氮氢混合气氛对SrBi2Ta2O9铁电薄膜和粉末性能的影响

用金属有机物分解法分别制备了SrBi₂Ta₂O₉（SBT）薄膜和粉末样品. XRD和SEM结果显示SBT粉末经历氮氢混合气氛400℃退火处理后发生了还原反应,金属Bi和δ-Bi₂O₃析出,成针状结构聚集在表面,晶体结构没有被破坏. SBT薄膜在500℃退火处理时,表面出现Bi的球形及针状结构聚集体,相对于薄膜结构,SBT粉末中的Bi元素在较低温度时更容易被还原. Bi的大量缺失严重影响薄膜的铁电性能,当退火时间为5.5min时,SBT薄膜剩余极化强度Pr下降了约43%,但是在109极化反转后仍然保持了良好的抗疲劳特性;退火时间超过8.5min时,薄膜被击穿,铁电性能消失.     

LiTa3O8薄膜制备与电性能研究

以乙醇锂和乙醇钽为起始反应物, 用溶胶-凝胶法在Pt/Ti/SiO₂/Si衬底上制备了新型钽酸锂LiTa₃O₈铁电薄膜. 经XRD图谱对比, 该薄膜结构不同于LiTaO₃晶体结构, 与正交相结构类似. SEM分析显示经过750℃结晶退火的LiTa₃O₈薄膜表面均匀平整无裂纹, 膜厚约为1μm. 实验结果表明, 在450kV/cm时, LiTa₃O₈薄膜剩余极化强度P_r为9.3μC/cm², 矫顽场强E_c为126.8kV/cm; 在9.5kV/cm时, LiTa₃O₈薄膜漏电电流为8.85×10^-9A/cm², 比LiTaO₃薄膜漏电小; 在1kHz时, LiTa₃O₈薄膜介电常数为58.4, 介电损耗为0.26. 溶胶-凝胶法制备的 LiTa₃O₈薄膜结晶温度比LiTaO₃薄膜高50℃以上.     

退火温度对Pt/SrBi2Ta2O9/Bi4Ti3O12/p-Si异质结微观结构与性能的影响

采用sol-gel工艺制备了Pt/SrBi₂Ta₂O₉/Bi₄Ti₃O₁₂/p-Si异质结. 研究了退火温度对异质结微观结构与生长行为、漏电流密度和C-V特性等的影响. 研究表明: 成膜温度较低时,SrBi₂Ta₂O₉、Bi₄Ti₃O₁₂均为多晶薄膜, 但随退火温度升高, Bi₄Ti₃O₁₂薄膜沿c轴择优生长的趋势增强; 经不同退火温度处理的Pt/SrBi₂Ta₂O₉/Bi₄Ti₃O₁₂/p-Si异质结的C-V曲线均呈现顺时针非对称回滞特性, 且回滞窗口随退火温度升高而增大, 经700℃退火处理后异质结的最大回滞窗口达0.78V; 在550～700℃范围内, Pt/SrBi₂Ta₂O₉/Bi₄Ti₃O₁₂/\\p-Si异质结的漏电流密度先是随退火温度升高缓慢下降, 当退火温度超过650℃后漏电流密度明显增大, 经650℃退火处理的异质结的漏电流密度可达2.54×10^-7A/cm²的最低值.     

快速退火工艺条件下温度对Bi4Ti3O12铁电薄膜微观结构与性能的影响

采用快速退火工艺在Pt/Ti/SiO2/p-Si衬底上制备了Bi4Ti3O12铁电薄膜.研究了退火温度对薄膜微观结构、铁电特性及介电性能的影响.研究表明:退火温度对Si基Bi4Ti3O12铁电薄膜晶相结构的影响显著,对晶粒尺寸和表面形貌的影响较小,但退火温度超过800℃后会出现焦绿石等杂相;低于750℃时,薄膜的剩余极化随退火温度升高而增大,高于750℃时却有所减小,但矫顽电场随退火温度升高而逐渐降低;退火温度对薄膜的漏电流密度有一定的影响,薄膜的漏电流密度在200kV/cm极化电场作用下低于3×10-9A/cm2,750℃时的剩余极化和矫顽电场分别为11μC/cm2和77kV/cm,具有较好的铁电和介电性能.     

