CN109252060A - A kind of preparation method of crystal-amorphous aluminum matrix composite - Google Patents
A kind of preparation method of crystal-amorphous aluminum matrix composite Download PDFInfo
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- CN109252060A CN109252060A CN201811157292.4A CN201811157292A CN109252060A CN 109252060 A CN109252060 A CN 109252060A CN 201811157292 A CN201811157292 A CN 201811157292A CN 109252060 A CN109252060 A CN 109252060A
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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
- C22C1/02—Making non-ferrous alloys by melting
- C22C1/026—Alloys based on aluminium
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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
- C22C1/11—Making amorphous alloys
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- 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
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- C—CHEMISTRY; METALLURGY
- C22—METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
- C22C—ALLOYS
- C22C45/00—Amorphous alloys
- C22C45/08—Amorphous alloys with aluminium as the major constituent
Abstract
The present invention provides a kind of preparation method of crystal-amorphous aluminum matrix composite, the following steps are included: (1) 86:6.75:2.25:3.25:1.75 weighs Al, Ni, Co, Y and La high pure metal simple substance respectively in molar ratio, mass fraction >=99.99wt.% of each metal simple-substance, mixing, melting；Alloy mother's ingot Al is prepared after melting several times86Ni6.75Co2.25Y3.25La1.75；(2) by alloy mother ingot after arc-melting under argon atmosphere, water cooled copper mould is used as cooling medium quickly carry out copper mold and prepare the crystal-amorphous aluminum matrix composite；The suction casting process and the cooling velocity of copper mold mold cooperation are 103K/s~106K/s, and the cooling rate of copper mold mould upstream is lower than the cooling rate of lower part.The composite material of controllable material property by the method for the invention, preparation has excellent mechanical property, and compressive strength at room temperature is between 625~865MPa, and for breaking strength in 650~1000MPa, compression plastic strain is 1.3~3.3%.
Description
Technical field
The present invention relates to cast aluminium alloy gold preparation field, specifically a kind of crystal-amorphous aluminum matrix composite preparation side
Method.
Background technique
Aluminium alloy is as a kind of lightweight structural material with high specific strength, and shared specific gravity is got in development of modern industry
Come higher, is especially increasingly becoming one of the basic material instead of steel in automobile and aerospace field.With the field skill
The continuous development of art, the requirement to structural material especially high strength high toughness casting aluminum alloy is also higher and higher, how to improve casting
The mechanical property of Aluminium alloy structural material becomes important one of research topic.So far, people develop various methods
The mechanical property of cast aluminium alloy gold is improved, wherein being important one of method to prepare Al alloy composite.Preparation
The method of aluminium alloy based composites have electro-deposition method, XD method, large plastometric set method, mechanical alloying method,
Sputtering method, sol-gel method, electromagnetism and mechanical stirring complex technique, blow and spray sedimentation, fast solidification technology at casting technique
Deng.In recent years, people are handled by fast solidification technology can successfully prepare al based amorphous alloy, to effectively improve aluminium base
The integral strength of composite material.
Domestic and foreign scholars have attempted directly to prepare various high-performance blocks using flash set technology in the past few decades
Body nanometer phase reinforced aluminum matrix composites.Compared with conventional cast aluminium alloy, the tensile strength of al based amorphous alloy can be
900MPa or more.But for al based amorphous alloy, although its tensile strength is significantly larger than conventional cast aluminium alloy,
Its temperature-room type plasticity is very poor.
Summary of the invention
It is an object of the invention to solve above-mentioned problems of the prior art, a kind of crystal-of high-strength and high ductility is provided
The preparation method of amorphous aluminum matrix composite.
For achieving the above object, the technical scheme adopted by the invention is that:
A kind of preparation method of crystal-amorphous aluminum matrix composite, comprising the following steps:
(1) 86:6.75:2.25:3.25:1.75 weighs Al, Ni, Co, Y and La high pure metal simple substance respectively in molar ratio,
Mass fraction >=99.99wt.% of each metal simple-substance, mixing, melting；Alloy mother's ingot is prepared after multiple melting
Al86Ni6.75Co2.25Y3.25La1.75；
(2) use water cooled copper mould as cooling medium after arc-melting under argon atmosphere on the alloy mother ingot
It quickly inhales casting and the crystal-amorphous aluminum matrix composite is prepared；The cooling velocity of the suction casting process and the cooperation of copper mold mold
It is 103K/s~106K/s, and the cooling rate of the copper mold mould upstream is lower than the cooling rate of lower part.
