New method for nanohardness measurement of single crystal aluminum(Al)

Shahjada Ahmed Pahlovy,Sadao momota

Intelligent mechanical system engineering department Kochi University of Technology Kochi, Japan 096402c@gs.kochi-tech.ac.jp
Abstract Nanohardness is an important mechanical properties of materials most used to characterize the wear resistance of materials. In this present paper a procedure is developed for calculation of nanohardness by nanoindentation and an atomic force microscope (A.F.M).A three sided pyramidal diamond tip has been used for the indentation experiment. Experiment has been concluded on single crystal aluminum (Al). The load displacement data have been used to obtain the nanoindentation hardness and the room temperature nanohardness properties of single crystal Al have been investigated at different indentation loads. Comparison of the data obtained using nano indenter with that obtained by using new technique was briefly discussed. It has been shown that the measured nanohardness values of the material sensitively depend on the applied load of indentation. It is also shown that the measured nanohardness is smaller than indentation hardness.

Yao Ying Xue

Mechanical electronics engineering department. Harbin Institute of Technology. Harbin, China yyx@hope.hit.edu.cn F and the contact depth h or the projected contact area A; where the hardness H under load F, H = F/A, can be evaluated II. EXPERIMENTAL PROCEDURE

Index TermsAtomic force microscopy, Nanohardness, Nano

indentation, Single crystal

I.

INTRODUCTION

The indentation experiments were completed on the NANO indenter II was manufactured by MTS nanoinstruments and is shown in Fig. 1. A schematic of the indenter is shown in Fig. 2. The indenter operates in load-control with the load applied by the electro-magnetic coil shown in Fig. 2 with a resolution of 75nN. Displacements are measured to 0.04 nm with noncontact capacitance transducers that are placed near the center of the loading column. When enabled, continuous stiffness measurements are made using a lock-in amplifier that records the ratio of the displacement and force voltage signals and their phase difference. In this experimental procedure, the Berkovich, a three-sided pyramidal diamond tip is utilized to push on the metal. The materials chosen for the present study was single crystal aluminum. Specimen was obtained commercially in the form of round shape with flat, parallel machined surfaces. A careful polishing was done on one surface of the specimens to produce an optical finish. The polished specimens were then subjected to Vickers diamond pyramid indentation. Care is taken to make indentations only on those areas which have no visible pores.

or nearly 100 years, indentation experiments have been performed to obtain the hardness of materials. In recent years significant improvements have been seen in indentation equipment and a growing need to measure the mechanical properties of materials on small scales. It is now possible to monitor, with high precision and accuracy, both the load and displacement of an indenter during indentation experiments [2]-[4]. However, questions remain, including what properties can be measured using instrumented indentation techniques and what is hardness in nano scale? Many authors have addressed these basic questions [5]-[8]. This paper describes a new technique for measuring nano hardness by using nano indenter and AFM, and summarizes the recent results that may be useful to consider the comparison of indentation hardness to measured hardness. A three-dimensional, rigid, pyramidal indenter was considered, indenting normally into a homogeneous solid. The friction coefficient at the contact surface between the indenter and the solid is assumed zero. The quantities of interest from the loading portion of indentation measurements include the force

Fig. 1. MTS Nanoinstruments

III. Area Area A1 = was

RESULT AND DISCUSSIONS calculated by using the formula:

the sides of triangle and S = ( A + B + C ) 2 . Finally nano hardness was calculated by using formula Hardness H = Fmax/A1.

S (S A)(S B )(S C ) , where A, B, C are

Fig. 2. A schematic diagram of indenter

The calculated area and nanohardness has shown in table I. About 25 indentations were completed on the same specimen . It is observed that the hardness increases due to decreases of load and also Hardness decreases due to in creases of load. In fig. 5 shown the comparison between calculated load vs calculated area and Indentation load vs indentation area. Series 1 and 2 indicates the calculated and indentation area-load respectively. It is observed that the calculated area is higher than the indentation area.
TABLEL . I CALCULATED AREA AND HARDNESS Depth limit Calculated Area in m2 77.05 77.52 76.71 77.98 73.36 90.23 90.07 91.01 88.56 91.96 42.08 41.35 41.69 42.17 41.59 40.01 38.95 41.22 41.52 38.90 12.75 15.47 15.25 15.10 16.60 Maximum Load In mN 26.35 26.32 26.70 26.92 27.43 33.18 33.04 33.44 33.35 33.43 18.49 18.12 18.15 17.42 18.01 12.85 13.32 13.73 13.20 12.76 9.70 9.04 8.82 8.70 7.72 Calculated Hardness IN GPa 0.34 0.34 0.35 0.35 0.37 0.37 0.37 0.37 0.38 0.36 0.43 0.44 0.44 0.41 0.43 0.32 0.34 0.33 0.31 0.33 0.76 0.58 0.58 0.57 0.46 Indentation Hardness In GPa 0.44 0.43 0.44 0.45 0.46 0.89 0.61 0.73 0.59 0.57 0.66 0.54 0.58 0.62 0.64 0.47 0.49 0.51 0.49 0.47 0.45 0.66 0.57 0.55 0.76

