CN109706357A - It is a kind of to change material of alloy structure and preparation method thereof - Google Patents
It is a kind of to change material of alloy structure and preparation method thereof Download PDFInfo
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- CN109706357A CN109706357A CN201910213400.3A CN201910213400A CN109706357A CN 109706357 A CN109706357 A CN 109706357A CN 201910213400 A CN201910213400 A CN 201910213400A CN 109706357 A CN109706357 A CN 109706357A
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Abstract
The present invention discloses a kind of material that can change alloy structure, be grouped as by the group of following weight ratio: aluminium hydroxide 0.3-0.9%, sodium acetate 3-8%, barium nitrate 11-15%, sodium dihydrogen phosphate 0.5-0.9%, sodium chloride 13-19%, potassium chloride 2-7%, kaolinite composite ceramic 12-18%, surplus is potassium fluotitanate；RE composite containing holmium, aluminium hydroxide can change the form and size of the harmful phase of impurity element formation, alterant element in kaolinite composite ceramics compound powder can effectively refine coarse primary silicon, while Metamorphism treatment can also degasification slagging-off, promoted smelting efficiency.The gap shrinks between powder raw material are made using the method for squeezing calcining in preparation method, be conducive to the metal salts such as sodium, aluminium, potassium, holmium to form metal complex and be fixed in porous ceramics particle, keep modification effect 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 material that can change alloy structure and its preparation side
Method.
Background technique
Silicon mutually president's slabbing under the conditions of autonomous growth, or even the polygonal that appearance is coarse in alusil alloy eutectic
Plate silicon phase, the silicon of these forms mutually isolate Al matrix for serious, cause stress to be concentrated at the tip of Si phase and edges and corners, close
Gold is easy to crack along the boundary of crystal grain or plate Si itself and form crackle, and alloy is made to become fragile, and mechanical performance is especially prolonged
Rate significant decrease is stretched, machining function is also bad.In order to change the existence of silicon, the mechanical property of alloy is improved, for a long time
Since always use Modification Treatment Technique.
There is the member of modification effect to be known as Eutectic Silicon in Al-Si Cast Alloys: sodium (Na), strontium (Sr), sulphur (S), lanthanum (La), cerium (Ce), antimony (Sb),
Tellurium (Te) etc..Current study is concentrated mainly on sodium, strontium, on several alterants such as rare earth, widely applied Al-5Ti-1B, Al-
10Sr fining modifier, there are titanium silicides to poison thinning effect, Sr aggravates " poisoning " mutual between alloy melt air-breathing and Sr, B now
As.It is industrial general also using elemental phosphorous as alterant, but the fierce burning of meeting in elemental phosphorous addition high temperature aluminium alloys liquid, it generates
A large amount of smog pollute air, while also enabling aluminum alloy to liquid and absorbing more gases, make occur hole in casting, are unfavorable for aluminium conjunction
The strength enhancing of golden casting and subsequent forging, and for intermediate alloy, as alterant, there are deterrorations using phosphorus and aluminum
Height, deteriorating time is long, the defect of preparation process complexity, and therefore, urgent need develops a kind of rare-earth base alterant and solves the above problems.
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 bubble, takes the hydrogen of dissolution out of aluminum alloy melt in floating-upward process using these bubbles, escapes into atmosphere.
Preferable refining effect in order to obtain should make the iron pipe for importing gas be pressed into molten bath depths as far as possible, so that the stroke of bubble floating
It lengthens, while the field trash for being sunken to aluminum alloy melt bottom being unlikely to stir again.Iron pipe should be made in aluminum alloy melt when being passed through gas
Inside slowly transverse shifting, so that molten bath has bubble to pass through everywhere.As far as possible using lower venting pressure and speed, because this
The bubble that sample is formed is smaller, expands the surface area of bubble, and since bubble is small, ascent rate is also slow, thus can remove more
Be mingled with and gas.Meanwhile to guarantee good refining effect, the selection of refining temperature should be appropriate, and temperature is excessively high, generates
Bubble is larger and floats quickly, and refining effect is made to be deteriorated.The viscosity of aluminum alloy melt is larger when temperature is too low, is unfavorable for aluminum alloy melt
In gas be sufficiently discharged, equally can also reduce refining effect.It also can effectively degasification with ultrasonication aluminum alloy melt.
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 CN201510732576.1 provides a kind of fining modifier for A356.2 aluminium alloy and refining
The method of A356.2 aluminium alloy, the alterant include 0.01-0.05 parts of Ce and 0.1-0.2 parts by weight by weight
Mg.Fining modifier and method can be realized preferable thin modification effect, and the α-Al and eutectic structure that enable aluminum alloy to are equal
There is apparent thinning effect, is remarkably improved the comprehensive mechanical performance of alloy.
Foregoing invention forms intermediate alloy only with Ce simple substance and magnesium to prepare alterant, and component is simple, and Ce content is high, mentions
High melting cost, and when melting Ce scaling loss amount it is larger, effective smelting time is shorter, although be better than Na or P modifier agent but still
It is unable to satisfy the demand of long-time melting, although Ce-Mg can enable aluminum alloy to α-Al dendrite and gill shape coarse in as-cast structure
Eutectic Silicon Refinement is rotten, but refining slagging-off degasification must be individually carried out before and after Metamorphism treatment, and slagging-off degassing effect directly affects most
Mechanical Properties of Aluminum Alloys afterwards influences aluminium alloy production efficiency, but can not save thus while slagging-off deaeration step is many and diverse.
