Synthesis of GaN nanowires on gold-coated SiC substrates by novel pulsed electron deposition technique

A two-step approach for macro-synthesis of GaN nanowires was developed in this study. GaN nanoparticles were firstly synthesized through a facile solid-state reaction using an organic reagent dicyandiamide (C₂N₄H₄) and Ga₂O₃ as precursors. Subsequently, single-crystalline wurtzite GaN nanowires were grown on gold-coated 6H-SiC substrates via novel pulsed electron deposition (PED) technique using the as-prepared GaN nanoparticles as target, which provides a new route employing nanoparticles as precursors to fabricate GaN nanowires. It is found that pulsed electron ablation induced Ga and N plasma directly towards the gold-coated substrate to initialize the vapor-liquid-solid (VLS) growth processes. The morphological and structural properties were investigated in detail and Raman scattering spectrum of these nanowires presented some new features.     

Synthesis of GaN nanowires by Tb catalysis

Rare earth metal seed Tb was employed as catalyst for the growth of GaN wires. GaN nanowires were synthesized successfully through ammoniating Ga₂O₃/Tb films sputtered on Si(1 1 1) substrates. The samples characterization by X-ray diffraction and Fourier transform infrared indicated that the nanowires are constituted of hexagonal wurtzite GaN. Scanning electron microscopy, transmission electron microscopy, and high-resolution transmission electron microscopy showed that the samples are single-crystal GaN nanowire structures. The growth mechanism of the GaN nanowires is discussed.     

Control of ZnO nanowire arrays by nanosphere lithography (NSL) on laser-produced ZnO substrates

Nanosphere lithography (NSL) is a successful technique for fabricating highly ordered arrays of ZnO nanowires typically on sapphire and GaN substrates. In this work, we investigate the use of thin ZnO films deposited on Si by pulsed laser deposition (PLD) as the substrate. This has a number of advantages over the alternatives above, including cost and potential scalability of production and it removes any issue of inadvertent n-type doping of nanowires by diffusion from the substrate. We demonstrate ordered arrays of ZnO nanowires, on ZnO-coated substrates by PLD, using a conventional NSL technique with gold as the catalyst. The nanowires were produced by vapor phase transport (VPT) growth in a tube furnace system and grew only on the areas pre-patterned by Au. We have also investigated the growth of ZnO nanowires using ZnO catalyst points deposited by PLD through an NSL mask on a bare silicon substrate.     

Synthesis,structural and ellipsometric evaluation of oxygen-deficient and nearly stoichiometric zinc oxide and indium oxide nanowires/nanoparticles

Oxygen-deficient (OD) and nearly stoichiometric (NST) ZnO and In₂O₃ nanowires/nanoparticles were synthesized by chemical vapor deposition on Au-coated silicon substrates. The OD ZnO and OD In₂O₃ nanowires were synthesized at 750 and 950°C, respectively, using Ar flow at ambient pressure. A mixture of flowing Ar and O₂ was used for synthesizing NST ZnO nanowires and NST In₂O₃ nanoparticles. Growth of OD ZnO nanowires and NST In₂O₃ nanoparticles was found to be via a vapor–solid (VS) mechanism and the growth of NST ZnO nanowires was via a vapor–liquid–solid mechanism (VLS). However, it was uncertain whether the growth of OD In₂O₃ nanowires was via a VS or VLS mechanism. The optical constants, thickness and surface roughness of the prepared nanostructured films were determined by spectroscopic ellipsometry measurements. A three-layered model was used to fit the calculated data to the experimental ellipsometric spectra. The refractive index of OD ZnO, NST ZnO nanowires and NST In₂O₃ nanoparticles films displayed normal dispersion behavior. The calculated optical band gap values for OD ZnO, NST ZnO, OD In₂O₃ nanowires and NST In₂O₃ nanoparticles films were 3.03, 3.55, 2.81 and 3.52?eV, respectively.     

