CN116815005B - A method for preparing nanoparticle-reinforced aluminum matrix composites by low-temperature in-situ synthesis - Google Patents
A method for preparing nanoparticle-reinforced aluminum matrix composites by low-temperature in-situ synthesisInfo
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Abstract
本发明公开了一种低温原位合成纳米颗粒增强铝基复合材料制备方法，具备以下特点：(1)采用本发明的计算方法，合理选择合金初始熔化量和坩埚尺寸，控制反应过程熔盐层的深度不大于3cm；(2)以Al‑Si共晶合金为基础熔体，在600℃加入混合盐，整个反应过程熔体温度不大于650℃；(3)反应完成后依次进行真空净化处理、升温添加合金元素。本发明采用合理的坩埚直径和极低的反应温度，有效降低反应速度、抑制反应产物长大速度，解决了传统原位合成方法反应产物颗粒尺寸分布范围大、副产物多的难题。通过严格控制金属熔体和熔盐的深度，增大合金‑熔盐的反应界面，反应产物更易分散，熔体中残余熔盐显著降低，降低了熔体净化难度。
This invention discloses a method for preparing nanoparticle-reinforced aluminum-based composite materials through low-temperature in-situ synthesis, which has the following characteristics: (1) Using the calculation method of this invention, the initial melting amount of the alloy and the crucible size are reasonably selected, and the depth of the molten salt layer during the reaction process is controlled to be no more than 3 cm; (2) Using Al-Si eutectic alloy as the base melt, mixed salt is added at 600℃, and the melt temperature during the entire reaction process is no more than 650℃; (3) After the reaction is completed, vacuum purification treatment and alloying elements are added sequentially by heating. This invention uses a reasonable crucible diameter and an extremely low reaction temperature to effectively reduce the reaction rate and inhibit the growth rate of reaction products, solving the problem of large particle size distribution and many by-products in the traditional in-situ synthesis method. By strictly controlling the depth of the metal melt and molten salt, the reaction interface between the alloy and molten salt is increased, the reaction products are more easily dispersed, the residual molten salt in the melt is significantly reduced, and the difficulty of melt purification is reduced.
Description
Technical Field
The invention belongs to the field of preparation of aluminum-based composite materials, and particularly relates to a preparation method of a low-temperature in-situ synthesized nanoparticle reinforced aluminum-based composite material.
Background
The nanoparticle reinforced aluminum matrix composite material not only has excellent mechanical properties, but also has the advantages of high wear resistance, good thermal conductivity, low thermal expansion coefficient, strong designability and the like, and has wide application prospect in the field of manufacturing of advanced equipment. The in situ synthesis method can directly react in the melt to produce the enhanced particles with thermodynamic stability. The reinforced particles are nucleated and grow up in the melt, and have natural wettability with the melt. The interface between the reinforced particles and the matrix is pure, and the bonding strength is high. Therefore, in-situ synthesis of particle reinforced aluminum matrix composites is considered to be the most promising composite preparation technique. The fluoride salt method has the advantages of simple process, low cost and the like, and is the most engineering potential method for synthesizing the nanoparticle reinforced aluminum matrix composite in situ.
However, the in-situ synthesis of the nanoparticle reinforced aluminum matrix composite material by the fluoride salt method still does not realize large-scale engineering application, and the main reason is that the bottleneck technical problem still exists but is not solved yet:
Firstly, the reinforced particles have wide size distribution range from hundreds of nanometers to microns, and the presence of large-size particles limits the reinforcing effect of the nanoparticles, secondly, the uniformity of the dispersion of the nanoparticles in a matrix is poor, the agglomerated nanoparticles reduce the mechanical properties of the matrix material instead, thirdly, the residual molten salt in the melt is difficult to completely discharge, the purity of the melt is poor, and the particle reinforcing effect is greatly reduced (Hu Dongfu. The preparation of the high-cleanness in-situ TiB2 reinforced aluminum-based composite material [ D ]. Dai.e. university of company, 2014.).
