Low-energy ion beamline scattering apparatus for surface science investigations

M. J. Gordon and K. P. Giapis

Citation: Review of Scientific Instruments 76, 083302 (2005); doi: 10.1063/1.1994987

View online: http://dx.doi.org/10.1063/1.1994987
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 REVIEW OF SCIENTIFIC INSTRUMENTS 76, 083302 共2005兲

Low-energy ion beamline scattering apparatus for surface science

investigations
M. J. Gordon and K. P. Giapisa兲
Division of Chemistry and Chemical Engineering, California Institute of Technology,
Pasadena, California 91125
共Received 9 May 2005; accepted 14 June 2005; published online 28 July 2005兲
We report on the design, construction, and performance of a high current 共monolayers/ s兲,
mass-filtered ion beamline system for surface scattering studies using inert and reactive species at
collision energies below 1500 eV. The system combines a high-density inductively coupled plasma
ion source, high-voltage floating beam transport line with magnet mass-filter and neutral stripping,
decelerator, and broad based detection capabilities 共ions and neutrals in both mass and energy兲 for
products leaving the target surface. The entire system was designed from the ground up to be a
robust platform to study ion-surface interactions from a more global perspective, i.e., high fluxes
共⬎100 ␮A / cm2兲 of a single ion species at low, tunable energy 共50–1400± 5 eV full width half
maximum兲 can be delivered to a grounded target under ultrahigh vacuum conditions. The high
current at low energy problem is solved using an accel-decel transport scheme where ions are
created at the desired collision energy in the plasma source, extracted and accelerated to high
transport energy 共20 keV to fight space charge repulsion兲, and then decelerated back down to their
original creation potential right before impacting the grounded target. Scattered species and those
originating from the surface are directly analyzed in energy and mass using a triply pumped, hybrid
detector composed of an electron impact ionizer, hemispherical electrostatic sector, and rf/dc
quadrupole in series. With such a system, the collision kinematics, charge exchange, and chemistry
occurring on the target surface can be separated by fully analyzing the scattered product flux. Key
design aspects of the plasma source, beamline, and detection system are emphasized here to
highlight how to work around physical limitations associated with high beam flux at low energy,
pumping requirements, beam focusing, and scattered product analysis. Operational details of the
beamline are discussed from the perspective of available beam current, mass resolution, projectile
energy spread, and energy tunability. As well, performance of the overall system is demonstrated
through three proof-of-concept examples: 共1兲 elastic binary collisions at low energy, 共2兲 core-level
charge exchange reactions involving 20Ne+ with Mg/ Al/ Si/ P targets, and 共3兲 reactive scattering of
CF+2 / CF+3 off Si. These studies clearly demonstrate why low, tunable incident energy, as well as mass
and energy filtering of products leaving the target surface is advantageous and often essential for
studies of inelastic energy losses, hard-collision charge exchange, and chemical reactions that occur
during ion-surface scattering. © 2005 American Institute of Physics.
关DOI: 10.1063/1.1994987兴

I. INTRODUCTION shell electronic excitation, momentum-assisted desorption,

secondary electron release, etc.兲.1,2 In addition, the kinetic
Ion-surface interactions are important in a variety of energy of the incoming ion can even “activate” surface-
fields such as plasma physics, surface analysis, materials specific processes, allowing epitaxy at lower temperature,
growth 共plasma-enhanced chemical vapor deposition and stimulation of surface reactions/adatom diffusion, synthesis
ion-beam assisted deposition兲, and semiconductor dry etch- of metastable material phases,3 and control of film density,
ing. In many of these application areas, collision energies are
texturing, and stress 共for a review, see Ref. 1兲. However, the
specifically kept below 1 keV to have preferential energy
research literature on low energy ion-surface collisions is
deposition at the target surface only, i.e., short collision cas-
relatively sparse because of the experimental challenges as-
cades to provide high selectivity to the topmost atomic layers
without damaging the underlying material. This regime of sociated with providing sufficient ion beam current at low
energies 共⬍1 keV兲 represents an important window in the impact energy for scattering, material growth, and etching
energy space of ion-surface interactions because many studies. We have set out to probe this little-studied energy
threshold processes occur at low energy 共sputtering, core range by developing an ion beamline scattering system to
investigate a wide variety of ion-surface interaction phenom-
a兲
Author to whom correspondence should be addressed; electronic mail:
ena below 1 keV. This article describes the design and con-
giapis@cheme.caltech.edu struction of our system and its application to three proof-of-

0034-6748/2005/76共8兲/083302/15/$22.50 76, 083302-1 © 2005 American Institute of Physics

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 083302-2 M. J. Gordon and K. P. Giapis Rev. Sci. Instrum. 76, 083302 共2005兲

FIG. 1. Schematic of the low-energy ion beamline scattering apparatus showing various sections: 共a兲 ICP plasma source and extraction optics, 共b兲 high-voltage
floating region including both steering magnets and decelerator, 共c兲 scattering chamber, and 共d兲 scattered product detector.

concept examples: elastic binary collisions at low energy, 共⬎100 ␮A / cm2兲 of a single ion species at low impact energy
core-shell charge exchange collisions involving Ne+, and re- 关50–1400± 5 eV full width half maximum 共FWHM兲兴 onto a
active scattering of CF+3 / CF+2 off Si. grounded target to facilitate ultrahigh vacuum 共UHV兲 scat-
Our design philosophy has been to take an inductively tering studies using both inert and reactive beams. Space
coupled plasma 共ICP兲 source and couple it to a high-voltage charge repulsion is controlled by transporting the ions at high
ion beam transport line with magnetic mass filtering to pro- voltage, with mass filtering, beam steer, and quality adjust-
vide a clean ion beam surface probe with high current ments all occurring on the accelerated beam.
共⬎100 ␮A / cm2兲 and tunable energy 共⬃50 eV–1 keV兲. The particle flux from the target is analyzed with a
Space charge repulsion between the ions, which usually pre- triple-differentially pumped hybrid detector with both energy
cludes high current at low energy, is circumvented using the and mass dispersion. This system combines an electron im-
accel-decel scheme for transport. In this arrangement, ions pact ionizer, hemispherical electrostatic sector, and quadru-
are created at the desired collision energy in the plasma pole mass filter in series with single ion counting on the rear
source, extracted and accelerated to high transport energy 共to end so that small signals of both ions and neutrals can be
fight space charge repulsion兲, and then decelerated back analyzed. With such a scheme, the collision kinematics,
down to their original creation potential right before impact- charge exchange, and chemistry occurring on the target sur-
ing the grounded target. In this way, the beam current is high, face can be separated by fully analyzing the scattered prod-
the collision energy is easily tunable 共by floating the plasma uct flux. In the next few sections, key design aspects of the
source above ground兲, and the target is always kept plasma source, beamline, and scattering system are empha-
grounded. The ICP-based beamline is a generic and robust sized to highlight why low-energy ion beam experiments are
system because any ion created in the plasma can be indi- so demanding and how to work around physical limitations
vidually singled out and delivered to the target as a clean associated with high beam flux at low energy, pumping re-
surface probe composed of only one species and one charge quirements, beam focusing, and scattered product detection.
state. Species scattered by or originating from the target sur-
face are analyzed with a hybrid detector which allows simul- A. Design philosophy
taneous mass and energy filtering—so the kinematics, charge
As inferred in the introduction, a high-current ion beam
exchange, and chemistry which occurs upon scattering can
cannot be exposed to decelerating fields during transport,
be investigated.
otherwise it will diverge. Unfortunately, space charge repul-
sion between the ions can only be “controlled” using
II. DESCRIPTION OF THE INSTRUMENT
high transport energy 共Langmuir–Child law兲,5 continual
The low-energy, ion beamline scattering system is refocusing,6 or by artificially neutralizing the beam by add-
shown schematically in Fig. 1, with technical specifications ing electrons externally 共see Lawson7兲. The latter two op-
given in Table I. The system is composed of four main sec- tions are usually reserved for very high current beams 共mA兲
tions: 共a兲 ICP ion source with extraction optics; 共b兲 high used in particle accelerators. On the laboratory scale, con-
voltage beamline with magnetic mass filter, focusing ele- tinual refocusing is cumbersome and usually limited to
ments, and deceleration optics; 共c兲 scattering chamber; and highly symmetric systems 共without a mass filter兲; as well,
共d兲 scattered product detector. Specific construction details of artificial neutralization is not an option because a neutralized
each section of the instrument can be found elsewhere.4 The beam cannot be mass filtered. The solution is therefore
design philosophy of the beamline was to provide high fluxes simple—just transport and mass filter the beam at high ac-
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 083302-3 Low-energy ion beam scattering apparatus Rev. Sci. Instrum. 76, 083302 共2005兲

TABLE I. Design and operational specifications for the low-energy ion beamline scattering system.

