CN110358943A - A kind of alterant and carbon nanomaterial coordinate system for aluminum matrix composite method - Google Patents

A kind of alterant and carbon nanomaterial coordinate system for aluminum matrix composite method Download PDF

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CN110358943A
CN110358943A CN201910588143.1A CN201910588143A CN110358943A CN 110358943 A CN110358943 A CN 110358943A CN 201910588143 A CN201910588143 A CN 201910588143A CN 110358943 A CN110358943 A CN 110358943A
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ultrasonic
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alterant
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CN110358943B (en
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闫洪
熊俊杰
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Nanchang University
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    • CCHEMISTRY; METALLURGY
    • C22METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
    • C22CALLOYS
    • C22C1/00Making non-ferrous alloys
    • C22C1/10Alloys containing non-metals
    • C22C1/1036Alloys containing non-metals starting from a melt
    • CCHEMISTRY; METALLURGY
    • C22METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
    • C22CALLOYS
    • C22C21/00Alloys based on aluminium
    • C22C21/02Alloys based on aluminium with silicon as the next major constituent
    • C22C21/04Modified aluminium-silicon alloys
    • CCHEMISTRY; METALLURGY
    • C22METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
    • C22CALLOYS
    • C22C26/00Alloys containing diamond or cubic or wurtzitic boron nitride, fullerenes or carbon nanotubes
    • C22C2026/002Carbon nanotubes

Abstract

A kind of alterant and carbon nanomaterial coordinate system for aluminum matrix composite method, matrix alloy is put into crucible and is warming up to 740-750 DEG C, Al-Sr intermediate mass is added portionwise after fusing, Sr additive amount accounts for total melt weight 0.04-0.06wt.%, and applying ultrasound simultaneously, ultrasonic probe protrudes into melt about 3-5mm, ultrasonic power 1.4-2.8kW, frequency is 20kHZ, time 5-10min.After ultrasound is complete, melt is warming up to 770-780 DEG C of heat preservation 30-40min.Then under argon gas protection, Al-C intermediate mass is added portionwise into melt by different angle, carbon additional amount accounts for total melt weight 0.5-1.0wt.%, and applies ultrasonic 10-15min simultaneously, after ultrasound is complete, is poured when melt temperature is down to 700 DEG C.Present invention process is stablized, and securely and reliably, uniformly, performance obtains larger raising for the material structure refinement of preparation.

