CN109182821A - A kind of pressure casting method of graphene enhancing ADC12 aluminium alloy - Google Patents
A kind of pressure casting method of graphene enhancing ADC12 aluminium alloy Download PDFInfo
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- CN109182821A CN109182821A CN201811079791.6A CN201811079791A CN109182821A CN 109182821 A CN109182821 A CN 109182821A CN 201811079791 A CN201811079791 A CN 201811079791A CN 109182821 A CN109182821 A CN 109182821A
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- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical compound [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 title claims abstract description 72
- 229910021389 graphene Inorganic materials 0.000 title claims abstract description 66
- 238000000034 method Methods 0.000 title claims abstract description 37
- 229910000838 Al alloy Inorganic materials 0.000 title claims abstract description 22
- 238000005266 casting Methods 0.000 title claims abstract description 12
- 230000002708 enhancing effect Effects 0.000 title claims abstract description 9
- GWEVSGVZZGPLCZ-UHFFFAOYSA-N Titan oxide Chemical compound O=[Ti]=O GWEVSGVZZGPLCZ-UHFFFAOYSA-N 0.000 claims abstract description 46
- 229960005196 titanium dioxide Drugs 0.000 claims abstract description 33
- OGIDPMRJRNCKJF-UHFFFAOYSA-N titanium oxide Inorganic materials [Ti]=O OGIDPMRJRNCKJF-UHFFFAOYSA-N 0.000 claims abstract description 33
- 239000000956 alloy Substances 0.000 claims abstract description 25
- 229910045601 alloy Inorganic materials 0.000 claims abstract description 20
- 229910052782 aluminium Inorganic materials 0.000 claims abstract description 19
- XAGFODPZIPBFFR-UHFFFAOYSA-N aluminium Chemical compound [Al] XAGFODPZIPBFFR-UHFFFAOYSA-N 0.000 claims abstract description 18
- 239000002245 particle Substances 0.000 claims abstract description 17
- 238000004512 die casting Methods 0.000 claims abstract description 15
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 claims abstract description 14
- 239000002131 composite material Substances 0.000 claims abstract description 12
- 239000000843 powder Substances 0.000 claims abstract description 12
- 239000004411 aluminium Substances 0.000 claims abstract description 10
- 239000002002 slurry Substances 0.000 claims abstract description 7
- XKRFYHLGVUSROY-UHFFFAOYSA-N Argon Chemical compound [Ar] XKRFYHLGVUSROY-UHFFFAOYSA-N 0.000 claims description 40
- PEDCQBHIVMGVHV-UHFFFAOYSA-N Glycerine Chemical compound OCC(O)CO PEDCQBHIVMGVHV-UHFFFAOYSA-N 0.000 claims description 20
- 229910052786 argon Inorganic materials 0.000 claims description 20
- 239000000463 material Substances 0.000 claims description 20
- 239000000243 solution Substances 0.000 claims description 20
- VXUYXOFXAQZZMF-UHFFFAOYSA-N titanium(IV) isopropoxide Chemical compound CC(C)O[Ti](OC(C)C)(OC(C)C)OC(C)C VXUYXOFXAQZZMF-UHFFFAOYSA-N 0.000 claims description 17
- 238000001816 cooling Methods 0.000 claims description 15
- 239000011248 coating agent Substances 0.000 claims description 13
- 238000000576 coating method Methods 0.000 claims description 13
- 239000006104 solid solution Substances 0.000 claims description 13
- 238000004458 analytical method Methods 0.000 claims description 12
- 230000032683 aging Effects 0.000 claims description 10
- 239000007789 gas Substances 0.000 claims description 10
- 235000011187 glycerol Nutrition 0.000 claims description 10
- 238000002347 injection Methods 0.000 claims description 10
- 239000007924 injection Substances 0.000 claims description 10
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims description 10
- 239000002893 slag Substances 0.000 claims description 9
- 238000010792 warming Methods 0.000 claims description 9
- 229910002804 graphite Inorganic materials 0.000 claims description 8
- 239000010439 graphite Substances 0.000 claims description 8
- 239000007788 liquid Substances 0.000 claims description 8
- 239000004615 ingredient Substances 0.000 claims description 7
- 239000011812 mixed powder Substances 0.000 claims description 7
- 239000000203 mixture Substances 0.000 claims description 7
- 238000004321 preservation Methods 0.000 claims description 7
- 238000007789 sealing Methods 0.000 claims description 7
- 238000002791 soaking Methods 0.000 claims description 7
- 238000002604 ultrasonography Methods 0.000 claims description 6
- 238000007872 degassing Methods 0.000 claims description 5
- 238000004033 diameter control Methods 0.000 claims description 5
- 238000001027 hydrothermal synthesis Methods 0.000 claims description 5
- 238000004886 process control Methods 0.000 claims description 5
- 239000000725 suspension Substances 0.000 claims description 5
- 238000002156 mixing Methods 0.000 claims description 4
- 239000003795 chemical substances by application Substances 0.000 claims description 2
- 238000005070 sampling Methods 0.000 claims description 2
