Agglomeration suppression behavior and mechanisms of Ag-Cu and Ag-Nb thin films

Agglomeration behavior of Ag-Cu and Ag-Nb thin films prepared by sputtering was investigated. The films were annealed at 400-600 °C in vacuum and their surface morphologies and resistivities were characterized. It was found that agglomeration was suppressed in both Ag-Cu and Ag-Nb films. The resistivity of Ag-Cu films remained low even when the Cu concentration was increased. However, the resistivity of the Ag-Nb films increased with Nb concentration. We found that 0.4 at% Nb and 2.1 at% Cu were optimum alloying concentrations from the standpoint of both morphology and resistivity. The mechanisms of agglomeration suppression for the Ag-Cu and Ag-Nb films appeared to be different. XRD measurements of the Ag-Cu films showed a marked preferential orientation for (111) in the case of as-deposited films. This suggested that the annealing-induced orientation change in the crystal grains of the Ag-Cu films was minimal. On the basis of XPS measurements, it is believed that the Nb oxides surrounding the Ag grains led to agglomeration suppression in the Ag-Nb film.     

Low temperature ordering of FePt films by in-situ heating deposition plus post deposition annealing

FePt thin films with 40 nm thickness were prepared on thermally oxidized Si (001) substrates by dc magnetron sputtering at the nominal growth temperature 375 °C. The effects of annealing on microstructure and magnetic properties of FePt thin films were investigated. The as-deposited FePt thin films show soft magnetic properties. After the as-deposited FePt thin films were annealed at various temperatures and furnace cooled, it is found that the ordering temperature of L1₀ FePt phase could be reduced to 350 °C. For FePt thin films annealed at 350 °C, the in-plane and out-of-plane coercivities of the films increased to 510 and 543 kA/m, respectively, and the films had hard magnetic properties. A highly (001) orientation was obtained, when FePt thin films were annealed at 600 °C. And the hysteresis loops of FePt thin films annealed at 600 °C show out-of-plane magnetic anisotropy.     

X-ray absorption spectroscopy study of thermally annealed Cu–Al–O thin films

Cu–Al–O thin films are deposited on (0001) sapphire substrates by radio-frequency sputtering using an Al–Cu mosaic target. The Cu/Al atomic ratio of as-deposited Cu–Al–O films is measured to be 1.1. After deposition, the Cu–Al–O films are annealed at 600, 800, and 1000 °C, respectively, for 1 h in a N₂ atmosphere. The film crystal structure, electronic structure, valence band, and electrical properties are studied. The as-deposited films are amorphous and films annealed at 600 °C contain the crystallized CuO phase; the structure becomes crystallized CuAlO₂ after annealing at 800 °C and 1000 °C. The 800 °C annealed film grows along the (00l) plane. The crystallization decreases with the growth of the (012) and (018) planes for films annealed at 1000 °C. The resistivity values of the 800 °C and 1000 °C annealed films were measured as 1.07 Ω-cm and 864.01 Ω-cm, respectively. The lower resistivity of the 800 °C annealed film is attributed to preferred (00l) growth orientation and a reduction of the energy band gap.     

Influence of thermal annealing on microstructural,morphological, optical properties and surface electronic structure of copper oxide thin films

In this study, effect of the post-deposition thermal annealing on copper oxide thin films has been systemically investigated. The copper oxide thin films were chemically deposited on glass substrates by spin-coating. Samples were annealed in air at atmospheric pressure and at different temperatures ranging from 200 to 600°C. The microstructural, morphological, optical properties and surface electronic structure of the thin films have been studied by diagnostic techniques such as X-ray diffraction (XRD), Raman spectroscopy, ultraviolet–visible (UV–VIS) absorption spectroscopy, field emission scanning electron microscopy (FESEM), atomic force microscopy (AFM), and X-ray photoelectron spectroscopy (XPS). The thickness of the films was about 520 nm. Crystallinity and grain size was found to improve with annealing temperature. The optical bandgap of the samples was found to be in between 1.93 and 2.08 eV. Cupric oxide (CuO), cuprous oxide (Cu₂O) and copper hydroxide (Cu(OH)₂) phases were observed on the surface of as-deposited and 600 °C annealed thin films and relative concentrations of these three phases were found to depend on annealing temperature. A complete characterization reported herein allowed us to better understand the surface properties of copper oxide thin films which could then be used as active layers in optoelectronic devices such as solar cells and photodetectors.     

