Lecture09 - Hubert - Annealing and Tempering

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IMI-NFG Course on Processing in Glass

Spring 2015
(available online www.lehigh.edu/imi)

Lecture 9: Annealing and Tempering

Mathieu Hubert, PhD

CelSian Glass & Solar


Eindhoven, The Netherlands

mathieu.hubert@celsian.nl
Outline of this lecture Photo: Erik Skaar

1. Annealing of glass
 Introduction - Principles
 Annealing in industrial
glass production

2. Tempering
 Principles
 Tempering in industrial glass production
 Tempered vs. Heat strengthened glass

IMI-NFG Course on Processing of Glass - Lecture 9: Annealing and Tempering


mathieu.hubert@celsian.nl 2
Introduction
Just a word on glass science – The glassy state

A: slower cooling
rate, Tga

B: faster cooling
rate, Tgb

From P. Debenedetti and F. Stillinger, “Supercooled liquids and the glass transition”, Nature 410, 259-267(March 2001)
IMI-NFG Course on Processing of Glass - Lecture 9: Annealing and Tempering
mathieu.hubert@celsian.nl 3
Introduction

Just a word on glass science – The glassy state

Crystal Glass
(e.g. quartz) (e.g. silica glass)

Ordered structure Disordered structure


(liquid-like)
IMI-NFG Course on Processing of Glass - Lecture 9: Annealing and Tempering
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Introduction

• Rapid cooling of the melt is necessary to obtain a glass (avoid


crystallization)
• This rapid cooling will generate constraints within the glass, which
will are detrimental for the mechanical properties
• This constraints can be relaxed by careful thermal treatment
• This relaxation of constraints is called annealing of the glass
• Good annealing is extremely important to produce good
commercial glasses and for their durability
• Non-annealed or poorly annealed glasses will be subject to low
resistance to cracks/failure under small thermal or mechanical
shocks

IMI-NFG Course on Processing of Glass - Lecture 9: Annealing and Tempering


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Annealing

• All along the cooling process, the viscosity of the glass increases,
from a low-viscosity melt, to a rigid material with a higher viscosity
• A certain “degree of freedom” is necessary for the glass to relax the
constraints caused by the rapid cooling (re-arrangements in the
glass structure)
• Good annealing can only be obtained in a relatively narrow range
of temperatures (thus of viscosity)
• For a good annealing of the constraints, the viscosity of the glass
should be:
 Not too high (constraints cannot be released anymore)
 Not too low (the glass will not retain its shape)

IMI-NFG Course on Processing of Glass - Lecture 9: Annealing and Tempering


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Characteristic temperatures vs. viscosity
• Strain point
η = 1014.5 Poise (1013.5 Pa.s)
Internal stresses are relieved in ~ 15 h

• Annealing point
η = 1013.4 Poise (1012.4 Pa.s)
Internal stresses are relieved in ~ 15 min

• Softening point
η = 107.65 Poise (106.65 Pa.s)
Glass deforms under its own weight at a
rate of 1mm/min

• Working point
η = 104 Poise (103 Pa.s)

Source: http://www.britannica.com
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Annealing point and stress point

Annealing point η =1012.4 Pa·s


• At this temperature, the internal thermal stresses present in the glass
are relieved by viscous relaxation within 15 minutes. In order to
relieve a glass product from its internal stresses the glass has to be
heated to just above the annealing point and subsequently cooled
down slowly.

Strain point η = 1013.5 Pa·s.


• Below this temperature relieving the internal stresses is practically
impossible (at the strain point it may last about 15 hours)
• Between the annealing and the strain point glass products should be
cooled down gradually, slowly and uniformly in order to avoid the
formation of internal stresses, due to temperature gradients

IMI-NFG Course on Processing of Glass - Lecture 9: Annealing and Tempering


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Temperature profile and stresses

• Stresses acquired during cooling and remaining from temperatures


above the strain point are permanent stresses (unless annealed)
• Stresses acquired during cooling below the strain point are
considered temporary stresses (but can still lead to failure in case
of a too important thermal shock)
• The goal of the annealing process is to relieve the permanent
stresses created by the fast cooling below the strain point which
occurred during the forming process of the glass
• To avoid creation of permanent stresses, the cooling of the glass
should be slow in the temperature (viscosity) range between the
annealing point and the strain point

IMI-NFG Course on Processing of Glass - Lecture 9: Annealing and Tempering


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Viscosity – Temperature profile of glasses

1 Pa.s = 10 Poise

= Tg

Working range

Melting range

In blue: Critical temperature range for annealing


IMI-NFG Course on Processing of Glass - Lecture 9: Annealing and Tempering
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Annealing in continuous glass furnaces

• Right after the forming process (e.g. molding for container glasses),
a rigid glass article is obtained
• The article did not experience a homogeneous cooling and a lot of
stresses are generated
• To reduce these stresses, the articles are brought to a temperature-
controlled kiln, or Lehr, for annealing
• The process from the forming of the article to the annealing Lehr is
continuous, the articles are conveyed on belts or rollers
• The temperature profile in the lehr must be controlled for an
efficient annealing
• After annealing (at the end of the lehr), the articles are continuously
conveyed to further processing steps (coatings, cutting,…)