- 238000004513 sizing Methods 0.000 claims description 2
- 238000001291 vacuum drying Methods 0.000 claims description 2
- 238000010438 heat treatment Methods 0.000 abstract description 8
- 230000000694 effects Effects 0.000 abstract description 5
- 238000005253 cladding Methods 0.000 abstract 1
- 125000000524 functional group Chemical group 0.000 abstract 1
- 150000002500 ions Chemical class 0.000 abstract 1
- 238000003825 pressing Methods 0.000 abstract 1
- 239000010936 titanium Substances 0.000 abstract 1
- 239000011159 matrix material Substances 0.000 description 10
- 238000007747 plating Methods 0.000 description 6
- PXHVJJICTQNCMI-UHFFFAOYSA-N Nickel Chemical compound [Ni] PXHVJJICTQNCMI-UHFFFAOYSA-N 0.000 description 4
- 238000004519 manufacturing process Methods 0.000 description 4
- 239000002243 precursor Substances 0.000 description 4
- 238000002360 preparation method Methods 0.000 description 4
- 239000000126 substance Substances 0.000 description 4
- -1 carboxyl graphite Alkene Chemical class 0.000 description 3
- 239000006185 dispersion Substances 0.000 description 3
- 230000005611 electricity Effects 0.000 description 3
- 239000010410 layer Substances 0.000 description 3
- 238000009210 therapy by ultrasound Methods 0.000 description 3
- 239000003575 carbonaceous material Substances 0.000 description 2
- 230000016507 interphase Effects 0.000 description 2
- 229910052759 nickel Inorganic materials 0.000 description 2
- 206010070834 Sensitisation Diseases 0.000 description 1
- 208000027418 Wounds and injury Diseases 0.000 description 1
- 230000004913 activation Effects 0.000 description 1
- 150000001336 alkenes Chemical class 0.000 description 1
- AZDRQVAHHNSJOQ-UHFFFAOYSA-N alumane Chemical compound [AlH3] AZDRQVAHHNSJOQ-UHFFFAOYSA-N 0.000 description 1
- 125000004432 carbon atom Chemical group C* 0.000 description 1
- 239000002041 carbon nanotube Substances 0.000 description 1
- 229910021393 carbon nanotube Inorganic materials 0.000 description 1
- 125000003178 carboxy group Chemical group [H]OC(*)=O 0.000 description 1
- 239000003153 chemical reaction reagent Substances 0.000 description 1
- 238000009833 condensation Methods 0.000 description 1
- 230000005494 condensation Effects 0.000 description 1
- 239000013078 crystal Substances 0.000 description 1
- 230000006378 damage Effects 0.000 description 1
- 230000007547 defect Effects 0.000 description 1
- 230000018109 developmental process Effects 0.000 description 1
- 238000005516 engineering process Methods 0.000 description 1
- 239000012530 fluid Substances 0.000 description 1
- 208000014674 injury Diseases 0.000 description 1
- 238000011031 large-scale manufacturing process Methods 0.000 description 1
- 238000011068 loading method Methods 0.000 description 1
- 229910052751 metal Inorganic materials 0.000 description 1
- 239000002184 metal Substances 0.000 description 1
- 239000007769 metal material Substances 0.000 description 1
- 230000000704 physical effect Effects 0.000 description 1
- 230000001681 protective effect Effects 0.000 description 1
- 239000011241 protective layer Substances 0.000 description 1
- 238000011084 recovery Methods 0.000 description 1
- 238000001953 recrystallisation Methods 0.000 description 1
- 230000003014 reinforcing effect Effects 0.000 description 1
- 239000012779 reinforcing material Substances 0.000 description 1
- 230000008313 sensitization Effects 0.000 description 1
- 238000005245 sintering Methods 0.000 description 1
- 230000035882 stress Effects 0.000 description 1
- 239000002344 surface layer Substances 0.000 description 1
- 231100000331 toxic Toxicity 0.000 description 1
- 230000002588 toxic effect Effects 0.000 description 1
- 239000002699 waste material Substances 0.000 description 1
Classifications
-
- 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
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B22—CASTING; POWDER METALLURGY
- B22D—CASTING OF METALS; CASTING OF OTHER SUBSTANCES BY THE SAME PROCESSES OR DEVICES
- B22D17/00—Pressure die casting or injection die casting, i.e. casting in which the metal is forced into a mould under high pressure
-
- C—CHEMISTRY; METALLURGY
- C22—METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
- C22B—PRODUCTION AND REFINING OF METALS; PRETREATMENT OF RAW MATERIALS
- C22B9/00—General processes of refining or remelting of metals; Apparatus for electroslag or arc remelting of metals
- C22B9/02—Refining by liquating, filtering, centrifuging, distilling, or supersonic wave action including acoustic waves
- C22B9/026—Refining by liquating, filtering, centrifuging, distilling, or supersonic wave action including acoustic waves by acoustic waves, e.g. supersonic waves
-
- 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
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- Chemical & Material Sciences (AREA)
- Engineering & Computer Science (AREA)
- Mechanical Engineering (AREA)
