退火温度对等离子体增强化学气相沉积方法生长的ZnO薄膜质量的影响

研究ZnO薄膜质量与退火温度的关系,为了获得高质量的晶体薄膜,采用PECVD方法在硅(100)衬底上生长ZnO薄膜,生长温度为120℃,然后分别在氧气环境下退火(600℃～1000℃)1 h.X射线衍射谱和原子力显微镜(AFM)照片结果表明随着退火温度的升高,晶体择优取向明显,晶粒平均尺寸增大,到900℃时,晶粒平均尺寸达到38 nm.光致发光谱的结果表明,随着退火温度的升高,发光峰的半高宽(FWHM)逐渐地变窄,到900℃时,达到92meV,晶体质量得到了明显提高.通过对变温光谱的拟合计算,得到激子束缚能为59 meV,表明紫外发射来自于自由激子辐射复合.     

退火温度对PLT铁电薄膜微结构和电畴的影响

常温下采用射频磁控溅射技术在Pt/TI/SiO2/Si(100)基片上淀积(Pb0.9La0.1)TiO3薄膜,分别在550℃、570℃、600℃、630℃退火1h.采用X射线衍射、原子力显微镜和压电响应力显微镜检测不同退火温度的薄膜,讨论退火温度对薄膜结构、表面形貌和电畴结构的影响.结果表明:随着退火温度的升高,薄膜中钙钛矿相的含量增多,表面粗糙度和颗粒尺寸不断增大,薄膜从无畴状态变为以90°畴为主的多畴,而在退火升降温过程中,由于应力的影响,面外畴更多为取向向下的负畴.     

退火处理对TiNi合金钽镀层微观组织结构的影响

采用多弧离子镀的方法在TiNi形状记忆合金表面镀覆了厚度为3μm的钽镀层,并对其进行了不同温度的真空退火处理.通过X射线衍射(XRD)研究发现,未经退火的镀层是由不稳定的β-Ta组成,分别经过700, 800, 900℃,1h退火后转变为α-Ta.透射电子显微镜(TEM)的观察发现,采用多弧离子镀的方法可以在TiNi合金表面得到纳米尺寸的β-Ta镀层.在700℃退火时可以得到由40 nm左右的微晶和150 nm左右的较大晶粒混合而成的α-Ta.当退火温度为900℃时,镀层主要由尺寸较大而且均匀的α-Ta组成.     

碳化硼球面薄膜及空心微球的制备

采用电子束蒸发镀膜技术, 结合磁控滚动方法在Φ1 mm的钢球基底上制备碳化硼球面膜层, 通过退火、打孔及腐蚀获得碳化硼空心微球. 主要研究了球面膜层的宏观形貌、微观结构、成分及初步探讨了不同退火温度(800~1100℃)对核膜结构空心化的影响. 利用扫描电子显微镜(SEM)、X射线光电子能谱分析(XPS)、原子力显微镜(AFM)对球面薄膜表面形态和薄膜元素组成进行了分析. 结果表明: 磁控滚动模式制备的球面膜层表面平整, 没有裂纹和孔洞, 元素分布均匀. 核膜结构(镀膜时间在5~70 h)经900℃以上温度退火, 空心化后的球面膜层可实现自支撑, 900℃退火的微球表面形貌最好, 壁厚可达10 μm以上.     

铌酸锶钡薄膜制备及椭偏光谱研究

用溶胶-凝胶法成功地制备出了退火温度分别为500、600、700、800、900℃的铌酸锶钡(SBN)薄膜;对制备出SBN薄膜分别进行了椭偏光谱测量研究,得到了不同退火SBN薄膜椭偏光谱参数曲线;并对测得的椭偏光谱进行了数值反演计算,得到了不同退火温度的SBN薄膜的光学常数谱.结果发现SBN薄膜的折射率和消光系数都随着退火温度的增高而增大.     

提拉法制备高透光率超亲水性TiO2薄膜及性能分析

采用溶胶-凝胶法结合提拉工艺在载玻片上制备TiO2薄膜,分别以不同温度(200℃、250℃、300℃、350℃、400℃、450℃、500℃)对薄膜进行退火处理2h.用X射线衍射及扫描电镜测试样品的微观结构和表面形貌,用紫外-可见分光光度计和接触角测量仪分别测试薄膜的透射光谱和水接触角.结果表明,所有样品均为透明薄膜,在可见光范围内平均透光率均大于70％;薄膜光学带隙随退火温度升高依次降低;水接触角随退火温度升高依次减少,当退火温度为450℃和500℃时,水接触角分别为2.5°和2°,薄膜表现为超亲水性.     

