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A multicollector, cycloidal focusing, magnetic mass spectrometer

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1974 J. Phys. E: Sci. Instrum. 7 759

(http://iopscience.iop.org/0022-3735/7/9/024)

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perpendicular electric and magnetic fields (first discussed by
A multicollector, cycloidal Bleakney and Hipple 1938), includes a novel form of detection
system and overcomes the above problems. It is thus capable
focusing, magnetic mass of mass separating and simultaneously and continuously
monitoring a whole series of ion signals from pulsed, continu-
spectrometer ously varying or steady state ion sources.

2 Ionic motion in spatially uniform, time invariant, mutually


perpendicular electric and magnetic fields
The motion of ions in this type of field configuration has
previously been discussed in detail in the literature (Bleakney
and Hipple 1938, Page and Adams 1969, Kuz'min 1971).
Therefore, only those features of the ionic motions essential
for an understanding of the mode of operation of the present
mass spectrometer will be discussed here. If an ion is injected
into a region of mutually perpendicular, uniform electric
and magnetic fields in a plane perpendicular to the magnetic
N G Adams and D Smith field then the locus of the ion motion will be a curtate,
Department of Space Research, University of Birmingham, common or prolate cycloid dependent on ion injection condi-
Birmingham B15 2TT tions. Only prolate cycloidal motion as illustrated in figure 1,
Received 15 November 1973, in final form I March 1974

Abstract The design and appraisal of a mass spectrometer,


based on the focusing properties of mutually perpendicular
electric and magnetic fields, is described. This field
geometry spatially separates ions as a linear function of
mass along a focal plane. This allows the spectrometer to be
used in applications requiring the simultaneous monitoring
of many ion species of independently varying intensities,
such as from transient or pulsed ion sources, a feature not
associated with other spectrometers. This instrument
incorporates a novel detection system comprising a channel
multiplier plate which considerably enhances sensitivity and
a 50 element slatted collector array which separately detects
the individual ion signals in the chosen mass range
20-70 U. To date a detailed experimental appraisal in the
scanned E field mode, in which the resolved ion current Figure 1 Schematic diagram of a prolate cycloidal ion
spectrum is swept across one of the collectors, has trajectory in mutually perpendicular electric and magnetic
provided data on the detailed mass peak profiles, the fields. The important parameters defining the trajectory are
resolving power of the analysing E x B field and the indicated
efficiency and dispersion of the detector system. The data
provided by this investigation has allowed a detailed will be discussed since this is the only type of motion which
appraisal to be presented concerning the modifications
is geometrically possible in the present spectrometer. If
required in order that the instrument can be operated in the positive ions of charge e and mass m are injected through an
constant E field mode in which the E field is fixed and the entrance slit at x=O, y=O in the z=O plane into an electric
resolved ion current is distributed amongst the 50 collectors
field E(0, E,, 0) and magnetic field B(0, 0, Bz)then the ions
located behind the focal plane. A report of the operation of recross the y = 0 plane travelling in the direction of injection
the spectrometer in the constant E field mode is presented in
at x = b where
a subsequent publication.
27imE
b= (1)
B2e
1 Introduction It can be seen from this expression that the focal distance b,
In the field of mass spectrometry, many static and dynamic and thus the focusing properties of this type of field configura-
mass spectrometers are available which enable ion species tion, are independent of both the initial energies and velocity
from a source to be sequentially scanned (Ewald 1956, Blauth vectors of the ions. Thus a spectrometer employing this field
1966, Greaves 1969). However, these devices in general possess configuration can be operated with a high transmission
a single ion collector and are thus unsuitable for systems in efficiency relative to spectrometers where energy selection or
which it is required to monitor several ion signals continuously, a limitation to the range of injection angles is necessary. The
or where the ion source is of a nonreproducible pulsed nature initial energies and velocity vectors however do affect the
(e.g. Smith and Adams 1973). Mass spectrometers have been shape of the trajectory. This more general situation has been
devised which, in conjunction with a photographic plate, can rigorously treated by Kuz'min (1971). No focusing occurs for
produce a complete spectrum of ions simultaneously, however the z component of the ion velocity since the electric and
with this type of system, the variation of ion signals with magnetic fields exert no forces in that direction. For initial
time cannot be monitored (Ewald 1956). The design of mass ion velocities with a zero x component of velocity (0=90",
spectrometer described in this paper, which is based on the see figure 1, is a good approximation to the present experi-
focusing and spatially mass resolving properties of mutually mental conditions) the maximum ion excursions in the + y ,

759
N G Adams and D Smith
-y and - x directions, denoted by yi,y- and s respectively, where C= 2rlB2ep.Equating these expressions gives equation
are (Bleakney and Hipple 1938) (7). This definition of resolving power is stringent as compared
with more often quoted definitions of resolving power
y+=a+p (2) (Greaves 1969). As defined thus, previous single collector
y-=a-p (3) cycloidal mass spectrometers have theoretical resolving
and powers varying from 64 to 100 (Bleakney and Hipple 1938;
Robinson and Hall 1956; Eberhardt 1960; Huber and
s=2[(pz-aZ)l/*-a COS -l(a/p)] (4)
Trendelenburg 1962) and the theoretical resolving power of
where the primary radius a and the secondary radius p are the present prototype multicollector mass spectrometer
given by varies from 43 to 143 between the limiting focal distances of
a = b12r (5) 2.14 and 7.14 cm (S1F1 and SlFz in figure 2) respectively and
and

