Applications note
PCI System
Cleanliness Inspection of Automotive
Lithium-ion Batteries Manufacture
Particle Contamination Inspection system for VDA19.2
Importance of cleanliness inspection
of the automotive lithium-ion batteries manufacture
Is the cleanliness of the assembly areas under control?
Critical particulate contamination existing in assembly areas can cause product defects.
For example, metallic particle contaminants mixing at the assembly areas of lithium-ion
batteries (LIBs) may induce short circuits in the final products causing them to fail or as a
worse case, ignite. Inspection for particulate contamination is recommended to comply
with the standard called VDA 19.2 for Technical Cleanliness in assembly. Complying with
this standard can improve product safety, yield and the reduction of recalled products.
The standard for the cleanliness in assembly: VDA19.2
ISO16232 is the international standard for the cleanliness control of automotive components.
ISO16232 is based on VDA 19 part 1 (VDA 19.1), which is the cleanliness inspection method advocated by the association of the
German automotive industry (VDA). VDA 19.1 describes the requirements for determining particulate contamination on functionally
relevant automotive components. For system components which cannot be cleaned after assembly, cleanliness inspection using
VDA 19 part 2 (VDA19.2) is recommended. This guideline for Technical Cleanliness in assembly is designed to help protect against
the entry of critical contamination via the environment during production. In automotive LIB assembly areas, the inspection of the
manufacturing environment to comply with VDA19.2 should be applied.
1 Particle Contamination Inspection system
JEOL’s Particle Contamination Inspection System
Inspection system complying with VDA19.2
Advantages of Particle Contamination Inspection System (PCI)
The PCI System uses a Scanning Electron Microscope (SEM) equipped
with an Energy Dispersive X-ray Spectrometer (EDS) to analyze particles
for size, shape and elemental composition. PCI offers several advantages
over optical microscope methods. The system is automated and
can detect smaller (sub-micron) particles versus optical methods. Not
only is size and shape information determined but also the elemental
composition. The PCI System can determine critical particulate
contamination in LIB assembly areas for ensuring VDA 19.2 compliance.
PCI
Optical
Microscope
Detectable metallic
particle size
> 0.1 µm
> 2 µm
Elemental composition
Possible
Impossible
Automation
Multiple
Single
Automated particle count and identification system
Particles are automatically identified
from the SEM images and detected
particles are analyzed by EDS. The
particles can be classified by size,
shape and elemental composition.
It is possible to screen for only
metallic particles which are a critical
contaminant in LIBs.
Image capture
Particle identification
Elemental analysis result of the particle
100 µm
Results
100 µm
100 µm
5 ≦ X<15
15 ≦ X<25
25 ≦ X<50
50 ≦ X<100
100 ≦ X<150
150 ≦ X<200
Aluminium ■
16
0
3
7
2
0
Copper alloy ■
2
7
11
8
1
1
28
16
26
38
0
0
Tin
0
0
1
0
0
0
Particle Size [μm]
Total
Iron steel ■
■
46
23
41
53
3
1
Easy management of the results
Results can be output in Microsoft® Excel®. Flexible management of the reporting, such as Illig value (sedimentation count), can be
performed in accordance with your operation.
■ Areas to inspect
Area
1
Area
5
■ Example of history management of Illig values
Area
2
Area
6
Area
3
Area
7
Area
8
Area
4
Area
9
■ Inspection results of each area
DATE
11/1
11/2
11/3
11/4
11/5
11/6
11/7
11/8
11/9
Area1
388
452
346
398
854
686
330
284
152
Area2
103
122
118
154
328
292
210
162
115
Area3
111
114
131
111
282
227
187
118
125
Area4
137
125
185
128
134
143
180
127
103
Area5
109
130
112
72
142
137
97
124
107
Event
Illig value ■ X ≧ 500
Area
1
Area
5
Area
2
Area
3
Area
4
x ≧ 500
200 ≦ x <500
x < 200
Area
6
Area
7
Area
8
・
・
・
Repair in
Area 1
■ 200 ≦ X<500 ■ X<200
With the history of Illig values, trends such as an increase in the
Illig values after an event, and the area affected by the event can
be determined.
Area
9
Particle Contamination Inspection system
2
Workflow
of cleanliness inspection
PCI System enables an easy daily routine for Cleanliness Inspection
1
Criteria/
condition
setting
・Specify inspection regions, target particles
・Determine criteria of Illig value.
・Set inspection conditions according to the target particles.
・This work is only necessary for the initial setup.
Area
2
Area
1
Area
5
2
Area
7
Area
2
Area
1
Collect particles
Data
Acquisition
Area
3
Area
8
Area
9
・Prepare samples by collecting the sedimented particles on filter or tape.
Sample
preparation
3
Area
6
Area
4
Place on holder
Conductive treatment
if neededArea
6
Area
7
Set to the
AreaPCI System
8
Area
9
・Particle analysis (identification and classification of particles) is performed on multiple regions automatically.
■
Area
5
Area
4
Area
3
Fully-automated analysis workflow
Particle identification
Sedimented particles can be identified by their brightness
difference compared to the substrate.
Image capture
Particles
Frequency
Substrate
sedimented
particles
Field of View movement
After the particle analysis of one field,
the system moves to the next.
View of interest
Sample
Measured region
3 Particle Contamination Inspection system
Brightness
Brightness histogram
Elemental analysis
Elemental analysis is
performed for each
identified particle. The
particles are classified by
the analysis result.
