The World’s Leading Micro Mechanical Tester

 

NOW THE WORLD'S LEADING

MICRO MECHANICAL TESTING

Prepared by

PIERRE LEROUX & DUANJIE LI, PhD

INTRODUCTION

Standard Vickers Micro Hardness Testers have usable load ranges from 10 to 2000 gram force (gf). Standard Vickers Macro Hardness Testers load from 1 to 50 Kgf. These instruments are not only very limited in range of loads but they are also inaccurate when dealing with rougher surfaces or low loads when indents become too small to be measured visually. These limitations are intrinsic to older technology and as a result, instrumented indentation is becoming the standard choice due to the higher accuracy and performance it brings.

With NANOVEA’s world leading micro mechanical testing systems, Vickers hardness is automatically calculated from depth versus load data with the widest load range on a single module ever available (0.3 grams to 2 Kg or 6 grams to 40 Kg). Because it measures hardness from depth versus load curves, the NANOVEA Micro Module can measure any type of materials including very elastic ones. It also can provide not only Vickers hardness but also accurate elastic modulus and creep data in addition to other types of test such as scratch adhesion testing, wear, fatigue testing, yield strength and fracture toughness for a complete range of quality control data.

NOW THE WORLD'S LEADING MICRO MECHANICAL TESTING

In this applications note, it will be explained how the Micro Module has been designed to offer the world’s leading instrumented indentation and scratch testing. The Micro Module’s wide range testing capability is ideal for many applications. For example, the load range allows for accurate hardness and elastic modulus measurements of thin hard coatings and can then apply much higher loads to measure the adhesion of these same coatings.

MEASUREMENT OBJECTIVE

The capacity of the Micro Module is showcased with the NANOVEA CB500 Mechanical Tester by
performing both indentation and scratch tests with superior precision and reliability using a wide load range from 0.03 to 200 N.

NANOVEA

CB500

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TEST CONDITIONS

A series (3×4, 12 indents in total) of Microindentations were performed on a standard steel sample using a Vickers indenter. The load and depth were measured and recorded for the complete indentation test cycle. The indentations were performed to different maximum loads ranging from 0.03 N to 200 N (0.0031 to 20.4 kgf) to showcase the capacity of the micro module in performing accurate indentation tests at different loads. It is worth noting that an optional load cell of 20 N is also available to provide 10 times higher resolution for tests in the lower load range from 0.3 gf up to 2 kgf.

Two scratch tests were performed using the Micro Module with linearly increased load from 0.01 N to 200 N and from 0.01 N to 0.5 N, respectively, using conico-spherical diamond stylus with tip radius of 500 μm and 20 μm.

Twenty Microindentation tests were carried out on the steel standard sample at 4 N showcasing the superior repeatability of the Micro Module’s results that contrast the performance of conventional Vickers hardness testers.

*microindenter on the steel sample

TEST PARAMETERS

of the Indentation Mapping

MAPPING: 3 BY 4 INDENTS

RESULTS AND DISCUSSION

The new Micro Module has a unique combination of Z-motor, high-force load cell and a high precision capacitive depth sensor. The unique utilization of independent depth and load sensors ensures high accuracy under all conditions.

Conventional Vickers hardness tests use diamond square-based pyramid indenter tips that create square shaped indents. By measuring the average length of the diagonal, d, the Vickers hardness can be calculated.

In comparison, the instrumented indentation technique used by NANOVEA‘s Micro Module directly measures the mechanical properties from indentation load & displacement measurements. No visual observation of the indent is required. This eliminates user or computer image processing errors in determining the d values of the indentation. The high accuracy capacitor depth sensor with a very low noise level of 0.3 nm can accurately measure the depth of indents that are difficult or impossible to be measured visually under a microscope with traditional Vickers hardness testers.

In addition, the cantilever technique used by competitors applies the normal load on a cantilever beam by a spring, and this load is in turn applied on the indenter. Such a design has a flaw in case a high load is applied – the cantilever beam cannot provide sufficient structural stiffness, leading to deformation of the cantilever beam and in turn misalignment of the indenter. In comparison, the Micro Module applies the normal load via the Z-motor acting on the load cell and then the indenter for direct load application. All the elements are vertically aligned for maximum stiffness, ensuring repeatable and accurate indentation and scratch measurements in the full load range.