! B
I
- - - - - _r -P- - -I- - - - I
where eVo is the ion injection energy.
It can be seen from equation (1) that, for a constant focal
distance b, various masses may be scanned across an exit
slit and collector placed at the focal point by varying the
electric field strength E. This mode of operation, subsequently
called the scanned E field mode (SEFM) has conventionally
been used with cycloidal focusing mass spectrometers. How-
ever for a fixed collector position, the mass of the focused
ion, m, is inversely proportional to E and thus the mass scale
is nonlinear with electric field strength, being progressively
more compressed towards the higher masses. It can also be
seen from equation (1) that, for constant E, m is directly
proportional to b and thus the various masses are focused
linearly with mass along the focal plane (in contrast to other
spatially resolving mass spectrometers which are nonlinear
(for example, Ewald 1956, Nier and Hayden 1971)). Thus by
placing a series of narrow slits and collectors along the focal 4
plane, simultaneous detection of all spatially resolved ions is, MP
in principle, possible. It is in this mode subsequently called the
constant E field mode (CEFM), that the present prototype
mass spectrometer is designed to operate.
The resolution of the mass spectrometer is clearly of great
ii ii
importance. Theoretically for the case of perfectly uniform,
mutually perpendicular electric and magnetic fields, the ( b1 (C) (d)
resolution is determined only by the widths of the entrance Figure 2 (a) Side and (6) and (c) sectional views of the
and exit slits of the spectrometer and the focal distance, b. prototype mass spectrometer showing the essential details.
For a spectrometer operating in the SEFM (scanned E field The dots represent the E field wires and the dashed lines
mode, the mode used to assess the performance of the present indicate the limits of the magnet pole pieces. The enlarged
spectrometer), the resolving power, defined as the ratio of the view ( d ) of part of the detection system is magnified
selected ion mass, m, to the base width of the mass peak, approximately 10 times relative to (a), (b) and ( c ) (the
Am, is from equation (1) given by distance w is not to scale). I, ion source; SI entrance slit to
analysing section; PI, Pa, P3 and P4, plates defining the Efield;
m b W, wires defining the E field; FI,Fz,focal plane (in (a) the
&%=ilb (7)
exit slits from the analysing section are shown as a dashed
+
where Ab is the sum (SI SZ) of the entrance (SI) and exit ( S Z ) line for clarity); M, channel multiplier plate; C, collector
strips; V, wall of vacuum housing; MP, magnet pole pieces;
slit widths. This relationship is obtained from a consideration
of the processes involved in scanning two masses, spatially SP, slit plate; L, copper leads
resolved on the focal plane and separated by a small mass
difference Am, across an exit slit (placed at a focal distance b)
by varying the E field voltage V ( =PE).For these two masses for a constant Ab of 0.5mm. The resolving power increases
to be just completely resolved on a SEFM mass spectrum linearly with focal distance. In the case of a multicollector
requires that the voltage width at the base of the peaks in the spectrometer operating in the CEFM the distance between
spectrum, hVb (that is the voltage change required to com- adjacent exit slits (d) is clearly also of importance in deter-
pletely scan one of the masses across the exit slit), is just less mining the resolution since ions of a specific mass are spread
than the voltage difference between the two peaks A Vm (that along the focal plane, over a distance equal to the entrance
is the difference in the voltages required to focus each of the slit width, SI,assuming no broadening due to inhomogeneities
masses onto the exit slit). Avb and h V , can be obtained in the analysing fields. The conventional concept of resolving
directly from equation (1) by differentiation with respect to power (m/Am) is not useful for this mode, since as can be
b and m respectively yielding seen from equation (l), the ions are focused at positions along
the focal plane which are linearly related to mass and thus the
spatial resolution between two masses differing by 1 U is
independent of the mass. This is in contrast to the SEFM in

760
Multicollector mass spectrometer
which the resolution decreases with increasing mass. To plates were equal and of opposite polarity (the slit plate
completely resolve between masses differing by 1 U requires being of negative polarity) about the potential of the electron
that s ~ < d + s z and d+sz=b/m where m is in U and d is beam thus providing a uniform electric field within the source.
the inter-exit slit distance. This field had no significant effect on the width of the electron
In practical spectrometers the volume over which the beam since the latter was closely confined by the ambient
electric and magnetic field strengths can be maintained sensibly magnetic field (0.1515 Wb m-2). Ions produced by electron
constant is limited and thus the maximum values of b, y-, impact with the ambient gas (either residual gas after evacu-
y- and s (equations 1 to 4) are limited. This therefore limits ation or sample gas) within the electron beam were thus
the range of trajectories (that is the range of pia values, accelerated towards the slit plate. The ion beam ejected
figure 1 ) which are possible for any value of b and since the from the source has an estimated energy spread of 210%
shape of the trajectory is to some extent determined by the due to the differing points of origin of the ions in the source
injection energy and the velocity vector, then for a constant electric field and an estimated angular divergence of about 20".
E field, this limits the range of these parameters. In the design For electron filament currents of the order of 1 A and an
of the present prototype, consideration was given to all the electron accelerating voltage of 70 V, electron beam currents
above constraints in addition to those imposed by mechanical of about 10-sA were obtained. For a source pressure of
constructional difficulties. 10-5 Torr (typical of the present experiments) this resulted in
the injection of an ion beam current of about 10-12 A into
3 Prototype spectrometer configuration the analysing section of the spectrometer.
A schematic diagram of the prototype mass spectrometer is
shown in figure 2. Ions from an ion source I, are injected 3.2 Analysing section of the mass spectrometer
through slit S1 into the mutually perpendicular electric and The ions from the source were injected with an energy eVo
magnetic fields of the analysing section of the spectrometer. through the 0.25 mm x 2.0 mm entrance slit, SI, into the
The ions then move in prolate cycloidal orbits (similar to that mutually perpendicular uniform electric and magnetic fields
shown in figure 2). If the orbits do not intersect any of the in a direction approximately antiparallel to the electric field
plates PI,Pz,P3, and P4 (defining the extent of the electric (as defined by the angular divergence of the ion beam from
field) or are otherwise lost from the spectrometer through the the source). The electric field was provided by a series of 28
E-field wires, W, then the ions are focused according to mass loops of 50 pm diameter nickel wire (W in figure 2 ) wound
on the focal plane F1F2. These ions are then electrostatically at 2 5 mm intervals around a former consisting of insulating
accelerated into the detection system, the signal amplified by Tufnol rods T supported on the brass plates PI,P3 and P4.
the channel multiplier plate M and the amplified spatially No change in the position of the wires was detected when
separated signals detected on an array of slat collectors C. this structure was placed in the magnetic field. Similarly no
detectable change in the magnetic field strength was observed
3.1 Zon sources due to the presence of this structure. The brass plates also
To test the operation of the mass spectrometer, ions were served to define the limits of the uniform E field in the y
created in both a Kunsmann (see for example, Elliot 1963) direction. The uniformity of this field was ensured by 1.5 kS1 i:
and an electron impact ion source. The Kunsmann source was 1 % resistors connected between adjacent wires and between
of a simple single filament type in which a 75 pm diameter the plates and the adjacent wires, the total potential difference
tungsten filament (5 mm long) coated with a mixture of being supplied by a variable DC power supply of stability better
sodium and potassium chlorides was positioned about 1 mm than 0.05% and AC ripple less than 200 pV peak to peak.
behind the 0.25 mm wide and 2.0 mm long entrance slit to Further immunity from AC pick-up was achieved by decoupling
the spectrometer. The slit was located in the focal plane the ends of the resistor chain with 1 pF capacitors. AC pick-up
parallel to the magnetic field. This source gave an ion beam is expected to have a serious effect on resolution since it is
of maximum angular divergence of about 15". Appreciable likely to vary the field strength over the whole spectrometer.
total ion emission currents of the order of A could be For example, for a focal distance of 5 cm and an entrance slit
obtained for filament Joule heating currents of approximately width of 0.25 mm, a small random modulation or AC pick-up
1 A. Since it is positioned in the centre of the spectrometer of 1 % superimposed on the E field voltage would result in a
(figure 2 ) the physical dimensions of the source were kept as factor of 3 broadening of the image at the focal plane. With
small as possible to minimise its effect on the allowed ion the above precautions it is estimated that, excluding effects
trajectories in the spectrometer. The source housing was due to contact potential differences, the field was uniform to
constructed of Tufnol to provide electrical insulation between within better than 1 % over the whole spectrometer. Contact
the component parts, and in order to minimize any disturbance potential differences are expected to increase the total non-
of the E field, a conducting plate PZ defined one side of the uniformity by a maximum of about 2% for a total applied
source and the slit plate the other, the potentials on these voltage of 50 V, a voltage typical of the present experiments.
plates maintaining the uniformity of the spectrometer E field. In principle, contact potential differences could be consider-
In order to obtain a greater number of ion masses with ably reduced by electroplating the spectrometer; however, in
which to test the operation of the mass spectrometer the the production of even the most carefully prepared surfaces,
thermionic emission, electron impact source illustrated in the presence of contamination would inevitably produce
figures 2(a) and (b) was used. In this source a 75 pm diameter some work function variations. Some additional non-unifor-
tungsten filament, 1.5 mm in length was positioned at one mity in the E field was introduced by the finite thickness of
end of and behind the mass spectrometer entrance slit and plate P3;however, the effect of nonuniformities in this region
electrons were injected, through a 0.25 mm hole, in a beam of the spectrometer are expected to be minimal (Bleakney
parallel to this slit and in the direction of the magnetic field, and Hipple 1938).
the beam being a distance of 1.25 mm from the slit. The By the above means an electric field uniform over a volume
electron beam was collected to a plate located at the opposite approximately 13 cm x 7 cm x 1a5 cm was achieved giving
end of the slit. In addition to the slit plate, a second plate maximum values of 7.14 cm, 4.5 cm, 2.5 cm and 5.0 cm for
was positioned also a distance of 1-25 mm the opposite side the trajectory parameters b, y+, y- and s. Minimum values
of the electron beam. The potentials applied to these two of b, y - and s of 2.14 cm, 0.5 cm and 1 cm were obtained as

