Spring 2015 Glass Processing Course

Lecture 14. Fiberglass Processing

Elam Leed
Johns Manville
[email protected]
www.jm.com

Lectures available at:

www.lehigh.edu/imi
Sponsored by US National Science Foundation (DMR-0844014)
 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

Winding
Glass rod drum
Fire

• 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
 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)
Process inherently creates
Pulled in a continuous filament
discontinuous sections of fiber
Processing parallel with other strands
that have somewhat random
(often chopped downstream)
orientation
Typical Fiber
Diameters
4-30 micron 0.2 to 10 micron
E-glass, C-glass, R-glass, Soft alkali borosilicates, mineral
Glass Types S-glass, AR-glass, A-glass, wool, modified slag & basalt,
D-glass, basalt, others RCF, others

Reinforcement (chopped fiber,

Thermal insulation (blanket,
rovings, wovens, non-wovens)
Uses board, pipe, paper), acoustic
filtration, separation, facers,
insulation, filtration, separation
thermal insulation, fireblocking
 Generalized Process Flow
Fiberization Cold (Warm) Packaging
Batching Melting Conditioning
Processing

1 to 300 Forehearth, dwell Bushing, rotary, Winding, chopping,

tons/day, gas tank, or just melt cascade, flame sizing, binding,
and/or electric stream attenuated twisting, assembling,
pressing, screening,
drying, curing

η < 100 poise

Temperature
(Viscosity)

η = 1000 poise
Fiberization

Softening Point Cold (Warm)

Glass Trans. (Tg) Processing
Room Temp

Preparing glass for fiberization Making fiber more useful

Time
 Viscosity
Softening point

Fiber
forming

η = 1000 poise

Tlog3 Melting &

conditioning

• 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……
 Viscosity & Liquidus Temperature
Softening point

Liquidus B (not so good)

Fiber
Liquidus A (good) forming

η = 1000 poise
A

B Melting &
conditioning

• 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
 Viscosity & Liquidus Temperature
Liquidus A (good) Liquidus C (bad)
Bushing Bushing
tip tip

Devitrification

Fiber
forming

η = 1000 poise

Melting &
conditioning

• Liquidus temperature can vary widely depending on composition

• Some processes are more tolerant of high liquidus temperature glass
 Continuous Filament Process
Typical E-glass Process

Melter & Forehearth Layout (top view) Leg/Bushing Cross Section

(end view)
Conditioning
channel
Burner
Melter Legs
Thermocouples
Distribution Glass melt
channel
Flow block
Forehearth Bushings Bushing
Water spray

• Originally marble re-melt, now almost all direct melt

• Many different forehearth layouts
• Forehearth designed to deliver target glass Sizing applicator
temperature and head pressure above each bushing
Guide pulley
• Enclosed and conditioned forming room(s)
underneath legs
• Electrically heated precious metal bushings
 Continuous Filament Bushings
• Platinum alloyed with 5-25% rhodium for ΔV
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 • 500 to 7000 tips per bushing
• Screen improves temperature distribution • Uniform temperature across the tip
and reduces effective head pressure plate is critical for uniform flow per tip
Screen Flange

Design Considerations
• Tip dia. and length
Terminal
(ear) • Tip number and spacing
Cooling fins Tips Support structure
(internal or external) • Screen thickness and
flow resistance
• Support structure
• Cooling fins
• Part thicknesses
(cooling fins not shown for clarity)
 Bushing Design Examples

Flange
Screen

External
mounting
brackets Sidewall Tips
Tip
plate
Support
structure

Terminal
(US Patent 7,980,099) (ear)
 Bushing Design Examples

Screen
Flange

Refractory

Sidewall Tip plate

Tips

Mounting
frame Support Fibers
structure

(US Patent Application 11/638,757)

 Bushing Design Examples
Sidewall
Tip plate Tips

Cooling fin
manifold

Support (US Patent Application 10/702,004)

Cooling fin
structure
Flange
Sidewall Refractory

Cooling fins
Mounting Tip plate Tips
frame

Support
structure

Fibers
(US Patent Application 11/320,135)
 Bushing Operation
Fiber Diameter
Flow
• Effective head pressure
• Tip geometry (dia., length)
• Glass temperature (visc.)
Pulling Speed
• Winder or chopper

