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Injection Molding of Elastomers

Presentation · December 2015


DOI: 10.13140/RG.2.2.30661.24806

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Hans-Joachim Graf
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Injection Molding of Elastomers

Raw Material Savings and Energy

Only Nine Experiment needed


to evaluate the Operating Window
and in Process Design

Dr. Hans-Joachim Graf Wuerzburg, den 02. December 2015


Introduction
Factors of Injection Molding Process
Building a Process Model
Operating Window
Process Evaluation and Design
Practical Implementation
Conclusion

 Introduction
 Factors Influencing Injection Molding
 Building a Process Model
 Operating Window
 Process Evaluation and Design
 Practical Implementation
 Conclusion

Dr. Hans-Joachim Graf 2


Introduction
Factors of Injection Molding Process
Building a Process Model
Operating Window
Process Evaluation and Design
Practical Implementation
Conclusion

 Thesis
G. Hellberg at University Hamburg in
1995

 Factors of four consecutive DOEs


1. Screw cylinder temperature
Screw speed
Back pressure
2. Plunger cylinder temperature
Injection speed
After pressure
Holding time
3. Mold temperature
Heating time
After pressure
Holding time
4. Plunger temperature
Injection speed
After pressure
Mold temperature

Dr. Hans-Joachim Graf 3


Introduction
Factors of Injection Molding Process
Building a Process Model
Operating Window
Process Evaluation and Design
Practical Implementation
Conclusion

 Process steps in injection


molding

1. Plastification
2. Injection
 Filling of cavity
 Reduced pressure
 After pressure phase
1. Vulcanization
2. De-molding

Dr. Hans-Joachim Graf 4


Introduction
Factors of Injection Molding Process
Building a Process Model
Operating Window
Process Evaluation and Design
Practical Implementation Source: Ankerwerke
Conclusion

 Advantages:
 Homogeneous
crosslinking
 Shorter vulcanization
Time
 Limit: Heat Rise

a -not-vulcanized
b -under vulcanized
c - vulcanized
d - over cured
1,2 – Plastification
2,3 - Time in plunger (before injection)
3,4 – Injection (with heat rise)
4,5 – Mold (heat rise by Temperature conductivity)

Dr. Hans-Joachim Graf 5


Introduction
Factors of Injection Molding Process
Building a Process Model
Operating Window
Process Evaluation and Design
Practical Implementation
Conclusion

 Higher compound cavity entrance temperature as a result of


plastification and injection process:
Heat transfer reduction = Reduction of vulcanization time
Temperature

End of injection

Time
Dr. Hans-Joachim Graf 6
Introduction
Factors of Injection Molding Process
Building a Process Model
Operating Window
Process Evaluation and Design
Practical Implementation
Conclusion

 Temperatures
 The Important and
 Plunger cylinder temperature
Independent factors in
Injection Molding:  Screw temperature
 Heating time is  Mold temperature
dependent from Mold /
Compound temperature
 Speeds
(or vice verse)  Screw speed
 Injection Pressure is a  Plunger speed
response of plunger  Opening and closing speed
speed!
 Ejection speed
 After Pressure and
Back pressure with no  Pressures
effect on heat rise!
 Injection pressure
 After pressure
 Back pressure
 Times
 Heating time
Dr. Hans-Joachim Graf 7
Introduction
Factors of Injection Molding Process
Building a Process Model
Operating Window
Process Evaluation and Design
Practical Implementation
Conclusion

 Factors important for Heat Rise of Compound:


 Temperatures 2 level factorial design
 Plunger cylinder temperature No of factors

 Screw temperature

No of experiments
 Mold temperature

 Speeds
 Screw speed
 Plunger speed

 Experimental analysis with DoE (Design of Experiments)


seems easy:
if Mold Temperature is constant:
only 4 factors needed

Dr. Hans-Joachim Graf 8


Introduction
Factors of Injection Molding Process
Building a Process Model
Operating Window
Process Evaluation and Design
Practical Implementation
Conclusion

 Factors important for Heat Rise of Compound:


 Temperatures 2 level factorial design
 Plunger cylinder temperature No of factors

 Screw temperature

No of experiments
 Mold temperature

 Speeds
 Screw speed
 Plunger speed

 Experimental analysis with DoE (Design of Experiments)


seems easy:
if Mold Temperature is constant:
only 4 factors needed

Dr. Hans-Joachim Graf 9


Introduction
Factors of Injection Molding Process
Building a Process Model
Operating Window
Process Evaluation and Design
Practical Implementation
Conclusion

