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Final Report
The University of Tennessee

Professor John D. Landes
Dr. Kang Lee

November 1998

Final Report on Computer Controlled Microindenter System
This is the final report for the University of Tennessee subcontract on "Study of the
Application of Microprobe Methodology to Material Response". It covers the period December
1,1996 to December 31, 1997. The work on this subcontract was conducted by John D. Landes,
Professor of Mechanical and Aerospace Engineering and Engineering Science (MAES) and
Kang Lee, Postdoctoral Associate in MAES.

During this period work was conducted on four topics:
1. Literature survey
2. Fatigue testing
3. Simulation analysis of indenter response
4. Numerical simulation of fatigue testing

The following contains a summary of the results in each area.

1. Literature survey

A computerized literature search was conducted at the main library of the University of
Tennessee, Knoxville (UTK). The object was to gather information on the state-of the-art models
and correlations between fatigue damage and associated changes in the stress-strain behavior of
materials, to study the results of indentation measurements on various material systems and to
study the effects of residual stresses on the uniaxial and multiaxial deformation of aluminum and


steel alloys. Two data bases were used in the searches, a compendex from UTK web-based
databases using ERL/Web SPIRS and an Internet Database Service (IDS) from Cambridge
Scientific Abstracts Web Service. The main part of this study was conducted in the first half year
of the program and the results were reported in the previous semi-annual report. The conclusion
from the literature survey was that no one had previously established a good quantitative
correlation between the stress-strain response and the amount of fatigue damage although it is
clear that a qualitative correlation exists between the two.

2. Fatigue testing and results

The fatigue testing which was in its initial stages last reporting period has been completed
during the past six months of the program. Two materials were tested, a 2024-T4 aluminum alloy
and a 7075-T6 aluminum alloy. The first alloy, 2024-T4, is one that exhibits extensive cyclic
hardening during the fatigue test; that is, the stress-strain curve increases during cyclic loading
relative to the monotonic stress-strain curve. The second alloy, 7075-T6, shows almost no
change in stress-strain properties during the cyclic test. A flat tensile geometry was used for the
fatigue testing rather the typical round low cycle fatigue geometry so that the specimens can be
directly indented without having to deal with the curvature problem that would be introduced by
a round specimen. This specimen is recommended as an alternative to the round fatigue
specimen in the ASTM Method E 606, "Standard Recommended Practice for Constant
Amplitude Low Cycle Fatigue Testing". The fatigue specimen geometry used is shown in Fig. 1.
The tests were conducted on a 22 kip closed loop servo-hydraulic machine. The test was
conducted in displacement control; this was close to strain control but was not as dangerous.


is made up of an elastic component. For low cycle fatigue the main result is the cyclic life. b and c are fitting constants and E is the elastic modulus.Initially the strain versus life behavior of the material was measured so that subsequent evaluations of indenter behavior could be made as a function of elapsed life. The cycles to failure are plotted as 2Nf so that 2Nf = 1 gives a relationship between a half cycle during the fatigue test and a monotonically loaded test. These have the form ε ea = σ' a ( 2 N f ) b + ε' f ( 2n f ) c E where σ'a. εpa. εa. This was to demonstrate the nondestructive nature of the indention test. εa. Nf. The 2024-T4 aluminum alloy has the code AL2 and the 7075-T6 aluminum alloy has the code AL7. The test is conducted in completely reversed strain control so εa represents the total positive strain range or the total negative strain range. After the strain versus life relationship was established. εea and a plastic component. The elastic and plastic components are fitted with straight lines on the log-log plots. 2Nf. ε'f. versus life. cycles to failure. 2 through 10. The plotted strain range. The results of the 2024-T4 and 7075-T6 aluminum fatigue tests are given in Figs. In addition fatigue tests were conducted on two specimens that had been subjected to multiple indentation tests prior to fatigue testing. measured as strain range. ε a = ε ea + ε pa Each component of strain is plotted as a function of 2Nf on log-log plots. When these fits are combined as given in eq. interrupted tests were conducted so that ABI tests could be made on specimens that had been cycled to a fraction of the failure life and also so that monotonic tensile tests could be conducted on specimens that were cycled to a fraction of the failure life. εa. εa versus life. the total strain range. A summary of all of the fatigue and tensile tests conducted is given in Table 1. The strain range. has the form 3 . is half of the total strain range. (1).

