多孔NiAl金属间化合物/陶瓷复合材料的研究
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摘要
多孔材料具有质轻和比表面大等优异的物理性能,是一类集物理功能与结构一体化的新型材料,在催化、分离、离子交换等工业领域有着广泛的应用。本文以Ni、Al粉末为原料,通过不同的合成工艺制备了高孔隙率多孔Ni-Al金属间化合物材料:通过添加不同含量的(Al+TiO_2+B_2O_3)陶瓷体系,原位合成TiB_2+Al_2O_3增强相,制备了性能优良的多孔NiAl/(TiB_2+Al_2O_3)复合材料,并对其进行了组织和性能的检测分析。
对制备工艺进行了探索和优化。分别采用松装震实和添加造孔剂、加压制坯工艺与燃烧合成技术相结合,制备了小孔径、大孔径三维连通型多孔材料,采用添加有机物,挤出成型与燃烧合成技术相结合的工艺制备了直通孔型多孔NiAl及其复合材料。
X射线衍射分析结果表明,Ni与Al原子比为1:1时,反应产物为单一的NiAl相,添加尿素做造孔剂,对反应产物无影响。随着Ni含量的提高,相组成为NiAl+Ni_3Al以及少量的Al_2O_3。多孔NiAl/TiB_2+Al_2O_3复合材料的相组成为NiAl相和TiB_2+Al_2O_3陶瓷相。结合体系示差扫描热分析的热反应特征,分析了其反应过程。
扫描电镜下观察并分析了三维连通型多孔NiAl及其复合材料的孔洞结构。反应生成的小孔,孔洞分布均匀,孔道曲折连通,孔壁粗糙,其上分布大量微孔,提高了孔洞的连通性。添加造孔剂尿素生成的大孔形貌与造孔剂基本一致,孔隙率可达85%。通过调整尿素粒径和含量可控制孔隙率和孔径分布。结合能谱和X射线衍射分析,孔壁上呈树枝状生长的为NiAl和Ni_3Al,孔洞内可见晶须状Al_2O_3,添加Al+TiO_2+B_2O_3体系后生成正方六面体或六棱柱TiB_2颗粒,尺寸小于5μm,Al_2O_3无规则外形,晶须更为粗壮。
压缩性能测试结果表明:压缩应力—应变曲线由弹性区、平台区和致密化区三个区域组成,表现出典型的脆性断裂特征。抗压强度随孔隙率的增加而下降,孔径大小没有明显的影响,随TiB_2+Al_2O_3含量的增加抗压强度先增大后减小。
腐蚀实验结果表明:多孔NiAl金属间化合物有较强的耐酸、碱腐蚀性能,但对酸和盐的混合溶液耐腐蚀性能较差。
Porous material is a new kind material of integrative physical function and structure, which offers excellent physical properties, such as low density and high specific surface, and has been extensively used in catalysis, separation and the ionic exchange domains. In this paper, high porosity NiAl intermetallics were prepared from Ni and Al powders by different technology. Porous NiAl/TiB_2+Al_2O_3 material were prepared by adding different ratio of (Al+TiO_2+B_2O_3). NiAl was reinforced by TiB_2+Al_2O_3 phases synthesized in situ. The structure and properties were analyzed.
The preparation technology were explored and optimized. Porous NiAl and NiAl/TiB_2+Al_2O_3 with three-dimensional connectivity structure were prepared by different technology combined with Combustion synthesis. Porous material with small pore could be prepared by loose-packed ram-jolt technology and macropore could be prepared by pressure preforming technology. Porous NiAl and NiAl/TiB_2+Al_2O_3 material with through-hole structure were prepared by extrusion molding technology.
The results of X-ray diffraction analysis showd that the reaction product of Ni and Al (atom ratio is 1:1) was single NiAl phase. There was no difference when urea was added as pore-forming agent. Phases were NiAl, Ni_3Al and a small quantity of Al_2O_3. The phases were NiAl, TiB_2 and Al_2O_3 of NiAl/TiB_2+Al_2O_3. According to the thermal reaction characters detected by Differential Scanning Calorimetry (DSC), the reaction process was analyzed.
Three-dimensional connectivity structures of porous NiAl and NiAl/TiB_2+Al_2O_3 materials were observed under Scanning Electron Microscope (SEM). Small pores formed in the reaction process were uniform distribution with twisted channel and rough pore wall. There were large quantities micropores penetrating through the wall, so the connectivity of porous materials becomes better. The appearance of macropore formed by urea volatilization was similar to urea, and the porosity could reach 85% by adding pore-forming agent. So the porosity and pore size could be controlled by adjusting the urea content and size. According to EDS and XRD results, NiAl and Ni_3Al were dendritically formed in the pore wall and Al_2O_3 whisker were observed inside the pores. TiB_2 particles, less than 5μm, formed in regular hexahedron or hexagonal prism in the system with Al-TiO_2+B_2O_3. Al_2O_3 showed no regular shape, and the whisker showed stronger.
