熔盐辅助煅烧法制备纳米MgO

以无水硫酸镁、氨水和月桂酸钠作为原材料,采用醇水体系一步法制备了表面修饰纳米 Mg(OH)₂,经熔盐LiNO₃辅助煅烧制备纳米MgO。用XRD和FT-IR表征前驱物Mg(OH)₂的结构及形貌,通过TG-DTA确定煅烧温度,用XRD和TEM对纳米MgO的结构和形貌进行表征。讨论了氨水浓度、氨水用量、煅烧温度、煅烧时间和熔盐添加量对纳米MgO颗粒尺寸和硬团聚程度的影响。初步认为纳米MgO是通过成核、长大过程形成的。通过调控煅烧时间、煅烧温度、熔盐比例,可以将MgO平均粒径有效控制在20～100nm范围。     

硼镁石与碳酸钙混合煅烧-还原提镁研究

基于硼镁石与碳酸钙混合料的煅烧实验和真空铝热还原实验,研究了碳酸钙量、成型压力、煅烧条件对熟料物相、原料烧损率、镁还原率的影响.结果表明,添加碳酸钙,在煅烧过程中Ca O可置换出Mg3B2O6,Mg2B2O5中的Mg O,并且在还原过程中Ca12Al14O33的形成有利于Mg O的还原.煅烧温度过高会降低Mg O活性,不利于后续铝热还原.增大成型压力,有利于Ca3B2O6的形成.但成型压力过大,在相同煅烧条件下,矿石的烧损率较低,镁还原率较低.碳酸钙与硼镁石以mCa/ms=1.9配比混合,在90 MPa压力制团,在1100℃下煅烧120 min后,铝热还原的镁还原率可达85%以上,实现硼、镁有效分离.     

用乙二醇为介质制备纳米氧化镁

用乙二醇为溶剂,Mg(NO3)2·6H2O为前驱物盐,NaOH和Na2CO3水溶液为沉淀剂,制备纳米MgO粉体,对样品进行了XRD、TEM、SEM表征.结果发现,煅烧前的沉淀物分别为纳米Mg(OH)2和Mg5(CO3)4(OH)2·4H2O,此沉淀物在430℃和530℃煅烧1.5 h,均得到晶粒较细、比表面积较大的纳米MgO粉体,其中最小晶粒尺寸和最大比表面积值分别为5.2 nm和259.8 m2·g-1.由Mg(OH)2分解得到的是重质MgO,由Mg5(CO3)4(OH)2·4H2O分解得到的是轻质MgO,且制得的MgO均保持了与相应沉淀物相似的形貌.     

以电解法氢氧化镁为原料制备纳米氧化镁

采用隔膜电解法以盐湖水氯镁石为原料制备前驱体Mg(OH)₂,煅烧后制备纳米氧化镁,实现盐湖废弃资源的高值化利用.对Mg(OH)₂煅烧过程进行热解动力学解析,结合热解机理和速率,考察煅烧条件对MgO性能的影响.结果表明：煅烧温度升高,MgO的比表面积降低,活性先升高后降低,晶粒变大;煅烧时间延长,MgO的比表面积和活性降低,晶粒尺寸增大,结构变得致密;升温速率增大,MgO比表面积与活性均先增大后平缓,晶粒尺寸基本不变;MgO比表面积最大为29.3 m²/g, CAA最小为66 s,晶粒尺寸最小为27.8 nm.     

Mg/Al和Zn/Al水滑石对富营养化水体中磷的去除研究

采用共沉淀法制备了Zn/Al和Mg/Al两种水滑石.研究了煅烧温度、金属摩尔比、磷初始浓度等对水滑石去除磷的影响以及水滑石的安全性能,用XRD、FTIR和Zeta电位对水滑石进行表征,并对除磷过程进行动力学拟合.研究结果表明,Mg/Al水滑石对磷的去除效果好于Zn/Al水滑石,煅烧有利于水滑石的吸附,水滑石对磷的吸附过程存在化学吸附.     

高纯度新型超导体MgB2的制备工艺研究

用固相反应法制备了T=39K的新型超导体MgB2,用X射线衍射研究了单相MgB2的实验室制备过程,探讨了锻烧温度、煅烧时间以及煅烧环境对产物纯度的影响。为进行高纯度MgB2化合物的工业化生产提供了原始资料。     

水热前驱体法低温合成Pb(Mg1/2W1/2)O3-PbTiO3

目的制备纯钙钛矿相的Pb(Mg1/2W1/2)O3-PbTiO3(PMW-PT)陶瓷。方法以Mg(Ac)2·4H2O,Pb(Ac)2.4H2O,Na2WO4·3H2O和Ti(OC4H9)4为原料,NaOH调节反应体系的pH值9～13,在200℃下12 h水热合成PMW-PT前驱体,通过煅烧该前驱体制备纯钙钛矿相的PMW-PT粉体。通过XRD分析研究水热处理温度、反应时间、溶液pH值以及煅烧温度对PMW-PT相和中间产物Pb2TiWO7相生成过程的影响。结果水热处理的粉体转化为钙钛矿相PMW-PT最佳煅烧温度为800℃,压片后1 000℃烧结2 h制备的PMW-PT陶瓷,介电常数为12 067(1 kHz)。结论与固相法和半化学法相比,这种方法制备的钙钛矿PMW-PT粉体在较低的温度下生成,而且陶瓷的介电常数较高。     

