具有c轴择优的CuCr1-xMgxO2多晶的热电输运性质及Mg掺杂效应

采用固相反应法制备了c轴择优的CuCr_(1-x)MgxO_2(0≤x≤0. 08)系列多晶,通过X射线衍射、扫描电镜和电阻率-温度曲线、Seebeck系数-温度曲线对样品的结构、热电输运和固溶度进行表征研究。随Mg掺杂量在x=0～0. 03范围内增加,多晶为铜铁矿单相结构,层状晶粒在ab面显著长大,(00l)取向因子最大达0. 53,晶界和孔隙显著减少,致密度依次提高;多晶呈热激活机制的半导体电输运行为,热激活能从0. 273 eV下降到0. 031 eV,室温电导率相应提高了3～4个数量级,高温下Seebeck系数从481. 2μV·K~(-1)减小到334. 7μV·K~(-1)。由于声子曳引的贡献,随温度升高,掺Mg样品的Seebeck系数增大。x0. 03后,样品的热电输运性质基本保持不变,微观结构变化不大,在晶界处观察到MgCr_2O_4八面体尖晶石第二相,分析认为Mg掺杂的最大固溶度约为0. 03。随Mg~(2+)替代Cr~(3+)的增加,在靠近价带顶的上方引入受主能级并展宽,使电输运的热激活能显著下降,空穴载流子浓度增大;同时c轴择优取向使面内的输运分量增加,这都是电导率提高的主要原因,而载流子迁移率浮动是电导率提高的次要原因。     

多晶CaB6陶瓷弱铁磁性能与气孔率关系

用常压烧结和热压烧结法分别制备了多晶Ca1＋xB6（x=-0．02、0、0．02）陶瓷样品并对其铁磁性能进行系统分析．结果表明，在烧结温度低于1500℃范围内，不论样品富Ca或赤Ca，所有的样品均呈现铁磁性能；另外，两种方法制备的陶瓷样品虽然气孔率明显不同，而其铁磁性能并没有显著差异，认为CaB6样品存在的铁磁性机制不决定于样品中的Ca空位浓度和气孔率．     

Mn掺杂的NaxCoO2多晶制备与电输运性质研究

采用固相反应法制备了沿(00l)面高度择优取向的γ相NaxCoO2(X=0.5+δ,0.7)和Na0.5+δCo0.95Mn0.05O2系列多晶,且微量Mn掺杂阻碍了晶粒的长大.77～300K电阻率-温度曲线表明,NaγCoO2为金属的电输运行为,在相同烧结工艺下,Mn掺杂导致Na0.5+δCo0.95Mn0.05O2...     

双A层MAX相Mo2Ga2C的热压烧结研究

本工作采用真空热压烧结的方法, 研究Mo₂Ga₂C粉体的烧结性能, 制备致密的Mo₂Ga₂C块体材料, 并且表征所制备材料的微观结构。实验发现750 ℃是合适的烧结温度, 过高的烧结温度(850 ℃)会导致样品分解, 主要产物为Mo₂C。在750 ℃烧结过程中, 随着烧结时间的延长, 样品的晶粒没有明显长大, 但是样品内部空隙显著变小, 内部织构增强, 相对密度明显提高。因为Mo₂Ga₂C晶体的片状结构, 热压烧结过程中, 部分片状晶粒会偏转, 导致烧结样品的多数晶粒的(00l)晶面会倾向垂直于热压方向。在750 ℃烧结8 h, 可以得到几乎完全致密(相对密度98.8%)的Mo₂Ga₂C块体材料。     

纳米Fe包覆Si3N4的制备及其高温烧结微观组织

采用非均相沉淀-热还原法制备了Fe/Si₃N₄颗粒复合粉末并在热处理温度1873K和0.1MPa氮气气氛下进行常压与热压烧结。通过扫描电镜(SEM)、透射电镜(TEM)、电子能谱(EDS)、X射线衍射(XRD)等方法观察Fe/Si₃N₄复合粉末的结构形貌及常压、热压烧结后的微观组织。结果表明：Fe/Si₃N₄复合粉末物相主要存在Fe相与Si₃N₄相,微观结构为纳米薄层 Fe均匀包覆Si₃N₄颗粒;高温烧结后的常压与热压样品的组织成分与微观结构有极大的不同,除了存在Si₃N₄相之外,常压样品金属Fe相衍射峰消失,并有晶粒粗大铁硅化合物生成,热压样品则保留有金属Fe相,并存在晶粒相对细小铁硅化合物及致密的玻璃态物质。     

不同烧结工艺对K0.5Na0.5NbO3陶瓷微结构的影响

采用普通烧结方法和热压烧结方法制备了K0.5Na0.5NbO3(KNN)无铅压电陶瓷.着重研究了两种烧结工艺对陶瓷的微观结构、晶粒形貌及致密度的影响.研究结果表明,两种烧结方法制备的陶瓷样品都具有单一的正交钙钛矿结构,与普通烧结工艺相比,利用热压烧结工艺制备的样品呈现较高的相对密度(大于98%)、较小的晶粒尺寸(0.6μm左右)及较低的介电损耗(1 kHz,tanδ≤2.8%).实验中发现对于热压烧结的样品,通过改变后期退火温度,样品的晶粒尺寸,致密度可以有规律地变化.     

