磁控溅射Ni-Mn-Ga合金薄膜的相变行为与性能
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摘要
本文利用磁控溅射方法制备了Ni-Mn-Ga磁性形状记忆合金薄膜,研究了溅射工艺对薄膜表面形貌、化学成分的影响规律,揭示了影响薄膜化学成分的物理机制;采用示差扫描热分析、X射线衍射分析、透射电子显微观察、磁学和光学性能测试等手段研究了薄膜的马氏体相变行为、微观组织、磁致应变和光学反射率,确定了大光学反射率薄膜的马氏体晶体结构。
研究表明,溅射工艺对Ni-Mn-Ga薄膜的表面粗糙度和化学成分有显著影响。薄膜表面粗糙度随Ar工作压强和溅射功率的增大以及衬底温度的升高而增大。薄膜中Ni含量随溅射功率的增大而减少,随衬底负偏压的增大而增加;Mn与Ga含量随溅射功率的增大而增加,随衬底负偏压的增大而减少。
研究发现,沉积态薄膜存在残余压应力,且随膜厚的增大而减小,随衬底负偏压的增加而增大。沉积于未加热衬底的薄膜室温下处于部分结晶状态,晶化过程中残余压应力有助于减小薄膜体积,促进晶化,导致晶化激活能降低,经823K退火1小时后,薄膜完全晶化。
Ni-Mn-Ga薄膜在冷却和加热过程中发生一步热弹性马氏体相变与逆相变。价电子浓度的增大导致母相稳定性降低,使薄膜马氏体相变温度升高。Ni56Mn27Ga17薄膜的Ms温度高达584K,可望成为有应用前景的高温形状记忆薄膜。采用纳米压痕测试发现Ni49.34Mn26.96Ga23.4、Ni48.82Mn27.14Ga24.04和Ni47.95Mn26.75Ga25.3薄膜具有超弹性行为。
透射电镜观察证实,薄膜晶粒尺寸仅为200～500nm,低于Ni-Mn-Ga合金块材晶粒尺寸约两个数量级以上。Ni54Mn25.1Ga20.9薄膜室温下处于马氏体状态,为七层调制正交结构,马氏体亚结构为(011)I型孪晶,马氏体变体界面清晰、平直。非调制四方结构Ni56Mn27Ga17薄膜马氏体基体内存在立方结构γ相,其马氏体亚结构为(111)I型孪晶。
磁学和光学性能测量表明,Ni-Mn-Ga薄膜的居里温度对成分不敏感。薄膜的饱和磁化强度、矫顽力和剩磁均随测试温度的降低而增大。Ni-Mn-Ga薄膜的磁致应变显著依赖于测试温度。当测试温度低于Af温度时,Ni49.34Mn26.96Ga23.4和Ni50.3Mn27.3Ga22.4薄膜的饱和磁致应变随测试温度的升高先增大后减小,在Ms温度附近达最大值。当测试温度低于Mf温度时,Ni49.33Mn30.1Ga20.57薄膜的饱和磁致应变随测试温度的降低而增大。处于马氏体状态的Ni-Mn-Ga薄膜的光学反射率显著依赖于表面粗糙度和晶体结构,随表面均方根粗糙度的增大而降低。在5M、7M和T型马氏体中,具有非调制四方结构的T型马氏体薄膜光学反射率最大。
Ni-Mn-Ga magnetic shape memory alloy thin films have been fabricated by usig magnetron sputtering technique. The results clarify the effect of sputtering parameters on surface morphology and chemical compositions of Ni-Mn-Ga thin films, revealing the physical mechanism of composition variations. At the same time, martensitic transformation, microstructure, magnetic-field-induced strain and optical reflectivity of the thin films have been systematically investigated by means of DSC, XRD, TEM, magnetic and optical properties measurements, respectively. The martensitic structure of Ni-Mn-Ga thin films with high reflectivity is determined.
The experimental results show that process parameters have remarkable influence on surface roughness and chemical compositions of Ni-Mn-Ga thin films. The surface roughness of the thin films increases with increasing Ar working pressure, sputtering power and substrate temperature. It is shown that Ni content in Ni-Mn-Ga thin films decreases with increasing the sputtering power and increases with the substrate negative bias voltage increasing, whereas Mn and Ga content increase with increasing the sputtering power and decrease with the substrate negative bias voltage increasing.
According to experimental results, residual compressive stress exists in Ni-Mn-Ga thin films. The residual compressive stress dramatically depends on film thickness and the substrate negative bias voltage, decreasing with increasing film thickness and increasing with the substrate negative bias voltage increasing. Based on XRD and DSC analysis, the as-deposited Ni-Mn-Ga thin films are in partially crystallized state when substrates are not heated. During crystallization the residual compressive stress is beneficial to reducing the volume of Ni-Mn-Ga thin films, consequently facilitating crystallization of the thin films. As a result, the crystallization activation energy decreases with increasing residual compressive stress. After annealing at 823K for 1 hour, the as-deposited Ni-Mn-Ga thin films are fully crystallized.
