CN104532046B - Method for preparing nano-aluminum-nitride reinforced aluminum-based composite semi-solid slurry based on ultrasonic and mechanical vibration combination - Google Patents
Method for preparing nano-aluminum-nitride reinforced aluminum-based composite semi-solid slurry based on ultrasonic and mechanical vibration combination Download PDFInfo
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Abstract
一种基于超声及机械振动复合制备纳米氮化铝增强铝基复合材料半固态浆料的方法,首先将纳米氮化铝颗粒与铝粉末按质量比为1:1~2:3混合60~70rpm球磨50~60h;将混合粉末放入坩锅内加热至660~670℃;空冷、碾碎,过筛;将铝合金放入坩锅内熔化,700~750℃时,按纳米氮化铝颗粒的加入量为铝合金熔体的1~4wt.%的量,将上述过筛后的混合粉末5~10min加入到铝合金熔体中,同时引入20KHz、1~3KW高能超声,之后继续超声5~10min;将熔体温度5~15℃/min降至合金半固态温度区间,并施加机械振动处理,功率1.5KW、频率400~600Hz及振幅0.5~1.5mm。本发明得到的铝基纳米复合材料组织中初生ɑ‑Al相细小且分布均匀,纳米氮化铝颗粒分布均匀,无团聚现象,工艺成本低、简单;安全可靠;操作方便。
A method for preparing semi-solid slurry of nano-aluminum nitride-reinforced aluminum-based composite materials based on ultrasonic and mechanical vibration. Firstly, nano-aluminum nitride particles and aluminum powder are mixed at a mass ratio of 1:1-2:3 at 60-70rpm Ball mill for 50-60 hours; put the mixed powder into the crucible and heat it to 660-670°C; air-cool, crush, and sieve; put the aluminum alloy into the crucible and melt it at 700-750°C, press nano-aluminum nitride particles % of the aluminum alloy melt, add the above-mentioned sieved mixed powder into the aluminum alloy melt for 5-10 minutes, introduce 20KHz, 1-3KW high-energy ultrasound at the same time, and then continue ultrasonication for 5 ~10min; reduce the melt temperature to 5~15℃/min to the semi-solid temperature range of the alloy, and apply mechanical vibration treatment, power 1.5KW, frequency 400~600Hz and amplitude 0.5~1.5mm. The primary α-Al phase in the structure of the aluminum-based nano-composite material obtained by the invention is fine and evenly distributed, the nano-aluminum nitride particles are evenly distributed, there is no agglomeration phenomenon, the process cost is low, simple, safe and reliable, and easy to operate.
Description
技术领域technical field
本发明属于金属材料制备领域,特别涉及铝基复合材料半固态浆料的制备方法。The invention belongs to the field of metal material preparation, in particular to a method for preparing semi-solid slurry of aluminum-based composite materials.
背景技术Background technique
半固态合金在成形过程中充型平稳,产生的热应力低,缩孔、缩松缺陷少,净近成形。颗粒增强铝基复合材料具有比强度、比刚度高、高耐磨性、高的减振性等许多优点。氮化铝颗粒因其具有良好的物理化学,机械及热性能,是理想的增强相,为广大学者所关注。微米颗粒可以改善基体的屈服强度及极限抗压强度,但使基体的延展性变差。纳米颗粒能在保持较低含量下明显提高基体的弹性模量、屈服强度、抗磨性及高温蠕变性,因而逐渐受到重视。大量研究发现纳米陶瓷颗粒与铝合金熔体的润湿性差,且在熔体中的状态不稳定。而通过传统的工艺制备纳米复合材料存在纳米颗粒易团聚、含量不高、工艺复杂、成型受限等问题使得铝基纳米复合材料的性能提高的潜力受到很大的影响。During the forming process, the semi-solid alloy has stable mold filling, low thermal stress, less shrinkage cavity and shrinkage defects, and a net near-formation. Particle-reinforced aluminum matrix composites have many advantages such as specific strength, high specific stiffness, high wear resistance, and high vibration damping. Aluminum nitride particles are an ideal reinforcement phase because of their good physical, chemical, mechanical and thermal properties, and have attracted the attention of many scholars. Micron particles can improve the yield strength and ultimate compressive strength of the matrix, but make the ductility of the matrix worse. Nanoparticles can significantly improve the elastic modulus, yield strength, wear resistance and high temperature creep of the matrix while maintaining a low content, so they are gradually being valued. A large number of studies have found that the wettability of nano-ceramic particles and aluminum alloy melt is poor, and the state in the melt is unstable. However, the preparation of nanocomposites by traditional processes has problems such as easy agglomeration of nanoparticles, low content, complex process, and limited molding, which greatly affects the potential of improving the performance of aluminum-based nanocomposites.