About 25 tests were performed with different loads for this experiment. All tests are carried out under ambient laboratory conditions. After load the specimen surface was observed with the resolution of the order of nm. Fig. 3. Shows the typical AFM images for the aluminum specimen given after indentation testing. Triangle indents are clearly seen. Fig. 4 shows AFM analysis that is the depth and the three sides of triangle are measured for area calculation.

For 1.5 m

For 1.7 m Fig. 3. AFM image . For 1.2 m

For 1.0m For 0.8 m

Fig. 4. AFM analysis.

In fig. 6 shown the comparison between calculated hardness vs. calculated load and indentation hardness vs. indentation load. Series 1 and 2 indicated the calculated and indentation hardness load respectively. It is observed that the calculated hardness value is lower than the indentation hardness. This happened, as the calculated area is higher than indentation area. The computed values of hardness differ from Indentation hardness due to various systematic errors that have been identified for this type of testing. The three most significant factors to be considered are: 1. The initial penetration depth; 2. The compliance of the loading system; and 3. The non-ideal shape of the indenter.

In addition to the above, there are a number of materialsrelated issues which are the subject of investigation but for which there appears to be no one universally accepted method of solution. The scale of overall deformation in the vicinity of the indenter in sub-micron testing can often be of the same order as that of the dislocations or other microstructural features within the specimen

IV.

CONCLUSIONS

100 Area in m2 80 60 40 20 0 8.79 13.2 18 26.7 33.3 Load in mN

Fig. 5 . Comparison load vs. area.( Calculated and indentation)

A method for determining the nanohardness has been developed. The comparison of calculated and Indentation were shown and briefly discussed. The measured hardness increases with decreasing indentation load in the low load range. From graph comparison, it shows that the curve nature of hardness and area between indentation and proposed new technique are almost same shape. By the same shape it indicates the proposed technique is acceptable. Hardness is shown along with a description of their limitations and required corrections. However, materials behavior may be much more complex. For hard materials, for example, the deformation mechanism responsible for the hardness impression may include a significant fracture component instead of the purely elasticplastic behavior. Likewise, alternative mechanisms may be responsible for the observed indentation size effects, including strain, gradient plasticity, imperfection in the indenter geometry, and surface roughness. Nevertheless, the conclusions of this study provide a framework for understanding indentation hardness measurements for single crystal of materials. These results of this work may also be used to identify new mechanisms responsible for deformation in indentation experiments. ACKNOWLEDGEMENTS

Series1 Series2

0.8 0.7 Hardness in GPa 0.6 0.5 0.4 0.3 0.2 0.1 0 8.79 13.17 18.03 26.74 33.29
Load in mN

The authors wish to acknowledge Mr.Cao and Mr.Tang for their considerable support, cooperation and help during the experiment time. REFERENCES
Series1 Series2
[1] [2] [3] Yang-Tse Chenga,U, Che-Min Chengb, what is nanohardness, Surface and Coatings Technology, 133-134 , pp. 417-424, 2000. J.B. Pethica, R. Hutchings, W.C. Oliver, Nanoindentation technique Phil. Mag. A48, pp. 593-597, 1983. Jianghong Gong a, Jianjun Wu b, Zhenduo Guan, Analysis of the indentation size effect on the apparent hardness, for ceramics, Materials Letters, 38 , pp. 197201, 1999. Bhushan, A. Kulkarni, W. Bonin, J. Wyrobek, Nanohardness calculation for single crystal aluminum, Phil. Mag. A 74, pp. 111117,1996. A.C. Fischer-Cripps,A review of analysis methods for sub-micron indentation testing Vacuum, 58 , 569-585. J.L. Loubet, J.M. Georges , G. Meille , in: P.J. Blau, B.R. Lawn, Eds Microindentation Techniques in Materials Science and Engineering, American Society for Testing and Materials Philadelphia, ASTM STP 889, 72-76, 1986.

[4]

[5] Fig. 6 . Comparison load vs. hardness.( Calculated and indentation) [6]

[7]

[8]

Jianghong Gong, Zhenduo Guan,Load dependence of low-load Knoop hardness in ceramics:a modified PSR Model Materials Letters, 47 , 140144, 2001. T.Ohmura, K. Tsuzaki, S.Matsuoka, Nanohardness measurement of high-purity Fe-C martensite, Scripta Materialia, 45, 889-894, 2001.