This review paper covers a topic of significant importance in micro- and nano-systems development and manufacturing, specifically the residual stresses in deposited thin-film material layers and methods to control or mitigate their impact on device behavior. A residual stress is defined as the presence of a state of stress in a thin-film material layer without any externally applied forces wherein the residual stress can be compressive or tensile. While many material properties of deposited thin-film layers are dependent on the specific processing conditions, the residual stress often exhibits the most variability. It is not uncommon for residual stresses in deposited thin-film layers to vary over extremely large ranges of values (100% percent or more) and even exhibit changes in the sign of the stress state. Residual stresses in deposited layers are known to be highly dependent on a number of factors including: processing conditions used during the deposition; type of material system (thin-films and substrate materials); and other processing steps performed after the thin-film layer has been deposited, particularly those involving exposure to elevated temperatures. The origins of residual stress can involve a number of complex and interrelated factors. As a consequence, there is still no generally applicable theory to predict residual stresses in thin-films. Hence, device designers usually do not have sufficient information about the residual stresses values when they perform the device design. Obviously, this is a far less than ideal situation. The impact of this is micro- and nano-systems device development takes longer, is considerably more expensive, and presents higher risk levels. The outline of this paper is as follows: a discussion of the origins of residual stresses in deposited thin-film layers is given, followed by an example demonstrating the impact on device behavior. This is followed by a review of thin-film deposition methods outlining the process parameters known to affect the resultant residual stress in the deposited layers. Then, a review of the reported methods used to measure residual stresses in thin-films are described. A review of some of the literature to illustrate the level of variations in residual stresses depending on processing conditions is then provided. Methods which can be used to control the stresses and mitigate the impact of residual stresses in micro- and nano-systems device design and fabrication are then covered, followed by some recent development of interest.

/pdf/review-paper-residual-stresses-in-deposited-thin-film-13d0oo4h.pdf

Review Paper: Residual Stresses in Deposited Thin-Film Material Layers for Micro- and Nano-Systems Manufacturing

Nano-multilayered films offer a multilayer structure arrangement at several to tens of nanometers. They have hardness, high-temperature oxidation resistance, and low wear rates, making them popular in surface protection fields, such as engineering machinery, cutting tools and molds, and electronic instruments. This paper reviews recent research progress on nano-multilayered films, including their general types, preparation methods, microstructures, mechanical properties, and corrosion resistance. Furthermore, the mechanisms of the high hardness and toughness in nano-multilayered films are analyzed in detail. The future research directions for designing nano-multilayered films with improved strengthening and toughening properties are discussed. 

A review on microstructures and mechanical properties of protective nano-multilayered films or coatings

Residual stress in electroplated hard magnetic layers is crucial to the stability and durability in end applications. We electrodeposited highly HCP (002) textured CoMnP hard magnetic layers on copper substrate. We characterized and compared the residual stresses of mono- and multi-layered configurations using sin2ψ X-ray diffraction (XRD) for the apparent crystallite stress (σXRD), and curvature measurement methods for the macro-stress (σf). Intermediate Cu layer having a fixed thickness of 1.4 μm was introduced as a stress reliever for the multilayered CoMnP/Cu through sequential electrodeposition. In multilayers, thickness of all single magnetic layers was added to around ~20 μm similar to that of a monolayer. The surface morphology, layer composition and microstructure remain the same regardless of individual CoMnP single layer thickness. XRD results of ϕ-scan and ψ-scan depict the transversely isotropic CoMnP layers are under an equi-biaxial stress status, making a simplified analytical solution of sin2ψ method. The residual stresses measured by XRD sin2ψ method have been correlated with those acquired by curvature method. Increasing the number of layers from 2, 3 to 6 in the CoMnP/Cu multilayers reduces the σXRD by 8.3%, 25%, 33%, respectively; while the σf by 7.7%, 15% and 23%, respectively, as compared to those of the CoMnP mono-layer. These reductions are attributed to the released strain energy due to soft interlayer confinement and stacking fault formation. Elaborated includes unambiguous understandings of residual stress and microstructures for the electrodeposited CoMnP layers. 

