Na和Al双掺杂P型Bi0.5Sb1.5Te3热电材料的制备及性能研究

采用真空熔炼及热压烧结技术制备了Na和Al双掺杂P型Bi0.5Sb1.5Te3热电材料。利用X射线衍射(XRD)、扫描电子显微镜(SEM)对样品的物相结构和表面形貌进行了表征。XRD分析结果表明,Na0.04Bi0.5Sb1.46-x Al x Te3块体材料的XRD图谱与块体材料Bi0.5Sb1.5Te3的图谱完全对应,所有块体材料的衍射峰均与衍射卡JCPDS 49-1713对应,这表明Na和Al元素已经完全固溶到Bi0.5Sb1.5Te3晶体结构中,形成了单相固溶体合金。SEM形貌表明材料组织致密且有层状结构特征。Na和Al双掺杂提高了Bi0.5Sb1.5Te3在室温附近的Seebeck系数。在Na掺杂量为0.04时,同时Al掺杂量由x=0.04增加至0.12,电导率逐渐降低,在实验掺杂浓度范围内,Na和Al双掺杂会使P型Bi0.5Sb1.5Te3材料的电导率受到较大的损失。在300~500 K时,通过Na和Al部分替代Sb,Na0.04Bi0.5Sb1.42Al0.04Te3和Na0.04Bi0.5Sb1.38Al0.08Te3样品的热导率均有不同程度地减小,在300K时双掺杂样品Na0.04Bi0.5Sb1.42Al0.04Te3的最大ZT值达到1.45。     

Cu纳米颗粒的晶格畸变研究

采用阳极弧放电等离子体技术成功地制备了Cu纳米颗粒,利用X射线衍射(XRD)、透射电子显微镜(TEM)和相应选区电子衍射(SAED)、BET氮吸附等测试手段对样品的晶体结构、形貌、比表面积和粒度等特征进行了表征分析,并计算了其不同晶面的晶格参数.结果表明:Cu纳米颗粒为fcc晶态结构,晶格畸变表现为晶格收缩.     

合金Co-Zr-B纳米粉末的相组成及磁性能研究

将硼氢化钠(NaBH4)的水溶液加入到氯化钴(CoCl2·6H2O)和硫酸锆(Zr(SO4)2·4H2O)的混合水溶液中,利用BH-4把混合溶液中的CO2 和Zr4 同时还原出来,首次成功制备出非晶态Co-Zr-B三元纳米合金粉末.用电感耦合等离子体发射光谱(ICP)、X射线衍射(XRD)、选区电子衍射(SAED)、透射电子显微镜(TEM)、差示扫描量热法(DSC)以及振动样品磁强计(VSM)分析了样品的成分、结构和磁性能.发现所制备的不同成分的粉末颗粒呈球形,粒径在20～60nm之间.纳米粉末由非晶相基体和少量晶体相杂质组成,而非晶相基体又由Zr基非晶颗粒和含有Zr的Co基非晶颗粒构成.还原产物中的Co原子和Zr原子的分数之比与金属盐混合溶液中的Co2 与Zr4 离子的分数之比几乎相等.提高NaBH4溶液的加入速度,可增加产物中B元素的含量.样品的晶化温度在765.1～771.3K之间,样品的热稳定性随Zr含量的增加而增加,样品的磁性能也与样品中Co、Zr原子的含量之比有关.当原子数x(Co)/x(Zr)比值从1.94增加到5.14时,饱和磁化强度从4.76emu/g增加到8.87emu/g,矫顽力在1271.66A/m(15.98Oe)到2133.49A/m(26.81Oe)之间不规则变化.     

溶剂热法合成CoS纳米晶及其表征

以六水合硝酸钴(Co(NO3)2·6H2O)和硫脲为原料,采用混合溶剂热法制备硫化钴(COS)纳米晶.利用X射线衍射(XRD),扫描电镜(SEM)和透射电镜(TEM)对硫化钴纳米晶的组成、粒径及表面形貌进行表征.结果表明,在180℃恒温条件下所得粉末样品为六方相CoS纳米粉末,粉末粒径在40nim左右.粉末的产率随温度...     