The research of rare-earth base magnesium alloy is more, is conventional alterant, Metamorphism treatment effect is it is contemplated that hypoeutectic aluminium alloy mechanical property
The promotion of energy is limited.
Summary of the invention
The technical problems to be solved by the invention: for the place that can not go bad simultaneously during current A356.2 aluminium alloy smelting
Reason and slagging-off degasification and the problem of common alterant is ineffective and easy scaling loss, the present invention, which provides, a kind of can change alloy structure
Material, solve the above problems.
In order to solve the above technical problems, the present invention provides technical solution below:
A kind of material that can change alloy structure, is grouped as by the group of following weight ratio: aluminium hydroxide 0.3-0.9%, second
Sour sodium 3-8%, barium nitrate 11-15%, sodium dihydrogen phosphate 0.5-0.9%, sodium chloride 13-19%, potassium chloride 2-7%, kaolinite
Composite ceramic 12-18%, remaining is potassium fluotitanate；
The kaolinite composite ceramic contains 21-26wt% RE composite containing holmium, 13-19wt% vanadium carbide, 0.8-
1.2%wt sodium carbonate, 11-14%wt pitch, remaining is kaolinite powder；The RE composite containing holmium is by phosphotungstic acid/holmium nitrate
Mixture and kaolinite powder composition.
Preferably, the aluminium hydroxide, sodium acetate, barium nitrate, sodium dihydrogen phosphate, sodium chloride, potassium chloride, potassium fluotitanate,
Vanadium carbide, sodium carbonate, phosphotungstic acid, holmium nitrate purity be all larger than 99.9wt%, partial size is 100~200 mesh, and the pitch is coal
Pyrobitumen；Content >=75wt% of rare earth holmium phosphotungstate in the phosphotungstic acid/holmium nitrate mixture.
A kind of preparation method of the above-mentioned material that can change alloy structure includes following specific steps:
(1) RE composite containing holmium is prepared as follows: 15-23g phosphotungstic acid being added in 1000mL dehydrated alcohol, sets
In the ethanol solution 1000mL on magnetic stirring apparatus, instilling the 15-20g containing holmium nitrate dropwise, 36-39h is stirred in 20 DEG C of constant temperature, it is molten
10-12h to dry, 350~400 DEG C of 1~4h of calcining is dried after agent volatilization in 60-70 DEG C of baking oven, obtains phosphotungstic acid/holmium nitrate mixing
Object is added 1L dehydrated alcohol and 200-210g kaolinite powder, filters after homogenate after being cooled to room temperature, take precipitating drying to obtain and contain
Holmium RE composite；
(2) it the preparation of kaolinite composite ceramic: is carbonized according to 21-26wt% RE composite containing holmium, 13-19wt%
Vanadium, 0.8-1.2wt% sodium carbonate, 11-14wt% pitch, remaining is kaolinite powder ingredient, by mix powder in addition to bitumen
Be 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
2%, 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) 250~350 DEG C of pitch pre- heat fusing back stirring sides are added in mix powders, it will after mixing evenly
Mixture is put into briquet in grinding tool after being cooled to 150 DEG C, compression moulding pressure is 35~55MPa, after being embedded with graphite powder
It is put into roaster, at 910-960 DEG C after sintering 1-2 hours, cooled to room temperature then takes out and grinds on grinder,
It, can be stand-by until particle size is at 11~14 microns；
(4) according to aluminium hydroxide 0.3-0.9wt%, sodium acetate 3-8wt%, barium nitrate 11-15wt%, sodium dihydrogen phosphate
0.5-0.9wt%, sodium chloride 13-19wt%, potassium chloride 2-7wt%, kaolinite composite ceramic 12-18wt%, remaining is fluorine
Potassium titanate ingredient, it is then uniform in ground and mixed in the ball mill, by mixture extrusion forming, 50~65MPa of squeeze pressure；
(5) batch briquetting is put into the vacuum drying oven of argon gas again and is sintered, after heat preservation 1-2 hours, taken at 120-140 DEG C
It is cooled to room temperature out, partial size is then ground on grinder at 30~40 microns, obtains alterant powder；
(6) disk is pressed after mixing according to the ratio of 2~4 parts by weight epoxy resin, 95~100 parts by weight alterant powder,
Alterant piece thickness 0.5cm, 1~2cm of diameter is to get the material that can change alloy structure.
Preferably, the salic 30.4~36.6wt% of kaolinite powder, 5.2~11.1wt% of water, iron oxide 0.1~
0.3wt%, 0.12~0.25wt% of antimony oxide, 0.5~0.8wt% of calcium oxide, 1.1~1.3wt% of magnesia, potassium oxide 0.03
~0.15wt%, 0.2~0.35wt% of sodium oxide molybdena, surplus SiO2；The partial size of the kaolinite composite ceramic be 150~
The weight ratio of 200 mesh, the graphite powder and mixture block is 1:300~900, and graphite linings thickness is at least 1~5cm.