磁控溅射非晶CNx薄膜的热稳定性研究

为了研究非晶CNx薄膜的热稳定性,采用射频磁控溅射方法沉积了非晶CNx薄膜样品,并在真空中退火至900℃,利用FTIR,Raman和XPS谱探讨了高温退火对CNx薄膜化学成分及键合结构的影响.研究表明:CNx薄膜样品中N原子分别与sp、sp2和sp3杂化状态的C原子相结合,退火处理极大地影响了CN键合结构的稳定性;当退火温度低于600℃时,膜内N含量的损失较少,CNx薄膜的热稳定性较好,退火温度超过600℃时,将导致CNx膜中大多数C、N间的键合分离,造成N大量损失,膜的热稳定性下降;退火可促使膜内sp3型键向sp2型键转变,在膜中形成大量的sp2型C键,导致CNx膜的石墨化.     

钛酸锶晶体退火过程中氧扩散的有限元分析

针对钛酸锶晶体退火过程中氧原子的扩散问题建立了二维有限元模型,研究了温度、晶体尺寸、退火时间时氧原子扩散状态的影响规律.结果表明:氧在短时间内以大通量从晶体表面扩散,然后以小通量比较稳定地向内部缓慢扩散,温度越高,氧扩散到中心时间越短,在700 K、800 K、900 K条件下退火50 h,氧从晶体表面扩散到中心的时间分别为8h、5h和3h,退火深度分别为1 mm、3mm和退透.     

Ta上生长的硅薄膜退火的微晶化研究

对射频溅射功率80W条件下Ta缓冲层上生长的硅薄膜进行退火并用Raman散射和X射线衍射技术对样品的微观结构进行检测,系统研究了退火温度和退火时间对硅薄膜结晶性的影响.分析结果表明,在560℃退火2h或680℃退火1h之后,硅薄膜开始晶化,并且随着退火温度的增加或退火时间延长,薄膜逐渐由非晶向微晶转变.获得了可用于太阳能电池的微晶硅薄膜的最佳晶化参数.     

退火工艺对磁控溅射生长的Pt薄膜微观结构及电性能的影响

铂(Pt)是温度传感器常见的敏感材料。为了改善退火工艺提高Pt薄膜的电学特性,采用射频磁控溅射法在蓝宝石衬底上制备了以钽(Ta)为粘附层的Pt敏感薄膜,研究了不同退火温度、退火气氛和退火时间下的Pt薄膜结构以及电学性能方面的差异。结果表明:退火增强了薄膜的结晶化且使晶粒发生长大,从而有效降低了薄膜的电阻率。但过度退火,如退火温度超过1 000℃或过长的退火时间,会导致粘附层中的Ta元素向Pt薄膜中过度扩散,从而增加Pt薄膜的电阻率。在高纯N_2(99.999%)、超纯N_2(99.999 9%)及空气三种气氛中退火,结果发现在空气中退火的Pt薄膜电阻率最小,原因是空气中的氧元素在高温下穿过Pt薄膜扩散至Ta粘附层,形成了稳定的Ta_2O_5相,Ta元素向Pt薄膜的扩散减少。退火还提升了薄膜电阻随温度变化的线性度及其电阻温度系数(TCR),在空气中900℃退火1 h,Pt薄膜的TCR达到3.909×10~(-3)/℃,接近于块状Pt材料的值。此结果对提高Pt薄膜温度传感器的灵敏度具有重要意义。     

热处理对TP347H钢组织结构及力学性能的影响

本文通过800--900℃的加速老化试验,研究热处理过程中TP347H钢的组织结构及力学性能的变化特征。结果表明：800℃,58h热处理,原奥氏体晶粒尺寸稳定,碳化物颗粒在晶界及晶内弥散析出;900℃,5．5h高温热处理后,析出碳化物聚集长大,导致晶界宽化。经900℃,5．5h高温处理后,TP347H钢仍为韧窝聚集型断裂,但断裂面相对平整,韧窝细而浅,且沿基体晶界有二次裂纹扩展。上述组织结构的变化导致热处理过程中TP347H钢的强度持续降低,而塑性先增加,后降低。     