Close-up view of the new Micro Module

INDENTATION FROM 0.03 TO 200 N

The image of the indentation map is displayed in FIGURE 1. The distance between the two adjacent indents above 10 N is 0.5 mm, while the one at lower loads is 0.25 mm. The high-precision position control of the sample stage allows users to select the target location for mechanical properties mapping. Thanks to the excellent stiffness of the micro module due to the vertical alignment of its components, the Vickers indenter keeps a perfect vertical orientation as it penetrates into the steel sample under a load of up to 200 N (400 N optional). This creates impressions of a symmetric square shape on the sample surface at different loads.

The individual indentations at different loads under the microscope are displayed alongside of the two scratches as shown in FIGURE 2, to showcase the capacity of the new micro module in performing both indentation and scratch tests in a wide load range with a high precision. As shown in the Normal Load vs. Scratch Length plots, the normal load increases linearly as the conico-spherical diamond stylus slides on the steel sample surface. It creates a smooth straight scratch track of progressively increased width and depth.

FIGURE 1: Indentation Map

Two scratch tests were performed using the Micro Module with linearly increased load from 0.01 N to 200 N and from 0.01 N to 0.5 N, respectively, using conico-spherical diamond stylus with tip radius of 500 μm and 20 μm.

Twenty Microindentation tests were carried out on the steel standard sample at 4 N showcasing the superior repeatability of the Micro Module’s results that contrast the performance of conventional Vickers hardness testers.

A: INDENTATION AND SCRATCH UNDER THE MICROSCOPE (360X)

B: INDENTATION AND SCRATCH UNDER THE MICROSCOPE (3000X)

FIGURE 2: Load vs Displacement plots at different maximum loads.

The load-displacement curves during the indentation at different maximum loads are shown in FIGURE 3. The hardness and elastic modulus are summarized and compared in FIGURE 4. The steel sample exhibits a constant elastic modulus throughout the test load ranging from 0.03 to 200 N (possible range 0.003 to 400 N), resulting in an average value of ~211 GPa. The hardness exhibits a relatively constant value of ~6.5 GPa measured under a maximum load above 100 N. As the load decreases to a range of 2 to 10 N, an average hardness of ~9 GPa is measured.

FIGURE 3: Load vs Displacement plots at different maximum loads.

FIGURE 4: Hardness and Young’s modulus of the steel sample measured by different maximum loads.

INDENTATION FROM 0.03 TO 200 N

Twenty Microindentation tests were performed at 4N maximum load. The load-displacement curves are displayed in FIGURE 5 and the resulting Vickers hardness and Young’s modulus are shown in FIGURE 6.

FIGURE 5: Load-displacement curves for microindentation tests at 4 N.

FIGURE 6: Vickers hardness and Young’s Modulus for 20 microindentations at 4 N.

The load-displacement curves demonstrate the superior repeatability of the new Micro Module. The steel standard possesses a Vickers hardness of 842±11 HV measured by the new Micro Module, compared to 817±18 HV as measured using the conventional Vickers hardness tester. The small standard deviation of the hardness measurement ensures reliable and reproducible characterization of mechanical properties in the R&D and quality control of materials in both the industrial sector and academia research.

In addition, a Young’s Modulus of 208±5 GPa is calculated from the load-displacement curve, which is not available for conventional Vickers hardness tester due to the missing depth measurement during the indentation. As load decrease and the size of the indent decreases, the NANOVEA Micro Module advantages in terms of repeatability compare to Vickers Hardness Testers increase until it is no longer possible to measure the indent through visual inspection.

The advantage of measuring depth to calculate hardness also becomes evident when dealing with rougher or when samples are more difficult to observe under standard microscopes provided on Vickers Hardness Testers.