- Materials Engineering (AREA)
- Metallurgy (AREA)
- Organic Chemistry (AREA)
- Physics & Mathematics (AREA)
- Acoustics & Sound (AREA)
- Manufacturing & Machinery (AREA)
- Manufacture Of Alloys Or Alloy Compounds (AREA)
- Carbon And Carbon Compounds (AREA)
Abstract
A kind of pressure casting method of graphene enhancing ADC12 aluminium alloy adsorbs Ti ion using alcohol thermal high, and in the case where carboxylated graphene GO carries functional group's effect, and TiO2(anatase titanium dioxide is obtained in after baking in water-less environment) cladding carboxylated graphene GO.Gained powder and pure aluminium powder are mixed in a certain ratio cold pressing and obtain intermediate alloy.Intermediate alloy is added in aluminium alloy melt on demand, titanium-oxide-coated graphene GO particle disperses under the action of high-energy ultrasonic instrument.Gained slurry is poured into die casting machine cast gate and carries out die casting, obtains die casting blank, blank is then subjected to T6 heat treatment, obtains high performance composite material under the effect of correct technological parameter.Product prepared by the present invention has excellent mechanical performance, meanwhile, the present invention has many advantages, such as simple, safe, easily operated and controllable.
Description
Technical field
The invention belongs to technical field of material.
Background technique
The two-dimensional material for the monoatomic layer thickness that graphene nanometer sheet is made of sp2 hydbridized carbon atoms, shows one
The unusual physical property of series.Graphene nanometer sheet causes physics, chemistry and materialogy because of its special two-dimensional structure
The great interest of boundary researcher, basic research and engineering Application Research in relation to graphene become research hotspot in recent years.
Since graphene has high intensity, tensile strength up to 130GPa, imply graphene have in material application study it is huge
Big application space.
In fact, enhancing using carbon material such as carbon nanotube or graphene the intensity and other mechanical properties of aluminium
Research is carrying out always, and achieves a degree of progress.However, due to physical characteristics such as its intensity extremely outstanding, people
Ignore its excellent attribute in material abrasiveness and hardness instead.
With the development of national economy, people have harsher requirement to the high speed and heavy loading of apparatus of transport.Such as
It is required that higher temperature is born on the brake disc surface layer of apparatus of transport in braking, corresponding aluminum material is needed to have superior resistance to
Grind performance and better heat resistance etc..A large number of studies show that the correct selection of reinforced phase can directly improve the wear-resisting of composite material
Performance and hardness.And carboxylated graphene is due to the essential attribute of its carbon material, its self-lubricating of natural succession and preferable
Thermal diffusivity etc. is different from the speciality of other reinforcing materials.Thus correctly using the loss that can efficiently reduce material.
The defect of right carboxylated graphene is also more obvious.Carboxylated graphene shows very poor similar to the structure of CNT
Wetability, this directly results in not strong with metallic matrix interfacial bonding property, is unfavorable for the preparation of composite material.Thus, improve
Its wetability with matrix simultaneously selects correct process to become the key using graphene enhancing metal_based material.
Carboxylated graphene, which improves wetability method, at present overlay coating etc., and such as chemical nickel plating, this method mainly will
The graphene of carboxylated is through sensitization plays, after activation, is put into plating in chemical plating fluid, as the progress of reaction can be in carboxyl graphite
Alkene surface obtains graininess coating, but expensive, and commonly uses toxic reagent, not environmentally and high production cost, is not suitable for big
Large-scale production.
In publication 106702193A, title are as follows: in " a kind of preparation method of graphene/aluminum composite material ".Benefit
Graphene is pre-processed with chemical plating to obtain the graphene of nickel plating.Powder is mixed again carries out conventional hot-press sintering.In fact the party
Method due to chemical plating limitation, it is larger to human injury, and it also requires the production cycle is long individually to graphene carboxylated,
It is higher for such powder waste degree, there is certain limitation.
Therefore, still lack a kind of cost-effective carboxylated graphene reinforced aluminum matrix composites preparation and forming at present
Technology.
