Reliability of High-Voltage MnO 2 Tantalum Capacitors

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1 Reliability of High-Voltage MnO 2 Tantalum Capacitors Erik Reed, George Haddox KEMET Electronics Corporation, 2835 Kemet Way, Simpsonville, SC Phone: , Fax: erikreed@kemet.com Abstract While tantalum polymer capacitors are making significant penetration into many applications previously dominated by MnO 2 tantalum capacitors, the present reality is that significantly more capacitors are manufactured with MnO 2 as the cathode material than are made with conducting polymer. There are reasons other than market inertia for the good market performance of MnO 2 capacitors. These include lower cost, good reliability, and robustness against high temperature and humidity. Recent work reported at CARTS focused on the reliability of tantalum polymer capacitors which display very long predicted lifetime. This work featured accelerated lifetesting of capacitors at various voltages and temperatures, and formulation of acceleration models that predict lifetime at normal use conditions. Even while the polymer capacitors were receiving this needed attention, improvements continued to be made in MnO 2 capacitors. The most improvement is seen in MnO 2 capacitors rated from 25 to 50V. The present work involves accelerated lifetesting of these improved high-voltage MnO 2 capacitors. The test strategy is similar to that employed with the polymer capacitors. Time-to-failure data are presented that were collected over a range of voltages and temperatures. Trends in the data are identified and models for voltage and temperature acceleration are discussed. Median lifetime at rated conditions is estimated, and comparisons and contrasts are drawn between MnO 2 and polymer capacitors and their underlying degradation mechanisms. Introduction While it is true that the market share of tantalum polymer capacitors in the tantalum capacitor industry is growing, high-volume manufacture of MnO 2 -cathode tantalum capacitors continues. The number of MnO 2 tantalum capacitors manufactured per year still outnumbers that of tantalum polymer capacitors by roughly 6:1 (revenue by about 3:1) and the MnO 2 parts are yielding their market share reluctantly. MnO 2 -cathode tantalum capacitors still cost less, have lower DC leakage current, withstand temperatures above 125 o C better, can be more stable in humid environments, and have a proven record of reliability that spans decades. The market share of tantalum polymer capacitors is growing because these parts offer some attractive performance advantages (lower ESR and somewhat higher volumetric efficiency with good reliability). Because they are a relatively new technology, they have received much recent research attention. Beside the obvious need to properly describe their electrical performance advantages, additional effort has been spent quantifying their reliability since they lack the long history of the MnO 2 -cathode parts, and traditional reliability assessment techniques such as Weibull grading do not appear to be directly applicable (often so few capacitors fail under normal test conditions that one cannot perform the calculations). Some benefits of these research efforts are the refinement of techniques for conducting accelerated lifetests, new insights into the Page 1 of 11