CONCLUSION

In this study, we have shown how the new world leading NANOVEA Micro Module (200 N range) performs unmatched reproducible and precise indentation and scratch measurements under a wide load range from 0.03 to 200 N (3 gf to 20.4 kgf). An optional lower range Micro Module can provide testing from 0.003 to 20 N (0.3 gf to 2 kgf). The unique vertical alignment of the Z-motor, high-force load cell and depth sensor ensures maximum structural stiffness during measurements. The indentations measured at different loads all possess a symmetric square shape on the sample surface. A straight scratch track of progressively increased width and depth is created in the scratch test of a 200 N maximum load.

The new Micro Module can be configured on the PB1000 (150 x 200 mm) or the CB500 (100 x 50 mm) mechanical base with a z motorization (50 mm range). Combined with a powerful camera system (position accuracy of 0.2 microns) the systems provide the best automation and mapping capabilities on the market. NANOVEA also offers a unique patented function (EP No. 30761530) which allows verification and calibration of Vickers indenters by performing a single indent across the full range of loads. In contrast, standard Vickers Hardness Testers can only provide calibration at one load.

Additionally, the NANOVEA software enables a user to measure the Vickers hardness via the traditional method of measuring the indent diagonals if needed (for ASTM E92 & E384). As shown, in this document, depth versus load hardness testing (ASTM E2546 and ISO 14577) performed by a NANOVEA Micro Module is precise and reproducible compared to Traditional Hardness Testers. Especially for samples that cannot be observed/measured with a microscope.

In conclusion, the higher accuracy and repeatability of the Micro Module design with its broad range of loads and tests, high automation and mapping options renders the traditional Vickers hardness testers obsolete. But likewise with scratch and micro scratch testers still currently offered but designed with flaws in the 1980’s.

The continuous development and improvement of this technology makes NANOVEA a world leader in micro mechanical testing.

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Multiphase Metal Nanoindentation

Metallurgy Study of Multiphase Material using Nanoindentation

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METALLURGY STUDY
OF MULTIPHASE MATERIAL

USING NANOINDENTATION

Prepared by

DUANJIE LI, PhD & ALEXIS CELESTIN

INTRODUCTION

Metallurgy studies the physical and chemical behavior of metallic elements, as well as their intermetallic compounds and alloys. Metals that undergo working processes, such as casting, forging, rolling, extrusion and machining, experience changes in their phases, microstructure and texture. These changes result in varied physical properties including hardness, strength, toughness, ductility, and wear resistance of the material. Metallography is often applied to learn the formation mechanism of such specific phases, microstructure and texture.

IMPORTANCE OF LOCAL MECHANICAL PROPERTIES FOR MATERIALS DESIGN

Advanced materials often have multiple phases in a special microstructure and texture to achieve desired mechanical properties for target applications in industrial practice. Nanoindentation is widely applied to measure the mechanical behaviors of materials at small scales ^{i ii}. However, it is challenging and time-consuming to precisely select specific locations for indentation in a very small area. A reliable and user-friendly procedure of nanoindentation testing is in demand to determine the mechanical properties of different phases of a material with high precision and timely measurements.

MEASUREMENT OBJECTIVE

In this application, we measure mechanical properties of a multiphase metallurgical sample using the Most Powerful Mechanical Tester: the NANOVEA PB1000.

Here, we showcase the capacity of the PB1000 in performing nanoindentation measurements on multiple phases (grains) of a large sample surface with high precision and user friendliness using our Advanced Position Controller.

NANOVEA

PB1000

TEST CONDITIONS

In this study, we use a metallurgical sample with multiple phases. The sample had been polished to a mirror-like surface finish before the indentation tests. Four phases have been identified in the sample, namely PHASE 1, PHASE 2, PHASE 3 and PHASE 4 as shown below.

The Advanced Stage Controller is an intuitive sample navigation tool which automatically adjusts the speed of sample movement under the optical microscope based on position of the mouse. The further the mouse is away from the center of field of view, the faster the stage moves toward the mouse’s direction. This provides a user-friendly method to navigate the entire sample surface and select the intended location for mechanical testing. The coordinates of the test locations are saved and numbered, along with their individual test setups, such as loads, loading/unloading rate, number of tests in a map, etc. Such a test procedure allows users to examine a large sample surface for specific areas of interest for indentation and perform all the indentation tests at different locations in one time, making it an ideal tool for mechanical testing of metallurgical samples with multiple phases.

