EFM3Omicron UserManual2013
EFM3Omicron UserManual2013
EFM3Omicron UserManual2013
9
April 08
_____________________________________________________________________
Limburger Str. 75 D-65232 Taunusstein Germany
Tel.: +49 (0)6128 / 987-0 , Fax: +49 (0)6128 / 987 185
2 EFM-Manual
Version 3.9
Field of Application 3
Copyright
The information in this document is subject to change without notice and does not repre-
sent a commitment on the part of Omicron Nanotechnology / Focus GmbH. No liability
shall be accepted for any damages resulting from the use of this documentation and the
related product.
No part of this manual may be reproduced or transmitted in any form or by any means,
electronic or mechanical, including photocopying and recording, for any purpose without
the express written permission of Omicron Nanotechnology / Focus GmbH.
Product names mentioned herein may be trademarks and/or registered trademarks of
their respective companies.
Related Manuals
EVC 300 / 300s
EVC 100 / 100s Power supplies for EFM
EVC 100 L
Power supply for EFM with
EVC 300i
IBAD functionality
April 08
4 EFM-Manual
Field of Application
The EFM 2, EFM 3, EFM 3s, EFM 4, EFM 3T or EFM 3i is an evaporator that can be
used to evaporate metals and other materials from rods or a crucible in vacuum.
The UHV evaporator EFM 2, EFM 3, EFM 3s, EFM 4, EFM 3T or EFM 3i must always be
used in combination with a CE-complying power supply e.g. EVC 300, EVC 300s,
EVC 300i, EVC 100, EVC 100s or EVC 100L.
The EVC power supplies and the EFM UHV evaporators must always be used:
• with original cable sets which are explicitly specified for this purpose
• with all cables connected between the evaporator and the power
supply
Version 3.9
Table of Contents 5
Table of Contents
Copyright ..................................................................................................................3
Related Manuals.......................................................................................................3
2. Installation..................................................................................................................20
2.1 Water Cooling...................................................................................................20
2.2. Electrical Connections EFM 2/3/3s/4/3i............................................................21
2.3. Electrical Connections EFM 3T........................................................................21
2.4. Shutter Positions EFM 3T ................................................................................23
2.5. Gas inlet of EFM 3i ..........................................................................................23
4. Operation....................................................................................................................28
4.1. Bakeout ...........................................................................................................28
4.2. Degassing the evaporator................................................................................28
4.3. Degassing a crucible .......................................................................................29
4.4. Degassing the evaporant .................................................................................30
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5. Maintenance .............................................................................................................. 34
5.1. Cleaning .......................................................................................................... 34
5.2. Filament Exchange.......................................................................................... 34
Changing the filament of EFM 2/3/3s/4: ........................................................ 35
Changing the filament of EFM 3T:................................................................. 36
Changing the filament of EFM 3i: .................................................................. 37
5.3. Replacing the Evaporant Holder Ceramics...................................................... 38
6. Fault diagnostics....................................................................................................... 39
Appendix........................................................................................................................ 41
A. Background for Material Selection and Evaporation Parameters ....................... 41
Material overview .......................................................................................... 44
B. List of Thermovoltage ........................................................................................ 48
C. Calibration of Flux Monitor ................................................................................. 49
D. Literature ........................................................................................................... 50
General literature .......................................................................................... 50
IBAD evaporation with EFM 3i....................................................................... 50
E. Options .............................................................................................................. 51
E 1. Crucibles................................................................................................ 51
E 2. Shutter Motor ......................................................................................... 53
E 3. Port Aligner............................................................................................ 53
E 4. Elongated target shift (50mm) ............................................................... 53
E 5. Barrel connectors for larger rods ........................................................... 54
E 6. Quick-lock water hose connectors ......................................................... 54
Decontamination Declaration....................................................................................... 57
Version 3.9
1. Description and Specifications 7
In the UHV evaporators EFM 2, EFM 3, EFM 3s, EFM 4, EFM 3T and EFM 3i the evapo-
rant is either evaporated from a bar, from a rod or from a crucible. This is achieved by
electron bombardment heating. The bombarding electron beam induces a temperature
rise of the evaporant, causing evaporation.
The crucible-free evaporation is characterised by an ultimate degree of cleanliness with
only slight increases of background pressure. From appropriate crucibles (see appendix
A) low melting point, low vapour pressure or reactive materials can be evaporated. The
instrument is designed for high precision sub-mono-layer up to multi-layer deposition of a
wide variety of evaporants including highly refractory materials.
A key feature of the EFM is the integrated flux monitor (not EFM 2, but the flux monitor
can be upgraded later). Once calibrated by a quartz thickness monitor, the flux monitor
can replace the quartz balance by continuously monitoring the evaporation rate. Flux is
measured directly, which allows a much more precise rate adjustment and much faster
rate control than an indirect, i.e. temperature measurement by a thermocouple. For preci-
sion layer control, an external signal of a calibrated monitor (quartz balance or MEED
oszillations) can be used for regulation with the EVC 300 series power supplies.
The beam exit column contains an ion collector which serves as a flux monitor. At a given
electron emission current (IEM) and e-beam energy the ion flux measured there is
directly proportional to the flux of evaporated atoms. The ion flux is shown on the
display of the EVC power supply; with the power supplies EVC 300 / EVC 300s /
EVC 300i the heating power (i.e. the high voltage) can be regulated to obtain a constant
growth rate. The flux monitor also operates with the shutter closed thus allowing to pre-
set the evaporation rate.
