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Joachim Frühauf, Eva Gärtner, Konrad Herrmann, Febo Menelao, Dieter Schwenk, Thomas Chudoba, Hans-Peter Vollmar
CALIBRATION OF INSTRUMENTS FOR HARDNESS TESTING BY USE OF A STANDARD

As a standard for the calibration of force and depth scales of hardness testing instruments a system of silicon springs is described. The standard shows a linear force-deflection characteristic F = k · f up to a stop point (typical: Fst = 420 mN; fst = 22 µm). For the calibration of stiffness and stop point of the standard the characteristic should be measured using a spherical indenter. In view of the practical application for the assessment of instruments also Vickers indenters can be used. In this case indentations are produced. The resulting wear can be minimized by reducing the maximum force and using only the measured stiffness k for a quick assessment.

Satoshi Takagi, Christian Ullner
CRITICAL CHECK OF THE REPEATABLITY AND BIAS OF HARDNESS TESTING MACHINES RESTRICTED BY THE HARDNESS STANDARDS

Since the ISO standards for four major hardness scales were revised in 2005, the indirect verification has been considered as the mainstream of the traceability chain of hardness. In the recommended procedure of ISO, the uncertainty of hardness machine should be estimated and added to the combined uncertainty of hardness measurement value. The equation to calculate this uncertainty component was introduced according to the rectangular distribution of bias of hardness machines. However, if the error propagation is investigated in detail, the uncertainty of hardness machines should be obtained by considering the probability distributions of the uniformity of hardness reference block, the repeatability and the bias of hardness machine. In addition, the distribution of verification results should be calculated after some hardness machines are screened out by the maximum permissible values requested in ISO. In this paper, the probability distribution of the hardness machines, which passed in the indirect verification, are obtained by means of the Monte Carlo method. Since a calibration value of hardness is obtained only by measuring a specimen, it is not possible to separate the uncertainties of hardness machine and hardness block. Then the result of indirect verification is affected by the uniformity of reference block. The relation between the distribution of passed hardness machines and the uniformity of reference blocks is presented for several hardness scales. In addition, the guideline to estimate the uncertainty of the measured hardness values can be verified by means of the Monte Carlo method.

Masayuki Fujitsuka, Makoto Yamaguchi, Shigeru Ueno, Genichiro Kamiyama, Shigeo Katayama
MEASUREMENT OF A RESIDUAL IMPRESSION BY THE LASER SCANNING MICROSCOPE WITH DIC UNIT

When the nanoindentation testing is carried out, it is very important to understand the residual impression and the surface around it. Generally Atomic Force Microscopy (AFM) is used to obtain them. However, it is necessary to understand correct shape in the point of cantilever in AFM procedure. And, measuring them by AFM procedure precisely, very long measurement time and very clean environment and so on are needed. So, there are many difficulties to use AFM procedure for measuring residual impression and the surface around it. On the other hand, there are some procedures to measure them. Scanning Electro Microscopy (SEM) is effective to the grasp of the shape of the surface and the ruggedness. But, this procedure needs the coating of the sample and the vacuum atmosphere. Therefore it is not a simple and quick procedure. In this paper, authors used the laser scanning microscope with a differential interference contrast unit to obtain the data of a residual impression and the surface around it. This procedure is the very simple and quick procedure in no contact and measuring in various environmental conditions. The data of indentation depth from this procedure is obtained at the nano-meter order. The results from this procedure compare with the results from displacement of nanoindentation test.

Yutaka Seino
ANALYSIS OF INDENTATION DEPTH DEPENDENCE OF ELASTIC PROPERTIES OF INTER-LAYER DIELECTRIC FILMS ON SILICON

Analysis of indentation depth dependence of elastic modulus of soft films on silicon substrate measured by nanoindentation was studied. The experimental results were compared with two existing models that describe the effects of the substrate on elastic modulus of layered solid. Saha-Nix model that is the recent modification of King model agreed well with the experimental results to a certain limit of the indentation depth. It was found that the depth limit which Saha-Nix model is valid depended almost linearly on the relative elastic modulus of the film to the substrate Ef/Es. We further introduced an additional scaling parameter that is a linear function of Ef/Es in Saha-Nix model. The improved model was applied to porous silica low-k films. The model predicted a constant intrinsic elastic modulus of the film up to a depth of 30 % of the film thickness.