Ion source Inductively coupled plasma, 2-turn solenoid, 1 kW @ 13.56 MHz

Source pressure 0.5–10 mTorr

Beamline acceleration voltage 10–20 keV
Magnetic mass filter 60°, 300 mm radius of curvature, 50 mm air gap
⬃0.8 T max field, water cooled, 300 V–16 A supply
Field stability: Hall feedback, ±3 G
Ion deflector magnet 10°, 1300 mm radius of curvature, 50 mm gap
共fast neutral removal兲 ⬃1800 G max field, 600 V–2 A supply
Extractor four elements 共1 floating extraction electrode+ 3 biased separately兲
Beam shaping four element asymmetric Einzel 共before 60° magnet兲
Y-axis divergence corrector 共after 60° magnet兲
dc quadrupole doublet 共eight elements — after mass defining slit兲
Decelerator Asymmetric Einzel triplet+ steering quadrupole+ guard electrode
Beam energy ⬃20–1500 eV± 5 eV FWHM 共maximum兲 共measured @ target with electrostatic sector兲
Beam size 1–3 mm diameter, tunable
Beam current 250 ␮A / cm2 Ar+ @ 50 eV, 150 ␮A / cm2 O+2 @ 50 eV
Scattering chamber pressure ⬍1 ⫻ 10−8 Torr 共beam on @ 500 ␮A / cm2, plasma source @ 5 mTorr兲
Scattered product detector Electron impact ionizer—10 mA emission
90° hemispherical sector filter with Herzog plates, 58 mm radius
rf/dc quadrupole: 19 mm diam poles @ 2.22 MHz, 300 W
Ion counter Daly-type conversion dynode @ -15–30 keV
Fast organic scintillator+ PMT tube 共in vacuum兲
Other facilities Sputter cleaning, anneal to 900 °C, Ar+ SIMS 共scattering chamber兲
XPS 共in-vacuum transfer兲

celeration voltage.8–11 What one desires is a symmetric 共usu- B. ICP plasma source and ion beam extraction
ally cylindrical兲, pumpable, high-voltage “shield” around the
ion beam column throughout the beam transport line 共includ- One of the most important choices in any beamline de-
ing the mass filter兲 while working with a grounded target. sign is the ion source itself. The source should have high
This situation is experimentally demanding because it re- conversion efficiency, low operating pressure 共to avoid gas
quires a pumpable high-voltage envelope around the propa- loading the beamline兲, well-defined ion creation potential,
gating ion beam to shield it from the grounded beamline narrow ion energy spread, and compatibility with both inert
chambers which maintain the vacuum. Such an approach has and reactive working gases. Traditionally, Freeman-type,
been used successfully for a 10 keV beamline by construct- low-voltage dc arcs have been the ion source of choice be-
ing an electrostatic mesh chamber inside a grounded vacuum cause of their high current and low pressure operation.3,12,13
shell.3 We have taken a different approach whereby the entire However, arc sources require frequent filament changes 共a
vacuum system itself 共chambers, valves, feedthrus, etc.兲 is few tens of hours for high beam currents兲 and contaminate
floating below ground at the beam transport energy the beam with useless ions resulting from reaction of the
共−20 keV兲. This philosophy avoids all the problems associ- working gas with the hot filament used to sustain the dis-
ated with high-voltage isolation inside vacuum where space charge. We have solved these problems by designing an ICP
is tight and pumping conductance must be maximized. All source and extraction system for our beamline which can
the isolation problems are brought outside of vacuum and we satisfy all the above criteria along with clean, sustained
can avoid making a chamber within a chamber. operation—even with corrosive working gases. The induc-
The high-voltage floating section of our beamline sys- tive coupling scheme is ideal because it can provide high ion
tem, shown in Fig. 1, extends from the end of the premagnet density 共1011–1013 / cm3兲 with low plasma potential
Einzel triplet up to and including the decelerator where it 共⬍20 eV兲 and narrow ion energy spread 共2–5 eV兲, all at low
joins to the grounded scattering chamber. The floating sec- working pressure 共0.1–5 mTorr兲 共for a summary of ICPs, see
tion includes the 60° sector magnet, mass slit, quadrupole Refs. 5 and 14兲.
doublet, 10° steering magnet, and decelerator. Electrical A schematic of the ICP plasma reactor and extraction
breaks are used at both ends to isolate the floating section electrode system is shown in Fig. 2. The plasma reactor is
from the rest of the system with the premagnet Einzel triplet constructed from a 4 in. o . d . ⫻ 4 in. alumina tube 共a Pyrex
共lens number 3兲 and decelerator 共lens numbers 2 and 3兲 func- version is also used兲 with alumina end caps sealed by o-rings
tioning as transfer lenses to shield the beam between sec- to an 8 in. Conflat flange fitted to the front of the beamline.
tions. The vacuum chambers themselves are supported using The plasma is excited by a two-turn, rf-solenoid antenna ex-
a poly-vinyl chloride scaffold system to stand off the floating cited through a ⌸ network at 13.56 MHz. A grounded, cop-
potential and the vacuum pumps 共CT7 cryopump after the per Faraday shield 共similar to Ref. 15兲 is situated between
60° sector, 200 L / s turbo on the quadrupole doublet兲 are also the antenna and reactor to eliminate all capacitive coupling
isolated with electrical breaks. between the plasma and rf antenna. It is imperative that ca-
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 083302-4 M. J. Gordon and K. P. Giapis Rev. Sci. Instrum. 76, 083302 共2005兲

