Local structure in perovskite relaxor ferroelectrics: high-resolution Nb 3QMAS NMR

Solid solutions of (1'-x)Pb(Mg(1/3)Nb(2/3))O3xPb(Sc(1/2)Nb(1/2))O3 (PMN/PSN) have been investigated using high-resolution 93Nb 3-quantum magic-angle spinning nuclear magnetic resonance experiments (3QMAS NMR). In previous MAS NMR investigations, the local B-cation ordering in these relaxor ferroelectric solid solutions was quantitatively determined. However, in conventional one-dimensional MAS spectra the effects of chemical shifts and quadrupole interaction are convoluted; this, in addition to the insufficient resolution, precludes reliable extraction of the values of isotropic chemical shift and quadrupole coupling product. In the current 3QMAS investigation, 93Nb spectra are presented for concentrations x=0, 0.1, 0.2, 0.6, 0.7, and 0.9 at high magnetic field (19.6 T) and fast sample spinning speed (35.7 kHz). Seven narrow peaks and two broad components are observed. The unique high-resolution of the two-dimensional 3QMAS spectra enables unambiguous and consistent assignments of spectral intensities to the specific 28 nearest B-site neighbor (nBn) configurations, (NMg, NSc, NNb) where each number ranges from 0 to 6 and their sum is 6. It is now possible to isolate the isotropic chemical shift and quadrupole coupling product and separately determine their values for most of the 28 nBn configurations. The isotropic chemical shift depends linearly on the number of Mg2+ cations in the configuration; delta iso CS=(13.7 +/- 0.1)NMg-970 +/- 0.4 ppm, regardless of the ratio NSc/NNb. For the seven Nb5+-deficient configurations (NMg, 6-NMg, 0) and the pure niobium configuration (0, 0, 6), the quadrupole coupling products (and hence the electric field gradients) are small (PQ approximately 6-12 MHz) and for the remaining configurations containing small, ferroelectric active Nb5+ ions, the quadrupole coupling products are significantly larger (PQ approximately 40 MHz), indicating larger electric field gradients.     

Local structure in perovskite relaxor ferroelectrics: high-resolution 93Nb 3QMAS NMR

Solid solutions of (1'-x)Pb(Mg(1/3)Nb(2/3))O3xPb(Sc(1/2)Nb(1/2))O3 (PMN/PSN) have been investigated using high-resolution 93Nb 3-quantum magic-angle spinning nuclear magnetic resonance experiments (3QMAS NMR). In previous MAS NMR investigations, the local B-cation ordering in these relaxor ferroelectric solid solutions was quantitatively determined. However, in conventional one-dimensional MAS spectra the effects of chemical shifts and quadrupole interaction are convoluted; this, in addition to the insufficient resolution, precludes reliable extraction of the values of isotropic chemical shift and quadrupole coupling product. In the current 3QMAS investigation, 93Nb spectra are presented for concentrations x=0, 0.1, 0.2, 0.6, 0.7, and 0.9 at high magnetic field (19.6 T) and fast sample spinning speed (35.7 kHz). Seven narrow peaks and two broad components are observed. The unique high-resolution of the two-dimensional 3QMAS spectra enables unambiguous and consistent assignments of spectral intensities to the specific 28 nearest B-site neighbor (nBn) configurations, (NMg, NSc, NNb) where each number ranges from 0 to 6 and their sum is 6. It is now possible to isolate the isotropic chemical shift and quadrupole coupling product and separately determine their values for most of the 28 nBn configurations. The isotropic chemical shift depends linearly on the number of Mg2+ cations in the configuration; delta iso CS=(13.7 +/- 0.1)NMg-970 +/- 0.4 ppm, regardless of the ratio NSc/NNb. For the seven Nb5+-deficient configurations (NMg, 6-NMg, 0) and the pure niobium configuration (0, 0, 6), the quadrupole coupling products (and hence the electric field gradients) are small (PQ approximately 6-12 MHz) and for the remaining configurations containing small, ferroelectric active Nb5+ ions, the quadrupole coupling products are significantly larger (PQ approximately 40 MHz), indicating larger electric field gradients.     

Field cooled and zero field cooled 207Pb NMR and the local structure of relaxor PbMg1/3Nb2/3O3

An isotropic 207Pb NMR spectrum corresponding to the glassy matrix with spherical shell type Pb shifts from the cubic sites, as well as an anisotropic spectral component corresponding to polar nanoclusters with a Pb shift parallel to the [111] direction, have been observed in a PbMg(1/3)Nb(2/3)O3 (PMN) single crystal. This represents a microscopic confirmation of the model of relaxors first proposed by Burns and Dacol. A sudden increase in the intensity of the anisotropic cluster line is seen for electric fields larger than the critical field around 210 K. This demonstrates the occurrence of an orientational percolation type transition to the field-induced ferroelectric phase with about 50% of the Pb nuclei still remaining in the spherical glass matrix. A similar though smaller increase of the intensity of this line is also seen in the zero field cooled data, demonstrating that relaxor PMN is an incipient ferroelectric.     

