Page 676 1995 IEEE 5th International Conference on

Conduction and Breakdown in Solid Dielectrics

ELECTRON MICROSCOPY OF WATER TREES IN XLPE

R.H.Olley, A.S.Vaughan, D.C.Bassett, S.M.Moody and V.A.A.Banks.

INTRODUCTION

Since the first observations of water trees in the 1960s, this phenomenon has attracted extensive
study; see for example the reviews by Shaw and Shaw [l] and Nunes and Shaw [2]. Although it
is accepted that water trees develop in the presence of polar solvents, from sites of high and
divergent stress, the details of their structure and the processes involved in their initiation and
growth are still unclear. In this communication we report on results obtained using a novel
technique developed by Olley [3], which is equally applicable to the low resolution (-lpm)
optical examination of water trees, detailed studies of tree microstructure in the scanning electron
microscope (SEM) and also to high resolution imaging in the transmission electron microscope
(TEM). Specifically, this paper s e a out to illustrate the range of water tree structures observed in
medium voltage cable insulation, and to describe how these are organised intemally.

EXPERIMENTAL

All the materials examined in this study were derived from triple extruded 11 kV cables made using
different grades of crosslinked, low density polyethylene (XLPE) insulation; the samples are
designated A to D. Cable specimens containing reamed holes were first aged for 3000hrs in
grounded water baths held at 70°C at an electrical stress of 6kVmm-'. The technique used for
subsequent structural study was based upon permanganic etching, Olley and Bassett [4], and since
technical details are provided elsewhere [ 3 ] .the procedure used to delineate the water trees is only
outlined below. Samples were initially prepared by infiltrating the tree channels with a commercial
low viscosity, UV-curable resin. After infiltration, the resin was polymerized in situ by exposure
to UV radiation, so fixing the structure in place. The water trees were then revealed by
microtoming and etching with a permanganic reagent that was specifically designed both to remove
the cured resin and to develop relief in the surrounding XLPE. For optical microscopy and SEM,
etched surfaces were simply sputter coated with gold before being examined. Where TEM data
were required, a conventional 2-stage procedure was used to produce a replica, Willison and Rowe
[W.

R.H.Olley, A.S.Vaughan and D.C.Bassett; J.J.Thomson Physical Laboratory, University of Reading,

Reading, RG6 2AF, UK.
S.M.Moody; Supertension Cables, Power Cable Systems, BICC Cables Ltd, Church Manorway,
Erith, Kent, DA8 lHS, UK.
V.A.A.Banks; Distribution Cables, Power Cable Systems, BICC Cables Ltd, Wrexham, Clwyd,
LL13 9PH, UK.

0-7803-2040-9195B4.00 0 1995 IEEE

 Page 1577

RESULTS

Figures 1 and 2 show an optical image of a portion of a water tree in sample A, together with an
SEM micrograph of the same tree; comparison of these 2 micrographs reveals good agreement
between the two techniques (the microtome knife mark is arrowed in each figure to aid
comparison). From figure 2, it is evident that this tree contains radiating units, which are clearly
visible at the periphery of the structure. Towards the centre of this micrograph, the overall
appearance is rather different. A highly voided region is arrowed and whilst this may be associated
with an increased density of damage at the core of the structure, orientational effects will also
contribute, since the local direction of tree growth will influence the appearance. of the structure.
Figure 3 shows a similar tree structure, which developed in sample D. At this magnification a
radiating texture can be seen, which is again made up of discrete elongated units. In this case, the
principal direction of tree growth lies close to the etched plane, and this factor contributes greatly
to the overall appearance of the structure. Although both the above trees have a rather congested
structure, both micrographs, nevertheless, demonstrate that these water trees are composedl of
extended units that tend to grow outwards from the base of the reamed hole.

A rather different water tree structure is shown in figure 4. Here the tree, which developed in
sample C, exhibits a very fine scale texture in which few clear structural units are evident.
Comparison with figure 3 reveals that where continuous elongated structures could be identified in
sample D, in figure 4,the bright radiating streaks appear to contain a sequence of dark voids. This
is particularly evident when the structure is viewed at higher magnifications. Although connectivity
above or below the etched plane, channels containing a craze-like texture or profuse branchiing
cannot be discounted, the texture of this water tree does seem to be significantly different from that
shown in figures 2 and 3. It is therefore unclear whether the constituent units within water trees

Figure 1: Reflected light optical micrograph FiEure 2: SEM micrograph of the water treed
of a portion of a water tree in sample A. region previously shown in figure 1.
Page 678

Figure 3: SEM micrograph showing a portion Figure 4: SEM micrograph showing the fine
of a water tree in sample D; continuous scale texture of water trees in sample C.
elongated structures are evident.

in sample C are connected. This notion of different degrees of void connectivity in different
materials was previously proposed by de Bellet [6] on the basis of their TEM observations,
and seems very reasonable in view of the results presented here.