It is shown that Ni-Mn-Ga thin films undergo one-step thermoelastic martensitic transformation during the process of cooling and heating. And martensitic transformation temperatures increase with increasing valence electron concentration due to the instability of parent phase with a larger valence electron concentration. It is found that the temperature Ms of Ni56Mn27Ga17 thin film can approach as high as 584K, which causes this thin film to be a potential high temperature shape memory alloy thin film. In addition, superelasticity in Ni-Mn-Ga thin films has been obtained during loading and unloading in Nanoindentation experiments.
Based on TEM observations, it is found that the grain size of Ni-Mn-Ga thin films is in the range between 200 and 500nm, two orders of magnitude smaller than that of Ni-Mn-Ga bulk alloys. Ni54Mn25.1Ga20.9 thin film is in martensite state at room temperature, and the film is determined to be seven-layered modulated orthorhombic structure. For Ni56Mn27Ga17 thin film, the body-centered cubicγphase exists in the matrix of non-modulated tetragonal martensite. From TEM and HREM observations, the interfaces of martensite variants in Ni-Mn-Ga thin films are clear and straight. And the substructure of martensite variants in Ni54Mn25.1Ga20.9 and Ni56Mn27Ga17 thin film are type I (011) and (111) twin relationship, respectively.
In terms of the analysis of magnetic properties, it is found that the Curie temperatures of Ni-Mn-Ga thin films are insensitive to film compositions, and the saturation magnetization, coercive force and residual magnetization of Ni-Mn-Ga thin films increase with decreasing operation temperature. It is also shown that the saturated magnetic-field-induced strains (MFIS) of Ni-Mn-Ga thin films remarkably depend on operation temperatures. The saturated MFIS of Ni49.34Mn26.96Ga23.4 and Ni50.3Mn27.3Ga22.4 thin films firstly increases and then decreases with increasing operation temperature below Af, and the maximum saturated MFIS can be obtained around Ms temperature. When the operation temperature is lower than Mf,the saturated MFIS of Ni49.33Mn30.1Ga20.57 thin film increases with decreasing operation temperature. It is found that reflectivity of Ni-Mn-Ga thin film through optical properties measurements is closely related to film surface roughness and crystallographic structure. The reflectivities of Ni-Mn-Ga thin films in martensite state have a remarkable dependence on crystal structure and surface roughness. The reflectivities of Ni-Mn-Ga thin films increase with increasing root-mean-square surface roughness of the thin films. Among Ni-Mn-Ga thin films with various martensitic structures (5M, 7M and T), the reflectivity of the non-modulated Ni-Mn-Ga thin film is larger than those of Ni-Mn-Ga thin films with 5M or 7M structure.
研究表明,溅射工艺对Ni-Mn-Ga薄膜的表面粗糙度和化学成分有显著影响。薄膜表面粗糙度随Ar工作压强和溅射功率的增大以及衬底温度的升高而增大。薄膜中Ni含量随溅射功率的增大而减少,随衬底负偏压的增大而增加;Mn与Ga含量随溅射功率的增大而增加,随衬底负偏压的增大而减少。
研究发现,沉积态薄膜存在残余压应力,且随膜厚的增大而减小,随衬底负偏压的增加而增大。沉积于未加热衬底的薄膜室温下处于部分结晶状态,晶化过程中残余压应力有助于减小薄膜体积,促进晶化,导致晶化激活能降低,经823K退火1小时后,薄膜完全晶化。
Ni-Mn-Ga薄膜在冷却和加热过程中发生一步热弹性马氏体相变与逆相变。价电子浓度的增大导致母相稳定性降低,使薄膜马氏体相变温度升高。Ni56Mn27Ga17薄膜的Ms温度高达584K,可望成为有应用前景的高温形状记忆薄膜。采用纳米压痕测试发现Ni49.34Mn26.96Ga23.4、Ni48.82Mn27.14Ga24.04和Ni47.95Mn26.75Ga25.3薄膜具有超弹性行为。
透射电镜观察证实,薄膜晶粒尺寸仅为200～500nm,低于Ni-Mn-Ga合金块材晶粒尺寸约两个数量级以上。Ni54Mn25.1Ga20.9薄膜室温下处于马氏体状态,为七层调制正交结构,马氏体亚结构为(011)I型孪晶,马氏体变体界面清晰、平直。非调制四方结构Ni56Mn27Ga17薄膜马氏体基体内存在立方结构γ相,其马氏体亚结构为(111)I型孪晶。
磁学和光学性能测量表明,Ni-Mn-Ga薄膜的居里温度对成分不敏感。薄膜的饱和磁化强度、矫顽力和剩磁均随测试温度的降低而增大。Ni-Mn-Ga薄膜的磁致应变显著依赖于测试温度。当测试温度低于Af温度时,Ni49.34Mn26.96Ga23.4和Ni50.3Mn27.3Ga22.4薄膜的饱和磁致应变随测试温度的升高先增大后减小,在Ms温度附近达最大值。当测试温度低于Mf温度时,Ni49.33Mn30.1Ga20.57薄膜的饱和磁致应变随测试温度的降低而增大。处于马氏体状态的Ni-Mn-Ga薄膜的光学反射率显著依赖于表面粗糙度和晶体结构,随表面均方根粗糙度的增大而降低。在5M、7M和T型马氏体中,具有非调制四方结构的T型马氏体薄膜光学反射率最大。
Ni-Mn-Ga magnetic shape memory alloy thin films have been fabricated by usig magnetron sputtering technique. The results clarify the effect of sputtering parameters on surface morphology and chemical compositions of Ni-Mn-Ga thin films, revealing the physical mechanism of composition variations. At the same time, martensitic transformation, microstructure, magnetic-field-induced strain and optical reflectivity of the thin films have been systematically investigated by means of DSC, XRD, TEM, magnetic and optical properties measurements, respectively. The martensitic structure of Ni-Mn-Ga thin films with high reflectivity is determined.