(Mg2Si1-xSbx)0.4-（Mg2Sn）0.6固溶体合金的制备及热电输运特性

以Mg、Si、Sn、Sb块体为原料,采用熔炼结合放电等离子烧结(SPS)技术制备了n型(Mg2Si1-xSbx)0.4-(Mg2Sn)0.6(0≤x≤0.0625)系列固溶体合金.结构及热电输运特性分析结果表明:当Mg原料过量8wt%时,可以弥补熔炼过程中Mg的挥发损失,形成单相(Mg2Si1-xSbx)0.4-(Mg2Sn)0.6固溶体.烧结样品的晶胞随Sb掺杂量的增加而增大;电阻率随Sb掺杂量的增加先减小后增大,当样品中Sb掺杂量x≤0.025时,样品电阻率呈现出半导体输运特性,Sb掺杂量x>0.025时,样品电阻率呈现为金属输运特性.Seebeck系数的绝对值随Sb掺杂量的增加先减小后增大;热导率κ在Sb掺杂量x≤0.025时比未掺杂Sb样品的热导率低,在Sb掺杂量x>0.025时高于未掺杂样品的热导率,但所有样品的晶格热导率明显低于未掺杂样品的晶格热导率.实验结果表明Sb的掺杂有利于降低晶格热导率和电阻率,提高中温区Seebeck系数绝对值;其中(Mg2Si0.95Sb0.05)0.4-(Mg2Sn)0.6合金具有最大ZT值,并在723 K附近取得最大值约为1.22.     

Al3+掺杂对La0.8Sr0.2Mn1–xAlxO3电输运性能的影响

钙钛矿锰氧化物La_1–xSr_xMnO₃ (LSMO)作为一种代表性庞磁阻材料,在磁传感器等领域具有广阔的应用前景,但在低磁场和室温下很难获得显著的庞磁阻效应。为提高LSMO磁电阻效应和转变温度,本研究采用传统固相反应法制备了La_0.8Sr_0.2Mn_1–xAl_xO₃ (0≤x≤0.25)(LSMAO)多晶样品,并系统分析了Al³⁺掺杂对LSMO电输运性质和磁电阻效应的影响。X射线衍射(XRD)图谱表明LSMAO样品具有单一的菱方结构,属于■空间群。电输运性质研究发现,样品的电阻率随Al³⁺的掺杂呈指数型上升,且外加磁场使金属-绝缘体转变温度有所提高。这可能是由于Al³⁺稀释了Mn³⁺/Mn⁴⁺离子网络,在减少载流子数量的同时增加了磁无序。此外,LSMAO陶瓷的导电机理随Al³⁺的掺杂从...     

TiB2/FeMo陶瓷的显微结构与力学性能

以Fe-Mo为助烧剂，通过热压制备了TiB2陶瓷．研究了烧结温度、烧结时间对材料显微结构和力学性能的影响，分析了烧结致密化过程．实验结果表明，随着热压烧结温度升高，材料抗弯强度、洛氏硬度出现峰值，热压烧结时间延长，抗弯强度有所下降．液相烧结的重排阶段致密化速率最快．     

FePt/B4C垂直磁记录介质薄膜的制备与表征

采用直流及射频磁控溅射结合真空退火的方法成功制备了（001）择优生长的FcPt/B4C多层薄膜并对其结构与磁性能做了初步的表征．结果表明，在每一个FbPt单元层中能得到较好（001）面择优的fet相FbPt合金，并且随着B4C含量的增大，薄膜的有序度提高．高分辨透射电子显微镜及其傅立叶变换表明，FePt层为具有（001）织构的fct相Fe55Pt45合金．样品的M-H曲线显示其垂直膜面方向矫顽力约为302.481kA/m；平行膜面方向矫顽力很小．     

高能球磨纳米CeO2/Zn复合粉末的热压烧结

采用真空热压工艺制备了纳米CeO2/Zn复合材料块体,并用正交实验法研究了热压工艺参数对复合材料块体相对密度的影响.结果表明:随着粉末球磨时间的增加,复合材料块体内纳米颗粒分散越均匀,基体晶粒不断细化;块体的相对密度随着热压温度、压力的提高和保温时间的延长而增加,其中热压温度的影响最大,压力影响次之,保温时间影响最小;制得的纳米复合材料块体可加入到热浸镀锌液中.     

