Gatan Solarus 950 Guide

Gatan, Inc.
5794 W. Las Positas Blvd.
Pleasanton, CA 94588 Tel. [phone] Fax. [phone]
Solarus 950
Gatan Advanced Plasma System
Owner’s Manual and User’s Guide
Part Number: 950.82001
July 2011
Revision 5

ii Solarus 950 Owner’s Manual and User’s Guide

APS Solarus 950 Owner’s Manual iii
Preface
About this Guide
This provides information on operation and basic maintenance of the Solarus
950 Advanced Plasma system.
The following typographical conventions are used for special comments:
NOTE:Recommendations for getting the best performance from the
equipment.
Disclaimer
Gatan, Inc., makes no express or implied representations or warranties with
respect to the contents or use of this manual, and specifically disclaims any
implied warranties of merchantability or fitness for a particular purpose. Gatan,
Inc., further reserves the right to revise this manual and to make changes to its
contents at any time, without obligation to notify any person or entity of such
revisions or changes.
Copyright and Trademarks
© 2007 Gatan, Inc. The Gatan logo is a registered trademark of Gatan, Inc.
The product names AutoFilter, BioScan, Clipring, DigiPEELS, DigiScan, Digi-
talMicrograph, DigitalMontage, Duo Mill, DuoPost, Gatan LowDose, GIF,
Hexlok, Hexring, HotHinge, MSC, PECS, PIPS, Toggle Tilt, and Whisperlok
are trademarks belonging to Gatan, Inc.
All rights reserved. No part of this publication may be reproduced, stored in a
retrieval system, or transmitted, in any form or by any means, electronic,
mechanical, photocopying, recording, or otherwise, without the prior written
permission of Gatan, Ltd.
The text and graphics are for the purpose of illustration and reference only. The
specifications on which they are based are subject to change without notice.
CAUTION:Precautionary notes and advice to avoid personal injury or damage to
the equipment.
!

iv APS Solarus 950 Owner’s Manual
Returns
If there is a need to return equipment to the factory, please call Gatan to obtain a
Returned Merchandise Authorization Number (RMA #). This RMA number must
appear on your shipping document, to help in tracking and to ensure that proper
actions will be taken to repair or replace your equipment.
Support
Gatan, Inc. provides free technical support via phone, fax, and email. Contact the
facility nearest you, or send email to [email protected].
USA, Canada &
Latin America Corporate Headquarters
Western USA Sales
Central USA & Latin America Sales
5794 W. Las Positas Blvd.
Pleasanton, CA 94588
Tel: [phone]
Fax: [phone]
Contact: [email protected]
Gatan, Inc.
Eastern USA Sales
780 Commonwealth Drive
Warrendale, PA 15086
Tel: [phone]
Fax: [phone]
Contact: [email protected]
Asia & Pacific Rim Nippon Gatan
3F Sakurai building
2-8-19 Fukagawa, Koto-ku
Tokyo 135-0033, Japan
Tel: [phone]
Fax: [phone]
Contact: [email protected]
Gatan Singapore
10 Eunos Road 8
#12-06
Singapore Post Centre
Singapore 408600
Tel: [phone]
Fax: [phone]
Contact: [e-mail]

APS Solarus 950 Owner’s Manual v
Europe Gatan GmbH, München, Germany
Ingolstadterstr. 12
D-80807 München
Germany
Tel: [phone]
Fax: [phone]
Contact: [email protected]
Gatan UK
25 Nuffield Way
Abingdon
OX14 1RL
UK
Tel: [phone]
Fax: [phone]
Contact: [email protected]
Gatan France
Division de ROPER Scientific SAS
8, rue du Forez
ZI petite montagne Sud - CE 1702
91017 EVRY Cedex
Tel: + 33 1 69 11 03 69
Fax: + 33 1 64 97 19 67
Contact: [email protected]

