纳米级钨基复合粉末的制备及其合金特性研究
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摘要
高密度钨基合金由于具有一系列优异的物理、力学性能,如密度高、强度高、延性好等,被广泛地应用于动能穿甲弹、平衡配重块、放射屏蔽和电触头材料,在国防军工、航空航天等领域中具有不可替代的作用。随着科学技术的飞速发展,对材料性能提出了更为苛刻的要求,制备高性能钨基合金材料已成为当今世界致力研究的热点之一。而制备高性能钨基合金材料的核心在于:粉末原料的纳米化及其合金的特性研究。本论文围绕这一核心课题,对纳米级W-Ni-Fe复合粉末的制备及其合金特性等方面进行了较系统、较深入的研究。
对含(W,Ni,Fe)盐溶胶体系的电化学特征进行了深入研究。研究了体系Zeta电位、pH值和所加表面活性剂,对含(W,Ni,Fe)盐溶胶体系的配制、颗粒分散性和稳定性的影响。着重研究了十六烷基三甲基溴化铵、N,N—二甲基甲酰胺和聚乙二醇-1000这三种表面活性剂对颗粒表面静电位阻、空间位阻及静电-空间位阻协调作用的影响。首次采用配置溶胶并进行喷雾干燥来制备(W,Ni,Fe)前驱体复合氧化物粉末。深入探讨了表面活性剂在喷雾干燥过程中的作用机制,并提出了颗粒在干燥过程中所受毛细管作用力的示意图模型。
对所制备的(W,Ni,Fe)复合氧化物粉末的还原机理进行了大量研究。结果表明:还原温度与时间均对W—Ni—Fe复合粉末的特性有显著的影响,其最佳还原参数是:温度700℃、时间90min,此时可得到颗粒的平均Fsss粒度小于0.61μm、平均BET粒度小于100nm、晶粒尺寸小于30nm、氧含量小于0.23%,且颗粒分散均匀、绝大部分为球形的纳米级W-Ni-Fe复合粉末。同时指出颗粒的长大机理主要是由还原过程中化学气相迁移所控制,随还原过程的进行,所生成的水蒸汽逐渐增多,钨的氧化物与水蒸汽化合成易挥发的水合物WO_x·nH_2O(一般认为是WO_2(OH)_2),而后通过气相迁移,沉积在低价氧化钨或金属钨粉的颗粒表面,导致颗粒长大,因此,采用两步还原和添加稀土La、Y来抑制其长大。所加稀土以钨酸盐La(Ni_(0.75)W(0.25))O_3或Y(Ni_(0.75)W_(0.25))O_3的形式附着在钨颗粒或钨氧化物颗粒表面,阻止了还原过程中钨的氧化物与水蒸汽化合生成易挥发水合物WO_2(OH)_2的生成速度,从而减少了其气相迁移,有效地阻止了粉末颗粒的长大。当稀土元素质量百分数在0-0.8%范围内(占90W-7Ni-3Fe复合粉末的质量百分数),随着稀土元素含量的增大,还原粉末特性有显著改善;添加相同含量稀土元素时,对粉末特性影响程度的大小顺序是Y>La-Y>La。
采用DTA仪测得纳米级90W-Ni-Fe复合粉末体系中固-液共存的温度区间是1341.2℃-1365.8℃,比传统粉末的温度区间降低了70-90℃。研究了烧结温度、时间对纳米粉90W-Ni-Fe合金烧结特性的影响,在此基础上建立了该合金的低温烧结制度。
深入研究了稀土元素对纳米粉90W-Ni-Fe合金性能和显微结构的影响,建立了合金中钨颗粒的三层微观结构模型图,并据此较好地解释了稀土元素与合金性能和显微
High density tungsten based alloys possess an unique combination of physical and mechanical properties, such as high density, strength and ductility, which are used extensively as kinetic energy penetrators, counterbalance weights, radiation shields and electrical contacts. They cannot be replaced in the field, such as national defence, military industry, aviation and spaceflight. With the quick development of science and technology, higher demand for material properties is put forward and preparation of tungsten based alloys with high properties is one of the hotspot in the world. But the cores of preparation of tungsten based alloys with high properties are preparation of nanometer powder and study for properties of alloy. Preparation of nanometer W-Ni-Fe composite powder and properties of alloy were systemic studied according to the cores.Electrochemistry characters of (W,Ni,Fe) solution colloid system were studied deeply. Influence of Zeta potential, pH value and surfactants added on particle dispersity and stability of colloid solution system were investigated. The roles of cetyl trimethyl ammonium bromide (CTAB), N,N-dimethylformampe and polyethylene glycol-1000 (PEG-1000) on electrostatic hindrance, steric hindrance and electrostatic-steric hindrance cooperation function of particle surface were studied in detail. (W,Ni,Fe) precursor composite oxide powders were first synthesized by preparation of solution colloid and spray drying. Action mechanism of surfactants in spray drying process was discussed deeply and schematics of capillary action force during particle drying was established.Reduction mechanism was studied deeply during reduction of (W,Ni,Fe) composite oxide powder. Results showed: influence of reduction temperature and time on properties of W-Ni-Fe composite powder was remarkable, and the best reduction condition was 700℃ for 90min. Nanometer W-Ni-Fe composite powder, average Fsss of which was smaller than 0.61 μm, BET sizes smaller than 100nm, crystalline size smaller than 30nm, oxide content of reduced powder smaller than 0.23%, homogeneous disperse and