CN106086500B - A kind of method for preparing the continuous reinforced Al matrix composite of in-situ three-dimensional - Google Patents
A kind of method for preparing the continuous reinforced Al matrix composite of in-situ three-dimensional Download PDFInfo
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- 239000002131 composite material Substances 0.000 title claims abstract description 43
- 238000011065 in-situ storage Methods 0.000 title claims abstract description 31
- 238000000034 method Methods 0.000 title claims abstract description 26
- 239000011159 matrix material Substances 0.000 title abstract description 11
- 239000000843 powder Substances 0.000 claims abstract description 30
- 239000011812 mixed powder Substances 0.000 claims abstract description 22
- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical compound [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 claims abstract description 13
- 238000006243 chemical reaction Methods 0.000 claims abstract description 8
- 239000000155 melt Substances 0.000 claims abstract description 6
- 238000000227 grinding Methods 0.000 claims abstract description 4
- 239000002245 particle Substances 0.000 claims description 24
- 230000002787 reinforcement Effects 0.000 claims description 13
- 229910000831 Steel Inorganic materials 0.000 claims description 9
- 239000010959 steel Substances 0.000 claims description 9
- 239000011521 glass Substances 0.000 claims description 7
- 239000004570 mortar (masonry) Substances 0.000 claims description 7
- 230000035484 reaction time Effects 0.000 claims description 2
- 238000001816 cooling Methods 0.000 abstract 1
- 239000000758 substrate Substances 0.000 abstract 1
- 238000002360 preparation method Methods 0.000 description 7
- 238000004880 explosion Methods 0.000 description 3
- 230000007547 defect Effects 0.000 description 2
- 238000005470 impregnation Methods 0.000 description 2
- 230000008595 infiltration Effects 0.000 description 2
- 238000001764 infiltration Methods 0.000 description 2
- 238000002156 mixing Methods 0.000 description 2
- 239000011148 porous material Substances 0.000 description 2
- 238000003825 pressing Methods 0.000 description 2
- 229910000838 Al alloy Inorganic materials 0.000 description 1
- 238000002679 ablation Methods 0.000 description 1
- 238000000498 ball milling Methods 0.000 description 1
- 230000009286 beneficial effect Effects 0.000 description 1
- 238000004512 die casting Methods 0.000 description 1
- 230000000694 effects Effects 0.000 description 1
- 238000001125 extrusion Methods 0.000 description 1
- 239000000835 fiber Substances 0.000 description 1
- 238000011049 filling Methods 0.000 description 1
- 238000005429 filling process Methods 0.000 description 1
- 239000006260 foam Substances 0.000 description 1
- 238000004519 manufacturing process Methods 0.000 description 1
- 239000000463 material Substances 0.000 description 1
- 239000002184 metal Substances 0.000 description 1
- 238000000465 moulding Methods 0.000 description 1
- 239000002243 precursor Substances 0.000 description 1
- 230000035939 shock Effects 0.000 description 1
- 238000005245 sintering Methods 0.000 description 1
- 238000003980 solgel method Methods 0.000 description 1
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- C22—METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
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- C22C32/0052—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 carbides
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Abstract
Description
技术领域technical field
本发明属于先进金属基复合材料制备领域，具体涉及一种制备原位三维连续增强Al基复合材料的方法。The invention belongs to the field of preparation of advanced metal-based composite materials, and in particular relates to a method for preparing in-situ three-dimensional continuous reinforced Al-based composite materials.
