3d过渡金属掺杂In_2O_3稀磁半导体材料的制备与研究
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摘要
稀磁半导体材料具有可以同时利用电子电荷和电子自旋的属性,表现出优异的磁、磁光、磁电性能,使其在自旋电子学领域有广阔的应用前景,已成为材料领域的研究热点。In203是一种透明的,宽禁带(3.75 eV)半导体,具有立方方铁锰矿结构,对过渡金属离子有较大的固熔量,可有效避免二次杂质相的产生,形成均相结构的稀磁半导体。因此,过渡金属掺杂In203稀磁半导体的研究备受人们的关注。本论文采用固相反应、真空退火技术和脉冲激光沉积方法在In203半导体中掺入了Fe、Mn和Cr过渡金属元素,通过分析样品的结构、磁性和电子输运特性等之间的关系,对样品的铁磁性来源和磁性机制进行了探讨。主要研究内容如下：
(1)采用固态反应方法和真空退火技术制备了(In1-xFex)2O3 (x=0.02,0.05,0.2)粉末。系统研究了Fe含量和真空退火温度对(In1-xFex)2O3粉末结构和磁性的影响。结果表明,Fe离子进入到In203的立方晶格取代了In离子,样品为均匀的单相结构,样品表现出明显的铁磁性,居里温度高达793 K,Fe含量和真空退火温度对样品的铁磁性有重要影响。一系列结构和磁性测量结果表明,(In1-xFex)2O3粉末的铁磁性不是来源于Fe团簇或者Fe的氧化物二次相,而是和氧空位密切相关。
(2)采用脉冲激光沉积技术在A12O3(0001)基片上制备了Fe掺杂In203薄膜,系统研究了Fe含量和氧气分压对薄膜的结构、组成、磁性和输运性质的影响。X射线衍射表明(In1-xFex)2O3薄膜为均匀的单相立方方铁锰矿In2O3结构,以In2O3 (222)择优取向,且Fe已取代了In203晶格中的In; X射线光电子能谱表明当氧气分压较低时,薄膜中Fe以Fe2+和Fe3+离子的形式存在,当氧气分压较高时Fe以Fe3+离子的形式存在。(In1-xFex)2O3薄膜表现出明显的室温铁磁性,其导电类型为n型。薄膜的载流子浓度与Fe含量和氧气分压密切相关,并且大部分薄膜处于金属区,一部分薄膜处于绝缘区。进一步分析表明,处于金属区的薄膜,其铁磁性与载流子浓度密切相关,载流子浓度越高,磁性越大,铁磁性来源符合载流子诱导机制；处于绝缘区的薄膜,其载流子浓度很小,在低温时的输运性质符合Mott的变程跳跃机制,铁磁性来源符合束缚磁极子理论。磁光效应测量结果进一步说明(In1-xFeX)203薄膜的铁磁性是本征的,来源于Fe取代了In的均相结构。
(3)采用真空退火技术和脉冲激光沉积技术制备了Sn和Cu共掺杂的(In0.92Fe0.05Sn0.03)2O3和(In0.92Fe0.05Cu0.03)2O3粉末和薄膜,研究了共掺杂剂Sn和Cu对样品结构、磁性与输运等性质的不同影响。虽然X射线衍射测量结果表明(In0.92Fe0.05Sn0.03)2O3和(In0.92Fe0.05Cu0.03)2O3粉末为均匀的单相结构,但是场冷却-零场冷却测量结果表明样品的室温铁磁性都来源于样品中的Fe3O4纳米颗粒。然而,(In0.92Fe0.05Sn0.03)2O3和(In0.92Fe0.05Cu0.03)2o3薄膜的铁磁性来源明显不同。(In0.92Fe0.05Sn0.03)2O3薄膜中Fe-Sn易于形成非补偿性p-n对,而p-n对受主和施主离子之间存在静电作用,很容易同时取代两个近邻位的阳离子,使整个体系能量降低,阻止了Fe离子的化合和团聚。同时各种表征手段也都没有检测到任何二次相,因此我们认为(In0.92Fe0.05Sn0.03)2O3薄膜的铁磁性是本征的,来源于Fe和Sn取代了In的均相结构；而且Sn的掺入可以有效增大体系的载流子浓度,其磁性来源于载流子诱导机制。对于Fe-Cu共掺杂的(In0.92Fe0.05Cu0.03)2O3薄膜中有金属Fe团簇生成,这是稀磁半导体所不期望的。
(4)采用脉冲激光沉积技术在A12O3 (0001)基片上成功制备了Mn和Cr掺杂的In203薄膜。Mn掺杂In203薄膜的铁磁性表现出可逆性,通过控制掺入薄膜中Sn的含量控制其载流子浓度,薄膜的铁磁性可在“开”和“关”之间转换。额外载流子的存在对Cr掺杂In203薄膜的铁磁性有重要影响,在薄膜中加入了1%的Sn后,由于载流子浓度的增加,薄膜的铁磁性明显增强,饱和磁化强度达2.10μB/Cr。重要的是,我们的实验结果表明载流子浓度和自旋对样品铁磁性的产生都非常重要。
总之,我们制备了不同过渡金属元素掺杂的In203基稀磁半导体,研究了样品的结构、磁性和输运等性质。发现载流子浓度对样品的铁磁性有重要影响,载流子浓度较大的铁磁性薄膜在新一代自旋电子器件中有广阔的应用前景。
Diluted magnetic semiconductos (DMSs) have attracted great interest for their potential applications in spintronic devices because the charge and spin of carriers can be simultaneously controlled. In2O3 is a wide band gap (3.75 eV) transparent semiconductor with cubic bixbyite crystal structure. The solubility of transition metal (TM) in In2O3 host lattice was found to be very high, which can effectively avoid the formation of magneitc impurities and also makes it possible to obtain homogenous DMSs for application. In this work, Fe, Mn and Cr doped In2O3 samples were prepared by solid state reaction, a vacuum annealing process and pulsed laser deposition technique. Based on the systematical studies of the structure, magnetism and transport properties of the samples, the origin and mechanism of ferromagnetism in In2O3-based DMSs were discussed. The results are summarized as follows:
(1) (In1-xFex)2O3 (x=0.02,0.05,0.2) powders were prepared by a solid state reaction method and a vacuum annealing process. A systematic study was done on the structural and magnetic properties of (In1-xFex)2O3 powders as a function of Fe concentration and annealing temperature. The (In1-xFex)2O3 powders appear to be homogeneous and single-phase materials, where Fe elements incorporate into the In sites of the In2O3 lattice rather than forming any secondary phases. The samples were ferromagnetic with the magnetic moment of 0.49-1.73μB/Fe and the Curie temperature around 793 K. The results indicate that the observed high temperature ferromagnetism of vacuum-annealed (In1-xFex)2O3 powders is intrinsic rather than from any magnetic impurities, and is attributed to the ferromagnetic coupling of Fe2+and Fe3+ions via an electron trapped in a bridging oxygen vacancy.
(2) Fe-doped In2O3 thin films are deposited on sapphire substrates using pulsed laser ablation. The effects of Fe concentration and oxygen partial pressure on the structure, magnetism and transport properties of (In1-xFex)2O3 films are studied systematically. A detailed analysis of the structural properties suggests the substitution of Fe dopant atoms into In lattice sites and the films are textured with (222) orientation. X-ray photoelectron spectroscopy indicates that the valence of substituted Fe in the (In1-xFex)2O3 films varies with oxygen partial pressure, at lower oxygen partial pressures, Fe behaves as a mixture of+2 and +3 valences, whereas Fe3+dominates in the films grown at higher oxygen pressures. Systematic investigations of transport properties for (In1-xFex)2O3 films with a wide range of carrier densities reveal that they occur in both metallic and insulating regimes. The insulating films exhibit variable range hopping at low temperatures and show temperature dependent ferromagnetism, which can be explained by bound magnetic polarons mechanism. For the metallic films, the carrier densities play a crucial role in their robust ferromagnetism and the resistivity and magnetization are independent of temperature; the carrier-mediated exchange mechanism has been suggested as responsible for magnetic ordering in these metallic films. Optical absorption and magneto-optic studies of (In1-xFex)2O3 films indicate further differences between metallic and semiconducting films and show significant magnetic circular dichroism below the In2O3 band edge at room temperature, which also implies intrinsic ferromagnetism.
