Low-temperature growth of highly c-oriented InN films on glass substrates with ECR-PEMOCVD

High quality InN films are deposited with an interlayer of high c-orientation (002) AZO (Aluminium-doped Zinc Oxide; ZnO:Al) films on glass substrates by electron cyclotron resonance plasma-enhanced metal organic chemical vapor deposition (ECR-PEMOCVD) at low temperature. AZO films used as a buffer layer are effective for the epitaxial growth of InN films. The influence of Trimethyl Indium (TMIn) flux on the properties of InN films is systematically investigated by reflection high energy electron diffraction (RHEED), X-ray diffraction analysis (XRD), atomic force microscopy (AFM) and optical transmittance spectra. The results indicate that high quality InN films with high c-orientation and small surface roughness are successfully achieved at an optimized Trimethyl Indium (TMIn) flux of 5.5 sccm. The InN/AZO structures have great potential for the development of full spectra solar cells.     

Deposition of diamond films on metal substrates

In this paper we report on the growth of polycrystalline diamond films on Mo, W, and Ni substrates using oxy-acetylene combustion flame technique. Effect of substrate temperature on the growth of diamond films has been studied in the temperature range 600–1100°C. The deposits and their surface morphology has been characterized by X-ray diffraction and scanning electron microscopy (SEM). A short duration pretreatment of Mo substrates by outer zone of the oxy-acetylene flame at lower substrate temperatures, results in the improvement of quality and adherence of the films. Growth of diamond as well as other intermediate compounds depending on the nature of substrates and interface layers is discussed. Paper presented at the poster session of MRSI AGM VI, Kharagpur, 1995     

Structure of diamond polycrystalline films deposited on silicon substrates

The article presents results of structural studies of polycrystalline diamond thin films deposited by hot filament CVD on silicon substrates. The films were characterized using Scanning Electron Microscopy (SEM), Raman Spectroscopy (RS), Electron Backscattered Diffraction (EBSD), Energy Dispersive Spectroscopy (EDS) and Secondary Ion Mass Spectroscopy (SIMS). Both the EBSD patterns and Raman spectra confirm that the grains visible in the electron micrographs are diamond micro-crystallites. The residual stress in the films is found to be in the range between −4.29 GPa and −0.56 GPa depending on the sample thickness. No evidence of lonsdalite and graphite has been registered in the polycrystalline material of the investigated samples. Evidence of the existence of silicon carbide at the diamond/silicon interface is presented. It is also suggested that an amorphous carbonaceous film covers the silicon surface in the regions of holes in the thin diamond layers.     

Growth of nanocrystalline diamond films in CCl4/H2 ambient

We investigated the growth characteristics of the nanocrystalline diamond films using CCl₄/H₂ as gas sources in a hot-filament chemical vapor deposition (CVD) reactor. Successful growth of nanocrystalline diamond at typical growth condition of 1.5-2.5% CCl₄ and 550-730 °C substrate temperature has been demonstrated. Glancing angle X-ray diffraction (XRD) clearly indicated the formation of diamond in the films. Typical root-mean-square surface roughness of 10-15 nm and an optimal root-mean-square surface roughness of 6 nm have been achieved. Transmission electron microscopy (TEM) analyses indicated that nanocrystalline diamond film with an average grain size in the range of 10-20 nm was deposited from 2.5% CCl₄/H₂ at 610 °C. Effects of different source gas composition and substrate temperature on the grain nucleation and grain growth processes, whereby the grain size of the nanocrystalline film could be controlled, were discussed.     

Synthesis of boron-doped diamond films by DC plasma CVD using a CH4+CO2+H2 gas mixture at lower substrate temperature and formation of an n-Si/p-diamond heterojunction

Diamond films were synthesized by direct current plasma chemical vapour deposition using a CH₄+CO₂+H₂ gas mixture on Si substrates. The optimum deposition conditions were determined. It was found that 0.4 A/cm² current density, at applied voltage of 1 kV, resulted in good-quality diamond films. The substrate temperature was 750 K which is considerably lower than the conventional requirement of ∼1100 K. Boron doping was achieved by passing a portion of the gas mixture through boric acid dissolved in methanol. The boron-doped p-type diamond films were deposited on an n-type single crystalline Si substrate and an n-Si/p-diamond heterojunction was fabricated. The p-n junction was characterized in terms of current-voltage (I-V) and capacitance-voltage (C-V) measurements.     

