混合物理化学气相沉积法(HPCVD)制备的MgB2超导厚膜样品的成分分析

本介绍了基于混合物理化学气相沉积法(HPCVD),以B2H6为硼源,在(000l)取向的Al2O3单晶衬底上,制备了MgB2超导体厚膜样品．该样品平均厚度约为40μm．其Tc(onset)=39K,Tc(0)=37．2K．X光衍射图显示该膜沿(101)方向生长,具有少量Mg和MgO杂相．SEM图像、X射线能量损失谱以及背散射电子衍射图证实了这两种杂相的存在,并显示该样品成分富镁．样品表面的镁与空气接触形成MgO膜,在一定程度上阻止了MgB2样品进一步被氧化．对于MgB2厚膜成膜过程及反应机理,我们提出了一种新的推断．     

A Study on the Components of MgB2 Thick Film Prepared via 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.     

MgB2超导晶须的研究

本文报道了用混合物理化学气相沉积法(hybrid physical-chemical vapor deposition,简称为HPCVD)在铜衬底上生长出了MgB2超导晶须.这些晶须几乎都是以垂直或接近垂直于衬底表面生长,互不接触.M～T测量给出了这些MgB2晶须的磁超导转变温度是39.0 K,但无法测得其具有超导转变温度值的R～T曲线.经过与铜衬底MgB2超导膜的相关数据比较和计算也确认了这些MgB2超导晶须的确实性.     

Preparation and characterization of MgB2 superconductor

The MgB₂ superconductor, synthesized using solid-state and liquid-phase sintering methods, have been characterized for various properties. The upper critical field, irreversibility line and critical current density have been determined using magnetization data. The current-voltage characteristics recorded under an applied magnetic field revealed the existence of vortex glass transition. The surface analysis using X-ray photoelectron spectroscopy shows that MgB₂ is sensitive to atmospheric degradation.     

MgB和MgB_2(~1A_1)的结构与解析势能函数

分别采用QCISD/6-311G和QCISD/6-311++G(df)方法,对MgB和MgB2分子的微观结构进行理论计算.在此计算基础上,运用多体展式理论方法,推导出MgB2分子的解析势能函数,其等值势能面图准确再现了MgB2分子的结构特征及势阱深度,并讨论了B+MgB和Mg+BB分子反应的势能面特征.这些结果可用于微观反应动力学的研究.     

Microwave absorption studies of MgB2 superconductor

Microwave absorption studies have been carried out on MgB₂ superconductor using a standard X-band EPR spectrometer. The modulated low-field microwave absorption signals recorded for polycrystalline (grain size ∼ 10 μm) samples suggested the absence of weak-link character. The field dependent direct microwave absorption has been found to obey a ✓H dependence with two different slopes, which indicated a transition from strongly pinned lattice to flux flow regime.     

MgB2 thick films with remarkable ductility on stainless steel substrate

We fabricated several superconducting MgB₂ thick films on stainless steel (SS) substrates by using hybrid physical-chemical vapor deposition (HPCVD) technique. The thickness was in the 10μm to 20μm range, and the onset critical transition temperature T _c (onset) and the width of the superconducting transition (ΔT) were about 37.8 and 1.2 K. They were dense and textured along (101) direction with high tenacity, despite the existence of a little amount of MgO and Mg. We bent the films at different degrees and studied the ductility and transport properties of these MgB₂ thick films under applied force. The results demonstrated that the superconducting properties of these thick films, prepared by HPCVD, stay almost unaffected even with the films bent to a large degree with a curvature of 0.5 mm. This indicated that the superconducting wires or tapes of MgB₂ with a core of SS had the advantages of avoiding rigidity and brittleness in industrial handling. The technique of HPCVD has, therefore, a high application potential. __________ Translated from Chinese Journal of Low Temperature Physics, 2005, 27(2) (in Chinese)     

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.     

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.      

Influence of shock-wave pressure up to 65 GPa on the crystal structure and superconducting properties of MgB2

The influence of shock-wave pressure treatment up to 65 GPa on the crystal structure and the superconducting transition temperature of a polycrystalline MgB₂ sample has been investigated. X-ray diffraction measurements have revealed that the shock-wave pressure does not result in any irreversible structural phase transitions in the MgB₂, except for microdistortions formed in the crystal structure of the shock-wave pressure-treated MgB₂ sample. This conclusion is in agreement with the results of superconducting transition temperature measurements of a MgB₂ sample performed before and after its shock-wave pressure treatment.     

