CN107119203B - A kind of method for preparing Yb, La and SiC composite inoculating A356.2 alloys - Google Patents

A kind of method for preparing Yb, La and SiC composite inoculating A356.2 alloys Download PDF

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CN107119203B
CN107119203B CN201710256439.4A CN201710256439A CN107119203B CN 107119203 B CN107119203 B CN 107119203B CN 201710256439 A CN201710256439 A CN 201710256439A CN 107119203 B CN107119203 B CN 107119203B
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ultrasonic
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张少辰
冷金凤
周庆波
王鹤
王�琦
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University of Jinan
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    • C—CHEMISTRY; METALLURGY
    • C22—METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
    • C22C—ALLOYS
    • C22C1/00—Making non-ferrous alloys
    • C22C1/10—Alloys containing non-metals
    • C22C1/1036—Alloys containing non-metals starting from a melt
    • C—CHEMISTRY; METALLURGY
    • C22—METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
    • C22C—ALLOYS
    • C22C1/00—Making non-ferrous alloys
    • C22C1/06—Making non-ferrous alloys with the use of special agents for refining or deoxidising
    • C—CHEMISTRY; METALLURGY
    • C22—METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
    • C22C—ALLOYS
    • C22C1/00—Making non-ferrous alloys
    • C22C1/10—Alloys containing non-metals
    • C22C1/1005—Pretreatment of the non-metallic additives
    • C22C1/101—Pretreatment of the non-metallic additives by coating
    • C—CHEMISTRY; METALLURGY
    • C22—METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
    • C22C—ALLOYS
    • C22C21/00—Alloys based on aluminium
    • C22C21/02—Alloys based on aluminium with silicon as the next major constituent
    • C22C21/04—Modified aluminium-silicon alloys

Abstract

The invention discloses a kind of method for preparing Yb, La and SiC composite inoculating A356.2 alloys, include the following steps：Using nano level SiC as reinforced particulate, after superhigh temperature oxidation processes, then using nano magnetic sputtering equipment, by the SiC particulate surface of high pure metal Ti parcels after the oxidising treat-ment；And gone bad and continuous ultrasound assisted melting using high-purity compound heavy rare earth, to further improve castability.The present invention uses the stent of independent research as ancillary equipment, and SiC particulate can be caused to be in suspended state and just poured into a mould.This preparation method is simple, cost is relatively low, with short production cycle, possesses good industrialization prospect.

Description

A kind of method for preparing Yb, La and SiC composite inoculating A356.2 alloys
Technical field
The present invention relates to the melting field of alloy, and in particular to one kind prepares Yb, La and SiC composite inoculating A356.2 alloys Method.
Background technology
A356.2 aluminium alloys are typical Al-Si-Mg systems ternary alloy three-partalloys, are compared with A356.0, A356.1, the content of Fe into One step reduces, and adds metal Ti, has preferably refined crystal grain.It is more complicated that A356.2 aluminium alloys can cast shape Thin-walled parts, because its casting character is outstanding, plasticity is high, so applied to above automotive hub.
The A356.2 alloys of alterant are not added, and thick plate tip-like primary silicon is included in its matrix.Crystal grain is thicker Greatly, distribution is more uneven, and the performance of material is more bad.At present, production industry is devoted to improve traditional A356.2 alloy properties Can, main method is exactly from source, improves thick particle, makes its distribution uniformity and mellow and fullization, rotten using which kind of Agent, how to carry out rotten A356.2 alloys be also domestic and international research and development it is common the problem of.
19th century Al-Si aluminium alloys it is found that rare earth element can go bad, and rare earth element can long-time burning Without reducing its thinning effect.Rare earth can also carry out degasification, slagging-off.Also there is improvement to the Hydrogen Brittleness Phenomena for reducing A356, still, Most of research is only limitted to individually add light rare earth elements at present, for heavy rare earth element, especially mixes high-purity heavy rare earth ytterbium It is limited with the research of lanthanum.
SiC-Al composite materials as structural material to be commonly applied on lifting airscrew, brake disc etc., still, due to The special nature of carborundum so that it is extremely difficult to prepare SiC-Al composite materials.The method that most people all uses powder metallurgy Prepared, but the method complex production process, sintering process are difficult to control, and are not easy to prepare the larger structural member of volume, and it is raw It is longer to produce the cycle.