金属Sn氧化薄膜的真空退火与原位XPS测量

本文研究了在真空退火过程中金属Sn氧化薄膜表面L元素Sn和O的化学性质．利用X射线光电子能谱（XPS）的表面分析方法,发现在金属Sn氧化薄膜的表面上存在大量的吸附氧粒子（O^-和O^-_2）提高真空退火温度,吸附氧粒子的数量增加;同时吸附氧粒子的负电性变弱．当退火温度低于350℃时,吸附氧粒子数量的增加是起因于SnO₂→Sn₂O₃的转变;在这种情况下,可以观察到Sn2O3是相对稳定的金属Sn氧化物,继续提高退火温度,达到400℃时,Sn在金属Sn中的相对含量急剧增大,Sn在金属Sn中相对含量增加的原因与金属Sn的价态Sn³⁺→Sn⁰的转变相关在这个转变过程中伴随着O的释放和薄膜表面氧粒子的进一步堆积．与温度低于350℃时的退火条件相比,XPS的测量也发现,在400℃的退火温度下;SnO₂相对于Sn₂O₃反而成为比较稳定的金属Sn氧化物．还讨论了金属Sn氧化薄膜表面上吸附氧粒子的吸附状态以及吸附状态与退火温度的关系．     

金属有机物分解法制备SrBi2Ta2O9铁电薄膜的开关特性

用金属有机物分解（MOD）以及sol-gel方法制备了SiBi2Ta2O9（STB）铁电薄膜。经测量在750℃晶化的SBT薄膜具有很好的铁电性能。通过对SBT样品极化反转过程进行测试,得出了外加电压（0．5－5V）与SBT薄膜的开关时间（100－600ms）及极化反转电荷的关系。并研究了不同气氛不退火对SBT铁电薄膜形状特性的影响。     

Sol-gel法制备Pb(Zr0.53Ti0.47)O3铁电薄膜

利用Sol-gel工艺在Pt/Ti/SiO2/Si衬底上制备了Pb(Zr0.53Ti0.47)O3(PZT)薄膜,研究了退火温度、保温时间和薄膜厚度对其晶相、微观结构和铁电性能的影响.在500℃退火处理的PZT薄膜开始形成钙钛矿相;在550℃退火处理的PZT薄膜基本形成钙钛矿相结构;升高退火温度(500～850℃)、延长保温时间(30～150min)、增加薄膜厚度(120～630nm)都有利于PZT晶粒的长大.在650～750℃退火的PZT薄膜具有较好的铁电性能,保温时间对PZT薄膜的铁电性能影响不大,PZT薄膜的厚度为200～300nm时可以得到比较好的铁电性能.在退火温度750℃、保温时间30min条件下退火处理厚310nm的PZT薄膜,其剩余极化值(2Pr)和矫顽电场(2Ec)分别是72μC/cm2、158kV/cm.     

高能球磨制备立方AlN及其高温相变

研究了高能球磨过程中Al₂O₃的相变, 随着球磨时间的延长, 粉末中发生了γ -Al₂O₃向α -Al₂O₃3的转变. 高能球磨20h, Al₂O₃部分非晶化, 同时, 有立方AlN生成. 增加球磨强度, 立方AlN生成量增加, 650r/min高能球磨40h, AlN生成量达到72%. 随后的氮气气氛退火实验发现, 在500℃以上, 立方氮化铝与氧化铝反应, 生成AlON相. AlON相的生成, 有效地降低了碳热还原氮化反应激活能.     

