CN107641727A - A kind of method that high-volume fractional SiC particulate reinforced Al matrix composite is prepared by high velocity compacted - Google Patents
A kind of method that high-volume fractional SiC particulate reinforced Al matrix composite is prepared by high velocity compacted Download PDFInfo
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- 239000002131 composite material Substances 0.000 title claims abstract description 76
- 238000000034 method Methods 0.000 title claims abstract description 38
- 239000011159 matrix material Substances 0.000 title abstract description 15
- HBMJWWWQQXIZIP-UHFFFAOYSA-N silicon carbide Chemical compound [Si+]#[C-] HBMJWWWQQXIZIP-UHFFFAOYSA-N 0.000 claims abstract description 107
- 229910010271 silicon carbide Inorganic materials 0.000 claims abstract description 82
- 238000003825 pressing Methods 0.000 claims abstract description 49
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- 239000000843 powder Substances 0.000 claims abstract description 41
- 238000005245 sintering Methods 0.000 claims abstract description 40
- 229910000838 Al alloy Inorganic materials 0.000 claims abstract description 25
- 238000001816 cooling Methods 0.000 claims abstract description 17
- 239000012299 nitrogen atmosphere Substances 0.000 claims abstract description 15
- 238000002156 mixing Methods 0.000 claims abstract description 7
- 238000000465 moulding Methods 0.000 claims abstract description 7
- 239000011812 mixed powder Substances 0.000 claims description 31
- 229910001094 6061 aluminium alloy Inorganic materials 0.000 claims description 26
- 239000012298 atmosphere Substances 0.000 claims description 18
- VYPSYNLAJGMNEJ-UHFFFAOYSA-N Silicium dioxide Chemical compound O=[Si]=O VYPSYNLAJGMNEJ-UHFFFAOYSA-N 0.000 claims description 14
- 229910052593 corundum Inorganic materials 0.000 claims description 12
- 239000010431 corundum Substances 0.000 claims description 12
- 238000012360 testing method Methods 0.000 claims description 9
- 229910052681 coesite Inorganic materials 0.000 claims description 7
- 229910052906 cristobalite Inorganic materials 0.000 claims description 7
- 239000000203 mixture Substances 0.000 claims description 7
- 239000000377 silicon dioxide Substances 0.000 claims description 7
- 235000012239 silicon dioxide Nutrition 0.000 claims description 7
- 229910052682 stishovite Inorganic materials 0.000 claims description 7
- 229910052905 tridymite Inorganic materials 0.000 claims description 7
- 238000005056 compaction Methods 0.000 claims description 6
- 238000000748 compression moulding Methods 0.000 claims description 6
- 239000008367 deionised water Substances 0.000 claims description 6
- 229910021641 deionized water Inorganic materials 0.000 claims description 6
- 230000032798 delamination Effects 0.000 claims description 6
- 238000004146 energy storage Methods 0.000 claims description 6
- 239000012535 impurity Substances 0.000 claims description 6
- 239000003921 oil Substances 0.000 claims description 6
- 238000005381 potential energy Methods 0.000 claims description 6
- 239000002994 raw material Substances 0.000 claims description 6
- 238000004381 surface treatment Methods 0.000 claims description 6
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Chemical compound O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims description 6
- XOOUIPVCVHRTMJ-UHFFFAOYSA-L zinc stearate Chemical compound [Zn+2].CCCCCCCCCCCCCCCCCC([O-])=O.CCCCCCCCCCCCCCCCCC([O-])=O XOOUIPVCVHRTMJ-UHFFFAOYSA-L 0.000 claims description 6
- 238000010438 heat treatment Methods 0.000 claims description 2
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- 238000005461 lubrication Methods 0.000 claims 1
- 230000009286 beneficial effect Effects 0.000 abstract description 5
- 230000003647 oxidation Effects 0.000 abstract description 4
- 238000007254 oxidation reaction Methods 0.000 abstract description 4
- 238000005516 engineering process Methods 0.000 abstract description 3
- 238000002844 melting Methods 0.000 abstract description 3
- 230000008018 melting Effects 0.000 abstract description 3
- 229910052782 aluminium Inorganic materials 0.000 abstract description 2
- XAGFODPZIPBFFR-UHFFFAOYSA-N aluminium Chemical compound [Al] XAGFODPZIPBFFR-UHFFFAOYSA-N 0.000 abstract description 2
- 239000007791 liquid phase Substances 0.000 abstract 2
- 239000000047 product Substances 0.000 description 15
- 238000002360 preparation method Methods 0.000 description 7
- 238000000280 densification Methods 0.000 description 6
- 230000008595 infiltration Effects 0.000 description 5
- 238000001764 infiltration Methods 0.000 description 5
- 239000000463 material Substances 0.000 description 5
- 238000004519 manufacturing process Methods 0.000 description 4
- 238000001228 spectrum Methods 0.000 description 4
- 230000002787 reinforcement Effects 0.000 description 3
- 238000011160 research Methods 0.000 description 3
- 238000013461 design Methods 0.000 description 2
- 238000011049 filling Methods 0.000 description 2
- 238000007731 hot pressing Methods 0.000 description 2
- 238000009776 industrial production Methods 0.000 description 2
- 238000004663 powder metallurgy Methods 0.000 description 2
- 238000001272 pressureless sintering Methods 0.000 description 2
- 238000009827 uniform distribution Methods 0.000 description 2
- 229910020068 MgAl Inorganic materials 0.000 description 1
- 229910004298 SiO 2 Inorganic materials 0.000 description 1
- 239000007795 chemical reaction product Substances 0.000 description 1
- 238000003776 cleavage reaction Methods 0.000 description 1
- 150000001875 compounds Chemical class 0.000 description 1
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- 230000002349 favourable effect Effects 0.000 description 1