CN106011507 A disclose a kind of Al-Mg-Si-Y rare earth aluminium alloys and preparation method thereof, during this method adds Between be stirred every 5 minutes after alloy, although can sufficiently stir evenly, due to stirred in frequent, easily Cause to enter gas in melt.And prepare rare earth intermediate alloy and increase the production cycle, also easily cause the secondary oxygen of rare earth element Change.CN 100516261C disclose a kind of cerium-rich mischmetal and go bad the methods of A356 alloy stostes, in fusion process into Magnetic agitation, this way easily cause gas to enter aluminium alloy solution to row twice, and after addition rare earth alterative, carry out magnetic force and stir Mix, cause rare earth and oxygen to come into full contact with, scaling loss is serious, reduces modification effect.CN 103451494A disclose a kind of aluminium - silicon-ytterbium cast aluminium alloy gold and preparation method.This method uses electromagnetic agitation, but the operating temperature of electromagnetic agitation is up to 840 DEG C, the serious scaling loss of rare earth and soaking time is too short, RE Modified has certain incubation period, and the time is too short, it is impossible to well Play rare-earth action.104178649 A of CN disclose a kind of preparation method of high-performance lanthanum ytterbium aluminium alloy, the method casting The alloy produced is not heat-treated and ultrasonic time is too short, has not been able to pour into a mould immediately after ultrasound, reduces the effect of ultrasound.
The content of the invention
To solve the above problems, the present invention provides a kind of method for preparing Yb, La and SiC composite inoculating A356.2 alloys, This method Environmental Safety, crystal grain refinement, castability is good, and reduces the production cycle.
What the present invention was achieved through the following technical solutions：
A kind of method for preparing Yb, La and SiC composite inoculating A356.2 alloys, comprises the following steps：
1）The pretreatment of carborundum：
（1）The carborundum of the average grain diameter 5nm-90nm of 5.25g is weighed, adds the alcohol of 20ml, ultrasonic disperse 30 minutes；
（2）The carborundum that ultrasound finishes is put into air dry oven, 70 DEG C carry out drying 2h；
（3）Drying finishes, and it is 2h to be put into milling time in grinding alms bowl；
（4）SiC puts silica crucible into, is heated to 300 DEG C of ± 5 DEG C of insulation 30min, then be warming up to 1200 DEG C of ± 5 DEG C of insulations 5h, is during which stirred, time 40s every 30min；
（5）SiC after pretreatment is rejected into the particle more than 100nm；
2）The subsequent treatment of SiC：Magnetron sputtering is carried out after the pretreatment of carborundum；
3）Fusion process
（1）Resistance furnace in ultrasonic wave crucible heater is heated to 500 DEG C ~ 550 DEG C, purity is added into graphite crucible For 99.9% aluminium ingot；
（2）730 DEG C are warming up to, treats aluminium ingot wholeFusing, add Al-20%Si intermediate alloys；
（3）Wait Al-20%Si completeFusing, the purity of addition aluminium foil tight is 99.99% Yb+La, wherein Aluminium foil and Yb+La mass ratioes are 3:1,5min is kept the temperature, adds coverture, keeps the temperature 40min-55min；
（4）Skim after insulation, be sufficiently stirred after the completion of skimming with graphite rod for the first time, continue to keep the temperature 15min；
（5）Added while stirring with graphite rod and have been warmed up 40 DEG C of SiC, the position that SiC is added is to stir semisolid Swirl center, stirs and all adds SiC within 2min；
（6）Ultrasound, time 30min are carried out when being warming up to 730 DEG C；
（7）The Mg of aluminium foil tight is added, the wherein mass ratio of aluminium foil and Mg is 3:1 and coverture is added immediately, protect Warm 5min；
（8）Al-5%Ti-1%C are added, Slag treatment is taken off for the second time, is poured into a mould, poured at 720 DEG C after stirring evenly Filtered during note with heat safe chemical fibre fine-structure mesh；
（9）It is heat-treated after cast, obtains Yb, La and SiC composite inoculating A356.2 alloys.
The mass percent of the component of Yb, La and SiC composite inoculating A356.2 alloys described above is：Si：6.5%- 7.5%, Mg：0.30%-0.45%, Ti：0.05%-0.1%, Yb：0.3%-0.5%, La：0.3%-0.5%, nano SiC：0.5%- 1.0%, Fe≤0.2%, Cu≤0.2%, Zn≤0.1%, remaining impurity element≤0.05%, surplus Al.
Preferably, the step of subsequent treatment of SiC is：
（1）After the silicon carbide substrate of average grain diameter 5nm-90nm is placed in the cavity, 30min first is vacuumized with mechanical pump, Then drive molecular pump to continue to vacuumize 15min, be evacuated to 1.3 × 10-3~4.0×10-3The vacuum of Pa, is passed through high-purity argon gas；
（2）Substrate heating mechanism is opened, substrate is heated to 120 DEG C, this process can be synchronous with molecular pump vacuum；
（3）It is 0.5 ~ 1.1Pa, sputtering current 0.25A, sputtering time 30s-300s to adjust vacuum room pressure.
