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Lectures available at:
www.lehigh.edu/imi
Sponsored by US National Science Foundation (DMR-0844014)
Spring 2015 Glass Processing Course
Lecture 14. Fiberglass Processing
Elam Leed
Johns Manville
Elam.Leed@jm.com
www.jm.com
Outline
• Brief background
• Quick note on viscosity and liquidus temperature
• Continuous filament fiber
• Process overview
• Bushings design and operation
• Importance of sizing
• Wool fiber (discontinuous)
• Rotary process (internal centrifuge)
• Cascade process (external centrifuge)
• Flame attenuation process (pot & marble)
• More about viscosity and liquidus temperature
• A few other process variations
Stretching Glass is Fun
• The first fibers might have been made by accident
• Glass fibers have been made for many centuries, originally for art and decoration
• Fiber started to be manufactured for practical uses in the late 1800’s
• The process was improved and scaled up over decades
• Manufacturing
improvements
continue to help
expand the
global usage of
glass fiber
Glass rod
Fire
Winding
drum
Fiber Forming
What is the fundamental purpose?
Making surface area
• 0.05 to 15 square meters per gram
• A large wool manufacturing line can
produce 2000m2/s or 170km2 per day
• Interface, coupling, filtration
Making tortured paths
• Acoustic paths
• Filtration paths (air, liquid)
• Fracture propagation paths (composites)
• Thermal paths (conduction, convection, radiation)
Continuous Filament vs. Wool
Continuous Filament Wool (Discontinuous)
Processing
Pulled in a continuous filament
parallel with other strands
(often chopped downstream)
Process inherently creates
discontinuous sections of fiber
that have somewhat random
orientation
Typical Fiber
Diameters
4-30 micron 0.2 to 10 micron
Glass Types
E-glass, C-glass, R-glass,
S-glass, AR-glass, A-glass,
D-glass, basalt, others
Soft alkali borosilicates, mineral
wool, modified slag & basalt,
RCF, others
Uses
Reinforcement (chopped fiber,
rovings, wovens, non-wovens)
filtration, separation, facers,
thermal insulation, fireblocking
Thermal insulation (blanket,
board, pipe, paper), acoustic
insulation, filtration, separation
Generalized Process Flow
Batching Melting Conditioning Fiberization Cold (Warm)
Processing
Packaging
Temperature
(Viscosity)
Time
Room Temp
Glass Trans. (Tg)
Softening Point
η = 1000 poise
η < 100 poise
Fiberization
Cold (Warm)
Processing
Preparing glass for fiberization Making fiber more useful
1 to 300
tons/day, gas
and/or electric
Forehearth, dwell
tank, or just melt
stream
Bushing, rotary,
cascade, flame
attenuated
Winding, chopping,
sizing, binding,
twisting, assembling,
pressing, screening,
drying, curing
Viscosity
Softening point
Melting &
conditioning
η = 1000 poise
Fiber
forming
• Glass passes through the fiber forming viscosity range very fast, so in many cases the slope
of the viscosity curve is not a key glass design parameter
• Liquidus temperature relative to viscosity can be a much more critical parameter……
T
log3
Viscosity & Liquidus Temperature
Softening point
Melting &
conditioning
η = 1000 poise
Fiber
forming
• The liquidus temperature relative to a viscosity reference point such as Tlog3 is important for
glass chemistry design
• As liquidus temperature increases, the risk of devitrification increases
Liquidus A (good)
Liquidus B (not so good)
A
B
Viscosity & Liquidus Temperature
Melting &
conditioning
η = 1000 poise
Fiber
forming
• Liquidus temperature can vary widely depending on composition
• Some processes are more tolerant of high liquidus temperature glass
Liquidus A (good) Liquidus C (bad)
Devitrification
Bushing
tip
Bushing
tip
Continuous Filament Process
Melter
Conditioning
channel
Distribution
channel
Legs
Bushings
Forehearth
Melter & Forehearth Layout (top view) Leg/Bushing Cross Section
(end view)
Burner
Glass melt
Thermocouples
Water spray
Bushing
Flow block
Sizing applicator
Guide pulley
• Originally marble re-melt, now almost all direct melt
• Many different forehearth layouts
• Forehearth designed to deliver target glass
temperature and head pressure above each bushing
• Enclosed and conditioned forming room(s)
underneath legs
• Electrically heated precious metal bushings
Typical E-glass Process
Continuous Filament Bushings
ΔV
Tips
Cooling fins Support structure
(internal or external)
• Platinum alloyed with 5-25% rhodium for
high temperature strength
• Low voltage applied across bushing for
resistive heating (high current)
• Usually mounted into a frame and
surrounded on sides with refractory for
insulation and support
• Screen improves temperature distribution
and reduces effective head pressure
Terminal
(ear)
Flange
Screen
• 500 to 7000 tips per bushing
• Uniform temperature across the tip
plate is critical for uniform flow per tip
Design Considerations
• Tip dia. and length
• Tip number and spacing
• Screen thickness and
flow resistance
• Support structure
• Cooling fins
• Part thicknesses
(cooling fins not shown for clarity)
Bushing Design Examples
(US Patent 7,980,099)
Flange
External
mounting
brackets Sidewall Tips
Tip
plate
Terminal
(ear)
Screen
Support
structure
Bushing Design Examples
(US Patent Application 11/638,757)
Flange
Sidewall
Tips
Tip plate
Screen
Support
structure
Fibers
Refractory
Mounting
frame
(US Patent Application 11/320,135)
Bushing Design Examples
(US Patent Application 10/702,004)
Flange
Sidewall
Tips
Tip plate
Support
structure
Fibers
Refractory
Mounting
frame
Cooling fins
Tips
Tip plate
Sidewall
Support
structure
Cooling fin
Cooling fin
manifold
Bushing Operation
η = 10,000 poise η = 1000 poise η = 200 poise
(estimated tip exit viscosity)
Fiber Diameter
Flow
• Effective head pressure
• Tip geometry (dia., length)
• Glass temperature (visc.)