 Conditions for statistic model of Injection molding


process
 Experimental Design Strategy

 Machine capability
 Process repeat-ability
 Plastification temperature
 Injection speed
 Mold temperature
 Pressures, at least in-mold-pressures

Dr. Hans-Joachim Graf 10


Introduction
Factors of Injection Molding Process
Building a Process Model
Operating Window
Process Evaluation and Design
Practical Implementation Source: Graf, RdoACS 00
Conclusion

Regression equations to describe fully the injection


molding process
 TMplast = f (VSc, PStau, Tcyl)

 TMinj = f (Vinj, TRunner, TMplast)

 tvulc = f (TMold, Vcure, TMinj)


Consequently
Consequentlythe
thetime
timeisisaaresponse
response(and
(andnot
nottaken
takenas
as
aafactor
factoranymore)
anymore)because
becauseititisisdependent
dependentfrom
from
TMold
TMoldandandTMinj
TMinj
Dr. Hans-Joachim Graf 11
Introduction
Factors of Injection Molding Process
Building a Process Model
Operating Window
Process Evaluation and Design
Practical Implementation Source: Graf, RdoACS 00
Conclusion

Regression equations to describe fully the


injection molding process target.
Equation converted:
(Mold Temperature and Cure Kinetic Constant)

 tvulc = f C(TMinj )
 tvulc = f C(Vinj, TRunner, Tmplast )
 tvulc = f C*(Vinj, VSc, PStau, Tcyl )

Dr. Hans-Joachim Graf 12


Introduction
Factors of Injection Molding Process
Building a Process Model
Operating Window
Process Evaluation and Design
Practical Implementation
Conclusion

 Result of statistic process model development:


 Vulcanization time is a response!
 4 Factors of influence
 Need an experimental strategy to identify the best and
shortest vulcanization time
 Variable vulcanization time as a consequence for the
production:
 Game changer:

Constant state of cure with temperature of


compound and mold as the leading factors

Consideration of Operating Window


may guide to an experimental strategy
Dr. Hans-Joachim Graf 13
Introduction
Factors of Injection Molding Process
Building a Process Model
Operating Window
Process Evaluation and Design
Practical Implementation
Conclusion

TP Moulding Rubber Moulding


Operating window: comparison with IM-moulding of rubber compound

Scorch

Underfill

Replace pressure with time!


Dr. Hans-Joachim Graf 14
Introduction
History of DOE in Injection Molding
Factors of Injection Molding Process
Building a Process Model
Conclusions

 Operating window in injection molding:


Thinking about an “Operating Window” opens the
view on process limits
 This limits depend on:
 Machine design
 Plastification Unit
 Nozzle length and diameter Scorch related to:
 Mold design RT-Residence
 Runner length, diameter, Time
 Gate cross section RTD -Residence
 Length of total flow path Time Distribution
 Processing parameter
 Plastification parameter setting
 Mold temperature
 Part design
 Pressure loss due to flow until cavity is filled

Dr. Hans-Joachim Graf 15


Introduction
Factors of Injection Molding Process
Building a Process Model
Operating Window
Process Evaluation and Design
Practical Implementation Source: Graf, DESMA
Conclusion

 Lines are showing


800 the injection time at
various pressures at
Max. Injection Pressure different mold
temperatures.
 No scorch during
700 filling
 The maximum
190 180 170C hydraulic pressure
Mold temperature (resp. specific
600 pressure) results the
0 10 15 shortest possible
time (sec) injection time.

Dr. Hans-Joachim Graf 16


Introduction
Factors of Injection Molding Process
Building a Process Model
Operating Window
Process Evaluation and Design
Practical Implementation Source: Graf, DESMA
Conclusion

 Lines are showing the


scorch index at
50 Mold temperature various mold
190 180 170 C temperatures.
Scorch Index (%)

 The maximum allowed


scorch index is
25 defined at 20% scorch
time consumption
before vulcanization.
 80% scroch time
0 remains for process
safety!
0 10 15
time (sec)

Dr. Hans-Joachim Graf 17


Introduction
Factors of Injection Molding Process
Building a Process Model
Operating Window
Process Evaluation and Design
Practical Implementation Source: Graf, DESMA
Conclusion
Mold Temperature (Grad C)

190

Maximum Mold Temperature

180
Best Mold Temperature

170 Safe Mold Temperature

0 10 15
time (sec)
Dr. Hans-Joachim Graf 18
Introduction
Factors of Injection Molding Process
Building a Process Model
Operating Window
Process Evaluation and Design
Practical Implementation Source: Graf, DESMA
Conclusion

 Stages of Processing.
Shortest possible cycle
time at maximum mold
Tcmpd 105C and compound
temperature
Mold Temperature (Grad C)

Best cycle time in an


190 95C operating window, which
fits demands of SPC due
to machine repeatability
Safe cycle time, which is
recommended, if
180 machine repeatability is
questionable.