磁控溅射Cu-Nb和Cu-Mo薄膜结构与性能

采用磁控溅射制备含1.16%～15.8%(原子分数)Nb的Cu-Nb及含2.2%～27.8%Mo的Cu-Mo合金薄膜,井采用EDX、XRD、SEM、显微硬度仪和电阻计对薄膜的成分、结构和性能进行研究。结果表明,Nb和Mo的添加分别使Cu-Nb及Cu-Mo薄膜晶粒显著细化,Cu-Nb和Cu-Mo薄膜呈纳米晶结构,存在Nb在Cu中的fcc Cu(Nb)和Mo在Cu中的fcc Cu(Mo)非平衡亚稳过饱和固溶体,固溶度随Nb或Mo含量增加而上升。添加Nb和Mo显著提高Cu-Nb及Cu-Mo薄膜的显微硬度和电阻率,且随Nb或Mo含量增加而升高。经650℃热处理1h后,Cu-Nb和Cu-Mo薄膜显微硬度和电阻率均下降,且分析表明均发生基体相晶粒长大,并出现微米-亚微米级富Cu第二相,Cu-Nb及Cu-Mo薄膜结构和性能形成及演变的主要原因是添加的Nb、Mo引起的晶粒细化效应以及退火中基体相晶粒度的增大。     

Effect of thickness on structural,optical, electrical and morphological properties of nanocrystalline CdSe thin films for optoelectronic applications

This paper presents effect of thickness on the physical properties of thermally evaporated cadmium selenide thin films. The films of thickness 445 nm, 631 nm and 810 nm were deposited employing thermal evaporation technique on glass and ITO coated glass substrates followed by thermal annealing in air atmosphere at temperature 300 °C. The as-deposited and annealed films were subjected to the XRD, UV–Vis spectrophotometer, source meter, SEM and EDS to find the structural, optical, electrical, morphological and compositional analysis respectively. The structural analysis shows that the films have cubic phase with preferred orientation (1 1 1) and nanocrystalline nature. The structural parameters like inter-planner spacing, lattice constant, grain size, number of crystallites per unit area, internal strain, dislocation density and texture coefficient are calculated. The optical band gap is found in the range 1.69–1.84 eV and observed to decrease with thickness. The electrical resistivity is found to increase with thickness for as-deposited films and decrease for annealed films. The morphological studies show that the as-deposited and annealed films are homogeneous, smooth, fully covered and free from crystal defects like pin holes and voids. The grains in the as-deposited films are densely packed, well defined and found to be increased with thickness.     

Microstructure of electroplated Cu(Ag) alloy thin films

Electroplated Cu(Ag) alloy thin films are potential candidates for future electronic devices in terms of lifetime and reliability compared to copper as the state of the art interconnect material. In the present paper we focus on the microstructure of Cu(Ag) alloy films considering the grain evolution as well as silver incorporation and segregation. We show that Ag alloying addition prevents room temperature recrystallization. Thermally induced grain growth occurs mainly between 180 °C and 330 °C. Silver can be incorporated as solid solution into the Cu matrix by up to 0.8 at.% after annealing and even in higher concentrations in the as-deposited state, which is significantly above the equilibrium solubility limit. Precipitations are formed by the continuous mode and can be mainly found at the film surface but also inside the Cu(Ag) grains as ball-shaped particles. Based on our results a reliability improvement is expected by mechanical strengthening due to alloying effects while maintaining a low electrical resistivity and a {111} fiber texture.     