Residual stress analysis of electrodeposited thick CoMnP monolayers and CoMnP/Cu multilayers

A novel diffusion barrier of electrodeposited CoWP layer between copper and silicon: Preparation and Performance

CO is the key reaction intermediate in the Cu-catalyzed electroreduction of CO2 to products containing C–C bonds. Herein, we investigate the impact of the particle size of CuO precursors on the direct electroreduction of CO (CORR) to C2+ products. Flame spray pyrolysis was used to prepare CuO particles with sizes between 4 and 30 nm. In situ synchrotron wide-angle X-ray scattering (WAXS), quasi-in situ X-ray photoelectron spectroscopy, and transmission electron microscopy demonstrated that, during CORR, the CuO precursors transformed into ∼30 nm metallic Cu particles with a crystalline domain size of ∼17 nm, independently of the initial size of the CuO precursors. Despite their similar morphology, the samples presented different Faradaic efficiencies (FEs) to C2+ products. The Cu particles derived from medium-sized (10–20 nm) CuO precursors were the most selective to C2+ products (FE 60%), while those derived from CuO precursors smaller than 10 nm displayed a high FE to H2. As the oxidation state, the particle and the crystallite sizes of these samples were similar after CORR, the differences in product distribution are attributed to the type and density of surface defects on the metallic Cu particles, as supported by studying electrochemical oxidation of the reduced Cu particles during CV cycling in combination with synchrotron WAXS. Cu particles derived from <10 nm CuO contained a higher density of more under-coordinated defects, resulting in a higher FE to H2 than Cu particles derived from 10 to 30 nm CuO. Bulk oxidation was most prominent and stable for Cu particles derived from medium-sized CuO, which indicated the more disordered nature of their surface compared to Cu particles derived from 30 nm CuO precursors and their lower reactivity compared to Cu particles derived from small CuO. Cu particles derived from <10 nm CuO initially displayed intense redox behavior, quickly fading during subsequent CVs. Our results evidence the significant restructuring during the electrochemical reduction of CuO precursors into Cu particles of similar size. The differences in CORR performance of these Cu particles of similar size can be correlated to different surface structures, qualitatively resolved by studying surface and bulk oxidation, which affect the competition between CO dimerization to yield C2+ products and undesired H2 evolution.

Restructuring of Cu-based Catalysts during CO Electroreduction: Evidence for the Dominant Role of Surface Defects on the C2+ Product Selectivity

Electrodeposited hard magnetic thick films have vast applications in the microelectromechanical systems (MEMS). Yet the very large residual stresses (σr) built-up in monolayered thick magnetic films leads to cracks, dimensional changes and deteriorated magnetic properties. Here, we explored quantitatively magnetic properties of CoMnP/Cu multilayers tuned by σr, which in turn are varied by the inserted soft Cu interlayer and thickness of single CoMnP magnetic layers. The configuration of the multilayers is an alternating CoMnP/Cu on Cu-substrate. The thickness of Cu interlayer was 1.4 μm. We kept a sum of all magnetic layers in the multilayers at ∼20 μm to benchmark with a 19.4 μm monolayered CoMnP. The magnetic layers are 94 wt.% Co and possess highly textured (002) hexagonal close packed microstructures. We characterized the apparent crystallite stresses through sin2ψ method by X-ray diffractometer (XRD) and residual film stress by curvature method. The insertion of Cu interlayers effectively reduces σr by 23% through stacking with six single-layered CoMnP. The out-of-plane (OP) anisotropy is slightly reduced. While the maximum energy product in the in-plane (IP) direction can be significantly enhanced by 430% ∼ 690% with increasing the number of the CoMnP single layer in the multilayers. The magneto-elastic behaviors well explain the evolution of the total anisotropy energy of the mono- and multi-layers. By CoMnP/Cu configurations we successfully worked out a strategy to preserve prestigious OP performance while to enhance IP properties by 4 to 6 times to meet ever increasing challenges in MEMS applications.

https://aip.scitation.org/doi/pdf/10.1063/9.0000319

Residual stress tuned magnetic properties of thick CoMnP/Cu multilayers

An adaptive disturbance compensation method for force-sensorless control systems applied to robotic milling

This article introduces an advanced methodology for optimal parametric design based on discrete-time analysis findings of a robust force control structure, integrating both a disturbance observer and a reaction force observer. While conventional continuous-time analyses are commonly employed to enhance system performance, offering guidance for stability and robustness improvement, they often fall short in explaining practical implementation instabilities. A significant knowledge gap persists in the systematic design approach for tuning the control system to meet specific desired behaviors. To bridge this gap, this article thoroughly investigates the system's frequency response. Design constraints derived from this analysis process formulate the nominal parameter design as a minimization problem, subsequently solved using a genetic algorithm to determine optimal parameter values. Simulations illustrate the control system behavior, emphasizing the design constraints and optimal parameter design process. The proposed method is applied to a force-controlled spindle via calibrated experiments, providing robust validation. The results unequivocally confirm the effectiveness of the proposed design approach, achieving stability, and robustness concurrently. 

Optimal Parametric Design of Discrete-Time Robust Force Control System Based on Disturbance and Reaction Force Observers

Development of a motion-decoupled finger exoskeleton with integrated joint stiffness estimation

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