纳米复合抑制剂对微波法制备WC-TiC-Co硬质合金组成和微观结构的影响

以纳米WC、TiC和Co粉为原料,用纳米V_8C_7-Cr_3C_2复合粉末作为晶粒抑制剂,研究了复合晶粒抑制剂对硬质合金的组成和微观结构的影响。结果表明:由微波原位合成的纳米V_8C_7-Cr_3C_2复合粉末显示出良好的分散性,主要由平均尺寸约30 nm的球形或类球形颗粒组成。WC基复合粉末经微波烧结后,主要由WC和TiC组成,并且WC衍射峰强度明显减弱。添加纳米复合晶粒抑制剂后,硬质相的分布较均匀,平均晶粒尺寸在500 nm左右。     

氧化镁稳定氧化锆纳米粉末的制备与物相分析

以草酸为络合剂,采用溶胶–凝胶法制备一系列氧化镁稳定氧化锆粉末Zr1 xMgxO2 x(0.04≤x≤0.10),利用X射线衍射(XRD)、场发射扫描电镜(FESEM)等分析技术对粉末进行表征。结果表明,掺杂氧化镁后,低温350~450℃煅烧产物晶型为四方相(t-ZrO2),随煅烧温度升高,t-ZrO2逐渐向m-ZrO2转变。在550℃下煅烧时,少部分四方相转变为单斜相(m-ZrO2),转变比例随掺杂量增加而降低。Mg2+取代Zr4+产生氧缺陷是ZrO2晶体结构稳定的主要因素。随煅烧温度从350℃升高到650℃,Zr0.92Mg0.08O1.92粉末中t-ZrO2晶粒尺寸从42 nm长大到100nm;随Mg掺杂量从0.04增加到0.10,t-ZrO2晶粒尺寸从110 nm减小到97.8 nm,而纳米尺寸晶粒有利于t-ZrO2稳定。     

Bi-2212超导体中氧原子位移调制的计算机模拟

根据Bi系超导体的结构特点提出了BiO层中O原子位移调制的结构模型.通过计算机模拟计算了Bi-2212相A型调制结构的选区电子衍射和会聚束电子衍射花样.计算结果表明,O原子的位移调制对电子衍射花样中调制衍射斑的影响甚大,不容忽视.而会聚束电子衍射对O原子的位移更敏感,利用这一特点,进一步调整BiO层中O原子的位移,使模拟计算的电子衍射花样和会聚束电子衍射花样与实验结果完全一致.     

等离子喷涂Ti涂层的微观组织及摩擦磨损性能研究

文章以Ti及TiH_(2)粉为原料,分别采用等离子喷涂技术制备了Ti涂层,分析了涂层的显微形貌及力学性能。研究表明,等离子喷涂制备Ti涂层厚度约100~200μm,可观察到明显的层片结构及较多微小孔隙。Ti粉所制备涂层XRD图谱的主衍射峰为TiO,而用TiH_(2)粉所制备涂层XRD图谱的主衍射峰为Ti。Ti粉所制备涂层摩擦系数及磨损量仅为0.179及5.8 mg, TiH_(2)粉末所制备涂层摩擦系数及磨损量分别为0.294及9.9 mg,均优于304不锈钢基体。     

复合溶剂热法合成Bi2S3纳米棒的研究

以铜试剂(二乙基二硫代氨基甲酸钠)为硫源、硝酸铋为铋源、丙三醇-水体系为溶剂,采用复合溶剂热法大规模合成了Bi2S3纳米棒.对所制备的样品用X射线粉末衍射(XRD)、透射电子显微镜(TEM)、场发射扫描电子显微镜(FESEM)等测试手段进行了表征.结果表明,所制备样品为纯相正交晶型,其形貌为分散性良好的单晶纳米棒,径向和轴向尺寸分别为30～50 nm和几微米.对Bi2S3纳米棒的形成机理进行了探讨,认为丙三醇-水复合溶剂及表面活性剂PVP对其形貌和尺寸均有重要影响. 复合溶剂热法;Bi2S3;纳米棒;丙三醇-水;PVP     

两种不同分散剂对ITO纳米粉末粒度和团聚的影响

利用溶胶凝胶法制取纳米铟锡氧化物(ITO)粉末，研究了两种不同的分散剂对粉末粒度、团聚的影响，并用差热分析(DTA)、X-射线衍射(XRD)、扫描电镜(SEM)分析了所制得粉末的形貌。结果表明：两种分散剂均有减少纳米粉末团聚程度的效果，二号分散剂效果优于一号分散剂，而添加一号分散剂所制备的ITO纳米粉末的晶粒度比添加二号分散剂的细小；二者都对纳米粉末的形貌影响不大。     

