Proceedings of the 1999 Workshop on RF Superconductivity, La Fonda Hotel, Santa Fe, New Mexico, USA

MIRCO-STRUCTURES OF RF SURFACES IN THE

ELECTRON-BEAM-WELD REGIONS OF NIOBIUM

R.L. Gengy z , J. Knobloch, H. Padamsee

Laboratory of Nuclear Studies, Cornell University, Ithaca, NY 14853

Abstract tion, the so called high-field-Q-drop [2]. Recent experi-

ments show that the same cavity would have quite differ-
Micro-structures of RF surfaces in the electron-beam-weld
ent performance with different surface treatments [3]. It is
(EBW) regions of niobium samples were studied. These
therefore of interest to have detailed studies on RF surfaces
surfaces were polished with different techniques,namely
following various preparations.
buffered chemical polish (1:1:2 BCP) and electrolytic pol-
ish (EP). It was found that there are three distinctively dif-
ferent regions near the EBW, characterized by different 2 SAMPLES AND PREPARATIONS
grain sizes, shapes, and orientations. Strikingly, we found Two EBW samples were studied, one of which, denoted
grain boundaries within the EBW are nicely lined up so as S3C1-3-EQUATOR, is cut from the equator of an well
that they form an angle of about 60 degree with respect to etched S-band cavity and the other is a flat sample, denoted
the weld seam. Upon being polished with BCP, these grain as TWC-155E, for weld testing with typical parameters.
boundaries evolve into micro-steps with sharp edges, due The raw material of these two samples came from the same
to preferential etching of different crystallographic planes. batch (by Teledyne Wah Chang) with a starting RRR of 300
There is evidence that the step height increases up to pos- and a starting thickness of about 1.6 mm.
sibly more than 30 microns with repeated chemical pol- The two EBW samples were welded with the so called
ish. In contrast to the result with BCP, dimensions of sur- “Rhombic raster weld” technique [4] with a beam volt-
face irregularities were reduced with EP and sharp edges age of 50kV. The beam current and beam traveling speed
were rounded off.These observations have important impli- (or cavity rotational speed) are 22 mA and 30 cm/min
cations in explanations of the high-field-Q-drop of niobium for the S3C1-3-EQUATOR sample, and 30 mA and
superconducting cavities. 45 cm/min for the TWC-155E sample respectively. The
apparent width of weld seams, as viewed with naked
1 INTRODUCTION eyes, is about 4-5 mm. Prior to the study described in
this paper, the S3C1-3-EQUATOR sample has been well
The performance of a superconducting cavity used in mod- etched (> 100 m) with 1:1:2 BCP at 15  C; while the
ern accelerators is intimately connected with the condition TWC-155E sample was not etched at all.
of its RF surface. For this reason, different surface prepara-
In this study, samples were etched by 1:1:2 BCP (see
tion techniques have been developed to get an ideal surface.
[1] for detailed information about the mixture), and/or EP
A newly fabricated bulk niobium cavity is usually etched
(with a mixture of HF(49% wt.) and H2 SO4 (96% wt.) in a
either by chemical polish (1:1:2 BCP) or by electrolytic
volume ratio of 10:105). The temperature of the acid was
polish (EP) [1].
in the range of 11 - 16  C for BCP and 25 - 34  C for EP
In case of cavities made of bulk niobium, different cav- respectively. For BCP, the acid was agitated manually at
ity parts are welded together with electron-beam-welding an interval of about 5 minutes; while for EP, the electrolyte
technique. Because of large amount of heat deposition, the was agitated continuously yet gently with a spin bar driven
electron-beam-weld (EBW) region is expected to distin- by a magnetic stirrer. In case of EP, the anode-cathode volt-
guish itself from a virgin niobium region. The significance age was regulated to be constantly at 12 V. With this config-
to differentiate EBW regions from virgin niobium regions uration, the anode current was almost constant with a slow
is underlined by the fact that these regions are subjected to increase as a result of temperature rise with time, due to
either peak electric fields (iris regions) or peak magnetic heat generated by the flowing current. The anode current
fields (equator regions) for modern niobium cavities with density ranged from 25 - 30 mA/cm2 . The average surface
elliptical shapes. removal rate is 1m/min for BCP and 0.3 m/min for EP
In this paper, micro-structures of RF surfaces near the respectively.
EBW regions of different niobium samples are studied.
This work is motivated by the experimental studies of a
newly observed fundamental cavity performance limita- 3 THREE REGIONS NEAR AN EBW
 Work supported by the National Science Foundation. After enough surface removal by etching, three regions can
y on leave from IHIP, Peking University, Beijing 100871, PRC. be easily distinguished near an EBW, namely the weld re-
z Email: [email protected] gion, the heat-affected region and the non-affected region.

