还原氮化对ZrO2薄膜SERS性能的影响研究

以八水氧氯化锆(ZrOCl2·8H2 O)为原料制备前驱体溶液,采用旋涂工艺制备ZrO2薄膜,并对其进行还原氮化.利用XRD、FE-SEM、UV-Vis-Nir和Raman测试薄膜结构、光学性能及SERS效应.结果表明,还原氮化后薄膜中出现了氮氧化合物,颗粒明显,薄膜厚度约为0.77μm.薄膜的紫外可见近红外光谱在350～650 nm附近展现出较强的吸收.利用R6G作为探针分子研究了薄膜的SERS效应,结果表明,还原氮化后的氧化锆薄膜拉曼增强效应显著提升,拉曼增强因子为2.479×102.     

浸渍工艺对ZrO2纤维布结构及性能的影响

采用前驱体浸渍工艺制备ZrO2纤维布.利用SEM、XRD研究粘胶织物及ZrO2纤维布的微观结构;测试了ZrO2纤维布的横向抗张强度,研究了浸渍工艺对ZrO2纤维布微观结构、面密度和抗张强度的影响.结果表明:粘胶织物是制备ZrO2纤维布的理想前驱体材料;改善浸渍方式、提高浸渍溶液浓度和温度均能提高ZrO2纤维布的面密度;浸渍方式显著影响单根纤维的致密程度,残液去除方式显著影响纤维的分散程度,采用辊压浸渍和离心甩干去除残液的方式能够显著提高ZrO2纤维布的抗张强度.     

改进的碳铵沉淀法中氧化钇粉体尺寸及形貌的调控研究

以商业氧化钇(Y2 O3)为原材料,采用改进的碳酸盐沉淀工艺合成钇碳酸盐前驱体,经随后的焙烧工艺获得Y2O3产品.X衍射技术(XRD)和扫描电镜(SEM)表征表明:合成的碳酸盐前驱体Y2(CO3)3·2H2O具有类球形形貌、粒度分布均匀,经950℃焙烧2 h,前驱体受热分解为Y2 O3粉体,粉体完整保留了前驱体的形貌特征.同时,基于对NH4 HCO3/NH4+不同摩尔比条件下NH4 HCO3/NH4 NO3混合溶液中pH值变化的理论计算,在保持其他条件不变化条件下,通过改变NH4 HCO3/NH4 NO3混合溶液的加入量以获得不同的稀土碳酸盐沉淀终点pH值,当碳酸盐沉淀过程中pH值从6.0降低至4.7时,可实现超细至大颗粒不同尺寸氧化钇粉体的制备.同时,公斤级的扩大试验证实该工艺具有良好的可推广性.进一步提出NH4+在碳酸氢铵沉淀制备氧化钇工艺中的作用机理:(1)改变反应体系中阳离子和阴离子的组成;(2)显著影响前驱体的晶型;(3)显著影响产品颗粒尺寸大小.     

片状ZnO薄膜的制备及其在DSSC中的光电性能研究

采用均匀沉淀法在导电玻璃基体上制备ZnO前驱体薄膜,然后热分解前驱体制备出ZnO薄膜用作染料敏化太阳能电池(DSSC)的光阳极.使用XRD和SEM对ZnO薄膜的结构和形貌进行表征.讨论了n(尿素)/n(Zn2+)、Zn2+浓度、均匀沉淀反应温度、薄膜焙烧温度等工艺因素对ZnO在DSSC中的光电性能影响.结果表明,均匀沉淀法制备ZnO薄膜为六方纤锌矿结构,ZnO薄膜以片状在基体上生长.优化的ZnO薄膜组装的DSSC在100mW/cm2下的短路电流为5.39 mA/cm2,开路电压为O.516 V.     

304不锈钢表面氧化锆薄膜的腐蚀特性研究

采用溶胶-凝胶工艺在304不锈钢基体表面制备了经600℃烧结热处理的一、二、三层ZrO2薄膜.利用X射线衍射仪(XRD)和扫描电子显微镜(SEM),对ZrO2薄膜晶体结构和表面形貌进行了表征.结果表明:ZrO2主要为四方相结构,并伴有少量的单斜相;随着薄膜层数的增加,薄膜表面形貌逐渐改善,晶粒尺寸逐渐减小.利用电化学工作站分析了涂膜前后样品在5; NaCl溶液中的电化学腐蚀行为.结果显示:ZrO2薄膜能够有效提高不锈钢的耐腐蚀能力,且随着薄膜层数的增加,样品的自腐蚀电流密度逐渐减小,自腐蚀电位与极化电阻值逐渐增大,耐腐蚀性能逐渐提高.     