Pulling Speed
• Winder or chopper
Operation can be very sensitive to defects in the glass
• Stones
• Refractory
• Batch/batch reactants
• Devitrification
• Contamination
High viscosity results in
high fiber forming stress
• Seeds
• Inhomogeneity (cord)
Low viscosity can
lead to cone instability
Fiber Forming Stress and Breaks
• A bushing is like an in-line high speed tensile strength test
• 100,000 to 500,000km of fiber per hour per bushing is tested
• Stress level from 10-200MPa at temperatures from RT to >Tg.
Modeling is used to
predict stress profiles
with varying conditions
and designs
S. Rekhson et al, “Attenuation and Breakage in the Continuous Glass Fiber Drawing
Process”, Ceramic Engineering & Science Proceedings, vol. 25, No. 1, page 179.
Failure stress
Failure
probability
(A)
(B)
Fiber forming
stress range
A) Sample size (length of
fiber) is so large that a weak
spot is eventually found
B) Defects cause an increase
in fiber forming stress to the
point of break
And/or
C) High stress from a cold tip
(C)
Tips and Contact Angle
(US Patent 5,017,205)
• Tips are typically 1.0 to 2.5mm
inside diameter
• Tips size needs to match process
requirements
• Tip size strongly influences flow rate
and fiber forming stress
• Some tips have restricted outlets to
reduce stress but still have
sufficiently high flow rate
• The wetting (contact angle) of the
molten glass on the alloy can
influence forming cone shape
• Wetting can also influence bead
formation when a fiber breaks
• It is desirable to have the glass
quickly form a bead that drops down
to allow for bushing restart
Wetting
(“flooding”)
Non-
wetting
Tapered
tip
Wetting
(“flooding”)
Non-wetting layer
(Pt-Au alloy)
Collecting Breakout Defects
Al-Si defect from contaminant
Collecting and identifying the cause of a break can be very difficult
• In some cases the tip that broke first can be identified and the bead collected
• Optical microscopy and SEM/EDS can help with identification
Identifying Defects
SEM/EDS
Optical Microscopy
Defect source: zircon refractory
Continuous Filament Process
Chopper
Wet Chopped Strand
(7-18% H2O, 0.1 to 0.5%
sizing solids)
Dryer
Dry Chopped Strand
(0.2 to 2% sizing solids)
Winder
Dryer
Chopper
Assembled Roving
(0.2 to 2% sizing solids)
Dryer
Winder
Direct Rovings
(0.2 to 2% sizing solids)
Sizing
Applicator
Leg
Bushing
Continuous Filament Sizing
glass
binder/matrix
interface/coupling
• Tailored to specific application
• Critical for downstream
processing, handling, and
physical performance
• Key roles
• Protection from damage
(physical & chemical)
• Lubrication
• Bundle/strand integrity
• Dispersion
• Coupling
• 1 to 10 components
• Silane (e.g. amino-propyl silane)
• Film-formers
• Lubricants
• Enhancers
• “Magic ingredients”
• Other
Sizing Performance: Coupling
Role of silane in the moisture resistance of a fiber/resin bond
Wet chop fiber Non-woven mat
Sized with
water or
water+silane
Tested as-made
versus hot water
aged
Mat tensile strength – dry Mat tensile strength – hot/wet
Without silane, the
interface is easily
weakened by water
Application Example: Reinforced Thermoplastic
• Proper sizing chemistry and
processing is very important
for composites
• Chopped fiber is further
broken down in compounding
but still delivers a significant
increase in strength
J.
H.
A.
van
der
Woude
and
E.
L.
Lawton,
‘Composite
Design
and
Engineering’
in
Fiberglass
and
Glass
Technology,
F.
T.
Wallenberger
and
P.
A.
Bingham
(Editors),
Springer,
New
York,
pp.
125-173,
2010
“Enhancers”
(lubrication, wetting,
hydrophobic interphase
promotion, etc)
Sizing Chemistry Example
C1 S26 S29
Modified Polypropylene Emulsion 40.71 43.00 43.00
Aminopropyltriethoxysilane 5.70 5.69 5.69
Saturated Fatty Acid 15.20 15.15 15.15
NH4BF4 1.54 0.68
Na2HPO4 1.45
Water 306.70 337.81 347.76
(Data from US Patent 7,732,047)
Film-former
Coupling agent
Sizing for chopped strand polypropylene reinforcement fiber
30% chopped fiber, 67.8% polypropylene resin, 2.2% polypropylene additive
Wool Processes
Rotary
(Internal Centrifuge)
Cascade
(External Centrifuge)
Flame Attenuation
(Pot & Marble)
Melter/FH
Pot
(or bushing)
Melter/FH
Melt stream
Spinner disc
Attenuation
burner
Melt stream
Spinner
wheels
Burner
Pull
rolls
Air
ring
• High throughput
• 1.5 to 8μm average diameter
• Good fiber quality
• Low temperature (soft)
glasses
• Sensitive to liquidus
• High energy
• Very high throughput
• 3 to 10μm average diameter
• Poor fiber quality (shot)
• Mineral wool and high temp.