Description

A kind of alterant and carbon nanomaterial coordinate system for aluminum matrix composite method
Technical field
The invention belongs to technical field of metal material manufacture, and in particular to alterant and carbon nano-fiber coordinate system are for Al- The method of Si-Cu composite material.
Background technique
The casting character of Al-Si-Cu system alloy is excellent, specific strength with higher, lesser thermal expansion coefficient, preferably Corrosion resistance and excellent electrical and thermal conductivity performance, but the α-Al dendrite in cast sturcture is coarse, silicon be mutually in coarse plate or Person's strip, Fe-riched phase is needle-shaped in coarse length, these will lead to the reduction of its mechanical property, greatly limits answering for the alloy With.Studies have shown that preferable refinement and modification effect can not only be reached by adding a small amount of alterant in alusil alloy, also have Purify the effect of melt and degasification.Therefore, alterant element is selected to be of great significance come the tissue and performance for improving alusil alloy. And Sr is a kind of long-acting alterant, has oxidization burning loss few as aluminum-silicon alloy alterative, deteriorating time is long, easily absorbs, casting High yield rate, the advantages that melting tool and equipment will not be corroded.So selecting Sr as the alterant of Al-Si-Cu system alloy is One good selection.
It is CN101871067A, title in publication number are as follows: " a kind of strontium modified silicon-containing high-strength magnesium alloy and its preparation side Do not consider that the rotten alloy melt of Sr has strong suction hydrogen tendency in method ", in experimentation, melt, which inhales hydrogen, will cause casting appearance A large amount of precipitation property hydrogen blisterings, reduce surface quality of continuous castings and properties, may occur in which Hydrogen Brittleness Phenomena when serious;Furthermore in the patent In do not account for the rotten uniformity of Sr yet, be easy to produce segregation.
Studies have shown that importing high-energy ultrasound in metal bath, sound cavitation effect, acoustic streaming effect, exhaust can be generated Clean effect.The transient high temperature high pressure that sound cavitation effect generates changes local equilibrium, reduces the surface tension of liquid level simultaneously Strong local assault is generated, effect can be smashed strongly to reuniting with mutually generating.Meanwhile injection and circulation caused by acoustic streaming effect Effect has promoted the reinforced phase smashed in melt further to separate and homogenize.In addition, high-energy ultrasonic may additionally facilitate crystal grain The degasification of refinement and melt.
In recent years, application of the reinforced phase of nano-scale on aluminum matrix composite becomes the heat of numerous scientists research Point, carbon nanotube (abbreviation CNTs) is due to its unique structure and excellent physicochemical property by favor.CNTs receives as one kind The one-dimensional carbon material of meter level shows extremely excellent specific strength and specific stiffness, and tensile strength is about 100 times of steel, and Density but only has 1/6 or so of steel.CNTs also has preferable toughness, structural stability, therefore CNTs is considered as a kind of ideal Aluminum matrix composite reinforced phase.
In Publication No. CN101565782A, title are as follows: " a method of addition carbon nanotube is into metal bath " in, Carbon nanotube, metal powder and stearic acid are subjected to ball milling during the experiment, carbon nanotube can be caused not in mechanical milling process With the damage of degree;In addition, active combustion can occur when binder stearic acid is added to high temperature solution, it is hidden to there is safety Suffer from.
It is entitled " carbon nanotube enhances magnesium, aluminum matrix composite and preparation method thereof " in publication number CN101376932 In, reho-forming method preparation carbon nanotube is mixed after heating using powder enhances magnesium, aluminum matrix composite.The defect of this method It is that carbon nanotube is easy to reunite under rheological condition, this will reduce the mechanical property of material to a certain extent.
Summary of the invention
The purpose of the present invention is to propose to the preparation sides of a kind of alterant and carbon nanomaterial collaboration reinforced aluminum matrix composites Method.
The present invention is achieved by the following technical solutions.
A kind of alterant of the present invention and carbon nanomaterial coordinate system for aluminum matrix composite method, including it is following Step.
(1) preparation of experimental material.The accounting of each element in Al-Si-Cu alloy are as follows: the mass percent of Si is 10.5%- The mass percent 3.0%-3.5% of 11.5%, Cu, surplus Al.Alterant Sr is added in the form of Al-Sr intermediate alloy: The mass percent of Sr is 8%-10%, surplus Al.Carbon nanotube is added in the form of Al-C intermediate prefabricated block: the matter of C Amount percentage is 5%-7%, surplus Al.By Al-Si-Cu matrix alloy, Al-Sr intermediate alloy and Al-C intermediate prefabricated block of material It is put into vacuum oven and is dried for standby.
