Electronics Materials Solutions Division Technical Service ... · Electronics Materials Solutions Division Technical Service Report . IMPORTANT NOTICE: All physical properties, statements,

Electronics Materials Solutions Division Technical Service Report

IMPORTANT NOTICE: All physical properties, statements, recommendations, opinions and technical information contained in this Report are based on tests we believe to be reliable, but the accuracy and completeness of the Report is not guaranteed. The use of this Report is at the sole discretion of the Report recipient and other users. Before using, the Report recipient and other users must determine the suitability of this Report for their intended application, and assume all risk and liability whatsoever in connection with any use of this Report. 3M makes no warranties, express or implied, including but not limited to any implied warranty of merchantability or fitness for a particular purpose, or implied warranty arising out of a course of dealing or of performance or usage of trade. 3M shall not under any circumstances be liable for any direct, indirect, incidental, special or consequential damages in any way related to the use or misuse of this report.

Company: Automotive Parts Manufacturer X Substrate: Stainless steel Contaminant(s): Metal particulate, cutting oil Industry: Automotive Contact: Mr./Ms. X, Senior Manufacturing Technician Date: November X, 2017

Overview A batch of approximately 400 small stainless steel parts used in automotive subassemblies were received from the customer for a cleaning evaluation using 3M™ Novec™ 73DE Engineered Fluid in a standard two sump vapor degreaser. The goal was to remove particulate (metal shavings, fines and other foreign debris) and cutting oil (hydrocarbon based, no water mix) from an upstream milling process. Procedure First, a single part was picked out of the lot as received and photographed under magnification to identify the general level and size of particulate contamination. See Pictures 1-3 below. Pictures 1, 2, 3. Left, side of part (30x); Middle, bottom of part (50x); Right, top of part (50x); as received, prior to cleaning

Electronics Materials Solutions Division – Technical Service Report

IMPORTANT NOTICE: All physical properties, statements, recommendations, opinions and technical information contained in this Report are based on tests we believe to be reliable, but the accuracy and completeness of the Report is not guaranteed. The use of this Report is at the sole discretion of the Report recipient and other users. Before using, the Report recipient and other users must determine the suitability of this Report for their intended application, and assume all risk and liability whatsoever in connection with any use of this Report. 3M makes no warranties, express or implied, including but not limited to any implied warrant y of merchantability or fitness for a particular purpose, or implied warranty arising out of a course of dealing or of performance or usage of trade. 3M shall not under any circumstances be liable for any direct, indirect, incidental, special or consequential damages in any way related to the use or misuse of this report.

Next a set of 5 parts were extracted with 250 µL of high purity heptane. The extract was pipetted onto a ZnSe crystal ATR (Attenuated Total Reflectance) accessory. The heptane was evaporated under a stream of dry nitrogen leaving the extracted surface residue from the part. The residue was scanned by Fourier-Transform Infrared (FT-IR) spectrophotometry. This allows the qualification and quantification of hydrocarbon residue from the cutting oil. See Figure 1. Figure 1. FT-IR spectrum of residue on parts prior to cleaning

Typical C-H (hydrocarbon) bond stretching

Typical C-H bond bending



The lot of parts received was then split into two approximately equal batches (by weight). The parts in the first batch, “Batch A”, were placed in a small steel mesh basket and all parts were oriented on their sides. This was thought to help orient the parts so that the particulate could be best removed from the tops and bottoms. “Batch B” was oriented similarly in an identical steel mesh basket. Picture 4. Parts as received, arranged on sides in basket prior to cleaning

The small basket was then placed into a larger steel basket that fits the hoist in the vapor degreaser. The parts were then processed as described in Table 1. Table 1. Cleaning process recipes

Batch A B

Immersion time in Novec 73DE with 40 kHz ultrasonics (min) 5 7.5

Vapor rinse time (min) 4 6

Freeboard dry time (min) 1 1.5

Total cycle time (min) 10 15



Pictures 5 and 6. Top, parts basket immersed in rinse sump being agitated with ultrasonication; Bottom, parts basket in the freeboard drying zone after immersion and vapor rinsing

Boil Sump

Rinse Sump



Results After cleaning, the dry parts were poured from the basket onto a sheet of pre-cleaned aluminum foil and lightly covered until they cooled to room temp. Then 5 parts from each batch were then rinsed with heptane and the extracts evaporated and analyzed by FT-IR as before. See Figures 2 and 3. One part from Batch B was also photograph under magnification to look for any residual particulate matter. See Pictures 7-9. Figure 2. FT-IR spectra of Batch A (top) and Batch B (bottom) parts after cleaning



Figure 3. FTI-IR spectra of top parts as received (top), Batch A (middle) and Batch B (bottom) on common-scale axes to show comparative residue levels

Significant hydrocarbon residue reduction

10 min cycle time

15 min cycle time

Parts as received



Pictures 7, 8, 9. Batch B part post cleaning: Left, side of part (30x); Middle, bottom of part (50x); Right, top of part (50 x)

Discussion/Conclusions Visual inspection under the microscope, comparing Pictures 1-3 to 7-9, showed that the metal shavings and other particulates were effectively eliminated from the parts during the cleaning process. Using slightly longer immersion and vapor rinse times had a definite impact on the resulting level of cutting oil residue (compare FT-IR spectra from Batch A and Batch B in Figure 2). Comparison of the spectra in Figure 3 also shows that the hydrocarbon residue (as noted by the strong absorbances at 2700-3000 and 1700-500 cm-1) from the cutting oil was effectively eliminated in the Batch B cleaning process. Any residue absorbances in the Batch B spectrum where practically buried in the background noise. Finally, each batch of parts was packaged in a heat-sealed plastic pouch and labeled. The parts were packaged for return to the customer for final inspection and validation of the cleaning process. If there are any questions about this report or the methods used, please contact Karl Manske of the 3M EMSD Technical Service group. Karl Manske Senior Technical Service Chemist 3M Electronics Materials Solutions Division

Electronics Materials Solutions Division Technical Service ... · Electronics Materials Solutions Division Technical Service Report . IMPORTANT NOTICE: All physical properties, statements,

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Electronics Materials Solutions Division Technical Service ... · Electronics Materials Solutions Division Technical Service Report . IMPORTANT NOTICE: All physical properties, statements,