Ni-Cu合金纳米粉的制备及其性能研究
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摘要
本文用直流电弧等离子蒸发法制备了纯Ni纳米粉、纯Cu纳米粉及Ni-Cu合金纳米粉，用正交实验法研究了工艺参数对三种纳米粉体产率及粒径的影响，并确定了各自的最优化工艺条件。以Ni-Cu合金纳米粉体为研究对象，研究了其在制备、烧结过程中的生长机制。用放电等离子烧结法（SPS）对Ni-Cu合金纳米粉进行固化成形，并研究了其力学性能及强化机制。以Ni、Cu纳米粉为参照，用差热扫描量热分析法研究了Ni-Cu合金纳米粉体对高氯酸铵（AP）的催化性能及催化机理。
制备Ni-Cu合金纳米粉的最优化工艺条件为：以产率为指标时，电流300A、氢氩比1/1、气体总压0.06MPa；以粒径为指标时，电流300A、氢氩比1/1、气体总压0.07MPa。制备纯Ni及纯Cu纳米粉的最优化工艺条件均为：电流300A、氢氩比1/1、气体总压0.07MPa。结合实验结果，以经典成核理论为基础，研究了Ni-Cu合金纳米粉的晶体生长驱动力。
研究了在不同温度（773K，823K，873K，923K，973K）下烧结的Ni-Cu合金块体材料的相组成、织构演变和颗粒形貌特征。XRD结果显示，Ni-Cu合金块体均具有单一的面心立方结构，但XRD图中（111）及（200）面的峰强比值I(111)/I(200)不同，表明烧结过程中材料发生了织构演变。扫描电镜照片显示，随着温度升高，粒子尺寸逐渐增加，粒子形状从球形渐渐向多面体形状演变。依据透射电镜结果判断，不同烧结温度下材料中孪晶、位错及孔洞数量是导致材料性能差异的根本原因。结合晶体动力学生长理论研究了Ni-Cu合金纳米粉在烧结过程中的生长机制，计算了不同温度下烧结的Ni-Cu合金块体的动力学生长指数及晶粒生长激活能。
用纳米压痕机械试验仪及维氏硬度计分别测试了不同温度下烧结的Ni-Cu合金块体的硬度，并通过拉伸实验测试了其拉伸强度、屈服强度及延展率。
结合形变断裂过程研究了Ni-Cu合金块体材料的强化机制。用细晶强化理论研究了烧结的Ni-Cu合金块体材料的力学性能，Ni-Cu合金块体强度大于Ni-Cu原料合金锭的强度，但强度与粒径的关系不符合Hall-Petch关系。孪晶强化是Ni-Cu合金块体材料的主要强化机制，Ni-Cu合金块体材料力学性能的提高主要是因为变形孪晶对位错滑移的阻碍作用。
从AP的高温放热温度、表观分解热及表观激活能等三方面评价了三种纳米粉的催化活性，高低次序为Ni-Cu合金纳米粉＞纯Ni纳米粉＞纯Cu纳米粉。用价键理论、能带理论研究了纯Ni纳米粉及纯Cu纳米粉催化AP的机理。结合多位理论研究了Ni-Cu合金纳米粉催化AP的机理，研究表明粉体内部结构中晶格畸变，孪晶、孔洞等缺陷，非均匀表面等多种因素的存在促进了粉体表面催化活性中心的形成。
Pure Ni, pure Cu, and Ni-Cu alloy nanopowders were prepared by the directcurrent arc plasma evaporation method. The effects of process parameters on the grainsize and yield of the three nanopowders were studied by an orthogonal experiment,and the optimal process conditions were determined. The growth mechanism of Ni-Cualloy nanopowders into Ni-Cu bulk alloys during the course of preparing and sinteringwas described. The mechanical properties and strengthening mechanism of Ni-Cualloy nanopowders consolidated by spark plasma sintering were studied. Comparedwith pure Ni and pure Cu nanopowders, the catalytic properties and catalyticmechanism of Ni-Cu alloy nanopowders on ammonium perchlorate (AP) were studiedby differential scanning calorimetry.
