Process Control of Ionic Contamination Achieving 6-Sigma Criteria in The

Assembly of Electronic Circuits

P. Eckold[1], M. Routley[2], L. Henneken[1], G. Naisbitt[2], R. Fritsch[1], U. Welzel[1]
[1]
Robert Bosch GmbH, Automotive Electronics, Stuttgart, Germany
[2]
Gen3 Systems Limited, Farnborough, UK
Abstract
Ionic contamination testing as a process control tool a newly developed testing protocol based on IPC-TM 650 2.3.25, was
established to enable monitoring of ionic contamination within series production.

The testing procedure was successfully implemented within the production of high reliability, safety critical electronic
circuits, involving multiple production sites around the world. I will be shown in this paper that the test protocol is capable
for meeting Six-Sigma-Criteria.

For a Gauge R&R study, a calibration solution of 0.1 wt.-% NaCl was used in order to investigate the repeatability and
reproducibility of the test protocol employing newly developed contamination testing systems, which were placed at five
locations worldwide. A total failure range of below 0.1 µg/cm² ≡ NaCl at a target value of 1.0 µg/cm² ≡ NaCl (± 8.8%)
was achieved, combined with manual laboratory handling of fluids (pipette, temperature).

For process control this value is acceptable and demonstrates that ionic contamination testing based on IPC-TM 650 2.3.25
is able to be used as a process control tool in manufacturing of electronic control units.

Introduction
The increasing use of electronic control units in harsh environments, in, especially, high reliability, safety-critical
applications, demands full understanding and rigorous control of electrochemical reliability. [1-3]

The production of electronic circuits involves more than 20 individual chemical process steps, most of which contain high
levels of ionic matter. Electric potentials when combined with a damp or moist operating environment, coupled with the
presence of ionic matter, can often increase the probability for dendritic, electrochemical reactions and premature,
unpredictable circuit failures. [4-6]

For these reasons the analysis of the surface insulation resistance (SIR) can be employed to assess electrochemical
reliability of assemblies and thereby establish a qualified manufacturing process. [7]
 Fig. 1: Influence factors for electrochemical migration (left) and schematic sketch of dendrite formation between
conductive paths (right).[8]

Electrochemical migration (ECM) is known as the migration of electrochemically mobile species between conductive paths
caused by an applied voltage. Consequently, metal can dissolve at the anode and deposit at the cathode which leads to the
growth of a metallic dendrite.[2] Figure 1 (left) illustrates the influence factors for ECM. The combination of a closed water
film and an applied voltage between two conductive paths is the necessity prerequisite for this failure mode.

Ionic contamination on the surface of printed circuit boards (PCBs) is an acceleration factor which can …
… reduce the dissolution enthalpy of metals.
… reduce the dew point.
… shift the pH value towards higher / lower regions.
… increase the conductivity of the water film.

Thus, ionic contamination is not essential but a supporting factor for ECM. Therefore, the level of ionic contamination has
to be controlled during the manufacturing of electronic assemblies using an appropriate process control tool in order to
ensure that the individual production process steps (e.g. surface-mount or through-hole technology) are in control in view
of the overall level of ionic contamination.

Validation of Humidity Robust Design Elements

The electrochemical reliability of design elements used in printed circuit board assemblies can be evaluated based on IPC-
9202[9] under defined climatic conditions. For this purpose the surface insulation resistance (SIR) has to assessed at design
elements which pertain to actual series production conditions as closely as possible (e.g. series PCB materials, solder paste,
…) applying the B52-test board. Applying specific climatic conditions the humidity robustness of design elements
produced using specific material combinations can be evaluated using SIR measurement technology.
 Fig. 2: IPC B52 board consisting of product specific design elements with SIR test structures for validation of
electrochemical reliability.

Figure 2 illustrates the principle layout of the B52 board proposed by IPC-9202. The corresponding design
elements can be adapted according to the advanced product requirements regarding miniaturization and
component portfolio. Consequently, a design element specific test has to be performed in order to ensure the
electrochemical reliability of PCBAs under high temperature and high humidity conditions.