IMI-NFG Course on Processing of Glass - Lecture 9: Annealing and Tempering


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Example: forming of glass bottles

Source: Eurotherm

Melting tank Forming Annealing, coatings,


Melting, fining, In this example, post-processing…
conditioning of molding of glass
the glass melt bottles

IMI-NFG Course on Processing of Glass - Lecture 9: Annealing and Tempering


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Example: forming of glass bottles

Source: Eurotherm
Annealing Lehr
Spouts

Molding Conveying Belt

“Solid” glass Further cooling during conveying


Source: BDF Industries
IMI-NFG Course on Processing of Glass - Lecture 9: Annealing and Tempering
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Temperature distribution right after forming

• Right after forming (and


before annealing), the
temperature distribution is not
uniform throughout the glass
article

• Different parts cooled down at


different rates, which can
result in constraints and
residual stresses

Source: NOGRID, www.nogrid.com/index.php/en/product/nogrid-points-blow1


IMI-NFG Course on Processing of Glass - Lecture 9: Annealing and Tempering
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Industrial annealing Lehr

Illustration of the continuous process for flat glass

Source: http://www.britannica.com
Controlled temperature profile
IMI-NFG Course on Processing of Glass - Lecture 9: Annealing and Tempering
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Industrial annealing Lehr

Controlled temperature profile

Source: http://newhudson.com/
IMI-NFG Course on Processing of Glass - Lecture 9: Annealing and Tempering
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Industrial annealing Lehr

IMI-NFG Course on Processing of Glass - Lecture 9: Annealing and Tempering


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Industrial annealing Lehr

• The viscosity-temperature profile for a glass depends on its


composition
• Thus, the annealing point and strain point depend on the type of
glass produced
• Different articles with different shapes (e.g. bottles, tubes, plates…)
and different characteristics (e.g. thickness, diameter, …) will
have different thermal behavior
• All these parameters have to be taken into account when designing
the annealing lehr
• The goal for an annealing lehr: it should be as short as possible
while guaranteeing an efficient annealing
• Equations exist to calculate the best temperature profile for the lehr

IMI-NFG Course on Processing of Glass - Lecture 9: Annealing and Tempering


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Temperature profiles and stresses in glass

• During cooling of glass, internal temperature gradients develop,


depending on cooling rate & internal thermal equalization within
the glass
• The internal temperature gradients will eventually lead to stresses
• The stress in the glass can be calculated from the cooling rate,
properties of the glass and shape of the article
• In return, the “best” cooling rate can be calculated for a maximum
allowable residual stress in the glass article
• Keep in mind: the goal of (industrial) annealing is to minimize the
stresses in the glass article in a duration as short as possible
(annealing = heating = energy consumption = costs)

IMI-NFG Course on Processing of Glass - Lecture 9: Annealing and Tempering


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Temperature profile in annealing Lehr

Annealing point
Strain point

IMI-NFG Course on Processing of Glass - Lecture 9: Annealing and Tempering


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Temperature profile in annealing Lehr

1 2 3 4

Annealing point
Strain point

① Rapid reheating to T > Tanneal


② Dwell – equalization of the
temperature throughout the article
③ Slow cooling
④ More rapid cooling

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Temperature profiles and stresses in glass

The relation for cooling rate h from above the annealing point to below
strain point and generated permanent thermal stress is given by:

Article
characteristics

Glass
characteristics

IMI-NFG Course on Processing of Glass - Lecture 9: Annealing and Tempering


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Temperature profiles and stresses in glass

We have

=M

E   ex   c p
With M=  in MPa·s·K-1·m-2
1  

𝜎
𝜎 = 𝑀. ℎ. 𝑑 2 . 𝑏 ℎ=
Thus 𝑀. 𝑑 2 . 𝑏
(σ in MPa) (h in K/s)

IMI-NFG Course on Processing of Glass - Lecture 9: Annealing and Tempering


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Glass characteristics

Survey of the expansion coefficient ex of some familiar glass types

ex 0-300°C [K-1] Tg [oC]


Soda-lime-silica glass 92 x 10-7 520-580
Pyrex borosilicate 33 x 10-7 565
E-glass 60 x 10-7 670
Vycor (97 SiO2, 3 B2O3) 8 x 10-7 910
Vitreous Silica 5 x 10-7 1100

For a soda-lime-silica glass, the factor M is equal to 1.2x106 MPa.s.K-1.m-2


which gives:
σ = 1.2 x 106 h.d2.b [MPa] with d in m and σ in MPa

IMI-NFG Course on Processing of Glass - Lecture 9: Annealing and Tempering


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Characteristic dimensions and shape factor

