One-Dimensional Perovskite Manganite Oxide Nanostructures: Recent Developments in Synthesis, Characterization, Transport Properties, and Applications
© Li et al. 2016
Received: 23 September 2015
Accepted: 22 February 2016
Published: 1 March 2016
One-dimensional nanostructures, including nanowires, nanorods, nanotubes, nanofibers, and nanobelts, have promising applications in mesoscopic physics and nanoscale devices. In contrast to other nanostructures, one-dimensional nanostructures can provide unique advantages in investigating the size and dimensionality dependence of the materials’ physical properties, such as electrical, thermal, and mechanical performances, and in constructing nanoscale electronic and optoelectronic devices. Among the one-dimensional nanostructures, one-dimensional perovskite manganite nanostructures have been received much attention due to their unusual electron transport and magnetic properties, which are indispensable for the applications in microelectronic, magnetic, and spintronic devices. In the past two decades, much effort has been made to synthesize and characterize one-dimensional perovskite manganite nanostructures in the forms of nanorods, nanowires, nanotubes, and nanobelts. Various physical and chemical deposition techniques and growth mechanisms are explored and developed to control the morphology, identical shape, uniform size, crystalline structure, defects, and homogenous stoichiometry of the one-dimensional perovskite manganite nanostructures. This article provides a comprehensive review of the state-of-the-art research activities that focus on the rational synthesis, structural characterization, fundamental properties, and unique applications of one-dimensional perovskite manganite nanostructures in nanotechnology. It begins with the rational synthesis of one-dimensional perovskite manganite nanostructures and then summarizes their structural characterizations. Fundamental physical properties of one-dimensional perovskite manganite nanostructures are also highlighted, and a range of unique applications in information storages, field-effect transistors, and spintronic devices are discussed. Finally, we conclude this review with some perspectives/outlook and future researches in these fields.
One-dimensional perovskite oxide nanostructures, including nanowires, nanorods, nanotubes, nanofibers, and nanobelts, have attracted much attention from scientists for their unique physical properties dependent on the size and dimensionality [1–5]. They are also expected to play important roles as both interconnects and key units in nanoscale electronic, optoelectronic, electrochemical, and electromechanical devices [6–8]. As compared to the zero-dimensional perovskite oxide nanostructures (or quantum dots) and two-dimensional perovskite nanostructures (or quantum wells), the research progress of one-dimensional perovskite oxide nanostructures has been slow until very recently, as hindered from the problems in fabrication and synthesis of these nanostructures with well-controlled dimensions, uniform sizes, phase purity, and homogenous chemical compositions. In recent years, many physical techniques such as advanced nanolithographic techniques (e.g., electron beam or focused ion beam (FIB) writing, proximal probe patterning, AFM lithography, X-ray, or extreme UV lithography) have been developed to fabricate one-dimensional perovskite oxide nanostructures with controllable sizes and morphology [9–14]. In the meantime, chemical synthesis approaches are also developed to synthesize one-dimensional perovskite oxide nanostructures with controllable sizes and morphology, crystalline structures, and chemical compositions, which provide an alternative and intriguing strategy for producing one-dimensional perovskite oxide nanostructures in terms of material diversity, cost, throughput, and the potential advantage of high-volume production [15–18]. Up to date, several reviews on one-dimensional perovskite oxide nanostructures have been published, which provide an overview of research directions in synthesis and applications of one-dimensional perovskite oxide nanostructures [19–22]. For example, the review from Rørvik et al. presents an excellent summary of the current status of one-dimensional perovskite ferroelectric nanostructures . The reviews contributed by Zhu et al. are focused on the synthesis, structural characterization, fundamental physical properties, and applications of perovskite oxide nanotubes and nanowires, respectively [20, 21]. A review on the behavior of one-dimensional perovskite oxide nanostructures, their properties, and the different fabrication approaches to achieve such structures is also available . Among the one-dimensional perovskite oxide nanostructures, one-dimensional perovskite manganite oxide nanostructures (in the forms of nanorods, nanowires, nanotubes, and nanobelts) play important roles in scientific researches and applications in microelectronic, magnetic, and spintronic devices due to their unusual electron transport and magnetic properties. Recently, the research progress on the electronic phase separation in low-dimensional perovskite manganite nanostructures (e.g., nanoparticles, nanowires/nanotubes, and nanostructured films and/or patterns) is reported . In this work, we focus on the recent research activities in the one-dimensional perovskite manganite nanostructures, which provide a comprehensive review of the state-of-the-art of the one-dimensional perovskite manganite nanostructures that covers their synthesis, characterization, transport properties, and applications. Finally, we conclude this article with some perspectives and outlook.