- 229910052751 metal Inorganic materials 0.000 description 1
- 239000002184 metal Substances 0.000 description 1
- 239000011156 metal matrix composite Substances 0.000 description 1
- 239000011148 porous material Substances 0.000 description 1
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- 238000012827 research and development Methods 0.000 description 1
- 230000007017 scission Effects 0.000 description 1
- 238000002490 spark plasma sintering Methods 0.000 description 1
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Abstract
本发明公开了一种通过高速压制制备高体积分数SiC颗粒增强Al基复合材料的方法,包括SiC粉体的氧化处理混料、高速压制成型、N2气氛保护烧结和冷却步骤。本发明通过高速压制技术制备高体积分数的SiC颗粒增强Al基复合材料的压坯,该过程制备的压坯密度高且密度分布均匀、生产率高、成本低廉,可经济成形大型零件。SiC颗粒增强Al压坯经高速压制技术单次压制后,相对密度为85‑92%,较高的压坯密度有利于降低烧结温度和烧结时间。在N2气氛保护下,压坯加热到铝合金熔点以上进行液相烧结,液相填充碳化硅颗粒之间的空隙和铝合金粉末间的冶金结合同时进行。烧结坯凝固冷却后的得到碳化硅分布均匀、相对密度94‑98%、热导率150‑190W/mK的碳化硅增强铝基复合材料。
The invention discloses a method for preparing high-volume SiC particle-reinforced Al-based composite materials through high-speed pressing, which includes the steps of oxidation treatment and mixing of SiC powder, high-speed press molding, N2 atmosphere protection sintering and cooling steps. The invention prepares a high-volume-fraction SiC particle-reinforced Al-based composite material green compact through a high-speed pressing technique. The green green compact prepared by the process has high density and uniform density distribution, high productivity, and low cost, and can form large parts economically. The relative density of SiC particle-reinforced Al compact is 85-92% after single pressing by high-speed pressing technology, and the higher compact density is beneficial to reduce the sintering temperature and sintering time. Under the protection of N2 atmosphere, the compact is heated to above the melting point of the aluminum alloy for liquid phase sintering, and the liquid phase fills the gaps between the silicon carbide particles and the metallurgical bonding between the aluminum alloy powders proceeds simultaneously. After the sintered compact is solidified and cooled, a silicon carbide reinforced aluminum matrix composite material with uniform silicon carbide distribution, a relative density of 94-98%, and a thermal conductivity of 150-190W/mK is obtained.
Description
技术领域technical field
本发明涉及金属基复合材料材料领域,具体是一种通过高速压制制备高体积分数SiC颗粒增强Al基复合材料的方法。The invention relates to the field of metal-based composite materials, in particular to a method for preparing high-volume SiC particle-reinforced Al-based composite materials through high-speed pressing.
背景技术Background technique
碳化硅颗粒作为增强材料具有高熔点、高热稳定性、低热膨胀系数、成本低廉等优点,其热膨胀系数为4.7×10-6K-1,热导率为80-240W/mK;同时Al作为基体材料,具有高热导率(170-220W/mK、低密度(2.7g/cm2))、价格低廉和易于加工等优点,结合二者的优势制备出的高体积分数SiC增强Al基复合材料具有密度低、高导热、热膨胀系数可控等优异性能,成为今金属基复合材料研究的热点之一,在航空航天、大规模集成电路、军事电子器材有着十分广阔的应用前景。As a reinforcing material, silicon carbide particles have the advantages of high melting point, high thermal stability, low thermal expansion coefficient, and low cost. Its thermal expansion coefficient is 4.7×10 -6 K -1 , and its thermal conductivity is 80-240W/mK. material, has the advantages of high thermal conductivity (170-220W/mK, low density (2.7g/cm 2 )), low price and easy processing, and the high volume fraction SiC reinforced Al-based composite material prepared by combining the advantages of the two has Excellent properties such as low density, high thermal conductivity, and controllable thermal expansion coefficient have become one of the hotspots in the research of metal matrix composites today, and have very broad application prospects in aerospace, large-scale integrated circuits, and military electronic equipment.
目前,高体积分数的SiC颗粒增强Al基复合材料的制备方法有粉末冶金法、真空热压烧结法、无压渗透法等。上几种方法中,放电等离子烧结法制备复合材料具有成分比例准确、增强体在A1基中分布均匀、烧结温度低保温时间短等优点,但是该设备主要用于实验室研究,极少用于工业化生产。真空热压法制备复合材料过程中有专门设备提供高压和真空,该设备成本高、生产效率低。无压浸渗制备SiC/Al复合材料过程中,熔渗温度远高于铝基体的熔点,易生成Al4C3,且在渗透的过程中基体和增强体的比例不易控制,在制备预制体的过程中一些闭气孔不能被基体填充。At present, the preparation methods of SiC particle reinforced Al matrix composites with high volume fraction include powder metallurgy, vacuum hot pressing sintering, pressureless infiltration and so on. Among the above methods, the preparation of composite materials by spark plasma sintering has the advantages of accurate composition ratio, uniform distribution of reinforcement in A1 matrix, low sintering temperature and short holding time, etc., but this equipment is mainly used for laboratory research and is rarely used for Industrial production. In the process of preparing composite materials by vacuum hot pressing, there are special equipment to provide high pressure and vacuum. The equipment has high cost and low production efficiency. In the process of preparing SiC/Al composites by pressureless infiltration, the infiltration temperature is much higher than the melting point of the aluminum matrix, and Al 4 C 3 is easily formed, and the ratio of the matrix to the reinforcement is not easy to control during the infiltration process. During the process some closed pores cannot be filled by the matrix.
发明内容:Invention content:
本发明所要解决的技术问题是:鉴于目前制备高体积分数SiC颗粒增强A1基复合材料所存在的技术缺限和不足,提供一种制备成本相对低廉,工艺流程简化,最终获得低孔隙率、热导率高、高体积分数的SiC增强Al基复合材料的方法,且适宜工业化大规模生产。The technical problem to be solved by the present invention is: in view of the current technical limitations and deficiencies in the preparation of high volume fraction SiC particle reinforced Al-based composite materials, to provide a relatively low preparation cost, simplified process flow, and finally obtain low porosity, thermal A method for SiC-reinforced Al-based composite materials with high conductivity and high volume fraction, and is suitable for large-scale industrial production.