Nb/Nb3Sn复合超导材料的高压电子显微镜观察

用1000kV高压电子显微镜观察了单芯和多芯Nb/Nb₃Sn复合材料的显微组织,看到了由Nb₃Sn/Nb₃Sn晶粒重叠而成的叠栅图和Nb基体/Nb₃Sn晶粒重叠而成的叠栅图。 关键词：     

Properties of superconducting Nb/Al/Nb/Al?AlOx?Al?AlOx?Al/Nb/Al/Nb tunnel junctions

Modified geometry (MG) devices, Nb/Al/Nb/Al−AlO_x−Al−AlO_x−Al/Nb/Al/Nb, have been fabricated and investigated in comparison with the basic geometry (BG) double-barrier Nb/Al−AlO_x−Al−AlO_x−Al/Nb devices. The enhancement of the critical temperature in the Al film is found to be weaker for the MG devices as compared with the BG devices at temperatures nearT=4.2 K but stronger at lowT. Indication of an enhancement of dc Josephson critical current density,j _c , at bias voltageV≠0 as compared withj _c (V=0) has been observed in the MG devices for the first time.     

93Nb NMR chemical shift scale for niobia systems

⁹³Nb solid-state NMR spectra of a series of inorganic niobates with Nb in different oxygen coordination environments were measured. For all studied compounds the chemical shielding and quadrupole tensor parameters were determined using conventional and ultrahigh field NMR facilities, ultrahigh speed MAS, DQ STMAS, solid-echo and computer modeling. It has been demonstrated that the ⁹³Nb isotropic chemical shift is sensitive to the coordination number of Nb sites. For the first time the ⁹³Nb NMR chemical shift scale for NbO_x polyhedra in solid materials has been proposed: for four-coordinated Nb sites, the isotropic shifts occur from −650 to −950 ppm; five-coordinated Nb sites have the isotropic shifts in the range of –900 to –980 ppm; for six-coordinated Nb sites the isotropic shifts vary from −900 to −1360 ppm; the shifts from −1200 to −1600 ppm are typical for seven-coordinated Nb sites; for eight-coordinated Nb sites the shifts are higher than −1400 ppm. The possible correlation between the value of the isotropic chemical shift and the ionic character of the NbO_x–MO_y polyhedra association has been suggested. The magnitude of the ⁹³Nb quadrupole coupling constant depends on the local symmetry of Nb sites and may vary from hundreds of kHz to hundreds of MHz.     

Ion channeling studies of KTaO3:Nb

Ion channeling measurements have been performed on KTaO₃:Nb (KTN) in order to check the position of Nb relative to the tantalum site. No evidence for “off-center” Nb was found in the limit of experimental accuracy. In addition, the carbon content of the samples was measured and large concentrations were found (?300 p.p.m. weight). Possible relationship between Nb location and carbon presence is discussed.     

Influence of the transparency of tunnel barriers in Nb/Al2O3/Al/Al2O3/Nb junctions on transport properties

The transparency of the tunnel barriers in double-barrier junctions influences the critical current density and the form of the current–voltage characteristics (IVC). Moreover, the barrier asymmetry is an important parameter, which has to be controlled in the technological process. We have performed a systematic study of the influence of the barrier transparency on critical current, I_C, and normal resistance, R_N, by preparing SIS and SINIS junctions under identical technological conditions and comparing their transport properties. We have fabricated Nb/Al₂O₃/Nb and Nb/Al₂O₃/Al/Al₂O₃/Nb devices with different current densities using a conventional fabrication process, varying pressure and oxidation time. The thickness of the Al middle electrode in all Nb/Al₂O₃/Al/Al₂O₃/Nb junctions was 6 nm. Patterning of the multilayers was done using conventional photolithography and the selective niobium etching process. The current density of SIS junctions was changed in the range from 0.5 to 10 kA/cm². At the same conditions the current density of SINIS devices revealed 1–100 A/cm² with non-hysteretic IVC and characteristic voltages, I_CR_N, of up to 200 μV. By comparing the experimental and theoretical temperature dependence of the I_CR_N product we estimated the barrier transparency and its asymmetry. The comparison shows a good agreement of experimental data with the theoretical model of tunneling through double-barrier structures in the dirty limit and provides the effective barrier transparency parameter γ_eff≈300. A theoretical framework is developed to study the influence of the barrier asymmetry on the current–phase relationship and it is proposed to determine the asymmetry parameter by measuring the critical current suppression as function of applied microwave power. The theoretical approach to determine the non-stationary properties of double-barrier junctions in the adiabatic regime is formulated and the results of calculations of the I–V characteristics are given in relevant limits. The existence and the magnitude of a current deficit are predicted as function of the barrier asymmetry.     