2 complexity of the resulting time-to-failure data, and a nascent effort to identify and quantify the various physical mechanisms that drive this complexity. But advancements continue to occur in the incumbent (and still dominant) MnO 2 technology as well. Some of the more significant improvements are being made in the higher-voltage devices where reliability has not always been as good as customers would hope. KEMET has developed superior MnO 2 capacitors by employing a package of the best available manufacturing technologies in conjunction with a newly patented screening technique. These MnO 2 capacitors have excellent reliability and are targeted primarily to meet the needs of hi-rel customers. So an obvious question is: How good are these new MnO 2 capacitors, and how does their reliability compare with the high voltage polymer capacitors? The purpose of this paper is to address this question, look for differences between the two cathode technologies, and uncover additional clues regarding the various degradation mechanisms at work in tantalum capacitors. The strategy of the work is to perform accelerated lifetests on high voltage MnO 2 capacitors that have similar case size and voltage rating as the high voltage tantalum polymer capacitors previously reported on at CARTS USA 1. The resulting time-to-failure data from these lifetests are compared and contrasted with the previously reported tantalum polymer results to determine similarities and differences, and to draw inferences regarding the various underlying degradation mechanisms. The tested MnO 2 capacitors performed very well and predicted life at rated conditions was much longer than required by any practical application. But the MnO 2 capacitors were not necessarily superior to the tantalum polymer capacitors when judged solely on the basis of short-term dielectric strength (somewhat inferior) and projected lifespan at comparable dielectric stress levels (similar). Test Protocol The reader is asked to review the descriptions of the test and data analysis techniques that are described in the previous paper 1 and its references 2-4. Briefly summarized, the process involves exposing 100-piece samples of capacitors to various test voltages and temperatures while tracking the time to failure of each device. These data are plotted in log-normal format and the resulting t 50 times (time when half the samples have blown a 1A fuse often called median life ) are estimated for each test condition. Further analysis of these t 50 times versus changing voltage and temperature yields constants for simple voltage and temperature acceleration models. The voltage acceleration model is a simple power law in the form A V =(V Test /V Ref ) n, where n is an empirically derived exponent, usually between 12 and 20. The temperature acceleration model is a simple Arrhenius model with activation energy between about 0.8 and 1.9 ev. These models are used to extrapolate back to expected median life at rated voltage and temperature (or actual application conditions). More sophisticated physics-based models are available that better account for the interdependence of voltage and temperature acceleration, but the simple models described above are sufficient for the present need and are very easy to work with. Use of highly accelerated test conditions is necessary to produce reliability predictions in a practical timeframe (weeks rather than years). But because the test voltages are generally much higher than rated voltage, it is not unusual for some of the capacitors to fail during the 60-second voltage ramp at the start of the test. This initial voltage ramp at the start of the lifetest is similar to the procedure for common voltage breakdown tests and the resulting failure data provide useful insight into the short-term dielectric strength of the capacitors. Page 2 of 11

3 The capacitors tested for this work were MnO 2 -cathode tantalum capacitors having EIA 7343 footprint rated at 25V, 35V, and 50V. These are the same rated voltages that were explored in the previous work on high voltage tantalum polymer capacitors. However, the formation voltages (formation voltage determines the dielectric thickness) were generally higher for the MnO 2 capacitors than for the tantalum polymer capacitors. This caused the capacitances of the MnO 2 parts to be somewhat lower at 35V and 50V. Specifically, the capacitances for the MnO 2 parts were 22uF, 10uF, and 4.7uF for 25V, 35V, and 50V ratings, respectively, while the capacitances for the polymer parts in the previous work were 22uF, 15uF, and 10uF. Figure 1. Lognormal Plot of Failure Percentile versus Time to Failure at 1.8V r, 1.9V r, 2.0V r, and 2.1V r for Tests Performed at 105 o C on 15uF, 35V Experimental Tantalum Polymer Capacitors. Review of Previous Tantalum Polymer Results Figure 1 is a reproduction of some 105 o C time-to-failure data from the previous paper concerning high voltage tantalum polymer capacitors. The significance of this plot is that it captures the complete complexity of the timeto-failure plots and, thus provides clues regarding the various degradation behaviors at work in the tested capacitors. What is seen is that the failure modes for tantalum polymer capacitors can be broken into four distinct categories: initial failures, a flat region with a relatively few additional failures, a wear out region, and in some cases an anti wear out region where catastrophic failures slowed down or stopped completely. In the previous paper, the significance of each of these categories was discussed in detail. The initial failures were caused by exceeding the dielectric strength of the failed capacitors during the initial voltage ramp to the test voltage. This does not mean that these capacitors were defective, only that the accelerated test voltage required to produce Page 3 of 11

