混合物理化学气相沉积法制备Al2O3衬底MgB2薄膜性质的研究

我们用混合物理化学气相沉积(Hybrid Physical-Chemical Vapor Deposition简称为HPCVD)法在Al2O3(00l)衬底上原位制备了MgB2超导薄膜样品.样品厚度约为1μm左右,最高的超导起始转变温度Tc(onset)＝40.3K,转变宽度ΔT为0.3K.ρ50K=2.3μΩcm,剩余电阻比率RRR=R300K/R50K=10.样品的X射线衍射分析表明,MgB2薄膜具有较好的c轴取向,晶粒大小约200nm.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=7.6×106A/cm2,不同磁场下测得R～T曲线可以外推得到Hc2(0K)约10T.这些结果表明HPCVD技术在MgB2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.     

化学气相沉积制备MgB2超导薄膜

本文报道了利用化学气相沉积技术制备MgB2超导薄膜.首先在MgO(111)基片上化学气相沉积一层B膜,然后在Mg蒸气环境下对B膜进行后退火处理.退火后得到的MgB2薄膜在MgO(111)基片上呈随即取向生长,Mg、B原子比接近于1∶2.4;薄膜表面光滑致密,晶粒粒度约为0.5μm.电阻测量和直流磁测量表明薄膜超导转变温度为38K,转变宽度仅为0.1K.毕恩公式计算结果显示MgB2薄膜的临界电流密度在0T、10K时高达2×107A/cm2.     

电子束快退火法制备MgB_2薄膜及性质研究

利用电子束快退火法制备了MgB2超导薄膜.该方法利用高能电子束,在中真空条件下照射Mg-B多层前驱膜,照射时间维持在1s以下.在电子束的作用下,前驱膜中的Mg和B迅速反应,形成MgB2相.整个退火过程没有Mg蒸气与氩气保护,极短的退火时间有效地限制了前驱膜中Mg的流失和Mg与其它物质的反应.与传统制备工艺相比,该方法避免了混合物理化学气相沉积法中乙硼烷的使用;省去异位退火法中提供高Mg蒸气压的限制,避免在有Mg块存在情况下退火后样品表面存在Mg污染的问题.利用该方法在SiC(001)衬底上生长了100nm厚的MgB2薄膜,其超导转变温度Tc～35K,均方根粗糙度为3.6nm,临界电流密度Jc(5K,0T)=3.8×106 A/cm2.该方法对MgB2薄膜的大规模工业生产提供了一个新思路.     

前驱B膜沉积时间对MgB_2薄膜超导特性的影响

利用化学气相沉积法(CVD)在多晶Al2O3衬底上制备出了系列MgB2超导薄膜,研究了前驱硼膜沉积时间对MgB2薄膜超导特性的影响,通过XRD、SEM和R-T曲线对超导MgB2薄膜进行了表征。延长前驱硼膜的沉积时间,得到的硼膜结晶度越高,结构更致密。经退火后制备的MgB2薄膜表面富余的Mg可以改善晶粒间的连接,提升T c值。该实验沉积10min前驱硼膜得到的MgB2超导薄膜T c值为34K,且超导转变宽度比较窄。延长前驱硼膜沉积时间到15min后,薄膜的T c值降低,这是由于前驱硼膜较多,Mg和硼反应不充分所导致的。     

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Rs、OK时的穿透深度λ(O)和超导能隙△(O)．λ(O)和△(O)的值是通过先测量样品穿透深度λ(T)的变化量△λ(T)，然后由BCS理论模型拟合△λ（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MgB2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，△(0)：1．13kTc．     

Mg、B配比对MgB2材料的影响

我们通过固态反应法制备了MgxB2(x=0.2,0.6,0.8,1.0,1.2,1.4,1.8,2.2,2.6)系列超导样品.用四引线法测量了每一个样品在制备烧结过程中的高温R～T曲线.由这些曲线的升温阶段数据得知MgxB2系列样品的起始成相温度Tonset随着x值的增加而降低.由它们的X光衍射图可知,x≤1.0时,没有Mg和MgO的杂相峰;到x＞1.0后,随x值的增大,杂相Mg和MgO的衍射峰强度逐渐增强.它们的低温R～T曲线表明随x值的增加,正常态电阻减小,起始超导转变温度在39.3 K到39.9 K之间.综合Tc(onset)和△Tc,Mg1.4B2样品呈现出最好的超导状态.这些样品的单位质量M～T测量数据表明起起转变温度处于37.4～38.6 K之间,且Mg1.4B2样品呈现出最高的磁测Tc(onset)=38.60 K.在Mg含量x大于或低于1.4时,磁测Tc(onset)均小于此值.综合R～T和M～T这两种测量,为得到高Tc的MgB2超导块材,胚体MgB2的配比应取x=1.4为好.     