本发明解决其技术问题采用以下的技术方案:The present invention solves its technical problem and adopts the following technical solutions:
一种高体积分数SiC增强Al基复合材料的制备方法,包括以下步骤:A method for preparing a high volume fraction SiC reinforced Al-based composite material, comprising the following steps:
(1)碳化硅粉体表面处理:(1) Surface treatment of silicon carbide powder:
将碳化硅粉末在去离子水中超声振动30-60分钟,除去碳化硅表面的杂质和油污,然后进行干燥处理,先在150-200℃烘箱中干燥10-12小时,将干燥后的碳化硅放到刚玉坩埚中,再放入高温炉中,在1000-1200℃的温度下保温2-4小时,升温速度2-5℃/min,使其表面形成一层致密的SiO2层,然后随炉冷却。Ultrasonic vibration of silicon carbide powder in deionized water for 30-60 minutes to remove impurities and oil stains on the surface of silicon carbide, and then dry it in an oven at 150-200°C for 10-12 hours, then put the dried silicon carbide Put it into a corundum crucible, then put it into a high-temperature furnace, keep it warm at a temperature of 1000-1200 ° C for 2-4 hours, and the heating rate is 2-5 ° C / min, so that a dense SiO2 layer is formed on the surface, and then with the furnace cool down.
(2)混料:(2) Mixing:
向氧化处理后的碳化硅粉体中加入铝合金粉末,其中碳化硅粉体占混合粉末的体积分数为30-50%,铝合金粉末占混合粉末的体积分数为50-70%,将混合原料置于滚筒式混料机中混12-15小时,转速为180r/min,得到均匀性良好的混合粉末;Add aluminum alloy powder to the oxidized silicon carbide powder, wherein the silicon carbide powder accounts for 30-50% of the volume fraction of the mixed powder, and the aluminum alloy powder accounts for 50-70% of the volume fraction of the mixed powder, and the mixed raw materials Mix in a drum mixer for 12-15 hours at a speed of 180r/min to obtain a mixed powder with good uniformity;
(3)高速压制成型:(3) High-speed compression molding:
采用重力势能作为蓄能方式,将步骤(2)制得的混合粉末高速压制实验机压制生坯,重锤重量的为50-100Kg,将重锤的升至0.2-1.0m的高处,通过调节重锤质量和压制高度改变压制能量,通过重锤的自由落体运动压制混合粉体,得到SiC增强Al基复合材料压坯;Using the gravitational potential energy as the energy storage method, the mixed powder obtained in step (2) is pressed into a green body by a high-speed compaction test machine, the weight of the weight is 50-100Kg, and the weight is raised to a height of 0.2-1.0m, and passed Adjust the quality of the hammer and the pressing height to change the pressing energy, and press the mixed powder through the free fall movement of the weight to obtain a SiC-reinforced Al-based composite compact;
(4)N2气氛保护烧结:(4) N 2 atmosphere protection sintering:
将SiC增强Al基复合材料压坯放置管式气氛炉中,设置烧结温度为680-720℃,N2气氛下保护烧结,升温速率3-4℃/min,到达预定烧结温度后保温2-3小时,得到SiC增强Al基复合材料预成品;Put the SiC-reinforced Al-based composite compact in a tubular atmosphere furnace, set the sintering temperature to 680-720°C, protect the sintering under N2 atmosphere, and heat up at a rate of 3-4°C/min. hour, obtain the SiC reinforced Al-based composite material pre-finished product;
(5)冷却:(5) cooling:
通过管式气氛炉控制SiC增强Al基复合材料预成品降温冷却至400-450℃,冷却速率2-3℃/min,保温1-3小时,随炉冷却,待其冷却至室温,取出样品,去除附着在样品表面的铝合金和氧化层,得到SiC颗粒增强Al基复合材料成品。Control the SiC reinforced Al-based composite material pre-finished product to cool down to 400-450°C through a tube-type atmosphere furnace, the cooling rate is 2-3°C/min, keep the temperature for 1-3 hours, and cool with the furnace. After it cools to room temperature, take out the sample. The aluminum alloy and oxide layer attached to the surface of the sample are removed to obtain the finished SiC particle reinforced Al-based composite material.
上述步骤(1)中,SiC颗粒粒径为5-40um。In the above step (1), the particle size of the SiC particles is 5-40um.
上述步骤(2)中,所述铝合金粉末为6061铝合金粉末,6061铝合金粉末的粒径为1-20um。In the above step (2), the aluminum alloy powder is 6061 aluminum alloy powder, and the particle size of the 6061 aluminum alloy powder is 1-20um.
上述步骤(3)中,高速压制为一次压制成型,使用硬脂酸锌润滑模具内壁,压坯压制后无分层或缺角,单次压制后,SiC颗粒增强Al压坯相对密度为85-92%。In the above step (3), the high-speed pressing is one-time pressing molding, and zinc stearate is used to lubricate the inner wall of the mold. After the compact is pressed, there is no delamination or missing corners. After a single pressing, the relative density of the SiC particle-reinforced Al compact is 85- 92%.
上述步骤(4)中,将压坯放在刚玉烧舟中,其上下表面覆盖2-3mm厚6061铝合金粉。烧结之前,管式气氛炉先通入0.5-1小时的N2以排除残余空气,防止压坯被氧化。In the above step (4), the compact is placed in a corundum burning boat, and its upper and lower surfaces are covered with 2-3mm thick 6061 aluminum alloy powder. Before sintering, the tube atmosphere furnace is fed with N 2 for 0.5-1 hour to remove residual air and prevent the green compact from being oxidized.
上述步骤(5)中,去除样品表面的铝合金和氧化层厚度为2-3mm。In the above step (5), the thickness of the aluminum alloy and oxide layer removed from the surface of the sample is 2-3 mm.
本发明方法制备的SiC增强Al基复合材料的技术参数为:致密率为94.0%-98.0%,热导率为150-190W/mK。The technical parameters of the SiC-reinforced Al-based composite material prepared by the method of the invention are: the density rate is 94.0%-98.0%, and the thermal conductivity is 150-190W/mK.
本发明方法制备的SiC增强Al基复合材料,可应用于航空航天、大规模集成电路、军事电子器材领域。The SiC reinforced Al-based composite material prepared by the method of the invention can be applied to the fields of aerospace, large-scale integrated circuits, and military electronic equipment.