4 failures in a practical timeframe was higher than the potential barrier at the dielectric-cathode interface per MIS (metal-insulator-semiconductor) theory. It was shown that this mechanism disappears into insignificance when the test voltage is reduced to more normal levels. The flat region is hypothesized to be the result of gradual deterioration of the potential barrier at the dielectriccathode interface. This deterioration is likely caused by trace mobile charge migration to the insulatorsemiconductor interface over time as occurs in traditional semiconductor devices. The failure rate declines rapidly in this region as the trace mobile charge available at a fixed test voltage reaches its destination and the available charge supply is depleted. In the case of the tantalum polymer capacitors, very little temperature dependence was seen in the flat region which is consistent with other characterizations of the insulator-semiconductor (dielectriccathode) interface in these devices. The wear out region is characterized by dramatically increasing failure rate. Natural thermodynamic processes, accelerated by both temperature and electric field, lead to creation of oxygen vacancies in the dielectric in the neighborhood of the metal-dielectric interface. The resulting free oxygen is absorbed into the tantalum substrate and the vacancies cause the dielectric near the interface to become progressively more conductive. This reduces the remaining good dielectric available to support the applied test voltage. The increased electric field in the remaining good dielectric further accelerates creation of more oxygen vacancies, and the field strength grows even stronger in a vicious wear out cycle characterized by sharply increasing failure rate. This mechanism is considered to be the dominant wear out mechanism at rated voltage. Its voltage and temperature dependence are easily characterized if sufficient time is available to test at conditions that clearly separate the failure regions in time. As test conditions are further accelerated, the various regions become less distinct as the underlying mechanisms start to overlap in time. The overlap occurs because the underlying mechanisms do not accelerate uniformly with voltage and temperature (e.g., the flat region is only slightly temperature dependent while the wear out region is highly temperature dependent). The anti wear out region is thought to occur only in tantalum polymer capacitors. It is thought that extended periods of exposure to very high electric field strength and elevated temperature can lead to de-doping of the cathode material where it contacts the dielectric, rendering a thin layer of it non-conductive. This process reduces the electric field in the dielectric as some of the field begins to appear in this thin but growing insulating layer adjacent to the dielectric. The capacitors stop blowing 1A fuses, but nevertheless suffer significant capacitance loss as the effective dielectric thickness increases. It is presently unknown whether this mechanism has any significance at more normal application conditions. New MnO 2 Test Results Figure 2 contains time-to-failure data collected from the 10uF, 35V MnO 2 samples at 125 o C. As was the case for the 35V tantalum polymer capacitors, the 35V MnO 2 samples provided the optimal mix of conditions to allow clear separation of the various regions in the time-to-failure distributions in a practical, but still fairly long test time. One can observe clear separation of the initial failures from the flat region, and clear separation of the flat region from the wear out region. As expected, there was no evidence of an anti wear out region for the MnO 2 capacitors. The first significant observation is that there is clearly a wear out mechanism at work in these capacitors that produces increasing failure rate. A popular mantra of the MnO 2 tantalum capacitor industry has been that MnO 2 capacitor failure rate is always declining in time, so there must not be a wear out mechanism. Figure 2 provides hard evidence to refute this assertion. The capacitors do wear out and the wear out rate is clearly voltage dependent. This voltage dependence will be explored further. Page 4 of 11

5 Figure 2. Lognormal Plot of Failure Percentile versus Time to Failure at 1.7V r, 1.8V r, 1.9V r, 2.0V r, and 2.1V r for Tests Performed at 125 o C on 10uF, 35V Experimental MnO 2 Tantalum Capacitors. Figure 3. Lognormal Plot of Failure Percentile versus Time to Failure at 1.8V r, 2.0V r, 2.1V r, and 2.2V r for Tests Performed at 105 o C on 10uF, 35V Experimental MnO 2 Tantalum Capacitors. Page 5 of 11

