Growth and characterization of MOMBE grown HfO2

HfO₂ dielectric layers were grown directly on the p-type Si (1 0 0) by metalorganic molecular beam epitaxy (MOMBE). Hafnium tetra-butoxide was used as a Hf precursor and pure oxygen was introduced to form an oxide layer. The properties of the layers with different thicknesses were evaluated by X-ray diffraction (XRD), X-ray photoelectron spectroscopy (XPS), high-resolution transmission electron microscopy (HRTEM), and capacitance–voltage (C–V) and current–voltage (I–V) analyses. XRD and HRTEM results showed that the HfO₂ films thinner than 12 nm were amorphous while the films thicker than 12 nm began to crystallize in the tetragonal and the monoclinic phases. The XPS spectra of O 1s show that the O---Si binding energies shifted to the lower binding energy with increasing the HfO₂ layer thickness. Moreover, the snap back phenomenon is observed in accumulation capacitance. These changes are believed to be linked with the decomposition of SiO and the crystallization of HfO₂ layer during the film growth.     

退火对EBE,IBS和ALD沉积HfO2薄膜的抗激光损伤性能影响

结合自身实验条件采用电子束蒸发(EBE)、离子束溅射(IBS)和原子层沉积(ALD)三种工艺制备了HfO2薄膜,对其进行退火实验,采用1064 nm Nd:YAG激光测定了即时沉积和退火后各HfO2薄膜的抗激光损伤能力。研究发现,ALD HfO2薄膜的激光损伤阈值最高,EBE HfO2薄膜次之,IBS HfO2薄膜的损伤阈值最低;300℃退火对各工艺薄膜抗激光损伤能力的影响均为负面,500℃退火则会显著降低ALD HfO2薄膜的抗激光损伤能力。     

溶胶凝胶法制备以HfO2为绝缘层和ZITO为有源层的高迁移率薄膜晶体管

采用溶胶凝胶法制备了h-k氧化铪HfO₂薄膜, 经500℃退火后, 获得了高透过率、表面光滑、低漏电流和相对高介电常数的HfO₂薄膜. 并采用氧化铪作为绝缘层和锌铟锡氧化物作为有源层成功地制备了底栅顶接触结构薄膜晶体管器件. 获得的薄膜晶体管器件的饱和迁移率大于100 cm²·V^-1·s^-1, 阈值电压为-0.5 V, 开关比为5×10⁶, 亚阈值摆幅为105 mV/decade. 表明采用溶胶凝胶制备的薄膜晶体管具备高的迁移率, 其迁移率接近低温多晶硅薄膜晶体管的迁移率.     

硼膜制备工艺、微观结构及其在硼化镁超导约瑟夫森结中的应用

MgB_2材料具备临界转变温度较高、相干长度大、临界电流和临界磁场高等优点,被认为有替代Nb基超导材料的潜力.研究了不同温度下以化学气相沉积法制备的硼(B)薄膜的微观结构.实验结果表明:较低温度沉积的B先驱薄膜为无定形B膜,可以与Mg蒸气反应生成MgB_2超导薄膜;当沉积温度高于550?C时,所得硼薄膜为晶型薄膜;以晶型硼薄膜为先驱膜在镁蒸气中退火,不能生成硼化镁超导薄膜.利用晶型B膜的这一特点,成功制备了以晶型硼薄膜为介质层的硼化镁超导约瑟夫森结.     

高压退火对0.65PMN-0.35PT薄膜结构、形貌及电学性能的影响

利用射频磁控溅射技术在LaNiO₃/SiO₂/Si(100)基底上制备了厚 度约为250 nm的0.65PMN-0.35PT(PMN-PT)薄膜. 研究高压氧氛围退火方式对PMN-PT薄膜晶体结构、形貌以及电学性能的影响. 经过XRD测试发现,在高压氧气氛围中, 温度为400℃下退火后的PMN-PT薄膜具有纯的钙钛矿相结构, 具有完全的(100)择优取向, 且衍射峰尖锐, 表明经过高压退火后的薄膜结晶极为充分. SEM表面形貌测试结果显示, 经高压退火处理的PMN-PT薄膜表面呈现出棒状或泡状的形貌. 铁电性能测试表明: 氧气氛围压强4 MPa, 退火时间4h的PMN-PT薄膜样品具有较好的铁电性能, 其剩余极化强度P_r达到10.544 μC/cm², 且电滞回线形状较好, 但漏电流较大, 这可能是由于其微结构所导致.同时介电测试发现: PMN-PT薄膜样品具有极好的介电性能, 其在1 kHz下测试的介电常数ε_r达到913, 介电损耗tgδ 较小, 仅为0.065. 关键词： 射频磁控溅射 高压退火 0.65PMN-0.35PT 介电     