In this study, we located the specific phases of the sample under the optical microscope integrated in the NANOVEA Mechanical Tester as numbered on FIGURE 1. The coordinates of the selected locations are saved, followed by automatic nanoindentation tests all at once under the test conditions summarized below

FIGURE 1: SELECTING NANOINDENTATION LOCATION ON THE SAMPLE SURFACE.

RESULTS: NANOINDENTATIONS ON DIFFERENT PHASES

The indentations at the different phases of the sample are displayed below. We demonstrate that the excellent position control of the sample stage in the NANOVEA Mechanical Tester allows users to precisely pinpoint the target location for mechanical properties testing.

The representative load-displacement curves of the indentations are shown in FIGURE 2, and the corresponding hardness and Young’s Modulus calculated using Oliver and Pharr Methodⁱⁱⁱ are summarized and compared in FIGURE 3.

The PHASES 1, 2, 3 and 4 possess an average hardness of ~5.4, 19.6, 16.2 and 7.2 GPa, respectively. The relatively small size for PHASES 2 contributes to its higher standard deviation of the hardness and Young’s Modulus values.

FIGURE 2: LOAD-DISPLACEMENT CURVES
OF THE NANOINDENTATIONS

FIGURE 3: HARDNESS & YOUNG’S MODULUS OF DIFFERENT PHASES

CONCLUSION

In this study, we showcased the NANOVEA Mechanical Tester performing nanoindentation measurements on multiple phases of a large metallurgical sample using the Advanced Stage Controller. The precise position control allows users to easily navigate a large sample surface and directly select the areas of interest for nanoindentation measurements.

The location coordinates of all the indentations are saved and then performed consecutively. Such a test procedure makes measurement of the local mechanical properties at small scales, e.g. the multi-phase metal sample in this study, substantially less time-consuming and more user friendly. The hard PHASES 2, 3 and 4 improve the mechanical properties of the sample, possessing an average hardness of ~19.6, 16.2 and 7.2 GPa, respectively, compared to ~5.4 GPa for PHASE 1.

The Nano, Micro or Macro modules of the instrument 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.

i Oliver, W. C.; Pharr, G. M., Journal of Materials Research., Volume 19, Issue 1, Jan 2004, pp.3-20
ii Schuh, C.A., Materials Today, Volume 9, Issue 5, May 2006, pp. 32–40
iii Oliver, W. C.; Pharr, G. M., Journal of Materials Research, Volume 7, Issue 6, June 1992, pp.1564-1583

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Ceramics: Nanoindentation Fast Mapping for Grain Detection

INTRODUCTION

Nanoindentation has become a widely applied technique for measuring mechanical behaviors of materials at small scales^{i ii}. The high-resolution load-displacement curves from a nanoindentation measurement can provide a variety of physicomechanical properties, including hardness, Young’s modulus, creeping, fracture toughness and many others.

Importance of Fast Mapping Indentation

One significant bottleneck for further popularization of the nanoindentation technique is time consumption. A mechanical property mapping by conventional nanoindentation procedure can easily take hours which hinders the application of the technique in mass production industries, such as semiconductor, aerospace, MEMS, consumer products such as ceramic tiles and many others.

Fast mapping can prove to be essential in the ceramic tile manufacturing industry, Hardness and Young’s modulus mappings across a single ceramic tile can present a distribution of data that indicates how homogeneous the surface is. Softer regions on a tile can be outlined in this mapping and show locations more prone to failure from physical impacts that happen on a day to day basis in someone’s residence. Mappings can be made on different types of tiles for comparative studies and on a batch of similar tiles to measure tile consistency in a quality control processes. The combination of measurements setups can be extensive as well as accurate and efficient with the fast mapping method.

MEASUREMENT OBJECTIVE

In this study, the Nanovea Mechanical Tester, in FastMap mode is used to map the mechanical property of a floor tile at high speeds. We showcase the capacity of the Nanovea Mechanical Tester in performing two fast nanoindentation mappings with high precision and reproducibility.

