电沉积制备铜钴系颗粒膜及其巨磁电阻效应研究
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摘要
自从巨磁电阻效应于1988年发现以来,巨磁电阻(GMR)材料的开发和应用引起了广大科研人员的密切关注,带动了在物理学和材料学领域飞速进步。巨磁电阻效应可视为纳米电子学的一部分,并逐渐开辟了全新的磁电子学领域。本文采用传统的材料制备手段-电沉积工艺,制备了铜钴系颗粒膜材料,研究和分析了影响颗粒膜巨磁电阻效应的主要因素。
首先分析了电化学沉积制备CuCo颗粒膜的影响因素,发现制备过程中膜层的组成、晶粒大小与镀液的主盐离子质量浓度、络合剂质量浓度、pH值以及沉积时的电流密度有着直接的联系；电沉积过程中膜层逐步生长,铜优先析出于阴极表面,而钴沉积于铜沉积层上,膜层处于介稳态结构。
分析了铜钴颗粒膜中影响巨磁电阻效应的因素,发现膜层的磁阻值随着膜层中的Co浓度变化而改变,磁性组分适当增加有利于提高巨磁电阻效应,磁性组分过高使巨磁电阻效应降低当膜层中Co粒子的浓度为20%时出现最大值。面扫描元素分析和XRD分析表明：经过退火处理,膜层结构发生变化,出现了Co粒子的偏析,即出现了局部富钴的区域。
真空退火处理可以明显提高膜层的巨磁电阻效应。铜钴颗粒膜在450℃退火后,Cu80Co20薄膜出现最大GMR值,达到3.85%。更高温度退火处理后膜层的GMR值开始下降。磁性能测量发现随着退火温度的提高,Cu80Co20膜层的饱和磁化强度Ms、矫顽力Hc和剩余磁化强度Mr也随着变大。
应用唯象理论对Cu80Co20膜层的GMR值和磁滞回线进行了拟合,以及应用铁磁性理论分析了膜层中超顺磁性相的浓度,发现随着退火处理的进行,膜层中磁性颗粒开始生长,超顺磁性颗粒尺寸增加。唯象理论和有效媒介理论分析表明膜层中的磁性粒子的组分和尺寸是影响巨磁电阻效应的重要因素。
为了改变膜层的相分离,通过在CuCo镀液中添加Ni2+的方法电沉积制备了CuCoNi颗粒膜,发现膜层中Ni的含量与溶液中Ni2+的含量接近直线关系。XRD分析表明适量添加Ni有利于膜层中磁性颗粒的析出,过多的Ni反而降低了膜层中磁性粒子的浓度。
磁阻测量表明添加Ni后制备态的CuCoNi膜层较CuCo颗粒膜具有较高的GMR值,当经过退火处理后,其GMR值反而低于CuCo颗粒膜。磁性测量发现镀态样品饱和磁化强度较高,矫顽力较低,而真空退火处理使超顺磁性粒子转变为铁磁性粒子,提高了矫顽力。450℃退火处理后含Ni2.7%的CuCoNi膜层GMR达到最大值2.4%,具有最佳结构；更高温度则降低了GMR值。
出于细化铜钻颗粒膜晶粒的目的,在稳恒磁场下电沉积制备了铜钴颗粒膜,发现磁场颗粒膜组成随磁场强度变化而改变。当B⊥J时0.6T～0.8T下沉积的膜层中Co含量较高,更强磁场下反而抑制了Co的沉积。而当B//J时膜层中Co含量均超过20%,0.7T时达到30%。这主要是由于磁场所产生的洛仑兹力及顺磁力作用,以及MHD效应综合作用的结果。
B⊥J时对镀层有明显的细化作用,而当B//J时由于Co含量较高及磁场对镀层搅拌作用的加强,反而使膜层结晶粗大。XRD分析表明磁场对膜层的结晶有一定的影响,使铜钴镀层(111)晶面择优生长。
B⊥J磁场下电沉积颗粒膜可提高膜层的GMR值,在0.6T下制备的CuCo颗粒膜经过500℃热处理后最大GMR值为4.81%,较未加磁场的颗粒膜最大值提高了约25%,同时最佳的退火温度也提高到500℃。磁性测量表明0.6T下制备的CuCo颗粒膜经过500℃真空热处理后,相对于其他处理温度具有更好的磁性能,膜层中磁性组分与超顺磁性组分比例合理,促进了界面相关散射,具有较高的GMR值。
Since the discovery of giant magnetoresistance(GMR) in 1988, the development and application of GMR material have attracted more attention from the scientists, and achieved great progress in the fields of physics and material science. Giant magnetoresistance can be considered as a part of nanoelectronics, and established new field of magnetoelectronics. The copper-cobalt series granular films were prepared by conventional method-electrodeposition in the paper, main influencing factors of giant magnetoresistance in granular films were studied and analyzed.