Influences of annealing on structural and compositional properties of Al_2O_3 thin films grown on 4H–SiC by atomic layer deposition

Annealing effects on structural and compositional performances of Al_2O_3 thin films on 4H–Si C substrates are studied comprehensively. The Al_2O_3 films are grown by atomic layer deposition through using trimethylaluminum and H_2 O as precursors at 300?C, and annealed at various temperatures in ambient N_2 for 1 min. The Al_2O_3 film transits from amorphous phase to crystalline phase as annealing temperature increases from 750?C to 768?C. The refractive index increases with annealing temperature rising, which indicates that densification occurs during annealing. The densification and grain formation of the film upon annealing are due to crystallization which is relative with second-nearest-neighbor coordination variation according to the x-ray photoelectron spectroscopy(XPS). Although the binding energies of Al 2p and O 1s increase together during crystallization, separations between Al 2p and O 1s are identical between as-deposited and annealed sample, which suggests that the nearest-neighbour coordination is similar.     

Dielectric and piezoelectric properties of(110) oriented Pb(Zr_(1-x)Ti_x)O_3 thin films

A phenomenological Landau–Devonshire theory is developed to investigate the ferroelectric, dielectric, and piezoelectric properties of(110) oriented Pb(Zr_(1-x)Ti_x)O_3(x = 0.4, 0.5, 0.6, and 0.7) thin films. At room temperature, the tetragonal a_1 phase, the orthorhombic a_2c phase, the triclinic γ_1 phase, and the triclinic γ_2 phase are stable. The appearance of the negative polarization component P_2 in the a_2c phase and the γ_1 phase is attributed to the nonlinear coupling terms in the thermodynamic potential. The γ phase of the Pb(Zr_(1-x)Ti_x)O_3 thin films has better dielectric and piezoelectric properties than the a_2c phase and the a_1 phase. The largest dielectric and piezoelectric coefficients are obtained in the Pb(Zr_(0.5)Ti_(0.5))O_3 thin film. The piezoelectric coefficient of 110–150 pm/V is obtained in the(110) oriented Pb(Zr_(0.5)Ti_(0.5))O_3 thin film, and the Pb(Zr_(0.3)Ti_(0.7))O_3 thin film has the remnant polarization and relative dielectric constant of 50 μC/cm~2 and 100, respectively,which are in agreement with the experimental measurements reported in the literature.     

采用快速升温烧结方法生长Tl-1223超导薄膜的研究

报道了在铝酸镧(00l)衬底上生长Tl-1223超导薄膜的快速升温烧结方法以及铊(Tl)源陪烧靶的配比对Tl-1223薄膜晶体结构的影响.扫描电子显微镜观测表明,采用快速升温烧结方法生长的Tl-1223超导薄膜具有致密的晶体结构.X-射线衍射等测试表明,采用合适配比的陪烧靶在氩气环境下可以制备出纯c轴取向的Tl-1223超导薄膜,充氧退火后的薄膜具有较好的电学性能,其临界转变温度T_(c onset)达到116K,临界电流密度达到1.5MA/cm~2(77 K,0 T).实验结果表明,采用这一新的烧结方法制备Tl系超导薄膜具有升降温时间和恒温时间短、生产成本低等特点.     

热处理对TbDyFe薄膜性能的影响

采用磁控溅射方法利用镶嵌靶材制备非晶TbDyFe薄膜,然后分别在150,300,450,550℃下退火,研究了热处理对TbDyFe薄膜性能的影响.结果显示,550℃温度下退火的样品出现RFe2相.随着退火温度的升高,晶粒逐渐长大,空洞网络变短而宽.薄膜的磁特性显示,其矫顽力及矩磁比均在出现RFe2相的550℃退火的样品中达到最大值.随着退火温度的增加,薄膜的易磁化轴从垂直膜面方向向平行膜面方向转动.     