本发明的基本机理为:在高速压制过程中,混合粉末主要以填充和变形方式进行致密化。同时碳化硅在高速碰撞时发生了碎化,填充到颗粒之间的间隙,进一步提高了压坯的致密度,在高速碰撞、摩擦过程中破坏了铝合金粉表面的氧化层,形成冷焊的界面和新鲜的表面,有利于烧结过程中的致密化。因此在压制阶段就可以得到相对密度较高的压坯。在烧结温度为680-720℃,N2气氛保护下,SiC颗粒表面的SiO2氧化层与融熔Al在界面处发生了有利于SiC颗粒增强Al基复合材料界面结合的反应:2Al+SiO2+Mg=MgAl2O4+Si,从而提高SiC颗粒增强Al基复合材料的力学性能,且反应产物中的Si填充到烧结坯中的间隙,降低其孔隙率,使材料的致密度增加。最终制备出高强度、高致密度、高体积分数的SiC颗粒增强Al基复合材料。The basic mechanism of the invention is: in the high-speed pressing process, the mixed powder is mainly densified by filling and deformation. At the same time, silicon carbide is fragmented during high-speed collision, filling the gap between particles, further improving the compactness of the compact, and destroying the oxide layer on the surface of aluminum alloy powder during high-speed collision and friction, forming a cold weld The interface and fresh surface are favorable for densification during sintering. Therefore, a compact with relatively high density can be obtained in the pressing stage. At a sintering temperature of 680-720°C under the protection of N 2 atmosphere, the SiO 2 oxide layer on the surface of SiC particles and molten Al react at the interface, which is beneficial to the interface bonding of SiC particles to strengthen the Al-based composite material: 2Al+SiO2+ Mg=MgAl 2 O 4 +Si, thereby improving the mechanical properties of the SiC particle reinforced Al-based composite material, and the Si in the reaction product fills the gap in the sintered body, reduces its porosity, and increases the density of the material. Finally, SiC particle-reinforced Al matrix composites with high strength, high density and high volume fraction were prepared.
本发明与现有技术相比,具有以下的有益效果:Compared with the prior art, the present invention has the following beneficial effects:
1、采用高速压制的方法压制SiC颗粒增强Al基复合材料,有效的提高了压坯的相对密度。由于压坯的高密度可以缩短烧结时间,所以进一步有利于晶粒度的控制,进而提升制品的性能,并降低了成本。整个高速压制过程可以实现全自动化,极大地提高了生产效率。1. The SiC particle-reinforced Al-based composite material is pressed by high-speed pressing, which effectively increases the relative density of the compact. Since the high density of the compact can shorten the sintering time, it is further beneficial to the control of the grain size, thereby improving the performance of the product and reducing the cost. The entire high-speed pressing process can be fully automated, which greatly improves production efficiency.
2、制备工艺简单,在所制备的SiC颗粒增强Al基复合材料中SiC颗粒的相对密度高、增强体在A1基中分布均匀、体积分数较大、烧结温度低、制作成本低廉。2. The preparation process is simple. In the prepared SiC particle reinforced Al-based composite material, the relative density of SiC particles is high, the reinforcement is evenly distributed in the Al matrix, the volume fraction is large, the sintering temperature is low, and the production cost is low.
3、最终制备出致密率为致密率为94.0%-98.0%,热导率为150-190W/mK、体积分数为50%的SiC颗粒增强Al基复合材料。3. Finally, a SiC particle-reinforced Al-based composite material with a density rate of 94.0%-98.0%, a thermal conductivity of 150-190W/mK, and a volume fraction of 50% is finally prepared.
目前,国内外大量的研究基本集中无压渗透法制备中高体积分数的SiC增强Al基复合材料的研究开发上,制备出的材料性能优良,可以满足先进电子构件的轻量化、高功率密度、高可靠性和长寿命设计要求,但是设备成本高、工艺复杂限制了高体积分数的SiC增强Al基复合材料的应用。采用粉末冶金法(高速压制+无压烧结)可低成本高效率制备高体积分数SiC增强Al基复合材料,性能可以满足设计要求。使高体积分数SiC增强Al基复合材料在航空航天、大规模集成电路、军事电子器材有更广阔的应用前景。At present, a large number of researches at home and abroad basically focus on the research and development of SiC reinforced Al-based composite materials with medium and high volume fractions prepared by pressureless infiltration method. The prepared materials have excellent performance and can meet the requirements of light weight, high power density and high Reliability and long-life design requirements, but high equipment costs and complex processes limit the application of SiC-reinforced Al-based composites with high volume fractions. The powder metallurgy method (high-speed pressing + pressureless sintering) can be used to prepare high-volume SiC-reinforced Al-based composites at low cost and high efficiency, and the performance can meet the design requirements. The high volume fraction SiC reinforced Al-based composite material has a broader application prospect in aerospace, large-scale integrated circuits, and military electronic equipment.
与背景技术中的其他方法相比,本发明的高速压制-无压烧结法制备工艺简单,高速压制技术使复合粉末压坯制备时间大大缩短,制备出的压坯密度高且分布均匀,有利于烧结过程中的复合的致密化使所制的SiC增强A1基复合材料孔隙率较低、导热性能好,该工艺生产效率高、成本低,促进了SiC增强A1基复合材料的大规模应用。Compared with other methods in the background technology, the preparation process of the high-speed pressing-pressureless sintering method of the present invention is simple, and the high-speed pressing technology greatly shortens the preparation time of the composite powder compact, and the prepared compact has high density and uniform distribution, which is beneficial to The densification of the compound during the sintering process makes the prepared SiC-reinforced A1-based composite material have low porosity and good thermal conductivity. This process has high production efficiency and low cost, which promotes the large-scale application of SiC-reinforced A1-based composite material.
附图说明Description of drawings
图1是本发明材料中实施例4制备的SiC颗粒增强Al基复合材料样品金相图谱;Fig. 1 is the metallographic spectrum of the SiC particle reinforced Al-based composite material sample prepared in Example 4 of the material of the present invention;
图2是本发明材料中实施例4制备SiC颗粒增强Al基复合材料样品SEM图谱。Fig. 2 is the SEM spectrum of the SiC particle-reinforced Al-based composite material sample prepared in Example 4 of the material of the present invention.