(2) Al-Si-Cu matrix alloy is put into graphite crucible and is warming up to 740-750 DEG C, taken off after it is completely melt Surface scum.Then Al-Sr intermediate alloy aluminium-foil paper cladding is added portionwise in graphite crucible, the total addition level of Sr accounts for molten The 0.04-0.06wt.% of body total weight.Apply high-energy ultrasonic auxiliary while Al-Sr is added, ultrasonic amplitude transformer probe protrudes into molten Depth in body is about 3-5mm, ultrasonic power 1.4-2.8kW, supersonic frequency 20kHZ, ultrasonic time 5-10min.It is super After sound is complete, alloy melt is warming up to 770-780 DEG C of heat preservation 30-40min, to ensure that Sr is melted into melt completely.
(3) it after having kept the temperature, is added portionwise into alloy melt by different angle and is cut into granular Al-C intermediate prefabricated block, The additional amount of carbon nano-fiber accounts for the 0.5-1.0wt.% of alloy melt total weight, applies high-energy ultrasonic in adition process, will be ultrasonic Amplitude transformer probe protrudes into about 3-5mm in melt, ultrasonic power 1.4-2.8kW, supersonic frequency 20kHZ, ultrasonic time 10- 15min.Whole applying argon gas is protected in the fusion-casting process.After ultrasound is complete, it is poured into when melt temperature is down to 700 DEG C pre- Heat cooperates with the aluminum matrix composite of enhancing in 300 DEG C of metal type dies, to can be prepared by alterant Sr and carbon nano-fiber.
Carbon nanotube of the present invention is commercially available conventional carbon nanotube.
Further, preferably, carbon nanotube of the present invention can be the vacuum gas-phase carbon nanometer of CVD method preparation Fiber, this kind of carbon nanotube have had both that curvature is low, and diameter change is small is not easy on the basis of having similar high elastic modulus and intensity The advantages that winding.Purity > 98% of carbon nano-fiber, diameter 50-200nm, length are 1-10 μm.Aluminium powder purity > 99.5%, grain Degree is 200-300 mesh.
Further, preferably, the preparation of Al-C intermediate prefabricated block of the present invention, can use following process: Carbon nano-fiber is matched in the ratio for accounting for mixed-powder (aluminium powder and carbon dust) mass fraction 5-7wt.%, first by carbon Nanowire Dimension mixed in beaker with dehydrated alcohol, after be put into ultrasonic cleaning instrument in carry out ultrasonic disperse processing 80-100min, ultrasound Power is 120W, frequency 42kHz.Then aluminium powder is uniformly sprinkled into the alcohol and carbon nano-fiber solution after ultrasound and continue Ultrasonic 40-60min.Mixed-powder alcohol liquid is placed under constant-temperature heating magnetic stirring apparatus effect after ultrasound is complete and is stirred, is added Hot temperature is 50 DEG C, mixing speed 1000r/min, mixing time 60-80min.Then mixed-powder vacuum is put into do Drying in dry case.Then the powder of drying is put into vacuum sintering funace and is sintered, sintering temperature is 430 DEG C -450 DEG C, hot pressing pressure is 60-80Mpa, finally obtains aluminium carbon intermediate prefabricated block, it is spare that the prefabricated section is finally cut into fine granularity.
Al-Sr intermediate alloy is added portionwise under conditions of high-energy ultrasonic assists in the present invention, not only reduces burn out rate, promotees Into rotten uniformity, moreover it is possible to effectively eliminate the suction hydrogen phenomenon in Sr metamorphic process.Carbon nanotube, the present invention are selected It is the vacuum gas-phase carbon nano-fiber of CVD method preparation, it is a kind of carbon nanotube of special construction, has similar high resiliency mould Have both that curvature is low, and diameter change is small is not easy the advantages that winding on the basis of amount and intensity.Addition for carbon nano-fiber, this hair Bright is and the Al-C intermediate prefabricated block by Al-C intermediate prefabricated block and with being added portionwise in the form of high-energy ultrasonic by different angle Preparation route be to be realized by way of pre-dispersed+vacuum heating-press sintering, this not only effectively reduces carbon nano-fiber Structural damage, while ensure that its dispersing uniformity in the melt.The present invention has gathered strontium and carbon nano-fiber simultaneously Advantage, process stabilizing are securely and reliably, easy to operate.Tissue is obviously refined in obtained aluminum matrix composite, carbon nanometer Fiber and matrix alloy interface cohesion are good, and distribution is also more uniform, the comprehensive mechanical property of obtained aluminum matrix composite Obtain larger raising.
Detailed description of the invention
Attached drawing 1 is the microstructure picture of aluminum matrix composite made from the embodiment of the present invention 2.
Specific embodiment
The present invention will be described further by following embodiment.
Embodiment 1.
(1) taking Al-Si-Cu alloy respectively, (mass percent that the mass percent of Si is 10.5%, Cu is 3.5%, surplus For Al), Al-8Sr intermediate alloy (mass percent of Sr is 8%), Al-5C intermediate prefabricated block (mass percent of C is 5%) is put Enter in vacuum oven and is dried for standby.