Temperature-controlled catalytic growth of one-dimensional gallium nitride nanostructures using a gallium organometallic precursor

Catalytic growth of 1-D GaN nanostructures is achieved at temperatures from 550 to 850 °C using NH₃ and gallium acetylacetonate. Structural characterization of the 1-D GaN nanostructures by HRTEM shows that straight GaN nanowires, needle-like nanowires (nanoneedles), and bamboo-shoot-like nanoneedles are synthesized at 750, 650, and 550 °C, respectively. In addition to selecting a proper catalyst, providing sufficient precursors has been demonstrated to be a crucial factor for the low-temperature growth of 1-D GaN nanostructures via the VLS mechanism. Possible mechanisms for forming nanoneedles at low temperatures are proposed. PACS 61.46.+w; 68.65.–k; 81.07.–b     

Formation of CuO nanowires by thermal annealing copper film deposited on Ti/Si substrate

Nanowires of various inorganic materials have been fabricated due to the realization of their applications in different fields. Large-area and uniform cupric oxide (CuO) nanowires were successfully synthesized by a very simple thermal oxidation of copper thin films. The copper films were deposited by electron beam evaporation onto Ti/Si substrates, in which Ti film was first deposited on silicon substrate to serve as adhesion layer. The structure characterization revealed that these nanowires are monoclinic structured single crystallites. The effects of different growth parameters, namely, annealing time, annealing temperature, and film thickness on the fabrication of the CuO nanowires were investigated by scanning electron microscopy. A typical procedure simply involved the thermal oxidation of these substrates in air and within the temperature range from 300 to 700 °C. It is found that nanowires can only be formed at thermal temperature of 400 °C. It is observed that the growth time has an important effect on the length and density of the CuO nanowires, whereas the average diameter is almost the same, i.e.50 nm. Different from the vapor-liquid-solid (VLS) and vapor-solid (VS) mechanism, the growth of nanowires is found to be based on the accumulation and relaxation of the stress.     

Room-temperature magnetic properties of SiC based nanowires synthesized via microwave heating method

Two kinds of ferromagnetic SiC based nanowires with and without Ni catalyst were successfully synthesized by employing microwave heating method. The comprehensive characterizations and vibrating sample magnetometer (VSM) have been applied to investigate the micro-structures and magnetic properties of as-grown nanowires. For the nanowires synthesized without using Ni catalyst, the diameters and lengths are in the range of 20–60 nm and dozens of micrometers, respectively. Particularly, the results of transmission electron microscopy (TEM) show that the nanowires consist of SiC core and SiO_x shell. The SiC/SiO_x coaxial nanowires exhibit room-temperature ferromagnetism with saturation magnetization (Ms) of 0.2 emu/g. As to the nanowires obtained using Ni catalyst, the scanning electron microscopy (SEM) results indicate that the Ni catalyzed nanowires have a nano-particle attached on the tip and a uniform diameter of approximately 50 nm. The vapor-liquid-solid (VLS) growth mechanism can be used to explain the formation of the Ni catalyzed nanowires. The detection result of VSM indicates that the Ni catalyzed nanowires possess the paramagnetism and the ferromagnetism, simultaneously. The enhancement of the ferromagnetism, compared with the SiC/SiO_x coaxial nanowires, could be attributed to the Ni₂Si and NiSi phases.     

Synthesis and characterization of GaN nanowires

In this work, GaN nanowires were fabricated on Si substrates coated with NiCl₂ thin films using chemical vapor deposition (CVD) method by evaporating Ga₂O₃ powder at 1100 °C in ammonia gas flow. X-ray diffraction (XRD), scanning electron microscopy (SEM), high-resolution transmission electron microscope (HRTEM) and photoluminescence (PL) spectrum are used to characterize the samples. The results demonstrate that the nanowires are single-crystal GaN with hexagonal wurtzite structure. The growth mechanism of GaN nanowires is also discussed.     

Synthesis and characterization of GaN nanowires by a catalyst assisted chemical vapor deposition

GaN nanowires have been fabricated on Si(1 1 1) substrates by chemical vapor deposition (CVD) method with NiCl₂ as catalyst and their compositions, microstructures, morphologies and light emitting properties were characterized by X-ray diffraction (XRD), FT-IR spectrophotometer (FTIR), scanning electron microscope (SEM), high-resolution transmission electron microscope (HRTEM), Raman spectroscopy and photoluminescence (PL). The results demonstrate that the nanowires are single-crystal GaN with hexagonal wurtzite structure and high crystalline quality, having the size of 20-50 nm in diameter and several tens of microns in length with some nano-droplets on their tips, which reveals that the growth mechanism of GaN nanowires agrees with vapor-liquid-solid (VLS) process. Five first-order Raman active phonon bands move to low shift and A₁(TO), E₁(TO), and E₂ (high) bands are overlapped and broaden, which is caused by uncertainty in the phonon wave vector. Five non-first-order active Raman phonons also appear, which is caused by the small dimension and high surface disorder degree. A blue-shift of the band-gap emission occurs due to quantum confinement effect.     

