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UV/Ozone Cleaning of Surfaces

Article  in  Journal of Vacuum Science & Technology A Vacuum Surfaces and Films · June 1985
DOI: 10.1116/1.573115 · Source: IEEE Xplore

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IEEE TRANSACTIONS ON PARTS, HYBRIDS, AND PACKAGING, VOL.
UV/Ozone Cleaning
JOHN R. VIG, MEMBER, IEEE, AND JOHN W. LE BUS, MEMBER,
I
Abstract-The ultraviolet (UV)/ozone cleaning procedure is
shown to be an effective method of rapidly removing a variety
of contaminants from surfaces. It is a simple-to-use dry process
which is inexpensive to set up and operate. It can produce
clean surfaces in air, at ambient temperatures. The experi-
ments were performed on quartz and metal surfaces. The
contaminants which were successfully removed include oils
and greases (including silicones), fluxes, skin oils, and con-
tamination adsorbed during prolonged exposure to air.
The experiments were aimed at defining the variables and
determining the optimum conditions for producing clean sur-
faces by UV irradiation. The important variables are: the
contaminants initially present, the precleaning procedure, the
wavelengths emitted by the UV source, the atmosphere be-
tween the source and sample, the distance between the source
and’sample, and the time of exposure. For surfaces which are
properly precleaned and placed within a few millimeters of an
ozone-producing UV source, the process can consistently pro-
duce a clean surface in less than 1 min.
Experiments performed with two low-pressure mercury dis-
charge UV sources, one which generates ozone and one which
does not, indicate that the combination of short-wave UV light
plus ozone produces a clean surface substantially faster than
either short-wave UV light without ozone or ozone without
UV light.
INTRODUCTION
The ability of ultraviolet (UV) radiation to decompose
hydrocarbons has been known for a long time, but it is only
recently that surface cleaning by UV radiation, and its possible
application to electronic parts manufacturing, has been ex-
plored. Bolon and Kunz [II investigated the ability of UV
light to depolymerize photoresist polymers and showed that
UV depolymerization produced an extremely clean surface. R.
R. Sowell [2] et al. reported that prolonged (= 15 h) exposure
to UV radiation produced clean surfaces on gold contacts and
glass slides in ambient air, as well as in a vacuum system when
a pressure of 10e4 torr of oxygen was present. J. R. Vig 131,
[4] et a/. investigated the UV/ozone cleaning procedure in
connection with the processing of precision quartz crystal
resonators, where even fractional monolayers of contamina-
tion can lead to significant aging effects. J. L. Jellison [51
recently showed that prolonged UV irradiation is highly effec-
tive in the removal of organic contaminants from gold films
and it can, thus markedly reduce the temperature dependence
of thermocompression bonding.
This paper discusses experiments aimed at defining the
Manuscript received March 15, 1976; revised July 28, 1976.
The authors are with the Electronics Technology and Devices Lab-
oratory, US Army Electrdnics Command, Fort Monmouth, NJ 07703.
PHP-12, NO. 4, DECEMBER 1976 365
of Surfaces
IEEE
Fig. 1. Contact-angle goniometer.
variables and determining the optimum conditions for pro-
ducing clean surfaces by UV irradiation.
TESTING FOR CLEANLINESS
The results of the cleaning experiments were evaluated by
contact-angle measurements and Auger electron spectroscopy
(AES). Two techniques were used to measure the contact
angle: the contact-angle goniometer and the steam test. Most
of the measurements were performed on polished quartz sur-
faces. The reasons for concentrating on polished quartz for
these studies were twofold. First, the cleanliness of these
surfaces is easy to evaluate by the steam test. Second, the
motivating force behind these studies was to improve the
stability of quartz resonators by finding the optimum cleaning
procedure. There is probably no other device whose perfor-
mance is so critically dependent on surface cleanliness. For
example, the aging requirement for a ~-MHZ resonator cur-
rently under development is that the frequency change no
more than two parts in IO’ ’ per week, whereas adsorption or
desorption of a monolayer of contamination changes the fre-
quency by about one part in 106!
Fig. 1 shows the contact-angle goniometer. It is a simplified
version of one previously described [61, 171. It can be as-
sembled simply from a protractor and about 25 cm of straight
tubing having a 3 - 4-mm inside diameter. The tube swings
radially about the point where the sample is placed. The light,
which can be an unfrosted incandescent bulb, is suspended
about 1 m directly above the sample. To assure that the light is
in the proper position, the tube is rotated to the 0’ position
and the goniometer is repositioned, if necessary, until the light
intensity passing through the tube is maximum.
To measure the contact angle, a small drop of pure water is
placed on the sample with an applicator made of a small loop
at the end of a short length of clean wire. The reflection of
 366 IEEE TRANSACTIONS ON PARTS, HYBRIDS, AND PACKAGING, DECEMBER 1976