(estimated tip exit viscosity) η = 10,000 poise η = 1000 poise η = 200 poise
High viscosity results in Low viscosity can
high fiber forming stress lead to cone instability

Operation can be very sensitive to defects in the glass

• Stones • Seeds
• Refractory
• Inhomogeneity (cord)
• Batch/batch reactants
• Devitrification
• Contamination
 Fiber Forming Stress and Breaks
Modeling is used to
predict stress profiles
with varying conditions
and designs

Fiber forming
stress range
Failure probability

(B)

(C)

(A) Failure stress

A) Sample size (length of

fiber) is so large that a weak
spot is eventually found
B) Defects cause an increase • A bushing is like an in-line high speed tensile strength test
in fiber forming stress to the
point of break • 100,000 to 500,000km of fiber per hour per bushing is tested
And/or • Stress level from 10-200MPa at temperatures from RT to >Tg.
C) High stress from a cold tip
S. Rekhson et al, “Attenuation and Breakage in the Continuous Glass Fiber Drawing
Process”, Ceramic Engineering & Science Proceedings, vol. 25, No. 1, page 179.
 Tips and Contact Angle
Non-wetting layer
(Pt-Au alloy)
• Tips are typically 1.0 to 2.5mm
inside diameter
• Tips size needs to match process
requirements Non-
wetting
• Tip size strongly influences flow rate Tapered
and fiber forming stress tip
Wetting
• Some tips have restricted outlets to (“flooding”)
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 Wetting
formation when a fiber breaks (“flooding”)

• It is desirable to have the glass

quickly form a bead that drops down
to allow for bushing restart

(US Patent 5,017,205)

 Collecting Breakout Defects
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

Al-Si defect from contaminant

 Identifying Defects
SEM/EDS

Optical Microscopy

Defect source: zircon refractory

 Continuous Filament Process
Leg

Bushing Wet Chopped Strand

Sizing (7-18% H2O, 0.1 to 0.5%
Applicator Chopper sizing solids)

Dryer
Winder
Dry Chopped Strand
(0.2 to 2% sizing solids)

Chopper
Dryer

Dryer

Assembled Roving
(0.2 to 2% sizing solids)
Direct Rovings
(0.2 to 2% sizing solids) Winder
 Continuous Filament Sizing
• Tailored to specific application
• Critical for downstream
processing, handling, and
physical performance
• Key roles
• Protection from damage
(physical & chemical)
• Lubrication
• Bundle/strand integrity
• Dispersion binder/matrix
• Coupling
• 1 to 10 components
interface/coupling
• Silane (e.g. amino-propyl silane)
• Film-formers
• Lubricants glass
• 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

Tested as-made
Sized with versus hot water
water or aged
water+silane

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

Wallenberger and P. A. Bingham (Editors),

J. H. A. van der Woude and E. L. Lawton,

Springer, New York, pp. 125-173, 2010

‘Composite Design and Engineering’ in
Fiberglass and Glass Technology, F. T.
 Sizing Chemistry Example
Sizing for chopped strand polypropylene reinforcement fiber
C1 S26 S29
Film-former Modified Polypropylene Emulsion 40.71 43.00 43.00
Coupling agent Aminopropyltriethoxysilane 5.70 5.69 5.69
Saturated Fatty Acid 15.20 15.15 15.15
“Enhancers”
(lubrication, wetting, NH4BF4 1.54 0.68
hydrophobic interphase Na2HPO4 1.45
promotion, etc)
Water 306.70 337.81 347.76

30% chopped fiber, 67.8% polypropylene resin, 2.2% polypropylene additive

(Data from US Patent 7,732,047)

 Wool Processes
Rotary Cascade Flame Attenuation
(Internal Centrifuge) (External Centrifuge) (Pot & Marble)

