Adhesive Manufacturing Processes

Chapter 6: Testing and Quality Assurance

Univ.-Prof. Dr.-Ing. Prof. h.c. Stefan Böhm

Department for Cutting and Joining Manufacturing Processes (tff)
University of Kassel, Germany

Quelle: Wikipedia
Agenda

 Introduction

 Destructive Testing Methods

 Non-Destructive Testing Methods

2
Introduction
 Testing & Quality Assurance is especially important
 joined elements can either not be reworked or only with much effort
 Criteria for the selection of a testing method for an adhesively joined bond:
● parameters that need to be examined
● destructive or non-destructive testing
● circumstances under which the test is to be carried out (i.e. production control or
individual examination)
 testing standards and regulations need to be followed

Source: Habenicht 3
Introduction
 Important aspects for the quality assurance for adhesive bonding:
1. Planning:
– Training measures for employees,

– Integration of the production of adhesively joined bonds into the construction phase,

– Development of company-specific regulations or production standards,

Source: Habenicht 4
Introduction
2. Adhesives:
– Checking of the supplier´s specifications on the label to avoid confusion

– For further identification of the adhesive, viscosity, density and, if necessary, solids content
and colour should be examined
 Checking of rheological characteristics (i.e. viscosity, thixotropy)
– Checking of storing time and temperature

– If necessary, execution of test samples and tests

3. Joint Elements:
– Assessment of the surface quality (how clean, free of grease)

– Testing of the wetting properties (water drop test)

– Assessment of roughness

– Required dimensions, tolerances

Source: Habenicht 5
Introduction
4. Surface Treatment:
– Blasting material (size of grains, free of grease (also the supply air)

– Pureness of the degreasing material

– Composition, concentration and temperature of the pickling and chemical pretreatment

baths
– Pureness of the rinsing baths

5. Application of the Adhesive:

– Preparation of the adhesive

– Degree of mixture and the relation of the components to each other

– Pot life, amount, thickness of the layer, adhesive wetting

– Checking if the system for the application, mixture and dosing functions properly

– Positioning and fixation of the joint elements

Source: Habenicht 6
Introduction
6. Environmental Conditions:
– Cleanliness in the production halls

– Temperature, if necessary, climatisation (adsorption of humidity at the surfaces)

– Degree of humidity in the air

7. Occupational and Environmental Safety (Disposal, Recycling):

– various legal standards, laws and guidelines

8. Documentation:
– Continuous documentation of the parameters that are important for the quality

Source: Habenicht 7
Introduction
 Classification of the Testing Methods for Bonds

Testing of the Bond

if necessary, inclusion of Non-Destructuve

Destructive Testing
specific circumstances Testing

Static Dynamic Highly Dynamic

Source: Habenicht 8
Agenda

 Introduction

 Destructive Testing Methods

 Non-Destructive Testing Methods

9
Destructive Testing Methods
static short-term stress
 Shear Stress:

● Shear Test
– According to DIN EN 1465 (DIN 53283): „Determination of the
shear strength of highly strong overlap bonds“

:Bond Strength, Fmax:Maximum Force, A: Bond Area)

Source: Habenicht 10
Destructive Testing
static short-term stress
 Shear Stress:
● Disadvantages:
– Influence of the expansion of the joint elements

– Eccentric fixation

– To avoid eccentric stress in testing machines, specimen reinforcement in the fixation

area is done (out of the same specimen material)
● Field of Application:
– Testing method serves to examine the usability and the quality of the adhesive:

– When developing and applying the adhesive,

– When controling the production to ensure the quality

– When comparing adhesives under chemical and physical stress and influence

Source: Habenicht 11
Destructive Testing
static short-term stress
 Tensile Stress:

● Shear Stress and Sliding Behaviour

– „Thick“ shear test

– Implementation according to ISO 11003-2 (before DIN 54451)

– No bending moment  pure shear stress

– Building elements quite thick

 Expansion of joint elements is avoided

Source: Habenicht 12
Destructive Testing
static short-term stress
 Torsion Shear Stress:

● Torsion Shear Stress

– according to: ISO 10033-1 and ISO 11003-2
– Two pipe sections are twisted longitudinally in opposite directions
– Advantage: very homogeneous distribution of the shear stress, eliminates
shear and bending stress
– Disadvantage: elaborate preparation of the specimen to ensure the
concentricity of the hollow cylinder and the compliance to the defined
thickness of the adhesive layer

Source: Habenicht 13
Destructive Testing
static short-term stress
 Tensile Stress:

● according to DIN EN 26922 (DIN 53288) „determination of tensile

strength“

● stress under normal forces (this means horizontal to the joint surface)

● advantages: defined stress ratio and information about adhesion and

cohesion behaviour of the bond

Source: Habenicht 14
Destructive Testing
static short-term stress
 Compression Shear Stress:

● according to DIN 54452

● determination of shear strength of adhesive rotationally symmetric bond gaps in
axial direction
● especially for anaerobic adhesives for shaft-hub-connections
● advantages: homogeneous distribution of shear stress

( : shear strength, FB: breaking strength, A: shearing area,

D: bolt diameter, l: case length)

Source: Habenicht 15
Destructive Testing
static short-term stresssche Kurzzeitbeanspruchungen
 Torsion Stress:

● also mainly for anaerobic adhesives

● if the geometry is round, it can be tested flatly (1.) or with a thread (2.):
1. Torsion Strength
– apply according to DIN 54455 „ Determination of shear strength of adhesives in a
rotationally symmetric joint gap in tangential direction“
– ( : torsion shear strength, MB: measured ultimate moment,
r: radius of the joint gap, A: shearing area)

Source: Habenicht 16
Destructive Testing
static short-term stress
 Torsion Stress:

● if the geometry is round, it can be tested flatly (1.) or with a thread (2.):
2. Breakaway torque
– according to DIN 54454  on adhesively joined threads (see picture)

– serves to compare the security effect of bonded threads

– the breakaway torque is ascertained from the rotational angle diagram MLB

(relative motion between nut and screw)

Source: Habenicht 17
Destructive Testing
static short-term stress
 Peel Stress:
● this stress must be avoided constructively  peeling
stress is always the worst for a bond
● examination of adhesion behaviour
● line loads instead of area loading
● testing occurs under constant load or
constant peel speed

Simple peel
stress

Source: Habenicht 18
Destructive Testing
static short-term stress
 Peel Stress:
● Four methods for testing:
1. Angle Peel Test:
– according to ISO 11339 and DIN EN 28510 „Determination of the resistance of metal
bonds to peeling forces that occur horizontally to the joint gap“
– mainly to compare adhesives or surface pretreatment methods

 smallest differences in the adhesive and cohesive behaviour

can be shown
– advantage: easy to apply

Source: Habenicht 19
Destructive Testing
static short-term stress
 Peel Stress:
● Four methods for testing:
1. Angle Peel Test: Example of a
peeling diagram
– result of the test: peel diagram

– high force at the beginning joint elements have

to be deformed first (absolute peeling resistance)
– continuous peeling (relative peeling resistance)

 30 – 90% of the length of the diagram is

Kraft F
necessary to show the inhomogeneity of a bond Middle separating force
Fm
– elastic adhesive layers

 higher peel resistance than brittle layers

Length of
diagram
20
Destructive Testing
static short-term stress

 Peel Stress:
● Four methods for testing:
2. RollerPeel Test:
– according to DIN EN 1464, ISO 4578

– thin sheet is peeled under a constand bending

radius (advantage: contant angle)
– Peeling resistance is also taken from the force-
path diagram (see testing method of before)
– thickness of sheet: 0,5mm +/- 0,1mm

21
Destructive Testing
static short-term stress
 Peel Stress:
● Four methods for testing:
3. Increasing drum peel stress:
– according to ASTM D 1781-98

– thin sheet is bonded to a solid plate

– this sheet is unwound over a rotating drum

– documentation through diagram and determination of peel speed

– advantage: peel angle is constant

Source: Habenicht 22
Destructive Testing
static short-term stress
 Peel Stress:

● Four methods for testing:

4. Foil Peel Test:
– according to DIN EN 28510

– specifically for adhesion strength

– a 0,1 – 0,15mm thick metal foil is bonded to a metal plate

– peeling at an angle of 180°

– peel radius very small  cracks are brought upon forcefully in the boundary layers

– boundary layers can be examined intensively (i.e. microscopically)

Source: Habenicht 23
Destructive Testing
static short-term stress
 Split Stress:

● Extension to peel tests

 the construction elements are thicker  therefore „split“
● Two main split tests:
tearing
force
1. Bending-Peel-Test:
– according to DIN 54461

Kraft F
– especially for synthetic-metal bonds

 adhesion behaviour can be examined

– a 12mm thick steel sheet is bonded to a 4mm thick plastic

path

Source: Habenicht 24
Destructive Testing
static short-term stress
 Split Stress:
● Two main split tests:
2. Wedge Test:
– was developed by Boeing for surface-treated aluminium sheets

