室温电化学法制备白钨矿SrWO4晶态膜的生长特性研究

采用恒电流电化学技术直接在金属钨片上制备了具有白钨矿结构的钨酸锶(SrWO4)晶态薄膜,通过SEM和EDX测试分析方法,研究了薄膜在不同的生长阶段(包括薄膜从最初成核并开始生长,到薄膜布满整个基片,即薄膜生长结束)的生长特性.研究结果表明,SrWO4晶核和晶粒优先选择在基片的缺陷处堆砌生长,在薄膜生长的初期,一定数量的WO4负离子配位多面体沉积在基片上并形成具有白钨矿结构的骨架,继而Sr2+对该骨架进行填充,由此形成晶核和晶粒;随着沉积时间的延长,晶粒密度不断增大,晶核和晶粒也不断长大,并沿着c轴生长的方向开始分叉,晶粒越大分叉越多;最终,当SrWO4薄膜生长过程结束时,团簇生长的花菜状晶粒布满整个基片,形成致密的薄膜.该研究结果对晶态薄膜电化学制备生长机制的认识、以及采用电化学方法制备晶态薄膜的工艺调控都具有重要意义.     

溶胶-凝胶法制备钛酸铝薄膜及其抗熔盐腐蚀性能

以钛酸四丁酯和硝酸铝为原料,乙醇为溶剂,通过溶胶-凝胶法在碳化硅基片上制备钛酸铝薄膜.借助DSC-TG、XRD、FE-SEM和SEM研究了钛酸铝干凝胶在热处理过程中的热重效应与相变化、薄膜的晶相组成、显微结构及其抗硝酸钠熔体腐蚀性能.结果表明:制备的钛酸铝薄膜表面均匀、致密,晶粒尺寸在100 nm左右,具有良好的抗硝酸钠熔体腐蚀性能.     

p型掺杂晶体硅的低温液相(001)外延生长研究

为寻求以低成本制备n型太阳电池的pn结,进行了Al-17.6wt;Si合金熔体中(001)n型单晶硅衬底上液相外延生长p型掺杂硅实验.所用方法为垂直浸渍法,实验了过冷恒温生长与回熔处理后连续冷却生长两种模式,过程中体系以流动高纯氩保护.对所得外延生长晶体结构、形貌及所得pn结开路电压进行了分析和测定.结果显示,合金熔体中硅晶体(001)液相外延生长能够实现,但一般呈离散分布的金字塔型岛状生长;只有衬底回熔处理后原位连续降温生长模式可获得连续外延薄膜,之后在其上出现岛状生长,呈现Stranski-Krastanov生长模式.所得连续外延薄膜形成的pn结开路电压比恒温生长所得的提升约100 mV;连续外延薄膜形成后期出现的岛状生长使开路电压明显下降;生长速度提高会使连续降温外延生长pn结开路电压略有降低.     

Tl-1223高温超导薄膜在蓝宝石单晶基片上的生长和性能研究

本文报道了采用射频磁控溅射法和快速升温烧结法在R面取向的蓝宝石单晶基片上生长CeO₂缓冲层和Tl-1223超导薄膜，研究了缓冲层生长情况和先驱膜后退火条件对超导薄膜结晶情况和超导特性的影响。AFM和XRD表征结果显示，蓝宝石基片经过退火后其表面形成具有光滑平台的台阶结构，同时基片的晶体质量得到了改善；本文所制备的CeO₂缓冲层和Tl-1223超导薄膜具有较好的c轴生长取向，而且两者呈现良好的ab面内织构。SEM表征结果显示，生长良好的Tl-1223超导薄膜呈层状结构，表面光滑平整、结构致密。在液氮环境下，测得所制备Tl-1223超导薄膜的临界转变温度T_c约为111 K,临界电流密度J_c(77 K,0 T)约为1.3 MA/cm²。     

用MOCVD法在玻璃和Si(100)基片上制备TiO2薄膜

采用大气开放式金属有机化合物化学气相沉积方法(AP-MOCVD),以四异丙醇钛(TTIP)为原料,在不同的实验条件下分别在Si(100)和玻璃基片上制备TiO2薄膜.当气化室温度为140℃,基片温度为350℃时,玻璃基片上生长的薄膜XRD谱中只出现了锐钛矿相(200)晶面的衍射峰,表明此时薄膜高度取向,在Si(100)基片上生长的TiO2薄膜也有取向性.通过SEM观察高度取向的TiO2薄膜表面出现四边形的微结构.     

