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Extem* Resin

Extem* Thermoplastic Polyimide


(TPI) Processing Guide

April 2008
2

Extem* Resin Portfolio


Extem UH Family Extem XH Family
Glass Transition up to 311C (592F) Glass Transition up to 267C (513F)
RTI or Continuous use temperature as Enhanced creep and strength
high as 230C (446F; preliminary) performance at elevated temperatures
Tensile strength comparable to die cast aluminum
Extreme amorphous chemical resistance at 200C (392F)
to chlorinated solvents Approximately 50% stronger at 170C than
Ultem* resin
Exceptional high temperature load
bearing performance Better capability to fill thin-wall,
complex, miniaturized parts
Offers potential lead free solderable
solutions

Additional Extem Resin Featuresall families


True thermoplastic melt processability with ultra-high performance as molded
Processable using high temperature injection molding equipment and conventional drying
Potential in film & profile extrusion, thermoforming, stock shapes & blow molding applications

Exceptional Dimensional Stability


High strength, stiffness and creep resistance at elevated temperatures
Inherent Flame Retardancy
Outstanding Flame Smoke & Toxicity
High Limiting Oxygen Index
3

Extem* UH Blend Product Tree


HDT @ 66 Filler
Product Family Filler Type Flow psi/0.45MPa % Grade Name
EXTEM* Thermoplastic Polyimide (TPI) Resin

Standard Flow 263C UH1006 (M)


(505F)

Unfilled

High Flow 263C UH1016 (M)


(505F)

~260C Under
Extem* Glass Filled Standard Flow (500F)
10-30%
development
UH Series

Mineral Filled

Thru
LNP
Carbon &/or >250C Under
Standard Flow 0-30%
PTFE Filled (480F) development

Commercial Name Description


F = Food contact approved
Marketed Max 1000 PEEK-Extem UH Blend M= Optimized mold release
By VICTREX for metallized reflectors
Max 2000 Extem UH-PEEK Blend P = Powder

Rapidly Growing Product Family


4

Extem* XH Resin Product Tree


HDT @ 66 Filler
Product Family Filler Type Flow psi/0.45MPa % Grade Name
EXTEM* Thermoplastic Polyimide (TPI) Resin

Standard Flow 250C XH1005


(482F)

Unfilled High Flow 250C XH1015


(482F)

High Flow 250C AUT250 (M)**


(482F)

**250C haze onset temperature


Extem*
XH Series
>250C Under
Standard Flow 10-20%
(482F) development
Glass Filled

Standard Flow 257C 30% XH2315


(495F)

Mineral Filled

Carbon Filled
F = Food contact approved
M= Optimized mold release
for metallized reflectors
P = Powder
5

Extem* Resin Trials Requirements for Successful Trial

The following steps have greatly improved the success rate of


customers Extem resin trials
Internal Prep call (and/or with customer) to review trial, tool, resin & customer
expectationsADS or AM, PDE, HPP PM & HPP Technology
Clear customer expectations
e.g., Understand existing tool, wall thickness, flow length, gating, etc.
PDE pre-assess molders drying & processing capability vs Extem resin
recommended conditions; & tool (flow length, gating, etc.) before sample sent
PDE present during trial
Moisture analyzer, calibrated for Extem resins present to ensure drying to <0.02%
moisture content
HPP purchased 5 Omnimark Mark 3 MAs to support trialswell ship to your molder
Closed loop, desiccant dryer with after-cooler is highly recommended
Post-trial call and/or detailed trial report

Thanks for your supportExtem resin is a great polymer!


We need to help our customers dry & process properly
6

Extem* Resin Processing Support Independent Data


Drying & Moisture Absorption Studies:
Novatech (USA): Novatec Extem
Drying Study

Matsui Manufacturing Co., Ltd. (Japan): Matsui Drying Study


- Extem

Piovan (EUR): (Evaluating if study required.) Piovan Dryers


http://www.piovan.com/prod_lista.asp?idapp=1&idfam=4

SEA uses 1) Hot air dryer. 2) Hot air heat regenerative dryer - circulated hot
air dryer. 3) Hot air dryer oven. (Evaluating if study required.)

ECOMAK (Japan) vacuum system in hopper jacket to minimize moisture uptake:


http://www.haruna-ltd.co.jp/technology/index.html (suggested by Moka team)

Moisture Analyzers:
Omnimark 3
Sartorius Omnimark: Mark 3 Calibration - Extem resin
www.sartorius-omnimark.com

Arizona Instruments: Computrac Vapor Pro 3100L & Max 200XL AZI Calibration -
www.azic.com Extem resins

Aquatrac: Commonly used in EUR (S-IP has not


validated with Aquatrac) Aquatac Moisture
Analyzer
7

Extem* Resin Capillary Rheology


10000
10000 EXTEM XH1005 380C (716F)
EXTEM XH1005 390C (734F)
XH1005 (390C) EXTEM XH1005 412C (774F)
XH2315 (390C) (734F) ULTEM 1000 355C (671F)

Apparent Viscosity
Viscosity (Pa-s)

UH1006 (415C) (779F) ULTEM 1000 375C (707F)


ULTEM 1000 395C (743F)

1000 1000

100 100
100 1000 10000 100 1000 10000
Shear Rate (1/s)
Apparent shear rate
EXTEM XH1015: App Viscosity vs Shear Rate
10000 10000
UH1016 (415C) (779F)
EXTEM XH1015 380 oC (716F)
EXTEM XH1015 390 oC (734F)
UH1016 (430C) (806F)
Apparent Viscosity (Pa-s)

Viscosity (Pa-s)
EXTEM XH1015 412 oC (774F) UH1006 (415C)
UH1006 (430C)

1000
1000

100
100 1000 10000
Shear Rate (1/s)
100
10 100 1000 10000

Apparent Shear Rate (1/s)


Extem XH resins flow ~10-20% better than Ultem* resin
Extem UH resins are more viscous than Ultem resin
8