Preferably, in the step (1), surface is carried out to high-purity Al, Ni, Co, Y and La metal simple-substance respectively and is beaten
Mill is with scale removal and attachment impurity；The number of the melting is 3~5 times.
Preferably, in the step (1), in the ethyl alcohol-the third that volume ratio is 4:1 after all kinds of elemental metals are mixed
Ultrasonic cleaning carries out melting after then ultrasound is dry to remove attachment impurity in ketone mixed solution.
Preferably, in the step (1), melting, the fusing electricity of each melting are carried out using high vacuum arc-melting furnace
Stream, melting voltage and fusing time control are in 220~350A, 250V, 60 ± 5s.
Preferably, in the step (2), using high vacuum melting-suction casting furnace to the alloy mother ingot carry out melting and
Inhale casting.
Preferably, in the step (2), before inhaling casting, control absolute vacuum degree is 8.0 × 10-4~2.5 × 10-
3Pa, the argon gas that then reversely charging purity is 99.999% to 0.5 ± 0.05 atmospheric pressure.
Preferably, it in the step (2), is inhaled and is cast using high vacuum arc-melting furnace, inhaled melting fusion current when casting, melt
Change voltage and fusing time control in 250~320A, 250V, 9 ± 2s.
Preferably, in the step (2), it is highly 120 millimeters that the outer diameter of the copper mold mold, which is 50 millimeters, inner core
Diameter is 1.5 millimeters.
Preferably, before melting, control absolute vacuum degree is 8.0 × 10-4~2.5 × 10-3Pa, and then reversely charging purity is
99.999% argon gas is to 0.5 ± 0.05 atmospheric pressure.
Preferably, it before carrying out melting and inhaling casting, is taken out in advance by mechanical pump, mechanical pump-molecular pump mixing pumping is to reach
To the vacuum ranges of requirement.
The beneficial effects of the present invention are:
(1) suction casting process of the invention and the cooling velocity of copper mould cooperation can reach 103K/s~106K/s, and tradition is cold
But method, if the rate of Slow cooling in crucible is 0.08K/s, the rate of natural cooling is 6.5K/s, water cooled copper mould in air
Cooling rate is 102K/s can be realized quick solidification, and due to the difference of mold top and the bottom cooling velocity, so that alloy
The content different from of middle amorphous and α (Al), so that different mechanical properties is presented, by the sample for choosing different location
Achieve the effect that regulation；
(2) preparation method provided by the invention prepares crystal-amorphous aluminum matrix composite by flash set technology, described
The microstructure of composite material mainly has intermetallic compound, fcc toughness dendrite and a small amount of amorphous phase, wherein having compared with multiple slip
The face-centred cubic structure α (Al) of system can be improved the plasticity of the composite material, and intermetallic compound and amorphous phase can mention
The intensity of the high composite material, interaction in fcc toughness dendrite and amorphous phase, intermetallic compound deformation process so that
The composite material have excellent mechanical property, compared with traditional aluminium alloy, compression yield strength 625~865MPa it
Between, breaking strength is reached for 1.3~3.3% in 650~1000MPa, room temperature compression plastic strain；
(3) method of the invention uses water cooled copper mould, and metal contacts closely with type wall in shape, and metal freezing speed is exceedingly fast,
It is not likely to produce gravity segregation, while cooling velocity is exceedingly fast, it is easier to form amorphous material
(4) method of the invention is cast in vacuum condition, and oxidation possibility is minimum；
(5) liquid metal is drawn into copper mold by method of the invention using the pressure difference in furnace body between copper mould,
Carried out under the ar gas environment of 0.5MPa due to inhaling casting, therefore inhaling gas density in casting furnace is about 0.69 times in air, at
Air resistance is smaller in relative atmospheric when type, it is often more important that mechanical pump further decreases the air-extraction function of type chamber when inhaling casting
Type intracavitary air resistance.Therefore, when inhaling casting, metal is can be improved in the intracavitary air resistance very little encountered of type in molten metal
The Packing character of liquid；
(6) outer diameter for the copper mold mold that method of the invention uses is highly 120 millimeters, inner core diameter is for 50 millimeters
1.5 millimeters, the specification of copper mold will affect the cooling velocity in process of setting, in the case where inner core diameter remains unchanged, use
The content of amorphous that smaller size copper mold prepares in crystal-amorphous aluminum matrix composite can increase, and crystalline content can drop
It is low.