TABLE I
Results of Steam Test

RESULT APPEARANCE
OF CONDENSATION CONTACT MONOLAYERS
OF
ONPOLISHED
QUARTZ ANGLE CONTAMINATION

EXCELLENT UNIFORM RAINBOWLIKE FRINGES DURING 40 <O.l

FRINGES BOTH CONDENSATIONAND EVAPORATION

GOODFRINGES UNIFORM FRINGES DURING CONDENSATION 40 <O,l

IRREGULAR FRINGES DURING EVAPORATION

POOR FRINGES IRREGULAR FRINGES DURING CONDENSATION 40 dO,l

ORANGEPEEL No COLORS, LARGE DROPLETS VISIBLE, 50 - 100 0,l - 1

TRANSPARENT

FOG TRANSLUCENTDUE TO LARGE NUMBEROF >loO >l

SMALL DROPLETS

light from the water droplet is observed through the tube. As
the tube angle is increased, the image of the light moves down
the surface of the water droplet and disappears when it reaches
the point where the droplet contacts the test surface. The tube
angle at this point is equal to twice the contact angle.
At low contact angles, the operator’s head obstructs the
light. Therefore, for measuring low contact angles, the
goniometer is moved until the light is incident o.n the water
droplet at a small angle, e.g., IO’. The contact angle is then
related to the tube angle by the following:
contact angle = % (tube angle -light angle)
where “tube angle” again denotes the angle at which the
reflected light disappears. The uncertainty in this method of
contact-angle measurement is about + 2’. This uncertainty
prevents the use of this technique for the accurate measure-
ment of fractional monolayers of hydrophobic contamination.
A simple method of measuring the contact angle, which is
sensitive to fractional monolayers, is the steam test. This
semiquantitative nondestructive test consists of. holding the
sample over a beaker of pure hot (but not boiling) water for
about a second, observing the condensation, then removing the
sample from above the beaker, and observing the evaporation
of the condensation. The sensitivity of wettability tests, of
which the steam test is one, has been discussed by Feder and
Koontz [S] While the sensitivity is a function of the con-
taminating molecules on the surface, wettability tests have
been shown to be capable of indicating the presence of small
fractions of a monolayer of hydrophobic contamination.. The
five possible results of the steam test and their approximate
correlation with hydrophobic contamination levels and con-
‘tact-angle-goniometer test results are shown in Table I. In
general, the better the appearance of the fringes, the less
contamination there is on the surface.
A convenient way of learning to recognize the results of the
steam test is to perform it on freshly cleaved mica, repeating
the test every few minutes as the mica adsorbs hydrophobic
contamination from the air. Depending on the composition of
the air, it will take on the order of 30 min to reach the “fog”
condition. The cleaved sample should be thick enough to have
a reasonable heat capacity, otherwise it will heat up quickly in
the steam and no condensation will occur.
Both the steam, test and the contact-angle-goniometer test
are sensitive only to hydrophobic, i.e., nonwettable, con-
tamination. Both tests are accurate only if there are no wetting
agents such as detergent residues on the surface. The steam
test is useful only on smooth surfaces. The contact-angle-
goniometer test can be used on rough surfaces; however, the
surface roughness can affect the results.
The results of these wettability tests were checked with
AES, which can detect all elements on the surface, except
hydrogen, with a sensitivity of 1 percent of a monolayer. The
Auger spectra of clean and contaminated quartz surfaces have
been discussed previously 131, [9] .
Samples which.had been cleaned without the use of deter-
gents and which ‘had shown fringes in the steam test prior to
insertion into the Auger electron spectrometer generally
showed no detectable contaminating elements other than a
trace of carbon in the AES spectrum. This seems to indicate
that, at least for. the types of surfaces, contaminants, and
cleaning procedures studied, if the hydrophobic contaminants
are removed from the surface, then so are all other con-
taminants which are detectable with AES.
The Auger spectra of clean quartz surfaces exposed to air
prior to AES examination invariably show a trace of carbon,
but generally no other contaminating elements. In an attempt
to learn the source of this carbon, quartz samples, which had
been ion-bombardment-cleaned until no carbon was visible in
the Auger spectrum, were exposed to air for the same 15 min
it generally took to mount the samples in the Auger spec-
VIG AND LE BUS: UV/OZONE CLEANING OF SURFACES 367