(2) matrix alloy is put into graphite crucible and is warming up to 740 DEG C, take surface scum off after it is completely melt.So The Al-8Sr intermediate alloy coated with aluminium-foil paper is added portionwise according to the ratio afterwards, the total addition level of Sr accounts for total melt weight 0.04wt.% applies high-energy ultrasonic while Sr is added, the depth that ultrasonic amplitude transformer probe protrudes into melt is about 3mm, ultrasound Power is 1.4kW, supersonic frequency 20kHZ, ultrasonic time 5min.After ultrasound is complete, alloy melt is warming up to 770 DEG C of heat preservations 30min, to ensure that Sr is melted into melt completely.
(3) it after having kept the temperature, is added portionwise into alloy melt by different angle and has been cut into granular Al-5C intermediate prefabricated Block, the additional amount of carbon nano-fiber account for the 0.6wt.% of alloy melt total weight, apply high-energy ultrasonic in adition process, will be ultrasonic Amplitude transformer probe protrudes into about 3mm in melt, ultrasonic power 1.4kW, supersonic frequency 20kHZ, ultrasonic time 10min.? Whole applying argon gas is protected in the fusion-casting process.After ultrasound is complete, it is 300 that preheating is poured into when melt temperature is down to 700 DEG C DEG C metal type dies in, can be prepared by alterant Sr and carbon fiber collaboration enhancing aluminum matrix composite.
The tensile strength and yield strength of the aluminum matrix composite prepared under this experiment condition are respectively than under the same terms Matrix alloy increases 56.4% and 32.7%.
Embodiment 2.
(1) taking Al-Si-Cu alloy respectively, (mass percent that the mass percent of Si is 11.0%, Cu is 3.2%, surplus For Al), Al-9Sr intermediate alloy (mass percent of Sr is 9%), Al-6C intermediate prefabricated block (the quality percentage of carbon nano-fiber Than being dried for standby 6%) to be put into vacuum oven.
(2) matrix alloy is put into graphite crucible and is warming up to 750 DEG C, take surface scum off after it is completely melt.So The Al-9Sr intermediate alloy coated with aluminium-foil paper is added portionwise according to the ratio afterwards, the total addition level of Sr accounts for total melt weight 0.05wt.% applies high-energy ultrasonic while Sr is added, the depth that ultrasonic amplitude transformer probe protrudes into melt is about 4mm, ultrasound Power is 2.1kW, supersonic frequency 20kHZ, ultrasonic time 8min.Then alloy melt is warming up to 780 DEG C of heat preservations 35min, to ensure that Sr is melted into melt completely.
(3) it after having kept the temperature, is added portionwise into alloy melt by different angle and has been cut into granular Al-6C intermediate prefabricated Block, the additional amount of C account for the 0.8wt.% of alloy melt total weight, apply high-energy ultrasonic in adition process, ultrasonic amplitude transformer is popped one's head in Protrude into about 4mm in melt, ultrasonic power 2.1kW, supersonic frequency 20kHZ, ultrasonic time 13min.
Whole applying argon gas is protected in the fusion-casting process.After ultrasound is complete, it is poured into when melt temperature is down to 700 DEG C Preheating cooperates with the aluminum matrix composite of enhancing in 300 DEG C of metal type dies, to can be prepared by alterant strontium and carbon fiber.
The tensile strength and yield strength of the aluminum matrix composite prepared under this experiment condition are respectively than under the same terms Matrix alloy increases 67.8% and 40.3%.
As can be seen that the tiny rounding of crystal grain, carbon nano-fiber are also distributed more uniformly from attached drawing 1, tissue obtains larger It refines to degree, therefore the comprehensive mechanical property of material has obtained larger raising.
Embodiment 3.
(1) taking Al-Si-Cu alloy respectively, (mass percent that the mass percent of Si is 11.5%, Cu is 3.0%, surplus For Al), Al-10Sr intermediate alloy (mass percent of Sr is 10%), the Al-7C intermediate prefabricated block (quality hundred of carbon nano-fiber Divide than being dried for standby 7%) to be put into vacuum oven.
(2) matrix alloy is put into graphite crucible and is warming up to 740 DEG C, take surface scum off after it is completely melt.So The Al-10Sr intermediate alloy coated with aluminium-foil paper is added portionwise according to the ratio afterwards, the total addition level of Sr accounts for total melt weight 0.06wt.% applies high-energy ultrasonic while Sr is added, the depth that ultrasonic amplitude transformer probe protrudes into melt is about 5mm, ultrasound Power is 2.8kW, supersonic frequency 20kHZ, ultrasonic time 10min.Then alloy melt is warming up to 780 DEG C of heat preservations 40min, to ensure that Sr is melted into melt completely.
(3) it after having kept the temperature, is added portionwise into alloy melt by different angle and has been cut into granular Al-7C intermediate prefabricated Block, the additional amount of carbon nano-fiber account for the 1.0wt.% of alloy melt total weight, apply high-energy ultrasonic in adition process, will be ultrasonic Amplitude transformer probe protrudes into about 5mm in melt, ultrasonic power 2.8kW, supersonic frequency 20kHZ, ultrasonic time 15min.? Whole applying argon gas is protected in the fusion-casting process.After ultrasound is complete, it is 300 that preheating is poured into when melt temperature is down to 700 DEG C DEG C metal type dies in, can be prepared by alterant strontium and carbon fiber collaboration enhancing aluminum matrix composite.
The tensile strength and yield strength of the aluminum matrix composite prepared under this experiment condition are respectively than under the same terms Matrix alloy increases 62.9% and 35.5%.

