MgB2 thick films deposited on stainless steel substrate with Tc higher than 39K

Thick MgB₂ (magnesium diborate) films, ∼10 μm, with T _c (onset) = 39.4 K and T _c (zero) = 39.2 K have been successfully grown on a stainless steel substrate using a technique called hybrid physical-chemical deposition (HPCVD). The deposition rate is high, ∼6.7 nm/s. The X-ray diffraction (XRD) indicates that it is highly (101) and c-axis oriented. The scanning electron microscope (SEM) images demonstrate that the film grown is in “island-mode”. The uniform superconducting phase in the film is shown by the M-T measurement.     

钛离子辐照对MgB2超导薄膜的载流能力和磁通钉扎能力的影响

利用混合物理化学气相沉积法(hybrid physical-chemical vapor deposition, HPCVD)可以制备出高性能的MgB₂超导薄膜, 再对薄膜进行钛(Ti)离子辐照处理.经过辐照处理后的样品被掺入了Ti元素, 与未处理的干净MgB₂样品相比,其超导转变温度没有出现大幅度的下降, 而在外加磁场下的临界电流密度得到了明显的提高,同时样品的上临界磁场也得到了提高. 在温度5 K, 外加垂直磁场为4 T的情况下, Ti离子辐照剂量为1× 10¹³/cm²的样品的临界电流密度达到了1.72× 10⁵ A/cm², 比干净的MgB₂要高出许多,而其超导转变温度仍能维持在39.9 K的较高水平.     

MgB2 coated superconducting tapes with high critical current densities fabricated by hybrid physical-chemical vapor deposition

The MgB₂ coated superconducting tapes have been fabricated on textured Cu (0 0 1) and polycrystalline Hastelloy tapes using coated conductor technique, which has been developed for the second generation high temperature superconducting wires. The MgB₂/Cu tapes were fabricated over a wide temperature range of 460-520 °C by using hybrid physical-chemical vapor deposition (HPCVD) technique. The tapes exhibited the critical temperatures (T_c) ranging between 36 and 38 K with superconducting transition width (ΔT_c) of about 0.3-0.6 K. The highest critical current density (J_c) of 1.34 × 10⁵ A/cm² at 5 K under 3 T is obtained for the MgB₂/Cu tape grown at 460 °C. To further improve the flux pinning property of MgB₂ tapes, SiC is coated as an impurity layer on the Cu tape. In contrast to pure MgB₂/Cu tapes, the MgB₂ on SiC-coated Cu tapes exhibited opposite trend in the dependence of J_c with growth temperature. The improved flux pinning by the additional defects created by SiC-impurity layer along with the MgB₂ grain boundaries lead to strong improvement in J_c for the MgB₂/SiC/Cu tapes. The MgB₂/Hastelloy superconducting tapes fabricated at a temperature of 520 °C showed the critical temperatures ranging between 38.5 and 39.6 K. We obtained much higher J_c values over the wide field range for MgB₂/Hastelloy tapes than the previously reported data on other metallic substrates, such as Cu, SS, and Nb. The J_c values of J_c(20 K, 0 T) ∼5.8 × 10⁶ A/cm² and J_c(20 K, 1.5 T) ∼2.4 × 10⁵ A/cm² is obtained for the 2-μm-thick MgB₂/Hastelloy tape. This paper will review the merits of coated conductor approach along with the HPCVD technique to fabricate MgB₂ conductors with high T_c and J_c values which are useful for large scale applications.     

MgB2 thick films deposited on stainless steel substrate with T c higher than 39 K

Thick MgB₂ (magnesium diborate) films, ～10 μm, with T _c (onset) = 39.4 K and T _c (zero) = 39.2 K have been successfully grown on a stainless steel substrate using a technique called hybrid physical-chemical deposition (HPCVD). The deposition rate is high, ～6.7 nm/s. The X-ray diffraction (XRD) indicates that it is highly (101) and c-axis oriented. The scanning electron microscope (SEM) images demonstrate that the film grown is in “island-mode”. The uniform superconducting phase in the film is shown by the M-T measurement.     