The tube of the UV lamp [I41 in box 1 consists of 91 cm

of “hairpin-bent’: fused quartz, which transmits both the
2537- and 1849-A lines. The lamp emits about 0.1 mW per
cm2 of 1849-A radiation measured at 1 cm from the tube.
The lamp in box 2 has two parallel 46-cm-long straight
high-silica glass tubes. Theo glass is Corning U,V Glass No. 9823
which transmits at 2537 A but not at 1849 A. Since this lamp
generates no measurable ozone, a separate Siemens-type ozone
lRAllSfORYER generator [I51 was built into box 2. This ozone generator
uv BOX I uv BOX 2
does not emit UV light. Ozone is produced by a “silent”
Fig. 2. Apparatus for IJV cleaning experiments.
discharge when high-voltage ac is applied across a discharge gap
trometer. The AES spectra of these air-exposed samples formed by two concentric glass tubes, each of which is
showed carbon peak heights which were the same, to within wrapped in aluminum-foil electrodes. The ozone-generating
the experimental uncertainty, as the other air-exposed clean tubes are parallel to the UV tubes, approximately 6 cm away.
samples. The carbon peak heights were about 1 percent the UV, box 1 w,as used to expose samples simultaneously t,”
size of the oxygen peak heights (due to’ the 0 in SiO2) and 2537 A, 1849 A, and the ozone generated by the 1849-A
were also about 1 percent of the carbon peak height observed radiation. UV, box 2 permitted the options of exposing sam-
when pure graphite was examined at the same sensitivity. The ples to 2537 A plus ozone, 2537 i only, or ozone only.
amount of carbonaceous contamination on these air-exposed
samples is therefore a small percent of a monolayer. When UV/OZONE CLEANING EXPERIMENTS
samples initially showing good or excellent fringes in the steam The UV cleaning procedure works consistently only if the
test were exposed to air, the fringes generally deteriorated to samples to be cleaned are properly precleaned prior to UV
“orange peel” or “fog” after 15 min. This indicates that the irradiation to remove gross contamination [3]. There are a
carbon peak heights found in the Auger spectra were probably large number of possible precleaning procedures to choose
due to contamination adsorbed during the 15-min air ex- from. Several excellent reviews of cleaning procedures have
posure. Therefore, for studying the effectiveness of UV/ozone appeared in recent years [I61 -[I81 . The one used throughout
cleaning in air, the steam test, which could be performed these experiments consists of the following steps:
immediately upon the completion of an experiment, was 1) scrub the sample with a swab while it is immersed in
found to be a more sensitive indicator of the fractional mono- ethyl alcohol;
layer of hydrophobic contamination than AES. 2) agitate it ultrasonically in fresh ethyl alcohol;
3) boil it in fresh ethyl alcohol, and then agitate it ultra-
UV CLEANING APPARATUS sonically while the alcohol is hot;
To study the variables of the UV cleaning procedure, the 4) rinse it in running ultrapure (18 Ma-cm) water;
two UV cleaning boxes shown in Fig. 2 were constructed. 5) spin dry it immediately after the running water rinse.
Both boxes are made of aluminum and contain low-pressure Regardless of the contamination initially present on the
mercury discharge lamps and an aluminum stand with surface, steam testing subsequent to this cleaning procedure
Alzak [IO] reflectors. The two lamps produce nearly equal always showed “fog”; the contact angle generally was between
intensities of short-wave UV light, about 1.6 mW per cm2 for a 10 and 20°. After exposure to the UV/ozone in box 1, the
sample 1 cm from the tube. Both boxes contained room air (in precleaned surfaces invariably showed good or excellent
a clean room) throughout these experiments. The boxes are fringes.
completely enclosed to reduce recontamination by air cir- A number of quartz wafers were precleaned and exposed to
culation. the UV light in box 1 until good fringes were obtained. Each
Since only the light which is absorbed can be effective in of the wafers was then thoroughly contaminated with human
producing photochemical changes, the wavelengths emitted by skin oil [19], which has been a difficult contaminant to re-
the UV sources are important variables. The low-pressure move. The wafers were precleaned again, groups were exposed
mercury discharge tubes generate two wavelengths of interest, to each of the four UV/ozone combinations mentioned earlier,
1849 i and 2537 A. The 1849-i wavelength is important and the time to attain “good fringes” was measured. In each
because it is absorbed by oxygen, and it thus leads to the UV box, the samples were placed within 5 mm of the UV