spherical morphology, was fabricated at 700℃ for 90min. Air phase transfer which mainly resulted in growth of particles during reduction was put forward. With the increasing of vapour produced during reduction, volatility WO_2(OH)_2 was easy synthesized by tungsten oxide and vapour. WO_2(OH)_2 deposited in surface of oxide tungsten with lower chemistry value or metal tungsten powder and resulted in growth of particles. Then two-stage reduction method and adding rare earth La or Y were put forward in order to inhibit growth of particles in this paper. When adding rare earth elements La or Y, new phase La(Ni_(0.75)W_(0.25))O_3 or Y(Ni_(0.75)W_(0.25))O_3 produced and adsorbed on surface of metal tungsten particles or tungsten oxide particles. Producing speed of volatility WO_2(OH)_2 was prevented from synthesizing of tungsten oxide and vapour, then air phase transfer was decreased. Growth of powder
particles were hold back. When the rare earth element content was below 0.8 wt%, with the increasing of the rare earth elements content, the properties of the composite powder improved distinctly. When same content of rare earth elements were added, the effect degree on powder properties was Y>La-Y(mixing rare earth)>La.Coexistence field of solid and liquid is in the temperature range of 1341.2°C to 1365.8 °C by means of DTA apparatus. The field is lower about 70-90 °C than conventional 90W-Ni-Fe powder. Influence of sintering temperature and time on sintering properties of nanometer powder 90W-7Ni-3Fe alloy were studied according to this viewpoint. Low-temperature sintering mechanism of nanometer powder 90W-7Ni-3Fe alloy was investigated.Influence of adding rare earth elements La or Y on properties and microstructure of 90W-Ni-Fe alloy were investigated deeply and three-layer microstructure model images of W particle in alloy was established. Relation between adding La or Y and properties or microstructure of alloy was explained commendably by three-layer microstructure model images of W particle.It was not evident that W crystal was prevented from growing and properties of alloys improved by adding rare earth La. Transgranular cleavage fracture of W crystal and ductile avulsion of matrix phase are main fracture modes in the samples when adding Y. Inhibiting function from growing of W crystal was distinct and W crystal sizes decreased from 20-25 u m to 12 u m by adding 0.4% Y. Emergence chance of cavities and vapour reduced during liquid sintering in dry-tb atmosphere was decreased, and properties of alloys improved prominently by adding some Y. Relative density, tensile strength and elongation of samples was 99.6%, 1027.5MPa and 18.6% by adding 0.4% Y, respectively. When adding 0.6% Y, relative density, tensile strength and elongation of samples was 99.3%, HOOMPa and 16.3%, respectively. The properties of alloys are enhanced 25-30% than conventional 90W-Ni-Fe alloys. But W crystal morphology changed by adding some Y, W crystal morphology was nearly spherical by adding 0.4% Y or polyhedron by adding 0.8% Y. When same content of rare earth elements were added, the effect degree on properties of alloys was Y>La-Y(mixing rare earth)>La.When adding some rare earth elements, diffuse speed and solubility of tungsten in matrix phase descended, and solubility of tungsten in matrix phase decreased from 58.65 wt%(without rare earth) to 29.86 wt%(adding 0.4% La-Y). Therefore, deformation adjustability of matrix phase enhanced greatly.