First, influencing factors of electrodeposited process were analyzed. The components and particle size of the Cu-Co film were related with the concentration of the main salts and concentration of complexing reagent, pH value and current density. The films grown stage by stage during electrodeposited, the copper deposited on the surface of the cathode prior to cobalt, the cobalt deposited on the thin copper coating. The film was metastable state.
Main influencing factors of giant magnetoresistance for CuCo granular film were analyzed. The results show that the MR of the films was changed by the content of Co content in the film, it was favorite to the GMR value that the content of magnetic component increase properly, the maximum of GMR was occurred when the content of cobalt is 20% in the films, the GMR would decrease if the ferromagnetic component was too much. Surface scanning for elements analysis and XRD show that the separation of Co grain was occurred during annealing, and part Co-rich regions was appeared.
The annealing in vacuum can improve the GMR of the film. The maximum value of GMR was 3.85% which occurred at Cu80Co20 film after annealing at 450℃for 1h. With the annealing temperature increase, the electrical resistivity was dropped. The saturated magnetization Ms、coercive force Hc、remanence magnetization Mr were increased with improved annealing temperature by magnetic measurement.
The phenomenological theory was used to fit the GMR value and magnetic data for Cu80Co20 film. The content of ferromagnetic phase was analyzed by the application of ferromagnetic theory, which indicated that the magnetic grain began to grow up and the size of supperparamagnetism particle increased in the films during annealing. The results were analyzed by phenomenological theory and effectiveness medium theory showed that the component and the size of magnetic grain in the film were important to GMR.
In order to improve the phase separation for the film, the CuCoNi films were electrodeposited from the CuCo plating solutions added Ni2+. There was a linear relationship between Ni content in the films and Ni ion concentration in the baths. XRD results showed that the suitable content of Ni was favorable to the separation of magnetic particle in the films. More Ni addition would decrease the content of magnetic particles.
The magnetic measurement indicated that GMR of as-deposited CuCoNi films was higher than that of the films without Ni addition, but after annealing, GMR of CuCoNi films was no more increase than the CuCo films. The saturated magnetization was bigger and coercive force was smaller than that of the films without Ni addition. The superparamagnetic particles changed to ferromagnetic particles during annealing process, and coercive force was promoted. The maximum value of GMR was 2.4% for 2.7% of Ni content in the films annealed at 450℃. The optimum structure of films was appeared. GMR decreased after annealing at temperature over 450℃.
In order to gain the fine grain in the film, CuCo granular film was prepared by electrodeposition in the stable magnetic field. The composition of the film was changed with the intensity of the magnetic fields. When the magnetic fields was 0.6-0.8T at B⊥J, the Co content in the films was higher, and the Co deposition was restrained by stronger magnetic fields. The Co content was higher than 20% at B//J generally, and attach to 30% in 0.7T, which was due to effect of the Lorentz force and paramagnetic, and the influence of MHD.
The magnetic field could promote the refined crystal grains of the plating at B⊥J. and the crystal grains of films were more bigger at B//J, which included more Co in the films, the condition that the agitation of the solution was strengthened at this case also effect the deposition. XRD result showed that Magnetic field effected the crystallization of the granular film at some extent, and preferred the orientation of (111) crystal plane.
The films which deposited in magnetic fields at B⊥J promoted the value of GMR. The maximum of GMR in CuCo granular films which deposited in 0.6T magnetic field was 4.81% after 500℃annealed, which increased 25% than the films prepared without magnetic field, and the optimal annealing temperature enhanced to 500℃. The hysteresis loops indicated that granular film which prepared in 0.6T magnetic field at B⊥J after 500℃annealing 1h showed more well magnetic property than the films annealed at other temperature. The proportion of magnetic and superparamagnetic component in the films was optimal state, which promoted the scatting at interface and showed higher GMR.
