Structural and electrical resistivity characteristics of vacuum arc ion deposited zirconium nitride thin films

Zirconium nitride (ZrN) thin films were grown on glass and aluminum substrates using a dual cathodic arc ion deposition technique. The effects of various negative bias voltages and flow ratios of N₂/Ar on the stoichiometric ratio of nitrogen to zirconium (N/Zr), deposition rate, structure, surface morphology and electrical resistivity of the ZrN layer were investigated. Rutherford backscattering spectroscopy measurements indicated a drop in the deposition rate and a slight increase in stoichiometric ratio (N/Zr) with the increase of bias voltage up to −400 V, although the latter still remained slightly less than unity (~0.92). Deposition rate of the film showed an increase with the argon addition. X-ray diffraction patterns depicted mostly polycrystalline nature of the films, with preferential orientation of (2 0 0) planes in the −100 V to −300 V bias voltage range. For 70–50% nitrogen and at a bias voltage of −400 V, the (1 1 1) orientation of ZrN film predominated. The films were smoother at a lower bias of −100 V, while the roughness increased slightly at a higher bias voltage possibly due to (increased) preferential re-sputtering of zirconium-rich clusters/islands. Changes in the resistivity of the films were correlated with stoichiometry, crystallographic orientation and crystalline quality.     

Effect of substrate biasing and temperature on AlN thin film deposited by cathodic arc ion

Aluminum nitride (AlN) films have been grown in pure N₂ plasma using cathodic arc ion deposition process. The films were prepared at different substrate bias voltages and temperatures. The aim was to investigate their influence on the Al macro-particles, structural and optical properties of deposited films. X-ray diffraction (XRD), Fourier transform infrared spectroscopy (FTIR), Raman spectroscopy, Scanning electron microscope (SEM) and Rutherford backscattering spectrometry (RBS) were employed to characterize AlN thin films. XRD patterns indicated the formation of polycrystalline (hexagonal) films with preferential orientation of (002), which is suppressed at higher substrate bias voltage. FTIR and Raman spectroscopic analysis were used to assess the nature of chemical bonding and vibrational phonon modes of AlN thin films respectively. FTIR spectra depicted a dominant peak around 850 cm^?1 corresponding to the longitudinal optical (LO) mode of vibration. A shift in this LO mode peak towards higher wavenumbers was observed with the increase of substrate bias voltage and temperature, showing the upsurge of nitrogen concentration in the deposited film. Raman spectra illustrated a peak at 650 cm^?1 corresponding to E₂ (high) phonon mode depicting the c-axis oriented (perpendicular to substrate) AlN film. SEM analysis showed the AlN film deposited at higher substrate bias voltage contains fewer amounts of Al macro-particles.     

The properties of annealed AlN films deposited by pulsed laser deposition

AlN films deposited on SiC or sapphire substrates by pulsed laser deposition were annealed at 1200°C, 1400°C, and 1600°C for 30 min in an inert atmosphere to examine how their structure, surface morphology, and substrate-film interface are altered during high temperature thermal processing. Shifts in the x-ray rocking curve peaks suggest that annealing increases the film density or relaxes the films and reduces the c-axis Poisson compression. Scanning electron micrographs show that the AlN begins to noticeably evaporate at 1600°C, and the evaporation rate is higher for the films grown on sapphire because the as-deposited film contained more pinholes. Rutherford backscattering spectroscopy shows that the interface between the film and substrate improves with annealing temperature for SiC substrates, but the interface quality for the 1600°C anneal is poorer than it is for the 1400°C anneal when the substrate is sapphire. Transmission electron micrographs show that the as-deposited films on SiC contain many stacking faults, while those annealed at 1600°C have a columnar structure with slightly misoriented grains. The as-deposited films on sapphire have an incoherent interface, and voids are formed at the interface when the samples are annealed at 1600°C. Auger electron spectroscopy shows that virtually no intermixing occurs across the interface, and that the annealed films contain less oxygen than the as-grown films.     

