Monitoring the Cleanliness of an Electrolytic Solution Used for Copper Plating

By AZoM

Table of Contents

Introduction
Materials and Methods
Instrument Set up and Calibration
Procedure
     Electrolyte
     Sample Analysis
Results
Conclusion
About Beckman Coulter

Introduction

Acid copper plating is an electrochemical process used to manufacture printed circuit boards. The action of the ionic current in an electrolytic copper plating tank is such that while plating, any and all suspended particulates are forced toward the cathode which is the panel that is being plated deposited. If the particles are large enough (size 5 to 20 µm), their presence can disrupt the local electrical field enough to reduce the effectiveness of the levelers present in the electrolyte. This electrophoretic migration results in rough plating with the contaminating particles trapped in the electrolytic layer formed on top of a critical circuit element. In a production setup, the plating electrolyte is normally continuously filtered using one or more 1 µm filters specially made for "polishing" electro-chemicals.

Materials and Methods

Instrument Set up and Calibration

A 100-μm aperture tube was utilized for the analysis of this case study. The linear dynamic range for any aperture is 2% to 60% of its diameter. A 100-mm aperture tube can analyze the particle concentration and size distribution from 2 to 60 μm. In case a different size range is needed, another aperture tube can be used. The instrument was calibrated as per the Multisizer 3 Operator’s Manual. In order to determine concentration and size distribution of particles in the sample, the results were obtained in number/mL. The size Interpolation feature in the software was utilised to quantify the number of particles at different size levels. The control mode for the instrument was Volumetric Mode choosing 500 μL as the run volume.

Procedure

Electrolyte

Since the sample is a conductive solution, it was analyzed with no further dilution into another electrolyte. For the external electrolyte jar, a 0.45-μm filtered sample was utilised. In the sample information dialog of the Multisizer 3 software the information below was entered:

          Sample Volume: 150 mL.
          Electrolyte Volume: 0 mL.
          Analytical Volume: 500 μL.

Sample Analysis

  • Running the sample.

A round bottom beaker having the sample preparation was analyzed using a 100-μm aperture. The aperture tube was flushed prior to each analysis. After each run, the electrode and aperture were rinsed before proceeding to the next sample.

Results

The results are expressed in particles/mL. The graph in figure 1 below shows the size distribution of a single sample.

Figure 1. Size distribution of a reference sample.

Particle Concentration: 3,758 particles/mL larger than 2 μm.

In order to establish the repeatability of the method, the same sample was analyzed five consecutive times. Table 1 shows the results.

Table 1. Repeatability of results.

Particles Mean d10 d50 d90
Run per mL μm μm μm μm
1 3,758 2.73 2.01 2.15 3.80
2 3,294 2.73 2.02 2.16 3.71
3 3,654 2.69 2.02 2.14 3.50
4 3,744 2.77 2.01 2.13 3.70
4 3,714 2.72 2.02 2.14 3.57
Aver. 3,633 2.73 2.02 2.14 3.66
C.V. 5.3% 1.0% 0.0% 0.6% 3.2%

Along with the total concentration of particles, by using the Interpolation Points feature in the software, it is possible to determine the concentration of particles above pre-set size levels.

Particles per mL larger than Diameter (μm)
3,758 2
668 3
323 4
187 5
58. 10
1 25
0 50

Conclusion

As the Coulter Principle is the highest resolution technology present for sizing and counting particles, it is an excellent tool for monitoring cleanness of the electrolytic solution in the copper plating process. The procedure described here may also be used to evaluate filtration efficiency during the cooper plating.

About Beckman Coulter

Precision measurement for research, development, and high-speed manufacturing is required in several industries to ensure quality, consistency and cost management. Beckman Coulter provide fully integrated, easy-to-use automation systems with numerous quality applications-from particle size, distribution and volume counting to cellular analysis. All systems are configurable to meet specific needs and provide efficient process automation for diverse businesses.

This information has been sourced, reviewed and adapted from materials provided by Beckman Coulter.

For more information on this source, please visit Beckman Coulter.

Date Added: Apr 25, 2012 | Updated: Apr 26, 2012
Ask A Question

Do you have a question you'd like to ask regarding this article?

Leave your feedback
Submit