(refractory) fiber
• Tolerates very high liquidus
• Low energy
• Low throughput
• 0.1 to 6μm average diameter
• Very good fiber quality
• Capable of relatively wide
viscosity range
• Very sensitive to liquidus
• Very high energy
Rotary Wool Process
Melter
Forehearth
Oven
Collection box
Collection chain
Collection
suction
Slitting, bisecting,
winding,
packaging, etc.
Milling
Conditioning
Packaging
Rotary
fiberizers
Boards & Blankets
Loose-Fill
Bonded products get 3-20%
binder just below fiberizers
-Acrylic -Starch based
-Phenolic -Sugar based
Typically direct
melt with gas or
electric melters.
Melt conditioning can range from
full forehearth to simple diverter
troughs and small holding vessels
Many collection box designs
• 1-10 fiberizers per box
• Collection by chain or drum
• 1-3 collection boxes per line
• Air lappers to distribute fiber
Shaft
Hub
Rotary Fiberizer Details
Combustion:
• Control disc temperature
• Add heat to attenuation
environment
• Attenuation force
Air Ring:
• Attenuation force
• Containment of fiberization
• Containment of column
Electric motor
driven shaft
Internal
burner
Melt
stream
External
burner
Air
ring
Disc
Binder
ring
Air
lapper
(US Patent 8,250,884)
Complex Fiberization Environment
(US Patent 5,601,628)
(US Patent 6,862,901)
The life of a disc is harsh and short
Burner
Air ring
Disc
Glass
• High temperatures
• High stress from rotation (500-1000g’s)
• Molten glass corrosion
• Combustion environment
Good materials science challenge Good modeling challenge
A more challenging strength, ductility, and
corrosion environment than jet turbine blades
Burner
Air ring
Disc
sidewall
Chaotic
Attenuation
Zone
Complex attenuation
zone outside the disc
• Turbulence
• Heat transfer
• Combustion
• Glass flow
• Glass viscosity
Temperature
“speculation”
Rotary Wool Design
Some Considerations
• Glass melt properties (viscosity, liquidus, heat transfer)
• Product requirements (thermal, mechanical)
• Disc alloy (composition, melting and forming process)
• Disc dimensions (diameter, thickness, wall height, flange, etc.)
• Hole pattern (diameter, count, profiling, banding, etc)
• Internal & external combustion energy and placement
• Air ring placement and pressure
• Conditions for disc removal (disc life)
• Glass stream temperature
• Disc throughput (loading)
• Disc rotational speed
• Number of fiberizers in collection box
• Number of collection boxes per line
• Fiber laydown pattern (column formation), air lapper operation)
Shaft
Hub
It is challenging to develop an optimized design because rotary fiberization
is a very complex system of interactions and competing parameters
(US Patent 8,250,884)
Rotary Wool Parameters
Some Typical Ranges
• Glass melt viscosity (temp. at 1000poise) 900 to 1100°C
• Glass melt liquidus temperature 700 to 1100°C
• Average fiber diameter 1.5 to 8 μm
• Average fiber length difficult to characterize
• Disc diameter 25 to 100 cm
• Disc alloy Co-Ni-Cr superalloy
• Number of holes thousands
• Hole diameter 0.4 to 1.0 mm
• Disc rotational speed 1500 to 2500 rpm
• Disc throughput 100 to 1100 kg/hr
• Disc life 20 to 400 hours
• Number of fiberizers in collection box 1 to 10
• Number of collection boxes per line 1 to 3
Rotary Fiberization
Hole Size Profiling
Top holes are typically larger because the glass
coming out of the top holes will experience
more attenuation than the bottom holes
Hole Wear
Hole size increases over
the life of the disc, causing
a fiber diameter increase if
no process adjustments
are made
(US Patent 4,689,061)
(US Patent 8,104,311)
(US Patent 8,250,884)
Devitrification in Discs
Glass chemistry or process upsets can cause devitrification in discs
Can occur in cold corners of disc or in holes as shown below
Rotary Design Variations
(US Patent 4,451,276)
There are many variations, including this “upside-down” disc design
A) Glass melt stream enters
through center of hollow disc shaft
B) Melt stream collects in small
interior slinger disc with large
holes around the sidewall
C) Glass from slinger disc
flies outward to collect in
large “upside-down” disc
D) Fiberization occurs
in a similar fashion to
other discs
Collection Designs
(US Patent 5,268,015)
(US Patent 4,451,276)
Typical Atypical
Cascade (External Centrifuge) Process
Spinner
wheels
Air
slot
Melter/FH
Melt
stream To oven, slitting,
winding, packaging
Collection
(chain or drum)
Cupola melters are commonly
used for mineral wool
Binder
spray
Shot
The cascade process is commonly used for mineral wool
and other high liquidus temperature glasses
• Melt stream temperature is >1400°C
• Viscosity is 15-40poise at the first wheel
• 15-50cm diameter wheels
• 3000-9000 RPM wheel speed
• Air slot around 30-80% of wheel
• Throughput of 2000-7000kg/hr
Cascade Process Detail
(US Patent 5,356,450)
Used for glasses with high liquidus temperature because the melt
doesn’t have an opportunity to devitrify
The melt stream drops onto the wheels at high temperature and isn’t
held in a containment device or pushed through any holes
Air slots
Wheel
Melt
stream
Cascade Design Examples
(US Patent 6,536,241)
(US Patent 5,954,852)
Shot and Fiber Quality
Cascade Advantages: High liquidus temperature glasses and high iron glasses
• Fiber has better high temperature and fire resistance performance
• Lower cost glass raw materials
Cascade Disadvantage: Fiber quality generally not as good as rotary
• Higher shot content
• Lower aspect ratio, shorter
fiber
• Higher thermal conductivity
for the same density (due
in part to shot)
Shot – Non-fiberized
pieces of glass, often
with attenuation “tails”
Mineral Wool Crystallization
• High liquidus temperature glass fibers can
crystallize upon reheating
• Can lead to desirable high temperature &
fire resistance properties
• Illustrates how challenging these glasses
can be for fiberization processes
Fiber cross sections
after heat treatment
Flame Attenuation (Pot & Marble)
Pot
(gas fired)
or
Bushing
(electrically
heated)
Burner
Pull rolls
(control primary
speed and diameter)
Typically marble re-melt
To oven, slitting,
winding, packaging
Collection
(chain or drum)
Binder
spray
Marble re-melt requires more energy than
direct-melt but allows for flexible fiberization
(start/stop, glass composition changes, etc.)
