镍基高温合金空心球多孔材料的制备与性能研究
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摘要
本文以INCO-617合金粉为原材料,聚乙烯醇为粘结剂,聚苯乙烯珠粒为造孔剂,采用粉末冶金法制备了Ni基高温合金空心球多孔材料及其夹芯结构。探讨了粉末类型、粘结剂浓度、液固比对合金粉浆涂覆性能的影响,并研究了空心球多孔材料的烧结工艺。利用扫描电子显微镜、X射线衍射等分析测试手段,对材料的烧结组织与相组成进行了分析,并对所制备的材料进行了压缩实验,研究空心球多孔材料压缩性能的变化规律。
实验制备了孔隙率为78.1~90.7%的INCO-617合金空心球多孔材料,对其制备工艺的研究表明,在适合的粘结剂浓度下,小尺寸的雾化细粉或不规则形状的球磨粉末均具有良好的涂覆性;采用低粘结剂浓度,雾化细粉或高比表面能的球磨细粉,采用更高的烧结温度、更长的烧结时间均有利于空心球多孔材料孔壁的致密化。多孔材料的相组成为基体γ相、高Cr碳化物M23C6和高Mo碳化物M6C两种碳化物组成。对于雾化细粉制备的空心球多孔材料,随着烧结温度的提高以及时间的延长,碳化物的尺寸增大,数量先增多后减少。相同工艺下,球磨粉末制备的空心球多孔材料的碳化物尺寸更小、析出更弥散。
空心球多孔材料的孔隙率主要受空心球的结构参数与排布方式的影响。显微硬度实验和压缩实验结果表明,粉末烧结情况和显微组织两类因素综合作用影响着高温合金空心球多孔材料的力学性能。雾化细粉制备的空心球多孔材料具有更优的压缩性能,随着孔壁致密化程度的提高,孔壁的硬度提高,空心球多孔材料的压缩强度以及弹性模量增加,应力-应变曲线开始出现明显的平台区,进一步提高烧结温度或延长烧结时间,由于碳化物的影响,平台区的应力波动有所增加。相同工艺以及密度条件下,薄壁小孔径空心球多孔材料的力学性能要优于厚壁大孔径空心球结构,BCC结构空心球多孔材料的力学性能要优于SC结构的空心球多孔材料。空心球结构与制备工艺相同时,空心球多孔材料的密度和压缩性能可以通过选用不同直径的造孔剂来控制。实测的σ*/σs值远高于开孔泡沫,烧结温度为1230℃时,其压缩强度甚至与闭孔泡沫理论值接近。高温合金空心球多孔材料的压缩断口主要为粉粒间烧结颈的断裂,随着粉末烧结程度的提高,断口处致密金属断面的面积越大,断裂前孔壁参与塑性变形的体积增多。当烧结温度高于1150℃时,空心球多孔材料压缩时呈现出逐层破坏的变形特征。空心球多孔材料具有良好的吸能能力以及高的吸收效率,致密化区前吸能效率大于70%。
以实验制备的INCO-617合金空心球多孔材料为芯体,采用球磨细粉粉浆连接法,制备了具有足够强度的冶金结合界面的高熔点三明治夹芯结构。空心球多孔材料夹芯管改变了薄管的变形机制,相同应变下增加外表面薄管的塑性变形,在保持空心球多孔材料轻质、高吸能效率的同时,增大了结构的吸能能力,致密化区前能量吸收效率超过85%。三明治夹芯板制备与性能研究表明,轻质芯体的使用增大了结构的刚度,并且由于空心球多孔材料芯体与面板之间界面结合强度足够高,在性能实验与计算过程中可忽略界面的影响,夹芯板的加载刚度和极限载荷与理论值吻合较好,展现出良好的发展前景。
Ni-base superalloy hollow sphere cellular materials(HSC) were fabricated by powder metallurgy, using INCO-617 alloy powders as raw material, polyvinyl alcohol as binder, polystyrene sphere as pore-forming agent. The influence of powder’s properties, binder concentration and liquid-to-solid ratio on coating properties of alloy slurry was discussed, and then the sintering process of HSC was researched. The microstructure and phase constitution of HSC were analyzed by means of scanning electron microscope(SEM) and X-ray diffraction(XRD). The compression test was conducted to investigate the variety in compressive properties of HSC.
