CN116815006B - Method for preparing in-situ synthesized nano-particle reinforced aluminum matrix composite material by centrifugal reaction - Google Patents
Method for preparing in-situ synthesized nano-particle reinforced aluminum matrix composite material by centrifugal reactionInfo
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- CN116815006B CN116815006B CN202310845498.0A CN202310845498A CN116815006B CN 116815006 B CN116815006 B CN 116815006B CN 202310845498 A CN202310845498 A CN 202310845498A CN 116815006 B CN116815006 B CN 116815006B
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- C22—METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
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- C22C1/00—Making non-ferrous alloys
- C22C1/10—Alloys containing non-metals
- C22C1/1036—Alloys containing non-metals starting from a melt
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- C22—METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
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- C22C21/00—Alloys based on aluminium
- C22C21/02—Alloys based on aluminium with silicon as the next major constituent
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- C—CHEMISTRY; METALLURGY
- C22—METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
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- C22C32/00—Non-ferrous alloys containing at least 5% by weight but less than 50% by weight of oxides, carbides, borides, nitrides, silicides or other metal compounds, e.g. oxynitrides, sulfides, whether added as such or formed in situ
- C22C32/0047—Non-ferrous alloys containing at least 5% by weight but less than 50% by weight of oxides, carbides, borides, nitrides, silicides or other metal compounds, e.g. oxynitrides, sulfides, whether added as such or formed in situ with carbides, nitrides, borides or silicides as the main non-metallic constituents
- C22C32/0073—Non-ferrous alloys containing at least 5% by weight but less than 50% by weight of oxides, carbides, borides, nitrides, silicides or other metal compounds, e.g. oxynitrides, sulfides, whether added as such or formed in situ with carbides, nitrides, borides or silicides as the main non-metallic constituents only borides
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Abstract
本发明涉及铝基复合材料技术领域，尤其涉及离心反应制备纳米颗粒增强铝基复合材料及其制备方法，包括：S1.将第一AlSi12共晶合金坩埚熔化，升温至600±10℃，保温，调整坩埚转速，直至共晶合金液面呈“U”形紧贴于坩埚内壁，得到材料1；S2.向材料1中加入混合盐，待混合盐完全熔化后，坩埚中继续加入第二AlSi12共晶合金，保持坩埚温度不高于650℃，反应10～20min后，缓慢降低转速为0，液面平稳后扒渣，并进行除盐处理，得到材料2；S3.将材料2升温至760～780℃，加入中间金属，控温至700～720℃，加入易烧损元素进行熔体精炼处理，浇注，得到纳米颗粒增强铝基复合材料，解决了传统工艺中反应界面小，反应持续时间长，放热量大等导致反应过程难以控制的问题。
The invention relates to the technical field of aluminum-based composite materials, and in particular to a method for preparing a nano-particle-reinforced aluminum-based composite material by centrifugal reaction, comprising: S1. melting a first AlSi12 eutectic alloy crucible, heating it to 600±10°C, keeping it warm, adjusting the crucible rotation speed, until the eutectic alloy liquid surface is in a "U" shape and closely attached to the inner wall of the crucible, so as to obtain a material 1; S2. adding a mixed salt to the material 1, and after the mixed salt is completely melted, continuously adding a second AlSi12 eutectic alloy to the crucible, keeping the crucible temperature not higher than 650°C, reacting for 10 to 20 minutes, slowly reducing the rotation speed to 0, skimming off the slag after the liquid surface is stable, and performing a desalting treatment, so as to obtain a material 2; S3. heating the material 2 to 760 to 780°C, adding an intermediate metal, controlling the temperature to 700 to 720°C, adding an easily burnt element for melt refining treatment, and casting, so as to obtain a nano-particle-reinforced aluminum-based composite material, which solves the problems in the traditional process of small reaction interface, long reaction duration, large heat release, etc., which lead to the reaction process being difficult to control.