761
N G Adams and D Smith
determined by the length of the collector array, C, and the and thus R constant so that the ionic species focused to the
physical size of the ion source. These geometrical factors collector follow a given allowed trajectory independent of
restrict the range of cycloidal trajectories by which ions can mass thus ensuring that all collected ions are subject to similar
pass from the spectrometer entrance slit to the focal plane. field inhomogeneities. This is the normal mode of operation
It is convenient to express the shape of the trajectories by a for conventional, single focal distance, cycloidal focusing
dimensionless parameter R= pia, since this assists in an mass spectrometers.
appreciation of the range of trajectories possible in a spectro- As stated earlier it is the volume over which an adequately
meter of a given size. The limiting values of this parameter uniform magnetic field of the required strength can be achieved
can then be determined as a function of the focal distance b. which determines the size of the spectrometer. Since the
The limiting values of R have been obtained from the magnetic field strength is related by equation (1) to the electric
limiting values of b, y-, y- and s imposed by the present field strength, the range of masses to be analysed and the length
spectrometer and are represented by the dashed lines on the of the focal plane along which these masses are to be spatially
plot of R against b in figure 3, the allowed values of R for a resolved, then a compromise situation has to be achieved.
Nomographs to assist in this compromise have been devised
by Bleakney and Hipple (1938) and Monk and Werner (1949).
Mechanical design estimates showed that an array of collectors
at about 1 mm intervals could readily be achieved and this
together with a prior knowledge of what magnetic field
strengths were possible over the required volume, showed that
a field strength of several tenths of a weber per square metre
would be appropriate.
From such considerations, a compromise of a 1 mm
collector separation and a magnetic field of strength (1515+
26) x 10-4 Wb m-2 uniform over an approximate volume of
13 cm x 7 cm x 3 cm was used. With this magnetic field,
masses in the range 20-70 U could be focused at intervals of
I I I I I I
1 mm/u along the focal plane using a reasonable E field
2 3 4 5 6 7 strength. The magnetic field was supplied by two Ticonal G
;3c31 d stcnce b (cm) C-shaped permanent magnets (supplied by Mullard Ltd)
Figure 3 Plots of R against focal distance b for a series of clamped to 1 cm thick planar soft iron pole pieces (approxi-
values of VjVo (solid lines) for the present prototype mass mately 15 cm x 9 cm in area) as shown in figure 2. Measure-
spectrometer. The dashed line encloses the geometrically ments of the uniformity of the magnetic field using a Hall
allowed values of R and D indicates a discontinuity in this effect gaussmeter showed it to be uniform to within better
line than If:1 % over most of the area of the analysing section.
A decrease in the magnetic field strength of up to 3 % occurred
in the region close to the edges of the uniform E field region.
given b being those enclosed within the dashed area. For the
present prototype the lower limit of R occurs when the ion 3.3 Detection system
trajectory intersects the source at the minimum value of s, After passing through the analysing section of the spectro-
no smaller R values being allowed. The upper limit of R meter and subsequently focusing spatially as a function of
occurs when the trajectory intersects plates P4 and PI for mass along the focal plane F1F2,ions arriving at appropriate
focal distances (b values) above and below 6.25 cm respec- positions on the focal plane passed through one of fifty
tively (this causes the discontinuity D at this point on figure 3). 0.25 mm x 6 mm exit slits equispaced at 1 mm intervals and
The limiting values of b are, of course, defined by the extent were subsequently accelerated by a uniform electric field of
FlFz (figure 2) of the collector array. R is also related via about 140 V mm-1 over a distance of 7 mm into a channel
equations (l), (5) and (6) to the focal distance b, the electric plate electron multiplier (Mullard Ltd) (Manley et al. 1969).
field strength E (= V/p) and the injection energy eVo (m is With this electric field strength the deflection of the ions due
known from equation (1) for given values of E and b). Thus, to the magnetic field, in the direction perpendicular to these
for a given value of b, R can be directly related to the para- field directions, was less than 0.25 mm (- 0.3 collector widths)
meters defining the orbit, that is to Y/:iVo,independent of ion even for the lightest ions considered (20 U). To further reduce
mass. this effect and to minimize effects due to ion dispersion, a
When the spectrometer is operated in the CEFM, singly second identical slit plate, SP, the potential of which could be
charged ions are focused at increasing focal distances for varied, was introduced between the focal plane and the channel
increasing mass as specified by equation (1). However, it can plate multiplier. The effect of varying this potential is discussed
be seen from equation (6) that since vivo is constant, as b in $4.1.2.
increases R decreases and it is thus necessary to ensure that An obvious alternative would be to position the detection
the R values are allowed for all possible values of b by using system outside the magnetic field. This would result in the
the appropriate value of ~ / V OThe . dependence of R on b ions travelling a distance of several centimetres in a spatially
for a series of values of VIVOis illustrated in figure 3 where it varying magnetic field with all of the attendant difficulties.
can be seen that only ~ / VvaluesO in the approximate range The suitability of present choice of detector position is justi-
1.5-6.0 are possible if ion collisions with the spectrometer are fied by the results presented in $4.1.2.
to be avoided. Thus this figure is, in effect, a ‘stability diagram’ The channel plate electron multiplier (gain lo3 at about
for this type of spectrometer (cf. the quadrupole mass filter 1 kV) was used to amplify the ion signals while maintaining
stability diagram, Paul et al. 1958). It can also be seen from spatial resolution by virtue of its honeycomb channel structure,
equation (6) that if the spectrometer is operated in the SEFM and the electrons produced were collected to a series of 50
then for a given collector it is advisable to keep the ratio copper film collectors, C, situated directly behind the channel
V;Vo constant (at a value within the limits defined by figure 3) plate but in line with the spectrometer exit slits. The collectors