A kind of aluminium alloy preparation method carries out rotten place to A356.2 alloy using the above-mentioned material that can change alloy structure
Reason, the specific steps are as follows:
(1) melting in induction furnace by A356.2 alloy adjusts 740-765 DEG C of smelting temperature, smelting time 30min；
(2) after A356.2 alloy is completely melt, under 500~700rpm stirring condition, can change in 750-765 DEG C of investment
The material of alloy structure, additional amount are 1.7~3.5wt% of A356.2 alloy, and disc-shaped material is completely forced into solution liquid
Face is hereinafter, being subsequently agitated for 5~7min, stopping stirring and standing heat preservation 15-25min；Solution is carried out at ultrasound when standing heat preservation
Reason, frequency are 30~60kHz, and the processing time is 10~20min, and melt is cooled to 725-735 DEG C, is cast in casting mold；
(3) it is demoulded after natural cooling, 380~440 DEG C of solid solution 30min are air-cooled, 120~140 DEG C of timeliness 20~40h, air-cooled
Up to aluminium alloy.
Preferably, the material that can change alloy structure is prepared using method described in claim 4.
Preferably, the component of the A356.2 alloy are as follows: Si 6.0~7.0wt%, Fe 0.02~0.06wt%, Cu
0.05~0.1wt%, Mg 0.21~0.33wt%, Mn 0.02~0.06wt%, Zn≤0.02wt%, Ti 0.09~
0.18wt%, impurity content≤0.1wt%, surplus Al.
It is that the present invention obtains the utility model has the advantages that
(1) RE composite containing holmium, aluminium hydroxide can change sodium acetate, barium nitrate, sodium dihydrogen phosphate, sodium chloride, chlorine
What the impurity elements such as zinc, lead were formed in change potassium, potassium fluotitanate, vanadium carbide, sodium carbonate, kaolinite, pitch and A356.2 alloy has
The form and size of evil phase, thus reduce the harm of impurity phase, and auxiliary improves kaolinite composite ceramic and cryolite to altogether
The fine degenerate effect of crystal silicon changes tissue morphology, improves the Metamorphism treatment efficiency for changing alloy phase material；Contain in kaolinite powder
There are a large amount of silica and aluminium oxide, silica can be reacted in melting with Al generates aluminum oxide and elementary silicon, and three
Al 2 O 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 and closes
The composition ratio of gold, further increases the mechanical property of hypoeutectic aluminium silico-aluminum alloy A356.2.
(2) this case treatment effect is stablized, and it is long and without incubation period to handle effective time.The power of alloy after processing
Performance, which has, more to be significantly improved.Sodium chloride described in this case, potassium chloride, RE composite containing holmium, sodium acetate, barium nitrate, phosphorus
Acid dihydride sodium, vanadium carbide, sodium carbonate, potassium fluotitanate can effective refining eutectic silicon, change tissue morphology；Barium nitrate, kaolinite
Powder helps degasification slagging-off.RE composite containing holmium can effectively refine coarse primary silicon, during overcoming alloy molten
Directly add elemental phosphorous generated phosphorus spontaneous combustion problems.RE composite containing holmium, aluminium hydroxide can change impurity element and be formed
Harmful phase form and size, thus reduce impurity phase harm.
(3) holimium oxide can be resolved under holmium nitrate hydrate heat-flash, and holimium oxide is mixed valence steady oxide, catalysis
Activity is low, reacts holmium nitrate, phosphotungstic acid in ethanol system in the present invention and generates rare earth phosphotungstate, and is compound with kaolinite
Carrier of the ceramic powder as rare earth phosphotungstate can eliminate the defect that Rare-earth Element Holmium catalytic activity reduces under high temperature, significantly mention
RE composite catalysis under the conditions of high high melt changes the form and size of impurity element harmful phase, improves aluminium alloy indirectly
Mechanical property after Metamorphism treatment.
(4) Rare-earth Element Holmium in kaolinite composite ceramics compound powder and sodium element cooperate, and can effectively refine
Coarse primary silicon and α-Al phase, overcomes number of drawbacks existing for alloy phosphor alterative, has and goes bad rapid-action, the incubation time
Short, effective deteriorating time range is big, dissolves rapidly, and modification effect stablizes excellent feature, the A356.2 alloy after processing
Mutually obvious refinement, crystal phase partial size can be down to 20 μm or so, obviously mention so that the mechanical property of alloy has middle crystalline silicon phase with α-Al
It is high.
(5) barium nitrate, kaolinite powder effectively can help degasification to remove the gred, ultrasonication solution also can effectively degasification, prevent
The material for only generating stomata in aluminium alloy castings, therefore being prepared in the present invention while Metamorphism treatment can also degasification slagging-off, save
Slagging-off deaeration step is removed, smelting efficiency is promoted.
(6) material that alloy structure can be changed in preparation method using the method preparation for squeezing calcining, so that powder raw material
Between gap shrinks, be conducive to the metal salts such as sodium, aluminium, potassium, holmium formed metal complex, the modification effect of multiple element is folded
Add, while kaolinite powder forms porous ceramics particle under high-temperature calcination, further the fixed metal complex formed of absorption, makes
Complex compound is more stable at high temperature, prevents or slows down the scaling loss of independent alterant when high melt, extends effective deteriorating time.
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 the material that can change alloy structure:
One, the preparation of raw material:
Kaolinite powder salic 30.4wt%, water 5.2wt%, iron oxide 0.1wt%, antimony oxide 0.12wt%, oxidation
Calcium 0.5wt%, magnesia 1.1wt%, potassium oxide 0.03wt%, sodium oxide molybdena 0.2wt%, surplus SiO2；The kaolinite is multiple
The partial size for closing ceramic powder is 150 mesh.
The component of A356.2 alloy are as follows: Si 6.0wt%, Fe 0.02wt%, Cu 0.05wt%, Mg 0.21wt%, Mn
0.02wt%, Zn 0.02wt%, Ti 0.09wt%, impurity content≤0.1wt%, surplus Al.
