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Category: Scratch Testing | Adhesive Failure

 

PTFE Coating Wear Test

PTFE COATING WEAR TEST

USING TRIBOMETER AND MECHANICAL TESTER

Prepared by

DUANJIE LI, PhD

INTRODUCTION

Polytetrafluoroethylene (PTFE), commonly known as Teflon, is a polymer with an exceptionally low coefficient of friction (COF) and excellent wear resistance, depending on the applied loads. PTFE exhibits superior chemical inertness, high melting point of 327°C (620°F), and maintains high strength, toughness, and self-lubrication at low temperatures. The exceptional wear resistance of  PTFE coatings makes them highly sought-after in a wide range of industrial applications, such as automotive, aerospace, medical, and, notably, cookware.

IMPORTANCE OF QUANTITATIVE EVALUATION OF PTFE COATINGS

The combination of a super low coefficient of friction (COF), excellent wear resistance, and exceptional chemical inert- ness at high temperatures makes PTFE an ideal choice for non-stick pan coatings. To further enhance its mechanical processes during R&D, as well as ensure optimal control over malfunction prevention and safety measures in the Quality Control process, it is crucial to have a reliable technique for quantity evaluating the tribomechanical processes of PTFE coatings. Precise control over surface friction, wear, and adhesion of the coatings is essential to ensure their intended performance.

MEASUREMENT OBJECTIVE

In this application, the wear process of a PTFE coating for a non-stick pan is simulated using NANOVEA Tribometer in linear reciprocating mode.

NANOVEA T50

Compact Free Weight Tribometer

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In addition, the NANOVEA Mechanical Tester was used to perform a micro scratch adhesion test to determine the critical load of the PTFE coating adhesion failure.

NANOVEA PB1000

Large Platform Mechanical Tester

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TEST PROCEDURE

WEAR TEST

LINEAR RECIPROCATING WEAR USING A TRIBOMETER

The tribological behavior of the PTFE coating sample, including the coefficient of friction (COF) and wear resistance, was evaluated using the NANOVEA Tribometer in linear reciprocating mode. A Stainless Steel 440 ball tip with a diameter of 3 mm (Grade 100) was used against the coating. The COF was continuously monitored during the PTFE coating wear test.

 

The wear rate, K, was calculated using the formula K=V/(F×s)=A/(F×n), where V represents the worn volume, F is the normal load, s is the sliding distance, A is the cross-sectional area of the wear track, and n is the number of strokes. The wear track profiles were evaluated using the NANOVEA Optical Profilometer, and the wear track morphology was examined using an optical microscope.

WEAR TEST PARAMETERS

LOAD 30 N
TEST DURATION 5 min
SLIDING RATE 80 rpm
AMPLITUDE OF TRACK 8 mm
REVOLUTIONS 300
BALL DIAMETER 3 mm
BALL MATERIAL Stainless Steel 440
LUBRICANT None
ATMOSPHERE Air
TEMPERATURE 230C (RT)
HUMIDITY 43%

TEST PROCEDURE

SCRATCH TEST

MICRO SCRATCH ADHESION TEST USING MECHANICAL TESTER

The PTFE scratch adhesion measurement was conducted using the NANOVEA Mechanical Tester with a 1200 Rockwell C diamond stylus (200 μm radius) in the Micro Scratch Tester Mode.

 

To ensure the reproducibility of the results, three tests were performed under identical testing conditions.

SCRATCH TEST PARAMETERS

LOAD TYPE Progressive
INITIAL LOAD 0.01 mN
FINAL LOAD 20 mN
LOADING RATE 40 mN/min
SCRATCH LENGTH 3 mm
SCRATCHING SPEED, dx/dt 6.0 mm/min
INDENTER GEOMETRY 120o Rockwell C
INDENTER MATERIAL (tip) Diamond
INDENTER TIP RADIUS 200 μm

RESULTS & DISCUSSION

LINEAR RECIPROCATING WEAR USING A TRIBOMETER

The COF recorded in situ is shown in FIGURE 1. The test sample exhibited a COF of ~0.18 during the first 130 revolutions, due to the low stickiness of PTFE. However, there was a sudden increase in COF to ~1 once the coating broke through, revealing the substrate underneath. Following the linear reciprocating tests, the wear track profile was measured using the NANOVEA Non-Contact Optical Profilometer, as shown in FIGURE 2. From the data obtained, the corresponding wear rate was calculated to be ~2.78 × 10-3 mm3/Nm, while the depth of the wear track was determined to be 44.94 µm.

