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Category: Scratch Testing | Adhesive Failure

 

Adhesion Properties of Gold Coating on Quartz Crystal Substrate

 

Adhesion Properties of Gold Coating

on Quartz Crystal Substrate

Prepared by

DUANJIE LI, PhD

INTRODUCTION

The Quartz Crystal Microbalance (QCM) is an extremely sensitive mass sensor capable of making precise measurements of small mass in the nanogram range. QCM measures the mass change on the surface through detecting variations in resonance frequency of the quartz crystal with two electrodes affixed to each side of the plate. The capacity of measuring extreme small weight makes it a key component in a variety of research and industrial instruments to detect and monitor the variation of mass, adsorption, density, and corrosion, etc.

IMPORTANCE OF SCRATCH TEST FOR QCM

As an extremely accurate device, the QCM measures the mass change down to 0.1 nanogram. Any mass loss or delamination of the electrodes on the quartz plate will be detected by the quartz crystal and cause significant measurement errors. As a result, the intrinsic quality of the electrode coating and the interfacial integrity of the coating/substrate system play an essential role in performing accurate and repeatable mass measurement. The Micro scratch test is a widely used comparative measurement to evaluate the relative cohesion or adhesion properties of coatings based on comparison of the critical loads at which failures appear. It is a superior tool for reliable quality control of QCMs.

MEASUREMENT OBJECTIVE

In this application, the NANOVEA Mechanical Tester, in Micro Scratch Mode, is used to evaluate the cohesive & adhesive strength of the gold coating on the quartz substrate of a QCM sample. We would like to showcase the capacity of the NANOVEA Mechanical Tester in performing micro scratch tests on a delicate sample with high precision and repeatability.

NANOVEA

PB1000

TEST CONDITIONS
The NANOVEA PB1000 Mechanical Tester was used to perform the micro scratch tests on a QCM sample using the test parameters summarized below. Three scratches were performed to ensure reproducibility of the results.

LOAD TYPE: Progressive

INITIAL LOAD

0.01 N

FINAL LOAD

30 N

ATMOSPHERE: Air 24°C

SLIDING SPEED

2 mm/min

SLIDING DISTANCE

2 mm

RESULTS & DISCUSSION

The full micro scratch track on the QCM sample is shown in FIGURE 1. The failure behaviors at different critical loads are displayed in FIGURE 2, where critical load, LC1 is defined as the load at which the first sign of adhesive failure occurs in the scratch track, LC2 is the load after which repetitive adhesive failures take place, and LC3 is the load at which the coating is completely removed from the substrate. It can be observed that little chipping takes place at LC1 of 11.15 N, the first sign of coating failure. 

As the normal load continues to increase during the micro scratch test, repetitive adhesive failures occur after LC2 of 16.29 N. When LC3 of 19.09 N is reached, the coating completely delaminates from the quartz substrate. Such critical loads can be used to quantitatively compare the cohesive and adhesive strength of the coating and select the best candidate for targeted applications.

FIGURE 1: Full micro scratch track on the QCM sample.

FIGURE 2: Micro scratch track at different critical loads.

FIGURE 3 plots the evolution of friction coefficient and depth that may provide more insight in the progression of coating failures during the micro scratch test.

FIGURE 3: Evolution of COF and Depth during the micro scratch test.

CONCLUSION

In this study, we showcased that the NANOVEA Mechanical Tester performs reliable and accurate micro scratch tests on a QCM sample. By applying linearly increased loads in a controlled and closely monitored fashion, the scratch measurement allows users to identify the critical load at which typical cohesive and adhesive coating failure occurs. It provides a superior tool to quantitatively evaluate and compare the intrinsic quality of the coating and the interfacial integrity of the coating/substrate system for QCM.

The Nano, Micro or Macro modules of the NANOVEA Mechanical Tester all include ISO and ASTM compliant indentation, scratch and wear tester modes, providing the widest and most user friendly range of testing available in a single system. NANOVEA‘s unmatched range is an ideal solution for determining the full range of mechanical properties of thin or thick, soft or hard coatings, films and substrates, including hardness, Young’s modulus, fracture toughness, adhesion, wear resistance and many others.

In addition, an optional 3D non-contact profiler and AFM module are available for high resolution 3D imaging of indentation, scratch and wear track in addition to other surface measurements, such as roughness and warpage.