matically removed by the sector field when the pass mass is

refocused after the magnet at the field image point 共the mass
slit兲.17,19 The 60° sector magnet has 8 in. diam poles, hex-
agonal shoes, 50 mm air gap to allow clearance for the beam-
line flight tube 共1.5 in. o.d., floating at −20 keV, insulated by
mica sheets兲, and adjustable mass slit 共0–13 mm wide
⫻ 18 mm high兲 downstream. Since the air gap was not small
compared to the shoe height 共and pole size兲, a significant
fringe field extended beyond the physical pole boundaries.
As such, it was necessary to account for the “virtual” pole
boundaries using an extended fringe field method20,21 to cal-
culate the effective radius of curvature 共⬃11 in. instead of 8
FIG. 2. Design schematic of the ICP plasma source and ion beam extraction in., as given by the pole diameter兲. In addition, it was abso-
electrodes. Both the reactor and electrode set have cylindrical symmetry. lutely necessary to actively control the magnet at ⬃10 Hz
The extraction aperture where the virtual plasma sheath forms is electrically
floating with the plasma itself. Also, two versions of the plasma reactor with Hall probe feedback to keep the ion beam from drifting
共pyrex and alumina兲 were used. on the target. With this system, the field could be held within
±3 G with the magnet at maximum strength 共⬃0.8 T兲.
pacitive coupling be minimized to keep the plasma potential One should note that a magnetic sector with parallel pole
low 共⬍20 V兲 and ion energy distribution narrow.14 The en- shoes does not produce a stigmatic image of the source
tire plasma volume can be floated above ground by an inter- point.17 Such an effect manifests as an ion beam which enters
nal molybdenum bias electrode 共Ti and Ta were also used, the magnet having circular cross section, but leaves the field
depending on the plasma chemistry兲 connected to a dc sup- elongated in the nondispersive 共Y兲 direction as an ellipse
ply which sets the final beam energy. Operating pressures are with less on-axis brightness.17 Stigmatic focusing with a sec-
typically 1–5 mTorr for input powers ranging from 300 to tor usually requires tilting the pole shoes to create a slightly
800 W. In addition, highly electronegative gases 共CF4 , O2兲 inhomogeneous field in the radial direction to offset the ra-
were frequently blended with small amounts of Ar to provide dius of curvature for different flight paths. The lack of a
sufficient electrons for good inductive coupling and power stigmatic image was not deemed so critical in our design;
transfer from antenna to plasma. Mixing gases in the source however, the loss of current due to divergence in the Y di-
is not a great concern because the beam is mass filtered rection was considered important. Therefore, a weak electro-
downstream. static “bunching” field in the Y direction 共+500–1000 V off
The ion beam 共plasma beam兲 is extracted from the ICP the beamline floating potential兲 after the magnet was added
source through a floating extraction aperture 共5 mm sharp- to recover the otherwise lost beam current rather than tilting
edged hole, 120° bevel兲 and triode accel-decel lens system the pole shoes.
共for example, see Refs. 16 and 17兲. Smooth field variation in When the ion beam passes through the mass slit, it ex-
the vicinity of the “virtual” sheath of the plasma is necessary hibits a crossover point in the dispersive direction 共X兲, but an
to form a uniform cross section ion beam column.17 In close elliptic cross section in the nondispersive direction 共Y兲. Un-
proximity are three cylindrically symmetric electrostatic fortunately, the sector removes the inherent cylindrical sym-
lenses in series 共puller, buncher, and front beamline accel metry of the ion beam as extracted from the plasma because
electrodes兲 with tantalum cover plates to prevent excessive of the field “handedness.” Since it is desirable to decelerate a
sputtering. The final design for the extractor electrode system symmetric, parallel beam having circular cross section and
was the result of both space charge simulations 共SIMION18兲 as small waist, we felt that an additional focusing step was nec-
well as extensive operational testing. The front beamline essary after the mass slit. A dc quadrupole doublet was used
electrode is the main acceleration step and is joined to the in the drift space between the mass slit and decelerator to
premagnet Einzel triplet 共see next section兲 through stainless affect the symmetry correction. A quadrupole field was cho-
steel mesh tubing. Since the gas load to the beamline is of sen because its planar symmetry seemed better suited to fix
paramount importance, the extractor was design to be as unequal divergences of the beam in the X and Y axes. In
“open” as possible to maximize pumping, so that background addition, a quadrupole field provides stronger focusing ac-
gas collisions are minimized. A 1000 L / s drag turbo directly tion and is shorter overall than an axially symmetric lens
below the extractor functions as the main differential pump- system.7 The doublet is operated with Y correction first, fol-
ing step, keeping the extraction chamber at 5 ⫻ 10−6 Torr lowed by X 共first quad - ±Y plates variable, second quad - ±X
with the plasma source running at 5 mTorr. plates variable兲 with the plate voltages derived from power
supplies floating on the beamline acceleration potential.
It is well known that collisions of energetic ions with
C. High voltage beamline background gas atoms can generate fast neutrals through
After the ion beam is extracted from the plasma and charge exchange processes.22,23 In fact, fast neutral beams
accelerated to ⬃20 keV by the front beamline electrode, the are produced using this method by sending a fast ion beam
beam waist is adjusted by an Einzel triplet to coincide with through a charge exchange cell containing background gas.
the source point of the magnetic sector field. In this way, The process of fast neutral generation, although much less
angular divergence of the beam at the source point is auto- significant in our system, could possibly influence scattering
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 083302-5 Low-energy ion beam scattering apparatus Rev. Sci. Instrum. 76, 083302 共2005兲

FIG. 3. Design schematic of the ion beam decelerator, high-voltage beam-

line electrical break, and target region.

results. Since it is extremely difficult to measure fast neutrals

quantitatively, we have therefore taken the approach to rid
the beam of fast neutrals on purpose, even if they may not FIG. 4. Simplified schematic of the power supply bias scheme for the beam-
exist to a significant degree in our system. This is simply line. All acceleration, focusing, and steering lens supplies float atop the main
done by deflecting the ion beam 10° with a small magnetic beamline bias 共20–1500 eV兲 which controls the final impact energy. A sepa-
rate plasma bias supply is ramped up in direct correspondence with the
sector field right before the decelerator entrance so that any beamline float bias.
fast neutrals in the upstream beam are not within line of sight
of the target. The short flight distance through the decelerator
quad centerline float, and the four steering plates are all in-
to the sample is unimportant because this region is held at
dependently adjustable. Finally, a fully grounded end cap
high vacuum conditions 共1 ⫻ 10−8 Torr兲. The small sector
over the quad exit shields the target from any high-voltage
has square pole shoes, 2 in. air gap, and gives a 10° deflec-
fields.
tion to the ion beam with ⬃1300 mm turning radius. Since
the deflection is small and the curvature radius extremely
large, the beam symmetry is not disturbed to any great E. Beamline bias scheme
extent. Due to the “floating beamline” design principle, it was
deemed easier to adopt a floating power supply bias scheme
D. Deceleration for the focusing elements on the HV section. In this design,
Deceleration lens schemes for high-energy ion beams smaller, more accurate supplies float on the main beamline
have traditionally been approached from two very different bias voltage to provide fine beam steering control. A sche-
points of view. Experiments using ion implanters 共⬎50 keV matic of this system is shown in Fig. 4. In addition, all beam-
transport energy, mA currents兲 have demonstrated that ul- line power supplies 共except the plasma bias兲 float on top of a
trashort, extremely strong slowing fields 共50 kV in 10–20 separate dc supply that is ramped up identically with the
mm兲 using two or three thin electrostatic lenses provide the plasma bias voltage. In this way, exactly the same extraction
best spots.13,24,25 On the other hand, ␮A beam currents at and focus conditions with respect to earth occur for all beam
lower transport energies are more successfully dealt with energies. It is necessary to separate these two voltages be-
using longer, more complex schemes 共3–6 tube-like cause the 13.56 MHz noise from the plasma electron oscil-
electrodes兲.26–29 Our decel system is rather simple 共Fig. 3兲 lation causes havoc in the regulator circuits for the rest of the
with an asymmetric Einzel triplet 共short-long-short兲 followed beamline power supplies. Incidentally, this oscillation is
by a large inner diameter, short quadrupole with a grounded too high in frequency to affect the inherent ion beam
end cap to shield the target from any high-voltage fields. The self-neutralization.3 Also, the vertical bunching plates and
Number 2 and 3 lenses of the triplet are run more negative quadrupole doublet float on the beamline high voltage
than lens Number 1 to pinch the beam after a first stage of 共−15–20 kV兲 while the steering quad supplies and quad
slowing occurs between the main beamline and decel Num- shield float atop the steering quad centerline potential
ber 1. It is thought that the potential drop of a few kV in this 共−6–10 kV兲.
region 共between decel Numbers 1 and 2兲 aids in neutralizing
the beam space charge for the rest of the deceleration be- F. Scattering chamber
cause slow electrons are trapped in the beam channel.27 The The UHV scattering chamber was custom built in-house
end of decel Number 3 and the entire quad extend into the to have two pumping stages mounted inside the overall
grounded scattering chamber. The quadrupole exit setup for chamber to differentially pump the scattered product beam
final beam steer is short and stubby so the field asymmetries leaving the target. Each stage has a 2 mm diam skimmer and
near its plate electrodes are so far away from the bunched its own dedicated turbopump. Also, a capacitor deflector is
beam that they are irrelevant. Operation of the quad is very situated between the two stages so charged species can be
weak with only 200–400 V of asymmetric steer capability on removed from the scattered product signal if desired. The
a centerline floating potential of −6 to −10 kV. A floating target sample rests on a five-axis goniometer with heating to
circular shield encloses the quad to screen the beam from the 900 °C and scattering experiments are usually carried out at
grounded walls of the scattering chamber. The quad shield, a 90° lab angle in specular reflection. The scattering chamber
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 083302-6 M. J. Gordon and K. P. Giapis Rev. Sci. Instrum. 76, 083302 共2005兲

