双氧水对溶胶-凝胶法制备硅酸锆薄膜的影响

以氧氯化锆和正硅酸乙酯为锆源和硅源,采用溶胶-凝胶法制备硅酸锆薄膜.借助SEM、DTA-TG、FT-IR、XRD等分析测试手段研究了添加双氧水(H2O2)对制备硅酸锆薄膜的影响,并研究了薄膜的抗腐蚀性能.结果表明:适量的双氧水可以有效地促进氧氯化锆的水解,进而克服薄膜高温失重造成孔洞和致密性差的问题;当H2O2/Zr的摩尔比小于2时,制备的薄膜不致密、不均匀;当H2O2/Zr的摩尔比大于2时,制备的样品有杂质相;最优的H2O2/Zr摩尔比为2,可制得均匀、致密的硅酸锆薄膜;所制备的薄膜具有较好的抗NaOH溶液腐蚀性能,单晶硅基片腐蚀前后质量损失为16.92;,而镀有硅酸锆薄膜的单晶硅基片腐蚀前后质量损失仅为0.56;.     

锆钛酸铅薄膜的溶胶-凝胶制备工艺及结构与物性的研究

采用溶胶-凝胶匀胶法制备锆钛酸铅铁电薄膜,研究了前驱体影响因素(如有机溶剂、前驱单体加入顺序、添加剂)、溶胶影响因素(如溶胶浓度、pH值)、匀胶速度和退火温度对成膜质量及薄膜微结构、铁电性的影响.结果表明:采用乙二醇甲醚为溶剂对pb2+、Zr4+和Ti4+金属盐进行溶解优于乙醇和乙二醇,但由于乙二醇甲醚对硝酸锆的溶解性差,对硝酸锆应先用乙醇溶解再加入乙二醇甲醚的方法来进行溶解;以硝酸锆为Zr源配制溶胶时,只有先将Pb前驱液滴加到Ti前驱液中,然后再滴入Zr前驱液的方式才能得到澄清前驱体.将锆钛酸铅溶胶浓度和pH值分别控制在0.2～0.3 mol/L和2～3较为适宜,与此溶胶相适应的匀胶参数:转速为4000 r/min,时间为60 s.随退火温度升高,薄膜的晶化程度增加,且逐渐表现出(100)晶面择优取向,晶格常数c和四方率c/a逐渐增加,而晶格常数a逐渐减小;随退火温度升高,晶粒尺寸逐渐增大,使得剩余极化强度逐渐增加,矫顽场强逐渐减小.当退火温度为850 ℃时制备的锆钛酸铅薄膜具有均匀的晶粒、较低的表面粗糙度和最为优异的铁电性.     

单晶硅外延生长晶化硅薄膜的研究

采用P型单晶硅片为衬底,并经混合酸溶液腐蚀抛光、清洗后,利用射频磁控溅射镀膜系统在其表面制备非晶硅薄膜;再结合快速光热退火工艺,于N2气氛下480℃退火30 min,得到晶化硅薄膜;利用光学金相显微镜、XRD衍射仪和拉曼散射光谱(Raman)仪对单晶硅衬底和晶化硅薄膜进行结构和性能表征.研究了混合酸溶液对单晶硅表面腐蚀效果、籽晶诱导外延生长晶化硅薄膜的物相结构和薄膜带隙.结果表明:采用混合酸溶液腐蚀后得到表面平整、光滑的单晶硅衬底;非晶硅薄膜经过快速退火后受籽晶诱导生成晶化硅薄膜,其晶相沿单晶硅衬底取向择优生长;随着非晶硅薄膜厚度从80 nm增加到280 nm,晶化后硅薄膜的表面粗糙度逐渐减小,晶化率从90.0;逐渐降低到37.0;;晶粒尺寸从6.65 nm逐渐减小到1.71 nm;带隙从1.18 eV逐渐升高到1.52 eV.     

热丝CVD法沉积固态扩散源制备晶硅太阳电池p+/n+发射极研究

为进一步提高晶硅太阳能电池发射极的性能,本文提出了一种新的发射极制备技术-低温CVD法沉积固态薄膜扩散源并进行高温扩散.采用热丝化学气相沉积法(HWCVD)在单晶硅片上沉积重掺杂硅基薄膜作为固态扩散源,然后在空气氛围下的管式炉中进行高温扩散,最后用稀HF溶液去除表面的BSG/PSG.通过掺磷薄膜扩散在P型单晶硅片上制备了方阻在50～250 Ω/□范围内可控的n+型发射极;通过掺硼薄膜扩散在N型硅片上制备了方阻在150 ～600Ω/□□范围内可控的p+型发射极.并且通过在源气体中加入CO2作为氧源,实现了扩散后硅片表面残留扩散源层的彻底去除.     