Summary of the invention
The object of the present invention is to provide a kind of pressure casting methods of graphene enhancing ADC12 aluminium alloy.It is to utilize alcohol heating method
One layer of titanium oxide is coated in carboxylated graphene surface, and utilizes the cavitation of high-energy ultrasonic and sound when reinforced phase is added to matrix
Stream effect is evenly dispersed in nanometer reinforcing phase in matrix.This method is at low cost, can produce in enormous quantities.Meanwhile institute's shape
AtAluminium/ graphene interface is by titanium oxide layer stable bond, and binding performance is preferable, and resulting composite material crystal grain is tiny, machine
Tool is had excellent performance.
The content of titanium-oxide-coated carboxylated graphene, the control of environment and technological parameter be really during die casting
Fixed extremely important, these three links are all linked with one another, all directly affect the quality of product.
Concrete principle of the invention are as follows: by the cavitation and acoustic streaming effect of high-energy ultrasonic, by titanium-oxide-coated carboxyl fossil
Black alkene particle uniformly diffuses in matrix.For reduce titanium-oxide-coated graphene particles reunion situation, by alcohol heating method to carboxylic
Base graphite alkene surface is handled, its surface is made to be coated with titanium oxide as stable particle protective layer.Meanwhile it is multiple in preparation
During condensation material slurry, high-energy ultrasonic vibration is introduced, reinforced phase and interphase can be effectively dispersed, improves composite machine
Tool performance.During die casting solidifies, it can effectively enhance aluminium/graphene interface bond strength, keep carboxylated graphene more steady
Fixed fixation in the base, to obtain the product of very good mechanical properties.
The present invention is achieved by the following technical solutions.
A kind of pressure casting method of graphene enhancing ADC12 aluminium alloy of the present invention, includes the following steps.
(1) by carboxylated graphene in analysis straight alcohol the pre-dispersed 1 ~ 3h of ultrasound, temperature is room temperature, and whole-process control is anhydrous
Vapour.Volume ratio is controlled in 0.2 ~ 0.4:50.
(2) the pretreated carboxylated graphene dispersing solution of step (1) is poured into glycerine and tetraisopropyl titanate forms
Precursor liquid in seal, and again be ultrasonically treated 1 ~ 1.5h.Wherein, glycerine and tetraisopropyl titanate volume ratio be 10:0.4 ~
1.2。
(3) forerunner's suspension of step (2) is imported in hydrothermal reaction kettle, wherein suspension volume accounts for the molten product of reaction kettle
35%~70%.Place into reacting furnace and heat, be warming up to 70~110 DEG C with 1~5 DEG C/min, keep the temperature 1~2h, then with 1~3 DEG C/
After min is warming up to 175 ~ 180 DEG C, 10~15h is kept the temperature；It takes out, reaction kettle sealing is air-cooled.
(4) solution obtained by step (3) is taken out, centrifugal treating, and be repeatedly centrifuged by pouring into analysis straight alcohol to solution
Colourless, revolving speed is controlled in 9000 ~ 16000rpm.Whole process sealing guarantees without steam.
(5) then the mixed-powder vacuum drying that step (4) is obtained roasts in 450 ~ 500 DEG C under protection of argon gas.When
Between control in 1 ~ 3h.The carboxylated graphene that surface has needle-shaped anatase type titanium oxide coating can be obtained.
(6) surface for obtaining step (5) have needle-shaped anatase type titanium oxide coating carboxylated graphene particles with it is pure
Aluminium powder mixing, mixing ratio 1:4 are prepared into titanium-oxide-coated carboxylic by mixed-powder by being cold-pressed the pressure maintaining 10min at 400MPa
Base graphite alkene/aluminium prefabricated section, then shreds prefabricated section.
(7) ADC12 aluminium alloy is put into graphite crucible, 750 °C are then heated in well formula resistance furnace and kept the temperature straight
To fusing.After ADC12 Al alloy block is completely melt, alloy melt is refined, degasification and except Slag treatment.Then by step
(6) the titanium-oxide-coated carboxylated graphene/aluminum prefabricated section obtained is added in alloy melt, by the additional amount of prefabricated section come
Controlling titanium-oxide-coated graphene particles content in product is 0.5 ~ 2.5wt%.
(8) then ultrasonic amplitude transformer is inserted into melt and high-energy ultrasonic processing is carried out to alloy melt, which is passed through argon
Gas is protected, argon flow 20L/min, argon pressure 0.45MPa.Its technological parameter are as follows: ultrasonic power be 1.5 ~
2.5Kw, supersonic frequency are 15000 ~ 25000Hz, and ultrasonic time is 10 ~ 20min.
(9) composite material sizing agent of step (8) is kept the temperature into 15min, gained blend melt is skimmed after heat preservation, is taken off
Melt temperature of the ingredient after qualified is down to 680 ~ 710 DEG C of heat preservation for standby use by sampling analysis after slag.