高温氢退火还原V2O5制备二氧化钒薄膜及其性能的研究

过渡金属氧化物二氧化钒(VO₂)在温度340 K附近会发生金属绝缘体的转变(metal-insulator transition, MIT). 基于金属绝缘体的转变性质, VO₂薄膜材料具有很好的应用前景. 本文首先采用脉冲激光沉积制备了高质量的V₂O₅薄膜, 再通过高温氢退火还原V₂O₅薄膜制备出VO₂多晶薄膜. 研究了不同的退火温度、退火时间、退火气氛对VO₂薄膜制备的影响, 采用X射线衍射、X射线光电子能谱、变温电阻特性测量等手段对样品进行分析, 发现在H₂(5%)/Ar退火气氛下, 在一定的退火温度范围内(500–525 ℃), 退火 3 h, 得到了B相和M相共存的VO₂薄膜, 具有M相的VO₂的MIT特性, 而相同退火温度下退火时间达到4.5 h, 薄膜完全变成B相的VO₂. 通过纯Ar气氛下对B相VO₂再退火, 得到了转变温度为350 K, 电阻突变接近4个数量级的M相的VO₂薄膜. 实现了VO₂的B相和M相的相互转变. 关键词： 2薄膜')" href="#">VO₂薄膜 金属绝缘体转变 氢退火     

Aspects of annealing and free surface crystallization of YBCO thin films

We describe a method of high temperature annealing in which the control of oxygen partial pressure is the principal experimental determinant in obtaining highly c oriented thin films of YBa₂Cu₃O_{7 − δ} on YSZ. Film crystallization, morphology and substrate interactions are discussed with detailed reference to the equilibria existing in the YBCO system. A model based on the melt-assisted crystallization of the precursor tetragonal compound, beginning at the free film surface, is used to explain the observed c texturing. Excellent Josephson coupling between grains of YBa₂Cu₃O_{7 − δ} in our films is related to melt-assisted growth. We discuss the adverse effects of annealing in pure oxygen at high temperatures.     

Effect of annealing temperature on microstructure of chemically deposited calcium modified lead titanate thin films

Thin ferroelectric films of calcium modified lead titanate Pb_1−xCa_xTiO₃(PCT) have been prepared by chemical deposition process. The as deposited amorphous films were thermally treated for crystallization and formation of perovskite structure. Characterization of these films by X-ray diffraction (XRD) have been carried out for various amounts of calcium (Ca)-doping (0.20, 0.24, and 0.28) on indium tin oxide (ITO) coated corning glass substrates. For a better understanding of the crystallization mechanism, the investigations were carried out at various annealing temperatures (450, 550, and 650 °C). Characterization of these films by XRD shows that the films exhibit tetragonal phase with perovskite structure. Atomic force microscope images (AFM) are characterized by slight surface roughness with a uniform crack-free, densely-packed structure. Also, Fourier transform infrared spectra (FT-IR) of the as deposited film and annealed thin films (x=0.24) at 650 °C on silicon (Si) substrates were taken to get more information about the film formation. Dielectric studies of the films were carried out and reported.     

退火温度对硼掺杂纳米金刚石薄膜微结构和p型导电性能的影响

采用热丝化学气相沉积法制备硼掺杂纳米金刚石 (BDND) 薄膜, 并对薄膜进行真空退火处理, 系统研究退火温度对BDND薄膜微结构和电学性能的影响. Hall效应测试结果表明掺B浓度为5000 ppm (NHB) 的样品的电阻率较掺B浓度为500 ppm (NLB) 的样品的低, 载流子浓度高, Hall迁移率下降. 1000 ℃退火后, NLB和NHB 样品的迁移率分别为53.3和39.3 cm²·V^-1·s^-1, 薄膜的迁移率较未退火样品提高, 电阻率降低. 高分辨透射电镜、紫外和可见光拉曼光谱测试结果表明, NLB样品的金刚石相含量较NHB样品高, 高的硼掺杂浓度使薄膜中的金刚石晶粒产生较大的晶格畸变. 经1000 ℃退火后, NLB和NHB薄膜中纳米金刚石相含量较未退火时增大, 说明薄膜中部分非晶碳转变为金刚石相, 为晶界上B扩散到纳米金刚石晶粒中提供了机会, 使得纳米金刚石晶粒中B浓度提高, 增强纳米金刚石晶粒的导电能力, 提高薄膜电学性能. 1000 ℃退火能够恢复纳米金刚石晶粒的晶格完整性, 减小由掺杂引起的内应力, 从而提高薄膜的电学性能. 可见光Raman光谱测试结果表明, 1000℃退火后, Raman谱图中反式聚乙炔 (TPA) 的1140 cm^-1峰消失, 此时薄膜电学性能较好, 说明TPA减少有利于提高薄膜的电学性能. 退火后金刚石相含量的增大、金刚石晶粒的完整性提高及TPA含量的大量减少有利于提高薄膜的电学性能. 关键词： 硼掺杂纳米金刚石薄膜 退火 微结构 电学性能     

