SEM Techniques Using the Gatan Precision Etching and Coating System (PECS )
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1 SEM Techniques Using the Gatan Precision Etching and Coating System (PECS )
2 The Tool The Technique The Total Solution PECS Precision Etching and Coating System
3 Not just another new tool But a NEW Sample Preparation Technique A Clean Green Technique: ION BEAM ETCHING The perfect match for a FESEM or Optical Microscope Eliminate: Chemical Mess Chemical Handling Chemical Spills Chemical Hazards Chemical Disposal
4 Cleaning a b 20kx SEM images of tungsten plugs, sample was first mechanically polished. Image A shows leftover debris and contamination from polishing process (arrow). Image B is after Etch, sample is cleaned and reveals a variety of micro structural features. 4
5 Coating High-resolution cross-section through different coating layers of C and Cr sputtered on Si substrate. 5
6 100 nm 200kx PECS Coating Sub-nanometer grain deposition of Chromium (Cr), thin amorphous Cr coatings can be deposited without masking delicate specimen features. 6
7 100 nm 200kx Magnetron Coating Chromium deposition by comparison is not sub-nanometer or amorphous. 7
8 Etching Before etch and after etch SEM images of bonded copper structures (Cu I. & Cu II). After etching shows grain size and grain morphology of each Cu structure is entirely different. Bonded interface area is also visible after etching (see arrows). 8
9 30kx SEM image of tungsten plugs and transistors, starting sample as cleaved. Sample etched and coated. Parameter: Etch gas I 2 Coating Pt 6 / 250 / 2 / 60 / Fix / Rotating 6 / 250 / 1 / 0-30 / Rock / Rotating 7.5 / 200 / 1.5 / 0-30 / Rock / Rotating 6 / 200 / 0.3 / 0-30 / Rock / Rotating 9
10 23kx SEM image of tungsten plugs and transistors, starting sample as cleaved. Sample etched and coated. Parameter: Etch gas I 2 Etch gas I 2 Coating Pt 5 / 250 / 1 / 60 / Fix / Rotating 5 / 250 / 1.5 / 0-45 / Rock / Rotating 5 / 250 / 1 / 50 / Fix / Rotating 5 / 250 / 1.5 / 0-45 / Rock / Rotating 6 / 200 / 0.3 / 0-30 / Rock / Rotating 10
11 22kx SEM image of tungsten plugs and transistors, starting sample as cleaved. Sample etched and coated. Parameter: Etch gas I 2 Etch gas I 2 Coating Pt 5 / 250 / 1 / 60 / Fix / Rotating 5 / 250 / 1.5 / 0-45 / Rock / Rotating 5 / 250 / 1 / 50 / Fix / Rotating 5 / 250 / 1.5 / 0-45 / Rock / Rotating 6 / 200 / 0.3 / 0-30 / Rock / Rotating 11
12 Metallographic High-Purity Titanium Structure, after Etching, Micrograph with POL Filters. 500x Parameters: 6 / 400 / 12 / 60º / Rotating 12
13 500x High-Purity Titanium Structure, after Etching, DIC Micrograph. Parameters: 6 / 400 / 8 / Vertical / Rotating 13
14 200x High-purity-Cu deformed and annealed with tin coating (< 2um) Grain Boundaries and Twins of high-purity-cu developed after etching, DIC Micrograph. Parameter: 6 / 370 / 2.4 / Vertical / Rotating 14
15 500x High-purity-Cu deformed and annealed with tin coating (< 2um) Grain Boundaries and Twins of high-purity-cu developed after etching, DIC Micrograph, Section of previous Figure. Parameter: 6 / 370 / 2.4 / Vertical / Rotating 15
16 500x Structure development for Machine Brass CuZn39Pb3, after etching, DIC Micrograph, Lead Droplets Retained, in part Twinning visible in Lead Droplets. Parameter: 6 / 400 / 0.5 / 65 / Rotating plus 6 / 400 / 1.2 / Vertical / Rotating 16
17 Structure of High-Purity-Aluminum, after etching, POL Micrograph (rough to grainy grain surfaces appear in color). 50x Parameter: 6 / 400 / 12 / 53 / Rotating plus 6 / 400 / 24 / 45 / Rotating 17
18 Section of previous figure, after etching, DIC Micrograph. 200x 18
19 1000x Structure of Al Casting AlloyAlMg4.5Mn after Etching Micrograph with DIC, Grain Boundaries and Intermetallic Phases Etched. Parameter: 6 / 400 / 10 / 65 / Rotating 6 / 400 / 3.4 / Vertical / Rotating 6 / 400 / 12 / 55 / Rotating 19
20 50x Superconductor CuSn+NbTi+Ta Covered with Cu Coating, after Etching, Overview Micrograph with DIC. Parameter: 6 / 400 / 12 / 45 / Rotating 6 / 400 / 2.4 / Vertical / Rotating 6 / 400 / 2 / 10 / Rotating 20
21 100x Superconductor CuSn+NbTi+Ta Covered with Cu Coating, after Etching, Lower Area of previous Figure, CuSn Matrix with NbTi fibers, Micrograph with DIC. 21
22 500x Structure from the Edge of Permanent Magnet FeNdB(1%) with protective layers of Cu and Ni, after Etching, Micrograph with DIC, improved contrast of tarnished layer by means of additional O 2 etching Parameter: Etch gas O / 480 / 5 / 40 / Rotating 6.5 / 510 / 7 / 10 / Rotating 8 / 450 / 4 / Vertical / Rotating 22
23 EBSD EBSP Indexed Pattern Detected Bands Crystallographic Orientation 23