Description
Technical Field
The invention relates to the technical field of aluminum-based composite materials, in particular to a nanoparticle reinforced aluminum-based composite material prepared by centrifugal reaction and a preparation method thereof.
Background
The nanoparticle reinforced aluminum matrix composite material has excellent comprehensive mechanical properties and wide application space in the fields of aerospace, weapons, ships, electronics, automobiles and the like. The fluoride salt method for preparing the nano-particle reinforced aluminum-based composite material has the advantages of simple process, low cost and the like, and is considered as the preparation method of the in-situ synthesized nano-particle reinforced aluminum-based composite material with the most engineering application potential. The fluorite method is to make liquid titanium aluminum react with titanium salt (or zirconium salt) and boron salt in an aluminothermic way to finally form TiB 2 (or ZrB 2) nano particles. On the one hand, the aluminothermic reaction is an exothermic reaction, the reaction process is intense, the reaction products are more and more complicated, the size range is wide, and the control is difficult, and the control is mainly carried out by adopting a method for properly reducing the reaction temperature at present. On the other hand, the contents of Ti element and B element in the titanium salt and the boron salt are low, and the mass fractions thereof are 19.9% and 8.6%, respectively. Even though the yields of Ti and B elements were 100% during the reaction, 7kg of mixed salt was required per 1kg of TiB 2 was synthesized. When preparing 5wt.% TiB 2/Al composite, the weight of the mixed salt is 36.8% of the weight of the alloy, i.e. the molten salt is one third of the volume of the crucible. A large amount of molten salt continuously reacts vigorously on an alloy liquid and molten salt interface by convection, so that the temperature of the melt at the reaction interface is continuously increased, a reaction product is rapidly grown, and in addition, a large amount of residual molten salt enters the melt, so that a plurality of problems of particle agglomeration, difficulty in melt purification and the like are caused. In order to obtain the reinforced particles with high size concentration and good dispersion, technicians at home and abroad generally choose lower reaction temperature and simultaneously implement strong stirring (including electromagnetic stirring and mechanical stirring).
Chinese patent 202011306962.1 discloses a method for preparing an in-situ nanoparticle reinforced aluminum matrix composite material at a low temperature, wherein the reaction temperature is 660-670 ℃, high-speed mechanical stirring is applied to the surface of a melt to form a vortex, and mixed salt is added into the vortex on the surface of the melt to react for 15min. According to the technology, particle agglomeration is restrained by applying rapid mechanical stirring on a reaction interface, the dispersibility and the size of particles are improved, a large amount of air is introduced into a melt when salt is added into a surface vortex, so that a large amount of residual molten salt, oxide and gas exist in the melt, the viscosity of the melt is increased, and difficulty is brought to melt purification treatment. Liu Zhengcai et al (mixed salt method TiB 2 particle reinforced aluminum matrix composite research status [ J ]. Thermal processing technology, 2021,12 (50) pp: 17-21) show that low-speed stirring cannot effectively break clusters, high-speed stirring can increase absorption and oxidation of hydrogen, and surface impurities can be introduced, so that the mechanical properties of the composite are reduced.
Chinese patent 202011571152.9, 202011571153.3 and 202011571141.0 propose a system and a method for preparing an in-situ self-generated aluminum-based composite material by adopting a pulse magnetic field, wherein the reaction temperature is 700-760 ℃, vacuum is pumped at the same time, chinese patent 200510029902.9 discloses a preparation method of an in-situ particle reinforced high-temperature-resistant aluminum-based composite material, the reaction temperature is 680-800 ℃, and after the reaction is completed, alloy elements are added, and vacuum pumping and standing are carried out. In order to avoid the problem that the melt purification is difficult due to the fact that residual molten salt is introduced into the melt from the fluoride salt, the preparation method of the adjustable TiB 2 in-situ reinforced aluminum-based composite material is proposed by China patent 202111585762.9, boron alloy and aluminum-titanium alloy or pure titanium are used as raw materials, the reaction is carried out at 800-850 ℃, and argon refining and degassing are adopted. It can be seen that the prior art does not relate to the residual molten salt purification technology, and does not relate to the technology of increasing the reaction interface through centrifugal force, thereby regulating the reaction rate, particle size and dispersibility.