Some growth processes require an ion free deposition. This requirements can be fulfilled
with the optional ion suppression lens (EFM 3s/EFM 3i). The lens deflects the ionised
material vapour back into the EFM. Only the neutral material vapour can reach the sam-
ple.
The EFM comes with a shutter at its outlet which can be opened and closed by a rotary
drive (not EFM 2, but the shutter can be upgraded later). This allows precise flux adjust-
ment prior to exposure, and exact control of the evaporation time. As an option, the shut-
ter can be motor operated under computer remote control together with the power sup-
plies EVC 300 / EVC 300s / EVC 300i.
The evaporation cell is enclosed in a water-cooled copper cylinder (cooling shroud). This,
and the fact that just a restricted region of the evaporant is heated, facilitates to keep the
background pressure during evaporation below 10-10 mbar. But this also depends on the
target material and on the pumping speed of the vacuum system. Some evaporants and
crucibles contain huge amounts of gas that are deliberated on heating.
1.1. EFM 2
The single evaporator EFM 2 is the basic version of the standard evaporator EFM 3. The
EFM 3 features shutter and flux monitor can be upgraded (user and factory upgrade pos-
sible) at the EFM 2.
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Version 3.9
1. Description and Specifications 9
Further properties and test results of the EFM 3i prototype are described in:
“An evaporation source for ion beam assisted deposition in ultrahigh vacuum”,
J. Kirschner, H. Engelhard and D. Hartung,
Rev. Sci. Intrum., Vol. 73, No. 11, Nov. 2002.
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1.6. Specifications
Specifications EFM
cooling water flow: > 0.5 l/min at T ≈ 30°C, max. pressure = 6 bar
Version 3.9
1. Description and Specifications 11
Specifications EFM 3T
beam spot diameter at the sample 15mm with 5mm I.D. exit aperture
11mm with 4mm I.D. exit aperture
8.5mm with 3mm I.D. exit aperture, see Fig. 1.2
Specifications EFM 3i
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E F M 4 - s p o t p ro file
F la n g e -s a m p le d is ta n c e 3 0 0 m m
M o -c ru c ib le , 8 m m d ia m e te r
layer thickness [arb. units]
u s e a b le s p o t d ia m e te r 3 6 m m
p o s itio n [m m ]
position [mm]
Version 3.9
1. Description and Specifications 13
EFM4
Beam diameter (mm)
EFM3
EFM3T
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EFM 2
Similar to the dimensions of the EFM 3, but without rotary and BNC feedthrough. The
evaporator outlet is a little bit smaller, but has the same length.
EFM 3/3s/4
Fig. 1.3: Outer dimensions and feedthroughs of the EFM 3/4 and EFM 3s. The HV-
feedthrough is mounted on a linear motion drive that moves only the evaporant. Its travel
is 25mm, 50mm optional. The EFM 3s has an additional ion lens (ION Suppressor), which
is connected to a SHV feedthrough.
Version 3.9
1. Description and Specifications 15
Fig. 1.3: (continued) Outer dimensions of the EFM 3 /EFM 3s from the rear view and
the shutter dimensions for EFM 3 /EFM 3s. A tube of 40mm diameter is
needed to fully open the shutter.
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EFM 3T
Version 3.9
1. Description and Specifications 17
Fig. 1.4: Outer dimensions and feedthroughs of the EFM 3T. The lower drawing
shows the max. space needed for the shutter. If no simultaneous evapora-
tion is needed 25mm is sufficient (Shutter Position C in Fig. 2.7). All HV-
feedthroughs are mounted on linear motion drives that move only the
evaporant (25mm travel)
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18 EFM-Manual
EFM 3i
Fig. 1.5 Outer dimensions and feedthroughs of the EFM 3i. The HV-feedthrough is
mounted on a linear motion drive that moves only the evaporant. Its travel
is 25mm, 50mm optional.
Version 3.9
1. Description and Specifications 19
Fig. 1.5: (continued) Outer dimensions of the EFM 3i shutter. A tube of 40mm di-
ameter is needed to fully open the shutter.
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20 EFM-Manual
2. Installation
The important outer dimensions for installation of the EFM-evaporators are shown in fig.
1.3-1.5.
For the EFM 2/3/3s/4/3i a chamber tube size with an inner diameter of at least 34 mm is
sufficient for pumping. The maximum tube length allowed is 180 mm (200mm for EFM 4),
otherwise the shutter cannot be fully opened.
The EFM 3T needs a tube of 35 mm diameter; the tube length should not exceed
145 mm, otherwise a tube diameter of 70mm is needed to fully open the shutter of 50mm
to open the individual cells (see. fig. 1.4).
For special length (optionally available) correct the dimensions for the insertion depth or-
dered.
For operation with a rod the EFM can be mounted in any orientation, although caution
should be applied when aiming downwards. At temperatures above the melting point the
evaporant may dislodge and fall out of the crucible used. When in operation with a cruci-
ble a minimum incline of 20° with respect to the horizontal (flange to sample) is recom-
mended. Many materials wet the crucible surface, in this case nearly horizontal mounting
is also possible. For changing the evaporant (rod or crucible) a free space of about
200 mm at the HV-feedthrough side of the EFM is required.