甲基乙酸铵及氯苯在有机-无机卤化铅钙钛矿 结晶过程中的协同作用

通过在钙钛矿前驱溶液中加入甲基乙酸铵(MAAc)并结合氯苯(CB)反溶剂工艺制备了MAPbI3及MA1-x FAx PbI3混合阳离子钙钛矿薄膜,并系统研究了其在薄膜结晶过程中的协同作用.发现MAAc可以诱导MAPbI3晶体在(112)/(200)而非(110)方向上的晶化,且CB反溶剂处理可以进一步促进MAPbI3(112)/(200)的晶化;在MA1-x FAx PbI3混合阳离子钙钛矿体系中则同时存在(110)和(112)/(200)结晶取向,且(110)取向上的结晶比例随FA+含量的增加而提高,CB反溶剂处理将促进晶粒在(110)取向上的生长.最终通过工艺优化,在前驱溶液中加入16;的MAAc并利用CB反溶剂工艺,实现了效率为～17.5;且无明显迟滞现象的MA0.9 FA0.1 PbI3钙钛矿太阳电池.     

沉积温度对磁控溅射生长SrRuO_3薄膜结构和性能的影响

采用射频磁控溅射法在(001)SrTiO_3基片上制备了SrRuO_3薄膜,采用X射线衍射(XRD)、原子力显微镜(AFM)、四探针测试仪等分析方法系统研究了沉积温度对SrRuO_3薄膜结构、表面形貌及输运性质的影响.实验结果表明:当生长温度低于550 ℃时,SrRuO_3薄膜为多晶结构;当温度在550～650 ℃范围内变化时,SrRuO_3薄膜可以在SrTiO_3基片上外延生长,薄膜的最低电阻率约为0.5 mΩ·cm.     

超声喷雾热分解法制备ZnO薄膜及衬底温度对其性能的影响

以醋酸锌水溶液为前驱体溶液,采用超声喷雾热分解法在玻璃衬底上制备得到了温度在350℃到450℃范围内的ZnO薄膜.用X射线衍射(XRD)、扫描电镜(SEM)及紫外-可见分光光度计分析了ZnO薄膜的晶体结构、微观形貌及其光学性质,重点探究了衬底温度对ZnO薄膜生长过程及微观结构的影响.分析表明:制备的ZnO薄膜为六角铅锌矿结构,衬底温度对薄膜的质量有着重要的影响;所得薄膜在400℃时结晶性能好,沿c轴择优取向生长,具有优良的均匀性和致密性;所制备的薄膜在可见光区透过率高达86;以上,在紫外光区吸收强烈.     

热处理工艺对超声电沉积制备CuInSe2薄膜的影响

采用三电极系统,在超声辅助下,以Mo薄片为柔性基底制备了CuInSe2(CIS)前驱体薄膜,经热处理得到了具有黄铜矿型晶体结构的CIS薄膜.研究了热处理温度,保温时间和升温速率对CuInSe2薄膜成分、物相及形貌的影响.结果表明:热处理使薄膜物相变得纯净,随着热处理温度的提高、保温时间的延长和升温速率的减慢,结晶度提高.温度过高、时间过长制备的CIS薄膜表面有大颗粒出现以至表面粗糙度增加、颗粒不均匀.     

GaAs/Ga2O3复合多晶薄膜的生长与光学性能研究

采用热蒸发沉积法,以砷化镓和氧化镓粉末为原料,以氧化铟为催化剂,在800 ℃的氩气气氛中,在(100)砷化镓基片表面上沉积生成GaAs/Ga2O3薄膜.以配有成分分析的场发射扫描电镜(FESEM)、X-射线衍射仪(XRD)、光致发光仪(PL)等测试方法对所得薄膜的成分、形貌、晶体结构和光学性能进行了表征.研究结果表明:薄膜以规整的波浪形均匀地覆盖在砷化镓基片表面上,所得薄膜为GaAs/Ga2O3复合多晶薄膜,光致发光峰为强的红光发射;薄膜的生长机理为固-气-固过程,薄膜中砷元素含量的增加与氧化铟的作用有关.     