氟金云母钛珠光颜料的制备及表征

利用硫酸沸腾水解法制备了氟金云母钛珠光颜料前驱体,并通过差热-热重分析确定了珠光颜料前驱体的煅烧工艺.通过正交实验考察了反应温度、初始pH值、反应时间、搅拌速度、钛液浓度、晶型促进剂(SnCl_4)对前驱体包覆率的影响,得到了制备珠光颜料前驱体的最佳工艺条件以及影响包覆率的各因素的主次顺序.借助SEM、XRD、FT-IR以及EDS对煅烧前后的粉体进行了表征.测试结果表明:在优化的工艺条件下制得的珠光颜料表面致密光滑,包覆层为金红石型TiO_2,包覆率为27.3;.     

卷对卷技术制备大面积柔性CIGS薄膜太阳电池吸收层

以轻质柔性聚酰亚胺(PI)材料为衬底,采用低温共蒸发"一步法"工艺制备四元化合物Cu(In,Ga)Se2(CIGS)薄膜.本文采用卷对卷(roll-to-roll)技术,在衬底幅宽300 mm的方向上实现了良好的成膜均匀性.利用XRD和XRF分别分析了所制备薄膜的晶相、组分和厚度,SEM分析了薄膜的表面形貌,讨论了不同衬底温度下制备的CIGS薄膜的性能.     

纳米Al2O3/GdAlO3共晶陶瓷复合粉体的醇-水加热法制备与表征

为制备分散均匀的纳米尺度的共晶陶瓷复合粉体,采用Al(NO3)3·9H2O和Gd2O3作为原材料,通过醇-水加热法制备了纳米尺度的Al2O3/GdAlO3共晶成分陶瓷粉体.研究了溶液初始浓度配比和pH值等对复合粉体粒径的影响.通过SEM、TEM、FT-IR和BET N2吸附法等手段表征了前驱体颗粒大小和分散性3确定最佳的前驱体制备工艺,对前驱体进行煅烧制得Al2O3/GdAlO3复合陶瓷粉体.结果表明,前驱体粒径和分散性受制备工艺影响较大;特别是,最佳工艺制备的前驱体平均粒径20 nm,分散性良好,形貌多呈球形;1250℃煅烧后得到的Al2O3/GdAlO3共晶陶瓷粉体的晶化良好、成分均匀,粉体粒径100～200 nm.     

乙醇溶液中电沉积CuInSe2(CIS)薄膜过程研究

采用三电极体系,以钼片为工作电极,大面积铂网为辅助电极,饱和甘汞电极(SCE)为参比电极,以氯化铜、氯化铟、亚硒酸为原料,在无水乙醇溶液中,用阴极恒流和恒压两种沉积方法制备出CIS前驱体薄膜,采用XRD和EDAX对制备的薄膜进行了表征,分析了沉积方式、镀液离子浓度、导电盐(LiCl)含量及热处理工艺等因素对薄膜成分及形貌的影响,并对电沉积CIS薄膜的机理进行了初步探讨.在最优条件下所制备的薄膜成分接近标准比且表面致密、均匀.     

电沉积二氧化钛功能薄膜的制备与组织转变研究

采用直流电沉积方法,在石墨板上成功制备了半导体二氧化钛功能薄膜前驱体,分析讨论了电沉积过程中实验参数对TiO2前驱体成膜的影响,获得了制备二氧化钛膜最佳工艺参数.TiO2前驱体沉积速率随着电流密度的增大而增加,为了保证薄膜质量,将电流密度控制在5～45mA/cm2之间;溶液浓度对沉积速率也有影响,当溶液中TiCl4:H2O2=1:2时沉积速率最大;最佳沉积温度为5-10℃.运用差热分析、XRD相结构分析和SEM等手段,研究了该前驱体到锐钛矿相(anatase)和金红石相(rutile)二氧化钛的组织相转变过程,300℃热处理得到锐钛矿相的二氧化钛,650℃热处理后出现金红石相.     