At present, the prior art adopts a mode of temperature reaction in the aspect of reaction temperature control. The invention discovers that the temperature of the melt rises by about 80-100 ℃ in the reaction process when the melting amount is hundreds of kilograms to the upper ton level. The great rise in melt temperature results in an increase in reaction rate, while the convection or diffusion rate (constant mechanical stirring or an equal power acousto-magnetic coupling field) remains unchanged, which tends to cause the growth or aggregation of the size of the reinforcing particles, ultimately resulting in a large span of the size range of the reinforcing particles and uneven dispersion. In the reaction process, molten salt inevitably enters the interior of the melt to increase the viscosity of the melt, and the disclosed technical scheme generally adopts a traditional mode to carry out melt purification treatment before casting. In practice, alloying causes a further increase in melt viscosity, which results in increased difficulties in melt purging. Further improving the controllable degree of the reaction process, obtaining nano reinforced particles with consistent size and morphology, uniform dispersion and pure melt is a problem which is solved by scientific research technicians in the field.
Disclosure of Invention
Aiming at the defects in the prior art, the invention provides a preparation method of an in-situ synthesized nanoparticle reinforced aluminum matrix composite material which can stably react at an extremely low temperature.
The first aspect of the present invention provides a method for preparing a nanoparticle-reinforced aluminum-based composite material by centrifugation, the method comprising the steps of:
S1, melting a first AlSi12 eutectic alloy crucible, heating to 600+/-10 ℃, preserving heat, adjusting the rotation speed of the crucible until the eutectic alloy liquid surface is in a U shape and is tightly attached to the inner wall of the crucible, and obtaining a material 1;
S2, adding mixed salt into the material 1, continuously adding a second AlSi12 eutectic alloy into a crucible after the mixed salt is completely melted, keeping the temperature of the crucible not higher than 650 ℃, slowly reducing the rotating speed to 0 after reacting for 10-20 min, removing slag after the liquid level is stable, and carrying out desalting treatment to obtain a material 2;
And S3, heating the material 2 to 760-780 ℃, adding intermediate metal, controlling the temperature to 700-720 ℃, adding an element easy to burn, carrying out melt refining treatment, and casting to obtain the nanoparticle reinforced aluminum matrix composite.
In some embodiments, the crucible rotation speed is adjusted to 3000-4000r/min as described in S1.
The applicant found during the exploration that too low a rotation speed of the crucible, insufficient level dishing, or difficulty in forming a "U" shaped level, is detrimental to establishing a sufficient reaction interface, resulting in a low reaction efficiency. Too high a rotational speed results in agglomeration of the high density reinforcing particles under the influence of centrifugal force against the crucible sidewall and increases energy consumption and equipment manufacturing costs. The definition of the U-shaped is that the liquid level of the crucible which is tightly attached to the inner wall of the crucible is higher than the liquid level of the bottom of the crucible in the rotating process of the crucible, and the U-shaped can be considered to be formed.
Further, the vertical distance from the highest point to the lowest point of the U-shaped liquid level is 2/3-3/4 of the height of the crucible.
In some embodiments, the mixed salt is a mixture of baked potassium fluorotitanate and potassium fluoroborate.
Further, the molar ratio of Ti atoms to B atoms in the potassium fluotitanate to the potassium fluoborate is 1:2.
In some embodiments, the second AlSi12 eutectic alloy is added in an amount of 5-10wt% of the mixed salt.
The addition amount of the second AlSi12 eutectic alloy is too low to achieve the expected cooling effect, and the addition amount is too high, so that the temperature of the melt is lower than the liquidus line, and the dispersion of micro-nano reinforced particles in the melt is not facilitated.