反应磁控溅射制备AZO薄膜相结构的演化及机理研究

在室温下,利用直流反应磁控溅射技术在不同的氧气流量下沉积ZnO∶ Al (AZO)薄膜.采用XRD、SEM和TEM技术分析薄膜相成分、表面截面形貌及微观结构.结果表明:氧气流量为2.5 sccm时,沉积形成的薄膜为不透明具有金属导电性能的AZO/Zn( AZO)双层复合膜结构;氧气流量为3.5 sccm时,沉积形成了透明导电的AZO薄膜;氧气流量为5.0 sccm时,形成了透明不导电且含有纳米Al2O3颗粒的AZO薄膜;此外,AZO薄膜在400℃退火后,薄膜晶粒长大和(002)晶面方向择优生长更加明显以及高氧气流量沉积的AZO薄膜中的纳米Al2O3颗粒消失.     

Optical properties of Al‐doped ZnO thin films deposited by two different sputtering methods

Aluminum‐doped zinc oxide (AZO) thin films were deposited on sapphire (002) and glass substrates by two different sputtering techniques radio frequency magnetron cosputtering of AZO and ZnO targets and sputtering of an AZO target. The dependence of the photoluminescence (PL) and transmittance properties of the AZO films deposited by cosputtering and sputtering on the AZO/ZnO target power ratio, R and the O₂/Ar flow ratio, r were investigated, respectively. Only a deep level emission peak appears in the PL spectra of cosputtered AZO films whereas both UV emission and deep level emission peaks are observed in the PL spectra of sputtered AZO films. The absorption edges in the transmittance spectra of the AZO films shift to the lower wavelength region as R and r increase. Also effects of crystallinity, surface roughness, PL on the transmittance of the AZO films were explained using the X‐ray diffraction (XRD), atomic force microscopy (AFM), and PL analysis results. (© 2006 WILEY‐VCH Verlag GmbH & Co. KGaA, Weinheim)     

外加氩气流下脉冲激光烧蚀制备纳米硅晶粒成核生长动力学研究

为研究纳米硅晶粒成核生长动力学过程,采用脉冲激光烧蚀(PLA)技术,在室温,50～200 Pa的氩气氛围中,通过引入垂直于烧蚀羽辉轴线的外加气流,在水平放置的衬底上沉积了一系列纳米Si晶薄膜.扫描电子显微镜( SEM)、拉曼(Raman)散射和X射线衍射(XRD)检测结果表明,未引入气流时,衬底上相同位置处晶粒尺寸随气体压强的增大逐渐减小;在距靶1 ～2cm范围内引入气流后,尺寸变化规律与未引入气流时相反.通过分析晶粒尺寸及其在衬底上的位置分布特点,结合流体力学模型和热动力学方程,分析得出在激光能量密度一定的条件下,环境气体压强、烧蚀粒子温度和密度共同影响着纳米晶粒的成核生长.     

Microstructure and Texture Formation in Vacuum-deposited Silver Films

The role of the recystallization in the processes of microstructure and texture formation of silver films is compared for films: 1) deposited at high substrate temperatures (up to 720 K) and slowly cooled or quenched to room temperature; 2) deposited at room temperature and annealed at high temperatures. The grain growth distribution curves and the texture perfection are analysed. It is shown that the recrystallization processes taking place both during the slow cooling and during the annealing of the films lead to a formation of identical film structure with lower degree of texture perfection than in the case of quenched films.     

Epitaxial growth of MgO films on Si(1 1 1) by metal organic chemical vapor deposition

Epitaxial MgO films were grown on Si(1 1 1) substrates at 800°C using methylmagnesium tert-butoxide (MeMgO^tBu) as a single precursor under high-vacuum conditions (5×10⁻⁶ Torr). The crystalline structure, morphology, and chemical composition of the deposited films were investigated by X-ray diffraction, X-ray pole figure analysis, scanning electron microscopy, and X-ray photoelectron spectroscopy. The results show that epitaxial MgO films with correct stoichiometry can be deposited on Si(1 1 1) at 800°C. The single precursor methylmagnesium tert-butoxide has been found suitable for the epitaxial growth of MgO on Si(1 1 1) substrates.     