The best direction to evaporate is along the sample normal. Then the evaporated layer
will be most homogenous. At other angles the evaporant spot looks elliptical and the den-
sity of deposited atoms is different along the small and the long ellipsoidal axes.
Adjustment:
If the sample itself can be adjusted a port aligner is not required. The optional port aligner
allows a tilt of ± 3°. If using a port aligner the inner diameter of the chamber tubing should
be larger than 35 mm and the tube length should be as short as possible, at best shorter
than 50 mm. Only then the full tilt of ± 3° can be used.
The glowing filament of the EFM makes a light spot at the sample (shutter opened). The
illuminated area is identical with the actual deposition area. A viewport looking towards
the sample helps to align its position.
Version 3.9
2. Installation 21
Using liquid nitrogen as the cooling fluid is possible in principle, but usually not needed
due to the low background pressure during evaporation if the source is properly degassed
before operation.
B
C
Fig. 2.4: Flange connector for thermocouple and filament from atmos-
pheric side:
A) Filament + B) Filament –
C)Thermocouple CuNi (neg.) D) Thermocouple NiCr (pos.)
Attention: The high voltage cable is attached to the SHV socket "HV" (at the rear of the
linear transfer). The flux monitor cable is attached to the lateral voltage feedthrough "FM"
(inclined stud with BNC connector).
Checks
Check the resistance between filament pins A and B at the 4 pin feedthrough. It should be
R < 1 Ω. None of these pins should have contact to ground.
The resistance R between pins D and C (thermoelement) and from each pin to ground
should be R < 2 Ω. Special length EFMs can have higher resistances.
For checking the short-circuit safety of the rod (or crucible) check the resistance between
HV and ground and HV and filament. It should be R > 2 MΩ. Connect HV-cable in the
non-evacuated state. For safety reasons the evaporator must be mounted at the vacuum
chamber. Switch on the electronics. Set the high voltage to approx. 400V. There should
be no spark-over noticeable.
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22 EFM-Manual
F
E
A
D B
Fig. 2.5 : Flange connector for Filament and Thermocouple from atmos-
pheric side:
F) Filament cell 1
A) Filament cell 2
B) Filament cell 3
C)Thermocouple CuNi (neg.)
D) Thermocouple NiCr (pos.)
E) Filament GND
A
D
B
C
Fig. 2.6 : Flange connector for Flux monitors from atmospheric side:
A) Flux monitor cell 1
B) Flux monitor cell 2
C) Flux monitor cell 3
D) not connected
Checks
Check the resistance between the filament pins F, A and B and pin E at the 6 pin
feedthrough. It should be R < 1 Ω. None of these pins should have contact to ground.
Version 3.9
2. Installation 23
A B C
D E F
G H
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24 EFM-Manual
3.1. Mounting the evaporant in EFM 2, EFM 3, EFM 3s, EFM 4 and
EFM 3i
For initial mounting and/or later changing of the evaporant the rear CF 16 flange (HV
feedthrough see fig. 1.3 and 1.5) is used. Loosen this flange and cautiously pull the sup-
port of the evaporant out of the furnace body. A Ø 2 mm molybdenum rod serves as a
mounting post.
The evaporant should be spot welded to the molybdenum post or the Mo-barrel connector
delivered with the EFM may be used to support the rod (see fig. 3.1). Always use ex-
tremely clean material.
Good dimensions for evaporation material are bars of 1.5-2.5 mm diameter. Optional Mo-
barrel connectors that support larger rods are available (see App. E). Two or three twisted
wires with a diameter of 1 mm or less are also possible. Only for materials with very high
evaporation temperatures smaller diameters can be used to reach the maximum tempera-
ture with lower heating powers.
With "soft" materials such as gold, good results can be obtained if the rod evaporant is
mechanically supported by an appropriate spiral of a non-alloying metal. For gold wire of
1 mm dia. a supporting tungsten spiral (made e.g. from 0.25 mm wire) can be used. For
easier handling use a tungsten crucible.
The total length of the evaporant must not exceed 50 mm (see fig. 3.1), or there would be
a danger of short-circuiting the tip of the rod to the housing. A typical length of evaporant
(to be on the safe side) would be 45mm. The tip of the evaporant should not intersect the
plane defined by the filament wire.
Centre the rod before inserting into the evaporator
For inserting the evaporant set the linear feedthrough to maximum length (fully counter-
clockwise), otherwise the filament wire may be destroyed whilst inserting. Carefully feed
the slide bearing through the centre of the rear opening into the copper cooling body. The
evaporant bar must not be bent.
Check the concentric position of the rod through the beam outlet (with the shutter
being open and a suitable illumination) and correct when necessary.
We recommend a careful ex-vacuum alignment of the evaporant to the centre (with about
± 1 mm accuracy). Note that the HV-flange and the end-flange of the linear motion
feedthrough both carry a mark for reproducible positioning.
Tighten the mini flange. Check that there is no short circuiting of the evaporant to the
filament or to the cooling shroud using an ohmmeter. Resistance between HV and ground
should be > 2 MΩ.