Preferably, step in the fusion process（6）Middle ultrasonic working frequency 20KHz, operating temperature is 720 DEG C, is shaken Width >=10 μm.
Preferably, step in the fusion process（9）Middle process of thermal treatment is：535 DEG C of ± 3 DEG C of solid solution 5h；During transfer Between 3s, the cool time is 30s ± 3s；Aging temp is 165 DEG C ± 3 DEG C, aging time 4h.
The ultrasonic wave crucible heating used in the method for preparing nano SiC, Yb, La enhancing A356.2 alloys described above Device, including supersonic generator（1）, resistance furnace for placing graphite crucible（5）And supporting rack（3）, the ultrasonic wave generation Device（1）It is connected with ultrasonic amplitude transformer（4）；
Support frame as described above（3）Including fixing sleeve（31）, N number of first support bar（32）Second support bar is vertically arranged with N number of （33）, the fixing sleeve（31）It is sleeved on supersonic generator（1）On, N number of first support bar（32）With fixing sleeve（31） It is uniformly distributed for axis；
The first support bar（32）One end be both connected to fixing sleeve（31）The upper, other end is and second support bar（33） Upper end connect to realize to supersonic generator（1）Supporting role；
The N is the natural number more than or equal to 2.
Preferably, the first support bar（32）For telescopic rod.
Preferably, second support bar（33）For telescopic rod.
Preferably, the first support bar（32）And second support bar（33）It is aluminum alloy material, the ultrasonic amplitude of fluctuation Bar（4）For full titanium alloy materialII typeUltrasonic transformer, the N are 3.
The useful achievement of the present invention：
1st, the present invention provides a kind of method for preparing Yb, La and SiC composite inoculating A356.2 alloys, is carrying out essence for the first time The protective layer of coverture is not destroyed during refining, avoids the further oxidation of Yb and La.
2nd, using high-purity Yb and La, solve the step of manufacture rare earth intermediate alloy, reduce the production cycle；Add Yb, La During with Mg, with aluminium foil tight, and nontoxic coverture is added immediately after adding, reduces Yb, La and Mg and be subject to height suddenly Warm and serious scaling loss.
3. the present invention use purity for 99.99% Ti metals, with magnetically controlled sputter method by the attached last layer of silicon carbide Ti films, the method can increase the wetability of nano level SiC and aluminum solutions with crystal grain thinning and Ti.
4. because of Ti easily scaling loss, therefore being splashed on the later SiC of high-temperature process, the effect of wetting is added.
5th, quenching shift time 3s, reduces scattering and disappearing for temperature；, will be miscellaneous in order to obtain the effect of more preferable crystal grain thinning Matter Ti and B is added in rational allowed band, and nucleation sites are provided for the heterogeneous forming core of solution.
When the 6th, carrying out Semi-solid Stirring, the position of SiC is added in the whirlpool of semisolid, preferably adds Sic into molten In liquid.
7th, the direction of ultrasonic wave is perpendicular to crucible, avoid due to lateral wave and caused by crucible impurity enter melt, The service life of crucible is added, has purified melt, and ultrasound is carried out using continuous mode, has preferably broken dendrite, has been shape Core provides place.
9th, optional equipment is independent research used by the experiment, its feature is to add high strength alumin ium alloy telescopic rod As support, avoid stove size and crucible size and limit the use of ultrasonic device, protective gas can also be passed through and carry out melting Oxidizable metal.
9th, the design can quickly withdraw ultrasonic device so that the time interval controls that ultrasound is finished between cast exist Within 10s, carborundum has not enough time to reunite and has just been poured, and improves casting quality.
10th, ultrasonic transformer used in ultrasonic device is entirely that titanium alloy is made, and titanium alloy chemical property is stablized, and it is miscellaneous to avoid remaining The introducing of matter.
11st, fining agent is served as using SiC-Yb-La, preferably rotten A356.2 aluminium alloys.
Brief description of the drawings
Fig. 1：1 metallograph of embodiment through Overheating Treatment；
Fig. 2：The metallograph of embodiment 2 through Overheating Treatment；
Fig. 3：3 metallograph of embodiment through Overheating Treatment；
Fig. 4：The metallograph of Yb+La+SiC is not added with through Overheating Treatment；
Fig. 5：Metallograph through Overheating Treatment addition Yb+La；
Fig. 6：The ultrasonic wave crucible heater stereogram that this experiment uses；
Fig. 7：The ultrasonic wave crucible heater front view that this experiment uses；
Fig. 8：The ultrasonic wave crucible heater top view that this experiment uses；
In figure：1. ultrasonic generator；2. graphite crucible；3. supporting rack；4. ultrasound becomes secondary bar；5. resistance furnace；31. fix Set；32. first support bar；33. second support bar.