Melter/FH Melter/FH
Pot
Melt stream
(or bushing)
Attenuation
Melt stream burner

Pull
Air rolls
Spinner disc ring

Burner
Spinner
wheels

• High throughput • Very high throughput • Low throughput

• 1.5 to 8μm average diameter • 3 to 10μm average diameter • 0.1 to 6μm average diameter
• Good fiber quality • Poor fiber quality (shot) • Very good fiber quality
• Low temperature (soft) • Mineral wool and high temp. • Capable of relatively wide
glasses (refractory) fiber viscosity range
• Sensitive to liquidus • Tolerates very high liquidus • Very sensitive to liquidus
• High energy • Low energy • Very high energy
 Rotary Wool Process
Typically direct Melt conditioning can range from
melt with gas or full forehearth to simple diverter
electric melters. troughs and small holding vessels
Boards & Blankets

Bonded products get 3-20%

Melter binder just below fiberizers
Forehearth
-Acrylic -Starch based
-Phenolic -Sugar based
Rotary
fiberizers
Oven
Collection box Slitting, bisecting,
winding,
Collection chain packaging, etc.

Collection Milling
suction
Loose-Fill

Many collection box designs

Conditioning
• 1-10 fiberizers per box
• Collection by chain or drum
• 1-3 collection boxes per line
Packaging
• Air lappers to distribute fiber
 Rotary Fiberizer Details
Combustion:
Electric motor
• Control disc temperature driven shaft
• Add heat to attenuation
environment Melt
• Attenuation force stream

External
burner

Shaft
Internal
burner

Hub

Air
Disc ring

Air Ring: Binder

ring
• Attenuation force
• Containment of fiberization (US Patent 8,250,884)
• Containment of column
Air
lapper
 Complex Fiberization Environment
The life of a disc is harsh and short
Chaotic
Attenuation
Burner Zone
Burner

Temperature
“speculation”

Glass Air ring

Air ring
Complex attenuation
zone outside the disc
(US Patent 6,862,901)
Disc • Turbulence
• Heat transfer
• High temperatures Disc
• Combustion
• High stress from rotation (500-1000g’s) sidewall
• Glass flow
• Molten glass corrosion
• Glass viscosity
• Combustion environment
A more challenging strength, ductility, and (US Patent 5,601,628)
corrosion environment than jet turbine blades

Good materials science challenge Good modeling challenge

 Rotary Wool Design
It is challenging to develop an optimized design because rotary fiberization
is a very complex system of interactions and competing parameters
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

Shaft
• Disc throughput (loading)
• Disc rotational speed
• Number of fiberizers in collection box Hub

• Number of collection boxes per line

• Fiber laydown pattern (column formation), air lapper operation)
(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

(US Patent 4,689,061)

(US Patent 8,104,311)

Hole Wear
Hole size increases over
the life of the disc, causing
a fiber diameter increase if
no process adjustments
are made

(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
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 C) Glass from slinger disc

interior slinger disc with large flies outward to collect in D) Fiberization occurs
holes around the sidewall large “upside-down” disc in a similar fashion to
other discs

(US Patent 4,451,276)

 Collection Designs
Typical Atypical

(US Patent 4,451,276)

(US Patent 5,268,015)
 Cascade (External Centrifuge) Process
The cascade process is commonly used for mineral wool
and other high liquidus temperature glasses

Melter/FH Cupola melters are commonly

used for mineral wool

Melt
stream Binder To oven, slitting,
spray winding, packaging

Air
slot Collection
(chain or drum)

Spinner
wheels
Shot
 Cascade Process Detail
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
Melt
stream

• Melt stream temperature is >1400°C

• Viscosity is 15-40poise at the first wheel
• 15-50cm diameter wheels Wheel
• 3000-9000 RPM wheel speed Air slots

• Air slot around 30-80% of wheel

• Throughput of 2000-7000kg/hr

(US Patent 5,356,450)

 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)
Typically marble re-melt
Marble feeder Marble re-melt requires more energy than
direct-melt but allows for flexible fiberization
(start/stop, glass composition changes, etc.)