奥氏体不锈钢物相的精细结构表征

以热轧态316L不锈钢为研究对象,首先利用X射线衍射仪(XRD)对其主要物相进行标定,进而利用透射电镜(TEM)的选区电子衍射和高分辨像功能确认了χ相的存在。然后利用透射电子背散射衍射技术(t-EBSD)对所有物相的分布进行表征,与常规电子背散射衍射(EBSD)的结果进行比较,准确显示了χ相的分布特征。结果表明,组织中以奥氏体基体相和带状组织为主,带状组织中主要含有σ相,还有少量的铁素体相和奥氏体相,χ相不仅存在于带状组织中,还存在于奥氏体基体中,且χ相和σ相中都富含Fe、Cr、Mo元素。     

Microstructure of Equal-Channel Angular Pressed Cu and Cu-Zr Samples Studied by Different Methods

Polycrystalline samples of technical-purity Cu (99.95 wt pct) and Cu with 0.18 wt pct Zr have been processed at room temperature by equal-channel angular pressing (ECAP). The microstructure evolution and its fragmentation after ECAP were investigated by transmission electron microscopy (TEM), electron backscattered diffraction (EBSD), positron annihilation spectroscopy (PAS), and by X-ray diffraction (XRD) line-profile analysis. The first two techniques revealed an increase in the fraction of high-angle grain boundaries (HAGBs), with increasing strain reaching the value of 90 pct after eight ECAP passes. The increase was more pronounced for pure Cu samples. The following two kinds of defects were identified in ECAP specimens by PAS: (1) dislocations that represent the dominant kind of defects and (2) small vacancy clusters (so-called microvoids). A detailed XRD line-profile analysis was performed by the analysis of individual peaks and by total profile fitting. A slight increase in the dislocation density with the number of ECAP passes agreed with the PAS results. Variations in microstructural features obtained by TEM and EBSD can be related to the changes in the XRD line-broadening anisotropy and dislocation-correlation parameter.     

Modified-EISA synthesis of mesoporous high surface area CeO_2 and catalytic property for CO oxidation

Mesoporous CeO2 particles with high surface area were synthesized using a modified evaporation-induced self assembly(EISA) method which combined citric acid as complexing agent.As-prepared powder and further thermal treatment samples were characterized by X-ray diffraction(XRD),transmission electron microscopy(TEM),selected area electron diffraction(SAED),Fourier transform infrared spectrometer(FTIR),thermogravimetry and differential thermal analysis(TG-DTA),Brunauer-Emmett-Teller(BET) and Barrett-Joyner-Ha...     

温度对水热法合成WO3亚微米棒形貌和光吸收特性的影响

以钨酸钠为W源和硫酸钾为辅助盐,在酸性体系中对水热法合成WO3亚微米棒进行了研究。利用X射线衍射(XRD)、热场发射扫描电子显微镜(SEM)、透射电子显微镜(TEM)和选区电子衍射(SAED)对试样进行分析,结果表明:随着反应温度的升高和pH值的增加,它们都有利于合成WO3亚微米棒;在反应温度为240℃、pH值为1.5和反应时间48h下合成径向尺寸<200nm的晶体结构的WO3亚微米棒,此WO3亚微米棒径向分布较均匀。对不同条件下水热法合成的WO3进行紫外可见光的吸收光谱(UV-VIS)分析可得:随着反应温度的升高和pH值的增加,获得的WO3的紫外光吸收能力是逐渐增加的;WO3亚微米棒具有良好的紫外光吸收能力。     

Synthesis and surface modification of the nanoscale cerium borate as lubricant additive

Nanoparticle of cerium borate with a size of about 50 nm was synthesized via sol-gel precipitation method under micro-emulsion by oleic acid,using Na2B4O7 and Ce(NO3)3 aqueous solution as raw materials,and the morphology and microstructure of as-prepared particles were characterized by means of scanning electron microscopy(SEM) equipped with an energy-dispersive X-ray spectrometer(EDS),X-ray diffraction(XRD),infrared spectroscopy(IR),and thermogravimetric analysis(TGA).Two methods to disperse the particles into base oil were employed,and the results derived from the four-ball tribotester indicated that the friction coefficient of the base oil by the addition of the nanoscale cerium borate particles diminished greatly,and the anti-wear properties also depended on the dispersion methods.     