Synthesis Techniques for One-Dimensional Perovskite Manganite Nanostructures
Up to date, a variety of techniques are developed to fabricate one-dimensional perovskite manganite nanostructures. Basically, these approaches can be classified into two strategies: (i) physical approach and (ii) chemical approach [5–7]. In the physical approach, one-dimensional perovskite manganite nanostructures are patterned from bulk or film counterpart materials by a combination of lithography and etching. The chemical approach, in which one-dimensional perovskite manganite nanostructures are assembled from basic building blocks such as atoms or molecules, much like the way nature uses proteins and other macromolecules to construct complex biological systems, represents a powerful alternative approach to conventional physical methods. In this section, we briefly describe various techniques used for fabricating one-dimensional perovskite manganite nanostructures.
Photolithography is an advanced technique to fabricate nanopatterns on substrates coated with polymer materials by mechanical force or sputtering technique. As it can manufacture extensive patterning tautologically, photolithography techniques have the advantages of being practicable, efficient, and economic [24–26]. For example, to understand the role of electronic phase separation (EPS) in the emergent transport behaviors of one-dimensional manganite structures, La0.33Pr0.34Ca0.33MnO3 (LPCMO) nanowires were fabricated from a single-crystalline LPCMO thin film via optical lithography, where the width of the manganite wires is reduced to a scale on the order of the inherent phase separation . It is found that by reducing a single-crystal LPCMO thin film to a wire with a width comparable to a scale on the order of the inherent EPS, the system exhibits ultra-sharp jumps in resistivity, and such resistivity jumps are attributed to a reduction of the transport lanes to a single channel. As the insulating barriers of the charge-ordered state are broken by the reduction of temperature or an increase in magnetic field, the resistance in the wire shows sharp jumps around the metal–insulator (M–I) transition, which reflects the nature of the first-order phase transition between ferromagnetic metal and charge-ordered insulator domains . Liu et al.  also prepared quasi-one-dimensional oxide nanoconstriction arrays via nanosphere lithography. They dropped a drop of aqueous suspension of SiO2 microspheres, with a diameter of 1.5 μm, onto a SrTO3 (100) substrate. These microspheres could self-assemble during the drying process and finally turned into a hexagon-like ordered monolayer. Then, a reactive ion etching process was proceeded to reduce the sizes of the microspheres. Subsequently, the substrate was put into a pulsed laser deposition (PLD) chamber for the deposition of La0.67Sr0.33MnO3; after that, the sample was transferred into a furnace and annealed at 750 °C. After removing the microspheres, a La0.67Sr0.33MnO3 nanoconstriction array was obtained. Under the low oxygen pressure, the La0.67Sr0.33MnO3 film was deposited with the oxygen deficiency in La0.67Sr0.33MnO3 nanoconstriction, the sample had to be further annealed at 900 °C for 8 h in air. Finally, the La0.67Sr0.33MnO3 size of nanoconstriction obtained was around 100 nm. Peña et al.  fabricated La2/3Sr1/3MnO3 microbridges by another method. They first deposited La2/3Sr1/3MnO3 films with a thickness range from 15 to 50 nm onto SrTiO3 substrates by RF sputtering. Then, the films were patterned into microbridges with different sizes by using standard photolithographic techniques.
