Microindentation hardness tests

B. W. Mott, Microindentation Hardness Testing, Btterworths, London (1957). 

P. J. Blau. Microindentation Hardness Testing of Coatings Techniques and Interpretation of Data. In American Vacuum Society Series 2 Physics and Chemistry of Protective Coatings. (G. Lucovsky, Series Ed. W. D. Sproul,... 

The modern microindentation hardness-testing equipment has been automated by coupling the indenter apparatus to an image analyzer that incorporates a computer and software package. The software controls important system functions, including indent location, indent spacing, computation of hardness values, and plotting of data. 

The two microindentation hardness testing techniques are the Knoop and Vickers tests. Small indenters and relatively light loads are employed for these two techniques. They are used to measure the hardnesses of brittle materials (such as ceramics) and also of very small specimen regions. 

P.J. Blau, A Comparison of Foixr Microindentation Hardness Test Methods Using Copper, 52100 Steel and an Amorphous Pd-Cu-Si Alloy, Metallography 16 (1983) 1. 

Microindentation hardness normally is measured by static penetration of the specimen with a standard indenter at a known force. After loading with a sharp indenter a residual surface impression is left on the flat test specimen. An adequate measure of the material hardness may be computed by dividing the peak contact load, P, by the projected area of impression1. The hardness, so defined, may be considered as an indicator of the irreversible deformation processes which characterize the material. The strain boundaries for plastic deformation, below the indenter are sensibly dependent, as we shall show below, on microstructural factors (crystal size and perfection, degree of crystallinity, etc). Indentation during a hardness test deforms only a small volumen element of the specimen (V 1011 nm3) (non destructive test). The rest acts as a constraint. Thus the contact stress between the indenter and the specimen is much greater than the compressive yield stress of the specimen (a factor of 3 higher). 

Analysis of Table II shows discrepancies in the hardness and stress behavior of a-C(N) H films. Although all the works reported a clear stress reduction upon nitrogen incorporation, the hardness sometimes is quoted as almost constant, or on the other hand clearly decreasing. In addition to the possible effect of different deposition methods and conditions, it can be easily seen that the differences in hardness testing methods are the major source for discrepancies. Constant hardness behavior is only reported with the use microindentation methods, like Vickers and Knoop microhardness. On the other hand, the use of low-load nanoindentation methods always led to a nitrogen-induced decrease in hardness. This is basically the consequence of two factors. The first one is the higher penetration... 

ASTM E384-07. (2007) Standard Test Method for Microindentation Hardness of Materials, American Society for Testing Materials. 

A 7X/2(NA) correction is incorporated in the ASTM Knoop standard C 730 for glass, but is not used in the master microindentation hardness of materials standard E 384, nor in the advanced ceramic standards C 1326 and ISO 14705, nor in the glass standards DIN 52333 or ISO 9385. This variability between the standards has created considerable confusion in hardness testing and probably accounts for a lot of inconsistent results in the literature. 

When the material to be tested is very thin, the indentation should be shallow and the applied load small. This is called microindentation hardness or nanoindentation and the indentation load can be as low as 0.05 milligrams. One commercial instrument is capable of performing indentation tests with a load of 2.5 millinewtons and depth resolutions of 0.4 nanometers. It detects penetration movement by changes in capacitance between stationary and moving plates. 

Fig. 1 Single cell elasticity measurements with microindentation technique. (A) AFM allows both live cell imaging and mechanical testing (e.g., microindentation) in near physiological conditions. The AFM tip attached to a cantilever descents slowly to a surface and causes an indentation. The depth of indentation is detected by laser light diffraction pattern. (B) Typical force-distance curves are obtained for hard and soft surfaces and usually analyzed with the classical Hertz model that relates the applied force to the indentation depth.

Westrich, R.M., 1986. Use of the scanning electron microscope in microhardness testing of high-hardness materials, microindentation techniques. Materials Science and Engineering ASTM STP 889, Philadelphia, p. 196. 

The indentation test is one of the simplest ways to measure mechanical properties of a material. The micromechanical behavior of polymers and the correlation with microstrnctnre and morphology have been widely investigated over the past two decades (23). Conventional microindentation instruments are based on the optical measnrement of the residual impression produced by a sharp indenter penetrating the specimen surface under a given load at a known rate. Microhardness is obtained by dividing the peak load by the contact area of impression. From a macroscopic point of view, hardness is directly correlated to the yield stress of the material, ie, the minimnm stress at which permanent strain is produced when the stress is snbseqnently removed. 

Nanoindentation is nowadays one of the most used methods to measure the mechanical properties of polymers, attracting great attention as a technique to mechanically characterize polymer nanocomposites [137-142]. This technique uses the same principle as microindentation, but with much smaller probe areas and very low loads (on the order of nanonewtons), so as to produce indentations from less than a hundred nanometers to a few micrometers in size and depth [143]. Although it has been vastly used to characterize the mechanical properties, particularly hardness, elastic modulus, yield stress, and fracture toughness, of several polymers [144—152] and shown to be mainly influenced by the testing procedure, penetration depths, and holding time, limited work has been dedicated to the characterization of the mechanical behavior of polymer nanocomposites using this technique. 

FIGURE 33.11 Comparison of hardness measurements and the oxidation index (01) for retrieved UHMWPE tibial bearing samples. Hardness was profiled with microindentation (after [19]) while the 01 was obtained by FTIR spectroscopy at the sites of the indentation testing so that direct correlations could be made. 

The microindentation tests are performed to measure the hardness and the elastic modulus of small specimens with low applied loads. One of the most difficult problems in the microindentation test is to determine the contact radius (Fischer-Cripps 2000). In this case, the contact radius is estimated by the following equation. 

The microhardness technique is used when the specimen size is small or when a spatial map of the mechanical properties of the material within the micron range is required. Forces of 0.05-2 N are usually applied, yielding indentation depths in the micron range. While microhardness determined from the residual indentation is associated with the permanent plastic deformation induced in the material (see section on Basic Aspects of Indentation), microindentation testing can also provide information about the elastic properties. Indeed, the hardness to Young s modulus ratio HIE has been shown to be directly proportional to the relative depth recovery of the impression in ceramics and metals (2). Moreover, a correlation between the impression dimensions of a rhombus-based pyramidal indentation and the HIE ratio has been found for a wide variety of isotropic poljuneric materials (3). In oriented polymers, the extent of elastic recovery of the imprint along the fiber axis has been correlated to Young s modulus values (4). 

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