Bond Process Qualification Protocols &

Adhesive Qualification Guidance for

Aircraft Design and Certification

2018 Technical Review

Waruna Seneviratne, John Tomblin, and Upul Palliyaguru
 Bond Process Qualification Protocols & Adhesive Qualification
Guidance for Aircraft Design and Certification
• Principal Investigators & Researchers
• John Tomblin, PhD, and Waruna Seneviratne, PhD

• Upul Palliyaguru, Anushi Amaranayake, and Tammy Nguyen

• FAA Technical Monitor

• Ahmet Oztekin

• Other FAA/CMH-17 Personnel Involved

• Larry Ilcewicz, PhD, Cindy Ashforth, and Curtis Davies,
• DoD & Industry Participation
• AFRL, Boeing, Bell Helicopter, Henkel, Honda Aircraft Co., Lockheed Martin, MMM, MTech Engineering
Services, NAVAIR, Solvey Industries , Textron Aviation, Boom Aerospace

2
 Road Map - Adhesive Qualification Guidance

• Adhesive Characterization Qualification (ACQ)

• Develop test matrices
• Bulk physical, chemical, and mechanical test matrices Qualify
Substrate &
Surface Prep
Qualify
Adhesive &
Bond Process

• Adhesive (joint) mechanical tests

Statistical
Bonding System
Qualification

•
Analysis

Fluid sensitivity Allowables Database Structural Bonding

•
Qualified Bonding System Structural Application
- Adhesive Guidelines/Data - Adhesive

Equivalency tests - Process

- Substrate
- Surface Prep
(CMH-17) - Process
- Substrate
- Surface Prep

• Develop databases Process

No

• Select adhesive bond systems Yes

•
Qualify New
Substrate No Bonding

Inclusion to CMH-17 data review group Yes

System

No
Surface Prep

Yes

3
 Road Map - Adhesive Qualification Guidance
Development of NCAMP Specifications
Guidelines and Recommended Criteria
Guideline Document
for the Development of Material/
(FAA Report) Process Specifications for Adhesive

Adhesive Process Control Document (PCD)

Adhesive NRP 102
Preparation and Maintenance Guide

Qualified Product List

NMS 300/1 (QPL)
Solvey FM300-2
FM300-2M 0.06 psf • NMS 300/1
NCAMP Material • NMS 394/1
Specification (NMS) • ...
NMS 394/1
Loctite EA9394
EA 9394 AERO

FAA Special Project Material Specifications

Codes (SPC)

Solvey FM300-2
Fabrication of
Development of NCAMP Test Plans NCAMP Process bulk and
Specification (NPS) mechanical
test panels
Authorized Inspection Loctite EA9394
Solvey FM300-2 Representative (AIR)
Process Specifications
Authorized Engineering
NCAMP Test Plan
Representative (AER) Conformity
(NTP)
Loctite EA9394 Data Collection
Templates (PMC)
Test Plans

Material Property
Data Report
Statistical Analysis
Report

4
 Development of NCAMP Specifications, Test Plans & Guidelines

• Adhesive System 1 – FM300-2M (Film Adhesive)

• NCAMP Material Specification (Base) – NMS300
• NCAMP Material Specification (Slash) – NMS300/1
• NCAMP Process Specifications - NPS 83002
• NCAMP Test Plan - NTP AC-3002Q1
• Adhesive System 2 – EA9394 bare (Paste Adhesive)
• NCAMP Material Specification (Base) – NMS394
• NCAMP Material Specification (Slash) – NMS394/1
• NCAMP Process Specifications - NPS 89394
• NCAMP Test Plan - NTP AC-9394Q1

• Adhesive Process Control Document (PCD) – NRP 105

• NCAMP - Adhesive Data Collection Forms

5
 NCAMP Material Specifications
Summary of documents -> NMS 300 (Base)
250°F Cure High Temperature and High Toughness Structural Film Adhesive
Uncured adhesive physical and chemical properties
• Covers Solvay FM300-2 types Property
Product
Form Test Standard
# of
Replicates
• Carrier material types HPLC
FTIR
Uncured
Uncured
SACMA SRM 20R-94
ASTM E-168 ASTM E-1252
3 per Batch
3 per Batch
• Type K – Wide open knit Viscosity & Gel Time Uncured ASTM D4473 3 per Batch

• Type M – Random mat

Resin Flow
Volatile Content
Uncured
Uncured
ASTM D3531
ASTM D3530
3 per Batch
3 per Batch

• Type U – Unsupported film Cured adhesive physical and thermal properties

Product
• Nominal weights
Property
Cured Panel Thickness
Form
Cured
Test Standard
SACMA SRM 10R-94
# of Replicates
10 per Panel
• 0.10 psf Tg
Density
Cured
Cured
ASTM D7028
ASTM D792 Method A
3 per Batch
3 per Batch
• 0.08 psf Thermal Conductivity &
Thermal Diffusivity
Cured
Cured
ASTM E1952
ASTM E1530
3 per Batch
3 per Batch
• 0.06 psf Cured adhesive mechanical properties
• 0.03 psf Property
Test
Test Method # of Replicates
•
Temperature
Changes to the qualified materials T e n sio n S tre n g th & M o d u lu s RT A S T M D 6 38 5

• Tests performed on adhesive C o m p re ssio n S tre n g th a n d

M o d u lu s
RT ASTM D 695 5

S h e a r S tre n g th a n d M o d u lu s RT A S T M D 38 46 5

6
 NCAMP Material Specifications
Summary of documents -> NMS 394 (Base)
150°F Cure High Temperature and High Toughness Structural Paste Adhesive
Uncured adhesive physical and chemical properties
• Covers Henkel EA9394 types Property
Product
Form Test Standard
# of
Replicates

• Bondline Control Mechanisms

HPLC
FTIR
Uncured
Uncured
SACMA SRM 20R-94
ASTM E-168 ASTM E-1252
3 per Batch
3 per Batch