Shigeo Sato, Masayuki Sato
HARDNESS MEASUREMENT OF COATING THIN FILM BY INDENTATION PROFILE OBSERVATION USING SCANNING PROBE MICROSCOPY

According to the principle of a conventional Vickers (Berkovich) hardness measurement, hardness is calculated from diagonal lengths or side lengths of indentation. The diagonal length, the conjunction line length of pyramidal indentation, and the distance from the vertex to the base of trigonal pyramidal indentation are measured accurately by observing a vertical cross section. Scanning probe microscopy (SPM) is a good method for observing the vertical and horizontal cross sections of the indentation. However, such parameters in the cross section profile must be defined as the principle of the method to obtain a reliable nano-hardness value.

Vytautas Vasauskas, Juozas Padgurskas, Raimundas Rukuiza
THE MICRO-HARDNESS ANISOTROPY OF FLUOR-OLIGOMERIC AND Fe-Co-W COATINGS

The influences of indenter micro-geometry on the micro-hardness performance in the film/substrate system are discussed. Experimental results verify the force required to produce hardness indents for thin films, the measurement of the size of plastic zone cross-sections of the indents, and the characterisation of the indenters. It was found that the deformation is highly localised beneath the indenter and failures in the corners of pyramidal indenters occurred.

Li Heping and Zhou Xing
THE APPLICATION AND EFFECTS OF THIN SHEET HARDNESS REFERENCE MATERIALS WITHOUT AGING EFFECT

Hardness test methods are widely used in mechanical properties test area. While reference materials are essential important tools to control test accuracy or uncertainty. According to current test method standards, the thickness of hardness reference materials must be not less than 6 mm for Rockwell hardness or not less than 5 mm for Vickers hardness. To measure thinner sample which is commonly used in industry, and to guarantee the test results, a thin sheet reference sample is demanded.

A. Štibler, K. Herrmann
INDIRECT VERIFICATION OF ELASTOMER HARDNESS TESTERS USING HARDNESS REFERENCE BLOCKS

Hardness measurement methods for rubber and plastics are described in the standards ISO 7619-1, ISO 7619- 2, ISO 868 and ISO 48. Rising requirements for the accuracy of this hardness measurement have led to the result that the users of rubber hardness testers and also metrology experts who deal with their calibration need a calibration method to check the overall function of the testers acknowledged by a standard. Therefore extensive experiments were conducted in a cooperation between the Physikalisch - Technische Bundesanstalt (PTB) in Braunschweig (Germany) and the ZAG Ljubljana (Slovenia). The results have been used as a basis for the elaboration of the relevant international standard ISO 18898 which was published in 2006. In this standard direct verification methods are laid down. An indirect verification method using rubber hardness reference blocks, which is also applicable for the verification of hardness testers, is presented in this paper. At present hardness reference blocks are available only for some of the hardness scales which are used for rubber materials. Suchwise, Shore A, IRHD N and IRHD M reference blocks are available in the market. During the verification process the hardness tester is calibrated by using rubber hardness reference blocks. The evaluation of the repeatability and the error of the hardness testers including the uncertainty of measurement of the calibration results is given in this paper.

D. Schwenk, K. Herrmann, G. Aggag, F. Menelao
INVESTIGATION OF A GROUP STANDARD OF ROCKWELL DIAMOND INDENTERS

The specific hardness deviations of a Rockwell diamond indenter can be determined by a group standard, consisting of several indenters, using correction functions. In this paper the establishment of an HRC group standard in the PTB and comparative investigations of the group standards in the PTB and the calibration laboratory MPA NRW in Germany are reported. Above all the group standard is advantageous for maintaining the stability of the Rockwell hardness scales.

O Kruger, L Mostert
THE USE OF A µCMM IN THE CALIBRATION OF HARDNESS INDENTERS

In order to perform traceable hardness measurements using Rockwell Hardness Indenters, the indenter must conform to the requirement of ISO 6508-3 standard. The standard defines specifications for the geometric parameters for this type of indenter. Conformance to this standard is of particular importance to all calibration laboratories which operate in accordance with ISO/IEC 17025. At present there is no facility in South Africa with the capability of calibrating indenters for conformance to ISO 6508-3. This situation is being addressed through a series of studies currently being conducted at the National Metrology Institute of South Africa. The following parameters are calibrated using the µCMM. ISO 6508-3 specifies a radius of 200 µm with an uncertainty of ± 5 µm for Rockwell Hardness Indenter tips. Also specified in the ISO standard is the cone perpendicularity between the axis of the diamond cone to the axis of the indenter holder, with a specification of ± 0,03°. The last part of the ISO standard which was investigated states: “The surface of the cone and the spherical tip shall blend in a truly tangential manner.” All these parameters were measured and associated uncertainties calculated to prove conformance with ISO 6508-3 for the calibration of hardness indenters.

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