Automatic Electropolisher for Copper

D. A. Lindholm

Citation: Review of Scientific Instruments 40, 1105 (1969); doi: 10.1063/1.1684165

View online: http://dx.doi.org/10.1063/1.1684165
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 NOTES 1105

transmission depends largely on the properties of the
incoming beam. The quadrupole instrument requires
lower ion energies to achieve adequate resolution and the
monopole instrument requires a beam which is better
collimated and less divergent to achieve adequate sensi-
tivity. As such, it is somewhat unfair to compare the
instruments on the basis of the same incoming beam.
Identical sensitivities are quoted for both instruments
under optimum operating conditions; the General Electric
monopole 600 mass spectrometer and the EAI quadrupole
250A residual gas analyzer have a claimed sensitivity of
about 100 A/Torr N 2.
However, on the basis of the theoretical considerations,
it was assumed that the monopole sensitivity could be
increased by deflecting the ion beam away from the V-
electrode by means of a weak external magnetic field
normal to the axis of the monopole. The direction of this
field should be such that the beam is deflected both
away from the apex of the V-electrode and towards the
center of the rod electrode. It has been found experi-
mentally that the imposition of such a magnetic field in-
creases the peak heights by a factor of 5 to 10. This result
might be questioned since the imposed field could have
increased the output of the Nier type ion source. The
direction of the field is parallel to the electron beam which
prevents its spread thus improving the ion source output.
In this case, a field in the opposite direction should have
the same effect on the ion source. Actually, the peak.
heights were observed to decrease by about an order of
magnitude. This indicates clearly that the observed effect
was attributable primarily to the ion beam deflection
where it has to be expected that a deflection towards the
V-electrode should reduce the sensitivity. A bar magnet
was located near the entrance aperture of the monopole
instrument at a distance of approximately 11.4 cm from
the axis. The field strength at the entrance aperture was
approximately 10 G and was observed to diminish gradu-
ally towards the exit aperture. The ion accelerating voltage
Imposition of the magnetic deflection field has a second
beneficial effect. The voltages on the rod are relatively
low in the vicinity of hydrogen 1 and 2 so that heavier
ions are hardly deflected and have a high probability of
being transmitted through the monopole filter. This causes
an increased background at the low end of the mass
scale which can be eliminated by the application of the
transversal magnetic field.
,.. Work performed under Contract NASw 1314.
1 U. von Zahn, Rev. Sci. lnstrum. 34, 1 (1963).
Automatic Electropolisher for Copper*
D. A. LINDHOLMt
University of California, Berkeley, California 94720
(Received 23 December 1968; and in final form, 11 March 1969)
A N automatic power supply control and an improved
sample mounting technique have been incorporated
into the system described by Powers1 for electropolishing
copper disk specimens.
In the electropolishing arrangement shown in Fig. 1,
the basic modifications are as follows: (1) The disk sample
is glued with conducting cement (two parts powdered
graphite to one part Duco cement) to a pedestal rather
than resting on a gold foil connected through a rubber
Cu wire in
(QpiUary tub. -i-i'~-.III
Guard rine
! IconfcrCffAul
Sampl. con'oct
(T.flon ca.ed wiret

was 31 V, which results in an orbit curvature of 4.3 m for

ions of a medium mass 28. This indicates that a relatively
slight beam deflection is sufficient to produce the desired
effect. This deflection has to be gradual and distributed
over a large part of the beam and cannot be replaced by a
beam deflection before the entrance aperture. The op-
timum magnet location which produces the largest peak
heights is slightly mass dependent. Fortunately, position-
ing of the magnet is not critical since significant sensi- l ..... ling .crew. (31/

tivity improvements can be realized over the entire mass

range at a single intermediate magnet position. However, CrOIl ... ctionol detail Tape "~- Sampl.
of lampl. mount
the degree of sensitivity improvement is slightly mass Conducting cement Ped.ltal
Sam pl. lead /'
dependent. The magnetic field has no effect on the resolu-
tion of the instrument. However a very slight shift of the FIG. 1. Electropolishing bath. The spring loaded screws were
covered with layers of paraffin (not shown) to prevent reaction with
peaks can be observed. the electrolyte.