背景技术Background technique
三维连续增强Al基复合材料又名网络交叉Al基复合材料，其增强体与Al基体在三维空间连续并相互贯通呈网络机构。此复合构型较传统颗粒、纤维增强Al基复合材料更有助于充分发挥增强体、基体性能。因此，三维连续增强Al基复合材料具有高强度、高硬度、良好的抗磨损性能和抗热震性能，较高的热导率，较低的热膨胀系数，在航空航天、汽车、电子、机械制造等领域具有广泛的应用前景。目前，三维连续增强Al基复合材料制备方法主要为预制件浸渗成型法，其一般包括多孔增强预制件制备与Al熔体填充两个步骤。多孔预制件可通过有机前驱体浸渍法、粉末烧结法、烧蚀法、泡沫塑料挂浆法、溶胶-凝胶法等制备，但以上方法往往存在制备工艺复杂、预制件强度较低等问题。另一方面，Al熔体填充过程中通常需借助浸渗、挤压、压铸等辅助工艺，且Al基体与增强体界面处易产生缺陷(裂纹、界面反应等)，进而影响复合材料使用性能。Three-dimensional continuous reinforced Al-based composites, also known as network crossed Al-based composites, the reinforcement and the Al matrix are continuous in three-dimensional space and interpenetrate to form a network structure. Compared with traditional particle and fiber reinforced Al-based composite materials, this composite configuration is more helpful to give full play to the performance of reinforcement and matrix. Therefore, three-dimensional continuous reinforced Al-based composites have high strength, high hardness, good wear resistance and thermal shock resistance, high thermal conductivity, low thermal expansion coefficient, and are widely used in aerospace, automotive, electronics, and mechanical manufacturing. and other fields have broad application prospects. At present, the preparation method of three-dimensional continuous reinforced Al-based composites is mainly the preform infiltration molding method, which generally includes two steps of porous reinforced preform preparation and Al melt filling. Porous preforms can be prepared by organic precursor impregnation method, powder sintering method, ablation method, foam hanging method, sol-gel method, etc., but the above methods often have problems such as complex preparation process and low preform strength. On the other hand, auxiliary processes such as impregnation, extrusion, and die-casting are usually used in the filling process of Al melt, and defects (cracks, interface reactions, etc.) are prone to occur at the interface between the Al matrix and the reinforcement, which will affect the performance of the composite material.
发明内容Contents of the invention
本发明的目的在于提供一种制备原位三维连续增强Al基复合材料的方法，以克服上述现有技术存在的缺陷，本发明利用Al-Ti-C体系热爆反应在Al熔体内原位内生三维连续增强体，实现原位三维连续增强Al基复合材料的简单快速制备。The purpose of the present invention is to provide a method for preparing in-situ three-dimensional continuous reinforced Al-based composite materials, so as to overcome the above-mentioned defects in the prior art. The endogenous three-dimensional continuous reinforcement realizes the simple and rapid preparation of in-situ three-dimensional continuous reinforced Al-based composites.
为达到上述目的，本发明采用如下技术方案：To achieve the above object, the present invention adopts the following technical solutions:
一种制备原位三维连续增强Al基复合材料的方法，包括以下步骤：A method for preparing an in-situ three-dimensional continuous reinforced Al-based composite material, comprising the following steps:
步骤1：将Ti粉、Al粉和石墨粉按照2:(1～1.2):1的摩尔比混合，然后研磨得到混合粉料；Step 1: Mix Ti powder, Al powder and graphite powder according to the molar ratio of 2:(1-1.2):1, and then grind to obtain mixed powder;
步骤2：将混合粉料放入模具中进行冷压得到生坯；Step 2: Put the mixed powder into a mold for cold pressing to obtain a green body;
步骤3：将生坯预热处理后加入到温度为700～900℃的Al熔体内，反应结束后将坯体从熔体内取出冷却，即得到原位三维连续增强Al基复合材料。Step 3: Add the green body to the Al melt at a temperature of 700-900° C. after preheating, and take the green body out of the melt to cool after the reaction, so as to obtain an in-situ three-dimensional continuous reinforced Al-based composite material.
进一步地，步骤1中Ti粉、Al粉和石墨粉的纯度均大于99％，粒度均≤100μm。Further, the purity of Ti powder, Al powder and graphite powder in step 1 is all greater than 99%, and the particle size is all ≤100 μm.
进一步地，步骤1中研磨时间为30～60min。Further, the grinding time in step 1 is 30-60 minutes.
进一步地，步骤2中模具为内径为10mm的圆柱形钢铁模具。Further, the mold in step 2 is a cylindrical steel mold with an inner diameter of 10mm.
进一步地，步骤2中进行冷压时，对模具中的混合粉料施加50～150MPa的径向压力，得到厚度为10～20mm的圆柱体生坯。Further, when performing cold pressing in step 2, a radial pressure of 50-150 MPa is applied to the mixed powder in the mold to obtain a cylindrical green body with a thickness of 10-20 mm.
进一步地，步骤3中生坯预热时的温度为700～900℃，时间为1～3min。Further, in step 3, the temperature during preheating of the green body is 700-900° C., and the time is 1-3 minutes.
进一步地，步骤3中反应时间为30～60s。Further, the reaction time in step 3 is 30-60s.