磁控溅射沉积Cu-W薄膜的特征及热处理的影响

采用磁控共溅射法制备含钨1.51%~14.20%(原子分数,下同)的Cu-W合金薄膜,并用EDX、XRD、SEM、显微硬度仪和电阻仪研究了其成分、结构及性能。结果表明,添加W可显著细化Cu-W薄膜基体相晶粒,晶粒尺寸随W含量的增加而减小,Cu-W薄膜呈纳米晶结构。Cu-W薄膜中存在W在Cu中形成的fcc Cu(W)非平衡亚稳过饱和固溶体,固溶度随W含量的增加而提高,最大值为10.65%。与纯Cu膜对比发现,薄膜的显微硬度和电阻率总体上随W含量的增加而显著增大。经200℃、400℃及650℃热处理1h后,Cu-W薄膜基体相晶粒长大,EDX分析显示晶界处出现富W第二相;薄膜显微硬度降低,电阻率下降,降幅与退火温度呈正相关。添加W引起的晶粒细化效应以及退火中基体相晶粒度增大分别是Cu-W薄膜微观结构和性能形成及演变的主要原因。     

Structural instability of Sn-doped In2O3 thin films during thermal annealing at low temperature

We report on observations of structural stability of Sn-doped In₂O₃ (ITO) thin films during thermal annealing at low temperature. The ITO thin films were deposited by radio-frequency magnetron sputtering at room temperature. Transmission electron microscopy analysis revealed that the as-deposited ITO thin films are nanocrystalline. After thermal annealing in a He atmosphere at 250 °C for 30 min, recrystallization, coalescence, and agglomeration of grains were observed. We further found that nanovoids formed in the annealed ITO thin films. The majority of the nanovoids are distributed along the locations of the original grain boundaries. These nanovoids divide the agglomerated larger grains into small coherent domains.     

Annealing induced reorientation of crystallites in Sn doped ZnO films

Tin doped ZnO thin films were prepared by employing a simplified spray pyrolysis technique using a perfume atomizer and subsequently annealed under different temperatures from 350 °C to 500 °C in steps of 50 °C. The structural, optical, electrical, photoluminescence and surface morphological properties of the as-deposited films were studied and compared with that of the annealed films. The X-ray diffraction studies showed that as-deposited film exhibits preferential orientation along the (0 0 2) plane and it changes in favour of (1 0 0) plane after annealing. The increase in crystallite size due to annealing is explained on the basis of Ostwald ripening effect. It is found that the optical transmittance and band gap increases with increase in annealing temperature. A slight decrease in resistivity caused by annealing is discussed in correlation with annealing induced defect modifications and surface morphology.     

Solution grown nanocrystalline ZnO thin films for UV emission and LPG sensing

Nanocrystalline ZnO thin films were successfully deposited by a simple and inexpensive solution growth technique. Photoluminescence (PL) and liquefied petroleum gas (LPG) sensing properties were investigated. Films were found to be uniform, pinhole free, and well adherent. As deposited and heat treated (at 673 K for 2 h) films were characterized by XRD, SEM, and EDAX. The dc electrical resistivity and LPG sensing property were measured. The change in morphology, from spherical particle to rod-like, was observed after air annealing. XRD results revealed that the obtained films were nanocrystalline and had a hexagonal wurtzite structure. The absorption edge was found to be at around 366 nm for the as-deposited film and 374 nm for the annealed film. The band gaps were found to be 3.29 and 2.9 eV for the as-deposited and annealed films, respectively. PL spectra of ZnO thin films showed strong peak at 384 nm, which corresponds to near band edge emission (UV emission) and a relatively weak peak at 471 nm. Further, the annealed film was used for detection of LPG in air. Maximum response was observed at 673 K. The maximum sensitivity of sensor was found to be 4.5 for 0.6 vol.% LPG. Sensing response got saturated after 0.6 vol.% of gas concentration. A possible mechanism of LPG sensing has been explained.     