• EA9394.3 -0.005 Glass beads

Viscosity & Gel Time
Resin Flow
Uncured
Uncured
ASTM D4473
ASTM D3531
3 per Batch
3 per Batch
Volatile Content Uncured ASTM D3530 3 per Batch
• Adhesive variations weights Cured adhesive physical and thermal properties
Product
• EA 9394
Property
Cured Panel Thickness
Form
Cured
Test Standard
SACMA SRM 10R-94
# of Replicates
10 per Panel
• EA 9394/C-2 Tg
Density
Cured
Cured
ASTM D7028
ASTM D792 Method A
3 per Batch
3 per Batch
• EA 9394.2 Thermal Conductivity
& Thermal Diffusivity
Cured
Cured
ASTM E1952
ASTM E1530
3 per Batch
3 per Batch
• Changes to the qualified materials Cured adhesive mechanical properties
Test # of
• Tests performed on adhesive
Property
Temperature
Test Method
Replicates

Tension Strength &

RT ASTM D638 5
Modulus
Compression Strength
RT ASTM D695 5
and Modulus
Shear Strength and
RT ASTM D3846 5
Modulus 7
 NCAMP Material Specifications
Summary of document -> NMS 300 (Base)
250°F Cure High Temperature and High Toughness Structural Film Adhesive

• Storage and Handling Requirements

• General requirements
• Adhesive life requirements
• Safety requirements
• Quality Assurance
• Classification of tests and Inspections
• Receiving inspections
• Delivery of Materials
• Packaging
• Shipping Requirements
• Material Rejection

8
 NCAMP Material Specifications
Summary of document -> NMS 300/1 (Slash)
(Solvay FM300-2M – 0.06psf)
Cured bulk adhesive mechanical properties
• QPL - Solvay FM300-2M – 0.06psf Number
Test of
• Technical Requirements Property Temperature Test Method1
Replicate
s
Requirements

Tension Strength &

Uncured adhesive physical and chemical properties Modulus RT ASTM D638 5 TBD
Product # of Replicates Compression Strength
Property Form Test Standard1 (Every roll) Requirements and Modulus RT ASTM D695 5 TBD
SACMA SRM Shear Strength and
HPLC Uncured 20R-94 3 TBD Modulus RT ASTM D3846 5 TBD

ASTM E168
FTIR Uncured ASTM E1252 3 TBD

Viscosity & Gel Adhesive mechanical properties

Time Uncured ASTM D4473 3 TBD
Minimum Average –575%; Number
Resin Flow Uncured ASTM D2183 3 Ind. Min 540.5% Test Test of
Property Temperature Method1 Requirements
Volatile Replicates
Content Uncured ASTM D3530 3
Average maximum –1%
Lap Shear ASTM Minimum Average 4850 psi; Ind.
Strength RT D1002 5 Min 4559 psi

Flatwise Tensile ASTM Minimum Average 892 psi; Ind.

Strength RT D897 5 Min 838 psi

ASTM Minimum Average 31 in-lb/in

Peel Strength RT D3167 5 psi; Ind. Min 29 in-lb/in
9
 NCAMP Material Specifications
Summary of document -> NMS 394/1 (Slash)
(Henkel EA9394 bare)
Cured bulk adhesive mechanical properties
• QPL - Henkel EA9394 bare Test
Number
of
Temperatur
• Technical Requirements
Property
e
Test Method1 Replicate
s
Requirements

Tension Strength & Minimum Average 6675 psi;

RT ASTM 638 5
Uncured adhesive physical and chemical properties Modulus Ind. Min 6274 psi
Compression
# of Strength and Minimum Average 10000 psi;
Product RT ASTM D695 5 Ind. Min 9400 psi
Property Test Standard1 Replicates Requirements Modulus
Form (Every roll)
Shear Strength and
SACMA SRM 20R- Modulus RT ASTM D3846 5 TBD
HPLC Uncured 94 3 TBD

ASTM E 168
FTIR Uncured 3 TBD
ASTM E 1252 Adhesive mechanical properties
Viscosity & Gel Minimum Average = 160 Pa·S Ind. Test Test Number of
Time Uncured ASTM D4473 3 Avg =150 Pa.S Property Temperature Method1 Replicates Requirements
Resin Flow Uncured ASTM D2183 3 TBD
Volatile Content Uncured ASTM D3530-97 3 TBD Lap Shear ASTM Minimum Average 4850 psi; Ind.
Strength RT D1002 5 Min 4559 psi

Flatwise Tensile Minimum Average 892 psi; Ind.

Strength RT ASTM D897 5 Min 838 psi

ASTM Minimum Average 31 in-lb/in psi;

Peel Strength RT D3167 5 Ind. Min 29 in-lb/in

10
 NCAMP Process Specifications
Summary of document -> NPS 83002
Fabrication of NMS 300 Qualification, Equivalency and Acceptance Test Panels
• Materials used for bonded panel fabrication
• Adhesive preparation
• Substrate preparation
• Aluminum (Al2024 T3) – PAA (ASTM D3933) + BR 127
• Pre-bond measurements
• Thickness
• Surface roughness
• Primer thickness
• Composite (Epoxyglass G10) – 120 grit sanding + water break test + cleaning
• Pre-bond measurements
• Thickness
• Surface roughness

11
 NCAMP Process Specifications
Summary of document -> NPS 83002
Fabrication of NMS 300 Qualification, Equivalency and Acceptance Test Panels
• Fabrication/Bonding of mechanical test panels
• Bonding of panels with a lap area
• Bonding of panels without a lap area (Full surface bond)
• Bonding of panels with a disbond

• Fabrication of bulk adhesive panels

• Bagging Scheme
• Cure Cycle –250°F for 90 minutes with 40 psi pressure.
• Quality control
• Visual inspection
• TTU c-scan 30 0 30 0

Vacuum/Pressure [psi]
Temperature [°F]

20 0 20 0
10 0 10 0
0 0
-10 0 -10 0
0 10 0 20 0 30 0
Time [min]

Va cuu m Tem per atu re Press ure 12

 NCAMP Test Plan
Summary of document -> NTP AC-3002Q1
Adhesive Property Data Acquisition and Qualification Test Plan for Solvay FM300-2M 0.06psf
• Nomenclature for specimen identification
• Physical, Chemical and Thermal tests performed on adhesive

Uncured adhesive physical and chemical properties

Cured adhesive physical and thermal properties
Min Replicates
Product Min Replicates
Property Test Standard per
Form Property Product Form Test Standard per
batch
HPLC Uncured SACMA SRM 20R-94 3 batch
FTIR Uncured ASTM-E168 & ASTM-E1252 3 Tg Cured ASTM D7028 3
Viscosity & Gel Time Uncured ASTM D4473 3 Density Cured ASTM D792 Method A 3
Resin Flow Uncured ASTM D2183 3 Thermal Conductivity & Cured ASTM E1952 3
Volatile Content Uncured ASTM D3530 3 Thermal Diffusivity Cured ASTM E1530 3