vi APS Solarus 950 Owner’s Manual

Solarus 950 Owner’s Manual and User’s Guide vii
Table of Contents
About this Guide. . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . iii
Disclaimer. . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . iii
Copyright and Trademarks . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . iii
Returns . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . iv
Support . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . iv
Overview 1
Features 3
Plasma Recipes. . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . .3
Hardware. . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . .4
Electronics . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . .4
Touch Screen User Interface. . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . .5
Description and Specifications 6
Physical Specifications. . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . .7
Gas Requirements. . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . .8
Safety and Serviceability 9
Cautionary Notes . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . .9
Servicing. . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . .9
Installation Recommendations for Gatan Customers—Flammable and
Oxidizing Gases . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . .10
Installation and Setup 12
Unpacking and Inspection . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . .12
Connections . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . .12
Cleaning Configurations. . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . .14
Configuring Gas 3. . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . .15
Purging the Gas Lines. . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . .16
Connecting Exhaust Lines . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . .18
Connecting Vent Gas Line . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . .18
Testing With Air as a Plasma Gas . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . .19
Loading Samples in the Solarus 950 22
Loading TEM Samples. . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . .22
Loading SEM Samples . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . .22

viii Solarus 950 Owner’s Manual and User’s Guide
Removing the Ion Shield 24
Operating the Gatan Advanced Plasma System 25
Theory of Operation . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 25
Operating Instructions. . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 26
Creating Custom Recipes . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 34
Maintenance 38
Maintenance Report . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 46
Troubleshooting 47
Spares and Consumables 48
Battery Considerations . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 48

Solarus 950 Owner’s Manual and User’s Guide ix
List of Figures
Figure 1 Gatan Advanced Plasma System, model Model 950. . . . . . . . . . . . . . . .2
Figure 2 Gatan Advanced Plasma System, front-accessible components . . . . . . . . . .6
Figure 3 Gatan Advanced Plasma System, rear panel . . . . . . . . . . . . . . . . . . . .7
Figure 4 Solarus 950 rear panel gas connection detail. . . . . . . . . . . . . . . . . . . 12
Figure 5 Gas line to filter connection . . . . . . . . . . . . . . . . . . . . . . . . . . . 13
Figure 6 Two-tank cleaning configuration. . . . . . . . . . . . . . . . . . . . . . . . . 14
Figure 7 Three-tank cleaning configuration . . . . . . . . . . . . . . . . . . . . . . . . 15
Figure 8 Two-tank purging configuration . . . . . . . . . . . . . . . . . . . . . . . . . 17
Figure 9 Air testing configuration . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 20
Figure 10 Loading TEM holder, holder adapter, and plug . . . . . . . . . . . . . . . . . 22
Figure 11 TEM holder and adapter in place. . . . . . . . . . . . . . . . . . . . . . . . . 22
Figure 12 Top-loading SEM chamber, side view . . . . . . . . . . . . . . . . . . . . . . 23
Figure 13 Sample loaded in SEM chamber . . . . . . . . . . . . . . . . . . . . . . . . . 23
Figure 14 TEM holder-adapter with ion shield removed . . . . . . . . . . . . . . . . . . 24
Figure 15 System in idle state. . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 27
Figure 16 System initiating vacuum state. . . . . . . . . . . . . . . . . . . . . . . . . . 29
Figure 17 System introducing gases. . . . . . . . . . . . . . . . . . . . . . . . . . . . . 30
Figure 18 Applying RF power to the unit . . . . . . . . . . . . . . . . . . . . . . . . . . 30
Figure 19 Cleaning in process. . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 31
Figure 20 Plasma cleaning complete . . . . . . . . . . . . . . . . . . . . . . . . . . . . 32
Figure 21 Venting the chamber . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 33
Figure 22 System ready for next sample . . . . . . . . . . . . . . . . . . . . . . . . . . 33
Figure 23 Recipe options . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 36
Figure 24 Access to Pirani gauge calibration button . . . . . . . . . . . . . . . . . . . . 45
Figure 25 Example maintenance report . . . . . . . . . . . . . . . . . . . . . . . . . . . 46
Figure 26 Battery Location . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 49