itself is pumped by a CT8 cryopump and 1300 L / s maglev

turbopump to maintain the pressure in the 10−9 Torr range
during bombardment at maximum beam current.
For specular reflection and 90° lab angle, the target is
inclined 45° from the beam propagation axis. With low en-
ergy beams, it is well documented that an inclined target can
have significant impact on the actual versus “desired” scat-
tering angle as the incident beam energy is varied.30 To avoid
this problem, a rotatable, tantalum beam flag with 2 mm
diam hole is place directly in front of the target as a shield,
perpendicular to the beam propagation axis. In this way, the
beam sees a totally symmetric decelerating field, rather than
the inclined target. Thus, the target angle does not modify the
overall lab scattering angle for different incident beam ener-
gies 共see Sec. III for verification of this fact兲. In addition, the
current on both the beam flag and target can be monitored
separately to tune the ion beam steering and focus.
Finally, the scattering chamber is outfit with a miniature
180° hemispherical sector energy analyzer that can be moved
into and out of the beam path directly at the target position to
measure the incident beam energy distribution for every in-
cident beam condition. The analyzer is ⬃23 mm radius with
Herzog corrector plates, inlet Einzel triplet, and channeltron
detector.

G. Scattered product detector

The most idealized scattering experiment would involve
the detection of all species leaving the target surface, both
ions and neutrals, within the space of mass and energy. This FIG. 5. 共a兲 Simplified schematic of the scattered product detector showing
differential pumping stages, ionizer, energy and mass filter, and Daly-type
scheme would allow the kinematics, charge exchange, and ion counting detector. 共b兲 Example ion trajectory calculation for 50 eV Ar+
chemistry of scattering phenomena to be separated. Toward at 15 eV pass energy showing various lenses in the scattered product detec-
this goal, our detection system combines an electron impact tor 共Rp= repeller, G = grid, Ex= ion extractor, L1 . . 3 = ionizer focus, E1 . . 3
ionizer, electrostatic sector energy filter, and high transmit- = Einzel transfer, Hz= Herzog plates, Ho, Hi= outer and inner hemispheres,
T1 . . 4 = quad transfer, and Q = quad centerline float兲. All lenses float off the
tance rf/dc quadrupole mass filter with an extremely sensi- sector retard voltage used to scan the kinetic energy pass band.
tive ion counting system. Figure 5共a兲 shows a simplified
schematic of the detector system. We believe the electrostatic
sector with sequential quad provides several advantages over ionizer can be sufficiently “tuned” to provide ionization at a
traditional time-of-flight 共TOF兲 techniques: 共1兲 the sector can uniform ion creation potential of narrow energy width
be placed very close to the sample surface; 共2兲 energy analy- 共艋1 eV兲.4 All lens elements in the ionizer are fully tunable
sis does not require beam chopping; 共3兲 energy and mass and emission currents up to 10 mA at 100 eV electron energy
dispersion are separated inherently; and 共4兲 it is easy to are possible. The ionizer itself is positioned directly behind
implement an electron impact ionization scheme to detect the second skimming aperture 共2 mm兲 on the back of the first
low energy neutrals 共TOF requires Eneutral ⬎ 1–3 keV for di- differential pumping stage with the ionizing volume situated
rect detection with a microchannel plate兲. only 80 mm from the sample surface. An Einzel triplet lens
The design of the scattered product detector was based system was added to the rear of the ionizer to provide better
on the ionizer and pole set 共19 mm diameter兲 from an Extrel extraction and imaging of ions on the inlet slit of the elec-
QPS system, with the electrostatic energy filter, transfer op- trostatic sector. The triplet lens system floats off the electro-
tics, and ion counting system designed and fabricated in- static sector retard voltage ramp to provide a nearly constant
house. The ionizer has a Whetstone bridge filament structure focusing power over all ion energies. SIMION was used to
with axial entrance and ion extraction, along with five lens design the lens system and operating voltages to provide
elements after the grid to enable different extraction modes. uniform transmittance of all ion energies irrespective of re-
Specifically, the ionization volume size and ion creation po- tardation level.
tential can be easily changed by tailoring the grid, extractor, For the 90° electrostatic sector, spherical electrodes
and focus plate voltage ratios. This is a very important point 共gold-plated oxygen-free high-conductivity copper兲 with 50
because any variation in ion creation potential in the ionizing and 65 mm radii were used, giving a mean sector radius of
volume 共most ionizers have this problem兲 causes an artificial 57.5 mm 共⬃2.25 in. 兲. Herzog corrector plates were posi-
linewidth in the energy spectrum. We made specific intent to tioned at the inlet and exit of the sector to appropriately
minimize this effect by fully characterizing our ionizer sys- terminate the deflection field, and a four-element Einzel-type
tem. Experiments with the electrostatic sector show that the transfer lens assembly is used to transport and tightly focus
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 083302-7 Low-energy ion beam scattering apparatus Rev. Sci. Instrum. 76, 083302 共2005兲