Nb/Al-AlO_x/Nb隧道结制备中压控电压源阳极氧化工艺研究

采用计算机程控的压控电压源阳极氧化模式研究制备出自对准Nb/Al-AlOx/Nb隧道结的绝缘层Nb2O5/Al2O3/Nb2O5。研究了氧化电压、氧化层的厚度和氧化时间的关系。当阳极氧化电压变化率低于8V/min时,阳极氧化层的厚度基本取决于氧化电压的大小,而与氧化电压变化率无关。我们已采用电压源阳极氧化技术成功制备出超导Nb/Al-AlOx/Nb隧道结。     

Electron-Spectroscopic Studies of Thermal Stability of Pd/Nb Surfaces

The room-temperature growth of Pd on a clean quasiamorphous, nanostructured Nb surfaces and thermal stability of Pd/Nb interface in the temperature range (295-660) K have been studied by X-ray photoelectron spectroscopy (XPS) and X-ray induced Auger electron spectroscopy. The measured spectra of Pd (3d) and Nb (3d) electrons indicate presence of a surface Pd-Nb alloy-like phase in the region of submonolayer Pd coverage at room temperature. The Pd (3d) core level shifts can be explained in terms of initial state effects. For multilayer deposits an intermetallic phase is observed in the Pd/Nb interface at room temperature. Inward diffusion of Pd occurs folowed by the formation of three-dimensional alloy at temperatures above 500 K.     

Nb/Al-AlOx/Nb隧道结的制备

本文报道了在射频磁控溅射装置上Nb/Al-AlO_x/Nb隧道结的制备工艺和所获得的结果。对SIS三层结构形成时基片的温度、势垒,以及电极形成方法等问题进行了讨论。 关键词：     

XPS valence band spectra of Nb3Sn,Nb and Sn

XPS valence band spectra of Nb₃Sn, Nb and Sn have been obtained under high resolution. The 4d band structure in the Nb₃Sn spectrum is similar to that seen in Nb metal.     

Synthesis and structural characterization of Znb3Nb2 powder

Science China Physics, Mechanics & Astronomy - Zinc nitride (Znb3Nb2) powder has been synthesized through the nitridation reaction of Zn powder with NH3 gas (at the flow rate of 500 ml/min) at...     

Satellite-transition MAS NMR of spin I = 3/2, 5/2, 7/2, and 9/2 nuclei: sensitivity,resolution, and practical implementation

The satellite-transition MAS (STMAS) experiment offers an alternative approach to established methods such as dynamic angle spinning (DAS), double rotation (DOR), and multiple-quantum MAS (MQMAS) for obtaining high-resolution NMR spectra of half-integer quadrupolar nuclei. Unlike the multiple-quantum experiment, STMAS involves two-dimensional correlation of purely single-quantum coherences; satellite transitions in t(1) (or F(1)) and the central transition in t(2) (or F(2)). To date, STMAS has primarily been demonstrated for nuclei with spin quantum numbers I = 3/2 and, to a lesser extent, I > 5/2. However, many chemically relevant nuclei possess I > 3/2, such as (17)O and (27)Al (both I = 5/2), (59)Co (I = 7/2), and (93)Nb (I = 9/2). Here, we discuss the application of STMAS to nuclei with spin quantum numbers from I = 3/2 to 9/2. First, we consider the practical implementation of the STMAS experiment using (87)Rb (I = 3/2) NMR as an example. We then extend the discussion to include nuclei with higher spin quantum numbers, demonstrating (27)Al, (45)Sc (I = 7/2), (59)Co, and (93)Nb STMAS experiments on both crystalline and amorphous samples. We also consider the possibility of experiments involving satellite transitions other than m(I) = +/- 1/2 <--> +/- 3/2 and, using (93)Nb NMR, demonstrate the correlation of all single-quantum satellite transitions up to and including m(I) = +/- 7/2 <--> +/- 9/2. The absolute chemical shift scaling factors in these experiments are discussed, as are the implications for isotropic resolution.     

Nb 3d and O 1s core levels and chemical bonding in niobates

A set of available experimental data on binding energies of Nb 3d_5/2 and O 1s core levels in niobates has been observed with using energy difference (O 1sNb 3d_5/2) as a robust parameter for compound characterization. An empirical relationship between (O 1sNb 3d_5/2) values measured with XPS for Nb⁵⁺-niobates and mean chemical bond length L(NbO) has been discussed. A range of (O 1sNb 3d_5/2) values possible in Nb⁵⁺-niobates has been defined. An energy gap ∼1.4–1.8 eV is found between (O 1sNb 3d_5/2) values reasonable for Nb⁵⁺ and Nb⁴⁺ states in niobates.     