Water Moisture Absorption


All Ultem* & Extem* resin grades Small swell can occur due to
absorb water/moisture. water/moisture uptake.
Level depends on Time, Temp, Pressure Proper predrying recommended prior to
and Humidity. processing. (Consult datasheet or GEP
Level depends on resin type and filler Technical Support)
levels. Moisture may effect secondary operations
and in some cases predrying is
Water absorption of various polymers recommended.
condition: 23C, saturation
6
5.9 5.9 Water vs Moisture absorption
Sources: GEP datasheets and internal data, supplier data 2.3
5.3
Norm ISO62, ASTMD570 5 Source: GEP datasheets and internal data 2.1
5 2

1.75
Norm ISO62, ASTMD570
23C, soak, saturation

4 1.5 23C, 50%RH, saturation

1.25

1.2
H2O [%]

H2O [%]
2.9
3

0.9
1

0.83

0.76
2.3

0.8
0.7
2.1 2.1

0.55
0.6

0.6
0.5

0.5
0.43
2 1.75

0.4
0.5

0.22
1.251.2
1.1
0.83 0.8
1
0.5 0.5
0.35 0

Extem UH
Extem XH
CRS5001

XH6050
ATX100

ATX200

1000

2100

2200

2300

2400
0.1 0.1 0.03
0
Extem XH
Extem UH

PPA
PAA
ATX100

LCP

PBI
PEEK

PAI
PPSU
XH6050

PI
PSU

PPS
PC
ATX200
1000
CRS5001

PES

sPS

Large variances exist between polymers Filled grades absorb less water
9

Extem* UH Resins Studies


10

Processing of EXTEM* UH1006 Resin

Flow Lengths (Spiral Flow) 750 F (400 C) 775 F (413 C) 800 F (427C)

EXTEM UH1006 (120 mil / 3.0 mm) EXTEM UH1006 (90 mil / 2.3 mm) EXTEM UH1006 (60 mil / 1.5 mm)

20 20 20

Flowlength (inch)
Flowlength (inch)

Flowlength (inch)
15 15 15

10 10 10

5 5 5

0 0 0
17000 19000 21000 23000 17000 19000 21000 23000 17000 19000 21000 23000
Injection pressure (psi) Injection pressure (psi) Injection pressure (psi)

Standard & High Flow Grades


10000
UH1006 (415C) Injection Molding:
Viscosity (Pa-s)

UH1016 (415C) Standard dehumidifying dryers ~ 350F (177C)


1000 Melt temperatures ~ 760 - 790F (404 - 421C)
Oil heated molds ~ 350F (177C)
Ultem-like screws, material of construction
100
100 1000 10000
Shear Rate (1/s)

Melt Processable on Standard Equipment


11

Drying & Moisture Pickup Extem* UH Resin


UH1006 Drying Curve
0.3

6-8 hours for < 0.02% 300 F 149C


0.25 350 F 177C
Moisture (wt %)

400 F 204C ~15-30 minutes exposure > 0.02%


0.2

0.15

0.1 Extem Working Range

0.05
Maximum Moisture Level
0
0.0 4.0 8.0 12.0
Time (hr)

25
Great RCCA Tool!!
Molded Part - MFR

20
(g/10min)

15
Wet Part; ~ 3x MFR
y = 6163.5x + 4.1108
10 2
R = 0.9991

0
0.0% 0.1% 0.2% 0.3%
Moisture in Pellets (wt %)

Critical Success Factor - Drying to 0.02% Moisture


12

Drying & Moisture Absorption Test Result Extem* UH1006 Resin


Matsui Mfg Co., Ltd., Japan

Drying Test
1.346% Moisture Absorption Test
when unseal
Moisture Wt%

Matsui Dehumidifying Dryer DMZ at


175C/347F and moisture absorption
conditions (35C/95F, 56% RH, typical
Japanese Summer)

Extem resins could absorb moisture to


exceed 0.02% within 15-30 minutes typically
(depending on the local environment)

0.02%

Time (min)
~2-3 hrs to achieve moisture content <0.02%
13

Novatec Drying & Moisture Absorption Study Extem* UH1006 Resin

Chart 1: NDB-25 dryer Extem UH1006 resin moisture content over time
 Novatec Duel Bed desiccant dryer with PLC control coupled with 100
pound insulated hopper loaded by hand.

(149C)
(177C)
~3 hrs to achieve
moisture content <0.02%

0.02%

The dew point remained at a constant 40 throughout testing


14

Novatec Drying & Moisture Absorption Study Extem* UH1006 Resin


Chart 3: VDR-30 dryer Extem UH1006 resin moisture content over time
 Vacuum dryer uses 3 canisters, each holding 10 pounds of material; filled
automatically using an internal level sensor.

(149C)
(177C)

0.02%

350F (177C), 45 minute cycles needed to achieve


moisture content <0.02%, Table 7 (no graph)
15

Novatec Drying & Moisture Absorption Study Extem* UH1006 Resin

Chart 5: N25 dryer Extem UH1006 resin moisture content over time
 Novadrier compressed air dryer coupled with 100 pound insulated hopper
loaded by hand

(149C)
(177C)
~4 hrs to achieve
moisture content <0.02%

0.02%

The dew point remained at a constant 40 throughout testing


16

Process Window Study Extem* UH1006 Resin

September 500 psi Back Pres. 1,000 psi Back Pres. 2,000 psi Back Pres.
07 Study

.5 / sec. Inject.
Speed

1 / sec. Inject.
Speed

3 / sec. Inject.
Speed

Higher back pressure may help with a more homogenous melt.