Version 3.9
3. Mounting and changing the evaporant 25
Evaporant (rod)
Cooling shroud Thermocouple
Filament
Flux monitor Slide bearing
Barrel connector
max. 50mm
Fig 3.1: Fitting a rod: We recommend to spot weld the evaporant to the
mounting post as it guarantees cleanliness. Where this is not
applicable use the Mo made barrel connectors (shown here).
Mounting a crucible
Available crucibles are made of tungsten, molybdenum, graphite, tantalum, Al2O3, pyro-
lytic boron nitride (pBN), zirconium oxide (ZrO2), beryllium oxide (BeO), or stainless steel
with nozzle. For sizes of the crucibles see section E.1. The EFM 3i is restricted to cruci-
bles with a maximum outer diameter of 8 mm A crucible is mounted using a molybdenum
barrel connector as shown in Fig. 3.2. Check the length of the crucible (40 mm). Note that
the HV-flange and the end-flange of the linear motion feedthrough both carry a mark for
reproducible positioning.
Check the concentric position through the beam outlet (with the shutter being open
and a suitable illumination) and correct when necessary.
We recommend a careful ex-vacuum alignment of the crucible to the centre (with about ±
1 mm accuracy). Note that the HV-flange and the end-flange of the linear motion
feedthrough both carry a mark for reproducible positioning.
The crucible can be refilled through the mini CF flange "HV" at the rear end. A new cruci-
ble should thoroughly be degassed (see 4.1 and 4.2) prior to initial loading with evaporant
material.
Crucible (S and L)
Filament Cooling shroud Thermocouple
Flux monitor Slide bearing
Barrel connector
∼40mm
April 08
26 EFM-Manual
The evaporant can be spot-weld to the 1.5 diameter molybdenum rod that is delivered
with the evaporator or alternatively can directly be inserted into the Mo barrel connector.
For the EFM 3T only the standard Mo barrel connector is available.
For mounting the rod into the evaporator proceed as described in sec. 3.1. referring to
fig. 3.3.
Slide bearing ceramics
Filament Evaporant (rod) Barrel connector
Fig 3.3: Fitting a rod in EFM 3T: in this picture the evaporant is directly
inserted in the barrel connector.
Mounting a crucible
All available crucibles are listed in section F.1. All crucibles with a maximum outer diame-
ter of 8 mm can be used with the EFM 3T. A crucible is mounted on a 1.5mm dia. molyb-
denum post which is directly inserted into the Mo-clamp that also serves as a slide bear-
ing (Fig. 3.4).
For mounting of the crucible into the evaporator proceed as described in sec. 3.1. refer-
ring to fig. 3.4.
Version 3.9
3. Mounting and changing the evaporant 27
Flux Monitor
max. 20mm
Cooling Shroud
∼ 40mm
• Move the evaporant forward. The top of the evaporant should be beyond the fila-
ment plane.
• Apply a HV of 600-800V; start to heat the evaporant with filament current regula-
tion. Wait until a constant emission current stabilizes (e.g. 5-10mA).
• Retract the evaporant using the linear motion until the emission current has
dropped to 75% - 80% of the initial value.
For rod evaporation the linear motion must be used to compensate for the shorten-
ing of the rod during evaporation!
This procedure also gives a good evaporant position for normal evaporation!
April 08
28 EFM-Manual
4. Operation
A thorough bake-out and degas of both the evaporator and the evaporant (respectively
the crucible) is required to obtain a good background pressure and clean evaporation.
4.1. Bakeout
The EFM evaporators are fully bakeable to 250° C. Remove all cabling and the water
hoses for bake-out. Before bake-out the cooling water should be blown out of the evapo-
rator.
• Set the high voltage to zero. Otherwise the e-beam voltage would heat the evaporant.
• Slowly increase the filament current up to about 2 A. Take care that the filament pro-
tection is set to 2.5 A at the power supply EVC 300/300s/100/100s.
• The copper cooling shroud gradually heats. It will take 1 to 2 hours until a temperature
of 200 to 300° C is reached.
Note that due to the smaller filament and larger mass the EFM 3T will heat up slower if a
single filament is used. It is recommended to degas all cells to be used. All three filaments
can be used simultaneously if the power supplies are available.
Degas with evaporant heating (EVC 100L, EVC 100/300)
• Gradually increase the current until emission starts (typically at 1.8 A filament
currrent). Set to an emission current of about 5 mA (1 W heating power).
Version 3.9
4. Operation 29
• If no emission can be obtained with the standard filament currents, cautiously move
the crucible, rod with the linear motion towards the filament. Take care not to touch
the filament with the crucible, because of the danger of destroying the filament.
• The temperature of the cooling shroud will rise faster during degassing than without a
crucible.
• Degas the evaporator until the desired shroud temperature is reached. The overheat
protection of the EVCs will switch of the heating power, when exceeding the overtemp
temperature (preset 300°C for all EVC)
If a low temperture melting target is used, this degas procedure cannot be used. If neces-
sary, degas the evaporator with an empty molybenum crucible before installing the target
This procedure can also combine the degas of an empty crucible and the evaporator.
First degas the evaporator without cooling, then degas the crucible with water cooling (
see sec. 4.3.
• Start heating the crucible as described in sec. 4.5 with a low heating power of about 5
to 10 W (2 to 5 W for small crucibles).