0. The two are compared on Fig. The 7075-T6 cyclic stress-strain curve is plotted in Fig.εa = σ' a ( 2 N f ) b + ε' f ( 2 N f ) c E The strain versus life plots for the 2024-T4 aluminum are given in Fig. For this the half stress range. It does not show much hardening. Considering typical scatter it is probably better to say only that the result of the tests with ABI 4 . For materials that change the stress-strain property during cycling. The 2024-T4 cyclic stress-strain curve is plotted in Fig. A second way that the low cycle fatigue data are treated is to plot the cyclic stress-strain. 2a and for the 7075-T6 aluminum in Fig. From this it is obvious that the material 2024-T4 continues to harden during entire fatigue life but experiences most of the hardening during the first half of life. εa. The 2024-T4 had extensive hardening and did not completely saturate at half life. the cyclic stress-strain is plotted near the half life. σa. 3b. Therefore the cyclic stress-strain was plotted at 50% life. 2b. It can be seen that these specimens appear to have slightly longer life than the specimens tested in the original condition. is plotted as a function of the half strain range. 0. One of the objectives of the fatigue testing was to see if the indenting of the specimen would have any effect on the fatigue life. hardening or softening.5 Nf and 90% life. 2c. Since it is stated that an indenter test is non-destructive. it is important to verify this for fatigue behavior. a point where there is no more increase in the stress-strain curve. 0.5 Nf with the hope that the hardening or softening reaches an equilibrium called saturation. Fatigue tests were conducted on two 2024-T4 aluminum alloy specimens with five indentations each. The median strain life curve for specimens tested in the original condition is compared with the tests that were subjected to Automatic Ball Indention (ABI) before fatigue testing in Fig. 4. 3a.9 Nf.

5. 6a through 6d. From Fig. In Fig. the load increased at constant displacement range as the test progressed. This material continues to harden somewhat throughout its entire life. The specimen appears to harden.pretest did not show any adverse effects and the ABI is completely non-destructive in terms of fatigue damage. 7 it is obvious that the stress-strain response for the 2024-T4 is increased with increasing cycles. 8. The monotonic stress-strain behavior for the various levels of cyclic loading is shown in for 2024-T4 in Fig. which is a little more than 10% of life the majority of the hardening already has occurred. Fig. and with cycle 700. but at 400 cycles. that is. 5c. This hardening could provide a measurement of the amount of fatigue damage that has occurred.0073 strain are given in Fig. which is more than 50% of life there is some additional hardening. Several specimens were cycled to a certain percentage of the life and then a monotonic stress-strain curve was conducted. with cycle 390. Fig. To see this more clearly the result from cycle 10 is plotted separately with the result from cycle 100. This alloy did not show much change in the load because it is not a hardening material. 8 is apparent that the 7075-T6 does not change its stress-strain response very much as a result of cyclic damage 5 . 5a. It has a neutral response to cyclic loading. Another objective of the fatigue testing was to look at the cyclic stress-strain changes during the test to see if this change could be an indicator of the fatigue damage. After 100 cycles. 5d. A composite of the cycles is in Fig. The same type of plot is made for a 7075-T6 specimen in Fig. Fig. The load versus displacement curves for a 2024-T4 specimen subjected to ±0. 7 and for 7075-T6 in Fig. 5b. To do this first the typical hardening behavior of the 2024-T4 aluminum is given in a series of figures that show the load and displacement values as measured during the test at various percentages of Nf. The total cyclic life for this specimen was 772 cycles. neither hardening nor softening.

It is clear from this result that the hardening resulting from the cyclic loading can be measured but that this nearly saturates with cyclic loading. 3. In addition the local details of the stress and deformation response of a material could be predicted in a way not possible from test results. 10a for all of the test results on 2024-T4. the finite element method could be used to study the effect of various indenter variables on material response. With a successful prediction of a test result.and therefore would not provide a way to use the stress-strain changes to measure the amount of fatigue damage. that is the tensile test versus ABI test stress-strain measurement. Fig. The comparison between the standard tensile test and the ABI test is made in Fig. This could include the indenter size. 10b shows a comparison of the tensile results. The ABI test measures the true stress-true strain result rather than the engineering stress and strain. The result of the ABI stress-strain measurements for the 2024-T4 is shown in Fig. This includes the stress-strain curves measured at 0. material. on virgin material. 70 and 400 cycles. A further objective was to see whether the ABI test could measure the stress-strain changes that accompany cyclic loading. To make comparisons between the ABI test result and the monotonic test result all tests were converted to true stress-true strain. Fig. 10c shows the comparison after 71 cycles and Fig. profile. 10d shows the comparison after 400 cycles. The first step in the analysis of the indenter response was to see if a typical loading response 6 . The standard tensile test and the ABI test follow the same hardening trends. 9. application of multiple indenters and spacing. Numerical Simulation of Indenter Response A finite element simulation of the indenter response on a material was conducted to see if it is possible to predict the indenter behavior during the loading cycle.