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 temperature of a melt is controlled to 660-670 ℃, high-speed mechanical stirring is applied to the upper surface of the melt to form a vortex, and mixed salt is added into the vortex on the surface of the melt to react for 15min. The reaction of the mixed salt with Al is exothermic, resulting in an increase in the melt temperature of about 90 ℃, and the technique does not take into account the effect of the increase in the melt temperature on the reaction process. In addition, the surface swirl rotating at high speed can cause mixed salt and air to be entrained into the melt, and a large amount of residual emulsified salt and a large amount of oxide are formed in the melt, so that the viscosity of the melt is increased, and difficulties are brought to the melt purification treatment. The method does not involve purification techniques of residual emulsifying salts and oxide inclusions. Liu Zhengcai et al (Liu Zhengcai, et al, mixed salt method TiB 2 particle reinforced aluminum matrix composites research status quo [ J ]. Thermal processing technique, 2021,12 (50) pp: 17-21) show that mechanical agitation can effectively promote melt flow and melt homogenization. However, the clusters cannot be effectively broken by low-speed stirring, and the absorption and oxidation of hydrogen are increased by high-speed stirring, and surface impurities are introduced, so that the mechanical properties of the composite material are reduced.
Team Wang Haowei presents a system and method for preparing in situ autogenous aluminum matrix composites using pulsed magnetic fields. Adding mixed salt at 700-760 ℃ while vacuumizing (a method for controlling an in-situ self-generated aluminum-based composite material by using a melt with electromagnetic stirring, china patent 202011571152.9, a system Chinese patent 202011571153.3 for controlling the in-situ self-generated aluminum-based composite material by using the melt with electromagnetic stirring, and a method for controlling the in-situ self-generated aluminum-based composite material by using a permanent magnet stirring, china patent 202011571141.0). The technology does not relate to the study of the influence of reaction exotherm and melt temperature rise on the reaction process, and does not relate to the study related to the residual molten salt purification technology.
In order to avoid the problem that residual molten salt in the aluminum melt is difficult to discharge due to the rising and stirring of the temperature of the melt in the fluorine method reaction process, china patent 202111585762.9 proposes a preparation method of an adjustable TiB 2 in-situ reinforced aluminum-based composite material. The method takes boron alloy and aluminum-titanium alloy or pure titanium as raw materials, reacts at 800-850 ℃, and adopts argon refining and degassing. The technology has higher reaction temperature, does not relate to mixed salt reaction, and does not relate to residual molten salt purification technology.
Chinese patent 200510029902.9 discloses a preparation method of an in-situ particle reinforced high-temperature resistant aluminum matrix composite. The reaction temperature range disclosed by the method is 680-800 ℃, and after the reaction is completed, alloy elements are added, and vacuumizing and standing are carried out. The method has higher reaction temperature, does not involve the influence of the rising reaction temperature on the reaction process, and does not treat the residual salt in the melt in time after the reaction is finished, and the addition of alloy elements can cause the further increase of the viscosity of the melt, so that the purification treatment of the melt is more difficult.
Wang et Al adopts a mechanical stirring mode in the reaction process, and reacts at 850 ℃ to obtain the tensile strength 375.3MPa of the TiB 2 (2.2 vol%)/A356 composite material, the yield strength 304.7MPa, the elongation 4.88％(Wang,Mechanical properties of in-situ TiB2/A356 composites[J].Materials Science&Engineering A,590(2014)246–254). He Yongsheng et Al adopts C 2Cl6 for refining, then mixed salt is added at 720 ℃, the mixture is fully stirred, and sand casting is carried out to obtain the tensile strength 300MP of the 5wt%/ZL114A composite material, the elongation 2.5% (He Yongsheng and the like. The tissue and mechanical properties [ J ] casting, 2000 (07): 396-397.) of the endophytic TiB 2 particle reinforced TiB 2/Al-7%Si-05%Mg composite material. The reaction temperatures studied above are all relatively high and do not involve the exothermic reaction and the effect of the rise in melt temperature on the reaction process.