Fabrication of high-quality submicron Nb/Al--AlOx/Nb tunnel junctions

Nb/Al-AlOx/Nb tunnel junctions are often used in the studies of macroscopic quantum phenomena and superconducting qubit applications of the Josephson devices. In this work, we describe a convenient and reliable process using electron beam lithography for the fabrication of high-quality, submicron-sized Nb/Al-AlOx/Nb Josephson junctions. The technique follows the well-known selective Nb etching process and produces high-quality junctions with Vm=100 mV at 2.3 K for the typical critical current density of 2.2 kA/cm^2, which can be adjusted by controlling the oxygen pressure and oxidation time during the formation of the tunnelling barrier. We present the results of the temperature dependence of the sub-gap current and in-plane magnetic-field dependence of the critical current, and compare them with the theoretical predictions.     

Proximity-Effect-Induced Superconductivity in Nb/Sb2Te3-Nanoribbon/Nb Junctions

Nanohybrid superconducting junctions using antimony telluride (Sb₂Te₃) topological insulator nanoribbons and Nb superconducting electrodes are fabricated using electron beam lithography and magnetron sputtering. The effects of bias current, temperature, and magnetic field on the transport properties of the junctions in a four-terminal measurement configuration are investigated. Two features are observed. First, the formation of a Josephson weak-link junction. The junction is formed by proximity-induced areas in the nanoribbon right underneath the inner Nb electrodes which are connected by the few tens of nanometers short Sb₂Te₃ bridge. At 0.5 K a critical current of 0.15 µA is observed. The decrease of the supercurrent with temperature is explained in the framework of a diffusive junction. Furthermore, the Josephson supercurrent is found to decrease monotonously with the magnetic field indicating that the structure is in the small-junction limit. As a second feature, a transition is also observed in the differential resistance at larger bias currents and larger magnetic fields, which is attributed to the suppression of the proximity-induced superconductive state in the nanoribbon area underneath the Nb electrodes.     

Temperature-dependent resistive switching behavior in the structure of Au/Nb:SrTiO3/Ti

Au/Nb:SrTiO₃/Ti structures were fabricated by depositing Au and Ti electrodes on a single crystal 0.5 wt% Nb:SrTiO₃ (NSTO) using rf-magnetron sputtering technique. Resistive switching properties at different temperature were investigated. The Ti/NSTO interface was ohmic contact, which indicated that the resistive switching behavior was attributed to Au/NSTO interface. The resistive switching behavior happened only at the temperature above 180 K, which was possibly caused by the increase of Schottky barrier height with the increase of temperature. The structure showed a semiconductor behavior at high-resistance state (HRS) and a metallic behavior at low-resistance state (LRS). The switching conduction mechanism of Au/NSTO/Ti device is primarily described as space-charge-limited conduction (SCLC) according to the electrical transport properties measurement.     

用于电压基准的Nb/NbxSi1-x/Nb约瑟夫森单结的研制

现代可编程约瑟夫森电压基准的核心器件是约瑟夫森结阵.目前最具有优势的约瑟夫森结阵是 Nb/Nb_xSi_1-x/Nb材料的结阵. Nb/Nb_xSi_1-x/Nb材料的约瑟夫森结 具有三层薄膜的制作过程简便, Nb和Nb_xSi_1-x刻蚀工艺相同以及Nb_xSi_1-x 势垒层成分可调等优点.中国计量科学研究院设计制作了Nb/Nb_xSi_1-x/Nb约瑟夫森单结. 通过在4.2 K低温下对所做单结进行直流电流-电压特性测量,观测到了清晰的超导隧穿电流和 从零电压态向电压态的跳变,最后就测量结果进行了分析讨论.此项工作属于国内首个开展 Nb/Nb_xSi_1-x/Nb材料约瑟夫森单结研究的工作.     

Nb/Al-AlOx/Nb junctions with controllable critical current density for qubit application

Nb/Al-AlOx/Nb tunnel junctions with controllable critical current density Jc are fabricated using the standard selective Nb etching process.Tunnel barriers are formed in different oxygen exposure conditions (oxygen pressure P and oxidation time t),giving rise to Jc ranging from 100 A/cm2 to above 2000 A/cm2.Jc shows a familiar linear dependence on P × t in logarithmic scales.We calculate the energy levels of the phaseand flux-type qubits using the achievable junction parameters and show that the fabricated Nb/Al-AlOx/Nb tunnel junctions can be used conveniently for quantum computation applications in the future.