PTFE coating wear test setup on the NANOVEA T50 Tribometer.

FIGURE 1: Evolution of COF during the PTFE coating wear test.

FIGURE 2: Profile extraction of wear track PTFE.

PTFE Before breakthrough

Max COF 0.217
Min COF 0.125
Average COF 0.177

PTFE After breakthrough

Max COF 0.217
Min COF 0.125
Average COF 0.177

TABLE 1: COF before and after breakthrough during the wear test.

RESULTS & DISCUSSION

MICRO SCRATCH ADHESION TEST USING MECHANICAL TESTER

The adhesion of the PTFE coating to the substrate is measured using scratch tests with a 200 µm diamond stylus. The micrograph is shown in FIGURE 3 and FIGURE 4, Evolution of COF, and penetration depth in FIGURE 5. The PTFE coating scratch test results are summarized in TABLE 4. As the load on the diamond stylus increased, it progressively penetrated into the coating, resulting in an increase in the COF. When a load of ~8.5 N was reached, the breakthrough of the coating and exposure of the substrate occurred under high pressure, leading to a high COF of ~0.3. The low St Dev shown in TABLE 2 demonstrates the repeatability of the PTFE coating scratch test conducted using the NANOVEA Mechanical Tester.

FIGURE 3: Micrograph of the full scratch on PTFE (10X).

FIGURE 4: Micrograph of the full scratch on PTFE (10X).

FIGURE 5: Friction graph showing the line of the critical point of failure for PTFE.

Scratch Point of Failure [N] Frictional Force [N] COF
1 0.335 0.124 0.285
2 0.337 0.207 0.310
3 0.380 0.229 0.295
Average 8.52 2.47 0.297
St dev 0.17 0.16 0.012

TABLE 2: Summary of Critical Load, Frictional Force, and COF during the scratch test.

CONCLUSION

In this study, we conducted a simulation of the wear process of a PTFE coating for non-stick pans using the NANOVEA T50 Tribometer in linear reciprocating mode. The PTFE coating exhibited a low COF of ~0.18 the coating experienced a breakthrough at around 130 revolutions. The quantitative evaluation of the PTFE coating adhesion to the metal substrate was performed using the NANOVEA Mechanical Tester which determined the critical load of the coating adhesion failure to be ~8.5 N in this test.

 

The NANOVEA Tribometers offer precise and repeatable wear and friction testing capabilities using ISO and ASTM-compliant rotary and linear modes. They provide optional modules for high-temperature wear, lubrication, and tribocorrosion, all integrated into a single system. This versatility allows users to simulate real-world application environments more accurately and gain a beer understanding of the wear mechanisms and tribological properties of different materials.

 

The NANOVEA Mechanical Testers offer Nano, Micro, and Macro modules, each of which includes ISO and ASTM compliant indentation, scratch, and wear testing modes, providing the widest and most user-friendly range of testing capabilities available in a single system.

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Nano Scratch & Mar Testing of Paint on Metal Substrate

Nano Scratch & Mar Testing

of Paint on Metal Substrate

Prepared by

SUSANA CABELLO

INTRODUCTION

Paint with or without hard coat is one of the most commonly used coatings. We see it on cars, on walls, on appliances and virtually anything that needs some protective coatings or simply for aesthetic purposes. The paints that are meant for the protection of the underlying substrate often have chemicals that prevent the paint from catching on fire or simply that prevent it from losing its color or cracking. Often the paint used for aesthetic purposes comes in various colors, but may not be necessarily meant for the protection of its substrate or for a long lifetime.

Nevertheless, all paint suffers some weathering over time. Weathering on paint can often change the properties from what the makers intended it to have. It can chip quicker, peel off with heat, loose color or crack. The different property changes of paint over time is why makers offer such a wide selection. Paints are tailored to meet different requirements for individual clients.