762
Multicollector mass spectrometer
were constructed by segmenting the copper on a 5 cm x 1-2cm since this enables the whole profiles of the individual mass
rectangle of copper-clad fibreglass laminate into a series of peaks to be obtained for any focal distance. This allows the
1 mm spaced 0-8mm x 7.5 mm strips. The electrical resistance mass calibration and resolving power to be investigated
between adjacent collectors provided by the glass fibre and across the whole collector plane. Such detailed information
the 0.2 mm gaps in the copper was greater than 1 TQ. The cannot be obtained with the spectrometer operating in the
copper surface of the laminate was flat to within 0.025 mm CEFM since this yields data only from the positions of the
and was positioned 0.075 mm behind the exit plane of the mass peaks. This detailed appraisal in the SEFM has enabled
channel plate. This close proximity was essential to prevent the behaviour of the spectrometer in the CEFM to be pre-
appreciable deflection along the collector array of the electrons dicted (04.2).
in the magnetic field and thus to minimize any deterioration
in spatial resolution. An electric field strength of 650 V mm-l 4.1 Operation in the scanned E field mode
resulted in a calculated deflection perpendicular to the field For these measurements, the slit plate normally situated at
directions of less than 0.05 mm which is considerably less the focal plane (F1F2) was replaced by a plate with slits only
than the collector width. Electrical connection to each of the at a series of spatially well-separated focal distances (slit
collectors was via a 0.5 mm copper lead, L, passing through the separation= 7 mm). The use of such a slit plate enabled the
glass fibre of the laminate and attached to the copper collector separate effects of the analysing section and the detection
by mechanical deformation followed by electroplating. system on the overall resolution to be assessed since ions
Electrical connections to the channel plate were pressure passing through a slit could only reach the collector directly
contacts. Clearly the detector arrangement is critically in line and to a small extent adjacent collectors ($4.1.2).
important in the operation of the spectrometer. Electrons from the channel plate output to a given collector
The operation of the channel plate in this situation requires strip were detected using a battery operated Keithley electro-
some discussion since this type of device has not, to the meter (Model 600A). Measurements were made by selecting
authors' knowledge, been previously operated in magnetic a single collector situated directly behind one of the focal
fields approaching the strength used in this application plane slits and observing the ion-produced electron current
(0.1515 Wb m-2). The effect of magnetic field strengths up to to this collector as a function of the E field voltage, V. The
0.03 Wb m-* on single channeltrons (Halm et al. 1972; mass spectra were recorded on an XY plotter. The ratio
Barnett and Ray 1970) has however been investigated and V,Vo was maintained constant at a value within the limits
these devices have shown a marked decrease in gain for indicated in figure 3 and several values of this parameter
magnetic field strengths of 0.014.03 Wb m-2 dependent on were used in order to determine the value giving the greatest
the field orientation and the operating voltage (for voltages
in the range 3 - 4 kV). Significant gain reduction is expected
to occur when the magnetic field appreciably perturbs the Calculated focal distance (cml
electron trajectories in the channels leading to a reduction in
their kinetic energy at impact and thus to a reduction in the
effective secondary electron emission coefficient. For the
channel plate used in the present experiments, with a gain of
-
-2 4
lo3 and an applied voltage of 1 kV and assuming a secondary 0
electron emission coefficient of 1 (Hachenberg and Brauer 3 3
U

1959), then about 10 stages of electron multiplication occur c

and thus the electron energy prior to impact is about 100 eV. f 2
U

The radius of gyration of electrons of this energy in the S I


L

magnetic field of the prototype spectrometer is of the order - OI

of 0.15 mm. This is substantially greater than the individual


channel diameter (40 pm) of the channel plate and thus the
' 020 25 30 30 35
E field voltage V ( V )
40 i

magnetic field is expected to have no appreciable effect on (U 1 (6)


the channel plate gain,

3.4 Spectvometer housing


To enable the pressure to be reduced to a value suitable €or
operating the mass spectrometer and the channel plate, the
spectrometer was enclosed in an aluminium alloy vacuum
jacket. The use of this material enabled the complicated
vacuum housing to be readily machined, The analysing section
and the detection system were mounted on separate flanges
and, when inserted into the housing, located accurately into
their operating positions. During operation the pressure
within this vacuum housing was maintained below 10-5 Torr I I I I I
using standard vacuum techniques. Also the electric potential 30 40 50 60
(c> E field vo:tage V ( V I
of the housing was maintained about lOV negative with
respect to the initial ion potential so that ions with velocity Figure 4 Typical mass scans in the SEFM for both the
components such that they passed through the sides of the electron impact source ((a)and (b))and the Kunsmann
spectrometer were collected to the housing and could not source (c). (a) and (b) were obtained for b= 3.89 cm with
re-enter the spectrometer, V/V0=2.5 and (c) for b=4*60cm with V/V0=4. The ion
masses in atomic mass units are as indicated. The focal
4 Experimental appraisal distance scale on (b) shows the focal points expected for
In the experimental appraisal of this mass spectrometer, the operation in the CEFM with mass 29 focused at b = 2.9 cm
SEFM has been used throughout in preference to the CEFM

