ARL-RP-0517 ● JAN 2015

US Army Research Laboratory

Characterization of Tape Adhesion to Chemical 

Agent Resistant Coatings

by Thomas A Considine, Thomas E Braswell, and 

Joseph P Labukas

Weapons and Materials Research Directorate, ARL

Reprinted from the Society for Materials Failure Prevention Technology website [accessed 

2014 Dec 8]. http://www.mfpt.org/Proceedings.htm. Paper presented at: MFPT 2014 

Conference; 2014 May 20–22; Virginia Beach, VA.

Approved for public release; distribution unlimited. 
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Destroy this report when it is no longer needed. Do not return it to the originator.
ARL-RP-0517 ● JAN 2015

US Army Research Laboratory

Characterization of Tape Adhesion to Chemical 

Agent Resistant Coatings

by Thomas A Considine, Thomas E Braswell, and 

Joseph P Labukas

Weapons and Materials Research Directorate, ARL

Reprinted from the Society for Materials Failure Prevention Technology website [accessed 

2014 Dec 8]. http://www.mfpt.org/Proceedings.htm. Paper presented at: MFPT 2014 

Conference; 2014 May 20–22; Virginia Beach, VA.

Approved for public release; distribution unlimited. 
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Characterization of Tape Adhesion to Chemical Agent Resistant Coatings

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Thomas A Considine, Thomas E Braswell, and Joseph P Labukas

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ARL-RP-0517

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Reprinted from the Society for Materials Failure Prevention Technology website [accessed 2014 Dec 8]. 

http://www.mfpt.org/Proceedings.htm. Paper presented at: MFPT 2014 Conference; 2014 May 20–22; Virginia Beach, VA.

14. ABSTRACT

Advanced military coating technologies have incorporated chemical agent resistance, desirable mechanical properties, and 

corrosion mitigating properties into CARC systems currently in use. The performance of these coatings is evaluated using 

MIL-DTL-530721. During the coating application phase and in the field, a tape pull off test is required by MIL-DTL-53072 to 

gauge adhesive strength of a coating to a primer or substrate. We have investigated the chemical and physical interactions of a 

variety of tapes used for the verification of coating adhesion with ASTM D33592 on several substrates using tensile pulltesting, infrared-spectroscopy, and contact-angle measurements. A correlation between tape adhesion and surface wetting 

characteristics has been established. Tapes meeting the minimum performance parameters of 80 inch ounce-force over the 

selected CARC systems were indentified.

15. SUBJECT TERMS

CARC, coatings, coating adhesion, ASTM D3359, cross hatch, surface wetting, tape adhesion

16. SECURITY CLASSIFICATION OF:

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OF ABSTRACT

UU

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OF PAGES

26

19a. NAME OF RESPONSIBLE PERSON

Thomas A Considine

a. REPORT

Unclassified

b. ABSTRACT

Unclassified

c. THIS PAGE

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19b. TELEPHONE NUMBER (Include area code)

410-306-2564

Standard Form 298 (Rev. 8/98)

Prescribed by ANSI Std. Z39.18
1

CHARACTERIZATION OF TAPE ADHESION TO CHEMICAL AGENT 

RESISTANT COATINGS

Thomas A. Considine, Thomas E. Braswell, and Joseph P. Labukas

4600 Deer Creek Loop

Aberdeen Proving Ground, MD 21005

Telephone: 410-306-2564

thomas.a.considine.ctr@mail.mil

Abstract: Advanced military coating technologies have incorporated chemical agent 

resistance, desirable mechanical properties, and corrosion mitigating properties into

CARC systems currently in use. The performance of these coatings is evaluated using

MIL-DTL-530721. During the coating application phase and in the field, a tape pull off 

test is required by MIL-DTL-53072 to gauge adhesive strength of a coating to a primer or 

substrate. We have investigated the chemical and physical interactions of a variety of 

tapes used for the verification of coating adhesion with ASTM D33592on several 

substrates using tensile pull-testing, infrared-spectroscopy, and contact-angle 

measurements. A correlation between tape adhesion and surface wetting characteristics

has been established. Tapes meeting the minimum performance parameters of 80 inch 

ounce-force over the selected CARC systems were indentified.