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(a)

Figure 1: The SEM photo of the weld and heat-affected

region of the sample TWC-155E after a surface removal of
177m by BCP. The length of the scale bar in the figure is
1mm.

Grains in different regions have different sizes, shapes and

orientations. Fig. 1 shows the weld surface of the sample
TWC-155E after a surface removal of 117 m by BCP. The
middle part of the photo shows the weld region and the re- (b)
gion next to the weld shows the heat-affected region. In the
weld region, Grain boundaries are lined up in a way that
they form an angle of about 60 with respect to the weld
joint line. Grains have elongated dimensions, comparable
to the half width of the weld, in the lining-up direction.
In the heat-affected region, grains have smaller dimensions
compared to that in the weld region and take random ori-
entations. The overall width of the weld and heat-affected
region is 12 mm.
A non-affected region is one that is not affected by the
heat deposition during electron-beam welding. Therefore it
bears the same appearance as that of a virgin niobium (see (c)
Fig. 6(a)). Grains in this region are even smaller than that
in the heat-affected region and their orientations are highly
random.

4 EVOLUTION OF WELD SURFACES

WITH REPEATED ETCHING
4.1 Weld surfaces after repeated BCP
The sample TWC-155E was etched by BCP repeatedly in
a step by step manner. Fig. 21 illustrates the evolution of
its weld surface with an increased amount of surface re-
moval. Fig. 2(a) shows the virgin surface, featuring me- (d)
chanical scratches and weld ripples. Grain boundaries are
Figure 2: The weld surface of the sample TWC-155E with
also clearly visible. The left border of the photo approxi-
different surface removal by BCP. Virgin surface (a). After
mately coincides with the joint line of the weld. Note the
a surface removal of 30m (b); 117m (c); 250m (d). The
grain boundary crossing over Fig. 2(a) from the lower left
left border of the photos coincides with the weld joint line.
corner to the upper right corner has already shown a step
nature at this stage. After a 30 m surface removal by BCP,
1 All the photos in this section were taken with an optical microscope. scratches are not effectively removed. In addition, many
Each photo covers an area of 1770 m wide by 1370 m high. circular defects with various dimensions emerge, as shown

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 Proceedings of the 1999 Workshop on RF Superconductivity, La Fonda Hotel, Santa Fe, New Mexico, USA

in Fig. 2(b). After a surface removal of 117m, surface

scratches are totally abated, as shown in Fig. 2(c). How-
ever, circular defects, especially those starting with larger
dimensions, still sit on the surface. This suggests that these
circular defects are actually spherical ones embedded in the
surface layer of the weld region. Only after a surface re-
moval of 250m are circular defects gone (see Fig. 2(d)).
Although it is scratch free and circular (or spherical, to
be accurate) defect free after a surface removal of 250 m,
the RF surface of the weld region is far less than perfect at
this stage. As can be seen from Fig. 2(d), the step crossing
over from the lower left corner to the upper right corner of (a)
the photo has grown into a much bigger one, with a very
sharp edge, due to preferential etching of different crystal-
lographic planes. One should also note that the emerging
bean-shaped defect, 310m long by 50 m wide, sitting
near the lower right corner in Fig. 2(c) has evolved into
a much bigger defect, 850 m long by 250 m wide in
Fig. 2(d) as a result of an extra 133 m etching.