The pre and post processing code used to prepare the finite element mesh was PATRAN 5.062 inch heads diameters. The stress-strain analysis is treated as a two-dimensional axisymmetric problem in which half of a diametrical cut through the center of the indenter ball and the plate is analyzed. 11 along with a schematic of the indenter head showing the definitions of the various symbols used to identify the measurements. ball and brazed attachment system.030 inch and 0.030 indenter head is shown in Fig.5-1. The element type used was a Quad 4. This included a convergence analysis and the stress and displacement predicted by the simulation during the indentation process. The detailed model near the indenting surface is shown in Fig. The finite element analysis code was ABAQUS 5. 2-D solid axisymmetric element. A summary of the measurements for nine indenters covering five different sizes is given in Fig. The material being indented in this second simulation is the 2024-T4 7 .0005 in. They were the 0. To conduct a more precise analysis the exact dimensions of the indenter were measured with a calibrated traveling microscope so that the simulated indentation procedure could be predicted based on actual dimensions. accuracy. The original system chosen for the simulation study was an A533B steel plate which was indented with a 0. Two of the indenter sizes were chosen to conduct a simulated indentation modeling. 12b. These software packages were run on a SUN workstation. The overall finite element model of the indenter 0. An overall analysis with results were given in the previous progress report.062 inch ball geometry of tungsten carbide. The indenting simulation is modeled as a non-linear contact problem.record from a test conducted with the Microprobe system at Advanced Technology Corporation Headquarters could be successfully modeled by the finite element system. 12a.1. This microscope can measure the dimensions to 0. rod. The first simulation analysis of the indenter response used nominal dimensions of the indenter.

The purpose of the finite element simulation in this section was to see if the ABI test could be simulated numerically. 14. that is. The finite element model for the simulation using a 0.5 lb load is given in Fig.062 inch indenter head is shown in Fig. After the 78. the ratio of indenter diameters squared. A comparison between the actual ABI test and the simulation of the test is shown in Fig. Fig.030 inch indenter head at 78. The load versus depth of penetration for the ABI test and the simulation is shown in Fig. Fig. 15b has the details near the indenter head. 17b for plastic depth. The larger diameter indenter requires a load increase of about the difference in area. 14b shows the plastic component of both test and simulation. Fig. For this material accurate stress-strain data is available from tensile tests. For this indenter head size the total displacement has a slight but constant difference but the plastic component of the displacement matches exactly. It was used for the indenter testing so that direct comparisons can be made between the indenter simulation and the actual indenter test. 17a for total depth and Fig. The deformation and stress distribution for the 0. For this case the plastic displacements also have a 8 . the stress pattern represents the residual stresses that are remaining as a result of the indentation. 15a has the entire indenter and Fig. 16b. The difference in total displacement match is in the order of 2x10-4 inch. The stress distributions shown are the von Mises equivalent stresses. Fig. These values more accurately indicate the stress value relative to a yielding condition. 13b. 16a and for the residual pattern after unload from 319 lb in Fig. Fig. measurements from ABI and predictions. 15. 14a has the load versus depth.aluminum alloy used in the fatigue tests. 13b. The same distributions after unload of the 78. The deformation and von Mises stress distribution is shown for a 319 lb load in Fig. 13a. 17.5 lbs is given in Fig.5 lbs has been unloaded.

a strain of negative 0. a simulation analysis of the fatigue test was performed numerically. The simulation measured the stress response to an applied strain level. a simulation could be first conducted to see if the desired result is obtained. this was applied as a displacement placed over the gripping area of the fatigue specimen in a manner that simulates the actual loading during the fatigue test. Things like changing indenter head geometry or material could require an expensive trial and error sequence to determine optimum test conditions. These software packages were run on a SUN workstation. The entire simulation 9 .1.small but constant difference. 4. Numerical Simulation of Fatigue To calibrate the instrumentation for the fatigue tests and to see that the results are acceptable. Each new head could require an expensive material purchase and machining operation. The specimen was then unloaded to the same strain level in the negative direction.02. The pre and post processing code used to prepare the finite element mesh was PATRAN 5. In the future when the parameters of the indenter system might be changed.02.5-1. The simulation was conducted with a finite element model that used the same software as the simulated indenter analysis. The finite element analysis code was ABAQUS 5. The total maximum strain level was positive 0. With the simulation the parameters can be easily changed without the need for costly machining or material purchases. This would suggest that a simulation of a test condition can predict actual behavior within a fairly good accuracy. The cycling was continued by again increasing to the same positive level of strain and unloading to the same negative strain level. For both indenter sizes the results of the simulation match the test results very well.

20b shows the von Mises stress for cycle 1. Figs 20c and d. The stress pattern. These regions of high stress occur in the parts of the specimen that 10 . 20a shows σyy for cycle 1 and Fig. σyy. 20a through 20f.02 strain level and one at the negative 0. 60 and 80.02 strain level. and second the von Mises equivalent stress. Each plot shows two models. The monotonic stress-strain properties measured in a tensile test were used to relate the strain to the stress. The original specimen shape is shown as a faint background outline. is uniform at cycle 1 and reaches a maximum of about 65 to 70 ksi. Fig. The stresses shown are first the y direction stress. A model on the finite element mesh is shown in Fig. The same pattern is repeated for cycle for cycle 60. 19a through 19e. 40. 20. The material simulated in fatigue was the 2024-T4 aluminum alloy.took approximately 20 hours of computer time to run. particularly. The deformation response is shown in Fig. It is possible to see in these plots a progressive shape change caused by the cyclic loading. σyy. The effect of the cyclic loading on the specimen model is shown on a series of figures showing the deformed grid after a set number of cycles. 20e and f. Although the actual test does not exhibit the dimensional change shown in the simulation. These plots correspond to cycles 1. and the for cycle 80. For example. The stress response is shown in Figs. At cycle 80 the small regions of high stress reach even higher maximum values. Figs. The actual test specimen failed before 80 cycles at this strain level. one for the deformation at the positive 0. 18. During each cycle the stress and deformation were measured so that a picture of the deformation and the stress changes could be recorded. the simulation does indicate a progressive damage in the fatigue test. After 60 cycles the stress pattern segregates into regions of high and low stresses with the highest regions reaching the range of 105 to 110 ksi.