Guide
Primaries
(0.1 to 1.0mm)
1 to 10 pots & burners
per collection box
Marble feeder
Holes
or tips
Can make fiber with average diameter <150nm
Non-bonded
Microfiber
Bonded
Microfiber
Flame Attenuation Close-Up
(US Patent 8,192,195)
Burner
drawing
Attenuation influenced by:
• Primary diameter
• Primary speed
• Primary spacing
• Burner temperature
• Burner pressure
• Burner distance
• Burner slot size
Viscosity and Liquidus Ranges
1000
1100
1200
1300
1400
1500
900
Temperature
(°C)
at
η=1000poise
(T
log3
)
800
700 900 1000 1100 1200 1300 1400 1500
Liquidus Temperature (°C) (Tliq)
Flame
Att.
RCF
(Cascade)
Mineral
Wool
(Cascade)
ΔT = Tlog3 - Tliq
Higher ΔT
Lower ΔT
Viscosity and Liquidus Ranges
1000
1100
1200
1300
1400
1500
900
Temperature
(°C)
at
η=1000poise
(T
log3
)
800
700 900 1000 1100 1200 1300 1400 1500
Liquidus Temperature (°C) (Tliq)
Continuous Filament (Bushing)
Basalt and S-glass fall
outside ideal glass fiber
forming property ranges
but both are produced
commercially
Viscosity and Liquidus Ranges
1000
1100
1200
1300
1400
1500
900
Temperature
(°C)
at
η=1000poise
(T
log3
)
800
700 900 1000 1100 1200 1300 1400 1500
Liquidus Temperature (°C) (Tliq)
Continuous Filament (Bushing)
Basalt and S-glass fall
outside ideal glass fiber
forming property ranges
but both are produced
commercially
What can happen if you go too far to the lower right
Viscosity and Liquidus Ranges
1000
1100
1200
1300
1400
1500
900
Temperature
(°C)
at
η=1000poise
(T
log3
)
800
700 900 1000 1100 1200 1300 1400 1500
Liquidus Temperature (°C) (Tliq)
Flame
Att.
RCF
(Cascade)
Mineral
Wool
(Cascade)
Wool Processes
High liquidus glasses
with limited fiberization
alternatives
Fiber Diameter Distributions
0 5 10 15 20
Fiber diameter (μm)
Diameter distribution size and shape can vary widely
depending on the process and how it is operated
Frequency
(normalized
to
peak
value)
Continuous
filament
bushing
Cascade
Rotary
Representative
examples
Glass Composition Considerations
• Raw material costs
• Viscosity
• Liquidus temperature
• Melting enthalpy
• Electrical conductivity (melt)
• Surface tension (melt)
• Fiber tensile strength (and retention)
• Elastic modulus
• Chemical durability
• Acidic
• Neutral
• Basic
• Unique environments
• Radiative heat transfer (melt & fiber)
• Density
• Refractive index
• Surface reactivity (sizing, binder, resin compatibility)
Glass compositions are designed to achieve viable balance of properties
Items on this partial list will
vary in importance depending
on process and application
Future Development
• Compositions and processes
are continually being modified
and improved
• Improved product properties
• Energy reduction
• Efficiency improvement
• New markets/applications
Other Methods & Variations
Paramelter
Small self-contained unit with
batch feed on top, electrically
heated, and a small CF bushing
on the bottom
(US Patent 4,262,158)
Rotary Continuous Filament
Using a rotary disc as a rotating
bushing to collect twisted
continuous filament strands
(US Patent 3,250,602)
(with varying degrees of practicality)
Other Methods & Variations
Hollow Fibers
(US Patent 4,758,259) (US Patent 5,674,307)
(with varying degrees of practicality)
Continuous filament Rotary
Other Methods & Variations
Bi-Component Fibers
Rotary process
(US Patent 6,167,729)
(with varying degrees of practicality)
Other Methods & Variations
• Basalt continuous filament (low throughput, small bushings)
• Rotary “Mineral Wool” (low throughput, high energy, extremes for disc metallurgy
• Sliver process (large drum, collection blade)
• Silica glass fiber (acid leach, draw from pre-form, sol-gel spun)
• Steam blown mineral wool (predecessor to cascade process)
• Non-round fiber cross section (oval or tri-lobed)
There are many variations on these methods (lots of strange and interesting patents)
(US Patent 5,462,571)
(US Patent 4,666,485)
References and Suggested Reading
Books
J. G. Mohr and W. P. Rowe, Fiber Glass, Van Nostrand Reinhold Company, New York,
1978
F. T. Wallenberger and P. A. Bingham (Editors), Fiberglass and Glass Technology,
Springer, New York, 2010
K. L. Loewenstein, The Manufacturing Technology of Continuous Glass Fibres,
Elsevier, 1993
Articles
F. T. Wallenberger, J. C. Watson, and H. Li, “Fiber Glass”, ASM Handbook, Vol. 21:
Composites (#06781G), 2001
S. Rekhson et al, “Attenuation and Breakage in the Continuous Glass Fiber Drawing
Process”, Ceramic Engineering & Science Proceedings, vol. 25, No. 1, page 179
S. Krishnan and L. R. Glicksman, “A Two-Dimensional Analysis of a Heated Jet at
Low Reynolds Numbers”, J. Am. Soc. Mech. Engineers, vol. 35D, page 355, 1971
US Patents
Continuous Filament Wool (Discontinuous)
7,980,099
5,017,205
7,732,047
8,250,884
4,451,276
5,356,450
Thanks for your attention!