4.2 Weld surfaces after BCP followed by

repeated EP
After having received a surface removal of 117 m, half of
the sample TWC-155E was etched by EP in a step by step (b)
manner.
Fig. 3 shows the evolution of its weld surface with an
increased amount of surface removal by EP. Note the tie-
shaped feature dominating the center of the photo is a
plateau with respect to the area surrounding it. Again, the
left border of the photo approximately coincides with the
joint line of the weld.
It turns out that EP is very effective in removing spher-
ical defects. As can be seen by comparing Fig. 3(a) and
Fig. 3(b), an etching of 26 m by EP suffices to remove
those spherical defects.
Another important effect of EP lies in the fact that those (c)
sharp edges left behind by BCP are rounded off to a large
extent, as can be seen from the evolution of the step edge Figure 3: The weld surface of the sample TWC-155E after
of the plateau. There is also evidence that the height of the BCP followed by repeated EP. After a surface removal of
plateau is reduced by EP. The height of the plateau was 117m by BCP (a). After an extra removal of 26m (b);
roughly measured by adjusting the distance between the 90m (c) by EP. The left border of the photos coincides
object and the lens to get the best focus when looking at with the weld joint line. The tie-shaped feature dominat-
different areas. Qualitatively speaking, more surface re- ing the photo center is a plateau with respect to the area
moval by EP, more pronounced rounding-off effect on step surrounding it.
edges and more step height reduction.

4.3 Weld surfaces after EP followed by lower side in the picture. The configuration of the other two
repeated BCP linear features is actually undercut, which is a frequently
observed feature for a weld surface etched by BCP.
In this study, the sample S3C1-3-EQUATOR was first
etched by EP until a surface removal of 100m was As can be seen from Fig. 4, the smooth RF surface is
reached. The sample was then etched by BCP in a step by easily destroyed by a light BCP. An extra etching of 12 m
step manner. Fig. 4 illustrates the evolution of its weld sur- by BCP is sufficient to re-establish sharp edges, although
face with an increased amount of surface removal by BCP. the step height is not that great. Again increasing of the
The linear feature starting from the center of the photo to step height with the amount of surface removal by BCP is
right is a going-down step if walking from the upper to the demonstrated.

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(a)

(a)

(b)

(b)

Figure 5: The RF surface of the weld and heat-affected

region of the sample TWC-155E after a surface removal of
117 m by BCP (a), and after an extra removal of 90 m
by EP. The length of scale bars in the photos is 1mm.

(c) TWC-155E after a surface removal of 117 m by BCP and

after an extra removal of 90 m by EP, respectively.
Figure 4: The weld surface of the sample S3C1-3- As can be seen in Fig. 5(a), there are a number of bright
EQUATOR after EP followed by repeated BCP. After a sur- features, both in the weld and heat-affected region after be-
face removal of 100m by EP (a). After an extra removal ing well etched by BCP. In contrast, after an extra etching
of 12m (b); 44m (c) by BCP. The linear feature start- by EP, both the number of bright features and their bright-
ing from the center to right is a going-down step if walking ness are greatly reduced. This suggests that [5] the number
from the upper to the lower side in the picture. of sharp edges and their sharpness are both reduced by EP.
However, one should bear in mind that not all the edges are
perfectly rounded off with the extra etching by EP, which
5 EP VS BCP IN A LARGER PICTURE means even further EP is needed to obtain an ideal weld
The effects of repeated BCP and EP on weld regions have surface.
been discussed in previous sections. In this section, RF sur-
faces of all the three regions after being well etched by BCP 5.2 The non-affected region
are comparatively presented with those being well etched
by EP. Fig. 6 shows the difference between the RF surface of a
non-affected region after a surface removal of 117 m by
BCP and that after a further removal of 90 m by EP. As
5.1 The weld and heat-affected region
can be seen from Fig. 6(a) the surface of the non-affected
Fig. 5(a) and (b) show low magnification SEM photos of region is rather rough after the etching by BCP, whereas it
the weld region and heat-affected region of the sample is significantly smoothed out by the further EP, as shown in

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6.1 Step height

Typical surface profiles of RF surfaces in different regions
being etched by different methods are shown in Fig. 7.
Fig. 7(a) and (b) show profiles of the weld and non-affected

Step Height (micron)

-5

-10

-15

-20
(a) 0 500 1000 1500 2000 2500 3000 3500 4000 4500 5000
Horizontal Scan (micron)

(a)
6

4
2

Step Height (micron)

0

-2

-4
-6

-8
-10
0 50 100 150 200 250 300 350 400 450 500
Horizontal Scan (micron)

(b)
(b) 10

8
Figure 6: The RF surface of the non-affected region of the
Step Height (micron)

sample TWC-155E after a surface removal of 117 m by

6

BCP (a) and after an extra 90 m removal by EP. The length

4

of scale bars in the photos is 100 m.