(10) slurry of the ingredient obtained by step (9) after qualified is poured into die casting machine cast gate, is cast into column aluminum alloy materials；
Die-casting process setting is as follows: pouring temperature control is 680 ~ 710 DEG C, and material handle thickness control is 25mm, and mold temperature control is 150
~170℃；The control of injection power is 330kN, and tup diameter control is 60mm；Injection pressure control is 116MPa, shot time control
For 3S, control cooling time is 2S, and mould remaining time control is 10S；Die shank actuating length position in press casting procedure are as follows: slow shot rises
Beginning position control is 80mm, and the control of fast shot initial position is 270mm, and pressurization position control is 280mm, and tracing positional control is
350mm。
(11) blank obtained to step (10), which is placed in resistance furnace, carries out first order solution treatment, and solid solution temperature is
It 440 ± 3 DEG C, soaking time 2.5 ~ 3.5 hours, is put into rapidly afterwards cooling in the water that temperature is 20 DEG C.
(12) material obtained to step (11), which is placed in resistance furnace, carries out second level solution treatment, and solid solution temperature is
It 480 ± 3 DEG C, soaking time 1.5 ~ 2.5 hours, is put into rapidly afterwards cooling in the water that temperature is 20 DEG C.
(13) ageing treatment is carried out at a temperature of step (12) resulting material being placed in 125 ± 3 DEG C, aging time is 5 ~ 6
Hour, it is then air-cooled.
The present invention using alcohol heating method handle titanium-oxide-coated carboxylated graphene surface, with improve carboxylated graphene and
Interface bond strength between ADC12 matrix, and uniformly disperse titanium-oxide-coated carboxylated graphene by introducing high-energy ultrasonic
Particle, wherein the content of titanium-oxide-coated carboxylated graphene in the product is 0.5wt% ~ 2.5wt%.
The present invention has following uniqueness: (1) making the enhancing in product using the cavitation of high-energy ultrasonic and acoustic streaming effect
It is mutually evenly dispersed.(2) the carboxylated graphene particles in coating are same with more preferable interface due to there is the protective effect of titanium oxide
When, the wetability with metal is increased, carboxylated graphene particles reunion probability is further reduced.(3) in T6 heat treatment
The internal stress that material internal generates in press casting procedure can be efficiently reduced in the process, and can effectively be divided by recovery and recrystallization
Reinforced phase and interphase are dissipated, to obtain the excellent product of mechanical performance.
Specific embodiment
The present invention will be described further by following embodiment.
Embodiment 1.
By carboxylated graphene in the analysis straight alcohol clock pre-dispersed 1h of ultrasound, temperature is room temperature, and whole-process control is without steam.Body
Product than control in 0.2:50, after gained dispersion liquid is poured into the precursor liquid of glycerine and tetraisopropyl titanate composition and seals ultrasound
Handle 1h.Among these, glycerine and tetraisopropyl titanate volume ratio are 10:0.9.Hydro-thermal process is carried out later, wherein suspension
Volume accounts for the molten product 60% of reaction kettle.Place into reacting furnace and heat, be warming up to 100 DEG C with 5 DEG C/min, keep the temperature 2h, then with 3 DEG C/
After min is warming up to 180 DEG C, 10h is kept the temperature.It is air-cooled after taking-up reaction kettle.Gained solution takes out, centrifugal treating, and by pouring into point
Analysis straight alcohol is repeatedly centrifuged colourless to solution.Whole process sealing guarantees without steam.It afterwards will be in gained powder under protection of argon gas 450 DEG C
Roasting.Time controls in 2h.The carboxylated graphene that surface has needle-shaped anatase type titanium oxide coating can be obtained.
There are the carboxylated graphene particles of needle-shaped anatase type titanium oxide coating to mix with pure aluminium powder obtained surface, mixes
Composition and division in a proportion is 1:4, by mixed-powder by being cold-pressed into prefabricated section.ADC12 aluminium alloy is put into graphite crucible, then in well formula electricity
It is heated to 750 DEG C in resistance furnace and keeps the temperature until fusing.After ADC12 Al alloy block is completely melt, alloy melt is refined,
Degasification and remove Slag treatment.Then prefabricated titanium-oxide-coated carboxylated graphene/aluminum prefabricated section is added in alloy melt,
It is 0.5wt% that titanium-oxide-coated carboxylated graphene particles content in composite material is controlled by the additional amount of prefabricated section.Then
Ultrasonic amplitude transformer is inserted into melt, high-energy ultrasonic processing, technological parameter are carried out to alloy melt are as follows: ultrasonic power is
1.5Kw, supersonic frequency 15000Hz, ultrasonic time 10min.The process is passed through argon gas and is protected, argon flow 20L/
Min, argon pressure 0.45MPa.15min is kept the temperature after ultrasonic treatment, and then alloy melt is carried out except Slag treatment.It will be at
Melt temperature after division lattice is down to 680 DEG C of heat preservation for standby use.
