echniques using the gatan precision etching and coating...

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

www.gatan.com/products/specimen_prep

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


Magnetron Coating

Chromium deposition by comparison is not sub-nanometer or amorphous.

100 nm

200kx

7


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


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



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



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


Metallographic

High-Purity Titanium Structure, after Etching, Micrograph with POL Filters.

Parameters: 6 / 400 / 12 / 60º / Rotating

500x

12


High-Purity Titanium Structure, after Etching, DIC Micrograph.

Parameters: 6 / 400 / 8 / Vertical / Rotating

500x

13


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


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


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


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


Section of previous figure, after etching, DIC Micrograph.

200x

18


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


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


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


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


EBSD

EBSP

Indexed Pattern

DetectedBands

CrystallographicOrientation

23


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.


24


Cu film, Image Quality = 228, 25 keV SEM acceleration voltage, spot size 4.


25


Aluminum film, Image Quality = 114, 25 keV SEM acceleration voltage, spot size 4.


26


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


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.


1500x

28


Die Package, after Ar etch, enlarged view from Left side of Via hole, No delamination. No grain structure visible before etch.


1500x

29


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


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


Die Package, after Ar etch, Overall view of Die attach, Solder resist and Metal trace of Pb, Cu and 6um Ag.


350x

32


Die Package, after Ar etch, Enlarged view of Die attach, Solder resist and Metal trace of Pb, Cu and 6um Ag.


2000x

33


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Gatan, Inc.Corporate Office5794 W. Las Positas Blvd.Pleasanton, CA 94588 USAtel +1.925.463.0200fax [email protected]

Gatan, Inc.780 Commonwealth Dr.Warrendale, PA 15086 USAtel +1.724.776.5260fax [email protected]

Gatan UK25 Nuffield WayAbingdon OxonOX14 1RL United Kingdomtel +44.0.1235.540160fax [email protected]

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Gatan Singapore10 Eunos Rd. 8 #12-06Singapore Post CentreSingapore 408600tel +1.65.6408.6230fax [email protected]

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Gatan FranceROPER Scientific–DivisionGatan8, rue du Forez–CE 1702ZI petite Montagne Sud91017 EVRY CedexFrancetel +33.1.69.11.03.69fax [email protected]

[email protected]

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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©Gatan, Inc. 2012. All rights reserved. 682 Booklet-CA-SEP12.CO

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