闪蒸法制备N型Bi2( Te0.95Se0.05)3薄膜的微结构及热电性能研究

采用闪蒸法在温度为473 K的玻璃基体上沉积了厚度为800 nm的N型Bi2(Te0.95Se0.05)3热电薄膜,并在373 ～573 K进行1h的真空退火处理.利用X射线衍射(XRD)、场发射扫描电子显微镜(FESEM)分别对薄膜的物相结构和表面形貌进行分析.采用表面粗糙度测量仪测定薄膜厚度,薄膜的电阻率采用四探针法进行测量,采用温差电动势法在室温下对薄膜的Seebeck系数进行表征.沉积态薄膜表明了(015)衍射峰为最强峰,退火处理后最强衍射峰为(006);沉积态薄膜由许多纳米晶粒组成,晶粒大小分布较均匀,平均晶粒尺寸大约45 nm,退火处理后出现了斜方六面体的片状晶体结构.退火温度从373 K增加到473 K,薄膜的电阻率和Seebeck系数增加,激活能也随退火温度的增加而增大,退火温度从523 K增加到573 K,薄膜的电阻率和Seebeck系数都缓慢下降.从373 ～473 K,热电功率因子随退火温度的升高而单调增加,退火温度为473 K时,电阻率和Seebeck系数分别是2.7 mΩ.cm和-180μV·K-1,热电功率因子最大值为12 μW.cmK-2.退火温度从523 K增加到573 K,热电功率因子的值逐渐下降.     

硫化退火温度对金属三靶顺序溅射CZTS薄膜性能的影响

通过XRD及Raman物相分析、SEM形貌观察和EDS成分分析等方法研究了硫化退火温度对金属三靶顺序溅射铜锌锡硫(CZTS)薄膜性能的影响。结果表明,在一定温度范围内(500~580℃),随着温度的升高薄膜的结晶性能有变好的趋势,形貌也得到了改善。当温度达到600℃时,CZTS薄膜会发生分解反应,该分解反应不但导致薄膜结晶性能及形貌恶化,也造成了锡元素的损失。580℃条件下获得的薄膜各项性能俱佳,是最适合本实验体系的退火温度。     

磁控溅射沉积Cu-Nb薄膜的特征及热退火的影响

用磁控共溅射法制备含铌1.16%～27.04%(原子分数)的Cu-Nb合金薄膜,运用EDX,XRD,SEM,TEM,显微硬度仪和电阻仪对沉积态和热退火态薄膜的成分、结构和性能进行了研究.结果表明,Nb添加显著影响Cu-Nb合金薄膜微结构,使Cu-Nb薄膜晶粒细化,含铌1.82%～15.75%的Cu-Nb膜呈纳米晶结构,存在Nb在Cu中的fec Cu(Nb)非平衡亚稳过饱和同溶体,固溶度随薄膜Nb浓度增加而上升,最大值为8.33%Nb.随Nb含量增加,薄膜中微晶体尺寸减小,Cu-27.04%Nb膜微结构演变至非晶态.与纯Cu膜对比表明,Nb添加显著提高沉积态Cu-Nb薄膜显微硬度和电阻率,总体上二者随膜Nb含量上升而增高.Nb含量高于4.05%时显微硬度增幅趋缓,非晶Cu-Nb膜硬度低于晶态膜,电阻卒则随铌含量上升而持续增加.经200,400及650℃退火1h后,Cu-Nb膜显微硬度降低、电阻率下降,降幅与退火温度呈正相关.XRD和SEM显示,650℃退火后晶态Cu-Nb膜基体相发生晶粒长大,并出现亚微米级富Cu第二相,非晶Cu-27.04%Nb膜则观察到晶化转变和随后的晶粒生长.Nb添加引起晶粒细化效应以及退火中基体相晶粒度增大是Cu-Nb薄膜微观结构和性能形成及演变的主要原因.     