Photoluminescence properties of the Yb:Er co-doped Al2O3 thin film fabricated by microwave ECR plasma source enhanced RF magnetron sputtering

The Yb:Er co-doped Al₂O₃ thin film was deposited on oxidized silicon wafers by microwave ECR plasma source enhanced RF magnetron sputtering, and annealed from 800 °C to 1000 °C. The photoluminescence at 1.53 μm of thin film was obtained under room temperature. The mixture phase structure of γ and θ is observed by XRD, and the compositions of the thin film are investigated by EPMA. The maximum PL intensity was achieved with O₂:Ar at 1:1, annealing temperature at 900 °C, and experimental ratio of Yb:Er at 1:3.6. The energy transfer mechanism between Er and Yb ions is supported by theoretical analysis and experiment results.     

掠射角溅射沉积纳米结构氧化钨薄膜

采用掠射角反应磁控溅射法在室温下沉积了纳米结构氧化钨(WO₃)薄膜, 并对薄膜进行热处理。利用场发射扫描电镜(FE-SEM)和X射线衍射仪(XRD)对氧化钨薄膜的形貌和结构进行了表征。当掠射角度为80°时, 采用直流电源沉积的氧化钨薄膜具有纳米斜柱状结构, 而采用脉冲直流电源沉积的薄膜呈现纳米孔结构。纳米薄膜经450℃热处理3 h后, 纳米斜柱彼此连接, 失去规整结构, 而纳米孔结构的孔尺寸变大。XRD分析表明室温沉积的氧化钨薄膜具有无定形结构, 经450℃热处理1 h后, 转变为单斜晶相。具有纳米斜柱状或纳米孔结构氧化钨薄膜的光学调制幅度在波长600 nm时达到60%, 且电致变色性能可逆。     

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.     

ZrO2/Cu复合材料内氧化制备工艺

采用非真空熔炼和高压水雾化法制得Cu-0.6%Zr(质量分数)合金粉末,经粒径分选后进行低温氧化、N₂+5%H₂(体积分数)混合气体还原和真空等离子放电烧结(SPS)成型,制备得到ZrO₂/Cu原位增强复合材料。结果表明: 对合金粉末低温氧化处理时,温度过低,氧化速度慢,温度过高,易发生过氧化和粉末结块现象,最佳氧化参数为230℃×1 h; N₂+5%H₂气体流量控制在200 mL/min条件下,通过烧氢实验确定最佳还原参数为250℃×1 h; 在30 MPa压力条件下,经850℃×2 h 真空放电等离子烧结(SPS),ZrO₂/Cu试样的导电率>83% IACS(international annealed copper standard),硬度>HB 75,软化温度为900℃。     

Ordering of the α-Fe(Si) Crystallization Phase in Annealed Fe_(73.5)Cu_1Mo_3Si_(13.5)B_9 Alloy

The ordering of the α-Fe(Si) crystallization phase in annealed Fe73.5Cu1Mo3Si13.5B9 alloy has been studied using XRD method. The α-Fe(Si) phase in Fe73.5Cu1Mo3Si13.5B9 alloy annealed at 460℃ for 1 h consists of the DO3-type ordered region with spherical shape and disordered region. The size of DO3 ordered region increases with the annealing temperature. When the annealing temperature is 560℃, the size of the ordered region in the α-Fe(Si) grain is 14.0nm,which is nearly as large as that of the α-Fe(Si) grain (14.2 nm) and the degree of order of the α-Fe(Si) phase is about 0.78. When Fe73.5Cu1 Mo3Si13.5B9 amorphous alloy is annealed at 520℃, with the increment of the annealing time, the shape of the DO3 ordered region in the α-Fe(Si) phase is spheroidal at the beginning of the annealing and becomes spherical and has asize of 12.8 nm when the annealing time is 60 min. In addition, the DO3 superlattice lines of the α-Fe(Si) phase will vanish if Fe73.5Cu1Mo3Si13.5 B9 amorphous alloy is annealed for 1 h at 750℃.     