Study of Cu emergence on the surface of TaN-Cu nanocomposite thin films and its effects on tribological property

TaN-Cu nanocomposite films, were deposited by reactive co-sputtering on Si and tool steel substrates. The films were then annealed using RTA (Rapid Thermal Annealing) at 400 °C for 2, 4, 8 min respectively to induce the nucleation and growth of Cu particles in the TaN matrix and on the film surface. SSPM (Scanning Surface Potential Microscopy) and SEM (Scanning Electron Microscopy) were applied to examine the Cu nano-particles that emerged on the surface of TaN-Cu thin films. Pin-on-Disk tribometer was used to study the effect of annealing on the films' tribological properties. The results reveal that annealing by RTA can cause Cu nano-particles to emerge on the TaN surface. Consequently, hardness and friction coefficients will change depending on annealing conditions, Cu content, and/or Cu particle emergence.     

生长温度对PLD原位生长SrTiO3薄膜结构与非线性介电性能的影响

采用脉冲激光沉积法 ( PLD ) 制备的Y1B2Cu3O7-x薄膜作为叉指底电极,然后生长 SrTiO3介质薄膜,形成叉指型压控电容结构。通过对 SrTiO3薄膜的原位生长温度与薄膜微观结构及非线性介电性能之间的关系研究,发现随生长温度的升高薄膜晶粒逐步增大然后变小,薄膜的介电常数可调率和本征介电损耗随晶粒大小的增大而增加,而非本征损耗则随晶粒取向的增加而减小。     

Structural,optical and electrical characteristics of transparent bismuth vanadate films deposited on indium tin oxide coated glass substrates

Bismuth vanadate (BVO) thin films were fabricated on indium tin oxide (ITO) coated glass substrates using pulsed laser ablation technique and investigated their structural, optical and electrical properties. The use of the indium tin oxide coated glass substrate resulted in reducing the leakage current characteristics of crystalline BVO thin films. The X-ray diffraction (XRD) studies confirmed the monophasic nature of the post annealed (500 °C/1 h) films. The atomic force microscopy indicated the homogeneous distribution of crystallites in the as-deposited films. The as-deposited and the post annealed films were almost 90% transparent (380–900 nm) as confirmed by optical transmission studies. Dielectric constant of around 52 was attained accompanied by the low dielectric loss of 0.002 at 10 kHz for post annealed films. The leakage current of the post annealed BVO films on ITO coated glass substrates measured at room temperature was 8.1 × 10⁻⁸ A at an applied electric field of 33 kV/cm, which was lower than that of the films with platinum and SrRuO₃ as the bottom electrodes.     

Effect of heat treatment on characteristics of nanocrystalline ZnO films by electron beam evaporation

Zinc oxide thin films have been grown on glass substrate at room temperature by electron beam evaporation and then were annealed in annealing pressure 600 mbar at different temperatures ranging from 250 to 550 °C for 30 min. Electrical, optical and structural properties of thin films such as electrical resistivity, optical transmittance, band gap and grain size have been obtained as a function of annealing temperature. X-ray diffraction has shown that the maximum intensity peak corresponds to the (002) predominant orientation for ZnO films annealed at various temperatures. The full width at half maximum, decreases after annealing treatment which proves the crystal quality improvement. Scanning electron microscopy images show that the grain size becomes larger by increasing annealing temperature and this result agrees with the X-ray diffraction analysis.     

Preliminary studies on molybdenum-doped indium oxide thin films deposited by radio-frequency magnetron sputtering at room temperature

Thin films of molybdenum-doped indium oxide (IMO) were prepared by a 3-source, cylindrical radio-frequency magnetron sputtering at room temperature. The films were post-annealed and were characterized by their structural (X-ray diffraction) and optical (UV-VIS-NIR spectrophotometer) properties. The films were studied as a function of oxygen volume percentage (O₂ vol.%) ranging from 3.5 to 17.5. The structural studies revealed that the as-deposited amorphous films become crystalline on annealing. In most cases, the (222) reflection emerged as high intensive peak. The poor visible transmittance of the films as-deposited without oxygen was increased from ∼ 12% to over 80% on introducing oxygen (3.5 O₂ vol.%). For the films annealed in open air, the average visible transmittance in the wavelength ranging 400-800 nm was varied between 77 and 84%. The films annealed at high temperatures (> 300 °C) decreased the transmittance to as low as < 1%. The optical band gap of the as-deposited films increased from the range 3.83-3.90 to 3.85-3.98 eV on annealing at different conditions.     