Detailed description of the invention
Fig. 1 .Al86Ni6.75Co2.25Y3.25La1.75The XRD diffraction pattern of composite material.
Fig. 2 .Al86Ni6.75Co2.25Y3.25La1.75The metallographic microscope of composite material.
Fig. 3 .Al86Ni6.75Co2.25Y3.25La1.75The room temperature compressive stress strain curve figure of composite material.
Fig. 4 .Al86Ni6.75Co2.25Y3.25La1.75The deformed shape appearance figure of composite material.
Specific embodiment
To make the object, technical solutions and advantages of the present invention clearer, the technical solution below in the present invention carries out clear
Chu is fully described by, it is clear that described embodiments are some of the embodiments of the present invention, instead of all the embodiments.It is based on
Embodiment in the present invention, it is obtained by those of ordinary skill in the art without making creative efforts every other
Embodiment shall fall within the protection scope of the present invention.
A kind of preparation method of crystal-amorphous aluminum matrix composite, comprising the following steps:
(1) 86:6.75:2.25:3.25:1.75 weighs Al, Ni, Co, Y and La high pure metal simple substance respectively in molar ratio,
Mass fraction >=99.99wt.% of each metal simple-substance, mixing, melting；Alloy mother's ingot is prepared after multiple melting
Al86Ni6.75Co2.25Y3.25La1.75；
(2) by alloy mother ingot after arc-melting under argon atmosphere, use water cooled copper mould quick as cooling medium
It inhales casting and crystal-amorphous aluminum matrix composite is prepared；The suction casting process and the cooling velocity of copper mold mold cooperation are 103K/s
~106K/s, and the cooling rate of copper mold mould upstream is lower than the cooling rate of lower part.
Liquid metal is drawn into copper mold by the present invention using the pressure difference in furnace body between copper mould, utilizes recirculated water
The cooling and good thermal diffusivity of copper, which reaches, makes liquid metal be quickly cooled down solidification.Melting liquid alloy temperature is high, and (temperature range exists
650 degrees Celsius -2500 degrees Celsius), select metal resistant to high temperature as material, and the metal wants good heat conductivity, fine copper is led
Hot good, affordable can be widely applied.In addition, metal contacts closely with type wall in shape, metal freezing using water cooled copper mould
Speed is exceedingly fast, and is not likely to produce gravity segregation, while cooling velocity is exceedingly fast, it is easier to form amorphous material.
Further, in step (1), surface polishing is carried out to go to high-purity Al, Ni, Co, Y and La metal simple-substance respectively
It descales and adheres to impurity；The number of melting is 3~5 times.
Further, it in step (1), is mixed after all kinds of elemental metals are mixed in the ethanol-acetone that volume ratio is 4:1
Ultrasonic cleaning carries out melting after then ultrasound is dry to remove attachment impurity in solution.
Further, in step (1), using high vacuum arc-melting furnace carry out melting, the fusion current of each melting,
Melting voltage and fusing time control are in 220~350A, 250V, 60 ± 5s.
Further, in step (2), alloy mother's ingot is carried out melting and inhaled to cast using high vacuum melting-suction casting furnace.