一种制备原位三维连续增强Al基复合材料的方法，包括以下步骤：A method for preparing an in-situ three-dimensional continuous reinforced Al-based composite material, comprising the following steps:
步骤1：将纯度大于99％，平均粒径为20μm的Ti粉、纯度大于99％，平均粒径为40μm的Al粉和纯度大于99％，平均粒径为40μm的石墨粉按照2:1:1的摩尔比混合，然后在玻璃研钵中充分研磨30min，得到混合粉料；Step 1: Ti powder with a purity greater than 99% and an average particle size of 20 μm, an Al powder with a purity greater than 99% and an average particle size of 40 μm, and a graphite powder with a purity greater than 99% and an average particle size of 40 μm according to 2:1: 1 molar ratio, and then fully ground in a glass mortar for 30 minutes to obtain a mixed powder;
步骤2：将混合粉料放入内径为10mm的圆柱形钢铁模具中，将其在130MPa的径向压力下冷压成厚度为15mm的圆柱体生坯；Step 2: Put the mixed powder into a cylindrical steel mold with an inner diameter of 10mm, and cold press it into a cylindrical green body with a thickness of 15mm under a radial pressure of 130MPa;
步骤3：将生坯在800℃的温度下预热2min，然后放入800℃的Al熔体内，静置45s后取出冷却，即得到原位三维连续增强Al基复合材料。Step 3: Preheat the green body at 800°C for 2 minutes, then put it into the Al melt at 800°C, let it stand for 45s, take it out and cool it, and then obtain the in-situ three-dimensional continuous reinforced Al-based composite material.
与现有技术相比，本发明具有以下有益的技术效果：Compared with the prior art, the present invention has the following beneficial technical effects:
本发明利用熔体内Al-Ti-C坯体热爆反应，能够在简单工艺下制备三维连续增强Al基复合材料。三维连续增强体在熔体内原位内生，省去了多孔预制体制备环节，且在多孔预制体生成过程中，Al熔体自发进入其孔径中，形成增强体与基体相互贯通网络结构的复合材料，且Al基体与增强体界面为冶金结合，而传统的浸渗工艺制备的三维连续增强Al基复合材料界面多为机械结合，故本发明方法中制备的复合材料界面结合强度更高。此外，通过改变初始反应粉末粒径、比例等，可实现原位三维增强体的可控设计。The invention utilizes the thermal explosion reaction of the Al-Ti-C body in the melt, and can prepare three-dimensional continuous reinforced Al-based composite materials under a simple process. The three-dimensional continuous reinforcement is in-situ grown in the melt, eliminating the need for the preparation of the porous preform, and during the generation of the porous preform, the Al melt spontaneously enters its pores to form a network structure in which the reinforcement and the matrix interpenetrate. Composite materials, and the interface between the Al matrix and the reinforcement is metallurgically bonded, while the interface of the three-dimensional continuous reinforced Al-based composite material prepared by the traditional infiltration process is mostly mechanically bonded, so the interface bond strength of the composite material prepared by the method of the present invention is higher. In addition, the controllable design of in-situ three-dimensional reinforcements can be realized by changing the initial reaction powder particle size, ratio, etc.
进一步地，选择纯度大于99％，粒度均≤100μm的Ti粉、Al粉和石墨粉可以保证熔体内热爆反应的充分进行。Furthermore, selecting Ti powder, Al powder and graphite powder with a purity greater than 99% and a particle size of ≤100 μm can ensure that the thermal explosion reaction in the melt proceeds fully.
进一步地，选择30-60min的混粉研磨时间，可保证粉末的充分混匀。Further, choosing a powder mixing and grinding time of 30-60 minutes can ensure sufficient mixing of the powder.
进一步地，选择50-150MPa径向压力，可保证制备过程中坯体具有足够强度。Further, choosing a radial pressure of 50-150 MPa can ensure that the green body has sufficient strength during the preparation process.
进一步地，选择700～900℃预热温度，可实现生坯的快速预热。Further, the rapid preheating of the green body can be realized by selecting the preheating temperature of 700-900°C.
附图说明Description of drawings
图1为实施例1中制备的原位三维连续增强Al基复合材料宏观照片；Fig. 1 is the macrophotograph of the in-situ three-dimensional continuously reinforced Al-based composite material prepared in Example 1;
图2为实施例1中制备的原位三维连续增强Al基复合材料微观组织形貌图，其中(a)为放大200倍下复合材料微观组织照片，(b)为放大3500倍下复合材料微观组织照片。Figure 2 is the microstructure morphology of the in-situ three-dimensional continuous reinforced Al-based composite material prepared in Example 1, where (a) is the microstructure photo of the composite material at 200 times magnification, and (b) is the microstructure photo of the composite material at 3500 times magnification Organize photos.