6 Figure 3 contains time-to-failure data collected on the 10uF, 35V MnO 2 samples at 105 o C. Only a small amount of wear out behavior is observed at the highest test voltages. Casual observation of Figures 2 and 3 indicates that it takes about 10 times longer to reach wear out at 105 o C as it does at 125 o C at a given test voltage and the time is stretching out into the thousands of hours, even at very high test voltages. A temperature acceleration factor of 10 between 105 o C and 125 o C implies activation energy of about 1.5 ev in the Arrhenius temperature acceleration model. This is entirely consistent with the results observed for the high voltage tantalum polymer parts when they are tested at similar electric field stress. It is likely that the time to wear out would extend by another factor of ten if the test temperature were reduced to 85 o C. This would put the onset of wear out into the tens of thousands of hours (a few years) at 2 times rated voltage at 85 o C. It might take 10 years to collect convincing evidence of wear out at 85 o C and 2V r for these samples, which is a dramatically long time for an accelerated lifetest. So it s not really surprising that wear out is not routinely observed in MnO 2 capacitors at more normal lifetest conditions. Figure 4. Lognormal Plot of Failure Percentile versus Time to Failure at 1.8V r, 1.9V r, 2.0V r, 2.1V r, and 2.2V r for Tests Performed at 125 o C on 22uF, 25V Experimental MnO 2 Tantalum Capacitors. Figure 4 contains time-to-failure data collected on the 22uF, 25V MnO 2 samples at 125 o C. The initial failure region is clearly visible in the plots, but there is overlap of the flat region and the wear out region. It appears that wear out is postponed at lower test voltages, as expected, but the blurring of the mechanisms where they overlap in time makes it all but impossible to accurately quantify the voltage dependence of the wear out mechanism. The only solution to this problem for these 22uF, 25V MnO 2 parts would be to further reduce the test voltages and wait longer. But, as observed above for the 35V parts, the wait could be very long. This situation clearly demonstrates the practical limits of accelerated testing of highly reliable devices. Page 6 of 11

7 Figure 5 is a plot of median time to failure versus test voltage for both the 10uF, 35V MnO 2 parts and the 15uF, 35V tantalum polymer parts previously tested. The test voltages are normalized as a percentage of the dielectric formation voltage where the thickness of the dielectric is related to the formation voltage by a factor of roughly 2 nm per volt. The MnO 2 parts occupy the upper left of the plot while the polymer parts occupy the lower right of the plot. A thin dashed line is drawn on the plot that represents voltage acceleration that obeys a power law with a voltage ratio exponent of Figure 5. Median Life versus Percent of Formation Voltage for 10uF, 35V Experimental MnO 2 Tantalum Capacitors and 15uF, 35V Experimental Polymer Tantalum Capacitors. The median life at 2 times rated voltage (~50%V f ) and 125 o C for the 35V MnO 2 capacitors is about 900 hours. With activation energy of about 1.5 ev and a voltage ratio exponent of 13.2, the expected median life at rated voltage and 85 o C is about 0.85 billion hours or roughly 100,000 years. This is certainly long enough life for any practical application. It is clear from the plot that the voltage dependence of the wear out mechanism is essentially the same for both kinds of parts. The similar temperature dependence of wear out mentioned earlier and the similar voltage dependence observed in Figure 5 suggest that both kinds of capacitor share a common wear out mechanism that is independent of the cathode material. This is consistent with the hypothesis that wear out occurs at the tantalum-dielectric interface, not the dielectric-cathode interface. Another comment on Figure 5 is in order. At very high percentages of formation voltage, the slope of the curve (the voltage ratio exponent in the voltage acceleration formula) increases, indicating additional acceleration. It is hypothesized that a second wear out mechanism begins to contribute to wear out at test voltages in excess of roughly 65% of formation voltage. Page 7 of 11

8 It is clear from Figure 5 that the polymer parts were tested at higher percentages of formation voltage than were the MnO 2 parts. The data of Figure 6 provide the reason why. Figure 6 displays the initial failures that occurred at 125 o C at the various test voltages for the 25V, 35V, and 50V MnO 2 and polymer capacitors. At a given test voltage, some percentage of a sample of parts does not survive the ramp up of the test voltage. This percentage appears as a data point on the curve related to that test sample. At higher test voltages, a higher percentage of the sample fails during ramp up and vice-versa. Figure 6. Percent of Initial Failures versus Percent of Formation Voltage Applied for 25V, 35V, and 50V Experimental MnO 2 and Polymer Tantalum Capacitors at 125 o C. The test voltages were chosen to be high enough to generate at least some failures in times less than 100 hours, but not so high as to cause all the parts to fail during ramp up. It turns out that the electric field strengths that meet these criteria are lower for the MnO 2 parts (they have thicker dielectric) than the polymer parts even though the ratios of test voltage to rated voltage are generally similar. This means that the cathode material impacts the short-term dielectric strength of the capacitor. This is consistent with the hypothesis that breakdown voltage is governed by the potential barrier at the insulator-semiconductor (oxide-cathode) interface, and that this barrier behaves somewhat differently for MnO 2 parts (MnO 2 is an n-type semiconductor) than for PEDT polymer parts (p-type semiconductor). Also observed in Figure 6 is that the test voltages -- as a percentage of formation voltage -- that cause early failures fall as the dielectric thickness rises. This is true for both cathode materials, and demonstrates that there are limits to the improvement in breakdown voltage that can be achieved by simply making the dielectric thicker. This implies that the road to substantially higher breakdown voltages for high-voltage tantalum capacitors is likely controlled as much by the properties of the chosen cathode material as by dielectric thickness. Page 8 of 11

