Deposition and properties of highly C-oriented GaN films on diamond substrates

High-quality GaN films are deposited on freestanding thick diamond films by electron cyclotron resonance plasma enhanced metal organic chemical vapor deposition (ECR-PEMOCVD). The TMGa flux dependent structural, morphological, and electrical characteristics of GaN films were investigated by x-ray diffraction analysis (XRD), reflection high-energy electron diffraction (RHEED), atomic force microscopy (AFM) and Hall effect measurement. The results indicate that it is feasible to deposit GaN films on freestanding thick diamond films under the proper deposition procedures. The high-quality GaN films with small surface roughness of 4.9 nm and high c-orientation are successfully achieved at the optimized TMGa flux of 0.5 sccm. The GaN/diamond structure has great potential for the development of SAW devices with high frequencies and low insertion.     

Etch Damage Evaluation in Integrated Ferroelectric Capacitor Side Wall by Piezoresponse Force Microscopy

The etch damage in integrated ferroelectric capacitors side wall fabricated by the typical integrated process (TIP-FeCAP) and the innovated integrated process (IIP-FeCAP) are investigated by piezoresponse force microscopy (PFM). The IIP-FeCAP side wall exhibits fine and clear nanoscale domain images and the same piezoresponse signal as the thin film, and the domains can also be easily switched by an external voltage. In the TIP-FeCAP side wall, owing to the effect of etch damage, the very weak piezoresponse signal and some discrete domains can be observed, and the discrete domains cannot be switched by the applied 9V and -9V dc voltage. The PFM results reflect the etch damage in the integrated ferroelectric capacitors and also suggest that the PFM can be used as an efficacious tools to evaluate the etch damage at nanoscale and spatial variations.     

Evaluation of the contact resonance frequencies in atomic force microscopy as a method for surface characterisation (invited)

The combination of ultrasound with atomic force microscopy (AFM) opens the high lateral resolution of scanning probe techniques in the nanometer range to ultrasonics. One possible method is to observe the resonance frequencies of the AFM sensors under different tip-sample interaction conditions. AFM sensors can be regarded as small flexible beams. Their lowest flexural and torsional resonance frequencies are usually found to be in a range between several kHz and several MHz depending on their exact geometrical shape. When the sensor tip is in a repulsive elastic contact with a sample surface, the local indentation modulus can be determined by the contact resonance technique. Contact resonances in the ultrasonic frequency range can also be used to improve the image contrast in other dynamic techniques as, for example, in the so-called piezo-mode. Here, an alternating electric field is applied between a conducting cantilever and a piezoelectric sample. Via the inverse piezoelectric effect, the sample surface is set into vibration. This excitation is localised around the contact area formed by the sensor tip and the sample surface. We show applications of the contact resonance technique to piezoelectric ceramics.     

溶胶-凝胶法制备氧化锌薄膜的压电行为

"采用溶胶-凝胶技术在单晶硅Si(111)上制备了ZnO压电薄膜,并以扫描电镜、X射线衍射仪(XRD)和原子力显微镜(AFM)进行了表征．XRD衍射实验表明ZnO薄膜随着膜厚的增大,其(002)取向逐渐增强;AFM研究了薄膜的表面形貌、粗糙度与晶粒大小的结果表明,ZnO压电薄膜的粗糙度与晶粒寸随着薄膜厚度的增大而减小．粗糙度为2.188~0.914 nm．利用PFM研究压电系数,发现随着薄膜厚度的增加,(002)生长方向增强,压电系数逐渐增大;当力参数小于薄膜的表面粗糙度时,压电系数测量不准确且在较大幅度     

Direct characterization of nanoscale domain switching and local piezoelectric loops of (Pb,La)TiO3 thin films by piezoresponse force microscopy

〈111〉 and 〈001〉, 〈100〉 preferentially oriented lanthanum-modified lead titanate thin films have been studied at the nanometre scale by means of piezoresponse force microscopy. The nanoscale domain structures, domain switching, and local piezoelectric loops of the films have been analysed. The imaging of the domain structures after the application of a dc field suggests the existence of 90° and 180° domains within the regions with intermediate contrast. The variation of piezoresponse under an electric field in domains of two types has been discussed. Significant differences have been found between the local piezoelectric loops measured in the films deposited on different substrates. These differences are related to the different textures present in the films. PACS 61.16.Ch; 77.84.Dy; 77.80.Dj     