Embodiment
To better understand the essence of the present invention, below by specific embodiment to technical scheme into traveling The elaboration of one step.
Embodiment 1
A kind of method for preparing Yb, La and SiC composite inoculating A356.2 alloys, comprises the following steps：
1）The pretreatment of carborundum：
（1）The carborundum of the average grain diameter 5nm-90nm of 5.25g is weighed, adds the alcohol of 20ml, ultrasonic disperse 30 minutes；
（2）The carborundum that ultrasound finishes is put into air dry oven, 70 DEG C carry out drying 2h；
（3）Drying finishes, and it is 2h to be put into milling time in grinding alms bowl；
（4）SiC puts silica crucible into, be heated to 300 DEG C insulation 30min, then be warming up to 1200 DEG C insulation 5h, during which every 30min is stirred, time 40s；
（5）SiC after pretreatment is rejected into the particle more than 100nm；
2）The subsequent treatment of SiC
（1）The glass slide of magnetron sputtering is placed in the beaker for filling acetone, is cleaned in ultrasonic cleaner 20min;Take out glass slide and it is risen to sound cleaning 20min in absolute ethyl alcohol；It is last to play sound cleaning 10min in deionized water, Taking-up is dried up from top to bottom with hair-dryer；
（2）It is first true with mechanical pumping after the silicon carbide substrate placement in the cavity of the average grain diameter 5nm of 5.25g will be placed with Sky about 30min, then drives molecular pump and continues to vacuumize about 15min, be evacuated to about 1.3 × 10-3The vacuum of Pa or so, is passed through high-purity Argon gas；
（3）Substrate heating mechanism is opened, substrate is heated to 120 DEG C, this process can be synchronous with molecular pump vacuum；
（4）Sputtering pressure is adjusted using the plate valve below instrument.Produce aura after first to high-purity Ti target material surface into The pre-sputtering of row 10min, is then passed through argon gas to cavity, and it is 0.5Pa to adjust vacuum room pressure, and sputtering current 0.25A, waits and splash Penetrate after stablizing and open baffle, sputtered.Sputtering time is 30s；
（5）After cooling, it is spare to take out SiC.
3）Fusion process
（1）Resistance furnace in ultrasonic wave crucible heater is heated to 500 DEG C, purity is added into graphite crucible is 99.9% aluminium ingot；
（2）730 DEG C are warming up to, treats aluminium ingot wholeFusing, add Al-20%Si intermediate alloys；
（3）Wait Al-20%Si completeFusing, the purity of addition aluminium foil tight is 99.99% Yb+La, wherein Aluminium foil and Yb+La mass ratioes are 3:1,5min is kept the temperature, adds coverture, keeps the temperature 40min；
（4）Skim after insulation, be sufficiently stirred after the completion of skimming with graphite rod for the first time, continue to keep the temperature 15min；
（5）The aluminum oxide film of bath surface is removed after taking out crucible 2min；
（6）Added while stirring with graphite rod and have been warmed up 40 DEG C of SiC, the position that SiC is added is to stir semisolid Swirl center, stirs and all adds SiC within 2min；
（7）Ultrasound, ultrasonic time 30min, ultrasonic working frequency 20 are carried out when being warming up to 730 DEG CKHz, work temperature Spend for 720 DEG C, amplitude >=10 μm；
（8）The Mg of aluminium foil tight is added, the wherein mass ratio of aluminium foil and Mg is 3:1 and coverture is added immediately, add Enter coverture, keep the temperature 5min；
（9）Al-5%Ti-0.2%C are added, Slag treatment is taken off for the second time, is poured into a mould after stirring evenly at 720 DEG C, Filtered during cast with heat safe chemical fibre fine-structure mesh；
（10）It is heat-treated after cast, process of thermal treatment is：535 DEG C of solid solution 5h；Transfer time 3s, cool time 30s； Aging temp is 165 DEG C, aging time 4h.Yb, La and SiC composite inoculating A356.2 alloys are obtained, the component of the alloy Mass percent is：Si：10.03%, Mg：0.41%, Ti：0.08%, Yb：0.21%, La：0.16%, SiC：0.58%, Al： 88.53%。
Attached drawing 1 is 1 metallograph of embodiment through Overheating Treatment.