Ionic Contamination Testing as a Process Control Tool

Currently used methods for detection of ionic contamination are described within IPC-TM 650 2.3.25.[10] The
original resistivity of solvent extract (ROSE) test was intentionally designed for process control of the cleaning
process within manufacturing of electronic control units. Currently applied measurement protocols can be
divided into two principal modes of operation: static and dynamic extraction. The different analyser designs
combined with the variety of slightly varying measurements procedures makes it almost impossible to compare
data from different equipment types. In addition, measurement data are often used focussing on an absolute
cleanliness level of no-clean assemblies. It has to be pointed out that these measurement technologies were not
designed for creating cleanliness data of electronic control units manufactured with no-clean processes.

However, ionic contamination testing is able to be used as a process control tool in order to monitor the level of
ionic residues on electronic assemblies caused by several production processes (e.g. reflow, selective soldering
…) over production time. For this purpose an optimized testing system and protocol based on IPC-TM 650
2.3.25 was implemented in collaboration with system suppliers in order to meet a Six-Sigma criteria, and also
between several production sites.

PICT – Process Ionic Contamination Testing

Process ionic contamination testing (PICT) is an optimized testing process compared to conventional ROSE test
procedures. PICT is applying a closed loop / static system according to the classification of IPC-TM 650 2.3.25. The
working principle is illustrated in Figure 3. Test and regeneration cycles are independent from one another and dissolved
ionic residues from the specimens are trapped into an ion exchange column during regeneration until the conductivity of
the extraction solution is reduced to a specified level.
 Fig. 3: Measurement Principle of PICT in testing (left) and regeneration (right) mode as a closed
loop / static testing system in accordance with IPC-TM 650 2.3.25.

The flow rate of the solution was optimized to avoid undue turbulence during the test cycle. Thus, a fast removal of ionic
contaminants from the printed circuit assembly is possible and the testing time can be reduced. Furthermore, the influence
of the atmospheric reaction of carbon dioxide to carbonic acid was decreased. Nevertheless, the carbon dioxide
compensation is a key factor in achieving reproducible measurement results for ionic contamination analyses. Dependent
on the environmental conditions (e.g. atmospheric composition, temperature, relative humidity …) the solvent conductivity
in increased due to the formation of carbonic acid and its subsequent decomposition to hydronium and carbonate ions. Test
measurements with the testing solution under the corresponding environmental conditions and the application of a
mathematical algorithm lead to a site-specific carbon dioxide tolerance factor for compensation. The analysis of solutions
with low concentrations of ionic matter requires a high accuracy of the conductivity measurement cell. For this purpose a
solid-state measuring cell is applied, which is connected to a ballistic amplifier. Thus, a measurement accuracy of ±0.005
µS/cm can be achieved.

In order to use ionic contamination as a process control tool in electronic manufacturing a gauge study was performed for
analysing the repeatability and the reproducibility over different production sites. The test equipment was installed in five
different production sites worldwide and set up according to the technical requirements of the supplier. In general, 2 ml of
a test solution of 0.1 wt.-% sodium chloride was injected and circulated through the conductivity probe in the analyser.
The constantly measured solution conductivity was recalculated to sodium chloride equivalent (NaCl eq. / µg/cm²) based on
a given surface area.

The results of the analysis on repeatability is shown in Figure 4. For this purpose, 40 measurements of a 0.1 wt.-% sodium
chloride solution was carried out over three days at one manufacturing site. No outlier in the data was detected. Based on
the existing data an internal failure of the analyser would have been detected with a probability of 96.8 %. Furthermore, a
slight increase of the instruments reading was observed during each of the three days, with the level dropping overnight.
This effect can be attributed to the temperature of the measurement solution during subsequently performed measurements
during one day. An increased temperature of the solution leads to an increased mobility of ionic species and consequently
to an increased conductivity level. The process was evaluated to be capable for allowing demand of tolerances (±10 %)
achieving a Cgk value of 2.23. In total the repeatability of the analyser meets Six-Sigma-requirements.
Fig. 4: Analysis of repeatability of NaCleq. / µg/cm² based on 40 measurements of 0.1 wt.-% sodium chloride solution at
one site.