Further, in step (2), before inhaling casting, control absolute vacuum degree is 8.0 × 10-4~2.5 × 10-3Pa,
Then the argon gas that reversely charging purity is 99.999% is to 0.5 ± 0.05 atmospheric pressure.Due to inhaling casting under the ar gas environment of 0.5MPa
It carrying out, standard atmospheric pressure 1MPa, the molal weight of air is about 29g/mol, and the molal weight of argon gas is about 40g/mol,
According to extension pM=ρ RT (wherein p-gas pressure intensity, M-substance molal weight, the ρ-gaseous material of Clapyron Equation
Density.R-gas constant, T-absolute temperature), therefore (including type chamber), gas density is about 0.69 in air in suction casting furnace
Times, air resistance is smaller in relative atmospheric at the time of molding, it is often more important that inhale casting when mechanical pump for type chamber air-extraction function into
One step reduces the intracavitary air resistance of type.Therefore, when inhaling casting, molten metal, can in the intracavitary air resistance very little encountered of type
The Packing character of molten metal is improved, the minimum wall thickness (MINI W.) of made casting is up to 1mm.
Further, it in step (2), is inhaled and is cast using high vacuum arc-melting furnace, melting fusion current, fusing when inhaling casting
Voltage and fusing time control are in 250~320A, 250V, 9 ± 2s.
Further, in step (2), it is highly 120 millimeters, inner core diameter is that the outer diameter of copper mold mold, which is 50 millimeters,
1.5 millimeter.The specification of copper mold will affect the cooling velocity in process of setting, in the case where inner core diameter remains unchanged, use
The content of amorphous that smaller size copper mold prepares in crystal-amorphous aluminum matrix composite can increase, and crystalline content can drop
It is low.
Further, before melting, control absolute vacuum degree is 8.0 × 10-4~2.5 × 10-3Pa, then reversely charging purity
For 99.999% argon gas to 0.5 ± 0.05 atmospheric pressure.
Further, before carrying out melting and inhaling casting, is taken out in advance by mechanical pump, mechanical pump-molecular pump mixing be evacuated with
Reach the vacuum ranges of requirement.
Method of the invention is designed for aluminium base crystal-amorphous composite material, the ingredient is selected, due to cooling velocity
It can reach 103K/s~106K/s, and the difference of mold top and the bottom cooling velocity so that in alloy amorphous and α (Al) content
Different from, to present different mechanical properties, the sample by choosing different location achievees the effect that regulation.
Al, Ni, Co, Y and La simple substance described in following embodiment are purchased from the good minoplatin industry non-ferrous metal Co., Ltd in Beijing, pure
Degree is 99.99wt.%.
Embodiment 1
A kind of preparation method of crystal-amorphous aluminum matrix composite, comprising the following steps:
(1) Al, Ni, Co, Y and La metal simple-substance are subjected to fine polishing scale removal and attachment impurity, massage respectively
You weigh Al, Ni, Co, Y and La simple substance (weighing error is controlled in ± 0.001g) than 86:6.75:2.25:3.25:1.75 respectively,
30g metal simple-substance mixture is prepared after mixing, it is clear that the metal simple-substance mixture is placed in ultrasound in ethanol-acetone mixed solution
10min is washed to remove attachment impurity, is put into after drying in high vacuum arc-melting furnace, alloy is prepared after melt back 5 times
Female ingot Al86Ni6.75Co2.25Y3.25La1.75, during vacuum arc melting, absolute vacuum degree is 8.0 × 10-4~2.5 × 10-3Within the scope of Pa, the argon gas that then reversely charging purity is 99.999% is to 0.5 ± 0.05 atmospheric pressure；
(2) the alloy mother's ingot prepared is cut into small pieces by cutting machine, 5 ± 0.2g or so is taken to be placed on high vacuum melting-
It inhales melting suction casting in casting furnace and the rod-like samples that diameter is 1.5mm, length is 90 ± 2mm is made, during vacuum arc is inhaled and is cast,
Absolute vacuum degree is 8.0 × 10-4~2.5 × 10-3Within the scope of Pa, the argon gas that then reversely charging purity is 99.999% to 0.5 ±
0.05 atmospheric pressure.
In step (1), since the fusing point of different metal simple substance is different, component distributing is likely to result in fusion process
Non-uniform phenomenon, to ensure that its ingredient is uniformly mixed, melting 3~5, number will lead to alloy mother's ingot too much for melt back
Scaling loss is excessive, and it is uneven then to will lead to alloy mother's ingot very little.