IMPORTANCE OF NANO SCRATCH TESTING FOR QUALITY CONTROL

A major concern for paint makers is the ability for their product to withstand cracking. Once paint begins to crack, it fails to protect the substrate that it was applied on; therefore, failing to satisfy their client. For example, if a branch happens to stroke the side of a car and immediately after the paint begins to chip off the makers of the paint would lose business due to their poor quality of paint. The quality of the paint is very important because if the metal under the paint becomes exposed it may begin to rust or corrode due to its new exposure.

 

Reasons like this apply to several other spectrums such as household and office supplies and electronics, toys, research tools and more. Although the paint may be resistant to cracking when they first apply it to metal coatings, the properties may change over time when some weathering has occurred on the sample. This is why it’s very important to have the paint samples tested at their weathered stage. Although cracking under a high load of stress may be inevitable, the maker must predict how weakening the changes may be over time and how deep the affecting scratch must be in order to provide their consumers with the best possible products.

MEASUREMENT OBJECTIVE

We must simulate the process of scratching in a controlled and monitored manner to observe sample behavior effects. In this application, the NANOVEA PB1000 Mechanical Tester in Nano Scratch Testing mode is used to measure the load required to cause failure to an approximately 7 year old 30-50 μm thick paint sample on a metal substrate.

A 2 μm diamond tipped stylus is used at a progressive load ranging from 0.015 mN to 20.00 mN to scratch the coating. We performed a pre and post scan of the paint with 0.2 mN load in order to determine the value for the true depth of the scratch. The true depth analyzes the plastic and elastic deformation of the sample during testing; whereas, the post-scan only analyzes the plastic deformation of the scratch. The point where the coating fails by cracking is taken as the point of failure. We used the ASTMD7187 as a guide to determine our testing parameters.

 

We can conclude that having used a weathered sample; therefore, testing a paint sample at its weaker stage, presented us with lower points of failure.

 

Five tests were performed on this sample in order to

determine the exact failure critical loads.

NANOVEA

PB1000

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TEST PARAMETERS

following ASTM D7027

The surface of a Roughness Standard was scanned using a NANOVEA ST400 equipped with a high-speed sensor that generates a bright line of 192 points, as shown in FIGURE 1. These 192 points scan the sample surface at the same time, leading to significantly increased scan speed.

LOAD TYPE Progressive
INITIAL LOAD 0.015 mN
FINAL LOAD 20 mN
LOADING RATE 20 mN/min
SCRATCH LENGTH 1.6 mm
SCRATCH SPEED, dx/dt 1.601 mm/min
PRE-SCAN LOAD 0.2 mN
POST-SCAN LOAD 0.2 mN
Conical Indenter 90° Cone 2 µm tip radius

indenter type

Conical

Diamond 90° Cone

2 µm tip radius

Conical Indenter Diamond 90° Cone 2 µm tip radius

RESULTS

This section presents the data collected on the failures during the scratch test. The first section describes the failures observed in the scratch and defines the critical loads that were reported. The next part contains a summary table of the critical loads for all samples, and a graphical representation. The last part presents detailed results for each sample: the critical loads for each scratch, micrographs of each failure, and the graph of the test.

FAILURES OBSERVED AND DEFINITION OF CRITICAL LOADS

CRITICAL FAILURE:

INITIAL DAMAGE

This is the first point at which the damage is observed along the scratch track.

nano scratch critical failure initial damage

CRITICAL FAILURE:

COMPLETE DAMAGE

At this point, the damage is more significant where the paint is chipping and cracking along the scratch track.

nano scratch critical failure complete damage

DETAILED RESULTS

* Failure values taken at point of substrate cracking.

CRITICAL LOADS
SCRATCH INITIAL DAMAGE [mN] COMPLETE DAMAGE [µm]
1 14.513 4.932
2 3.895 4.838
3 3.917 4.930
AVERAGE 3.988 4.900
STD DEV 0.143 0.054
Micrograph of Full Scratch from nano scratch test(1000x magnification).