共沉淀法制备Mg-PSZ粉末的工艺优化

采用氯离子检验、激光粒度分析、XRD等手段对共沉淀法制备Mg—PSZ粉末工艺中洗涤条件、煅烧温度及保温时间等工艺参数进行了实验比较。试验结果表明：采用稀氨水洗涤，洗涤次数越多，制得粉末的粒度越细小：煅烧可以基本除去残留的氯离子；球磨工艺可以明显去除前工序引起的团聚。获得最佳粒度的工艺参数是：煅烧温度800℃，保温时间2h。     

硼酸镁晶须多孔陶瓷的原位固相合成及其性能

采用热分析仪、X线衍射仪(XRD)、扫描电子显微镜(SEM)及力学实验方法,研究碱式碳酸镁和硼酸反应体系的相变过程,研究Mg与B摩尔比和烧成温度对原位固相合成硼酸镁(Mg2B2O5)多孔陶瓷的组织结构、形貌和性能的影响,并探讨Mg2B2O5晶须的生长机制。结果表明:采用碱式碳酸镁和硼酸为原料可以制备出Mg2B2O5晶须多孔陶瓷;在Mg与B摩尔比为1∶1.5和加热温度为900℃条件下,合成多孔陶瓷中Mg2B2O5晶须的直径和长度分别为0.2~0.3μm和4.0~8.0μm;多孔陶瓷的抗压强度可达4.72 MPa。Mg2B2O5晶须生长符合固-液-固生长机制。     

非均相油脂酯交换法制备生物柴油工艺研究

以沉淀法制备了以水滑石为前驱体的Mg—Al复合氧化物催化剂。该系列催化剂活性受制备条件,如加料方式、煅烧温度、Mg/Al比等因素影响。反应工艺条件也是影响生物柴油收率的重要因素。该工艺操作简单,催化剂可回收再生,整个过程无污染,是个环境友好的过程。     

MgB2超导体的相图及其对薄膜制备的指导作用

MgB2适合于制备约瑟夫森结,在超导电子学领域有很好的应用前景。制备高质量的MgB2薄膜至关重要,应用Mg-B/Mg-B-O体系的相图指导MgB2薄膜生长意义重大。总结MgB2相体系及相关系,详细对比分析Mg-B/Mg-B-O体系的热力学相图,总结分析富氧区杂项MgO的生成机理及其对MgB2薄膜质量和性能的影响,研究分析有氧体系下Mg-B/Mg-B-O热力学相图对MgB2薄膜材料制备生长的指导意义,探讨HPCVD环境下采用原位生长技术制备MgB2超导薄膜时热力学相图的指导作用及相关制备工艺。     

MgB2制备过程中退火效应和热稳定性的实验研究

报道了关于 MgB₂ 超导体制备过程中的退火效应和热稳定性的实验研究。把硼片在不同的温度 Mg 气氛中退火不同时间得到 MgB₂,制备样品的测量结果显示制备 MgB₂ 的合适温度范围是 700～1000℃,并且较高的制备温度下只需要相对短的退火时间内就能得到较高转变温度的样品。热稳定性实验的结果显示在没有 Mg 的气氛中 MgB₂ 在 700℃ 下是稳定的,从 800℃ 开始分解,直到完全失去超导电性。实验还观测到利用 MgB₂ 混合物薄膜前驱代替硼片制备 MgB₂ 时,在 600℃ 退火时样品就显示超导电性。     

多晶MgB2相形成中纳米尺寸硼粉的作用

原料硼粉在MgB2相形成中的作用已经利用原位高温电阻率(HT-ρT)的测量技术进行了研究.MgB2相形成中的起始转变温度Tonset和相转变完成温度TPF在完成了的热处理过程中已直接确定了.用纳米硼粉和镁粉制备MgB2样品(简称为NanoB-MgB2)时的Tonset和TPF这2个温度值分别是440和 490 ℃,类似于用微米硼粉和纳米镁粉制备MgB2样品(简称为MicroB-MgB2)的情况.这表明MgB2相形成的温度并不特别依赖于硼粉的尺寸.另外,烧结温度的上极限TN是750 ℃,在此温度下NanoB-MgB2样品的超导电性将丧失.此温度远低于用微米硼粉和毫米尺寸的镁粉制备的MgB2样品(简称为DM-MgB2)的TN= 980 ℃.把直接在650 ℃＜T N,烧结的样品与先在750 ℃下烧结,之后又再次重磨和处理后,并于富镁的环境中在650 ℃下再烧结处理的样品相比较,观察到了MgB2的不可逆的晶体结构转变.     