Keywords: CARC; Coatings; Coating Adhesion; ASTM D3359; Cross Hatch; Surface 

Wetting; Tape Adhesion

Introduction: Under regulation AR 750-1

3

, Army based ground equipment must have a 

full Chemical Agent Resistant Coating (CARC) system as defined in MIL-DTL-53072, 

“CHEMICAL AGENT RESISTANT COATING (CARC) SYSTEM APPLICATION 

PROCEDURES AND QUALITY CONTROL INSPECTION”. Several performance test 

requirements for CARC are specified in MIL-DTL-53072. One such performance 

requirement is adhesion testing of the system in accordance with ATSM D3359 Methods 

A and B, “Standard Test Methods for Measuring Adhesion by Tape Test”. The primary 

test for coating adhesion is the cross-hatch tape adhesion method described in ASTM 

D3359 Method B. Applicators of CARC at OEM’s, depots, and suppliers can provide 

objective quality evidence (OQE) that the integrity of the CARC adhesion is within the 

established limits of MIL-DTL-53072. 

Recently, reports from the users in the field indicate that there is a significant fault with 

the tape adhesion testing used on Army assets4,5. More specifically, many of the tapes 

that are currently used in dry adhesion testing of CARCs reportedly do not adhere well to 

CARC topcoats containing polymer-beads used for gloss reduction6,7. In prior revisions 

of ASTM D3359 a single tape was specified for use in adhesion testing. Without 

adequate tape adhesion to the CARC surface, false positive results of satisfactory CARC 

adhesion to the substrate can easily result in unacceptable fielded materiel, thereby 
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exposing the warfighter to significant risk of IR detection and a coating system that is no

longer resistant to chemical agents. To emphasize the problem more clearly, a schematic 

representation of a tape pull-off test on identical substrates with different tapes is shown 

in Figure 1. The performance specification, MIL-DTL-53072 does not specify the type of 

tape that should be used for adhesion testing or the required peel strength needed to verify the 

coating adhesion. In order to mitigate this risk, it would require the closing of the 

technology gap by identifying suitable tapes for dry adhesion testing and developing a 

fundamental understanding of their adhesive properties with respect to various CARC 

surfaces. 

Figure 1: Diagram displaying differences in tapes used in cross hatch adhesion

In this research, the adhesion of several commercially available tapes to various CARC 

surfaces was evaluated. These tapes were selected based on interviews with several 

OEMs and military coating applicators as to which are commonly used in the field for 

adhesion testing8,9,10. The CARC formulations were varied to investigate the relationship 

between the tapes and the different types of CARC’s available for use by OEM’s and 

depots. More specifically, each tape was tested on water dispersible and solvent borne 

polyurethane topcoats in the two most common colors (Green 38311 and 686A Tan

12) that 

were prepared and provided by four different paint manufacturers. Attenuated total 

reflectance Fourier transform infrared spectroscopy (ATR-FTIR) was used to investigate 

chemical differences in the adhesives used for each tape. Advancing water contact angles 

were measured to provide insight on variations in the surface energies of various CARCs 

and the adhesive backing on the tapes. 

Performance criterion for tape adhesion has been set by the CARC Commodity Manager 

at 80 inch ounce-force using IAW ASTM D 3330, Peel Adhesion of Pressure Sensitive 

Tape, which used a 180 degree pull angle and 1-inch wide tape 13 Tapes that meet or 

exceed the 80 inch ounce-force minimum on CARC systems will be recognized by ARL 

for qualifying the adhesion strength at interfaces within the CARC system. Typically, 

adhesion throughout the various interfaces in this system is verified using IAW ASTM D 

3359.
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That the governing specification for tape adhesion testing has become less precise with 

respect to what tapes are acceptable for use which has created an opening for many 

different types and brands of tapes with varied adhesive compositions. These variations

in tape adhesive composition can lead to differences in adhesion to a substrate. CARC 

formulations within the same specification vary between manufacturers and because of 

this, not all CARCs have similar surface energies. We hypothesize that the wide 

variation in surface energy of CARCs affects adhesion between various tapes and the 

substrate. 