Vary the back pressure as needed for optimal appearance
17

Purge Comparison @ Various Moisture Levels Extem* UH1006 Resin

Moisture Level .251% .066% .022% .017%

Lighter Darker
As moisture level decreases

Moisture Level .251% .066% .022% .017%

Extem UH resins foamy appearance is due to the die


swell effect since it is a blended product.
For a well dried (<0.02%) resin, the swelling does not
adversely effect part performance.
18

Extem* XH Resin Studies


19

EXTEM* XH Resin Spiral Flow Analysis


Spiral Flow Extem* XH1005 (3.05 mm)
600

500
Flowlength (mm)

400

300
390 C (734F)

400 C (752F)
200
413 C (775F)

100

0
1200 1300 1400 1500 1600

injection pressure (Bar)

Spiral Flow Extem* XH1005 (2.28 mm) Spiral Flow Extem* XH1005 (1.54 mm)
600
600
390 C
400 C
500
500

Flowlength (mm)
413 C
flow length (mm)

400
400 390 C
400 C
300 413 C
300

200
200

100
100

0
0
1200 1300 1400 1500 1600
1200 1300 1400 1500 1600
Injection pressure (Bar)
Injection pressure (Bar)
20

Drying & Moisture Absorption Test Result Extem* XH1005 Resin


Matsui Mfg Co., Ltd., Japan

Drying Test
Moisture Absorption Test

Matsui Dehumidifying Dryer DMZ at


Moisture Wt%

175C/347F and moisture absorption


conditions (35C/95F, 56% RH, typical
Japanese Summer)

0.1029%
When unseal Extem resins could absorb moisture
to exceed 0.02% within 15-30
minutes typically (depending on
the local environment)

0.02%

Time (min)

~1-2 hrs to achieve moisture content <0.02%


21

Novatec Drying & Moisture Absorption Study Extem* XH1005 Resin

Chart 2: NDB-25 dryer Extem XH1005 resin moisture content over time
 Novatec Duel Bed desiccant dryer with PLC control coupled with 100
pound insulated hopper loaded by hand.

(149C)
(177C)
~2 hrs to achieve
moisture content <0.02%

0.02%

The dew point remained at a constant 40 throughout testing


22

Novatec Drying & Moisture Absorption Study Extem* XH1005 Resin


Chart 4: VDR-30 dryer Extem XH1005 resin moisture content over time
 Vacuum dryer uses 3 canisters, each holding 10 pounds of material; filled
automatically using an internal level sensor.

(149C)
(177C)

0.02%

350F (177C) needed to achieve moisture


content <0.02% using a 20 or 30 minute cycle
23

Novatec Drying & Moisture Absorption Study Extem* XH1005 Resin

Chart 6: N25 dryer Extem XH1005 resin moisture content over time
 Novadrier compressed air dryer coupled with 100 pound insulated hopper
loaded by hand

(149C)
(177C)

~3 hrs to achieve
moisture content <0.02%

0.02%

The dew point remained at a constant 40 throughout testing


24

Drying Recommendations for Extem* Resin


25

Extem* Resin Drying Recommendations


Requirements After-cooler location
Closed Loop, Dehumidifying, Recirculating hot air (not shown)
hopper. Dryer conveying equipment recommended
to minimize moisture exposure
After-cooler highly recommended
Drying Conditions:
350F (177C) for 6-8 hours
Moisture content < 0.02%
Air Flow : 1 CFM per lb of resin per hour
Dew point of Air -20F to -40F
(hopper inlet); (-29C to -40C)
Do not dry in excess of 24 hours
Minimize resin in feed hopper
Do not rely 100% on Dewpoint Meter
Potential Processing Issues Typical Dryer Setup
Splay Thermocouple

Poor Impact Properties (Brittleness) The Most Neglected Part of the & Dewpoint
Monitor
Excessive Flow Molding Process!

Drying is Critical in Successfully Processing Extem


Resins! RE-absorption of Water Occurs Quickly
Extem* UH Resin - Injection Molding Guidelines
26

EXTEM* UH Resin Processing Guidelines Summary


Best Practices:
Maximum Moisture Content % 0.02
Drying Temperature C (F) 175 (347) Barrel temperature profile depends on residence time
Drying Time (Minimum) Hrs 6 Flat profile for ~2-3 min residence time
Drying Time (Cumulative) Hrs 24 Ramp profile for longer residence time
Melt Temperature C (F) 400-415 (752-779) Use 40-70% of barrel capacity per cycle to reduce
Nozzle Temperature C (F) 395-415 (743-779) residence time
Front - Zone 3 Temperature C (F) 395-415 (743-779) Extem UH resins are amorphous and do not need long
Middle Zone 2 Temperature C (F) 390-405 (734-761) cooling times (unlike crystalline resins)
Rear - Zone 1 Temperature C (F) 380-390 (716-734) Use low shear screw to minimize shear (similar to Ultem*
Mold Temperature C (F) 150-175 (302-347) resin)
Bac k Pressure bar 3- 5 Higher back pressure may help surface appearance.
Screw Speed rpm 30 - 50 Minimize decompression/suckback (can cause splay)
Shot to Cylinder Size % 40 - 70
Use slow injection velocity to reduce shear splay
Vent Depth mm 0.025-0.076 decoupled molding preferred
Purge with Ultem* 1000 or XH6050 resin when possible
CRITICAL SUCCESS FACTORS: During shut-down, heaters can be banked at 200-225C
(392-437F) after all the residual resin is run out of the
DRYINGmust dry to 0.02% moisture. Good dehumidifying barrel
dryer is critical (verify dew point; must target -40C (-40F).
If needed, dry longer than 6 hours and at a higher temperature (200C (392F). After-cooler recommended
FEEDINGminimize exposure of dried resin to humid air to avoid moisture absorption. Cover the feed hopper in case
of an open hopper.
RESIDENCE TIMEuse a ramp profile for residence times > 2-3 minutes.
INJECTION SPEEDslow speed (e.g., 15-25 mm/sec) is better for part appearance.
GATESpin-gates (used for crystalline resins) cause shear degradation. Use generous gates when possible.
27

Extem* XH Resin - Processing Guidelines Summary

Maximum Moisture Content % 0.02


Drying Temperature C (F) 175 (347)
Drying Time (Minimum) Hrs 6
Drying Time (Cumulative) Hrs 24
Melt Temperature C (F) 380-410 (716-770)
Nozzle Temperature C (F) 375-405 (707-761)
Front - Zone 3 Temperature C (F) 380-410 (716-770)
Middle Zone 2 Temperature C (F) 370-400 (698-752) Process Capability:
Rear - Zone 1 Temperature C (F) 360-385 (680-725)
Mold Temperature C (F) 150-175 (302-347) Minimal equipment investment
Back Pressure bar 3- 5 Able to leverage existing mold assets
Screw Speed rpm 70 - 100
Increased productivity via reduced cycle time
Shot to Cylinder Size % 40 - 70
Vent Depth mm 0.025-0.076 Reduced scrap fully recyclable
Process development assistance available via PPDC
and Field Tech Service
CRITICAL SUCCESS FACTORS:
Ramp-up barrel temperature from rear zone to nozzle. Avoid pin gates.
Use 40-70% of barrel capacity per cycle to reduce residence time
Use low shear screw design to minimize shear
Use high heat rated (ceramic) heater bands
Minimize back pressure & do not use decompression/suckback (causes splay)
Slow injection speed (e.g., 15-25 mm/sec) is better for part appearance.
Higher injections speeds give higher gloss, but watch for shear induced splay
Purge using Ultem* 1000 resins
28
Format