2

-2

Fig. 6(b). -4
0 500 1000 1500 2000 2500 3000 3500 4000 4500 5000
Horizontal Scan (micron)

6 SURFACE PROFILES (c)

As shown in previous sections, RF surfaces being well 2

etched by BCP are characterized by steps with sharp edges 1.5

1
in the weld and the heat-affected region and a high rough-
Step Height (micron)

0.5
ness in the non-affected region.
0
In order to have a better understanding about these sur-
-0.5
face irregularities, data in the vertical dimension are highly
-1
desired. Although the height of a particular step in the weld
-1.5
region can be measured with an SEM by tilting the sample,
-2
statistical data about the steps in the weld region and the 0 50 100 150 200 250 300 350 400 450 500
Horizontal Scan (micron)
roughness of the surface in a non-affected region can not
be yielded effectively in this manner. Yet these data are (d)
crucial in determining the distribution function of the field
enhancement factor discussed in [6]. For this reason, the Figure 7: Surface profiles of the sample TWC-155E. The
surfaces of the samples were measured with a surface pro- weld (a) and non-affected region (b) after a surface removal
filer. The stylus of the profiler used in this study (Alpha- of 117 m by BCP. The weld (c) and non-affected region
step-500 by Tencor) has a curvature radius of 5 m and a (d) after an extra 90 m removal by EP. Note the difference
shank angle of 60  . in horizontal scale for the weld and non-affected region.

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region of the sample TWC-155E after a surface removal of 16

117 m by BCP. Fig. 7(c) and (d) show profiles of the weld BCP 117 micron

and non-affected region after a surface removal of 117 m

14

by BCP followed by an extra 90 m surface removal by EP. 12

The rounding-off effect of step edges by EP is borne out 10

again by the surface profile measurement, which is inde-

Counts
8
pendent to the microscopic photography described in pre-
vious sections. Unfortunately, limited by the curvature ra- 6

dius of the stylus, curvature radius of step edges could not 4

be resolved. An approach was developed in [6] to gauge the
2
curvature radius of steps and an upper limit was outlined.
Despite the difficulty in curvature radius measurement, 0
0 5 10 15 20 25 30 35 40
the step height can be accurately measured with the sty- Step Height (micron)
lus used in this study. Measurements with the sample
(a)
TWC-155E after repeated etching by EP reveal a gradual
reduction of the step height in the weld and heat-affected 16
BCP 250 micron
region and a vigorous roughness reduction in the non- 14
affected region. In contrast, the step height in the weld
12
region increase significantly with repeated BCP (see the
RMS step height in the following section). No step height 10
saturation is seen up to a 250 m surface removal by BCP
Counts
8
in the weld region.
6

4
6.2 Step height statistics
2
In order to compare the surface characteristics after differ-
0
ent surface treatments, statistical data are needed due to the 0 5 10 15 20 25 30 35 40
fact that large number of steps with diverse configurations Step Height (micron)
are involved. Here the distribution of step height is em-
(b)
phasized because of its close relationship with the distri-
35
bution function of the magnetic field enhancement factor
BCP 117 micron + EP 90 micron
discussed in [6]. The RMS step height is cited only for a 30
general comparison purpose.
Fig. 8 depicts histograms of step height in the weld re- 25

gion of the sample TWC-155E after different surface treat- 20

Counts

ment. Here the effects of different polishing techniques are

clearly illustrated. More surface etching by BCP greatly in- 15

creases the number of larger steps. The highest registered 10

step height is even close to 40 m after a surface removal of
250 m ( see Fig. 8(b) ). In contrast, the number of larger 5
steps is significantly reduced with surface etching by EP.
Most steps have a height of less than 10 m after an extra
0
0 5 10 15 20 25 30 35 40
surface removal of 90 m following an original removal of Step Height (micron)

117 m by BCP ( see Fig. 8(c) ). (c)

