluminate 6.5wt%, strontium nitrate 14.5wt%, chlorine are pressed
Changing potassium 5wt%, cryolite 14wt%, clay composite powder 13.5wt%, sodium chloride 3wt%, surplus is that Al weighs raw material, will be pure
Aluminium ingot is heated to 725 DEG C, is added after fine aluminium ingot is completely melt as aluminium solution using clay composite powder as first part of raw material, and
2000rpm stirs 10min, the slag that removal aluminium melt surface generates after standing the 5min time；
(5) aluminum melt temperature is increased to 875 DEG C, while the mixing that strontium nitrate and aluminium oxide composition is added to aluminum melt again is equal
Second part of even raw material, 750rpm are stood after stirring 5min, skimming, and use CaF2Powder thoroughly removes surface scum, heat preservation
10min is passed through high pure nitrogen to melt simultaneously and completes slagging-off and degassing processing；
(6) after aluminium solution being added in Sodium acetate trihydrate, potassium fluoroaluminate, cryolite, potassium chloride, sodium chloride, 7min is carried out
Mechanical stirring, carry out 3min degasification operation with rotary degassing machine again later, and dynamic measures H2Content works as H2Content reaches
Aluminum melt is cast into the cylinder bar of diameter 300mm when 0.3mL/100g Al, the cylinder bar is carried out heat at 500 DEG C
It is squeezed and deformed processing, extrusion ratio 15:1 finally obtains combined processing agent material.
Metamorphism treatment is carried out to transcocrystallized Al-Si alloy using above-mentioned combined processing agent material, the specific steps are as follows:
(1) melting in induction furnace by transcocrystallized Al-Si alloy adjusts 745 DEG C of smelting temperature, smelting time 25min；It will
The powder that combined processing agent material is ground to 23 μm of partial size is spare；
(2) after transcocrystallized Al-Si alloy is completely melt, under 600rpm stirring condition, in 750 DEG C of investment composite treating agents
Material, additional amount are the 1wt% of transcocrystallized Al-Si alloy, and combined processing agent material is completely forced into solution liquid level hereinafter, with
After stir 4.5min, stop stirring and simultaneously stand heat preservation 15min；Solution is ultrasonically treated when standing heat preservation, frequency is
45kHz, processing time are 8min, and melt is cooled to 728 DEG C, adds 0.4wt% composite treating agent material powder to fill out
Rotten scaling loss amount is mended, is cast in casting mold after mixing evenly；
(3) it is demoulded after natural cooling, 370 DEG C of solid solution 30min are air-cooled, 115 DEG C of timeliness 30h, air-cooled up to aluminium alloy.
Comparative examples 1: other are same as Example 3, the difference is that RE composite replaces with praseodymium nitrate.
Comparative examples 2: other are same as Example 3, the difference is that pyrophyllite powder is replaced using simple substance aluminium powder.
Comparative examples 3: other are same as Example 3, the difference is that original is added regardless of three steps in preparation process
Other whole raw materials are directly added after fine aluminium fusing and carry out melting for material, and heat preservation stands 30min after 750rpm stirs 10min, altogether
Melting 40min.
Comparative examples 4: using alterant and Modification Manners disclosed in Chinese patent CN201610732543.1 to mistake
Cocrystallized Al-Si alloy carries out Metamorphism treatment, and gained aluminium alloy is compareed for subsequent mechanical property test.
1, Mechanics Performance Testing
The hypereutectic aluminum-silicon alloy casting prepared in Examples 1 to 3 and comparative examples 1~4 is subjected to mechanical property inspection
It surveys and SEM observes crystal phase size.
By obtained sample by GB6397-86, it is machined to the short tensile test bar of 8mm of standard, it is omnipotent in Controlled by micro computer
Tension test is carried out on testing machine, surveys its tensile strength, hardness and elongation, and final result takes the average value of 4 samples.As a result
It is shown in Table 1.
