Category: Mechanical Testing

Humidity-Controlled Nanoindentation of Polymer Materials

Application Note | Environmental Nanoindentation

Humidity-Controlled Nanoindentation of Polymer Films

Measuring Hardness and Creep Under Controlled Relative Humidity

Research & Experimental Testing

Duanjie Li, PhD & Andrea Novitsky

Visual Design & Editorial

Andrew Shore

Introduction

Polymers are viscoelastic materials, meaning their mechanical response can change with time and environmental conditions. Under sustained loading, they can gradually deform through creep, with the rate of deformation influenced by factors such as material properties, exposure time, temperature, and humidity.

As environmental humidity changes, the mechanical behavior of polymer materials can change as well. Measuring hardness and creep under controlled relative humidity provides a quantitative way to evaluate how moisture exposure affects polymer performance.

Why Humidity-Controlled Nanoindentation Matters

The mechanical properties of polymers can change as environmental humidity increases. As moisture is absorbed, polymers may exhibit mechano-sorptive effects, including accelerated creep and changes in deformation behavior under load.

Reliable characterization therefore requires more than measuring the material at a single ambient condition. Humidity-controlled nanoindentation enables hardness and creep to be measured while both the sample and indenter are maintained in a uniform controlled environment.

The NANOVEA Mechanical Tester uses an isolated humidity enclosure around the indentation tip and sample surface to maintain consistent relative humidity during testing. This helps minimize measurement drift caused by humidity gradients and provides a quantitative way to evaluate moisture-dependent mechanical behavior.

Measurement Objective

The objective of this study was to evaluate how controlled relative humidity influences the hardness and creep behavior of a polymer film using nanoindentation.

The polymer film was tested in an isolated environment with uniform humidity surrounding both the sample and indenter, allowing its mechanical response to be measured under controlled moisture conditions.

NANOVEA PB1000 Advanced

Mechanical Tester

Test Conditions

A polymer film was tested by nanoindentation at 25, 35, 45, 55, 65, and 75% relative humidity. Both the sample and indenter were maintained inside an isolated enclosure with uniform humidity controlled throughout the test.

Polymer film sample used for humidity-controlled nanoindentation testing.

A Berkovich diamond indenter was used with a maximum load of 10 mN. The load was applied and removed at 20 mN/min, and creep was measured from the change in indentation depth during a 10 s hold at maximum load.

Hardness was calculated using ASTM E2546 and the Oliver & Pharr method. The test conditions are summarized below.

Humidity (%)	25, 35, 45, 55, 65, 75
Maximum load	10 mN
Loading rate	20 mN/min
Unloading rate	20 mN/min
Creep time	10 s
Computation method	ASTM E2546 & Oliver & Pharr
Indenter type	Berkovich diamond

Results and Discussion

The load-displacement curves show a progressive increase in penetration depth as relative humidity rises, indicating that the polymer film becomes more susceptible to deformation under the same applied load.

Between 25% and 55% relative humidity, hardness decreased gradually from approximately 0.60 to 0.54 GPa, while creep depth increased from 36 to 48 nm. At higher humidity, the changes became substantially more pronounced. Hardness decreased to 0.46 GPa at 65% RH and 0.31 GPa at 75% RH, while creep depth increased to 80 nm and 105 nm, respectively.

The original study attributes this stronger response at elevated humidity to moisture absorption and swelling of the polymer film. It identifies the transition between 55% and 65% RH as the range where swelling becomes significant, corresponding with the sharp increase in creep observed during indentation.

These results demonstrate why humidity can be an important test variable when evaluating polymers intended for moisture-rich environments. Measuring both hardness and creep across controlled humidity levels provides a more complete view of how the material responds mechanically as environmental conditions change.

Nanoindentation load-displacement curves at relative humidity levels from 25% to 75%.

Polymer hardness decreases while creep depth increases as relative humidity rises from 25% to 75%.

Conclusion

Humidity-controlled nanoindentation revealed a clear change in the mechanical response of the polymer film as relative humidity increased. Across the tested range from 25% to 75% RH, hardness progressively decreased while creep increased.

At 65% RH and above, the polymer exhibited substantially greater creep deformation during the hold at maximum load, corresponding with the sharper reduction in hardness observed at higher humidity.

By maintaining both the sample and indenter within an isolated environment of uniform relative humidity, the NANOVEA Mechanical Tester enables hardness and creep to be measured while minimizing the influence of humidity-gradient drift. This provides a quantitative method for evaluating the moisture-dependent mechanical behavior of polymer materials under controlled environmental conditions.

Frequently Asked Questions About Humidity-Controlled Nanoindentation

Why does humidity affect polymer hardness and creep?

Polymers can absorb moisture from the surrounding environment, which can alter their mechanical response. Depending on the material, increased moisture can reduce resistance to deformation and increase time-dependent creep. In this study, increasing relative humidity corresponded with decreasing hardness and increasing creep depth.

Can nanoindentation be performed under controlled humidity?