利用电泳法在金属基底上制备MgB2超导厚膜

利用电泳技术在高熔点金属基底Ta，Mo和W上制备MgB₂超导厚膜.厚膜中的MgB2晶粒结合紧密，粒度小于1μm，呈随机取向生长.电阻测量表明沉积在Ta，Mo，W上的MgB₂厚膜的超导起始转变温度分别为36.5K，34.8K，33.4K，对应的转变宽度为0.3K，1.5K和2.0K.三种基底上制备的MgB₂厚膜的临界电流密度在不同温度下随外磁场的变化情况 基本相同，MgB₂/Mo厚膜的临界电流密 关键词： 2超导厚膜')" href="#">MgB₂超导厚膜 电泳 金属基底     

High-density MgB2 superconducting bulk samples prepared at ambient pressure

High-density MgB₂ (HD-MgB₂) superconducting samples (D ⩾ 2.2 g/cm³), using different sources of magnesium powder as raw material, were synthesized in ambient pressure in a rich Mg environment. The magnesium powders used in the fabrication process include nanometer-sized magnesium particles, powders from Alfa Aesar, ordinary off-the-shelf powder, and magnesium chip. The fabrication procedure involved a double-sintering process in a rich-Mg environment. A transition temperature T _c of 39 K was observed. Samples with the equally high density and matching superconducting properties were obtained as well by a triple sintering process of the MgB₂ powder directly from Alfa Aesar.      

A Study on the Components of MgB2 Thick Film Preparedvia HPCVD

Superconducting MgB₂ thick film has been prepared via hybrid physical-chemical vapor deposition method on Al₂O₃ (0001) substrate by using B₂H₆ and magnesium ingot as raw materials reacted from 730 to 830°C for 40 min under 20 to 30 kPa. Its thickness is about 40 μm. The MgB₂ thick film shows T _c (onset) = 39.0 K and T _c (0) = 37.2 K. X-ray diffraction pattern shows that the film grown along (101) direction has small amount of impurities of Mg and MgO. Scanning electron microscopy and energy dispersive X-ray spectroscopy indicated that these impurities existed indeed and were Mg rich. The MgO film was formed on the surface of the MgB₂ thick film to further protect the sample from oxidation. We presented a new mechanism for the formation of the thick film. Translated from Chinese Journal of Low Temperature Physics, 2005, 27(1) (in Chinese)     

MgB2 coated conductors directly grown on flexible metallic Hastelloy tapes by hybrid physical–chemical vapor deposition

MgB₂ coated conductors (CCs), which can avoid the low packing density problem of powder-in-tube (PIT) processed wires, can be a realistic solution for practical engineering applications. Here we report on the superior superconducting properties of MgB₂ CCs grown directly on the flexible metallic Hastelloy tapes without any buffer layer at various deposition temperatures from 520 to 600 °C by using hybrid physical–chemical vapor deposition (HPCVD) technique. The superconducting transition temperatures (T_c) are in the range of 38.5–39.4 K, comparable to bulk samples and high quality thin films. Clear (101) and (002) reflection peaks of MgB₂ are observed in the X-ray diffraction patterns without any indication of chemical reaction between MgB₂ and Hastelloy tapes. From scanning electron microscopy, it was found that connection between MgB₂ grains and voids strongly depend on the growth temperature. A systematic increase in the flux pinning force density and thereby the critical current density with decreasing growth temperature was observed for the MgB₂ CCs. The critical current density (J_c) of J_c(5 K, 0 T) ～10⁷ A/cm² and J_c(5 K, 2.5 T) ～10⁵ A/cm² has been obtained for the sample fabricated at a low growth temperature of 520 °C. The enhanced J_c (H) behavior can be understood on the basis of the variation in the microstructure of MgB₂ CCs with growth temperature.     

Effect of substitution of Ce on superconducting properties of Bi1.7Pb0.3Sr2Ca2−x Ce x Cu3O10+δ system

We have investigated the superconducting properties of the Bi_1.7 Pb_0.3Sr₂Ca_2−xCe _x Cu₃O_10+δ system with x=0.00, 0.02, 0.04, 0.08 and 0.1 by X-ray diffraction and magnetic susceptibility. The substitution of Ce for Ca has been found to drastically change the superconducting properties of the system. X-ray diffraction studies on these compounds indicate decrease in the c-parameter with increased substitution of Ce at Ca site and volume fraction of high T _c (2 : 2 : 2 : 3) phase decreases and low T _c phase increases. The magnetic susceptibility of this compound shows that the diamagnetic on set superconducting transition temperature (onset) varies from 109 K to 51 K for x=0.00, 0.02, 0.04, 0.08 and 0.1. These results suggest the possible existence of Ce in a tetravalent state rather than a trivalent state in this system; that is, Ca²⁺ → Ce⁴⁺ replacement changes the hole carrier concentration. Hole filling is the cause of lowering T _c of the system.     