Focused Ion Beam Milling
Recently, large aspect-ratio (length-to-width >300) single-crystal nanowires of La2/3Ca1/3MnO3 were also fabricated by combined optical and FIB lithographies, which preserved their functional properties . Remarkably, an enhanced magnetoresistance value of 34 % in an applied magnetic field of 0.1 T in the narrowest 150-nm nanowire was obtained. Such behavior is ascribed to the strain release at the edges together with a destabilization of the insulating regions. This opens new strategies to implement these structures in functional spintronic devices. FIB is also used to fabricate manganite oxide nanobridges [28–31]. For example, Singh-Bhalla et al. [28, 29] fabricated (La0.5Pr0.5)0.67Ca0.33MnO3 nanobridges and microbridges with a width ranging from 100 nm to 1 μm. They first deposited single-crystalline, epitaxial 30-nm-thick (La0.5Pr0.5)0.67Ca0.33MnO3 films on the NdGaO3 (110) substrates at 820 °C by PLD. Then, a combination of photolithography and a FIB was employed to fabricate the (La0.5Pr0.5)0.67Ca0.33MnO3 nanobridges and microbridges. Pallecchi et al.  deposited La0.7Sr0.3MnO3 films on SrTiO3 (001) substrates by pulsed laser ablation and obtained La0.7Sr0.3MnO3 narrow channels with widths of 0.2–1.0 μm by a Ga+ FIB. Céspedes et al.  also patterned a manganite nanobridge by FIB. They grew La0.7Sr0.3MnO3 films by PLD. Then, a focused Ga+ beam was used to fabricate a La0.7Sr0.3MnO3 nanobridge with dimensions of less than 20 nm.
Electron Beam Lithography
Electron beam lithography (EBL) is a nanofabrication technique in rapid development . Guo et al.  grew La0.67Ca0.33MnO3 films with thickness of ~100 nm on SrTiO3 (100) substrates by a PLD technique and fabricated La0.67Ca0.33MnO3 microbridges with different widths (e.g., 1.5 μm, 1 μm, and 500 nm) by EBL technology. Beekman et al.  also grew thinner La0.7Ca0.3MnO3 films (with a thickness range of 20–70 nm) on SrTiO3 (001) substrates by DC sputtering. And then, they fabricated a La0.7Ca0.3MnO3 microbridge with a width of 5 μm by using EBL technology and Ar etching.
One-Dimensional Perovskite Manganite Oxide Nanostructures Synthesized by Hydrothermal Process
A hydrothermal method is a common method to fabricate manganite nanowires, which usually involves heating an aqueous suspension of precursor in a Teflon vessel at befitting temperatures and pressures. A mineralizer which is conducive to the crystallization is generally injected to control the morphology of products [34–37]. For example, Zhu et al.  used KMnO4, MnCl2·4H2O, La(NO3)3·6H2O, Ba(OH)2·8H2O, and Sr(NO3)2 as raw materials and KOH as a mineralizer to synthesize La0.5Ba0.5MnO3 nanowires. The reaction reagents were dissolved into deionized water to form a solution, to which KOH was added with stirring to adjust the alkalinity of the solution. The aqueous solution was reacted at 270 °C for 25 h to get La0.5Ba0.5MnO3; furthermore, another crystallization reaction occurred at 280 °C for 50 h to get La0.5Sr0.5MnO3 nanowires. The nanowire diameters were in the range of 30–150 nm for La0.5Ba0.5MnO3 and 50–400 nm for La0.5Sr0.5MnO3. By the same method, Datta et al.  also synthesized the single-crystalline La0.5Sr0.5MnO3 nanowires with a diameter of ~50 nm and a length up to 10.0 μm. It was found that these La0.5Sr0.5MnO3 nanowires had a ferromagnetic–paramagnetic transition temperature (Curie temperature, T C) at around 325 K, which was very close to the bulk value (~330 K) of the single crystal with the same composition. It was also found that the functional behavior was likely to be retained even after the diameter size of the nanowires was reduced to 45 nm. The electrical transport measurements on a single nanowire demonstrated that the nanowire exhibited an insulating behavior within the measured temperature range, which was similar to the bulk system. Single-crystalline La0.5Ca0.5MnO3 nanowires with lengths ranging from several to several tens of micrometers and a uniform diameter of ~80 nm were also grown by a hydrothermal method . The La0.5Ca0.5MnO3 nanowires had an orthorhombic perovskite structure with very clean surfaces and grew along the (100) direction. An enhanced T C was observed in these nanowires, which was ascribed to the unit cell contraction and anisotropy. Rao et al.  also reported the hydrothermal synthesis of the charge-ordering Pr0.5Ca0.5MnO3 (PCMO) single-crystalline nanowires with a diameter of ~50 nm and a length of a few microns. They found that in these PCMO nanowires, the charge-ordered phase was weakened and the antiferromagnetic phase disappeared, whereas a ferromagnetic phase was observed in this one-dimensional manganite oxide nanowire.