– standardised in DIN 65448

– joint elements are held on one side (picture)

Sheet-thickness:
example:
Aluminium 3,2mm
Titanium 2,0mm
100 bis 150

Source: Habenicht 25
Destructive Testing
static short-term stress
 Split Sress:
● Two main split testing methods:
2. Wedge Test:
– wedge is brought into adhesive layer  crach occurs (up to l0)

– then a specimen is brought into a climatic chamber with the wegde still in (i.e. 75
min. at 50 °C and 95% rel. F.)
– the advance of the crack is measured in relation to the time (from l0 to l1)

– advantage: influence of ageing processes can be examined

Source: Habenicht 26
Destructive Testing
static short-term stress
 Split Stress:

2. Wedge Test: degrease

d
– further advantage: different surface
treatments can be compared pickled + chromic acid anodisation

Rissverlängerung
blasted

pickled

pickled + Phosphoric acid anodisation

Time
t
Source: Habenicht 27
Destructive Testing
Static & dynamic long-term stress
● Static long-term stress of practical interest
● adhesive layers tend to creep
 if deformation possibilities are exceeded, the bond can break
● Creep Strength:
– resting stress on a bonding surface A under the impact of force F

 after the period of time t has ended, the bonded elements break apart ( creep)
for the fatigue strength this means: (t: time until the separation always shown)
● Creep Resistance:
– no separation of joint elements (no creeping) Zeitstandfestigkeit

Belastung
this means: ( )

F
Dauerstandfestigkeit

Source: Habenicht time until break 28

Destructive Testing
Static & dynamic long-term stress
 Testing of the Creep Strength:

● according to DIN 53284

● to „determine the creep strength and the creep resistance of
overlap bonds in resting shear stress“

Source: Habenicht 29
Introduction
 Classification of the Testing Methods for Bonds

Testing of Bonds

if necessary, inclusion of
Non-Destructive
Destructive Testing specific circumstances
Testing

Static Dynamic Highly Dynamic

Source: Habenicht 30
Destructive Testing
dynamic and highly dynamic stress

Impact-Peel-Test
according to DIN EN ISO 11343

speed of over 3 m/s

often in combination with metal substrates

usage in car industry, as the crash

characteristics can be examined in the
laboratory

31
Destructive Testing
dynamic and highly dynamic stress

Impact-Peel-Test

32
Destructive Testing
dynamic and highly dynamic stress

Quick Tear Test

different geometries of the
specimens possible
in bonding technology, U-
profiles are used that are
connected at the head piece
very high speeds of up to 20
m/s

Source: Keuerleber (2006): Bestimmung des Elastizitätsmoduls von Kunststoffen

bei hohen Dehnraten am Beispiel von PP. Stuttgart, 2006.
33
Destructive Testing
dynamic and highly dynamic stress

Drop Test
falling height up to 15 m

speed rates up to 16 m/s

when testing adhesive bonds, double

hat profiles are normally used
energy of the hit is regulated through
the fall mass and height
force measurement through plate in
ground and speed measurement
through light barrier
can be combined with Impact-Peel-
Prüfung

34
Destructiv Testing
dynamic and highly dynamic stress

Drop Test brittle epoxy resin crash-modified epoxy

adhesive resin adhesive

Source: Droste (2006): Crash stable adhesives in application and simulation. LS-DYNA
Anwenderforum, Ulm ,2006.

35
Introduction
 Classification of the Testing Methods for Bonds

Testing of the Bond

if necessary, inclusion of Non-Destructive

Destructive Testing
specific circumstances Testing

Static Dynamic Highly Dynamic

Source: Habenicht 36
Destructive Testing Methods
long-term stress under ageing influence
 In General:
● normal circumstances for bonds are rather rare
 tests under different environmental conditions
● standardised testing bonds are exposed to certain circumstances and then tested
● not aged (specimens for comparison) and aged specimens are compared
 a decrease in hardness is (often) established

Source: Habenicht
37
Destructive Tests
long-term stress under ageing influence
 In General:

● climatic tests are a compromise between the

shortest period of time and a system that is as
close to reality as possible
 the results should alwas be examined critically

Graphic comparison:
● Egg: 5min at 100C°  breakfast egg
● Egg: 28 days at 37C°  chick

Source: Habenicht und blog.essen-und-trinken.de 38

Destructive Testing
long-term stress under ageing influences
 Three forms of stress in short-time tests:

1. Humidity
– diffusion of moisture into the polymer layer (can take up to 5% of water)

 is often increased through heat (DIN 50017)