13
 NCAMP Test Plan
Summary of document -> NTP AC-3002Q1
Adhesive Property Data Acquisition and Qualification Test Plan for Solvay FM300-2M 0.06psf
• Adhesive Mechanical Property Testing
• Test Environments -> CTD (-65F), RTD (70F), ETD (180F Dry), and ETW (180F Wet)
• Dry – as fabricated moisture content
• Wet – specimens conditioned at 145°F/85%RH for 1000 hrs. (FM300-2M)
• Specimen distribution methodology

14
 NCAMP Test Plan
Summary of document -> NTP AC-3002Q1
Adhesive Property Data Acquisition and Qualification Test Plan for Solvay FM300-2M 0.06psf
• Adhesive Mechanical Property Testing
• Test Matrix
Test
Number of Batches x No. of Panels x No.
Test of Specimens
Test Description Standar Property
Code Test Temperature/Moisture Condition
d
CTD RTD ETD ETW
Thin Metal Adherend SLS – ASTM
Strength 3x2x3 3x2x3 1x2x3 3x2x3
Single Lap Shear MThin D1002
Thick Metal Adherend SLS - ASTM Strength and
1x2x3 1x2x3 1x2x3 1x2x3
Single Lap Shear MThick D5656 Modulus
Thin Laminate
SLS - ASTM
Adherend Single Lap Strength 3x2x3 3x2x3 1x2x3 3x2x3
CThin D3165
Shear
Mode I Fracture ASTM Fracture
M-I 1x2x3 1x2x3 1x2x3 1x2x3
Toughness D3433 Toughness Gic
Mode II Fracture ASTM Fracture
M-II 1x2x3 1x2x3 1x2x3 1x2x3
Toughness D7905 Toughness Giic
ASTM
Floating Roller Peel FRP Peel Load 3x2x3 3x2x3 1x2x3 3x2x3
D3167
ASTM
Flatwise Tensile FWT Strength 3x2x3 3x2x3 1x2x3 3x2x3
D897

15
 NCAMP Test Plan
Summary of document -> NTP AC-3002Q1
Adhesive Property Data Acquisition and Qualification Test Plan for Solvay FM300-2M 0.06psf
• Adhesive Mechanical Property Testing – Fluid Sensitivity
• Test Matrix

Test
Extended Contact: Exposure Code
Condition
30 days min. @ 70°F±10°F 70°F FS11RT
SAE AMS 2629 Jet Reference Fluid
30 days min. @ 70°F±10°F 180°F FS11ET
30 days min. @ 70°F±10°F 70°F FS12RT
MIL-PRF-5606 Hydraulic Oil
30 days min. @ 70°F±10°F 180°F FS12ET
30 days min. @ 70°F±10°F 70°F FS13RT
Sea Water (ASTM D1141 or equiv.)
30 days min. @ 70°F±10°F 180°F FS13ET
30 days min. @ 70°F±10°F 70°F FS14RT
Skydrol LD-4 (SAE AS1241, Type IV, Class 1)
30 days min. @ 70°F±10°F 180°F FS14ET
Short Duration Contact:
90 minutes min. @ 70°F±10°F 70°F FS21RT
MEK washing fluid. ASTM D740
90 minutes min. @ 70°F±10°F 180°F FS21ET
Control Tests:
1000 hrs. at 145°F±5°F /85%±5%
70°F
RH FS31RT
85% Relative Humidity
1000 hrs. at 145°F±5°F /85%±5%
180°F
RH FS31ET

16
 Preliminary Test Results
EA 9394 – D1002 – Property Value – Shear Strength (ksi)
Batch A
Cure Cycle 1 Cure Cycle 2

Higher % of Cohesive / Adhesive

17
 Preliminary Test Results
EA 9394 – D3165 – Property Value – Shear Strength (ksi)
Batch A
Cure Cycle 1 Cure Cycle 2

Adhesive Failure Adhesive Failure

18
 Preliminary Test Results
EA 9394 – D3167 – Property Value – Peel Load (lbf)

Batch A
Cure Cycle 1 Cure Cycle 2

Adhesive Failure Adhesive Failure

19
 Preliminary Test Results
EA 9394 – D3433 – Property Value – Fracture Toughness (lbf/in)

Batch A

Cure Cycle 1 Cure Cycle 2

Cohesive Failure Cohesive Failure

20
 Preliminary Test Results
EA 9394 – D5656 (T1) – Property Value – Shear Strength (ksi)
T1
Batch A
Cure Cycle 1 Cure Cycle 2

Cohesive / Adhesive

21
 Preliminary Test Results
EA 9394 – D5656 (T2) – Property Value – Shear Strength (ksi)
T2
Batch A
Cure Cycle 1 Cure Cycle 2

Cohesive / Adhesive

22
 Shear Strength (ksi)

0.0
0.5
1.0
1.5
2.0
2.5
3.0
3.5
4.0
4.5

SA Ba
EA se
M il ne
S2
629
Jet
M Re
IL- f ere
PR n ce…
F-5
60
6 Hy
dr
Se aul
aW ic
Oi
at e l
r (A
ST
M
D1
Sk 14
yd 1
r ol or…
L D-
4
Fluid Sensitivity
(SA
E
AS
M 124
EK
wa 1, …
sh
i ng
fl u
id .
Preliminary Test Results