FIGURE 2: Micrograph of Full Scratch (1000x magnification).

Micrograph of Initial Damage from nano scratch test (1000x magnification)

FIGURE 3: Micrograph of Initial Damage (1000x magnification).

Micrograph of Complete Damage from nano scratch test (1000x magnification).

FIGURE 4: Micrograph of Complete Damage (1000x magnification).

Linear Nano Scratch Test Friction Force and Coefficient of Friction

FIGURE 5: Friction Force and Coefficient of Friction.

Linear Nano Scratch Surface Profile

FIGURE 6: Surface Profile.

Linear Nano Scratch Test True Depth and Residual Depth

FIGURE 7: True Depth and Residual Depth.

CONCLUSION

The NANOVEA Mechanical Tester in the Nano Scratch Tester mode allows the simulation of many real-life failures of paint coatings and hard coats. By applying increasing loads in a controlled and closely monitored manner, the instrument allows to identify at what load failures occur. This can then be used as a way to determine quantitative values for scratch resistance. The coating tested, with no weathering, is known to have a first crack at about 22 mN. With values closer to 5 mN, it is clear that the 7 year lap has degraded the paint.

Compensating for the original profile allows obtaining corrected depth during the scratch and measuring the residual depth after the scratch. This gives extra information on the plastic versus elastic behavior of the coating under increasing load. Both cracking and the information on deformation can be of great use for improving the hard coat. The very small standard deviations also show the reproducibility of the instrument’s technique which can help manufacturers improve the quality of their hard coat/paint and study weathering effects.

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Industrial Coatings Scratch and Wear Evaluation

INDUSTRIAL COATING

SCRATCH AND WEAR EVALUATION USING A TRIBOMETER

Prepared by

DUANJIE LI, PhD & ANDREA HERRMANN

INTRODUCTION

Acrylic urethane paint is a type of fast-dry protective coating widely used in a variety of industrial applications, such as floor paint, auto paint, and others. When used as floor paint, it can serve areas with heavy foot and rubber-wheel traffic, such as walkways, curbs and parking lots.

IMPORTANCE OF SCRATCH AND WEAR TESTING FOR QUALITY CONTROL

Traditionally, Taber abrasion tests were carried out to evaluate the wear resistance of acrylic urethane floor paint according to the ASTM D4060 standard. However, as mentioned in the standard, “For some materials, abrasion tests utilizing the Taber Abraser may be subject to variation due to changes in the abrasive characteristics of the wheel during testing.”1 This may result in poor reproducibility of test results and create difficulty in comparing values reported from different laboratories. Moreover, in Taber abrasion tests, abrasion resistance is calculated as loss in weight at a specified number of abrasion cycles. However, acrylic urethane floor paints have a recommended dry film thickness of 37.5-50 μm2.

The aggressive abrasion process by Taber Abraser can quickly wear through the acrylic urethane coating and create mass loss to the substrate leading to substantial errors in the calculation of the paint weight loss. The implant of abrasive particles in the paint during the abrasion test also contributes to errors. Therefore, a well-controlled quantifiable and reliable measurement is crucial to ensure reproducible wear evaluation of the paint. In addition, the scratch test allows users to detect premature adhesive/cohesive failures in real-life applications.

MEASUREMENT OBJECTIVE

In this study, we showcase that NANOVEA Tribometers and Mechanical Testers are ideal for evaluation and quality control of industrial coatings.

The wear process of acrylic urethane floor paints with different topcoats is simulated in a controlled and monitored manner using the NANOVEA Tribometer. Micro scratch testing is used to measure the load required to cause cohesive or adhesive failure to the paint.

Compact Pneumatic Tribometer T100
NANOVEA T100

The Compact Pneumatic Tribometer

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NANOVEA PB1000

The Large Platform Mechanical Tester

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TEST PROCEDURE

This study evaluates four commercially available water-based acrylic floor coatings that have the same primer (basecoat) and different topcoats of the same formula with a small alternation in the additive blends for the purpose of enhancing durability. These four coatings are identified as Samples A, B, C and D.