Yes. Nanoindentation can be performed inside a controlled environmental enclosure so that both the sample and indenter are exposed to a defined relative humidity during testing. This makes it possible to compare mechanical properties under different moisture conditions rather than relying solely on uncontrolled ambient laboratory conditions.

Why test polymers at controlled relative humidity instead of ambient conditions?

Ambient humidity can vary and may not represent the conditions a polymer experiences during storage, processing, or use. Controlling relative humidity allows the environmental condition to become a defined test variable, making it possible to determine whether changes in hardness, creep, or deformation behavior are associated with moisture exposure.

What mechanical properties can be measured under controlled humidity?

Depending on the test method, nanoindentation can evaluate properties including hardness, elastic modulus, and time-dependent creep behavior under controlled environmental conditions. In this study, hardness and creep were measured as relative humidity changed.

What materials can benefit from humidity-controlled nanoindentation?

Humidity-controlled testing can be particularly useful for polymers, thin films, coatings, and other materials whose mechanical behavior may be influenced by moisture absorption. The appropriate humidity range and indentation conditions depend on the material and application.

How can humidity-controlled nanoindentation support material development?

Testing across multiple relative humidity levels can reveal whether a material maintains its mechanical properties as environmental moisture changes. This can support material comparison, formulation development, coating evaluation, failure investigation, and the assessment of materials intended for humidity-sensitive applications.

Can NANOVEA perform humidity-controlled nanoindentation as a laboratory service?

Yes. NANOVEA can perform nanoindentation testing under controlled environmental conditions to evaluate properties such as hardness and creep as humidity changes. Test parameters can be selected according to the material, expected service conditions, and the specific engineering question being investigated.

Need Humidity-Controlled Nanoindentation for Your Material?

High Temperature Brinell Hardness Testing

Application Note | High Temperature Mechanical Testing

High Temperature Hardness Testing of Steel Using Brinell Indentation

Mapping Steel Hardness Loss from Room Temperature to 925°C with NANOVEA T2000 Tribometer

Research & Experimental Testing

Frank Liu

Visual Design & Editorial

Andrew Shore

Introduction

High temperature hardness testing provides insight into how the mechanical behavior of metals changes as temperature increases. Materials that exhibit high hardness at room temperature can soften significantly when exposed to elevated temperatures, making temperature-dependent hardness an important consideration when selecting materials for applications such as jet engines, high-temperature processing equipment, and other thermally demanding environments.

In this study, a steel sample was evaluated using Brinell indentation with the NANOVEA T2000 Tribometer. Hardness measurements were performed at 25, 200, 400, 600, 800, and 925°C to map the change in steel hardness with temperature. The results show a gradual reduction in hardness through approximately 600°C, followed by a much sharper decline at higher temperatures, resulting in an 84% decrease in hardness between room temperature and 925°C.

Why High Temperature Hardness Testing Matters

Hardness is a mechanical property that describes a material’s resistance to localized deformation. Higher hardness generally corresponds to greater resistance to indentation and permanent surface deformation.

Temperature can significantly alter this behavior. A material that remains hard at room temperature may soften as temperature increases, changing its mechanical response under elevated-temperature conditions. For materials intended for high-temperature applications, understanding these changes is important when evaluating their mechanical limits.

High temperature hardness testing makes it possible to measure these changes directly as temperature increases rather than relying only on room-temperature properties. In this study, the steel sample provides a clear example of how hardness can remain relatively stable over part of the temperature range before declining rapidly at higher temperatures.

Measurement Objective

The objective of this study was to evaluate how the Brinell hardness of steel changes as temperature increases from room temperature to 925°C.

Using a 10 mm tungsten carbide (WC) ball, a load of 1000 N (~100 kgf) was applied to the steel sample at 25, 200, 400, 600, 800, and 925°C. The resulting indentations were measured using NANOVEA’s 3D Line Sensor to determine their diameter for Brinell hardness calculation.

NANOVEA T2000 High Load

Pneumatic Tribometer

Test Procedure

High temperature Brinell hardness testing was performed with the steel sample mounted inside the NANOVEA T2000 heated chamber. The sample was tested at six temperatures from 25°C to 925°C using a 10 mm tungsten carbide (WC) ball with an applied test force of 1000 N (~100 kgf).

The test parameters used throughout the study are summarized below.

Steel sample mounted in the NANOVEA T2000 high temperature chamber for Brinell hardness testing from 25°C to 925°C.

Test Parameters

Test Parameter	High Temperature Brinell Hardness Setup
Temperature	25, 200, 400, 600, 800, 925°C
Test force	1000 N (~100 kgf)
Force-diameter ratio	1
Ball material	Tungsten carbide (WC)
Ball diameter	10 mm

Steel samples used in the high temperature Brinell hardness study from room temperature to 925°C.