Ultraviolet photovoltaic characteristic of MgB2 thin film

Fast photoelectric effects have been observed in MgB₂ thin film fabricated by chemical vapour deposition. The rise time was $\sim $10 ns and the full width at half-maximum was \sim185\,ns for the photovoltaic pulse when the film was irradiated by a 308\,nm laser pulse of 25\,ns in duration. X-ray diffraction and the scanning electron microscope revealed that the film was polycrystalline with preferred c-axis orientation. We propose that nonequilibrium electron--hole pairs are excited in the grains and grain boundary regions for MgB₂ film under ultraviolet laser and then the built-in electric field near the grain boundaries separates carriers, which lead to the appearance of an instant photovoltage.     

纳米镁粉对制备MgB2超导样品的作用

我们对用纳米镁粉(平均颗粒度≤40nm)在常压下制备MgB2超导样品(以下简称纳米MgB2超导样品)进行了研究.得到了一组与用普通颗粒镁粉分别在真空条件下和流动氩气下制备MgB2超导样品时得到的原位ρ-T曲线不同的曲线.实验结果表明纳米MgB2超导样品的成相温区是430℃到490℃之间,低于用普通颗粒镁粉分别在真空条件下和流动氩气下制备MgB2超导样品时的成相温度:640℃～700℃和530℃～630℃.所得到的纳米MgB2超导样品的密度是1.46g/cm3.它高于用其他各种镁粉原料在常压下制备通过一次烧结制得的MgB2超导样品.     

混合物理化学气相沉积法制备蓝宝石衬底外延MgB2薄膜性质的研究

我们用混合物理化学气相沉积(Hybridphysicalchemicalvapordeposition简称为HPCVD)法在αAl2O3(00l)衬底上原位制备了一批超导性能良好的外延MgB2超导薄膜样品.用10%浓度的乙硼烷(B2H6)氢气混合气作为原料,研究了不同条件对MgB2薄膜沉积速率的影响.在一定条件下制备了一批MgB2薄膜,厚度为200nm左右,样品的零电阻转变温度(Tc0)最高达到39K.X射线衍射分析的θ～2θ扫描表明,MgB2薄膜的晶粒都具有较好的C轴取向,对样品的(101)面Φ扫描结果显示MgB2薄膜晶格与衬底有很好的外延取向,取向关系为[1010]MgB2∥[1120]Al2O3.由毕恩模型计算求得在5K和零场条件下,样品的临界电流密度Jc=9.8×106A/cm2.这些结果表明HPCVD技术在MgB2外延薄膜原位制备方面有着很大的优势,从而有利于实现MgB2薄膜在电子器件方面的应用.     

由纳米管和纳米颗粒构成的TiO2膜的制备与机理研究

采用聚苯乙烯小球修饰Ti片表面,并进行阳极氧化,制备出一种由纳米颗粒和纳米管构成的TiO₂膜．通过数值模拟,分析了氧化表面附近的局部电场分布对TiO₂膜形貌的影响．结果表明,覆盖物增强了局部电场,从而加快了O^2-与Ti的反应速率,有利于TiO₂的生长;与此同时,[TiF₆]^6-的扩散受到阻碍,使得TiO₂的溶解速率减慢．可见,覆盖物打破了TiO₂纳米管形成的平衡条件,导致纳米颗粒的生成．此外,通过X射线衍射和Raman光谱的测试分析发现,所制备的TiO₂为锐钛矿结构.     

