CCB4423

Polymer Process Engineering

SEPTEMBER 2016
EXPERIMENT 6
Determination of coating adhesion between epoxy and steel by pull adhesion
tester
Laboratory Report
Group Members :
Name Matrix ID
MUHAMMAD FAKHARUDIN BIN SHAHARUDIN 17556
JASVINDER SINGH 15477
MUHAMMAD ADAM AKMAL BIN RAMON ZAHEDIN 18344
MIELAN RAJ 17183
KUEK YEE RUI 18053

Group Number : 10
Lecturer : DR. ZAKARIA BIN MAN
Date of Experiment : 21th of NOVEMBER 2016
Date of Submission : 28th of NOVEMBER 2016

1
INTRODUCTION

This experiment is designed to assist students to understand the phenomenon of coating adhesion
and relate the effects of multiple curing times, curing temperature and effect of water on mechanical
properties of the coating materials.
The most common technique used to measure the coating adhesion is the pull off adhesion tester
(ASTM D 4541). After the metal coating process, this testing quantifies the strength of the bond
between substance and coating. The adhesion tester employs a pull-off method to determine the
required force to pull an area of coating away from the base material.
1. Material and Equipment
I. Steel Plate
II. Araldite Glue
III. Elcometer 10e Pull Off Adhesion tester with Elcometer accessories
IV. 20 Dollies
V. Epoxy
VI. Base Support Ring
VII. Magnetic Dolly Clamp
VIII. Ratchet Spanner (Scale 3 and 4 only)
IX. Polypropylene Carrying Case

Figure 1: ASTM D 4541 with metal dollies

2
PROCEDURE

X. The surface of the dolly and the test area should be cleaned and be oil free, moisture
free and dust free to ensure good bonding between coating and dolly face.
XI. The dolly surface is prepared and coating where the dolly is to be applied by
roughening with an abrasive paper. Both surface are to be cleaned and de-degreased
with a suitable solvent.
XII. The adhesive supply with the instrument is Regular Araldite which is a two
component epoxy paste. When mixed, it has to be used by the hour. Both components
should be mixed in a 1:1 ratio
XIII. Curing condition 1: Allow the adhesive to cure the coating on the dolly and leave it to
settle for 1 hour in room temperature and measure the strength.
XIV. Curing condition 2: Prepare 2 dollies and put it in an oven at 120C for 1 hour and
measure the strength of one dolly
XV. After following the curing process, place the dolly onto the prepared test surface and
apply pressure
XVI. Set the drag indicator to zero (0) and start turning the claw carefully with the dolly
XVII. Hold the adhesion tester steady with one hand to prevent rotation and tighten the hand
wheel or nut slowly and evenly apple increasing force to the dolly and hence, stress to
the coating. Continue until the coating fails and the dolly is removed from the
surface, or until the specified stress level is reached, then valve is then read from the
position of the dragging indicator after the test in complete
XVIII. According to Standards, the load should be applied uniformly. The hand wheel can be
turned in four or five stages to make a complete revolution. The wrench should be
rotated without stopping.
XIX. To record the result, first inspect the face of the dolly. In most cases the coating will
fully adhere to the dolly and the test can be claimed as 100% valid. In some cases, the
coating will covered only partially of the area of the dolly and a partial adhesion
failure should be removed

3
RESULT AND DISCUSSION

1. Report the relevant information as stated in ASTM D 4541

ASTM D 4541 test method covers the procedures governed for pull-off
strength (adhesion) of a coating on rigid substrates such metal, wood or concrete. This
test determines the maximum perpendicular force required (tension) that a surface can
handle before detaching or pass/fail analysis whether the surface remains intact at
prescribed force. This test is usually carried out using portable pull-off adhesion tester
which are classified in five instrument types; Test Method A-E. The measurement
using this instrument are limited by adhesion bonds strength between loading fixture
and specimen surface or the cohesive strength of the adhesive, coating layers or
substrate.