Aluminium hydroxide, sodium acetate, barium nitrate, sodium dihydrogen phosphate, sodium chloride, potassium chloride, potassium fluotitanate, vanadium carbide, carbonic acid
Sodium, phosphotungstic acid, holmium nitrate purity be all larger than 99.9wt%, partial size is 100 mesh；Pitch is coal tar pitch；
Two, the preparation of the material of alloy structure can be changed
(1) RE composite containing holmium is prepared as follows: 15g phosphotungstic acid being added in 1000mL dehydrated alcohol, is placed in
On magnetic stirring apparatus, the ethanol solution 1000mL of the 15g containing holmium nitrate is instilled dropwise, 36h is stirred in 20 DEG C of constant temperature, after solvent volatilization
10h is dried in 60 DEG C of baking ovens to dry, 350 DEG C of calcining 1h obtain phosphotungstic acid/holmium nitrate mixture, after being cooled to room temperature addition 1L without
Water-ethanol and 200g kaolinite powder, filter after homogenate, and precipitating drying is taken to obtain RE composite containing holmium；Phosphotungstic acid/the nitre
The content of rare earth holmium phosphotungstate is 75wt% in sour holmium mixture, should improve the content of rare earth holmium phosphotungstate as far as possible,
The higher catalytic effect of content is better.
(2) preparation of kaolinite composite ceramic: according to 21wt% RE composite containing holmium, 13wt% vanadium carbide,
0.8wt% sodium carbonate, 11wt% pitch, remaining is kaolinite powder ingredient, and mix powder in addition to bitumen 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 2%, 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) 250 DEG C of pitch pre- heat fusing back stirring sides are added in mix powder, by mixture after mixing evenly
Briquet in grinding tool is put into after being cooled to 150 DEG C, compression moulding pressure is 35MPa, is put into roaster after being embedded with graphite powder
In, at 910 DEG C after sintering 1- hours, cooled to room temperature then takes out and grinds on grinder, until particle size is 11
Micron, can be stand-by；The weight ratio of the graphite powder and mixture block is 1:300, and graphite linings thickness is at least 1cm.
(4) according to aluminium hydroxide 0.3wt%, sodium acetate 3wt%, barium nitrate 11wt%, sodium dihydrogen phosphate 0.5wt%, chlorine
Change sodium 13wt%, potassium chloride 2wt%, kaolinite composite ceramic 12wt%, remaining is potassium fluotitanate ingredient, then in ball milling
Ground and mixed is uniform in machine, by mixture extrusion forming, squeeze pressure 50MPa；
(5) batch briquetting is put into the vacuum drying oven of argon gas again and is sintered, after 120 DEG C keep the temperature 1 hour, take out cooling
To room temperature, it is then ground to partial size on grinder at 30 microns, obtains alterant powder；
(6) disk, alterant piece are pressed after mixing according to the ratio of 2 parts by weight epoxy resin, 95 parts by weight alterant powder
Thick 0.5cm, diameter 1cm is to get the material that can change alloy structure.
Metamorphism treatment is carried out to A356.2 alloy using the above-mentioned material that can change alloy structure, the specific steps are as follows:
(1) melting in induction furnace by A356.2 alloy adjusts 740 DEG C of smelting temperature, smelting time 30min；
(2) after A356.2 alloy is completely melt, under 500rpm stirring condition, alloy structure can be changed in 750 DEG C of investments
Material, additional amount is the 1.7wt% of A356.2 alloy, and disc-shaped material is completely forced into solution liquid level hereinafter, then stirring
5min is mixed, stops stirring and standing heat preservation 15min；Solution is ultrasonically treated when standing heat preservation, frequency 30kHz, processing
Time is 10min, and melt is cooled to 725 DEG C, is cast in casting mold；
(3) it is demoulded after natural cooling, 380 DEG C of solid solution 30min are air-cooled, 120 DEG C of timeliness 20h, air-cooled up to aluminium alloy.
Embodiment 2: it is prepared as follows the material that can change alloy structure:
One, the preparation of raw material:
Kaolinite powder salic 36.6wt%, water 11.1wt%, iron oxide 0.3wt%, antimony oxide 0.25wt%, oxidation
Calcium 0.8wt%, magnesia 1.3wt%, potassium oxide 0.15wt%, sodium oxide molybdena 0.35wt%, surplus SiO2；The kaolinite is multiple
The partial size for closing ceramic powder is 200 mesh,
The component of A356.2 alloy are as follows: Si 7.0wt%, Fe 0.06wt%, Cu 0.1wt%, Mg 0.33wt%, Mn
0.06wt%, Zn 0.01wt%, Ti 0.18wt%, impurity content≤0.1wt%, surplus Al.
Aluminium hydroxide, sodium acetate, barium nitrate, sodium dihydrogen phosphate, sodium chloride, potassium chloride, potassium fluotitanate, vanadium carbide, carbonic acid
Sodium, phosphotungstic acid, holmium nitrate purity be all larger than 99.9wt%, partial size is 200 mesh；Pitch is bitumen；
Two, the preparation of the material of alloy structure can be changed
(1) RE composite containing holmium is prepared as follows: 23g phosphotungstic acid being added in 1000mL dehydrated alcohol, is placed in
On magnetic stirring apparatus, the ethanol solution 1000mL of the 20g containing holmium nitrate is instilled dropwise, 39h is stirred in 20 DEG C of constant temperature, after solvent volatilization
12h is dried in 70 DEG C of baking ovens to dry, 400 DEG C of calcining 4h obtain phosphotungstic acid/holmium nitrate mixture, after being cooled to room temperature addition 1L without
Water-ethanol and 210g kaolinite powder, filter after homogenate, and precipitating drying is taken to obtain RE composite containing holmium；Phosphotungstic acid/the nitre
The content of rare earth holmium phosphotungstate is 85wt% in sour holmium mixture, should improve the content of rare earth holmium phosphotungstate as far as possible,
The higher catalytic effect of content is better.