Effect of electron irradiation on morphological,compositional and electrical properties of nanocluster carbon thin films grown using room temperature based cathodic arc process for large area microelectronics

The influence of 8 MeV electron beam bombardment on room temperature grown nanocluster carbon using cathodic arc process has been studied here. Atomic force microscopy (AFM) study shows that surface roughness varies with varying electron doses. High doses of electrons could causes thermal induce graphitization and morphological changes in the films. Raman spectroscopy analysis reveals that G-peak vary from 1555 cm⁻¹ to 1570 cm⁻¹ and D-peak varying from 1361 cm⁻¹ to 1365 cm⁻¹ indicating the disorderness and presence of both graphitic and diamond-like phases. Room temperature conductivity changes by two to three orders in magnitude. The conductivity in the films could be due to conduction of charge carriers through neighboring islands of conductive chains. Defect states calculated using the differential technique varies from 8 × 10¹⁷cm⁻³ eV⁻¹ to 1.5 × 10¹⁹ cm⁻³ eV⁻¹. Irradiation of nanocluster carbon thin films could be helpful to tune the electrical properties and defect densities of the nanocluster carbon films for various large area, flexible electronic and nano electronic applications.     

Raman scattering of polycrystalline 3C-SiC film deposited on AlN buffer layer by using CVD with HMDS

This paper presents the Raman scattering characteristics of poly (polycrystalline) 3C-SiC thin films deposited on AlN buffer layer by atmospheric pressure chemical vapor deposition (APCVD) using hexamethyldisilane (MHDS) and carrier gases (Ar+H₂). The Raman spectra of SiC films deposited on AlN layer of before and after annealing were investigated according to the growth temperature of 3C-SiC. Two strong Raman peaks, which mean that poly 3C-SiC admixed with nanoparticle graphite, were measured in them. The biaxial stress of poly 3C-SiC/AlN was calculated as 896 MPa from the Raman shifts of 3C-SiC deposited at 1180 °C on AlN of after annealing.     

AlN薄膜有源SAW滤波器集成及性能研究

在AlN压电薄膜上(以SiO2/Si为衬底),使用MOS集成电路工艺制作叉指电极和单元电路,制成中心频率为320MHz的有源SAW滤波器并进行了测试。结果表明,该滤波器的插入损耗低于10dB,带外衰减高于45dB。     

离子束增强沉积AlN薄膜的研究

利用离子束增强沉积9IBED）法成功地在Si(100）衬底上合成了大面积均匀的非晶AlN薄膜。XRD和XPS测试结果证实该薄膜为非晶且无单质Al和N2存在,随着Al蒸发速率的提高,N/Al下降,在0.05nm/s及0.10nm/s的蒸发速率下制得的薄膜N／Al分别为0.402:1和0.250:1。SRP测试结果表明,随着Al蒸发速率的提高,表面电阻下降,并助在0.05nm/s的速率下制得的薄均匀致密,表面电阻高于10^8Ω,性能良好,而当蒸发速率≥0.25nm/s时,薄膜绝缘性能迅速下降。AFM分析显示薄膜呈岛状分布,且0.05nm/s制取的样品表面呈鹅卵石密堆积,颗粒均匀,表面比0.10nm/s样品起伏平缓、光滑,薄膜的生长机制可能是三维岛状生长。     

c轴择优取向AlN薄膜的制备研究

采用MOCVD法在蓝宝石(0001)单晶衬底上生长AlN压电薄膜。用XRD和原子力显微(AFM)技术表征薄膜的微观结构。研究了衬底温度、TMA和NH3流量、反应室气压对AlN薄膜织构特性的影响,并对薄膜生长的工艺参数进行了相应优化。结果表明:在优化条件下制备的AlN薄膜高度c轴择优取向,(0002)峰摇摆曲线半高宽仅为0.10°,且薄膜表面平整,椭圆偏振法测出其折射率为2.0～2.4。     

The significant effect of film thickness on the properties of chalcopyrite thin absorbing films deposited by RF magnetron sputtering

In this paper, thickness dependent structural, surface morphological, optical and electrical properties of RF magnetron sputtered CuIn_0.8Ga_0.2Se₂ (CIGS) thin films were studied using X-ray diffraction (XRD), Transmission electron microscopy (TEM), Field emission scanning electron microscopy (FE-SEM), Atomic force microscopy (AFM), UV–vis–NIR spectrophotometer and Keithley electrical measurement unit. The peak intensity along (112) plane as well as crystallite size was found to increase with thickness. However, for higher film thickness >1.16 μm, crystallinity reduced due to higher % of Cu content. TEM analysis confirmed pollycrysallinity as well as chalcopyrite phase of deposited films. The band gap was found to decrease with increase in thickness yielding a minimum value of 1.12 eV for film thickness 1.70 μm. The I–V characteristics showed the ohmic behavior of metal semiconductor contact with higher conductivity for film thickness 1.16 μm.     