1 hypereutectic aluminum-silicon alloy casting mechanics properties testing result of table
2, metallographic measures
Sample is taken at the centre of alloy coupon sample, and by polishing, polishing, it is microcosmic to observe its under an optical microscope
Tissue takes 5 different visuals field, and α-Al phase and eutectic silicon crystal size, statistical result are shown in Table 2 in each visual field of Observe and measure.
2 α-Al phase of table and eutectic silicon crystal size testing result
| Group | α-Al phase size (μm) | Eutectic silicon size (μm) |
| Embodiment 1 | 28.1±2.0 | 21.1±1.1 |
| Embodiment 2 | 26.2±1.7 | 18.8±1.7 |
| Embodiment 3 | 26.3±3.3 | 19.3±1.3 |
| Comparative examples 1 | 47.9±2.2 | 42.3±5.3 |
| Comparative examples 2 | 34.3±2.3 | 30.3±1.4 |
| Comparative examples 3 | 39.8±2.1 | 35.8±1.2 |
| Comparative examples 4 | 44.2±2.8 | 36.8±3.1 |
Table 1 combine table 2 the result shows that, comparative examples 1 due to use praseodymium nitrate, forged in the preparation process high temperature of material
Burning is depleted by the catalytic activity of praseodymium with melting, the modification effect for improving sodium, strontium alterant can not be assisted, with reality
It applies example 3 to compare, modification effect is poor, so that α-Al phase and eutectic silicon crystal are larger, causes the mechanical property of alloy significant
It reduces.But the crystal size of Examples 1 to 3 illustrates the change alloy phase prepared in the present invention significantly less than comparative examples 4
The Metamorphism treatment significant effect of material is better than Cu-P intermediate alloy alterant, and crystal more refines, and solid solution and timeliness are in preferred temperature
Under degree and time, crystal habit is uniformly tiny graininess, and modification effect is stablized, so that the power of hypereutectic aluminum-silicon alloy casting
Performance is learned also to be obviously improved.Comparative examples 3 are in the preparation process of combined processing agent material not according to alterant property point
The preparation of cloth adding raw materials, product mesometamorphism agent loss of activity is serious, causes its modification effect significantly lower than comparative examples 1~3.
3, hole is observed
After sample SEM scanning, each sample takes 5 different visuals field, observes in the single visual field with the presence or absence of hole and each
Average cell number in the visual field, the results are shown in Table 3.
3 sample hole of table observes result
| Group | With the presence or absence of hole | Numbers of hole |
| Embodiment 1 | It is no | 0 |
| Embodiment 2 | It is no | 0 |
| Embodiment 3 | It is no | 0 |
| Comparative examples 1 | It is | 0.2 |
| Comparative examples 2 | It is | 3.6 |
| Comparative examples 3 | It is | 0.4 |
| Comparative examples 4 | It is | 0.6 |
Table 1 combine table 3 statistics indicate that, without using pyrophyllite powder in comparative examples 2, also do not carry out slagging-off except jia bombardier
Suddenly, cause alloy-steel casting Hole number more, so that the mechanical property of alloy significantly reduces.It is not also carried out in Examples 1 to 3
Remove the gred degasification operation, but due to joined pyrophyllite powder, degasification operation is completed while Metamorphism treatment, and degassing effect is preferable,
So that hole is not present in final alloy-steel casting.Although using refinement step in comparative examples 4, since Cu-P becomes
Matter agent deteriorating time is longer, causes solution air-breathing serious, so that casting inevitably has hole, and there are copper segregation is existing
As the formation of hole and segregation is unfavorable for subsequent forging molding and mechanical property is promoted.