Pot
(gas fired)
or 1 to 10 pots & burners Bonded
Microfiber
Bushing per collection box
(electrically
heated)

Primaries Holes To oven, slitting,

(0.1 to 1.0mm) Binder
or tips winding, packaging
spray
Pull rolls
(control primary
speed and diameter)

Guide Collection Non-bonded

(chain or drum) Microfiber

Burner

Can make fiber with average diameter <150nm

 Flame Attenuation Close-Up
Attenuation influenced by:
• Primary diameter
• Primary speed
• Primary spacing
• Burner temperature
• Burner pressure
• Burner distance
• Burner slot size

Burner
drawing
(US Patent 8,192,195)
 Viscosity and Liquidus Ranges
1500

ΔT = Tlog3 - Tliq
Temperature (°C) at η=1000poise (Tlog3)

1400

Higher ΔT
1300 Lower ΔT

(Cascade)
RCF
1200
Mineral
Wool
(Cascade)
1100
Flame
Att.

1000

900
700 800 900 1000 1100 1200 1300 1400 1500
Liquidus Temperature (°C) (Tliq)
 Viscosity and Liquidus Ranges
1500

Continuous Filament (Bushing)

Temperature (°C) at η=1000poise (Tlog3)

1400

1300

1200

Basalt and S-glass fall

outside ideal glass fiber
1100 forming property ranges
but both are produced
commercially
1000

900
700 800 900 1000 1100 1200 1300 1400 1500
Liquidus Temperature (°C) (Tliq)
 Viscosity and Liquidus Ranges
1500

Continuous Filament (Bushing)

Temperature (°C) at η=1000poise (Tlog3)

1400

1300

1200

Basalt and S-glass fall

outside ideal glass fiber
1100 forming property ranges
but both are produced
What can happen if you go too far to the lower right commercially
1000

900
700 800 900 1000 1100 1200 1300 1400 1500
Liquidus Temperature (°C) (Tliq)
 Viscosity and Liquidus Ranges
1500

Wool Processes
Temperature (°C) at η=1000poise (Tlog3)

1400

1300

(Cascade)
RCF
1200
Mineral
Wool
(Cascade)
1100
Flame
Att.
High liquidus glasses
with limited fiberization
1000
alternatives

900
700 800 900 1000 1100 1200 1300 1400 1500
Liquidus Temperature (°C) (Tliq)
 Fiber Diameter Distributions
Diameter distribution size and shape can vary widely
depending on the process and how it is operated

Representative
examples
Continuous
Cascade filament
(normalized to peak value)

bushing
Frequency

Rotary

0 5 10 15 20
Fiber diameter (μm)
 Glass Composition Considerations
Glass compositions are designed to achieve viable balance of properties
• Raw material costs
• Viscosity
• Liquidus temperature Items on this partial list will
vary in importance depending
• Melting enthalpy
on process and application
• Electrical conductivity (melt)
• Surface tension (melt)
• Fiber tensile strength (and retention)
Future Development
• Elastic modulus
• Compositions and processes
• Chemical durability are continually being modified
• Acidic and improved
• Neutral • Improved product properties
• Basic
• Energy reduction
• Unique environments
• Efficiency improvement
• Radiative heat transfer (melt & fiber) • New markets/applications
• Density
• Refractive index
• Surface reactivity (sizing, binder, resin compatibility)
 Other Methods & Variations
(with varying degrees of practicality)

Paramelter Rotary Continuous Filament

Small self-contained unit with Using a rotary disc as a rotating
batch feed on top, electrically bushing to collect twisted
heated, and a small CF bushing continuous filament strands
on the bottom

(US Patent 4,262,158) (US Patent 3,250,602)

 Other Methods & Variations
(with varying degrees of practicality)

Hollow Fibers

Continuous filament Rotary

(US Patent 4,758,259) (US Patent 5,674,307)

Other Methods & Variations
(with varying degrees of practicality)

Bi-Component Fibers
Rotary process

(US Patent 6,167,729)

 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)

(US Patent 4,666,485) (US Patent 5,462,571)

There are many variations on these methods (lots of strange and interesting patents)
 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 8,250,884
5,017,205 4,451,276
7,732,047 5,356,450
 Thanks for your attention!

Questions?

Elam Leed
Johns Manville Lectures available at:
[email protected] www.lehigh.edu/imi
www.jm.com