The optimal process conditions of Ni-Cu nanopowders were determined atcurrent of300A,1:1ratio of hydrogen to argon, and total gas pressure of0.06MPawhen the effect of the yield was evaluated. A current of300A, ratio,1:1ratio ofhydrogen and argon, and total gas pressure of0.07MPa were used when the effect ofthe grain size was evaluated. The optimal process conditions for both pure Ni and pureCu nanopowders were determined to be a current of300A,1:1ratio of hydrogen toargon, and total gas pressure of0.06MPa. Based on the classical nucleation theory,the growth driving force of Ni-Cu alloy nanopowders was studied according to theexperimental results.
We studied the phase composition, texture evolution, and grain morphologies ofNi-Cu bulk alloys sintered at different temperatures (773,823,873,923, and973K).The Ni-Cu bulk alloys had a single face-centered cubic phase. However, the peakintensity ratio of face (111) to face (200) I(111)/I(200)differed, indicating that the textureof the bulk materials evolved during sintering. FESEM photos showed that the particleshape gradually varied from spherical to polygonal. Based on TEM photos, thequantities of twins, dislocations, and pores were the primary reasons for the differentmechanical properties of the materials. The growth mechanism during the sintering of Ni-Cu alloy nanoparticles was discussed according to the crystal dynamic growththeory. The dynamic growth index and grain growth activation energy weredetermined.
The hardness values of Ni-Cu bulk alloys sintered at different temperatures wereseparately measured using a nanoindentation mechanical test machine and the Vickershardness test. The tensile strength, yield strength, and elongation were determined bytensile tests.
The strength mechanism of the Ni-Cu bulk alloys was discussed according to themechanism of deformation and fracture. The mechanical properties of the Ni-Cu bulkalloys was discussed based on the fine grain strengthening theory, which states that themechanical properties of Ni-Cu bulk alloys are superior to those of Ni-Cu bulk rawingots. However, the relationship between the strength and grain size did not obey theHall-Petch rule. The primary strength mechanism of the Ni-Cu bulk alloys was twinsstrength; their good mechanical properties mainly resulted from deformation twins,which prevented dislocation slip.
The catalytic properties of the three nanopowders were evaluated based on threeaspects, including exothermic peak at high temperatures, apparent decomposition heat,and apparent activation energy. The following trend was observed: Ni-Cu nanopowders>Ni nanopowders> Cu nanopowders. The catalytic mechanism of Ni and Cunanopowders on AP was investigated according to the valence bond and energy bandtheories. The catalytic mechanism of Ni-Cu alloy nanopowders on AP was studiedaccording to the multiplet theory, which states that various factors such as latticedistortion, defects (e.g., twins and pores), and non-uniform surface promote theformation of surface catalytic activity centers.
制备Ni-Cu合金纳米粉的最优化工艺条件为：以产率为指标时，电流300A、氢氩比1/1、气体总压0.06MPa；以粒径为指标时，电流300A、氢氩比1/1、气体总压0.07MPa。制备纯Ni及纯Cu纳米粉的最优化工艺条件均为：电流300A、氢氩比1/1、气体总压0.07MPa。结合实验结果，以经典成核理论为基础，研究了Ni-Cu合金纳米粉的晶体生长驱动力。
研究了在不同温度（773K，823K，873K，923K，973K）下烧结的Ni-Cu合金块体材料的相组成、织构演变和颗粒形貌特征。XRD结果显示，Ni-Cu合金块体均具有单一的面心立方结构，但XRD图中（111）及（200）面的峰强比值I(111)/I(200)不同，表明烧结过程中材料发生了织构演变。扫描电镜照片显示，随着温度升高，粒子尺寸逐渐增加，粒子形状从球形渐渐向多面体形状演变。依据透射电镜结果判断，不同烧结温度下材料中孪晶、位错及孔洞数量是导致材料性能差异的根本原因。结合晶体动力学生长理论研究了Ni-Cu合金纳米粉在烧结过程中的生长机制，计算了不同温度下烧结的Ni-Cu合金块体的动力学生长指数及晶粒生长激活能。
用纳米压痕机械试验仪及维氏硬度计分别测试了不同温度下烧结的Ni-Cu合金块体的硬度，并通过拉伸实验测试了其拉伸强度、屈服强度及延展率。
结合形变断裂过程研究了Ni-Cu合金块体材料的强化机制。用细晶强化理论研究了烧结的Ni-Cu合金块体材料的力学性能，Ni-Cu合金块体强度大于Ni-Cu原料合金锭的强度，但强度与粒径的关系不符合Hall-Petch关系。孪晶强化是Ni-Cu合金块体材料的主要强化机制，Ni-Cu合金块体材料力学性能的提高主要是因为变形孪晶对位错滑移的阻碍作用。
从AP的高温放热温度、表观分解热及表观激活能等三方面评价了三种纳米粉的催化活性，高低次序为Ni-Cu合金纳米粉＞纯Ni纳米粉＞纯Cu纳米粉。用价键理论、能带理论研究了纯Ni纳米粉及纯Cu纳米粉催化AP的机理。结合多位理论研究了Ni-Cu合金纳米粉催化AP的机理，研究表明粉体内部结构中晶格畸变，孪晶、孔洞等缺陷，非均匀表面等多种因素的存在促进了粉体表面催化活性中心的形成。