Synthesis of large-scale GaN nanowires by ammoniating Ga2O3 films on Co layer deposited on Si（111） substrates

A mass of GaN nanowires has been successfully synthesized on Si（111） substrates by magnetron sputtering through ammoniating Ga2O3/Co films at 950℃. X-ray diffraction, scanning electron microscopy, high resolution transmission electron microscope and Fourier transformed infrared spectra are used to characterize the samples. The results demonstrate that the nanowires are of single-crystal GaN with a hexagonal wurtzite structure and possess relatively smooth surfaces. The growth mechanism of GaN nanowires is also discussed.     

Two-step synthesis of one-dimensional single crystalline GaN nanowires

Straight and smooth GaN nanowires were synthesized on quartz substrates through the direct reaction of Ga₂O₃ thin films with flowing ammonia in a horizontal oven without using a template or catalyst. X-ray diffraction (XRD), scanning electron microscopy (SEM), energy-dispersive X-ray (EDX), transmission electron microscopy (TEM) and photoluminescence (PL) were used to characterize the samples. The straight and smooth cylindrical nanostructures are high quality single crystalline hexagonal wurtzite GaN nanowires with diameters ranging from 5 to 30 nm and lengths up to 20 μm. The near-band-edge emission peak located at 367 nm was observed at room temperature.     

ZnO纳米线的合成与生长机理

采用化学气相沉积系统制备ZnO纳米线,以覆盖一层约5nm厚的Ag薄膜的单晶Si(001)为衬底,纳米线的生长遵循气-液-固(VLS)机理。对得到的样品采用X射线衍射(XRD)和扫描电镜(SEM)进行晶体结构和形貌的表征。XRD结果表明衬底温度在600~700℃时生长的ZnO纳米线具有六方结构和统一的取向。通过扫描电子显微镜分析,比较了生长温度对纳米线直径和长度的影响。实验表明我们可以通过催化剂和温度来实现ZnO纳米线生长的可控。与传统的VLS生长方式不同的是在我们制备的ZnO纳米线顶端并没有看到催化剂颗粒,表明纳米线的生长方式是底部生长,我们对其生长机理进行了研究。     

常压下金催化硅纳米线生长实验研究

采用固一液一固（SLS）生长机制,研究常压下金催化硅纳米线的制备方法。实验中将硅基Au薄膜在氩氢气中退火,退火温度为1050℃和1080℃,退火完成后在扫描电镜下观察硅片表面的形貌变化,分析不同退火温度、通气量和金膜厚度下的实验结果,并在此基础上进一步讨论了各变量对硅纳米线的生长影响及其机理。     

Surface characteristics of Ni catalystic films on growth behavior of multi-walled carbon nanotubes

The effect of the surface characteristics of Ni catalyst films on the growth behavior of multi-walled carbon nanotubes (MWCNTs) were investigated using Ni catalyst films prepared by different physical vapor deposition methods, electron-beam evaporation and sputtering. The growth behavior of MWCNTs was dependent upon the surface roughness of the Ni films. After a pretreatment process with NH₃, the root mean squares of surface roughness of e-beam evaporated and sputtered Ni catalyst films increased to 16.6 and 3.2 nm, respectively. Curled-MWCNTs and carbon-encapsulated Ni nanoparticles were formed on the Ni film deposited by e-beam evaporation while vertically aligned-MWCNTs were grown on the sputter-deposited film. In addition, the surface roughness of the Ni films affected the field emission properties of the MWCNTs. This was considered to originate from the specific growth behavior of the MWCNTs which was primarily caused by the initial surface roughness of the Ni films.     

Synthesis and characterization of GaN nanowires by ammoniating Ga2O3/Cr thin films deposited on Si(1 1 1) substrates

GaN nanowires have been successfully synthesized on Si(1 1 1) substrates by magnetron sputtering through ammoniating Ga₂O₃/Cr thin films at 950 °C. X-ray diffraction (XRD), X-ray photoelectron spectroscopy (XPS), FT-IR spectrophotometer, scanning electron microscopy (SEM), high-resolution transmission electron microscopy (TEM), and photoluminescence (PL) spectrum were carried out to characterize the microstructure, morphology, and optical properties of GaN samples. The results demonstrate that the nanowires are single-crystal GaN with hexagonal wurtzite structure and high-quality crystalline, have the size of 30-80 nm in diameter and several tens of microns in length with good emission properties. The growth direction of GaN nanowires is perpendicular to the fringe of (1 0 1) plane. The growth mechanism of GaN nanowires is also discussed in detail.     