generation of ozone [I I]. The 2537-i radiation is not ab- source.
sorbed by oxygen; it therefore does not contribute to ozone The wafers exposed to 2537 A + 1849 A + ozone in UV
generation. However, it is absorbed by most hydro- box 1 reached the “good-fringes” condition in 20 s. The
carbons [12], [I31 and also by ozone [I 11. The absorption samples exposed to 2537 i + ozone in UV box two reached
by ozone is principally responsible for the destruction of that condition in 90 s. With samples exposed to 2537 i with-
ozone in the UV box. Therefore, when both wavelengths are out ozone and to ozone without UV light it took 1 and IO h,
present, ozone is continuously being formed and destroyed. respectively, before “good fringes” could be observed.
An intermediate product of both the formation and destruc- The conclusion one can draw is that while both UV light
tion processes is atomic oxygen, which is a very strong oxidiz- without ozone and ozone without UV light can produce a slow
ing agent. cleaning effect, the combination of short-wavelength UV light
368 IEEE TRANSACTIONS
plus ozone such as is obtained from a quartz UV lamp prod.
duces a clean surface substantially faster. Although the 1849-A
radiation is also absorbed by many hydrocarbons, since the
ozone concentrations were different in the two UV boxes, it is
not possible from these experiments to isolate the cleaning
effect of the 1849-i radiation. The ozone concentrations were
not measured.
A “black-light” long-wave UV source, with an output
mostly between 3400 and 3800 i produced no noticeable
cleaning (as one would expect) even after 24 h of irradiation.
Another variable which can greatly affect the cleaning rate
is the distance between the sample and the UV source. Because
of the shapes of the UV tubes and of the Alzak reflectors
above the tubes and below the samples, the lamps in both
boxes are essentially plane sources. One might, therefore,
expect that the intensity of UV light reaching a sample would
be nearly independent of distance. This is not so, however,
when ozone is present, b:cause ozone has a broad absorption
band centered at 2600 A [I 1 I. At 2537 A, the absorption
coefficient is 130 cm-’ atm -I. The intensity I of the 2537-i
radiation reaching a sample therefore decreases as I =
, .e -130pd , where p is the average ozone pressure between
t;e sample and the UV source in atmospheres at O°C anddis
the distance to the sample in centimeters. Since the absorption
of photons precipitates the destruction of ozone, when a
quartz UV tube is used, both the ozone concentration and the
UV radiation intensity decrease with distance from the UV
source.
Two sets of identically precleaned samples were placed in
UV box 2. One set was placed within 5 mm of the UV tube;
the other, at the bottom of the box, about 8 cm from the
tube. With the ozone generator off, there was less than a
30-percent difference in the time it took for the two sets of
samples to show signs of fringes (about 60 versus 75 min).
When the experiment was repeated with the ozone generator
on, the samples near the bottom of the box took nearly ten
times as long to show fringes as the samples near the tube
(about 13 min versus 90 s). Similarly in UV box 1, samples
placed within 5 mm of the tube were cleaned up in 20 s versus
20 - 30 min for samples placed near the bottom of the box,
13 ems away.
The effectiveness of the UV/ozone cleaning procedure was
tested on a variety of contaminants with which a quartz
resonator may possibly come into contact during processing.
The contaminants were:
1) a cutting oii used with a diamond saw [20] ;
2) a beeswax and rosin mixture used to cement the crystals
into a loaf during the rounding operation;
3) a lapping vehicle [21 I ;
4) a mechanical vacuum pump oil [22] ;
5) DC 704 silicone diffusion pump oil [23] ;
6) DC 705 silicone diffusion pump oil [231 ;
7) a silicone vacuum grease 1231 ;
8) an acid (solder) flux [241 ;
9) a rosin flux from a rosin core lean-tin solder;
IO) human skin oils;
11) contamination adsorbed during prolonged exposure to
air;
ON PARTS, HYBRIDS, AND PACKAGING, DECEMBER 1976
12) a thin film of carbon (vacuum-evaporated to make the’
quartz surface conductive for an electron microscope study).
The contaminants were applied to clean pol.ished quartz
wafers. After the contamination, the wafers were precleaned,
and then exposed to UVlozone by being placed within a few
millimeters of the tube in UV box 1. When tested with the
steam test after a 60-s exposure, all the samples showed good
or excellent fringes. Samples showing fringes remained clean
