Effect of substrate bias voltage on the texture and microstructure of Cu thin films deposited by ion beam deposition

Cu thin films deposited by non-mass separated ion beam deposition under various substrate bias voltages were investigated. The film textures and microstructure were analyzed by X-ray diffraction and field emission scanning electron microscopy, and the resistivity of the film was measured with the Van der Pauw method. It was found that the optimum negative substrate bias voltage for Cu films was −50 V. The Cu films deposited without substrate bias voltage showed a columnar grain structure with small grains and random orientation. However, when a substrate bias voltage of −50 V was applied, the Cu films had a non-columnar structure with a strong (111) texture and large grains. The electrical resistivity of the Cu films decreased remarkably with increasing negative substrate bias voltage, and reaching a minimum value of 1.8±0.13 μΩ cm at the substrate bias voltage of −50V.     

Nucleation of highly oriented diamond on silicon

Highly oriented diamond particles were deposited on the mirror-polished (100) silicon substrates in the belljar type microwave plasma deposition system. The diamond films were deposited by a three-step process consisting of carburization, bias-enhanced nucleation and growth. The bias-enhanced nucleation was performed under the deposition conditions such as 2-3% of methane concentration in hydrogen, 1333-2666 Pa of total pressure, the negative bias voltage below 200V and the substrate temperature of 1073 K. By adjusting the geometry of the substrate and substrate holder, very dense disc-shaped plasma was formed on the substrate when the bias voltage was below 200V. As characterized by transmission electron microscopy (TEM), almost perfectly oriented diamond particles were obtained only in this dense plasma. From the results of the optical emission spectra of disc-shaped dense plasma, it was found that the concentrations of atomic hydrogen and hydrocarbon radicals were increased with negative bias voltage. As a result, it was suggested that the highly oriented diamonds were obtained by the combination of the high dose of hydrocarbon radicals and the increased hydrogen etching effects.     

基片偏压对电弧离子镀ZrN薄膜微结构和表面形貌的影响(英文)

在不同的基片偏压下利用电弧离子镀技术制备氮化锆薄膜,以考察基片偏压对氮化锆薄膜微结构和表面形貌的影响。利用XRD、EPMA和FE-SEM等技术对不同偏压时得到ZrN薄膜的相结构、成分和表面形貌进行表征。结果表明,薄膜中存在立方氮化锆和六方纯锆相;随着基片偏压的增大,薄膜的择优取向由(111)变为(200),最后变为(111),晶粒尺寸由30nm减小至15nm。同时发现,随着基片偏压的增大,薄膜微结构由明显的柱状特征变为致密的等轴晶特征,表明由偏压增强的离子轰击能有效抑制柱状晶生长;薄膜沉积速率和锆氮摩尔比随着基片偏压的增大先增大后减小,在-50V时达到最大。     

基体脉冲偏压对TiN/Cu纳米复合薄膜组织结构、力学及耐磨性能的影响

本文采用轴向磁场增强电弧离子镀在高速钢基体上沉积了TiN/Cu纳米复合薄膜,研究了基体脉冲偏压幅值对薄膜成分、结构、力学性能及耐磨性能的影响。结果表明,薄膜中铜含量随着脉冲偏压幅值的增加先增加而后降低,在一个较低的范围内(1.3-2.1at.%)。X射线衍射结果表明所有的薄膜均出现TiN相,并未观察到Cu相。薄膜的择优取向随着脉冲偏压幅值的增加而改变。薄膜的最高硬度为36GPa,是在脉冲偏压幅值为-200V时得到的,对应了1.6at.%的Cu含量。与纯的TiN薄膜相比,Cu的添加明显增强了薄膜的耐磨性能。     

Influence of substrate bias on microstructure and morphology of ZrN thin films deposited by arc ion plating

Zirconium nitride thin films were fabricated using arc ion plating under negative substrate biases to investigate the influence of substrate bias on the ZrN films. The phase, composition, and surface morphology of the ZrN ?lms, with respect to substrate bias, were studied by XRD, EPMA, and FE-SEM, respectively. The results show that cubic ZrN and hexagonal Zr phases form in the ZrN films. The competition between surface energy and strain energy makes the preferred orientation change from (111) to (200) and then back to highly (111) preferred orientation as a function of substrate bias. With the increase of bias voltage, the crystallite size of ZrN films reduces from 30 to 15 nm. Meanwhile, the film microstructure evolves from an apparent columnar structure to a highly dense equiaxed structure, indicating that the ion bombardment enhanced by substrate bias can suppress the columnar growth in the ZrN films. Deposition rate and mole ratio of Zr to N increase with the increase of bias voltage and reach the maximum at –50 V, and then show a decline trend when bias voltage further increases.     

