Excimer laser-assisted planarization of thick diamond films

The planarization of polycrystalline diamond films is critical for a large number of industrial applications. We have investigated a laser-assisted method for planarization of thick diamond films. This method is based on the application of excimer laser combined with simultaneous rotation of the sample. Thick diamond films (average surface roughness: ∼20 μm and thickness ∼500 μm) were fabricated by plasma jet chemical vapor deposition process. The planarization of diamond films was found to be critically dependent on the angle of incidence of laser beam. Smoother surfaces were obtained at higher incidence angles (θ = 80°). However, by combination of sample rotation with laser irradiation at higher incidence angles (θ = 80°), maximum surface planarization was achieved. Under optimum conditions, the surface roughness of the samples were reduced from 20 to 0.1 μm. The mechanisms for surface planarization of thick diamond films are discussed.     

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.     

Microwave and hot filament chemical vapour deposition of diamond multilayers on Si and WC-Co substrates

A serious problem in the use of chemical-vapour-deposited polycrystalline diamond coatings in electronics, optics as well as in cutting tools is the high surface roughness. In our work, microcrystalline and nanocrystalline diamond films with a thickness of 0.5-5 μm were deposited using microwave chemical vapour deposition (MW CVD), and with a thickness of 1-4 μm by hot filament chemical vapour deposition (HF CVD). For both deposition technologies, we investigated the effect of a negative bias upon the formation of microcrystalline and nanocrystalline diamond multilayers. In the cases of smooth Si and relief WC-Co substrate surfaces, the multilayers were found to have a “cauliflower” look. The structure and composition of deposited layers were checked by scanning electron microscopy and Raman spectroscopy.     

异质外延立方氮化硼薄膜的微结构研究

利用离子束辅助沉积技术在金刚石薄膜衬底上制备立方氮化硼薄膜,傅立叶变换红外谱的结果表明,在高度(001)织构金刚石薄膜衬底上沉积的立方氮化硼薄膜是纯的立方相,而在多晶金刚石薄膜衬底上制备的立方氮化硼薄膜中还含少量的六角氮化硼。高分辨透射电镜的分析表明,在金刚石晶粒上异质外延的c-BN直接成核于金刚石衬底,界面没有六角氮化硼过渡层;而在含有大量缺陷的晶粒边界,存在六角氮化硼的成核与生长。     

The effects of substrate bias,substrate temperature,and pulse frequency on the microstructures of chromium nitride coatings deposited by pulsed direct current reactive magnetron sputtering

Recently, great attention has been devoted to the pulsed direct current (DC) reactive magnetron sputtering technique, due to its ability to reduce arcing and target poisoning, and its capability of producing insulating thin films. In this study, chromium nitride (CrN) coatings were deposited by the bipolar symmetric pulsed DC magnetron reactive sputtering process at different pulse frequency, substrate bias voltage, and the substrate temperature. It was observed that the texture of CrN changed from (111) to (200) as substrate temperature increased to 300°C as deposited at 2 kHz without substrate bias. With increasing pulsing bias and pulse frequency of target, predominated (200) orientation of CrN film was shown due to the ion bombardment/channeling effect to preferentially sputter those unaligned planes. For the CrN coatings deposited with pulsed biasing, the grain size decreased with increasing pulse frequency and substrate bias, whereas the surface roughness showed a reverse trend. The deposition rate of the CrN films decreased with increasing pulse frequency. It was concluded that the pulse frequency, substrate bias, and substrate temperature played important role in the texture, microstructure, and surface roughness of the CrN coatings deposited by the pulsed DC magnetron sputtering process.     

Improvement of diamond X-ray mask membrane: Optical transmittance, surface roughness and irradiation durability

A viable method for the improvement of the polycrystalline diamond X-ray mask membrane is proposed. The use of an ionized cluster beam yields the smoothest surface. Sol-gel planarization film coating with indium tin oxide is the most effective method for obtaining high optical transmittance without sacrificing high synchrotron irradiation durability.     