磁控溅射制备钛基薄膜研究进展

磁控溅射技术是制备钛基薄膜常用的方法。本文综述了磁控溅射法的基本原理、特点及方法种类,并总结了磁控溅射法制备TiO_2、TiN、TiC薄膜和Ti复合薄膜的最新研究进展,最后展望了磁控溅射技术制备Ti基薄膜的发展方向。     

Thermoelectric Properties of CexCo4Sb12 Prepared by MA-SPS

Starting with elementary powders, thermoelectric materials CexCo4Sb12 were prepared by mechanical alloying and spark plasma sintering (MA-SPS). XRD analyses reveal that the expected major phase, named skutterudite was formed in MA process and was kept after SPS. The thermoelectric properties of MA-SPS samples including resistivity, Seebeck coefficient, power factor, thermal conductivity and the dimensionless figure of merit (ZT) were studied by varying Ce content and temperature. Depending on Ce levels, both P and N types of thermoelectric semiconductors were obtained. MA-SPS sintered Ce1.0Co4Sb12 exhibits the highest ZT in the range of 100-500℃ and the maximum ZT is found at x=1.0 and 400℃.     

不同S值磁控阴极溅射沉积Mo薄膜的结构与性能研究

在室温下,利用不同磁感应强度相对分布因子S的磁控阴极溅射沉积了金属Mo薄膜.实验研究了磁控阴极S值对放电参数、Mo薄膜的结构、形貌及性能的影响.分别利用XRD,SEM和四探针技术对Mo薄膜的相结构、表面和截面形貌及电阻率进行表征分析.结果表明,随着磁控阴极S值的增加,Mo靶放电电压降低,而放电电流增加;不同S值的磁控阴极沉积的Mo薄膜均呈现多晶结构,且具有柱状生长特征;随着磁控阴极S因子的增加Mo膜的厚度和电导率呈现先增加而后减小的变化规律,电阻率最小可达4.9×10-6Ω·cm.     

退火对CoSb3块体热电性能的影响

采用烧结和退火工艺制备了CoSb3块体热电材料，并探讨了退火对热电性能的影响。用X射线衍射分析了样品的相组成，用电常数测试仪和激光热导仪测试了样品的热电性能。结果表明，退火前后样品具有相同的相组成，其电阻率随着温度的升高而降低，具有典型的半导体电学特征；在相同温度下退火样品的ZT值低于或近似于未退火的样品，因此退火对于提高和改善CoSb3块体材料的热电性能没有明显作用。     

Characterisation of ZrAl and ZrAlN Thin Films Prepared by Pulsed DC Magnetron Sputtering

Thin films of ZrAl and ZrAlN were deposited on Si(100) substrates in the temperature range 300–773 K and with varying nitrogen flow rate from 0 to 10 sccm by co-sputtering of Zr (99.9 % purity) and Al (99.9 % purity) targets using a single pulsed power supply. At substrate temperature of 773 K, ZrAl thin films crystallized in hcp structure. The nitrogen flow rate was found to significantly influence the phase formation in ZrAlN films with the formation of fcc structure with a nitrogen flow rates in the range 1–2 sccm. The electrical resistivity of ZrAl films decreased from 62 to 24 μΩ cm with increase of substrate temperature, while it increased with nitrogen flow rate as a consequence of change in crystal structure and decrease in the crystallite size. Nanohardness measurements indicated a maximum hardness and elastic modulus of 20 and 369 GPa, respectively for ZrAlN films deposited at 773 K and 1 sccm of nitrogen flow rate.     

退火温度对0.2C-1.5Si-1.5Mn-(0.5Cu)TRIP 钢组织的影响

用彩色金相法、X 射线衍射、扫描电镜研究了成分(%)为 0.2C-1.5Si-1.5Mn和0.2C-1.5Si-1.5Mn-0.5Cu TRIP钢 750～780℃不同退火温度对组织的影响。结果表明,含0.5 %Cu TRIP钢750℃、760℃、780℃退火的残余奥氏体体积含量为15.2 %～17.2 % ,770℃退火为15.2 %～15.7% ;不含CuTRIP钢760℃和770℃退火的残余奥氏体体积含量分别为12.5 %～12.9%和14.6 %～15.1% ,低于750℃和780℃退火的奥氏体量分别为17.0 %～17.5%和16.0 %～16.4%。随退火温度由750℃提高至780℃ ,两种钢中的铁素体量由～70%降至～5 0% ,贝氏体量由～10%增至～30%     