Slurry after ingredient is qualified pours into die casting machine cast gate, is cast into column aluminum alloy materials；Die-casting process setting is as follows:
Pouring temperature control is 680 DEG C, and material handle thickness control is 25mm, and mold temperature control is 150 DEG C；The control of injection power is 330kN,
Tup diameter control is 60mm；Injection pressure control is 116MPa, and shot time control is 3S, and cooling time, control was 2S, was stayed
The control of mould time is 10S；Die shank actuating length position in press casting procedure are as follows: the control of slow shot initial position is 80mm, fast shot
Initial position control is 270mm, and pressurization position control is 280mm, and tracing positional control is 350mm.Resulting blank is carried out
Obtained blank is placed in progress first order solution treatment in resistance furnace by T6 heat treatment, and solid solution temperature is 420 ± 3 DEG C, is protected
2.5 hours warm time was put into rapidly cooling in the water that temperature is 20 DEG C afterwards.It is subsequently placed in resistance furnace and carries out at the solid solution of the second level
Reason, solid solution temperature are 460 ± 3 DEG C, soaking time 1.5 hours, are put into rapidly afterwards cooling in the water that temperature is 20 DEG C.Finally
Ageing treatment is carried out at a temperature of resulting material is placed in 125 ± 3 DEG C, aging time is 5 hours, subsequent air-cooled, obtained production
Its ultimate tensile strength of product improves 19.48% compared with matrix.
Embodiment 2.
By carboxylated graphene in the analysis straight alcohol clock pre-dispersed 1h of ultrasound, temperature is room temperature, and whole-process control is without steam.Body
Product ratio is strict controlled in 0.2:50, after gained dispersion liquid poured into the precursor liquid that glycerine and tetraisopropyl titanate form seal
It is ultrasonically treated 1h.Among these, glycerine and tetraisopropyl titanate volume ratio are 10:0.4.Hydro-thermal process is carried out later, wherein hanging
Turbid volume accounts for the molten product 50% of reaction kettle.It places into reacting furnace and heats, be warming up to 90 DEG C with 5 DEG C/min, keep the temperature 2h, then with 2
DEG C/after min is warming up to 180 DEG C, keep the temperature 10h.It is air-cooled after taking-up reaction kettle.Gained solution takes out, centrifugal treating, and by pouring into
Analysis straight alcohol is repeatedly centrifuged colourless to solution.Whole process sealing guarantees without steam.Afterwards by 480 DEG C under protection of argon gas of gained powder
Middle roasting.Time controls in 1.5h.The carboxylated graphene that surface has needle-shaped anatase type titanium oxide coating can be obtained.
There are the carboxylated graphene particles of needle-shaped anatase type titanium oxide coating to mix with pure aluminium powder obtained surface, mixes
Composition and division in a proportion is 1:4, by mixed-powder by being cold-pressed into prefabricated section.ADC12 aluminium alloy is put into graphite crucible, then in well formula electricity
It is heated to 750 DEG C in resistance furnace and keeps the temperature until fusing.After ADC12 Al alloy block is completely melt, alloy melt is refined,
Degasification and remove Slag treatment.Then prefabricated titanium-oxide-coated carboxylated graphene/aluminum prefabricated section is added in alloy melt,
It is 1.5wt% that titanium-oxide-coated carboxylated graphene particles content in composite material is controlled by the additional amount of prefabricated section.Then
Ultrasonic amplitude transformer is inserted into melt, high-energy ultrasonic processing, technological parameter are carried out to alloy melt are as follows: ultrasonic power is
2.5Kw, supersonic frequency 25000Hz, ultrasonic time 15min.The process is passed through argon gas and is protected, argon flow 20L/
Min, argon pressure 0.45MPa.15min is kept the temperature after ultrasonic treatment, and then alloy melt is carried out except Slag treatment.It will be at
Melt temperature after division lattice is down to 710 DEG C of heat preservation for standby use.