定向离子清洗对基片表面性质的影响

为提高高功率激光薄膜的抗激光损伤能力，研究了定向离子清洗对玻璃基片表面性质的影响。用End-Hall型离子源在不同清洗参数下对K9玻璃基片进行了清洗，用光学显微镜验证了基片的二次污染和离子的清洗效果，用静滴接触角仪测量了基片在离子清洗前后对水滴的接触角，用原子力显微镜和轮廓仪分别观测了不同参数的离子清洗前后的基片表面形貌和粗糙度，分析了基片清洗后表面性质如清洁、表面能、接触角、表面粗糙度、表面形貌的变化机理。研究表明定向离子清洗可有效去除二次污染、增加基片表面能、控制基片表面粗糙度和表面形貌，是一种有效改善基片表面性质的处理方法。     

微米金刚石聚晶薄膜场发射点的研究

采用微波等离子化学气相沉积方法,以甲烷和氢气为反应气体,在镀有金属钛的陶瓷衬底上,制备了微米金刚石聚晶薄膜.利用扫描电镜、拉曼光谱、X射线光电子能谱对薄膜的化学组成、微观结构和表面形貌进行了表征.用二级结构的场发射仪和扫描隧道显微镜研究了薄膜的场发射性能,结果表明微米金刚石聚晶薄膜发射点主要来源于聚晶颗粒.进一步研究了单个聚晶颗粒表面不同区域的发射性能,发现多种因素对场发射的性能有影响.     

In situ deposition of Au on plasma-prepared GaAs substrates

In situ deposition of single crystal epitaxial and textured polycrystalline gold films on plasma-cleaned or plasma-etched GaAs substrates is accomplished in an ultrahigh vacuum integrated processing facility. Au/GaAs samples are characterized using reflection high energy electron diffraction, Auger electron spectroscopy, and ion channeling. Au crystallinity in films deposited at 100° C is shown to strongly depend on the GaAs surface cleanliness after plasma processing. Heating the substrate to 250° C after plasma processing subsequently yields epitaxial Au films; omitting the heating procedure results in polycrystalline Au films. The substrate thermal treatment removes residual physisorbed gas molecules and reaction products from the GaAs surface. Epitaxial Au films contain significantly less Ga and As on the free surface of Au than polycrystalline films, and no interaction between epitaxial Au and GaAs is observed.     

Surface Control of Planarization Layer on Embossed Glass for Light Extraction in OLEDs

We developed a highly refractive index planarization layer showing a very smooth surface for organic light‐emitting diode (OLED) light extraction, and we successfully prepared a highly efficient white OLED device with an embossed nano‐structure and highly refractive index planarization layers. White OLEDs act as an internal out‐coupling layer. We used a spin‐coating method and two types of TiO₂ solutions for a planarization of the embossed nano‐structure on a glass substrate. The first TiO₂ solution was TiO₂ sol, which consists of TiO₂ colloidal particles in an acidic aqueous solution and several organic additives. The second solution was an organic and inorganic hybrid solution of TiO₂. The surface roughness (R_a) and refractive index of the TiO₂ planarization films on a flat glass were 0.4 nm and 2.0 at 550 nm, respectively. The J–V characteristics of the OLED including the embossed nano‐structure and the TiO₂ planarization film were almost the same as those of an OLED with a flat glass, and the luminous efficacy of the aforementioned OLED was enhanced by 34% compared to that of an OLED with a flat glass.     

磁存储器驱动电路界面平坦化研究

利用原子力显微镜（AFM）和扫描电镜（SEM）对磁存储器(MRAM)驱动电路与存储单元--磁性隧道结(MTJ)的连接界面的表面平坦化进行了研究. 原子力显微镜照片表明：磁控溅射沉积的金属铝膜的表面由尺寸约为300nm的颗粒组成，其表面粗糙度约为几十纳米的量级，用统计平均值（均方根值root mean square,RMS）描述约为10nm；在铝膜的表面沉积一层难溶金属Ti或Ta膜以后，可很好地改善过渡层金属表面的平坦化效果. 通过用化学机械平坦化设备(chemical mechanical planarization,CMP) 在小压力和低转速的条件下，可使过渡层金属表面的RMS值达到小于1nm的平坦化效果. 扫描电镜照片的结果也显示：利用光刻胶平坦化，然后通过调节反应离子刻蚀的条件，使刻蚀的过程中对氧化硅和光刻胶的刻蚀速率相等，去掉光刻胶，达到平坦化整个芯片表面的效果.     