Embodiment 2
A kind of method for preparing Yb, La and SiC composite inoculating A356.2 alloys, comprises the following steps：
1）The pretreatment of carborundum：
（1）The carborundum of the average grain diameter 5nm-90nm of 5.25g is weighed, adds the alcohol of 20ml, ultrasonic disperse 30 minutes；
（2）The carborundum that ultrasound finishes is put into air dry oven, 70 DEG C carry out drying 2h；
（3）Drying finishes, and it is 2h to be put into milling time in grinding alms bowl；
（4）SiC puts silica crucible into, be heated to 295 DEG C insulation 30min, then be warming up to 1195 DEG C insulation 5h, during which every 30min is stirred, time 40s；
（5）SiC after pretreatment is rejected into the particle more than 100nm；
2）The subsequent treatment of SiC
（1）The glass slide of magnetron sputtering is placed in the beaker for filling acetone, is cleaned in ultrasonic cleaner 20min；Take out glass slide and it is risen to sound cleaning 20min in absolute ethyl alcohol;It is last to play sound cleaning 10min in deionized water, Taking-up is dried up from top to bottom with hair-dryer；
（2）It is first true with mechanical pumping after the silicon carbide substrate placement in the cavity of the average grain diameter 90nm of 5.25g will be placed with Sky about 30min, then drives molecular pump and continues to vacuumize about 15min, be evacuated to about 4.0 × 10-3The vacuum of Pa or so, is passed through high-purity Argon gas；
（3）Substrate heating mechanism is opened, substrate is heated to 120 DEG C, this process can be synchronous with molecular pump vacuum；
（4）Sputtering pressure is adjusted using the plate valve below instrument.Produce aura after first to high-purity Ti target material surface into The pre-sputtering of row 10min, is then passed through argon gas to cavity, and it is 1.1Pa to adjust vacuum room pressure, and sputtering current 0.25A, waits and splash Penetrate after stablizing and open baffle, sputtered.Sputtering time is 300s；
（5）After cooling, it is spare to take out SiC.
3）Fusion process
（1）Resistance furnace in ultrasonic wave crucible heater is heated to 550 DEG C, purity is added into graphite crucible is 99.9% aluminium ingot；
（2）730 DEG C are warming up to, treats aluminium ingot wholeFusing, add Al-20%Si intermediate alloys；
（3）Wait Al-20%Si completeFusing, the purity of addition aluminium foil tight is 99.99% Yb+La, wherein Aluminium foil and Yb+La mass ratioes are 3:1,5min is kept the temperature, adds coverture, keeps the temperature 40min；
（4）Skim after insulation, be sufficiently stirred after the completion of skimming with graphite rod for the first time, continue to keep the temperature 15min；
（5）The aluminum oxide film of bath surface is removed after taking out silica crucible 2min；
（6）Added while stirring with graphite rod and have been warmed up 40 DEG C of SiC, the position that SiC is added is to stir semisolid Swirl center, stirs and all adds SiC within 2min；
（7）Ultrasound, ultrasonic time 30min, ultrasonic working frequency 20 are carried out when being warming up to 730 DEG CKHz, work temperature Spend for 720 DEG C, amplitude >=10 μm；
（8）The Mg of aluminium foil tight is added, the wherein mass ratio of aluminium foil and Mg is 3:1 and coverture is added immediately, protect Warm 5min；
（9）Al-5%Ti-0.2%C are added, is taken off Slag treatment, time 1.5min, 720 after stirring evenly for the second time DEG C poured into a mould, when cast is filtered with heat safe chemical fibre fine-structure mesh；
（10）It is heat-treated after cast, process of thermal treatment is：538 DEG C of solid solution 5h；Transfer time 3s, cool time 33s； Aging temp is 168 DEG C, aging time 4h.Yb, La and SiC composite inoculating A356.2 alloys are obtained, the component of the alloy Mass percent is：Si：9.83%, Mg：0.35%, Ti：0.10%, Yb：0.25%, La：0.18%, SiC：0.62%, Al: 88.67%；
Attached drawing 2 is 2 metallograph of embodiment through Overheating Treatment.