Fig. 5: Results from round robin test of ionic contamination measurement at five different production site worldwide.

A reproducibility study was carried out using five different analysers, located at different production sites worldwide. Using
a set of unified work place instructions and directions regarding the local calibration procedure, an aligned test procedure
was ensured. Especially consistency in the laboratory handling of fluids (e.g. pipette, temperature …) has to be taken into
consideration when analysing the results. The total failure range was calculated to be ± 8.8 % which is an acceptable value
for chemical analysis. For the charts in Figure 5 just slight deviation of the measurement values achieved in one site can
be observed. Summarized, ionic contamination testing with optimized parameters is able to be used as a process control
tool detecting ionic contamination on printed circuit board assemblies.

Influence of Process Parameters and Process Optimization

The previously described testing protocol can be used to study the influence of certain process parameters on the level of
ionic contamination. Figure 6 illustrates a selection of influence factors on the final NaCleq. value on product level.

Fig. 6: Ionic Contamination measurements of different products applying different materials and
processes.

Variations in materials (e.g. solder paste, flux for selective soldering …) are strongly affecting the absolute value for ionic
matter. Depending on the chemical activity and the encapsulation of flux residues after soldering, the NaCl eq. value is
varying. It has to be pointed out, that the scattering of the absolute value is increased on product level caused by numerous
process steps during the assembly. However, it is possible to detect process deviations and corresponding root cause
analysis focussing on process stability can be started and monitored.

Consequently, an overall limit of ionic contamination does not fit to the pool of materials and processes used in electronic
manufacturing. Furthermore, ionic contamination testing has to be performed product specific as a process control tool.

Conclusions
As previously emphasised, electrochemical migration is caused by an electric field and a closed water film between
neighbouring conductive paths. Ionic contamination is given by materials and processes and can accelerate the
electrochemical processes under high temperature and high humidity conditions. Consequently, the measurement of ionic
contamination does not predict the humidity reliability of printed board assemblies. The humidity robustness of design
elements can be ensured by SIR measurement technology according to the principle of IPC 9202.
The implementation of ionic contamination testing as process control tool (PICT) exhibits advantages to current ROSE test
protocols. Due to system optimization and the implementation of unified work place instructions, it was possible to achieve
6σ criteria for the repeatability and a sufficient reproducibility of recorded ionic contamination data at five different
production sites worldwide. Using this approach, process control and methods of process optimizations are possible.

Acknowledgements
The authors would like to acknowledge their respective companies for providing financial support for this research.

References
[1] D. Minzari, M.S. Jellesen, P. Moller, R. Ambat, Corros. Sci. 2011, 53, 3366-3379.
[2] P.-E. Tegehall, Impact of Humidity and Contamination on Surface Insulation Resistance and Electrochemical
Migration, Springer Verlag London, New York 2011, 227-253.
[3] B.-I. Noh, S.-B. Jung, Circuit World 2008, 34, 8-13.
[4] V. Verdingovas, M.S. Jellesen, R. Ambat, Corros. Eng. Sci. Tech. 2013, 48, 426-435.
[5] D. Mizari, M.S. Jellesen, P. Moller, P. Wahlberg, R. Ambat, IEEE Trans. Dev. Mater. Reliab. 2009, 9, 392-402.
[6] B.-I. Noh, S.-B. Jung, J. Mater. Sci.: Mater. Electron. 2008, 19, 952-956.
[7] D.Q. Yu, W. Jillek, E. Schmitt, J. Mater. Sci.: Mater. Electron. 2006, 17, 229-241.
[8] IPC-9201A – Surface Insulation Resistance Handbook, 2007.
[9] IPC-9202 – Material and Process Characterization/Qualification Test Protocol for Assessing Electrochemical
Performance, 2011.
[10] IPC-TM-650 2.3.25. – Detection and Measurement of Ionizable Surface Contaminants by Resistivity of Solvent
Extract (ROSE), 2012.
 Process Control of Ionic Contamination achieving
6-Sigma Criteria in the Assembly of Electronic Circuits