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.     

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×10mm,均匀、平整的超导薄膜的制备,Tc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 (A)时薄膜的成相规律,发现当样品厚度减薄后,Te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 (A)的MgB2薄膜,在20 K时的临界电流密度为2.4×106 A/cm2.     

MgB_2和Mg_(0.93)Li_(0.07)B_2的电阻率与霍尔效应研究

测量了MgB2 和Mg0 .93Li0 .0 7B2 的电阻率 ρ(T)与霍尔系数RH(T)的温度依赖关系 .电阻率的测量结果表明 ,MgB2 和Mg0 .93Li0 .0 7B2 的正常态电阻率与温度有平方的依赖关系 .MgB2 和Mg0 .93Li0 .0 7B2 的超导转变温度几乎相同 .霍尔系数的测量结果表明 ,MgB2 和Mg0 .93Li0 .0 7B2 的载流子类型为空穴型 ,二者的霍尔系数都随温度升高而减小 ,且Mg0 .93Li0 .0 7B2 的霍尔系数比MgB2 略有减小 ,这可能与Li掺杂引入空穴有关 .二者的霍尔角都与温度平方呈线性关系 .     

不同厚度的MgB_2超薄膜的制备和性质研究

本文报导了利用混合物理化学气相沉积法(Hybrid physical-chemical vapor deposition,HPCVD)在SiC(0001)衬底上制备干净的MgB2超薄膜.在背景气体压强、载气H2流量等条件一定的情况下,改变B2H6流量及沉积时间,制备不同厚度的MgB2超薄膜样品,并研究了超导转变温度Tc、剩余电阻率ρ(42K)、上临界场Hc2等与膜厚的关系.这系列超薄膜生长沿c轴外延,随膜厚度的变小Tc(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10nm厚的膜,Tc(0)~32.4K,ρ(42K)~124.92μΩ·cm,其表面连接性良好,平均粗糙度为2.72nm,上临界磁场Hc2(0K)~12T,零场4K时的临界电流密度Jc~107A/cm2,为迄今为止所观测到的10nm厚MgB2超薄膜的最高Jc值,这也证明了10nm厚的MgB2膜在超导纳米器件上具有很强的应用潜力.     

原位法MgB_2-B_4C复相超导体合成及相含量调控研究

以B4C和Mg为原料合成的MgB2-B4C复相超导体具有高的临界电流密度(Jc)和高的超导转变温度(Tc),是一种有潜力的实用MgB2超导材料,其成相机理对复相MgB2超导体的相含量调控和磁通钉扎研究具有重要意义。结合经典烧结理论,研究了B4C-Mg真空固相烧结制备MgB2-B4C复相超导体的超导相形成和晶粒生长过程,给出了B4C-Mg的金斯特林格扩散模型和MgB2晶粒生长过程。通过选择B4C原料粒径,MgB2-B4C复相超导体超导相体积相含量在18%-88%范围可控。相含量88%的MgB2-B4C复相超导体临界转变温度达33.5K,转变宽度1.5K。10 K环境6T外场下电流密度可以达到1×104A/cm2,表明MgB2-B4C复相超导体具有良好的磁通钉扎行为。     

Systematic effects of carbon doping on the superconducting properties of Mg(B1-xCx)(2)

The upper critical field, H(c2), of Mg(B1-xCx)(2) has been measured in order to probe the maximum magnetic field range for superconductivity that can be attained by C doping. Carbon doped MgB2 filaments were prepared, and for carbon levels below 4% the transition temperatures are depressed by about 1 K/% C and H(c2)(T=0) rises by about 5 T/% C. This means that 3.8% C substitution will depress T(c) from 39.2 to 36.2 K and raise H(c2)(T=0) from 16.0 to 32.5 T. These rises in H(c2) are accompanied by a rise in resistivity at 40 K from about 0.5 to about 10 microOmega cm.     

电子束蒸发在Si衬底上制备MgB2超导薄膜

利用电子束蒸发法在 Si(111)衬底上制备了 Mg B2 超导薄膜。首先在衬底上按照 1∶ 2的原子比交替蒸发 Mg和 B,所形成的夹层先驱膜在 15 0 Pa99.99% Ar气氛下进行原位热处理 6 30℃× 30 m in。实验发现超导薄膜在正常态下无半导体电阻特性 ,超导起始转变温度为 2 4 .7K,零电阻温度为 16 .5 K。     

Boron isotope effect in superconducting MgB2

We report the preparation method of and boron isotope effect for MgB2, a new binary intermetallic superconductor with a remarkably high superconducting transition temperature T(c)(10B) = 40.2 K. Measurements of both temperature dependent magnetization and specific heat reveal a 1.0 K shift in T(c) between Mg11B2 and Mg10B2. Whereas such a high transition temperature might imply exotic coupling mechanisms, the boron isotope effect in MgB2 is consistent with the material being a phonon-mediated BCS superconductor.     