(3) (In0.92Fe0.05Sn0.03)2O3 and (In0.92Fe0.05Cu0.03)2O3 powders and films were prepared by a vacuum annealing process and a pulsed laser deposition technique, respectively. The effects of codpants Sn and Cu on the structure, magnetism and transport properties of samples have been investigated. The zero-field-cooled and field-cooled magnetic measurement indicated that the room temperature ferromagnetism of (In0.92Fe0.05Sn0.03)2O3 and (In0.92Fe0.05Cu0.03)2O3 powders both originate from the Fe3O4 nanoparticles although the x-ray diffraction results revealed no crystalline phase other than cubic bixbyite structure In2O3 to be present in the powders. However, the origin of ferromagnetism for (In0.92Fe0.05Sn0.03)2O3 and (In0.92Fe0.05Cu0.03)2O3 films is very different. In (In0.92Fe0.05Sn0.03)2O3 film, the Fe-Sn can constitute p-n pairs. The Columbic attraction between the n- and p-type dopants with opposite charge state substantially enhances both the thermodynamic and, in particular, the kinetic solubilities of the dopant pairs in concerted substitutional doping. More profoundly, the noncompensated p-n pairs of Fe-Sn prevented the aggregation of Fe ions. The mictostructure and magnetic analyses also confirmed that there was no segregation of any secondary phases. So the room temperature ferromagnetism of (In0.92Fe0.05Sn0.03)2O3 film is intrinsic rather than from any other magnetic impurity phases. The magnetic behavior is consistent with a carrier-induced ferromagnetism model. While, the (In0.92Fe0.05Cu0.03)2O3 film was superparamagnetic, and the observed ferromagnetism originated from the nanometer-sized Fe clusters, which is not desirable for device application.
(4) Mn and Cr-doped In2O3 films with Sn co-doping were deposited on sapphire substrate by pulsed laser deposition. The ferromagnetism of Mn-doped In2O3 films shows reversible behavior, which can be switched between "on" and "off" states by controlling the carrier density via varying Sn concentration. The enhanced ferromagnetism in Cr-doped In2O3 films is observed due to the significant increase in the carrier density with Sn doping, and the saturation magnetization can reach 2.10μB/Cr. Most importantly, both of the experiment results reveal that the carrier density and the net spin are two crucial factors for producing and tuning ferromagnetism.
In summary, we have prepared different TMs doped In2O3 DMSs materials and studied the various properties of the samples. The results reveal that the carrier densities play a crucial role in the ferromagnetism and the dependence of the magnetism on the carrier density lend support to carrier-mediated mechanism. This clear demonstration of carrier-mediated ferromagnetism at high carrier concentration implies that TMs-doped In2O3 can be used as n-type DMSs at RT, with consequent potential for exploitation in spintronic applications.
(1)采用固态反应方法和真空退火技术制备了(In1-xFex)2O3 (x=0.02,0.05,0.2)粉末。系统研究了Fe含量和真空退火温度对(In1-xFex)2O3粉末结构和磁性的影响。结果表明,Fe离子进入到In203的立方晶格取代了In离子,样品为均匀的单相结构,样品表现出明显的铁磁性,居里温度高达793 K,Fe含量和真空退火温度对样品的铁磁性有重要影响。一系列结构和磁性测量结果表明,(In1-xFex)2O3粉末的铁磁性不是来源于Fe团簇或者Fe的氧化物二次相,而是和氧空位密切相关。