Loss of superconductivity with the addition of Al to MgB2 and a structural transition in Mg1-x AlxB2

The basic magnetic and electronic properties of most binary compounds have been well known for decades. The recent discovery of superconductivity at 39 K in the simple binary ceramic compound magnesium diboride, MgB2, was therefore surprising. Indeed, this material has been known and structurally characterized since the mid 1950s (ref. 2), and is readily available from chemical suppliers (it is commonly used as a starting material for chemical metathesis reactions). Here we show that the addition of electrons to MgB2, through partial substitution of Al for Mg, results in the loss of superconductivity. Associated with the Al substitution is a subtle but distinct structural transition, reflected in the partial collapse of the spacing between boron layers near an Al content of 10 per cent. This indicates that superconducting MgB2 is poised very near a structural instability at slightly higher electron concentrations.     

Superconducting Properties and Microstructure in MgB2 Bulks, Wires and Tapes

We prepared a series of MgB2 bulk samples under different temperatures, holding time and increasing rates in temperature by the solid state reaction. The thermodynamic behavior and phase formation in the Mg-B system were studied by using DTA, XRD and SEM. The results indicate that the formation of the MgB2 phase is very fast and the high increasing rate in temperature is necessary to obtain high quality MgB2. In addition, the effects of the Zr-doping in Mg1-xZrxB2 bulk samples fabricated by the solid state reaction at ambient pressure on phase compositions, microstructure and flux pinning behavior were investigated by using XRD, SQUID magnetometer, SEM and TEM. Critical current density Jc can be significantly enhanced by the Zr-doping and the best data are achieved in Mg0.9Zr0.1B2. For this sample, Jc values are remarkably improved to 1. 83 × 106 A/cm2 in self-field and 5. 51 × 105 A/cm2in 1T at 20K. Also, high quality MgB2/Ta/Cu wires and tapes with and without Ti-doping, MgB2/Fe wires and 18 filamen     

High critical currents in iron-clad superconducting MgB2 wires

Technically useful bulk superconductors must have high transport critical current densities, Jc, at operating temperatures. They also require a normal metal cladding to provide parallel electrical conduction, thermal stabilization, and mechanical protection of the generally brittle superconductor cores. The recent discovery of superconductivity at 39 K in magnesium diboride (MgB2) presents a new possibility for significant bulk applications, but many critical issues relevant for practical wires remain unresolved. In particular, MgB2 is mechanically hard and brittle and therefore not amenable to drawing into the desired fine-wire geometry. Even the synthesis of moderately dense, bulk MgB2 attaining 39 K superconductivity is a challenge because of the volatility and reactivity of magnesium. Here we report the successful fabrication of dense, metal-clad superconducting MgB2 wires, and demonstrate a transport Jc in excess of 85,000 A cm-2 at 4.2 K. Our iron-clad fabrication technique takes place at ambient pressure, yet produces dense MgB2 with little loss of stoichiometry. While searching for a suitable cladding material, we found that other materials dramatically reduced the critical current, showing that although MgB2 itself does not show the 'weak-link' effect characteristic of the high-Tc superconductors, contamination does result in weak-link-like behaviour.     

新型超导体材料MgB_2的电子结构随压强的变化关系

根据密度泛函理论运用全势能线性muffin tin轨道 (FP LMTO :full potentiallinear muffin tin orbital)方法计算了不同压强下MgB2 晶格常数发生变化时的电子结构的变化情况 ,得出态密度的倒数与临界温度的自然对数成线性关系 ,符合BCS理论 ,从而进一步证实了MgB2 的超导机制为电—声子耦合BCS机制     

紧束缚近似解释MgB_2超导电性

作者在BCS理论对于超导体电声耦合组成库珀对解释超导电性的基础上,从MgB2 能带结构出发,通过紧束缚近似理论对其的详细计算和系统分析,比较合理的解释了MgB2 的超导电性。     

掺杂二硼化镁体系超导电性与平均价电子数的关系

用平均价电子数作为掺杂二硼化镁超导电性的一个判断标准，对二硼化镁超导体及掺杂二硼化镁超导体系平均电子数进行研究．结果表明，二硼化镁体系超导材料的平均价电子数值在Tc-Zv图中集中分布在2.61附近.     

The origin of multiple superconducting gaps in MgB2

Magnesium diboride, MgB2, has the highest transition temperature (T(c) = 39 K) of the known metallic superconductors. Whether the anomalously high T(c) can be described within the conventional BCS (Bardeen-Cooper-Schrieffer) framework has been debated. The key to understanding superconductivity lies with the 'superconducting energy gap' associated with the formation of the superconducting pairs. Recently, the existence of two kinds of superconducting gaps in MgB2 has been suggested by several experiments; this is in contrast to both conventional and high-T(c) superconductors. A clear demonstration of two gaps has not yet been made because the previous experiments lacked the ability to resolve the momentum of the superconducting electrons. Here we report direct experimental evidence for the two-band superconductivity in MgB2, by separately observing the superconducting gaps of the sigma and pi bands (as well as a surface band). The gaps have distinctly different sizes, which unambiguously establishes MgB2 as a two-gap superconductor.