Pure Ni, pure Cu, and Ni-Cu alloy nanopowders were prepared by the directcurrent arc plasma evaporation method. The effects of process parameters on the grainsize and yield of the three nanopowders were studied by an orthogonal experiment,and the optimal process conditions were determined. The growth mechanism of Ni-Cualloy nanopowders into Ni-Cu bulk alloys during the course of preparing and sinteringwas described. The mechanical properties and strengthening mechanism of Ni-Cualloy nanopowders consolidated by spark plasma sintering were studied. Comparedwith pure Ni and pure Cu nanopowders, the catalytic properties and catalyticmechanism of Ni-Cu alloy nanopowders on ammonium perchlorate (AP) were studiedby differential scanning calorimetry.
The optimal process conditions of Ni-Cu nanopowders were determined atcurrent of300A,1:1ratio of hydrogen to argon, and total gas pressure of0.06MPawhen the effect of the yield was evaluated. A current of300A, ratio,1:1ratio ofhydrogen and argon, and total gas pressure of0.07MPa were used when the effect ofthe grain size was evaluated. The optimal process conditions for both pure Ni and pureCu nanopowders were determined to be a current of300A,1:1ratio of hydrogen toargon, and total gas pressure of0.06MPa. Based on the classical nucleation theory,the growth driving force of Ni-Cu alloy nanopowders was studied according to theexperimental results.
We studied the phase composition, texture evolution, and grain morphologies ofNi-Cu bulk alloys sintered at different temperatures (773,823,873,923, and973K).The Ni-Cu bulk alloys had a single face-centered cubic phase. However, the peakintensity ratio of face (111) to face (200) I(111)/I(200)differed, indicating that the textureof the bulk materials evolved during sintering. FESEM photos showed that the particleshape gradually varied from spherical to polygonal. Based on TEM photos, thequantities of twins, dislocations, and pores were the primary reasons for the differentmechanical properties of the materials. The growth mechanism during the sintering of Ni-Cu alloy nanoparticles was discussed according to the crystal dynamic growththeory. The dynamic growth index and grain growth activation energy weredetermined.
The hardness values of Ni-Cu bulk alloys sintered at different temperatures wereseparately measured using a nanoindentation mechanical test machine and the Vickershardness test. The tensile strength, yield strength, and elongation were determined bytensile tests.
The strength mechanism of the Ni-Cu bulk alloys was discussed according to themechanism of deformation and fracture. The mechanical properties of the Ni-Cu bulkalloys was discussed based on the fine grain strengthening theory, which states that themechanical properties of Ni-Cu bulk alloys are superior to those of Ni-Cu bulk rawingots. However, the relationship between the strength and grain size did not obey theHall-Petch rule. The primary strength mechanism of the Ni-Cu bulk alloys was twinsstrength; their good mechanical properties mainly resulted from deformation twins,which prevented dislocation slip.
The catalytic properties of the three nanopowders were evaluated based on threeaspects, including exothermic peak at high temperatures, apparent decomposition heat,and apparent activation energy. The following trend was observed: Ni-Cu nanopowders>Ni nanopowders> Cu nanopowders. The catalytic mechanism of Ni and Cunanopowders on AP was investigated according to the valence bond and energy bandtheories. The catalytic mechanism of Ni-Cu alloy nanopowders on AP was studiedaccording to the multiplet theory, which states that various factors such as latticedistortion, defects (e.g., twins and pores), and non-uniform surface promote theformation of surface catalytic activity centers.
引文
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