AN104

Application Note # 104
XRF inline solution analysis of zinc-nickel concentration of

electroplating baths
Zinc-nickel coatings are widely used because of their
excellent corrosion-protective characteristics. It is
important for the quality of these and other metallic
coatings that the composition of the electroplating bath
is within a narrow tolerance window. This is the only
way to achieve the required coating properties. For effi-
cient bath monitoring and control, inline measurement
by X-ray fluorescence analysis is a suitable method.
Status quo and challenges
Electroplating baths are subject to process fluctuations

which can have a considerable influence on the deposi-
tion behavior and the resulting coating thickness. Conti- Figure 1: The solution for your solutions: The FISCHERSCOPE® XAN®
nuous monitoring of the solutions is therefore essential. LIQUID ANALYZER
For this, the zinc-nickel (ZnNi) concentrations of the baths
are regularly checked manually in the company labora- A more frequent bath control is desirable for process-re-
tory, for example using wet chemistry, AAS or ICP-OES lated reasons. In order to be able to run the deposition
methods. In general, such measurements take place 1 to process safely and without much waste, at least four
2 times a day. The disadvantage of these chemical proce- zinc-nickel bath analyses per hour should have been car-
dures is that they are time-consuming and cost-intensive. ried out. These frequent measurements can no longer be
Due to the time offset between sampling and testing, reasonably carried out manually, so automating the mea-
real-time bath control is also not possible. surement would lead to more efficiency in the process.
In theory, the chemical measurement methods listed
above can be automated. Due to the high salt load and
aggressiveness of the ZnNi baths, the X-ray fluorescence
measurement method is particularly suitable for automa-
tion, as it does not require any further sample preparation
compared to the other methods.
Automated inline quality control for

electrolyte solutions
The FISCHERSCOPE® XAN® LIQUID ANALYZER in combi-

nation with the powerful and proven WinFTM® software
combines all requirements: The fully automated inline
XRF measuring instrument continuously delivers mea-
surement results and analyzes the metal concentration
of up to four electroplating baths with high precision. The
calibration is also fully automatic and the intuitive and
large touch display ensures easy operation. The instru-
ment is not only suitable for the control of zinc-nickel
baths, but also for the monitoring of other galvanic baths
such as zinc, nickel, gold, chromium, rhodium and palla-
dium. Figure 2: Functionality of the FISCHERSCOPE® XAN® LIQUID
ANALYZER
The high-tech measuring cell is unique: the flow cell is
suitable for the temperatures, pH values, salt loads, sol- Market leading measurement performance
vents and particle loads typical for the process and, due
to the design, no change of the measuring cell is necessa- As an example, measurements were carried out on vari-
ry. In combination with intelligent material selection and ous typical ZnNi baths. The typical ZnNi bath is composed
automatic rinsing and monitoring processes, a maximum of 5 - 15 g/l zinc and 0.5 - 2 g/l nickel.
tested uptime of more than one year is guaranteed,
depending on rinsing and cleaning cycles and the com- In a first step, the comparability of the XRF measurement
position of the coating baths, among other factors. The with a classical wet chemical analysis (titration) was
design of the measuring device with four separate inline compared. For this purpose, the concentration of zinc and
measuring cells as well as inlets and outlets - a separate nickel was measured over a measurement time of 10
measuring cell for each bath to be monitored - simplifies seconds each.
bath inlet, saves valves and prevents contamination.
Functionality
The FISCHERSCOPE® XAN® LIQUID ANALYZER is connec-

ted to the electroplating bath either directly via a line or
via a ring line. The solution to be analyzed is delivered
to the flow cell in the device, in which the metal content
is determined fully automatically by X-ray fluorescence
measurement.
The measured values are displayed on a screen (HMI) or

exported to the higher-level control system. The special
feature: The measured data can be displayed simulta-
neously on additional monitors directly at the electropla-
ting bath. The plant operator can therefore monitor the
current measured values and react quickly in the event of
deviations, even if the measuring device is located in a
separate room. Figure 3: Comparative measurements of zinc by XRF and titration
The FISCHERSCOPE® XAN® LIQUID ANALYZER shows a
very good repeatability in measurements. At the measu-
red value of 6.82 g/l zinc and 10 s measuring time, the
coefficient of variation (COV) is only 0.26 %. At 1.26 g/l
nickel and also 10 s measuring time, the COV is 0.71 %.
Zink Nickel
Average value [g / l] 6,82 1,26
Standard deviation [g / l] 0,018 0,009
Coefficient of variation COV [%] 0,26 0,71
Figure 6: Measurement results
Conclusion:
For efficient analysis of metal concentrations in elec-
troplating baths, the XRF inline instrument FISCHER-
Figure 4: Comparative measurements of nickel by XRF and titration SCOPE® XAN® LIQUID ANALYZER is the perfect answer.
By analyzing up to 4 electroplating baths in a row and
As can be seen from Figures 3 and 4, the determination of in real time, it eliminates the need to change measuring
metal concentration by XRF measurement provides very cells, time-consuming sampling, and information gaps.
good comparability to titration. The instrument measures your electroplating bath
automatically and with the highest precision. It ensures
In another measurement, the long-term measurement reproducible measurement results that you can rely on.
behavior over a period of 48 h was observed on a typical Without loss of time, the bath control can be adapted to
ZnNi bath. the results of the measurements. This makes your so-
lution analysis more precise, faster, more economical
and essentially maintenance-free.
For further information, please contact our Fischer

experts: [email protected]
Figure 5: Results of the long-term measurement of zinc and

nickel concentrations over 48 hours

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Application Note # 104

XRF inline solution analysis of zinc-nickel concentration of

Status quo and challenges

Electroplating baths are subject to process fluctuations

Automated inline quality control for

The FISCHERSCOPE® XAN® LIQUID ANALYZER in combi-

The FISCHERSCOPE® XAN® LIQUID ANALYZER is connec-

The measured values are displayed on a screen (HMI) or

Figure 6: Measurement results

For further information, please contact our Fischer

Figure 5: Results of the long-term measurement of zinc and

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