The addition sequence of the second AlSi12 eutectic alloy plays a key role, the melting speed of AlSi12 added into the melt is far higher than that of the mixed salt, the melt temperature is firstly rapidly reduced before the mixed salt is added or is added together with the mixed salt, and then the melt temperature is rapidly increased under the influence of reaction heat, so that the effect of controlling the melt temperature to be greatly increased in the reaction process is not achieved, and the purpose of enhancing the particle size regulation cannot be realized.
In some embodiments, the second AlSi12 eutectic alloys each have a profile dimension of less than 30 x 30mm.
The second AlSi12 eutectic alloy has overlarge outline size, which can cause large local temperature drop, and long time for reaching the equilibrium temperature through heat conduction, which is unfavorable for realizing the control of the temperature uniformity of the melt. While too small a profile will introduce a significant amount of oxide film into the melt.
In some embodiments, the temperature of the desalting treatment is controlled to be 600-630 ℃, the pressure is not more than 500Pa, and the time is 15-30 min.
In some embodiments, the melt refining treatment specifically comprises the step of carrying out melt refining treatment by adopting an argon rotary blowing method, wherein the rotating speed is 300-600 r/min, the argon pressure is 1-2 MPa, and the refining time is 15-25 min.
Further, the intermediate metal may be selected from the types commonly used in the art, including but not limited to pure aluminum ingots.
Further, the burnable elements may be selected from the species commonly used in the art, including but not limited to pure magnesium.
The reaction temperature in the prior art is generally 750-900 ℃, and the minimum temperature in the report is 660-670 ℃. The invention starts from adding mixed salt (600+/-10 ℃) until the reaction is finished and the slag skimming operation is finished, and the temperature of the melt in the reaction process is obviously lower than that in the prior art. Applicants have found that the reaction temperature has the most pronounced effect on the size of the reinforcing particles, the higher the reaction temperature the larger the size of the reinforcing particles produced. When the reaction temperature is greater than 1000 ℃, a large amount of reinforcing particles with the size of micrometers are generated. When the reaction temperature is 700-900 ℃, the generated reinforced particle size distribution range is wide, and nano-scale particles and micro-scale particles exist at the same time. The reaction temperature is lower than 650 ℃, and the generated reinforced particles are almost all in nanometer scale. The higher reaction temperature is adopted, so that the subsequent melt purification treatment is facilitated, and the residual salt or alkali metal in the melt volatilizes under the high-temperature effect, so that the difficulty of the subsequent purification is reduced. At low reaction temperature, residual salt or alkali metal in the melt is difficult to volatilize, and the subsequent melt purification treatment is difficult. The invention adopts vacuum desalting treatment after the reaction is finished, and the volatilization of residual salt or alkali metal in the melt is promoted and accelerated by establishing vacuum above the liquid level, so that the difficulty of subsequent melt purification is reduced, and the problem of high melt purification difficulty caused by low-temperature reaction is solved.
In some embodiments, the size of the nanoparticles in the nanoparticle-reinforced aluminum matrix composite is 80-90 nm.
In some embodiments, the nanoparticle-reinforced aluminum-based composite has an elongation of no less than 6%.
In the present invention, the relationship between the centrifugal force to which the nanoparticle is subjected and its own volume and rotational speed is as follows:
wherein F is the centrifugal force to which the nano-particles are subjected, ρ is the density of the nano-particles, V is the volume of the nano-particles, V is the linear velocity of the nano-particles, and r is the distance from the nano-particles to the rotation center.
The density of the reaction product TiB 2 (or ZrB 2) particles is greater than that of the aluminum melt, and the reaction product TiB 2 rapidly breaks away from the reaction interface under the action of centrifugal force, so that the subsequent growth is inhibited. The rotating speed of the crucible is adjusted, the centrifugal force applied to the nano particles is changed, the volume of the nano particles separated from the reaction interface is controlled, and the size of the nano particles is regulated and controlled. At the same time, centrifugal forces help to improve the dispersibility of the nanoparticles.