具体实施方式Detailed ways
下面对本发明的实施方式做进一步详细描述：Embodiments of the present invention are described in further detail below:
一种制备原位三维连续增强Al基复合材料的方法，包括以下步骤：A method for preparing an in-situ three-dimensional continuous reinforced Al-based composite material, comprising the following steps:
步骤1：将纯度均大于99％，粒度均≤100μm的Ti粉、Al粉和石墨粉按照2:(1-1.2):1的摩尔比混合，而后在玻璃研钵中充分研磨30～60min(或采用球磨工艺)，得到混合粉料；Step 1: Mix Ti powder, Al powder and graphite powder with a purity greater than 99% and a particle size of ≤100 μm in a molar ratio of 2:(1-1.2):1, and then fully grind them in a glass mortar for 30 to 60 minutes ( Or adopt ball milling process) to obtain mixed powder;
步骤2：将混合粉料放入内径为10mm的圆柱形钢铁模具中，将其在50～150MPa的径向压力下冷压成厚度为10～20mm的圆柱体生坯；Step 2: Put the mixed powder into a cylindrical steel mold with an inner diameter of 10mm, and cold press it under a radial pressure of 50-150MPa to form a cylindrical green body with a thickness of 10-20mm;
步骤3：将生坯在700～900℃的温度下预热1～3min，然后放入700～900℃的Al熔体内，静置30～60s后取出冷却，得到原位三维连续增强Al基复合材料。Step 3: Preheat the green body at a temperature of 700-900°C for 1-3 minutes, then put it into an Al melt at 700-900°C, let it stand for 30-60s, take it out and cool it, and obtain an in-situ three-dimensional continuous reinforced Al matrix composite material.
需要说明的是，基体材料还可以选用除纯Al以外的其它Al合金。It should be noted that other Al alloys other than pure Al can also be selected as the base material.
下面结合实施例对本发明做进一步详细描述：Below in conjunction with embodiment the present invention is described in further detail:
实施例1Example 1
步骤1：将Ti粉(纯度大于99％，平均粒径20μm)、Al粉(纯度大于99％，平均粒径40μm)和石墨粉(纯度大于99％，平均粒径40μm)按照2:1:1的摩尔比混合，而后在玻璃研钵中充分研磨30min，得到混合粉料；Step 1: Ti powder (purity greater than 99%, average particle size 20 μm), Al powder (purity greater than 99%, average particle size 40 μm) and graphite powder (purity greater than 99%, average particle size 40 μm) according to 2:1: 1 molar ratio mixed, and then fully ground in a glass mortar for 30min to obtain a mixed powder;
步骤2：将混合粉料放入内径为10mm的圆柱形钢铁模具中，将其在130MPa的径向压力下冷压成厚度为15mm的圆柱体生坯；Step 2: Put the mixed powder into a cylindrical steel mold with an inner diameter of 10mm, and cold press it into a cylindrical green body with a thickness of 15mm under a radial pressure of 130MPa;
步骤3：将生坯在800℃的温度下预热2min，然后放入800℃的Al熔体内，静置45s后取出冷却，从而得到原位三维连续增强Al基复合材料。Step 3: Preheat the green body at 800°C for 2 minutes, then put it into an Al melt at 800°C, let it stand for 45s, take it out and cool it, so as to obtain an in-situ three-dimensional continuous reinforced Al-based composite material.
图1为Al-Ti-C坯体在Al熔体内热爆反应后得到的原位三维连续增强Al基复合材料照片。从图可知，原位内生的三维增强体为连续结构，Al基体充满增强体孔径。图2(a)为复合材料的微观组织照片。从图可知，此工艺制备的三维增强相较为致密，增强相主要包含层片状三元MAX相(Ti2AlC/Ti3AlC2)、颗粒状TiC，此两相存在于Al3Ti相中，如图2(b)所示。Figure 1 is a photo of the in-situ three-dimensional continuous reinforced Al-based composite material obtained after the thermal explosion reaction of the Al-Ti-C body in the Al melt. It can be seen from the figure that the in-situ endogenous three-dimensional reinforcement is a continuous structure, and the Al matrix fills the pores of the reinforcement. Figure 2(a) is a photo of the microstructure of the composite material. It can be seen from the figure that the three-dimensional reinforcement phase prepared by this process is relatively dense, and the reinforcement phase mainly includes lamellar ternary MAX phase (Ti 2 AlC/Ti 3 AlC 2 ) and granular TiC, and these two phases exist in the Al 3 Ti phase , as shown in Figure 2(b).