Combined piezoresponse force microscopy and Raman scattering investigation of domain boundaries in BiFeO3 ceramics

Domain structure of BiFeO₃ ceramics has been investigated using a combination of piezoresponse force microscopy (PFM) and Raman scattering techniques. Both methods demonstrate the presence of ferroelastic domains, separated by almost parallel planar domain walls, as well as the presence of large homogeneous single ferroelastic domain regions. In addition to highly resolved domain pattern obtained by PFM, small frequency shifts of the Raman-active modes give us complementary information about the angle φ between the surface normal and the rhombohedral axis of the BiFeO₃ crystal for any measured position at the surface of the sample.     

New design of nozzle structures and its effect on the surface and crystal qualities of thick GaN using a horizontal HVPE reactor

High-quality thick GaN films without cracks were achieved by using a new nozzle structure in the reactor grown by the hydride vapor phase epitaxy on sapphire substrates. Optical contrast microscopy, scanning electron microscopy (SEM), atomic force microscopy (AFM), X-ray double diffraction (XRD) and cathodoluminescence (CL) were carried out to reveal the surface, crystal and optical properties of the GaN epilayer. It was found that the nozzle structure in the reactor has a large effect on the growth rate, surface flat, crystal quality, and the uniformity of the growth. Compared with the old one, the new nozzle structure (denoted as multi-layers nozzle) can improve dramatically the properties of thick GaN. Mirror, colorless and flat GaN thick film was obtained and its (0 0 0 2) FWHM results were reduced from 1000 to 300 arcsec when the new nozzle was used. AFM result revealed a step flow growth mode for GaN layer with the new nozzle. Room-temperature CL spectra on the GaN films showed a strong near-band-edge peak for the new nozzle, but there is only weak emitting peak for the old nozzle. New nozzle structure can improve the uniform of flow field near the surface of substrates compared with the old one, which leads to the improvement of properties of GaN thick film by hydride vapor phase epitaxy (HVPE).     

Relationship between the microstructure and the microscopic piezoelectric response of the <Emphasis Type="Italic">α</Emphasis>- and <Emphasis Type="Italic">β</Emphasis>-phases of poly(vinylidene fluoride)

The piezoelectric and pyroelectric properties of PVDF mainly depend on its β-phase. This work reports the study by scanning force microscopy in a piezoresponse mode of the variations in the topological morphology and piezoelectric surface response of β-PVDF prepared by the main preparation methods of this phase. Clear differences in the poled region distribution and size, as well as in the local piezoactivity, have been identified. The piezoelectric activity at a mesoscale reflects the semicrystalline phase of the polymer.     

YMnO_3薄膜的铁电行为及其纳米尺度铁电畴的研究

六方YMnO_3是一种特殊的多铁性材料,因其具有介电常数低、单一极化轴、无挥发性元素等特点,在磁电领域具有独特的优势,但目前关于YMnO_3薄膜的铁电性特别是畴结构的研究相对较少.本文采用溶胶-凝胶法在Si(100)基片上制备了多铁性YMnO_3薄膜,利用掠入射X-射线衍射、原子力显微镜对薄膜的结构及表面形貌进行了分析,用压力显微镜(PFM)技术研究了纳米尺度畴结构及微区电滞行为,并通过I-V,P-E曲线进一步研究了薄膜的漏电流和宏观电滞行为.结果表明,该薄膜为六方钙钛矿结构,YMnO_3晶粒大小均匀并且结晶性较好,薄膜表面粗糙度为7.209 nm.PFM图显示出清晰的电畴结构,结合典型的微区振幅蝴蝶曲线和相位电滞回线,证实该YMnO_3薄膜具有较好的铁电性.由于受内建电场的作用,振幅曲线和相位曲线都向正向偏移,表现出非对称特征.该薄膜的漏电流密度低于10~(-6)A·cm~(-2),因而其电滞回线基本能够达到饱和.     