Experimental: 

CARC coated substrates were tested as received from the manufacturers. Table 1 

summarizes the manufacturer, specification, type, color, and extender. 

Table 1: CARC 

Information

Manufacturer Spec Type Color Extender

Green 383

686A Tan

Green 383

686A Tan

Green 383

686A Tan

Green 383

686A Tan

Green 383

686A Tan

Green 383

686A Tan

Green 383

686A Tan

Green 383

686A Tan

Green 383

686A Tan

Green 383

686A Tan

Green 383

686A Tan

Green 383

686A Tan

Green 383

686A Tan

Polymer Beads

Polymer Beads

Silica Particles/Flake

Polymer Beads

Silica Particles/Flake

MIL-DTL-53039C

MIL-DTL-64159B I

Polymer Beads

Polymer Beads

Silica Particles/Flake

Polymer Beads

Silica Particles/Flake

Polymer Beads

Silica Particles/Flake

Silica Particles/Flake

MIL-DTL-64159B I

IV

I

MIL-DTL-53039D IV

II

I

MIL-DTL-53039C

MIL-DTL-53039C II

MIL-DTL-64159B I

MIL-DTL-64159A I

Hentzen

NCP

Sherwin Williams

Spectrum

MIL-DTL-64159A I

MIL-DTL-64159B I

MIL-DTL-53039D IV
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Tapes were used as received from the manufacturers. Table 2 summarizes the 

manufacturer and type of tape used in this work. 

Table 2: Tape Information

Manufacturer Product Name Adhesive Type Cost/roll

3M 250 Flatback Masking Tape Rubber ~$55

3M 396 Super Bond Polyester Film Tape Rubber Resin ~$13

Intertape LA-26 Polyester/Rope-Fiber Laminate Tape Thermosetting Rubber ~$16

SEMicro Cross Hatch Tape (CHT) Synthetic Rubber ~$35

An Instron model #8871 load frame mechanical test system was used to measure pull-off 

forces of the different tapes on various CARC surfaces. The Instron was equipped with a 

+/- 5kN dynamic load cell, a 90° panel clamping apparatus, and a pulling arm which 

gripped and performed the 180° tape pull. The Instron was connected to a personal 

computer (PC). This PC served as both digital controller and data logger. A picture of 

the experimental set-up is shown in Figure 2. The tape was pressed onto the CARC 

surface using an applicator in accordance with ASTM D3359. A suitable length of tape 

was used to cross the surface of the test panel and double back 180° up into the test 

fixture. A photo of this can be seen in Figure 3. Air bubbles were removed from the 

tape/surface interface by applying an even pressure with the backside of a plastic spoon 

until no air pockets could be seen. A common plastic spoon was selected and a limit of 10 

seconds was established to remove air pockets so as to make every application as 

consistent as possible and to establish an accommodating reference for future field 

applications. The tape covered sample was clamped into place on the panel mount at the

base of the Instron. After the test panel was properly secured, and tape attached to the 

tape pull apparatus, the tape was pulled from the surface over 25mm at a rate of 

125mm/s. A total of 18 pulls were collected for each coating specification, type, color, 

and vendor tested. All data was recorded utilizing the Instron WaveMatrix14 software 

suite and output to excel files. 
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Figure 2: Instron load frame, panel mount, and tape pull apparatus 

Figure 3: Close-up of panel mount and tape pull apparatus.

Panel Mount

Tape Pull Apparatus
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A Nexus 870 (Thermo-Nicolet) FTIR spectrophotometer was fitted with a Gateway ATR 

accessory (Specac). The accessory was allowed to purge with dry nitrogen for 10 

minutes prior to collecting a background spectrum of the ZnSe crystal that was mounted 

in the accessory. Tape was applied onto the crystal and air bubbles were removed with

finger pressure. The entire assembly was placed onto the ATR accessory through the 

sliding window in the FTIR sample compartment. The accessory compartment was 

purged with N2 for 10 min prior to collecting the spectrum. The spectra were the 

summation of 32 scans collected between 650 and 4000 cm-1at a 2 cm-1resolution. 