磁过滤阴极真空弧沉积薄膜研究

采用磁过滤阴极真空弧沉积技术对从弧源引起离子束中的大颗粒进行过滤后,在硅和聚合物表面进行离子注入和低能离子束沉积,可获得特性优异的沉积金属膜、超硬膜（类金刚石,CN膜）、陶瓷膜（TiN,TiC）等。电子显微镜观察表明,大颗粒已被过滤,表面结构致密,由于先进行离子注入,在基体表现预先形成了过滤层,从而改善了沉积膜的粘合特性,膜与基体的粘合特性有了明显提高。测量结果表明,沉积膜的硬度、抗磨损和抗腐蚀特性均有了明显提高。非晶金刚石薄膜表面硬度可达到56GPa。     

Mo基底的粗糙度对C轴择优取向AlN的影响

通过物理气相沉积的方法制备出Si／非晶／Mo／AlN多层膜器件,利用透射电子显微学方法研究了截面样品和AlN薄膜平面样品,确定了AlN和 Mo的界面形态和生长方式。研究表明二者取向关系为[2110] AlN／／[111]Mo,（0002）AlN／／（110）Mo,且Mo表面的粗糙程度对AlN的生长有影响,因此本文为改进器件性能提供了参考方向。     

衬底温度对AlN薄膜结构及电阻率的影响

采用直流反应磁控溅射法在Si(111)基片上制备了AlN薄膜,利用XRD、原子力显微镜(AFM)、电流-电压(I-V)测试仪等对不同衬底下制备薄膜的结构、形貌及电阻率等进行了分析表征。结果表明:随着衬底温度的升高,晶粒逐渐长大,AlN(002)择优取向明显改善,600℃达到最佳。一定范围内提高温度使晶粒均匀、致密,有利于改善表面粗糙情况和提高电阻率,550℃时表面粗糙度达到最低(2.8 nm)且有最大的电阻率(3.35×1012Ω.cm);同时薄膜应力随温度升高有增大趋势。     

直接氮化法制备单晶AlN纳米线

采用直流电弧放电装置,通过金属铝和氮气直接反应,在钼阴极上沉积出大量的AlN纳米线。利用XRD、SEM、TEM和拉曼(Raman)光谱对所制样品的结构、形貌和光学特性进行了表征。结果表明:大部分AlN纳米线沿着[001]方向生长,平均直径为45nm,长度5μm左右;Raman光谱的峰值与单晶体材料AlN的结果一致,说明AlN纳米线结晶质量较好。     

HVPE法生长AlN薄膜材料

利用自制立式HVPE设备,在蓝宝石衬底上进行了不同载气情况下AlN的生长试验,生长温度1 000℃。在采用H2作载气情况下,由于预反应严重,没能生长出AlN薄膜,只得到一些白色AlN粉末;而在分别采用Ar和N2作载气的情况下,则成功生长出AlN薄膜,但由于生长温度低,AlN生长均为岛状生长模式。在生长速率较快时,AlN薄膜是以〈0001〉AlN为主的AlN多晶;而在较低生长速率下,得到的AlN薄膜由为〈0001〉取向的AlN岛组成。试验还发现:用Ar作载气更有利于AlN晶核的横向生长,用N2作载气则有相对高得多的AlN成核密度。     