直流磁控溅射一步法原位制备MgB2超导薄膜

用MgB2靶,控制直流磁控溅射工作在异常辉光放电或弧光放电状态,在SrTiO3衬底上原位一次性得到了MgB2超导薄膜,其起始转变温度为32K,零电阻温度为15K. 关键词： 高温超导体 超导薄膜 磁控溅射 二硼化镁     

Superconductivity in dense MgB2 wires

MgB2 becomes superconducting just below 40 K. Whereas porous polycrystalline samples of MgB2 can be synthesized from boron powders, in this Letter we demonstrate that dense wires of MgB2 can be prepared by exposing boron filaments to Mg vapor. The resulting wires have a diameter of 160 microm, are better than 80% dense, and manifest the full chi = -1/4pi shielding in the superconducting state. Temperature-dependent resistivity measurements indicate that MgB2 is a highly conducting metal in the normal state with rho(40 K) = 0.38 microOmega cm. By using this value, an electronic mean-free path, l approximately 600 A can be estimated, indicating that MgB2 wires are well within the clean limit. Tc, Hc2(T), and Jc data indicate that MgB2 manifests comparable or better superconducting properties in dense wire form than it manifests as a sintered pellet.     

Specific heat of single crystal MgB2: a two-band superconductor with two different anisotropies

Heat-capacity measurements of a 39 microg MgB2 single crystal in fields up to 14 T and below 3 K allow the determination of the low-temperature linear term of the specific heat, its field dependence, and its anisotropy. Our results are compatible with two-band superconductivity, the band carrying the smaller gap being isotropic, that carrying the larger gap having an anisotropy of approximately 5. Three different upper critical fields are thus needed to describe the superconducting state of MgB2.     

基于碳化硼复相MgB2超导体制备及特性

以廉价的B4C粉和Mg粉为原料,用真空固相反应法成功制备了复相MgB2-B4C超导材料,通过X-射线和扫描电子显微镜分析了样品的成相和织构,除MgB2、B4C和MgB2C2外样品中未明显检测到其它杂相,其中MgB2相含量高达87.7%.电阻-温度特性测量表明,所制备的样品零电阻温度Tc(0)=31.5 K,转变宽度(T...     

Metallurgical phases and their magnetism at the interface of nanoscale MgB2/Fe layered structures

We report on the characterization of metallurgical phases and their magnetism at the interfaces of nanoscale MgB(2)/Fe layered structures. MgB(2)/(57)Fe multilayers with varying layer thicknesses were prepared by vacuum deposition and investigated, before and after annealing by electrical resistance measurements, x-ray diffraction and (57)Fe conversion-electron M?ssbauer spectroscopy (CEMS) down to 5 K. Interfacial Fe-B phases, such as Fe(2)B, were identified by CEMS. A superparamagnetic-to-ferromagnetic transition is observed with increasing (57)Fe film thickness. Ultrahigh vacuum annealing at 500 °C of the multilayers leads to strong diffusion of Fe atoms into the boundary regions of the MgB(2) layers. MgB(2) in the as-grown multilayers is non-superconducting. Structural disorder and the effect of Fe interdiffusion contribute to the suppression of superconductivity in the MgB(2) films of all the as-grown multilayers and the thinner annealed multilayers. However, an annealed MgB(2)/(57)Fe/MgB(2) trilayer with thicker (500 ?) MgB(2) layers is observed to be superconducting with an onset temperature of 25 K. At 5 K, the annealed trilayer can be conceived as being strongly chemically modulated, consisting of two partially Fe-doped superconducting MgB(2) layers separated by an interdiffused weakly magnetic Fe-B interlayer, which is characterized by a low hyperfine magnetic field B(hf) of ～11 T. This chemically modulated layer structure of the trilayer after annealing was verified by Rutherford backscattering.     

化学气相沉积-后退火法制备MgB2超导薄膜

本文提出在高真空镀膜系统中通过化学气相沉积(CVD)的方法沉积高纯度的先驱B膜,再经过后退火工艺,Mg扩散进入先驱膜而反应生成了MgB2超导薄膜.经过多种实验方法检测,这种薄膜具有较为优异的超导性能,是一种和传统微电子工艺兼容、适宜于工业化大规模生产MgB2超导薄膜的方法.