WEAR TEST

The NANOVEA Tribometer was applied to evaluate the tribological behavior, e.g. coefficient of friction, COF, and wear resistance. A SS440 ball tip (6 mm dia., Grade 100) was applied against the tested paints. The COF was recorded in situ. The wear rate, K, was evaluated using the formula K=V/(F×s)=A/(F×n), where V is the worn volume, F is the normal load, s is the sliding distance, A is the cross-sectional area of the wear track, and n is the number of revolution. Surface roughness and wear track profiles were evaluated by the NANOVEA Optical Profilometer, and the wear track morphology was examined using optical microscope.

WEAR TEST PARAMETERS

NORMAL FORCE

20 N

SPEED

15 m/min

DURATION OF TEST

100, 150, 300 & 800 cycles

SCRATCH TEST

The NANOVEA Mechanical Tester equipped with a Rockwell C diamond stylus (200 μm radius) was used to perform progressive load scratch tests on the paint samples using the Micro Scratch Tester Mode. Two final loads were used: 5 N final load for investigating paint delamination from the primer, and 35 N for investigating primer delamination from the metal substrates. Three tests were repeated at the same testing conditions on each sample to ensure reproducibility of the results.

Panoramic images of the whole scratch lengths were automatically generated and their critical failure locations were correlated with the applied loads by the system software. This software feature facilitates users to perform analysis on the scratch tracks any time, rather than having to determine the critical load under the microscope immediately after the scratch tests.

SCRATCH TEST PARAMETERS

LOAD TYPEProgressive
INITIAL LOAD0.01 mN
FINAL LOAD5 N / 35 N
LOADING RATE10 / 70 N/min
SCRATCH LENGTH3 mm
SCRATCHING SPEED, dx/dt6.0 mm/min
INDENTER GEOMETRY120º cone
INDENTER MATERIAL (tip)Diamond
INDENTER TIP RADIUS200 μm

WEAR TEST RESULTS

Four pin-on-disk wear tests at different number of revolutions (100, 150, 300 and 800 cycles) were performed on each sample in order to monitor the evolution of wear. The surface morphology of the samples were measured with a NANOVEA 3D Non-Contact Profiler to quantify the surface roughness prior to conducting wear testing. All samples had a comparable surface roughness of approximately 1 μm as displayed in FIGURE 1. The COF was recorded in situ during the wear tests as shown in FIGURE 2. FIGURE 4 presents the evolution of wear tracks after 100, 150, 300 and 800 cycles, and FIGURE 3 summarized the average wear rate of different samples at different stages of the wear process.

 

Compared with a COF value of ~0.07 for the other three samples, Sample A exhibits a much higher COF of ~0.15 at the beginning, which gradually increases and gets stable at ~0.3 after 300 wear cycles. Such a high COF accelerates the wear process and creates a substantial amount of paint debris as indicated in FIGURE 4 – the topcoat of Sample A has started to be removed in the first 100 revolutions. As shown in FIGURE 3, Sample A exhibits the highest wear rate of ~5 μm2/N in the first 300 cycles, which slightly decreases to ~3.5 μm2/N due to the better wear resistance of the metal substrate. The topcoat of Sample C starts to fail after 150 wear cycles as shown in FIGURE 4, which is also indicated by the increase of COF in FIGURE 2.

 

In comparison, Sample B and Sample D show enhanced tribological properties. Sample B maintains a low COF throughout the whole test – the COF slightly increases from~0.05 to ~0.1. Such a lubricating effect substantially enhances its wear resistance – the topcoat still provides superior protection to the primer underneath after 800 wear cycles. The lowest average wear rate of only ~0.77 μm2/N is measured for Sample B at 800 cycles. The topcoat of Sample D starts to delaminate after 375 cycles, as reflected by the abrupt increase of COF in FIGURE 2. The average wear rate of Sample D is ~1.1 μm2/N at 800 cycles.

 

Compared to the conventional Taber abrasion measurements, NANOVEA Tribometer provides well-controlled quantifiable and reliable wear assessments that ensure reproducible evaluations and quality control of commercial floor/auto paints. Moreover, the capacity of in situ COF measurements allow users to correlate the different stages of a wear process with the evolution of COF, which is critical in improving fundamental understanding of the wear mechanism and tribological characteristics of various paint coatings.