exiting ions onto the entrance aperture of the rf/dc quad. The side by sputter coating with 1500 Å of aluminum to provide
energy filtering action of the sector is accomplished by slow- a grounded surface and light shield for the PMT. The PMT
ing down or speeding up ions which enter the sector to the tube itself was housed inside vacuum with a ␮-metal mag-
pass energy of the analyzer 关constant acceptance energy netic shield and pressed firmly against the rear of the scintil-
共CAE兲 mode兴 by sweeping the retarding voltage from lator. The tube is run in pulse count mode with the photo-
−Epass kinetic energy 共KE= 0兲 up to some maximum scanned cathode at positive high voltage to further reduce spurious
energy. A pass energy of 15 eV was used for most of our electron pulses.
scattering experiments because it provided good energy reso-
lution and adequate transport energy through the quadrupole. III. BEAMLINE PERFORMANCE
Both the inlet triplet and four-lens exit system on the sector The major goal of our endeavor was to construct a mass-
analyzer were designed through extensive SIMION simulation. filtered ion beam system which could deliver reasonable flu-
An example ion trajectory calculation for a 50 eV Ar+ beam ence 共100s of ␮A / cm2兲 at low beam energy 共50–1000 eV兲
retarded to the 15 eV pass energy of the analyzer is shown in for surface scattering studies. The real test of such a system
Fig. 5共b兲. Very specific voltage ratios between the inlet and indeed lies in the mass-filtering capability, available current,
exit lens elements were required for proper focus over a wide and scattered product detector performance. As such, we
range of ion energies. As such, a custom, computer con- sought to answer several questions, which are addressed in
trolled power supply system was built for the sector analyzer, the following sections:
inlet, and exit Einzel lens systems.
For the quadrupole, the dc rod voltages were derived 共1兲 Can isotopically pure beams be generated from a com-
directly from the rf drive to the poles by vacuum tube diodes. plex plasma gas mixture 共i.e., one commonly used for
This unique feature allowed the entire rod set and match box dry etching兲?
circuitry to be floated above ground. The ability to artificially 共2兲 What is the current delivery versus beam energy?
move the quad centerline potential above ground was abso- 共3兲 Is the ion beam energy distribution at the target suffi-
lutely necessary because the ion flight energy within the ciently narrow for scattering experiments?
quad must ramp with the energy analyzer retard voltage— 共4兲 Can the impact energy be tuned easily by floating the
otherwise, the flight energy through the quad is not constant. entire ICP plasma source above ground?
The centerline quad potential was attached directly to the
main retarding voltage ramp of the energy filter. In this way,
A. Mass separation
ions fly through the quad at exactly the pass energy of the
energy filter, irrespective of what kinetic energy is being The mass resolution of the ion beamline system was
scanned. Finally, to further decrease the residual gas back- evaluated by forming isotopically clean ion beams from a
ground and prevent ion forming collisions within the quad, a complex plasma gas mixture that is typically used for dry
special cryocooled shroud at 30 K was placed around the etching of SiO2. This situation represents an extreme case of
quad pole set 共not shown兲. beam contamination and can be used to test the ability of an
The extremely small ion signals 共10−15–10−17 Torr effec- ion beam system to give high mass resolution and produce
tive pressure兲 that are generated by electron impact ioniza- clean, pure beams. Figure 6 shows a typical mass sweep of
tion of secondary neutrals leaving the target surface require the beams that can be formed by extracting all the ions from
an extremely sensitive, single-ion type counting system. The a CF4 / Ar/ O2 plasma mixture running at 500 W plasma
problem is unavoidable because ionization by electron im- power. The plot was formed by sweeping the field strength of
pact is quite inefficient. The most well-designed magneti- both the 60° sector and 10° deflector magnets simultaneously
cally confined ionizers running in space charge limited mode via computer control while maintaining the beam energy at
at 10 mA of emission current can only provide a conversion 100 eV and beamline transport voltage at −12 keV. The mass
efficiency of maybe one part in 104.31 This dictates that the exit slit on the 60° magnet was set to a 3 mm width and the
ion detector must be able to count every single ion that is beam current at the target location was measured with a Far-
generated. For this purpose, we developed a hybrid ion aday cup 共500 ␮m diam inlet aperture兲. It can be seen that all
counting system based on the approach of Daly.32 Ions exit- the ions in the plasma source are easily resolved by the sec-
ing the quad are “bunched” by a three element immersion tor magnet and can be transported to the sample as isotopi-
lens 共+200 V , −3 kV, −6 kV兲 at the rear of the quad and they cally pure beams for scattering experiments. Higher resolu-
are subsequently accelerated to −15 to −30 kV by a conver- tion is possible with smaller exit slit size, but better mass
sion dynode. When the high energy ions strike the aluminum separation is not needed for most of the beams shown. Mass
dynode surface 共⬃45°, angle of maximum secondary elec- sweeps of this type demonstrate the power of the beamline
tron emission兲, a shower of secondary electrons 共15–30 keV system for plasma diagnostics as well as a direct feedback
with respect to ground兲 is created. These secondary elec- mechanism for tuning plasma operation to obtain the highest
trons, in turn, are accelerated away from the dynode and yield of the ion species of interest.
converted to light 共␭max = 408 nm兲 by a plastic scintillator
共⬃3–4 photons/ e− for Bicron BC408兲. Finally, the resulting B. Target current
photon pulses are registered by a special bi-alkali photocath- One of the most important design criteria for the beam-
ode photomultiplier tube 共PMT兲 with maximum sensitivity at line was high beam current at low impact energy. This is
400–420 nm. The scintillator was metallized on the dynode made possible by the accel-decel scheme where ions are cre-
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 083302-8 M. J. Gordon and K. P. Giapis Rev. Sci. Instrum. 76, 083302 共2005兲

FIG. 6. Beam currents measured via Faraday cup 共0.5 mm inlet diameter兲 at
the target position for a CF4 / O2 / Ar 共48: 14: 38兲 plasma running at 3.5 mT
and 500 W. Beamline transport voltage was −12 keV and the mass slit was
set to 3 mm width. SiF+ and SiF+2 species result from attack of the pyrex
plasma reactor used for this experiment. Also, O2 was added to the plasma
mix to prevent CF2-like polymer deposition on the reactor walls at high CF4
blending ratios.

ated in the plasma at the impact energy, accelerated to high

transport energy, and then decelerated near the target back to
their initial creation potential. The success of such a scheme
depends on having high ion density in the plasma, efficient
extraction, minimal current loss during transport, and proper
focus correction during deceleration. However, the entire
system cannot deliver high current at low energy unless
all of the beamline components function together in unison
through proper beam transport between each stage. Thus, FIG. 7. Current density at the target for: 共a兲 Ar+ and 共b兲 O+2 and O+ ion
beams for different final beam energies. In each case, the beamline transport
overall system performance can be evaluated directly voltage was maintained at ⬃13 keV, decelerator was tuned to optimize
through the available beam current. Typical data for our sys- beam current through the 2 mm diam beam flag aperture. A neat Ar plasma
tem are shown in Fig. 7. The ion arrival rate is represented in and O2 / Ar plasma at ⬃500 W and 3–5 mTorr were used.
terms of beam current density on the target delivered through
the 2 mm diam flag aperture 共see discussion in Sec. II F兲.
Current density at the target is more useful for direct com- In general, higher currents are possible if the ICP plasma is
parison with an arrival rate of one monolayer per second driven harder and stronger extraction conditions are used to
共1 ML/ s ⬃ 320 ␮A / cm2 for Si兲. Figure 7共a兲 shows an Ar+ compensate the increased space charge density that occurs
beam extracted from a pure Ar plasma discharge running at when ions leave the virtual sheath at the floating extraction
500 W and 5 mTorr. Atomic and molecular oxygen beams aperture 共see Sec. II B兲. Beam currents below 100 eV can
extracted from an Ar/ O2 plasma are also given in panel共b兲. also be increased 共up to ⬃1.5 times兲 if the decelerator is
Argon was added to the oxygen discharge to increase induc- specifically tuned for stronger focusing action and the steer-
tive power coupling with the rf antenna using a mixing ratio
ing quad plates directly in front of the target are run signifi-
of Ar: O2 of 1.3: 1 and 5 mTorr operating pressure. The beam
cantly positive to pinch the beam inward. The ion fluxes
currents on these plots were measured for identical extraction
shown for the Ar+ and O+2 beams are at least 1 ML/ s for
conditions 共puller and buncher voltages held constant兲 over
all beam energies with the main beamline transport energy at Eimpact 艌 100 eV. This current level into a 2 mm spot at such
⬃13 keV. As one might expect, the beam current increases low impact energy represents several orders of magnitude
with increasing impact energy until a saturation condition is higher arrival rate than most mass-filtered ion beam sources.
reached. The saturation current depends strongly on the For example, electron impact sources typically used for ion
plasma operating conditions as well as the field strength in scattering spectroscopy 共ISS兲 共even without mass filtering兲
the beam extraction region. When the beam energy is low- can barely approach 0.01–0.1 ML/ s.12 These sources typi-
ered below 100–150 eV, the beam current begins to fall off cally provide up to 100 nA into a beam spot of 1 mm at 1
because of excessive space charge spreading during extrac- keV with the spot size becoming significantly larger and
tion from the plasma and during the beam deceleration step. beam current smaller as the impact energy is lowered.
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 083302-9 Low-energy ion beam scattering apparatus Rev. Sci. Instrum. 76, 083302 共2005兲