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。     

Photoluminescence from RF sputtered SiCBN thin films

Silicon carbon boron nitride (SiCBN) thin films were synthesized by reactive co-sputtering of silicon carbide (SiC) and boron nitride (BN) targets. As-deposited samples show distinct photoluminescence (PL) peaks at 465, 483 and 497 nm. The films were annealed in dry oxygen ambient at different temperatures to investigate the effect of annealing on film properties. Subsequent measurements on the annealed samples show diminished PL peak intensities. X-ray diffraction analysis shows that the as-deposited films are amorphous in nature and there is no change in the microstructure even after high temperature annealing. Surface characterization of the films by X-ray photoelectron spectroscopy reveals change in chemical composition at different annealing temperatures. Carbon concentrations in the films are sensitive to annealing temperatures and could cause the change in photoluminescence properties.     

Structural,optical and electrical studies on nanocrystalline tin oxide (SnO<Subscript>2</Subscript>) thin films by electron beam evaporation technique

Nanocrystalline tin oxide (SnO₂) thin films were coated using electron beam evaporation technique on glass substrates. To study the gleaming out look of the structure and surface morphological changes, the films were annealed in the temperature 350–550 °C for 1 h. The annealed films were subjected to X-ray diffraction (XRD) and atomic force microscopy (AFM) studies. The XRD patterns of SnO₂ thin films as-deposited and annealed at 350 °C illustrate that the films were amorphous, and beyond 350 °C and thereafter they became polycrystalline with tetragonal structure. The crystallite size of the annealed films, obtained through the XRD analysis, increased with the increasing annealing temperature, and it was found to be from 3.6 to 12 nm. The photoluminescence (PL) studies on these films were also carried out. The origin of luminescence was assigned to the defects of the nanocrystalline SnO₂ films. The Optical studies (UV-VIS) were performed and the optical band gab energy (Eg) calculations, the dependence of absorption coefficient on the photon energy at short wavelengths, were found to be increasing from 3.65 to 3.91 eV is also investigated.     

Influences of post-annealing on structural and electrical properties of Bi1.5Zn1.0Nb1.5O7 thin films prepared by pulsed laser deposition

Bi_1.5Zn_1.0Nb_1.5O₇ (BZN) thin films were prepared on Pt/TiO₂/SiO₂/Si(100) substrates at 650 °C under an oxygen pressure of 10 Pa by using pulsed laser deposition process. The crystallinity, microstructure and electrical properties of BZN thin films were investigated to verify the influences of post-annealing thermal process on them. The X-ray diffractometer (XRD) results indicate that all Bi_1.5Zn_1.0Nb_1.5O₇ thin films without post-annealing process or with post-annealing in situ vacuum chamber and in oxygen ambient exhibit a cubic pyrochlore structure. The improved crystallinity of BZN thin films through post-annealing was confirmed by XRD and scanning electron microscope (SEM) analysis. Dielectric constant and loss tangent of the as-deposited BZN thin films are 160 and 0.002 at 10 kHz, respectively. After annealing, dielectric properties of thin films are significantly improved. Dielectric constant and loss tangent of the in situ annealed films are 181 and 0.0005 at 10 kHz, respectively. But the films post-annealed in O₂ oven show the largest dielectric constant of 202 and the lowest loss tangent of 0.0002, which may attribute to the increase in grain size and the elimination of oxygen vacancies. Compared with the as-deposited BZN thin films, the post-annealed films also show the larger dielectric tunability and the lower leakage current density.