• Watch the pressure in the main chamber, in order to prevent internal HV break
through. The pressure should not exceed 5⋅10-6 mbar during degassing.
• Watch the Flux monitor reading, if available! A decreasing flux vs. time
characteristics indicates that impurities are degassing, whereas a constant or
increasing flux shows that bulk material is evaporating.
• Slowly increase the heating power. Take care not to exceed the maximum allowed
temperature. The crucibles may not be degassed with the maximum allowed tempera-
ture if the evaporation temperature needed is quite low.
The different crucibles can be degassed with different maximum heating powers due to
their maximum allowed temperature and size (compare with Fig. 5.1 and table E1).
For standard size W, Mo and Ta crucibles you may apply up to 150 Watts heating power,
where Mo itself will start to evaporate weakly from the crucible. For small size crucibles
use only 40 Watts for degassing. If the purity of the crucible material is insufficient it may
need cleaning procedures as referred to in sec 4.4.
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30 EFM-Manual
For PBN and the oxide crucibles only considerably lower heating powers may be applied,
depending on the size of the crucibles. E.g. for a medium size crucible a degassing power
of less than 30 W is recommended.
Note: Gas or contaminations desorbing from the evaporant and the inner
walls of the cooling shroud are indicated by the flux monitor. Such
impurities show a decreasing flux vs. time, whereas the evaporant
material yields a stable or increasing flux. This initial degassing can
take several hours. Generally the cleanness of evaporants will im-
prove even after several days of operation
If the purity of your evaporant material ("as bought") is insufficient, it may be worthwhile to
apply a combination of thermal and chemical cleaning procedure. Refer, e.g.,. to :
R.G. Musket et al., "Preparation of Atomically Clean Surfaces of Selected Ele-
ments: A Review", Appl. Surf. Sci. 10 (1982) 143-207.
Although these procedures are applied to surfaces, many of them, such as heating in
oxygen in order to remove carbon impurities, will also work well for the depletion of bulk
material.
4.5. Evaporation
After sufficient degassing start with evaporation:
• Set the HV to about 600V to 800V and the filament current to about 1.5 A
• Slowly increase the filament current until emission starts and the flux monitor indicates
an ion flux (positive polarity) in the 1 nA range.
• Slowly increase the heating power to obtain the flux needed. Wait always until the flux
monitor reading stabilises. In case of a sudden increase of the flux monitor current
immediately reduce the emission current.
• Especially when using crucibles the warming up time makes the reaction time slow.
Take your time to find the correct settings for a new material!
The ion current is proportional to the evaporation rate and the emission current. At a
given HV and sample position this current is directly proportional to the flux of evaporated
atoms.
The operational conditions depend strongly on the evaporated material and on the choice
of rod or crucible evaporation. Typical operational parameters are given in Appendix A. A
typical value for the evaporation rate is about one monolayer per minute.
For crucible operation Fig. 4.1 shows typical temperatures reached with given heating
powers. Together with the parameters given in App. A the needed heating power can be
estimated.
For low-temperature materials such as C60 or organic materials a small high voltage of
only 100V or a few 100V may be appropriate. It may be necessary to increase the high
voltage to 900V or 1000V for high-temperature materials such as tungsten or generally
for rod-evaporation due to electronoptical properties of this geometry. Owing to space
charge effects there will be a drastic increase in the emission current with the same fila-
ment current and thus in the heating power that can be obtained.
With small evaporation rates of about hundred Å per day one filling may last for months.
Of course, rod-evaporation (diffuse in all directions) is less effective than crucible-
evaporation (more directional) and also the evaporant volume of a rod is comparably
small. However, since there is no crucible involved, the cleanness of rod-evaporation is
generally higher if one uses very clean material. In certain cases (e.g. Fe) crucible evapo-
ration can be cleaner, because it is possible to clean the evaporant by melting it entirely.
medium
Crucible temperature (°C)
large
April 08
32 EFM-Manual
• self ions that are created from the metal vapour itself
• add-ions of the additional gas, e.g. noble gas atoms, that are provided by the gas
inlet flange with a leak valve.
The ions are then focussed onto the sample using the ion lens; the flux monitor measures
the remaining fraction of the . Proceed as follows:
• Connect the ion lens (SHV-feedthrough Lens) to the lens voltage at the EVC300i
Version 3.9
4. Operation 33
• Start with evaporation as described. Allow additional gas for ion production as
necessary.
• Set the lens voltage to 75%-80% of the high voltage applied to the evaporant to
maximize the ion current reaching the sample. Watch the sample current.
A pulsed ion beam can be obtained by switching the lens voltage from it optimum focus-
sing condition (75-80%) to its minimal value (ca. 10V). Then the ion beam is not focused
and only a very small fraction of the initial ion flux reaches the sample.
Attention: The ion flux may differ from the value measured with
“SUPR OFF”, because of the deflected ions.
• Connect the ion lens electrode (SHV-feedthrough Lens) to Flux In at the EVC 300i
• Start evaporation; all ions are suppressed (no sample current measurable).
Attention: The ion flux may differ from the value measured with
“SUPR OFF”, because of the deflected ions.
April 08
34 EFM-Manual
5. Maintenance
In all cases the power supply must be switched off and disconnected from the evaporator.
The evaporator is removed from the chamber.