Embodiment 3
A kind of method for preparing Yb, La and SiC composite inoculating A356.2 alloys, comprises the following steps：
1）The pretreatment of carborundum：
（1）The carborundum of the average grain diameter 5nm-90nm of 5.25g is weighed, adds the alcohol of 20ml, ultrasonic disperse 30 minutes；
（2）The carborundum that ultrasound finishes is put into air dry oven, 70 DEG C carry out drying 2h；
（3）Drying finishes, and it is 2h to be put into milling time in grinding alms bowl；
（4）SiC puts silica crucible into, be heated to 305 DEG C insulation 30min, then be warming up to 1205 DEG C insulation 5h, during which every 30min is stirred, time 40s；
（5）SiC after pretreatment is rejected into the particle more than 100nm；
2）The subsequent treatment of SiC
（1）The glass slide of magnetron sputtering is placed in the beaker for filling acetone, is cleaned in ultrasonic cleaner 20min;Take out glass slide and it is risen to sound cleaning 20min in absolute ethyl alcohol;It is last to play sound cleaning 10min in deionized water, Taking-up is dried up from top to bottom with hair-dryer；
（2）It is first true with mechanical pumping after the silicon carbide substrate placement in the cavity of the average grain diameter 40nm of 5.25g will be placed with Sky about 30min, then drives molecular pump and continues to vacuumize about 15min, be evacuated to about 2.0 × 10-3The vacuum of Pa or so, is passed through high-purity Argon gas；
（3）Substrate heating mechanism is opened, substrate is heated to 120 DEG C, this process can be synchronous with molecular pump vacuum；
（4）Sputtering pressure is adjusted using the plate valve below instrument.Produce aura after first to high-purity Ti target material surface into The pre-sputtering of row 10min, is then passed through argon gas to cavity, and it is 0.8Pa to adjust vacuum room pressure, and sputtering current 0.25A, waits and splash Penetrate after stablizing and open baffle, sputtered.Sputtering time is 150s；
（5）After cooling, it is spare to take out SiC.
3）Fusion process
（1）Resistance furnace in ultrasonic wave crucible heater is heated to 520 DEG C, purity is added into graphite crucible is 99.9% aluminium ingot；
（2）730 DEG C are warming up to, treats aluminium ingot wholeFusing, add Al-20%Si；
（3）Wait Al-20%Si completeFusing, the purity of addition aluminium foil tight is 99.99% Yb+La, wherein Aluminium foil and Yb+La mass ratioes are 3:1,5min is kept the temperature, adds coverture, keeps the temperature 40min；
（4）Skim after insulation, be sufficiently stirred after the completion of skimming with graphite rod for the first time, continue to keep the temperature 15min；
（5）The aluminum oxide film of bath surface is removed after taking out silica crucible 2min；
（6）Added while stirring with graphite rod and have been warmed up 40 DEG C of SiC, the position that SiC is added is to stir semisolid Swirl center, stirs and all adds SiC within 2min；
（7）Ultrasound, ultrasonic time 30min, ultrasonic working frequency 20 are carried out when being warming up to 730 DEG CKHz, work temperature Spend for 720 DEG C, amplitude >=10 μm；
（8）The Mg of aluminium foil tight is added, the wherein mass ratio of aluminium foil and Mg is 3:1 and coverture is added immediately, add Enter coverture, keep the temperature 5min；
（9）Al-5%Ti-0.2%C are added, Slag treatment is taken off for the second time, is poured into a mould after stirring evenly at 720 DEG C, Filtered during cast with heat safe chemical fibre fine-structure mesh；
（10）It is heat-treated after cast, process of thermal treatment is：532 DEG C of solid solution 5h；Transfer time 3s, cool time 27s； Aging temp is 162 DEG C, aging time 4h.Yb, La and SiC composite inoculating A356.2 alloys are obtained, the component of the alloy Mass percent is：Si：9.33%, Mg：0.32%, Ti：0.08%, Yb：0.26%, La：0.19%, SiC：0.65%, Al：89.17%
Attached drawing 3 is 3 metallograph of embodiment through Overheating Treatment.
Ultrasonic wave crucible heater used in embodiment 1-3, including supersonic generator 1, for placing graphite crucible 2 Resistance furnace 5 and supporting rack 3, the supersonic generator 1 is connected with ultrasonic amplitude transformer 4；Support frame as described above 3 includes fixing sleeve 31st, 3 first support bars 32 and 3 are vertically arranged second support bar 33, and the fixing sleeve 31 is sleeved on supersonic generator 1 On, 3 first support bars 32 are uniformly distributed with fixing sleeve 31 for axis；One end of the first support bar 32 is both connected to solid Surely cover on 31, the other end is connected with the upper end of second support bar 33 to realize the supporting role to supersonic generator 1.It is described First support bar 32 is telescopic rod, and second support bar 33 is telescopic rod.First support bar 32 and second support bar 33 are Aluminum alloy material, the ultrasonic amplitude transformer 4 are full titanium alloy materialII typeUltrasonic transformer.
Comparative example 1
A kind of method for preparing A356.2 alloys, comprises the following steps：
（1）Resistance furnace is heated to 500 DEG C, adds the aluminium ingot that purity is 99.9%；
（2）Resistance furnace is warming up to 730 DEG C, treats aluminium ingot wholeFusing, add Al-20%Si；
（3）Wait Al-20%Si completeFusing, coverture is added, keeps the temperature 40min；
（4）Insulation 40 minutes, was during which stirred once every 5 minutes with graphite rod, continued to keep the temperature 15min；
（5）Add Mg and add coverture immediately, add coverture, keep the temperature 5min；
（6）Removal of impurities, suction pouring：Under keeping warm mode, after removal of impurities, the vacuum suction casting forming at 710 DEG C；
（7）Process of thermal treatment is after shaping：535 DEG C of solid solution 5h；Cold water quenches, transfer time 20s, and the cool time is 30s；Aging temp is 165 DEG C, aging time 4h, obtain ytterbium and go bad A356.2 alloys.The mass percent of component is：Si： 12.34%, Mg：0.36%, Ti：0.05%, Al：87.25%.