AS
T M…
M
oi s
RT

t ure
C on
di t
i on
ET
EA 9394 – D1002 – Fluid Sensitivity Test Results

23
 Current Status
EA 9394 FM300-2M
EA9394 FM300-2M
Test Test
Property Test Method Batch A Batch B Batch C Property Test Method Batch A Batch B Batch C
Environment Environment
C1 C2 C1 C2 C1 C2
C1 C2 C1 C2 C1 C2
CTD 3 3 3 3 3 3
Thin Metal CTD 3 3 3 3 3 3
Adherend D1002
ETD 3 3 Thin Metal
ETW 3 3 3 3 3 3 ETD 3 3
Lap Shear Adherend D1002
RTD 3 3 3 3 3 3 ETW 3 3 3 3 3 3
Lap Shear
CTD 3 3 RTD 3 3 3 3 3 3
Thick Metal
ETD 3 3 CTD 3 3
Adherend D5656 (T1) Thick Metal
ETW 3 3 ETD 3 3
Lap Shear Adherend D5656
RTD 3 3 ETW 3 3
CTD 3 3 Lap Shear
Thick Metal RTD 3 3
ETD 3 3
Adherend D5656 (T2) CTD 3 3 3 3 3 3
Lap Shear
ETW 3 3 Composite
RTD 3 3
ETD 3 3
Adherend D3165
CTD 3 3 3 3 3 3 ETW 3 3 3 3 3 3 Waiting on Adhesive Batch
Composite Lap Shear
ETD 3 3 RTD 3 3 3 3 3 3 Specimen/Panel Bonding in Progress
Adherend D3165
ETW 3 3 3 3 3 3 CTD 3 3 Specimen Machining in Progress
Lap Shear Mode I
RTD 3 3 3 3 3 3 ETD 3 3
CTD 3 3 Fracture D3433 Conditioning in Progress
Mode I ETW 3 3
ETD 3 3 Toughness Testing in Progress
Fracture D3433 RTD 3 3
Toughness
ETW 3 3
CTD 3 3 Testing Complete
RTD 3 3 Mode II
CTD 3 3 ETD 3 3
Mode II Fracture D7905
ETD 3 3 ETW 3 3
Fracture D7905 Toughness
ETW 3 3 RTD 3 3
Toughness
RTD 3 3 CTD 3 3 3 3 3 3
CTD 3 3 3 3 3 3 Floating ETD 3 3
Floating ETD 3 3 D3167
D3167 Roller Peel ETW 3 3 3 3 3 3
Roller Peel ETW 3 3 3 3 3 3 RTD 3 3 3 3 3 3
RTD 3 3 3 3 3 3
CTD 3 3
CTD 3 3 3 3 3 3
Flatwise ETD 3 3
Flatwise ETD 3 3 D897
D897 Tensile ETW 3 3
Tensile ETW 3 3 3 3 3 3
RTD 3 3 3 3 3 3 RTD 3 3 3 3 3 3
Fluid ET 30 Fluid ET 30
D1002FS D1002FS
Sensitivity RT 30 Sensitivity RT 30

24
 Look Forward

• Future Activities
• Generate the B-Basis allowable for EA9394 and FM300-2M material systems
• Focus on performing equivalency on adhesive materials.
• Analyze failure modes for different test environments and report them accordingly
• Benefit to the Aviation Community
• Guidance on test matrices for mechanical, physical and chemical characterization of adhesives
• Generate adhesive material databases under NCAMP protocols that can be used for a wide variety
of applications be different end users

25
 Bond Process Qualification Protocols - Road Map

• Bond Process Qualification (BPQ) Qualify

Substrate &
Surface Prep
Qualify
Adhesive &
Bond Process

•
Bonding System
Qualification

Develop an acceptance criteria Statistical

Analysis

• Requirements (based on information in AC’s and FAR’s , etc.) Allowables Database Structural Bonding

•
Qualified Bonding System Structural Application
- Adhesive Guidelines/Data - Adhesive

Applicability of existing standards and/or develop new - Process

- Substrate
- Surface Prep
(CMH-17) - Process
- Substrate
- Surface Prep

standards
•
Process
No

Select known bond system failures Yes

• Simulate and investigate the BPQ methodology flags the Substrate No

Qualify New
Bonding
System

“bad” bonds Yes

• Develop protocols
Surface Prep

Yes
No

• Quantify process reliability

• Assess repeatability/maturity

26
 Bond Process Qualification (Critical Factors)
Bond Process Qualification
[Critical Factors]

Substrate Adhesive

Metal Composites Material Batch Variability Process Variability History Quality

Shelf life Tg
Storage life Viscosity
Outtime

Material & Process

Type Surface Preparation Surface Preparation Variability Paste Film
(Material Qualification)

Plasma (Ionized Gas)

Degreasing Abrasion Chemical Treatment Grit Blasting Hand Sanding Peel-Ply Removal
Treatment
Mixing
Adhesive Application Bondline Thickness Control Cure Environment Effects of Defects
(for Paste)
Can be combined
Tolerances Multiple Cure Options Temperature
Vacuum or not Tooling Humidity
Mixing Technique CTE Mismatch Field Repair Conditions
Primer Temperature Controls
Ramp Rate(s)
Pressure
Open Time
Pre-Bond Surface Characterization Application Method
(ex., Amine Blush)

Application side(s)

• Substrate type
Applicator
Sessile Drop Contact Angle X-Ray Photoelectron Fourier Transform IR Preheat Substrate
(CA) Spectroscopy Spectroscopy (FTIR) Preheat Adhesive
Adhesive Fillets

• Metal Paste Film

• Composite
• Adhesive types Pre-Mixed Glass Beads
Glass Bead Mixing into
Adhesive Mix

• Film
Applicator Mix Ratio Unsupported
Mixing Technique

• Paste
Micro Beads Mixed into
Scrim Cloth Knit Random Mat
Adhesive

27
 Summary of Activities

• Current Activities
• Task 1 – Substrate and adhesive compatibility
• Task 2 – Use of peel ply for composite substrate preparation
• Completed Activities
• Effects of Mix-ratio in two part paste adhesives
• Evaluation of assembly time in paste adhesives
• Amine blush effects
• Fluid Sensitivity of adhesive
• Efficient adhesive screening method testing.

28
Qualification of a Bond Process
Substrate Adhesive Substrate Surface Bonding
System Preparation Process/Curing

1. Composite 1. Paste 1. Abrasion 1. Cure Cycle –

2. Metal 2. Film 1. Grid Blasting Compatibility with
2. Hand Sanding Substrate
2. Peel Ply 2. Vacuum or Pressure
1. Nylon 3. Bondline Control
2. Polyester 4. Assembly Time
3. Chemical 5. Adhesive Preparation
1. PAA + Priming 6. Environment
4. Other 7. Bond Configuration –
1. Plasma Treatment Co-bond/Secondary
bond

29
Qualification of a Bond Process
Task 1

Substrate Adhesive Substrate Surface Bonding

System Preparation Process/Curing

1. Composite 1. Paste 1. Abrasion 1. Cure Cycle –

2. Metal 2. Film 1. Grid Blasting Compatibility with
Task 2 2. Hand Sanding Substrate
2. Peel Ply 2. Vacuum or Pressure
1. Nylon 3. Bondline Control
2. Polyester 4. Assembly Time
3. Chemical 5. Adhesive Preparation
1. PAA + Priming 6. Environment
4. Other 7. Bond Configuration –
1. Plasma Treatment Co-bond/Secondary
bond

30
 Task 1 –Qualification of a Bond Process – Substrate and Adhesive
Compatibility - Background and Goals
• When using bonded joints for primary or secondary structure applications, there is a wide variety of substrates and
adhesive materials that are available for use. Providing Guidance on selecting a compatible substrate and a
adhesive combination is important for designers.
• Main factors to consider during adhesive and substrate selection are the mechanical property requirements,
physical compatibility of the substrates (hybrid and non-hybrid) and adhesives for bonding, thermal compatibility
of the bond system during the bonding process and service life.
• Objective of this task is to provide establish a set of guidelines to use when selecting an adhesive and substrate
combination for a given bond process.