indefinitely when stored under UV light in UV box 1.
Since AES could not differentiate between the silicon peaks
due to silicon in quartz and those due to the silicon in
silicon-containing contaminants, the removal of silicone dif-
fusion pump fluids was also tested on Alzak, which normally
has a silicon-free oxide surface, and on gold. AES examination
of the Alzak and gold surfaces following UVlozone cleaning
showed no traces of silicon present.
During the course of these studies, it was learned from
colleagues working on ion implantation for integrated circuits
that the usual wet cleaning procedures (with hot acids) failed
to remove the photoresist from silicon wafers which had been
exposed to radiation in an ion-implantation accelerator, pre-
sumably because of cross-linking of the photoresist. lon-
implanted silicon wafers, each with approximately a l-urn
coating of exposed Kodak Micro Resist 747 [251, were placed
within a few millimeters of the source in UV box 1. After 10 h
of exposure to UV/ozone, all traces of the photoresist were
removed from the wafers, as confirmed by AES.
IMPORTANCE OF PRECLEANING
While the UV/ozone successfully removed contaminants
such ,as the thick photoresist coatings and the carbon film
without any precleaning, the procedure cannot, in. general,
remove gross contamination. For example, when a clean
quartz wafer was coated with human skin oils and placed in
UV box 1 without any precleaning, even prolonged exposure
to UV/ozone failed to produce a low-contact-angle surface.
This is possibly due to the fact that human skin oils contain
inorganic sa!ts which cannot be removed by photosensitized
oxidation. The UV/ozone removed silicone vacuum grease
from surfaces which had been precleaned with ethyl alcohol,
as described earlier, and also from surfaces which had been just
wiped with a cloth to leave a thin film. However, when the
removal of a thick film was attempted, the UV/ozone removed
most of the film upon prolonged exposure; but it also left a
hard cracked residue on the surface. This may be due to.the
fact that many chemicals respond to radiation differently
depending on whether or not oxygen is present. In the presence
of oxygen many polymers, for instance, degrade when ir-
radiated; whereas, in the absence of oxygen (as would be the
case for the bulk of a thick film) these same polymers cross-
link. In the study of the radiation degradation of polymers in
air, the “results obtained with thin films are often markedly
different from those obtained using thick specimen . . .I’ [26] .
For the UV/ozone cleaning procedure to work reliably, the
surfaces must be precleaned: first, to remove contaminants
such as dust and salts which cannot be changed to volatile
products by the oxidizing action of UV/ozone, and, second, to
VIG AND LE BUS: UV/OZONE CLEANING OF SURFACES
remove thick films whose bulk could be transformed into an
UV resistant film by the cross-linking action of the UV light
which penetrates the surface.
UV CLEANING’OF METALS
The effectiveness of the UV/ozone cleaning procedure was
studied on several metal samples. After precleaning and UV/
ozone exposure, the steam test on oxide forming metal parts
such as nickel, copper, and silver produced a thin, continuous,
and uniform water film, thus indicating that the surfaces were
free of hydrophobic contaminants [27], [28]. The wettability
tests were confirmed again by AES. The wettability test was
not applied to gold surfaces because gold surfaces exposed to
air have always been found to be hydrophobic. This may be
due to the fact that gold is inherently hydrophobic, as has
been suggested by White [281, or because a clean gold surface
instantaneously adsorbs hydrophobic contaminants from the
air. If the hydrophobic nature of UVlozone-cleaned gold sur-
faces is due to adsorbed contaminants, these contaminants
must be adsorbed weakly enough to be readily desorbed in
vacuum because AES examination of UV/ozone-cleaned gold
surfaces indicated only trace amounts of carbonaceous con-
taminants to be present.
The accuracy of the AES examination of gold surfaces was
somewhat limited due to recontamination by carbonaceous
matter upon exposure to air. Gold samples, which had been
ion-bombardment-cleaned until no carbon was visible in the
Auger spectrum, were exposed to air for the same time it took
to mount the UV/ozone-cleaned samples in the Auger spec-
trometer. The carbon peak heights for the UV/ozone-cleaned
samples were the same, to within the experimental uncer-
tainty, as found for the ion-bombardment-cleaned samples,