The inventor groups find through experimental research that the temperature of the melt rises by about 80-100 ℃ in the reaction process when the melting amount is hundreds of kilograms to up to ton. 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.
The release of a large amount of gas (KBF 4＝KF+BF3↑,K2TiF6＝2KF+TiF4 ≡) during the reaction is one of the important reasons for the low yield of TiB 2 particles, and the higher the reaction temperature is, the more severe the reaction (KBF 4＝KF+BF3↑,K2TiF6＝2KF+TiF4 ≡), resulting in the lower the yield of TiB 2.
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
In order to solve the problems in the prior art, the invention provides a preparation method of a low-temperature in-situ synthesized nanoparticle reinforced aluminum matrix composite.
The technical scheme adopted for solving the technical problems is as follows:
The invention provides a preparation method of a low-temperature in-situ synthesized nanoparticle reinforced aluminum matrix composite, which specifically comprises the following steps:
s1, filling a raw material AlSi12 eutectic alloy with the weight of m1 into a crucible with the diameter of D for melting, heating to a certain temperature after melting, preserving heat, and uniformly stirring the preserved eutectic alloy melt;
S2, adding mixed salt of potassium fluotitanate and potassium fluoborate into a melt for reaction, and slowly adding AlSi12 eutectic alloy blocks with the weight of m2 into the melt after the mixed salt is completely melted;
s3, after the reaction is completed, slag skimming is carried out, and vacuum desalting treatment is carried out on the melt;
s4, heating the melt, adding pure aluminum ingot with the weight of m3, and then controlling the temperature and adding pure magnesium with the weight of m 4;
And S5, carrying out melt refining treatment by adopting an argon rotary blowing method, adjusting the temperature and casting.
Preferably, the crucible diameter D, the total weight m of the prepared composite material and the mass fraction of TiB 2 nano-particles contained in the prepared composite material conform to the following relationship:
wherein:
d is the diameter of the crucible;
m is the total weight of the prepared composite material, and the unit is g;
w t is the design content of TiB 2, which is a percentage;
Gamma Ti is the preset yield of Ti in K 2TiF6, which is 100% in the invention;
gamma B is the preset yield of B in KBF 4, and 100% is taken in the invention;
w K2TiF6 is the relative molecular weight of K 2TiF6;
W TiB2 is the molecular weight of TiB 2;
W KBF4 is the molecular weight of KBF 4;
ρ Salt is the density of the molten mixed salt in g/cm 3;
h Salt is the depth of the molten mixed salt, which is not more than 3cm depending on the actual production.
Preferably, in step S1, the temperature is 590 to 610 ℃.
Preferably, in the step S2, the mixed salt of potassium fluotitanate and potassium fluoborate is subjected to preheating treatment at 400 ℃ for 2 hours, the mixed salt of potassium fluotitanate and potassium fluoborate is added into a melt for reaction, an AlSi12 eutectic alloy block with the weight of m2 is slowly added into the melt in the reaction process, the temperature of the melt in the reaction process is controlled to be not more than 650 ℃, and the weight m2 of the added AlSi12 eutectic alloy block is 5-10% of the weight of the added mixed salt.
Preferably, in the step S3, the condition during the vacuum desalination treatment is that the temperature of the melt is 600-630 ℃, the pressure is not more than 500Pa, and the vacuum desalination treatment time is 15-30 min.
Preferably, in the step S4, the temperature of the melt is raised to 760-780 ℃ before the pure aluminum ingot is added, and the temperature of the melt is controlled to 700-720 ℃ before the pure magnesium is added.
Preferably, in step S5, the rotational speed of the argon rotary blowing method is 300-600 r/min, the pressure of the argon is 1-2 mpa, and the refining time of the argon rotary blowing method is 15-25 min.
The invention also provides a nanoparticle reinforced aluminum matrix composite material, which is prepared by the preparation method.