One-Dimensional Perovskite Manganite Nanostructures Synthesized by Template Assistance
Template synthesis of manganite nanotubes and nanowires is a versatile and inexpensive technique, which combines a sol–gel process and the use of porous sacrificial substrates of either silicon or alumina as templates [38–45]. The size, shape, and structural properties of the assembly are simply controlled by the templates used, which form ordered arrayed nanowires and nanotubes. As a result, the diameter and length of the nanowires/nanotubes are corresponded closely to the pore. By this method, Li et al.  synthesized the LPCMO/MgO core–shell nanowires with diameters about tens of nanometers in two steps. First, chemical vapor deposition was used to grow MgO nanowires on the MgO (100) substrates coated with Au nanoparticles. Then, the LPCMO shell layers were deposited on the MgO nanowires by a PLD process. They finally obtained the LPCMO/MgO core–shell nanowires with diameters of 30 nm and lengths in a range of several micrometers to tens of micrometers. Similarly, Beltran-Huarac et al.  grew bamboo-like carbon nanotubes (BCNTs) and then deposited the La0.67Sr0.33MnO3 films onto the bamboo-like carbon nanotubes. Finally, they obtained one-dimensional La0.67Sr0.33MnO3/BCNTs with diameters ranging from 100 to 160 nm and lengths over 10 μm. Atalay et al.  used Ca(NO3)2·XH2O, La(NO3)3·6H2O, and Mn(NO3)2·XH2O as raw materials and ethylene glycol as a solvent. The solution with a pH value of 2–6 was stirred in high temperature until a gel was formed. Then, the gel was filled into a porous anodized aluminum oxide (AAO) template. Finally, the template was annealed at 400 °C for 2 h and at 700 °C for 2 h with a rate of 2 °C/min. After dissolution in 1 M NaOH, the nanowires with a diameter of 185–195 nm were obtained. Similarly, Ma et al.  also used an AAO template and a sol–gel process to fabricate La0.8Ca0.2MnO3 nanowires with a diameter of 30 nm. Carretero-Genevrier et al.  produced single-crystalline La0.7Sr0.3MnO3 nanowires by polymer template-directed chemical solution synthesis. In addition, perovskite rare-earth manganese tubes such as La0.67Sr0.33MnO3, La0.67Ca0.33MnO3, and La0.325Pr0.300Ca0.375MnO3 are also fabricated using a sol–gel template synthesis process [43, 44]. Their typical length was about 6 to 8 μm, and the average wall thickness is 45, 60, and 150 nm for La0.67Sr0.33MnO3, La0.67Ca0.33MnO3, and La0.325Pr0.300Ca0.375MnO3, respectively. The walls of the tubes were composed of magnetic nanograins, and their sizes are less than the critical size for multidomain formation in manganites. As a consequence, each particle that constituted the nanotube walls was a single magnetic domain. The La0.6Sr0.4CoO3 nanotubes with a diameter of 100 nm and the nanowires with a diameter of 40–60 nm were also formed by shaping the sol with the cylinder pores in an AAO template .