Attached drawing 4 is the metallograph of the comparative example 1 through Overheating Treatment.
Comparative example 2
It is a kind of to prepare ytterbium and lanthanum goes bad the methods of A356.2 alloys, comprise the following steps：
（1）Resistance furnace is heated to 500 DEG C, adds the aluminium ingot that purity is 99.9%；
（2）Resistance furnace is warming up to 730 DEG C, treats aluminium ingot wholeFusing, add Al-20%Si；
（3）Wait Al-20%Si completeFusing, the purity of addition aluminium foil tight is 99.99% Yb+La, wherein Aluminium foil and Yb+La mass ratioes are 3:1,5min is kept the temperature, adds coverture, keeps the temperature 40min；
（4）Insulation 40 minutes, was during which stirred once every 5 minutes with graphite rod, continued to keep the temperature 15min；
（5）The Mg of aluminium foil tight is added, the wherein mass ratio of aluminium foil and Mg is 3:1 and coverture is added immediately, protect Warm 5min；
（6）Removal of impurities, suction pouring：Under keeping warm mode, after removal of impurities, the vacuum suction casting forming at 710 DEG C；
（7）Process of thermal treatment is after shaping：535 DEG C of solid solution 5h；Cold water quenches；Aging temp is 155 DEG C, aging time For 4h, obtain ytterbium and lanthanum goes bad A356.2 alloys.The mass percent of component is：Si：10.81%, Mg：0.41%, Yb：0.15%, La：0.12%, Al：88.51%.
Attached drawing 5 is the metallograph of the comparative example 2 through Overheating Treatment.

Claims (8)

  1. A kind of 1. method for preparing Yb, La and SiC composite inoculating A356.2 alloys, it is characterised in that comprise the following steps：
    1）The pretreatment of carborundum：
    （1）The carborundum of the average grain diameter 5nm-90nm of 5.25g is weighed, adds the alcohol of 20ml, ultrasonic disperse 30 minutes；
    （2）The carborundum that ultrasound finishes is put into air dry oven, 70 DEG C carry out drying 2h；
    （3）Drying finishes, and it is 2h to be put into milling time in grinding alms bowl；
    （4）SiC puts silica crucible into, is heated to 300 DEG C of ± 5 DEG C of insulation 30min, then is warming up to 1200 DEG C of ± 5 DEG C of insulation 5h, phase Between every 30min stir, time 40s；
    （5）SiC after pretreatment is rejected into the particle more than 100nm；
    2）The subsequent treatment of SiC：Magnetron sputtering is carried out after the pretreatment of carborundum；
    3）Fusion process
    （1）Resistance furnace in ultrasonic wave crucible heater is heated to 500 DEG C ~ 550 DEG C, purity is added into graphite crucible is 99.9% aluminium ingot；
    （2）730 DEG C are warming up to, treats that aluminium ingot all melts, adds Al-20%Si intermediate alloys；
    （3）Al-20%Si is waited to be completely melt, the purity of addition aluminium foil tight is 99.99% Yb+La, wherein aluminium foil It is 3 with Yb+La mass ratioes:1,5min is kept the temperature, adds coverture, keeps the temperature 40min-55min；
    （4）Skim after insulation, be sufficiently stirred after the completion of skimming with graphite rod for the first time, continue to keep the temperature 15min；
    （5）Added while stirring with graphite rod and have been warmed up 40 DEG C of SiC, the position that SiC is added is the whirlpool for stirring semisolid Center, stirs and all adds SiC within 2min；
    （6）Ultrasound, time 30min are carried out when being warming up to 730 DEG C；
    （7）The Mg of aluminium foil tight is added, the wherein mass ratio of aluminium foil and Mg is 3:1 and coverture is added immediately, keep the temperature 5min；
    （8）Al-5%Ti-1%C are added, Slag treatment is taken off for the second time, is poured into a mould after stirring evenly at 720 DEG C, during cast Filtered with heat safe chemical fibre fine-structure mesh；
    （9）It is heat-treated after cast, obtains Yb, La and SiC composite inoculating A356.2 alloys；
    The mass percent of the component of Yb, La and SiC composite inoculating A356.2 alloys is：Si：6.5%-7.5%, Mg： 0.30%-0.45%, Ti：0.05%-0.1%, Yb：0.3%-0.5%, La：0.3%-0.5%, nano SiC：0.5%-1.0%, Fe≤ 0.2%, Cu≤0.2%, Zn≤0.1%, remaining impurity element≤0.05%, surplus Al.