具体实施方式detailed description
下面结合实施例及附图对本发明作进一步说明,但不限定本发明。The present invention will be further described below in conjunction with the embodiments and accompanying drawings, but the present invention is not limited.
实施例1:Example 1:
一种高体积分数SiC增强Al基复合材料的制备方法,包括以下步骤:A method for preparing a high volume fraction SiC reinforced Al-based composite material, comprising the following steps:
(1)碳化硅粉体表面处理:(1) Surface treatment of silicon carbide powder:
将碳化硅粉末在去离子水中超声振动45分钟,除去碳化硅表面的杂质和油污,然后进行干燥处理,先在200℃烘箱中干燥12小时,将干燥后的碳化硅放到刚玉坩埚中,再放入高温炉中,在1200℃的温度下保温2小时,升温速度5℃/min,使其表面形成一层致密的SiO2层,然后随炉冷却。Ultrasonic vibration of silicon carbide powder in deionized water for 45 minutes to remove impurities and oil stains on the surface of silicon carbide, and then dry it in an oven at 200°C for 12 hours, put the dried silicon carbide into a corundum crucible, and then Put it into a high-temperature furnace, keep it warm at 1200°C for 2 hours, and heat up at a rate of 5°C/min to form a dense SiO2 layer on the surface, and then cool with the furnace.
(2)混料:(2) Mixing:
向氧化处理后的碳化硅粉体中加入6061铝合金粉末,其中碳化硅粉体占混合粉末的体积分数为40%,6061铝合金粉末占混合粉末的体积分数为60%,将混合原料置于滚筒式混料机中混12小时,转速为180r/min,得到均匀性良好的混合粉末;Add 6061 aluminum alloy powder to the oxidized silicon carbide powder, wherein the silicon carbide powder accounts for 40% of the volume fraction of the mixed powder, and the 6061 aluminum alloy powder accounts for 60% of the volume fraction of the mixed powder, and the mixed raw material is placed in Mix in a drum mixer for 12 hours at a speed of 180r/min to obtain a mixed powder with good uniformity;
(3)高速压制成型:(3) High-speed compression molding:
采用重力势能作为蓄能方式,将步骤(2)制得的混合粉末高速压制实验机压制生坯,重锤重量的为50Kg,将重锤的升至0.2m的高处,通过调节重锤质量和压制高度改变压制能量,通过重锤的自由落体运动压制混合粉体,得到SiC增强Al基复合材料压坯;Adopt gravitational potential energy as the energy storage method, press the mixed powder high-speed compaction test machine that step (2) makes green body, the weight of the weight is 50Kg, the height of the weight is raised to 0.2m, by adjusting the weight of the weight Change the pressing energy with the pressing height, and press the mixed powder through the free fall motion of the weight to obtain a SiC-reinforced Al-based composite compact;
(4)N2气氛保护烧结:(4) N 2 atmosphere protection sintering:
将SiC增强Al基复合材料压坯放置管式气氛炉中,设置烧结温度为700℃,N2气氛下保护烧结,升温速率3℃/min,到达预定烧结温度后保温2小时,得到SiC增强Al基复合材料预成品;Place the SiC-reinforced Al-based composite compact in a tubular atmosphere furnace, set the sintering temperature to 700 °C, protect the sintering under N2 atmosphere, and heat up at a rate of 3 °C/min. After reaching the predetermined sintering temperature, keep it for 2 hours to obtain SiC-enhanced Al matrix composite pre-finished products;
(5)冷却:(5) cooling:
通过管式气氛炉控制SiC增强Al基复合材料预成品降温冷却至400℃,冷却速率2℃/min,保温2小时,随炉冷却,待其冷却至室温,取出样品,去除附着在样品表面的铝合金和氧化层,得到SiC颗粒增强Al基复合材料成品。Control the pre-finished product of SiC-reinforced Al-based composite material through a tube-type atmosphere furnace to cool down to 400°C, with a cooling rate of 2°C/min, keep warm for 2 hours, and cool with the furnace. After cooling to room temperature, take out the sample and remove the particles attached to the surface of the sample aluminum alloy and an oxide layer to obtain a SiC particle reinforced Al-based composite material finished product.
上述步骤(1)中,SiC颗粒粒径为5-40um。In the above step (1), the particle size of the SiC particles is 5-40um.
上述步骤(2)中,所述铝合金粉末为6061铝合金粉末,6061铝合金粉末的粒径为1-20um。In the above step (2), the aluminum alloy powder is 6061 aluminum alloy powder, and the particle size of the 6061 aluminum alloy powder is 1-20um.
上述步骤(3)中,高速压制为一次压制成型,使用硬脂酸锌润滑模具内壁,压坯压制后无分层或缺角,单次压制后,SiC颗粒增强Al压坯相对密度为88.4%。In the above step (3), the high-speed pressing is one-time pressing molding, using zinc stearate to lubricate the inner wall of the mold, and there is no delamination or missing corners after pressing the green compact. After a single pressing, the relative density of the SiC particle-reinforced Al green compact is 88.4%. .
上述步骤(4)中,将压坯放在刚玉烧舟中,其上下表面覆盖2-3mm厚6061铝合金粉。烧结之前,管式气氛炉先通入1小时的N2以排除残余空气,防止压坯被氧化。In the above step (4), the compact is placed in a corundum burning boat, and its upper and lower surfaces are covered with 2-3mm thick 6061 aluminum alloy powder. Before sintering, the tube atmosphere furnace was fed with N2 for 1 hour to remove residual air and prevent the green compact from being oxidized.
上述步骤(5)中,去除样品表面的铝合金和氧化层厚度为2-3mm。In the above step (5), the thickness of the aluminum alloy and oxide layer removed from the surface of the sample is 2-3 mm.
实验测试:Experimental test:
所得到的SiC颗粒增强Al基复合材料成品的致密率为96.32%,热导率为157.9W/mK。The densification rate of the obtained SiC particle-reinforced Al-based composite material is 96.32%, and the thermal conductivity is 157.9 W/mK.