9 One final graph appears in Figure 7. This graph demonstrates the relative temperature dependence of the initial failures (breakdown voltages) for the 35V MnO 2 and 35V polymer capacitors. It is clear that there is more temperature dependence of breakdown voltage in the MnO 2 capacitors than in the polymer capacitors. This difference in temperature dependence provides additional corroboration that the dielectric strength is governed by the oxide-cathode interface and that this interface has different properties for the different cathode materials. Figure 7. Percent of Initial Failures versus Percent of Formation Voltage Applied at 85 o C, 105 o C, and 125 o C for 10uF, 35V Experimental MnO 2 Tantalum Capacitors and 15uF, 35V Experimental Polymer Tantalum Capacitors. It is interesting to note that while the temperature dependence is very small with no easily discerned positive or negative temperature characteristic for the tantalum polymer capacitors, it is larger with clearly negative temperature coefficient for the MnO 2 capacitors. At this time it is unknown why this is true, but it is speculated that this could be related to the n-type/p-type difference in the semiconductor cathode materials and related differences in the temperature dependence of the concentration and mobility of their respective charge carriers. Summary and Conclusions In previous work, accelerated time-to-failure lifetesting of high voltage (25-50V) tantalum polymer capacitors was performed to determine voltage and temperature acceleration models so that lifetime could be predicted at less stressful conditions in a practical timeframe. The motivation was to assess the reliability of a new capacitor technology when traditional test methods (Weibull grading) proved inadequate. These polymer-cathode capacitors demonstrated excellent projected median life at rated conditions and very good volumetric efficiency. Page 9 of 11

