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Dr.

Hans-Joachim Graf
Rubber Molding ASIA 2014

Determination
of the
Shortest Possible
Vulcanization Time
in
Rubber Injection Molding
TechnoBiz – Asia
March 2014
Dr. Hans-Joachim Graf Bangkok, Thailand
Introduction
Determination of shortest Porous Point
possible cycle time in Cycle Time and Porous Point
Injection molding Operating Window
Shortest Vulcanization Time
Summary

 Content of this presentation


 Introduction
 Operating window
 Porous point of different Rubbers
 Vulcanization time and physical properties
 Experiments guiding to shortest molding time
 Summary

Dr. Hans-Joachim Graf 3


Introduction
Porous Point
Finding of the Cycle Time in Cycle Time and Porous Point
Injection Molding Operating Window
Shortest Vulcanization Time
Summary

 The vulcanization time is Dependent from:


 Mold temperature
 Compound cavity entrance temperature
 Thickness of the part due to restricted
temperature conductivity

 Determined by trials
 No simulation tool, because of lack of
precision
 Physical properties must be evaluated

Dr. Hans-Joachim Graf 4


Introduction
Porous Point
Finding of the Cycle Time in Cycle Time and Porous Point
Injection Molding Operating Window
Shortest Vulcanization Time
Summary

 Heat rise in injection unit


Reason for heat rise – shortening of the vulcanization time
Temperatur
e

End of injection

Time
Dr. Hans-Joachim Graf 5
Introduction
Porous Point
Finding of the Cycle Time in Cycle Time and Porous Point
Injection Molding Operating Window
Shortest Vulcanization Time
Summary

Dr. Hans-Joachim Graf 6


Introduction
Porous Point
Finding of the Cycle Time in Cycle Time and Porous Point
Injection Molding Operating Window
Shortest Vulcanization Time
Summary

Regression equations to describe 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
asaa
factor
factoranymore)
anymore)because
becauseititisisdependent
dependentfrom
fromTMold
TMoldand
and
TMinj
TMinj

Dr. Hans-Joachim Graf 7


Introduction
Porous Point
Finding of the Cycle Time in Cycle Time and Porous Point
Injection Molding Operating Window
Shortest Vulcanization Time
Summary

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

Dr. Hans-Joachim Graf 8


Introduction
Porous Point
Finding of the Cycle Time in Cycle Time and Porous Point
Injection Molding Operating Window
Shortest Vulcanization Time
Summary

 Vulcanization of rubber in injection molding happens under


pressure of 250 bar – 450 bar
 All volatiles are compressed and probably expand if mold opens
and pressure is reduced to atmospheric pressure.

 The definition of the porous point:


Modulus of rubber, which just prevent pores.

 Question:
What is the correlation between porous point and physical
properties?

Dr. Hans-Joachim Graf 9


Introduction
Porous Point
Finding of the Cycle Time in Cycle Time and Porous Point
Injection Molding Operating Window
Shortest Vulcanization Time
Summary

 In this work to evaluate the cycle time 3


WOCO compounds used:
 NBR 1 – 51D50 (polar)
 NR 1 – 51A45 (slightly polar)
 EPDM 1 – 51M50 (none polar)
 All 3 materials are sulphur cured.

 The test mold: rectangular cup

Dr. Hans-Joachim Graf 10


Introduction
Porous Point
Finding of the Cycle Time in Cycle Time and Porous Point
Injection Molding Operating Window
Shortest Vulcanization Time
Summary

 1. Trial
 Vulcanization time until none 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 11


Introduction
Porous Point
Finding of the Cycle Time in Cycle Time and Porous Point
Injection Molding Operating Window
Shortest Vulcanization Time
Summary Source: Putera Thesis

Dr. Hans-Joachim Graf 12


Introduction
Porous Point
Finding of the Cycle Time in Cycle Time and Porous Point
Injection Molding Operating Window
Shortest Vulcanization Time
Summary Source: Putera Thesis

Dr. Hans-Joachim Graf 13


Introduction
Porous Point
Finding of the Cycle Time in Cycle Time and Porous Point
Injection Molding Operating Window
Shortest Vulcanization Time
Summary

 Conclusion from compression set measurement


(in conjunction with the other tests):

 NBR1 tpores + 45 sec


 NR1 tpores + 55 sec
 EPDM1 tpores + 40 sec

Dr. Hans-Joachim Graf 14


Introduction
Porous Point
Finding of the Cycle Time in Cycle Time and Porous Point
Injection Molding Operating Window
Shortest Vulcanization Time
Summary

force

EPDM

NBR

NR

t90 time

Dr. Hans-Joachim Graf 15


Introduction
Porous Point
Finding of the Cycle Time in Cycle Time and Porous Point
Injection Molding Operating Window
Shortest Vulcanization Time
Summary

 Operating window in injection molding:


The “Operating Window” gives a view about
process limits due to:
 Machine design
 Plastification Unit
 Nozzle length and diameter
 Mold design
 Runner length, diameter,
 Gate cross section
 Length to total flow path
 Processing parameter
 Plastification parameter setting
 Mold temperature
 Compound Cure
 Part design
 Pressure loss due to flow until cavity is filled