forms sharp corners as a consequence of the fatigue deformation. 22. The maximum stresses in these regions increase with increased cycling. The overall increases in the local stresses correspond to the cyclic hardening character of the material. In addition the stresses which are fairly uniformly distributed at the first cycle. 11 . The effect of fatigue test simulation is interesting and should be studied further to understand the full implications of the result. The original monotonic stress-strain behavior of the material was used for the entire simulation. 21 and the cyclic stress-strain for the simulation is in Fig. the cyclic load versus displacement from the simulation test is shown in Fig. In both cases a cyclic hardening behavior was predicted. not from a change of the stress-strain property used in the model. become segregated into high and low stress regions with continued cycling. This prediction comes from the simulation model itself. The fatigue simulation does not predict and actual failure point but does show that the continued cycling causes severe deformation changes. To show how the fatigue simulation predicts the cyclic hardening behavior of the material. These deformation patterns simulate the formation of stress concentration areas that could lead to the formation of a crack and subsequent failure of the specimen.

12 .

1 – Low-Cycle Fatigue Test Specimen Configuration .13 Fig.

14 Fig. 2a – Strain Amplitude versus Fatigue life for 2024-T4 Aluminum .

15 Fig. 2b – Strain Amplitude versus Fatigue Life for 7075-T6 Aluminum .

2c – A Comparison of 2024-T4 and 7075-T6 Aluminum Srain-Life Plots .16 Fig.

3a – Cyclic Stress-Strain Relationship From Low Cycle Fatigue Test for 2024-T4 Aluminum .17 Fig.

18 Fig. 3b – Cyclic Stress-Strain Relationship From Low Cycle Fatigue Test for 7075-T6 Aluminum .

19 Fig. Non-ABI Data vs. 4 – Strain Amplitude versus Fatigue life for 2024-T4 Aluminum. Pre-ABI Points Data .

20 Fig. Specimen AL209. 5a – Typical Cyclic Load versus Displacement Curve for 2024-T4 Aluminum. All Cycles .

Specimen AL209.21 Fig. Cycle 10 vs. Cycle 100 . 5b – Typical Cyclic Load versus Displacement Curve for 2024-T4 Aluminum.

Cycle 10 vs. Cycle 390 .22 Fig. Specimen AL209. 5c – Typical Cyclic Load versus Displacement Curve for 2024-T4 Aluminum.

23 Fig. Cycle 700 . 5d – Typical Cyclic Load versus Displacement Curve for 2024-T4 Aluminum. Specimen AL209. Cycle 10 vs.

24 Fig. Specimen AL705. All Cycles . 6a – Typical Cyclic Load versus Displacement Curve for 7075-T6 Aluminum.

6b – Typical Cyclic Load versus Displacement Curve for 7075-T6 Aluminum. Cycle 2 vs.25 Fig. Specimen AL705. Cycle 10 .

26 Fig. 6c – Typical Cyclic Load versus Displacement Curve for 7075-T6 Aluminum. Specimen AL705. Cycle 155 . Cycle 2 vs.

7 – Monotonic Stress-Strain Curve from Standard Tensile Test for 2024-T4 Aluminum at Different Precycle Stages .27 Fig.

8 – Monotonic Stress-Strain Curve from Standard Tensile Test for 7075-T6 Aluminum at Different Precycle Stages .28 Fig.

29 Fig. 9 – Monotonic True Stress-True Plastic Strain Curves from ABI Tests for 2024-T4 Aluminum at Different Precycle Stages .

10a – A Comparison of True Stress-True Strain Curves from Standard Tensile Test and from ABI Test. 2024-T4 Aluminum. All Curves .30 Fig.

10b – A Comparison of True Stress-True Strain Curves from Standard Tensile Test and from ABI Test.31 Fig. All Virgin Materials . 2024-T4 Aluminum.

32 Fig. At About 15% Fatigue Life . 2024-T4 Aluminum. 10c – A Comparison of True Stress-True Strain Curves from Standard Tensile Test and from ABI Test.

33 Fig. 10d – A Comparison of True Stress-True Strain Curves from Standard Tensile Test and from ABI Test. At About 65% Fatigue Life . 2024-T4 Aluminum.

34 .

Indenter Head .35 Fig. 12a – A Finite Element Simulation Model of ABI Test with 0.030 in.

Indenter Head.36 Fig. 12b – A Finite Element Simulation Model of ABI Test with 0.030 in. Details Near the Indenter Head Tip .

37 .

