LCM Resin Characterisation for Aviation Applications

8/14/2019 LCM Resin Characterisation for Aviation Applications

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SummaryOutline

Properties of RelevanceTesting Methods

ResultsConcluding Remarks

LCM Resin Characterisation forAviation Applications

Semester Thesis AS09

Gokturk Kuru

ETH ZurichCentre of Structure Technologies

Dr. Markus Zogg

IMES-ST 09-048

MAAXIMUS-RTM 09-005

10 December 2009

Gokturk Kuru LCM Resin Characterisation 1 / 2 3
http://find/http://goback/


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SummaryOutline



Summary

This thesis presents a systematic methodology forcharacterisation of resins used in Liquid Composite Mouldingprocesses by



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SummaryOutline



Summary

This thesis presents a systematic methodology forcharacterisation of resins used in Liquid Composite Mouldingprocesses by

evaluating the relevance of various properties with regardsto processing and performance

examining standard methods for applicability to the testingneeds

developing new methods when necessary and providingrigorous documentation in the form of test manuals

exemplifying the proposed methods throughcharacterisation of three resin systems



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SummaryOutline



Outline1 Properties of Relevance

Overview of Material PropertiesLiquid Resin PropertiesCured Resin Properties

2 Testing MethodsMethods Based on Existing StandardsElectrical Resistivity TestImpregnation Speed Test

3 ResultsHexion EPIKOTETM/ EPIKURETM04908Huntsman LME 101142 / LME 101143Sika Biresin R L84 / Biresin R L84T

4 Concluding Remarks


S


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SummaryOutline




Properties of Relevance1 Properties of Relevance






Summary


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SummaryOutline




Overview of Material Properties

Material property related toliquid resin cured neat resin reinforced product

Viscosity Tensile properties Interlaminar shear strength

Pot life Flexure properties Impact resistanceElectrical resistivity Impact resistance Compression after impactElectrical permittivity Tg In plane shear

Toxicity Fatigue behaviour PorosityWetting Fracture toughness

Impregnation speed Water uptakeCuring time Refractive index

Gel time Curing shrinkageShelf life Thermal expansionResistance to chemicals

Thermal conductivity


Summary


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SummaryOutline






Viscosity Tensile properties Interlaminar shear strength

Pot life Flexure properties Impact resistanceElectrical resistivity Impact resistance Compression after impactElectrical permittivity Tg In plane shear

Toxicity Fatigue behaviour PorosityWetting Fracture toughness

Impregnation speed Water uptakeCuring time Refractive index

Gel time Curing shrinkageShelf life Thermal expansionResistance to chemicals

Thermal conductivity


Summary


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SummaryOutline






Viscosity Interlaminar shear strength

Pot life Flexure properties Impact resistanceElectrical resistivityTg

Impregnation speedCuring time


Summary


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SummaryOutline




Liquid Resin Properties - 1

Viscosity and Pot Life: Crucial input for selection ofproduction parameters and simulation purposes.


Summary


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SummaryOutline






Viscosity vs. temperature @ certain instant


Summary


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OutlineProperties of Relevance

Testing MethodsResults

Concluding Remarks





Viscosity vs. time @ certain T


Summary


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Concluding Remarks





Viscosity vs. time @ certain TElectrical Resistivity: An important characteristic data forresistance-based process monitoring.


Summary


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Concluding Remarks






Resistivity vs. temperature @ certain instantNormally, only the resistivity value at infusion temperature is

relevant for flow front monitoring applications. If infusion isplanned to be carried out at various themperatures,resistivity can be measured for the whole temperature range.


SummaryO


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Concluding Remarks






Resistivity vs. temperature @ certain instantNormally, only the resistivity value at infusion temperature is

relevant for flow front monitoring applications. If infusion isplanned to be carried out at various themperatures,resistivity can be measured for the whole temperature range.Resistivity vs. time @ constant T Could be used for in-mouldmonitoring of the curing degree.


SummaryO n


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Concluding Remarks



Impregnation speed: Although the only resin specific

parameter is viscosity, fabric permeability can be influencedby the type of liquid that is used for infusion, especially inthe range where impregnation through capillary effect isdominant.


SummaryOutline


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Concluding Remarks



Impregnation speed: Although the only resin specific

parameter is viscosity, fabric permeability can be influencedby the type of liquid that is used for infusion, especially inthe range where impregnation through capillary effect isdominant.

Curing behaviour: Curing time and temperature is an

important processing parameter that influences the cycletime and the production costs of a part.


SummaryOutline


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Concluding Remarks


Cured Resin Properties

Flexural properties, neat resin: Flexural properties such asflexure strength, modulus and strain at fracture provide anindication of the mechanical properties.


SummaryOutline

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Concluding Remarks




Glass transition temperature: Most of the time, glasstransition temperature of the resin system defines the limitsof operating temperatures for a certain fibre reinforcedplastic.