Dr. Hans-Joachim Graf 16


Introduction
Porous Point
Finding of the Cycle Time in Cycle Time and Porous Point
Injection Molding Operating Window
Shortest Vulcanization Time
Summary

TP Moulding Rubber Molding


Operating window: comparison with IM-moulding of rubber compound

Scorch

Underfill

Dr. Hans-Joachim Graf 17


Introduction
Porous Point
Finding of the Cycle Time in Cycle Time and Porous Point
Injection Molding Operating Window
Shortest Vulcanization Time
Summary Source: Graf, DESMA

 Lines are showing


the injection time at
Pressure loss (bar)

800
Max. Injection Pressure various pressures at
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 18


Introduction
Porous Point
Finding of the Cycle Time in Cycle Time and Porous Point
Injection Molding Operating Window
Shortest Vulcanization Time
Summary Source: Graf, DESMA

 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%
prevulcanization.

0
0 10 15
time (sec)

Dr. Hans-Joachim Graf 19


Introduction
Porous Point
Finding of the Cycle Time in Cycle Time and Porous Point
Injection Molding Operating Window
Shortest Vulcanization Time
Summary Source: Graf, DESMA

 Crossing points from


Mold Temperature (Grad C)

previous Curves are


now transferred to a
Mold Temperature /
190
Time Diagram
 Both curves showing
the operating window
180

170
0 10 15
time (sec)
Dr. Hans-Joachim Graf 20
Introduction
Porous Point
Finding of the Cycle Time in Cycle Time and Porous Point
Injection Molding Operating Window
Shortest Vulcanization Time
Summary Source: Graf, DESMA

 Dotted Line shows


in addition the 90%
Tcmpd 95C state of cure.
Mold Temperature (Grad C)

 This Line is parallel


190 to scorch index
line if activation
energy of cure is
similar for scorch
180 and vulcanization
time

170
0 10 15 2 3
time (sec) time (min)
Dr. Hans-Joachim Graf 21
Introduction
Porous Point
Finding of the Cycle Time in Cycle Time and Porous Point
Injection Molding Operating Window
Shortest Vulcanization Time
Summary Source: Graf, DESMA

 In case of compound
temperature variation
the line will shift.
Tcmpd 105C  For increase of
compound temperature
Mold Temperature (Grad C)

Line will schift to shorter


190 95C times.
 The operating window
will also move to shorter
times

180

170
0 10 15 2 3
time (sec) time (min)
Dr. Hans-Joachim Graf 22
Introduction
Porous Point
Finding of the Cycle Time in Cycle Time and Porous Point
Injection Molding Operating Window
Shortest Vulcanization Time
Summary Source: Graf, DESMA

 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 23
Introduction
Porous Point
Finding of the Cycle Time in Cycle Time and Porous Point
Injection Molding Operating Window
Shortest Vulcanization Time
Summary

 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)
 3 Factor Design,
 but detect the porous point,
 add the appropriate time or increase stepwise
Design-Expert® Software
Factor Coding: Actual

 mold t + taddition swell

porous X1 = A: T mass
X2 = B: T mold

Actual Factors 220


C: V inj = 20.00
D: t vulc = 75.00

Name Units Low High


210

200

swell
T mass °C 95 115 190

180

T mold °C 160 200


200.00

V inj mm/sec 15 25 192.00

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

Dr. Hans-Joachim Graf 24


Introduction
Porous Point
Finding of the Cycle Time in Cycle Time and Porous Point
Injection Molding Operating Window
Shortest Vulcanization Time
Summary

 Vulcanization to meet physical properties


 Porous point of rubbers is a good orientation, if the correlation
between
 Crosslink density and physical properties are known
 Croslink density can be measured with equilibrium swelling test
precisely
 Physical properties with the standard methods in rubber industry

 As a rule of thumb the following can be conluded:


 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 25


Introduction
Porous Point
Finding of the Cycle Time in Cycle Time and Porous Point
Injection Molding Operating Window
Shortest Vulcanization Time
Summary

 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: T mold 105.00
168.00 100.00
160.00 95.00 A: Tmass

Dr. Hans-Joachim Graf 26


Introduction
Porous Point
Finding of the Cycle Time in Cycle Time and Porous Point
Injection Molding Operating Window
Shortest Vulcanization Time
Summary

 Post cure operation


 For parts with even higher thickness post cure operation is
saving machine time
 Vulcanization time must succeed the porous point!
 It is recommended for compounds based on NR
with an early porous point
and high wall thickness

 Post cure is a pressure less vulcanization, but there is no negative


effect on physical properties because the starting modulus is high
enough to prevent pores.

Dr. Hans-Joachim Graf 27


Introduction
Porous Point
Finding of the Cycle Time in Cycle Time and Porous Point
Injection Molding Operating Window
Shortest Vulcanization Time
Summary

 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
 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.
 Introducing the vulcanization time as a factor, the shortest
vulcanization time can be determined with 9 experiments

Dr. Hans-Joachim Graf 28


Introduction
Porous Point
Finding of the Cycle Time in Cycle Time and Porous Point
Injection Molding Operating Window
Vulcanization to performance
Summary

 Thank you for attention and your comments

Dr. Hans-Joachim Graf 29

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