Advancing contact angles were measured using a Rame-Hart Model 290 Automated 

Contact Angle Goniometer. Water was used as the probe liquid and was purified before 

use to 18 MΩ cm using a Milipore water purification system. A droplet of water was 

placed on the surface and the volume of the water droplet was increased until the 3-phase 

contact line advanced. After an equilibrium angle was observed (i.e.- the drop edge 

stopped advancing), a measurement was recorded. Five drops were measured at random 

locations across the sample surfaces. 

Figure 4: Rame-Hart Model 290 Automated Contact Angle Goniometer
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Results and Discussion

Table 3: Average Pull-off Adhesion Strengths for Tapes on Hentzen Coatings

Green 383 686a Tan

Tape ID

3M 250 116.4343418 115.5536483

3M 396 209.9502469 131.2387126

CHT 75.30919954 98.0246156

LA-26 170.2137478 172.8680479

3M 250 118.3693817 142.2385995

3M 396 102.3657472 162.7249841

CHT 80.23762291 100.8733565

LA-26 165.0913277 193.604993

3M 250 143.5390277 137.2690834

3M 396 195.0037631 191.8542441

CHT 154.3933372 156.001803

LA-26 200.3762747 198.6664471

3M 250 131.3566168 136.2262631

3M 396 190.6538985 186.2936355

CHT 126.095947 122.2181742

LA-26 178.2005384 170.9017335

53039C TIV

53039C TI

64159B

64159A

Adhesive Torque (inch oz-F)
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Figure 5: Average Pull-off Strength across Hentzen Green 383 CARCs

Figure 6: Average Pull-off Strength across Hentzen 686A Tan CARCs
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All tapes tested met the established performance criteria of 80 inch ounce-force on all 

Hentzen coatings with the exception of Cross Hatch Tape over the Green 383 MIL-DTL64159A. This coating is a silacious flattened waterborne CARC which had an average 

adhesive strength of 75.3 inch ounce-force, though standard deviation would meet the 80 

inch ounce-force threshold. During testing it was noted that the CHT had issues with 

some adhesive residues left behind on the green silacious waterborne Hentzen coating, at 

first delaminating from the surface before the Instron was able to initiate the test. The 

baseline 3M 250 Flatback Masking Tape adhered similarly to each Hentzen coating. The 

3M 396 Super Bond Film Tape and the LA-26 Intertape had higher adhesion values than 

the baseline 3M 250 on each Hentzen coating with the exception of 3M 396 having a 

lower adhesion strength on the Green 383 Hentzen MIL-DTL-64159B beaded waterborne 

CARC. The CHT typically had the lowest adhesion strengths of all the tapes tested on 

the Hentzen coatings with the exception of the type I solvent-borne CARC.

Table 4: Average Pull-off Adhesion Strengths for Tapes on NCP Coatings

Green 383 686a Tan

Tape ID

3M 250 132.7503765 120.9349896

3M 396 158.3875335 195.7080301

CHT 192.4183165 173.1846228

LA-26 119.2778943 88.94703369

3M 250 125.0854736 99.3807805

3M 396 202.6268211 208.8347205

CHT 172.1919435 189.4485205

LA-26 115.1765149 120.2415306

3M 250 140.4451796 112.6309499

3M 396 144.2195001 155.3683186

CHT 177.3376463 163.4457609

LA-26 111.9850009 90.36489506

3M 250 98.90985427 83.13689632

3M 396 63.41534713 77.779158

CHT 106.9569749 91.40965219

LA-26 41.97781413 45.33741022

53039C TIV

53039C TI

64159B

64159A

Adhesive Torque (inch oz-F)
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Figure 7: Average Pull-off Strength across NCP Green 383 CARCs

Figure 8: Average Pull-off Strength across NCP 686A Tan CARCs
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All tapes tested met the established performance criteria of 80 ounce-force inch on all 

Hentzen beaded waterborne CARCs with the exception of 3M 396 and CHT. In the case 

of the 396 on the 686A Tan version of the beaded waterborne CARC, the standard 

deviation was greater than the margin by which the failure occurred. The standard 

deviation of the other failures mentioned above were less than the margin of failure. The 

396 adhered strongly to the other coatings in the matrix, occasionally in excess of 200 

inch ounce-force . The LA-26 adhered strongly to these other coatings as well, and 

performed adequately on the beaded waterborne CARCs. The baseline 3M 250 

performed similarly across all coatings, and with the lower end of standard deviation 

could have been considered a failure on the beaded waterborne CARCs.