非水解-溶胶凝胶法制备锆铁红色料影响因素的研究

以工业纯无水四氯化锆、正硅酸乙酯为前驱体,铁的无机盐为着色剂,氟化物为矿化剂,采用非水解溶胶-凝胶法低温制备了锆铁红色料.应用DTA-TG、XRD、色度仪和TEM研究了凝胶化工艺、矿化剂和铁源对锆铁红色料的影响.结果表明:回流结合容弹热处理工艺可以促进ZrSiO4晶体发育充分,有利于ZrSiO4对色料的包裹;由于铁源转变为氧化铁的温度与矿化剂条件下ZrSiO4的合成温度须相适应,当以UF为矿化剂时,ZrSiO4的合成温度降至650℃,FeCl3为适宜的着色剂;而以MgF2为矿化剂时,ZrSiO4的合成温度提高至850℃,FeSO4为适宜的着色剂.     

基于温和等离子体CVD的非晶硅薄膜的制备与钝化研究

采用容性放电模式(E-mode)的电感耦合等离子体化学气相沉积技术(ICPCVD),以硅烷( SiH4)和氢气(H2)作为气源,通过改变沉积气压来制备氢化非晶硅薄膜(a-Si:H).采用少子寿命测试仪(Sinton WCT-120)研究薄膜在n型单晶硅片表面的钝化效果.并通过傅里叶红外光谱仪(FTIR)和扫描电子显微镜(SEM)进一步表征薄膜的氢含量、微结构因子和表面形貌.结果表明,气压偏低或者偏高都会影响薄膜质量,生成多孔隙的薄膜,从而影响薄膜的钝化性能.最优沉积气压为65 Pa,并进一步优化少子寿命到445 μs,复合速度减小到48 cm/s,隐开路电压接近700 mV.     

LPCVD法在制绒单晶硅片衬底上制备ZnO∶B透明导电薄膜及其性能的研究

采用低压化学气相沉积法(LPCVD)在制绒的单晶硅片衬底上制备了B掺杂ZnO(BZO)的透明导电薄膜,研究了B2H6掺杂量、沉积时间对BZO薄膜的微观形貌、导电性能及光学减反性能的影响.结果表明,在制绒单晶硅片衬底上制备的BZO薄膜均呈现“类金字塔”的绒面结构,其平均晶粒尺寸在200 ～ 500 nm之间,并随B2H6掺杂量增加而减小;BZO薄膜的方阻随沉积时间的增加而呈线性迅速减小的趋势,当沉积时间为420 s时,BZO薄膜的方块电阻低至28 Ω/□;在制绒单晶硅片上制备BZO薄膜后,表面平均反射率由15;明显降低至5;左右,表现出优异的光学减反性能.     

磁控溅射技术室温生长氢化ZnO∶Ga薄膜及其特性研究

采用直流脉冲磁控溅射方法,在室温下生长氢化Ga掺杂ZnO薄膜(GZO/H),并通过湿法后腐蚀技术获得绒面结构.研究了室温下H2流量对薄膜结构、光电性能及表面形貌的影响.实验表明,氢化GZO(GZO/H)薄膜具有良好的(002)晶面择优取向生长,引入适当流量的H2可以有效提高薄膜的电学特性,GZO/H薄膜具有更低的电阻率以及较高的迁移率和载流子浓度.当通入H2流量为6 sccm时,薄膜电阻率为6.8 ×10-4 Ω·cm,Hall迁移率达34.2 cm2/Ⅴ·s,制备的GZO/H薄膜可见光区域平均透过率优于85;.此外,研究了H2流量对湿法腐蚀后绒面GZO/H薄膜表面形貌的影响,提出了一种薄膜绒面结构形成过程模型.     

稀HNO3对银纳米线薄膜电极光电性能影响的研究

本文以自制的银纳米线分散液为镀膜前驱体,利用不锈钢棒在聚对苯二甲酸乙二酯(PET)基底表面制备银纳米线薄膜电极,讨论HNO3溶液的浓度和处理时间对薄膜光电性能与表面形貌的影响.结果表明,当利用浓度为1:50(浓HNO3与蒸馏水体积比)的稀HNO3溶液处理薄膜30 min时,银纳米线薄膜的方块电阻可降低95;～97;,而薄膜的可见光透过率则提高3;～4;.     