VO$lt;sub$gt;2$lt;/sub$gt;/AZO复合薄膜的制备及其光电特性研究

采用直流磁控溅射和后退火氧化的方法在掺铝氧化锌(AZO)导电玻璃上制备了二氧化钒(VO₂)薄膜,研究了不同的退火温度、退火时间对VO₂/AZO复合薄膜制备的影响,并对复合薄膜的结构、组分、光电特性进行了测试与分析. 结果表明,导电玻璃上的AZO没有改变VO₂的取向生长,但明显改变了VO₂薄膜的表面形貌特征. 与用相同工艺和条件在普通玻璃基底上制备的VO₂薄膜相比,VO₂/AZO复合薄膜的相变温度降低约25 ℃,热滞回线宽度收窄至6 ℃,相变前后可见光透过率均在50%以上,1500 nm处红外透过率约为55%和21%,电阻率变化达3 个数量级. 该复合薄膜表面平滑致密,制备工艺简单,性能稳定,可应用于新型光电器件. 关键词： 2')" href="#">VO₂ AZO 热致相变 光电特性     

Ge20Sb15Se65薄膜的热致光学特性变化研究

采用磁控溅射法制备了Ge₂₀Sb₁₅Se₆₅薄膜, 研究热处理温度(150—400 ℃)对薄膜光学特性的影响. 通过分光光度计、X射线衍射仪、显微拉曼光谱仪对热处理前后薄膜样品 的光学特性和微观结构进行了表征, 并根据Swanepoel方法以及Tauc公式分别计算了薄膜折射率色散曲线和光学带隙等参数. 结果表明当退火温度(T_a)小于薄膜的玻璃转化温度(T_g)时,薄膜的光学带隙(E_g^opt)随着退火温度的增加由1.845 eV上升至1.932 eV, 而折射率由2.61降至2.54; 当退火温度大于薄膜的玻璃转化温度时,薄膜的光学带隙随退火温度的增加由1.932 eV降至1.822 eV, 折射率则由2.54增至2.71. 最后利用Mott和Davis提出的非晶材料由非晶到晶态的结构转变模型对结果进行了解释, 并通过薄膜XRD和Raman光谱进一步验证了结构变化是薄膜热致变化的重要原因. 关键词： 20Sb₁₅Se₆₅薄膜')" href="#">Ge₂₀Sb₁₅Se₆₅薄膜 热处理 光学带隙 折射率     

C+注入a-SiNx：H薄膜的微结构及光发射的研究

常温下对低压化学气相沉积制备的纳米硅镶嵌结构的a-SiN_x:H薄膜进行低能量高剂量的C⁺注入后,在800~1200℃高温进行常规退火处理。X射线光电子能谱(XPS)及X射线光电子衍射(XRD)等实验结果表明,当退火温度由800℃升高到1200℃后,薄膜部分结构由SiC_xN_y转变成SiN_x和SiC的混合结构。低温下利用真空紫外光激发,获得分别来自于SiN_x、SiC_xN_y、SiC的,位于2.95,2.58,2.29 eV的光致发光光谱。随着退火温度的升高,薄膜的结构发生了变化,发光光谱也有相应的改变。     