Table 5: Average Pull-off Adhesion Strengths for Tapes on Sherwin Williams Coatings

Green 383 686a Tan

Tape ID

3M 250 121.924166 126.2662192

3M 396 143.1628696 121.4726765

CHT 99.86779499 92.92666367

LA-26 161.7851218 154.8465372

3M 250 98.1758155 86.83773152

3M 396 68.95000138 52.87354516

CHT 27.07132894 13.84469814

LA-26 125.8186814 129.0627346

3M 250 144.8774794 129.4325893

3M 396 188.2608935 160.4740078

CHT 137.1784956 114.8251067

LA-26 183.5808988 138.7905794

3M 250 128.1307735 119.04685

3M 396 152.6848133 149.5709988

CHT 110.9296079 104.1712998

LA-26 149.5745858 138.7905794

53039C TIV

53039C TI

64159B

64159A

Adhesive Torque (inch oz-F)
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Figure 9: Average Pull-off Strength across Sherwin Williams 383 Green CARCs

Figure 10: Average Pull-off Strength across Sherwin Williams 383 Green CARCs
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The baseline 3M 250 met and exceeded the established performance criteria of 80 inch 

ounce-force on each of the Sherwin Williams coatings, as did the LA-26. The 396 and 

CHT met/exceeded 80 inch ounce-force on each of the Sherwin Williams coatings except 

for the beaded waterborne CARCs. The standard deviations do not exceed the margin of 

failure in the case of either the 396 or the CHT.

Table 6: Average Pull-off Adhesion Strengths for Tapes on Spectrum Coatings

Green 383 686a Tan

3M 250 126.12747 134.24676

3M 396 98.256272 77.959094

CHT 73.289886 62.05658

LA-26 165.85749 171.37503

Figure 11: Average Pull-off Adhesion Strength across Spectrum 64159B CARCs
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Table 7: Water Break Test Results

Figure 12: Example of Failed Water Break Test (Top) and Passed Water Break Test 

(Bottom)
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The water break testing was done by running DI water over the test panels after the tape 

testing had been completed. For the purposes of this test, water that beaded up over the 

areas where tape had been applied to the surface was considered a failure and can be seen 

on the upper panel in Figure 11. The lower panel in Figure 11 in which you can see the 

water evenly spread out over the panel surface is an example of a pass. The instances in 

which failure occurs are attributed to adhesive residue left on the surface of the panel. 

These results could affect field application whereby these tapes would be used for 

masking during painting operations. There were few failures in the water break testing 

and were limited to LA-26 over Sherwin Williams’ silacious waterborne CARCs, 396 

over Hentzen’s silacious waterborne (green only), every tape over Hentzen’s silacious 

solvent-borne, 396 over Hentzen’s beaded solventborne, and every tape over NCP’s 

53039D beaded solventborne (tan only).

Surface properties such as roughness, chemical composition, and homogeneity are well 

known to influence the wettability of surfaces. CARC topcoats used by the Army can 

exhibit a wide range of surface properties that result from subtle differences in 

formulation,, from variations in application parameters, and even ambient conditions, 

andGenerally, systems formulated to be water dispersible produced films that were 

slightly hydrophilic (water contact angle < 90°) whereas systems formulated with organic 

solvents that are not miscible with water cured to yield polymer films that were 

hydrophobic (water contact angle > 90°) (Table 8). 