Claims (3)

1. a kind of alterant and carbon nanomaterial coordinate system be for the method for aluminum matrix composite, it is characterized in that the following steps are included:
(1) material prepares: the accounting of each element in Al-Si-Cu alloy are as follows: the mass percent of Si is 10.5%-11.5%, Cu's Mass percent 3.0%-3.5%, surplus Al;Alterant Sr is added in the form of Al-Sr intermediate alloy: the quality hundred of Sr Divide than being 8%-10%, surplus Al;Carbon nanotube is added in the form of Al-C intermediate prefabricated block: the mass percent of C is 5%-7%, surplus Al;Al-Si-Cu matrix alloy, Al-Sr intermediate alloy and Al-C intermediate prefabricated block of material are put into vacuum and done It is dried for standby in dry case;
(2) Al-Si-Cu matrix alloy is put into graphite crucible and is warming up to 740-750 DEG C, take surface off after it is completely melt Dross;Then Al-Sr intermediate alloy aluminium-foil paper cladding is added portionwise in graphite crucible, it is total that the total addition level of Sr accounts for melt The 0.04-0.06wt.% of weight;Apply high-energy ultrasonic auxiliary while Al-Sr is added, ultrasonic amplitude transformer probe protrudes into melt Depth be about 3-5mm, ultrasonic power 1.4-2.8kW, supersonic frequency 20kHZ, ultrasonic time 5-10min;Ultrasound is complete Afterwards, alloy melt is warming up to 770-780 DEG C of heat preservation 30-40min, to ensure that Sr is melted into melt completely;
(3) it after having kept the temperature, is added portionwise into alloy melt by different angle and is cut into granular Al-C intermediate prefabricated block, carbon is received The additional amount of rice fiber accounts for the 0.5-1.0wt.% of alloy melt total weight, applies high-energy ultrasonic in adition process, by ultrasonic amplitude of fluctuation Bar probe protrudes into about 3-5mm in melt, ultrasonic power 1.4-2.8kW, supersonic frequency 20kHZ, ultrasonic time 10- 15min;Whole applying argon gas is protected in the fusion-casting process;After ultrasound is complete, it is poured into when melt temperature is down to 700 DEG C pre- Heat cooperates with the aluminum matrix composite of enhancing in 300 DEG C of metal type dies, to can be prepared by alterant Sr and carbon nano-fiber.
2. a kind of alterant according to claim 1 and carbon nanomaterial coordinate system be for the method for aluminum matrix composite, It is characterized in that the carbon nanotube is the vacuum gas-phase carbon nano-fiber of CVD method preparation.
3. a kind of alterant according to claim 1 and carbon nanomaterial coordinate system be for the method for aluminum matrix composite, It is characterized in the preparation of the Al-C intermediate prefabricated block, using following process: first by carbon nano-fiber and dehydrated alcohol in beaker In mixed, after be put into ultrasonic cleaning instrument and carry out ultrasonic disperse processing 80-100min, ultrasonic power 120W, frequency is 42kHz;Then aluminium powder is uniformly sprinkled into the alcohol and carbon nano-fiber solution after ultrasound and continue ultrasonic 40-60min;Ultrasound Mixed-powder alcohol liquid is placed under constant-temperature heating magnetic stirring apparatus effect after complete and is stirred, heating temperature is 50 DEG C, stirring Speed is 1000r/min, mixing time 60-80min;Then mixed-powder is put into vacuum oven and is dried;Then will The powder of drying, which is put into vacuum sintering funace, to be sintered, and sintering temperature is 430 DEG C -450 DEG C, and hot pressing pressure is 60- 80Mpa finally obtains aluminium carbon intermediate prefabricated block, and it is spare that the prefabricated section is finally cut into fine granularity.
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CN112941360A (en) * 2021-01-11 2021-06-11 南昌大学 Preparation method of carbon nanotube reinforced aluminum alloy semi-solid slurry
CN112941359A (en) * 2021-01-11 2021-06-11 南昌大学 Preparation method of refined aluminum alloy semi-solid structure
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CN112941359A (en) * 2021-01-11 2021-06-11 南昌大学 Preparation method of refined aluminum alloy semi-solid structure
CN112941360B (en) * 2021-01-11 2022-05-20 南昌大学 Preparation method of carbon nano tube reinforced aluminum alloy semi-solid slurry
CN113088742A (en) * 2021-02-20 2021-07-09 南昌大学 Preparation method of modifier and graphene composite refined magnesium alloy semi-solid structure

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