发明内容Contents of the invention
本发明的目的是提供一种纳米氮化铝颗粒增强铝基复合材料半固态浆料的制备方法The purpose of the present invention is to provide a method for preparing semi-solid slurry of nano-aluminum nitride particles reinforced aluminum-based composite materials
本发明是通过以下技术方案实现的。The present invention is achieved through the following technical solutions.
本发明所述的制备方法为:首先将纳米氮化铝颗粒与铝粉末混合进行球磨50~60h,其中纳米氮化铝颗粒与铝粉末的质量比为1:1~2:3,球磨速度为60~70rpm;将混合粉末放入坩锅内加热,温度控制在660~670℃;空冷、碾碎,过筛,其中网孔尺寸为1000~850μm;将铝合金放入坩锅内加热、熔化,在温度700~750℃时,按纳米氮化铝颗粒的加入量为铝合金熔体的1~4wt.%的量,将上述过筛后的混合粉末加入到铝合金熔体中,加入时间为5~10min,在加入过程中引入高能超声到铝合金熔体中,超声频率20KHz、功率1~3KW,之后继续超声处理5~10min;将熔体温度降至合金半固态温度区间,降温速率为5~15℃/min,此过程施加机械振动处理,振动功率1.5KW、频率400~600Hz及振幅0.5~1.5mm;即可获得纳米氮化铝增强铝基复合材料半固态浆料。The preparation method of the present invention is as follows: first, mix the nano-aluminum nitride particles and the aluminum powder and perform ball milling for 50-60 hours, wherein the mass ratio of the nano-aluminum nitride particles to the aluminum powder is 1:1-2:3, and the ball-milling speed is 60~70rpm; put the mixed powder into the crucible to heat, the temperature is controlled at 660~670℃; air cooling, crushing, and sieving, wherein the mesh size is 1000~850μm; put the aluminum alloy into the crucible to heat and melt , when the temperature is 700-750°C, the added amount of nano-aluminum nitride particles is 1-4wt.% of the aluminum alloy melt, and the above-mentioned mixed powder after sieving is added to the aluminum alloy melt, and the addition time is 5-10 minutes, introduce high-energy ultrasound into the aluminum alloy melt during the addition process, the ultrasonic frequency is 20KHz, the power is 1-3KW, and then continue the ultrasonic treatment for 5-10 minutes; the melt temperature is reduced to the semi-solid temperature range of the alloy, and the cooling rate The temperature is 5-15°C/min, and mechanical vibration treatment is applied during this process. The vibration power is 1.5KW, the frequency is 400-600Hz, and the amplitude is 0.5-1.5mm; the nano-aluminum nitride-reinforced aluminum matrix composite material semi-solid slurry can be obtained.
纯铝颗粒塑性较好,容易被陶瓷颗粒压入。低能球磨尽可能很好地分散颗粒又可以避免有害的化学反应。熔体表面张力的作用可以使小颗粒很难加入而大颗粒因其自身重力可以很容易克服这种抗力。超声对熔体产生的空化、声流对颗粒的润湿及分散有很大的促进作用。机械振动产生的正弦波能够在介质传播,且有强烈冲击力产生。Pure aluminum particles have better plasticity and are easily pressed into by ceramic particles. Low energy ball milling disperses the particles as well as possible while avoiding harmful chemical reactions. The effect of melt surface tension can make it difficult for small particles to join, while large particles can easily overcome this resistance due to their own gravity. Ultrasound can greatly promote the cavitation produced by the melt, and the acoustic flow can greatly promote the wetting and dispersion of particles. The sine wave generated by mechanical vibration can propagate in the medium and produce strong impact force.