(2)采用脉冲激光沉积技术在A12O3(0001)基片上制备了Fe掺杂In203薄膜,系统研究了Fe含量和氧气分压对薄膜的结构、组成、磁性和输运性质的影响。X射线衍射表明(In1-xFex)2O3薄膜为均匀的单相立方方铁锰矿In2O3结构,以In2O3 (222)择优取向,且Fe已取代了In203晶格中的In; X射线光电子能谱表明当氧气分压较低时,薄膜中Fe以Fe2+和Fe3+离子的形式存在,当氧气分压较高时Fe以Fe3+离子的形式存在。(In1-xFex)2O3薄膜表现出明显的室温铁磁性,其导电类型为n型。薄膜的载流子浓度与Fe含量和氧气分压密切相关,并且大部分薄膜处于金属区,一部分薄膜处于绝缘区。进一步分析表明,处于金属区的薄膜,其铁磁性与载流子浓度密切相关,载流子浓度越高,磁性越大,铁磁性来源符合载流子诱导机制；处于绝缘区的薄膜,其载流子浓度很小,在低温时的输运性质符合Mott的变程跳跃机制,铁磁性来源符合束缚磁极子理论。磁光效应测量结果进一步说明(In1-xFeX)203薄膜的铁磁性是本征的,来源于Fe取代了In的均相结构。
(3)采用真空退火技术和脉冲激光沉积技术制备了Sn和Cu共掺杂的(In0.92Fe0.05Sn0.03)2O3和(In0.92Fe0.05Cu0.03)2O3粉末和薄膜,研究了共掺杂剂Sn和Cu对样品结构、磁性与输运等性质的不同影响。虽然X射线衍射测量结果表明(In0.92Fe0.05Sn0.03)2O3和(In0.92Fe0.05Cu0.03)2O3粉末为均匀的单相结构,但是场冷却-零场冷却测量结果表明样品的室温铁磁性都来源于样品中的Fe3O4纳米颗粒。然而,(In0.92Fe0.05Sn0.03)2O3和(In0.92Fe0.05Cu0.03)2o3薄膜的铁磁性来源明显不同。(In0.92Fe0.05Sn0.03)2O3薄膜中Fe-Sn易于形成非补偿性p-n对,而p-n对受主和施主离子之间存在静电作用,很容易同时取代两个近邻位的阳离子,使整个体系能量降低,阻止了Fe离子的化合和团聚。同时各种表征手段也都没有检测到任何二次相,因此我们认为(In0.92Fe0.05Sn0.03)2O3薄膜的铁磁性是本征的,来源于Fe和Sn取代了In的均相结构；而且Sn的掺入可以有效增大体系的载流子浓度,其磁性来源于载流子诱导机制。对于Fe-Cu共掺杂的(In0.92Fe0.05Cu0.03)2O3薄膜中有金属Fe团簇生成,这是稀磁半导体所不期望的。
(4)采用脉冲激光沉积技术在A12O3 (0001)基片上成功制备了Mn和Cr掺杂的In203薄膜。Mn掺杂In203薄膜的铁磁性表现出可逆性,通过控制掺入薄膜中Sn的含量控制其载流子浓度,薄膜的铁磁性可在“开”和“关”之间转换。额外载流子的存在对Cr掺杂In203薄膜的铁磁性有重要影响,在薄膜中加入了1%的Sn后,由于载流子浓度的增加,薄膜的铁磁性明显增强,饱和磁化强度达2.10μB/Cr。重要的是,我们的实验结果表明载流子浓度和自旋对样品铁磁性的产生都非常重要。
总之,我们制备了不同过渡金属元素掺杂的In203基稀磁半导体,研究了样品的结构、磁性和输运等性质。发现载流子浓度对样品的铁磁性有重要影响,载流子浓度较大的铁磁性薄膜在新一代自旋电子器件中有广阔的应用前景。
Diluted magnetic semiconductos (DMSs) have attracted great interest for their potential applications in spintronic devices because the charge and spin of carriers can be simultaneously controlled. In2O3 is a wide band gap (3.75 eV) transparent semiconductor with cubic bixbyite crystal structure. The solubility of transition metal (TM) in In2O3 host lattice was found to be very high, which can effectively avoid the formation of magneitc impurities and also makes it possible to obtain homogenous DMSs for application. In this work, Fe, Mn and Cr doped In2O3 samples were prepared by solid state reaction, a vacuum annealing process and pulsed laser deposition technique. Based on the systematical studies of the structure, magnetism and transport properties of the samples, the origin and mechanism of ferromagnetism in In2O3-based DMSs were discussed. The results are summarized as follows:
(1) (In1-xFex)2O3 (x=0.02,0.05,0.2) powders were prepared by a solid state reaction method and a vacuum annealing process. A systematic study was done on the structural and magnetic properties of (In1-xFex)2O3 powders as a function of Fe concentration and annealing temperature. The (In1-xFex)2O3 powders appear to be homogeneous and single-phase materials, where Fe elements incorporate into the In sites of the In2O3 lattice rather than forming any secondary phases. The samples were ferromagnetic with the magnetic moment of 0.49-1.73μB/Fe and the Curie temperature around 793 K. The results indicate that the observed high temperature ferromagnetism of vacuum-annealed (In1-xFex)2O3 powders is intrinsic rather than from any magnetic impurities, and is attributed to the ferromagnetic coupling of Fe2+and Fe3+ions via an electron trapped in a bridging oxygen vacancy.