Questions?
Lectures available at:
www.lehigh.edu/imi
Elam Leed
Johns Manville
Elam.Leed@jm.com
www.jm.com

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Lecture14_Leed_Fiberglass production and engineering

  • 1. Lectures available at: www.lehigh.edu/imi Sponsored by US National Science Foundation (DMR-0844014) Spring 2015 Glass Processing Course Lecture 14. Fiberglass Processing Elam Leed Johns Manville Elam.Leed@jm.com www.jm.com
  • 2. Outline • Brief background • Quick note on viscosity and liquidus temperature • Continuous filament fiber • Process overview • Bushings design and operation • Importance of sizing • Wool fiber (discontinuous) • Rotary process (internal centrifuge) • Cascade process (external centrifuge) • Flame attenuation process (pot & marble) • More about viscosity and liquidus temperature • A few other process variations
  • 3. Stretching Glass is Fun • The first fibers might have been made by accident • Glass fibers have been made for many centuries, originally for art and decoration • Fiber started to be manufactured for practical uses in the late 1800’s • The process was improved and scaled up over decades • Manufacturing improvements continue to help expand the global usage of glass fiber Glass rod Fire Winding drum
  • 4. Fiber Forming What is the fundamental purpose? Making surface area • 0.05 to 15 square meters per gram • A large wool manufacturing line can produce 2000m2/s or 170km2 per day • Interface, coupling, filtration Making tortured paths • Acoustic paths • Filtration paths (air, liquid) • Fracture propagation paths (composites) • Thermal paths (conduction, convection, radiation)
  • 5. Continuous Filament vs. Wool Continuous Filament Wool (Discontinuous) Processing Pulled in a continuous filament parallel with other strands (often chopped downstream) Process inherently creates discontinuous sections of fiber that have somewhat random orientation Typical Fiber Diameters 4-30 micron 0.2 to 10 micron Glass Types E-glass, C-glass, R-glass, S-glass, AR-glass, A-glass, D-glass, basalt, others Soft alkali borosilicates, mineral wool, modified slag & basalt, RCF, others Uses Reinforcement (chopped fiber, rovings, wovens, non-wovens) filtration, separation, facers, thermal insulation, fireblocking Thermal insulation (blanket, board, pipe, paper), acoustic insulation, filtration, separation
  • 6. Generalized Process Flow Batching Melting Conditioning Fiberization Cold (Warm) Processing Packaging Temperature (Viscosity) Time Room Temp Glass Trans. (Tg) Softening Point η = 1000 poise η < 100 poise Fiberization Cold (Warm) Processing Preparing glass for fiberization Making fiber more useful 1 to 300 tons/day, gas and/or electric Forehearth, dwell tank, or just melt stream Bushing, rotary, cascade, flame attenuated Winding, chopping, sizing, binding, twisting, assembling, pressing, screening, drying, curing
  • 7. Viscosity Softening point Melting & conditioning η = 1000 poise Fiber forming • Glass passes through the fiber forming viscosity range very fast, so in many cases the slope of the viscosity curve is not a key glass design parameter • Liquidus temperature relative to viscosity can be a much more critical parameter…… T log3
  • 8. Viscosity & Liquidus Temperature Softening point Melting & conditioning η = 1000 poise Fiber forming • The liquidus temperature relative to a viscosity reference point such as Tlog3 is important for glass chemistry design • As liquidus temperature increases, the risk of devitrification increases Liquidus A (good) Liquidus B (not so good) A B
  • 9. Viscosity & Liquidus Temperature Melting & conditioning η = 1000 poise Fiber forming • Liquidus temperature can vary widely depending on composition • Some processes are more tolerant of high liquidus temperature glass Liquidus A (good) Liquidus C (bad) Devitrification Bushing tip Bushing tip
  • 10. Continuous Filament Process Melter Conditioning channel Distribution channel Legs Bushings Forehearth Melter & Forehearth Layout (top view) Leg/Bushing Cross Section (end view) Burner Glass melt Thermocouples Water spray Bushing Flow block Sizing applicator Guide pulley • Originally marble re-melt, now almost all direct melt • Many different forehearth layouts • Forehearth designed to deliver target glass temperature and head pressure above each bushing • Enclosed and conditioned forming room(s) underneath legs • Electrically heated precious metal bushings Typical E-glass Process
  • 11. Continuous Filament Bushings ΔV Tips Cooling fins Support structure (internal or external) • Platinum alloyed with 5-25% rhodium for high temperature strength • Low voltage applied across bushing for resistive heating (high current) • Usually mounted into a frame and surrounded on sides with refractory for insulation and support • Screen improves temperature distribution and reduces effective head pressure Terminal (ear) Flange Screen • 500 to 7000 tips per bushing • Uniform temperature across the tip plate is critical for uniform flow per tip Design Considerations • Tip dia. and length • Tip number and spacing • Screen thickness and flow resistance • Support structure • Cooling fins • Part thicknesses (cooling fins not shown for clarity)
  • 12. Bushing Design Examples (US Patent 7,980,099) Flange External mounting brackets Sidewall Tips Tip plate Terminal (ear) Screen Support structure