38 .

39 .

0.030 in. Comparing with ABI Test Result. Indenter Head . 14a – Load Versus Depth from Finite Element ABI Test Simulation.40 Fig.

14b – Load Versus Plastic Depth from Finite Element ABI Test Simulation. Comparing with ABI Test Result.41 Fig. 0.030 in. Indenter Head .

42 Fig. 15a – A Finite Element Simulation Model of ABI Test with 0.062 in. Indenter Head .

Indenter Head.030 in. Details Near the Indenter Head Tip . 15b – A Finite Element Simulation Model of ABI Test with 0.43 Fig.

44 .

45 .

17a – Load Versus Depth from Finite Element ABI Test Simulation. 0. Comparing with ABI Test Result. Indenter Head .46 Fig.062 in.

062 in. Comparing with ABI Test Result. Indenter Head .47 Fig. 0. 17b – Load Versus Plastic Depth from Finite Element ABI Test Simulation.

48 Fig. 18 – A Finite Element Simulation Model of Fatigue Test .


Fig. 19a – A Deformation Plot from Finite Element Fatigue
Test Simulation, 2024-T4 Aluminum, Strain = ±0.02, Cycle 1


Fig. 19b – A Deformation Plot from Finite Element Fatigue
Test Simulation, 2024-T4 Aluminum, Strain = ±0.02, Cycle 20


Fig. 19c – A Deformation Plot from Finite Element Fatigue
Test Simulation, 2024-T4 Aluminum, Strain = ±0.02, Cycle 40

Strain = ±0. 2024-T4 Aluminum. 19d – A Deformation Plot from Finite Element Fatigue Test Simulation. Cycle 60 .52 Fig.02.


Fig. 19e – A Deformation Plot from Finite Element Fatigue
Test Simulation, 2024-T4 Aluminum, Strain = ±0.02, Cycle 80



56 .

57 .

58 .

59 .

60 Fig.02 . 21 – The Cyclic Load Versus Gage Line Displacement from Finite Element Fatigue Test Simulation. 2024-T4 Aluminum. Strain = ±0.

61 Fig. Strain = ±0.02 . 2024-T4 Aluminum. 22 – The Cyclic Stress-Strain Curves from Finite Element Fatigue Test Simulation.

APPENDIX B Final Report Professor K. Linga Murty North Carolina State University November 1998 .

423 and 473 K at stresses varying from 1. NCSU group was to investigate and demonstrate the capabilities of SSM based on ABI technology in characterizing the έ-σ-T relationship for various lowtemperature alloys commonly used for solder applications in microelectronics. we have performed at elevated temperatures to obtain activation energy for creep/deformation in Sn5%Sb while the variations of έ with σ were also characterized for the Pb-alloys at an additional temperature. as mentioned earlier. First type of testing included ABI tests under constant indenter velocity with velocity varied by several orders of magnitude. Notwithstanding this cut-back. In addition to tests at ambient. KL Murty page 1 . and the creep strains were measured using LVDT. Tensile creep specimens with a gauge length of 12. Sn5 %Sb Tin-antimony alloy with chemical composition Sn-5%Sb was obtained in the form of 1 mm thick sheet from Alpha Metals.25 to 30 MPa. However. class-A and superplastic. these results do demonstrate the capability (this being the major objective of the substudy). we have considered Sn5%Sb. the viability of SSM in obtaining the desired information. Pb5%Sn and Pb62%Sn which comprise various classes of materials from the deformation/creep constitutive equation point-of-view: class -M. To this end. Second type of testing included load relaxation tests using cylindrical indenter so that constant load corresponds to constant stress. Linga (KL) Murty (919) 515-3657 FAX 515-5115 Study of Solder-Alloys As a part of the DoD-SBiR-II (Contract No. we demonstrate from the first two types of test methods. we have not considered the third type here which involves development of new algorithm and time consuming tests. The results need further analyses which involves more funding and time. N00421-96-C-1121 to the Advanced Technology Corporation).4 mm were prepared from the sheet parallel to the rolling direction. pure lead. Constant load creep tests were performed at 298. due to the change in the time and cost (reduced by about 50%). Inc.North Carolina State University Department of Nuclear Engineering College of Engineering Box 7909 Raleigh NC 27695-7909 Prof. Third type of tests that were contemplated in the beginning were the creep tests under constant stress/load again first using cylindrical indenter and then followed by ball indenters. 373. however. K.