Domain configuration and dielectric properties of Ba0.6Sr0.4TiO3 thin films

The microstructure and electrical properties of Ba_0.6Sr_0.4TiO₃ thin films have been investigated. Nanometer-sized domains, ranging from 8 to about 30 nm, were observed by piezoresponse force microscopy (PFM). The critical size, below which only single domains exist, is found to be about 31 nm. The film exhibits ferroelectric behavior characterized by polarization hysteresis loop and capacitance-voltage curve.     

Effects of Sm substitution on ferroelectric domains and conductivity in bismuth ferrite ceramics

The large piezoelectric coefficient and multiferroicity of bismuth ferrite (BFO) make it an attractive candidate for lead-free ferroelectric devices. However, large leakage currents have limited broader applications. Rare-earth substitutions in BFO have been shown to improve ferroelectric and magnetic properties. In this work, we employed piezoresponse and conductive atomic force microscopy to study ferroelectric domains in Bi_1-xSm_xFeO₃ (x = 0–0.150) grown by the co-precipitation method. The combined piezoresponse and conductivity measurements can directly visualize the local ferroelectric domains under different sample bias. At Sm mol% > 7.5, Sm-substitution effectively lowers defect-generated conductivity. At Sm mol% < 7.5, conductivity increases due to conductive domain walls inside sample grains. The surfaces of these conductive samples exhibit a p-type rectifying behavior while the bulk is n-type. Our work details how the local piezoelectric properties and transport behaviors of BFO ceramics change as a function of Sm-substitution.     

Observation of antiphase domains in Cd<Subscript>x</Subscript>Hg<Subscript>1−<Emphasis Type="Italic">x</Emphasis></Subscript>Te films on silicon by the phase contrast method in atomic force microscopy

It has been shown that phase contrast in atomic force microscopy (AFM) can be used to obtain adequate information on the density and distribution of antiphase domains on the surface of CdHgTe films grown by molecular beam epitaxy on a Si(301) substrate. By comparing the AFM phase images of the film surface with TEM images of structural defects in the near-surface region, the relation between microstructure and micromorphology of the films is revealed.     

Piezoresponse imaging and local characterization of ferroelectric domains in Pb(Zn1/3Nb2/3)O3–7%PbTiO3 single crystals

Ferroelectric domain structures of (001)‐oriented Pb(Zn_1/3Nb_2/3)O₃–7%PbTiO₃ (PZN‐7%PT) single crystals were visualized and characterized by piezoresponse force microscopy (PFM). Locally regular domain configurations are found to be possibly related to the stable macroscopic properties in the PZN‐7%PT single crystals. Nanoscale piezoresponse hysteresis loops measured by PFM tip revealed no evidence of local domain switching behavior in the PZN‐7%PT single crystal. (© 2007 WILEY‐VCH Verlag GmbH & Co. KGaA, Weinheim)     

Unusual domain configurations and local piezoresponse in the [720]‐cut BaTiO3 single crystal

The domain configurations and local piezoresponse property of the [720]‐cut BaTiO₃ single crystal and [001]‐oriented BaTiO₃ crystal were investigated by high‐resolution piezoresponse force microscopy. Large differences in their surface topography features, domain configurations and local piezoresponse were found between [720]‐cut and [001]‐oriented BaTiO₃ crystals. The large surface bending angle due to ferroelastic domain walls leads to a high strain energy appearing in the [720]‐cut BaTiO₃, further resulting in unique band‐like topographic features, needle domains for stress compensation and locally ultrahigh piezoelectric response as well. (© 2013 WILEY‐VCH Verlag GmbH & Co. KGaA, Weinheim)     

Characteristics of low-temperature-grown GaN films on Si(111)