  • 13. Bushing Design Examples (US Patent Application 11/638,757) Flange Sidewall Tips Tip plate Screen Support structure Fibers Refractory Mounting frame
  • 14. (US Patent Application 11/320,135) Bushing Design Examples (US Patent Application 10/702,004) Flange Sidewall Tips Tip plate Support structure Fibers Refractory Mounting frame Cooling fins Tips Tip plate Sidewall Support structure Cooling fin Cooling fin manifold
  • 15. Bushing Operation η = 10,000 poise η = 1000 poise η = 200 poise (estimated tip exit viscosity) Fiber Diameter Flow • Effective head pressure • Tip geometry (dia., length) • Glass temperature (visc.) Pulling Speed • Winder or chopper Operation can be very sensitive to defects in the glass • Stones • Refractory • Batch/batch reactants • Devitrification • Contamination High viscosity results in high fiber forming stress • Seeds • Inhomogeneity (cord) Low viscosity can lead to cone instability
  • 16. Fiber Forming Stress and Breaks • A bushing is like an in-line high speed tensile strength test • 100,000 to 500,000km of fiber per hour per bushing is tested • Stress level from 10-200MPa at temperatures from RT to >Tg. Modeling is used to predict stress profiles with varying conditions and designs S. Rekhson et al, “Attenuation and Breakage in the Continuous Glass Fiber Drawing Process”, Ceramic Engineering & Science Proceedings, vol. 25, No. 1, page 179. Failure stress Failure probability (A) (B) Fiber forming stress range A) Sample size (length of fiber) is so large that a weak spot is eventually found B) Defects cause an increase in fiber forming stress to the point of break And/or C) High stress from a cold tip (C)
  • 17. Tips and Contact Angle (US Patent 5,017,205) • Tips are typically 1.0 to 2.5mm inside diameter • Tips size needs to match process requirements • Tip size strongly influences flow rate and fiber forming stress • Some tips have restricted outlets to reduce stress but still have sufficiently high flow rate • The wetting (contact angle) of the molten glass on the alloy can influence forming cone shape • Wetting can also influence bead formation when a fiber breaks • It is desirable to have the glass quickly form a bead that drops down to allow for bushing restart Wetting (“flooding”) Non- wetting Tapered tip Wetting (“flooding”) Non-wetting layer (Pt-Au alloy)
  • 18. Collecting Breakout Defects Al-Si defect from contaminant Collecting and identifying the cause of a break can be very difficult • In some cases the tip that broke first can be identified and the bead collected • Optical microscopy and SEM/EDS can help with identification
  • 20. Continuous Filament Process Chopper Wet Chopped Strand (7-18% H2O, 0.1 to 0.5% sizing solids) Dryer Dry Chopped Strand (0.2 to 2% sizing solids) Winder Dryer Chopper Assembled Roving (0.2 to 2% sizing solids) Dryer Winder Direct Rovings (0.2 to 2% sizing solids) Sizing Applicator Leg Bushing
  • 21. Continuous Filament Sizing glass binder/matrix interface/coupling • Tailored to specific application • Critical for downstream processing, handling, and physical performance • Key roles • Protection from damage (physical & chemical) • Lubrication • Bundle/strand integrity • Dispersion • Coupling • 1 to 10 components • Silane (e.g. amino-propyl silane) • Film-formers • Lubricants • Enhancers • “Magic ingredients” • Other
  • 22. Sizing Performance: Coupling Role of silane in the moisture resistance of a fiber/resin bond Wet chop fiber Non-woven mat Sized with water or water+silane Tested as-made versus hot water aged Mat tensile strength – dry Mat tensile strength – hot/wet Without silane, the interface is easily weakened by water
  • 23. Application Example: Reinforced Thermoplastic • Proper sizing chemistry and processing is very important for composites • Chopped fiber is further broken down in compounding but still delivers a significant increase in strength J. H. A. van der Woude and E. L. Lawton, ‘Composite Design and Engineering’ in Fiberglass and Glass Technology, F. T. Wallenberger and P. A. Bingham (Editors), Springer, New York, pp. 125-173, 2010
  • 24. “Enhancers” (lubrication, wetting, hydrophobic interphase promotion, etc) Sizing Chemistry Example C1 S26 S29 Modified Polypropylene Emulsion 40.71 43.00 43.00 Aminopropyltriethoxysilane 5.70 5.69 5.69 Saturated Fatty Acid 15.20 15.15 15.15 NH4BF4 1.54 0.68 Na2HPO4 1.45 Water 306.70 337.81 347.76 (Data from US Patent 7,732,047) Film-former Coupling agent Sizing for chopped strand polypropylene reinforcement fiber 30% chopped fiber, 67.8% polypropylene resin, 2.2% polypropylene additive
  • 25. Wool Processes Rotary (Internal Centrifuge) Cascade (External Centrifuge) Flame Attenuation (Pot & Marble) Melter/FH Pot (or bushing) Melter/FH Melt stream Spinner disc Attenuation burner Melt stream Spinner wheels Burner Pull rolls Air ring • High throughput • 1.5 to 8μm average diameter • Good fiber quality • Low temperature (soft) glasses • Sensitive to liquidus • High energy • Very high throughput • 3 to 10μm average diameter • Poor fiber quality (shot) • Mineral wool and high temp. (refractory) fiber • Tolerates very high liquidus • Low energy • Low throughput • 0.1 to 6μm average diameter • Very good fiber quality • Capable of relatively wide viscosity range • Very sensitive to liquidus • Very high energy