(2) preparation of kaolinite composite ceramic: according to 26wt% RE composite containing holmium, 19wt% vanadium carbide,
1.2wt% sodium carbonate, 14wt% pitch, remaining is kaolinite powder ingredient, and mix powder in addition to bitumen 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 2%, 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) 350 DEG C of pitch pre- heat fusing back stirring sides are added in mix powder, by mixture after mixing evenly
Briquet in grinding tool is put into after being cooled to 150 DEG C, compression moulding pressure is 55MPa, is put into roaster after being embedded with graphite powder
In, after 960 DEG C are sintered 2 hours, cooled to room temperature then takes out and grinds on grinder, until particle size is 14
Micron, can be stand-by；The weight ratio of the graphite powder and mixture block is 1:900, and graphite linings thickness is at least 5cm.
(4) according to aluminium hydroxide 0.9wt%, sodium acetate 8wt%, barium nitrate 15wt%, sodium dihydrogen phosphate 0.9wt%, chlorine
Change sodium 19wt%, potassium chloride 7wt%, kaolinite composite ceramic 18wt%, remaining is potassium fluotitanate ingredient, then in ball milling
Ground and mixed is uniform in machine, by mixture extrusion forming, squeeze pressure 65MPa；
(5) batch briquetting is put into the vacuum drying oven of argon gas again and is sintered, after 140 DEG C keep the temperature 2 hours, take out cooling
To room temperature, it is then ground to partial size on grinder at 40 microns, obtains alterant powder；
(6) disk, alterant piece are pressed after mixing according to the ratio of 4 parts by weight epoxy resin, 100 parts by weight alterant powder
Thick 0.5cm, diameter 2cm is to get the material that can change alloy structure.
Metamorphism treatment is carried out to A356.2 alloy using the above-mentioned material that can change alloy structure, the specific steps are as follows:
(1) melting in induction furnace by A356.2 alloy adjusts 765 DEG C of smelting temperature, smelting time 30min；
(2) after A356.2 alloy is completely melt, under 700rpm stirring condition, alloy structure can be changed in 765 DEG C of investments
Material, additional amount is the 3.5wt% of A356.2 alloy, and disc-shaped material is completely forced into solution liquid level hereinafter, then stirring
7min is mixed, stops stirring and standing heat preservation 25min；Solution is ultrasonically treated when standing heat preservation, frequency 60kHz, processing
Time is 20min, and melt is cooled to 735 DEG C, is cast in casting mold；
(3) it is demoulded after natural cooling, 440 DEG C of solid solution 30min are air-cooled, 140 DEG C of timeliness 40h, air-cooled up to aluminium alloy.
Embodiment 3: it is prepared as follows the material that can change alloy structure:
One, the preparation of raw material:
Kaolinite powder salic 33.1wt%, water 8.6wt%, iron oxide 0.2wt%, antimony oxide 0.19wt%, oxidation
Calcium 0.65wt%, magnesia 1.2wt%, potassium oxide 0.09wt%, sodium oxide molybdena 0.28wt%, surplus SiO2；The kaolinite
The partial size of composite ceramic is 180 mesh,
The component of A356.2 alloy are as follows: Si 6.5wt%, Fe 0.04wt%, Cu 0.07wt%, Mg 0.27wt%, Mn
0.04wt%, Zn 0.01wt%, Ti 0.13wt%, impurity content≤0.1wt%, surplus Al.
Aluminium hydroxide, sodium acetate, barium nitrate, sodium dihydrogen phosphate, sodium chloride, potassium chloride, potassium fluotitanate, vanadium carbide, carbonic acid
Sodium, phosphotungstic acid, holmium nitrate purity be all larger than 99.9wt%, partial size is 150 mesh；Pitch is asphalt；
Two, the preparation of the material of alloy structure can be changed
(1) RE composite containing holmium is prepared as follows: 19g phosphotungstic acid being added in 1000mL dehydrated alcohol, is placed in
On magnetic stirring apparatus, the ethanol solution 1000mL of the 17g containing holmium nitrate is instilled dropwise, 37h is stirred in 20 DEG C of constant temperature, after solvent volatilization
11.5h is dried in 65 DEG C of baking ovens to doing, 375 DEG C of calcining 2.5h obtain phosphotungstic acid/holmium nitrate mixture, are added after being cooled to room temperature
1L dehydrated alcohol and 205g kaolinite powder, filter after homogenate, and precipitating drying is taken to obtain RE composite containing holmium；The phosphorus tungsten
The content 88wt% of rare earth holmium phosphotungstate in acid/holmium nitrate mixture, should improve as far as possible containing for rare earth holmium phosphotungstate
Amount, the higher catalytic effect of content are better.