In this paper, we report on the characteristics of GaN films grown on Si(111) at a low temperature (200 °C) by electron cyclotron resonance (ECR) plasma-assisted metalorganic chemical vapor deposition (PA-MOCVD). Structural analysis of the GaN films was performed by using scanning electron microscopy (SEM), atomic force miscroscopy (AFM), X-ray diffraction (XRD), energy dispersive X-ray analysis (EDX), and Rutherford backscattering spectrometry (RBS). Post deposition analysis revealed high quality crystalline GaN was obtained at this low temperature. Electrical analysis of the GaN films was done by using current-voltage (I-V) measurements where electrical characterizations were carried on GaN/Si heterojunction and Schottky barrier diodes. Rectification behaviour was observed for the isotype GaN/Si (n-n) heterojunction. Ideality factors and Schottky barrier heights for Ni and Cr Schottky barriers on GaN, were deduced to be 1.4 and 1.7; and 0.62 and 0.64 eV, respectively.     

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.     

Effect of Ⅲ/Ⅴ Ratio of HT-AIN Buffer Layer on Polarity Selection and Electrical Quality of GaN Films Grown by Radio Frequency Molecular Beam Epitaxy

We investigate the effect of A/N ratio of the high temperature （HT） AIN buffer layer on polarity selection and electrical quality of GaN films grown by radio frequency molecular beam epitaxy. The results show that low Al/N ratio results in N-polarity GaN films and intermediate Al/N ratio leads to mixed-polarity GaN films with poor electrical quality. GaN films tend to grow with Ga polarity on Al-rich AIN buffer layers. GaN films with different polarities are confirmed by in-situ reflection high-energy electron diffraction during the growth process. Wet chemical etching, together with atomic force microscopy, also proves the polarity assignments. The optimum value for room-temperature Hall mobility of the Ga-polarity GaN film is 703cm^2/V.s, which is superior to the N-polarity and mixed-polarity GaN films.     

Temperature dynamics of triglycine sulfate domain structure according to atomic force microscopy and dielectric spectroscopy data

A hydrogen-containing ferroelectric triglycine sulfate (TGS) was comprehensively studied with an atomic force microscopy (AFM) and dielectric spectroscopy. The domain structure dynamics was in situ investigated with piezoresponse force microscopy (PFM) during heating and cooling the TGS crystal near phase transition. Relaxation dependencies of domain boundaries general perimeter and domain dimensions were obtained. TGS dielectric spectra measured at the frequency range from 10 to 10¹¹ Hz were analyzed on basis of significant contribution of conductivity into the dielectric response of ferroelectrics and a good agreement with the experimental data was received. It allows us to obtain more information about temperature dynamics of the domain structure.     

Electronic structure of GaN(0001)‐2 × 2 thin films grown by PAMBE

Gallium nitride thin films were grown on silicon carbide (0001) by plasma‐assisted molecular beam epitaxy (PAMBE). The samples were cooled down in nitrogen plasma and characterized in situ by reflection high energy electron diffraction (RHEED), photoelectron spectroscopy (XPS/UPS), and atomic force microscopy (AFM) revealing stoichiometric and smooth GaN films virtually free of contaminations. We present valence band data obtained by UPS with strong emission from surface states inside the fundamental band gap. These states and the observed 2 × 2 surface reconstruction are highly sensitive towards residual molecules. Once these surface states have disappeared the original state could not be recovered by surface preparation methods underlining the necessity of in situ investigations on as‐grown surfaces. (© 2008 WILEY‐VCH Verlag GmbH & Co. KGaA, Weinheim)     

Acoustic Imaging Frequency Dynamics of Ferroelectric Domains by Atomic Force Microscopy

We report the acoustic imaging frequency dynamics of ferroelectric domains by low-frequency acoustic probe microscopy based on the commercial atomic force microscopy. It is found that ferroelectric domain could be firstly visualized at lower frequency down to 0.5 kHz by AFM-based acoustic microscopy. The frequency-dependent acoustic signal revealed a strong acoustic response in the frequency range from 7kHz to 10 kHz, and reached maximum at 8.1 kHz. The acoustic contrast mechanism can be ascribed to the different elastic response of ferroelectric microstructures to local elastic stress fields, which is induced by the acoustic wave transmitting in the sample when the piezoelectric transducer is vibrating and exciting acoustic wave under ac electric fields due to normal piezoelectric effects.