Dr Pierre Eckold of Robert Bosch GmbH & Mark Routley of Gen3 Systems Ltd
Content
1. Modern Day Electronics

2. Interaction of Humidity with Interconnect Technology

3. Validation of Humidity Robust Design Elements

4. Measurement Technologies for Ionic Contamination

5. Ionic Contamination Testing as Process Control Tool

6. PICT – Process Ionic Contamination Testing

7. Conclusions
 Modern Electronic Control Units
• … are the products behind the products

100 µm

• highly reliable electronic control units under high temperature / humidity conditions

Product Design
Increasing Requirements

• material / housing
• miniaturization
motor management ABS/ESP wiper systems concept
• high voltage / current
• chemical interactions
applications e-bike
• knowledge of detailed
• increased lifetime
transmission control camera systems steering cause-effect-relations
 Interaction of Humidity with Interconnect Technology
• combination of closed water film and electric field between
neighbouring conductive paths causes electrochemical migration
MUST MUST
• electrochemical migration (ECM): voltage
• migration of electrochemically mobile species from anode towards cathode through electrolyte
→ metal deposition at cathode
→ dendrite growth
• deep understanding of used materials regarding their properties under high temperature /
humidity conditions during release process
CAN
• validation of design elements applying B52 approach under high temperature / humidity
VENN Diagram illustrating influence
factors on ECM [1]
• influence of ionic contamination:
• ionic matter is given by materials / processes with technical grade
• can … reduce dissolution enthalpy of metals
… reduce local dew point
… shift pH value
… increase conductivity of water film
• no essential factor for electrochemical migration
→ to be controlled during manufacturing of electronic assemblies
[1] IPC-9201A - Surface Insulation Resistance Handbook, 2007
Validation of Humidity Robust Design Elements
• absolute contamination level is design-dependent and does not predict humidity
robustness of specific assembly / product
• electrochemical reliability evaluated on PCB assembly level acc. to IPC-9202
• as close to actual series production conditions as possible (e.g. series PCB material, solder paste, …)
• measurement of surface insulation resistance (SIR) using model components under defined climatic conditions
• measurement of ionic contamination can be referenced to SIR results
→ BUT: no direct correlation between level of ionic contamination and its robustness against ECM

1000 h
40 °C
93 % r.h.

IPC B52 Board Examples of SIR measurement data

Measurement Technologies for Ionic Contamination
• Ion Chromatography
• separation and analysis of ionic species dissolved from
PCBA after extraction
• fingerprint of ionic species in µg/cm² (integral value)

• Resistivity of Solvent Extraction

• measurement of solution conductivity after PCBA extraction
• sum of ionic species in µg/cm² (integral value)

• Local Extraction
Schematic of Ion Chromatography measurement system
• potentiostatic measurement of electrical current through
an extraction solution locally extracted from PCBA
• sum of ionic species soluble in extract in µA (local value)

• Fourier Transform Infrared Spectroscopy

• detection of characteristic molecular vibrations caused
by excitation via monochromatic light Schematic of FTIR measurement system
• fingerprint of organic ionic species (local value)
Ionic Contamination Testing as Process Control Tool
• original Resistivity Of Solvent Extract test
• PCB rinsed with deionized water / isopropanol mixture
• measurement of solvent conductivity and recalculation to NaCleq. / µg/cm²

• current applied methods

• static extraction: keep same extraction solution, just circulated
• dynamic extraction: solution passed through ion exchange filter Original ROSE measurement
→ results from different equipment types cannot be compared