Slurry after ingredient is qualified pours into die casting machine cast gate, is cast into column aluminum alloy materials；Die-casting process setting is as follows:
Pouring temperature control is 710 DEG C, and material handle thickness control is 25mm, and mold temperature control is 170 DEG C；The control of injection power is 330kN,
Tup diameter control is 60mm；Injection pressure control is 116MPa, and shot time control is 3S, and cooling time, control was 2S, was stayed
The control of mould time is 10S；Die shank actuating length position in press casting procedure are as follows: the control of slow shot initial position is 80mm, fast shot
Initial position control is 270mm, and pressurization position control is 280mm, and tracing positional control is 350mm.Resulting blank is carried out
Obtained blank is placed in progress first order solution treatment in resistance furnace by T6 heat treatment, and solid solution temperature is 420 ± 3 DEG C, is protected
3.5 hours warm time was put into rapidly cooling in the water that temperature is 20 DEG C afterwards.It is subsequently placed in resistance furnace and carries out at the solid solution of the second level
Reason, solid solution temperature are 460 ± 3 DEG C, soaking time 1.5 hours, are put into rapidly afterwards cooling in the water that temperature is 20 DEG C.Finally
Ageing treatment is carried out at a temperature of resulting material is placed in 125 ± 3 DEG C, aging time is 5 hours, subsequent air-cooled, obtained production
Its ultimate tensile strength of product improves 23.21% compared with matrix.
Embodiment 3.
By carboxylated graphene in the analysis straight alcohol clock pre-dispersed 1h of ultrasound, temperature is room temperature, and whole-process control is without steam.Body
Product ratio is strict controlled in 0.2:50, after gained dispersion liquid poured into the precursor liquid that glycerine and tetraisopropyl titanate form seal
It is ultrasonically treated 1h.Among these, glycerine and tetraisopropyl titanate volume ratio are 10:0.4.Hydro-thermal process is carried out later, wherein hanging
Turbid volume accounts for the molten product 50% of reaction kettle.It places into reacting furnace and heats, be warming up to 90 DEG C with 5 DEG C/min, keep the temperature 2h, then with 2
DEG C/after min is warming up to 180 DEG C, keep the temperature 10h.It is air-cooled after taking-up reaction kettle.Gained solution takes out, centrifugal treating, and by pouring into
Analysis straight alcohol is repeatedly centrifuged colourless to solution.Whole process sealing guarantees without steam.Afterwards by 480 DEG C under protection of argon gas of gained powder
Middle roasting.Time controls in 1.5h.The carboxylated graphene that surface has needle-shaped anatase type titanium oxide coating can be obtained.
There are the carboxylated graphene particles of needle-shaped anatase type titanium oxide coating to mix with pure aluminium powder obtained surface, mixes
Composition and division in a proportion is 1:4, by mixed-powder by being cold-pressed into prefabricated section.ADC12 aluminium alloy is put into graphite crucible, then in well formula electricity
It is heated to 750 DEG C in resistance furnace and keeps the temperature until fusing.After ADC12 Al alloy block is completely melt, alloy melt is refined,
Degasification and remove Slag treatment.Then prefabricated titanium-oxide-coated carboxylated graphene/aluminum prefabricated section is added in alloy melt,
It is 1.5wt% that titanium-oxide-coated carboxylated graphene particles content in composite material is controlled by the additional amount of prefabricated section.Then
Ultrasonic amplitude transformer is inserted into melt, high-energy ultrasonic processing, process parameter control are carried out to alloy melt are as follows: ultrasonic power is
2.5Kw, supersonic frequency 25000Hz, ultrasonic time 15min.The process is passed through argon gas and is protected, argon flow 20L/
Min, argon pressure 0.45MPa.15min is kept the temperature after ultrasonic treatment, and then alloy melt is carried out except Slag treatment.It will be at
Melt temperature after division lattice is down to 710 DEG C of heat preservation for standby use.
Slurry after ingredient is qualified pours into die casting machine cast gate, is cast into column aluminum alloy materials；Die-casting process setting is as follows:
Pouring temperature control is 710 DEG C, and material handle thickness control is 25mm, and mold temperature control is 170 DEG C；The control of injection power is 330kN,
Tup diameter control is 60mm；Injection pressure control is 116MPa, and shot time control is 3S, and cooling time, control was 2S, was stayed
The control of mould time is 10S；Die shank actuating length position in press casting procedure are as follows: the control of slow shot initial position is 80mm, fast shot
Initial position control is 270mm, and pressurization position control is 280mm, and tracing positional control is 350mm.Resulting blank is carried out
Obtained blank is placed in progress first order solution treatment in resistance furnace by T6 heat treatment, and solid solution temperature is 420 ± 3 DEG C, is protected
3.5 hours warm time was put into rapidly cooling in the water that temperature is 20 DEG C afterwards.It is subsequently placed in resistance furnace and carries out at the solid solution of the second level
Reason, solid solution temperature are 460 ± 3 DEG C, soaking time 2.5 hours, are put into rapidly afterwards cooling in the water that temperature is 20 DEG C.Finally
Ageing treatment is carried out at a temperature of resulting material is placed in 125 ± 3 DEG C, aging time is 6 hours, subsequent air-cooled obtained product
Its ultimate tensile strength improves 20.38% compared with matrix.