xSolarus 950 Owner’s Manual and User’s Guide

Solarus 950 Owner’s Manual and User’s Guide 1
Gatan Advanced Plasma System
Owner’s Manual and User’s Guide
Overview
Optimal imaging and microanalysis in electron microscopy requires a clean, well-
prepared specimen. This is especially important for FEG TEM, because specimen
contamination rates tend to increase as probe size decreases and beam current
density increases. The high performance now possible with the FESEM under-
scores the need for eliminating hydrocarbon contamination, especially for those
applications involving low voltage, high-resolution operation.
An RF-generated gas plasma cleaning process, originating within the semi-
conductor industry for wafer cleaning, has been known and available for some
time. A version of this technique was adapted for EM applications by Nestor
Zaluzek at Argonne National Laboratory and University of Chicago (US Patent
5,510,624, dated April 23, 1996).
The Solarus Advanced Plasma System expands this process to a new level.
Solarus is a low power hydrogen and oxygen radical generator producing glow-
discharge plasma within the generator housing. The hydrogen and oxygen radicals
disperse from the generator by convection, passing over and around the specimen/
specimen holder tip to clean hydrocarbons from the surfaces. The process pro-
duces H2O, CO2, and CO gases that are pumped away by the vacuum system.
Solarus incorporates a multi-stage diaphragm pump backing a turbomolecular
drag pump to assure fast, reliable pumping. The pump package enables pump and
vent cycles of less than two minutes. With cleaning times of 1-2 minutes, the full
Solarus 950 cleaning cycle takes less than four minutes.

2Solarus 950 Owner’s Manual and User’s Guide
ƒigure 1 Gatan Advanced Plasma System, model Model 950

Solarus 950 Owner’s Manual and User’s Guide 3
Features
The Solarus 950 is unique in automatically managing all critical plasma parame-
ters, offering a reliable one-touch cleaning solution. With this system, every user
can obtain consistent, high quality results.
The Gatan Advanced Plasma System consists of four main elements:
Oplasma recipes
Ohardware
Oelectronics
Osoftware
These elements are integrated into a highly flexible system that allows a great deal
of control over the sample cleaning process.
Plasma Recipes
Gatan provides cleaning recipes developed to maximize contamination removal
rates while minimizing damage to even the thinnest TEM samples. These recipes
have been tuned for efficiency using a mass spectrometer and crystal and thick-
ness monitors, tuned for minimal sputtering and sample damage using Langmuir
probes, and exhaustively verified with TEM and SEM samples in a wide variety
of conditions.
The unique H2/O2 recipe prevents or reduces buildup of contamination after about
one minute of cleaning. Even the worst burned-on contamination takes less than
ten minutes to clean. Holey carbon films have been cleaned in this recipe for more
than nine minutes without damage. Alternate Ar/O2 (Ar 75% - O2 25%) recipes
can also be selected.
The two primary gas chemistries used are H2/O2 and Ar/O2.
H2/O2
Gatan has found this chemistry to provide superior cleaning rates, less sputtering
damage, and significantly less sample heating than Ar/O2over a wide range of
samples.
Ar/O2(option)
This is the traditionally used process gas combination in electron microscopy.
Gatan has not yet found a processing advantage to Ar/O2over H2/O2, but some
sites may have restrictions on the use of pure H2or O2. An optional third mass
flow controller and a supply of Ar 75%/O 25% is required to use this recipe.
The use of this recipe requires optional hardware.