The effect of Cu addition on the sintering process and superconductive properties of?μm-SiC-doped MgB2 bulks

Based on the phase identification and microstructural observation, it is found that the Cu addition in the μm-SiC-doped samples could depress the reaction between Mg and SiC and thus decrease the amount of both C substitution for B and the Mg₂Si nanoparticles. As a result, compared to the only μm-SiC-doped MgB₂ sample, the T _c of the Cu and μm-SiC multi-doped MgB₂ sample is improved and the J _c in high fields is deteriorated.     

Anisotropic magnetoresistance of partially relaxed SrRuO3 films

The SrRuO₃ films (50 nm thick) grown by laser evaporation on (001)(LaAlO₃)_0.3 + (Sr₂AlTaO₆)_0.7 substrates were under partially relaxed biaxial compressive mechanical stresses. The films consisted of crystallites with lateral dimensions of 40–100 nm and a relative azimuthal misorientation of about 0.9°. Ferromagnetic ordering of spins in the SrRuO₃ films was manifested by a change in the slope of the temperature dependence of their electrical resistivity ρ at T ≈ 155 K. For a magnetic field H parallel to the measuring current, the maximum values (∼7.5%) of the magnetoresistance MR = [ρ(μ₀ H = 5 T) − ρ(μ₀ H = 0)]/ρ(μ₀ H = 0) were observed at temperatures of about 100 K. At T = 95 K (μ₀ H = 5 T), the anisotropic magnetoresistance of the films was 8% and increased by a factor of approximately 1.5 with decreasing temperature to 4.2 K.     

高性能MgB2长线材制备及性能表征

采用原位粉末装管工艺，分别以Mg粉(99.5%)，无定形B粉(99.9%)为原料，以纳米SiC(10—30nm)作为掺杂材料制备铁基MgB₂线.首先将已混合的原料在丙酮介质中球磨，真空干燥后，将粉末填入铁管内，然后通过孔型轧制、旋锻和拉拔等冷加工工艺得到11m长外径Ф1.75mm铁基MgB₂超导线.用扫描电镜，电子能谱，X射线衍射仪和超导量子干涉仪测试发现，样品微观结构整齐，晶粒大小均匀，内部仅含微量MgO，T_C(onset)=35.1K，ΔT_C＝5.3K.纳米SiC掺杂后，其中C造成MgB₂晶格畸变，形成有效磁通钉扎中心，C元素在MgB₂中分布均匀.标准四引线测试结果表明，11m线均分10段后，各点的J_c(4.2K,10T)均超过1.0×10⁴A/cm^{2，最高值达到1.2×104A/cm2.在10—18T范围各点临界电流值分布均匀，变化率小于10%.}     

Pulsed laser deposition conditions and superconductivity of FeSe thin films

We report the effects of growth conditions on the superconducting properties of FeSe films epitaxially grown on LaAlO₃ substrates by pulsed laser deposition (PLD). Customary materials characterization techniques [X-ray diffraction (XRD), in-situ X-ray photoelectron spectroscopy (XPS), in-situ ultra-violet photoelectron spectroscopy (UPS), and scanning electron microscopy (SEM)] revealed the films had a c-axis oriented tetragonal structure with lattice constants dependent on the growth temperature (varied from 100 to 600°C). The standard four-point probe method was used to measure the resistivity and superconducting transitions. Films grown at 400–550°C showed a clear superconducting onset but no zero resistance down to 2 K. The highest superconducting onset temperature (T_c^onsetT_{\mathrm{c}}^{\mathrm{onset}}) of 8 K was observed in films grown at 500°C and the onset temperature was clearly correlated to the ratio of the lattice constants (c/a). As the thickness of the FeSe films increased from 27 nm to 480 nm, T_c^onsetT_{\mathrm{c}}^{\mathrm{onset}} also increased as the strain in the system was relaxed.     

On the preparation and the characterization of superconducting thin films of YBa2Cu3O7−x

The results of our initial efforts to deposit thin films of YBa₂Cu₃O_7−x system on sapphire substrate are described. The deposited films are shiny black in appearance and are of quite uniform chemical composition. The annealed films exhibit zero resistance superconducting transition temperatureT _c(R=0) ranging between 23 K and 30 K.     

Electronic states of boron in superconducting MgB2 studied by11B NMR

Nuclear magnetic resonance (NMR) spectra and nuclear spin-lattice relaxation rateT ₁⁻¹ of¹¹B have been measured in superconducting polycrystalline MgB₂ with 7_c^ons = 39.5 K. It is shown that (T ₁T⁻¹ and the Knight shiftK _s are independent of temperature and nearly isotropic aboveT _c. Both of these quantities are decreased gradually in going to the superconducting state. According to NMR data the density of states near the Fermi level is flat at the scale of about 500 K. Some conclusions on the orbital content of the density of states at the Fermi level were drawn and compared with the results of the band structure calculations.     