Test Conditions

The Nanovea Mechanical Tester was used to perform a series of nanoindentations with the FastMap Mode on a floor tile using a Berkovich indenter. The test parameters are summarized below for the two indent matrices created.

Table 1:  Test parameter summary.

RESULTS & DISCUSSION 

Figure 1:  2D and 3D view of 625-indent hardness mapping.

Figure 2:  Micrograph of 625-indent matrix showcasing grain.

A 625-indent matrix was conducted on a 0.20mm² area with a large visible grain present. This grain (Figure 2) had an average hardness lower than the overall surface of the tile. The Nanovea Mechanical Software allows the user to see the hardness distribution map in 2D and 3D mode which are depicted in Figure 1. Using the high-precision position control of the sample stage, the software allows users to target areas such as these for in depth mechanical properties mapping.

Figure 3:  2D and 3D view of 1600-indent hardness mapping.

Figure 4:  Micrograph of 1600-indent matrix.

A 1600-indent matrix was also created on the same tile to measure the homogeneity of the surface. Here again the user has the ability to see the hardness distribution in 3D or 2D mode (Figure 3) as well as the microscope image of the indented surface. Based on the hardness distribution presented, it can be concluded that the material is porous due to the even scattering of high and low hardness data points.

Compared to conventional nanoindentation procedures, FastMap mode in this study is substantially less time-consuming and more cost-effective. It enables speedy quantitative mapping of mechanical properties including Hardness and Young’s Modulus and provides a solution for grain detection and material consistency which is critical for quality control of a variety of materials in mass production.

CONCLUSION

In this study, we showcased the capacity of the Nanovea Mechanical Tester in performing speedy and precise nanoindentation mapping using FastMap mode. The mechanical property maps on the ceramic tile utilize the position control (with 0.2µm accuracy) of the stages and force module sensitivity to detect surface grains and measure homogeneity of a surface at high speed.

The test parameters used in this study were determined based on the size of the matrix and sample material. A variety of test parameters can be chosen to optimize the total indentation cycle time to 3 seconds per indent (or 30 seconds for every 10 indentations).

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 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, 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.

Author: Duanjie Li, PhD        Revised by Pierre Leroux & Jocelyn Esparza

Biological Tissue Hardness Evaluation using Nanoindentation

Importance of Biological Tissue Nanoindentation

Traditional mechanical tests (hardness, adhesion, compression, puncture, yield strength, etc.) require greater precision and reliability in today’s quality control environments with a wide range of advanced materials from tissues to brittle materials. Traditional mechanical instrumentation fails to provide the sensitive load control and resolution required for advanced materials. The challenges associated with biomaterials require developing mechanical tests capable of accurate load control on extremely soft materials. These materials require very low sub mN testing loads with large depth range to ensure proper property measurement. In addition, many different mechanical test types can be performed on a single system allowing for greater functionality. This provides a range of important measurements on biomaterials including hardness, elastic modulus, loss and storage modulus, and creep in addition to scratch resistance and yield strength failure points.

 

Measurement Objective

In this application Nanovea’s mechanical tester in nanoindentation mode is used to study the hardness and elastic modulus of 3 separate areas of a biomaterial substitute on fat, light meat, and dark meat regions of prosciutto.

Nanoindentation is based on instrumented indentation standards ASTM E2546 and ISO 14577. It uses established methods where an indenter tip of known geometry is driven into a specific site of the test material with a controlled increasing normal load. When reaching a pre-set maximum depth, normal load is reduced until complete relaxation occurs. Load is applied by a piezo actuator and measured in a controlled loop with a high sensitivity load cell. During experiments the indenter position relative to the sample surface is monitored with a high precision capacitive sensor. The resulting load and displacement curves provide data specific to the mechanical nature of the tested material. Established models calculate quantitative hardness and modulus values with the measured data. Nanoindentation is suited to low load and penetration depth measurements at nanometer scales.

Results and Discussion

These tables below present measured values of hardness and Young’s modulus with averages and standard deviations. High surface roughness may cause large variations in the results due to small indentation size.