4, the measurement and comparison of deteriorating time range
By the rotten agent material prepared in comparative examples 4 and embodiment 3 according to the alloy preparation method in embodiment 3 at
Transcocrystallized Al-Si alloy is managed, the measurement of deteriorating time range is carried out, the method is as follows:
After transcocrystallized Al-Si alloy is melted, it is separately added into different rotten agent materials, mixing time 5min stands and becomes
The vacuum time is 1min, 5min, 10min, 15min, and 20min, 40min, 80min, 160min, 240min are measured not respectively
With the crystal size of Eutectic Silicon in Al-Si Cast Alloys in the alloy prepared under deteriorating time, it the results are shown in Table 4:
In 4 alloy of table Eutectic Silicon in Al-Si Cast Alloys crystal size with time-histories variation
| Deteriorating time (min) | Comparative examples 4 | Comparative examples 3 | Embodiment 3 |
| 1 | 99.2μm | 70.8μm | 40.7μm |
| 5 | 89.1μm | 53.4μm | 26.8μm |
| 10 | 77.6μm | 43.7μm | 23.4μm |
| 15 | 68.3μm | 37.6μm | 21.7μm |
| 20 | 55.6μm | 35.1μm | 18.3μm |
| 40 | 37.4μm | 44.4μm | 19.5μm |
| 80 | 45.8μm | 73.3μm | 20.1μm |
| 160 | 66.3μm | 88.6μm | 23.8μm |
| 240 | 89.8μm | 94.3μm | 33.2μm |
As seen from the results in Table 4, the rotten agent material prepared in embodiment 3 it is rotten breed 1min after can quickly generate change
Matter effect, and reach rotten stationary phase in 10min, the sustainable 240min or more of stable modification effect, effective deteriorating time
Range spans are big, can meet effective rotten duration demand of most of aluminium alloy smeltings, and prepare in comparative examples 4 rotten
Material just starts to generate optimal modification effect in 20min, and modification effect is obviously deteriorated after 80min, and effective deteriorating time is only
For 1h or so, although this is because Cu-P alloy can significantly extend deteriorating time compared with Na alterant, under high melt,
With the extension of deteriorating time, alterant still can gradually scaling loss, modification effect be deteriorated, and in rotten 80min, modification effect is aobvious
Work is worse than embodiment 3.It is directly added into whole raw materials in comparative examples 3 and carries out melting, the scaling loss of sodium alterant in fusion process
Seriously, modification effect works more slow, goes bad loss of effect in 80min totally, deteriorating time is shorter, modification effect
Mainly from strontium alterant, but due in material prescription strontium element raw material it is less, modification effect be deteriorated.
5, luminous power is tested
The luminous power under aluminium alloy dark room conditions is detected, the results are shown in Table 5:
The measurement of 5 aluminium alloy luminous power of table
For 5 result of table as it can be seen that comparative examples 4 are without rare earth element and without luminous power, the present invention becomes aluminium alloy
Matter processing is simultaneously because introduce praseodymium molybdic acid sodium salt so that aluminium alloy has certain aura, and in comparative examples 1 by
In do not form praseodymium molybdic acid sodium salt and make praseodymium do not have luminous power.
In conclusion the pyrophyllite powder and praseodymium element in molybdic acid RE composite can change Sodium acetate trihydrate, oxygen
Change aluminium, potassium fluoroaluminate, strontium nitrate, potassium chloride, cryolite, sodium chloride, boron carbide, calcium oxide, sodium molybdate, praseodymium nitrate, oxidation
The form and size for the harmful phase that the impurity elements such as calcium, iron, lead are formed in zinc, tar, pyrophyllite powder and transcocrystallized Al-Si alloy,
Thus the harm for reducing impurity phase, saves slug removing step；Praseodymium element can also assist improving sodium, strontium alterant to Eutectic Silicon in Al-Si Cast Alloys
Fine degenerate effect changes tissue morphology, improves the Metamorphism treatment efficiency for changing alloy phase material；Meanwhile praseodymium nitrate and molybdic acid
Sodium calcines the praseodymium molybdic acid sodium salt to be formed with weaker luminous power, and a small amount of addition may make aluminium alloy under dark surrounds
It shines, is suitable for the fields such as automobile and interior decoration, without brushing or install luminescent material again.Meeting under praseodymium nitrate hydrate heat-flash
Praseodymium oxide is resolved into, and praseodymium oxide is mixed valence steady oxide, catalytic activity is low, by praseodymium nitrate, sodium molybdate in the present invention
