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This x-direction allows a visible contrast image of 3.2 y-direction sectioning
the active area under optical microscope (Fig. 2). With Fig. 4 as a reference, section is now made in
y-direction approaching the hot spot (Fig. 5).
y
z
x
Figure 3: A failed capacitor in an application Figure 5: Optical (dark view) of the sample after
circuit. both x and y-direction sectioning.
Thanks to the unique nature of capacitor, physical 4. Photon Emission Microscope (PEM) Analysis
cross-section parallel to x and y direction does not with Micro-Probing
affect its electric behavior other than reducing its Upon y-direction sectioning, the connection of the
capacitance in proportion to the area being multi-layer electrodes at one end is removed. Each
removed. The sectioned sample is subjected to pair of parallel electrodes can be individually
thermal imaging microscope analysis at the side probed. Micro-probing narrows the leakage down
view. The hot spot location in x-direction is to two specific layers. With the advantage of high
confirmed, and its position in z-direction can also magnification lens in PEM, the hot spot can now
be estimated at the sectioned surface (Fig. 3). be precisely localized in x, y, z dimensions by
alternating between y-direction polishing and
PEM emission acquisition (Fig. 6).
y-direction
5. SEM Examination
Figure 7, 8 are SEM images of the failure site.
There is no sign of physical damage or defect
observed except some contrast between grains.
Unfortunately, the limited resolution of beam spot
size of SEM prevents EDS analysis from
Figure 4b: Optical (dark view) of Figure 4 differentiating any compositional variation in the
showing the contrast of the active area. grains or grain boundaries.
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Figure 10: A transgranular micro-crack observed
at a high leakage site. It is considered the effect of
failure, i.e. electric over stress.
6. Localized Cracks in High Leakage Failure Figure 11: An intergranular micro-crack observed
In the analysis of capacitors that have high leakage at a high leakage site. It is considered the effect of
current (in the range of tens to hundreds mA), high failure, i.e. electric over stress.
contrast spot at the failure site can be readily seen
under dark field view (Fig. 9). SEM imaging 7. STEM and High Resolution EDS Analysis
shows that localized micro-cracks are present at STEM imaging of atomic contrast shows
the failure site, some trans-granular some inter- significant variation between adjacent grains and
granular (Fig. 10, 11). even within a single grain (Fig. 12, 13).
In light of the evidence observed on the low
leakage caps, and the fact that micro-hardness test
conducted by an independent lab shows no
difference in material hardness, fracture toughness
between good and failed parts, even no difference
in various spots within a failed one, these micro-
cracks are considered to be the effect of the
failure,
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Figure 14-17: High concentration of S, Bi, Pb, Sr
and Nb are detected in grains and in certain area
within a grain (spot 7) and grain boundary (spot
Figure 13: Close-up of Figure 12 showing high 5).
contrast in grain boundary (spot 5, 6), and also
within a single grain (spot No. 7). 8. TEM Selected Area Electron Diffraction
It is reported that when BaTiO3 is doped with
When high resolution EDS spectrums are impurities, it can become a semiconductor [1]. In
collected (with reported beam spot <10nm), high order to examine the possibility of crystal structure
content of S and Pb, Bi, Nb, Ag are detected in change, selective area electron diffraction (SAD)
grains and boundaries with localized, concentrated patterns are acquired on the sample in Fig. 9.
spots and/or regions (Fig. 14, 15, 16, 17). Distinguishingly different diffraction patterns are
obtained in the area where STEM/EDS analysis is
performed (Fig. 18, 19).
Although these patterns are not quantitatively
characterized, the most likelihood of these are
tetragonal and cubic centered crystal structures.
The former is ferroelectric and the latter is
paraelectric in nature.
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Result and Discussion: A combination of relatively low sintering
1. The evidences obtained in the current study temperature and uncontrolled contamination in
demonstrate that this type of low leakage in raw materials in certain lot in the capacitor
BaTiO3 capacitor is not caused by observable manufacturing process is considered to be the
physical defect such as fractures, voids, etc. in the most probable root cause of this failure.
ceramic matrix.
Conclusion:
2. Since CCD camera on photon emission A complete failure analysis process flow for low
microscope is designed to detect photons with leakage capacitor is developed. By employing
wavelength around 1010nm, which is mechanical cross-section and emission
approximately the band gap energy of Si (1.1eV). microscopic analysis, precise localization of
Since BaTiO3 is a dielectric material with band failure site is made possible even without any
gap energy of 3.3eV, the fact that PEM can detect observable physical sign. This failure analysis
strong emission signals manifests that narrow gap process is easily applicable to any lab equipped
leakage, i.e. semi-conducting behavior is taking with basic failure analysis instrument.
place in these leaky capacitors.
Acknowledgement:
3. It is known that when the crystal structure of The author would like to express sincere
BaTiO3 undergoes a phase transition from appreciation to Mr. Clifford Schuring, Dr. James
tetragonal to a cubic unit cell, the material will Qu at IR, to Mr. Terry at Material Analysis
change from ferroelectric to paraelectric. Thomas Services for technical discussions. Special thanks
Research Group recently reported that when doped are due to the administrative support from the
with impurities, BaTiO3 can be transferred from organization of Center of Excellence, International
dielectric material into semiconductor, and grain Rectifier, Corp.
boundary region is concluded in control of such
phase transition [4]. Reference
[1] H. Kihsi, Y. Mizuno and H. Chazono, “Base
4. It is well known that being at the state of lowest Metal Electrode Ceramic Capacitors: Past,
free energy, grain boundaries easily gathers Present and Future Perspectives”, AAPPS Bulletin
impurities inside crystal structure. Vol. 14, No.2, April 2004 pp2-16
[2] B.A.Marinkovi, B.D.Stojanovic, VP.Malberti,
5. In light of the above information, and based on M.Ciappa, P.Scacco, A .B.Pavlovic, M.M.Ristic,
the evidences collected in this analysis, a failure “Correlation of Microstructure and Dielectrical
mechanism is proposed for these low leakage Properties of BaTiO3 Sintered from Mechanically
capacitors as follows: Activated Powders”, Materials Structure, Vol. 6,
No. 2, 1999, pp96-99
Localized high concentration of impurities at grain [3] Y.Kim, C.H.Chen, A.Saiki, N. Wakiya,
boundaries and inside certain grains induced K.Shinozaki and N. Mizutani “Effect of Nb and Sr
partial transition of the ferroelectric BaTiO3 into doping on Crystal Structure of Epitaxial BaTiO3
paraelectric and/or exhibiting semiconductor Thin Films on MgO Substrate”, J. of Phys D:
behavior that resulted in failures under bias at Appl. Phys. 35, 2002 pp1499-1503.
assembly final test as well as latent field failures. [4].D.Thomas, “Interfacial States in
Semiconducting BaTiO3”, Thomas Research
Furthermore, the fact that these latent field failures Group
did pass initial test suggests that a redistribution of http://www.chembio.uoguelph.ca/thomas/batio3_r
impurities inside the BaTiO3 matrix has taken esearch.html
place under the influence of electric field. [5]A.R. West, “Solid State Chemistry and Its
Statistics shows that most field failures occurred in Application”, published by John Wiley and Sons,
regions with climate of high temperature. Hence 1987, pp540-548.
temperature plays an important role in the
redistribution of the impurities, i.e. it acts as a
driving force for the diffusion of impurities along
grain boundaries.
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