170
0 10 15 2 3
time (sec) time (min)
Dr. Hans-Joachim Graf 19
Introduction
Factors of Injection Molding Process
Building a Process Model
Operating Window
Process Evaluation and Design
Practical Implementation
Conclusion

 Vulcanization to meet physical properties


Experimental strategy
to identify shortest vulcanization time
Stepwise increase of time
Mold Temperature variation
Compound temperature variation
Time consuming / Laboratory capacity consuming

Statistic Experimental Design Strategy


Fewer experiments – more information
3 factors + centre point = 9 experiments
with 2k-full factorial
4 factors + centre point = 9 experiments
with 2k-fractional factorial

Dr. Hans-Joachim Graf 20


Introduction
Factors of Injection Molding Process
Building a Process Model
Operating Window
Process Evaluation and Design
Practical Implementation
Conclusion

 Vulcanization to meet physical properties


Porous point of moulding as orientation to deviate
under cure – cure,
Evaluation necessary of correlation between
Crosslink density and physical properties are known
Crosslink density can be measured with equilibrium swelling test
precisely
Physical properties measured with the standard methods in rubber
industry

Dr. Hans-Joachim Graf 21


Introduction
Factors of Injection Molding Process
Building a Process Model
Operating Window
Process Evaluation and Design
Practical Implementation
Conclusion

 Evaluate of the cycle time with three different


compounds:

NBR – 51D50 (polar)


NR – 51A45 (slightly polar)
EPDM – 51M50 (none polar)

 All 3 materials are sulfur cured.

Dr. Hans-Joachim Graf 22


Introduction
Factors of Injection Molding Process
Building a Process Model
Operating Window
Process Evaluation and Design
Practical Implementation
Conclusion

 The test mold: rectangular cup

Dr. Hans-Joachim Graf 23


Introduction
Factors of Injection Molding Process
Building a Process Model
Operating Window
Process Evaluation and Design
Practical Implementation
Conclusion

 1. Trial
Vulcanization time until pores observed

 2. Trial
None pores time +20 sec
None pores time +40 sec
None pores time +60 sec

 Measurement of
Crosslink density with equilibrium swelling (Flory
Rehner)
Compression set

Dr. Hans-Joachim Graf 24


Introduction
Factors of Injection Molding Process
Building a Process Model
Operating Window
Process Evaluation and Design
Practical Implementation Source: Putera Thesis
Conclusion

 Porous Point (NBR).


Compound Temperature (°C)

Dependent from Mold


and Stock Temperature
But Porous Point gives
not the specified
properties of the part.

Mold Temperature (°C)

NBR Units Process Conditions

LL UL
Mold Temp °C 170 200
Compound Temp °C 105 125
Injection Speed % 30 90

Dr. Hans-Joachim Graf 25


Introduction
Factors of Injection Molding Process
Building a Process Model
Operating Window
Process Evaluation and Design
Practical Implementation Source: Putera Thesis
Conclusion

 Porous Point (NR).


Dependent from Mold
and Stock Temperature
But Porous Point gives
not the specified
properties of the part.

Mold Temperature (°C)

NR Units Process Conditions

LL UL
Mold Temp °C 170 200
Compound Temp °C 90 110
Injection Speed % 30 90

Dr. Hans-Joachim Graf 26


Introduction
Factors of Injection Molding Process
Building a Process Model
Operating Window
Process Evaluation and Design
Practical Implementation Source: Putera Thesis
Conclusion

 Porous Point (EPDM).


Dependent from Mold
and Stock Temperature
But Porous Point gives
not the specified
properties of the part.

