echniques using the gatan precision etching and coating...
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SEM Techniques
Using the Gatan
Precision Etching
and Coating
System (PECS™)
The Tool
The Technique
The Total Solution
PECS™
Precision Etching and Coating System
The perfect match for a FESEM or
Optical Microscope
Eliminate:Chemical Mess
Chemical HandlingChemical Spills
Chemical HazardsChemical Disposal
Not just another new tool
But a NEW
Sample Preparation
Technique
A Clean Green Technique:
ION BEAM ETCHING
Cleaning
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.
a
b
20kx
4
Precision Etching Coating System
High-resolution cross-section through different coating layers of C and Cr sputtered on Si substrate.
Coating
5
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PECS Coating Sub-nanometer grain deposition of Chromium (Cr), thin amorphous Cr coatings can be deposited without masking delicate specimen features.
100 nm
200kx
6
Precision Etching Coating System
Magnetron Coating
Chromium deposition by comparison is not sub-nanometer or amorphous.
100 nm
200kx
7
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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).
Etching
8
Precision Etching Coating System
SEM image of tungsten plugs and transistors, starting sample as cleaved. Sample etched and coated.
Parameter: 6 / 250 / 2 / 60° / Fix / Rotating 6 / 250 / 1 / 0 - 30° / Rock / RotatingEtch gas I2 7.5 / 200 / 1.5 / 0 - 30° / Rock / RotatingCoating Pt 6 / 200 / 0.3 / 0 - 30° / Rock / Rotating
30kx
8 9
Precision Etching Coating System
SEM image of tungsten plugs and transistors, starting sample as cleaved. Sample etched and coated.
Parameter: 5 / 250 / 1 / 60° / Fix / Rotating 5 / 250 / 1.5 / 0 - 45° / Rock / RotatingEtch gas I2 5 / 250 / 1 / 50° / Fix / RotatingEtch gas I2 5 / 250 / 1.5 / 0 - 45° / Rock / RotatingCoating Pt 6 / 200 / 0.3 / 0 - 30° / Rock / Rotating
23kx
8 9 10
Precision Etching Coating System
SEM image of tungsten plugs and transistors, starting sample as cleaved. Sample etched and coated.
Parameter: 5 / 250 / 1 / 60° / Fix / Rotating 5 / 250 / 1.5 / 0 - 45° / Rock / RotatingEtch gas I2 5 / 250 / 1 / 50° / Fix / RotatingEtch gas I2 5 / 250 / 1.5 / 0 - 45° / Rock / RotatingCoating Pt 6 / 200 / 0.3 / 0 - 30° / Rock / Rotating
22kx
8 9 10 11
Precision Etching Coating System
Metallographic
High-Purity Titanium Structure, after Etching, Micrograph with POL Filters.
Parameters: 6 / 400 / 12 / 60º / Rotating
500x
12
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High-Purity Titanium Structure, after Etching, DIC Micrograph.
Parameters: 6 / 400 / 8 / Vertical / Rotating
500x
13
Precision Etching Coating System
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
200x
14
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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
500x
15
Precision Etching Coating System
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
500x
16
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Structure of High-Purity-Aluminum, after etching, POL Micrograph (rough to grainy grain surfaces appear in color).
Parameter: 6 / 400 / 12 / 53° / Rotating plus 6 / 400 / 24 / 45° / Rotating
50x
17
Precision Etching Coating System
Section of previous figure, after etching, DIC Micrograph.
200x
18
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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
1000x
19
Precision Etching Coating System
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
50x
20
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Superconductor CuSn+NbTi+Ta Covered with Cu Coating, after Etching, Lower Area of previous Figure, CuSn Matrix with NbTi fibers, Micrograph with DIC.
100x
21
Precision Etching Coating System
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 O2 etching
Parameter: 6.5 / 480 / 5 / 40° / Rotating 6.5 / 510 / 7 / 10° / RotatingEtch gas O2 8 / 450 / 4 / Vertical / Rotating
500x
22
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EBSD
EBSP
Indexed Pattern
DetectedBands
CrystallographicOrientation
23
Precision Etching Coating System
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
Precision Etching Coating System
Cu film, Image Quality = 228, 25 keV SEM acceleration voltage, spot size 4.
Parameters: 2.5 / 60 / 115 / 50°/ Rotating
25
Precision Etching Coating System
Aluminum film, Image Quality = 114, 25 keV SEM acceleration voltage, spot size 4.
Parameters: 2.5 / 60 / 30 / 50°/ Rotating
26
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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: 7 / 200 / 3 / 50° / Fix / Rotating 5 / 200 / 5 / 0 - 30° / Rock / RotatingEtch gas I2 5 / 200 / 5 / 0 - 30° / Rock / Rotating 6 / 200 / 0.5 / 0 - 30° / Rock / Rotating
300x
DIE Package
27
Precision Etching Coating System
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: 7 / 200 / 3 / 50° / Fix / Rotating 5 / 200 / 5 / 0 - 30° / Rock / RotatingEtch gas I2 5 / 200 / 5 / 0 - 30° / Rock / Rotating 6 / 200 / 0.5 / 0 - 30° / Rock / Rotating
1500x
28
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Die Package, after Ar etch, enlarged view from Left side of Via hole, No delamination. No grain structure visible before etch.
Parameter: 7 / 200 / 3 / 50° / Fix / Rotating 5 / 200 / 5 / 0 - 30° / Rock / RotatingEtch gas I2 5 / 200 / 5 / 0 - 30° / Rock / Rotating 6 / 200 / 0.5 / 0 - 30° / Rock / Rotating
1500x
29
Precision Etching Coating System
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
1000x
30
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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. Parameter: 7 / 200 / 3 / 50° / Fix / Rotating 5 / 200 / 5 / 0 - 30° / Rock / Rotating 6 / 200 / 0.5 / 0 - 30° / Rock / Rotating
Die AttachSolderResist
5000x
31
Precision Etching Coating System
Die Package, after Ar etch, Overall 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
350x
32
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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
2000x
33
Precision Etching Coating System
Worldwide Sales Offices
Gatan, Inc.Corporate Office5794 W. Las Positas Blvd.Pleasanton, CA 94588 USAtel +1.925.463.0200fax +1.925.463.0204info@gatan.com
Gatan, Inc.780 Commonwealth Dr.Warrendale, PA 15086 USAtel +1.724.776.5260fax +1.724.776.3360info@gatan.com
Gatan UK25 Nuffield WayAbingdon OxonOX14 1RL United Kingdomtel +44.0.1235.540160fax +44.0.1235.540169ukinfo@gatan.com
Gatan GmbHIngolstädterstr. 12D-80807 München Germanytel +49.89.358084-0fax +49.89.358084-77gatangmbH@gatan.com
Gatan Singapore10 Eunos Rd. 8 #12-06Singapore Post CentreSingapore 408600tel +1.65.6408.6230fax +1.65.6293.3307gatansingapore@gatan.com
Nippon Gatan3F Sakurai bldg. 2-8-19Fukagawa, Koto-ku Tokyo135-0033 Japantel +81.3.5639.2772fax +81.3.5639.2763nippongatan@gatan.com
Gatan FranceROPER Scientific–DivisionGatan8, rue du Forez–CE 1702ZI petite Montagne Sud91017 EVRY CedexFrancetel +33.1.69.11.03.69fax +33.1.64.97.19.67gatanfrance@gatan.com
www.gatan.cominfo@gatan.com
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.
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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. 2012. All rights reserved. 682 Booklet-CA-SEP12.CO
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