Claims (1)
1. a kind of pressure casting method of graphene enhancing ADC12 aluminium alloy, it is characterized in that the following steps are included:
(1) by carboxylated graphene in analysis straight alcohol the pre-dispersed 1 ~ 3h of ultrasound, temperature is room temperature, and whole-process control is without steam；
Volume ratio is controlled in 0.2 ~ 0.4:50；
(2) before the pretreated carboxylated graphene dispersing solution of step (1) being poured into glycerine and tetraisopropyl titanate composition
It drives in liquid and seals, and be ultrasonically treated 1 ~ 1.5h again；Wherein, glycerine and tetraisopropyl titanate volume ratio are 10:0.4 ~ 1.2；
(3) forerunner's suspension of step (2) is imported in hydrothermal reaction kettle, wherein suspension volume account for the molten product of reaction kettle 35%~
70%；It places into reacting furnace and heats, be warming up to 70~110 DEG C with 1~5 DEG C/min, keep the temperature 1~2h, then with 1~3 DEG C/min liter
Temperature keeps the temperature 10~15h to after 175 ~ 180 DEG C；It takes out, reaction kettle sealing is air-cooled；
(4) solution obtained by step (3) is taken out, centrifugal treating, and by pour into analysis straight alcohol be repeatedly centrifuged it is colourless to solution,
Revolving speed is controlled in 9000 ~ 16000rpm；Whole process sealing guarantees without steam；
(5) then the mixed-powder vacuum drying that step (4) is obtained roasts in 450 ~ 500 DEG C under protection of argon gas；Time control
System is in 1 ~ 3h；The carboxylated graphene that surface has needle-shaped anatase type titanium oxide coating can be obtained；
(6) surface for obtaining step (5) has the carboxylated graphene particles and pure aluminium powder of needle-shaped anatase type titanium oxide coating
Mixing, mixing ratio 1:4 are prepared into titanium-oxide-coated carboxylated by mixed-powder by being cold-pressed the pressure maintaining 10min at 400MPa
Graphene/aluminum prefabricated section, then shreds prefabricated section；
(7) ADC12 aluminium alloy is put into graphite crucible, 750 °C are then heated in well formula resistance furnace and kept the temperature until molten
Change；After ADC12 Al alloy block is completely melt, alloy melt is refined, degasification and except Slag treatment；Then by step (6)
Obtained titanium-oxide-coated carboxylated graphene/aluminum prefabricated section is added in alloy melt, is controlled by the additional amount of prefabricated section
Titanium-oxide-coated graphene particles content is 0.5 ~ 2.5wt% in product processed；
(8) then by ultrasonic amplitude transformer be inserted into melt in alloy melt carry out high-energy ultrasonic processing, the process be passed through argon gas into
Row protection, argon flow 20L/min, argon pressure 0.45MPa；Its technological parameter are as follows: ultrasonic power is 1.5 ~ 2.5Kw,
Supersonic frequency is 15000 ~ 25000Hz, and ultrasonic time is 10 ~ 20min；
(9) composite material sizing agent of step (8) is kept the temperature into 15min, gained blend melt is skimmed after heat preservation, after skimming
Melt temperature of the ingredient after qualified is down to 680 ~ 710 DEG C of heat preservation for standby use by sampling analysis；
(10) slurry of the ingredient obtained by step (9) after qualified is poured into die casting machine cast gate, is cast into column aluminum alloy materials；Die casting
Technique initialization is as follows: pouring temperature control is 680 ~ 710 DEG C, and material handle thickness control is 25mm, and mold temperature control is 150 ~ 170
℃；The control of injection power is 330kN, and tup diameter control is 60mm；Injection pressure control is 116MPa, and shot time control is
3S, control cooling time are 2S, and mould remaining time control is 10S；Die shank actuating length position in press casting procedure are as follows: slow shot starting
Position control is 80mm, and the control of fast shot initial position is 270mm, and pressurization position control is 280mm, and tracing positional control is
350mm；
(11) blank obtained to step (10), which is placed in resistance furnace, carries out first order solution treatment, solid solution temperature 440
It ± 3 DEG C, soaking time 2.5 ~ 3.5 hours, is put into rapidly afterwards cooling in the water that temperature is 20 DEG C；
(12) material obtained to step (11), which is placed in resistance furnace, carries out second level solution treatment, solid solution temperature 480
It ± 3 DEG C, soaking time 1.5 ~ 2.5 hours, is put into rapidly afterwards cooling in the water that temperature is 20 DEG C；
(13) ageing treatment is carried out at a temperature of step (12) resulting material being placed in 125 ± 3 DEG C, aging time is 5 ~ 6 hours,
It is then air-cooled.
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