(2) Fe-doped In2O3 thin films are deposited on sapphire substrates using pulsed laser ablation. The effects of Fe concentration and oxygen partial pressure on the structure, magnetism and transport properties of (In1-xFex)2O3 films are studied systematically. A detailed analysis of the structural properties suggests the substitution of Fe dopant atoms into In lattice sites and the films are textured with (222) orientation. X-ray photoelectron spectroscopy indicates that the valence of substituted Fe in the (In1-xFex)2O3 films varies with oxygen partial pressure, at lower oxygen partial pressures, Fe behaves as a mixture of+2 and +3 valences, whereas Fe3+dominates in the films grown at higher oxygen pressures. Systematic investigations of transport properties for (In1-xFex)2O3 films with a wide range of carrier densities reveal that they occur in both metallic and insulating regimes. The insulating films exhibit variable range hopping at low temperatures and show temperature dependent ferromagnetism, which can be explained by bound magnetic polarons mechanism. For the metallic films, the carrier densities play a crucial role in their robust ferromagnetism and the resistivity and magnetization are independent of temperature; the carrier-mediated exchange mechanism has been suggested as responsible for magnetic ordering in these metallic films. Optical absorption and magneto-optic studies of (In1-xFex)2O3 films indicate further differences between metallic and semiconducting films and show significant magnetic circular dichroism below the In2O3 band edge at room temperature, which also implies intrinsic ferromagnetism.
(3) (In0.92Fe0.05Sn0.03)2O3 and (In0.92Fe0.05Cu0.03)2O3 powders and films were prepared by a vacuum annealing process and a pulsed laser deposition technique, respectively. The effects of codpants Sn and Cu on the structure, magnetism and transport properties of samples have been investigated. The zero-field-cooled and field-cooled magnetic measurement indicated that the room temperature ferromagnetism of (In0.92Fe0.05Sn0.03)2O3 and (In0.92Fe0.05Cu0.03)2O3 powders both originate from the Fe3O4 nanoparticles although the x-ray diffraction results revealed no crystalline phase other than cubic bixbyite structure In2O3 to be present in the powders. However, the origin of ferromagnetism for (In0.92Fe0.05Sn0.03)2O3 and (In0.92Fe0.05Cu0.03)2O3 films is very different. In (In0.92Fe0.05Sn0.03)2O3 film, the Fe-Sn can constitute p-n pairs. The Columbic attraction between the n- and p-type dopants with opposite charge state substantially enhances both the thermodynamic and, in particular, the kinetic solubilities of the dopant pairs in concerted substitutional doping. More profoundly, the noncompensated p-n pairs of Fe-Sn prevented the aggregation of Fe ions. The mictostructure and magnetic analyses also confirmed that there was no segregation of any secondary phases. So the room temperature ferromagnetism of (In0.92Fe0.05Sn0.03)2O3 film is intrinsic rather than from any other magnetic impurity phases. The magnetic behavior is consistent with a carrier-induced ferromagnetism model. While, the (In0.92Fe0.05Cu0.03)2O3 film was superparamagnetic, and the observed ferromagnetism originated from the nanometer-sized Fe clusters, which is not desirable for device application.
(4) Mn and Cr-doped In2O3 films with Sn co-doping were deposited on sapphire substrate by pulsed laser deposition. The ferromagnetism of Mn-doped In2O3 films shows reversible behavior, which can be switched between "on" and "off" states by controlling the carrier density via varying Sn concentration. The enhanced ferromagnetism in Cr-doped In2O3 films is observed due to the significant increase in the carrier density with Sn doping, and the saturation magnetization can reach 2.10μB/Cr. Most importantly, both of the experiment results reveal that the carrier density and the net spin are two crucial factors for producing and tuning ferromagnetism.
In summary, we have prepared different TMs doped In2O3 DMSs materials and studied the various properties of the samples. The results reveal that the carrier densities play a crucial role in the ferromagnetism and the dependence of the magnetism on the carrier density lend support to carrier-mediated mechanism. This clear demonstration of carrier-mediated ferromagnetism at high carrier concentration implies that TMs-doped In2O3 can be used as n-type DMSs at RT, with consequent potential for exploitation in spintronic applications.
引文
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