about 3 percent of the Au 70-eV peak height. Such a small
carbon peak height corresponds to much less than 0.1 mono-
layer of carbonaceous contamination on the surface [29), and
represents an upper limit to the amount of hydrocarbons
remaining on the surface after UV/ozone cleaning. Although
reports have appeared in the literature which indicate that
atomic oxygen is strongly adsorbed on gold [30], [311, even
at room temperature, the Auger spectra of clean UV/ozone-
cleaned gold surfaces showed no evidence of such adsorption.
Prolonged exposure of the oxide forming metals to UV
light produced rapid corrosion. Silver samples, for example,
turned black in UV box 1 within 1 h. The corrosion was
observed even in UV box 2 when no ozone was being gen-
erated. The rate of corrosion increased substantially when a
beaker of water was placed in the UV boxes to increase the
humidity.
The corrosion can be explained by the fact that, as is
known in the science of air-pollution control, in the presence
of short-wave UV light impurities in the air-such as oxides of
nitrogen and sulfur combine with water vapor to form a
corrosive mist of nitric and sulfuric acids. However, in the
1 min or less which is required to clean a properly precleaned
surface, the corrosion problem is negligible for most ap-
plications. For extended storage of clean metal parts, the use
of controlled atmospheres in the UV box should eliminate this
problem.
369
UV/OZONE CLEANING-FACILITY
CONSTRUCTION CONSIDERATIONS
In the construction of a UV cleaning facility, one should be
aware of the safety hazards associated with short-wave UV
light. Exposure to intense short-wave UV light can cause
serious skin and eye injury within a short time. For the UV
boxes used in the above experiments, switches are attached to
the doors in such a manner that when the doors are opened,
the UV lamps are shut off automatically. If the application
demands that the UV lamps be used without being completely
enclosed (as might be the case, for example, if a UV cleaning
facility is incorporated into a thermocompression bonder),
then proper clothing and eye protection should be worn to
prevent skin burns and eye injury.
Another safety hazard is ozone, which is highly toxic. In
.setting up an UV cleaning facility, one must assure that the
ozone levels to which people are exposed do not exceed
0.1 ppm, the OSHA standard 1321.
Aluminum was chosen for the construction of the UV
cleaning boxes because it is resistant to corrosion and is also
the best easily available reflector in the short-wave UV range.
Most other metals, including silver, are poor reflectors in this
range.
Organic materials such as the plastic insulation on the leads
of some UV lamps should not be present in the UV cleaning
box. The box should be enclosed so as to minimize recon-
tamination by circulating air and to prevent accidental UV
exposure.
The most widely available sources of short-wave UV light
are the mercury arc lamps. Low-pressure mercury lamps in
pure fused quartz envelopes operate neat room temperature,
emit approximately 90 percent at. 2537 A, and generate suf-
ficient ozone for effective surface cleaning. ApproOximately 5
percent of the output of these lamps is at 1849 A. Medium-
and high-pressure UV lamps [33] generally have a much higher
output in the short-wave UV range. These lamgs also emit a
variety of additional wavelengths below 2537 A, which may
enhance their cleaning action. However, they operate at high
temperatures (the envelopes are near red hot), have a shorter
lifetime and a higher cost, and present a greater safety hazard.
The mercury tubes can be fabricated in a variety of shapes to
fit different applications.
In setting up an UV cleaning facility, one should choose an
UV source which will generate enough UVlozone to allow for
rapid photosensitized oxidation of contaminants; however, too
high an output at the ozone generating wavelengths may be
counterproductive because a high concentration of ozone can
absorb most of the UV light before it reaches the samples. To
maximize the UV intensity reaching the samples, the samples
should be placed as close to the UV source as possible.
One must exercise caution in using a mercury UV source in
a vacuum system because should the lamp envelope break or
leak, mercury would enter and ruin the usefulness of the
system. Mercury has a high vapor pressure; its removal from a
vacuum chamber is a difficult and time-consuming task. The
UV light can, however, be radiated into vacuum systems
through sapphire or high-purity quartz windows. A small
 370 IEEE TRANSACTIONS ON PARTS, HYBRIDS, AND PACKAGING, DECEMBER 1976