Goal – Develop guidelines on how to select compatible substrate and adhesive combinations to obtain a robust
bond system

32
 Task 1 - Qualification of a Bond Process – Substrate and Adhesive
Compatibility
Substrate Adhesive Substrate Surface Bonding
System Preparation Process/Curing

Compatibility

Mechanical Physical Thermal

1. Material allowable properties 1. Surface Characterization 1. CTE Mism atch
1. Substrate data -> NCAMP 1. Surface roughness 2. Glass Transition
2. Adhesive data -> NCAMP (in 2. Surface energy/ Contact angle 3. Cure Cycle Com patibility
progress) 3. Wettability envelope 1. Secondary bond
2. Joint m echanical capability
2. Co-bonded
1. Static
2. Durability

33
 Task 1 - Substrate and Adhesive Compatibility
• Substrates • Adhesives • Surface Preparation Methods
• Carbon Fiber Composites • Paste Adhesives • Carbon fiber composites
• Henkel EA9394 • As fabricated – MEK wipe only
• UNI – T800/3900-2
• Peel ply only
• PW - T300/3900-2 • Henkel EA9390
• Peel ply + Light abrasion (180 grit)
• Glass Fiber Composites • Cytec 680-3 • Abrasion only (120 grit)

• Fabric – Epoxyglass G10 • Film Adhesive • Glass fiber composites

• •
• Metallic Cytec FM300-2M
•
As fabricated

• • 3M-AF163 Abrasion only(120 grit)

AL 2024-T3
• Metallic substrates
• Ti – Grade 2 • Cure Cycles • MEK wipe only
• Manufacturer • PAA+BR127
recommended cure cycle • 3M - AC 130-2 surface treatment
• Abrasion
• Chemical treatment – ASTM D2651
(Ti)
34
 Task 1 - Substrate and Adhesive Compatibility Assessment
Physical Compatibility
• Objective
• Generate guidelines to ensure the surface preparation + substrates are physically compatible for bonding.
• Physical Compatibility 40

Dispersive / mN m-1
• Surface morphology related tests for substrates 30 A
C
• Surface roughness 20

• Contact angle 10 D

• Surface Energy
0
• Wettability envelope development 10 20 0 30
Polar / mN m-1
• Measure polar and dispersive surface energies for substrate and com pare the surface energy of the adhesive.
• Objective:- A sim plistic rapid approach to evaluate if the adhesive surface tension falls within the wettability envelope
== Good bond

• Perform qualitative tests to assess the bond failures

• Wedge crack
• Rapid adhesion test
• Flatwise tensile

35
 Task 1 - Substrate and Adhesive Compatibility Assessment
Physical Compatibility
• Develop the relationship between the 60 00

• Contact angle of substrates vs. bond quality. 50 00

Bond Strength
40 00
• Elapsed time vs contact angle
30 00

• Use in-situ surface energy measurement 20 00

techniques (BTG-Labs - Surface Analysts) to 10 00

assess the substrate characterizations 0
20 30 40 50 60 70 80
• Repeat the process for a given adhesive for Contact angle [°]
different mechanical properties (Shear, Peel, 50
Fracture Toughness)
45

Contact Angle [²]

40

35

30

25
0 10 20 30 40 50 60
Time [hrs]
36
 Task 1 - Substrate and Adhesive Compatibility Assessment
Physical Compatibility – Current Status
• Fabrication of composites test panels completed.
• Preliminary experiments completed for surface energy/contact angle measurements
• Guideline development for substrate preparation timeline is in progress

90
60 Se cond r ound
85
Tw o days
80 55
A v erag e C o n tact A n g le [d eg rees]

75
50

A n g le [d e g re e s]
70
45
65

60 40

55
35
50
120 gr it S an dB la s t 120 gr it H and 150 gr it H and 180 gr it H and 30
Sand Sand Sand
Po int 1 Po int 2 Po int 3 Po int 4 Po int 5 Po int 6 Po int 7
S u rface P rep aratio n P ro cess

37
 Task 1 - Substrate and Adhesive Compatibility Assessment
Thermal Compatibility
• Objective
• Generate guidelines to ensure the thermal properties of substrates and adhesives are compatible
for bonding and during service life.
• Thermal Compatibility
• CTE mismatch
• Between substrates and adhesives cured at elevated temperatures

In - Progress
• CTE mismatch in bonded structures during service life – Cold and elevated temperature environments –
formation of micro cracks during thermal cycling
• Glass Transition Temperatures
• Mismatch in glass transition temperatures and out it could potentially effect the bond integrity
• Pose cure effect on the substrates (composites) for secondary bonded structures
• Understand how the critical mechanical and thermal properties change after exposing to high temperatures for
long durations (cure profile of a adhesive)

38
 Substrate and Adhesive Compatibility Assessment
Mechanical Properties
• Mechanical Properties
• Coupon level testing
• Perform coupon level testing to evaluate static and durability capability. (using the actual bond process that
will be used for the application)
• Shear
• Peel
• Fracture toughness
• Element/Component level testing
Future Activities

• Fabricate a representative bonded structures

• Perform mechanical testing (static and fatigue)
• Assess the bond quality / Perform NDI

39
 Task 1 - Substrate and Adhesive Compatibility
Additional Tasks
• Extend current research with industry partners to further investigate substrate adhesive compatibility.