C. Ion beam energy distributions and energy

tunability
The success of any ion beam scattering experiment relies
heavily on a well-defined scattering geometry and incident
beams with narrow energy spread if the energy distributions
of surface scattered products are to be meaningful. Further-
more, tuning the projectile energy provides a direct means of
varying the distance of closest approach 共Rmin兲 that occurs
during the close encounter between the two colliding nuclei.
These two features, tunable energy and narrow width, are
fundamental requirements for any ion source and beam sys-
tem used for scattering studies, especially at low impact
energy.
ICP plasma discharges have been shown to have a rela-
tively narrow ion energy distribution function 共IEDF兲 by sev-
eral different measurement techniques.33,34 Typical IEDFs
are 5–10 eV FWHM with low- or high-energy tails in some
cases. However, an ICP plasma has not been used as a beam- FIG. 8. Ion beam energy distributions for 20Ne+ measured at the target
position using a miniature hemispherical sector energy analyzer with chan-
line ion source for low-E studies before and most of the neltron detector. For each case, the difference between the plasma float
beamline experience that exists in the literature 共Freeman potential and the average beam energy 共11–12 V兲 is dictated by the Ne
sources兲 pertains to much higher impact energies plasma self-potential. Narrow FWHMs over a wide impact energy range can
共⬎1–5 keV兲, where an energy width of 20–50 eV is usually be seen.
inconsequential. Therefore, we felt that a concrete measure
of the beam energy distribution at the sample location was particle exit energies when hyperthermal projectiles 共50–500
necessary. Just because the ICP can be tuned to give a nar- eV兲 are scattered from a surface. Also, inelastic energy loss
row IEDF does not mean that the beam hitting the target mechanisms typically account for ⬍10% of the total loss
sample will be narrow as well. Broadening of the distribution upon scattering.2 Careful measurements of these losses can-
due to collisions with background gas atoms in the extraction not be accomplished if the incident beam energy width is too
region and during transport as well as ion creation along the large. Discrete losses during the close encounter may occur
flight path through electrode collisions can potentially pol- but they can be frequently overshadowed or “smeared out”
lute the beam hitting the sample.3 Any capacitive coupling by an incident energy distribution that is too broad.
from the rf drive antenna to the ICP will also cause inher-
ently bimodal beams 共IEDF for a capacitive discharge is
bimodal兲.5,14 Finally, our technique for adjusting the impact D. Scattered product detector performance
energy, by floating the entire plasma volume above ground Energetic ion bombardment of a solid sample generates
with a dc bias, must be tested. a whole range of particle fluxes leaving the target surface
The energy tunability of the ion beamline system was 共see Ref. 36兲. The major species are sputtered neutrals and
evaluated by measuring the IEDF of the incoming ion beam secondary ions with kinetic energies of a few eV up to tens
directly at the target location with the 180° energy sector of eV. These species are a mix of projectile and target atoms
analyzer mentioned earlier. A typical energy distribution for that are generated as a result of multiple collisions and sput-
both a low and high energy 20Ne+ beam measured at the tering processes. At higher exit energies, surface atom re-
target location is given in Fig. 8. The sector was run in CAE coils, and directly scattered projectiles that survive neutral-
mode 共Epass = 15 eV兲 while ion energy scans were performed ization 共or those that are reionized on the exit path from the
by ramping the retard voltage on the whole analyzer. Figure target surface兲 are observed. The energy spectrum of these
8 shows that the beam energy can be varied easily by in- directly scattered species contains information about single
creasing the dc voltage on the plasma bias plate, where the collision processes and the energy losses that can occur dur-
offset between applied bias and measured energy represents ing the close encounter between the projectile and target nu-
the Ne plasma potential 共⬃10–12 eV兲. The IEDFs are con- clei. The inelasticity in these single collisions can manifest
sistently narrow 共⬍10 eV FWHM兲 and peaks are unimodal, itself as electron excitation of the projectile or target atoms,
indicating that capacitive coupling from the rf antenna is photon generation, or energetic electron release.37 A product
efficiently stopped by the Faraday shield, i.e., power transfer detection system capable of distinguishing the energy spec-
to the plasma electrons is purely inductive. Similar plasma trum of many of the species leaving the surface could prove
potentials in the 10–20 eV range have been measured by very useful in understanding the fundamental processes oc-
other authors with Langmuir probe techniques for inert gas curring on the surface during bombardment.
ICP discharges in the 2–5 mTorr range.35 Thus, the beamline As a test case, the neutral detection capabilities of our
can simply transport the plasma IEDF all the way to the system 关secondary neutral mass spectroscopy 共SNMS兲兴 were
sample without significant broadening. A narrow energy dis- evaluated by looking for directly scattered hyperthermal Ar0
tribution for the incoming ion beam is very important be- from Ar+ bombardment of an Ag surface at 110 eV impact
cause this inherent energy width can be comparable to the energy. Results of this experiment are shown in Fig. 9. En-
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 083302-10 M. J. Gordon and K. P. Giapis Rev. Sci. Instrum. 76, 083302 共2005兲

Ar+ exit energy taking into account the 15 eV kick. Fast

neutrals seem to appear ⬃3–5 eV faster than the directly
scattered ions. The offset likely occurs because the electron
straggling of the projectile on the incoming and outgoing
trajectories near the surface is charge state dependent.39 It
has also been shown by Xu et al.40 that the continuous strag-
gling loss, as represented by the Oen and Robinsen
approach,41 depends on the particle charge state.
The neutral experiments conducted with our scattered
product detector indicate that having an energy filter between
the ionizer and the rest of the detection system can be suc-
cessfully used to separate residual gas neutrals from those
originating from the target. In addition, the peak energy po-
sitions of both the ion and neutral signals can be identified
and make good sense when the operation of the detection
FIG. 9. Energy scans of Ar0 and Ar+ exit channels from Ar+ scattering off system is clearly understood. As well, the detection of neu-
an Ag target at 110 eV and 90°. Neutrals were detected with the ionizer trals generated at the target surface has been demonstrated,
running at 2 mA emission current, 70 eV electron energy, and the capacitor
deflector in the first pumping stage set to +200 V. In the hyperthermal Ar0
suggesting that scattering experiments with reactive systems
case, the ion creation potential in the ionizer is ⬃15 eV above ground, 共where most of the reaction products are neutral兲 will be
giving the fast neutrals leaving the surface a kinetic energy kick of 15 eV possible.
when electron impact ionization occurs. Thus, the single scattered Ar+
which is neutralized to Ar0 by the surface should occur at ⬃15 eV above the
SS position shown for the ion peak. IV. APPLICATIONS
A. Elastic scattering at low energy
ergetic Ar neutrals are formed from single collision binary Low energy He+ ion scattering has been used for a long
events of Ar+ projectiles with Ag target atoms that are neu- time to determine the composition and structure of the top-
tralized along the incoming or outgoing portion of the trajec- most atomic layers of a target surface 共for example, see Ref.
tory in the near surface region. Single collisions of Ar+ with 42兲. This technique is based on the binary collision approxi-
the surface result in a large fast scattered ion signal near mation 共BCA兲 model, where the projectile is deflected by a
45–50 eV. This energy represents the single scattering events sequence of pairwise interactions with individual target at-
that occur in one binary collision, where the energy transfer oms. Each deflection event is assumed to be totally elastic,
can be approximated by the binary collision approximation.2 so the energy transfer during the hard collision event can be
The kinematic factor 共energy transfer ratio兲 for Ar+ on Ag for described by conservation of energy and momentum. As
a 90° scattering angle is ⬃0.46, which would predict such, the projectile energy after a single collision can be
⬃50 eV exit energy for the 110 eV incident projectile. Also simply calculated using the well-known “kinematic factor”
shown are the neutral signals, with one large peak at low 共K兲:2
energy along with a much smaller, broad Ar0 peak occurring
共cos ␪L + 冑␥2 − sin2 ␪L兲2E0 ,
1
near 65 eV. All neutral scans were conducted with the ca- Eexit = KE0 = 共1兲
pacitor ion deflector in the first pumping stage set to +200 V 共1 + ␥兲2
to prevent any charged species from ever reaching the detec- where E0 and Eexit are the incident and scattered projectile
tor. The ionizer was run at 2 mA electron emission current energies, ␥ is the target-to-projectile mass ratio 共M T / M P兲,
with 70 eV electrons and the quadrupole was locked at 40 and ␪L is the lab scattering angle. Application of the BCA
amu with ⌬m ⬃ 1 amu pass mass width. In addition, the scan theory to He+ ISS using keV impact energies is beyond
was taken in a single pass with 0.5 s dwell time for each debate.39,42 However, systematic studies of scattering phe-
energy bin 共⌬E = 1 eV兲. The large Ar0 peak at low energy nomena involving heavier inert ions at lower impact energies
represents the residual gas background and thermal species have not been so widespread. To this end, it seems most
leaving the target which are ionized near the 15 V grid po- natural that we use our beamline system to investigate BCA
tential of the ionizer. The ⬃3 eV shift to lower energy occurs predictions at low collision energies. Indeed, any discussion
because of the space charge potential depression created in of inelastic energy losses that occur in hard collision events
the ionizing volume by the high emission current 共2 mA兲.38 共i.e., electronic excitation of projectile or target兲 must first
The 65 eV neutral peak can be attributed to single-scattered include an assessment of how realistic the BCA model is at
projectiles that are neutralized along the incoming or outgo- low energy. In addition, it has already been mentioned that
ing scattering trajectory by the Ag surface. This peak is equipment issues, such as scattering angle change with im-
shifted upward by 15–20 eV from the directly scattered ion pact energy, broad IEDFs for the incident beam, and high
peak because the ionizing volume is run 15 V above ground. surface neutralization rates frequently hamper low energy
When fast neutrals enter the ionizer, they are given a “kick” scattering experiments. Evaluating the BCA over a wide
in energy the moment they are converted to ions by electron range of target-to-projectile mass ratio serves as a test plat-
impact due to the 15 V accelerating field. A question may form to assess if such effects are important for our beamline
arise why the Ar0 exit kinetic energy is not exactly equal the scattering system.
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 083302-11 Low-energy ion beam scattering apparatus Rev. Sci. Instrum. 76, 083302 共2005兲