→ current use of applied methods focus on absolute cleanliness level

Contamination
• Ionic Contamination Testing as Process Control Tool time

Computer
• measurement principle according to IPC-TM 650 2.3.25
Software

• used only as process control tool → SPC chart (no cleanliness testing)
Calibration
Integration

• requirement: repeatability (6σ) + sufficient reproducibility between production sites Schematic of automated ROSE measurement

• optimized testing system and protocol in cooperation with system suppliers

→ process control focussed on relative comparison over production time

PICT – Process Ionic Contamination Testing
• optimization of testing process compared to conventional ROSE test procedure
• closed loop / static testing system
→ testing and regeneration cycle are independent from one another
→ calibration of system using test solutions
→ regeneration towards a known “base line” for testing to commence

testing cycle regeneration cycle

PICT – Process Ionic Contamination Testing
• optimization of testing process compared to conventional ROSE test procedure

• flow rate
→ high circulation rate without creating undue turbulence during test cycle
→ fast removal of ionic contaminants from PCBA
→ reduction of testing time

• CO2 compensation
→ increased solvent conductivity during test cycle due to CO32- formation
→ strongly dependent on environment (important for plant implementation)
→ implementation of site specific CO2 tolerance factor for compensation

• accuracy of conductivity measurement cell

→ sold state measuring cell connected to ballistic amplifier
→ measurement accuracy of ±0.005 µS/cm
Ionic Contamination Testing as Process Control Tool
• Gauge Study - Measurement of fluids (one site)
• general procedure
• injection of test solution (0.1 wt. -% NaCl)
• circulation through the conductivity probe in analyser (record of time course)
• recalculation of NaCleq. / µg/cm² at the end of measurement time based on given surface area

2ml of 0,1 wt% NaCl solution 2ml of 0,1 wt% NaCl solution
Increase by time due to CO2 absorption Correction of CO2 absorption by software
Ionic Contamination Testing as Process Control Tool
• Gauge Study - Measurement of fluids (one site)
• factors of influence
• CO2 compensation → important for plant implementation
• solvent type / temperature

Ionic Contamination
ionische Kontamination Influence of Temperature on Ionic Contamination
0,35

0,33
µg NaCl equiv. / cm²

0,31
2,00E-08
variation of factors for CO2 compensation
3,00E-08
using equal injection volumes of NaCl
0,29 5,00E-08
6,00E-08

0,27

0,25
0 100 200 300 400 500 600 700 800 900
time [min]
Ionic Contamination Testing as Process Control Tool
• Gauge Study - Measurement of fluids (one site)
• factors of influence
• chemical nature of injection solution: sodium chloride vs. glutaric acid

→ linearity is given by applying PICT test procedure

Linearity of Analyzer
Linearity using PICT
by CM22 analyzer Linearity of Analyzer
Linearity using PICT
by CM22 analyzer
6 type 6 type
constant surface area: 10.000 mm² Glutaric Acid constant surface area: 10.000 mm²
Glutaric Acid
Fluids: molar concentration = const. (1,711 mmol/l) Fluids: molar concentration = const. (1,711 mmol/l)
NaCl NaCl
0,01 wt% NaCl, 0,026 wt% Glutaric Acid 0,01 wt% NaCl, 0,026 wt% Glutaric Acid
5 5
CM22: RT, 50/50 Vol% IPA/water, 15min CM22: RT, 50/50 Vol% IPA/water, 15min
NaCl-equi / µg/cm²

NaCl-equi / µg/cm²
4 4 NaCleq. is
chemical directly
3 nature of salt 3 proportional
influences to
NaCleq. conductivity
2 2
(independent
on chemical
1 1 nature of
salt)
0 0
0 1 2 3 4 5 0,00 0,02 0,04 0,06 0,08 0,1 0 0,1 2
Volume / mL Conductivity / µS/cm
Ionic Contamination Testing as Process Control Tool
• Gauge Study - Measurement of fluids (one site)
T-trend is seen;
Measurements at three different days
Type 1 Gage Study for NaClequi / µg/cm²
• 40 measurements with 0.1 wt.-% Reported by: L. Henneken, AE/EAI1
NaCl solution were carried out Gage name:
Date of study:
NaCleq. analyzer
CM22 NaCl-equivalent
07.1 2.201 5
analyzer Tolerance:
Misc:
1
2mL, 0.1 wt% NaCl-solution