Haggag. and Figure 2 shows the variation of minimum creep rate with stress at different temperatures. K. R. Mahidhara et. These results are similar to the tensile test data which also indicated the transition at 473 K. The minimum creep rates were evaluated from the creep curves. Model PortaFlow-Pl (patented by the Advanced Technology Corporation. the corresponding diameter of the indentation was about 0. M. At 473 K. 323. Each indentation covered a large number of grains since the grain size of the material was small ( 10 µm).575 mm diameter was used and the maximum depth of penetration of the indenter was about 0. The creep curves were generally characterized by normal primary creep. ABI tests involve pushing a spherical indenter into a specimen while monitoring the load versus depth of penetration. TN). KL Murty page 2 . έ = Aσ n .375 mm. Oak Ridge. Mahidhara. 1. a transition occurred from a value of n=5 in the high stress region to a value of n=3 in the low stress region (below 2 MPa). L. 373 and 423 K. short steady-state regime and relatively long tertiary region as shown in Fig. (1) was found to be obeyed over the entire stress range at 298. in Design and Reliability of Solders and solder Interconnections. Tests were carried out using a table top Stress-Strain Microprobe (SSM) System. 373 and 423 K with a value of n≈5. K. A power law relationship of the form. This was typical of all the test conditions.Automated ball indentation tests were carried out at 298.1 mm.1 Figure 1 Typical creep curves (sn5%Sb) 1 R. no specific specimen preparation was required except that the specimen should be flat and the surfaces must be parallel. For ABI tests. A tungsten carbide ball indenter of 1. Creep and Mechanical Properties of Sn5%sb Solder.. ( 1997) 75. Murty and F. al. A light mechanical polish (600 grade polish) was given in order to ensure that surface contamination did not influence the ABI test results and also to achieve flat parallel surfaces. K.

from an Arrhenius plot of ln(strain-rate) against reciprocal of absolute temperature (Figure 3). the tensile test data yielded much lower values (~6. it has been well established that ABI can be employed for studying the stress-strain behavior of materials and that the results agree very well with conventional tensile KL Murty page 3 .Figure 2 Minimum creep rate vs stress at various temperatures The activation energy for creep was determined in the high stress (n=5) region. As reported earlier.4 kCal/mole).1 kCal/mole. Least squares analysis of the data yielded a value of Q=12. Figure 3 Activation Energy Plot (Creep Data) ABI Results From previous studies.6±1.

rapid and non-destructive technique and requires small amounts of material with minimum material preparation. The primary data generated in an ABI test is the indentation load versus depth of penetration curve. With ABI technique. 4. (2) ε p = 0 . σ= 4P πd p2 δ . ABI is a relatively simple.2 p D where dp and D are the plastic indentation diameter and diameter of indenter respectively. The flow curve is usually represented by the equation. 323. From the fact that the strain hardening parameter n is equal to the true uniform strain (εu) at the ultimate tensile stress of the material. 373 and 423 K over a range of indenter velocities (strain-rates). the true ultimate tensile stress can be evaluated as. tensile strength. and the work hardening parameters of the material are evaluated directly from the flow curve. Single cycle method is used in lieu of the standard partial unloading technique because of the relatively fast rates employed in characterizing the strain-rate variation of flow behavior. Typical indentation load versus depth curves at various indenter speeds. In the present investigation. σ = Kεn . yield stress.results. ABI tests were carried out at 294. d . (3) where x is the true indentation stress and x is a parameter which depends among other things also on the system compliance. Indentation load versus depth of penetration curves for Sn5%Sb obtained at two different indenter speeds are shown in Fig. Figure 4. (4) where K and n are the strength coefficient and strain hardening exponent respectively. The true plastic strain is determined from the equation. The corresponding true stress and true strain values are calculated by the system software. The corresponding flow stress is calculated from the following equation. and all the relevant mechanical properties are evaluated by further analysis of this data. KL Murty page 4 . The principle of the test technique and the calculation procedures have been reported previously.

SSM can be adopted for in-service or in-situ application for characterizing the solder-condition leading to the predictability of their remaining life. 6). n n . KL Murty page 5 . the engineering value) is then obtained from the equation. From the Arrhenius plot (Fig.4 which agrees closely with that determined from creep experiments at high stresses. The values of n and Q obtained from both ABI and creep point out to the same deformation mechanism which we propose to be viscous glide as described below.1±1. It is clear from the study that by decreasing the ball diameters to micron-size.σTS = Knn . Stress relaxation tests offer the possibility of studying the deformation behavior over a wider range of strain rates compared to conventional creep tests. UTS = K { e } (6) The indenter velocity (vi) is converted into tensile strain rate using the relationship. it is capable of evaluating stress relaxation behavior of the material. A power law relationship was found to be obeyed with a value of n=5.9 έ = 2 vi 5 dp (7) Figure 5 shows the variation of strain rate with true ultimate tensile stress at these temperatures. Figure 5 Variation of strain rate with UTS from ABI tests Figure 6 Arrhenius plot – ABI Data SSM is a versatile tool in the sense that apart from stress-strain properties.8 kCal/mole corresponding to a stress level of 60 MPa which is also in good agreement with that for creep. the activation energy for deformation was determined to be 13. (5) The ultimate tensile strength (UTS.