本发明所述的纳米氮化铝及铝的颗粒尺寸优选纳米氮化铝30~100nm,铝58~75μm。The particle size of nano-aluminum nitride and aluminum in the present invention is preferably 30-100 nm for nano-aluminum nitride and 58-75 μm for aluminum.
本发明得到的铝基纳米复合材料组织中初生ɑ-Al相细小且分布均匀,纳米氮化铝颗粒分布均匀,无团聚现象。此工艺成本低、简单;安全可靠;操作方便。The primary α-Al phase in the structure of the aluminum-based nano-composite material obtained by the invention is fine and evenly distributed, and the nano-aluminum nitride particles are evenly distributed without agglomeration. The process is low in cost, simple, safe and reliable, and easy to operate.
附图说明Description of drawings
图1为本发明制备制备的半固态A356铝基纳米复合材料浆料的显微组织。Fig. 1 is the microstructure of the semi-solid A356 aluminum-based nanocomposite slurry prepared by the present invention.
具体实施方式detailed description
本发明将通过以下实施例作进一步说明。The invention will be further illustrated by the following examples.
实施例1。Example 1.
首先将纳米氮化铝颗粒与铝粉末混合进行球磨60h,其中纳米氮化铝颗粒与铝粉末的质量比为2:3,球磨速度为70rpm;将混合粉末放入坩锅内加热,温度控制在660℃;空冷、碾碎,过筛,其中网孔尺寸为850μm;将7075铝合金放入坩锅内加热、熔化,在温度700℃时,按纳米氮化铝颗粒的加入量为铝合金熔体的1wt.%的量,将上述过筛后的混合粉末加入到7075铝合金熔体中,加入时间为5min,在加入过程中引入高能超声到铝合金熔体中,超声频率20KHz、功率1KW,之后继续超声处理5min;将熔体温度降至635℃,降温速率为5℃/min,此过程施加机械振动处理,振动功率1.5KW、频率400Hz及振幅0.5mm;即可获得纳米氮化铝增强铝基复合材料半固态浆料。First, mix the nano-aluminum nitride particles and aluminum powder for ball milling for 60 hours, wherein the mass ratio of nano-aluminum nitride particles to aluminum powder is 2:3, and the ball milling speed is 70rpm; put the mixed powder into the crucible for heating, and the temperature is controlled at 660°C; air cooling, crushing, and sieving, the mesh size of which is 850μm; put the 7075 aluminum alloy into the crucible to heat and melt, at a temperature of 700°C, the amount of nano-aluminum nitride particles added is the aluminum alloy melting The amount of 1wt.% of the body, the above-mentioned mixed powder after sieving is added to the 7075 aluminum alloy melt, the addition time is 5min, and high-energy ultrasound is introduced into the aluminum alloy melt during the addition process, the ultrasonic frequency is 20KHz, and the power is 1KW , and then continue ultrasonic treatment for 5 minutes; reduce the melt temperature to 635 ° C, the cooling rate is 5 ° C / min, this process is applied mechanical vibration treatment, vibration power 1.5KW, frequency 400Hz and amplitude 0.5mm; nano aluminum nitride can be obtained Reinforced semi-solid slurry for aluminum matrix composites.
实施例2。Example 2.