UV,violet and blue‐green luminescence from RF sputter deposited ZnO:Al thin films

The mechanism of ultraviolet (UV), violet and blue green emission from ZnO:Al (AZO) thin films deposited at different radio frequency (r.f.) powers on glass substrates was investigated. The structure and surface morphology of AZO films have also been observed. The optical transmittance spectra shows more than 80% transmittance in the visible region and the band gap is found to be directly allowed. From the photoluminescence measurement, intense UV and blue green luminescence is obtained for the samples deposited at higher sputtering powers. The mechanism of luminescence suggests that UV luminescence of AZO thin film is related to the transition from near band edge to the valence band and the concentration of antisite oxide (O_zn) increases with increase in r.f. power which in turn increases the intensity of green band emission while the violet PL is due to the defect level transition in the grain boundaries of AZO films. (© 2005 WILEY‐VCH Verlag GmbH & Co. KGaA, Weinheim)     

金刚石膜在Si(100)衬底上的选择沉积

采用自行设计的微波等离子体化学气相沉积系统,利用铜网作为模板实现了在Si(100)衬底上金刚石膜的选择沉积.用场发射扫描电子显微镜(SEM)、Raman散射谱对样品进行了表征与分析.并与同样生长条件下未采用模板时得到的金刚石样品进行了比较.结果发现,采用模板后,金刚石膜的成核密度和质量都得到很大提高.     

A kinetic treatment of glass formation VII: Transient nucleation in non-isothermal crystallization during cooling

The analysis of crystallization statistics has been modified to allow for time-dependent (transient) nucleation. To establish its accuracy, the numerical analysis has been applied to isothermal crystallization kinetics and shown to yield crystallization versus time curves which compare very closely with curves calculated analytically with or without the inclusion of transient nucleation.The numerical analysis including transient has been used to calculate the critical cooling rates for glass formation in anorthite and o-terphenyl considering (1) only homogeneous nucleation and (2) homogeneous nucleation + heterogeneous nucleation for 10⁷ heterogeneities cm^?3 with contact angles between 40° and 100°. It has been shown that inclusion of time-dependent nucleation in the calculations does not change the critical cooling rates for glass formation calculated assuming steady-state homogeneous nucleation in both materials. The critical cooling rate in anorthite calculated including steady-state heterogeneous nucleation was found to be decreased only slightly by the inclusion of time-dependent nucleation; while the critical cooling rates calculated for o-terphenyl were not change at all by the inclusion of time-dependent nncleation.The lack of an effect of time-dependent nucleation on the critical cooling rates calculated assuming only homogeneous nucleation is explained by the relatively small transient times on the high temperature side of the nucleation peak (a temperature range which has an overwhelming effect on the overall crystallization process because of the relatively high crystal growth rates in this range).Although the critical cooling rates associated with heterogeneous nucleation are large, the nucleation here takes place at relatively small undercooling where the transient times are relatively small. Thus, transient nucleation causes only a temporary delay in the over all crystallization, and its effect on the critical cooling rate is small.     

Crystalline and electrical properties of pulsed laser deposited BST on platinized silicon substrates

In order to produce thin film capacitors with elevated capacitance and breakdown strength, pulsed laser deposition of the ferroelectric material Ba_0.6Sr_0.4TiO₃ (BST) has been made on (1 1 1)Pt/Ti/SiO₂/Si substrates. The films are in situ crystallized at 700 °C, polycrystalline in nature, and exhibit a single perovskite phase. This paper reports on both the effect of the oxygen pressure during heating and deposition, and the influence of different modes of introduction during the deposition stage, on the crystalline and electrical properties of the BST films. Orientation of films depends on the deposition oxygen pressure, with a (1 1 1) preferential orientation obtained when depositing under vacuum. XRD characterization reveals that the out-of-plane parameter of BST films increases when depositions are made under lower oxygen pressure. This phenomenon is related to a higher concentration of vacancies and defects in the films grown under low-pressure environment. However, a local introduction of oxygen on the substrate improves the annihilation of these defects. The crystalline orientation of the films is also highly dependent on the residual oxygen pressure during heating. A high (1 1 1) preferentially oriented BST film is obtained when heating and depositing under 0.1 mbar oxygen pressure. The heating atmosphere is thought to influence the out-diffusion of titanium on the surface of the Pt layer, thus modifying the nucleation and growth of BST films. Aluminum electrodes have been deposited on top of the BST films by dc sputtering to measure electrical capacitances. The calculated dielectric constant of in situ crystallized films deposited under 0.1 mbar oxygen pressure exceeds 500 at 100 kHz under zero dc bias. This high dielectric constant value obtained without post-deposition treatment appears to be of great technological interest.     

The dependence of the grain size of continuous epitaxial films on the growth conditions

A systematic investigation on the dependence of the grain size of continuous (after coalescence) PbTe films on the growth conditions is carried out. The films were deposited epitaxially on BaF₂ substrates. The practical applications of such a study are pointed out. Also we point out that this type of investigation of continuous films can contribute a body of experimental data that can be used to test theories on epitaxial nucleation and growth.