实施例2:Example 2:
一种高体积分数SiC增强Al基复合材料的制备方法,包括以下步骤:A method for preparing a high volume fraction SiC reinforced Al-based composite material, comprising the following steps:
(1)碳化硅粉体表面处理:(1) Surface treatment of silicon carbide powder:
将碳化硅粉末在去离子水中超声振动45分钟,除去碳化硅表面的杂质和油污,然后进行干燥处理,先在200℃烘箱中干燥12小时,将干燥后的碳化硅放到刚玉坩埚中,再放入高温炉中,在1200℃的温度下保温2小时,升温速度5℃/min,使其表面形成一层致密的SiO2层,然后随炉冷却。Ultrasonic vibration of silicon carbide powder in deionized water for 45 minutes to remove impurities and oil stains on the surface of silicon carbide, and then dry it in an oven at 200°C for 12 hours, put the dried silicon carbide into a corundum crucible, and then Put it into a high-temperature furnace, keep it warm at 1200°C for 2 hours, and heat up at a rate of 5°C/min to form a dense SiO2 layer on the surface, and then cool with the furnace.
(2)混料:(2) Mixing:
向氧化处理后的碳化硅粉体中加入6061铝合金粉末,其中碳化硅粉体占混合粉末的体积分数为50%,6061铝合金粉末占混合粉末的体积分数为50%,将混合原料置于滚筒式混料机中混12小时,转速为180r/min,得到均匀性良好的混合粉末;Add 6061 aluminum alloy powder to the silicon carbide powder after the oxidation treatment, wherein the silicon carbide powder accounts for 50% of the volume fraction of the mixed powder, and the 6061 aluminum alloy powder accounts for 50% of the volume fraction of the mixed powder, and the mixed raw material is placed in Mix in a drum mixer for 12 hours at a speed of 180r/min to obtain a mixed powder with good uniformity;
(3)高速压制成型:(3) High-speed compression molding:
采用重力势能作为蓄能方式,将步骤(2)制得的混合粉末高速压制实验机压制生坯,重锤重量的为50Kg,将重锤的升至0.3m的高处,通过调节重锤质量和压制高度改变压制能量,通过重锤的自由落体运动压制混合粉体,得到SiC增强Al基复合材料压坯;Adopt gravitational potential energy as the energy storage mode, press the mixed powder high-speed compaction test machine that step (2) makes into green body, the weight of the weight is 50Kg, the height of the weight is raised to 0.3m, by adjusting the weight of the weight Change the pressing energy with the pressing height, and press the mixed powder through the free fall motion of the weight to obtain a SiC-reinforced Al-based composite compact;
(4)N2气氛保护烧结:(4) N 2 atmosphere protection sintering:
将SiC增强Al基复合材料压坯放置管式气氛炉中,设置烧结温度为680℃,N2气氛下保护烧结,升温速率3℃/min,到达预定烧结温度后保温2小时,得到SiC增强Al基复合材料预成品;Place the SiC-reinforced Al-based composite compact in a tubular atmosphere furnace, set the sintering temperature to 680°C, protect the sintering under N2 atmosphere, and heat up at a rate of 3°C/min. After reaching the predetermined sintering temperature, keep it for 2 hours to obtain SiC-reinforced Al matrix composite pre-finished products;
(5)冷却:(5) cooling:
通过管式气氛炉控制SiC增强Al基复合材料预成品降温冷却至400℃,冷却速率2℃/min,保温2小时,随炉冷却,待其冷却至室温,取出样品,去除附着在样品表面的铝合金和氧化层,得到SiC颗粒增强Al基复合材料成品。Control the pre-finished product of SiC-reinforced Al-based composite material through a tube-type atmosphere furnace to cool down to 400°C, with a cooling rate of 2°C/min, keep warm for 2 hours, and cool with the furnace. After cooling to room temperature, take out the sample and remove the particles attached to the surface of the sample aluminum alloy and an oxide layer to obtain a SiC particle reinforced Al-based composite material finished product.
上述步骤(1)中,SiC颗粒粒径为5-40um。In the above step (1), the particle size of the SiC particles is 5-40um.
上述步骤(2)中,所述铝合金粉末为6061铝合金粉末,6061铝合金粉末的粒径为1-20um。In the above step (2), the aluminum alloy powder is 6061 aluminum alloy powder, and the particle size of the 6061 aluminum alloy powder is 1-20um.
上述步骤(3)中,高速压制为一次压制成型,使用硬脂酸锌润滑模具内壁,压坯压制后无分层或缺角,单次压制后,SiC颗粒增强Al压坯相对密度为88.4%。In the above step (3), the high-speed pressing is one-time pressing molding, using zinc stearate to lubricate the inner wall of the mold, and there is no delamination or missing corners after pressing the green compact. After a single pressing, the relative density of the SiC particle-reinforced Al green compact is 88.4%. .
上述步骤(4)中,将压坯放在刚玉烧舟中,其上下表面覆盖2-3mm厚6061铝合金粉。烧结之前,管式气氛炉先通入1小时的N2以排除残余空气,防止压坯被氧化。In the above step (4), the compact is placed in a corundum burning boat, and its upper and lower surfaces are covered with 2-3mm thick 6061 aluminum alloy powder. Before sintering, the tube atmosphere furnace was fed with N2 for 1 hour to remove residual air and prevent the green compact from being oxidized.
上述步骤(5)中,去除样品表面的铝合金和氧化层厚度为2-3mm。In the above step (5), the thickness of the aluminum alloy and oxide layer removed from the surface of the sample is 2-3mm.
实验测试:Experimental test:
所得到的SiC颗粒增强Al基复合材料成品的致密率为94.59%,热导率为165.7W/mK。The densification rate of the obtained SiC particle-reinforced Al-based composite material is 94.59%, and the thermal conductivity is 165.7W/mK.