(2) preparation of kaolinite composite ceramic: according to 23.5wt% RE composite containing holmium, 16wt% vanadium carbide,
1.0wt% sodium carbonate, 12.5wt% pitch, remaining is kaolinite powder ingredient, and mix powder in addition to bitumen is placed in planet
Ball grinder ground and mixed, using vacuumize three times pour hydrogen by the way of guarantee in vacuum tank that oxygen content is lower than 2%, prevent object
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
In drying box, mixed powder is obtained after vaporized alcohol is complete；
(3) 300 DEG C of pitch pre- heat fusing back stirring sides are added in mix powder, by mixture after mixing evenly
Briquet in grinding tool is put into after being cooled to 150 DEG C, compression moulding pressure is 45MPa, is put into roaster after being embedded with graphite powder
In, after 935 DEG C are sintered 1.5 hours, cooled to room temperature then takes out and grinds on grinder, until particle size exists
It 12.5 microns, can be stand-by；The weight ratio of the graphite powder and mixture block is 1:600, and graphite linings thickness is at least 3cm.
(4) according to aluminium hydroxide 0.6wt%, sodium acetate 5.5wt%, barium nitrate 13wt%, sodium dihydrogen phosphate 0.7wt%,
Sodium chloride 16wt%, potassium chloride 4.5wt%, kaolinite composite ceramic 15wt%, remaining be potassium fluotitanate ingredient, then
Ground and mixed is uniform in ball mill, by mixture extrusion forming, squeeze pressure 58MPa；
(5) batch briquetting is put into the vacuum drying oven of argon gas again and is sintered, after 130 DEG C keep the temperature 1.5 hours, taken out cold
But to room temperature, it is then ground to partial size on grinder at 35 microns, obtains alterant powder；
(6) disk, alterant piece are pressed after mixing according to the ratio of 3 parts by weight epoxy resin, 98 parts by weight alterant powder
Thick 0.5cm, diameter 1.5cm is to get the material that can change alloy structure.
Metamorphism treatment is carried out to A356.2 alloy using the above-mentioned material that can change alloy structure, the specific steps are as follows:
(1) melting in induction furnace by A356.2 alloy adjusts 750 DEG C of smelting temperature, smelting time 30min；
(2) after A356.2 alloy is completely melt, under 600rpm stirring condition, alloy structure can be changed in 758 DEG C of investments
Material, additional amount is the 2.6wt% of A356.2 alloy, and disc-shaped material is completely forced into solution liquid level hereinafter, then stirring
6min is mixed, stops stirring and standing heat preservation 20min；Solution is ultrasonically treated when standing heat preservation, frequency 45kHz, processing
Time is 15min, and melt is cooled to 730 DEG C, is cast in casting mold；
(3) it is demoulded after natural cooling, 410 DEG C of solid solution 30min are air-cooled, 130 DEG C of timeliness 30h, air-cooled up to aluminium alloy.
Embodiment 4: other are same as Example 3, the difference is that rare earth element uses lanthanum (La), cerium (Ce), antimony
(Sb), one of tellurium (Te).
Comparative examples 1: other are same as Example 3, the difference is that RE composite replaces with holmium nitrate.
Comparative examples 2: other are same as Example 3, the difference is that kaolinite powder is replaced using simple substance aluminium powder.
Comparative examples 3: other are same as Example 3, the difference is that step (3) and (4) are no in preparation process
Extrusion operation is carried out, is directly calcined.
Comparative examples 4: using alterant disclosed in Chinese patent CN201510732576.1 to A356.2 aluminium alloy
Metamorphism treatment is carried out, gained aluminium alloy is compareed for subsequent mechanical property test.
1, Mechanics Performance Testing
The A356.2 aluminium alloy castings prepared in Examples 1 to 3 and comparative examples 1~4 are subjected to mechanics properties testing
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 A356.2 Mechanical Property in Aluminum Alloy Castings 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
Table 1 combine table 2 the result shows that, comparative examples 1 due to using holmium nitrate carry out Metamorphism treatment, with 3 phase of embodiment
Than modification effect is poor, so that α-Al phase and eutectic silicon crystal are larger, the mechanical property of alloy is caused to significantly reduce.But
The crystal size of Examples 1 to 3 illustrates the change alloy phase material prepared in the present invention significantly less than comparative examples 4
Metamorphism treatment significant effect is better than RE-Mg intermediate alloy alterant, and crystal more refines, solid solution and timeliness preferable temperature and when
Between under, crystal habit is uniform tiny graininess, and modification effect is stablized, so that the mechanical property of A356.2 alloy-steel casting is also shown
It writes and is promoted.Comparative examples 3 do not take pressing steps, calcined product in the preparation process of material that can change alloy structure
It is formed not good enough, 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 | 2.4 |
| Comparative examples 3 | It is | 0.6 |
| Comparative examples 4 | It is | 0.6 |
Table 1 combine table 3 statistics indicate that, without using kaolinite 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 kaolinite 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, but still there are holes
Hole, the formation of hole 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
A356.2 aluminium alloy is managed, the measurement of deteriorating time range is carried out, the method is as follows:
After A356.2 aluminum alloy melting, it is separately added into different rotten agent materials, mixing time 30s is stood rotten
Soaking time is 1min, 5min, 10min, 15min, and 20min, 40min, 80min, 160min, 240min, measurement is different respectively
The crystal size of Eutectic Silicon in Al-Si Cast Alloys in the alloy prepared under deteriorating time, 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 1 | Embodiment 3 |
| 1 | 80.7μm | 84.3μm | 41.7μm |
| 5 | 69.1μm | 53.2μm | 28.1μm |
| 10 | 42.7μm | 43.9μm | 22.2μm |
| 15 | 31.4μm | 49.8μm | 20.6μm |
| 20 | 36.8μm | 57.6μm | 19.8μm |
| 40 | 34.3μm | 99.8μm | 20.4μm |
| 80 | 42.6μm | 110.9μm | 22.8μm |
| 160 | 66.4μm | 122.3μm | 26.8μm |
| 240 | 91.3μm | 150.3μm | 35.8μm |
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 10min, and modification effect is obviously deteriorated after 80min, and effective deteriorating time is only
For 1h or so, although this is because RE-Mg alloy can significantly extend deteriorating time, in high melt compared with Na, P alterant
Under, with the extension of deteriorating time, alterant still can gradually scaling loss, modification effect be deteriorated, the rotten effect in rotten 160min
Fruit is significantly worse than embodiment 3.Holmium nitrate is directlyed adopt in comparative examples 1 as main alterant, is changed into oxygen rapidly under high temperature
Change holmium and inactivate, modification effect is to start to be deteriorated in 15~20min, goes bad loss of effect in 40min totally, deteriorating time
Shorter, the short-acting modification effect of early period may be from sodium element alterant.