Results and Discussion

Brinell hardness was calculated from the applied force, ball diameter, and measured indentation diameter using the equation below:

Where F (kgf) is the applied force expressed in kilogram-force, D is the ball diameter, and d is the measured indentation diameter. Two diameter measurements were taken for each indent and averaged to determine the value of d used in the hardness calculation.

Load vs. time profile for the 1000 N Brinell indentations performed during high temperature hardness testing.

The loading curve shows the applied load profile used during indentation. A consistent 1000 N (~100 kgf) test force was used throughout the temperature series so that the resulting indentation dimensions and calculated hardness values could be compared across each test condition.

Distance	Unit	A	B
HDist	mm	1.807	1.830

Brinell indentation measured at 800°C. Two diameter measurements of 1.807 mm and 1.830 mm were averaged to determine the indentation diameter used for hardness calculation.

At 800°C, the measured indentation diameters were 1.807 mm and 1.830 mm, producing an average diameter of approximately 1.819 mm. The indentation diameter increased substantially at the higher test temperatures as the steel became softer under the same applied load.

The measured indentation diameters were then used to calculate Brinell hardness at each temperature. The results show a relatively gradual decrease from 96.12 HBW at 25°C to 79.69 HBW at 600°C, followed by a much sharper decrease to 38.18 HBW at 800°C and 15.40 HBW at 925°C.

Brinell Hardness Results

Temperature (°C)	Diameter 1 (mm)	Diameter 2 (mm)	Average Diameter (mm)	HBW (10/100)
High Temperature Brinell Hardness Results
25	1.153	1.145	1.149	96.12
200	1.150	1.201	1.176	91.82
400	1.165	1.261	1.213	86.21
600	1.265	1.258	1.262	79.69
800	1.807	1.830	1.819	38.18
925	2.858	2.833	2.846	15.40

The temperature-dependent trend is clear. Steel hardness decreased moderately between room temperature and 600°C, then declined rapidly at higher temperatures. Between 25°C and 925°C, the measured Brinell hardness decreased from 96.12 to 15.40 HBW, representing an overall hardness loss of approximately 84%.

These results demonstrate why hardness measured at room temperature alone may not fully represent material behavior in high-temperature applications. For this steel sample, the most substantial loss in hardness occurred above approximately 600°C.

Conclusion

High temperature hardness testing revealed a strong temperature-dependent change in the Brinell hardness of the steel sample. Hardness decreased gradually as temperature increased from 25°C to 600°C, then declined much more sharply at higher temperatures. By 925°C, the measured hardness had fallen from 96.12 HBW to 15.40 HBW, representing an overall decrease of approximately 84%.

The study demonstrates the ability of the NANOVEA T2000 Tribometer to perform Brinell hardness measurements under elevated-temperature conditions. Using a 1000 N (~100 kgf) test force, the steel sample was evaluated from 25°C to 925°C, allowing its change in hardness to be measured directly across the tested temperature range.

The results also highlight the importance of selecting an appropriate force-diameter ratio across a wide temperature range. Because of the large difference in hardness between room temperature and high temperature, the study recommends a force-diameter ratio of 5 or 10 at lower temperatures, while a ratio of 1 is suitable above 900°C.

Frequently Asked Questions About High Temperature Hardness Testing

What is high temperature hardness testing used for?

High temperature hardness testing evaluates how a material’s resistance to indentation changes as temperature increases. It is useful for materials intended for thermally demanding applications where room-temperature hardness may not represent mechanical behavior at operating temperature.

Can Brinell hardness be measured at elevated temperatures?

Yes. Elevated-temperature Brinell hardness testing applies a controlled force using a ball of known diameter while the specimen is heated to the required test temperature. In this study, steel was tested from 25°C to 925°C using a 10 mm tungsten carbide ball and a 1000 N test force.

Why measure hardness while the material is hot?

Testing at temperature measures hardness under the thermal condition of interest rather than only after the specimen returns to room temperature. This makes it possible to directly characterize temperature-dependent softening and identify changes that may not be represented by room-temperature hardness values.

What equipment is used for high temperature hardness testing?

High temperature hardness testing requires controlled specimen heating, precise mechanical loading and measurement of the resulting indentation. The NANOVEA T2000 can integrate high-temperature environmental control with mechanical testing for evaluating material behavior under elevated-temperature conditions.

Can high temperature hardness testing be used for aerospace materials?

Yes. Elevated-temperature hardness measurements are relevant when evaluating materials intended for thermally demanding aerospace environments, including jet-engine and other high-temperature components. Testing helps characterize how hardness changes as exposure temperature increases.

Can NANOVEA perform high temperature hardness testing as a laboratory service?

NANOVEA provides materials testing services using its mechanical testing and tribology platforms. Application requirements, temperature range, load, specimen geometry and measurement method can be reviewed with a NANOVEA applications engineer to determine an appropriate high-temperature testing approach.

Need High Temperature Hardness Testing for Your Material?