Influence of the reactive N2 gas flow on the properties of rf-sputtered ZnO thin films

Nitrogen (N)-doped ZnO thin films were RF sputtered with different N₂ volume (ranging from 10% to 100%) on sapphire (001) substrates. The influence of N₂ vol.% on the properties of ZnO films was analyzed by various characterization techniques. The X-ray diffraction studies showed that the films grow along the preferential (002) crystallographic plane and the crystallinity varied with varying N₂ vol.%. The films sputtered with 25 vol.% N₂ showed better crystallinity. The transmittance was decreased with increasing N₂ volume until 25% and was almost constant above 25%. A maximum optical band gap (2.08 eV) obtained for 10 vol.% N₂ decreased with increasing N₂ volume to reach a minimum of 1.53 eV at 100%. The compositional analysis confirmed the incorporation of N into ZnO films, and its concentration increased with increasing N₂ volume to reach a maximum of ∼ 3.7 × 10²¹ atom/cm³ at 75% but then decreased slightly to 3.42 × 10²¹ atoms/cm³. The sign of Hall coefficient confirmed that the films sputtered with ≤ 25 vol.% N₂ possess p-type conductivity which changes to n-type for > 25 vol.% N₂.     

衬底氮化时间对玻璃衬底上低温沉积GaN薄膜结晶性的影响

采用电子回旋共振-等离子体增强金属有机物化学气相沉积(ECR-PEMOCVD)方法,在康宁7101型普通玻璃衬底上低温沉积氮化镓(GaN)薄膜.利用反射高能电子衍射(RHEED)、X射线衍射(XRD)、原子力显微镜(AFM)和霍尔测量系统检测样品,研究了衬底氮化时间对GaN薄膜质量的影响.结果表明,氮化时间为5min时,得到的GaN薄膜呈高度c轴择优取向,结晶性较好,薄膜表面是由许多亚微米量级的表面岛按一致的取向规则堆砌而成的,薄膜表面较为平整且呈n型导电;氮化时间增加,薄膜结晶性反而变差.     

Synthesis of GaN nanorods by ammoniating Ga2O3 films on TiO2 (rutile) layer deposited on Si(111) substrates

GaN nanorods have been synthesized by ammoniating Ga₂O₃ films on a TiO₂ middle layer deposited on Si(111) substrates. The products were characterized by X-Ray diffraction (XRD), scanning electron microscopy (SEM), Fourier transformed infrared spectra (FTIR) and high-resolution transmission electron microscopy (HRTEM). The XRD analysis indicates that the crystallization of GaN film fabricated on TiO₂ middle layer is rather excellent. The FTIR, SEM and HRTEM demonstrate that these nanorods are hexagonal GaN and possess a rough morphology with a diameter ranging from 200 nm to 500 nm and a length less than 10 μm, the growth mechanism of crystalline GaN nanorods is discussed briefly.     

Synthesis of GaN nanorods by ammoniating Ga2O3 films on In2O3 layer deposited on Si (111) substrates

GaN nanorods were synthesized by ammoniating Ga₂O₃/In₂O₃ thin films deposited on Si (111) with magnetron sputtering. X-ray diffraction, Scanning electronic microscope and high-resolution TEM results show that they are GaN single crystals, the sizes of which vary from 2 to 7 μm in length and 200 to 300 nm in diameter. In₂O₃ middle layer plays an important role in the GaN nanorod growth.     

N2 decomposition by hot wire and N2 post-deposition treatment on hydrogenated microcrystalline silicon thin films

Post-deposition treatment of hydrogenated microcrystalline silicon (µc-Si:H) was carried out using a hot wire in atmospheres of N₂, N₂/H₂ or H₂ and the states of the bonds in the µc-Si:H films were investigated using X-ray photoelectron spectroscopy. For the µc-Si:H film treated in N₂ at the filament temperature (T_f) of 1600 °C, a weak N1s peak was observed. It increased slightly with increasing T_f from 1600 to 1900 °C and increased dramatically with increasing T_f from 1900 to 2000 °C. The N1s peak of the µc-Si:H film treated in N₂/H₂ at T_f = 2000  °C was one order of magnitude lower than that in N₂ at T_f = 2000 °C. These findings indicate that N₂ molecules decompose on the heated filament and that the addition of H₂ prevents N₂ decomposition.     