According to the invention, vacuum desalting treatment is carried out after the reaction is finished, and free K +、H+、F- ions in the melt can be quickly separated from the melt, so that the purpose of removing residual molten salt in the melt is achieved, and the effects of degassing and deslagging are achieved. Residual molten salt is removed firstly, and then the melt is heated for alloying, so that the melt purification difficulty can be reduced, and the problem that reinforcing particles continue to grow up due to further reaction of the residual molten salt after the temperature is raised is avoided, thereby being beneficial to obtaining nano reinforcing particles with uniform and fine size and pure alloy melt.
The second aspect of the invention provides a nanoparticle reinforced aluminum matrix composite material obtained by the preparation method.
Compared with the prior art, the invention has the following beneficial effects:
According to the invention, the motor arranged at the bottom of the crucible drives the crucible to rotate to generate centrifugal force, the alloy liquid clings to the wall of the crucible under the action of the centrifugal force to form a U-shaped liquid level, the mixed salt spreads on the U-shaped liquid level after being melted, the contact area of the alloy liquid and molten salt is obviously increased, the reaction efficiency is improved, the diffusion of reaction products is facilitated, and the dispersibility of particles is improved. In addition, the large reaction interface increases the heat dissipation area, is favorable for heat conduction released by the reaction, and further improves the stability of the reaction process. Solves the problem that the reaction process is difficult to control due to small reaction interface, long reaction duration, large heat release amount and the like in the traditional process.
Drawings
FIG. 1 is a schematic diagram of an apparatus for preparing a nanoparticle-reinforced aluminum matrix composite of the present invention, wherein the apparatus comprises a 1-crucible, a 2-alloy melt, a 3-molten salt, and a 4-motor drive keyway.
Fig. 2 is a particle size, morphology and distribution diagram of TiB 2 (10 wt.%)/ZL 101A composites prepared in example 1.
Fig. 3 is a particle size, morphology and distribution diagram of TiB 2 (10 wt.%)/ZL 114A composites prepared in example 2.
Fig. 4 is a particle size, morphology and distribution diagram of TiB 2 (10 wt.%)/ZL 101A composites prepared in comparative example 1.
Fig. 5 is a particle size, morphology and distribution diagram of TiB 2 (10 wt.%)/ZL 114A composite prepared in comparative example 2.
Detailed Description
The following description of the technical solutions in the embodiments of the present invention will be clear and complete, and it is obvious that the described embodiments are only some embodiments of the present invention, but not all embodiments. All other embodiments, which can be made by those skilled in the art based on the embodiments of the invention without making any inventive effort, are intended to be within the scope of the invention.
Example 1
The present example provides a method of preparing a TiB 2 (10 wt.%)/ZL 101A composite material, the method comprising the steps of:
s1, adding a first AlSi12 eutectic alloy (51.3 kg) into a crucible for melting, heating to 600+/-10 ℃, preserving heat, adjusting the rotation speed of the crucible to 4000r/min until the eutectic alloy liquid surface is in a U shape and is tightly attached to the inner wall of the crucible, and obtaining a material 1, wherein the vertical distance from the highest point to the lowest point of the U-shaped liquid surface is 2/3 of the height of the crucible;
S2, adding 70.8kg of mixed salt (potassium fluotitanate and potassium fluoborate, wherein the molar ratio of Ti to B is 1:2) into the material 1, continuously adding 7kg of second AlSi12 eutectic alloy (the outline size is less than 30 multiplied by 30mm, the addition amount is 10% of the weight of the mixed salt) into a crucible after the mixed salt is completely melted, keeping the temperature of the crucible not higher than 650 ℃, slowly reducing the rotating speed to 0 after 15min of reaction, slagging off after the liquid level is stable, controlling the temperature to 620-650 ℃, controlling the pressure not higher than 500Pa, and carrying out desalting treatment for 20min to obtain a material 2;
s3, heating the material 2 to 770 ℃, adding 32kg of pure aluminum ingot and 2.5kg of AlTi4 intermediate metal, controlling the temperature to 710 ℃, adding 0.7kg of easily burnt element pure magnesium, carrying out melt refining treatment by adopting an argon rotary blowing method, carrying out melt refining treatment at the rotating speed of 500r/min and the argon pressure of 1MPa for 20min, and casting to obtain the nanoparticle reinforced aluminum matrix composite material.
