Rinsing: A Critical Process in Contamination

Removal
Kurt K. Christenson
FSI International, Inc.
Chaska, Minnesota

IMPEDIMENTS TO EFFECTIVE RINSING

ABSTRACT

The rinsing process of silicon wafers is normally

carriedout in an "overf7ow" bath in which waterflows
past the wafers at average velocity of I c m k But the
velocity is zero at the wafer sugace. The efficiency of
rinsing is limited by the rate at which contaminants
diffuse away from the silicon sugace and into the flow
stream. This paper reports the improvement in rinsing
efficiency gained by repeating a I-min cycle offirst
allowing the contaminants to diffuse into the stagnant
layer and then "dumping" the rinse tank to remove
most of the contaminated stagnant layer. A further 10fold improvement in rinsing efficiency per rinse cycle
can be achieved by spinning the wafer and using
centr@gal force to remove a greater fraction of the
stagnant layer This allows the complete removal of
soluble contaminants with a 20-fold reduction in water
usage compared to present immersion techniques.

hen rinsing in an overflow bath, the water flows

past the wafers at an average velocity of 1 cmls.
The fluid dynamics of the system result in a
parabolic velocity distribution with the maximum flow
midway between the wafers and zero velocity at the wafer
surface. The efficiency of rinsing is limited by the rate at
which contaminants diffuse through the almost stagnant fluid
and into the flow stream. Typical reported rinse-water
requirements for 100-mmwafers range from 13to 20 Llwafer
for each chemical step.' This paper reports the improvement
in rinsing efficiency gained by repeating a 1-min cycle of first
allowing the contaminants to diffuse into the stagnant layer
and then "dumping" the rinse tank to remove most of the
contaminated stagnant layer. If centrifugal force is used to
remove a greater fraction of the stagnant layer, a further 10fold improvement in rinsing efficiency per rinse cycle can be
a~hieved.~
The use of centrifugal force allows the complete
removal of soluble contaminants with a 20-fold reduction in
water usage compared to present immersion techniques.

Carryover Layer
The success of aqueous-based cleaning of silicon wafers
depends on the complete removal of both the residual
contaminants and the cleaning solutions by a rinse process.
The primary component to be rinsed is the "carryover" layer,
the film of process chemical that clings to the wafer as it is
transferred from the process tank to the rinse tank. Spearow
et al. gives the thickness of the carryover film h in microns as

where V is the extraction velocity of the wafers from the

liquid in ~ m / s . ~
Figure 1 shows the thickness of the carryover layer of
20C DI water as a function of extraction velocity. An
extraction velocity of 5 c d s corresponds to a carryover film
of 20 pm. High-throughput automated wet stations extract in
the range of 20 to 60 c d s , giving a thickness range of 50 to
100 pm.
Hot, aqueous-based chemistries have a lower viscosity
than cold and carry over approximately 50 percent less fluid.
Viscous chemistries such as H2S0,:H202 have carryover
layers over three times the values shown in Figure 1.
Areas of the wafer that are hydrophobic (not wetted by the
process chemical) have negligible carryover films. However,
on patterned wafers, hydrophobic areas can act to block the
drainage of the fluid from the wetted hydrophilic areas.
Patterned wafers can carry out a substantial amount of dilute
HF into a rinse bath.

Keywords: cleaning, rinsing, dump rinsing, ramped rinsing,

centrifugal force, diffkion, spray processor, wet bench, spin
rinse drier, w t e r usage

10

20

30

40

50

60

ExtractionVelocity (cmlsec)

Figure I . Thicknessof carryover as afunction of extraction veloci ~ .

10' l o n d d InitialSurface Concentration

0.05

0.1

0.15

0.2

Distance Fmm Surface (cm)

0.01

0.02

0.03

0.04

0.05

Distance From Surface (em)

Figure 2. Distribution ofionic and molecular contaminants in rinse

water following diffusionfrom the su$ace of a wafer.

Figure 4. Diffusion of ionic contaminants compared to the velocity

distribution between the wafers.

species are typically in the range of 10-5cm2/s,which allows

an average diffusion length of approximately 1 mm during a
15-min rinse.7 Figure 2 shows the approximate distribution
of small ionic and molecular contaminants in a stagnantwater rinse bath 60, 300,600, and 900 sec after insertion of
a contaminated wafer. For typical rinse times, the carryover
layer is much thinner than the diffusion length, justifying the
assumption of an initial aerial (two-dimensional) surface
concentration. As seen from Equation 2, the concentration at
the wafer surface falls as t -'I2.