10共b兲 as a function of target-to-projectile mass ratio, along

with the BCA predicted K value for single scattering at 90°
关Eq. 共1兲兴. Agreement between the experimental data and
theory is excellent, despite the oversimplified view of the
collision process given by the BCA model. It should be noted
here that the K factor determination for Ne–Al and Ne–Si are
based on impact energies ⬍400–500 eV only. In the next
section, we will see that inelastic energy losses become im-
portant for the Ne–Al and Ne–Si systems once a critical dis-
tance of closest approach has been reached in the binary hard
collision. We can also determine that the constant K factor
seen in all cases verifies that the lab scattering angle does not
change as the impact energy is varied for our system.

B. Charge exchange involving Ne+ with light targets

We have shown in the previous section that the BCA
model is quite successful in predicting energy transfer for
Ne+ projectiles with impact energies between ⬃50 and 1000
eV on a variety of targets. However, inelastic loss processes
can sometimes occur where the translational KE of the in-
coming ion is converted into electronic excitation or ioniza-
tion of the atoms in the colliding pair.37 The existence of
such channels is often seen as shifts in exit energies of the
projectile or target recoil from their elastic positions, changes
in the scattered particle charge state, or emission of charac-
teristic electrons and photons as excited states 共created in the
hard collision兲 decay 共see Ref. 37 for a review兲. In particular,
inelastic losses, high ion yields 共⬎50% Ne+ off Mg兲,43–45
and multiply-charged scattered projectiles 共Ne++ and Ne3+
off Mg, Al, and Si兲40,46–50 have been seen for single binary
collisions involving Ne+ projectiles at keV impact energies.
Such “richness” in the scattering behavior is intimately
linked to local charge exchange phenomena which occur as
the atomic orbital 共AO兲 states of the collision partners quan-
FIG. 10. 共a兲 Experimental exit energies for single-scattered 20Ne+ and Ar+ tum mechanically mix into hybrid molecular orbitals 共MOs兲
off several targets showing the constant kinematic energy transfer factor. 共b兲
Summary of experimental kinematic factors for collision energies between
during the hard collision step 共the Fano-Lichten MO
50 and 1000 eV, measured from the slope of the Eexit vs E0 data. The mechanism兲.51 Although many studies have been conducted
theoretical prediction from the BCA model for 90° scattering is given by the with Ne+ on Mg, Al, and Si at high collision energies, little
line. For Al and Si targets, only the data below E0 = 500 eV was used for the experimental data exist for the threshold region at low im-
K-factor determination.
pact energy where local charge exchange processes and in-
elastic losses begin to occur. We present a brief summary
Figure 10共a兲 shows the measured exit energy for single- here of our experiments on Ne+ collisions with light targets
scattered 20Ne+ and Ar+ off several target surfaces 关Pb, Au, 共Mg, Si, Al, and P兲 for impact energies ⬍1400 eV to empha-
Ti, Ge共111兲兴 at 90° lab angle for collision energies starting at size why tunable incident energy, as well as mass and energy
⬃50 eV. Regression lines using a hard zero intercept are also filtering of scattered products, is necessary. Details of these
given, allowing an experimental kinematic factor to be deter- scattering experiments are presented elsewhere.52 Simulta-
mined directly from the slope. For these experiments, each neous mass and energy dispersion of scattered products is
target was sputter cleaned 共5 keV Ar+, 60° incidence兲, an- highly advantageous because the energy distributions of
nealed, and amorphized with the low-E projectile beam at Ne+共m / e = 20兲 and Ne++共m / e = 10兲 can be measured
300 eV for ⬃15 min before taking data. In each case, the separately—eliminating signal overlap and confusion from
exit energy dependence is seen quite linear with collision multiple charge states which can occur for electrostatic-only
energy, even down to the low energy range. The small upturn and TOF-type analyzers 共see Refs. 45 and 49 for overlap
in the Ge data 共Eexit ⬎ Eexit,BCA兲 is likely caused by increased issues兲.
multiple deflection events 共one glancing, one near 90°兲 due Exit energies of Ne+ and Ne++ resulting from single bi-
to the underlying 共111兲 crystal structure being insufficiently nary collisions of Ne+ with an Al target from ⬃100 to 1400
amorphized at E0 ⬍ 150 eV. eV are shown in Fig. 11共a兲, along with the BCA prediction
Experimental K factors for ⬃50–1000 eV impact were 共K = 0.149兲 for single scattering 共SS兲 at 90°. The total Ne+
also measured for a wide variety of target materials using scattered intensity is also given, where the raw detector
20
Ne+ and Ar+ projectiles. These results are given in Fig. counts in the lab frame have been converted to a term pro-
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 083302-12 M. J. Gordon and K. P. Giapis Rev. Sci. Instrum. 76, 083302 共2005兲

trend with impact energy; and 共3兲 significant hard collision

losses in the Ne+ and Ne++ exit channels. The Rmin value
where Ne++ first occurs 共470 eV= 0.64 Å Thomas–Fermi–
Molière or 0.56Å Ziegler–Bierszack–Littmark interatomic
potentials兲 agrees well with the theoretical distance required
for L-shell orbital overlap for the Ne–Al collision pair 共0.57
Å兲.54 This observation suggests that a local charge exchange
process, driven by atomic orbital overlap of the 2s and 2p
shells of Ne and Al, is likely responsible. Going one step
further, binary collision inelasticities can be evaluated by ad-
justing the lab frame energy loss to the center-of-mass frame
and accounting for electron straggling on the incoming and
outgoing trajectory paths 共see Ref. 52 for details兲. This in-
elasticity data 共Qbin兲 for Ne–Al is given in Fig. 11共b兲, where
saturation-like behavior for both the Ne+ and Ne++ exit chan-
nels can be seen. Furthermore, we can identify the saturation
energy loss values 共⬃40–45 eV for Ne+, 70–75 eV for Ne++兲
as associated with double excitation events, which occur in
the hard collision step as the 4f ␴ MO from the Ne 2p is
highly promoted at small Rmin