Photocatalytic degradation of methyl orange by polyoxometalates supported on yttrium-doped TiO_2

A series of novel photocatalysts, H3PW12O40-Y-TiO2 nanocomposites with different H3PW12O40 loading levels (10%-40%) were prepared by impregnation method. And the Y-TiO2 support, doped with yttrium, was synthesized via sol-gel technique. The prepared catalysts were characterized by Fourier transform infrared spectroscopy (FT-IR), powder X-ray diffraction (XRD), nitrogen adsorption-desorption analysis and scanning electron microscopy (SEM). The processes allowed obtaining Keggin structure and crystallized anatase with large BET surface area as well as uniform distribution. The effects of H3PW12O40 loadings, catalyst dose, initial pH and concentration of dye solution on the degradation kinetics of methyl orange under UV light (λ≥365 nm) were discussed. Kinetics studies showed that the photocatalytic degradation of methyl orange fitted the apparent first-order reaction. Methyl orange was totally degraded in 21 min under optimum conditions: 20% loading, 0.03 g dose and pH 1.0. The catalyst was stable and easily to be separated from reaction system for recovery.     

形变强化和逆相变细晶强化对Fe-18Cr-8Ni钢组织和性能的影响北大核心CSCD

奥氏体不锈钢较低的屈服强度限制了它在结构件中的使用。采用形变和相逆转变方法分别制备出了高屈服强度的奥氏体不锈钢。利用X射线衍射仪、光学显微镜、扫描电子显微镜、透射电子显微镜、电子背散射衍射技术和万能试验机分别对奥氏体钢进行组织表征和力学性能测试,结果表明粗大的奥氏体晶粒在形变过程中形成位错、剪切带、应变诱导马氏体等组织,相逆转变方法获得了超细的无缺陷等轴奥氏体晶粒。形变强化和细晶强化均能明显提高奥氏体不锈钢屈服强度(280 MPa提升至550 MPa)的同时保持较好的塑性(伸长率46%和55%)。     

A Quantified Complex Strengthening Mechanism in Solid-State Recycled Titanium

Machining chips of commercially pure titanium (ASTM Grade 2) were recycled into fully dense bulk material by equal channel angular pressing (ECAP). The morphology of the oxide layer derived from chip surfaces was characterized by focused ion beam miller and transmission electron microscopy. Electron backscatter diffraction and chemical analysis were used to propose quantitatively a complex strengthening mechanism considering interstitials, ultrafine grains (with misorientation ≥15 deg), and subgrains (<15 deg) substantially in existence after ECAP.     

Microstructure Evolution of Atomized Al-0.61 wt pct Fe and Al-1.90 wt pct Fe Alloys

The microstructure evolution of impulse atomized powders of Al-0.61 wt pct and Al-1.90 wt pct Fe compositions have been investigated with a scanning electron microscope, transmission electron microscope, neutron diffraction, and backscattering electron diffraction (EBSD). Both hypoeutectic and hypereutectic compositions demonstrated similar macrostructure (i.e., primary α-Al dendrites/cells with eutectic Al-Fe intermetallics decorated at the dendritic/cellular walls). Selected area electron diffraction (SAED) analysis and SAED pattern simulation identified the eutectic Al-Fe intermetallic as Al_mFe (m = 4.0-4.4). This is verified by neutron diffraction analysis. Cubic texture was observed by EBSD on the droplets with dendritic growth direction close to 〈111〉. The possible reasons are discussed.     

Si(100)衬底上CeO2薄膜的脉冲激光制备及性能研究

用CeO2陶瓷靶材,使用脉冲激光沉积(PLD)技术在Si(100)衬底上制备了CeO2薄膜.研究了衬底温度、沉积氧压对薄膜性能的影响,实验制备出了高度(111)取向的CeO2薄膜.使用X射线衍射(XRD)、反射式高能电子衍射(RHEED)对薄膜进行晶体结构的表征.结果表明:随着衬底温度的增加,薄膜中的残余宏观应力(拉应力)及微观应力逐渐减小,薄膜结晶质量不断提高,而沉积氧压对此影响较小.RHEED图像显示使用PLD方法在Si衬底上沉积的薄膜具备较高的结晶性及原子级平整的表面.使用原子力显微镜(AFM)对样品进行表面粗糙度分析,发现不同温度下生长的薄膜均具有光滑的表面,方均根粗糙度(RMS)均在0.4 nm以下.使用Keithley 4200半导体测试仪、椭偏仪对薄膜进行电性能及光学性能分析,发现衬底温度对薄膜的电学性能有显著影响,并且CeO2薄膜结晶状态与电学性能有直接的联系.