5.1. Cleaning
When evaporating only small amounts of material (e.g. from monolayer production), no
cleaning of the cooling shroud or shutter is required on changing the evaporant. The cool-
ing facility keeps contamination negligible.
There is very little maintenance necessary on the EFM evaporator. However it may be
occasionally necessary to change a broken filament or inspect and replace a ceramic
insulator which has become coated with conducting material. Also, after prolonged use all
inner parts including the flux monitor at the front of the oven may become covered with
material, such that mechanical cleaning becomes necessary (small metal brush or sand-
paper recommended). After evaporation of large amounts of material the inner region of
the copper cooling shroud should be cleaned after removal of the top flange (procedure
see 5.2) using a small brush or similar device. Especially, thin sheets of loose evaporant
must be carefully removed from the inner region.
EFM 2/3/3s/4/3i/3T
The ceramic insulators of the slide bearing need inspection (see fig. 3.1) if a resistance of
<1MΩ is measured between the HV-feedthrough and ground.
Every filament is isolated from ground potential by two small ceramics which may also be
contaminated by the evaporant. This can gradually lead to leakage currents. If no suffi-
cient emission current can be reached, the filament need to be replaced.
Version 3.9
5. Maintenance 35
April 08
36 EFM-Manual
1. Loosen the six collets which connect the current leads to the ceramic feedthroughs of
the filament holders at the front of the cooling body (allen wrench 0.8 mm).
2. Remove the shutter bearing at the top of the flux-monitor (M2 screws).
3. Unplug the flux monitor cables at the feedthrough.
4. Loosen the M3 bolts of the front copper flange on the cooling body. Note that the front
copper flange can be tight after extended use. It may be necessary to use a small
screw driver or a razor blade to loosen it.
5. Move the shutter and the filament current leads with their holding plates some mm
away from the front flange. Take care not to brake the ceramics with the filament cur-
rent leads.
6. Remove the two screws on the lower side of the copper cooling shroud. Lift the cop-
per flange fluxmonitor assembly with the flux monitor cabeling. The filament plates
are now assessable.
7. Remove the fixing screw of the filament plate, which needs inspection. Take care not
to brake a still intact filament.
8. This applies only for the case of do-it-yourself repair of the filament:
Spot weld a spiral filament (thoriated tungsten of 0.125 mm thickness, see above,
length = ca. 45 mm) to the holding bars of the filament holder. The tungsten wire must
be bent into a spiral of 8-10 mm diameter with a pitch of about 4 mm. Keep to the
drawing of fig. 5.2. The insulated filament posts are made of molybdenum. For spot-
welding a piece of tantalum ribbon (thickness about 0.1 mm) should be positioned be-
tween the filament wire and the post (alternatively use the old cleaned Ta-ribbon) .
9. Check that all filaments make no short to the main cooling body. To do this, set the
filaments to their original positions on the cooling body and make a visual inspection
(use appropriate illumination) that the filament wires do not touch the cooling shroud
from inside. Check the resistance between filament and ground.
10. Cautiously replace the new or repaired filaments in their mounts on the copper flange.
In doing so, touching the filament must be avoided because of the danger of weaken-
ing the spot weld connections. Refit the fixing screw of the filament plate. Carefully
replace the copper flange onto the cooling body.
Version 3.9
5. Maintenance 37
11. Fix the copper flange the cable holding plates and the shutter bearing plate by means
of the M3 screws. Fix the current leads by means of the collets. Hold the collets while
fastening the M2 screws so as not to break the fragile ceramics of the filament holder.
A new filament should be "tuned" in vacuum by gradually increasing the current from 1 A
upwards (up to its operating current) over a period of about 10 min.
Before May 2004, the filaments have one insulated filament post. The second filament
lead is directly connected to ground. Evaporators delivered later have both filament posts
insulated (see chapter 2.3).
April 08
38 EFM-Manual
EFM 3T
After prolonged use of the evaporator the insulating ceramic tube between the molybde-
num barrel connector and the cooling shroud can be coated (slide bearing ceramics in
Fig. 3.3). To remove this ceramics carefully loosen the headless M2 screw in the cooling
shroud and remove the ceramics. The ceramics can be cleaned with acid or by heating it.
Alternatively a replacement ceramics can be obtained by the manufacturer.
Version 3.9
6. Fault diagnostics 39
6. Fault diagnostics
No filament current:
• Cables disconnected
• Filament broken. Filament check is made in the startup-procedure of the EVC-power
supplies
No high voltage
• There may be a short circuit of evaporant rod to ground or to filament. Check with
ohmmeter at high voltage socket. If there is a short check concentricity of evaporant
and its correct length according to sec. 3.1 and 3.2 (maybe it has been moved too far
forward). Before switching on again disconnect the cable from EFM and rise the high
voltage to 1 kV to see whether the electronics alone is all right; refer to the corre-
sponding manuals.
April 08
40 EFM-Manual
Version 3.9
Appendix 41
Appendix
21 p ⋅ r2
Deposition rate [atoms/(cm2 s)] ≈ 8 ⋅ 10 .
L2 M ⋅ T
As this formula does not contain a sticking coefficient it is an arrival rate.
r: radius of evaporant bar or rod (typically 1 mm)
L: distance from tip of evaporant to substrate (typically 110-150mm);
That corresponds to a distance of 10 - 50mm from the end of EFM to the sample.