In conclusion RE composite containing holmium, aluminium hydroxide can change sodium acetate, barium nitrate, sodium dihydrogen phosphate, chlorination
The impurity elements such as zinc, lead are formed in sodium, potassium chloride, potassium fluotitanate, vanadium carbide, sodium carbonate, kaolinite, pitch and A356.2 alloy
Harmful phase form and size, thus reduce the harm of impurity phase, auxiliary improves kaolinite composite ceramic and cryolite
To the fine degenerate effect of Eutectic Silicon in Al-Si Cast Alloys, change tissue morphology, improves the Metamorphism treatment efficiency for changing alloy phase material；Kaolinite powder
In contain a large amount of silica and aluminium oxide, silica can react generation aluminum oxide and silicon list in melting with Al
Matter, 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 for becoming alloy, further increases the mechanical property of hypoeutectic aluminium silico-aluminum alloy A356.2.This case treatment effect is stablized,
And processing effective time is long and without incubation period.The mechanical property of alloy after processing, which has, more to be significantly improved.In this case
The sodium chloride, potassium chloride, RE composite containing holmium, sodium acetate, barium nitrate, sodium dihydrogen phosphate, vanadium carbide, sodium carbonate, fluorine titanium
Sour potassium can effective refining eutectic silicon, change tissue morphology；Barium nitrate, kaolinite powder help degasification slagging-off.Rare earth containing holmium is compound
Object can effectively refine coarse primary silicon, in order to overcome alloy molten directly to add elemental phosphorous generated phosphorus in the process certainly
Combustion problem.RE composite containing holmium, aluminium hydroxide can change the form and size of the harmful phase of impurity element formation, thus drop
The harm of low impurity phase.Holimium oxide can be resolved under holmium nitrate hydrate heat-flash, and holimium oxide is mixed valence steady oxide,
Catalytic activity is low, reacts holmium nitrate, phosphotungstic acid in ethanol system in the present invention and generates rare earth phosphotungstate, and with kaolinite
Carrier of the composite ceramic as rare earth phosphotungstate can eliminate the defect that Rare-earth Element Holmium catalytic activity reduces under high temperature, show
Form and size that the RE composite catalysis under the conditions of improving high melt changes impurity element harmful phase are write, improves aluminium indirectly
Alloy modification treated mechanical property.Rare-earth Element Holmium and sodium element phase interworking in kaolinite composite ceramics compound powder
It closes, can effectively refine coarse primary silicon and α-Al phase, overcome number of drawbacks existing for alloy phosphor alterative, have and go bad
Effect is fast, and the incubation time is short, and effective deteriorating time range is big, dissolves rapidly, modification effect stablizes excellent feature, after handling
A356.2 alloy in crystalline silicon phase and α-Al mutually obvious refinement, crystal phase partial size can be down to 20 μm or so, so that the mechanics of alloy
Performance is significantly improved.Barium nitrate, kaolinite powder effectively can help degasification to remove the gred, and ultrasonication solution also can be removed effectively
Gas, prevent the material for generating stomata in aluminium alloy castings, therefore being prepared in the present invention while Metamorphism treatment can also degasification remove
Slag saves slagging-off deaeration step, promotes smelting efficiency.Alloy group can be changed using the method preparation for squeezing calcining in preparation method
The material knitted, so that the gap shrinks between powder raw material, are conducive to the metal salts such as sodium, aluminium, potassium, holmium and form metal complex, it will
The modification effect of multiple element is superimposed, while kaolinite powder forms porous ceramics particle under high-temperature calcination, and further absorption is solid
Fixed established metal complex, keeps complex compound more stable at high temperature, prevents or slows down independent alterant when high melt
Scaling loss, extend effective deteriorating time.
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 material that can change alloy structure, which is characterized in that be grouped as by the group of following weight ratio: aluminium hydroxide 0.3-
0.9%, sodium acetate 3-8%, barium nitrate 11-15%, sodium dihydrogen phosphate 0.5-0.9%, sodium chloride 13-19%, potassium chloride 2-
7%, kaolinite composite ceramic 12-18%, surplus are potassium fluotitanate；
The kaolinite composite ceramic contains 21-26wt% RE composite containing holmium, 13-19wt% vanadium carbide, 0.8-1.2%wt
Sodium carbonate, 11-14%wt pitch, remaining is kaolinite powder；The RE composite containing holmium by phosphotungstic acid/holmium nitrate mixture and
Kaolinite powder composition.