The experimental results show that process parameters have remarkable influence on surface roughness and chemical compositions of Ni-Mn-Ga thin films. The surface roughness of the thin films increases with increasing Ar working pressure, sputtering power and substrate temperature. It is shown that Ni content in Ni-Mn-Ga thin films decreases with increasing the sputtering power and increases with the substrate negative bias voltage increasing, whereas Mn and Ga content increase with increasing the sputtering power and decrease with the substrate negative bias voltage increasing.
According to experimental results, residual compressive stress exists in Ni-Mn-Ga thin films. The residual compressive stress dramatically depends on film thickness and the substrate negative bias voltage, decreasing with increasing film thickness and increasing with the substrate negative bias voltage increasing. Based on XRD and DSC analysis, the as-deposited Ni-Mn-Ga thin films are in partially crystallized state when substrates are not heated. During crystallization the residual compressive stress is beneficial to reducing the volume of Ni-Mn-Ga thin films, consequently facilitating crystallization of the thin films. As a result, the crystallization activation energy decreases with increasing residual compressive stress. After annealing at 823K for 1 hour, the as-deposited Ni-Mn-Ga thin films are fully crystallized.
It is shown that Ni-Mn-Ga thin films undergo one-step thermoelastic martensitic transformation during the process of cooling and heating. And martensitic transformation temperatures increase with increasing valence electron concentration due to the instability of parent phase with a larger valence electron concentration. It is found that the temperature Ms of Ni56Mn27Ga17 thin film can approach as high as 584K, which causes this thin film to be a potential high temperature shape memory alloy thin film. In addition, superelasticity in Ni-Mn-Ga thin films has been obtained during loading and unloading in Nanoindentation experiments.
Based on TEM observations, it is found that the grain size of Ni-Mn-Ga thin films is in the range between 200 and 500nm, two orders of magnitude smaller than that of Ni-Mn-Ga bulk alloys. Ni54Mn25.1Ga20.9 thin film is in martensite state at room temperature, and the film is determined to be seven-layered modulated orthorhombic structure. For Ni56Mn27Ga17 thin film, the body-centered cubicγphase exists in the matrix of non-modulated tetragonal martensite. From TEM and HREM observations, the interfaces of martensite variants in Ni-Mn-Ga thin films are clear and straight. And the substructure of martensite variants in Ni54Mn25.1Ga20.9 and Ni56Mn27Ga17 thin film are type I (011) and (111) twin relationship, respectively.
In terms of the analysis of magnetic properties, it is found that the Curie temperatures of Ni-Mn-Ga thin films are insensitive to film compositions, and the saturation magnetization, coercive force and residual magnetization of Ni-Mn-Ga thin films increase with decreasing operation temperature. It is also shown that the saturated magnetic-field-induced strains (MFIS) of Ni-Mn-Ga thin films remarkably depend on operation temperatures. The saturated MFIS of Ni49.34Mn26.96Ga23.4 and Ni50.3Mn27.3Ga22.4 thin films firstly increases and then decreases with increasing operation temperature below Af, and the maximum saturated MFIS can be obtained around Ms temperature. When the operation temperature is lower than Mf,the saturated MFIS of Ni49.33Mn30.1Ga20.57 thin film increases with decreasing operation temperature. It is found that reflectivity of Ni-Mn-Ga thin film through optical properties measurements is closely related to film surface roughness and crystallographic structure. The reflectivities of Ni-Mn-Ga thin films in martensite state have a remarkable dependence on crystal structure and surface roughness. The reflectivities of Ni-Mn-Ga thin films increase with increasing root-mean-square surface roughness of the thin films. Among Ni-Mn-Ga thin films with various martensitic structures (5M, 7M and T), the reflectivity of the non-modulated Ni-Mn-Ga thin film is larger than those of Ni-Mn-Ga thin films with 5M or 7M structure.
引文
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