Scratch Resistance Testing of Phone Screen Protectors

Prepared by

Stacey Pereira, Jocelyn Esparza, and Pierre Leroux

Understanding Scratch Resistance in Phone Screen Protectors

Protective coatings on phone screens play a critical role in scratch resistance, adhesion strength, and long-term durability. Over time, scratches, micro-cracks, and coating delamination can reduce optical clarity and reliability — especially in high-use environments. To evaluate how different screen protectors resist mechanical damage, instrumented scratch testing provides quantifiable insight into coating failure mechanisms, including adhesion, cohesion, and fracture behavior.

In this study, NANOVEA PB1000 Mechanical Tester is used to compare TPU vs. tempered-glass screen protectors under controlled progressive loading. Using precise acoustic emission detection, we identify critical failure loads and characterize how each material responds to increasing mechanical stress.

Why Scratch Resistance Testing Matters for Screen Protectors

Many users assume that thicker or harder protectors automatically perform better, but real durability depends on how the material behaves under progressive load, surface deformation, and localized stress. Instrumented scratch testing allows engineers to measure coating adhesion, cohesive strength, surface wear resistance, and the exact loads at which failures initiate or propagate.

By analyzing crack initiation points, delamination behavior, and failure modes, manufacturers can validate screen-protector performance for R&D, quality control, or comparative benchmarking. Nano- and micro-scratch testing offer repeatable, data-driven insight into real-world durability far beyond traditional hardness ratings.

ℹ️ Learn more about scratch and adhesion testing services for coatings and screen protectors.

Scratch Testing Objective:
Measuring Failure Loads in Screen Protectors

The objective of this study is to demonstrate how the NANOVEA PB1000 Mechanical Tester performs repeatable, standardized scratch resistance testing on both polymeric and glass screen protectors. By progressively increasing the applied load, the system detects critical loads for cohesive and adhesive failure, captures acoustic emission signals, and correlates these events with scratch depth, friction force, and surface deformation.

This methodology provides a complete mechanical profile of each protective coating, allowing manufacturers and R&D teams to evaluate material formulations, coating adhesion strength, surface durability, and optimal coating thickness for improved product performance. These scratch evaluations are part of NANOVEA’s broader suite of mechanical testing solutions used to characterize coatings, films, and substrates across R&D, quality control, and production environments.

NANOVEA PB1000 Large-Platform
Mechanical Tester

Scratch Test Parameters and Instrument Setup

The scratch resistance evaluation of TPU and tempered-glass screen protectors was conducted under controlled conditions to ensure repeatability and accurate failure-load detection. The following parameters define the progressive-load scratch testing setup used on the NANOVEA PB1000 Mechanical Tester.

LOAD TYPE	PROGRESSIVE
INITIAL LOAD	0.1 N
FINAL LOAD	12 N
SLIDING SPEED	3.025 mm/min
SLIDING DISTANCE	3 mm
INDENTER GEOMETRY	ROCKWELL (120° CONE)
INDENTER MATERIAL (TIP)	DIAMOND
INDENTER TIP RADIUS	50 µm
ATMOSPHERE	AIR
TEMPERATURE	24 °C (ROOM TEMP)

TABLE 1: Test parameters used for scratch testing

Screen protector sample mounted on the NANOVEA PB1000 Mechanical Tester during progressive-load scratch measurement.

Screen Protector Samples Used for Scratch Resistance Testing

Two commercially available screen protector materials were selected to compare differences in scratch resistance, failure behavior, and mechanical durability. Both samples were mounted securely on the NANOVEA PB1000 Mechanical Tester and evaluated under identical progressive-load conditions to ensure a consistent and unbiased comparison.

The TPU screen protector represents a flexible polymeric film with high elasticity but lower abrasion resistance, while the tempered-glass protector represents a rigid, brittle material designed for high hardness and enhanced impact protection. Testing both materials under the same load profile allows a clear assessment of how material composition, elasticity, and hardness influence scratch failure modes.

TPU Screen Protector

Tempered Glass

FIGURE 1: TPU and tempered-glass screen protectors prepared for scratch resistance testing.

Scratch Test Results: Failure Modes in TPU vs. Tempered Glass Screen Protectors

TYPE OF SCREEN PROTECTOR	CRITICAL LOAD #1 (N)	CRITICAL LOAD #2 (N)
TPU	n/a	2.004 ± 0.063
TEMPERED GLASS	3.608 ± 0.281	7.44 ± 0.995

TABLE 2: Summary of critical loads for each screen protector sample.

Because TPU and tempered-glass screen protectors have fundamentally different mechanical properties, each sample exhibited distinct failure modes and critical load thresholds during progressive-load scratch testing. Table 2 summarizes the measured critical loads for each material.

Critical Load #1 represents the first observable point of cohesive failure under optical microscopy, such as crack initiation or radial fracture.

Critical Load #2 corresponds to the first major event detected through acoustic emission (AE) monitoring, typically representing a larger structural failure or penetration event.

TPU Screen Protector — Flexible Polymer Behavior

The TPU screen protector exhibited only one significant critical event (Critical Load #2). This load corresponds to the point along the scratch track where the film began to lift, peel, or delaminate from the phone screen surface.