The fat area had about half the hardness of the meat areas. Meat treatment caused the darker meat area to be harder than the light meat area. Elastic modulus and hardness are in direct relation to mouth feel chewiness of the fat and meat areas. The fat and light meat area have creep continuing at a higher rate than the dark meat after 60 seconds.

Detailed Results – Fat

Detailed Results – Light Meat

Detailed Results – Dark Meat

Conclusion

In this application, Nanovea’s mechanical tester in nanoindentation mode reliably determined mechanical properties of the fat and meat areas while overcoming high sample surface roughness. This demonstrated the wide and unmatched capability of Nanovea’s mechanical tester. The system simultaneously provides precise mechanical property measurements on extremely hard materials and soft biological tissues.

The load cell in closed loop control with the piezo table ensures precise measurement of hard or soft gel materials from 1 to 5kPa. Using the same system, it is possible to test biomaterials at higher loads up to 400N. Multi-cycle loading can be used for fatigue testing and yield strength information in each zone can be obtained using a flat cylindrical diamond tip. In addition, with Dynamic Mechanical Analysis (DMA), the viscoelastic properties loss and storage moduli can be evaluated with high accuracy using the closed loop load control. Tests at various temperatures and under liquids are also available on the same system.

Nanovea’s mechanical tester continues to be the superior tool for biological and soft polymer/gel applications.

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Tooth Hardness Evaluation using Nanoindentation

Importance of Nanoindentation for Bio Materials

 
With many traditional mechanical tests (Hardness, Adhesion, Compression, Puncture, Yield Strength, etc.), today’s quality control environments with advanced sensitive materials, from gels to brittle materials, now require greater precision and reliability control. Traditional mechanical instrumentation fails to provide the sensitive load control and resolution required; designed to be used for bulk materials. As the size of material being tested became of greater interest, the development of Nanoindentation provided a reliable method to obtain essential mechanical information on smaller surfaces such as the research being done with biomaterials. The challenges specifically associated with biomaterials have required the development of mechanical testing capable of accurate load control on extremely soft to brittle materials. Also, multiple instruments are needed to perform various mechanical tests which can now be performed on a single system. Nanoindentation provides a wide range of measurement with precise resolution at nano controlled loads for sensitive applications.

 

 

Measurement Objective

In this application, the Nanovea Mechanical Tester, in Nanoindentation mode, is used to study the hardness and elastic modulus of the dentin, decay, and pulp of a tooth. The most critical aspect with Nanoindentation testing is securing the sample, here we took a sliced tooth and epoxy mounted leaving all three areas of interest exposed for testing.

 

 

Results and Discussion

This section includes a summary table that compares the main numerical results for the different samples, followed by the full result listings, including each indentation performed, accompanied by micrographs of the indentation, when available. These full results present the measured values of Hardness and Young’s modulus as the penetration depth with their averages and standard deviations. It should be considered that large variation in the results can occur in the case that the surface roughness is in the same size range as the indentation.

Summary table of main numerical results:

 

 

Conclusion

In conclusion, we have shown how the Nanovea Mechanical Tester, in Nanoindentation mode, provides precise measurement of the mechanical properties of a tooth. The data can be used in the development of fillings that will better match the mechanical characteristics of a real tooth. The positioning capability of the Nanovea Mechanical Tester allows full mapping of the hardness of the teeth across the various zones.

Using the same system, it is possible to test teeth material fracture toughness at higher loads up to 200N. A multi-cycle loading test can be used on more porous materials to evaluate the remaining level of elasticity. Using a flat cylindrical diamond tip can give yield strength information in each zone. In addition, with DMA “Dynamic Mechanical Analysis”, the viscoelastic properties including loss and storage moduli can be evaluated.

The Nanovea nano module is ideal for these tests because it uses a unique feedback response to control precisely the load applied. Because of this, the nano module can also be used to do accurate nano scratch testing. The study of scratch and wear resistance of tooth material and filling materials adds to the overall usefulness of the Mechanical tester. Using a sharp 2-micron tip to quantitatively compare marring on filling materials will allow better prediction of the behavior in real applications. Multi-pass wear or direct rotative wear testing are also common tests providing important information on the long term viability.

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