Mold Temperature (°C)

EPDM Units Process Conditions

LL UL
Mold Temp °C 170 200
Compound Temp °C 90 120
Injection Speed % 30 90

Dr. Hans-Joachim Graf 27


Introduction
Factors of Injection Molding Process
Building a Process Model
Operating Window
Process Evaluation and Design
Practical Implementation
Conclusion

 Conclusion from compression set, equilibrium


swelling and other physical property
measurements:

 EPDM tpores + 40 sec (170 sec)


 NBR tpores + 45 sec (140 sec)
 NR tpores + 55 sec (220 sec)

Dr. Hans-Joachim Graf 28


Introduction
Factors of Injection Molding Process
Building a Process Model
Operating Window
Process Evaluation and Design
Practical Implementation
Conclusion

force
EPDM

NBR

NR

t90 time
As a rule of thumb the following can be concluded:

NR + 55 sec (for 10 mm thickness)

EPDM / NBR + 40 sec for 10 mm thickness)
This is in line with experience

Dr. Hans-Joachim Graf 29


Introduction
Factors of Injection Molding Process
Building a Process Model
Operating Window
Process Evaluation and Design
Practical Implementation
Conclusion

 Vulcanization to meet physical properties


Porous point of moulding as orientation to deviate
under cure – cure,

As a rule of thumb the following can be concluded:


NR + 55 sec (for 10 mm thickness)
EPDM / NBR + 40 sec for 10 mm thickness)
This is in line with experience

Number of Experiments:
30 Experiments:
(5 trials per evaluation point X 3 mold temperature settings X 2 Compound temperature,
all Samples have to tested in the laboratory)
No Information about general relation between factor and process
possible (One Step a Time - Strategy)

Dr. Hans-Joachim Graf 30


Introduction
History of DOE in Injection Molding
Factors of Injection Molding Process
Building a Process Model
Conclusions

Regression equations to describe the injection molding process

tvulc = f (TMold, Vcure,V inj , VSc, PStau, Tcyl)

In
Incase
casethat the TTmold
thatthe is a constant as well as the compound
mold is a constant as well as the compound
((VVcure ))vulcanization
vulcanizationtimetimedepends
dependson
onfour
four[[44!]!]factors.
factors.
cure

The
Thedifficulty
difficultyis,
is,totodetermine
determinethe
thevulcanization
vulcanizationtime
timewhich
which
corresponds
correspondstotothe
themold
moldtemperature
temperature

tvulc = f (TMold, V inj , Tcmpd )


with Tcmpd = f (VSc, PStau, Tcyl)

Dr. Hans-Joachim Graf 31


Introduction
Factors of Injection Molding Process
Building a Process Model
Operating Window
Process Evaluation and Design
Practical Implementation
Conclusion

 Evaluation with DoE


 Factor – Response Correlation
 4 / 5 Factors manageable with 9 experiments
 But need to gather about
Mold temperature

T-mold

 Compound temperature ulca


t-v
 Vulcanization time
at same time!!
T-compound

 Integration of vulcanization time as Factor


 Experiment “porous point identification” only needed once
 Selection of edge point in DoE

Dr. Hans-Joachim Graf 32


Introduction
Factors of Injection Molding Process
Building a Process Model
Operating Window
Process Evaluation and Design
Practical Implementation
Conclusion

Experimental Procedure to achieve best molding Cycle:


Regression equation:

tvulc = f (TMold,Vinj, Tcmpd)

 But tvulc has to become a factor


Because of a dependency of tvulc on Tmold,
none linear effects have to be expected
9 Experiments away from maximum
process performance
Dr. Hans-Joachim Graf 33
Introduction
Factors of Injection Molding Process
Building a Process Model
Operating Window
Process Evaluation and Design
Practical Implementation
Conclusion


Experimental Procedure to achieve best molding Cycle:

t
Design of Experiment with vulc as the additional Factor:

Property = f (Tmold,tvulc ,Vinj, Tmass)


 With 2-level fractional factorial design + centre point there
are 9 experiments.