one would expect the dislocations to break away from the solute atmospheres as high stresses are applied.5 Hence.2 These are sequential processes so that the slower of the two acts as the rate controlling step. 7 (1973) 899. Solid solution alloys are broadly categorized as class-M alloys if the value of n is equal to 5. and climb of edge dislocations being slower.9 The activation energy for deformation would be equal to that for solute diffusion via vacancy mechanism. becomes the rate controlling mechanism. the rate controlling mechanism is the climb of edge dislocations just as in the case of pure metals. Dislocation creep in pure metals is characterized by a value of n=5. Kanert. 3). It may hence be concluded that in the present study the rate controlling mechanism is dislocation climb at all the test conditions except at very low stresses at 473 K (Fig.L.. 18 (1957) 1185. W 2 c . the activation energy for the mechanism could not be evaluated. at higher stresses.3 In class-M alloys. Weertman. 13 (1967) 325. 4 J. Such a mechanism which is also known as microcreep4 predicts an activation energy for creep which is equal to that for diffusion of solute elements. the rate controlling mechanism is solute-diffusion controlled dislocation glide since the dislocations are locked by solute atmospheres such that the rate of glide becomes slower than that of climb. J. 2 K. Progress in Mater.2. In class-A alloys. Vol. 3 KL Murty page 6 .D. Murty and O. the critical stress for the transition from viscous glide to climb should correspond to that for the breakaway of the dislocations from the solute atmospheres. In either case. co is the solute concentration and β is a factor dependent on the nature of the impurity cloud with a value between 2 and 4. Phys. Vol.L.. Murty. climb would be the rate controlling mechanism with a value of n≈5. Since the low stress behavior has been exhibited only at one temperature. Burke. creep deformation is perceived to be controlled by viscous glide of dislocations..M. Vol. Appl. 4 Dislocation creep occurs as a result of glide and climb of edge dislocations. Sci. Phys. As Murty17 has shown in the case of an Al-Mg alloy. Scripta Met. (8) τc = β m o 3 2 kT b where Wm is the binding energy between the solute atom and the dislocation. Appl. recovery takes place by the climb of dislocations. 67 (1990) 2866. Due to the uncertainty in the values for the various parameters in this equation.. and class-A alloys if the value of n is equal to 3. On the basis of the n value in the low stress region at 473 K. Sherby and P.Deformation Mechanisms (SnS%Sb) Creep deformation mechanisms are identified mainly by the value of the stress exponent n and the activation energy Q. O. 5 K. Vol. J. Assuming that the low stress region is in fact controlled by viscous glide of dislocations.

έ = A' e-QPipe σ5.A. The lamellar eutectic microstructure is evident in Pb62Sn. in Proc. Langdon. E is the elastic modulus.17. solute diffusion through dislocation pipes could dominate so that the strain-rate would be proportional to the dislocation density. 15 It is possible that viscous glide is the rate controlling mechanism in both the regimes. J.5" thick x 1.G. It is clear that both pure lead exhibits relatively large grain size while Pb5Sn depicts solid solution microstructure with relatively smaller grain size. Further work is needed to unequivocally prove this contention. However. London (1985) 221. the range for this critical stress corresponds to 2x10-4E to 1x10-3E.) TMS (1997) 69. Our data is not sufficient to determine the activation energy for creep while cube-rate dependence is observed. measuring about 0.Al loys Pure lead. (9b) This implies that at low stresses and high temperatures. Acta Met. The Institute of Metals. 6 Such transitions were reported in many class-A alloys.Yavari and T.G. Vol.8 The transitional stress in the present investigation does fall in this regime. Langdon. T. the activation energy of 13 kCal/mole determined from both creep and ABI experiments is nearly half that for self diffusion (QSD) in this alloy system.7 A review on the transition mechanisms in class-A alloys has been made recently by Murty. in that case. However. At low temperatures and/or high stresses. however. (9a) since ρ α σ2. were obtained from Indium Corp from which appropriate specimens were made without any further heat treatment. Typical microstructures at lower magnification are being taken for grain-size and/or phase size evaluation. viscous glide operates with the steady state creep-rate varying as σ3 with an activation energy close to that for solute diffusion through the lattice. in Dislocations and Properties. Seventh International Conference on Creep and Fracture of Engineering Materials and Structures. Pb5%Sn and Pb62%Sn alloy ingots. 30 (1982) 2181. This value of Q agrees with the activation energy for low temperature dislocation climb assisted by vacancy diffusion through dislocation core. and thus we believe that the high stress region is due to the climb of edge dislocations. 7 KL Murty page 7 .an exact transition stress (τc) cannot be determined. The optical metallographs depicting the grain structures of the three alloys are included in figures 7a to 7c which were taken at 500X. Murty. έ = A1 ρ e-Qpipe σ3 .5" wide x 5" long. the stress exponent will be higher by a value of 2 or equal to 7. 6 P. the stress exponent of 5 along with the activation energy for creep of about one-half of that for lattice diffusion are in good agreement with low-temperature viscous glide. However.C. Lead.L. Mohamed (Eds.9. earthman and F. At high stresses. 8 K.