4.1

0.1

0.2

0.3

0.4

0.5

0.6

Distance Fmm Surface (cm)

Figure 3. Velocity distribution of rinse water between the wafers.

Ionic Diffusion
An analysis by Tonti indicates that after 15 min in an
overflow rinse tank, 0.88 percent of the initial surface
contamination is still carried over into the subsequent process
bath or dry sequence in the 20-pm layer of water on the wafer
carried over from the rinse tank.4
This poor rinsing performance is caused by a nearly
stagnant boundary layer near the surface of the wafer where
there is little bulk motion of the fluid. Contaminants must
diffuse through this boundary layer to reach the flowing rinse
water and be swept away.
The problem can be treated as diffusion in one dimension
from a finite source (i.e., the total amount of contaminant is
constant). Fick's First Law applied to these boundary
conditions gives a solution of the form
M

c (x,t ) = --( m t y 2 ex.

[&I

where x is the distance from the wafer surface, D is the

diffusion coefficient, t is the time, and M is the initial aerial
concentration at the s ~ r f a c e . ~ , ~
Diffusion coefficients for dissolved ionic and molecular

Velocity Profile
Rinse tanks are normally not stagnant, but have average
flow velocities parallel to the surface of the wafers near
1 cmls. The fluid motion in these "overflow" rinse tanks acts
to sweep away contaminants that have diffused into the flow
stream from the surface of the wafers. Figure 3 shows the
velocity distribution of the water between two 200-mm
wafers with 0.25-in. pitch and 1 c d s average water velocity.
The distribution is parabolic with a velocity profile

where uOVe
is the average velocity of the fluid, d is the distance
between the wafers, and h is the distance from the midpoint
between the wafer^.^ The maximum velocity is 1.5 times the
average velocity and occurs midway between the wafers.
Fluid dynamic boundary conditions fix the flow at zero at the
surfaces of the wafers. The interstitial space between the
wafers is rinsed very effectively.Unfortunately, at the surfaces
of the wafers where the contaminants are concentrated, there
is no bulk fluid motion.

Diffusion vs. Water Velocity

Figure 4 shows the velocity distribution near the surface of
a 200-mm wafer for a 1 - c d s average flow as described in
Figure 3 compared with typical diffusion profiles. Only at a
distance of 0.033 cm from the wafer does the fluid reach 0.33
c d s , the velocity necessary to transit a 200-mm wafer in
1 min. At a distance of 0.0033 cm, the fluid transits the wafer
once in 10 min. Over 2 percent of the contaminants never
JOURNAL OF THE INSTITUTE OF ENVIRONMENTAL SCIENCES

6E+05

IMEC Owflow Rinse Data

-$

5E+05

-g 4EM5

52 3E+05
U

2E+05
1EM5

1
0

120

240

360

480

600

Time (sec)

OE+OO
0

0.005

0.01
0.015
0.02
Distance Fmm Surface (cm)

0.025

0.03

Figure 5. Theoretical "diflusion only " model vs. experimentally

determined rate of rinsing in an overjlow bath.

Figure 6.Dzfision of 0.3-pm particles into rinse waterfrom wafer

sugace compared to the velocity distribution of water.

diffuse to a distance of 0.0033 cm during a 10-minrinse cycle

and so are not transported away from the wafer at any time
during the rinse. Therefore, the flow of water between the
wafers in an overflow rinser does remove most of the
contaminants, but does not provide a thorough rinse at the
surface of the wafers.

contaminants.
Figure 6 shows the concentration profile for 0.3-pm
particles for diffusion times of 60,300,600, and 900 sec. Less
than half of the particles would diffuse 0.0033 cm into the
flow streamduring a 10-minoverflow rinse. Overflow rinsing
is a very inefficient means of removing particles.