Reaction generates rare earth molybdenum acid sodium-salt in ethanol system, and using clay composite powder as the carrier of rare earth molybdenum acid sodium-salt, can eliminate
The defect that Rare Earth Elements of Praseodymium catalytic activity reduces under high temperature significantly improves the RE composite catalysis change under the conditions of high melt
The form and size of impurity element harmful phase improve Aluminum alloy modification treated mechanical property indirectly.Pyrophyllite powder can have
Effect help degasification to remove the gred, ultrasonication solution also can effectively degasification, prevent from generating stomata in hypereutectic aluminium alloy castings, therefore
The material prepared in the present invention while Metamorphism treatment can also degasification slagging-off, save slagging-off deaeration step, promote smelting efficiency,
Contain a large amount of silica and aluminium oxide in pyrophyllite powder, silica can be reacted in melting with Al generates aluminum oxide
And elementary silicon, aluminum oxide is mingled with the hardness that can further promote alloy, and Eutectic Silicon in Al-Si Cast Alloys in alloy can be improved in elementary silicon
Content changes the composition ratio of alloy, further increases the mechanical property of transcocrystallized Al-Si alloy.The present invention is primary using raw material
Melting prepares sodium, strontium, RE multiple modification, and raw material is added in three times when melting, due to the more resistance to scaling loss of rare earth element, thus
It is firstly added clay composite powder, second of addition strontium nitrate and aluminium oxide, strontium nitrate and fine aluminium form the conduct of Al-Sr intermediate alloy
Strontium alterant, without additional preparation Al-Sr intermediate alloy as raw material, aluminium oxide is then used as dispersed phase to be present in composite treating agent
In material, the hardness of transcocrystallized Al-Si alloy is improved；Since sodium alterant is intolerant to scaling loss, be eventually adding Sodium acetate trihydrate,
Potassium fluoroaluminate, cryolite, potassium chloride, sodium chloride.Raw material is added in the order described above, raw material can be retained to greatest extent
Rotten activity, and the characteristic of three kinds of alterants is superimposed, reach Metamorphism treatment effect stability, and handle effective time length and nothing
Preclinical effect, the mechanical property of the alloy after processing, which has, more to be significantly improved.Sodium alterant itself has excellent
Modification effect, but there are deteriorating time is short and poisoning effect, praseodymium modification effect itself is unobvious, but sodium and strontium can be assisted to become
Matter agent improves modification effect, and strontium alterant itself has the shortcomings that air-breathing, expensive, but deteriorating time is long, and modification effect is good,
And pyrophillite as carrier can degasification, overcome the defect of strontium alterant, coarse primary crystal can be effectively refined after triplicity
Silicon and α-Al phase, overcome number of drawbacks existing for single alterant, and rapid-action with going bad, the incubation time is short, when effectively rotten
Between range it is big, dissolve rapidly, modification effect stablizes excellent feature, crystalline silicon phase in the transcocrystallized Al-Si alloy after processing
With α-Al mutually obvious refinement, crystal phase partial size can be down to 20 μm or so, so that the mechanical property of alloy is significantly improved.
The above examples only illustrate the technical idea of the present invention, and this does not limit the scope of protection of the present invention, all
According to the technical idea provided by the invention, any changes made on the basis of the technical scheme each falls within the scope of the present invention
Within；The technology that the present invention is not directed to can be realized by the prior art.
Claims (7)
1. a kind of combined processing agent material, which is characterized in that be grouped as by the group of following weight ratio: Sodium acetate trihydrate 13-18%,
Aluminium oxide 5-9%, potassium fluoroaluminate 5-8%, strontium nitrate 13-16%, potassium chloride 3-7%, cryolite 12-16%, clay are compound
Powder 12-15%, 2~4% sodium chloride, surplus Al；
The clay composite powder boron carbide containing 25-28wt%, 20-28wt% calcium oxide, 5-8wt% molybdic acid RE composite, 15-
18wt% zinc oxide, 5-8wt% tar, surplus are pyrophyllite powder；The molybdic acid RE composite is calcined by sodium molybdate/praseodymium nitrate
Object and pyrophyllite powder composition.
