Application Note | Thin Film Adhesion Testing

Adhesion Properties of Gold Coating on a Quartz Crystal Substrate

Micro Scratch Quality Control of the Electrode Coating on a Quartz Crystal Microbalance (QCM)

Spacecraft and solar arrays in orbit, where QCM sensors monitor contamination

Research & Experimental Testing

Duanjie Li

Visual Design & Editorial

Andrew Shore

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 extremely 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.

Why Scratch Testing Matters for QCM Electrodes

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 Large Platform

Mechanical Tester

Nanoindenter and scratch tester platform NANOVEA PB1000 with nano and micro modules

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.

ParameterValue
Load typeProgressive
Initial load0.01 N
Final load30 N
AtmosphereAir, 24°C
Sliding speed2 mm/min
Sliding distance2 mm
IndenterRockwell diamond 120° cone, 100 µm tip radius

Micro scratch test parameters.

Indenter type: Rockwell diamond 120 degree cone with 100 µm tip radius
Two quartz crystal microbalance discs with gold electrode coatings

Rockwell diamond indenter and the QCM samples with gold electrode coating.

Results and Discussion

The full micro scratch track on the QCM sample is shown in Fig. 1. The failure behaviors at different critical loads are displayed in Fig. 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.

Full micro scratch track on the gold-coated QCM, widening into delamination toward the end
Fig. 1: Full micro scratch track on the QCM sample.
Scratch track at the first critical load LC1 of 11.15 N, with little chipping
Scratch track at LC2 of 16.29 N, with repetitive adhesive failures
Scratch track at LC3 of 19.09 N, with the gold coating delaminated from the quartz

Fig. 2: Micro scratch track at different critical loads.

Critical loadFailureLoad (N)
LC1First sign of adhesive failure (little chipping)11.15
LC2Repetitive adhesive failures begin16.29
LC3Coating completely removed from the substrate19.09

Table 1: Critical loads of the gold coating on the quartz substrate.

Fig. 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.

Coefficient of friction and true depth versus scratch length on the gold-coated QCM, with the critical loads marked
Fig. 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.

Frequently Asked Questions About QCM Gold Coating Adhesion

What is a quartz crystal microbalance (QCM)?

A QCM is an extremely sensitive mass sensor that measures mass change in the nanogram range by detecting variations in the resonance frequency of a quartz crystal with two electrodes affixed to each side of the plate. It is used to detect and monitor the variation of mass, adsorption, density and corrosion.

Why does electrode coating adhesion matter for a QCM?

A QCM measures mass change down to 0.1 nanogram, so any mass loss or delamination of the electrodes on the quartz plate is detected by the crystal and causes significant measurement errors. The intrinsic quality of the electrode coating and the coating/substrate interface are essential for accurate, repeatable measurement.

How does a micro scratch test evaluate coating adhesion?

A diamond stylus scratches the coating under a linearly increasing load, here from 0.01 N to 30 N over 2 mm. The critical loads at which failures appear allow a comparative evaluation of the relative cohesion or adhesion of coatings.

What critical loads did the gold coating on quartz show?

Little chipping, the first sign of coating failure, appeared at LC1 of 11.15 N; repetitive adhesive failures occurred after LC2 of 16.29 N; and the coating completely delaminated from the quartz substrate at LC3 of 19.09 N.

What else is recorded during the scratch test?

The coefficient of friction and depth are recorded throughout the scratch, providing more insight into the progression of coating failures.

Which NANOVEA instrument was used for QCM scratch testing?

The NANOVEA PB1000 Mechanical Tester in Micro Scratch Mode, with a Rockwell diamond 120° cone of 100 µm tip radius. An optional 3D non-contact profiler and AFM module give high resolution 3D imaging of scratch tracks.

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