Once Critical Load #2 (≈2.00 N) was exceeded, the indenter penetrated sufficiently to cause a visible scratch directly on the phone screen for the remainder of the test. No separate Critical Load #1 event was detectable, consistent with the material’s high elasticity and lower cohesive strength.

Tempered Glass Screen Protector — Brittle Failure Behavior

The tempered-glass screen protector showed two distinct critical loads, characteristic of brittle materials:

Critical Load #1 (≈3.61 N): Radial fractures and crack initiation were observed under the microscope, indicating early cohesive failure of the glass layer.
Critical Load #2 (≈7.44 N): A large AE spike and a sharp increase in scratch depth indicated protector penetration at higher loads.

Although the AE magnitude was higher than TPU, no damage was transferred to the phone screen, demonstrating the tempered-glass protector’s ability to absorb and distribute load before catastrophic failure.

In both materials, Critical Load #2 corresponded to the moment when the indenter broke through the screen protector, confirming the protective limit of each sample.

TPU Screen Protector: Scratch Test Data and Failure Analysis

SCRATCH	CRITICAL LOAD #2 (N)
1	2.033
2	2.047
3	1.931
AVERAGE	2.003
STANDARD DEVIATION	0.052

TABLE 3: Critical loads measured during TPU screen protector scratch testing.

FIGURE 2: Friction force, normal load, acoustic emission (AE), and scratch depth vs. scratch length for the TPU screen protector. (B) Critical Load #2

FIGURE 3: Optical microscopy image of the TPU screen protector at Critical Load #2 (5× magnification; image width 0.8934 mm).

FIGURE 4: Full-length post-scratch image of the TPU screen protector showing the complete scratch track following progressive-load testing.

Tempered Glass Screen Protector: Critical Load Data and Fracture Behavior

SCRATCH	CRITICAL LOAD #1 (N)	CRITICAL LOAD #2 (N)
1	3.923	7.366
2	3.382	6.483
3	3.519	8.468
AVERAGE	3.653	6.925
STANDARD DEVIATION	0.383	0.624

TABLE 4: Critical loads measured during tempered-glass screen protector scratch testing.

ℹ️ For comparison with non-silicate polymer coatings, see our study on PTFE coating wear testing, which highlights failure behavior in low-friction polymer films under similar progressive-load conditions.

FIGURE 5: Friction force, normal load, acoustic emission (AE), and scratch depth vs. scratch length for the tempered-glass screen protector. (A) Critical Load #1 (B) Critical Load #2

FIGURE 6: Optical microscopy images showing the failure locations for Critical Load #1 (left) and Critical Load #2 (right) at 5× magnification (image width: 0.8934 mm).

FIGURE 7: Post-test optical microscopy image of the tempered-glass scratch track, highlighting fracture initiation (CL#1) and the final penetration zone (CL#2) following progressive-load testing.

Conclusion: Scratch Performance Comparison of TPU vs. Tempered Glass Screen Protectors

This study demonstrates how the NANOVEA PB1000 Mechanical Tester delivers controlled, repeatable, and highly sensitive scratch resistance measurements using progressive loading and acoustic emission (AE) detection. By precisely capturing both cohesive and adhesive failure events, the system enables a clear comparison of how TPU and tempered-glass screen protectors behave under increasing mechanical stress.

The experimental results confirm that tempered glass exhibits significantly higher critical loads than TPU, providing superior scratch resistance, delayed fracture initiation, and reliable protection against indenter penetration. TPU’s lower cohesive strength and earlier delamination highlight its limitations in high-stress environments.

After identifying failure loads, the resulting scratch tracks can also be analyzed using a non-contact 3D optical profilometer to measure groove depth, residual deformation, and post-scratch topography. This helps complete the mechanical profile of each material.

The NANOVEA Mechanical Tester is engineered for accurate and repeatable indentation, scratch, and wear testing, and supports ISO- and ASTM-compliant nano and micro modules. Its versatility makes it an ideal solution for evaluating the full mechanical profile of thin films, coatings, polymers, glasses, and substrates across R&D, production, and quality control.

Frequently Asked Questions
About Scratch Resistance Testing

What is scratch resistance testing?

Scratch resistance testing evaluates how a material or coating responds when a diamond stylus applies a progressively increasing load. The test identifies the critical loads where cohesive or adhesive failures occur, providing a quantifiable measure of durability, adhesion strength, and resistance to surface damage.

What’s the difference between cohesive and adhesive failure?

Cohesive failure occurs within the coating or material, such as cracking, tearing, or internal fracture.
Adhesive failure happens when the coating detaches from the substrate, indicating insufficient bonding strength.

The NANOVEA PB1000 detects both using synchronized acoustic emission monitoring, scratch depth tracking, and friction analysis.

Why use a mechanical tester instead of manual methods?