氮气含量对AlCrTaTiZrMoN_x高熵合金氮化物薄膜扩散阻挡性能的影响

国内对高熵合金的研究主要集中于其优异的力学性能,还未见有关高熵合金扩散阻挡性能的报道。采用直流磁控反应溅射方法在不同N_2流量占比气氛中制备了AlCrTaTiZrMoNx薄膜与Cu/AlCrTaTiZrMoNx/Si复合试样,并对样品真空退火1h。用X射线衍射仪(XRD)、原子力显微镜(AFM)、四探针电阻测试仪(FPP)、场发射扫描电镜(SEM)对退火前后样品的物相结构、表面粗糙度、形貌以及方块电阻进行了分析表征,研究了薄膜的热稳定性和扩散阻挡性能。结果表明:随着N_2流量占比的增加,高熵合金氮化物薄膜表面粗糙度增加,方块电阻也单调增加;N_2流量变化会改变薄膜结构,未通入N_2时,薄膜为非晶结构,当通入N_2后,N原子会与金属原子形成氮化物,使结晶性能得到提高,薄膜结构为面心立方,N_2流量占比为20%时,薄膜结晶较好,晶粒细小;当N_2流量占比为0时,复合试样在700℃退火时失效;N_2流量占比为10%时,复合试样在800℃退火时失效;N_2气流量占比为20%和30%时,复合试样在800℃退火后,其X射线衍射峰没有明显的变化,复合试样表面较为平整,此温度为极限温度;在900℃退火后,复合试样界面发生了相互扩散,生成了高阻态铜硅化合物,表面粗糙度显著升高,表明扩散阻挡层已经彻底失效;可见,随着N_2流量占比的增加,高熵合金涂层的扩散阻挡性能和热稳定性得到提高,但当N_2流量占比大于20%时,其阻挡性能和热稳定性提高不明显。     

Methods and mechanisms for uniformly refining deformed mixed and coarse grains inside a solution-treated Ni-based superalloy by two-stage heat treatment

The uniform refinement mechanisms and methods of deformed mixed and coarse grains inside a solution-treatment Ni-based superalloy during two-stage annealing treatment have been investigated.The two-stage heat treatment experiments include an aging annealing treatment(AT)and a subsequent recrystallization annealing treatment(RT).The object of AT is to precipitate some δ phases and consume part of storage energy to inhibit the grain growth during RT,while the RT is to refine mixed and coarse grains by recrystallization.It can be found that the recrystallization grains will quickly grow up to a large size when the AT time is too low or the RT temperature is too high,while the deformed coarse grains cannot be eliminated when the AT time is too long or the RT temperature is too low.In addition,the mixed microstructure composed of some abnormal coarse recrystallization grains(ACRGs)and a large number of fine grains can be observed in the annealed specimen when the AT time is 3 h and RT tem-perature is 980℃.The phenomenon attributes to the uneven distribution of δ phase resulted from the heterogeneous deformation energy when the AT time is too short.In the regions with a large number of δ phases,the recrystallization nucleation rate is promoted and the growth of grains is limited,which results in fine grains.However,in the regions with few δ phases,the recrystallization grains around grain boundaries can easily grow up,and the new recrystallization nucleus is difficult to form inside grain,which leads to ACRGs.Thus,in order to obtain uniform and fine annealed microstructure,it is a prereq-uisite to precipitate even-distributed δ phase by choosing a suitable AT time,such as 12 h.Moreover,a relative high RT temperature is also needed to promote the recrystallization nucleation around δ phase.The optimal annealing parameters range for uniformly refining mixed crystal can be summarized as:900℃×12 h+990℃×(40-60 min)and 900℃×12 h+1000℃×(10-15 min).     

晶粒尺寸对氧化钒薄膜电学与光学相变特性的影响

采用直流对靶磁控溅射方法制备氧化钒薄膜,通过改变热处理温度获得了具有不同晶粒尺寸的相变特性氧化钒薄膜,对氧化钒薄膜相变过程中电阻和红外光透射率随温度的突变性能进行研究.结果表明:经300℃和360℃热处理后,薄膜内二氧化钒原子分数达到40%,氧化钒薄膜具有绝缘体-金属相变特性,薄膜的晶粒尺寸分别为50nm和100nm;...     

Effect of Annealing Temperature on GMR of [NiFeCo(10 nm)/Ag(10 nm)]×20 Multilayer

The composition, phase structure, and microstructure of the discontinuous multilayer films [NiFeCo(10 nm)/Ag(10 nm)]×20 annealed at temperature 280, 320, 360 and 400℃, respectively were investigated GMR (giant magnetoresistance) ratios of the multilayer films were measured at different temperature. The results showed that FeNi3 precipitated at 360℃ and dissolved at 400℃. The films annealed at 360℃ for 1 h exhibited the highest GMR ratio 11% when saturation field was equal to 79.6 kA/m.