Wet chemical route to transparent BiFeO3 films on SiO2 substrates

BiFeO₃ nanoparticles were prepared by a wet chemical synthesis method. Transparent films were deposited on glass and quartz substrates by dip and spin coating processes from the synthesized sol. We obtained thicker films (~ 2 µm) by dip coating process and thinner films (~ 200 nm) by spin coating process. Transmission electron microscopy images confirmed that the particles are nanocrystalline in size. From the optical transmittance spectra the band gap of the BiFeO₃ nanoparticles was determined in the range of ~ 3.03-2.88 eV (~ 410-430 nm). Electrical resistivity, polarization, zero-field-cooled and field-cooled magnetizations versus temperature characteristics were also studied for these films.     

Diamond films deposited on WC-Co substrates by use of barrier interlayers and nano-grained diamond seeds

Results on the structure, composition and properties of diamond films deposited onto WC-Co cemented carbides via special multilayer barrier interlayers preliminary seeded by nano-grained diamond particles are presented. The barrier interlayers comprise a layer adjacent to the substrate, which completely prevents substrate decarburization and Co diffusion from the substrate, and a diamond-bonding layer needed to obtain an enhanced adhesion of the PACVD diamond coating. Preliminary seeding the barrier interlayers with nano-grain diamond particles by use of a laser ablation technique allows a fine-grained, uniform and highly adherent diamond coating of high quality to be deposited by use of a conventional PACVD technique. Results on the nature of the interaction between the diamond nano-grained seeds and barrier interlayer are also presented.     

氨化温度对氨化Si基Ga2O3/Cr膜制备GaN纳米结构的影响

采用磁控溅射的方法在Si(111)衬底上溅射沉积Ga2O3/Cr膜,并通过氨化的方法在Si(111)衬底上成功合成了六方纤锌矿GaN纳米结构材料,研究了不同的氨化温度对合成GaN纳米材料的影响.采用扫描电子显微镜(SEM)、X射线衍射仪(XRD)、透射电子显微镜(TEM)、高分辨透射电子显微镜(HR-TEM)、傅里叶红外吸收(FTIR)光谱来检测样品的形态,结构和成分,并且讨论了GaN纳米结构的生长机理.研究结果表明,在Cr催化合成GaN纳米结构的过程中,氨化温度对其有重要影响,最佳温度是950℃.     

Electroless deposition of superconducting MgB2 films on various substrates

The superconducting properties of magnesium diboride (MgB₂) films prepared by electroless deposition on various substrates including silver, gold and silicon are reported. In this study, MgB₂ films were fabricated on silver, gold, and silicon using an electroless plating technique, while controlling the redox potential to improve the deposition quality. The structure, morphology, and superconducting properties of the samples were investigated using X-ray diffraction, magnetometry, scanning electron microscopy, and Raman spectroscopy. X-ray diffraction and Raman spectroscopy confirmed that the films are polycrystalline MgB₂ but also contain some impurity phases. All the MgB₂ films show superconducting transitions near 39 K, the value for bulk MgB₂, with the superconducting volume fraction ranging from approximately 1 to 2%. We find a strong dependence of film quality with the oxidation potential of the bath.     

Deposition of HfO2 thin films on ZnS substrates

HfO₂ thin films with columnar microstructure were deposited directly on ZnS substrates by electron beam evaporation process. SiO₂ thin films, deposited by reactive magnetron sputtering, were used as buffer layers, HfO₂ thin films of granular microstructure were obtained on SiO₂ interlayer by this process. X-ray diffraction patterns demonstrate that the as-deposited HfO₂ films are in an amorphous-like state with small amount of crystalline phase while the HfO₂ films annealed at 450 °C in O₂ for 30 min and in Ar for 150 min underwent a phase transformation from amorphous-like to monoclinic phase. Antireflection effect in certain infrared wave band, such as 3–6 μm, 4–12 μm, 4–8 μm and 3–10 μm, can be observed, which was dependent on the thickness of thin films. The cross-sectional images of HfO₂ films, obtained by field emission scanning electron microscopy, revealed that there was no distinct morphological change upon annealing.     