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Wear and Scratch Evaluation of Surface Treated Copper Wire

Wear and Scratch Evaluation of Surface Treated Copper Wire

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Importance of Wear and Scratch Evaluation of Copper Wire

Copper has a long history of use in electric wiring since the invention of the electromagnet and telegraph. Copper wires are applied in a wide range of electronic equipment such as panels, meters, computers, business machines, and appliances thanks to its corrosion resistance, solderability, and performance at elevated temperatures up to 150°C. Approximately half of all mined copper is used for manufacturing electrical wire and cable conductors.

Copper wire surface quality is critical to application service performance and lifetime. Micro defects in wires may lead to excessive wear, crack initiation and propagation, decreased conductivity, and inadequate solderability. Proper surface treatment of copper wires removes surface defects generated during wire drawing improving corrosion, scratch, and wear resistance. Many aerospace applications with copper wires require controlled behavior to prevent unexpected equipment failure. Quantifiable and reliable measurements are needed to properly evaluate the wear and scratch resistance of the copper wire surface.


Measurement Objective

In this application we simulate a controlled wear process of different copper wire surface treatments. Scratch testing measures the load required to cause failure on the treated surface layer. This study showcases the Nanovea Tribometer and Mechanical Tester as ideal tools for evaluation and quality control of electric wires.


Test Procedure and Procedures

Coefficient of friction (COF) and wear resistance of two different surface treatments on copper wires (Wire A and Wire B) were evaluated by the Nanovea tribometer using a linear reciprocating wear module. An Al₂O₃ ball (6 mm diameter) is the counter material used in this application. The wear track was examined using Nanovea’s 3D non-contact profilometer. Test parameters are summarized in Table 1.

A smooth Al₂O₃ ball as a counter material was used as an example in this study. Any solid material with different shape and surface finish can be applied using a custom fixture to simulate the actual application situation.



Nanovea’s mechanical tester equipped with a Rockwell C diamond stylus (100 μm radius) performed progressive load scratch tests on the coated wires using micro scratch mode. Scratch test parameters and tip geometry are shown in Table 2.




Results and Discussion

Wear of copper wire: Figure 2 shows COF evolution of the copper wires during wear tests. Wire A shows a stable COF of ~0.4 throughout the wear test while wire B exhibits a COF of ~0.35 in the first 100 revolutions and progressively increases to ~0.4.



Figure 3 compares wear tracks of the copper wires after tests. Nanovea’s 3D non-contact profilometer offered superior analysis of the detailed morphology of wear tracks. It allows direct and accurate determination of the wear track volume by providing a fundamental understanding of the wear mechanism. Wire B’s surface has signi¬ficant wear track damage after a 600-revolution wear test. The profilometer 3D view shows the surface treated layer of Wire B removed completely which substantially accelerated the wear process. This left a flattened wear track on Wire B where copper substrate is exposed. This may result in significantly shortened lifespan of electrical equipment where Wire B is used. In comparison, Wire A exhibits relatively mild wear shown by a shallow wear track on the surface. The surface treated layer on Wire A did not remove like the layer on Wire B under the same conditions.







Scratch resistance of the copper wire surface: Figure 4 shows the scratch tracks on the wires after testing. The protective layer of Wire A exhibits very good scratch resistance. It delaminates at a load of ~12.6 N. In comparison, the protective layer of Wire B failed at a load of ~1.0 N. Such a significant difference in scratch resistance for these wires contributes to their wear performance, where Wire A possesses substantially enhanced wear resistance. The evolution of normal force, COF, and depth during the scratch tests shown in Fig. 5 provides more insight on coating failure during tests.






Conclusion



In this controlled study we showcased the Nanovea’s tribometer conducting quantitative evaluation of wear resistance for surface treated copper wires and Nanovea’s mechanical tester providing reliable assessment of copper wire scratch resistance. Wire surface treatment plays a critical role in the tribo-mechanical properties during their lifetime. Proper surface treatment on Wire A significantly enhanced wear and scratch resistance, critical in the performance and lifespan of electrical wires in rough environments. Nanovea’s tribometer offers precise and repeatable wear and friction testing using ISO and ASTM compliant rotative and linear modes, with optional high temperature wear, lubrication, and tribo-corrosion modules available in one pre-integrated system. Nanovea’s unmatched range is an ideal solution for determining the full range of tribological properties of thin or thick, soft or hard coatings, films, and substrates.

Understanding Coating Failures using Scratch Testing

Introduction:

Surface engineering of materials plays a significant role in a variety of functional applications, ranging from decorative appearance to protecting the substrates from wear, corrosion and other forms of attacks. An important and overriding factor that determines the quality and service lifetime of the coatings is their cohesive and adhesive strength.