  2. 2. according to the method described in claim 1, it is characterized in that, the step of subsequent treatment of SiC be：
    （1）After the silicon carbide substrate of average grain diameter 5nm-90nm is placed in the cavity, 30min first is vacuumized with mechanical pump, then Drive molecular pump to continue to vacuumize 15min, be evacuated to 1.3 × 10-3~4.0×10-3The vacuum of Pa, is passed through high-purity argon gas；
    （2）Substrate heating mechanism is opened, substrate is heated to 120 DEG C, this process can be synchronous with molecular pump vacuum；
    （3）It is 0.5 ~ 1.1Pa, sputtering current 0.25A, sputtering time 30s-300s to adjust vacuum room pressure.
  3. 3. according to the method described in claim 1, it is characterized in that, step in the fusion process（6）Middle ultrasonic work frequency Rate 20kHz, operating temperature are 720 DEG C, amplitude >=10 μm.
  4. 4. according to the method described in claim 1, it is characterized in that, step in the fusion process（9）Middle process of thermal treatment For：535 DEG C of ± 3 DEG C of solid solution 5h；Transfer time 3s, cool time are 30s ± 3s；Aging temp is 165 DEG C ± 3 DEG C, during timeliness Between be 4h.
  5. 5. the method for preparing Yb, La and SiC composite inoculating A356.2 alloys described in a kind of one of claim 1-4 uses super Sound wave crucible heater, it is characterised in that：Including supersonic generator（1）, resistance furnace for placing graphite crucible（5）And branch Support（3）, the supersonic generator（1）It is connected with ultrasonic amplitude transformer（4）；
    Support frame as described above（3）Including fixing sleeve（31）, N number of first support bar（32）Second support bar is vertically arranged with N number of（33）, The fixing sleeve（31）It is sleeved on supersonic generator（1）On, N number of first support bar（32）With fixing sleeve（31）It is equal for axis Even distribution；
    The first support bar（32）One end be both connected to fixing sleeve（31）The upper, other end is and second support bar（33）It is upper End is connected to realize to supersonic generator（1）Supporting role；
    The N is the natural number more than or equal to 2.
  6. 6. ultrasonic wave crucible heater according to claim 5, it is characterised in that：The first support bar（32）For that can stretch Contracting bar.
  7. 7. ultrasonic wave crucible heater according to claim 5, it is characterised in that：Second support bar（33）To be scalable Bar.
  8. 8. ultrasonic wave crucible heater according to claim 5, it is characterised in that：The first support bar（32）With second Supporting rod（33）It is aluminum alloy material, the ultrasonic amplitude transformer（4）For II type ultrasonic transformer of full titanium alloy material, the N is 3。
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Citations (4)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN103484707A (en) * 2013-09-23 2014-01-01 同济大学 Preparation method for SiC particle reinforced aluminum-based composite material
CN105063562A (en) * 2015-07-29 2015-11-18 西北有色金属研究院 Preparation method of fiber-reinforced titanium/aluminum base composite material precursor
CN106435283A (en) * 2016-03-07 2017-02-22 中安顺兴（北京）安全技术有限公司 Rare earth high-strength foam aluminum prepared through melt foaming method and preparation process of rare earth high-strength foam aluminum
CN106521252A (en) * 2016-12-07 2017-03-22 中南大学 Silicon carbide particle reinforcement aluminum-based composite for train brake disc and preparation method

Patent Citations (4)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN103484707A (en) * 2013-09-23 2014-01-01 同济大学 Preparation method for SiC particle reinforced aluminum-based composite material
CN105063562A (en) * 2015-07-29 2015-11-18 西北有色金属研究院 Preparation method of fiber-reinforced titanium/aluminum base composite material precursor
CN106435283A (en) * 2016-03-07 2017-02-22 中安顺兴（北京）安全技术有限公司 Rare earth high-strength foam aluminum prepared through melt foaming method and preparation process of rare earth high-strength foam aluminum
CN106521252A (en) * 2016-12-07 2017-03-22 中南大学 Silicon carbide particle reinforcement aluminum-based composite for train brake disc and preparation method

Non-Patent Citations (1)

* Cited by examiner, † Cited by third party
Title
SiCp +Gr/024Al 复合材料的力学性能和加工性能;冷金凤;《稀有金属》;20161230;第30卷;第20-23页 *

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