热分解气氛对溶胶-凝胶法制备BLT铁电薄膜性能的影响

研究了热分解气氛对溶胶-凝胶法制备在Pt/Ti/SiO2/Si衬底上的Bi3.25La0.75Ti3O12 (BLT)薄膜铁电性能的影响.在400℃时空气或氧气气氛下热分解20min,接着在700℃时氧气气氛下退火30min.氧气气氛下的热分解能充分分解掉薄膜中的有机成分,而空气气氛下的热分解使炭、氢有机成分部分残留在薄膜中.有机成分的不完全分解影响了退火过程中BLT薄膜晶化时晶粒的生长.表现出生长取向和晶粒尺寸对BLT薄膜铁电性能的影响.氧气和空气气氛下热分解的薄膜的剩余极化(Pr)和矫顽电场(Ec)分别为18.85μC/cm2,119.7kV/cm和12.56μC/cm2、112.5kV/cm.氧气气氛下热分解的薄膜的剩余极化值显著提高.所以热分解是控制铁电性能的重要步骤.     

不同退火方式对0.7BiFeO3-0.3PbTiO3薄膜的铁电性能及漏电流的影响

利用溶胶凝胶法在LaNiO3/SiO2/Si衬底上制备了0.7BiFeO3-0.3PbTiO3(BFPT7030)薄膜,研究了快速退火及常规退火两种不同的后续退火处理方式对薄膜铁电性能及漏电流性能的影响.XRD测试表明,经快速退火处理的BFPT7030薄膜结晶完好,呈现出单一的钙钛矿相.SEM测试结果显示,经快速退火处理的BFPT7030薄膜结晶充分,但经常规退火处理的BFPT7030薄膜表面致密性较好,且在升温速率为2℃/min时薄膜的晶粒更细小.经快速退火处理的BFPT7030薄膜的铁电性能较为优异,在升温速率为20℃/s时,其剩余极化Pr为22μC/cm2,矫顽场Ec为70 kV/cm,并具有较小的漏电流.XPS测试结果表明,经常规退火处理的BFPT7030薄膜其铁离子的价态波动较小.     

微晶玻璃的制备与光谱特性

高温熔制摩尔组分为32CaO-12Y₂O₃-24Al₂O₃-31SiO₂-1Yb₂O₃的玻璃, 制得的玻璃于950、1050、1100℃三个不同温度进行热处理, 用XRD分析热处理后样品的相变, 用TEM观察1050℃热处理后的样品, 并研究了1050℃热处理前后样品的光谱特性. 研究结果表明: 玻璃在1050℃热处理后, 在玻璃中产生单一YAG相微晶颗粒; 热处理前后样品光谱特性的变化表明热处理后掺杂的Yb ³⁺离子择优进入到YAG晶格位, 制备得到了透明Yb:YAG微晶玻璃.     

Synthesis and ferroelectric properties of SrBi2Ta2O9/Bi4Ti3O12/p-Si multilayer thin films by Sol-Gel

SrBi₂Ta₂O₉(SBT)/Bi₄Ti₃O₁₂(BIT) multilayer thin films were prepared on p-Si substrates by Sol-Gel method, the effect of thickness of SBT and annealing temperature on structure, morphology, ferroelectric and fatigue properties of SBT/BIT ferroelectric films were investigated. The SBT/BIT multilayer films annealed at above 600 ^∘C were uniform and crack free as well as exhibited no pyrochlore phase. The remanent polarization and the coercive field of SBT/BIT multilayer films both increases with the increase of annealing temperature due to better crystallization and larger grain size. The SBT/BIT multilayer thin films consisting of 1 layer of SBT and 3 layers of BIT annealed above 650 ^∘C obtained its best ferroelectric properties with a P_r of 8.1 μC/cm² and a E_c of 130 kV/cm which is comparable to that of pure BIT films and had a fatigue-free property up to 10¹¹ switching cycles, but P_nv appeared under the cycle field of 175 kV/cm and increased with the decrease of cycle field.     