 [A] = A + BCD
 [B] = B + ACD
 [C] = C + ABD
 [D] = D + ABC

Dr. Hans-Joachim Graf 34


Introduction
Factors of Injection Molding Process
Building a Process Model
Operating Window
Process Evaluation and Design
Practical Implementation
Conclusion

 Statistic Experimental Design (DoE) procedure


 Factor 1 = TM Mass Temperature
 Factor 2 = Tmold Mold Temperature
 Factor 3 = vinf Injection Speed
(little influence EPDM, but big with NBR)
 Factor 4 = tvulc vulcanization time, but dependent from factor 2
Design-Expert® Software
Factor Coding: Actual
swell

X1 = A: T mass
X2 = B: T mold
Name Units Low High
Actual Factors 220
C: V inj = 20.00
D: t vulc = 75.00
210
T mass °C 95 115
200

swell
T mold °C 160 200 190

180

V inj mm/sec 15 25
200.00

t vulc sec 30 120 192.00


115.00
184.00
110.00
176.00
B: Tmold 105.00
168.00 100.00
160.00 95.00 A: Tmass

Dr. Hans-Joachim Graf 35


Introduction
Factors of Injection Molding Process
Building a Process Model
Operating Window
Process Evaluation and Design
Practical Implementation
Conclusion

 Statistic Experimental Design (DoE)


Resulting operating Window for a NR Compound at
different Mass Temperatures (= Nozzle Valve Positions with LWB-EFE)
Design-Expert® Software
 Nozzle position 0 – open / 40 – half closed / 70 – almost closed
Factor Coding: Actual Overlay Plot
Overlay Plot 170.00

DVR M100: 4.500


Quellung
Quellung: 121.000
Hardness
M 100 148.00 tanDelta: 10.000
tan Delta DVR: 28.000
Design Points
C: Cure Time

X1 = A: WKZ Temp
Design-Expert® Software
X2 = C: Cure Time 126.00
Factor Coding: Actual Overlay Plot
Overlay Plot 170.00
Actual Factor Hardness: 71.000 Quellung: 115.000 DVR: 28.000
B: Drossel = 0.00 M100: 4.800 DVR
Quellung
104.00 Hardness
tanDelta: 9.500 M 100 148.00
tan Delta
Design Points

82.00
C: Cure Time

Design-Expert® Software
DVR: 35.000 X1 = A: WKZ Temp
X2 = C: Cure Time 126.00 Factor Coding: Actual Overlay Plot
Overlay Plot 170.00
tanDelta: 10.000 Hardness: 69.000
Actual Factor Quellung: 115.000 Quellung: 121.000 DVR
B: Drossel = 40.00
60.00 tanDelta: 9.500 M100: 4.500 Quellung
Hardness
160.00 165.00 170.00 175.00 180.00 104.00 M 100 148.00
tan Delta

A: WKZ Temp X1 = A: WKZ Temp


M100: 4.800 X2 = C: Cure Time

C: Cure Time
DVR: 35.000
82.00 126.00
Actual Factor
B: Drossel = 69.19 Hardness: 69.000
Quellung: 115.000 Quellung: 121.000
tanDelta: 9.500 tanDelta: 10.000
60.00 104.00 M100: 4.500 DVR: 35.000
160.00 165.00 170.00 175.00 180.00

A: WKZ Temp 82.00


M100: 4.800

60.00
160.00 165.00 170.00 175.00 180.00

A: WKZTemp

Dr. Hans-Joachim Graf 36


Introduction
Factors of Injection Molding Process
Building a Process Model
Operating Window
Process Evaluation and Design
Practical Implementation
Conclusion

 Injection Speed consideration


 Optimization possible with CAS-Jidoka
 Scorch index observation online!
Adjustment either automatic or by hand
 Property control with calculated Number,
 Correlated to crosslink density and Property

Dr. Hans-Joachim Graf 37


Introduction
Factors of Injection Molding Process
Building a Process Model
Operating Window
Process Evaluation and Design
Practical Implementation
Conclusion

 Conclusion
Precondition for DoE Operating window identification
Plastification:
Knowledge about influence of plastification process on compound
temperature.
Consider dependency from Compound and plastification unit.
Porous Point
Dependency of Compound
Normally this is known from traditional machine start-up

Dr. Hans-Joachim Graf 38


Introduction
Factors of Injection Molding Process
Building a Process Model
Operating Window
Process Evaluation and Design
Practical Implementation
Conclusion

 Conclusion
Optimum cycle time depends on temperatures in injection
molding:
Compound cavity entrance temperature
Mold temperature
None porous point depends on compound modulus at a time,
when the vulcanization has progressed to prevent expansion of
volatiles and enclosed air
Porous point is different for each compound / polymer
With the knowledge about the correlation between porous point
an physical properties a optimum cycle time can be determined.
In production the knowledge about the process window is
important for a safe but fast cure cycle with shortest possible
vulcanization time.

Dr. Hans-Joachim Graf 39


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