MOCVD growth of GaN on Si(1 1 1) substrates using an ALD-grown Al2O3 interlayer

GaN thin films have been grown on Si(1 1 1) substrates using an atomic layer deposition (ALD)-grown Al₂O₃ interlayer. This thin Al₂O₃ layer reduces strain in the subsequent GaN layer, leading to lower defect densities and improved material quality compared to GaN thin films grown by the same process on bare Si. XRD ω-scans showed a full width at half maximum (FWHM) of 549 arcsec for GaN grown on bare Si and a FWHM as low as 378 arcsec for GaN grown on Si using the ALD-grown Al₂O₃ interlayer. Raman spectroscopy was used to study the strain in these films in more detail, with the shift of the E₂(high) mode showing a clear dependence of strain on Al₂O₃ interlayer thickness. This dependence of strain on Al₂O₃ thickness was also observed via the redshift of the near bandedge emission in room temperature photoluminescence (RT-PL) spectroscopy. The reduction in strain results in a significant reduction in both crack density and screw dislocation density compared to similar films grown on bare Si. Screw dislocation density of the films grown on Al₂O₃/Si substrates approaches that of typical GaN layers on sapphire. This work shows great promise for the use of oxide interlayers for growth of GaN-based LEDs on Si.     

乙酰丙酮对PMMA负载锐钛矿型TiO2薄膜及其光催化性能影响

以钛酸丁酯作为钛源,水为溶剂,乙酰丙酮(AcAcH)为表面修饰剂,采用微波水热辅助溶胶-凝胶法制备了纳米晶二氧化钛水溶液,利用提拉镀膜法在聚合物聚甲基丙烯酸甲酯(PMMA)基板上沉积得到了透明TiO2纳米晶薄膜.通过X射线衍射(XRD)、红外光谱(FTIR)、透射电子显微镜(TEM)、原子力显微镜(AFM)和紫外-可见光吸收光谱(UV-Vis)等对TiO2纳米颗粒和薄膜的晶相组成、表面形貌及光学性能进行表征.同时通过紫外光光催化降解罗丹明B研究了TiO2薄膜的光催化性能.结果表明:通过引入乙酰丙酮,可以得到高度分散、晶相为锐钛矿型的TiO2水溶胶,在PMMA基板上沉积得到的薄膜表面平整、致密,具有良好的透光率,经过180 min紫外光照射,对罗丹明B的降解率达到90;以上.     

Crystallization of bismuth titanate and bismuth silicate grown as thin films by atomic layer deposition

Bismuth silicate and bismuth titanate thin films were deposited by atomic layer deposition (ALD). A novel approach with pulsing of two Bi-precursors was studied to control the Si/Bi atomic ratio in bismuth silicate thin films. The crystallization of compounds formed in the Bi₂O₃–SiO₂ and Bi₂O₃–TiO₂ systems was investigated. Control of the stoichiometry of Bi–Si–O thin films was studied when deposited on Si(1 0 0) and crystallization was studied for films on sapphire and MgO-, ZrO₂- and YSZ-buffered Si(1 0 0). The Bi–Ti–O thin films were deposited on Si(1 0 0) substrate. Both Bi–Si–O and Bi–Ti–O thin films were amorphous after deposition. Highly a-axis oriented Bi₂SiO₅ thin films were obtained when the Bi–Si–O thin films deposited on MgO-buffered Si(1 0 0) were annealed at 800 °C in nitrogen. The full-width half-maximum values for 200 peak were also studied. An excess of bismuth was found to improve the crystallization of Bi–Ti–O thin films and the best crystallinity was observed with Ti/Bi atomic ratio of 0.28 for films annealed at nitrogen at 1000 °C. Roughness of the thin films as well as the concentration depth distribution were also examined.     

低温热处理温度对SiC衬底上CuAlO2薄膜特性的影响

为了解决双极型碳化硅(SiC)功率器件中由于p型SiC在室温下难以完全电离所导致的p+n发射结注入效率低的问题,提出将p型CuAlO₂与n型SiC形成的异质结作为发射结以提高该结的注入效率。本文利用溶胶凝胶(sol-gel)方法,在4H-SiC衬底上制备了CuAlO₂薄膜,研究了低温热处理温度对CuAlO₂薄膜晶体结构、表面形貌、光学特性的影响。结果表明:较高的热处理温度可以促进中间产物CuO的生成,进而在固相反应阶段促进CuAlO₂相的产生,最终制备的CuAlO₂薄膜主要以CuAlO₂相的(012)晶向择优取向。随着低温热处理温度的升高,薄膜的表面均匀致密,空位缺陷含量降低,结晶质量提高。当低温热处理温度为300 ℃时,CuAlO₂薄膜晶粒尺寸约为35 nm。此外,CuAlO₂薄膜在可见光范围内的透过率超过70%,且随着预处理温度升高,薄膜光学带隙略有增加。     