Microstructure Characterization of Sol-gel Prepared MoO3-TiO2 Thin Films for Oxygen Gas Sensors

Binary metal oxide MoO3-TiO2 films have been prepared using the sol-gel technique. The thin films were annealed at several temperatures including 400℃,450℃,500℃,550℃ and 600℃ for lhour. The morphology, crystalline structure and chemical composition of the films have been analysed using SEM,XRD,RBS and XPS techniques. The SEM analysis showed that the films annealed at 450℃ are mainly smooth and uniform with 20-100nm-sized grains and with few particles as large as a micrometre or more. The XRD analysis revealed that the films annealed at 400℃ were a mixture of orthorhombic and hexagonal MoO3phases. The films annealed at 450℃ increased in hexagonal phase. The preferential orientation growth along(100) plane of the hexagonal phase and (010) plane of the orthorhombic phase has been found in both samples. RBS and XPS analysis showed that the films were stoichiometric. When the annealing temperature is increased to more than 500℃, the concentration ratio of MoO3 to TiO2 decreased due to the evaporation of MoO3. For the study of the electrical and gas sensing properties, films were deposited on sapphire substrates with interdigital electrodes on the front-side and a Pt heater on the backside. The O2 gas sensing properties of MoO3-TiO2 thin films are discussed.     

Fabrication of robust Bi3.25La0.75Ti3O12 thin film resistant to hydrogen damage

Ferroelectric bismuth lanthanum titanate (Bi_3.25La_0.75Ti₃O₁₂; BLT) thin films were deposited on Pt/TiO₂/SiO₂/Si substrate by chemical solution deposition method. The films were crystallized in the temperature range of 600–700 °C. The spontaneous polarization (P_s) and the switching polarization (2P_r) of BLT film annealed at 700 °C for 30 min were 22.6 μC/cm² and 29.1 μC/cm², respectively. Moreover, the BLT capacitor did not show any significant reduction of hysteresis for 90 min at 300 °C in the forming gas atmosphere.     

Reactions in Au/Nb bilayer thin films

The interdiffusion and intermetallic compound formation of Au/Nb bilayer thin films annealed at 200–400 °C have been investigated. The bilayer thin films were prepared by electron beam deposition. The Nb film was 50 nm thick and the Au film was 50–200 nm thick. The interdiffusion of annealed specimens was examined by measuring the electrical resistance and depth-composition profile and by transmission electron microscopy. Interdiffusion between the thin films was detected at temperatures above 325 °C in a vacuum of 10^-4 Pa. The intermetallic compound Au₂Nb₃ and other unknown phases form during annealing at over 400 °C. The apparent diffusion constants, determined from the penetration depth for annealing at 350 °C, are 3.5 × 10⁻¹⁵ m² s⁻¹ for Nb in Au and 8.6 × 110^7minus;15 m² s⁻¹ for Au in Nb. The Au surface of the bilayer films becomes uneven after annealing at over 400 °C due to the reaction.     

Fabrication and characterization of (1−x)SrBi2Ta2O9–xBi3TaTiO9 layered structure solid solution thin films for ferroelectric random access memory (FRAM) applications

We report on the properties of (1−x)SrBi₂Ta₂O₉–xBi₃TaTiO₉ solid solution thin films for ferroelectric non-volatile memory applications. The solid solution thin films fabricated by modified metalorganic solution deposition technique showed much improved properties compared to SrBi₂Ta₂O₉. A pyrochlore free crystalline phase was obtained at a low annealing temperature of 600°C and grain size was found to be considerably increased for the solid solution compositions. The film properties were found to be strongly dependent on the composition and annealing temperatures. The measured dielectric constant of the solid solution thin films was in the range 180–225 for films with 10–50% of Bi₃TaTiO₉ content in the solid solution. Ferroelectric properties of (1−x)SrBi₂Ta₂O₉–xBi₃TaTiO₉ thin films were significantly improved compared to SrBi₂Ta₂O₉. For example, the observed remanent polarization (2P_r) and coercive field (E_c) values for films with 0.7SrBi₂Ta₂O₉–0.3Bi₃TaTiO₉ composition, annealed at 650°C, were 12.4 μC/cm² and 80 kV/cm, respectively. The solid solution thin films showed less than 5% decay of the polarization charge after 10¹⁰ switching cycles and good memory retention characteristics after about 10⁶ s of memory retention. The improved microstructural and ferroelectric properties of (1−x)SrBi₂Ta₂O₉–xBi₃TaTiO₉ thin films compared to SrBi₂Ta₂O₉, especially at lower annealing temperatures, suggest their suitability for high density FRAM applications.     