SrNb2O6-NaNbO3-LiNbO3赝三元系相图的研究

本文用X射线衍射、热处理及差热分析等方法测定了SrNb₂O₆-NaNbO₃-LiNbO₃赝三元系的室温截面及相应的SrNb₂O₆-NaNbO₃,SrNb₂O₆-LiNbO₃和NaNbO₃-LiNbO₃等三个赝二元系相图;粗略地研究了Sr_0.42Na_0.16NbO₃-LiNbO₃系的纵截面;含5mol％LiNbO₃及10mol％LiNbO₃的SrNb₂O₆-NaNbO₃的纵截面。确定了室温Sr₂Na(NbO₃)₅(以下略为S₂N)相为四方钨青铜结构。其点阵常数为a=12.36?,c=3.906?.LiNbO₃在S₂N相内的溶解度可达～10mol％,当LiNbO₃含量超过5mol％时,S₂N相畸变为S₂N′相。S₂N′相为正交晶系。实验确定室温S₂N(S₂N′)相系亚稳相。在900-1100℃长时间退火即分解为SrNb₂O₆和以NaNbO₃为基的固溶体的混合物。 关键词：     

退火温度对溶胶-凝胶法制备锌锡氧化物薄膜晶体管的影响

采用溶胶-凝胶法制备了非晶锌锡氧化物(ZTO)薄膜晶体管(TFT),通过热重-差热分析(TG-DTA)对ZTO胶体中的化学反应进行了分析,研究了不同退火温度对ZTO TFTs性能的影响。结果表明:当退火温度在300~500℃范围内时,薄膜为非晶态结构,薄膜表面致密、平整。当退火温度达到400℃时,薄膜在可见光范围内具有高透过率(>85%)。随着退火温度的升高,器件阈值电压明显降低,由15.85 V降至3.76 V,载流子迁移率由0.004 cm²·V^-1·s^-1提高到5.16 cm²·V^-1·s^-1,开关电流比达到10⁵。退火温度的升高明显改善了ZTO TFT的电学性能。     

ZnSb掺杂的Ge2Sb2Te5薄膜的相变性能研究

本文采用双靶(ZnSb靶和Ge₂Sb₂Te₅靶)共溅射制备了系列ZnSb掺杂的Ge₂Sb₂Te₅(GST)薄膜. 利用X射线衍射、透射电子显微镜、原位等温/变温电阻测量、X射线光电子能谱等测试研究了薄膜样品的非晶形态、电学及原子成键特性. 利用等温原位电阻测试表明ZnSb掺杂的Ge₂Sb₂Te₅薄膜具有更高的结晶温度. 采用Arrhenius 公式计算发现ZnSb掺杂的Ge₂Sb₂Te₅薄膜的十年数据保持温度均高于传统的Ge₂Sb₂Te₅薄膜的88.9℃. 薄膜在200, 250, 300和350℃ 下退火后的X射线衍射图谱表明ZnSb的掺杂抑制了Ge₂Sb₂Te₅薄膜从fcc态到hex态的转变. 通过对薄膜的光电子能谱和透射电镜分析可知Zn, Sb, Te原子之间键进行重组, 形成Zn–Sb 和Zn–Te 键, 且构成非晶物质存在于晶体周围. 采用相变静态检测仪测试样品的相变行为发现ZnSb掺杂的Ge₂Sb₂Te₅薄膜具有更快的结晶速度. 特别是(ZnSb)_24.3(Ge₂Sb₂Te₅)_75.7薄膜, 其结晶温度达到250℃, 十年数据保持温度达到130.1℃, 并且在70 mW激光脉冲功率下晶化时间仅～64 ns, 远快于传统Ge₂Sb₂Te₅薄膜的晶化时间～280 ns. 以上结果表明(ZnSb)_24.3(Ge₂Sb₂Te₅)_75.7薄膜是一种热稳定性好且结晶速度快的相变存储材料.     

First-Principles Calculations of Structural,Elastic and ElectronicProperties of Tetragonal HfO2under Pressure

Structural, elastic and electronic properties of tetragonal HfO₂ at applied hydrostatic pressure up to 50 GPa have been investigated using the plane-wave ultrasoft pseudopotential technique based on the first-principles density-functional theory (DFT). The calculated ground-state properties are in good agreement with previous theoretical and experimental data. Six independent elastic constants of tetragonal HfO₂ have been calculated at zero pressure and high pressure. From the obtained elastic constants, the bulk, shear and Young's modulus, Poisson's coefficients, acoustic velocity and Debye temperature have been calculated at the applied pressure. Band structure shows that tetragonal HfO₂ is an indirect band gap. The variation of the gap versus pressure is well fitted to a quadratic function.