763
N G Adams and D Smith
resolution. When values of V/VO outside the limits indicated the errors due to random scatter of the points about the line.
in figure 3 were used no significant ion signals above back- Other random errors in the measurement of focal distance
ground were collected. This procedure was carried out for and E field voltage are negligible. The error in determining
each of the focal plane slits at focal distances of 2.46, 3.89, the magnetic field strength is not included since this is a
4.60, 5.31 and 6.02 cm with both the electron impact and systematic error. This is equivalent to less than a 2.5% error
Kunsmann ion sources. Typical mass spectra for both sources in the mass determination, Errors due to any nonuniformities
are given in figure 4 for sample focal distances of 3.89 and in the magnetic field are however indirectly included since, as
4.60 cm. The current levels shown on these figures represent the focal distance is varied, the region of the magnetic field
the electron current flowing from the anode of the channel through which the ions pass also varies. The mass peaks at
plate to the collector strip and are thus about lo3 greater 2 2 5 and 3 8 . 2 ~obtained using the Kunsmann source
than the incident ion currents. It should be noted that, obviously refer to the ions Na+ ( 2 2 . 9 9 ~ )and K + ( 3 8 . 9 6 ~ )
because of the lack of experimental evidence on the secondary and thus indicate the likely error in the experiment. Clearly
electron yield for ion impact on these relatively new devices, in both cases the experimentally determined masses are less
a yield of one secondary electron per incident ion has been than the true masses indicating a systematic error probably
assumed throughout this discussion when ion and electron associated with the measurement of magnetic field strength.
currents are interrelated via the gain of the channel plate. The measured field strength would then be low by about
It can be seen from figure 4(a) and (b) that, with the electron 1 %, within the 1.75% error bar of the measurement. There-
impact source, two groups of ion mass peaks appear in the fore for the accurate mass determination required in mass
ranges 27-33 U and 38-48 U. Additional mass peaks, due to spectrometry, a calibration procedure is obviously essential.
the presence of water, were observed at lower masses (17 and Using the NaT and K+ ion peaks as calibration establishes
18 U) and were more highly resolved than the spectra illus- the other ion masses as 29 and 46 U.
trated in figure 4(a) and (b). In figure 4(c) typical mass peaks Equation (1) also predicts that the curves in figure 5 should
from the Kunsmann source are shown, where it can be seen converge to the origin; however, it can be seen that in practice
that, as expected, the Naf and K + peaks are prominent. In a nonzero intercept is obtained. This effect has not, to the
addition the K + isotope at 41 U is observed in approximately author’s knowledge, been observed experimentally (although
the expected isotopic ratio. The other peaks appearing in it may have been present) in previous spectrometers of the
this spectrum are difficult to identify but may be due to cycloidal focusing type since a single focal length has always
metastable molecular ions which undergo unimolecular been used and the effect would not therefore have been
decomposition in their transit through the spectrometer recognized. The intercept is not due to errors in determining
(Jennings 1971). the focal distance since this is readily determined to an accur-
4.1.1 Calibration From the data in figure 4 and from similar acy of bctter than 1%. It may however be due in part to
data at a series of other focal distances, plots of focal distance contact potential differences effecting errors in the E field
b as a function of the E field voltage at which a particular voltage. This can only be expected to result in errors of less
ion mass is focused, have been made for many ion masses than about a volt which is smaller than the observed dis-
using both types of ion sources. Several of these plots are crepancy which is equivalent to 2 to 4 V. Additionally effects
reproduced in figure 5 where it can be seen that in all cases of this type would be expected if the electric and magnetic
b is linearly related to the focus voltage as predicted by fields were not absolutely mutually perpendicular. The general
equation (1). From the magnetic field strength of (1515+ 26) x equations of motion for this situation have been analysed in
lo-* Wb m-2 and the slopes of the lines in figure 5, values of detail by Kuz’min (1971) who has shown that this would
the ion masses were determined to be 22.5k0.8, 28.8k1.0, result in a nonzero intercept on the b axis. Following this
38.2 k 1.0 and 44.8 k 1.4 U, where the errors quoted include theory, estimates show that this alone is quite inadequate to
explain the experimental observations. The effects of field
nonuniformities (both in the electric and magnetic fields) as
‘I / opposed to field alignment errors have been reviewed by
Robinson (1956a). These effects lead to nonzero intercepts
on the b and Vaxes in specific cases and also to the possibility
of a reduction in resolution. It is difficult to determine the
magnitude of these effects, however, in the present case, their
magnitudes appear to be adequate to explain the observed
nonzero intercept.
4.1.2 Resohtion The resolving power of the analysing section
may be determined directly from an analysis of SEFM mass
spectra of the type illustrated in figure 4. From these figures
it can be seen that the voltage spacing between adjacent
peaks and the width of the peaks both decrease with increasing
mass as expected from equation (1) (this nonlinear behaviour
does not occur in the CEFM, the mass peaks in this mode
being spread linearly along the focal plane). In addition, the
peaks are approximately symmetrical and triangular in form
I I I I I I I as is expected if the focal plane exit slit is equal in width to the
0 20 $0 60
Focus voltage ( V I beam width due to a single ionic mass incident on the focal
plane. Since the entrance and exit slits are equal in width, this
Figure 5 Plot of focal distance, 6 , against focus voltage for implies that there was no excessive broadening of the image
several ions of the masses indicated. Open circles refer to at the focal plane due to field distortions in the analysing
values obtained using the electron impact source and solid section. If the beam width at the focal plane is appreciably
circles to those obtained using the Kunsmann source less than the exit slit width then the peak profile is expected
to be trapezoidal, whereas for a relatively large beam width,