Run Chart of NaClequi / µg/cm²

1,10 Ref + 0,10 × Tol
• no outlier in data detected

NaClequi / µg/cm²
1,05
(based on existing data: 96.8 % probability T-trend T-trend T-trend

for occurrence of one failure for internal 1,00 Ref

failure of analyser)
0,95

• temperature trend was observed 0,90 Ref - 0,10 × Tol

1 5 9 13 17 21 25 29 33 37
Observation
• capable for allowing demand of tolerance
(± 10 %) Basic Statistics Bias Capability
Reference 1 Bias 0,01 Cg 2,46
Mean 1 ,01 T 4,354 Cgk 2,23
StDev 0,01 4 PValue 0,000
• repeatability of analyser meets 6σ 6 × StDev (SV) 0,081 (Test Bias = 0)
%Var(Repeatability) 8,1 3%
requirements Tolerance (Tol) 1
%Var(Repeatability and Bias) 8,96%
Ionic Contamination Testing as Process Control Tool
• Gauge Study - Measurement of fluids (different sites)

• round robin test at five different R Chart by Operators

Site
AnP 1 EAISite 2 Site
Szh 3 Clj Site 4 JuPSite 5
production sites UCL=0,06652

Sample Range
→ unified work place instruction and directive 0,050

_
incl. local calibration 0,025 R=0,02036

0,000 LCL=0
1 2 3 4 5 1 2 3 4 5 1 2 3 4 5 1 2 3 4 5 1 2 3 4 5
Parts
• five different analysers combined with
laboratory handling of fluids (e.g.: pipette, NaClequi /µg/cm² By Parts ( Operators )
temperature, …) for measurements
→ total failure range of ± 8.8 % 1 ,2

• acceptable for chemical analyses

0,6

• capable measurement system of detecting

improper changes in contamination level 0,0
Parts 1 2 3 4 5 1 2 3 4 5 1 2 3 4 5 1 2 3 4 5 1 2 3 4 5
Operators AnP1
Site EAI2
Site Szh3
Site Clj4
Site JuP
Site 5
Ionic Contamination Testing as Process Control Tool
• Influence of Manufacturing Processes on Ionic Contamination Level

• larger scattering of data in ionic variation in variation in THT with and without with and without THT
contamination on product level solder pastes processes THT process process / surface re-calc.

→ caused by numerous process steps

• control tool in assembly process due to

comparable measurement capability

• ionic contamination strongly influenced by

materials, processes and rules for surface
calculation
→ process deviations can be detected and
root cause analysis started

• comparison of like with like

Ionic Contamination Testing as Process Control Tool
• Process Control and Optimization Tool

• value for ionic contamination to

be used as characteristic value
for process optimization

• optimized fluxing parameters for specific

product were evaluated

• reduction of flux application without any

influences on production quality was
achieved

• PICT is used as process control tool at

different manufacturing sites aligning
manufacturing processes
Conclusions
• humidity robustness of design elements ensured by SIR measurement technology
under high temperature and high humidity conditions

• absolute value of ionic contamination does not predict reliability

• ionic contamination testing as process control exhibits advantages to current

ROSE test protocols

→ achieving 6σ criteria for manufacturing of electronic control units

→ complementary to material / design element release based on SIR
measurements applying B52 approach

• process control / optimization at different manufacturing site world wide possible

Acknowledgements
• Lothar Henneken, Roman Fritsch and Udo Welzel, Robert Bosch GmbH

• Graham Naisbitt and Alasdair Naisbitt, Gen3 Systems Ltd

• Brian Ellis, “System” founder

Thank you for your attention

Any Questions?