Effects of the sputtering time of ZnO buffer layer on the quality of GaN thin films

ZnO thin films with different thickness (the sputtering time of ZnO buffer layers was 10 min, 15 min, 20 min, and 25 min, respectively) were first prepared on Si substrates using radio frequency magnetron sputtering system and then the samples were annealed at 900 °C in oxygen ambient. Subsequently, a GaN epilayer about 500 nm thick was deposited on ZnO buffer layer. The GaN/ZnO films were annealed in NH₃ ambient at 950 °C. X-ray diffraction (XRD), atom force microscopy (AFM), X-ray photoelectron spectroscopy (XPS) and photoluminescence (PL) were used to analyze the structure, morphology, composition and optical properties of GaN films. The results show that their properties are investigated particularly as a function of the sputtering time of ZnO layers. For the better growth of GaN films, the optimal sputtering time is 15 min.     

Applications of electron microscopy to the characterization of semiconductor nanowires

We review our current progress on semiconductor nanowires of β-Ga₂O₃, Si and GaN. These nanowires were grown using both vapor–solid (VS) and vapor–liquid–solid (VLS) mechanisms. Using transmission electron microscopy (TEM) we studied their morphological, compositional and structural characteristics. Here we survey the general morphologies, growth directions and a variety of defect structures found in our samples. We also outline a method to determine the nanowire growth direction using TEM, and present an overview of device fabrication and assembly methods developed using these nanowires. PACS 61.14.-x; 81.07.-b; 61.14.Lj; 81.05.-t     

The effect of substrate surface roughness on ZnO nanostructures growth

The ZnO nanowires have been synthesized using vapor-liquid-solid (VLS) process on Au catalyst thin film deposited on different substrates including Si(1 0 0), epi-Si(1 0 0), quartz and alumina. The influence of surface roughness of different substrates and two different environments (Ar + H₂ and N₂) on formation of ZnO nanostructures was investigated. According to AFM observations, the degree of surface roughness of the different substrates is an important factor to form Au islands for growing ZnO nanostructures (nanowires and nanobelts) with different diameters and lengths. Si substrate (without epi-taxy layer) was found that is the best substrate among Si (with epi-taxy layer), alumina and quartz, for the growth of ZnO nanowires with the uniformly small diameter. Scanning electron microscopy (SEM) reveals that different nanostructures including nanobelts, nanowires and microplates have been synthesized depending on types of substrates and gas flow. Observation by transmission electron microscopy (TEM) reveals that the nanostructures are grown by VLS mechanism. The field emission properties of ZnO nanowires grown on the Si(1 0 0) substrate, in various vacuum gaps, were characterized in a UHV chamber at room temperature. Field emission (FE) characterization shows that the turn-on field and the field enhancement factor (β) decrease and increases, respectively, when the vacuum gap (d) increase from 100 to 300 μm. The turn-on emission field and the enhancement factor of ZnO nanowires are found 10 V/μm and 1183 at the vacuum gap of 300 μm.     

Surface morphology of ZnO buffer layer and its effects on the growth of GaN films on Si substrates by magnetron sputtering

ZnO thin films were first prepared on Si(111) substrates using a radio frequency magnetron sputtering system. Then the as-grown ZnO films were annealed in oxygen ambient at temperatures of 700, 800, 900, and 1000°C , respectively. The morphologies of ZnO films were studied by an atom force microscope (AFM). Subsequently, GaN epilayers about 500 nm thick were deposited on the ZnO buffer layers. The GaN/ZnO films were annealed in NH₃ ambient at 900°C. The microstructure, morphology and optical properties of GaN films were studied by x-ray diffraction (XRD), AFM, scanning electron microscopy (SEM) and photoluminescence (PL). The results are shown, their properties having been investigated particularly as a function of the ZnO layers. For better growth of the GaN films, the optimal annealing temperature of the ZnO buffer layers was 900°C.