Crystallization and electrical characteristics of 0.95 (Na0.5Bi0.5)TiO3-0.05 BaTiO3 thin films under different annealing temperature and atmosphere

0.95 (Na0.5Bi0.5)TiO3-0.05 BaTiO3 +1 wt% Bi2O3 (NBT-BT3) ceramic is used as target to deposit the NBT-BT3 thin films. The excess 1wt% Bi2O3 is used to compensate the vaporization of Bi2O3 during the sintering and annealing processes. NBT-BT3 thin films are successfully deposited using radio frequency (RF) magnetron sputter method and crystallized subsequently using a conventional furnace annealing (CFA) process. The annealed process is conducted in air and in oxygen atmosphere at temperatures ranging from 600-800 degrees C for 60 min. As compared with the as-deposited NBT-BT3 thin films, the CFA-treated process has improved the grain growth and crystallization. We will show that the annealing atmosphere is the more important parameter to influence the grain growth and crystallization of NBT-BT3 thin films than the annealing temperature. The influences of CFA-treated temperature and atmosphere on the electrical characteristics of NBT-BT3 thin films, including the polarization characteristics (Pr, Ps, and Ec values), the capacitance-voltage (C-V) curves, and the leakage current density-electric field (J-E) curves, are also investigated in this study.     

N掺杂Cu2O薄膜的低温沉积及快速热退火研究

采用氧化亚铜(Cu_2O)陶瓷靶,利用射频磁控溅射沉积法在氮气和氩气的混合气氛下制备了N掺杂Cu_2O(Cu_2O∶N)薄膜,并在N_2气氛下对薄膜进行了快速热退火处理,研究了N_2流量和退火温度对Cu_2O∶N薄膜的生长行为、物相结构、表面形貌及光电性能的影响。结果显示,在衬底温度300℃、N_2流量12sccm条件下生长的薄膜为纯相Cu_2O薄膜;在N_2气氛下对预沉积薄膜进行快速热退火处理不影响薄膜的物相结构,薄膜的结晶质量随退火温度(450℃)的升高而显著改善;快速热退火处理能改善薄膜的结晶质量和缺陷,降低光生载流子的散射,增强载流子的传输,预沉积Cu_2O∶N薄膜经400℃退火处理后展示出较好的电性能,薄膜的霍尔迁移率(μ)为27.8cm~2·V~(-1)·s~(-1)、电阻率(ρ)为2.47×10~3Ω·cm。研究表明低温溅射沉积和快速热退火处理能有效改善Cu_2O∶N薄膜的光电性能。     

高能球磨Al-Y2O3粉体固相反应制备YAG陶瓷的研究

用高纯Al粉体和Y₂O₃粉体(Al-Y₂O₃粉体)为原料采用固相反应法制备了YAG陶瓷. Al-Y₂O₃粉体高能经过球磨, 煅烧生成YAG粉体, 再真空烧结制备高致密YAG陶瓷. 采用DTA-TG对球磨Al-Y₂O₃粉体进行分析, 采用XRD、SEM对球磨的Al-Y₂O₃粉体、YAG粉体及YAG陶瓷进行了表征. 实验表明: Al-Y₂O₃粉体在～569℃时, Al粉强烈氧化, 并与Y₂O₃粉反应, 600℃煅烧出现YAM相, 随煅烧温度升高出现YAP相, 1200℃煅烧生成YAG粉体. 成型YAG素坯在1750℃保温2h真空烧结出YAG相陶瓷, YAG陶瓷相对密度可达98.6%, 晶粒生长均匀, 晶粒尺寸为810μm.