Table 8: Average water contact angle of various CARC systems.

advancing contact angle of water (degrees)

waterborne polyurethane solventborne polyurethane

silica extender 80 +/- 5 112 +/- 8

polymeric bead extender 79 +/- 9 106 +/- 4

The results in Table 8 also suggest that the type of extender has little or no impact on the 

wettability of the virgin polyurethane surfaces. A comparison of wetability for 686 tan

and 383 green pigmented polyurethane coated samples obtained from several different 

vendors is shown in figure 12. 
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0

2 0

4 0

6 0

8 0

100

120

140

Waterborne Silicaceous Waterborne Beaded Solventborne Silaceous Solventborne Beaded advancing water contact angle

type of polyurethane topcoat 

green Hentzen tan Hentzen

green Sherwin Williams tan Sherwin Williams

green NCP tan NCP

green Spectrum tan spectrum

Figure 13: Advancing water contact angles of polyurethane topcoats formulated in tan 

and green from four different vendors.

There is little or no difference in the water contact angle measured on samples differing 

only in pigment composition. Although this observation suggests that pigment does not 

affect surface properties, additives used to disperse the pigments and extenders may 

preferentially migrate to the surface of the coating. Similarly, surfactants utilized for 

increasing the solubility of urethane precursors in waterborne formulations may reside at 

the surface preferentially. A more detailed and systematic study on a model system 

should provide clarity regarding surface segregation of particular additives used in 

formulation. Our research clearly shows waterborne polyurethanes have lower contact 

angles (higher surface free energies) than their solvent borne counterparts. 

The relationship between wettability and work of adhesion is described by the YoungDupré equation:

WSVL = γLV(1 + cos θ), (1) 

where WSVL is commonly referred to as the work of adhesion, γLV is the interfacial free 

energy at the liquid-vapor interface, and θ is the contact angle at the three-phase contact 

line. From this equation we expect the work of adhesion between a liquid and solid to 

decrease as the contact angle increases as shown in Figure 13.

15

 
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0 2 0 4 0 6 0 8 0 100 120 140 160 180 Inceasing Work of Adhesion (arbitrary units)

θ (deg)

Figure 14: Theoretical behavior of the work of adhesion with respect to contact angle 

based on the Young-Dupré equation.

Extending this expected behavior to a solid-solid system such as an 

elastomer/polyurethane interface is more complicated. The Johnson-Kendall-Roberts 

(JKR)16 and the Derjaguin-Muller-Toporov (DMT)1718 theories are typically used to 

describe the work of adhesion for polymer-solid systems. Although these relationships 

will be useful in fundamental studies that model our system, they are beyond the scope of 

this report and are mentioned here to highlight the relationship between work of 

adhesion, pull-off-force, and contact angle. In our research the lack of a clear correlation 

between contact angle and pull-off strength is most likely due to the complexity of the 

systems studied. 

Attenuated total reflectance-fourier transform infrared spectroscopy was used to identify 

chemical differences in the adhesive of the tapes used for pull-off tests. Figure 14 shows 

the region of the spectrum where –CH , –OH, and -NH stretching vibrations occur. Small 

stretches observed at ~3280 cm-1for the adhesive on the 3M® 250 tape and 3330 cm-1for 

the LA-26 tape indicate –OH or –NH groups within the adhesive or adsorbed water. 

Hydroxyl, amine, or amide functionality within an adhesive can hydrogen bond with free 

chain ends of the urethane and with the oxide surfaces of pigment particles and hydroxyl

groups may have enough mobility to chemically react with any residual isocyanate 

groups present at the polyurethane surface. The likelihood that these hydroxyl groups 

would contribute significantly to tape pull-off forces is low due to the relatively low 
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intensity of the normally strong –OH stretch. It is common, however, for –NH groups of 

secondary amines to be quite weak. Other evidence that supports the presence of –NH 

groups is seen in figure IRB (vide infra). Evidence for the presence of vinyl groups in all 

of the tape samples analyzed is seen by the –CH stretch just above 3000cm-1. Although 

vinyl functionality may contribute to an increase in the overall adhesion to a substrate 

that contains thiol groups, the low intensity of this stretch complicated quantification of 

the differences in –C=C concentration between the various tapes. 