• Substrate Material – Tencate T350-1/IM7

• Adhesive System – EA 9394
Bondline CTD RTD ETD ETW
Test Type Test Method
Thickness [in] #Batch #Spec. #Batch #Spec. #Batch #Spec. #Batch #Spec.
0.015 1 6 1 6 1 6 1 6
0.04 3 18 3 18 3 18 3 18
Single Lap Shear ASTM D3165 - Composites
0.08 1 6 1 6 1 6 1 6
0.125 1 6 1 6 1 6 1 6
Single Lap Shear ASTM D1002 - (Al -thin) 0.015 1 6 3 18 1 6 1 6
Lap Shear and Stress/Strain ASTM D5656 - (Al – thick) 0.015 1 6 3 18 1 6 1 6
T-Peel ASTM D1876 - Composites 0.015 1 6 3 18 1 6 1 6
Floating Roller Peel ASTM D3167 0.015 1 6 3 18 1 6 1 6
Fracture Toughness ASTM D3433 0.015 1 6 3 18 1 6 1 6
Flatwise Tensile ASTM D897 0.015 1 6 3 18 1 6 1 6

40
 Task 2 - Peel Ply Surface Preparation Evaluation
Background and Goals
• Use of peel ply as a surface preparation method reduces the amount of labor involved and simplify the substrate
preparation process. It also provides a uniform and repeatable surface for bonding
• Peel ply prepared surface quality vary on many substrate and surface preparation process parameters. Bond surface
quality directly effects the bond integrity. Understanding the effects of these parameters is critical. Development of
reliable and rapid inspection methods is crucial to ensure the bond process (surface preparation) method is
appropriate for a given bond system.
• After an appropriate peel ply surface preparation method is chosen, there are many other parameters associated
with handling substrates that could potentially change the quality of the bond surfaces. These parameters and their
adverse effect on the bond integrity needs to be evaluated to provide Guidance and Develop Protocols to have a
robust bond system.

Surface Surface
ü
Substrates Preparation Bonding
Inspections

X
Goal – Develop guidelines and protocols to handle peel ply prepared surfaces to obtain a robust bond system

41
 Peel Ply Surface Preparation Evaluation

• Peel ply removal preparation method provides a repeatable uniformly prepared surface
for bonding with, minimum labor.
• For guideline development, need to understand
• The effect of different peel ply materials and thicknesses

• Surface contamination created and ways to reduce it (during application and removal of peel ply and the
timeframe of removal)
• Rapid inspection methods to ensure the surface quality of the substrates
• Peel ply prepared surface exposure to extreme environments (hot/wet)
• Any adverse effects to the laminate due to having the peel ply during cure cycle.
• Effects of peel ply prepared surfaces going through multiple cure cycles.

42
 Peel Ply Surface Preparation Evaluation
• Types of Peel Ply • Carbon Composites Substrates
• Polyester (Non Released) • Toray T800/3900-2
• Wet (Henkel EA 9895) • Adhesive Systems
• Dry • Film – FM300-2M
• T1 – 60002 (0.005 – 0.006-inch) • Paste – EA 9394
• T2 – 60005 (0.006 – 0.007 –inch) • Cure Cycles
• Nylon (Non Released) • FM300-2M – 250F for 2 hrs. at 40 psi pressure + full
• Wet (Henkel EA 9896) vacuum
• Dry • EA 9394 – 150F for 1 hr. 6psi vacuum
• T1 – 60004 (0.0045 – 0.0055-inch)
• T2 – 60005 (0.006 – 0.007 –inch)
• Polyester (Released)
• Dry
• T1 – 60001 (0.005 – 0.006-inch) (SRB)

43
 Peel Ply Surface Preparation Evaluation
• Surface Preparation Details
• Peel ply rem oval only

• Peel ply rem oval and light sanding (120 grit)

• Exposure to environment (Room temperature ambient and Elevated temperature wet)

• Rem ove peel ply im m ediately after curing

• Rem ove peel ply im m ediately before bonding (30 days)

• Effects of prepared substrates going through multiple cure cycles

• Co-bond and repair applications

• Therm al cycle substrates for m ultiple tim es to evaluate the effects

• Controlled/non peel ply configuration

• Carbon epoxy lam inates without peel ply

• Hand Abrasion (120 grit)

• No surface preparation (MEK wipe only)

44
 Peel Ply Surface Preparation Evaluation
Methods of Bond Surface Quality Assessment
• Surface Characterization
• Surface roughness measurements
• Contact angle measurements
• Scanning electron microscopic (SEM) inspection for surface details
• X-ray photoelectron spectroscopy (XPS) to detect surface contamination

• Wettability Envelope Development

40
35
Dispersive / mN m-1

30 A
25
C
20
15
D
10
5
0
0 5 10 15 20 25
Polar / mN m-1 45
 Peel Ply Surface Preparation Evaluation
Methods of Mechanical and Physical Property Evaluation
• Fiber Volume Fraction Quantification
• Due to the resin absorption in peel plies, fiber volume fraction is affected
• Flatwise tensile testing to quantify the effect.
• Mechanical Property Assessment
• ASTM D1002/D3165 type Single lap shear to determine the shear strength
• ASTM D5528 to determine the fracture toughness properties
• Peel Ply Prepared surfaces going through multiple cure cycles
• Measure the degree of cure for repeated cure cycle – simulation of core bond and repair
applications.

46
 Summary of Activities

• Current Activities
• Task 1 – Substrate and adhesive compatibility
• Task 2 – Use of peel ply for composite substrate preparation
• Completed Activities
• Effects of mix-ratio in two part paste adhesives
• Evaluation of assembly time in paste adhesives
• Amine blush effects
• Fluid sensitivity of adhesive
• Efficient adhesive screening method testing.