In step (1) and (2), the purpose for the argon gas that recoils is: playing prevents from aoxidizing, while being subsequent electric arc melting process
Starting the arc medium is provided.
In step (1), the fusion current range of melting is big, and smelting time is long, and fusion current is high, in order to allow
The metal simple-substance of different melting points melts completely while is sufficiently mixed alloying element uniformly.In step (2), melting is molten when inhaling casting
Galvanic current range is small, as long as the short purpose of fusing time is to melt the uniform alloy pig of the ingredient of melting before completely to carry out
Inhale casting.
Test case 1
X-ray diffraction analysis
The bar that will be inhaled the rod-like samples prepared of casting with cutting machine and be cut into 3mm long is ground bar by mold half-sectional
Face carries out X-ray diffraction analysis after being cleaned by ultrasonic in ethanol-acetone mixing, the angle of diffraction (2 θ) range is 20 °~80 °, is used to
The phase composition in Bar samples is measured, as a result as shown in Figure 1, as seen from Figure 1 including face-centered cubic in the composite material
α (Al) solid solution of structure and a large amount of intermetallic compound exist, and are Al respectively4NiY、AlCo、Al4La。
Test case 2
Metallographic microstructure analysis
Metallographic microanalysis is carried out after the bar prepared in test case 1 progress metallographic is inlayed, polished, is formed with obtaining it
The pattern of phase determines pattern, distribution and the grain size of crystal phase and amorphous phase, as a result as shown in Fig. 2, as seen from Figure 2
It is that α (Al) solid solution of face-centred cubic structure and a large amount of intermetallic compound exist inside bar, is non-in bar edge
Crystal phase.
Test case 3
Mechanics Performance Testing
Rod-like samples made of suction casting are cut into the sample of diameter 1.5mm, length 3.5mm by precision gas cutting machine, so
It is polished afterwards by polishing clamp parallel for both ends, end face and axially vertical diameter are that 1.5mm, 3 ± 0.2mm of length are vertical
Standard compression sample, universal testing machine is newly thought carefully by MTS, 2.5 × 10-4s-1Compression strain rate under compressed
Performance test, as a result as shown in figure 3, as seen from the figure, the rod-like samples for inhaling the diameter 1.5mm of casting preparation can table in compression process
Reveal different mechanical properties: high breaking strength sample (high-intensitive sample in Fig. 3) and high-ductility sample further confirm this hair
Bright method is to the adjustable effect of mechanical property, and it is cold due to inhaling cast copper mould or more for generating the reason of this mechanical property changes
But rate is different so that bar top and the bottom structure also different from.Mold upper end is due to the copper crucible close to molten alloy
And upper end enters the entrance of molding die as melting liquid, so its cooling rate will be lower than lower end, and the formation of amorphous needs
Very high cooling velocity is wanted, thus it is more in the amorphous that mold lower end is formed, therefore the sample integral strength in lower end is also wanted
It is higher, and the α (Al) of the preferable face-centred cubic structure of plasticity is some more in the sample of upper end, the Plastic phase shown
It is more preferable to lower end, but intensity due to the content of amorphous reduction and slightly decline.As shown in figure 3, the compression yield of sample is strong
Degree is between 625~865MPa, and for breaking strength in 650~1000MPa, room temperature compression plastic strain can between 1.3~3.3%
It adjusts.
Test case 4
Sem analysis
It is analyzed by pattern of the SEM to the sample surfaces after compressive deformation in test case 3 to determine its texturing machine
System, as shown in figure 4, alloy produces the big slight crack (a) through sample after compression verification, it can be seen that fracture covering weave has
It is apparent different, two regions: non-crystalline areas and crystal region can be divided into, wherein being typical non-close to the region of Surface of Rod Bar
Brilliant brittle fracture pattern (b), this also further demonstrates alloy, and there are the suppositions of amorphous, and the section at bar center is in
Reveal the dimple feature (c, white circle) with plastic deformation feature, while there is the cleavage fracture of a small amount of brittle deformation feature
Mode.Finally, it should be noted that the above embodiments are merely illustrative of the technical solutions of the present invention, rather than its limitations；Although ginseng
According to previous embodiment, invention is explained in detail, those skilled in the art should understand that: it still can be with
It modifies the technical solutions described in the foregoing embodiments or equivalent replacement of some of the technical features；And
These are modified or replaceed, the spirit and model of technical solution of various embodiments of the present invention that it does not separate the essence of the corresponding technical solution
It encloses.