764
Multicollector mass spectrometer
the form of the ion distribution across the beam would be extremities results in departures from ideal behaviour. This
approximately reproduced. is thought, at least in part, to result in the experimental
If it is assumed that the triangular shapes of the peaks are observation that the resolving power is optimum at a V/VO
maintained over the whole peak width then, by determining value of about 2-3 at small focal distances increasing to
the peak width at half height, the full width and thus the 3-5 at larger focal distances. Results of this type manifestly
resolving power as defined by equation (7) may be approxi- indicate yet again the need for a highly uniform magnetic
mately determined. The relationship between the resolving field, a factor which is of prime importance in the design of
power and voltage separation of masses on the SEFM mass future spectrometers.
spectrum may be obtained from equation (8). Applying these In the detection system, illustrated in figure 2(d), ions which
equations to two masses in the SEFM spectrum separated by pass through each of the focal plane slits and through the
a small mass difference AM, then eliminating C from these second slit plate, SP, produce electrons at the cathode of the
equations and rearranging yields the experimentally obtained channel plate which multiply in the channel plate and are
resolving power collected by the appropriate collector strip located behind the
channel plate. If the detection system is to operate without
detriment to the resolution, then there must be no significant
electron current to adjacent collector strips. This is especially
where AI,is now equal to (n+se+s3), where (Sl+S3) is the important in the CEFM where spatial resolution and thus
spatial width of the image of a single ion mass along the focal closely spaced focal plane slits and collector strips are required.
plane, the term SS resulting from broadening of the ion focus The spatial spreading of the ion beam was determined
in the analysing section of the spectrometer. Thus the experi- experimentally by allowing ions to pass through only one of
mentally obtained resolving power is directly related to the the focal plane slits and monitoring the electron currents to
spatial width of an ion peak along the focal plane and is collector strips adjacent to the primary collector strip. It
directly applicable to the CEFM. was found that significant currents were collected to adjacent
This procedure results in resolving powers which, for collector strips, larger currents being detected on the low
optimum conditions, are approaching 40 at a focal distance mass side (smaller focal distances) as would be expected since
of 2.46 cm increasing to approaching 75 at a focal distance of the magnetic field between the focal plane and the channel
4.60 cm. These resolving powers, by comparison with the plate deflects the ions in this direction. This undesirable
theoretical values of 49 and 92 respectively, show that the effect could be decreased by increasing the voltage on the
experimentally obtained resolution is up to 80% of that second slit plate relative to the focal plane slit plate and thus
expected theoretically. However, with resolving powers of increasing the average energy of the ions in the detection
this order, it would be expected that the peaks in the mass system. For a maximum possible potential difference of 1 kV
ranges illustrated in figure 4(a) and (b) would be completely (limited by the onset of electrical breakdown), the relative
resolved. Since this is not the case, this indicates that although signals to the collectors in order of increasing focal distance
the triangular peak shape is maintained over most of the peak were 0.01, 0.06, 1, 0-008 and 0.002. This situation is expected
width, the region of base of the peak is wider than predicted. to be further improved by the inclusion of a modified collector
This imposes a limitation on the relative heights of adjacent array in which the width of the collector strips is reduced
peaks for which the individual peaks can be distinguished. thereby increasing the gap between collector strips for a given
There is also some indication, as yet unexplained, that the intercollector distance.
resolving power decreases with increasing mass although
insufficient evidence is available to express this effect quanti- 4.2 The constant E field mode
tatively. This effect may be to some extent due to inadequacies The ultimate objective of this mass spectrometer development
in the present data acquisition system for the closely voltage program is to operate the spectrometer in the CEFM. Little
spaced, higher mass peaks. An experimental resolution which experience has been gained to date in operating the device
is less than the theoretical limit is not unexpected since the in this mode since, for the reasons discussed in the introduction
factors which are thought to produce the nonzero intercept to $4.1, the SEFM has been used almost exclusively in the
in figure 5 may also affect the resolution by moving the focal present study. A detailed experimental appraisal in the CEFM
point out of the focal plane (Robinson 1956a, Kuz’min 1971). will logically follow the thorough appraisal in the SEFM
Nevertheless this experimentally obtained resolution is very presented above after minor, but important, modifications
adequate for many purposes and could undoubtedly be have been made to the detection system (§4.1,2).This will be
improved with further experimental investigation. In parti- reported in a second publication. Nevertheless, it is pertinent
cular, when the spectrometer is operated in its design mode, here to discuss the relationship between the two modes of
CEFM, with masses in the range 20-70 U focused at 1 mm operation.
intervals at focal distances from 2-7 cm, then a large propor- Equation (1) can be expressed in the form b/V= Cm where
tion of the adjacent masses would be expected to be well C is a constant for a particular spectrometer. When the
spatially resolved. spectrometer is operated in the SEFM, b is kept constant
At focal distances greater than about 5.3 cm the resolving (= bc) and Vis varied; whereas in the CEFM V is kept con-
power determined in the SEFM decreased, contrary to stant ( = V,) and b is varied. Thus if a mass scan is obtained
theoretical predictions (equation (7)). This behaviour may for the SEFM with b=bc, then the positions of the mass
be explained in terms of the increase in the size of the trajec- peaks for the CEFM with V= Vc may readily be derived
tories for the larger focal distances, the trajectories moving from the expression bcVc=bV, provided that there are no
into regions close to the E field plates and thus into less significant effects due to differences in ion trajectories for the
definable areas of the magnetic field. It is also predicted two cases. Mass scans obtained in the SEFM for a series of
theoretically that, provided the trajectories are within the b values across the focal plane have shown that such effects
limits defined by the stability diagram (figure 3), the resolving only occur for the more extreme trajectories. Using the data
power should be independent of V/ VO.Clearly this is unrealistic shown in figure 4(b) as an illustration of the relationship
where real boundaries exist such as the E field plates, and this between the SEFM and CEFM, the equivalent focal distances
coupled with the small magnetic field gradients at these have been calculated for the CEFM situation for which the

765
N G A d a m and D Smith
spectrometer was designed, that is with the masses focused to the values of 10 ps (Na-) and 17 ps (KT) expected from
at 1 mm intervals along the focal plane. These focal distances equation (10).
were obtained using the E field voltage Vc at which mass In this mode of operation it was possible to use larger
29 U focused at 2.9 cm as an appropriate normalisation point instantaneous currents than in the steady current case. This
and are indicated at the top of figure 4(b). It can be seen that resulted in larger electron currents after multiplication in the
the mass peaks occur at 1 mm intervals as expected and this channel plate for which the transfer characteristic (the
indicates that few difficulties will be encountered in CEFM relationship between the input and output currents) of the
operation, plate under steady conditions was nonlinear (94.4). However,
In order to determine the resolution in the CEFM, it is it has been shown by Goodrich and Love (1968) that for
necessary to know the spatial extent, SI fs3, of the individual pulsed operation with single channeltron multipliers, linear
mass peaks along the focal plane. This can be calculated transfer characteristics could be obtained for output currents
from the experimentally and theoretically determined resolving many times the multiplier strip conduction current provided
powers as given by equations (7) and (9). For an experimental that the pulse width was small (of the order of a few micro-
resolving power equal to 80% of the theoretical resolving seconds) and the duty cycle was low. This additional linearity
power, the spatial extent of each mass peak is (1*25sl+0,2532) is obtained by virtue of the stored charge in the distributed
where SI and s 2 are the entrance and exit slit widths respec- capacitance along the channel length. In the present case
tively for which the experimental resolving power was pulsed ion currents of up to about 10-8 A for a few micro-
obtained. In the present case the slit widths were 0.25 mm seconds could be detected before nonlinearity in the transfer
and thus the extent of each mass peak was 0.38". With characteristic became important. Therefore, for pulsed source
mass peaks focused at 1 mm intervals this would give mass operation, the current range over which the channel plate is
peaks which were totally resolved and an exit slit width of useful in the detection system is greatly extended. Operation
0.38 mm could be used with no loss in resolution and with of the mass spectrometer is however not possible at the highest
maximum sensitivity. However, in the prototype spectrometer, current levels since severe space charge repulsion occurs in
some broadening occurs in the wings of the mass peak and the analysing section of the spectrometer (54.4).When oper-
thus total resolution is not obtained. In this case, the cross- ating the mass spectrometer in the pulsed mode it is essential
talk (defined as the contribution at the centre of one mass to prevent the signal to one collector from being capacitively
peak by an adjacent mass peak expressed as a fraction of the coupled to adjacent collectors. For the present detection
height of the adjacent peak) can be reduced by reducing the system, it was found that about 8 % of a 4 ps voltage pulse,
exit slit width; this however also results in a reduction in derived from a pulse generator and applied to any collector
sensitivity. In common with other magnetic mass spectro- strip relative to the other collector strips, is induced onto the
meters the degree to which the reduction in slit width is adjacent collectors, This imposes an additional limitation
necessary, is therefore dependent on the cross-talk and the on the ability of the detection system to distinguish a small
signal intensities which can be tolerated and on the detailed mass peak at a mass 1 U different from a large peak. This
shape of the mass peaks (the detailed peak profile can be effect could be reduced by decreasing the collector strip width
experimentally obtained in the SEFM using very narrow exit and thus reducing the intercollector capacitance and is, of
slits). course, no problem in the steady current case.