基片负偏压对Cu膜纳米压入硬度及微观结构的影响

测试了不同溅射偏压下Cu膜的纳米压入硬度，探讨了溅射偏压、残余应力及压痕尺寸效应对Cu膜硬度的影响。结果表明，随着溅射偏压的增大，薄膜晶粒尺寸及残余压应力均减小，导致薄膜的硬度增大，并在-80V达到最大值，随后有所降低。同时薄膜中的压痕尺寸效应对薄膜硬度随压入深度的分布有很大的影响。     

直流等离子体-热丝化学气相沉积金刚石薄膜的研究

通过在传统热丝化学气相沉积装置中引入直流等离子体,设计了直流等离子体-热丝化学气相沉积金刚石薄膜的设备,设备中既包括相互独立的灯丝电压和施加的偏压。通过调节偏压可以控制所形成的等离子体的偏流。在这一改进的系统中研究了金刚石薄膜形核和生长过程,利用扫描电子显微镜（SEM）、X射线衍射（XRD）分析了金刚石的样品,结果表明,施加偏压不仅能大大促进金刚石的形核密度（10^10cm^-2）、提高金刚石薄膜的生长速率,金刚石薄膜的取向也随机取向变为（111）定向生长。     

The effect of applied substrate negative bias voltage on the structure and properties of Al-containing a-C:H thin films

Al-containing hydrogenated amorphous carbon (Al-C:H) films were prepared using a magnetron sputtering Al target in the CH₄ and Ar mixture atmosphere with various applied substrate pulse negative bias voltages. The hydrogen content and internal stress of the film decrease dramatically with the substrate pulse bias voltage increase. However, the hardness values of the films keep at high level (∼ 20 GPa) without any obvious changes with the increase of the applied substrate pulse bias voltages. The Al-C:H film prepared at applied substrate high bias voltage shows a long wear life and low friction coefficient.     

Preparation of ZrO<Subscript>2</Subscript> dielectric layers by subsequent oxidation after Zr film deposition with negative substrate bias voltage

ZrO₂ dielectric layers were prepared by a two-step process, a deposition of pure Zr film with and without a negative substrate bias voltage and a subsequent oxidation of the Zr films. We focused on the effect of the negative substrate bias voltage on the Zr film deposition and the subsequent oxidation of the Zr films. As a result, the Zr film deposited at the substrate bias voltage of −50 V (Vs = −50 V) was found to have a high intensity peak of Zr (100) and a uniform and smooth surface. From the capacitance-voltage and current-voltage measurements of the ZrO₂ films, a high dielectric constant of 21 and the equivalent oxide thickness (EOT) of 2.6 nm were obtained on the oxidation layer of the Zr film deposited at Vs = −50 V. On the other hand, a low dielectric constant of 15 and the EOT of 3.6 nm was obtained on that of the Zr film deposited at Vs = 0 V. The leakage current density of the ZrO₂ film (Vs = −50 V) was 5.69×10⁻⁴ A/cm², and this value was much lower than the 1.21×10⁻⁴ A/cm² for the ZrO₂ film (Vs = 0 V). It was found that the two-step process by subsequent oxidation after film deposition using a negative substrate bias voltage is useful for obtaining high-quality dielectric layers.     

Study on nanocrystalline Cr2O3 films deposited by arc ion plating: I. composition, morphology, and microstructure analysis

Nanocrystalline Cr₂O₃ thin films were deposited on silicon wafers with (100) orientation by arc ion plating (AIP) technique at various negative bias voltages. By virtue of X-ray diffraction analysis, scanning electron microscope, and high-resolution transmission electron microscope, the influence of substrate bias voltage on the film growth process, microstructure, and characteristics was investigated systematically, including the phase constituents, grain size, lattice constant, chemical compositions, as well as surface and cross-section morphologies. With increasing the bias voltage, the grain size and lattice constant of AIP Cr₂O₃ films first decreased slightly, and then increased gradually again. Both reached the minimum (35 nm and 13.57 Å) when the bias voltage was − 100 V. However, the bias voltage had little effect on the phase constituents and chemical compositions of AIP Cr₂O₃ films. During the film growth process, the surfaces of Cr₂O₃ films were getting smoother with the negative bias voltage increase, in the meantime, their microstructures evolved from coarse columnar grains to fine columnar grains, short columnar recrystallized grains, and fine columnar grains again.     