实施例2Example 2
步骤1：将Ti粉(纯度大于99％，平均粒径20μm)、Al粉(纯度大于99％，平均粒径40μm)和石墨粉(纯度大于99％，平均粒径40μm)按照2:1.1:1的摩尔比混合，而后在玻璃研钵中充分研磨50min，得到混合粉料；Step 1: Ti powder (purity greater than 99%, average particle size 20 μm), Al powder (purity greater than 99%, average particle size 40 μm) and graphite powder (purity greater than 99%, average particle size 40 μm) according to 2:1.1: The molar ratio of 1 was mixed, and then fully ground in a glass mortar for 50min to obtain a mixed powder;
步骤2：将混合粉料放入内径为10mm的圆柱形钢铁模具中，将其在50MPa的径向压力下冷压成厚度为20mm的圆柱体生坯；Step 2: Put the mixed powder into a cylindrical steel mold with an inner diameter of 10mm, and cold press it under a radial pressure of 50MPa into a cylindrical green body with a thickness of 20mm;
步骤3：将生坯在850℃的温度下预热1.5min，然后放入850℃的Al熔体内，静置45s后取出冷却，从而得到原位三维连续增强Al基复合材料。Step 3: Preheat the green body at a temperature of 850°C for 1.5min, then put it into an Al melt at 850°C, let it stand for 45s, take it out and cool it, so as to obtain an in-situ three-dimensional continuous reinforced Al-based composite material.
实施例3Example 3
步骤1：将Ti粉(纯度大于99％，平均粒径20μm)、Al粉(纯度大于99％，平均粒径40μm)和石墨粉(纯度大于99％，平均粒径40μm)按照2:1:1的摩尔比混合，而后在玻璃研钵中充分研磨60min，得到混合粉料；Step 1: Ti powder (purity greater than 99%, average particle size 20 μm), Al powder (purity greater than 99%, average particle size 40 μm) and graphite powder (purity greater than 99%, average particle size 40 μm) according to 2:1: 1 molar ratio mixed, and then fully ground in a glass mortar for 60min to obtain a mixed powder;
步骤2：将混合粉料放入内径为10mm的圆柱形钢铁模具中，将其在100MPa的径向压力下冷压成厚度为10mm的圆柱体生坯；Step 2: Put the mixed powder into a cylindrical steel mold with an inner diameter of 10mm, and cold press it into a cylindrical green body with a thickness of 10mm under a radial pressure of 100MPa;
步骤3：将生坯在700℃的温度下预热3min，然后放入700℃的Al熔体内，静置60s后取出冷却，从而得到原位三维连续增强Al基复合材料。Step 3: Preheat the green body at 700°C for 3 minutes, then put it into the Al melt at 700°C, let it stand for 60s, take it out and cool it, so as to obtain the in-situ three-dimensional continuous reinforced Al-based composite material.
实施例4Example 4
步骤1：将Ti粉(纯度大于99％，平均粒径20μm)、Al粉(纯度大于99％，平均粒径40μm)和石墨粉(纯度大于99％，平均粒径40μm)按照2:1.2:1的摩尔比混合，而后在玻璃研钵中充分研磨30min，得到混合粉料；Step 1: Ti powder (purity greater than 99%, average particle size 20 μm), Al powder (purity greater than 99%, average particle size 40 μm) and graphite powder (purity greater than 99%, average particle size 40 μm) according to 2:1.2: 1 molar ratio mixed, and then fully ground in a glass mortar for 30min to obtain a mixed powder;
步骤2：将混合粉料放入内径为10mm的圆柱形钢铁模具中，将其在150MPa的径向压力下冷压成厚度为15mm的圆柱体生坯；Step 2: Put the mixed powder into a cylindrical steel mold with an inner diameter of 10mm, and cold press it into a cylindrical green body with a thickness of 15mm under a radial pressure of 150MPa;
步骤3：将生坯在900℃的温度下预热1min，然后放入900℃的Al熔体内，静置30s后取出冷却，从而得到原位三维连续增强Al基复合材料。Step 3: Preheat the green body at a temperature of 900°C for 1 min, then put it into an Al melt at 900°C, let it stand for 30s, take it out and cool it, so as to obtain an in-situ three-dimensional continuous reinforced Al-based composite material.
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