Claims (10)
1. a kind of crystal-amorphous aluminum matrix composite preparation method, which comprises the following steps:
(1) 86:6.75:2.25:3.25:1.75 weighs Al, Ni, Co, Y and La high pure metal simple substance, each gold respectively in molar ratio
Belong to mass fraction >=99.99wt.% of simple substance, mixing, melting；Alloy mother's ingot is prepared after multiple melting
Al86Ni6.75Co2.25Y3.25La1.75；
(2) use water cooled copper mould quick as cooling medium after arc-melting under argon atmosphere on the alloy mother ingot
It inhales casting and the crystal-amorphous aluminum matrix composite is prepared；The cooling velocity that the suction casting process cooperates with copper mold mold is
103K/s~106K/s, and the cooling rate of the copper mold mould upstream is lower than the cooling rate of lower part.
2. crystal according to claim 1-amorphous aluminum matrix composite preparation method, which is characterized in that in the step
Suddenly in (1), it is miscellaneous with scale removal and attachment that surface polishing is carried out to high-purity Al, Ni, Co, Y and La metal simple-substance respectively
Matter；The number of the melting is 3~5 times.
3. crystal according to claim 1-amorphous aluminum matrix composite preparation method, which is characterized in that in the step
Suddenly in (1), will all kinds of elemental metals mix after in the ethanol-acetone mixed solution that volume ratio is 4:1 ultrasonic cleaning with
Removal attachment impurity, carries out melting after then ultrasound is dry.
4. crystal according to claim 1-amorphous aluminum matrix composite preparation method, which is characterized in that in the step
Suddenly in (1), melting, fusion current, melting voltage and the fusing time control of each melting are carried out using high vacuum arc-melting furnace
System is in 220~350A, 250V, 60 ± 5s.
5. crystal described in any one of-4-amorphous aluminum matrix composite preparation method, feature exist according to claim 1
In in the step (2), using high vacuum melting-, suction casting furnace carries out melting to the alloy mother ingot and suction is cast.
6. crystal according to claim 1-amorphous aluminum matrix composite preparation method, which is characterized in that in the step
Suddenly in (2), before inhaling casting, control absolute vacuum degree is 8.0 × 10-4~2.5 × 10-3Pa, then reversely charging purity is 99.999%
Argon gas to 0.5 ± 0.05 atmospheric pressure.
7. crystal according to claim 1-amorphous aluminum matrix composite preparation method, which is characterized in that in the step
Suddenly it in (2), is inhaled and is cast using high vacuum arc-melting furnace, melting fusion current, melting voltage and fusing time control exist when inhaling casting
250~320A, 250V, 9 ± 2s.
8. crystal according to claim 1-amorphous aluminum matrix composite preparation method, which is characterized in that in the step
Suddenly in (2), it is highly 120 millimeters that the outer diameter of the copper mold mold, which is 50 millimeters, and inner core diameter is 1.5 millimeters.
9. the crystal according to any one of claim 6-8-amorphous aluminum matrix composite preparation method, feature exist
In before melting, control absolute vacuum degree is 8.0 × 10-4~2.5 × 10-3Pa, the argon that then reversely charging purity is 99.999%
Gas is to 0.5 ± 0.05 atmospheric pressure.
10. crystal according to claim 9-amorphous aluminum matrix composite preparation method, which is characterized in that melted
It before refining and suction casting, is taken out in advance by mechanical pump, mechanical pump-molecular pump mixes pumping to reach the vacuum ranges of requirement.
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| CN114507827A (en) * | 2021-06-30 | 2022-05-17 | 季华实验室 | Preparation method of aluminum-based amorphous composite material and aluminum-based amorphous composite material |
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