Extem* Resin Processing Support Start-up, Shut-down & Purging

Purging: Purge with Ultem* 1000 or XH6050 resin


Potentially use high temperature purge from RapidPurge, UltraPurge, or other purge
manufacturers
Has not been validated with trials
1-800-243-4203; Stratford, CN, USA

Shutting-down & Starting-up:


When Shutting-Down the machine, the hopper should be shut off at the throat and
the machine run until all residual resin is run out of the barrel. The screw should be
0.5 inches or less from its forward most position with the barrel heaters off.
When Starting-Up the machine, set the barrel heaters to normal processing
temperatures and purge the barrel again to ensure that all resin, having a previous
heat history, has been eliminated from the barrel and begin molding.

Interruptions:
Short (15 minutes): Empty barrel,
Short (30 minutes): Empty barrel, reduce temp to 400F (204C).
Long (day/night): Empty barrel, lower temp to 400F (204C), screw in
forward position.
Long (weekend): Total purge

If a Hot Runner System is being Used, the manifold should be purged by the material
to be molded prior to start-up.

Minimize Process-Related
Issues By Observing Best Practices
29

Ultem* & Extem* Resin Annealing


Annealing is the process in which the material is heated close to its glass transition temperature Tg. At the Tg the
amorphous molecules become mobile and can therefore relieve internal stresses. It is always best to start with
optimal design, then process as optimal as possible to have as low stress as possible before annealing should be
considered. Annealing takes time and money and may also change other properties (increased notch sensitivity,
reduced chem resistance for certain chemicals).

Annealing procedure guidelines:


Use a programmable circulating air oven to ensure a homogenous temperature in the oven
Place parts in a cool oven on a meshed grid/plate to allow hot air to reach all sides of the part and ramp
up the heat in 50C/hr to the required temperature.
Anneal at constant temperature for the time given in the table.
Gentle cool down of max 50C/hr is key to avoid building new stresses again.
These are typical guidelines. Dependent on application, optimization of parameters is recommended.
IR annealing is also done. No known experiences with Ultem. It is claimed to be much faster.
Grade Tg [C] Annealing temp [C] Wall thickness [mm] Annealing time [min]
ATX100 174/217 160 2 45
1285 180 165-170 3 45
ATX200 174/217 165 4 60
1000/1010 217 200-205
5 75
CRS5xxx 227 210-215
>5 +10 min/mm
XH6xxx 247 230-235
Extem XH 267 250-255
This may not be long enough for stock shapes thick parts
Extem UH 250/305 260-265
Inert atmosphere (e.g., Nitrogen) may be more suitable
than air at higher temperatures / longer times
30

Extem* Resin Injection Molding Screw Design

Screw length: Suggested 20 D (1040 mm)


Europe Typical
Screw configuration: GP Screw
Feeding zone 20 - 25 % (4 - 5 flights) ~50 %
Transition zone 50 - 55 % (10 - 11 flights) ~25%
Metering zone 20 - 25 % (4 - 5 flights) ~25%

Flight depth feed. 7.2 - 7.8 mm


Flight depth meter. 3.4 - 3.6 mm hm D
hf
Compression ratio 2.0 - 2.3 : 1

No flow back valve Metering Transition Feed

Angle of back ring 45 degree L

- Do Not Use A Ball Check Valve


- Nitrided Materials Are Not Recommended for Screw Or Barrel

Low Shear Screw Design Recommended


GP Screws have been Successful!
31

EXTEM* UH Resin Drying Study

Drying Time (hour) at 175C (347F)

ASTM Properties (at 23C) 4 8 24 48


(73F)

Tensile Modulus MPa 3,840 3,810 3,700 3,800


Tensile Strength MPa 114 108 109 111

Flexural Modulus MPa 3,430 3,410 3,430 3,440


Flexural Strength MPa 162 178 179 177

Izod Impact (Notched) J/m 61 62 66 58

Extem UH Resin can be dried for 48 hrs at


175oC (347oF) with little effect on properties
32

EXTEM* XH Resin Drying Study

Effect of Drying @ 150C (302F) on Resin Property Performance


MECHANICAL PROPERTIES VS DRY TIME Time = 6 hrs Time = 24 Time = 72 % Change
Oven Temperature = 150C Unit at 72 hrs
MECHANICAL
Tensile Modulus MPa 3500 3620 3600 2.9%
Tensile Stress, yield MPa 79.6 84.2 81.6 2.5%
Flexural Modulus MPa 3500 3620 3600 2.9%
Flexural Strength MPa 168 163 171 1.8%
IMPACT
Izod Impact, unnotched, 23C Ft-lb/in 0.8 0.8 0.8 0.0%
THERMAL
Glass Transition Temp., Tg C 268 268 269 0.4%
HDT, 0.45 Mpa, 3.2mm (un-annealed) C 251 251 251 0.0%
HDT, 1.82 Mpa, 3.2mm (un-annealed) C 236 234 232 -1.7%
PHYSICAL
MFR, 367C, 6.6 kgf g/10mi 5.4 5.2 5.1 -5.8%

Extem XH Resin can be dried for 72 hrs at


150oC (302oF) with little effect on properties
33

Extem* Resins Processing Methods & Secondary Operations

Processing Methods
Demonstrated Potential future ops
Injection molding Sheet extrusion / Thermoforming
Extrusion rod/tube & plate/slab Fiber solution spinning
(Stock shapes) Foam
Extrusion film Blow Molding

Secondary Operations similar to Ultem* resin


Bonding - Solvent, adhesive, ultrasonic, vibration, staking. Hot plate may be less
effective(?)
Marking - Silk Screen, Laser marking, Tampo(?), Hot Stamp
Metalization - Vacuum, Electroless (need etching, GF only?), Sputtering
Machining - Conventional & Laser
Painting Pre-clean (alcohol, aliphatics, detergents); waterborne. Solvent based may
be less effective
Mechanical assembly metal inserts, heat & ultrasonic, thread forming screw, rivets,
snapfits
Mold Temperature Control Ultem* & Extem* Resins

Control Strategy
Uniform Tool Temperature Control Is Critical For Cycle Time and Part
Property Optimization

Mold Temperature Requirements for Ultem & Extem resins Exceed


Capability of Conventional Water-Cooling Systems

Most Customers Incorporate Oil Cooling Systems

Thermolator efficiency increased by using mold insulating sheets and


short braided hoses with few restrictions.