Compressive performance tests showed that the stress-strain curve was separated into three ranges: elastic range, stress plateau range and densification range. It was the classic character of brittle fracture. Pressive strength declines with the porosity increased. The influence on pressive strength of pore size was unobvious. However, the pressive strength first increased, and then decreased with the increase of TiB_2+Al_2O_3 content.
Corrosion test showed that porous NiAl intermetallic compounds had excellent corrosion resistance to acid and alkaline, but poor resistance to the solution of acid and salt.
对制备工艺进行了探索和优化。分别采用松装震实和添加造孔剂、加压制坯工艺与燃烧合成技术相结合,制备了小孔径、大孔径三维连通型多孔材料,采用添加有机物,挤出成型与燃烧合成技术相结合的工艺制备了直通孔型多孔NiAl及其复合材料。
X射线衍射分析结果表明,Ni与Al原子比为1:1时,反应产物为单一的NiAl相,添加尿素做造孔剂,对反应产物无影响。随着Ni含量的提高,相组成为NiAl+Ni_3Al以及少量的Al_2O_3。多孔NiAl/TiB_2+Al_2O_3复合材料的相组成为NiAl相和TiB_2+Al_2O_3陶瓷相。结合体系示差扫描热分析的热反应特征,分析了其反应过程。
扫描电镜下观察并分析了三维连通型多孔NiAl及其复合材料的孔洞结构。反应生成的小孔,孔洞分布均匀,孔道曲折连通,孔壁粗糙,其上分布大量微孔,提高了孔洞的连通性。添加造孔剂尿素生成的大孔形貌与造孔剂基本一致,孔隙率可达85%。通过调整尿素粒径和含量可控制孔隙率和孔径分布。结合能谱和X射线衍射分析,孔壁上呈树枝状生长的为NiAl和Ni_3Al,孔洞内可见晶须状Al_2O_3,添加Al+TiO_2+B_2O_3体系后生成正方六面体或六棱柱TiB_2颗粒,尺寸小于5μm,Al_2O_3无规则外形,晶须更为粗壮。
压缩性能测试结果表明:压缩应力—应变曲线由弹性区、平台区和致密化区三个区域组成,表现出典型的脆性断裂特征。抗压强度随孔隙率的增加而下降,孔径大小没有明显的影响,随TiB_2+Al_2O_3含量的增加抗压强度先增大后减小。
腐蚀实验结果表明:多孔NiAl金属间化合物有较强的耐酸、碱腐蚀性能,但对酸和盐的混合溶液耐腐蚀性能较差。
Porous material is a new kind material of integrative physical function and structure, which offers excellent physical properties, such as low density and high specific surface, and has been extensively used in catalysis, separation and the ionic exchange domains. In this paper, high porosity NiAl intermetallics were prepared from Ni and Al powders by different technology. Porous NiAl/TiB_2+Al_2O_3 material were prepared by adding different ratio of (Al+TiO_2+B_2O_3). NiAl was reinforced by TiB_2+Al_2O_3 phases synthesized in situ. The structure and properties were analyzed.
The preparation technology were explored and optimized. Porous NiAl and NiAl/TiB_2+Al_2O_3 with three-dimensional connectivity structure were prepared by different technology combined with Combustion synthesis. Porous material with small pore could be prepared by loose-packed ram-jolt technology and macropore could be prepared by pressure preforming technology. Porous NiAl and NiAl/TiB_2+Al_2O_3 material with through-hole structure were prepared by extrusion molding technology.
The results of X-ray diffraction analysis showd that the reaction product of Ni and Al (atom ratio is 1:1) was single NiAl phase. There was no difference when urea was added as pore-forming agent. Phases were NiAl, Ni_3Al and a small quantity of Al_2O_3. The phases were NiAl, TiB_2 and Al_2O_3 of NiAl/TiB_2+Al_2O_3. According to the thermal reaction characters detected by Differential Scanning Calorimetry (DSC), the reaction process was analyzed.
Three-dimensional connectivity structures of porous NiAl and NiAl/TiB_2+Al_2O_3 materials were observed under Scanning Electron Microscope (SEM). Small pores formed in the reaction process were uniform distribution with twisted channel and rough pore wall. There were large quantities micropores penetrating through the wall, so the connectivity of porous materials becomes better. The appearance of macropore formed by urea volatilization was similar to urea, and the porosity could reach 85% by adding pore-forming agent. So the porosity and pore size could be controlled by adjusting the urea content and size. According to EDS and XRD results, NiAl and Ni_3Al were dendritically formed in the pore wall and Al_2O_3 whisker were observed inside the pores. TiB_2 particles, less than 5μm, formed in regular hexahedron or hexagonal prism in the system with Al-TiO_2+B_2O_3. Al_2O_3 showed no regular shape, and the whisker showed stronger.
Compressive performance tests showed that the stress-strain curve was separated into three ranges: elastic range, stress plateau range and densification range. It was the classic character of brittle fracture. Pressive strength declines with the porosity increased. The influence on pressive strength of pore size was unobvious. However, the pressive strength first increased, and then decreased with the increase of TiB_2+Al_2O_3 content.
Corrosion test showed that porous NiAl intermetallic compounds had excellent corrosion resistance to acid and alkaline, but poor resistance to the solution of acid and salt.
引文
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