The water trees discussed thus far are broadly similar in that the defect density within the envelope
of the tree is high in all cases. However, water trees grown in sample B are very different. Figure
5 contains an SEM image showing a portion of a tree grown in this material and, from this, it is
clear that such water trees are made up of relatively few coarse units that are widely spaced from
one another. In no region is there any evidence of the congested appearance that is so evident in
figures 2 to 4. In addition, figure 5 is also notable for the voided appearance of the matrix beyond
the limits of the tree itself; all the SEM samples shown were prepared in a similar manner, yet this
is the only specimen that revealed evidence of such voiding. As discussed by Blacker [7], the
matrix morphology in this cable well away from the treed region shows no evidence of such
extensive voids, and thus it would seem that, in this material, matrix damage extends many tens
of microns beyond the apparent limits of the tree itself. This is consistent with the work of
Shinozaki a [8] who reported an accumulation of water at the tips of water trees and, in sample
B, it would appear that this has condensed to form droplets, rather than being present in a more
disperse form. It is also interesting to note that these dark features are all approximately circular
in shape and exhibit a size distribution that, statistically, is not inconsistent with a plane intersecting
with a 3-D distribution of -1 pm diameter spheres.

Simultaneous examination of water tree and matrix microstructures provides additional information
concerning the interactions that occur during growth; figure 6 contains a TEM image of the edge
Figure 5: SEM micrograph showing the coarse Figure 6: TEM micrograph in which cracks can
structure of water trees in sample B. be seen emanating from the tip of a water tree
channel: sample B.

of a water tree, again in sample B. This micrograph illustrates the high contrast and lack of
structural detail that is always seen within tree channels but, more importantly, provides evidence
conceming the mechanism by which water tree growth occurs.

Many workers (see for example de Bellet e [6] and Golz [9])have suggested that water trees
develop through the condensation of water molecules within amorphous regions: the subsequent
growth of the tree is determined by both the local electric field and the local lamellar orientation.
Figure 6, which shows the extreme tip of a water tree channel within the etched plane, contains a
number of important features which relate to the mechanism by which water trees develop. First
consider the line joining the points A and B. Initially, there is well defined lamellar texture made
up of extensive lamellae, separated by finer scale units. A darker region is then encountered where
the texture is ill-defined, followed by a generally bright region. From the known shadow direction,
this variation in contrast implies that the point B is situated within a channel below the plane of
the etched surface. This means of deducing information conceming the third diimension from the
shadow contrast has a great bearing on the interpretation of the three high contrast regions
(arrowed) that emanate from the tip of the tree channel itself. Although the significance of these
features cannot be deduced unambiguously, the shadow contrast seen on proceeding along the line
from C to D indicates a rough surface, in which the anowed features correspond to cracks in the
matrix around the channel. These cracks, which clearly follow the local lamellar orientation,
therefore provide evidence in support of a mechanism of tree growth based upon interlaniellar
failure, illustrate the means by which morphology can influence the process and are consistent with
the reported correlations between water tree suppression and resistance to environmental stress
cracking, de Bellet [6].
CONCLUSIONS

The infiltratiodpermanganic etching technique employed. allows water trees to be examined using
a variety of optical and electron imaging techniques. In addition to the gross structure of the tree,
examination of the water treed regions by TEM enables both the tree itself and the surrounding
matrix morphology to be examined simultaneously and in unprecedented detail. The technique has
revealed a wide variety of tree structures, ranging from trees composed of a small number of coarse
radiating units, through a congested array of channels, to structures where the envelope of the tree
appeared to be filled with small voids. Thus, it is proposed that whilst some water trees are made
up of radiating channels, others may contain discrete voids. Only in one material was it possible
to detect voiding beyond the envelope of the tree.

On the basis of the observations of the tree and matrix microstructures it is proposed that water
channels tend to grow between the lamellar units, i n line with previous proposals. However, whilst
it is believed that morphological factors do play an appreciable part in the propagation of water
trees, for such a wide range of tree structures to develop in materials which are morphologically
similar, Blacker [7], clearly demonstrates that other factors are also of great importance.

ACKNOWLEDGEMENTS

The authors would like to thank BICC Cables Ltd for supporting the work described above and for
giving permission for the results to be published.

REFERENCES

2.
1. Nunes, S.L. and Shaw, M.T., 1980, IEEE Trans. Electr. Insul., U,437-450
Shaw, M.T. and Shaw, S.H., 1984. IEEE Trans. Electr. Insul., U , 419-452
3. Olley, R.H., Bassett, D.C., Vaughan, A.S., Banks. V.A.A., McAllister, P.B. and Moody,
S.M., 1992, J. Mater. Sci., 27, 5192-5198
4. Olley, R.H. and Bassett, D.C., 1982, Polvm. Commun..a, 1707-1710
5. Willison, J.H.M. and Rowe, A.J., 1980, "Practical Methods in Electron Microscopy", vol.
8, "Replica, Shadowing and Freeze-Etching Techniques" ed. A. M. Glauert, North Holland,
Amsterdam, Holland.
6. de Bellet, J.J.. Matey, G., Rose, L.J.. Rose, V., Filippini. J.C., Poggi, Y. and Raharimalala,
V., 1987, IEEE Trans. Electr. Insul., EI-22, 21 1-217
I. Blacker, R.S., Vaughan, A S . , Bassett, D.C. and Moody, S.M. to be published.
8. Shinozaki, D.M., Cheng, P.C., Haridoss, S., Mitchell. R. and Fenster, A., 1991, J. Mater.
Sci., 26, 6151-6160
9. Golz, W., 1985, Colloid & Polym. Sci.. 263, 286-292