Monitor actual mold surface temperature, a drop of 25-30F/C, common


for Oil Cooling Systems.

Monitor Supply and Return Oil temperatures to access efficiency

Reduce Cycle Time by using lowest Mold Temperature possible


35

Mold Insulation Ultem* & Extem* Resins

Prevents Heat Mold Insulation Prevents Heat


Loss to Platens Loss to Platens

Mold Insulating Sheets may be


applied to the top, bottom &,
side perimeters of the Mold
Insulation sheets
reduces Start-up
time

Mold Insulating Optional Mold Insulating


sheet
Sheet
Prevents Heat Loss to Machine
Platens Increases Efficiency
36

Mold Temperature Control Ultem* & Extem* Resins

Thermolators Function

Mold Temperature Controller Requirement - Achieving & Maintaining 150-175F (302-347C)


at Mold Surface
Oil Cooling @ T > 200F (93C)
Most Common Methods
Water Cooling @ T < 200F

Other methods Many customers Resist to


Pressurized Water Cooling @ T > 200F use Oil-Cooling Systems
Pulsed Cooling

Potential Processing Issues


Molded Part Surface Quality
Why not
Molded-in Stress Reduce Properties
Water?
Flow Length if Mold temperature is too low

Potential Advantages
Faster Cycle, No Dedicated Equipment Cost & Maintenance, Oil Disposal (Mess)

Type of Mold Temperature Controller


Dependant on Application
37

Molded-In Stress

Comments
Stress Levels
Polarized light/Birefringence
Qualitative Analysis

Part As-Molded
No Cracks Visually Present
Molded Part Visually Good
Stress
Molded Part Acceptable? Concentration

Grease Patch
(ignore)
Field Failure
Cracks through Gate

3 Cracks through Gate


Exposure to Hot Grease
Exposure to Chemicals

Cracks!
Field Failure
38

Molded-In Stress

Comments
Part As Molded
Different Process Used
Low Stress Level

Low Stress
Levels at
Gate!

Part As Molded
Same Part Dimensions
Different Molder/Mold
Low Stress Level

Process Conditions Can Effect Stress Levels


39

Extem* XH Resins - Regrind Study

Virgin vs. 50% Regrind, Three Passes


100% 50% 50% 50%
XH1005 XH1005, XH1005, XH1005,
pass 1 pass 2 pass 3
Tensile Stress, yield, 5 mm/min 97.4 101 96.5 97 MPa
Tensile Elongation, yield, 5 mm/min 4.8 4.7 4.2 4.3 %
Tensile Modulus, 5 mm/min 3230 3300 3300 3340 MPa
Flex Stress, yield, 1.3 mm/min, 50 mm 168 167 170 165 MPa
Flex Modulus, 1.3 mm/min, 50 mm 3120 3180 3170 3110 MPa
Izod Impact, notched 23C , 2 lb 43.5 33.6 33.4 35.4 J/m
Izod Impact, Unnotched 23C , 5 lb 1950 1923 1850 1780 J/m
MFR @ 367C, 6.7 kg 10.5 10.6 12.8 13.8 gm/10min
Melt vis @ 400 oC, 5000s-1 162.8 151.4 140.5 125.5

Extem Regrind Demonstrates Excellent


Recyclability & Property Retention
40

Extem* XH Resin - Metallization Study


GoalDetermine the influence of Haze Temperature Results
Heating rate on haze temperature 260
Part annealing prior to metallization Non-Annealed Slow Temp Ramp
Non-Annealed Fast Temp Ramp
250
Sample Preparation:

H aze Temperature ( o C)
Annealed Slow Temp Ramp

Aluminum Coated 4 Disk by Vacuum Metallization 240


Annealed Fast Temp Ramp

Annealing: Temperature:Tg - 20oC; Rate -20


oC/hour
230

Testing: Samples heated for 15 min after temp


equilibration (visual inspection) 220
Slow Temperature Ramp:Same sample with
temperature increments of 2oC
210
Fast Temperature Ramp: New Sample Placed in
Preheated Oven
200
Ultem 1010 Extem XH1015
Results:
Part failure defined as the temperature for the surface to show haze
Extem and Ultem have similar metal adhesion properties and failure modes
For Ultem/Extem Haze generally equates to material HDT for 3.2mm @ 0.45 MPa
Similar results observed for non-annealed vs annealed parts with slow heating rate
Thermal shock resulted in lowest haze temperatures
Annealing can boost haze temperature by +10oC for fast heating rates
Molding conditions should be optimized to minimize molded in stress
41

Extem* XH Resin Vibration Welding Study


Vibration welding strength of unreinforced Extem XH Extem XH1005 resin
resin at different welding conditions; at BoZ Jan 2006 Unreinforced Extem* XH Weld strength
sample Intrusion Amplitude Pressure Average st.dev
30 [mm] [bar] [Mpa]
1] Intr 1mm, Ampl 1, Pres 2bar 1 1 1 2 17.9 2.6
2] Intr 1mm, Ampl 1, Pres 3bar
2 1 1 3 12.4 2.7
3] Intr 1mm, Ampl 1, Pres 4bar
25 3 1 1 4 10.9 1.4
4] Intr 1mm, Ampl 1.5, Pres 2bar
5] Intr 1mm, Ampl 1.5, Pres 3bar 4 1 1.5 2 10.5 2
Weld strength [MPa]