In-Drain Conductivity Monitors

A conductivity monitor in the drain of an overflow system
sees primarily water that has passed near the center of the gap
between the wafers. The contaminated water from near the
wafer surface flows to drain very slowly-at time scales
longer than the total rinse time. Therefore, the readings of indrain conductivity monitors do not reflect the concentration
at the surface of the wafer in an overflow system.
Overflow Experimental vs. Theoretical Results
Figure 5 shows the theoretical t-'12rinsing efficiency of an
overflow rinse along with experimental data from ~ e u r i s ?
Experimental data were gathered by contaminating wafers
with KCl, rinsing the wafers, and measuring the residual
potassium on the wafers with TXRF. The experimental
results are significantly better than the theoretical prediction,
with the surface concentration dropping 1 log reduction value
(1 LRV = 1 O-fold decrease) every 4 min. This improvement
over "diffusion only" rinsing is brought about by the flowing
water. Ions far from the wafer, in the tail of the distribution,
are washed away. This increasesthe net concentrationgradient
in the distributionand speeds diffusion away from the surface.
Particle Diffusion
Once detachedfrom the surface by chemical or mechanical
means, particles, like ions, move away from the surface by
diffusion. But the limiting effects of diffusion in rinsing are
far more extreme for particles. The diffusion coefficient for
particles is given by the Stokes-Einstein relation

where k is the Boltzmann constant, T is the temperature, o i s

' ~ diffusion
the particle diameter, and 77 is the v i s c ~ s i t y .The
coefficient for 0.3-pm particles is near 1.4 x
cm2/s,
nearly three orders of magnitude lower than for typical ionic

SOLUTIONS FOR EFFICIENT RINSING

While overflow rinsing is not an efficient means of

removing contaminants from wafers, its efficiency can be
greatly improved with some simple modifications.

Limiting the Carryover Layer

The concentration of the contaminants on the wafer at the
endofthe rinse is proportional to the initial aerialconcentration
at the beginning of the rinse (M in Equation 2). This is most
easily achieved by reducing the thickness of the carryover
layer. In bath systems, this can be done in two ways:
A. Increasing the temperature of the process bath to decrease
its viscosity. Because the bath temperature is set by other
process parameters, this is rarely an option. It may be
possible to increase the final rinse temperature to decrease
the carryover layer into the drier.
B. Reducing the extraction velocity. The extra 10 sec added
to the process by extracting a 200-rnm wafer at 2 c d s vs.
50 c d s is easily compensated by the reduced challenge to
the rinse process.

Dump Rinsing
"Dumping" and refilling the rinse tank periodically during
the rinse cycle allows contaminants that have diffused some
distance into the bulk of the boundary layer to drain away.
Only the contaminants in the "carryover film" remain on the
wafer.
Figure 7 shows the thickness of the carryover layer in
comparison to the diffusion profiles for ionic contaminants.
Like the carryover layer from the process to the rinse tank, the
thickness of the carryover layer between rinse cycles is
primarily determined by the bath drain time (extraction
velocity), the viscosity and density of the water, and the force
of g r a ~ i t y . ~

z micron carryover layer)

-6OSeconds
-3WSeconds
,600Seconds
900Seconds

300
600 Seconds
,900Seconds

c
.O 0.05

LL

0
0

0.005

0.01

0.015

0.02

Figure 7. Thickness of the carryover layer vs. typical diffusion

profiles.

-g

IE*

6- lEW

+DlvnpRinsa

R IE+OZ

-Rmped

4:

OverRowRi~

Rinse

~ ' l Iondad
e
Initial Areal Density in dmp rinse
9lO' l a d u d lnilialAma! Density in ramp rinse
lodadlec Difhasii Coefficient

lE+Ol
1EaO

Repeated40 sec DiflusionRO see removal sequence

1E-01
0

50

100
150
Time (sec)

0.002

0.004

0.006

0.008

0.01

Thickness of Canyover Layer (cm)

Distance Fmm Wafer (cm)

200

Figure 8. Theoretical comparison of the sugace contaminant

concentration between "difisiononly" rinsing, dump rinsing with
a 2 0 - p carryover layer, and ramped rinsing with a 2 - p carryover
layer.

The gray bar in Figure 7 represents a 20-pm carryover

layer typical of a 5-cmls extraction velocity (The black, 2-pm
bar is described in the following section titled "Ramped
Rinsing.") After 60 sec of diffusion, less than 5 percent of the
ionic contaminants remain in the layer and 95 percent of the
contaminants are washed down the drain. Figure 9 shows the
fraction of contaminant remaining in the carryover layer vs.
layer thickness and diffusion time.
An efficient rinse sequence is as follows:

1. Submerge the wafers and allow contaminants to diffuse

freely from the wafer surface into the water.
2. Slowly drain the bath to remove all the contaminants
except the 5 percent entrained in the carryover layer.
3. In a second rinse cycle, resubmerge the wafer and allow
the remaining 5 percent of contaminants in the thin
carryover layer to again diffuse into the water.
4. Repeat steps 2 and 3.
Figure 8 shows the calculated aerial concentration of
contaminants in a 20-pm layer at the surface of the wafer for
a stagnant bath (smooth line) and for a dump rinsing sequence
(upper "terraced line). The model uses a diffusion time of 40
sec followed by a 20-sec drain period in which no diffusion

Figure 9. Fraction of contaminants remaining in the carryover

layer vs. layer thickness and diffusion time.

takes place. These calculations indicate that dump rinsing

achieves a 20-fold reduction in the contamination levels at
the surface of the wafer after each 1-min rinseldump cycle. A
single, I-min rinseldump cycle leaves 5 percent of the initial
contaminants. A second I-min cycle would reduce the
contamination level by another 20-fold to 0.25 percent of the
initial contamination level. This should be compared to
Tonti's calculation of 0.88 percent remaining after 15rnin in
an overflow rinse.4
While dump rinsing is effective in removing ions, it is of
little help in removing particles. Only 12 percent of 0.3-pm
particles would diffuse out of the 20-pm carryover layer in 1
min to be removed during a "dump" of the rinse bath.

Ramped Rinsing
The most critical parameter in determining the efficiency
of the dump rinse sequence is the thickness of the carryover
layer. Figure 9 shows the fraction of contaminants remaining
in the carryover layer as a function of diffusion time and layer
thickness. For a60-sec diffusion time, reducing the carryover
layer from 20 mm to 10 pm would reduce the remaining
contaminants by a factor of two. After four such cycles, the
net reduction in contamination remaining on the wafer would
be 24 or 16 fold.
The thickness of the carryover layer can be reduced
greatly by supplementing the force of gravity with centrifugal
force by spinning the wafers either about their axis as, in a
spin-rinse drier, or off axis, as in a multiple-position spray
processor. The carryover thickness after a 10-secramp at 500
rpm in a multiple-position spray processor was measured to
be less than 2 pm. At 500 rpm, the fluids are removed by a
centrifugal force approximately 50 times as strong as gravity.
Reducing the thickness of the carryover layer from 20 pm
to 2 pm results in areduction in the residual contamination in
the carryover film from 5 percent to 0.5 percent-a 10-fold
reductionforevery rinse cycle. Figure 7 shows the contaminant
distribution in the rinse water after 60 sec. The 2-pm (0.0002cm) layer that remains after the 500-rpm ramp is approximately
equal to the thickness of the y-axis.
Ramped rinsing is also effective in removing particles.
While only 12 percent of 0.3-pm particles diffuse through the
20-pm carryover layer in a dump rinse, 88 percent diffuse
through the 2-pm carryover layer left after a ramp. Thus, 88
JOURNAL OF THE INSTITUTE OF ENVIRONMENTAL SCIENCES

percent of the particles that are dislodged from the surface are
removed in each 1-min ramped rinsing cycle. Ramped rinsing
has a strong, positive effect on particle removal efficiency.
The bottom terraced line of Figure 8 shows the theoretical
performance of ramped rinsing. As with the dump rinsing
data, the model uses a diffusion time of 40 sec followed by a
20-sec ramp period in which no diffusion takes place. The
initial surface concentration for the ramp rinse data is 10
times less than that of the dump rinse data because the
carryover of process chemicals is 10 times less in the ramped
case. After three I-min rinse cycles, the ramped wafers are
1000 times cleaner thun the dump rinse wafers.
A further benefit of ramped rinsing over dump or overflow
rinsing is reduced water usage. As seen in Figure 2, water
farther than 0.05 cm from the surface of the wafer plays a
small role in the diffusion process and therefore the rinse
process. In immersion, 80 percent of the water in the 0.5-cm
gap between the wafers is wasted. If the water is dispensed by
spray, ramped rinsing achieves a five-fold reduction in water
usage by only wetting the top and bottom surfaces of the
wafer.