首先将纳米氮化铝颗粒与铝粉末混合进行球磨50h,其中纳米氮化铝颗粒与铝粉末的质量比为1:1,球磨速度为60rpm;将混合粉末放入坩锅内加热,温度控制在670℃;空冷、碾碎,过筛,其中网孔尺寸为1000μm;将6063铝合金放入坩锅内加热、熔化,在温度750℃时,按纳米氮化铝颗粒的加入量为铝合金熔体的2wt.%的量,将上述过筛后的混合粉末加入到6063铝合金熔体中,加入时间为10min,在加入过程中引入高能超声到铝合金熔体中,超声频率20KHz、功率2KW,之后继续超声处理5min;将熔体温度降至652℃,降温速率为10℃/min,此过程施加机械振动处理,振动功率1.5KW、频率500Hz及振幅0.5mm;即可获得纳米氮化铝增强铝基复合材料半固态浆料。First, mix the nano-aluminum nitride particles and aluminum powder for ball milling for 50 hours, wherein the mass ratio of nano-aluminum nitride particles to aluminum powder is 1:1, and the ball milling speed is 60rpm; put the mixed powder into a crucible for heating, and the temperature is controlled at 670°C; air cooling, crushing, and sieving, the mesh size of which is 1000μm; put the 6063 aluminum alloy into the crucible to heat and melt, at a temperature of 750°C, the amount of nano-aluminum nitride particles added is the aluminum alloy melting The amount of 2wt.% of the body, the above-mentioned mixed powder after sieving is added to the 6063 aluminum alloy melt, the addition time is 10min, and high-energy ultrasound is introduced into the aluminum alloy melt during the addition process, the ultrasonic frequency is 20KHz, and the power is 2KW , and then continue ultrasonic treatment for 5 minutes; reduce the melt temperature to 652 ° C, the cooling rate is 10 ° C / min, this process is applied mechanical vibration treatment, vibration power 1.5KW, frequency 500Hz and amplitude 0.5mm; nano-aluminum nitride can be obtained Reinforced semi-solid slurry for aluminum matrix composites.
实施例3。Example 3.
首先将纳米氮化铝颗粒与铝粉末混合进行球磨60h,其中纳米氮化铝颗粒与铝粉末的质量比为1:1,球磨速度为70rpm;将混合粉末放入坩锅内加热,温度控制在660℃;空冷、碾碎,过筛,其中网孔尺寸为850μm;将A356铝合金放入坩锅内加热、熔化,在温度700℃时,按纳米氮化铝颗粒的加入量为铝合金熔体的1wt.%的量,将上述过筛后的混合粉末加入到A356铝合金熔体中,加入时间为5min,在加入过程中引入高能超声到铝合金熔体中,超声频率20KHz、功率1KW,之后继续超声处理5min;将熔体温度降至605℃,降温速率为15℃/min,此过程施加机械振动处理,振动功率1.5KW、频率600Hz及振幅1.5mm;即可获得纳米氮化铝增强铝基复合材料半固态浆料。First, mix the nano-aluminum nitride particles and aluminum powder for ball milling for 60 hours, wherein the mass ratio of nano-aluminum nitride particles to aluminum powder is 1:1, and the ball milling speed is 70rpm; put the mixed powder into a crucible for heating, and the temperature is controlled at 660°C; air-cooled, crushed, and sieved, with a mesh size of 850 μm; put the A356 aluminum alloy into a crucible to heat and melt, and at a temperature of 700°C, the amount of nano-aluminum nitride particles added is The amount of 1wt.% of the body, the above-mentioned mixed powder after sieving is added to the A356 aluminum alloy melt, the addition time is 5min, and high-energy ultrasound is introduced into the aluminum alloy melt during the addition process, the ultrasonic frequency is 20KHz, and the power is 1KW , and then continue ultrasonic treatment for 5 minutes; reduce the melt temperature to 605 ° C, the cooling rate is 15 ° C / min, this process is applied mechanical vibration treatment, vibration power 1.5KW, frequency 600Hz and amplitude 1.5mm; nano-aluminum nitride can be obtained Reinforced semi-solid slurry for aluminum matrix composites.
附图1为实施例3条件下获得的的半固态A356铝基纳米复合材料浆料的组织,图中可见,所获得的铝基复合材料组织中没有粗大的树枝初生晶出现,初生ɑ-Al相被超声空化效应及机械振动产生的强大冲击力击碎,明显细化。超声空化及声流作用使得纳米氮化铝粉末在熔体中均匀分布。Accompanying drawing 1 is the structure of the semi-solid A356 aluminum-based nanocomposite slurry obtained under the conditions of Example 3. It can be seen from the figure that no coarse primary dendrites appear in the obtained aluminum-based composite structure, and the primary α-Al The phase is crushed by the strong impact force generated by the ultrasonic cavitation effect and mechanical vibration, and is obviously refined. Ultrasonic cavitation and acoustic flow make the nano-aluminum nitride powder evenly distributed in the melt.
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