6] Intr 1mm, Ampl 1.5, Pres 4bar 5 1 1.5 3 9.8 2.1


7] Intr 1.6mm, Ampl 1, Pres 2bar 6 1 1.5 4 9 0.7
20 8] Intr 1.6mm, Ampl 1, Pres 3bar 7 1.6 1 2 20.1 1.6
9] Intr 1.6mm, Ampl 1, Pres 4bar 8 1.6 1 3 11.8 1.7
10] Intr 1.6mm, Ampl 1.5, Pres 2bar 9 1.6 1 4
11] Intr 1.6mm, Ampl 1.5, Pres 3bar 10 1.6 1.5 2 13.7 1.9
15 12] Intr 1.6mm, Ampl 1.5, Pres 4bar
11 1.6 1.5 3 10.7 2.1
12 1.6 1.5 4

Extem XH2315 resin


10
30% glass-filled Extem* XH Weld strength
sample Intrusion Amplitude Pressure Average st.dev
[mm] [bar] [Mpa]
5 1 1 1 2 16.7 6.4
4 1 1.5 2 15.2 3.4
7 1.6 1 2 19.6 2.3
10 1.6 1.5 2 20.2 1.9
0
1 2 3 4 5 6 7 8 9 10 11 12
Welding conditions

Conclusions: Based on this initial studymore DOE required

Unreinforced Extem XH1005 resin 30% glass filled Extem XH2315 resin
Sensitive for vibration welding Difficult to vibration weld
parameters Low pressure required, 2 bar
Higher pressures yield lower the Need to re-run DOE with machine that
vibration weld strength can reach required amplitude
Low amplitude gives best weld strength Slightly better weld strength when
results intrusion is 1.6mm vs 1mm
Slightly better weld strength when
intrusion is 1.6mm vs 1mm
42

Unreinforced Extem* Resin Ultrasonic Welding Study

Ultrasonic welding of Extem* Weld strength Amplitude Weld pressure weld time weld energy Extem* UH1006
25.0
[Mpa] [um] [kN] [s] [J] Average st. dev
Extem* UH1006 Condition 1 0.45 70 0.84 409.0 18.6 1.7
Extem* XH1015 Condition 2 0.45 140 0.56 340.0 18.8 1.4
20.0 Condition 3 0.45 210 0.45 275.0 16.4 2.0
Condition 4 0.80 70 0.63 321.0 20.8 0.7
Weld strength [MPa]

Condition 5 0.80 140 0.29 265.0 15.0 1.2


15.0 Condition 6 0.80 210 0.22 207.0 9.8 3.7

10.0
Weld strength Amplitude Weld pressure weld time weld energy Extem* XH1015
[Mpa] [um] [kN] [s] [J] Average st. dev
5.0 Condition 1 0.45 70 0.62 265.0 21.3 0.9
Condition 2 0.45 140 0.27 193.0 21.9 2.3
Condition 3 0.45 210 0.24 210.0 13.5 1.3
0.0 Condition 4 0.80 70 0.56 299.0 17.3 2.2
1 [A0.45/P70] 2 [A0.45/P140] 3 [A0.45/P210] 4 [A0.80/P70] 5 [A0.80/P140] 6 [A0.80/P210]
Condition 5 0.80 140 0.25 224.0 17.9 1.2
Conditions
Condition 6 0.80 210 0.23 239.0 16.1 1.7