Pr掺杂量对镨锆黄陶瓷颜料性能的影响

以氯氧化锆、正硅酸乙酯为主要原料,氧化镨作为着色剂,采用溶剂热法制备镨锆黄陶瓷颜料前驱体,经1050℃煅烧得到镨锆黄陶瓷颜料,考察镨掺杂量对该颜料呈色的影响.采用扫描电镜和X射线衍射仪对样品的显微结构进行分析,样品性能采用色度分析、粒度分析和紫外-可见光光谱分析仪测试.实验结果表明:相对于其它掺镨样品,当镨掺杂含量为0.15 g,样品的ZrSiO4结晶度较高且Pr4+固溶到ZrSiO4晶格中,颗粒尺寸分布较小且较均匀,使样品在400~480 nm对蓝紫光有非常强的吸收,样品呈现较纯正的黄色色调.     

Effect of metalloidal elements on corrosion resistance of amorphous iron-chromium alloys

Corrosion and electrochemical behaviours of amorphous iron-chromium alloys containing different sets of glass-forming metalloidal elements, boron, carbon, silicon and phosphorus, have been investigated. The corrosion resistance in 0.1N H₂SO₄ increases in the order of alloys containing silicon, boron, carbon and phosphorus, and the corrosion resistance in 3% NaCl increases in the order of alloys containing boron, silicon or carbon, and phosphorus. Difference in the corrosion resistance of amorphous alloys containing various metalloids has been interpreted in terms of the difference in the formation rate of the chromium-enriched protective film on the surface of alloys.     

XPS characterization of corrosion films formed on the crystalline, amorphous and nanocrystalline states of the alloy Ti60Ni40

X-ray photoelectron spectroscopy investigations were carried out on the crystalline, amorphous and nanocrystalline states of the alloy Ti₆₀Ni₄₀ after corrosion test in 1 M HNO₃ aqueous medium using potentiodynamic polarization method. Polarization plots revealed that the nanocrystalline state is more corrosion resistant than the amorphous and crystalline states of the alloy Ti₆₀Ni₄₀. The XPS characterization of the oxide film formed after corrosion tests revealed that a multiple phase oxide film is formed on the crystalline and amorphous specimens of the alloy Ti₆₀Ni₄₀ consisting of Ti²⁺, Ti³⁺ and Ti⁴⁺ species along with some unoxidized Ti in metallic form (Ti⁰) in the case of crystalline specimen whereas the oxide film formed on nanocrystalline specimen consists of only Ti²⁺ and Ti⁴⁺ species. The high corrosion resistance of nanocrystalline state is attributed to the presence of fewer oxide species in the oxide film than that of the amorphous and crystalline states of the alloy Ti₆₀Ni₄₀.     

Ca0.6Mg0.4Zr4(PO4)6涂层改善堇青石陶瓷

本文采用溶胶-凝胶法和浸渍涂覆技术在致密堇青石陶瓷表面制备了Ca0.6Mg0.4Zr4(PO4)6(C0.6M0.4ZP) 涂层,采用XRD、SEM等分析手段研究了涂层的相组成和微观结构,并通过分别测定涂覆和未涂覆涂层试样在1000℃下受腐蚀后的质量损失和强度变化,对涂层的耐碱腐蚀性能进行了表征.结果表明,在堇青石表面制备的涂层均匀致密,由单相的C0.6M0.4ZP组成.SEM分析表明涂层与堇青石基体间结合良好.C0.6M0.4ZP涂层具有较好的耐碱腐蚀性能,可显著提高堇青石陶瓷的高温耐碱腐蚀性能.     

Fabrication of nano-crystalline silicon thin film at low temperature by using a neutral beam deposition method

Low temperature (<80 °C) neutral beam deposition (LTNBD) was investigated as a new approach to the fabrication and development of nano-crystalline silicon (nc-Si), which has better properties than that of amorphous silicon (α-Si). The difference between LTNBD and conventional PECVD is that the film formation energy of the nc-Si in LTNBD is supplied by controlled neutral beam energies at a low temperature rather than by heating. Especially, in this study, the characteristics of the nc-Si thin film were investigated by adding 10% of an inert gas such as Ne, Ar or Xe to SiH₄/H₂. Increasing the beam energy resulted in an increase in the deposition rate, but the crystallinity was decreased, due to the increased damage to the substrate. However, the addition of a higher mass inert gas to the gas mixture at a fixed beam energy resulted not only in a higher deposition rate but also in a higher crystallization volume fraction. The high resolution transmission electron microscopy image showed that the grown film is composed of about 10 nm-size grains.     