partial pressure of oxygen must be present in the system compression bondability of gold,” IEEE Trans. Parts, Hybrids,
oackag., vol. PHP-11, pp. 206-211, Sept. 1975.
during UV cleaning.
[‘31 V. E. Bottom, private communication.
[71 M. L. White, “Clean surface technology,” in Proc. 27th Annu.
SUMMARY AND CONCLUSIONS Symp. Frequency Control, US Army Electronics Command, Ft.
Monmouth, NJ, AD 771042, pp. 79-88,1973.
Bl D. 0. Feder and D. E. Koontz, “Detection, removal.and control
The UVlozone cleaning procedure has been shown’to be a
of organic contaminants in the production of electron devices,”
highly effective method of removing a variety of contaminants in Symp. Cleaning of Electronic Device Components and Mate-
from surfaces. It is a simple-to-use dry process which is in- rials (ASTM Special Tech. Pub. 246), pp. 40-65, 1958.
I91 J. Vig, H. Wasshausen, C. Cook, M. Katz, and E. Hafner,
expensive to set up; and operate. It can produce clean surfaces “Surface preparation and characterization techniques for
at room temperature, in a room atmosphere. quartz resonators,” in Proc. 27th Annu. Symp. Frequency
The variables of the UV cleaning procedure are: the con- Control, US Army Electronics Command, Ft. Monmouth, NJ,
AD 771042, pp.-98-1 12, 1973.
taminants initially present, the precleaning procedure, the
[IO1 Alzak is an aluminum alloy processed to provide high reflectiv-
wavelengths emitted by the UV source, the atmosphere be- ity. The Alzak process is licensed to several manufacturers by
tween ttie source and’sample, the distance between the source the Aluminum Co. of America, Pittsburgh, PA.
[III See, e.g., J. G. Calvert and J. N,. Pitts, Jr., Photochem-
and sample, and the time of,exposure. For surfaces which were is try, New York: Wiley, 1966, pp. 689-695,205-209.
properly (jrecleaned and placed within a few millimeters of an iI21 V. S. Fikhtengol’ts et al., Ultraviolet Spectrum of Elastomers
ozone producing UV source, the process consistently produced and Rubber Chemicals, New York: Plenum Press Data Div.,
1966.
a clean surface in less than 1 min. The combination of short- L. Lang, Absorption Spectra in the Uftraviolet and Visible
[I31
s wave UV light plus ozone produces a clean surface sub- Region, New York: Academic Press, Inc., 1965.
stantially faster than either short-wave UV light without ozone (141 Model No. R-52 Mineralight Lamp, Ultraviolet Products, Inc.,
San Gabriel, CA 91778.
or ozone without UV light. Clean surfaces remained clean