Compared with the prior art, the invention has the following beneficial effects:
(1) The invention firstly discloses that the depth of molten salt in the reaction process is limited to be not more than 3cm, and in order to meet the requirement, the crucible diameter needs to be designed according to the content of reinforced particles in the composite material and the total weight of the prepared composite material. According to the calculation method provided by the invention, on the premise of the same initial melting quantity, the cross section area of the crucible used by the method is 4-9 times that of the traditional crucible, and the diameter of the crucible is about 2-3 times that of the traditional crucible. The method has the advantages that the contact area of the metal melt and the molten salt is increased, the reaction efficiency is improved, the diffusion distance of reaction products is increased, the reaction products are dispersed, the heat dissipation area is increased, the heat conduction released by the reaction is facilitated, the abrupt increase of the reaction temperature is avoided, and the reinforced particles with high shape and size consistency are obtained.
(2) According to the invention, by utilizing the characteristic of low melting point of the AlSi12 eutectic alloy, the AlSi12 with the weight of m1 is melted and then is controlled to be at the temperature of about 600 ℃, compared with the temperature in the prior art, the reaction speed is effectively inhibited, and the problem of poor consistency of reaction products caused by rapid local temperature rise of a melt due to rapid reaction is avoided. After the added mixed salt is melted, slowly adding an AlSi12 eutectic alloy block with the weight of m2 into the melt, further improving the controllability of the temperature of the melt in the reaction process, and being beneficial to continuous and stable reaction, thereby obtaining reinforced particles with uniform morphology and size;
(3) After the reaction is finished, the vacuum desalting treatment is carried out under the reasonable electromagnetic stirring condition, 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.
Drawings
The foregoing and/or additional aspects and advantages of the invention will become apparent and may be better understood from the following description of embodiments taken in conjunction with the accompanying drawings in which:
Fig. 1 is an SEM detection result diagram of particle size and morphology of nano reinforced particles of TiB 2/ZL 101A composite material with 3% of TiB2 mass fraction prepared in example one.
Fig. 2 is an SEM detection result diagram of particle size and morphology of nano reinforced particles of the TiB 2/ZL 114A composite material with the mass fraction of TiB2 of 5% prepared in example two.
Fig. 3 is an SEM detection result diagram of particle size and morphology of nano reinforced particles of the TiB 2/ZL 101A composite material with 3% of TiB2 mass fraction prepared in example three.
Fig. 4 is an SEM detection result diagram of the nano enhanced granularity and morphology of the TiB 2/ZL 114A composite material with the mass fraction of TiB2 of 5% prepared in example four.
Detailed Description
Embodiments of the present invention are described in detail below, examples of which are illustrated in the accompanying drawings, wherein like or similar reference numerals refer to like or similar elements or elements having like or similar functions throughout. The embodiments described below by referring to the drawings are illustrative only and are not to be construed as limiting the invention.
Example 1
The embodiment provides a preparation method of a low-temperature in-situ synthesized nanoparticle reinforced aluminum matrix composite (ZL 101A-3wt.% TiB 2), which specifically comprises the following steps:
S1, calculating the crucible diameter D according to the following formula:
wherein:
m is the total weight of the composite material prepared;
w t is the design content of TiB 2, 3%;
Gamma Ti is the preset yield of Ti in K 2TiF6, taking 100%;
Gamma B is the preset yield of B in KBF 4, and 100 percent is taken;
W K2TiF6 is the relative molecular weight of K 2TiF6, 240.07;
W TiB2 is the relative molecular weight of TiB 2, 69.49;
w KBF4 is the relative molecular weight of KBF 4, 125.91;
ρ salt is the density of the molten mixed salt, 2.2g/cm 3;
h salt is the depth of the molten mixed salt, which is not more than 3cm depending on the actual production, here taken as 3cm.
This example prepares 100kg of ZL101A-3wt.% TiB 2 composite, so m=100 kg=1× 5 g, preparing ZL101A-3wt.% TiB 2 composite requires 11.4kg of potassium fluotitanate, 11.0kg of potassium fluoborate, 58.4kg (m) of AlSi12 total, 38.0kg (m 3) of pure Al, and 0.45kg (m 4) of pure Mg. m2 is 5% by weight of the mixed salt, i.e. m2=1.1 kg. M1=m-m 2=57.3 kg.