Cu互连中Zr嵌入层对ZrN阻挡层热稳定性的影响

在不同的衬底偏压下,用射频反应磁控溅射的方法在Si(100)衬底和Cu膜间制备了ZrN/Zr/ZrN堆栈结构的阻挡层。研究了Zr层的插入对ZrN扩散阻挡性能的影响,结果表明:随着衬底偏压的升高,阻挡层的电阻率降低,ZrN呈(111)择优取向;Zr层的插入使ZrN阻挡层的失效温度至少提高100℃,750℃仍能有效地阻止Cu的扩散,阻挡性能提高的主要原因可能是高温退火时形成的ZrO2阻塞了Cu快速扩散的通道。     

阴极电弧制备TiAlN薄膜工艺参数的正交分析研究

为深入理解不同工艺参数对阴极电弧制备TiAlN薄膜性质的影响重要性,文中设计了L9(34)正交试验表,研究了基体负偏压、N2流量、阴极弧流对TiAlN沉积速率、表面粗糙度的影响,给出了工艺参数优化组合。结果表明:负偏压对TiAlN薄膜的沉积速率影响最大,其次是N2流量、弧流;对表面粗糙度的影响次序则为N2流量、弧流、负偏压。薄膜沉积速率随N2流量的升高而增大,随负偏压增加先增加后降低,随弧流的增大变化不明显。薄膜表面粗糙度随N2流量的升高逐渐减小,随负偏压的增加而增加,随弧流的增大而增大。     

负偏压对多弧离子镀制备的(Ti,Cr)N膜的影响

利用扫描电子显微镜、原子力显微镜等手段研究负偏压对多弧离子镀制备的(Ti,Cr)N薄膜表面缺陷、表面粗糙度、化学成分、沉积速率及硬度的影响。结果发现:随着负偏压的增加,(Ti,Cr)N薄膜的液滴受到抑制,表面粗糙度下降,沉积速率降低,硬度增加,但负偏压对薄膜的Cr含量影响较小。     

Synthesis and characterization of cubic boron nitride thin films using the ME-ARE method

Cubic boron nitride (cBN) films were deposited by a magnetically enhanced activated reactive evaporation (ME-ARE) technique. Pulsed DC instead of r.f. power was used to bias the substrate. The effect of deposition parameters such as substrate bias voltage, plasma discharge current and gas flow ratio on the formation of cBN was investigated. BN films were characterized by FTIR and TEM. CBN films with a high content of cubic phase were successfully synthesized. It was found that formation of cBN film requires the bombardment of ions with both high flux and high energy. TEM observation showed that the cBN film had grain sizes of 15-50 nm and that a non-cubic phase BN, 10-15 nm was initially grown.     

Influence of dc bias on amorphous carbon deposited by pulse laser ablation

Amorphous carbon films were deposited on single-crystalline silicon and K9 glass by pulse laser ablation using different negative substrate bias.Scanning electron microscope(SEM) was used to observe morphology of the surface.Thickness and refractive index of the film deposited on K9 glass were measured by ellipsometry.Micro-hardness of films was measured relatively to single crystal silicon.All films deosited on silicon were analyzed by Raman spectra.All spectra were deconvoluted to three peaks.Line-width ratios varied similarly with bias voltage when the laser energy was kept invariant.     