ITO薄膜的电阻并联效应研究

采用电子束蒸发镀膜方法在K9玻璃基底上分别镀制了ITO/SiO₂/ITO,ITO/Ti₂O₃/ITO和ITO/MgF₂/ITO结构的多层薄膜,用四探针方块电阻仪测量薄膜表面的方块电阻,用原子力显微镜观测样品的表面微观形貌。结果显示,当ITO薄膜的粗糙度较大且介质薄膜的物理厚度小于100nm时,各层ITO薄膜之间通过山峰状的凸起结构相连通,导致样片表面的方块电阻测量值与各层ITO薄膜电阻的并联值相当。这表明,当ITO薄膜的粗糙度较大且介质薄膜厚度较小时,各层ITO薄膜表现出电阻并联效应。利用多层ITO薄膜的电阻并联效应设计并制备了450～1200nm超宽光谱透明导电薄膜,用四探针方块电阻仪测量了试验样片的表面方块电阻,用紫外-可见-近红外分光光度计测试了样片的光谱透射率。结果显示,在相同表面方块电阻条件下,相比于单层ITO薄膜,利用ITO薄膜电阻并联效应所制备的多层透明导电薄膜具有更高的光谱透射率。     

Preparation of CuInxGa1−xSe2 solar cells by electron beam evaporation of powdered evaporants

Cu(In,Ga)Se₂ (CIGS) thin films were deposited by electron beam evaporation of ball-milled powders containing various amounts of gallium. The effects of the gallium concentration in the Cu(In,Ga)Se₂ on the structure, surface morphology and optical properties of the films were investigated using X-ray diffraction, energy-dispersive X-ray analysis, atomic force microscopy and optical spectroscopy. All of the films, which were deposited at 450 °C, were polycrystalline and exhibited a chalcopyrite structure with a (112) preferred orientation. The optical constants of the films were calculated. The grain size, the roughness and the band gap increased with increasing amounts of gallium in the films. A glass/TCO/CdS/CIGS/Au solar cell with 12.87% efficiency was prepared directly from the powdered material.     

Defect formation in epitaxial oxide dielectric layers due to substrate surface relief

Defects were characterized in epitaxial (001) CeO₂ films deposited and planarizedin situ on patterned (001) LaAlO₃ substrates by ion beam assisted deposition (IBAD). A hill and valley structure with steps running parallel to the [100] LaAlO₃ axis was produced on the surface of the substrate by photolithography and ion beam etching prior to film deposition. A conformai epitaxial CeO₂ layer of ∼ 100 nm thickness was deposited on the heated substrate by e-beam evaporation. Lattice-matching between the e-beam film and the substrate was of the type: (001) CeO₂∥(001) LaAlO₃ and [110] CeO₂∥[100] LaAlO₃. Evaporative deposition of additional film onto the conformai layer was accompanied by bombardment with a 500 eV argon/oxygen ion beam to promotein situ planarization. Extreme lattice misfit for the orientation (001) CeO₂∥(001)LaAlO₃ and [001] CeO₂∥[001] LaAlO₃ caused formation of dislocations in the e-beam CeO₂ film in the vicinity of individual ledges in the substrate surface. Coherence of the CeO₂ film was locally lost in the step regions of the hill and valley structure. The large patterned steps, which are composed of numerous adjacent ledges in the LaAlO₃ surface, caused nucleation of CeO₂ with a tilt misalignment of up to ∼5‡ about the substrate [100]. Nucleation and growth of nonepitaxial CeO₂ crystallites was observed along the step regions of the film during the IBAD portion of deposition. Defect formation in the e-beam ceria layer due to substrate surface relief indicates that “lattice engineering≓ of multilayer epitaxial structures may not be possible when nonplanar surfaces are created during device fabrication. The IBAD CeO₂ layer was more defective than the conformai layer deposited without the impinging ion beam, even in the portions of the film where epitaxy was maintained throughout both layers.     

The development of biaxial alignment in yttria-stabilized zirconia films fabricated by ion beam assisted deposition

Yttria-stabilized zirconia (YSZ) films were deposited using ion assisted, electron beam deposition (IBAD) on Pyrex, quartz, Hastelloy, and polycrystalline zirconia substrates. Film orientation was studied as a function of IBAD fabrication conditions. Film texture from several populations of biaxially aligned grains has been observed. The ion beam is shown to induce biaxial alignment of all grain orientations. Specifically, grains with (200), (311), and (111) normal to the substrate surface are biaxially aligned. The ion beam induces biaxial alignment at all angles of incidence, not just those corresponding to YSZ channeling directions. The development of (200) biaxial alignment on Pyrex is examined as a function of thickness. Biaxially aligned IBAD YSZ films were deposited on amorphous and polycrystalline substrates without active heating. Biaxial alignment development with IBAD is shown to be consistent with a previously proposed growth and extinction model.     