电弧离子镀薄膜中的颗粒尺寸及其影响的扫描电镜观察

用扫描电镜对比分析了电弧离子镀增加直线磁场过滤对沉积TiN和TiAIN薄膜中颗粒的密度和尺寸的影响。结果表明,TiN薄膜中颗粒的最大直径,从14μm减小到3μm,颗粒密度从10^9／cm。降低到10^5／cm^2。TiAIN薄膜由于靶材中含有低熔点金属AI,因而发射出更大的颗粒,有的颗粒集团达到20／μm,磁场过滤后颗粒尺寸减小,颗粒密度降低到10^6／cm^2。分析了脉冲叠加直流偏压对TiCrZrN复合薄膜相组成的影响。颗粒可使电弧离子镀TiN／CrN多层膜的结合力降低,并使针孔产生遗传。使用直线型磁场过滤及脉冲叠加直流偏压不仅使颗粒密度和尺寸显著降低和减小,而且多层化对小颗粒产生了包覆作用。     

AlN薄膜体声波谐振器性能分析

采用体硅微细加工工艺制备了背空腔型AlN薄膜体声波谐振器。研究了压电层、上电极及支撑层厚度对谐振器性能的影响。测试结果表明,谐振器所用AlN压电薄膜具有(002)择优取向,器件频率特性良好。当上电极、压电层、底电极和支持层的厚度分别为110,2600,110,200nm时,谐振频率为1.759GHz,机电耦合系数3.75%,品质因数79.5。结合Mason等效电路模型模拟分析与实验结果,分析了各层厚度对频率特性的影响机理。     

脉冲激光沉积制备TiN/AlN多层膜的变形机理研究

本文采用纳秒脉冲激光沉积法在单晶硅试样表面制备了调制周期为20nm和200nm的TiN/AlN硬质多层膜,通过有限元模拟和纳米压痕方法研究了调制周期对多层膜的开裂机理的影响。结果表明:调制周期200nm时,载荷致使能量表层积累形成应力集中,一定程度后界面应变梯度劣化促使界面裂纹萌生、扩展。载荷继续增加后,主裂纹沿纵向扩展,其两侧也形成新的应力集中区,原有应力释放。薄膜应力近表层的应力集中超过多层膜的强度极限时,多层膜表层发生开裂。调制周期20nm时,加载诱导应力沿着AlN软膜向多层薄膜内部传递,能量在纵深方向累积储存,直至超过薄膜的屈服极限时,多层膜内部损伤失效。     

AlN基板用厚膜浆料发展评述

介绍了AlN基片所用厚膜浆料的产品性能。从金属粉体的制备,粘结方式探索和烧结工艺的改进等方面综述了该领域的研究进展。目前粉体制备还是以化学还原为主。粘结方式中,玻璃相粘结具有较高的可靠性;反应粘结因导热性和热应力等方面的优势,使其成为AlN基板厚膜浆料粘结的重要方式。     

沉积在聚合物表面上的金属薄膜自发形成图案的实验研究

用离子溅射法在聚二甲基硅氧（polydimethylsiloxane,PDMS）表面沉积的金膜因金属与聚合物之间热膨胀系数的差异从而导致了具有正弦界面、微米尺度的波长和振幅的复杂而有序的褶皱图案。用光刘技术在硅片制备图形结构作为模板,通过复制模铸得到表面具有浮雕结构的聚二甲基硅氧烷基片。改变浮雕结构可以调控其上沉积的金膜的褶皱图案呈规则有序的排列。这种多尺度的复合结构将光刘技术、复制模铸和物理自组装等有效结合,可广泛应用于微纳制造领域。     

Deposition Characteristics of AlN Thin Film Prepared by the Dual Ion Beam Sputtering System

In this experiment, a radio frequency dual ion beam sputtering (DIBS) system was used to prepare aluminum nitride (AlN) films with a bottom Al electrode on a Si (100) substrate. After systematic testing of the processing variables, a high-quality film with preferred c-axis orientation was grown successfully on the Si (100) substrate with an Al target under 700 eV energy flux, N₂/(N₂ + Ar) ratio of 55%, and 4 × 10⁻⁴ torr in vacuum. The characteristics of the deposited AlN thin films were studied by x-ray diffraction (XRD), scanning electron microscope (SEM), transmission electron microscope (TEM), secondary ion mass spectrometry (SIMS), and electronic spectroscopy for chemical analysis (ESCA). The surface roughness was also measured. It was found that AlN films prepared by DIBS at room temperature are better than those prepared at 300°C, and those prepared with an Al target are better than those prepared with an AlN target. The inferiority of AlN films prepared with AlN targets is due to the AlN bond being broken down by the ion beam source.