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 1106
FIG. 2. Block diagram of electropolishing system.
sheet. The advantage of this arrangement is that a low
resistance (typically 0.5 0) electrical and semipermanent
mechanical connection is made to the sample. The sample
and pedestal can be mounted on a spark machine and
simply transferred to the electropolishing jig. Mter com-
pletion of the electropolish the sample is removed by
dissolving the cement bond in acetone. (2) The support
for the guard ring (necessary for small samples to prevent
rounding of edges) is mounted on three spring-loaded
screws rather than being threaded into the jig neck. This
allows a small angular adjustment of the guard ring with
respect to the sample surface. Hence the guard ring can
be adjusted accurately parallel to and flush with the
sample surface even if the sample is slightly nonparallel
to the normal to the jig. axis.
As has been previously emphasized, l the best electro-
polish results if the anodic overvoltage (measured by a
probe just above the sample or guard ring) is about
-1 V with resPect to the cathode. In principle the over-
voltage can be kept fixed by manually controlling the
bath power supply. But this method is very inefficient
for several reasons: (1) It is difficult to track the over-
voltage in the oscillating region of the polarization plot
(see Fig. 2 of Ref. 1). (2) It may take 1 h or longer for
the bath voltage to stabilize, during which time the
current density may change by a factor of 20. (3) If the
overvoltage exceeds a certain critical value (about 1.3 V)
the sample is pitted by violent evolution of oxygen. To
overcome these difficulties an automatic control circuit
was designed which keeps the overvoltage fixed at a
preset value and incorporates an upper limiting voltage
Manllol
100 adj","
o
180
o
"311 '- -~- i- - J\~
7.5 kG
7.2
.0
510n(ol 7W
P.<l096 ~---.-~- -- --------
L ________________
0-5 A
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NOTES
(clamp) to prevent sample damage. A block diagram of
the circuit is shown in Fig. 2.
The bath power supply (Fig. 3) was designed to provide
5 V at 5 A although 3 V at 3 A is sufficient. When used in
the automatic control mode, the center tap on the manual
adjust potentiometer is positioned at the top of the 200 0
resistor. The 2N3565 transistor Q., in conjunction with
the 0.27 010 W resistor, provides short circuit protection.
When the clamp circuit is not in operation (Q2 off) the
series control element, consisting of the Darlington pair
of transistors 2N3714 and 2N3766, responds to the
transistor Ql whose base current is derived from the
amplified difference between reference and probe. If the
clamp is actuated, a small negative voltage at the base
of Q2 causes it to conduct. In this mode, the power supply
is virtually off, since the series control element is by-
passed and current from Ql is directed through Q4 to the
negative terminal (ground).
The error signals are derived from the circuit of Fig. 4.
In the scheme shown, the reference voltage is adjustable
within the range -0.9 to -1.1 V and the clamp within
-1.2 to -1.4 V. The dual 2N3958 FET provides high
impedance inputs for both reference and probe voltages.
The 2N3565 transistors provide a constant current source
for the FET and are biased differently (2.78 and 2.94 kO)
to equalize the characteristics of both arms of the com-
parison circuit. The probe and reference signals reach the
lower operational amplifier where the amplified difference
forms the control output to the bath power supply. Al~
though the feedback loop of this amplifier is provided
with variable gain and high frequency attenuation, the
circuit always worked well at full gain and minimal
attenuation.
The upper operational amplifier of Fig. 4 compares the
probe and clamp voltages. In the feedback loop of this
amplifier, the diodes and 100 kO resistors act as a fast
recovery clamp for the amplifier, effectively limiting the
output to '" ± 7 V according to whether the probe is less
or more negative than the clamp. In the latter case, the
-7 V error signal results in V b.>'::: -1 V on the switching
transistor Q2 in the bath power supply (Fig. 3), effectively
FIG. 3. Schematic of the bath power supply.
~
H.al,ink

6190
m 0-2
Ref, voltage ~ _ _-----l
FIG. 4. Schematic of the operational
200n
amplifier module.
8.2 kG
1%
1 kG
5,6 Iron
1~.
O.01~f
turning off the bath as described above. Nonnal control
resumes if the output of this amplifier reverts to ",+7 V.
The performance of the system was excellent. Within a
few seconds after switching on the electronics the over-
voltage reached the desired value and stayed that way as
long as desired. The unit has been effectively used up to
two days in continuous operation. By suitable modifica-
tions of the power supply voltage and clamp voltages, the
basic circuitry could be used in the electropolishing of
other metals. 2
A Simple High Voltage Vacuum Seal*
K. R. MACKENZIE
Department of Physics, University of California,
Los Angeles, California 90024
(Received 1 April 1969)
I Ncases
some studies with rf superimposed on dc (in some
up to 5 k V) we were bothered by faint glow
discharges on surfaces near the electrode seals. l We sus-
pected that the cause might be vapors from O-ring seals
or surface effects due to the use of soft solder joints. To
eliminate these suspicions and also solve a space problem
we tried the simple seal shown in Fig. 1. We have found
it very useful in situations where a high voltage seal is
needed very quickly in a restricted space. However, the
vacuum plate in which it is installed must have a thick-
ness which is about twice the diameter of the seal.
Construction is very simple. The first step is a hole in
the vacuum plate, followed by slight expansion with a 3°
Morse tape reamer. The insulator is a piece of slightly
oversize Teflon stock in which a hole is drilled a few
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NOTES 1107
-15 V
lOHl
12 kfl
+15 V Probe input
aNe
(lamp yoltage
2500
2N39S8 ~
1 kG
10 kG
v r;::========-r:-~4.-:::
0.2 V
I kn
2N3565
2.78 Ir.fi
1~.
-15 v
+15 v
The author wishes to acknowledge the contribution "of
A. J. George who designed the circuit to specifications,
and the support provided by Professor A. F. Kip.
t Present address: Franklin Institute, Philadelphia, Pennsylvania
19103.
* Supported in part by the U. S. Air Force Office of Scientific
Research Grant No. AF-AFOSR 290-63.
1 R. W. Powers, Electrochem. Techno!. 2, 274 (1964).
2 See, for example, tables in W. J. Tegart, The Electrolytic ,!nd
Chemical Polishing of Metals (Pergamon Press, Inc., Long Island CIty,
New York, 1960), 2nd ed.
hundredths of a millimeter smaller than the inner electrode
(in our cases practically always a 6.35 rum stainless rod).
After the rod is pressed through the Teflon the assembly
is chucked in a lathe and the Teflon is then cut to shape
as shown in Fig. 1. The center portion forms the seal
while the remainder provides a creepage path as long as
desired to inhibit surface breakdown. At first we roughly
matched the Morse taper but later found that the plas-
ticity of the Teflon made this unnecessary. The seal as-
sembly is then driven into the tapered hole, using a
hollow "drift" tube which approximately matches the
diameter of the shoulder on the Teflon cylinder. The
Teflon flows until it conforms to the tapered hole, at
which point the behavior is the same as trying to drive
the hollow tube into a piece of solid Teflon. We found that
it took several months for the Teflon to relax to the point
where one could detect further motion by repeating this
driving operation.
We have no long tenn infonnation on these seals since
none of our studies have required continual use longer
than six months. For example, we would frequently change
the internal electrode position by driving the center elec-