实施例3:Example 3:
一种高体积分数SiC增强Al基复合材料的制备方法,包括以下步骤:A method for preparing a high volume fraction SiC reinforced Al-based composite material, comprising the following steps:
(1)碳化硅粉体表面处理:(1) Surface treatment of silicon carbide powder:
将碳化硅粉末在去离子水中超声振动45分钟,除去碳化硅表面的杂质和油污,然后进行干燥处理,先在200℃烘箱中干燥12小时,将干燥后的碳化硅放到刚玉坩埚中,再放入高温炉中,在1200℃的温度下保温2小时,升温速度5℃/min,使其表面形成一层致密的SiO2层,然后随炉冷却。Ultrasonic vibration of silicon carbide powder in deionized water for 45 minutes to remove impurities and oil stains on the surface of silicon carbide, and then dry it in an oven at 200°C for 12 hours, put the dried silicon carbide into a corundum crucible, and then Put it into a high-temperature furnace, keep it warm at 1200°C for 2 hours, and heat up at a rate of 5°C/min to form a dense SiO2 layer on the surface, and then cool with the furnace.
(2)混料:(2) Mixing:
向氧化处理后的碳化硅粉体中加入6061铝合金粉末,其中碳化硅粉体占混合粉末的体积分数为50%,6061铝合金粉末占混合粉末的体积分数为50%,将混合原料置于滚筒式混料机中混12小时,转速为180r/min,得到均匀性良好的混合粉末;Add 6061 aluminum alloy powder to the silicon carbide powder after the oxidation treatment, wherein the silicon carbide powder accounts for 50% of the volume fraction of the mixed powder, and the 6061 aluminum alloy powder accounts for 50% of the volume fraction of the mixed powder, and the mixed raw material is placed in Mix in a drum mixer for 12 hours at a speed of 180r/min to obtain a mixed powder with good uniformity;
(3)高速压制成型:(3) High-speed compression molding:
采用重力势能作为蓄能方式,将步骤(2)制得的混合粉末高速压制实验机压制生坯,重锤重量的为50Kg,将重锤的升至0.3m的高处,通过调节重锤质量和压制高度改变压制能量,通过重锤的自由落体运动压制混合粉体,得到SiC增强Al基复合材料压坯;Adopt gravitational potential energy as the energy storage mode, press the mixed powder high-speed compaction test machine that step (2) makes into green body, the weight of the weight is 50Kg, the height of the weight is raised to 0.3m, by adjusting the weight of the weight Change the pressing energy with the pressing height, and press the mixed powder through the free fall motion of the weight to obtain a SiC-reinforced Al-based composite compact;
(4)N2气氛保护烧结:(4) N 2 atmosphere protection sintering:
将SiC增强Al基复合材料压坯放置管式气氛炉中,设置烧结温度为700℃,N2气氛下保护烧结,升温速率3℃/min,到达预定烧结温度后保温2小时,得到SiC增强Al基复合材料预成品;Place the SiC-reinforced Al-based composite compact in a tubular atmosphere furnace, set the sintering temperature to 700 °C, protect the sintering under N2 atmosphere, and heat up at a rate of 3 °C/min. After reaching the predetermined sintering temperature, keep it for 2 hours to obtain SiC-enhanced Al matrix composite pre-finished products;
(5)冷却:(5) cooling:
通过管式气氛炉控制SiC增强Al基复合材料预成品降温冷却至400℃,冷却速率2℃/min,保温2小时,随炉冷却,待其冷却至室温,取出样品,去除附着在样品表面的铝合金和氧化层,得到SiC颗粒增强Al基复合材料成品。Control the pre-finished product of SiC-reinforced Al-based composite material through a tube-type atmosphere furnace to cool down to 400°C, with a cooling rate of 2°C/min, keep warm for 2 hours, and cool with the furnace. After cooling to room temperature, take out the sample and remove the particles attached to the surface of the sample aluminum alloy and an oxide layer to obtain a SiC particle reinforced Al-based composite material finished product.
上述步骤(1)中,SiC颗粒粒径为5-40um。In the above step (1), the particle size of the SiC particles is 5-40um.
上述步骤(2)中,所述铝合金粉末为6061铝合金粉末,6061铝合金粉末的粒径为1-20um。In the above step (2), the aluminum alloy powder is 6061 aluminum alloy powder, and the particle size of the 6061 aluminum alloy powder is 1-20um.
上述步骤(3)中,高速压制为一次压制成型,使用硬脂酸锌润滑模具内壁,压坯压制后无分层或缺角,单次压制后,SiC颗粒增强Al压坯相对密度为89.6%。In the above step (3), the high-speed pressing is one-time pressing molding, and zinc stearate is used to lubricate the inner wall of the mold. After the compact is pressed, there is no delamination or missing corners. After a single pressing, the relative density of the SiC particle-reinforced Al compact is 89.6%. .
上述步骤(4)中,将压坯放在刚玉烧舟中,其上下表面覆盖2-3mm厚6061铝合金粉。烧结之前,管式气氛炉先通入1小时的N2以排除残余空气,防止压坯被氧化。In the above step (4), the compact is placed in a corundum burning boat, and its upper and lower surfaces are covered with 2-3mm thick 6061 aluminum alloy powder. Before sintering, the tube atmosphere furnace was fed with N2 for 1 hour to remove residual air and prevent the green compact from being oxidized.
上述步骤(5)中,去除样品表面的铝合金和氧化层厚度为2-3mm。In the above step (5), the thickness of the aluminum alloy and oxide layer removed from the surface of the sample is 2-3 mm.
本实施例所得到的SiC颗粒增强Al基复合材料成品的致密率为96.11%,热导率为170.5W/mK。The densification rate of the finished SiC particle-reinforced Al-based composite material obtained in this example is 96.11%, and the thermal conductivity is 170.5 W/mK.
实施例4:Example 4:
一种高体积分数SiC增强Al基复合材料的制备方法,包括以下步骤:A method for preparing a high volume fraction SiC reinforced Al-based composite material, comprising the following steps:
(1)碳化硅粉体表面处理:(1) Surface treatment of silicon carbide powder:
将碳化硅粉末在去离子水中超声振动45分钟,除去碳化硅表面的杂质和油污,然后进行干燥处理,先在200℃烘箱中干燥12小时,将干燥后的碳化硅放到刚玉坩埚中,再放入高温炉中,在1200℃的温度下保温2小时,升温速度5℃/min,使其表面形成一层致密的SiO2层,然后随炉冷却。Ultrasonic vibration of silicon carbide powder in deionized water for 45 minutes to remove impurities and oil stains on the surface of silicon carbide, and then dry it in an oven at 200°C for 12 hours, put the dried silicon carbide into a corundum crucible, and then Put it into a high-temperature furnace, keep it warm at 1200°C for 2 hours, and heat up at a rate of 5°C/min to form a dense SiO2 layer on the surface, and then cool with the furnace.