A mechanical tester like the NANOVEA PB1000 provides precise, repeatable, and standardized measurements, ensuring reliable data for R&D, production validation, and quality control. It also offers advanced features, such as acoustic emission detection and real-time depth monitoring, that manual methods cannot deliver.

Need Reliable Scratch Testing for Your Materials?

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

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

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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Dynamic Mechanical Analysis of Cork Using Nanoindentation

DYNAMIC MECHANICAL ANALYSIS

OF CORK USING NANOINDENTATION

Prepared by

FRANK LIU

INTRODUCTION

Dynamic Mechanical Analysis (DMA) is a powerful technique used to investigate the mechanical properties of materials. In this application, we focus on the analysis of cork, a widely used material in wine sealing and aging processes. Cork, obtained from the bark of the Quercus suber oak tree, exhibits distinct cellular structures that provide mechanical properties resembling synthetic polymers. In one axis, the cork has honeycomb structure. The two other axes are structured in multiple rectangular-like prisms. This gives cork diﬀerent mechanical properties depending on the orientation being tested.

IMPORTANCE OF DYNAMIC MECHANICAL ANALYSIS (DMA) TESTING IN ASSESSING CORK MECHANICAL PROPERTIES

The quality of corks greatly relies on their mechanical and physical properties, which are crucial for their eﬀectiveness in wine sealing. Key factors determining cork quality include ﬂexibility, insulation, resilience, and impermeability to gas and liquids. By utilizing dynamic mechanical analysis (DMA) testing, we can quantitatively assess the ﬂexibility and resilience properties of corks, providing a reliable method for evaluation.

The NANOVEA PB1000 Mechanical Tester in the Nanoindentation mode enables the characterization of these properties, speciﬁcally Young’s modulus, storage modulus, loss modulus, and tan delta (tan (δ)). DMA testing also allows for the collection of valuable data on phase shift, hardness, stress, and strain of the cork material. Through these comprehensive analyses, we gain deeper insights into the mechanical behavior of corks and their suitability for wine sealing applications.

MEASUREMENT OBJECTIVE

In this study, perform dynamic mechanical analysis (DMA) on four cork stoppers using the NANOVEA PB1000 Mechanical Tester in the Nanoindentation mode. The quality of the cork stoppers is labeled as: 1 – Flor, 2 – First, 3 – Colmated, 4 – Synthetic rubber. DMA indentation tests were conducted in both the axial and radial directions for each cork stopper. By analyzing the mechanical response of the cork stoppers, we aimed to gain insights into their dynamic behavior and evaluate their performance under diﬀerent orientations.

NANOVEA

PB1000

TEST PARAMETERS

MAX FORCE	75 mN
LOADING RATE	150 mN/min
UNLOADING RATE	150 mN/min
AMPLITUDE	5 mN
FREQUENCY	1 Hz
CREEP	60 s

indenter type

Ball

51200 Steel

3 mm Diameter

RESULTS

In the tables and graphs below, the Young’s modulus, storage modulus, loss modulus, and tan delta are compared between each sample and orientation.

Young’s modulus: Stiﬀness; high values indicate stiﬀ, low values indicate ﬂexible.

Storage modulus: Elastic response; energy stored in the material.

Loss modulus: Viscous response; energy lost due to heat.

Tan (δ): Dampening; high values indicate more dampening.

AXIAL ORIENTATION

*Stopper*	*YOUNG’S MODULUS*	*STORAGE MODULUS*	*LOSS MODULUS*	*TAN*
#	*(MPa)*	*(MPa)*	*(MPa)*	*(δ)*
1	22.5675	22.27209	3.624947	0.162964
2	18.54664	18.27153	3.162349	0.17409
3	23.75381	23.47267	3.617819	0.154592
4	23.6972	23.58064	2.347008	0.099539

RADIAL ORIENTATION

*Stopper*	*YOUNG’S MODULUS*	*STORAGE MODULUS*	*LOSS MODULUS*	*TAN*
#	*(MPa)*	*(MPa)*	*(MPa)*	*(δ)*
1	24.78863	24.56542	3.308224	0.134865
2	26.66614	26.31739	4.286216	0.163006
3	44.07867	43.61426	6.365979	0.146033
4	28.04751	27.94148	2.435978	0.087173

YOUNG’S MODULUS

STORAGE MODULUS

LOSS MODULUS

TAN DELTA

Between cork stoppers, the Young’s modulus is not very different when tested in the axial orientation. Only Stopper #2 and #3 showed an apparent difference in the Young’s modulus between the radial and axial direction. As a result, the storage modulus and loss modulus will also be higher in the radial direction than in the axial direction. Stopper #4 shows similar characteristics with the natural cork stoppers, except in the loss modulus. This is quite interesting since it means the natural corks has a more viscous property than the synthetic rubber material.

CONCLUSION

The NANOVEA Mechanical Tester in the Nano Scratch Tester mode allows 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 to obtain corrected depth during the scratch and also to measure 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 technique of the instrument which can help manufacturers improved the quality of their hard coat/paint and study weathering eﬀects.