Fig. 9 depicts histograms of step height in the non-
affected region of the sample TWC-155E after different Figure 8: Histograms of step height in the weld region of
surface treatments. Unlike in the weld region, a step height the sample TWC-155E. After a surface removal of 117 m
saturation is observed here in the non-affected region. The (a). After a surface removal of 117 m by BCP followed
maximum and the RMS step height are nearly the same still by an extra 133 m removal by BCP (b). After a sur-
with an etching of 117 m and 250 m by BCP. Again, EP face removal of 117 m by BCP followed by an extra 90
plays an important role in reducing the surface roughness m removal by EP (c).
in the non-affected region.
From these statistical data, one can calculate the root
mean square step height, which can be used as a general
gauge of the surface irregularity. Table 1 lists the root mean ments. Table 2 lists the root mean square step height and
square step height and the maximum height in the weld re- the maximum height in the non-affected region of the sam-
gion of the sample TWC-155E after different surface treat- ple TWC-155E after different surface treatments.

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14
BCP 117 micron
Table 1: Statistics of step height in the weld region of the
12 sample TWC-155E
surface removal RMS [m] Max. [m]
10 117 m BCP 8.8 17.8
8 250 m BCP 16.2 36.8
117 m BCP + 90 m EP
Counts

5.5 13
6

4
Table 2: Statistics of step height in the non-affected region
2 of the sample TWC-155E
surface removal RMS [m] Max. [m]
117 m BCP
0
0 2 4 6 8 10 12 14 4.8 11.4
Step Height (micron) 250 m BCP 4.3 12.6
(a) 117 m BCP + 90 m EP 2.2 6.7
45
BCP 250 micron
40 ferent from that of the bulk due to either morphological fac-
35 tors or compositional factors. Recent studies have shown
30 that a cavity etched by BCP may suffer from high-field Q
25
drop. whereas, after certain amount of further etching by
Counts

EP, the Q drop could be removed and the quench field could
20
also be raised [3]. Among others, a model based on the
15 magnetic field enhancement has been developed to explain
10 this phenomenon [6]. Studies presented in this paper have
5 important implications in the context of the high-field Q
0
drop of a superconducting cavity.
0 2 4 6 8 10 12 14
Step Height (micron)
7.1 Magnetic field enhancement
(b)
Magnetic field can be enhanced locally on the surface of the
35
BCP 117 micron + EP 90 micron corner of a step. The dependence of the enhancement fac-
30 tor on the curvature radius of the corner of a step has been
dealt with in great detail in [6]. Preliminary simulations
25
in a 3-D fashion with the code MAFIA [9] suggest that the
20 field enhancement factor is also a strong function of the ori-
Counts

entation of a step and its aspet ratio. The enhancement is

15
maximized if the step edge is oriented to be perpendicular
10 to the magnetic field lines, whereas the enhancement is triv-
ial if the step edge is oriented to be parallel to the magnetic
5 field lines. The magnetic field enhancement factor was also
0
found to be proportional to the aspect ratio of the step. Ba-
0 2 4 6 8 10 12 14 sically, a longer or higher step will result in a stronger mag-
Step Height (micron)
netic field enhancement factor. In this study, we found most
(c) steps in the weld region have a elongated dimension in the
direction of about 60  away from the joint line. Magnetic
Figure 9: Histograms of step height in the non-affected re- field lines of the working mode in an elliptical supercon-
gion of the sample TWC-155E. After a surface removal of ducting cavity is unfortunately parallel to the joint line. As
117 m by BCP (a); 250 m (b). After a surface removal a result, steps in the weld region are more perpendicular
of 117 m by BCP followed by an extra 90 m removal by than parallel to the magnetic field lines. For these reasons
EP (c). (both orientational and dimensional), a stronger magnetic
field enhancement is expected in the weld region compared
to in the other regions.
7 DISCUSSIONS
7.2 Linearity of the step
RF surfaces of niobium experience substantial changes on
the microscopic scale over the course of surface polishing. Step edges on the RF surface of a niobium can be viewed as
As a result, the surface may manifest some properties dif- some kind of defects in case that the local surface is driven