Bi2Te3基热电材料输运性质优化策略研究进展

随着能源需求的持续增长和不可再生资源的不断耗竭,世界各国高度关注新型能源的开发,同时也致力于提高工业废热的回收率和利用率。热电材料是一种能够实现热能和电能直接转换的固态介质,以其为核心的热电器件不含运动附件且不排放污染物,已在半导体制冷和局部热管理领域实现商业化,例如户外制冷机、车载冷柜、光电芯片和功率激光器的控温装置等。热电制冷非常适于小空间热源的主动冷却,可能成为下一代通讯和信息技术的热管理难题中唯一可行的解决方案。Bi2Te3基化合物作为近室温区兼具稳定理化性质和优异输运性质的热电材料,一直受到学术界和产业界的广泛关注。本文在概述热电材料研究背景和制备方法的基础上,从能带工程、声子散射工程、热变形工艺、结构低维化等方面对热电性能的优化方法进行了归纳,并对未来机遇进行了展望。     

Influence of Magnetic Annealing on Properties of SmFe Thin Films

SmFe thin films were prepared by DC magietron sputtering at room temperature and 300 %. The influence of magnetic annealing temperature on the phase structure and magnetic properties was investigated. Results showed that thermal sputtering followed by a heat treatment process helped to obtain a structure with a relatively large fraction of SmFe2. Residual phases observed were α-Fe, Sm2O3, and unknown phases. During the annealing treatment, the intrinsic compressive stress in SmFe films was relieved and could become tensile at higher annealing temperatures. The degree of in-plane anisotropy weakened, and furthermore, the anisotropy transformed into out-of-plane anisotropy.     

溅射沉积Cu-W合金薄膜的结构及力学性能

用磁控共溅射法制备Cu-W合金薄膜,运用EDX,XRD,TEM,SEM和纳米压痕仪对薄膜成分、结构和力学性能及其关系进行了研究。结果表明,含W较低的Cu82.1W17.9(%,原子分数)和W浓度较高的Cu39.8W60.2薄膜为晶态结构且出现固溶度扩展,分别存在fccCu(W)亚稳过饱和固溶体(固溶度4.8%W)和bccW(Cu)亚稳过饱和固溶体(固溶度5.7%Cu),W含量为31.8%,45.7%,54.8%的Cu-W薄膜呈非晶态,表面粗糙度较晶态Cu-W薄膜低。总体上非晶Cu-W薄膜弹性模量E和硬度H值较低,fccCu-W膜实测E值介于Voigt和Reuss规则预测值之间,bcc和非晶Cu-W膜实测E值分别高于和低于预测值;晶态Cu-W膜实测H值与Voigt规则计算值的符合性优于非晶膜,薄膜结构对力学性能预测可靠性影响较大。     

基片温度对氧化铋薄膜光学性质的影响

在玻璃基片上直流磁控溅射沉积氧化铋薄膜,基片温度从室温增加到300℃并保持其它沉积条件一致,研究基片温度对薄膜光学性能的影响.样品的晶体结构、表面形貌和透射光谱分别用X射线衍射仪、原子力显微镜和分光光度计进行测量.结果表明,随着基片温度的增加,样品中Bi2O3的(120)衍射峰强度增强,表面颗粒直径逐渐减小;基片温度为250,300℃样品出现了Bi2O2.75的(006)衍射峰.采用拟合透射光谱数据的方法计算薄膜的折射率,消光系数及厚度,并求出光学带隙.随基片温度的增加,氧化铋薄膜的折射率减小,消光系数在10-2～10-1数量级,光学带隙在3.51～3.04 eV递减.     

Thermodynamic Properties of the Quasibinary System Bi2Se3 - Bi2Te3 over a Broad Temperature Range

We have studied the heat capacity and enthalpies of solid solutions in the quasibinary system Bi₂Se₃ - Bi₂Te₃ at low and high temperatures. Based on low-temperature measurements of the heat capacity, we have calculated the values of the enthalpy, entropy, and reduced Gibbs energy of the compounds under standard conditions. We have determined the temperature dependences of the thermodynamic functions for the solid solutions Bi₂Se₃ - Bi₂Te₃ (50, 70, and 80 mole% Bi₂Te₃) in the temperature range 298.15 K - T_mp. __________ Translated from Poroshkovaya Metallurgiya, Nos. 7–8(444), pp. 80–85, July–August, 2005.     