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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

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

indenter type

Conical

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.

CRITICAL FAILURE:

COMPLETE DAMAGE

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

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

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

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

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

FIGURE 5: Friction Force and Coeﬃcient of Friction.

FIGURE 6: Surface Profile.

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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High Temperature Scratch Hardness using a Tribometer

HIGH TEMPERATURE SCRATCH HARDNESS

USING A TRIBOMETER

Prepared by

DUANJIE, PhD

INTRODUCTION

Hardness measures the resistance of materials to permanent or plastic deformation. Originally developed by a German mineralogist Friedrich Mohs in 1820, scratch hardness test determines the hardness of a material to scratches and abrasion due to friction from a sharp object¹. The Mohs’ scale is a comparative index rather than a linear scale, therefore a more accurate and qualitative scratch hardness measurement was developed as described in ASTM standard G171-03². It measures the average width of the scratch created by a diamond stylus and calculates the scratch hardness number (HSP).

IMPORTANCE OF SCRATCH HARDNESS MEASUREMENT AT HIGH TEMPERATURES

Materials are selected based on the service requirements. For applications involving significant temperature changes and thermal gradients, it is critical to investigate the mechanical properties of materials at high temperatures to be fully aware of the mechanical limits. Materials, especially polymers, usually soften at high temperatures. A lot of mechanical failures are caused by creep deformation and thermal fatigue taking place only at elevated temperatures. Therefore, a reliable technique for measuring hardness at high temperatures is in need to ensure proper selection of the materials for high temperature applications.

MEASUREMENT OBJECTIVE

In this study, the NANOVEA T50 Tribometer measures scratch hardness of a Teflon sample at different temperatures from room temperature to 300ºC. The capability of performing high temperature scratch hardness measurement makes the NANOVEA Tribometer a versatile system for tribological and mechanical evaluations of materials for high temperature applications.

NANOVEA

T50

TEST CONDITIONS

The NANOVEA T50 Free Weight Standard Tribometer was used to perform the scratch hardness tests on a Teflon sample at temperatures ranging from room temperature (RT) to 300°C. Teflon has a melting point of 326.8°C. A conical diamond stylus of apex angle 120° with tip radius of 200 µm was used. The Teflon sample was fixed on the rotative sample stage with a distance of 10 mm to the stage center. The sample was heated up by an oven and tested at temperatures of RT, 50°C, 100°C, 150°C, 200°C, 250°C and 300°C.

TEST PARAMETERS

of the high temperature scratch hardness measurement

NORMAL FORCE	2 N
SLIDING SPEED	1 mm/s
SLIDING DISTANCE	8mm per temp
ATMOSPHERE	Air
TEMPERATURE	RT, 50°C, 100°C, 150°C, 200°C, 250°C, 300°C.

RESULTS & DISCUSSION

The scratch track profiles of the Teflon sample at different temperatures are shown in FIGURE 1 in order to compare the scratch hardness at different elevated temperatures. The material pile-up on the scratch track edges forms as the stylus travels at a constant load of 2 N and ploughs into the Teflon sample, pushing and deforming the material in the scratch track to the side.

The scratch tracks were examined under the optical microscope as shown in FIGURE 2. The measured scratch track widths and calculated scratch hardness numbers (HSP) are summarized and compared in FIGURE 3. The scratch track width measured by the microscope is in agreement with that measured using the NANOVEA Profiler – the Teflon sample exhibits a wider scratch width at higher temperatures. Its scratch track width increases from 281 to 539 µm as the temperature elevates from RT to 300oC, resulting in decreased HSP from 65 to 18 MPa.

The scratch hardness at elevated temperatures can be measured with high precision and repeatability using the NANOVEA T50 Tribometer. It provides an alternative solution from other hardness measurements and makes NANOVEA Tribometers a more complete system for comprehensive high-temperature tribo-mechanical evaluations.

FIGURE 1: Scratch track profiles after the scratch hardness tests at different temperatures.

FIGURE 2: Scratch tracks under the microscope after the measurements at different temperatures.

FIGURE 3: Evolution of the scratch track width and scratch hardness vs. the temperature.

CONCLUSION

In this study, we showcase how the NANOVEA Tribometer measures the scratch hardness at elevated temperatures in compliance to ASTM G171-03. The scratch hardness test at a constant load provides an alternative simple solution for comparing the hardness of materials using the tribometer. The capacity of performing scratch hardness measurements at elevated temperatures makes the NANOVEA Tribometer an ideal tool for evaluating the high temperature tribo-mechanical properties of materials.

The NANOVEA Tribometer also 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. Optional 3D non-contact profiler is available for high resolution 3D imaging of wear tracks in addition to other surface measurements such as roughness.

1 Wredenberg, Fredrik; PL Larsson (2009). “Scratch testing of metals and polymers: Experiments and numerics”. Wear 266 (1–2): 76
2 ASTM G171-03 (2009), “Standard Test Method for Scratch Hardness of Materials Using a Diamond Stylus”

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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.