Pb5Sn (500X) c. Pb62Sn (500X) Figure 7.a. relaxation during tests at the lowest strain-rate of 2x10-1 sec-1 KL Murty page 8 . Pure Lead (500X) b. lead with 5%Sn solid solution alloy and eutectic Pb62%Sn at room temperature at varied strain-rates by varying the indenter velocity from 2x10-5 sec-1 to 2x10-2 sec-l. Optical Metallographs at 500X for pure Lead (top-a). Pb5%Sn (middle-b) and Pb62%Sn Eutectic (bottom-c) Strain-Rate vs Stress Results at Room Temperature: ABI tests were performed on pure lead. In many cases.

18σ for Pb62Sn 9 H.45σ for Pb5Sn έ = 4. where G is the shear modulus).7 for Pb5Sn έ = 4. Haggag and R. in print. “Phenomenological Analysis of Plastic Spherical Indentation. 272-281.643x10-6 e0. these data are plotted on semi-log scale in Figure 9 which depicts lines with varied slopes. έ = 1. έ = 4.L. K.K. “Tensile. έ = A σn.” Trans.4 for Pure Lead έ = 1. These results are first analyzed assuming power-law dependence of the strain-rate. Strain-rates were evaluated at load maximum using Francis' equation9 following the procedure outlined by Murty et al.8x10-19 σ9. Thus.62σ for Pure Lead έ = 2.50x10-7 e0. Creep and ABI Tests on Sn5%Sb Solder for Mechanical Property Evaluation. Murty.18x10-3 G. July (1976) pp. Mahidhara.precluded in obtaining reliable load-penetration curves.3x10-26 σ15. 10 KL Murty page 9 . where n is the stress exponent.6 for Pb62Sn Figure 8.94x10-9 e0. Francis.” Journal of Electronic Materials. F.10 True stresses are evaluated at the maximum load along with true strain-rates. ASME. Log-Log Plot of ABI Results at Room Temperature Representing Power-Law Dependence The relatively large values for n indicate that an exponential stress dependence may be appropriate at these relatively high stresses (10 MPa is around 1.M. Figure 8 shows these data on log-log plot and the results for the three materials yielded the following relationships.8x10-17 σ12.

These analyses indicate that at these stress levels at room temperature. Further data analyses will be performed following tests at elevated temperatures which are now in progress. The strengthening due to Sn-solute additions is clearly noted in these data. Pb5Sn solid solution alloy and Pb62Sn eutectic alloy at room temperature. These tests were performed on the three Pb-alloys at room temperature and 50°C. and clearly demonstrate the decreased load as a KL Murty page 10 . Tests were performed on SSM at constant indenter velocity (1x10-3 in/s) and load versus depth were monitored to about 15 mils (approximately 22-25% strain) at which point the indenter was arrested/stopped. RT ABI Results Plotted on a Semi-Log Form Representing Exponential Variation of Strain-Rate Load Relaxation (using Cylindrical Indenter): Load relaxation tests were performed using a 62mil diameter WC cylindrical indenter. these correspond to the strain-rate versus applied stress once the modulus and indenter cross-sectional area were taken into account. These data at room temperature do indicate plausible deviations at the lowest stress level in pure lead which reveals trend towards power-law with far lower values for the stress exponents which correspond to dislocation climb regime (of about 5 or so). Figure 9. strain-rates follow deformation mechanism with stress-independent activation area as found earlier for SnSb. The load relaxation is monitored for about 30 minutes from which the load-rate versus load was followed. Figures 10a to 10c show the load relaxation data for pure lead.

Pb5Sn (lo-left) and Pb62Sn (c-right) KL Murty page 11 . Corresponding load-rate versus load are shown in double-log plots for the three cases in figure 11 for pure lead. Figure 10 Load vs time for Pb (a-top).function of time in a very orderly manner. Pb5Sn and eutectic Pb62Sn.

Pb5Sn and Pb62Sn Figure 12 Load vs time curves for Pb (a-top).Figure 11 Load-Rate vs Load for RT for Pb. Pb5Sn (b-left) and Pb62Sn (c-right) KL Murty page 12 .

Figure 13 compiles and compares the load-rate versus load for the three materials at 50°C tests. As pointed out earlier.Similar study was made at 50°C and figures 12a to 12c include load versus time curves for the three alloys which are very similar to but shifted on the stress axis to lower stresses (due to higher temperature). In addition. in-situ recrystallization of lead alloys is known to give rise to oscillatory behaviors as seen here. KL Murty page 13 . It is recommended that these results be extended to other temperatures and creep tests at constant load/stress using closed-loop control be included as further study. further data analyses will shed light on the underlying deformation mechanisms but warrant more funding and time. Pb5Sn and Pb62Sn at 50°C) Varying slopes of these curves as a function of load (or stress) clearly indicate the transitions in deformation mechanisms which include dislocation controlled creep at high stresses and point-defect dominated mechanisms such as Nabarro Herring and/or Coble creep mechanisms. These results indeed point out to the viability of SSM in characterization of deformation kinetics of materials. Figure 13 Double-Log Plot of Load-Rate vs Load (Pb.

APPENDIX C Final Report Sample Tensile and ABI Test Results on Aluminum 2024-T4 in the As-Received Condition November 1998 .

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