Deposition of GaN films on (1 1 1) Si substrates by alternate supply of TMG and NH3

GaN films were grown on (1 1 1) Si substrates at 1000 °C by separate admittances of trimethylgallium (TMG) and ammonia (NH₃). To achieve high quality GaN films, the optimization in growth temperature and layer thickness of AlN buffer layer between GaN film and Si substrate is required. Cross-sectional transmission electron microscopic observations of the GaN/(1 1 1)Si samples show a nearly parallel orientation relationship between the (0 0 0 1) planes of GaN film and the (1 1 1) planes of Si substrate. Room temperature photoluminescence spectra of high quality GaN films show a strong near band edge emission and a weak yellow luminescence. The achievement of high quality GaN films on (1 1 1) Si substrates is believed to be attributed to enhancement in surface mobilities of the adsorbed surface species and adequate accommodation of lattice mismatch between high temperature AlN buffer layer and Si substrate.     

Ferroelectric properties of Bi3.4Dy0.6Ti3O12 thin films crystallized in N2

Bi_3.4Dy_0.6Ti₃O₁₂ (BDT) ferroelectric thin films were deposited on Pt/Ti/SiO2/Si substrates by chemical solution deposition (CSD) and annealed in an N₂ environment after pre-annealing in air at 400 °C. The effect of crystallization temperature on the structural and electrical properties of the BDT films was studied. The BDT films annealed in N₂ in the temperature range of 600 °C to 750 °C were crystallized well and the average grain size increased with increasing crystallization temperature, while the remanent polarization of the films is not a monotonic function of the crystallization temperature. The BDT films crystallized at 650 °C have the largest remanent polarization value of 2P_r = 39.4 μC/cm², and a fatigue-free characteristic.     

Investigation on the structure of TiO2 films sputtered on alloy substrates

Titanium dioxide (TiO₂) films have been successfully deposited on metal alloy substrates by radio-frequency magnetron reactive sputtering in an Ar+O₂ gas mixture. The effects of gas total pressure on the structure and phase transition of TiO₂ films were studied by X-ray diffraction and Raman spectra. It is suggested that the film structure changes from rutile to anatase while work gas total pressure changes from 0.2 to 2 Pa. The structure of TiO₂ films is not affected by the film thickness.     

Effect of N2 sintering atmosphere on the hardness of sol-gel films of 3 mol% Y2O3-stabilized ZrO2

A one-pot approach to hardening ZrO₂-based films prepared by the sol-gel method is presented. It entails performing the sintering in a nitrogen atmosphere, instead of in the conventional air atmosphere. It is shown that, when the sintering temperature is high enough, gas nitriding takes place in the ceramic film, leading to a 15% increase in its hardness. This occurs because more nitrogen solutes are incorporated into the crystal lattice of the 3YSZ host, forming solid solutions (i.e., greater solid-solution-effect hardening). The proposed gas nitriding is simple and cost-effective, and adds no additional steps to the processing routine. This suggests that it may have an important role to play in the fabrication of hard ceramic films from liquid precursors.     

A study of textured non-stoichiometric MoTe2 thin films used as substrates for textured stoichiometric MoS2 thin films

Textured MoTe₂ films have been prepared by sequential evaporation of the constituents followed by annealing under a tellurium pressure. The films are systematically textured with the c-axis of the crystallites perpendicular to the plane of substrate, however, the film composition is difficult to control and even after process optimization the films are tellurium deficient. This is thought to be caused by the electro negativity difference of the constituents.The textured MoTe₂ films have been used as substrates on which to grow MoS₂ films by annealing under a pressure of sulfur that allows textured MoS₂ films to be grown with good crystalline properties. The presence of sulfur at the surface and annealing under dynamic vacuum is important for this process and moreover, suppresses the superficial oxidation of the Mo and Te constituents.