Intensity
Intensity
Intensity
Substrate
Particle identification
Fe
Fe
Fe
X-ray energy [keV]
X-ray energy [keV]
X-ray energy [keV]
4
Analysis/
Confirmation
・PCI system makes it possible to relate the inspected area and the analysis results.
・The particles are classified for each size in compliance with ISO16232/VDA19.1.
・The Illig value is calculated from the results of the size classification to show the contamination grades on a map.
・It’s possible to filter the results to report only metallic particles.
■ Example
Area
of the size classification and Illig values at each inspected
area Area
2
Area
Size
class
/
Size [μm]
1
Sampling
area
Illig
Value
Sampling
Time [h]
Measurement
area [cm²]
Total
Area01
220.8
168
12.56
Area02
655.0
168
Area03
88.6
Area04
Area05
B
C
5 ≦ X<15
15 ≦ X<25
46410
40546
4180
12.56
52282
38038 10032
168
12.56
23331
19016
382.5
168
12.56
52928
879.1
168
12.56
61023
■ Example
D
E
Area
1254
5
418
12
0
2926
1254
Area
6
32
0
3614
538
163
6
41785
8778
1672
655
50160
6270
3344
1072
H
I
J
K
Area
7 0
Area
80
0
0
0
38
0
0
0
0
0
162
15
0
0
0
0
0
0
Legend
Color
Illig value
■
x ≧ 500
■
200 ≦ x <500
■
x < 200
Area
1
Area
5
Reporting
G
25 ≦ X<50 50 ≦ X<100 100 ≦ X<150 150 ≦ X<200 200 ≦ X<400 400 ≦ X<600 600 ≦ X<1000 1000 ≦ X
0
0
0
Area
09
0
0
of the contamination map
The contamination map
can be made by color
from the Illig values.
5
F
3
Area
4
Area
2
Area
6
Area
3
Area
7
Area
8
Area
4
Area
9
・The report shows the results including the contamination map in various formats.
■ Example
report
x ≧ 500
200 ≦ x <500
x < 200
Particle Contamination Inspection system
4
Features
of PCI System
Functions and attachments to easily perform routine work
■ Automation
and intuitive GUI
PCI system includes a variety of automated functions to ensure
that even novice users can operate the system easily with only a
minimum of buttons displayed within the graphical user interface.
SEM GUI with an optical image*1
The step-by-step routine “Sample Exchange Navi” will guide users
through the sample insertion and microscope setup steps ending
in an suitable SEM image.
■ Offline
Data Processing Software*1
Offline Data Processing Software is available to view and review
inspection data and create reports from another PC. This frees up
the PCI System for additional testing streamlining workflow and
productivity.
■ Large-area
Stage and Large Specimen Holder
Dedicated holder for filter *1
Inspect multiple filters with the large, fully-motorized stage.
For example, 6 filters (47 mm diameter) can be mounted
simultaneously using a dedicated holder.
Automated inspections can be performed at night, increasing
inspection throughput and system availability.
Fits 6 filters(47 mm-diameter)
■ Carbon
Coater
JEOL recommends using the integrated low vacuum mode in the
PCI system or to coat the samples with carbon when analyzing
samples on non-conductive filters or substrates or for inspecting
non-conductive particles. The JEOL Carbon Coater is a sample
preparation instrument that evaporates carbon to create a
conductive thin film on the sample surface.
Carbon Coater*1
EC-32010CC
*1: optional
5 Particle Contamination Inspection system
Microscope line-up
for the inspection
JEOL Scanning Electron Microscopes ideal for this inspection
■ JSM-IT700HR
■ JSM-IT510
( LaB6 )
This model uses a high-resolution Schottky field-emission
electron gun.
The stable emission and long lifetime of this emitter
enables reproducible results and un-interrupted operation
for years without gun exchange.
This model can be equipped with an economically friendly
a longer lifetime LaB6 electron gun.
Filaments can be exchanged by users.
■ Specifications
JSM-IT700HR
JSM-IT510 (LaB6)
Electron gun
Schottky field emission (lifetime >25,000 hrs)
LaB6 electron gun (LaB6 lifetime >500 hours）
Resolution
High vacuum mode：1.0 nm@20 kV
3.0 nm@1 kV
Low vacuum mode： 1.8 nm@15 kV
For analysis
： 3.0 nm@15 kV, 3 nA
High vacuum mode： 3.0 nm@30 kV
15.0 nm@1 kV
Low vacuum mode： 4.0 nm@30 kV
Maximum
specimen size
200 mm diameter
200 mm diameter
EDS Detectors
(elemental analysis)
JEOL EDS Detectors in different sizes available (60 mm² recommended),
fully hard- and software-integrated
■ JEOL
benefits
・“One-stop shop”: Complete system by one manufacturer (SEM, EDS, Software, Holder, Coating)
・Dedicated development team for particle analysis to ensure excellent customer support
・Full bandwidth of emitters to ensure cost-friendly solutions for all budgets
・Easy installation – no water or nitrogen needed!
・Dedicated to particle analysis – yet ready to be used for other SEM purposes (quality control,…)
・Close collaboration with existing customers – Customer feedback ensures future optimizations
Microsoft and Excel are registered trademarks or trademarks of Microsoft
Corporation in the United States and/or other countries.
Particle Contamination Inspection system
6
No.0201B338C(Bn)