SummaryOutline

O M P


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Concluding Remarks





Impact properties, laminate: Toughness of the resin system

has a crucial influence on the impact properties of thelaminate.


SummaryOutline



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Impact properties, laminate: Toughness of the resin system

has a crucial influence on the impact properties of thelaminate.

Interlaminar shear strength: The matrix material is solelyresponsible for the interlaminar shear strength of alaminate.


SummaryOutline

Methods Based on Existing Standards


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Methods Based on Existing StandardsElectrical Resistivity TestImpregnation Speed Test

Testing Methods

1 Properties of RelevanceOverview of Material PropertiesLiquid Resin PropertiesCured Resin Properties





SummaryOutline



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Viscometry: Performed using a rotational viscometer undercontrolled temperature, based on standard DIN 53019. Doneimmediately after mixing the resin.

Gokturk Kuru LCM Resin Characterisation 10/23

SummaryOutline

P RMethods Based on Existing Standards


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Differential Scanning Calorimetry: Performed after differentcuring intervals, to determine the time required to reach fullcuring. Tg is also determined with the fully cured sample.


SummaryOutline

P s R aMethods Based on Existing Standards


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Three-Point Bending: Performed with neat resin samples,according to the standard ISO 178.


SummaryOutline

Properties of RelevanceMethods Based on Existing Standards


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Electrical Resistivity TestImpregnation Speed Test





Pendulum Impact: Performed with glass fibre reinforcedsamples, according to the standard ISO 179.


SummaryOutline



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Pendulum Impact: Performed with glass fibre reinforcedsamples, according to the standard ISO 179.

Interlaminar Shear Test: Performed with glass-fibrereinforced specimens, according to norm ISO 14130.


SummaryOutline



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Electrical Resistivity Test - 1

The relation of electrical resistancefor a wire with resistivity , length l,

cross-sectional area A:

R = l

A(1)


SummaryOutline

Properties of RelevanceMethods Based on Existing StandardsE R T


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R = l

A(1)

In the case of resistance through two

rods immersed in resin:R = f{, l,A}with being theresistivity, lbeing the spacingbetween the rods and A being theimmersed area of the rods.


SummaryOutline

Properties of RelevanceMethods Based on Existing StandardsElectrical Resistivity Test


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Concluding Remarks





R = l

A(1)

In the case of resistance through two

rods immersed in resin:R = f{, l,A}with being theresistivity, lbeing the spacingbetween the rods and A being theimmersed area of the rods.

[Fickel, 2009]


SummaryOutline

Properties of RelevanceMethods Based on Existing StandardsElectrical Resistivity Test


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Concluding Remarks



With the model of parallel resistances through the tip andthe sides of the rods:

R1 = R1tip + R1side

(2)


SummaryOutlineProperties of Relevance

Methods Based on Existing StandardsElectrical Resistivity Test


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Concluding Remarks




R1 = R1tip + R1side

(2)

Analogous to the wire, the resistances can be expressedeffective quantities l = i land A = j A.

R1 =

l1Atip

1+

l2A

side1

(3)



T M



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Concluding Remarks




R1 = R1tip + R1side

(2)

Analogous to the wire, the resistances can be expressedeffective quantities l = i land A = j A.

R1 =

l1Atip

1+

l2A

side1

(3)

After filling in for the cylindrical geometry of the rods andsolving for :

= C1 Rr2

l+ C2 R

2rh

l(4)



T M



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Concluding Remarks



Constants C1 and C2 relate to thegeometry of the set up. Equation 4 issuitable for using an estimationmethod to find C1 and C2 when theresistivity is known.

= C1 Rr2

l

+ C2 R2rh

l

(4)



Testing Methods



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Concluding Remarks

Impregnation Speed Test



= C1 Rr2

l

+ C2 R2rh

l

(4)

Doing a set of measurement with aliquid of known resistivity, theconstants can be determined usingthe LSE. (Least Squares Estimator)

0 0.02 0.04 0.06 0.08 0.1 0.12 0.14 0.160

0.5

1

1.5

2

2.5

3

3.5x 10

5 Acetone resistance vs immersion depth

Immersion depth [m]

Resistance[]

Measurements

Model



Testing Methods



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Concluding Remarks




= C1 Rr2

l

+ C2 R2rh

l

(4)

Doing a set of measurement with aliquid of known resistivity, theconstants can be determined usingthe LSE. (Least Squares Estimator)

0 0.02 0.04 0.06 0.08 0.1 0.12 0.14 0.160

0.5

1

1.5

2

2.5

3

3.5x 10

5 Acetone resistance vs immersion depth

Immersion depth [m]

Resistance[]

Measurements

Model

C1 = 1.67 104 andC2 = 6.22 10

2



Testing Methods



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Concluding Remarks



Based on taking photographs anddetermining the flow front position.



Testing Methods

Methods Based on Existing StandardsElectrical Resistivity TestI S T


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Concluding Remarks




Incorporates a MATLAB script to doimage analysis.