Conclusions:
Optimum ultrasonic welding conditions for the geometry used in this Vibration
study is amplitude 45 m and pressure 140 kN. study
Vibration welding parameters influence weld strength for Extem XH1015 & UH1006.
Critical to optimize the parameters for highest weld strength & the lowest standard
deviation. Extem Vibration
Study
The calculated weld factor: Extem UH1006 17.6%
Extem XH1005 21.6%
Weld factor is indication of the weld ability. The found weld strength is divided
with the tensile strength of the material in percentage.
Good weld factor [50-70%] can be achieve with ultrasonic welding.
Ultem* & Extem* Resin Injection Molding Questions & Answers
1. On what sized press should I mold my ULTEM*/EXTEM* products? 5. What is the best purging procedure for ULTEM/EXTEM?
The size of the press is dependent on the clamping force and the barrel If running another resin after Ultem, purge with either high density polyethylene
capacity of the machine. First determine the total projected area of the (HDPE) with a melt index of 0.30 to 0.35 g/10 min. or use glass reinforced
complete shot, 4 to 6 tons of clamp force should be provided for each square LEXAN. Begin purging at ULTEM processing temperatures and reduce barrel
inch of projected area to avoid flashing of the part. However, the total shot temperatures to approximately 500oF (260oC) while continuing to purge. For
weight (all cavities plus runners and sprue) should be 30 to 80% of the EXTEM, purge with ULTEM 1000 or XH6050 resin.
machine capacity. Very small shots in a large machine may create
unnecessarily long residence times which may result in streaking, discoloration 6. What type of hot runner system is best for ULTEM/EXTEM?
or part embrittlement. Internally heated runnerlesss molding systems are not suggested because of the
no-flow areas inherent in these systems, leading to extended residence time and
2. How much regrind can I add to my virgin ULTEM/EXTEM resins? material degradation. Externally heated systems are recommended for molding
Typically a maximum of 25% is recommended. Although, larger percentages ULTEM/EXTEM grades. Individually controlled heat zones are strongly
have been used with minimal losses in physical properties. Because regrind suggested. Also, wire insulation must be adequate for over 700oF (371oC).
usually absorbs more moisture than virgin resin, extra drying time may be
necessary to avoid problems such as splay and part brittleness. Also, grinder 7. Should glass filled ULTEM/EXTEM be processed differently than
screen sizes should be at least 5/16 to 3/8 inch. If a smaller size is used, too unfilled ULTEM grades?
many fines could be generated, creating molding problems such as streaking To maximize part performance, glass reinforced ULTEM/EXTEM grades should be
and burning. It is also important to keep the ground parts clean to avoid processed at lower screw speeds and relatively low back pressure. This will
contamination from other materials. reduce glass fiber damage during plastication. Also, increase the rear zone
temperature to promote improved flow and decrease glass fiber damage.
3. Why are my molded ULTEM/EXTEM parts brittle or cracking?
Brittle or cracking parts can be caused by a wide variety of sources such as 8. What chemicals cause stress cracking with ULTEM/EXTEM?
poor drying, abusive molding conditions, weld lines, chemical attack, improper Chlorinated solvents such as Trichloroethane, 1,1,2 Trichloroethylene,
design, and/or tooling problems. However, most ULTEM/EXTEM cracking Chloroform, Methylene Chloride, Ethylene Chloride; ketones and aldehydes such
problems are caused by poor drying and abusive molding conditions. as Methyl Ethyl Ketone and Acetone at high stress level; and aromatic
ULTEM/EXTEM resin should be dried as recommended on the ULTEM & EXTEM hydrocarbons such as Toluene. High stress levels either molded-in stresses or
injection molding page. A closed loop, dehumidifying, recirculating hopper external stresses applied in the application increase the likelihood of an ULTEM
dryer with an after-cooler is suggested for drying ULTEM/EXTEM resins. Also part cracking while in contact with chemicals. EXTEM XH resins have chemical
long barrel residence times and excessive melt temperatures may promote resistance similar to ULTEM resins. EXTEM UH resins have enhanced chemical
brittleness. Keep residence times short and melt temperatures below 750oF resistance to organic solvents (e.g., hydrocarbons, ketones & chlorinated
(400oC) preferably 660-730oF (350-390oC) for ULTEM resin; 716-779oF (380- solvents).
415oC) for EXTEM resin.
9. How long after molding can I test my ULTEM/EXTEM parts?
4. What mold temperature should I use to mold my ULTEM/EXTEM Ultem/EXTEM parts should be tested at least 24 hours after molding to allow
product? sufficient time for after mold shrinkage and moisture absorption. These parts
For best part performance a mold temperature of 250-350oF (120-175oC) for will also be more representative of the actual performance in the application.
ULTEM and 300-350oF (150-175oC) for EXTEM are recommended for thin
walled parts. However, there is always a trade-off between product NOTE: For more details see the ULTEM & EXTEM Injection Molding guide.
performance and cycle time. A higher mold temperature is recommended for a
glossy surface and lower molded in stresses resulting in the best part
performance.
Ultem* & Extem* Resin Injection Molding Troubleshooting Tips
BLACK SPECKS DISCOLORATION SINK MARKS
Small black areas (spots) inside the material, mostly present in The appearance of a non-uniform color distribution in the Visible defects resulting from insufficient cooling before removal
transparent ULTEM/EXTEM grades. molding. from the mold. A heavy rib intersecting a thin wall may show
up as sink marks: these are very difficult to eliminate by
Purge with ULTEM/EXTEM regrind or un-dried Purge heating cylinder varying processing conditions.
ULTEM/EXTEM resin
Lower melt temperature by: Increase injection hold time
Purge periodically after shut-off until cylinder temperature
falls below 660oF (350oC); then continue with purging a. Decrease cylinder temperature Increase injection pressure
until shutdown is complete. b. Decrease screw speed Reduce melt temperature
Bank set temperatures of machine at 350oF (180oC) when c. Decrease back pressure
not molding (EXTEM @ 400oF (204oC) Reduce mold temperature
Lower nozzle temperature Decrease injection speed
Decrease nozzle temperature
Shorten overall cycle Enlarge and/or add vents to mold parting line
Check temperature at feed section, low temperatures may
cause mechanical degradation. Increase back pressure to improve melt homogeneity Increase size of sprue and /or runners
Check heater bands and control Check hopper and feed zones for contaminants Increase gate size and reduce gate land length
Check nozzle tip, check ring assembly, nozzle adapter, Check for proper cooling of ram and feed zone Relocate gate next to heavy or thicker areas
and end-cap for hang-up areas.
Provide additional vents in mold Core out heavy wall sections where possible
BRITTLENESS/CRACKING Move mold to a smaller shot size press to reduce barrel
residence time.
The molded product is failing prematurely either after molding, SPLAY MARKS, SILVER STREAKS
during testing, or during normal usage. Check screw design, a high compression ratio screw
may cause excessive shear heating. The result of:
Dry resin properly (<0.02% moisture content)
(a) moisture on the pellets which should be removed under
Improve weld line strength (see weld lines) recommended drying times & temperatures
GLOSS
Decrease molded in stresses (see stresses) (b) products of degradation due to overheating
Increase mold temperature
Lower melt temperature by: (c) residual non-aqueous volatiles in material
Increase melt temperature
a. Decrease cylinder temperatures Dry resin properly excess moisture may cause splay
Increase injection speed
b. Decrease screw speed Lower melt temperature by:
Increase injection pressure
c. Decrease back pressure a. Decrease cylinder temperatures
Check surface of the mold for polish
Check for voids in the part b. Decrease screw speed
Clean vents
Check for contamination c. Decrease back pressure
Increase venting
Decrease the amount of regrind in feed Lower nozzle temperature
Check part design (sharp corners, wall thickness Decrease injection speed
transitions, bosses etc,..) JETTING / WORMING
Shorten or eliminate screw decompression
Check tooling (venting, ejection system) A serpentine line on the part surface emanating from the gate.
Shorten overall cycle
Investigate for chemical attack Decrease injection speed
Increase or decrease mold temperature
Increase melt temperature by:
BURN MARKS. Check for contamination (e.g.., water or oil leaking into
a. Increase cylinder temperature mold cavity)
They are usually caused by overheating of the material due to
entrapped air (diesel effect): this causes the darkening in color. b. Increase screw speed (unfilled) Move mold to a smaller shot size press
Decrease injection speed c. Increase back pressure (unfilled) Check for drooling
Decrease booster time Increase mold temperature Open gates
Decrease injection pressure Increase gate size Check hot runner system
Check venting channels for dirt Decrease gate land length Increase nozzle orifice
Use programmed injection Modify gate location or angle: directly into wall or pin Increase sprue and runner size
Improve venting of tool Avoid gating at thick section
Alter position of gate and/or increase gate size
Ultem* & Extem* Resin Injection Molding Troubleshooting Tips (continued)
STICKING IN CAVITY/CORE STREAKS WARPAGE, PART DISTORTION
At the end of cycle, the part does not release from the mold Decrease melt temperature A dimensional distortion in the molded part, usually bowing
but sticks on the core or cavity. or bending of the part.
Decrease nozzle temperature
Decrease injection pressure Equalize temperature of both mold halves
Decrease back pressure
Decrease hold time Observe mold for uniform part ejection
Decrease injection speed
Decrease booster time Check handling of parts after ejection from mold
Decrease screw speed
Adjust feed for constant cushion Increase injection hold time until gate freezes
Decrease cushion size
Increase mold closed time Increase mold closed time
Check for contamination
Adjust the cavity/core temperatures to a 20o Increase or reduce injection pressure
Increase the cavity venting
differential between mold halves
Increase or reduce mold temperature
Increase gate size
Decrease cylinder and nozzle temperature
Set differential mold temperatures to counteract
Increase nozzle orifice diameter
Check mold for undercuts and /or sufficient draft warpage due to part geometry
Check for material hang-up
Use shrink fixtures and jigs for uniform cooling of the
STICKING IN SPRUE BUSHING part
MOLDED IN STRESS
At end of cycle, the sprue does not release from the mold Check gate locations and total number of gates to
but sticks in the sprue bushing. These molded in stresses can result in part brittleness. reduce orientation
Usually caused by highly oriented polymer flow.
Decrease injection pressure Increase gate dimensions
Decrease injection speed
Increase injection hold time Redesign part to equalize wall variation in molded
Increase melt temperature part-thick and thin walls in the same part create
Decrease booster time
Increase mold temperature differential shrinkage stresses
Increase mold close time
Decrease injection pressure Check cooling line layout, unbalanced cooling promotes
Decrease mold temperature at sprue bushing warpage
Increase gate size
Leave nozzle against mold: no pull back
Increase nozzle orifice diameter WELD LINES/KNIT LINES
Raise nozzle temperature
These lines occur where two melt flow fronts in the mold
Check for correct seat between nozzle and sprue VOIDS meet. The streams of plastic should be hot enough to fuse
Check sizes and alignment of holes in nozzle and sprue Vacuole hollows in the molding, due to thermal shrinkage adequately. Weld lines are not just surface marks, but can
bushing that draws material away from the fluid core of a part. be points of weakness: notches, stress raisers.
Nozzle orifice should be .030 smaller in diameter than Decrease injection speed Increase injection speed
sprue bushing O diameter Increase injection pressure
Increase holding time
Check polishing of sprue Increase injection hold time
Reduce melt temperature
Provide more effective sprue puller Increase mold temperature Raise the mold temperature
Make sure sprue has enough draft angle for easy Check gate size and reduce gate land length Raise melt temperature by increasing cylinder
release temperatures
Increase gate size and reduce gate land length
If the sprue is stringing, increase or add screw Vent the cavity in the weld area
Increase nozzle size and/or runner system
decompression Provide an overflow well next to the weld area
Redesign part to obtain equal wall sections
Change gate location to alter flow pattern