多层膜外退火方法制备MgB2超导薄膜

报道了利用电子束蒸发的Mg/B多层膜作为前驱体，然后退火制备MgB₂薄膜的工作. 实验中发现，采用翻转膜面的退火处理方式可以有效地避免降温过程中Mg蒸气在薄膜表面形成的颗粒凝结，由此稳定地实现了面积为10 mm×10 mm，均匀、平整的超导薄膜的制备，T_c达35 K，转变宽度为0.8 K，在5 μm×5 μm的区域内薄膜的平均粗糙度小于10 nm. 为了便于后续器件制作过程中的微加工工艺，研究了膜厚小于1000 ?时薄膜的成相规律，发现当样品厚度减薄后，T_c会有明显降低. 通过调整前驱薄膜中的不同分层厚度，仍可实现转变温度达30 K以上、厚度约600 ?的MgB₂薄膜，在20 K时的临界电流密度为2.4×10⁶ A/cm².     

Sputtered magnesium diboride thin films: Growth conditions and surface morphology

Magnesium diboride (MgB₂) thin films were deposited on C-plane sapphire substrates by sputtering pure B and Mg targets at different substrate temperatures, and were followed by in situ annealing. A systematic study about the effects of the various growth and annealing parameters on the physical properties of MgB₂ thin films showed that the substrate temperature is the most critical factor that determines the superconducting transition temperature (T_c), while annealing plays a minor role. There was no superconducting transition in the thin films grown at room temperature without post-annealing. The highest T_c of the samples grown at room temperature after the optimized annealing was 22 K. As the temperature of the substrate (T_s) increased, T_c rose. However, the maximum T_s was limited due to the low magnesium sticking coefficient and thus the T_c value was limited as well. The highest T_c, 29 K, was obtained for the sample deposited at 180 °C, annealed at 620 °C, and was subsequently annealed a second time at 800 °C. Three-dimensional (3D) AFM images clearly demonstrated that the thin films with no transition, or very low T_c, did not have the well-developed MgB₂ grains while the films with higher T_c displayed the well-developed grains and smooth surface. Although the T_c of sputtered MgB₂ films in the current work is lower than that for the bulk and ex situ annealed thin films, this work presents an important step towards the fabrication of MgB₂ heterostructures using rather simple physical vapor deposition method such as sputtering.     

Orthorhombic structure: a necessity in superconducting 1-2-3 compounds

X-ray and resistivity measurements on YBa₂Cu₃O_7−δ (1-2-3) samples show that for the same but low oxygen concentration,δ⋍0·55, no superconducting transition down to 4·2 K is observed for the tetragonal phase samples while the orthorhombic phase shows aT _c ∼ 31 K. The effect of oxygen concentration onT _c is isolated.T _c=91±1 K has, however, been observed continuously for the normal oxygen annealed samples,δ⋍0·07. The experimental results suggest strongly the necessity of the 1-2-3 compound to be in the orthorhombic phase for the superconducting mechanism to be operative.     

An “EPR” study of YBa2Cu3O7 and related high-temperature superconductors

Besides ag ≈ 2 signal which disappears on cooling to the superconductingT _c , YBa₂Cu₃O₇ and related oxides show a near-zero-field signal in the superconducting state with certain unusual features attributable to a “superconducting glassy state”. Contribution No. 443 from Solid State and Structural Chemistry Unit.     

Non-resonant microwave absorption studies of superconducting MgB2 and MgB2 + MgO

Non-resonant microwave absorption (NRMA) studies of superconducting MgB₂ and a sample containing ∼10% by weight of MgO in MgB₂ are reported. The NRMA results indicate near absence of intergranular weak links in the pure MgB₂ sample. A linear temperature dependence of the lower critical field H _c1 is observed indicating a non-s wave superconductivity. However, the phase reversal of the NRMA signal which could suggest d wave symmetry is also not observed. In the MgB₂ + MgO sample, much larger low field dependent absorption is observed indicating the presence of intergranular weak links. The hysteretic behavior of NRMA is compared and contrasted in the two samples. In the pure MgB₂ sample, a large hysteresis is observed between the forward and the reverse scans of the magnetic field indicating strong pinning of flux lines. This hysteresis saturates a few degrees below T _c while in the MgB₂ + MgO sample, a much slower increase of hysteresis with decreasing temperature is observed, a signature of weaker pinning.