4000 3800 3600 3400 3200 3000 2800 2600 2400 2200 2000 1800 intensity (arbitrary units)

cm-1

250

CHT

396

LA-2 6

Figure 15: ATR-FTIR spectra of various tapes in the region of 4000-1800 cm-1

Spectra from 650 – 2000 cm-1for of each tape are seen in figure 15. Once again 

there is evidence that the 3M® 250 and the LA-26 tape contain chemical functional 

groups consistent with hydrogen bonding groups such as the – NH bend of an amide 

(~1585 cm-1), an amine (1218 and 1236 cm-1) for LA-26 and 3M® 250 respectively, and 

a strong stretch at 911 (3M® 250) and a weaker one at 918 cm-1

(LA-26) that is indicative 

of the double bond of an acrylate functional group. Several smaller peaks are present in 

spectra of the tapes that are difficult to confidently assign functionality to without 

complementary analytical techniques. 
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1850 1650 1450 1250 1050 850 650 intensity (arbitrary units)

cm-1

250

CHT

396

LA-2 6

Figure 16: ATR-FTIR spectra of various tapes in the region of 650-1950 cm-1

Conclusions

1) Waterborne formulations have lower advancing contact angles (higher surface 

free eneries) than solvent borne counterparts. 

2) There is no clear difference in the wettability of CARC that contains 

polymeric beads and a CARC system that contains silica as an extender. The 

caveat here is that each system has unique additives (dispersants, surfactants, 

solvents) that allow for a final film with specific properties and these variables 

may be the underlying cause of the similarities in contact angles.

3) Green and tan pigments do not affect the wettablilty of the cured film. The 

same caveat that is described in #2 applies here.

4) Tapes that contain functional groups such as hydroxyl, amine, amide, or vinyl 

typically correlate with higher pull off forces on most samples. 

5) A more fundamental study is needed to develop a more fundamental 

understanding.
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References

 

1 MIL-DTL-53072. Chemical Agent Resistant Coating (CARC) System Application 

Procedures And Quality Control Inspection. 2003

2 ASTM D3359-09e2. “Standard Test Methods for Measuring Adhesion by Tape Test”. 

Annu. Book ASTM Stand. 2009.

3 AR-750-1. “Army Materiel Maintenance Policy”. Army Regulations. 2007.

4

J. Adams and G. Somerville, telephone conversation with author, December 2009

5

J. Mort, telephone conversation with author, December 2010

6

 M. Flory, telephone conversation with author, May 2010

7

L. Knisley, telephone conversation with author, December 2010

8

P. Do, telephone conversation with author, December 2010

9 B. Tucker, telephone conversation with author, December 2010

10 T. Tuttle, telephone conversation with author, December 2010

11 FED-STD-595/34094. Colors Used in Government Procurement/Green, Flat or 

Lusterless. 1984.

12 FED-STD-595/33446. Colors Used in Government Procurement/Yellow, Flat or 

Lusterless. 1984.

13 ASTM D3330/D3330M-04(2010). “Standard Test Method for Peel Adhesion of 

Pressure-Sensitive Tape”. Aunnu. Book ASTM Stand. 2010.

14 Wave Matrix. Computer software. WaveMatrix Dynamic Testing Software. Vers. 

1.3.232.

15 Frederick M. Fowkes. Contact Angle, Wettability, and Adhesion, Volume 43

AMERICAN CHEMICAL SOCIETY, 1964.

16 K. L. Johnson and K. Kendall and A. D. Roberts, Surface energy and the contact of 

elastic solids, Proc. R. Soc. London A 324 (1971) 301-313
MFPT 2014 Proceedings

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17 Derjaguin, BV and Muller, VM and Toporov, Y.P., 1975, Effect of contact 

deformations on the adhesion of particles, Journal of Colloid and Interface Science, 

53(2), pp. 314-326

18 Muller, VM and Derjaguin, BV and Toporov, Y.P., 1983, On two methods of 

calculation of the force of sticking of an elastic sphere to a rigid plane, Colloids and 

Surfaces, 7(3), pp. 251-259.
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