– air humidity between 0 % and 100 %

Source: Habenicht 39
Destructive Testing
long-term stress under ageing influences
 Three forms of stress in short-time tests:

2. Stress through corrosive media:

– especiall strong influence through humidity and
corrosion
– i.e. according to DIN 50021: „salt spray test“

– bond is sprayed with salt for several hours

Source: Habenicht und www.sulzer.com 40

Destructive Testing
long-term stress under ageing influence
 Three forms of stress in short-time tests:

3. Temperature:
– change of temperature as in reality simulated in the laboratory

 -40 C° to 80 C°
– cooling down is critical:

 the humidity diffuses into the adhesively joined bond as it expands (at low temperatures,
or frost)
 a type of „dynamical“ stress occurs (constantly changing temperatures)

Source: Habenicht 41
Destructive Testing
long-term stress under ageing influences

 Selection of Ageing Tests:

● standardised tests have been developed especially in the car industry

 specific varnish systems have been developed

a. VW P-1200 Test:
– climate-change test (high humidity without strong corrosion)
– 4 hs 80 °C, 95% rel.F. & cooling down 2 hs to –40 °C then 4 hs stay at –40 °C
– then heating up 2 hs to 80 °C, 95% rel.F.  time altogether (30-90 days)

Source: Habenicht 42
Destructive Testing
long-term stress under ageing influences
 Selection of Ageing Tests:

changing climate
b. VDA exchange test:
test chamber
– 24 hs salt spraying test according to DIN 50021,

– 6 hs sweat water test according to DIN 50017,

– 3 hs storage at room temperature

– 6 hs storage at 100 °C,

– 2 hs storage at room temperature,

– 5 hs storag at –30°C,

– 66 hs storage at room temperature

 strong changes in temperature with quite high stresses (is according real use in 6 to 10
years)
Source: Habenicht und www.vlm-labtec.com 43
Destructive Testing
long-term stress under ageing influences
 Selection of ageing tests:

c. Cataplasma-Test:
– difference to other testing methods: corrosion products are not separated  closed
atmosphere
– bonding specimen and a water-soaked piece of cotton are wrapped into an aluminium
foil and additionally into an air-tight polyethylene foil
– testing cyclus: 21 days storage at 70 °C and then 16 hs storage at –30 °C
 after that the bonding strength can be determined with this testing method

Source: Habenicht 44
Agenda

 Introduction

 Destructive Testing

 Non-Destructive Testing

45
Introduction
 Classification of the Testing Methods for Bonds

Testing of the Bond

if necessary, inclusion of
Non-Destructive
Destructive Testing specific circumstances
Testing

Static Dynamic Highly Dynamic

Source: Habenicht 46
Exclusion of NDT - Methods

Non-Destructive Testing Methods

Penetrating Magnetical- Mechanical Chemical-
Visual Thermical electrical
Radiation electric Vibration

•CCD-Camera
•Light-Section •Eddy Current
•Speckle-Interf. •X-ray
•Alternating Current •Colour Intrusion
•Moiré-Method •Microwaves
Method
•FTIR
Metalic joint Adhesive not
•Laser Scanning
elements electrical or
Bonding seams
Bonding seam disturb magetical
not
not visible the radiation conductive
visible

• Neutronen-
Radiographie Passive / Aktive
Shearografie Ultraschall
• Terahertz Thermography
• Röntgen / CT
47
Method of Active Thermography
Optical Radiation Mechanical Stress
Anregungs-
IR-Kamera quelle
Mess- und
Steuerrechner
Halogen , Laser,
LED, Flaslight Ultrasound

Anregungsenergie Steuerung der Conduction Induction

Anregung
Thermische
Welle

Defekt
Bauteil Induced Eddy
Hot, Cold Air Current

Imperfektionen (Fehlstellen, Aufzeichnung der von der Auswertung der lokalen

Anregung eines
Grenzflächen) erzeugen Körperoberflächen transienten (zeitabhängigen)
instationären
lokale Änderung des abgestrahlten Energie durch Temperaturänderungen der
Wärmetransports im Bauteil
Wärmeflusses eine Infrarotkamera Bauteiloberfläche

[Source: Srajbr, Böhm et al. – Zerstörungsfreie Prüfung geklebter Bauteile] 48

Ultrasound Shearographie
 Delaminationen in CfK- Sandwichstructures
Example: Exmanination of aviation structures

Piezo-Shaker with
vacuum suction cup

[Source: isi-sys GmbH]

49