As shown in fig. 2, the particle size of TiB 2 (10 wt.%)/TiB 2 of the ZL101A aluminum matrix composite material prepared in this example is concentrated at 80-90 nm, and after T6 heat treatment, the tensile strength is 398MPa, the yield strength is 354MPa, and the elongation is 8% by using the test method of GB/T228.1-2010.
Example 2
The present example provides a method of preparing a TiB 2 (10 wt.%)/ZL 114A composite material, the method comprising the steps of:
S1, adding a first AlSi12 eutectic alloy (52.6 kg) into a crucible for melting, heating to 600+/-10 ℃, preserving heat, adjusting the rotation speed of the crucible to 3000r/min until the eutectic alloy liquid surface is in a U shape and is tightly attached to the inner wall of the crucible, and obtaining a material 1, wherein the vertical distance from the highest point to the lowest point of the U-shaped liquid surface is 3/4 of the height of the crucible;
S2, adding 70.8kg of mixed salt into the material 1, wherein the atomic ratio of Ti to B is 1:2, continuously adding 5.7kg of a second AlSi12 eutectic alloy (the outline size is smaller than 30 multiplied by 30mm, the addition amount is 8% of the weight of the mixed salt) into a crucible after the mixed salt is completely melted, keeping the temperature of the crucible not higher than 650 ℃, slowly reducing the rotating speed to 0 after the reaction is carried out for 30min, slagging off after the liquid level is stable, controlling the temperature to 620-650 ℃, controlling the pressure not higher than 500Pa, and carrying out desalination treatment for 20min to obtain the material 2;
S3, heating the material 2 to 770 ℃, adding 35kg of pure Al ingot and 2.5kg of AlTi4 intermediate metal, controlling the temperature to 710 ℃, adding 0.9kg of easily burnt element pure magnesium, carrying out melt refining treatment by adopting an argon rotary blowing method, carrying out melt refining treatment at the rotating speed of 600r/min and the argon pressure of 2MPa for 25min, and casting to obtain the nanoparticle reinforced aluminum matrix composite material.
As shown in fig. 3, the particle size of TiB 2 (10 wt.%)/TiB 2 of the ZL114A aluminum matrix composite material prepared in this example is concentrated at 80-90 nm, and after T6 heat treatment, the tensile strength is 428MPa, the yield strength is 363MPa, and the elongation is 6% by using the test method of GB/T228.1-2010.
Comparative example 1
The comparative example provides a preparation method of TiB 2 (10 wt.%)/ZL 101A composite material, and the specific embodiment is the same as example 1, except that in the step S1, a first AlSi12 eutectic alloy crucible is melted, heated to 600+ -10 ℃, and heat-preserved to obtain a material 1.
As shown in fig. 4, the particle size of TiB 2 of the prepared TiB 2 (10 wt.%)/ZL 101A aluminum matrix composite was concentrated at 80-90 nm. After T6 heat treatment, the tensile strength is 334MPa, the yield strength is 195MPa, and the elongation is 1.5%.
Comparative example 2
This comparative example provides a method for preparing TiB 2 (10 wt.%)/ZL 114A composite, the specific embodiment is the same as example 2, except that no second AlSi12 eutectic alloy is added in step S2.
As shown in fig. 5, the TiB 2 (10 wt.%)/TiB 2 particle size of the ZL114A aluminum-based composite material prepared was concentrated at 300nm, and the agglomeration tendency was severe. After T6 heat treatment, the tensile strength is 355MPa, the yield strength is 280MPa, and the elongation is 3.5%.
While the foregoing is directed to the preferred embodiments of the present invention, it will be appreciated by those skilled in the art that various modifications and adaptations can be made without departing from the principles of the present invention, and such modifications and adaptations are intended to be comprehended within the scope of the present invention.
Claims (5)
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