4Solarus 950 Owner’s Manual and User’s Guide
Air
Air can be used as a substitute for Ar/O2in a pinch. Some concerns exist about
forming C-N compounds that won’t volatilize and remain on the sample.
NOTE:Any of the cleaning chemistries can be used to treat carbon films that
have become hydrophobic.
Cl2/Br2
Other Gases
Please contact Gatan for compatibility of other gases.
Hardware
The Gatan Advanced Plasma System hardware offers fast cycle times and a broad
range of sample cleaning options. Both TEM and SEM samples can be accommo-
dated.
TEM Samples
Two front ports on the Solarus 950 accept TEM adapters compatible with all side-
entry TEM or SEM specimen holders. For slightly faster cleaning, use the left
port.
SEM Samples
A top-loading chamber accepts multiple SEM stubs and large irregular-shaped
samples.
Electronics
The electronics subsystem offers a powerful RF power supply, an auto-tuning RF
match network, and mass flow controllers.
RF Source
The Solarus 950 contains a 65 Watt RF power supply (13.56 MHz) with an auto-
tuning network to assure effective plasma coupling to the generator and chamber.
The RF supply is CE certified to comply with FCC guidelines.
The auto-tuning network is critical for achieving consistent results. It measures
the amplitude and phase of the forward and reflected power and automatically
minimizes reflected power. This ensures that the power delivered to the plasma is
CAUTION:Donot useCl2/Br2withthealuminum GatanAdvancedPlasmaSystem
chamber!
!

Solarus 950 Owner’s Manual and User’s Guide 5
consistent, even as the impedance varies due to aging, odd sized samples, or
changes in gas pressure or species.
Vacuum/Gas Pumping
A two-stage variable-speed diaphragm pump (electronic speed control) backs a 70
liters/second turbo molecular drag pump.
Chamber
The chamber is 3.5” in diameter x 2.0” deep, and includes multiple entry ports. A
front viewing port displays plasma when activated. An inline electromagnetic
valve isolates the vacuum pump from the chamber, resulting in less than one
minute pump down and less than a ten-second vent cycle.
Mass Flow Controllers
Mass flow controllers accurately gauge gas levels to achieve superior and repeat-
able cleaning results.
Touch Screen User Interface
A touch screen interface to the Solarus 950 software offers one touch operation
through user-programmable recipes, providing greater flexibility and repeatability
than competitive products.
Simple Four-Step Cleaning
1. Load a sample, either from the front (TEM holders) or top (stand-alone
TEM/SEM samples)
2. Select a recipe for TEM, STEM, SEM or carbon film cleaning using either
H2/O2or Ar/O2plasma cleaning.
3. Touch START to begin the cleaning cycle.
4. Touch VENT to vent the chamber and permit sample removal.

6Solarus 950 Owner’s Manual and User’s Guide
Description and Specifications
The Solarus 950 consists of a single self-contained unit as shown in the following
photos.
ƒigure 2 Gatan Advanced Plasma System, front-accessible components
The front of the unit contains a touch screen for executing all actions, two TEM
holder ports, and a viewing port. The door to the top-loading specimen chamber is
on the top of the unit, above the TEM holder ports.
All gas and venting connections are made at the rear of the unit. The rear panel
also contains the on/off power switch, connectors for power cable, USB ports and
network cable, and a storage area for the DP locking screw mentioned in the
unpacking instructions.

Solarus 950 Owner’s Manual and User’s Guide 7
ƒigure 3 Gatan Advanced Plasma System, rear panel
Physical Specifications
NOTE:Although the instrument is a compact bench-top system, it is relatively
heavy and should not be lifted by a single individual.
SPECIFICATION VALUE
Weight 145 lbs/65 kg (see Note)
Dimensions The system requires a stable bench with a surface area of:
O39 inches (1m) in length
O24 inches (62cm) in depth
O18 inches (46cm) in height
Clearance Allow clearance on both sides for ventilation, and to the rear
for gas line connections and ventilation.
Do not block the fan vents.
Power 100-240 VAC, 50/60 Hz, 1000 Watts
A molded power cord is supplied to fit the local
standard power socket. Be sure to use a properly grounded AC
outlet.
Maximum Ambient
Temperature 35 degrees Celsius