Experimental Performance
Figure 10 shows a comparison of the experimental
performance of ramped and overflow r i n ~ i n g . ~
In both cases, challenge wafers were prepared by dipping
wafers in a saturated KC1 solution and spinning them dry.
Residual potassium was measured with TXRF. The
contamination is reduced in the overflow rinser by only 1
LRV each 4 min. A clear potassium signal is still detectable
after a 10-min rinse.
The simple theoretical model in Figure 8 predicts a 2.3
LRVImin for ramped rinsing. Experimentally,ramped rinsing
reduced the signal by 3.5 LRV in 30 sec, three times faster
than the theory and 28 times faster than the overflow rinser.
No potassium signal is detectable after 30 sec of ramped
rinsing. There are two reasons that ramped rinsing performs
so much better than the prediction of the simple model:
Diffusion continues during the 20-sec ramp-off period.
If rinse water is dispensed during the ramp, a thin layer of
clean water above the 2-pm carryover layer will be
refreshed constantly, as if there were an infinite sink for
contaminants a few microns from the wafer surface.
While these mechanisms can also be active in dump
rinsing, the 50-fold ratio in the centrifugal force in the ramp
to the gravitational force in the dump renders them far less
significant in dump rinsing.
RINSING IN TRENCHES

The previous arguments have all referred to the rinsing of

planar surfaces, not wafers with topography. But just as
diffusion is a very slow means of transport for ions that are
over thousands of microns from the wafer surface, it is a very
fast means of transport on the few-micron vertical scale of
semiconductor feature^.".'^ As seen in Figure 2, typical
diffusion distances are of the order of (Dt)'I2. While it takes
1000 sec for ions to travel 1 mm, it takes only 1ms to diffuse
1 pm. Even the bottom of a high-aspect-ratio trench
equilibrates very rapidly with the fluid above the trench.
SEPTEMBEWOCTOBER 1997

120

240

360

480

600

Secondsof Rnsing

Figure 10. Experimental rinsing eficiencies of oveijlow and ramped

rinsing.

Table 1. Maximum Concentration in a

Trench as a Function of Time
Time

Cmax'c

(t = 0)

0.27

0.058

5.7E-4

2.5E-7

5.1E-14

Table 1 gives the results of a finite element analysis by

Olim of the concentration at the bottom of a 4-pm-deep by
0.5-pm-wide trench.13 The trench was initially filled with
water with a unit concentration of an ionic contaminant (D =
cm2/s).After 100 ms, the concentration at the bottom of
the trench has dropped by a factor of 1 million, effectively
equilibrating with the fluid above the trench. For rinse
processes longer than one second, even deep trenches can be
considered to be in equilibrium with the surface at all times.
CONCLUSION:

Overflow rinsing is not an efficient method of removing

contaminants from a wafer, especially particulates. Many of
the contaminants never diffuse far enough from the wafer to
be transported away by the moving fluid. Dump rinsing,
where the bulk of the contaminants are washed down the
drain in each dump cycle, is substantially more efficient than
overflow rinsing. Ramped rinsing, the logical extension of
dump rinsing to very thin carryover layers, is by far the most
efficient, simultaneously allowing a far better rinse, a shorter
rinse time, and a 20X reduction in water usage compared to
overflow rinsing. Deep trenches are easily rinsed by diffusion
and can be considered to be in equilibrium with the surface.
REFERENCES

1. Ching, G., and Murtha, R., "Cost of Ownership Comparisons

for 200-mm vs. 150-mmImmersionWet Cleaning Equipment,"
Proceedings of the Microcontaminaton Conference, p. 378,
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3.

4.

5.
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10.
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13.

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Ionic salt rinsing data courtesy of Marc Meuris, IMEC.
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Parker, J., Verhaverbeke, S., and McConnell, C., "Wet
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ACKNOWLEDGMENTS

The author thanks Brent Carlson, Jim Oikari, and Moshe Olim
of FSI International for helpful discussions and significant
laboratory andfield work in testing these ideas.

Updated version of a paper presented at the 43rd Annual

Technical Meeting of the Institute of Environmental Sciences, May
4-8, 1997, Los Angeles, California.

AUTHOR BIOGRAPHY
Dr. Kurt K. Christenson, a senior process physicist, joined FSI
International in 1990. He works in process development for the
centrifugal spray processor product line. He received his B.A. in
Physics in 1980 at Bethel College, St. Paul, Minnesota, and his M.S.
andPh.D. in Physics from theuniversity of Illinois aturbanain 1983
and 1988,respectively.His postdoctoral workinE-beam lithography
was completed at the IBM T.J. Watson Research Center in 1990. He
has written over 45 papers on microanalysis, E-beam lithography,
and semiconductor wafer cleaning.

50

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