Testing Methods



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Incorporates a MATLAB script to doimage analysis. Requires precisepositioning of the camera



Testing Methods



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Taking a number of pictures during

infusion



Testing Methods



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infusion

Luminance plot



Testing MethodsR



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infusion

Luminance plot

Wet area vs. time

0 20 40 60 80 100 1200

1

2

3

4

5

6x 10

4

Time [min]

Wetarea

[mm

2]

Calculated data

Smoothened curve



Testing MethodsR

Hexion EPIKOTETM/ EPIKURETM04908Huntsman LME 101142 / LME 101143Sika BiresinR L84 / BiresinR L84T


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Sika Biresin L84 / Biresin L84T

Results

1 Properties of RelevanceOverview of Material PropertiesLiquid Resin PropertiesCured Resin Properties









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/

Hexion EPIKOTETM/ EPIKURETM04908Electrical Resistivity

At 30C resistivity is found to be = 6.5 109cm from thefollowing resistance vs immersion depth measurements:

0 0.02 0.04 0.06 0.08 0.1 0.12 0.14 0.160

1

2

3

4

5

6

7

8x 10

7 Hexion - resistance vs immersion depth

Immersion depth [m]

Res

istance

[]

MeasurementsModel






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/

Hexion EPIKOTETM/ EPIKURETM04908Impregnation speed

At 28 C the following wet area vs time plot is obtained:

0 10 20 30 40 50 600

1

2

3

4

5

6

7x 10

4

Time [min]

Wetarea

[mm

2]

Calculated data

Smoothened curve






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Huntsman LME 101142 / LME 101143Electrical Resistivity

At the range 70 C 45 C resistivity is found to be = 8.6 109cm from the following measurements:

0.02 0.04 0.06 0.08 0.1 0.12 0.14 0.160.5

1

1.5

2

2.5

3

3.5

4

4.5

5x 10

7 Huntsman - resist ance vs immersion depth

Immersion depth [m]

R

esistance[]

MeasurementsModel






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Sika Biresin R L84 / Biresin R L84TElectrical Resistivity

At 30C resistivity is found to be = 6.5 109cm from thefollowing resistance vs immersion depth measurements:

0 0.02 0.04 0.06 0.08 0.1 0.12 0.14 0.160

1

2

3

4

5

6

7

8

9x 10

7 Sika - resistance vs immersion depth

Immersion depth [m]

Resistance[]

Measurements

Model






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RConcluding Remarks

Sika Biresin R L84 / Biresin R L84TImpregnation Speed

At 32 C the following wet area vs time plot is obtained:

0 20 40 60 80 100 1200

1

2

3

4

5

6x 10

4

Time [min]

Wetarea

[mm

2]

Calculated data

Smoothened curve


SummaryOutline


Results



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Concluding Remarks

Rest of the Results

Hexion Huntsman SikaViscosity 0.14 Pa s @ 30 C 0.16 Pas @ 80 C 0.27 Ps @ 30 C

Curing Heat 435 J/g 390 J/g 390 J/gTg 96 C 186 C 125 C

Flexure strength 119 MPa 106 MPa 141 MPaFlexure modulus 2949 MPa 2647 MPa 3055 MPaUltimate strain 10% 5% 7%

ILS (longitudinal) 54.0 MPa 61.3 MPa 59.2 MPa

ILS (tansverse) 54.6 MPa 60.7 MPa 60.7 MPaImpact strength 356.1 kJ/m2 368.1 kJ/m2 365 kJ/m2


SummaryOutline


Results


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Concluding Remarks

Concluding Remarks

Comprehensive enough characterisation, also focusing onspecific needs for LCM


SummaryOutline


ResultsC


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Concluding Remarks

Concluding Remarks


New methods prove to be accurate enough for the purposes


SummaryOutline


ResultsC R


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Concluding Remarks

Concluding Remarks



Electrical resistivity test potentially suitable for a wide rangeof liquids


SummaryOutline




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Concluding Remarks

Concluding Remarks




Image analysis in impregnation speed test an improvementon the manual inspection


SummaryOutline




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Concluding Remarks

Concluding Remarks




Image analysis in impregnation speed test an improvementon the manual inspection

Various other methods can be used for image analysis, toenhance the accuracy of the test, while requiring morestable testing conditions (lighting, no movement of thecamera etc.)



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Important References

M. Fickel.Sensor Recommendation for MAAXIMUS.Technical Report - Centre of Structure Technologies, 2009 .

W. Hellerich, G. Harsch and S. Haenle.Werkstoff-Fuhrer Kunststoffe: Eigenschaften, Prufungen,Kennwerte. Munchen: Carl Hanser Verlag, 2001.

R. J. Yates, M. M. Munzer and F. D. Hook.Liquid conductivity measurement system using avariable-frequency AC voltage.United States Patent 5.708.363 13 January 1988.


Documents

LCM Resin Characterisation for Aviation Applications