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into normal conducting due to magnetic field enhancement. mensions in the lining-up direction, as a result their bound-
Theoretical work regarding the relationship between the aries are highly linear.
breakdown field and the geometry of a defect has shown The step edge is significantly rounded off and step height
that linear defects are more vulnerable to thermal instabili- is appreciably reduced with extra surface etching by EP. A
ties compared with circular ones [10]. As can be seen from surface removal of more than 150 m is needed to smooth
Fig. 1, steps in the weld region of a niobium being well out the weld region of a niobium having been previously
etched by BCP have elongated dimension in the direction well etched by BCP. Reversely, a smooth surface obtained
of about 60  away from the weld joint line, and hence by heavy EP can be easily destroyed by further BCP, even
they are highly linear. As a result, a superconducting cav- as light as a surface removal of 12 m.
ity will be more likely to quench in the EBW region than in
the other regions (here we limit ourselves to a cavity work- 9 REFERENCES
ing in the high gradient regime, > 20 MV/m, assuming it
is free from thermal breakdown and field emission). This [1] H. Padamsee, J. Knobloch, and T. Hays, RF superconduc-
tivity for accelerators, Chapter 6, John Wiley & Sons, Inc.,
claim goes even stronger considering the fact that the mag-
1998.
netic field enhancement factor is higher in the EBW region,
as discussed in previous section. [2] H. Safa, Proc. of the 8th workshop on superconductivity,
Abano Terme (Padova), Italy, 1997, p814.
[3] E. Kako et. al., Proc. of the 1999 Particle Accelerator Con-
7.3 How much etching is needed ference, New York, USA, 1999, p432.
It has been established that a surface removal of more than [4] J. Kirchgessner, Proc. of the 4t h Workshop on RF Supercon-
100 m is needed to reach an ideal accelerating gradient ductivity, Argonne National Lab., Argonne, IL, USA, 1998,
[7][8]. In this study, we found the RF surface in the weld p533.
region is dominated by circular defects until a surface re- [5] These SEM photos were taken in the secondary electron
moval of about 120 m was reached. One could argue that mode with the secondary electron detector located over the
there may be some correlation between these circular de- top of the sample. The sample was titled 80 with respect
fects and cavity performance at gradients < 20 MV/m. to the ground level. Photos presented in the paper have been
More surface etching by BCP is helpful in eliminating converted with tilt correction taken into account. In this con-
these circular defects and pushing the gradient to higher figuration, a bright feature in the photo represents a step
levels in the < 20MV/m regime. However, aggresive sur- facing towards the detector as a result of the combination
face etching by BCP beyond 150 m may be unfavorable, of the emission contrast and detection contrast. Due to the
surface sensitive nature of secondary electron emission, the
as it will trigger the high-field Q drop when the cavity
brightness of a step edge can be in a way translated into its
works at higher gradients ( > 20 MV/m ). Because the step sharpness.
height will increase with more etching by BCP and a higher
[6] J. Knobloch, R.L. Geng, M. Liepe, H. Padamsee, these pro-
field enhancement is resulted. For this reason, we suggest
ceedings, TUA004.
an aggressive etching by BCP of more than 150 m surface
removal should be cautioned. [7] P. Kneisel, Proc. of the 8th workshop on superconductivity,
Abano Terme (Padova), Italy, 1997, p830.
Basically surface etching by EP will round off step edges
and reduce the step height on a niobium surface. Studies [8] K. Saito et. al., Proc. of the 8th workshop on superconduc-
presented in this paper show that even after a surface re- tivity, Abano Terme (Padova), Italy, 1997, p795.
moval of 90 m by EP is reached, the step height is still [9] A step-loaded rectangular cavity, big enough compared with
rather high, 10 m, in the weld region of a surface pre- the dimension of the step, was used to simulate the magnetic
viously well etched by BCP. It is therefore expected that field enhancement effect with different step orientations.
more surface removal, presumably more than 150 m, is [10] N. A. Buznikov and A. A. Pukhov, Supercond. Sci. Technol.,
needed to smooth out a weld surface having received sig- 11(1998), P1201-1208.
nificant etching by BCP.

8 CONCLUSIONS
The RF surface in the EBW region of niobium after suffi-
cient etching by BCP is characterized by micro-steps with
sharp edges near grain boundaries. The step height in-
creases with repeated etching by BCP and can be as high
as more than 30 m. No step height saturation in the weld
region was seen up to a surface removal of 250 m.
The steps in the weld region are lined up in a way that
they form an angle of about 60  with respect to the weld
joint line. The grains in the weld region have elongated di-

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