Ne0共2p6兲 + 41–45 eV → Ne**共2p43s2兲, 共2兲

Ne+共2p5兲 + 69–72 eV → Ne+**共2p33s2兲. 共3兲

In the first case, Ne+ is Auger neutralized to Ne0 in the in-

coming path to the surface and is doubly excited by transfer-
ring two electrons out of the promoted 2pz 共4f ␴2 MO兲 as it
crosses the 3s. Ne** can leave the hard collision intact 共Ne**
lifetime ⬎1.5⫻ 10−14 s兲55 and autoionize in vacuum far from
the surface region. For the latter, a projectile ion which has
survived neutralization on the incoming path is doubly ex-
FIG. 11. 共a兲 Exit energies of Ne+ and Ne++ resulting from single binary
collisions of 20Ne+ projectiles with polycrystalline Al for 90° lab scattering
cited in the same manner but significantly more excitation
angle in specular reflection. Elastic scattering behavior for a single collision energy is required to promote two electrons in the ion. Auto-
is indicated with K = 0.149. Error bars 共±5 eV兲 on the energy data are par- ionization decay of Ne+** then results in the Ne++ exit chan-
tially shown to avoid clutter. 共b兲 Binary collision inelasticities determined nel, which shows ⬃70 eV hard collision inelastic loss.
from the data in 共a兲. Energy requirements for various electronic excitations
of Ne0 and Ne+ are shown, along with the theoretically predicted overlap
The reversal in Ne+ yield with impact energy is dis-
distance of the n = 2 orbitals of the collision partners 共grey area兲. The colli- cussed in depth in Ref. 52, but it is clear that a transition
sion Rmin has been calculated using the Thomas–Fermi–Molière potential. from nonlocal neutralization at low-E impact 共Auger type兲 to
Rmin-dependent collision induced neutralization occurs as the
Rmin decreases. The critical Rmin requirement for the yield
portional to the ion yield by normalizing by the incident
reversal is intimately tied to the 4f ␴ MO promotion as well.
beam current and scattering cross section.53 Two regions are
If the incoming Ne+ 2p vacancy evolves as 3d␲44f ␴1, reso-
seen where the Ne+ and Ne++ exit energies are markedly
nant transfer from the target bands to the promoted 4f ␴1 can
different. At low impact energy 共region 1兲, the SS Ne+ exit
neutralize the projectile, causing the total Ne+ yield to de-
appears totally elastic and Ne++ is not seen in the scattered
crease. This mechanism, because it involves resonant trans-
ion spectrum. Since the collision Rmin 共distance of closest
fer, should only be operable if the 4f ␴ is promoted enough
approach兲 is relatively large 共⬎0.8 Å兲 at low-E impact,
so as to cross the target conduction band energy levels. As
straggling losses are small 共a few eV maximum兲 and signifi-
such, a strong Rmin dependence, or minimum impact energy
cant overlap of the core-shell atomic orbitals of the collision
threshold, would be seen. This is indeed the case.
partners does not occur. As such, elastic scattering behavior
for Ne+ is seen and no excitation channels exist to form Ne++
共due to MO promotion in the hard collision兲. However, as the
collision energy is raised 共region 2兲, a transition occurs
where the Ne+ exit becomes inelastic and Ne++ is suddenly
C. Reactive scattering of CF2+ / CF3+ off Si
generated at ⬃470 eV with a large energy offset from the SS
elastic line. At this threshold 共minimum Rmin requirement兲, Scattering studies using reactive projectiles on Si共100兲
three phenomena occur simultaneously in the scattered ion were conducted as preliminary work towards a larger goal of
spectrum: 共1兲 Ne++ generation; 共2兲 reversal of the Ne+ yield understanding the fundamental energetics and reaction
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 083302-13 Low-energy ion beam scattering apparatus Rev. Sci. Instrum. 76, 083302 共2005兲

mechanisms that occur during reactive ion bombardment of

Si—as applied to dry plasma etching processes. These ex-
periments with pure, mass-filtered beams of reactive projec-
tiles in the low energy range from 50 to 500 eV are, in fact,
one of the main driving forces behind our ion beamline sys-
tem. The 50–500 eV range is required in plasma etching to
provide momentum assist to surface chemical reactions and
stimulate etch product removal from the wafer surface with-
out causing damage to the substrate from heavy sputtering at
high impact energies.5 The experiments presented here only
provide a taste of the complex processes occurring in CFx
etching of Si, but they demonstrate why one needs a single
ion species at well defined energy along with broad based
detection capabilities of the particle flux leaving the target
surface. Fundamental understanding of the complex mecha-
nisms involved requires all the beamline components: 共1兲
robust, high density ion source, 共2兲 mass-filtered ion beam-
line, 共3兲 low tunable energy, 共4兲 high current, and 共5兲 detec-
tion of mass and energy of ions and neutrals leaving the
substrate surface.
As a first step, we looked at the ion species leaving the
target surface for CF+3 and CF+2 bombardment of Si共100兲 as a
function of impact energy to give hints about the influence of
ion energy on removal of surface reaction products in
Si/ SiO2 etching environments. Although this experiment
seems rather simple, it has not been done before with a
single ion species and simultaneous product detection. CF+3
and CF+2 beams were formed from CF4 / Ar/ O2 plasmas run-
ning at 500–700 W and ⬃5 mTorr, giving target currents
⬎200 ␮A / cm2共CF+3 兲 and ⬃50 ␮A / cm2共CF+2 兲. For this scat-
tering experiment, we sought to answer two questions: 共1兲
what is the fate of the molecular ion as it hits the surface?
and 共2兲 which ion species are preferentially released from the
reactive SiCxFy layer that forms on the Si surface during
bombardment? Figure 12 summarizes the results for CF+3 and FIG. 12. Charged exit channels leaving an Si共100兲 surface for: 共a兲 CF+3 and
CF+2 bombardment of Si at 90° lab angle 共45° incidence兲 for 共b兲 CF+2 projectiles. SiF+2 and SiF+3 ion species were not seen in the scattered
impact energies from ⬃50 to 500 eV. As shown, the main ion spectrum for any impact energy tested. The total scattered ion intensity
ion species leaving the surface are CF+ , C+ , Si+, and has been normalized by the incident beam current and was obtained by
integrating the detector counts of each species 共quad at fixed mass兲 obtained
surprisingly—SiF+. At the lowest impact energy 共⬃70 eV兲, during an energy sweep of the hemispherical sector. CF4 / O2 / Ar plasmas
some CF+3 and CF+2 are seen, but they quickly disappear running at 1–5 mTorr and 500–700 W were used.
above 100 eV impact energy. The presence of CF+3 at low
energy 关Fig. 12共a兲兴 is likely molecular ion survival while the
CF+2 may be caused by F-atom abstraction of the incoming sputtered away as SiF+ only 共if they exit the surface in a
projectile 共dissociative scattering兲 or physical sputtering of charged state兲. We specifically looked for SiF+2 and SiF+3 leav-
CF2-like species from the surface. An analogy is drawn here ing the surface and did not detect any signal for all the im-
to CF+3 scattering off fluorinated liquid surfaces,56 where the pact energies tested. It is curious why SiF+ is the only
perfluoropolyether 共PFPE兲 surface is terminated entirely by charged Si-containing species leaving the surface, but one
–CF3 and –F species with the ether oxygen atoms buried could explain such an observation as being due to an
beneath the surface.57,58 Collision phenomena should be F-deficient surface. Finally, the spectra show the onset of Si+
similar because it is a generally held belief that CFx etching for impact energies above ⬃200 eV, which is a sure sign that
of Si proceeds through a reactive SiCxFy layer with dangling the increased momentum of the projectile is beginning to just
–CFx and –SiFy moieties on the surface.5 For the PFPE case, sputter the target surface.
the predominant ion exit for CF+3 scattering at ⬎250 eV im- This simple study gives a flavor for the physical scatter-
pact was CF+, with little or no CF+2 or CF+3 . Our preliminary ing behavior as well as some of the chemical reactions that
work echoes this behavior as well. What is interesting at are occurring on the surface during bombardment with just
energies above 100 eV in our case is the rise of C+ and SiF+ one incident ion species. It is also clear from this one experi-
exit channels. The large increase in SiF+ from the surface ment that complex scattering behavior, especially for a reac-
suggests that as the impact energy gets higher, more projec- tive system, absolutely requires mass filtering of the particle
tile F atoms react to form dangling SiFx species which are flux leaving the target surface to sort out all the exit chan-
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 083302-14 M. J. Gordon and K. P. Giapis Rev. Sci. Instrum. 76, 083302 共2005兲

nels. Turning on the ionizer to look at the neutrals along with Foundation and Applied Materials for personal scholarship
energy analysis of the scattered flux will add a whole new support.
dimension to fundamental scattering studies.
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