溶胶-凝胶法制备紫外及蓝光双截止润眼镀膜玻璃

采用溶胶-凝胶法,在3 mm厚的普白玻璃含锡面镀制镶嵌Ag纳米粒子的氧化硅薄膜,达到吸收蓝光的效果,在其非锡面镀制纤锌矿结构的氧化锌薄膜,达到阻隔紫外效果.通过双膜层的相互作用,达到对紫外和短波蓝光有效阻隔吸收,从而获得具有紫外蓝光防护及润眼功能的镀膜玻璃.研究了热处理温度和膜层厚度对近紫外和蓝光阻隔率的影响.结果表明:随着退火温度的升高,膜层更加致密,且退火温度越高,蓝光的吸收率也逐渐提高,吸收峰位红移.利用浮法玻璃本体的富锡表面还原AgNO3成Ag纳米粒子分散镶嵌在氧化硅薄膜的结构,能有效吸收380～450 nm的短波蓝光.实验样品呈现出美观的淡金黄色,且随着膜厚的增大,金黄色程度逐渐加深.以样品a为例,所制备的氧化锌膜层为稳定的纤锌矿结构,膜厚为438 nm,表面为球状颗粒,对380 nm以下的紫外光阻隔率为98.83;;所制备氧化硅薄膜厚为200 nm,表面致密,对380～450 nm的蓝光阻隔率为90.73;,样品整体450～780 nm可见光透过率为77.8;.     

Analysis of IBAD silicon oxynitride film for anti-reflection coating application

A SOI-based optoelectronic device needs a high-quality anti-reflection coating on both faces of the device to minimize the optical reflectance from the face. In this work amorphous silicon oxynitride films were deposited on silicon substrates by ion beam assisted deposition (IBAD). The main purpose was to use silicon oxynitride film as single layer anti-reflection coating for SOI-based optoelectronic devices. This application is primarily based on the ability to tune the silicon oxynitride optical functions to the values optimal by changing deposition parameters. The chemical information was measured by X-ray photoelectron spectroscopy (XPS). Spectroscopic ellipsometry (SE) was applied to measure the refractive index and thickness. Single-side polished silicon substrate that was coated with silicon oxynitride film exhibited low reflectance. Double-side polished silicon substrate that was coated with silicon oxynitride film exhibited high transmittance. The results suggested silicon oxynitride film was a very attractive single layer anti-reflection coating for SOI-based optoelectronic device.     

甲烷浓度对碳化硅基底金刚石薄膜摩擦性能影响

利用热丝化学气相沉积法(HFCVD)在碳化硅基底上制备金刚石薄膜,采用场发射扫描电子显微镜、拉曼光谱仪、原子力显微镜研究了在不同甲烷浓度条件下制备的金刚石薄膜表面形貌及物相组成,在干摩擦条件下通过往复式摩擦磨损实验测试并计算了已制备金刚石薄膜的摩擦系数和磨损率,结合物相分析及摩擦磨损实验结果分析了甲烷浓度的改变对金刚石薄膜摩擦磨损性能的影响。结果表明,由于甲烷气体含量的升高,金刚石薄膜结晶质量下降,薄膜由微米晶向纳米晶转变。摩擦磨损实验结果显示:3%甲烷浓度条件下制备的金刚石薄膜耐磨性较好,磨损率为2.2×10^-7 mm³/mN;5%甲烷浓度条件下制备的金刚石薄膜摩擦系数最低(0.032),磨损率为5.7×10^-7 mm³/mN,制备的金刚石薄膜的耐磨损性能相比于碳化硅基底(磨损率为9.89×10^-5 mm³/mN)提升了两个数量级,显著提高了碳化硅基底的耐磨性。     

PECVD法制备不同衬底微晶硅薄膜的研究

采用等离子体增强化学气相沉积(PECVD)法分别在玻璃衬底和p型薄膜硅衬底上制备了微晶硅薄膜。使用拉曼谱仪、紫外-可见分光光度计、傅里叶红外光谱仪等对微晶硅薄膜进行检测,重点研究了硅烷浓度、衬底温度对薄膜沉积速率和晶化率的影响。实验结果表明:两种衬底上薄膜的沉积速率均随硅烷浓度的增大、衬底温度的升高而变大。硅烷浓度对两种衬底的薄膜晶化率影响规律相同,即均随其升高而降低;但两种衬底的衬底温度影响规律存在差别:对玻璃衬底而言,温度升高,样品晶化率减小;而p型薄膜硅衬底则在温度升高时,样品晶化率先增大后减小。此外还发现,晶化率与薄膜光学性能及含氧量存在较密切关联。