Focused-ion-beam direct structuring of fused silica for fabrication of nano-imprinting templates

A dual beam scanning electron microscopy (SEM)/focused-ion-beam (FIB) system was used to pattern fused silica coated with a thin Cr layer. Features were characterised by atomic force microscopy (AFM) and SEM. The milled depth, surface roughness and the evolution of feature profiles as a function of ion fluence were investigated. It was found that the milled depth in fused silica substrates was linearly dependent on the ion fluence within the studied range. Features topography measurement revealed that after removing completely the Cr layer, an increase of the ion fluence resulted in a slight rise of surface roughness, however, the maximum root mean square (RMS) values were still less than 2.5 nm. More importantly, compared with the roughness of an unprocessed area on the substrate, an improvement of the surface finish of about 300% was obtained. The results demonstrated that FIB technology could be an alternative solution for producing nano-imprinting templates.     

H2 carrier gas dependence of Young's modulus and hardness of chemical vapor deposited polycrystalline 3C-SiC thin films

This paper presents the mechanical properties of poly (polycrystalline) 3C-SiC thin films according to 0%, 7%, and 10% carrier gas (H₂) concentrations using nano-indentation. When H₂ concentration was 10%, it has been proved that the mechanical properties, Young's modulus, and hardness of poly 3C-SiC films are the best of them. In the case of 10% H₂ concentration, Young's Modulus and hardness were obtained as 367 and 36 GPa, respectively. The surface roughness according to H₂ concentrations was investigated by AFM (atomic force microscope). When H₂ concentration was 10%, the roughness of 3C-SiC thins was 9.92 nm, which is also the best of them. Therefore, in order to apply poly 3C-SiC thin films to MEMS (micro-electromechanical system) applications, H₂ concentration's rate should increase to obtain better mechanical properties and surface roughness.     

Growth of WSi2 in phosphorous-implanted W/«Si» couples

The thermal reaction of rf-sputter-deposited tungsten films with a (100) silicon substrate is investigated by vacuum furnace annealing and rapid thermal annealing. An irradiation of the W/Si interface by a phosphorous ion beam at room temperature prior to annealing promotes a uniform interfacial growth of WSi₂. The growth of WSi₂ follows diffusion-controlled kinetics during both furnace annealing and rapid thermal processing. A growth law of x² = kt is obtained for furnace annealing between 690 and 740° C, where x is the thickness of the compound, t is the annealing duration after an initial incubation period and k = 62 (cm²/s) exp (−-3.0 eV/kT). The surface smoothness of the suicide films improves with increasing ion dose.     

热处理对离子束溅射SiO2薄膜结构特性的影响分析

采用离子束溅射沉积技术,在熔融石英基底上制备了SiO2薄膜,研究了热处理对离子束溅射SiO2薄膜结构特性的影响。热处理温度对表面粗糙度影响较大,低温热处理可降低表面粗糙度,高温热处理则增大表面粗糙度,选择合适的热处理温度,可以使表面粗糙度几乎不变。采用X射线衍射仪（XRD）物相分析方法,分析了热处理对离子束溅射SiO2薄膜的无定形结构特性的影响,当退火温度为550 ℃,离子束溅射SiO2薄膜的短程有序范围最大、最近邻原子平均距离最小,与熔融石英基底很接近,结构稳定。实验结果表明,采用合适的热处理温度,能大大改善离子束溅射SiO2薄膜的结构特性。     

Mechanistic study of borosilicate glass growth by low-pressure chemical vapor deposition from tetraethylorthosilicate and trimethylborate

A reaction mechanism and film morphology as a function of reactor conditions and post growth thermal annealing for borosilicate glass (BSG), (SiO₂)_x(B₂O₃)_1−x, films deposited from tetraethylorthosilicate (TEOS), trimethylborate (TMB), and oxygen (O₂) precursors by low-pressure chemical vapor deposition (LPCVD) was determined. An empirically derived reaction model for BSG film growth is proposed that predicts the growth rate and composition of BSG films up to 70 mole% B₂O₃. The BSG reaction model includes a strongly adsorbed TEOS-derived intermediate that forms SiO₂ and a direct surface reaction of TMB, in O₂, to form B₂O₃. This model is supported by growth rate and mass spectroscopic data. The BSG film morphology, investigated using atomic force microscopy, was found to have a root-mean-square roughness of 0.5 nm, with the precise film morphology being a function of reactor conditions. The BSG film roughness increases with film thickness, temperature, and boron content. Thermal annealing of the films in a water-free environment leads to planarization of the BSG governed by the film composition and anneal temperature.