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Multi Scratch Automation of Similar Samples using the PB1000 Mechanical Tester

Introduction :

Coatings are widely used in various industries because of their functional properties. A coating’s hardness, erosion resistance, low friction, and high wear resistance are just some of the many properties that make coatings important. A commonly used method to quantify these properties is scratch testing, this allows for a repeatable measurement of a coating’s adhesive and/or cohesive properties. By comparing the critical loads at which failure occurs, the intrinsic properties of a coating can be evaluated.

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Scratch Testing on Multi-Layered Thin Film

Coatings used extensively throughout multiple industries to preserve the underlying layers, to create electronic devices, or to improve surface properties of materials. Due to their numerous uses coatings are extensively studied, but their mechanical properties can be difficult to understand. Failure of coatings can occur in the micro/nanometer range from surface-atmosphere interaction, cohesive failure, and poor substrate-interface adhesion. A consistent method to test for coating failures is scratch testing. By applying a progressively increasing load, cohesive (e.g. cracking) and adhesive (e.g. delamination) failures of coatings can be quantitatively compared.

Scratch Testing on Multi-Layered Thin Film

Mechanical Properties of Silicon Carbide Wafer Coatings

Understanding the mechanical properties of silicon carbide wafer coatings is critical. The fabrication process for microelectronic devices can have over 300 different processing steps and can take anywhere from six to eight weeks. During this process, the wafer substrate must be able to withstand the extreme conditions of manufacturing, since a failure at any step would result in the loss of time and money. The testing of hardness, adhesion/scratch resistance and COF/wear rate of the wafer must meet certain requirements in order to survive the conditions imposed during the manufacturing and application process to insure a failure will not occur.

Mechanical Properties of Silicon Carbide Wafer Coatings

Micro Scrape Test Of Polymeric Coating

Scratch testing has developed to be one of the most widely applied methods to evaluate the cohesive and adhesive strength of the coatings. The critical load, at which a certain type of coating failure occurs as the applied load progressively increases, is widely regarded as a reliable tool to determine and compare the adhesive and cohesive properties of the coatings. The most commonly used indenter for scratch testing is the conical Rockwell diamond indenter. However, when the scratch test is performed on the soft polymeric coating deposited on a brittle substrate such as silicon wafer, the conical indenter tends to plough through the coating forming grooves rather than creating cracks or delamination. Cracking of the brittle silicon wafer takes place when the load further increases. Therefore, it is vital to develop a new technique to evaluate the cohesion or adhesion properties of soft coatings on a brittle substrate.

Micro Scrape Test Of Polymeric Coating

Industrial Coating Scratch & Wear Evaluation

The wear process of the acrylic urethane floor paints with different topcoats is simulated in a controlled and monitored manner using the Nanovea Tribometer as shown in Fig. 1. Micro scratch testing is used to measure the load required to cause cohesive or adhesive failure to the paint. In this study, we would like to showcase that Nanovea Mechanical Tester and Tribometer are ideal tools for evaluation and quality control of commercial floor and automotive coatings.

Industrial Coating Scratch & Wear Evaluation

Grooved Stent Coating Failure Using Nano Scratch Testing

Drug–eluting stent is a novel approach in stent technology. It possesses a biodegradable and biocompatible polymer coating that releases medicine slowly and continuously at the local artery to inhibit intimal thickening and prevent the artery from being blocked again. One of the major concerns is the delamination of the polymer coating that carries the drug-eluting layer from the metal stent substrate. In order to improve the adhesion of this coating to the substrate, the stent is designed in different shapes. Specifically in this study, the polymer coating locates at the bottom of the groove on the mesh wire, which brings enormous challenge to the adhesion measurement. A reliable technique is in need to quantitatively measure the interfacial strength between the polymer coating and the metal substrate. The special shape and the small diameter of the stent mesh (comparable to a human hair) require ultrafine X-Y lateral accuracy to locate the test position and proper control and measurement of the load and depth during the test.

Grooved Stent Coating Failure Using Nano Scratch Testing

Coating Inspection of TIN by Scratch Testing

Coating inspection of residual stress in protective PVD/CVD coatings plays a critical role in the performance and mechanical integrity of the coated component. The residual stress derives from several major sources, including growth stress, thermal gradients, geometric constraints and service stresses. The thermal expansion mismatch between the coating and the substrate created during coating deposition at elevated temperatures leads to high thermal residual stress. Moreover, the TiN coated tools are often used under very high concentrated stresses, e.g. drill bits and bearings. It is critical to develop a reliable quality control process to quantitatively inspect the cohesive and adhesive strength of the protective functional coatings.

Coating Inspection of TIN by Scratch Testing

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