  • 26. Rotary Wool Process Melter Forehearth Oven Collection box Collection chain Collection suction Slitting, bisecting, winding, packaging, etc. Milling Conditioning Packaging Rotary fiberizers Boards & Blankets Loose-Fill Bonded products get 3-20% binder just below fiberizers -Acrylic -Starch based -Phenolic -Sugar based Typically direct melt with gas or electric melters. Melt conditioning can range from full forehearth to simple diverter troughs and small holding vessels Many collection box designs • 1-10 fiberizers per box • Collection by chain or drum • 1-3 collection boxes per line • Air lappers to distribute fiber
  • 27. Shaft Hub Rotary Fiberizer Details Combustion: • Control disc temperature • Add heat to attenuation environment • Attenuation force Air Ring: • Attenuation force • Containment of fiberization • Containment of column Electric motor driven shaft Internal burner Melt stream External burner Air ring Disc Binder ring Air lapper (US Patent 8,250,884)
  • 28. Complex Fiberization Environment (US Patent 5,601,628) (US Patent 6,862,901) The life of a disc is harsh and short Burner Air ring Disc Glass • High temperatures • High stress from rotation (500-1000g’s) • Molten glass corrosion • Combustion environment Good materials science challenge Good modeling challenge A more challenging strength, ductility, and corrosion environment than jet turbine blades Burner Air ring Disc sidewall Chaotic Attenuation Zone Complex attenuation zone outside the disc • Turbulence • Heat transfer • Combustion • Glass flow • Glass viscosity Temperature “speculation”
  • 29. Rotary Wool Design Some Considerations • Glass melt properties (viscosity, liquidus, heat transfer) • Product requirements (thermal, mechanical) • Disc alloy (composition, melting and forming process) • Disc dimensions (diameter, thickness, wall height, flange, etc.) • Hole pattern (diameter, count, profiling, banding, etc) • Internal & external combustion energy and placement • Air ring placement and pressure • Conditions for disc removal (disc life) • Glass stream temperature • Disc throughput (loading) • Disc rotational speed • Number of fiberizers in collection box • Number of collection boxes per line • Fiber laydown pattern (column formation), air lapper operation) Shaft Hub It is challenging to develop an optimized design because rotary fiberization is a very complex system of interactions and competing parameters (US Patent 8,250,884)
  • 30. Rotary Wool Parameters Some Typical Ranges • Glass melt viscosity (temp. at 1000poise) 900 to 1100°C • Glass melt liquidus temperature 700 to 1100°C • Average fiber diameter 1.5 to 8 μm • Average fiber length difficult to characterize • Disc diameter 25 to 100 cm • Disc alloy Co-Ni-Cr superalloy • Number of holes thousands • Hole diameter 0.4 to 1.0 mm • Disc rotational speed 1500 to 2500 rpm • Disc throughput 100 to 1100 kg/hr • Disc life 20 to 400 hours • Number of fiberizers in collection box 1 to 10 • Number of collection boxes per line 1 to 3
  • 31. Rotary Fiberization Hole Size Profiling Top holes are typically larger because the glass coming out of the top holes will experience more attenuation than the bottom holes Hole Wear Hole size increases over the life of the disc, causing a fiber diameter increase if no process adjustments are made (US Patent 4,689,061) (US Patent 8,104,311) (US Patent 8,250,884)
  • 32. Devitrification in Discs Glass chemistry or process upsets can cause devitrification in discs Can occur in cold corners of disc or in holes as shown below
  • 33. Rotary Design Variations (US Patent 4,451,276) There are many variations, including this “upside-down” disc design A) Glass melt stream enters through center of hollow disc shaft B) Melt stream collects in small interior slinger disc with large holes around the sidewall C) Glass from slinger disc flies outward to collect in large “upside-down” disc D) Fiberization occurs in a similar fashion to other discs
  • 34. Collection Designs (US Patent 5,268,015) (US Patent 4,451,276) Typical Atypical
  • 35. Cascade (External Centrifuge) Process Spinner wheels Air slot Melter/FH Melt stream To oven, slitting, winding, packaging Collection (chain or drum) Cupola melters are commonly used for mineral wool Binder spray Shot The cascade process is commonly used for mineral wool and other high liquidus temperature glasses
  • 36. • Melt stream temperature is >1400°C • Viscosity is 15-40poise at the first wheel • 15-50cm diameter wheels • 3000-9000 RPM wheel speed • Air slot around 30-80% of wheel • Throughput of 2000-7000kg/hr Cascade Process Detail (US Patent 5,356,450) Used for glasses with high liquidus temperature because the melt doesn’t have an opportunity to devitrify The melt stream drops onto the wheels at high temperature and isn’t held in a containment device or pushed through any holes Air slots Wheel Melt stream
  • 37. Cascade Design Examples (US Patent 6,536,241) (US Patent 5,954,852)
  • 38. Shot and Fiber Quality Cascade Advantages: High liquidus temperature glasses and high iron glasses • Fiber has better high temperature and fire resistance performance • Lower cost glass raw materials Cascade Disadvantage: Fiber quality generally not as good as rotary • Higher shot content • Lower aspect ratio, shorter fiber • Higher thermal conductivity for the same density (due in part to shot) Shot – Non-fiberized pieces of glass, often with attenuation “tails”
  • 39. Mineral Wool Crystallization • High liquidus temperature glass fibers can crystallize upon reheating • Can lead to desirable high temperature & fire resistance properties • Illustrates how challenging these glasses can be for fiberization processes Fiber cross sections after heat treatment