[I51 See, e.g., Encyclopaedic Dictionary of Physics, vol. 5, New
indefinitely during storage under UV/ozone, but prolonged York: Pergamon Press, 1962, p. 275.
exposure of oxide forming metals to UV/ozone in room air [I61 D. M. Mattox, “Surface cleaning in thin film technology,:’
Sandia Laboratories, Rep. SAND 74-0344, Jan. 1975. Copies are
produced rapid corrosion.
available from the National Technical Information Service,
The cleaning mechanism seems to be a photosensitized Springfield, VA 22151. This paper has also been reprinted and
oxidation process in which the contaminant molecules are distributed by the Thin Films Division, American Vacuum
Society, 335 East 45 Street, New York, NY 10017.
excited and/or dissociated by the absorption of short-wave UV [171 P. W. Morrison, Ed., Environmental Control in Electronic
light. Simultaneously, atomic oxygen is generated when Manufacturing, New York: Van Nostrand Reinhold Co.,
molec$ar oxygen is dissociated by the absorption of the (1973, chs. 6 and 7.
t181 Contamination Control Handbook, National Aeronautics and
1849-A radiation acd when ozone is dissociated by the absorp- Space Administration, NASA SP-5076, 1969. Copies available
tion of the 2537-A and longer wavelengths of radiation. The from NTIS, Accession No. N70-13566.
products of the excitation of contaminant molecules react [I91 The skin oils were applied by rubbing each of the clean wafers
against the forehead of one of the authors (J. W. L.).
with atomic oxygen to form simpler molecules such as CO;,
I201 P. R. Hoffman Co., Carlisle, PA.
and HgO, which desorb from the surfaces. f211 John Crane lapping Vehicle 3M. Crane Packing Co., Morton
Grove, IL 60053.
D21 Welch Duo-Seal, Sargent-Welch Scientific Co., Skokie, IL
ACKNOWLEDGMENT 60076.
[231 Dow Corning Corp., Midland, MI 48640.
The authors wish to thank E. Hafner for his advice [Xl Dutch Boy No. 205, National Lead Co., New York, NY 10006.
and continuing interest. The valuable contributions of K. [251 Eastman Kodak Co., Rochester, NY 14650.
Schwidtal and D. Fox, who performed the Auger electron WI H. V. Boenig, Structure and Properties of Polymers. New
York: Wiley, 1973, p. 246.
spectroscopy, are also gratefully acknowledged. 1271 ASTM standard method of test for hydrophobic surface films
by the atomizer test, designation F21-65, 1974 Annual Book of
ASTM Standards, Pt. 43, American Society for Testing and
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