M: molecular weight of evaporant (g)
T: temperature of evaporant (K)
p: vapour pressure (mbar) - which is a function of temperature for a given material.
Consult appropriate tables.
The leading term in this formula is the partial presser of the material, because it can cover
several orders of magnitude within the possible temperature range. Rod evaporation
should be possible if a high enough pressure can be reached at the melting point or at
lower temperatures. If the evaporant has to be molten to reach the deposition rates
needed a crucible should be used.
The choice of evaporation rate depends upon the experimental conditions, such as back-
ground pressure, and experimental requirements of purity and duration of the experiment.
In general evaporation from bars is preferred, as heating of a crucible will deliberate gas
from it. Also the heat loss due to the increased surface is higher. For the selection of cru-
cible materials the table from the Balzers AG is very helpful (see the chapter on literature)
The basic equation from which the above has been derived, can be found in:
L. Holland, W. Steckelmacher, J. Yarwood: Vacuum Manual, London 1974
April 08
42 EFM-Manual
Fig. A1 illustrates this formula for parameters typical for EFM as discussed in the exam-
ples below. These are theoretical results giving a good starting point for planning an ex-
periment.
Example 2: Platinum
1) The evaporation rate (or better say arrival rate at the sample) R at the melting point of
Pt (1770°C) is quite small. The calculation gives 0.1 monolayers per minute. The experi-
ment shows that the actual rate is a little bit higher: up to 0.5 ML/minute.
If in the actual experiment this small evaporation rate is sufficient, we strongly recom-
mend evaporation from a bar as this is the most clean evaporation method.
In case a higher evaporation rate is needed the following two methods are applicable:
2) A piece of Pt-wire (some centimetres in length and some tenth of a millimetre diame-
1
ter) is wound around the end of a straight carbon rod of about 1 to 2 mm diameter, and 4
cm length. On heating the rod by electron bombardment, the Pt will melt and form a little
droplet at the end of the bar. As it is only a small amount of material it will not drop off.
Because of the surface tension it can be heated above the melting temperature of Pt. To
be sure the molten Pt accumulates at the tip of the bar the EFM should point downward.
3) If it is necessary to have high evaporation rates and the EFM should point upwards, a
carbon crucible should be selected.
1
Any additional material that is heated during the evaporation, will degas itself and degrade the cleanliness of
evaporation. This is especially the case with carbon. So it is best to avoid this situation. If it cannot be avoided
take the minimum amount of carbon that is possible, so a rod is preferred compared to a graphite crucible.
Version 3.9
Appendix 43
April 08
44 EFM-Manual
Material overview
3
Density g/cm
ration possi-
Rod evapo-
suitability*
Crucible
Material
-8 -6 -4
e-beam
Symbol
ble **
Wets crucibles. Fill crucible to max. 10% to
Aluminum Al 660 2.70 677 821 1010 Ex PBN N
avoid creeping
< 10E-6
Barium Ba 725 3.51 545 627 735 F Metals Wets without alloying, reacts with ceramics.
torr
Bismuth Bi 271 9.80 330 410 520 Ex Al2O3 N Toxic vapor. Resistivity high.
Boron Car-
B4 C 2350 2.52 2500 2580 2650 Ex C N
bide
Carbon
C ~3652 1.8-2.1 1657 1867 2137 Ex - Y E-beam preferred. Poor film adhesion.
(Graphite)
Al2O3,
Cerium Ce 798 ~6.70 970 1150 1380 G N
BeO, W
Chromium Cr 1857 7.20 837 977 1157 G W Y Films very adherent. High rates possible.
< 10E-2
Cobalt Co 1495 8.9 850 990 1200 Ex BeO Alloys with refractory metals.
torr
< 10E-2
Europium Eu 822 5.24 280 360 480 F Al2O3 Low tantalum solubility.
torr
< 10E-2
Gadolinium Gd 1313 7.90 760 900 1175 Ex Mo, W High tantalum solubility.
torr
Gallium Ga 30 5.90 619 742 907 G PBN N May condense at crucible exit.
Germanium Ge 937 5.35 812 957 1167 Ex W, C, < 10E-6 Excellent films from E-beam guns.
Version 3.9
Appendix 45
Ta torr
Gold PBN, < 10E-6 reacts with W in e-beam guns. Films soft, not
Au 1064 19.32 807 947 1132 Ex
Al2O3 torr very adherent.
< 10E-5
Hafnium Hf 2227 13.31 2160 2250 ---- G C
torr
Ni/Cr/
Inconel 1425 8.5 - - - G Y Low rate required for smooth films
Fe
Lanthanum La 921 6.15 990 1212 1388 Ex W, Ta N Films will burn in air if scraped.
Molybde-
Mo 2610 10.2 1592 1822 2117 Ex - Y Films smooth, hard. Careful degas required.
num
Molybde-
MoO3 795 4.69 - - ~900 - Mo, Pt N Slight oxygen loss.
num Oxide
< 10E-5
Neodymium Nd 1021 7.01 731 871 1062 Ex Ta Low tantalum solubility.
torr
Nichrome IV Ni/Cr 1395 8.50 847 987 1217 Ex - Y Alloys with refractory metals.