溅射参数对SmCo/Cr薄膜铬底层晶面取向及磁学性能的影响

采用直流磁控溅射法制备SmCo／Cr薄膜磁记录材料，通过改变Cr底层制备过程中的功率、靶基距、溅射压强和溅射时间，得到了磁性能不同的SmCo／Cr薄膜。利用X射线衍射法对Cr底层晶面取向和磁控溅射参数之间的关系进行了研究，结果表明：如果改变溅射参数，使沉积cr原子获得较大的能量，则有利于Cr底层最终以(110)晶面择优取向。本实验中Cr底层以(110)晶面择优取向的最佳实验条件为：溅射功率在50～70w左右，靶基距为6cm，压强为0．5Pa，溅射时间为15min。利用振动样品磁强计(VSM)测定SmCo／Cr薄膜的磁学性能，结果表明，如果Cr底层能以(110)晶面择优取向，所得到的SmCo／Cr薄膜的磁学性能较好。     

离子束溅射法制备La0.5Sr0.5CoO3薄膜的拉曼光谱分析

采用离子束溅射在氧化钇稳定的氧化锆(YSZ)和铝酸镧(LaAlO3)上制备了La0.5Sr0.5CoO3的钙钛矿薄膜.利用拉曼光谱,研究了不同热处理温度和不同衬底对LSCO薄膜材料的晶体结构、分子振动模式和化学键的影响.研究发现La0.5Sr0.5CoO3钙钛矿薄膜的晶体结构随着热处理温度的升高发生明显的相变,由排列无规则态朝着正交晶系结构转变,Co-O键构成的八面体间的相对运动强度逐渐减弱.另外,还发现La0.5Sr0.5CoO3钙钛矿薄膜在衬底氧化锫(YSZ)上的Co-O键振动频率要小于在衬底铝酸镧(LaAlO3)上的振动频率,这与两者的品格失配程度有关.     

Effect of Post Annealing on the Microstructure and Magnetic Properties of NdFeB/α-Fe/NdFeB Thin Films

A series of nanocomposite thin films, composed of Nd2Fe14B and α-Fe, has been prepared by DC-magnetron sputtering combined ion beam sputtering onto Si (100) substrates. The effects of post annealing on the microstructure and magnetic properties of [NdFeB/α-Fe/NdFeB]-type thin films have been investigated. The X-ray diffraction (XRD) study showed that annealing of the films for 30min at temperatures 550,600,650,700℃ resulted in the appearance of diffraction peaks, characteristic for Nd2Fe14B tetragonal structure, α-Fe and Nd2O3 phases. The investigation using the Vibrating Sample Magnetometer (VSM) with a maximum applied field of 2 T indicated that with the increase of the annealing temperature, the magnetic properties of the multilayer films were improved and reached peak value at 650℃ (Hci=41.72kA·m-1, Mr/Ms=0.4, (BH)max=30.35kJ·m-3), after which the magnetic properties were decreased greatly. Along with the increase of the thickness of α-Fe layer from Tα-Fe16nm, the coercivity Hci, saturation magnetization Ms, and remanence ratio Mr/Ms all declined. As the Atomic Force Microscope (AFM) indicated, after being annealed at 650℃ for 30min, the sample was showed fine surface morphology with grain size 60nm≤dα-Fe≤80nm and 100nm≤dNdFeB≤150nm.     

磁控溅射Ti/WO_3薄膜的微结构及光学性能

采用直流反应磁控溅射技术在玻璃基片上制备不同氧分压的Ti掺杂的WO3薄膜。用X射线衍射(XRD)、分光光度计、台阶仪等对薄膜的结构、光学性质进行表征;分析不同的氧分压对气敏薄膜透光率和结构的影响。结果表明,氧分压增大,膜厚减小,薄膜的平均晶粒尺寸增大,晶面间距增大,光学带隙变小。并用包络线法和经验公式法计算出薄膜的光学常数,结果表明,折射率和消光系数随氧分压的增加而增大。     

氧分压对直流磁控溅射铟锡氧化物(ITO)导电薄膜结构和性能的影响

通过直流磁控溅射热等静压铟锡氧化物(ITO)靶材制备ITO导电薄膜,并且针对O2-Ar混合气氛中氧的分压对ITO膜的结构、表面形貌、透光率以及导电率的影响进行了研究.结果表明,在低氧分压的条件下溅射,膜的(400)面非常显著地择优取向平行于玻璃表面,而随着氧分压的升高却表现为膜的(222)面择优取向平行于玻璃表面.同时,随着氧分压的升高,膜的表面粗糙度变小,膜的结构变得更细腻.膜的可见光透过率在氧分压增大的情形下有少许增大,但是膜的导电率却略有下降.