2. a kind of material that can change alloy structure according to claim 1, it is characterised in that: the aluminium hydroxide,
Sodium acetate, barium nitrate, sodium dihydrogen phosphate, sodium chloride, potassium chloride, potassium fluotitanate, vanadium carbide, sodium carbonate, phosphotungstic acid, holmium nitrate
Purity is all larger than 99.9wt%, and partial size is 100~200 mesh, and the pitch is coal tar pitch；The phosphotungstic acid/holmium nitrate mixing
Content >=75wt% of rare earth holmium phosphotungstate in object.
3. the preparation method that one kind can change the material of alloy structure as claimed in claim 1 or 2, which is characterized in that comprising such as
Lower specific steps:
(1) RE composite containing holmium is prepared as follows: 15-23g phosphotungstic acid being added in 1000mL dehydrated alcohol, is placed in magnetic
On power blender, the ethanol solution 1000mL of the 15-20g containing holmium nitrate is instilled dropwise, stirs 36-39h in 20 DEG C of constant temperature, solvent is waved
10-12h is dried after hair in 60-70 DEG C of baking oven to doing, 350~400 DEG C of 1~4h of calcining obtain phosphotungstic acid/holmium nitrate mixture, cold
But it to addition 1L dehydrated alcohol and 200-210g kaolinite powder after room temperature, is filtered after homogenate, takes precipitating drying to obtain dilute containing holmium
Native compound；
(2) preparation of kaolinite composite ceramic: according to 21-26wt% RE composite containing holmium, 13-19wt% vanadium carbide,
0.8-1.2wt% sodium carbonate, 11-14wt% pitch, remaining is kaolinite powder ingredient, and mix powder in addition to bitumen 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 2%, 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) 250~350 DEG C of pitch pre- heat fusing back stirring sides are added in mix powder, by mixing after mixing evenly
Material is put into briquet in grinding tool after being cooled to 150 DEG C, compression moulding pressure is 35~55MPa, is put into after being embedded with graphite powder
In roaster, at 910-960 DEG C after sintering 1-2 hours, cooled to room temperature then takes out and grinds on grinder, until
Particle size, can be stand-by at 11~14 microns；
(4) according to aluminium hydroxide 0.3-0.9wt%, sodium acetate 3-8wt%, barium nitrate 11-15wt%, sodium dihydrogen phosphate 0.5-
0.9wt%, sodium chloride 13-19wt%, potassium chloride 2-7wt%, kaolinite composite ceramic 12-18wt%, remaining is fluotitanic acid
Potassium ingredient, it is then uniform in ground and mixed in the ball mill, by mixture extrusion forming, 50~65MPa of squeeze pressure；
(5) batch briquetting is put into the vacuum drying oven of argon gas again and is sintered, at 120-140 DEG C after heat preservation 1-2 hours, taken out cold
But to room temperature, it is then ground to partial size on grinder at 30~40 microns, obtains alterant powder；
(6) according to disk is pressed after the ratio mixing of 2~4 parts by weight epoxy resin, 95~100 parts by weight alterant powder, go bad
Agent piece thickness 0.5cm, 1~2cm of diameter is to get the material that can change alloy structure.
4. a kind of preparation method of material that can change alloy structure according to claim 3, it is characterised in that: described
Kaolinite powder salic 30.4~36.6wt%, 5.2~11.1wt% of water, 0.1~0.3wt% of iron oxide, antimony oxide 0.12
~0.25wt%, 0.5~0.8wt% of calcium oxide, 1.1~1.3wt% of magnesia, 0.03~0.15wt% of potassium oxide, sodium oxide molybdena
0.2~0.35wt%, surplus SiO2；The partial size of the kaolinite composite ceramic be 150~200 mesh, the graphite powder with
The weight ratio of mixture block is 1:300~900, and graphite linings thickness is at least 1~5cm.
5. a kind of aluminium alloy preparation method, which is characterized in that using the material that can change alloy structure described in claims 1 or 2
Material carries out Metamorphism treatment to A356.2 alloy, the specific steps are as follows:
(1) melting in induction furnace by A356.2 alloy adjusts 740-765 DEG C of smelting temperature, smelting time 30min；
(2) after A356.2 alloy is completely melt, under 500~700rpm stirring condition, alloy can be changed in 750-765 DEG C of investment
The material of tissue, additional amount be A356.2 alloy 1.7~3.5wt%, and by disc-shaped material be completely forced into solution liquid level with
Under, it is subsequently agitated for 5~7min, stops stirring and standing heat preservation 15-25min；Solution is ultrasonically treated when standing heat preservation, frequency
Rate is 30~60kHz, and the processing time is 10~20min, and melt is cooled to 725-735 DEG C, is cast in casting mold；
(3) demoulded after natural cooling, 380~440 DEG C of solid solution 30min are air-cooled, 120~140 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 material that alloy structure can be changed
Material is prepared using method described in claim 4.
7. a kind of aluminium alloy preparation method according to claim 6, it is characterised in that: the component of the A356.2 alloy
Are as follows: Si 6.0~7.0wt%, Fe 0.02~0.06wt%, Cu 0.05~0.1wt%, Mg 0.21~0.33wt%, Mn
0.09~0.18wt% of 0.02~0.06wt%, Zn≤0.02wt%, Ti, impurity content≤0.1wt%, surplus Al.
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