2. a kind of combined processing agent material according to claim 1, it is characterised in that: the Sodium acetate trihydrate, oxidation
Aluminium, potassium fluoroaluminate, strontium nitrate, potassium chloride, cryolite, sodium molybdate, praseodymium nitrate, sodium chloride, boron carbide, calcium oxide, zinc oxide,
The purity of Al is all larger than 99.9wt%, and partial size is 150~250 mesh, and the tar is middle coalite tar；Sodium molybdate/the nitre
55.3~80.9wt% of content of praseodymium molybdic acid sodium salt in sour praseodymium calcined material.
3. a kind of preparation method of combined processing agent material as claimed in claim 1 or 2, which is characterized in that comprising following specific
Step:
(1) molybdic acid RE composite is prepared as follows: 10-13g sodium molybdate being added in 1000mL dehydrated alcohol, is placed in magnetic
On power blender, the ethanol solution 1000mL of the 4-8g containing praseodymium nitrate is instilled dropwise, stirs 16-29h, solvent volatilization in 20 DEG C of constant temperature
10-12h is dried in 60-80 DEG C of baking oven afterwards to doing, 450~550 DEG C of 1~4h of calcining obtain sodium molybdate/praseodymium nitrate calcined material, cooling
1L dehydrated alcohol and 110-125g pyrophyllite powder are added after to room temperature, is filtered after homogenate, precipitating drying is taken to obtain molybdic acid rare earth
Compound；
(2) preparation of clay composite powder: multiple according to 25-28wt% boron carbide, 20-28wt% calcium oxide, 5-8wt% molybdic acid rare earth
Object, 15-18wt% zinc oxide are closed, 5-8wt% tar, remaining is pyrophyllite powder ingredient, and the mix powder outside tar removing is set
In planetary ball mill tank ground and mixed, using vacuumize three times pour hydrogen by the way of guarantee that oxygen content is lower than 1% in vacuum tank,
Prevent material from aoxidizing；The troubled liquor containing alterant is obtained with the steel ball in alcohol rinse ball grinder and tank, which is set
In a vacuum drying oven, mixed powder is obtained after vaporized alcohol is complete；
(3) tar is added in mix powder while stirring, mixture after mixing evenly is put into briquet in grinding tool,
Compression moulding pressure is 15~25MPa, is put into roaster after being embedded with graphite powder, at 980-1150 DEG C after heat preservation 1-2 hours,
Cooled to room temperature is ground on grinder after removing graphite powder, until particle size is multiple to get clay at 10~15 microns
Close powder；
(4) Sodium acetate trihydrate 13-18wt%, aluminium oxide 5-9wt%, potassium fluoroaluminate 5-8wt%, strontium nitrate 13-16wt%, chlorine are pressed
Change potassium 3-7wt%, cryolite 12-16wt%, clay composite powder 12-15wt%, 2~4wt% sodium chloride, surplus to weigh for Al
Fine aluminium ingot is heated to 700-750 DEG C by raw material, using clay composite powder as first part after fine aluminium ingot is completely melt as aluminium solution
Raw material is added, and 1000~3000rpm stirs 10min, the slag that removal aluminium melt surface generates after standing the 5min time；
(5) aluminum melt temperature is increased to 850-900 DEG C, while the mixing that strontium nitrate and aluminium oxide composition is added to aluminum melt again is equal
Second part of even raw material, 500~1000rpm are stood after stirring 3~8min, skimming, and use CaF2It is floating that powder thoroughly removes surface
Slag, heat preservation 10min are passed through high pure nitrogen to melt simultaneously and complete slagging-off and degassing processing；
(6) after aluminium solution being added in Sodium acetate trihydrate, potassium fluoroaluminate, cryolite, potassium chloride, sodium chloride, 5~10min is carried out
Mechanical stirring, carry out degasification operation with rotary degassing machine again later, and dynamic measures H2Content works as H2Content reaches 0.2~
Aluminum melt is cast into the cylinder bar of 200~400mm of diameter, the cylindrical rod at 450-550 DEG C when 0.4mL/100g Al
Material carries out hot extrusion deformation processing, finally obtains combined processing agent material.