对含(W,Ni,Fe)盐溶胶体系的电化学特征进行了深入研究。研究了体系Zeta电位、pH值和所加表面活性剂,对含(W,Ni,Fe)盐溶胶体系的配制、颗粒分散性和稳定性的影响。着重研究了十六烷基三甲基溴化铵、N,N—二甲基甲酰胺和聚乙二醇-1000这三种表面活性剂对颗粒表面静电位阻、空间位阻及静电-空间位阻协调作用的影响。首次采用配置溶胶并进行喷雾干燥来制备(W,Ni,Fe)前驱体复合氧化物粉末。深入探讨了表面活性剂在喷雾干燥过程中的作用机制,并提出了颗粒在干燥过程中所受毛细管作用力的示意图模型。
对所制备的(W,Ni,Fe)复合氧化物粉末的还原机理进行了大量研究。结果表明:还原温度与时间均对W—Ni—Fe复合粉末的特性有显著的影响,其最佳还原参数是:温度700℃、时间90min,此时可得到颗粒的平均Fsss粒度小于0.61μm、平均BET粒度小于100nm、晶粒尺寸小于30nm、氧含量小于0.23%,且颗粒分散均匀、绝大部分为球形的纳米级W-Ni-Fe复合粉末。同时指出颗粒的长大机理主要是由还原过程中化学气相迁移所控制,随还原过程的进行,所生成的水蒸汽逐渐增多,钨的氧化物与水蒸汽化合成易挥发的水合物WO_x·nH_2O(一般认为是WO_2(OH)_2),而后通过气相迁移,沉积在低价氧化钨或金属钨粉的颗粒表面,导致颗粒长大,因此,采用两步还原和添加稀土La、Y来抑制其长大。所加稀土以钨酸盐La(Ni_(0.75)W(0.25))O_3或Y(Ni_(0.75)W_(0.25))O_3的形式附着在钨颗粒或钨氧化物颗粒表面,阻止了还原过程中钨的氧化物与水蒸汽化合生成易挥发水合物WO_2(OH)_2的生成速度,从而减少了其气相迁移,有效地阻止了粉末颗粒的长大。当稀土元素质量百分数在0-0.8%范围内(占90W-7Ni-3Fe复合粉末的质量百分数),随着稀土元素含量的增大,还原粉末特性有显著改善;添加相同含量稀土元素时,对粉末特性影响程度的大小顺序是Y>La-Y>La。
采用DTA仪测得纳米级90W-Ni-Fe复合粉末体系中固-液共存的温度区间是1341.2℃-1365.8℃,比传统粉末的温度区间降低了70-90℃。研究了烧结温度、时间对纳米粉90W-Ni-Fe合金烧结特性的影响,在此基础上建立了该合金的低温烧结制度。
深入研究了稀土元素对纳米粉90W-Ni-Fe合金性能和显微结构的影响,建立了合金中钨颗粒的三层微观结构模型图,并据此较好地解释了稀土元素与合金性能和显微
High density tungsten based alloys possess an unique combination of physical and mechanical properties, such as high density, strength and ductility, which are used extensively as kinetic energy penetrators, counterbalance weights, radiation shields and electrical contacts. They cannot be replaced in the field, such as national defence, military industry, aviation and spaceflight. With the quick development of science and technology, higher demand for material properties is put forward and preparation of tungsten based alloys with high properties is one of the hotspot in the world. But the cores of preparation of tungsten based alloys with high properties are preparation of nanometer powder and study for properties of alloy. Preparation of nanometer W-Ni-Fe composite powder and properties of alloy were systemic studied according to the cores.Electrochemistry characters of (W,Ni,Fe) solution colloid system were studied deeply. Influence of Zeta potential, pH value and surfactants added on particle dispersity and stability of colloid solution system were investigated. The roles of cetyl trimethyl ammonium bromide (CTAB), N,N-dimethylformampe and polyethylene glycol-1000 (PEG-1000) on electrostatic hindrance, steric hindrance and electrostatic-steric hindrance cooperation function of particle surface were studied in detail. (W,Ni,Fe) precursor composite oxide powders were first synthesized by preparation of solution colloid and spray drying. Action mechanism of surfactants in spray drying process was discussed deeply and schematics of capillary action force during particle drying was established.Reduction mechanism was studied deeply during reduction of (W,Ni,Fe) composite oxide powder. Results showed: influence of reduction temperature and time on properties of W-Ni-Fe composite powder was remarkable, and the best reduction condition was 700℃ for 90min. Nanometer W-Ni-Fe composite powder, average Fsss of which was smaller than 0.61 μm, BET sizes smaller than 100nm, crystalline size smaller than 30nm, oxide content of reduced powder smaller than 0.23%, homogeneous disperse and spherical morphology, was fabricated at 700℃ for 90min. Air phase transfer which mainly resulted in growth of particles during reduction was put forward. With the increasing of vapour