24 Cu sample, Image Quality = 193 Votes = 35, 15 kev SEM acceleration voltage. Parameters: 7.5 / 175 / 240 / 70 / Rotating Cu sample, Image Quality = 204 Votes = 35, 30 kev SEM acceleration voltage. Parameters: 7.5 / 175 / 240 / 70 / Rotating 24
25 Cu film, Image Quality = 228, 25 kev SEM acceleration voltage, spot size 4. Parameters: 2.5 / 60 / 115 / 50 / Rotating 25
26 Aluminum film, Image Quality = 114, 25 kev SEM acceleration voltage, spot size 4. Parameters: 2.5 / 60 / 30 / 50 / Rotating 26
27 DIE Package 300x Die Package, after Ar etch, overall view of Via hole, Delamination between solder resist and via hole inner wall. Metal grain structure not visible at all before etch. See following pages for indicated areas. Parameter: Etch gas I 2 7 / 200 / 3 / 50 / Fix / Rotating 5 / 200 / 5 / 0-30 / Rock / Rotating 5 / 200 / 5 / 0-30 / Rock / Rotating 6 / 200 / 0.5 / 0-30 / Rock / Rotating 27
28 1500x Die Package, after Ar etch, enlarged view from Right side of Via hole, Delamination between solder resist and via hole inner wall. No grain structure visible before etch. Parameter: Etch gas I 2 7 / 200 / 3 / 50 / Fix / Rotating 5 / 200 / 5 / 0-30 / Rock / Rotating 5 / 200 / 5 / 0-30 / Rock / Rotating 6 / 200 / 0.5 / 0-30 / Rock / Rotating 28
29 1500x Die Package, after Ar etch, enlarged view from Left side of Via hole, No delamination. No grain structure visible before etch. Parameter: Etch gas I 2 7 / 200 / 3 / 50 / Fix / Rotating 5 / 200 / 5 / 0-30 / Rock / Rotating 5 / 200 / 5 / 0-30 / Rock / Rotating 6 / 200 / 0.5 / 0-30 / Rock / Rotating 29
30 1000x Die Package, after Ar etch, Overall view of Die attach and Solder resist with delamination between Metal trace of Cu and 0.5um Ag. No grain structure visible before etch. See enlarged area on next page. Parameter: 7 / 200 / 3 / 50 / Fix / Rotating 5 / 200 / 5 / 0-30 / Rock / Rotating 6 / 200 / 0.5 / 0-30 / Rock / Rotating 30
31 Die Attach Solder Resist Die Package, after Ar etch, enlarged view from previous page, Die attach and Solder resist with delamination between Metal trace of Cu and 0.5um Ag. 5000x Parameter: 7 / 200 / 3 / 50 / Fix / Rotating 5 / 200 / 5 / 0-30 / Rock / Rotating 6 / 200 / 0.5 / 0-30 / Rock / Rotating 31
32 Die Package, after Ar etch, Overall view of Die attach, Solder resist and Metal trace of Pb, Cu and 6um Ag. 350x Parameter: 7 / 200 / 3 / 50 / Fix / Rotating 5 / 200 / 5 / 0-30 / Rock / Rotating 6 / 200 / 0.5 / 0-30 / Rock / Rotating 32
33 2000x Die Package, after Ar etch, Enlarged view of Die attach, Solder resist and Metal trace of Pb, Cu and 6um Ag. Parameter: 7 / 200 / 3 / 50 / Fix / Rotating 5 / 200 / 5 / 0-30 / Rock / Rotating 6 / 200 / 0.5 / 0-30 / Rock / Rotating 33
34 CONTACT Gatan is the leading supplier of Specimen Preparation Tools for the materials science market, offering a full line of instruments that are the premier choice for the complete EM specimen prep lab. High milling/etching rates coupled with rapid specimen exchange yield high throughput to meet the demands of today s overworked lab. Consistent performance delivers quality specimens in less time and with less effort. When your specimen preparation work depends on staying ahead of the competition, the right tools can make a world of difference. Our specimen preparation tools signify quality, ease of use and long term reliability. Designed to go the distance. This publication is the copyright of Gatan, Inc. and contains information which may not be used or reproduced unless agreed by the company in writing. Gatan, Inc. has a policy of continued improvement. The company reserves the right to alter, without notice, the specifications, design or conditions of any product or service. PECS is a registered trademarks of Gatan, Inc. Gatan, Inc All rights reserved. 682 Booklet-CA-SEP12. Worldwide Sales Offices Gatan, Inc. Corporate Office 5794 W. Las Positas Blvd. Pleasanton, CA USA tel fax info@gatan.com Gatan, Inc. 780 Commonwealth Dr. Warrendale, PA USA tel fax info@gatan.com Gatan UK 25 Nuffield Way Abingdon Oxon OX14 1RL United Kingdom tel fax ukinfo@gatan.com Gatan GmbH Ingolstädterstr. 12 D München Germany tel fax gatangmbh@gatan.com Gatan Singapore 10 Eunos Rd. 8 #12-06 Singapore Post Centre Singapore tel fax gatansingapore@gatan.com Nippon Gatan 3F Sakurai bldg Fukagawa, Koto-ku Tokyo Japan tel fax nippongatan@gatan.com Certified Quality Management System Gatan France ROPER Scientific Division Gatan 8, rue du Forez CE 1702 ZI petite Montagne Sud EVRY Cedex France tel fax gatanfrance@gatan.com info@gatan.com
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