47
 Effects of incorrect mix-ratio in two part paste adhesives
• Two part adhesive for smaller quantities are Adhesive Adherend Percent Adhesive Quantity 0.005" Glass Bead
Identification Material Mismatch A [g] B [g] Weight [g]

available in cartridge form. (Mix ratio is not a -40% 30.000 3.060 0.00331

concern) For applications that require larger -20% 30.000 4.080 0.00341
quantities, common method is to obtain them in EA9394
Aluminum
0% 30.000 5.100 0.00351
separate containers and manually mix it. It is 0.063"

20% 30.000 6.120 0.00361

important to evaluate the sensitivity of mix ratio in
these applications 40% 30.000 7.140 0.00371

• Experimental Approach – used PAA+BR127 and

Abrasion + AC120-2 prepared aluminum and
carbon composite substrates and fabricated panels
with different mix ratios for Part A and part B. Test
methods evaluated are D1002 – single lap shear,
mode I fracture toughness, and floating roller peel
specimens (selected incorrect mix ratios).
• EA 9394 was used for the study with Part A mix
ratio error ranging from -40% to +40%

48
 Effects of incorrect mix-ratio in two part paste adhesives
Test Results – Single Lap Shear – ASTM D1002
45 00

40 00
-40% -20% 0% 20% 40%

35 00
Average Strength [psi]

30 00

25 00

20 00

15 00

10 00
Less than nominal More than nominal
50 0 Component B Component B

0
-40 % -20 % 0% 20 % 40 %
Incorrect Mix Ratio – Part A Mismatch
Adhesive/Cohesive Failures
Batch 1 -P AA Batch 2 -AC-1 30 -2

49
 Effects of incorrect mix-ratio in two part paste adhesives
Test Results – Mode I – ASTM D5528

0.4 0 25 %

0.3 5
-40% -0% 40%
20 %
0.3 0

Coefficient of Variation [%]

GIC (5% / MAX) [KJ/m2]

0.2 5
15 %

0.2 0

10 %
0.1 5

0.1 0
More than nominal 5%
Less than nominal
0.0 5 Component B Component B

0.0 0 0%
First Ply/Adhesive Failures
-40 % 0% 40 %
Incorrect Mix Ratio – Part A Mismatch

50
Effects of incorrect mix-ratio in two part paste adhesives
Test Results – Viscosity Response

1 .2 3 20 0

Normalized Strength Ratio 1 .1 2 70 0

1 .0 2 20 0

Viscosity[p]
0 .9 1 70 0

0 .8 1 20 0

0 .7 7 00

0 .6 2 00

0 .5 -3 00
-5 0 -4 0 -3 0 -2 0 -1 0 0 10 20 30 40 50
Part A - % M ix Ratio
Less than nominal More than nominal
Component B Component B
Viscosity during bonding
M inimum viscosity during cure
51
 Effects of incorrect mix-ratio in two part paste adhesives
Test results – Summary
• EA9394 adhesive system showed a ~±15% change
1. 5
in the mechanical properties of single lap shear 1. 4
and fracture toughness at the extreme mix ratios 1. 3

between -40% & +40% 1. 2

•
1. 1
Repeatability of the experiment was validated 1. 0

N o rm a lize d P ro p e rty
with a second data set. Data correlates will with 0. 9

the original testing. 0. 8

0. 7

• No change in the failure modes was seen between 0. 6

0. 5
the extreme ends of the experimental procedure.
0. 4

• Static response of the properties are desirable. 0. 3 D 1002 - P AA

However, understanding of the mix ratio effect on 0. 2

D 1002 - A C- 130- 2
0. 1
fatigue properties needs to be investigated. D 5528 - C ar bon Fi ber S ubst r at es
0. 0
- 50 - 40 - 30 - 20 - 10 0 10 20 30 40 50

P a rt A - % M ix R a tio

52
 Evaluation of assembly time in paste adhesives
• Manufacturer provided pot life is to be used as a
material specification. In bonding applications,
assembly time is defined as the time it takes to
mix, apply adhesive and mate the two parts
together. Depending on the bond area and the
complexity (contour) of the structure, this could be
a critical parameter.
• Experimental Approach – used PAA+BR127 and
Abrasion + AC120-2 prepared aluminum and
carbon composite substrates and fabricated panels
with different assembly times. Test methods
evaluated are D1002 – single lap shear, mode I
fracture toughness, and floating roller peel
specimens (selected incorrect mix ratios).
• Assembly time for EA 9394 was varied from 0, 5,
45, 60, 90, and 120 minutes

53
 Evaluation of assembly time in paste adhesives
Test Results – Single Lap Shear – ASTM D1002
45 00

40 00
5 min 45 min 60 min 90 min 120 min

35 00
Average Strength [psi]

30 00

25 00

20 00

15 00

10 00

50 0

0
5M IN 45 MIN 60 MIN 90 MIN 12 0M IN
Assembly Time [min] Higher % Adhesive Adhesive/
Failures Cohesive
Cohesive Failures
Batch 1 -P AA Batch 2 -AC-1 30 -2

54
 Evaluation of assembly time in paste adhesives
Test Results – Mode I – ASTM D5528
0.25 90 %

80 %
5 min 60 min 120 min
0.20
70 %
GIC (5% / MAX) [KJ/m2]

Coefficient of Variation [%]

60 %
0.15
50 %

40 %
0.10
30 %

20 %
0.05

10 %

First Ply/Adhesive Adhesive/Cohesive

0.00 0% Cohesive Failures
5M IN 60 MIN 12 0MIN Failures Failures

55
 Evaluation of assembly time in paste adhesives
Test Results – Viscosity Response

1 .10 Viscosity during bonding 1 20 0 0

1 .00 M inimum viscosity during cure

0 .90 1 00 0 0

0 .80
Normalized Strength

8 00 0
0 .70

Viscosity [p]
0 .60
6 00 0
0 .50

0 .40
4 00 0
0 .30

0 .20 2 00 0
0 .10

0 .00 0
0 20 40 60 80 1 00 1 20 1 40
Assembly Time [min]

56
 Evaluation of assembly time in paste adhesives
Test results – Summary
• EA9394 adhesive system showed very significant
effect for longer assembly times.
•
1. 5
Single lap shear strength reduced by ~ 20% when 1. 4
assembly time was 60 minutes. This started dropping 1. 3
to ~50% for 90 minutes (pot life) 1. 2

• Mode I fracture toughness data showed a large 1. 1

scatter in test data for increased assembly times. 1. 0

N o rm a lize d S tre n g th
•
0. 9
Mode I data showed an increase in the properties for 0. 8
60 minutes assembly and rapidly dropped when the 0. 7
assembly time was increased to 120min. 0. 6

• Failure modes throughout all the failure modes 0. 5

indicated cohesive/adhesive failures until 60 minute 0. 4

D 1002 - P AA
0. 3
assembly time and changed to cohesive after 60 D 1002 - A C- 130- 2
minute mark. 0. 2

0. 1 D 5528 - C ar bon Fi ber S ubst r at es

• Static response of the properties are desirable. 0. 0

However, understanding of the mix ratio effect on 0 20 40 60 80 100 120 140

fatigue properties needs to be investigated. A sse m b ly T im e [m in ]