4. a kind of preparation method of combined processing agent material according to claim 3, it is characterised in that: pyrophillite ingredient
Are as follows: Al2O326~36wt%, K2O+Na2O is 0.05~0.5wt%, Fe2O3+TiO2It is for 0.1~0.8wt%, CaO+MgO
0.04~1.0wt%, surplus SiO2, loss on ignition≤5%, for water content less than 0.3%, the partial size of the pyrophyllite powder is 150
The extrusion ratio of~250 mesh, the hot extrusion deformation processing is 10~20:1.
5. a kind of aluminium alloy preparation method, which is characterized in that using combined processing agent material described in claims 1 or 2 to mistake
Cocrystallized Al-Si alloy carries out Metamorphism treatment, the specific steps are as follows:
(1) melting in induction furnace by transcocrystallized Al-Si alloy adjusts 740-750 DEG C of smelting temperature, smelting time 25min；It will
The powder that combined processing agent material is ground to 20~25 μm of partial size is spare；
(2) after transcocrystallized Al-Si alloy is completely melt, under 400~800rpm stirring condition, at the 740-760 DEG C of compound place of investment
Agent material is managed, additional amount is 0.6~1.5wt% of transcocrystallized Al-Si alloy, and combined processing agent material is completely forced into solution
Liquid level is hereinafter, being subsequently agitated for 3~6min, stopping stirring and standing heat preservation 10-20min；Ultrasound is carried out to solution when standing heat preservation
Processing, frequency are 30~60kHz, and the processing time is 6~10min, and melt is cooled to 725-730 DEG C, add 0.3~
0.5wt% composite treating agent material powder, is cast in casting mold after mixing evenly；
(3) demoulded after natural cooling, 340~400 DEG C of solid solution 30min are air-cooled, 100~130 DEG C of timeliness 20~40h, it is air-cooled to obtain the final product
Aluminium alloy.
6. a kind of aluminium alloy preparation method according to claim 5, it is characterised in that: the combined processing agent material uses
It is prepared by method described in claim 4.
7. a kind of aluminium alloy preparation method according to claim 6, it is characterised in that: the transcocrystallized Al-Si alloy ingredient
It is by weight percentage Si 20-24%, Cu1.0-2.0%, Ni 1.1-1.6%, Mg1.0-1.6%, impurity≤0.6% is remaining
Amount is Al.
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Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US4099314A (en) * | 1976-03-10 | 1978-07-11 | Societe De Vente De L'aluminium Pechiney | Method of producing hollow bodies in aluminum-silicon alloys by powder-extrusion |
| CN103173642A (en) * | 2011-12-23 | 2013-06-26 | 秦皇岛开发区美铝合金有限公司 | Refining agent for aluminum alloy in smelting process for automobile hub |
| CN107779618A (en) * | 2016-08-27 | 2018-03-09 | 沈井仁 | A kind of method that Metamorphism treatment prepares transcocrystallized Al-Si alloy |
-
2019
- 2019-04-10 CN CN201910285394.2A patent/CN109943740A/en active Pending
Patent Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US4099314A (en) * | 1976-03-10 | 1978-07-11 | Societe De Vente De L'aluminium Pechiney | Method of producing hollow bodies in aluminum-silicon alloys by powder-extrusion |
| CN103173642A (en) * | 2011-12-23 | 2013-06-26 | 秦皇岛开发区美铝合金有限公司 | Refining agent for aluminum alloy in smelting process for automobile hub |
| CN107779618A (en) * | 2016-08-27 | 2018-03-09 | 沈井仁 | A kind of method that Metamorphism treatment prepares transcocrystallized Al-Si alloy |
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