Inasmuch as the SABIC Innovative Plastics has no control over the use to which others may put the material, it does not guarantee that the same results as those described herein will be obtained.
Each user of the material should make his own test to determine the materials suitability for his own particular use. Statements concerning possible or suggested uses of the materials described
herein are not to be construed as constituting a license under any SABIC-IP patent covering such use or as recommendations for use of such materials in the infringment of any patent.
46

HPP Product Management Team Resin


You are welcome to visit SABIC Innovative Plastics website to learn more about the Extem resin
family by following this link:
http://www.geplastics.com/gep/Plastics/en/ProductsAndServices/ProductLine/extem.html

For more information on SABIC Innovative Plastics new Extem UH and XH resin families, please contact:

Americas: Europe: Korea:


Shawn Lee: Peter Catsman Hang-Rae Kim
Tel: +1 812-831-7787 Tel: +31 164 291323 Tel: +82-11-9765-6569
Email: shawn.lee@sabic-ip.com Email: peter.catsman@sabic-ip.com Email: hang-rae.kim@sabic-ip.com
or call toll free 1-800-PLASTIC

China: Japan, South East Asia India:


Wilson Chan Munetaka Uchimura Ranji Varghese
Tel: +(852)-90389103 Tel: +81-3-3568-1546 Tel: +91-98-86774205
Email: wilson.chan@sabic-ip.com Email: munetaka.uchimura@sabic-ip.com Email: ranji.varghese@sabic-ip.com
Katsura Hayashi
Extem Product PM: Tel: +81-3-5544-3590 HPP Product GM:
Rob Costella Email: katsura.hayashi@sabic-ip.com Brian Herington
or call toll free in Japan 0120-800-312
Tel: +1-812-204-8067 Tel: +1-812-831-4247
Email: rob.costella@sabic-ip.com Email: brian.herington@sabic-ip.com
47

Disclaimer:

Disclaimer for product literature and pitches:


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SUBSIDIARIES AND AFFILIATES (SELLER), ARE SOLD SUBJECT TO SELLERS STANDARD CONDITIONS OF
SALE, WHICH CAN BE FOUND AT http://www.sabic-ip.com AND ARE AVAILABLE UPON REQUEST. ALTHOUGH
ANY INFORMATION OR RECOMMENDATION CONTAINED HEREIN IS GIVEN IN GOOD FAITH, SELLER MAKES
NO WARRANTY OR GUARANTEE, EXPRESS OR IMPLIED, (i) THAT THE RESULTS DESCRIBED HEREIN WILL BE
OBTAINED UNDER END-USE CONDITIONS, OR (ii) AS TO THE EFFECTIVENESS OR SAFETY OF ANY DESIGN
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RESULTING FROM ANY USE OF ITS PRODUCTS OR SERVICES DESCRIBED HEREIN. Each user is responsible for
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grant any license under any patent or other intellectual property right of Seller or as a recommendation for the use of such
product, service or design in a manner that infringes any patent or other intellectual property right.

SABIC Innovative Plastics is a trademark of Sabic Holding Europe BV


*Trademark of SABIC Innovative Plastics IP BV

Cycolac, Cycoloy, Extem, Geloy, Lexan, Lexan SLX, Lexan EXL, Noryl, Ultem, Valox, Verton, Visualfx, Xenoy, Xylex and LNP
are trademarks of SABIC Innovative Plastics IP BV.