produced during reduction, volatility WO_2(OH)_2 was easy synthesized by tungsten oxide and vapour. WO_2(OH)_2 deposited in surface of oxide tungsten with lower chemistry value or metal tungsten powder and resulted in growth of particles. Then two-stage reduction method and adding rare earth La or Y were put forward in order to inhibit growth of particles in this paper. When adding rare earth elements La or Y, new phase La(Ni_(0.75)W_(0.25))O_3 or Y(Ni_(0.75)W_(0.25))O_3 produced and adsorbed on surface of metal tungsten particles or tungsten oxide particles. Producing speed of volatility WO_2(OH)_2 was prevented from synthesizing of tungsten oxide and vapour, then air phase transfer was decreased. Growth of powder
particles were hold back. When the rare earth element content was below 0.8 wt%, with the increasing of the rare earth elements content, the properties of the composite powder improved distinctly. When same content of rare earth elements were added, the effect degree on powder properties was Y>La-Y(mixing rare earth)>La.Coexistence field of solid and liquid is in the temperature range of 1341.2°C to 1365.8 °C by means of DTA apparatus. The field is lower about 70-90 °C than conventional 90W-Ni-Fe powder. Influence of sintering temperature and time on sintering properties of nanometer powder 90W-7Ni-3Fe alloy were studied according to this viewpoint. Low-temperature sintering mechanism of nanometer powder 90W-7Ni-3Fe alloy was investigated.Influence of adding rare earth elements La or Y on properties and microstructure of 90W-Ni-Fe alloy were investigated deeply and three-layer microstructure model images of W particle in alloy was established. Relation between adding La or Y and properties or microstructure of alloy was explained commendably by three-layer microstructure model images of W particle.It was not evident that W crystal was prevented from growing and properties of alloys improved by adding rare earth La. Transgranular cleavage fracture of W crystal and ductile avulsion of matrix phase are main fracture modes in the samples when adding Y. Inhibiting function from growing of W crystal was distinct and W crystal sizes decreased from 20-25 u m to 12 u m by adding 0.4% Y. Emergence chance of cavities and vapour reduced during liquid sintering in dry-tb atmosphere was decreased, and properties of alloys improved prominently by adding some Y. Relative density, tensile strength and elongation of samples was 99.6%, 1027.5MPa and 18.6% by adding 0.4% Y, respectively. When adding 0.6% Y, relative density, tensile strength and elongation of samples was 99.3%, HOOMPa and 16.3%, respectively. The properties of alloys are enhanced 25-30% than conventional 90W-Ni-Fe alloys. But W crystal morphology changed by adding some Y, W crystal morphology was nearly spherical by adding 0.4% Y or polyhedron by adding 0.8% Y. When same content of rare earth elements were added, the effect degree on properties of alloys was Y>La-Y(mixing rare earth)>La.When adding some rare earth elements, diffuse speed and solubility of tungsten in matrix phase descended, and solubility of tungsten in matrix phase decreased from 58.65 wt%(without rare earth) to 29.86 wt%(adding 0.4% La-Y). Therefore, deformation adjustability of matrix phase enhanced greatly.
引文
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