首先分析了电化学沉积制备CuCo颗粒膜的影响因素,发现制备过程中膜层的组成、晶粒大小与镀液的主盐离子质量浓度、络合剂质量浓度、pH值以及沉积时的电流密度有着直接的联系；电沉积过程中膜层逐步生长,铜优先析出于阴极表面,而钴沉积于铜沉积层上,膜层处于介稳态结构。
分析了铜钴颗粒膜中影响巨磁电阻效应的因素,发现膜层的磁阻值随着膜层中的Co浓度变化而改变,磁性组分适当增加有利于提高巨磁电阻效应,磁性组分过高使巨磁电阻效应降低当膜层中Co粒子的浓度为20%时出现最大值。面扫描元素分析和XRD分析表明：经过退火处理,膜层结构发生变化,出现了Co粒子的偏析,即出现了局部富钴的区域。
真空退火处理可以明显提高膜层的巨磁电阻效应。铜钴颗粒膜在450℃退火后,Cu80Co20薄膜出现最大GMR值,达到3.85%。更高温度退火处理后膜层的GMR值开始下降。磁性能测量发现随着退火温度的提高,Cu80Co20膜层的饱和磁化强度Ms、矫顽力Hc和剩余磁化强度Mr也随着变大。
应用唯象理论对Cu80Co20膜层的GMR值和磁滞回线进行了拟合,以及应用铁磁性理论分析了膜层中超顺磁性相的浓度,发现随着退火处理的进行,膜层中磁性颗粒开始生长,超顺磁性颗粒尺寸增加。唯象理论和有效媒介理论分析表明膜层中的磁性粒子的组分和尺寸是影响巨磁电阻效应的重要因素。
为了改变膜层的相分离,通过在CuCo镀液中添加Ni2+的方法电沉积制备了CuCoNi颗粒膜,发现膜层中Ni的含量与溶液中Ni2+的含量接近直线关系。XRD分析表明适量添加Ni有利于膜层中磁性颗粒的析出,过多的Ni反而降低了膜层中磁性粒子的浓度。
磁阻测量表明添加Ni后制备态的CuCoNi膜层较CuCo颗粒膜具有较高的GMR值,当经过退火处理后,其GMR值反而低于CuCo颗粒膜。磁性测量发现镀态样品饱和磁化强度较高,矫顽力较低,而真空退火处理使超顺磁性粒子转变为铁磁性粒子,提高了矫顽力。450℃退火处理后含Ni2.7%的CuCoNi膜层GMR达到最大值2.4%,具有最佳结构；更高温度则降低了GMR值。
出于细化铜钻颗粒膜晶粒的目的,在稳恒磁场下电沉积制备了铜钴颗粒膜,发现磁场颗粒膜组成随磁场强度变化而改变。当B⊥J时0.6T～0.8T下沉积的膜层中Co含量较高,更强磁场下反而抑制了Co的沉积。而当B//J时膜层中Co含量均超过20%,0.7T时达到30%。这主要是由于磁场所产生的洛仑兹力及顺磁力作用,以及MHD效应综合作用的结果。
B⊥J时对镀层有明显的细化作用,而当B//J时由于Co含量较高及磁场对镀层搅拌作用的加强,反而使膜层结晶粗大。XRD分析表明磁场对膜层的结晶有一定的影响,使铜钴镀层(111)晶面择优生长。
B⊥J磁场下电沉积颗粒膜可提高膜层的GMR值,在0.6T下制备的CuCo颗粒膜经过500℃热处理后最大GMR值为4.81%,较未加磁场的颗粒膜最大值提高了约25%,同时最佳的退火温度也提高到500℃。磁性测量表明0.6T下制备的CuCo颗粒膜经过500℃真空热处理后,相对于其他处理温度具有更好的磁性能,膜层中磁性组分与超顺磁性组分比例合理,促进了界面相关散射,具有较高的GMR值。
Since the discovery of giant magnetoresistance(GMR) in 1988, the development and application of GMR material have attracted more attention from the scientists, and achieved great progress in the fields of physics and material science. Giant magnetoresistance can be considered as a part of nanoelectronics, and established new field of magnetoelectronics. The copper-cobalt series granular films were prepared by conventional method-electrodeposition in the paper, main influencing factors of giant magnetoresistance in granular films were studied and analyzed.