INCO-617 alloy HSC with porosity ranging from 74.1% to 90.7% were prepared in the experiment. The research on preparation of HSC indicates that good coating properties can be achieved by choosing the atomized fine powders or irregular shape milling powders with appropriate concentration binder. The lower concentration binder, atomized fine powder/milling fine powder with high specific surface energy, higher sintering temperature and longer holding time are conducive to the densification of the cell wall of HSC. The microstructure of HSC comprisesγmatrix, M23C6 type carbides, having high chromium content, and M6C type carbides, having high molybdenum content. With sintering temperature increase and extension of holding time, the size of carbides increase, and the quantity of carbides increase firstly and then decrease. For HSC prepared at same process by using milling powder, the size of carbides become smaller, and precipitations distribute dispersedly.
The porosity of HSC is determined by structure parameters and packing of hollow sphere. The results of micro-hardness test and compression test show that the powder sintering extent and microstructure effect mechanical properties of HSC. The HSC fabricated by atomized fine powder have better compression performance, with the densification of cell wall increasing, the compression strength and elastic modulus increase, the stress-strain curves began to appear obvious platform, but with the further increase of sintering temperature and holding time, the stress fluctuations of platform increase due to carbides. At the same density and preparation process, the mechanical properties of HSC with thin cell wall are higher than those of HSC with thick cell wall, and the BCC packing HSC’s mechanical properties are higner than those of SC packing. When the hollow sphere packing and preparation process are same, the compression properties of HSC are controlled by choosing different diameter pore-forming agent. The measured values ofσ*/σs are well above the strength of metallic open-cell foam, which is close to the theoretical values for closed-cell foams when sintering temperature is 1230℃. Most of the compressive fractures of superalloy HSC occure at the sintering necks between powders. With cell wall’s densification improved, the dense metal cross-section area in the fracture and the plastic deformation volume of cell wall increase. When the sintering temperature is higher than 1150℃, the compressive deformations of HSC are conduct by a layer-by-layer destruction mechanism. HSC have good energy absorption capacity and energy absorption efficiency which exceed 70% before densification stage.
The high-melting sandwich structure with adequate strength of the metallurgical interface were fabricated by using milling fine slurry and INCO-617 alloy HSC as bonding layer and core respectively. The deformation mechanism of HSC core sandwich tube is different from tube. In the same compressive strain core make the plastic deformation of outer tube increase, which increase the energy absorption of sandwich structure, remaining the lightweight and high-energy absorption efficiency of HSC. The energy absorption efficiency is above 70% before densification stage. The investigation of fabrication and properties of sandwich panel indicates that lightweight core increase the stiffness of sandwich structure. Because of good interface bonding with enough strength between the HSC core and face, the influence of interface can be neglected in the property test and calculation. The calculated value of loading stiffness and limit load is in good agreement with the theoretical value, showing good prospects for development.
实验制备了孔隙率为78.1~90.7%的INCO-617合金空心球多孔材料,对其制备工艺的研究表明,在适合的粘结剂浓度下,小尺寸的雾化细粉或不规则形状的球磨粉末均具有良好的涂覆性;采用低粘结剂浓度,雾化细粉或高比表面能的球磨细粉,采用更高的烧结温度、更长的烧结时间均有利于空心球多孔材料孔壁的致密化。多孔材料的相组成为基体γ相、高Cr碳化物M23C6和高Mo碳化物M6C两种碳化物组成。对于雾化细粉制备的空心球多孔材料,随着烧结温度的提高以及时间的延长,碳化物的尺寸增大,数量先增多后减少。相同工艺下,球磨粉末制备的空心球多孔材料的碳化物尺寸更小、析出更弥散。
空心球多孔材料的孔隙率主要受空心球的结构参数与排布方式的影响。显微硬度实验和压缩实验结果表明,粉末烧结情况和显微组织两类因素综合作用影响着高温合金空心球多孔材料的力学性能。雾化细粉制备的空心球多孔材料具有更优的压缩性能,随着孔壁致密化程度的提高,孔壁的硬度提高,空心球多孔材料的压缩强度以及弹性模量增加,应力-应变曲线开始出现明显的平台区,进一步提高烧结温度或延长烧结时间,由于碳化物的影响,平台区的应力波动有所增加。相同工艺以及密度条件下,薄壁小孔径空心球多孔材料的力学性能要优于厚壁大孔径空心球结构,BCC结构空心球多孔材料的力学性能要优于SC结构的空心球多孔材料。空心球结构与制备工艺相同时,空心球多孔材料的密度和压缩性能可以通过选用不同直径的造孔剂来控制。实测的σ*/σs值远高于开孔泡沫,烧结温度为1230℃时,其压缩强度甚至与闭孔泡沫理论值接近。高温合金空心球多孔材料的压缩断口主要为粉粒间烧结颈的断裂,随着粉末烧结程度的提高,断口处致密金属断面的面积越大,断裂前孔壁参与塑性变形的体积增多。当烧结温度高于1150℃时,空心球多孔材料压缩时呈现出逐层破坏的变形特征。空心球多孔材料具有良好的吸能能力以及高的吸收效率,致密化区前吸能效率大于70%。