(2)混料:(2) Mixing:
向氧化处理后的碳化硅粉体中加入6061铝合金粉末,其中碳化硅粉体占混合粉末的体积分数为50%,6061铝合金粉末占混合粉末的体积分数为50%,将混合原料置于滚筒式混料机中混12小时,转速为180r/min,得到均匀性良好的混合粉末;Add 6061 aluminum alloy powder to the silicon carbide powder after the oxidation treatment, wherein the silicon carbide powder accounts for 50% of the volume fraction of the mixed powder, and the 6061 aluminum alloy powder accounts for 50% of the volume fraction of the mixed powder, and the mixed raw material is placed in Mix in a drum mixer for 12 hours at a speed of 180r/min to obtain a mixed powder with good uniformity;
(3)高速压制成型:(3) High-speed compression molding:
采用重力势能作为蓄能方式,将步骤(2)制得的混合粉末高速压制实验机压制生坯,重锤重量的为50Kg,将重锤的升至0.8m的高处,通过调节重锤质量和压制高度改变压制能量,通过重锤的自由落体运动压制混合粉体,得到SiC增强Al基复合材料压坯;Adopt gravitational potential energy as energy storage mode, the mixed powder high-speed compaction test machine that step (2) makes is pressed green body, and the heavy hammer weight is 50Kg, and the heavy hammer is raised to the height of 0.8m, by adjusting the heavy hammer quality Change the pressing energy with the pressing height, and press the mixed powder through the free fall motion of the weight to obtain a SiC-reinforced Al-based composite compact;
(4)N2气氛保护烧结:(4) N 2 atmosphere protection sintering:
将SiC增强Al基复合材料压坯放置管式气氛炉中,设置烧结温度为700℃,N2气氛下保护烧结,升温速率3℃/min,到达预定烧结温度后保温2小时,得到SiC增强Al基复合材料预成品;Place the SiC-reinforced Al-based composite compact in a tubular atmosphere furnace, set the sintering temperature to 700 °C, protect the sintering under N2 atmosphere, and heat up at a rate of 3 °C/min. After reaching the predetermined sintering temperature, keep it for 2 hours to obtain SiC-enhanced Al matrix composite pre-finished products;
(5)冷却:(5) cooling:
通过管式气氛炉控制SiC增强Al基复合材料预成品降温冷却至400℃,冷却速率2℃/min,保温2小时,随炉冷却,待其冷却至室温,取出样品,去除附着在样品表面的铝合金和氧化层,得到SiC颗粒增强Al基复合材料成品。Control the pre-finished product of SiC-reinforced Al-based composite material through a tube-type atmosphere furnace to cool down to 400°C, with a cooling rate of 2°C/min, keep warm for 2 hours, and cool with the furnace. After cooling to room temperature, take out the sample and remove the particles attached to the surface of the sample aluminum alloy and an oxide layer to obtain a SiC particle reinforced Al-based composite material finished product.
上述步骤(1)中,SiC颗粒粒径为5-40um。In the above step (1), the particle size of the SiC particles is 5-40um.
上述步骤(2)中,所述铝合金粉末为6061铝合金粉末,6061铝合金粉末的粒径为1-20um。In the above step (2), the aluminum alloy powder is 6061 aluminum alloy powder, and the particle size of the 6061 aluminum alloy powder is 1-20um.
上述步骤(3)中,高速压制为一次压制成型,使用硬脂酸锌润滑模具内壁,压坯压制后无分层或缺角,单次压制后,SiC颗粒增强Al压坯相对密度为91.5%。In the above step (3), the high-speed pressing is one-time pressing molding, using zinc stearate to lubricate the inner wall of the mold, and there is no delamination or missing corners after pressing the green compact. After a single pressing, the relative density of the SiC particle-reinforced Al green compact is 91.5%. .
上述步骤(4)中,将压坯放在刚玉烧舟中,其上下表面覆盖2-3mm厚6061铝合金粉。烧结之前,管式气氛炉先通入1小时的N2以排除残余空气,防止压坯被氧化。In the above step (4), the compact is placed in a corundum burning boat, and its upper and lower surfaces are covered with 2-3mm thick 6061 aluminum alloy powder. Before sintering, the tube atmosphere furnace was fed with N2 for 1 hour to remove residual air and prevent the green compact from being oxidized.
上述步骤(5)中,去除样品表面的铝合金和氧化层厚度为2-3mm。In the above step (5), the thickness of the aluminum alloy and oxide layer removed from the surface of the sample is 2-3mm.
实验测试:Experimental test:
本实施例所得到的SiC颗粒增强Al基复合材料成品的致密率为97.61%,热导率为174.9W/mK。The densification rate of the finished SiC particle reinforced Al-based composite material obtained in this embodiment is 97.61%, and the thermal conductivity is 174.9 W/mK.
图1是实施例4制备的SiC颗粒增强Al基复合材料样品金相图谱,可以看出碳化硅均匀的分布在基体中且空隙较少。Figure 1 is the metallographic spectrum of the SiC particle-reinforced Al-based composite material sample prepared in Example 4. It can be seen that silicon carbide is uniformly distributed in the matrix with fewer voids.
图2是实施例4制备50%SiC颗粒增强Al基复合材料样品SEM图谱,断口形貌表明,碳化硅的断裂方式为解理断裂,基体为韧性断裂。Figure 2 is the SEM spectrum of the 50% SiC particle-reinforced Al-based composite material sample prepared in Example 4. The fracture morphology shows that the fracture mode of silicon carbide is cleavage fracture, and the matrix is ductile fracture.
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CN113755719A (en) * | 2021-08-09 | 2021-12-07 | 昆明理工大学 | High-strength, wear-resistant and antifriction aluminum-based composite material and preparation method thereof |
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