Substituting the parameters into the above formula, and calculating to obtain the crucible with the diameter of 65cm. Charging a raw material AlSi12 eutectic alloy with the weight of 57.3kg into a crucible with the diameter of 65cm for melting, heating to 600 ℃ after melting, preserving heat, and uniformly stirring the preserved eutectic alloy melt;
S2, adding mixed salt of potassium fluotitanate and potassium fluoborate which is preheated at 400 ℃ for 2 hours into a melt, slowly adding AlSi12 eutectic alloy blocks with the weight of 1.1kg into the melt after the mixed salt is completely dissolved in the melt, and controlling the temperature of the melt to be not more than 650 ℃;
s3, after the reaction is finished, slag skimming is carried out, and vacuum desalination treatment is carried out on the melt for 20min, wherein the temperature of the melt is controlled to be 615 ℃ and the pressure is controlled to be 500Pa in the treatment process;
S4, heating the melt to 770 ℃, adding 38.0kg of pure aluminum ingot, then controlling the temperature to 710 ℃ and adding 0.45kg of pure magnesium;
And S5, carrying out melt refining treatment by adopting an argon rotary blowing method, wherein the rotating speed is 450r/min, the pressure of argon is 1.5MPa, the refining time of the argon rotary blowing method is 20min, regulating the temperature and casting to obtain the nano reinforced particles of the TiB 2/ZL 101A composite material with the mass fraction of TiB2 being 3%, and the morphology chart is shown in figure 1.
TiB 2 (3 wt.%)/ZL 101A aluminum-based composite material prepared in this example, tiB 2 particle size is concentrated at 90-100 nm, and after T6 heat treatment specified by HB 962-2001 and a room temperature tensile test method of GB/T228-2002, the average tensile strength of the composite material prepared once is 340MPa, the average yield strength is 260MPa, and the average elongation is 7%.
Example two
The embodiment provides a preparation method of a low-temperature in-situ synthesized nanoparticle reinforced aluminum matrix composite (ZL 114A-5wt.% TiB 2), which specifically comprises the following steps:
S1, calculating the crucible diameter D according to the following formula:
wherein:
m is the total weight of the composite material prepared;
w t is the design content of TiB 2, 5wt%;
Gamma Ti is the preset yield of Ti in K 2TiF6, taking 100%;
Gamma B is the preset yield of B in KBF 4, and 100 percent is taken;
W K2TiF6 is the relative molecular weight of K 2TiF6, 240.07;
W TiB2 is the relative molecular weight of TiB 2, 69.49;
w KBF4 is the relative molecular weight of KBF 4, 125.91;
ρ salt is the density of the molten mixed salt, 2.2g/cm 3;
h salt is the depth of the molten mixed salt, which is not more than 3cm depending on the actual production, here taken as 2.5cm.
This example prepares 100kg of ZL114A-5wt.% TiB 2 composite material, so m=100 kg=1× 5 g, preparing 100kg of ZL114A-5wt.% TiB 2 composite material requires 17.3kg of potassium fluotitanate salt, 18.1kg of potassium fluoborate salt, 58.4kg (m) of alsi12 total, 36.0kg (m 3) of pure Al, and 0.7kg (m 4) of pure Mg. m2 is 10% by weight of the mixed salt, i.e. m2=3.5 kg. M1=m-m 2=54.9 kg.