To avoid any adhesion failure, the dolly and the steel plate must be properly
cleaned before the testing. Regular equipment calibration is required to avoid any
error during data gathering. In order to promote adhesion of the adhesive material, the
dolly and steel plate must be cleaned with solvent and only light abrasion of the
coating is permitted. If the coating is on a thin substrate, the back of each substrate
test panel is coated with an adhesive and pressed down onto a four inch square
ceramic tile to avoid distortion of the substrate. Following are general testing
procedure according to ASTM D 4541:
Select and clean the test site
Prepare the test dollies
Apply adhesive to dolly and/or surface and allow to cure
Remove the leftover adhesive on the outside of material adhesion area
Connect an adhesion tester and pull to failure or to a specified max
force
Record the final pulling force and qualify the nature of the failure

4
2. Record the strength of the sample.

The pull-off test was carried out using Elcometer 108. Following are the results
obtained.

Temperature (C) Stress (MPa) Observation

Room Temperature 3 Araldite not completely removed from the surface.
120 7 Araldite completely removed from the surface.

3. Discuss the results and explain the difference between the cases
For this experiment, Elcometer 108 was used to obtain the data. The condition that we will
study is the curing temperature. One sample was cured at 120C and one sample was cured at
room temperature. Based on the results, cure conditions will give different adhesion strength
betweem the material and coating. Low cured temperature will result in slow cure and low
crosslink density. Typically, higher temperatures produce a more complete reaction with a
greater degree of cross-linking than lower temperatures. So proper cure conditions are
dependent on the chemistry of the adhesives. For optimal cross-link density, curing at a high
enough temperature will provide sufficient kinetic energy to quickly initiate chemical
reactions at even the most hindered locations and give the molecules enough mobility to fully
network. High cross-link density formation will enable your cured material to exhibit the best
possible mechanical and physical properties for that formulation. Properties such as Tg,
hardness, modulus, electrical conductivity, thermal conductivity, strength and degradation
temperature will be maximized and properties such as CTE, outgassing, and moisture uptake
will be minimized.

4. Give TWO (2) examples of application and discuss it.

Application for the Elcometer 108 Hydraulic Adhesion Tester is an extremely versatile gauge
which can be used for many adhesion requirements. Tests can be made on flat or curved
(concave and convex) surfaces. Elcometer 108 is suitable to be used for coating test on tanks
pipelines and others. This is because this equipment is hand-powered and portable which
makes it ideal for site work. It also comes with reusable stainless steel dollies. Elcometer
application also include test for paint or plasma spray on bridge decking, coatings on steel,
aluminium and concrete. In genereal, it is widely being applied in Chemical or Process
Coating as well as Paint and Pigments. There are three categories for test using Elcometer.
The first one is Cross Hatch / Cross Cut Method where the coating is cut into small squares,

5
thereby reducing lateral bonding, and the adhesion assessed against ISO, ASTM or Corporate
Standards. Secondly, Pull Off Adhesion Method where tensile dollies (or stubs) are glued to
the coating and, once the adhesive has cured, the force required to pull the dolly off the
surface is measured. The third method is Push Off Adhesion Method that is almost similar to
the second method. However, the dolly is pushed off the surface by the adhesion gauge

CONCLUSION
In this experiment, the concept of coating adhesion was thought to and explained to
student and the curing temperature effect and curing temperature time was studied. Based on
the results of the experiment, it was proven that the higher curing temperature gave a stronger
coating adhesion when compared to room temperature and that the coating of adhesion to the
surface of the material was evenly distributed. This is due to the fact that the higher curing
temperature allows a more complete reation to occur and as a result, a shorter curing time is
needed to achieve better adhesion.

REFERENCES
Elcometer (2012). Elcometer 108 Hydraulic Adhesion Tester: Operating Instructions.
Retrieved from
http://www.elcometer.com/images/stories/PDFs/InstructionBooks/108.pdf

Epoxy Technology. (2015). Cure Temperature Considerations. Retrieved from

http://www.epotek.com/site/files/brochures/pdfs/Cure_Matters_Final.pdf