Characterization of a β-FeSi2 p-n junction formed by the PECS method

We have fabricated semiconducting β-FeSi₂ bulks without doping and with Mn and Co doping by using a pulse electric current sintering (PECS) method, and explored the possibility of a direct bonding of n-type and p-type β-FeSi₂ bulks to form a p-n junction structure. P-type Mn-doped and n-type Co-doped β-FeSi₂ bulks were obtained by an annealing process at 800-850 °C for 100 h. The PECS was applied to bond the n-type and p-type bulks together for forming a p-n junction structure. We confirmed that the bonding was processed without any change in the β-FeSi₂ phase and was strongly joined with each other. Although we could not obtain the electrical characteristics of the p-n junction, Seebeck coefficients for n-type and p-type β-FeSi₂ in the bonded sample were determined to be −356 and 778 μV/K, respectively. We propose that these results should lead to an expanded use of the sintered β-FeSi₂ bulks in thermoelectric devices.     

Co掺杂CeO2稀磁氧化物陶瓷和纳米颗粒的铁磁性能

分别采用固相烧结法及激光液相烧蚀(LAL)技术,成功制备出Co掺杂CeO_2稀磁氧化物陶瓷块体和纳米颗粒。XRD和SEM研究发现所制备的材料具有良好的结晶性和形貌。Co掺杂CeO_2稀磁氧化物陶瓷块体和纳米颗粒均为多晶立方结构,与纯立方相的CeO_2结构相同,说明Co掺杂未形成其他结构和杂相。磁性测量表明固相烧结法和激光烧蚀液相法制备的Co掺杂CeO_2样品均具有较高的室温铁磁性,且远高于文献中报道的结果。将陶瓷块材经激光烧蚀成纳米颗粒后,纳米颗粒的铁磁性与陶瓷块材保持一致。这说明激光烧蚀法制备的纳米材料可以很好地保持母材的特性,是一种很好的纳米颗粒制备方法。根据XRD和SEM研究结果,笔者认为Co掺杂CeO_2陶瓷块材及纳米颗粒的室温铁磁性是内禀性质;磁性产生的机理源于氧空位诱导的铁磁性耦合。     

TiO2和WO3复合掺杂金属陶瓷的致密化及抗高温氧化性

采用真空烧结技术制备TiO_2和WO_3复合掺杂17Ni/(NiFe_2O_4-10NiO)金属陶瓷试样,研究TiO_2和WO_3复合掺杂剂对试样物相组成、显微组织、烧结致密化和抗高温氧化性的影响。结果表明:TiO_2和WO_3复合掺杂后无新相生成,而是固溶到NiFe_2O_4晶格中,产生晶格畸变和空位,使致密度提高;TiO_2和WO_3复合掺杂有利于17Ni/(NiFe2O_4-10NiO)金属陶瓷形成更加致密的具有氧化保护性的致密层,阻碍金属Ni向外迁移,提高试样的抗高温氧化性,其中TiO_2和WO_3复合掺杂量为2%(比例为3∶1)和3%(比例为1∶3)时,试样的抗高温氧化性最好,其氧化30h后的氧化层厚度大约为80μm,比未掺杂试样降低了38.46%。     

各向异性Nd2Fe14B／α-Fe纳米晶复合磁体的制备和性能

采用声化学法、放电等离子烧结技术(SPS)和热变形工艺制备致密各向同性和各向异性Nd_2Fe_(14)B/αFe复合磁体,研究了软磁相包覆对磁体的结构和性能的影响.结果表明,软磁相α-Fe对各向同性Nd_2Fe_(14)B/α-Fe复合磁体的影响主要表现为增强两相间的交换耦合作用,从而提高剩磁.当α-Fe体积分数的数值适当(不超过2%)时,各向异性Nd_2Fe_(14)B/α-Fe磁体形成较好的c轴晶体织构,具有较高的磁性能.α-Fe体积分数为1%的磁体性能最高:B_r=1.367 T,H_(ci)=712 kA/m,(BH)_m=327 kJ/m~3.     

Spray pyrolyzed β-In2S3 thin films: Effect of postdeposition annealing

Indium sulfide thin films prepared using spray pyrolysis, with In/S ratio 2/3 in the solution, were annealed in vacuum at 300 and 400 °C. The effect of this treatment on properties of the films was studied using X-ray diffraction, scanning electron microscopy, X-ray photoelectron spectroscopy, optical absorption, transmission and electrical measurements. Optical constants of the films were calculated using the envelope method. Annealing did not affect the optical properties of the film much, but the resistivity of the films showed a drastic decrease and the grain size increased. In₂S₃ thin films have potential use as buffer layer in photovoltaic heterojunction devices.     