From the above equation, the crucible diameter was calculated to be 90cm. Charging a raw material AlSi12 eutectic alloy with the weight of 54.9kg into a crucible with the diameter of 90cm for melting, heating to 600 ℃ after melting, preserving heat, and uniformly stirring the preserved eutectic alloy melt;
S2, adding mixed salt of potassium fluotitanate and potassium fluoborate which is preheated at 400 ℃ for 2 hours into a melt, slowly adding AlSi12 eutectic alloy blocks with the weight of 3.5kg into the melt after the mixed salt is completely dissolved in the melt, and controlling the temperature of the melt to be not more than 650 ℃;
s3, after the reaction is finished, slag skimming is carried out, and vacuum desalination treatment is carried out on the melt for 20min, wherein the temperature of the melt is controlled to be 615 ℃ and the pressure is controlled to be 500Pa in the treatment process;
S4, heating the melt to 770 ℃, adding 36.0kg of pure aluminum ingot, then controlling the temperature to 710 ℃ and adding 0.7kg of pure magnesium;
And S5, carrying out melt refining treatment by adopting an argon rotary blowing method, wherein the rotating speed is 450r/min, the pressure of argon is 1.5MPa, the refining time of the argon rotary blowing method is 20min, regulating the temperature and casting to obtain the nano reinforced particles of the TiB 2/ZL 114A composite material with the mass fraction of TiB2 being 5%, and the morphology chart is shown in figure 2.
TiB 2 (5 wt.%)/ZL 114A aluminum-based composite material prepared in the embodiment has the particle size of TiB 2 concentrated at 90-100 nm, and the average tensile strength of the composite material prepared in a single step is 395MPa, the average yield strength is 325MPa and the average elongation is 6% after T6 heat treatment specified by HB 962-2001 and a room temperature tensile test method of GB/T228-2002.
Example III
The embodiment provides a preparation method of a low-temperature in-situ synthesized nanoparticle reinforced aluminum matrix composite (ZL 101A-3wt.% TiB 2), which specifically comprises the following steps:
s1, loading a raw material AlSi12 eutectic alloy with the weight of 57.3kg into a crucible with the diameter of 30cm for melting, heating to 600 ℃ after melting, preserving heat, and uniformly stirring the heat-preserving eutectic alloy melt;
S2, adding mixed salt of potassium fluotitanate and potassium fluoborate which is preheated at 400 ℃ for 2 hours into a melt, slowly adding AlSi12 eutectic alloy blocks with the weight of 1.1kg into the melt after the mixed salt is completely dissolved in the melt, and controlling the temperature of the melt to be not more than 650 ℃;
s3, after the reaction is finished, slag skimming is carried out, and vacuum desalination treatment is carried out on the melt for 20min, wherein the temperature of the melt is controlled to be 615 ℃ and the pressure is controlled to be 500Pa in the treatment process;
S4, heating the melt to 770 ℃, adding 38kg of pure aluminum ingot, then controlling the temperature to 710 ℃ and adding 0.45kg of pure magnesium;
And S5, carrying out melt refining treatment by adopting an argon rotary blowing method, wherein the rotating speed is 450r/min, the pressure of argon is 1.5MPa, the refining time of the argon rotary blowing method is 20min, regulating the temperature and casting to obtain the nano reinforced particles of the TiB 2/ZL 101A composite material with the mass fraction of TiB2 being 3%, and the morphology chart is shown in figure 3.
TiB 2 (3 wt.%)/ZL 101A aluminum-based composite material prepared in this example, tiB 2 particle size was concentrated at 90-100 nm, and a large amount of large grain TiB 2 phase with a size close to 2 μm was observed on SEM photographs. After T6 heat treatment prescribed by HB 962-2001 and a room temperature tensile test method of GB/T228-2002, the average tensile strength of the composite material prepared once is 315MPa, the average yield strength is 240MPa, and the average elongation is 4%.
The nano reinforced particles of the TiB 2/ZL 101A composite material with the mass fraction of 3% prepared in the first embodiment and the third embodiment are prepared under the same experimental conditions except for the diameter of a crucible, and compared with fig. 1 and 3, the nano reinforced particles prepared in the first embodiment have better dispersibility, and the size of the particles is more uniform, because the increase of the cross-sectional area of the crucible is beneficial to the dispersion of reaction products, and meanwhile, the heat dissipation area is increased, the heat conduction released by the reaction is facilitated, and the reinforced particles with high shape and size consistency are obtained.