NANOVEA T100

The Compact Pneumatic Tribometer

NANOVEA PB1000

The Large Platform Mechanical Tester

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 TYPE	Progressive
INITIAL LOAD	0.01 mN
FINAL LOAD	5 N / 35 N
LOADING RATE	10 / 70 N/min
SCRATCH LENGTH	3 mm
SCRATCHING SPEED, dx/dt	6.0 mm/min
INDENTER GEOMETRY	120º cone
INDENTER MATERIAL (tip)	Diamond
INDENTER TIP RADIUS	200 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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Scratch Hardness Measurement using Mechanical Tester

SCRATCH HARDNESS MEASUREMENT

USING A MECHANICAL TESTER

Prepared by

DUANJIE LI, PhD

INTRODUCTION

In general, hardness tests measure the resistance of materials to permanent or plastic deformation. There are three types of hardness measurements: scratch hardness, indentation hardness and rebound hardness. A scratch hardness test measures a material’s resistance to scratch and abrasion due to friction from a sharp object1. It was originally developed by German mineralogist Friedrich Mohs in 1820 and is still widely used to rank the physical properties of minerals2. This test method is also applicable to metals, ceramics, polymers, and coated surfaces.

During a scratch hardness measurement, a diamond stylus of specified geometry scratches into a material’s surface along a linear path under a constant normal force with a constant speed. The average width of the scratch is measured and used to calculate the scratch hardness number (HSP). This technique provides a simple solution for scaling the hardness of different materials.

MEASUREMENT OBJECTIVE

In this study, the NANOVEA PB1000 Mechanical Tester is used to measure the scratch hardness of different metals in compliance with ASTM G171-03.

Simultaneously, this study showcases the capacity of the NANOVEA Mechanical Tester in performing scratch hardness measurement with high precision and reproducibility.

NANOVEA

PB1000

TEST CONDITIONS

The NANOVEA PB1000 Mechanical Tester performed scratch hardness tests on three polished metals (Cu110, Al6061 and SS304). A conical diamond stylus of apex angle 120° with tip radius of 200 µm was used. Each sample was scratched three times with the same test parameters to ensure reproducibility of the results. The test parameters are summarized below. A profile scan at a low normal load of 10 mN was performed before and after the scratch test to measure the change in the surface profile of the scratch.

TEST PARAMETERS

NORMAL FORCE

10 N

TEMPERATURE

24°C (RT)

SLIDING SPEED

20 mm/min

SLIDING DISTANCE

10 mm

ATMOSPHERE

Air

RESULTS & DISCUSSION

The images of the scratch tracks of three metals (Cu110, Al6061 and SS304) after the tests are shown in FIGURE 1 in order to compare the scratch hardness of different materials. The mapping function of the NANOVEA Mechanical Software was used to create three parallel scratches tested under the same condition in an automated protocol. The measured scratch track width and calculated scratch hardness number (HSP) are summarized and compared in TABLE 1. The metals show different wear track widths of 174, 220 and 89 µm for Al6061, Cu110 and SS304, respectively, resulting in a calculated HSP of 0.84, 0.52 and 3.2 GPa.

In addition to the scratch hardness computed from the scratch track width, the evolution of coefficient of friction (COF), true depth and acoustic emission were recorded in situ during the scratch hardness test. Here, the true depth is the depth difference between the penetration depth of the stylus during the scratch test and the surface profile measured in the pre-scan. The COF, true depth and acoustic emission of Cu110 are shown in FIGURE 2 as an example. Such information provides insight into mechanical failures taking place during scratching, enabling users to detect mechanical defects and further investigate the scratch behavior of the tested material.

The scratch hardness tests can be finished within a couple of minutes with high precision and repeatability. Compared to conventional indentation procedures, the scratch hardness test in this study provides an alternative solution for hardness measurements, which is useful for quality control and the development of new materials.

Al6061

Cu110

SS304

FIGURE 1: Microscope image of the scratch tracks post test (100x magnification).

	*Scratch track width (μm)*	*HS_p (GPa)*
Al6061	174±11	0.84
Cu110	220±1	0.52
SS304	89±5	3.20

TABLE 1: Summary of scratch track width and scratch hardness number.

FIGURE 2: The evolution of coefficient of friction, true depth and acoustic emissions during the scratch hardness test on Cu110.

CONCLUSION

In this study, we showcased the capacity of the NANOVEA Mechanical Tester in performing scratch hardness tests in compliance to ASTM G171-03. In addition to coating adhesion and scratch resistance, the scratch test at a constant load provides an alternative simple solution for comparing the hardness of materials. In contrast to conventional scratch hardness testers, NANOVEA Mechanical Testers offer optional modules for monitoring the evolution of coefficient of friction, acoustic emission and true depth in situ.

The Nano and Micro modules of a NANOVEA Mechanical Tester 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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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

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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