偏压对离子源辅助HiPIMS制备纳米TiN薄膜力学性能和耐蚀性能的影响

为提高磁控溅射制备薄膜的致密度,减少结构缺陷,研究薄膜显微结构对硬度、韧性及耐蚀性能的影响,尝试在改变离子源和基材偏压的条件下,采用离子源辅助HiPMIS技术在304不锈钢和P型（100）晶向硅片上制备TiN纳米薄膜。采用扫描电子显微镜、小角X射线衍射仪对薄膜的形貌和晶体结构进行分析;采用纳米压痕仪和维氏硬度计分别测量计算薄膜的硬度和韧性,并通过电化学工作站对薄膜的耐蚀性能进行检测。结果表明：随着偏压的增加以及离子源的引入,离子的轰击效应增强,薄膜的沉积速率下降,致密度增加。偏压为-200 V时,薄膜的硬度达到最大值16.2 GPa,且对应的晶粒尺寸最小,（111）晶面衍射峰的强度最高。离子源的加入使所制备薄膜的硬度略有下降。此外,随着偏压的增加,薄膜的韧性和耐腐蚀性能也有一定提高。     

Structure and properties of Ti–Al–Y–N coatings deposited from filtered vacuum-arc plasma

Ti_0.5Al_0.5N coatings with a small amount of Y (up to 1 at.%) were deposited by filtered vacuum arc plasma at pulsed high voltage negative substrate bias potential with amplitude up to 2.5 kV and their microstructure was studied. X-ray fluorescence analysis showed that this deposition method allows ensuring well the conformity of the elemental composition of the metallic components of cathodes and films. X-ray diffraction measurements of the films with yttrium revealed a solid solution (Ti,Al)N phase with a cubic NaCl-type structure as the only crystalline phase. The films deposited with an amplitude of the substrate bias potential in the range of 1–1.5 kV were characterized by a strong axial texture [110]. In these films an increase of the yttrium content leads to the reduction of the nitride lattice parameter and growth of coherent scattering zone dimension as well as to a decrease of the surface roughness. Coatings containing 1 at.% Y exhibited high hardness of 32–36 GPa and oxidation resistance.     

Effect of bias voltage on microstructure and nanomechanical properties of Ti films

In order to investigate nanomechanical properties of nanostructured Ti metallic material, pure Ti films were prepared by magnetron sputtering at the bias voltage of 0-140 V. The microstructure of Ti films was characterized by X-ray diffraction (XRD), scanning electron microscopy (SEM) and high-resolution transmission electron microscopy (HRTEM). It is interesting to find that the microstructure of pure Ti films was characterized by the composite structure of amorphous-like matrix embodied with nanocrystallines, and the crystallization was improved with the increase of bias voltage. The hardness of Ti films measured by nanoindentation tests shows a linear relationship with grain sizes in the scale of 6-15 nm. However, the pure Ti films exhibit a soft tendency characterized by a smaller slope of Hall-Petch relationship. In addition, the effect of bias voltage on the growth orientation of Ti films was discussed.     

Synthesis of cubic boron nitride thin films by low-energy ion beam assisted deposition by applying substrate bias

Cubic boron nitride (c-BN) films are synthesized with low-energy ions of 100eV from a gridless ion gun by applying negative substrate bias. Boron is evaporated by an electron beam at rates of 0.8 to 2.3Å/sec onto silicon substrate. Substrate temperature and bias are varied from 400 to 800°C and from 0 to -700V, respectively. Due to the low-operating pressure of the ion beam assisted deposition (IBAD) process, applying substrate bias efficiently accelerates ions enough for synthesis of the c-BN phase. With increasing substrate bias, the major phase changes in the sequence of hexagonal boron nitride (h-BN) to c-BN to h-BN. The reappearance of the hexagonal phase at high bias voltage is thought to be due to the stress annealing effect. Intermediate temperatures have produced higher c-BN contents. Far-off stoichiometric film (N/B≈0.72) consists of h-BN phase even under the c-BN parameter but a little off stoichiometry has led to higher c-BN contents. The maximum contents of c-BN phase is about 70%. DC type bias and oxygen/hydrogen incorporation into the films are presumed to limit the content. The IBAD process with proper substrate bias is promising for large areas of and high rate growth of the c-BN phase.     

Si和316L基片上TiN薄膜微观结构和应力的对比分析

目的 比较Si和316L基片上TiN薄膜的微观结构和应力,分析基片材料和基片初始曲率对薄膜应力的影响.方法 采用电弧离子镀技术在Si基片和316L基片上制备了TiN薄膜,实测了薄膜应力,通过XRD、SEM、TEM等方法对薄膜的微观结构进行了分析.运用有限元分析技术,以结构力学为原理,分别对不同初始曲率的Si基片和316...