电沉积法制备Bi2S3薄膜研究

采用阴极恒电压法在ITO导电玻璃表面沉积了Bi2S3薄膜,利用X射线衍射(XRD)、原子力显微镜(AFM)对制备的薄膜进行了表征.研究了pH值、沉积时间、沉积液浓度等工艺因素对薄膜的影响.结果表明:电沉积制备Bi2S3薄膜的过程中,合适的Bi3+与S2O32-的浓度水平是至关重要的;在电沉积溶液pH=6.5,沉积时间为20 min,沉积电压为1 V,加入柠檬酸三钠作络合剂的情况下,得到沿(240)晶面生长良好的Bi2S3薄膜,薄膜组成均匀致密;增加沉积溶液pH值,薄膜的结晶程度逐渐提高,红外透过比提高.     

Gadolinium nitride films deposited using a PEALD based process

Gadolinium nitride films have been deposited on Si(100) using a plasma-enhanced ALD (PEALD) based process. The deposition was carried out using tris(methylcyclopentadienyl)gadolinium {Gd(MeCp)₃} and remote nitrogen plasma, separated by argon pulses. Films were deposited at temperatures between 150 and 300 °C and capped with tantalum nitride to prevent post-deposition oxidation. Film composition was initially assessed using EDX and selected samples were subsequently depth profiled using medium energy ion scattering (MEIS) or AES. X-ray diffraction appears to show that the films are effectively amorphous. Films deposited at 200 °C were found to have a Gd:N ratio close to 1:1 and a low oxygen incorporation (～5%). Although the growth was affected by partial thermal decomposition of the Gd(MeCp)₃, it was still possible to obtain smooth (Ra.=～0.7 nm) films with good thickness uniformity (97%). Less successful attempts to deposit gadolinium nitride using thermal ALD with ammonia or mono-methyl-hydrazine are also reported.     

铜锌锡硫正极全固态薄膜锂离子电池的研究

采用铜锌锡硫(CZTS)四元硫化物材料作为全固态薄膜锂离子电池(TFLB)的正极功能层.通过磁控溅射及硫化工艺制备了CZTS多晶薄膜,并经过组分调控及硫化工艺控制等方案,提高了CZTS正极薄膜的电子导电性.此外,通过引入疏松的微观结构,抑制了由充放电过程中的体积膨胀所导致的容量衰减,提升了TFLB循环性能.所制得的TFLB结构为玻璃/Mo/CZTS/LiPON/Li,首圈放电容量高达200μAh·cm-2 ·μm-1(482 mAh ·g-1),放电平台约为1.1V.     

pH值对电沉积PbS薄膜结构和性能的影响

采用阴极恒电压法在ITO导电玻璃表面沉积了PbS薄膜,并用X射线衍射仪(XRD)、原子力显微镜(AFM)以及傅立叶变换红外光谱仪(FT-IR)对薄膜的结构和光学性能进行了表征,研究了沉积液pH值对薄膜的相组成、显微形貌以及光学性质的影响.结果表明:在U=3 V,pH=2.4,沉积时间为20 min,加入EDTA作络合剂的情况下,可制备出沿(111)和(200)晶面取向生长的立方相PbS薄膜.薄膜均匀而致密,随pH值增加,薄膜的压应力及禁带宽度呈现先减小后增大的变化趋势.所制备的微晶PbS薄膜的禁带宽度约为0.38～0.39 eV.     

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.     

XPS and electroluminescence studies on SrS1−xSex and ZnS1−xSex thin films deposited by atomic layer deposition technique

SrS_1−xSe_x and ZnS_1−xSe_x thin films were deposited by the atomic layer deposition (ALD) technique using elemental selenium as the Se source, thus avoiding use of H₂Se or organometallic selenium compounds. X-ray diffraction (XRD) analysis showed that the films were solid solutions and X-ray photoelectron spectroscopy (XPS) data showed that the surface of both ZnS_1−xSe_x and SrS_1−xSe_x were covered with an oxide and carbon-containing contaminants from exposure to air. The oxidation of SrS_1−xSe_x extended into the film and peak shifts from sulfate were found on the surface. Luminance measurements showed that emission intensity of the ZnS_1−xSe_x:Mn alternating current thin film electroluminescent (ACTFEL) devices at fixed voltage was almost the same as that of the ZnS:Mn device, while emission intensity of the SrS_1−xSe_x:Ce devices decreased markedly as compared to the SrS:Ce device. Emission colors of the devices were altered only slightly due to selenium addition.