< 10E-4
Permalloy Ni/Fe 1395 8.7 947 1047 1307 G W Film low in nickel.
torr
< 10E-4
Platinum Pt 1772 21.45 1292 1492 1747 Ex C Alloys with metals. Films soft, poor adhesion.
torr
Rhenium Re 3180 20.53 1928 2207 2571 P C N Fine wire will self-evaporate.
April 08
46 EFM-Manual
Mo, Ta,
Selenium Se 217 4,2 89 125 170 G Y
Al2O3
W, Mo, < 10E-4 Rod evaporation with W-wire wound around the
Silver Ag 962 10.5 847 958 1105 Ex
Ta torr silver rod.
W,
Thorium Th 1875 11.7 1430 1660 1925 Ex Y Toxic, radioactive.
Ta,Mo
Titanium Ti 1660 4.5 1067 1235 1453 Ex - Y Alloys with refractory metals; outgas gently.
Tungsten W 3410 19.35 2117 2407 2757 G - Y Forms volatile oxides. Films hard and adherent.
< 10E-6
Zirconium Zr 1852 6.49 1477 1702 1987 Ex C Alloys with tungsten. Films oxidize readily.
torr
** Y = rod always possible, N = not recommended due to melting point or e-beam suitability. Otherwise recommeded pres-
sure limit is given.
NOTE: This information has been collected to give customers a brief overview
about material deposition techniques. The provider of this information is
not responsible for the performance of any evaporation process which is
developed based on the informations provided in this table.
Some materials in this table are hazardous. Determine toxicity, flamma-
bility radioactivity or any other risks for health, environment or system
components before using.
Version 3.9
Appendix 47
For some materials experimental hints for evaporation with the EFM evaporators are addi-
tionally given below. The provider of this information is not responsible for the perform-
ance of the described evaporation process in this table.
Pb, Cu, Ag, Au: W or Mo crucible, Cu gives max values exceeding
10 ML/ sec., Cu wets Mo.
April 08
48 EFM-Manual
B. List of Thermovoltage
Nickelchromium (NiCr) / coppernickel (CuNi), type E (steps by 10)
Reference temperature 0°C
°C µV °C µV °C µV
Version 3.9
Appendix 49
f) Hall Effect
see W.D. King et al, J. Vac. Sci. Technol. B9 (1991) 2771
g) Ellipsometry
Meyer, F.: Ellipsometric Study of Adsorption Complexes on Silicon
Surf.Sci. 27 (1971) 107
Habraken, F. et.al.: Ellipsometry of Clean Surfaces, Submonolayers and Mono-
layer Films, Surf.Sci. 96 (1980) 482
April 08
50 EFM-Manual
D. Literature
General literature
[7] J. Kirschner, H. Engelhard and D. Hartung, Rev. Sci. Intrum., Vol. 73, No. 11,
Nov. 2002.
(Description of EFM 3i)
and references therein.
Version 3.9
Appendix 51
E. Options
E 1. Crucibles O.D.
I.D.
Dimensions of crucibles
* can be used with EFM 3T
and EFM 3i
L
I.D./mm O.D./mm L / mm capacity Tmax (°C) order
3 -4
/ mm @10 Torr code
vapor
pressure
April 08
52 EFM-Manual
Notes:
PBN-crucibles: For temperatures above 1300° the heating of the PBN results in a
raising N2 background pressure
Version 3.9
Appendix 53
E 2. Shutter Motor
The shutter motor is either mounted at the factory or can easily be refitted by the cus-
tomer. It serves to operate the shutter for all EFM evaporators including EFM 3T.
The shutter electronics is integrated in the evaporator power supply EVC 300, EVC 300s
or EVC300i, which can be driven from RS232 interface of a computer. See related EVC
manual for details.
Order Code: EFM SM
E 3. Port Aligner
92,2
9,4
ø3
ø70
51,7
46±2
April 08
54 EFM-Manual
Different barrel connectors are availbel to support the use of crucibles and rods with dif-
ferent diameter. The evaporators EFM2/3/3s/4, EFM 3i and EFM 3T use different models,
please refer to the table:
To facilitate the connection and de-connection of the water hose for e.g. baking the sys-
tem.
Order Code: EFM QWC
Version 3.9
Service at OMICRON 55
Service at OMICRON
http://www.omicron.de/contact/representatives.html
or via e-mail reply service under
contact.info@omicron.de
April 08
56 EFM-Manual
Problem:
Date: Signature:
Version 3.9
Decontamination Declaration 57
Decontamination Declaration
April 08
58 EFM-Manual
This declaration may only be completed and signed by authorised and qualified staff.
1. Description of components
3. Equipment condition
Has the equipment ever come into contact with the following (e.g. gases, liquids, evaporation products,
sputtering products…)
For all harmful substances, gases and dangerous by-products which have come into contact with the
vacuum equipment/components please list the following information on (a) separate sheet(s): trade
name, product name, manufacturer, chemical name and symbol, danger class, precautions associated with
substance, first aid measures in the event of an accident.
The manufacturer reserves the right to refuse any contaminated equipment / component without writ-
ten evidence that such equipment/component has been decontaminated in the prescribed manner.
4. Decontamination Procedure
Please list all harmful substances, gases and by-products which have come into contact with the vacuum
equipment/components together with the decontamination method used.
Version 3.9