First, influencing factors of electrodeposited process were analyzed. The components and particle size of the Cu-Co film were related with the concentration of the main salts and concentration of complexing reagent, pH value and current density. The films grown stage by stage during electrodeposited, the copper deposited on the surface of the cathode prior to cobalt, the cobalt deposited on the thin copper coating. The film was metastable state.
Main influencing factors of giant magnetoresistance for CuCo granular film were analyzed. The results show that the MR of the films was changed by the content of Co content in the film, it was favorite to the GMR value that the content of magnetic component increase properly, the maximum of GMR was occurred when the content of cobalt is 20% in the films, the GMR would decrease if the ferromagnetic component was too much. Surface scanning for elements analysis and XRD show that the separation of Co grain was occurred during annealing, and part Co-rich regions was appeared.
The annealing in vacuum can improve the GMR of the film. The maximum value of GMR was 3.85% which occurred at Cu80Co20 film after annealing at 450℃for 1h. With the annealing temperature increase, the electrical resistivity was dropped. The saturated magnetization Ms、coercive force Hc、remanence magnetization Mr were increased with improved annealing temperature by magnetic measurement.
The phenomenological theory was used to fit the GMR value and magnetic data for Cu80Co20 film. The content of ferromagnetic phase was analyzed by the application of ferromagnetic theory, which indicated that the magnetic grain began to grow up and the size of supperparamagnetism particle increased in the films during annealing. The results were analyzed by phenomenological theory and effectiveness medium theory showed that the component and the size of magnetic grain in the film were important to GMR.
In order to improve the phase separation for the film, the CuCoNi films were electrodeposited from the CuCo plating solutions added Ni2+. There was a linear relationship between Ni content in the films and Ni ion concentration in the baths. XRD results showed that the suitable content of Ni was favorable to the separation of magnetic particle in the films. More Ni addition would decrease the content of magnetic particles.
The magnetic measurement indicated that GMR of as-deposited CuCoNi films was higher than that of the films without Ni addition, but after annealing, GMR of CuCoNi films was no more increase than the CuCo films. The saturated magnetization was bigger and coercive force was smaller than that of the films without Ni addition. The superparamagnetic particles changed to ferromagnetic particles during annealing process, and coercive force was promoted. The maximum value of GMR was 2.4% for 2.7% of Ni content in the films annealed at 450℃. The optimum structure of films was appeared. GMR decreased after annealing at temperature over 450℃.
In order to gain the fine grain in the film, CuCo granular film was prepared by electrodeposition in the stable magnetic field. The composition of the film was changed with the intensity of the magnetic fields. When the magnetic fields was 0.6-0.8T at B⊥J, the Co content in the films was higher, and the Co deposition was restrained by stronger magnetic fields. The Co content was higher than 20% at B//J generally, and attach to 30% in 0.7T, which was due to effect of the Lorentz force and paramagnetic, and the influence of MHD.
The magnetic field could promote the refined crystal grains of the plating at B⊥J. and the crystal grains of films were more bigger at B//J, which included more Co in the films, the condition that the agitation of the solution was strengthened at this case also effect the deposition. XRD result showed that Magnetic field effected the crystallization of the granular film at some extent, and preferred the orientation of (111) crystal plane.
The films which deposited in magnetic fields at B⊥J promoted the value of GMR. The maximum of GMR in CuCo granular films which deposited in 0.6T magnetic field was 4.81% after 500℃annealed, which increased 25% than the films prepared without magnetic field, and the optimal annealing temperature enhanced to 500℃. The hysteresis loops indicated that granular film which prepared in 0.6T magnetic field at B⊥J after 500℃annealing 1h showed more well magnetic property than the films annealed at other temperature. The proportion of magnetic and superparamagnetic component in the films was optimal state, which promoted the scatting at interface and showed higher GMR.
引文
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