MgB2超导薄膜的微波测量

报道了利用蓝宝石介质谐振器技术测量MgB₂超导薄膜的微波表面电阻R_{s、0K时的穿透深度λ(0)和超导能隙Δ(0).λ(0)和Δ(0)的值是通过先测量样品穿透深度λ(T)的变化量Δλ(T)，然后由BCS理论模型拟合Δλ(T)的实验数据得到的.测试样 品是利用化学气相沉积技术在MgO(111)基片上制备的c轴织构的MgB2超导薄膜， 薄膜的超导转变温度和转变宽度分别为38K和01K.微波测试结果表明在10K，18GHz下M gB2薄膜的Rs约为100μΩ，可以和高质量的YBCO薄膜的Rs值相比拟；BCS理论拟合得到的MgB2超导薄膜的λ(0)=102nm，Δ(0)=113k Tc.}     

用SAXS和XRD方法研究TiO2纳米颗粒微观结构

用溶胶-凝胶方法制备了TiO₂纳米样品,并对该样品在300℃到800℃温度区域进行了退火处理.应用同步辐射X射线粉末衍射(XRD)方法研究了经不同热处理温度的TiO₂纳米颗粒的结构相变.应用同步辐射小角X射线散射(SAXS)方法研究了TiO₂纳米颗粒的表面分形与界面特性.得到纳米颗粒粒度与退火温度的变化规律,讨论了表面界面特征与相变的关系. 关键词： X射线小角散射 X射线衍射 2纳米颗粒')" href="#">TiO₂纳米颗粒     

MgB2 超薄膜的制备和性质研究

利用混合物理化学气相沉积法在6H-SiC(001)衬底上制备干净的MgB₂超导超薄膜.在本底气体压强、载气氢气流量等条件一定的情况下,改变B₂H₆流量及沉积时间,制备得到不同厚度的系列MgB₂超薄膜样品,并研究了超导转变温度T_c、剩余电阻率ρ_(42K)、上临界磁场H_c2等与膜厚的关系.该系列超薄膜沿c轴外延生长,随膜厚度的变小,T_c(0)降低,ρ_(42K)升高.膜在衬底上的生长遵循Volmer-Weber岛状生长模式.对于厚度为7.5 nm的MgB₂超薄膜,T_c(0) =32.8 K,ρ_(42K) =118 μΩcm,是迄今为止所观测到的厚度为7.5 nm的MgB₂超薄膜最高的T_c值;对于厚度为10 nm的MgB₂膜,T_c(0)=35.5 K,ρ_(42K)=17.7 μΩcm,上临界磁场μ₀H_c2估算为12 T左右,零磁场、4 K时的临界电流密度J_c=1.0×10⁷ A/cm²,是迄今为止10 nm厚MgB₂超薄膜的最高J_c值,且其表面连接性良好,均方根粗糙度为0.731 nm.这预示MgB₂超薄膜在超导纳米器件上具有广阔的应用前景. 关键词： 2超薄膜')" href="#">MgB₂超薄膜 薄膜生长 氢气流量 混合物理化学气相沉积     

氧氩比对SnO2/Ag/SnO2透明导电膜光电性能的影响

在室温及不同的氧氩比条件下,采用射频磁控溅射Ag层和直流磁控溅射SnO₂层,在载玻片衬底上制备出了SnO₂/Ag/SnO₂多层薄膜.用霍尔效应测试仪、四探针电阻测试仪和紫外-可见-近红外光谱仪等表征了薄膜的电学性质和光学性质.实验结果表明:当氧氩比为1:14时,所制得的薄膜的光电性质优良指数最大,为1.69×10^-2 Ω^-1;此时,薄膜的电阻率为9.8×10^-5 Ω·cm,方电阻为9.68 Ω/sq,在400~800 nm可见光区的平均光学透射率达85%;并且,在氧氩比为1:14时,利用射频磁控溅射Ag层和直流磁控溅射SnO₂层在PET柔性衬底上制备出了光电性质优良的柔性透明导电膜,其在可见光区的平均光学透过率达85%以上,电阻率为1.22×10^-4 Ωcm,方电阻为12.05 Ω/sq.     

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     

MgB2混合态热导率的反常增强

测量了MgB₂多晶样品的混合态热导率，磁场强度为0—7 T，温度范围为5—45 K .实验结果显示MgB₂热导率在低场下迅速上升，高场下趋于饱和，这与MgB₂的 二能隙电子结构有关.对实验结果的分析指出，低温强场下MgB₂多晶样品热导率的显著增强无法完全 用电子热导来解释，并对此进行了讨论. 关键词： 2')" href="#">MgB₂ 热导率 混合态