  • 40. Flame Attenuation (Pot & Marble) Pot (gas fired) or Bushing (electrically heated) Burner Pull rolls (control primary speed and diameter) Typically marble re-melt To oven, slitting, winding, packaging Collection (chain or drum) Binder spray Marble re-melt requires more energy than direct-melt but allows for flexible fiberization (start/stop, glass composition changes, etc.) Guide Primaries (0.1 to 1.0mm) 1 to 10 pots & burners per collection box Marble feeder Holes or tips Can make fiber with average diameter <150nm Non-bonded Microfiber Bonded Microfiber
  • 41. Flame Attenuation Close-Up (US Patent 8,192,195) Burner drawing Attenuation influenced by: • Primary diameter • Primary speed • Primary spacing • Burner temperature • Burner pressure • Burner distance • Burner slot size
  • 42. Viscosity and Liquidus Ranges 1000 1100 1200 1300 1400 1500 900 Temperature (°C) at η=1000poise (T log3 ) 800 700 900 1000 1100 1200 1300 1400 1500 Liquidus Temperature (°C) (Tliq) Flame Att. RCF (Cascade) Mineral Wool (Cascade) ΔT = Tlog3 - Tliq Higher ΔT Lower ΔT
  • 43. Viscosity and Liquidus Ranges 1000 1100 1200 1300 1400 1500 900 Temperature (°C) at η=1000poise (T log3 ) 800 700 900 1000 1100 1200 1300 1400 1500 Liquidus Temperature (°C) (Tliq) Continuous Filament (Bushing) Basalt and S-glass fall outside ideal glass fiber forming property ranges but both are produced commercially
  • 44. Viscosity and Liquidus Ranges 1000 1100 1200 1300 1400 1500 900 Temperature (°C) at η=1000poise (T log3 ) 800 700 900 1000 1100 1200 1300 1400 1500 Liquidus Temperature (°C) (Tliq) Continuous Filament (Bushing) Basalt and S-glass fall outside ideal glass fiber forming property ranges but both are produced commercially What can happen if you go too far to the lower right
  • 45. Viscosity and Liquidus Ranges 1000 1100 1200 1300 1400 1500 900 Temperature (°C) at η=1000poise (T log3 ) 800 700 900 1000 1100 1200 1300 1400 1500 Liquidus Temperature (°C) (Tliq) Flame Att. RCF (Cascade) Mineral Wool (Cascade) Wool Processes High liquidus glasses with limited fiberization alternatives
  • 46. Fiber Diameter Distributions 0 5 10 15 20 Fiber diameter (μm) Diameter distribution size and shape can vary widely depending on the process and how it is operated Frequency (normalized to peak value) Continuous filament bushing Cascade Rotary Representative examples
  • 47. Glass Composition Considerations • Raw material costs • Viscosity • Liquidus temperature • Melting enthalpy • Electrical conductivity (melt) • Surface tension (melt) • Fiber tensile strength (and retention) • Elastic modulus • Chemical durability • Acidic • Neutral • Basic • Unique environments • Radiative heat transfer (melt & fiber) • Density • Refractive index • Surface reactivity (sizing, binder, resin compatibility) Glass compositions are designed to achieve viable balance of properties Items on this partial list will vary in importance depending on process and application Future Development • Compositions and processes are continually being modified and improved • Improved product properties • Energy reduction • Efficiency improvement • New markets/applications
  • 48. Other Methods & Variations Paramelter Small self-contained unit with batch feed on top, electrically heated, and a small CF bushing on the bottom (US Patent 4,262,158) Rotary Continuous Filament Using a rotary disc as a rotating bushing to collect twisted continuous filament strands (US Patent 3,250,602) (with varying degrees of practicality)
  • 49. Other Methods & Variations Hollow Fibers (US Patent 4,758,259) (US Patent 5,674,307) (with varying degrees of practicality) Continuous filament Rotary
  • 50. Other Methods & Variations Bi-Component Fibers Rotary process (US Patent 6,167,729) (with varying degrees of practicality)
  • 51. Other Methods & Variations • Basalt continuous filament (low throughput, small bushings) • Rotary “Mineral Wool” (low throughput, high energy, extremes for disc metallurgy • Sliver process (large drum, collection blade) • Silica glass fiber (acid leach, draw from pre-form, sol-gel spun) • Steam blown mineral wool (predecessor to cascade process) • Non-round fiber cross section (oval or tri-lobed) There are many variations on these methods (lots of strange and interesting patents) (US Patent 5,462,571) (US Patent 4,666,485)
  • 52. References and Suggested Reading Books J. G. Mohr and W. P. Rowe, Fiber Glass, Van Nostrand Reinhold Company, New York, 1978 F. T. Wallenberger and P. A. Bingham (Editors), Fiberglass and Glass Technology, Springer, New York, 2010 K. L. Loewenstein, The Manufacturing Technology of Continuous Glass Fibres, Elsevier, 1993 Articles F. T. Wallenberger, J. C. Watson, and H. Li, “Fiber Glass”, ASM Handbook, Vol. 21: Composites (#06781G), 2001 S. Rekhson et al, “Attenuation and Breakage in the Continuous Glass Fiber Drawing Process”, Ceramic Engineering & Science Proceedings, vol. 25, No. 1, page 179 S. Krishnan and L. R. Glicksman, “A Two-Dimensional Analysis of a Heated Jet at Low Reynolds Numbers”, J. Am. Soc. Mech. Engineers, vol. 35D, page 355, 1971 US Patents Continuous Filament Wool (Discontinuous) 7,980,099 5,017,205 7,732,047 8,250,884 4,451,276 5,356,450
  • 53. Thanks for your attention! Questions? Lectures available at: www.lehigh.edu/imi Elam Leed Johns Manville Elam.Leed@jm.com www.jm.com