57
 Fluid sensitivity of adhesive
• Current method used to evaluate the fluid sensitivity of adhesives is
the D1002 single lap shear specimen configurations.
• D1002 Lap Shear specimen configurations requires treated
substrate materials which involves numerous steps form
preparation to storage.
• The adhesive area exposed to fluids is minimum. (Adhesive
Thickness)
• A relatively simpler (test method + specimen geometry) bulk
adhesive specimens were fabricated using the adhesive systems
and simpler test configuration (3-pt bending) was used to evaluate
the effects and compared with the current D1002 method.
• EA 9394 and FM300-2m material systems were used for the
evaluation.
• Fluids used in this study
• Skydrol LD-4 (SAE AS1241, Type IV, Class 1) – 90 days
• MEK washing fluid. ASTM D740 – 90 minutes
• 145F/85% Relative Humidity 1000hrs – Controlled Condition

58
 Fluid sensitivity of adhesive
Test Results
EA9394 FM300-2M
1. 2
1. 2

1. 0
1. 0
N o rm a lized S tren g th

N o rm a lized S tren g th
0. 8
0. 8

0. 6
0. 6

0. 4
0. 4

0. 2
0. 2

0. 0
0. 0
BA SE LI NE M EK - 90M i nut es Skydr ol L D- 4 - 90 days M oi st ur e C ondi ti oni ng
BA SE LI NE M EK - 90M i nut es Skydr ol L D- 4 - 90 days M oi st ur e C ondi ti oni ng
3- pt Bend - E A 9394 D 1002- EA 9394
3- pt Bend - F M3 00-2 M D 1002- FM 300- 2M

59
 Adhesive Screening Test Methods
ASTM D1002
• Currently ASTM D1002 test m ethod is being used to perform
screening test/receiving inspections of adhesive m aterial. ASTM
D1002 requires a specialized substrates – treated chem ical
treatm ent/preparation m ethod.

• As an alternate to this test m ethod/substrate, Epoxyglass G10

substrates has been evaluated to be used in this type of screening
testing.

• Different substrate thicknesses has been evaluated as well as a

added new test m ethod.
• ASTM D1002 – Al substrates – 0.063-in thick (PAA+BR127)
ASTM D3165
• ASTM D1002 – Epoxyglass G10 substrates – 0.063-in thick (Abrasion) –
Thickness matched
• ASTM D1002 – Epoxyglass G10 substrates – 0.093-in thick (Abrasion) –
EI matched

• ASTM D3165 – Epoxyglass G10 substrates – 0.25-in thick (Abrasion) -

Standard
• Adhesive system s evaluated

• FM300-2M and EA9394

60
 Adhesive Screening Test Methods
Test Results
EA 9394 FM300-2M
4500 5% 5000 7%

4000 4500
6%
4% 4000
A p p a ren t S h ea r S tren g th [p si]

3500

C o efficien t o f V a ria tio n [% ]

C o efficien t o f V a ria tio n [% ]

A p p a ren t S h ea r S tren g th [p si]
3500 5%
3000
3% 3000
2500 4%

2500
2000
2% 3%
2000
1500
1500 2%
1000
1% 1000
1%
500
500

0 0% 0 0%
EPO XYG LASS 0.25' ' EPO XYG LASS 0.093' ' EPO XYG LASS 0.063' ' AL 20240. 063'' EPO XYG LASS 0.25' ' EPO XYG LASS 0.093' ' EPO XYG LASS 0.063' ' AL 20240. 063''

Adhesive Failures A d h e siv e /C o h e siv e

F a ilu re s
Adhesive Adhesive/Cohesive Failures
Failures

61
 Adhesive Screening Test Methods
Summary
• In a receiving inspection/screening tests, it is usually a Pass/Fail criteria
• Epoxyglass substrates can be used for screening/receiving inspection tests. Baseline
tests needs to be performed for the identical specimen configurations.
• Higher variation is seen in the bondline thickness for 0.25-inch thick epoxyglass
substrates. Bonding process/bondline control mechanism needs to be revisited to get
the required bondline thicknesses.

62
 Looking Forward
• Future Works
• Generate bond process protocols for
• Selecting compatible substrate and adhesive combinations for a robust bond structure
• Provide guidelines on how to select and use peel ply for composite substrate preparation

• Benefit to Aviation
• Generate bond process protocols
• Provide guidance on the critical parameters in the bond process and how to mechanically test them to
generate protocols

63
 Acknowledgement
• Advisory Committee and Program • Document Review
Guidance (FAA)
• Rachael Andrulonis (NIAR)
• Cindy Ashforth
• Curt Davies
• Bryce Floryancic
• Shannon Jones (Textron Aviation)
• Larry Ilcewicz
• Wei Kwan
• Ahmet Oztekin
• Royal Lovingfoss (NIAR)
• Program Support
• Molly Stone
• Shannon Jones (Textron Aviation)
• Mike Stuart (Solvay)
• Tony Hinman (Solvay)

• John Marsicano (Henkel)

64
Questions and Comments ???

65
 Development of NCAMP Specifications
Guideline Document
(FAA Report)
Guidelines and Recommended Criteria
for the Development of Material/
Process Specifications for Adhesive

Adhesive Process Control Document (PCD)

Adhesive NRP 102
Preparation and Maintenance Guide

Qualified Product List

NMS 300/1 (QPL)
Solvey FM300-2
FM300-2M 0.06 psf • NMS 300/1
NCAMP Material • NMS 394/1
Specification (NMS) • ...
NMS 394/1
Loctite EA9394
EA 9394 AERO

Material Specifications

Solvey FM300-2
Fabrication of
NCAMP Process bulk and
Specification (NPS) mechanical
test panels
Loctite EA9394

Process Specifications

70
 Development
FAA Special Project
of NCAMP Test Plans
Codes (SPC)

Authorized Inspection
Solvey FM300-2 Representative (AIR)
Authorized Engineering
NCAMP Test Plan
Representative (AER) Conformity
(NTP)
Loctite EA9394 Data Collection
Templates (PMC)
Test Plans

Material Property
Data Report
Statistical Analysis
Report

71
 Road Map - Adhesive Qualification Guidance

Specs
Guidelines Test Plans Procedures
(MS/PS)

Data Data Maintaining

Testing
Analysis Reports Data

Data Submit Data Yellow

CMH-17
Review to CMH-17 Pages

72