FIGURE 1: 3D morphology and roughness of the paint samples.

FIGURE 2: COF during pin-on-disk tests.

FIGURE 3: Evolution of wear rate of different paints.

FIGURE 4: Evolution of wear tracks during the pin-on-disk tests.

SCRATCH TEST RESULTS

FIGURE 5 shows the plot of normal force, frictional force and true depth as a function of scratch length for Sample A as an example. An optional acoustic emission module can be installed to provide more information. As the normal load linearly increases, the indentation tip gradually sinks into the tested sample as reflected by the progressive increase of true depth. The variation in the slopes of frictional force and true depth curves can be used as one of the implications that coating failures start to occur.

FIGURE 5: Normal force, frictional force and true depth as a function of scratch length for scratch test of Sample A with a maximum load of 5 N.

FIGURE 6 and FIGURE 7 show the full scratches of all four paint samples tested with a maximum load of 5 N and 35 N, respectively. Sample D required a higher load of 50 N to delaminate the primer. Scratch tests at 5 N final load (FIGURE 6) evaluate the cohesive/adhesive failure of the top paint, while the ones at 35 N (FIGURE 7) assess the delamination of the primer. The arrows in the micrographs indicate the point at which the top coating or the primer start to be completely removed from the primer or the substrate. The load at this point, so called Critical Load, Lc, is used to compare the cohesive or adhesive properties of the paint as summarized in Table 1.

 

It is evident that the paint Sample D has the best interfacial adhesion – exhibiting the highest Lc values of 4.04 N at paint delamination and 36.61 N at primer delamination. Sample B shows the second best scratch resistance. From the scratch analysis, we show that optimization of the paint formula is critical to the mechanical behaviors, or more specifically, scratch resistance and adhesion property of acrylic floor paints.

Table 1: Summary of critical loads.

FIGURE 6: Micrographs of full scratch with 5 N maximum load.

FIGURE 7: Micrographs of full scratch with 35 N maximum load.

CONCLUSION

Compared to the conventional Taber abrasion measurements, the NANOVEA Mechanical Tester and Tribometer are superior tools for evaluation and quality control of commercial floor and automotive coatings. The NANOVEA Mechanical Tester in Scratch mode can detect adhesion/cohesion problems in a coating system. The NANOVEA Tribometer provides well-controlled quantifiable and repeatable tribological analysis on wear resistance and coefficient of friction of the paints.

 

Based on the comprehensive tribological and mechanical analyses on the water based acrylic floor coatings tested in this study, we show that Sample B possesses the lowest COF and wear rate and the second best scratch resistance, while Sample D exhibits the best scratch resistance and second best wear resistance. This assessment allows us to evaluate and select the best candidate targeting the needs in different application environments.

 

The Nano and Micro modules of the NANOVEA Mechanical Tester all include ISO and ASTM compliant indentation, scratch and wear tester modes, providing the widest range of testing available for paint evaluation on a single module. The NANOVEA 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 mechanical/tribological 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. Optional NANOVEA Non-Contact Optical Profilers are available for high resolution 3D imaging of scratchs and wear tracks in addition to other surface measurements such as roughness.

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Titanium Nitride Coating Scratch Test

TITANIUM NITRIDE COATING SCRATCH TEST

QUALITY CONTROL INSPECTION

Prepared by

DUANJIE LI, PhD

INTRODUCTION

The combination of high hardness, excellent wear resistance, corrosion resistance and inertness makes titanium nitride (TiN) an ideal protective coating for metal components in various industries. For example, the edge retention and corrosion resistance of a TiN coating can substantially increase the work efficiency and extend the service life of machine tooling such as razor blades, metal cutters, injection molds and saws. Its high hardness, inertness and non-toxicity make TiN a great candidate for applications in medical devices including implants and surgical instruments.