One-Dimensional Perovskite Manganite Nanostructures Produced from Electrospinning Process
Electrospinning is a time and cost-effective technique that produces ultra-fine fibers with diameters in the dozens-of-nanometers range through the action of an external electric field imposed on a precursor solution [46–48]. Hayat et al.  added barium acetate and manganese acetate tetrahydrate into acetic acid separately followed by stirring for 10–15 min, then poured the barium acetate and manganese acetate solution into the mixture of ethanol and polyvinyl pyrrolidone, and stirred them at room temperature for 16 h. The applied electric voltage between the needle tip and the collector was 10 kV. Finally, the collected nanofibers were heated at 600 °C for 2 h. Nanofibers with an average diameter of less than 100 nm were obtained. Jugdersuren et al.  dissolved La(NO3)3·6H2O, Mn(NO3)2·2H2O, and Sr(NO3)2 into water and added polyvinyl pyrrolidone (PVP) beads to bind the solution. Then, the electrospinning process proceed; after that, nanowires were collected and annealed at 550 °C for 3 h in argon and 3 % hydrogen gas mixture, additionally at 730 °C for 1 h in argon and 10 % oxygen atmosphere. Finally, they got La0.67Sr0.33MnO3 nanowires with diameters in a range of 80–300 nm and length in 200 μm. Zhou et al.  obtained thinner LaMnO3 nanofibers (50–100 nm) by a semblable way using lanthanum acetate and manganese acetate as raw materials and an applied electric voltage of 15 kV between the collector and the needle tip.
Structural Characterization of One-Dimensional Perovskite Manganite Nanostructures
Contemporarily, all kinds of techniques have been used to characterize the nanostructures of one-dimensional manganite, like X-ray diffraction (XRD), scanning electron microscope (SEM), transmission electron microscopy (TEM), selected area electron diffraction (SAED), and so on. Moreover, some techniques such as electron energy loss spectroscopy (EELS) and energy-dispersive X-ray spectrometer (EDX) can be utilized to analyze the chemical composition [20, 21].
Manganite Nanobridges and Microbridges
Fundamental Transport Properties of One-Dimensional Perovskite Manganite Oxide Nanostructures
One-dimensional perovskite manganite nanostructures are attractive for their size and dimensionality dependence of physical properties such as electrical and magnetic performances. These properties make it widely used for applications in microelectronic, magnetic, and spintronic devices. In this section, we introduce the electrical and magnetic transport properties of one-dimensional perovskite manganite nanostructures [20, 21].
Electrical Transport Properties
Magnetic Transport Properties
Applications of One-Dimensional Perovskite Manganite Nanostructures
One-dimensional manganite oxide has an attractive commercial value for the adhibition in information storages. Among sundry manganites, perovskite manganite is of particular importance due to its colossal magnetoresistance (CMR) . Peña et al.  investigated the electronic transport properties of La2/3Sr1/3MnO3 microfabricated bridges. The local I–V curves are nearly symmetric in the ON state (prior to the transition between low resistance and high resistance states) but present a rectifying performance in the OFF state (high resistance state, HRS). A metal–insulator–metal (M–I–M) geometry with an interface-switching mechanism is introduced: the topmost unit cells of the La2/3Sr1/3MnO3 are the I layer and the remaining La2/3Sr1/3MnO3 layer and scanning probe microscope (SPM) conducting tip which act as the M layer. This geometry allows the research of the electronic properties of the HRS and their dependence on temperature and magnetic field for the first time. The results indicate that the electronic effects are the biggest contributor in the charge depletion, even though mobile ions or ionic defects might affect the current transport. These results represent an important step forward to the oxide-based memory devices.