10 In the mean time, significant improvements were made in the manufacture and screening of the corresponding 25-50V MnO 2 -cathode part types, and there was interest in comparing the performance of these improved MnO 2 - cathode parts to the polymer-cathode parts. This motivated an accelerated lifetest investigation to determine the voltage and temperature acceleration models for the improved MnO 2 capacitors. Representative samples were tested at various voltages and temperatures and the resulting time-to-failure data were analyzed using the same techniques as were applied to the polymer-cathode capacitors. The first observation was that the structure and complexity of the time-to-failure distributions for the MnO 2 capacitors were substantially similar to those of the polymer-cathode capacitors. Initial failures, a relatively flat region of declining failure rate, and a distinct wear out mode were present in the failure distributions in response to the highly accelerated test conditions. Only the anti wear out mode was absent, as was expected (no degradation of MnO 2 conductivity was expected at the test conditions employed). The existence of a wear-out mode -- characterized by rapidly increasing failure rate -- was expected, but is contrary to common claims that MnO 2 tantalum capacitors do not have a wear out mechanism. The wear out mechanism for both the polymer-cathode capacitors and MnO 2 -cathode capacitors is thought to be the natural diffusion of oxygen from the dielectric into the tantalum substrate metal. This process leaves behind oxygen vacancies in the nearby dielectric, degrading its insulating properties. The applied voltage is now forced to drop across less good dielectric, progressively increasing the electric field stress. This speeds up the loss of more oxygen and the cycle continues, leading to increasing failure rate over time. This mechanism is accelerated by both temperature and voltage, and is believed to be the dominant failure mechanism at normal application conditions, albeit only after very long time periods at normal stress levels. The voltage and temperature acceleration models for this wear out mechanism were found to be essentially the same for both kinds of tantalum capacitor with a voltage ratio exponent of 13.2 in the power law voltage acceleration formula and an activation energy of about 1.5 ev in the Arrhenius temperature acceleration formula (for 35V devices tested at 125 o C and ~50% of formation voltage). For the 35V MnO 2 capacitors, projected median life of the capacitors is roughly 100,000 years at rated voltage and 85 o C. In absolute terms, the projected median life of the MnO 2 capacitors is longer than the projected median life of the polymer capacitors. But once the result is adjusted to account for the lower electric field stress in the MnO 2 capacitors (because of their thicker dielectric), the results are essentially identical. Attention was then directed toward the initial failure region of the time-to-failure distributions. These capacitors fail because the highly accelerated test voltage overcomes the potential barrier at the dielectric-cathode interface. This is consistent with MIS theory where the insulator-semiconductor interface corresponds to the dielectric-cathode interface. Because these failures occur during the 60s voltage ramp at the start of testing, they provide dielectric strength data at the test temperature for the failed capacitors. It was demonstrated that the initial failure behavior of the MnO 2 capacitors is significantly different from the initial failure behavior of the polymer capacitors. The failures occur at lower electric field stress for the MnO 2 capacitors than the polymer capacitors. Also, the percentage of failures at a given stress level is distinctly temperature dependent for the MnO 2 capacitors while it is not significantly temperature dependent for the polymer capacitors. These differences support the assertion that dielectric strength and its temperature dependence are substantially determined by the choice of cathode material in tantalum capacitors according to MIS theory. For the MnO 2 capacitors the MnO 2 cathode is an n-type semiconductor while for the polymer-cathode capacitors the cathode is a p-type semiconductor. It is thought that this distinction may play some role in the temperature dependence difference between the two cathode materials. Page 10 of 11

11 The MnO 2 tantalum capacitors tested for this paper have much longer median life at rated conditions than is necessary for any practical application. But they have similar percentages of initial failures at similar percentages of rated voltage when comparison is made with the polymer-cathode capacitors. This suggests that MnO 2 capacitors will have excessive lifespan when the dielectric is thick enough to produce breakdown voltages that are competitive with the polymer capacitors. This presents an opportunity for both the user and the designer of MnO 2 capacitors in high-reliability applications. Clearly the MnO 2 capacitors studied here could be used without any voltage de-rating (user decision) under steadystate application conditions without any practical impact on long-term reliability. Alternatively, these capacitors could be made with thinner dielectric to provide more capacitance in the same volume (designer decision) without practical reduction of reliability. But some applications do not provide steady state conditions. These more dynamic applications expose the capacitors to high peak charging currents and occasional voltage transients of significant magnitude (or both). For these applications it is likely a good tradeoff to build in additional dielectric strength at the cost of lower volumetric efficiency. This situation provides manufacturers of MnO 2 capacitors an opportunity to provide different product designs custom-tailored to the nature of the hi-rel application and an opportunity for the user to consider less conservative de-rating guidelines or higher capacitance density for well-behaved circuits. References 1 E. Reed and G. Haddox, Reliability of High Voltage Tantalum Polymer, CARTS USA 2011 Proceedings of the 31 st Symposium for Passive Components, p. 195 (2011). 2 J. Paulsen, E. Reed, and J. Kelly, Reliability of Tantalum Polymer Capacitors, CARTS 04 Proceedings of the 24 th Capacitor and Resistor Technology Symposium, p. 114 (2004). 3 E. Reed, J. Kelly, and J. Paulsen, Reliability of Low-Voltage Tantalum Polymer Capacitors, CARTS USA 2005 Proceedings of the 25 th Symposium for Passive Components, p. 189 (2005). 4 Y. Freeman, W. Harrell, I. Luzinov, B. Holman, and P. Lessner, Electrical Characterization of Tantalum Capacitors with Poly(3,4-ethylenedioxythiophene) Counter Electrodes, Journal of the Electrochemical Society, p. G65 (2009). Page 11 of 11

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