以实验制备的INCO-617合金空心球多孔材料为芯体,采用球磨细粉粉浆连接法,制备了具有足够强度的冶金结合界面的高熔点三明治夹芯结构。空心球多孔材料夹芯管改变了薄管的变形机制,相同应变下增加外表面薄管的塑性变形,在保持空心球多孔材料轻质、高吸能效率的同时,增大了结构的吸能能力,致密化区前能量吸收效率超过85%。三明治夹芯板制备与性能研究表明,轻质芯体的使用增大了结构的刚度,并且由于空心球多孔材料芯体与面板之间界面结合强度足够高,在性能实验与计算过程中可忽略界面的影响,夹芯板的加载刚度和极限载荷与理论值吻合较好,展现出良好的发展前景。
Ni-base superalloy hollow sphere cellular materials(HSC) were fabricated by powder metallurgy, using INCO-617 alloy powders as raw material, polyvinyl alcohol as binder, polystyrene sphere as pore-forming agent. The influence of powder’s properties, binder concentration and liquid-to-solid ratio on coating properties of alloy slurry was discussed, and then the sintering process of HSC was researched. The microstructure and phase constitution of HSC were analyzed by means of scanning electron microscope(SEM) and X-ray diffraction(XRD). The compression test was conducted to investigate the variety in compressive properties of HSC.
INCO-617 alloy HSC with porosity ranging from 74.1% to 90.7% were prepared in the experiment. The research on preparation of HSC indicates that good coating properties can be achieved by choosing the atomized fine powders or irregular shape milling powders with appropriate concentration binder. The lower concentration binder, atomized fine powder/milling fine powder with high specific surface energy, higher sintering temperature and longer holding time are conducive to the densification of the cell wall of HSC. The microstructure of HSC comprisesγmatrix, M23C6 type carbides, having high chromium content, and M6C type carbides, having high molybdenum content. With sintering temperature increase and extension of holding time, the size of carbides increase, and the quantity of carbides increase firstly and then decrease. For HSC prepared at same process by using milling powder, the size of carbides become smaller, and precipitations distribute dispersedly.
The porosity of HSC is determined by structure parameters and packing of hollow sphere. The results of micro-hardness test and compression test show that the powder sintering extent and microstructure effect mechanical properties of HSC. The HSC fabricated by atomized fine powder have better compression performance, with the densification of cell wall increasing, the compression strength and elastic modulus increase, the stress-strain curves began to appear obvious platform, but with the further increase of sintering temperature and holding time, the stress fluctuations of platform increase due to carbides. At the same density and preparation process, the mechanical properties of HSC with thin cell wall are higher than those of HSC with thick cell wall, and the BCC packing HSC’s mechanical properties are higner than those of SC packing. When the hollow sphere packing and preparation process are same, the compression properties of HSC are controlled by choosing different diameter pore-forming agent. The measured values ofσ*/σs are well above the strength of metallic open-cell foam, which is close to the theoretical values for closed-cell foams when sintering temperature is 1230℃. Most of the compressive fractures of superalloy HSC occure at the sintering necks between powders. With cell wall’s densification improved, the dense metal cross-section area in the fracture and the plastic deformation volume of cell wall increase. When the sintering temperature is higher than 1150℃, the compressive deformations of HSC are conduct by a layer-by-layer destruction mechanism. HSC have good energy absorption capacity and energy absorption efficiency which exceed 70% before densification stage.
The high-melting sandwich structure with adequate strength of the metallurgical interface were fabricated by using milling fine slurry and INCO-617 alloy HSC as bonding layer and core respectively. The deformation mechanism of HSC core sandwich tube is different from tube. In the same compressive strain core make the plastic deformation of outer tube increase, which increase the energy absorption of sandwich structure, remaining the lightweight and high-energy absorption efficiency of HSC. The energy absorption efficiency is above 70% before densification stage. The investigation of fabrication and properties of sandwich panel indicates that lightweight core increase the stiffness of sandwich structure. Because of good interface bonding with enough strength between the HSC core and face, the influence of interface can be neglected in the property test and calculation. The calculated value of loading stiffness and limit load is in good agreement with the theoretical value, showing good prospects for development.
引文
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