Co掺杂ZnO块材的晶体结构和磁性能研究

采用固相法制备了Zn1-xCoxO（x=0．05-0．25）块材,烧结温度和Co含量对Zn1-xCoxO（x=0．05-0．25）块材的晶体结构和室温磁性能影响强烈,当x≤0．1,烧结温度从800增加到1100℃时,Zn1-xCoxO（x=0．05-0．25）呈现出单相结构,但当x〉0．1,烧结温度为800℃时,样品中出现CoO相;随着烧结温度提高到900℃,样品再次获得纯的单相结构。为了获得高的饱和磁化强度Ms,最佳烧结温度应该根据Co含量进行调整。在最佳烧结温度条件下,当x从0．05提高到0．1时,Ms从0．79增加到了1．06μB/Co,但当x继续提高到0．2和0．25时,Ms分别降低到了0．59和0．41μB/Co。     

Microstructure and electrical properties of Al2O3-ZrO2 composite films for gate dielectric applications

Al₂O₃-ZrO₂ composite films were fabricated on Si by ultrahigh vacuum electron-beam coevaporation. The crystallization temperature, surface morphology, structural characteristics and electrical properties of the annealed films are investigated. Our results indicate that the amorphous and mixed structure is maintained up to an annealing temperature of 900 °C, which is much higher than that of pure ZrO₂ film, and the interfacial oxide layer thickness does not increase after annealing at 900 °C. However, a portion of the Al₂O₃-ZrO₂ film becomes polycrystalline after 1000 °C annealing and interfacial broadening is observed. Possible explanations are given to explain our observations. A dielectric constant of 20.1 is calculated from the 900 °C-annealed ZrO₂-Al₂O₃ film based on high-frequency capacitance-voltage measurements. This dielectric characteristic shows an equivalent oxide thickness (EOT) as low as 1.94 nm. An extremely low leakage current density of ∼2×10⁻⁷ A/cm² at a gate voltage of 1 V and low interface state density are also observed in the dielectric film.     

Microstructural features and deformation-induced lattice defects in hot-extruded Bi2Te3 thermoelectric compound

Bismuth telluride (Bi₂Te₃) bulk material was prepared by a powder hot-extrusion technique. The microstructure, texture evolution, and deformation-induced lattice defects, as well as the effect of heat treatment on its microstructure and thermoelectric properties were investigated. As-extruded Bi₂Te₃ compound was found to be characterized by a dynamically and statically recrystallized microstructure with fine-equiaxed grains and low dislocation density. The majority of boundaries in the extruded specimens were large-angle boundaries with average misorientation angles of more than 30°. There was no significant change in dislocation configuration, even after heat treatment at a temperature higher than the extrusion temperature. Moreover, the Seebeck coefficient and electrical resistivity of the extruded specimens could not be improved by annealing. Microstructural examinations indicated the existence of a deformation-induced stacking disorder with local atomic shift, which we term “phase disorder,” on the basal plane in the extruded Bi₂Te₃ compound. The presence of this structural defect may be one of the main reasons for the slightly lower values of thermoelectric properties for the hot-extruded Bi₂Te₃ compound, compared with a unidirectionally solidified specimen.     

微波烧结LiCo1/3Ni1/3Mn1/3O2电磁场与温度场的仿真模拟

分析了微波烧结的原理和特点,利用COMSOL Multi-physics模拟软件对矩形微波炉进行了仿真模拟,研究了微波烧结正极材料LiCo_(1/3)Ni_(1/3)Mn_(1/3)O_2时电磁场与温度场的分布,测量了粉末样品LiCo_(1/3)Ni_(1/3)Mn_(1/3)O_2的介电常数,并与模拟结果相对照.研究表明:微波在烧结LiCo_(1/3)Ni_(1/3)Mn_(1/3)O_2样品时,炉腔内电磁场的分布受到影响,微波炉内表面的电场强度减弱;材料内部温度场的分布不均匀,材料的下半部分温度较高;同时,在仿真模拟计算过程中,求得LiCo_(1/3)Ni_(1/3)Mn_(1/3)O_2在微波中烧结到不同温度时的能量损耗,根据李赫德涅凯法则计算出其对应的相对介电常数,发现在20~620℃,相对介电常数随温度的上升而变大.根据实验测得的复合介电常数,求出对应温度点LiCo_(1/3)Ni_(1/3)Mn_(1/3)O_2的相对介电常数.利用Origin对仿真模拟计算和实验求得的两组相对介电常数数据进行拟合对比,发现实验求得的LiCo_(1/3)Ni_(1/3)Mn_(1/3)O_2的相对介电常数与仿真模拟计算所得数据趋势吻合.