Example IV
The embodiment provides a preparation method of a low-temperature in-situ synthesized nanoparticle reinforced aluminum matrix composite (ZL 114A-5wt.% TiB 2), which specifically comprises the following steps:
S1, calculating the crucible diameter D according to the following formula:
wherein:
d is the diameter of the crucible;
m is the total weight of the composite material prepared;
w t is the design content of TiB 2, 5wt%;
Gamma Ti is the preset yield of Ti in K 2TiF6, taking 100%;
Gamma B is the preset yield of B in KBF 4, and 100 percent is taken;
W K2TiF6 is the relative molecular weight of K 2TiF6, 240.7;
W TiB2 is the relative molecular weight of TiB 2, 69.49;
W KBF4 is KBF4 and the molecular weight is 125.91;
ρ salt is the density of the molten mixed salt, 2.2g/cm 3;
h salt is the depth of the molten mixed salt, which is not more than 3cm depending on the actual production, here taken as 2.5cm.
This example prepares 100kg of ZL114A-5wt.% TiB2 composite material, so m=100 kg=1×10 5 g, preparing 100kg of ZL101A-5wt.% TiB 2 composite material requiring 17.3kg of potassium fluotitanate, 18.1kg of potassium fluoborate salt, 58.4kg (m) AlSi12 total, 36.0kg (m 3) of pure Al and 0.7kg (m 4) of pure Mg.
From the above equation, the crucible diameter was calculated to be 90cm. Charging raw material AlSi12 eutectic alloy with the weight of 58.4kg into a crucible with the diameter of 90cm for melting, heating to 600 ℃ after melting, preserving heat, and uniformly stirring the preserved eutectic alloy melt;
s2, adding mixed salt of potassium fluotitanate and potassium fluoborate which are preheated at 400 ℃ for 2 hours into the melt, and waiting for the mixed salt to be completely dissolved in the melt;
s3, after the reaction is finished, slag skimming is carried out, and vacuum desalination treatment is carried out on the melt for 20min, wherein the temperature of the melt is controlled to be 615 ℃ and the pressure is controlled to be 500Pa in the treatment process;
S4, heating the melt to 770 ℃, adding 36.0kg of pure aluminum ingot, then controlling the temperature to 710 ℃ and adding 0.7kg of pure magnesium;
And S5, carrying out melt refining treatment by adopting an argon rotary blowing method, wherein the rotating speed is 450r/min, the pressure of argon is 1.5MPa, the refining time of the argon rotary blowing method is 20min, regulating the temperature and casting to obtain the nano reinforced particles of the TiB 2/ZL 114A composite material with the mass fraction of TiB2 being 5%, and the morphology chart is shown in figure 4.
TiB 2 (5 wt.%)/ZL 114A aluminum-based composite material prepared in the embodiment has a large amount of TiB 2 particles with a size of 400-800 nm, and the average tensile strength of the composite material prepared in a single process is 360MPa, the average yield strength is 315MPa and the average elongation is 4% by adopting a T6 heat treatment specified by HB 962-2001 and a room temperature tensile test method of GB/T228-2002.
Compared with the nano reinforced particles prepared in the second embodiment, the nano reinforced particles of the TiB 2/ZL 114A composite material prepared in the fourth embodiment, except that the fourth embodiment is prepared under the same experimental conditions without adding Al-Si eutectic alloy blocks into the melt for cooling, and compared with the fig. 2 and 4, it can be observed that the nano reinforced particles prepared in the fourth embodiment form a large number of clusters, and the dispersing effect and uniformity are far lower than those of the nano reinforced particles prepared in the second embodiment, because the process of adding the Al-Si eutectic alloy blocks for cooling further improves the controllability of the melt temperature in the reaction process, the reaction is continuously and stably carried out, so that the reinforced particles with uniform morphology and size are obtained.
Although embodiments of the present invention have been shown and described, it will be understood by those skilled in the art that various changes, modifications, substitutions and alterations can be made therein without departing from the spirit and scope of the invention as defined by the appended claims and their equivalents.
Claims (7)
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