4.4 Mass discrimination: current and pressure limitations


4.3 Operation with a pulsed ion source
In principle in this type of mass spectrometer no mass discri-
The ability of this spectrometer to mass analyse ions from a
mination should occur since any ion injected into the analysing
pulsed source is clearly important in cases where the source
section will be focused to the focal plane. However, in practice
of ionization exists for only a short period of time (for example
discrimination can occur due to the mass dependent loss of
in microparticle impacts (Adams and Smith 1971; Smith and
ions to the defining plates of the spectrometer or through the
Adams 1973)) or where signal intensities are low and phase
sides of the analysing section. The former process can effec-
sensitive detection is desired. In this mode of operation a
tively be eliminated by operating within the limits set by
further feature of the spectrometer becomes apparent, this
figure 3. The loss of ions through the sides of the analysing
being that the flight time of an ion through the spectrometer
section is determined jointly by the component of ion energy,
from entrance to exit slit is mass dependent. The flight time
eVp, in the direction parallel to the magnetic field and the
is simply given by ion flight time. This effect can be eliminated by correct design
of the ion source such that the time for an ion to reach the
side of the spectrometer is greater than the flight time. This
is represented by the inequality eVp< l2B2e2/87i2m where
(for example Page and Adams 1969) and is thus independent 21= (12 - h), 11 and 12 being the lengths of the entrance and
of the electric field strength, the ion injection energy and the exit slits respectively. In the present spectrometer this limits
focal distance. the maximum ion energy eVp parallel to the magnetic field to
A study has been made of the operation of the spectrometer (10 m)-1 eV, where m is the ion mass in atomic mass units,
with a pulsed ion source using the Kunsmann source (83.1). if there is to be no mass discrimination. This is difficult to
Pulses of ions of a few microseconds duration were injected achieve in practice and thus some discrimination against the
into the spectrometer at 0.5 s intervals by pulsing the ion higher masses is expected to occur, the degree of discrimina-
injection voltage, and the ion flight times were determined tion being dependent on the magnitudes of ion velocity
using a storage oscilloscope directly connected to the appro- components parallel to the magnetic field and on the ion mass.
priate collector strip. In this mode of operation, the individual Limitations to the ion currents for which the present
ion signals were focused on the collector by adjusting the spectrometer can be successfully operated are to a large
E field and the ion flight times determined for both the Na+ degree determined by the detection system. At low ion currents
and K+ ions. This was repeated for several focal distances, the dark current of the channel plate becomes important.
the ion flight times being found to be independent of the Under the operating conditions of the present experiments
focal distance and to be equal to within experimental limits and for the type of channel plate used, the dark current to

766
Multicollector mass spectrometer
each collector strip is equal to about 5 x 10-l5to 5 x 10-14 A voltage. Also a channel plate multiplier has been included
(Guest 1970). Thus, in practice, the lower current detection between the slits and the collector slats to improve the
limit will generally be set by the sensitivity of the post-channel detection sensitivity of the spectrometer. This multiplier has
plate detector. In the work reported here a limiting sensitivity been operated, for the first time to the authors’ knowledge,
of 10-13 A has been achieved, thus resulting in a minimum in a strong ambient magnetic field which has allowed the
detectable ion current of about A with a channel plate channel plate to be positioned close to the focal plane of the
gain of about 103. spectrometer and thus avoids the inevitable loss of resolution
At the higher current levels, as mentioned above, the transfer associated with operating remotely from the magnetic field
characteristic of the channel plate becomes nonlinear and (and hence from the focal plane). Such was possible since no
thus the usefulness of the device for determining relative ion loss of gain was apparent when the channel plate was operated
signals js impaired. Noticeable departures from linearity in the magnetic field.
occur when the electron current through the channels irradiated The use of a Kunsmann ion source to provide ions of
by the ion beam becomes an appreciable fraction of the known mass (Na+ and KT)has demonstrated that the location
current passing through the walls of those channels due to of individual mass peaks on the focal plane is accurate to
the potential difference applied across the channel plate. For about 1 mm (equivalent to 1 U) along the complete length of
channel plates of the type used in the present experiments, the the focal plane if their position is calculated using the measured
operation is linear up to constant output currents of less than E and B values in conjunction with the elementary theory
5% of the conduction current (Manley et al. 1969). Thus for (equation (1)). Final calibration of the device is also achieved
exit slit areas of 2 x 10-2 cm2 and an applied voltage of 1 kV, by determining the foci of the Na+ and K + ions. The relative
a maximum constant output current of about 5 x 10-10 A is magnitudes of adjacent peaks which can be distinguished is
possible. This is equivalent to an ion input current of 5 x 10-13 limited by a small amount of broadening at the base of the
A. The data of figure 4 was obtained at currents approaching mass peaks. From a detailed study of the mass spectra, it is
this value yet no flattening of the peak tops was observed as concluded that this broadening could be reduced, a consequent
would be expected if the transfer characteristic became signi- improvement in resolving power obtained and a reduction in
ficantly nonlinear. The spectrometer could of course be used the unexpected and undesirable dependence of resolving
at even higher current levels if the channel plate was omitted power on the ratio V/VOachieved by an increase in the
and in this case the maximum permissible current would be uniformity of the magnetic field. The effect of nonuniformities
determined by space charge repulsion in the passage of the in the magnetic field is exaggerated by the large angular
ion beam through the spectrometer. Robinson (1956b) has divergence and energy spread of the ions emanating from
considered the effect of space charge repulsion on the focusing the ion source; if this were reduced then an overall improve-
properties of cycloidal focusing mass spectrometers under ment in the spectrometer resolution would result. Some
steady conditions. From his theoretical analysis, it can be reduction in resolution also occurs in the detection system
shown that for the present instrument a factor of two decrease due to significant overlap of ion beams from adjacent focal
in the resolution would be expected to occur in the analysing plane slits at the cathode of the channel plate. It then becomes
section at an ion beam current of about 5 x 10-11 A for an important, if acceptable resolution in the CEFM is to be
ion mass of 70 U. The effect would be considerably less for obtained, to ensure that the separation between the collector
lower masses since the broadening is dependent on the square slats is greater than the distance by which the beams overlap.
of the ionic mass. Thus it is possible for this spectrometer to These are the guiding principles by which the new collector
be operated with ion currents varying over many orders of array has been designed, details of which will be presented in
magnitude with no change in resolution. a future publication.
As in all mass spectrometers, there is a maximum operating
pressure above which the spectrometer cannot be operated
due to ion-neutral collisions within the analysing section and Acknowledgments
above which high voltage electron multipliers cannot be used The authors wish to express their thanks to Professor J Sayers
because of the dangers of electrical breakdown. For the present and Professor A P Willmore for their interest in this work
spectrometer the maximum length of a focused ion trajectory and for the provision of laboratory facilities. Thanks are also
is about 20cm. Thus operation at pressures for which the due to the department’s mechanical workshop staff for the
ion-neutral mean free path is less than this value is unsatis- construction of the mass spectrometer and its vacuum
factory and this limits the maximum pressure to about housing. We are also grateful to Dr A G Dean for helpful
5x Torr. This is well within the operating pressure range discussions and to Mr D C Newey for technical assistance.
of channel multiplier plates since these devices have been
satisfactorily operated at much higher pressures (Turner et al. References
1969). Adams N G and Smith D 1971 Planet. Space Sci. 19
195-204
5 Conclusions Barnett C F and Ray J A 1970 Reu. Sei. Instrum. 41 1665
The object of this paper has been to present a new approach
to the problem of simultaneously detecting and separately Blauth E W 1966 Dynamic Mass Spectrometers (Amsterdam :
monitoring the individual ionic species generated in an Elsevier)
ionisation source which may be fluctuating in intensity or of Bleakney W and Hipple J A 1938 Phys. Rev. 53 521-9
only very short duration. To this end, the design, construction Eberhardt P 1960 C. R. Soc. R i m Suisse Phys. 33 588-90
and experimental appraisal of a prototype cycloidal focusing
Elliott R M 1963 Mass Spectrometry ed C A McDowell
multi-collector mass spectrometer and an associated detection
(London : McGraw-Hill) pp 69-103
system are discussed in detail. This instrument is designed to
monitor species in the mass range 20-70 U, though this mass Ewald H 1956 Handbuch der Physik Vol 33 (Springer-Verlag)
range can be varied by altering the number and spacings of pp 546-608
the individual slit and collector slat combinations in the Goodrich G W and Love J L 1968 IEEE Trans. Nucl. Sci.
detection system and by operating at an appropriate E field NS15 190-4