8Solarus 950 Owner’s Manual and User’s Guide
Gas Requirements
NOTE:All gas connections are compression fittings (1/8 inch OD Tube),
4.5 grade is 99.995% pure (50 PPB).
Gas Used During Cleaning (Standard Gatan Recipes)
NOTE:* sccm = standard cubic centimeters per minute
For example, a 2 cubic foot (~57 liter) lecture bottle of H2will last for ~147 hours
of continuous use. An 80 cubic foot (~2265 liter) bottle of O2will last for ~1373
hours of continuous use.
GAS PURITY PSI
O2Grade = 4.5 25 psi (1.7 bar)
H2Grade = 4.5 25 psi (1.7 bar)
Ar (option) Grade = 4.5 25 psi (1.7 bar)
GAS USAGE
H2/O2H2= 6.4 sccm*
O2= 27.5 sccm
Ar/O2Ar = 35.0 sccm
O2= 11.5 sccm

Solarus 950 Owner’s Manual and User’s Guide 9
Safety and Serviceability
Cautionary Notes
Servicing
The turbo-molecular drag pump and diaphragm pumps require periodic mainte-
nance. Please see the individual operator manuals of these instruments (included
in the shipping crate) for instructions. See the maintenance section in this manual
for instructions to remove these pumps from the instrument.
CAUTION:UnplugtheACmainscablebeforeopening the system, toavoid electric
shock. Dangerous high voltages and currents may be present inside the case
during operation. Do not reach your hands inside the system while the power is on
or if the AC mains cable is plugged in.
CAUTION:High pressure cylinders can be dangerous when not properly secured.
Be sure all cylinders are secured according to applicable safety codes..
CAUTION:TheRFpowersupplycangenerate85Wattsof power,whichcancause
burns if the live conductors are touched. Do not operate the unit unless the RF
cables arepluggedin properly. Do not defeat the safety mechanisms and touch the
RF antenna when the system is attempting to generate a plasma.
CAUTION:Hydrogen and Oxygen are combustible gasses. During normal
operation these gasses are fully combusted in the plasma and are not a danger. If
the gas supply connections or lines leak into an enclosed space, it is possible for
a dangerous concentration to accumulate. It is important to install and maintain
these connections properly in order to prevent leaks.
!
!
!
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10 Solarus 950 Owner’s Manual and User’s Guide
Installation Recommendations for Gatan Customers—Flammable and
Oxidizing Gases
Hydrogen Guidance
OEnclosure/Cabinet: Store a lecture bottle of hydrogen within a one hour fire
barrier such as a “semiconductor type” rated lecture bottle gas cabinet. Secure
the compressed gas cylinder inside cabinet.
OSeismic Bracing and Mechanical Integrity: Ensure that the enclosure is
seismically braced in accordance with applicable Building Codes and that the
distribution line is properly braced between the cabinet and the Solarus 950.
OGas Detection: Install listed and/or approved hydrogen gas monitoring for
the lecture bottle gas cabinet providing both local and remote alarm
annunciation.
ODistribution System: Piping, tubing, valves, and fitting shall be compatible
with flammable gases and be of adequate strength and durability to withstand
the pressure expected.
OGrounding and Bonding: Provide for appropriate grounding and bonding to
minimize the potential for static electricity buildup.
OMaintenance and Inspections: Place safety critical equipment such as flam-
mable gas detection and grounding on a periodic calibration and test schedule.
Oxygen Guidance
OCompressed gas cylinder: Secure oxygen compressed gas cylinders to a
fixed object with one or more restraints stored upright with valve end up. Pro-
tect compressed gas cylinder valves from physical damage, by using valve
caps and ensure compressed gas cylinder caps are in place when not in use
ODistribution System: Ensure oxygen piping is free from oil residues and for-
eign material. Oil-free and noncombustible materials must be used for leak
testing oxygen lines.
OSegregation: Store oxygen compressed gas cylinder separately from incom-
patible materials, such as hydrogen gas. Note: If hydrogen gas cylinder is
located within a 1-hour rated fire barrier such as a semiconductor type gas
cabinet, then adequate segregation is provided. If no enclosure is used for
hydrogen, then the oxygen compressed gas cylinder shall be located at least
20 feet away.
Oxygen Guidance Applicable to both Hydrogen and Oxygen
OLeak Testing: Conduct pressure leak testing of delivery piping and associated
fittings prior to introducing hydrogen to the Solarus 950.