In the one-dimensional perovskite manganite oxide nanostructures, their magnetic, electronic, and lattice degrees of freedom interact with each other through double exchange and Jahn–Teller interaction, leading to delicate unbalances between the magnetic, electronic, and lattice degrees of freedom in these materials at the nanoscale, and thus, new outstanding properties can be achieved . Therefore, one-dimensional perovskite manganite nanostructures are viewed as functional building blocks for the transport of charge and spins for the assembly of electronic, magnetic, and sensing devices [60, 61]. By using manganite oxide nanowires as building blocks, one can create manganite oxide nanowire-based lateral spin valves or magnetic tunneling junction (MTJ) devices. A possible scheme starts with a bottom-up synthesized FM manganite oxide nanowire, and a small portion of which is be converted into nonmagnetic (NM) by using selective Ar+ ion milling, leading to an FM–NM–FM lateral device. Such a manganite oxide nanowire-based spintronic device is attractive, whereas the centrally modified region must be thin enough to retain the spin coherent transport. The enhanced low-field MR [47, 62] and the Curie temperature  and significant magnetic anisotropy  have also been observed in the perovskite manganite oxide nanowires. In addition, the morphology of manganite oxide nanowire can be also controlled by annealing or growing on engineered substrates, which could significantly affect their physical properties [60, 64]. Therefore, such large MR and the great tunability of one-dimensional perovskite manganite nanostructures are much attractive for spintronic applications. By using La0.67Sr0.33MO and SrTiO3 as FM and insulating layer, respectively, all-oxide MTJ devices were first fabricated by Lu et al.  and Sun et al. . Furthermore, a record tunneling magnetoresistance ratio of 1850 % was also reported by Bowen et al. . Despite these promising results have been made, the working temperature of all the perovskite oxide-based MTJ devices remains lower than the room temperature, which is the major issue to be resolved before commercial applications of all perovskite oxide-based MTJ devices.
In summary, this article provides a comprehensive review on recent developments in synthesis, characterization, transport properties, and applications of one-dimensional manganite oxide nanostructures (including nanorods, nanowires, nanotubes, and nanofibers). Nowadays, one-dimensional manganite oxide nanostructures are widely used for applications in nanostructure-based devices because of their fascinating electrical and magnetic transport properties. Although many exciting progresses and potential applications of one-dimensional manganite oxide nanostructures have been made, considerable challenges remain to be resolved. In terms of the fabrication techniques, the top-down (physical approach) fabrication technique often requires expensive equipment and complicated processing and also usually faces the challenge of structural defects (such as edge roughness) in the lithographically patterned one-dimensional manganite oxide nanostructures. In addition, most of the perovskite manganite oxide materials need high deposition temperature and the typical electron beam and photo resists are incompatible with this requirement. The bottom-up (chemical approach) synthesis of one-dimensional manganite oxide nanostructures with precise and reproducible controls in composition, morphology, and physical properties is challenging for one-dimensional manganite oxide nanostructures used for spintronic devices. In terms of microelectronic devices, there have been some revolutionary breakthroughs in spintronics, such as spin valves, magnetic tunneling junctions, and spin field-effect transistors. However, several problems for one-dimensional manganite oxide nanostructures used for spintronic devices remain unresolved and some technical challenges lie ahead. For example, the spin polarization of manganite oxides decays rapidly with temperature, and the working temperature of the one-dimensional manganite oxide nanostructure-based spintronic device is often lower than the room temperature. The low-dimensional spin-dependent transport exists in the one-dimensional manganite oxide nanostructures, and the physical properties of the interfaces within one-dimensional manganite oxide nanostructure-based devices remain elusive. Furthermore, the defect chemistries and the stoichiometry-property correlations in the one-dimensional perovskite manganite oxide nanostructures are quite complex. In addition, new device processing techniques are also urgent to be developed. With the researches into one-dimensional manganite oxide nanostructures spreading their wings and becoming more extensive, it is expected that the fascinating achievements towards the practical applications of one-dimensional manganite oxide nanostructures in the fields of microelectronics, magnetics, and spintronics will be made. An exciting new era for the applications of one-dimensional manganite oxide nanostructures in oxide microelectronics is on the horizon!
This work was partially supported by the National Natural Science Foundation of China (grant nos. 11174122 and 11134004); National Basic Research Program of China (grant nos. 2015CB654900); open projects from State Key Laboratory of Materials-Oriented Chemical Engineering (MCE), Nanjing University of Technology (grant no. KL14-10); National Laboratory of Solid State Microstructures, Nanjing University (grant no. M26012); and six big talent peak project from Jiangsu Province (grant no. XCL-004).
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