IMPORTANCE OF TiN COATING SCRATCH TESTING

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 stress¹. The thermal expansion mismatch between the coating and the substrate created during coating deposition at elevated temperatures leads to high thermal residual stress. Moreover, TiN coated tools are often used under very high concentrated stresses, e.g. drill bits and bearings. It is critical to developing a reliable quality control process to quantitatively inspect the cohesive and adhesive strength of protective functional coatings.

[1] V. Teixeira, Vacuum 64 (2002) 393–399.

MEASUREMENT OBJECTIVE

In this study, we showcase that the NANOVEA Mechanical Testers in Scratch Mode are ideal for assessing the cohesive/adhesive strength of protective TiN coatings in a controlled and quantitative manner.

NANOVEA

PB1000

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nanoindenter and scratch tester Nanovea PB1000

TEST CONDITIONS

The NANOVEA PB1000 Mechanical Tester was used to perform coating scratch tests on three TiN coatings using the same test parameters as summarized below:

LOADING MODE: Progressive Linear

INITIAL LOAD

0.02 N

FINAL LOAD

10 N

LOADING RATE

20 N/min

SCRATCH LENGTH

5 mm

INDENTER TYPE

Sphero-Conical

Diamond, 20 μm radius

RESULTS & DISCUSSION

FIGURE 1 shows the recorded evolution of penetration depth, coefficient of friction (COF) and acoustic emission during the test. The full micro scratch tracks on the TiN samples are shown in FIGURE 2. The failure behaviors at different critical loads are displayed in FIGURE 3, where critical load Lc1 is defined as the load at which the first sign of cohesive crack occurs in the scratch track, Lc2 is the load after which repeated spallation failures take place, and Lc3 is the load at which the coating is completely removed from the substrate. The critical load (Lc) values for the TiN coatings are summarized in FIGURE 4.

The evolution of penetration depth, COF and acoustic emission provides insight into the mechanism of the coating failure at different stages, which are represented by the critical loads in this study. It can be observed that Sample A and Sample B exhibit comparable behavior during the scratch test. The stylus progressively penetrates into the sample to a depth of ~0.06 mm and the COF gradually increases to ~0.3 as the normal load increases linearly at the beginning of the coating scratch test. When the Lc1 of ~3.3 N is reached, the first sign of chipping failure occurs. This is also reflected in the first large spikes in the plot of penetration depth, COF and acoustic emission. As the load continues to increase to Lc2 of ~3.8 N, further fluctuation of the penetration depth, COF and acoustic emission takes place. We can observe continuous spallation failure present on both sides of the scratch track. At the Lc3, the coating completely delaminates from the metal substrate under the high pressure applied by the stylus, leaving the substrate exposed and unprotected.

In comparison, Sample C exhibits lower critical loads at different stages of the coating scratch tests, which is also reflected in the evolution of penetration depth, coefficient of friction (COF) and acoustic emission during the coating scratch test. Sample C possesses an adhesion interlayer with lower hardness and higher stress at the interface between the top TiN coating and the metal substrate compared to Sample A and Sample B.

This study demonstrates the importance of proper substrate support and coating architecture to the quality of the coating system. A stronger interlayer can better resist deformation under a high external load and concentration stress, and thus enhance the cohesive and adhesive strength of the coating/substrate system.

FIGURE 1: Evolution of penetration depth, COF and acoustic emission of the TiN samples.

FIGURE 2: Full scratch track of the TiN coatings after the tests.

FIGURE 3: TiN coating failures under different critical loads, Lc.

FIGURE 4: Summary of critical load (Lc) values for the TiN coatings.

CONCLUSION

In this study, we showcased that the NANOVEA PB1000 Mechanical Tester performs reliable and accurate scratch tests on TiN-coated samples in a controlled and closely monitored manner. Scratch measurements allow users to quickly identify the critical load at which typical cohesive and adhesive coating failures occur. Our instruments are superior quality control tools that can quantitatively inspect and compare the intrinsic quality of a coating and the interfacial integrity of a coating/substrate system. A coating with a proper interlayer can resist large deformation under a high external load and concentration stress, and enhance the cohesive and adhesive strength of a coating/substrate system.

The Nano and Micro modules of a 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.

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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

nanoindenter and scratch tester 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
 

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.

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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

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