767
N G A d a m and D Smith
Greaves C 1969 Vacuum 20 65-73
Guest A J 1970 Mullard Tech. Commun. 11 170-6 Rotation between
Hachenberg 0 and Brauer W 1959 Adv. Electronics. Electron
Phys. 11 413-99 micrographs from the
Hahn Y B, Hebner R E, Kastelein D R and Nygaard K J
1972 Rev. Sci. Instrum. 43 695-6
scan n i ng electron
Huber W K and Trendelenburg E A 1962 Trans. 8th Nut. microscope and electron
Vac. Symp. 1961 (London: Pergamon) pp 592-7
Jennings K R 1971 Mass Spectrometry, Techniques and
channelling patterns
Applications ed G W A Milne (London: Wiley) pp 419-58
Kuz'min A F 1971 Soviet Phjs.-Tech. Phys. 16 599-602
Manley B W, Guest A and Holmshaw R T 1969 Ado.
Electronics Electron Physics A28 471-86
Monk G W and Werner G K 1949 Rev. Sci. Instrum. 20
93-6
Nier A 0 and Hayden J L 1971 Int. J . Mass Spectrom. Ion. C G van Essen? and J D Verhoeven
Phys. 6 339-46 Ames Laboratory USAEC and Department of Metallurgy,
Iowa State University, Ames, Iowa 50010, USA
Page L and Adams N I 1969 Principles of Electricity
4th edn (Amsterdam: Van Nostrand) pp 237-40
Received 26 hrovember 1973
Paul W, Reinhard H P and von Zahn U 1958 Z . Phys. 152
143-82 Abstract When a large single crystal is examined in the
Robinson C F 1956a Rev. Sci. Instrum. 27 509-12 scanning electron microscope, micrograph and electron
Robinson C F 1956b Rev. Sci. Insfrum. 27 512-3 channelling pattern (ECP) may be obtained simultaneously.
When obtaining the selected area ECP of a small crystal, a
Robinson C F and Hall L G 1956 Rev. Sei. Instrum. 27
separate micrograph must be taken. Relating the ECP to
504-8
the micrograph in either case, the crystallographic direction
Smith D and Adams N G 1973 J. Phys. D : Appl. Phys. 6 of the centre of the micrograph is correctly indicated by the
700-1 9 pole direction of the centre of the ECP. But the directions
Turner P J, Cartwright P, Southon M J, Van Oostrom A of planes with normals orthogonal to the optic axis may not
and Manley B W 1969 J. Phys. E: Sci. Instrum. 2 731-3 be correctly indicated, errors of up to 30" having been
measured. The error may occur in any scanning electron
microscope with a double-deflection scan system, whether
above or below the final lens, and is due to a relative
rotation of the planes of the upper and lower scan
deflections. The error can be eliminated by using a single
scan deflection, as in the deflection-focusing method of
obtaining selected-area ECPs.

1 Introduction
A crystalline specimen examined in the scanning electron
microscope (SEM) may exhibit an electron channelling pattern
(ECP). The conditions necessary are a high probe current,
a low probe divergence and a sufficient variation in direction
of incidence in the course of a scan (Coates 1969, Booker
1970). The conditions of probe current and divergence are
set by a suitable choice of condenser lens currents and aper-
ture sizes. The variation in direction of incidence is commonly
achieved by one of two scanning methods, double-deflection
or deflection-focusing (van Essen et al. 1971).
Double deflection scanning is the normal method of
scanning used in the majority of commercial SEMs. The large
change in direction of incidence is accompanied by a large
change in position, so this method is only of use for large
specimens (several millimetres across). It is clear that the
ECP and micrograph may be relatively rotated if the final
lens current has to be changed between ECP and micrograph.
However, it is possible to adjust the probe so that ECP and
micrograph are visible at the same time, and it might be
assumed that the ECP then gives the orientation of surface
features.

Journal of Physics E: Scientific Instruments 1974 Volume 7 ? Now at PA Technology and Science Centre, Winship Road,
Printed in Great Britain 0 1974 Milton, Cambridge

768

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