𝜎= 𝑀. ℎ. 𝑑2 . 𝑏 With d: characteristic dimension


b: shape factor

Characteristic dimension “d ”

d = thickness for one-sided cooled plate


d = 0.5 thickness for double-sided cooled plate
d = radius for spheres and cylinders
d = √(d.L) for pots and bottles with wall thickness d and bottom thickness L
d = L for pots and bottles with thick bottoms (L = bottom thickness)

IMI-NFG Course on Processing of Glass - Lecture 9: Annealing and Tempering


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Characteristic dimensions and shape factor

𝜎= 𝑀. ℎ. 𝑑2 . 𝑏 With d: characteristic dimension


b: shape factor

Shape factor “b ”

b = 0.336 for flat plates


b = 0.126 for massive cylinders
b = 0.066 for spheres
b = 0.3 for hollow products

IMI-NFG Course on Processing of Glass - Lecture 9: Annealing and Tempering


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Example annealing (cooling) rate

When a maximal permanent stress of 1 MPa is permitted after cooling,


the limit for the cooling rate h for a glass with M = 0.8 MPa·s·K-1·m-2
becomes:

1
h ≤ [K/s]
0.8x106 .𝑑 2 .𝑏

h ≤ 6 K/min. for 10 mm plate glass cooled double-sided

h ≤ 36 K/min. for 4 mm plate glass cooled double-sided

h ≤ 36 K/min. for 2 mm hollow glass cooled one-sided

IMI-NFG Course on Processing of Glass - Lecture 9: Annealing and Tempering


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Example annealing (cooling) rate

• The cooling rate h must be maintained (should not exceed the


above given limits) in the critical annealing range between Tap and
Tstr, because this is the determining range for the build-up of a
permanent stress.
• Below this range a faster cooling rate is allowed, because this will
cause only a temporary stress
• However fracture or crack formation during cooling, caused by too
large value of DT still to be prevented
• The limitations on the cooling rates will determine the needed length
and temperature profiles in the annealing lehr
• As an example: the annealing range for soda-lime-silica glass is
about 20-30oC (± 515 - 545oC).

IMI-NFG Course on Processing of Glass - Lecture 9: Annealing and Tempering


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Temperature profile in annealing Lehr

Example: annealing curve for tube glass, 10 cm diam. & 1 cm wall thickness

IMI-NFG Course on Processing of Glass - Lecture 9: Annealing and Tempering


mathieu.hubert@celsian.nl 29
Example: forming of glass bottles

Temp.
Source: Eurotherm
Time

• At the exit of the annealing lehr, the glass article is (continuously)


conveyed to further steps, including coatings, cutting, inspection…

IMI-NFG Course on Processing of Glass - Lecture 9: Annealing and Tempering


mathieu.hubert@celsian.nl 30
Inspection – residual stresses in the glass
• Perfect glass is optically isotropic, its refractive index is the same
in all directions
• Mechanical stresses causes deformations in the glass that lead to
(local) changes in the refractive index within the material
• A difference in the refractive index within the glass article will lead to
birefringence
• This birefringence can be analyzed and quantified with a
polarimeter (or polariscope), in which the angle of rotation of the
polarization direction of linearly polarized light passing through the
sample is determined
• Thus, polariscopes can be used to determine the presence of
residual stresses within the glass article
• Automated devices based on this principle are used in the glass
industry for systematic inspection of the articles produced
IMI-NFG Course on Processing of Glass - Lecture 9: Annealing and Tempering
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Polariscopes and stresses in glass

Example of stress distribution in glass


(university Erlangen, Germany

Example of polariscope

IMI-NFG Course on Processing of Glass - Lecture 9: Annealing and Tempering


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Polariscopes and stresses in glass

• Articles with a too high amount


of residual stress (e.g. jar on
the left of the picture) are
rejected (automatic process)
• The rejected product are (often)
collected and re-injected in the
furnace as raw material
(internal cullet)

http://www.vision-systems.com

IMI-NFG Course on Processing of Glass - Lecture 9: Annealing and Tempering


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Tempering

IMI-NFG Course on Processing of Glass - Lecture 9: Annealing and Tempering


mathieu.hubert@celsian.nl 34
Introduction – what is tempered glass?

• Glass is stronger in compression than is tension (compressive


strength ~10 times higher than tensile strength)
• Glass failure almost invariably originates from flaws at the surface
(stress multipliers for local tensile stresses)
• A compressive stress at the surface of the glass can thus increase
glass strength

IMI-NFG Course on Processing of Glass - Lecture 9: Annealing and Tempering


mathieu.hubert@celsian.nl 35
Introduction – what is tempered glass?

• Tempered glass is a glass that has been subjected to an additional


heat treatment after annealing in order to increase its mechanical
strength
• The tempering process lies on the controlled creation of
permanent stresses in the glass
• The surface is under compressive stress while the core is under
tensile stress
• Tempered glass can be as much as 4 to 5 times stronger than
annealed glass (without tempering)
• When fracturing, tempered glass breaks into small fragments. It is
often referred to as “safety glass”

IMI-NFG Course on Processing of Glass - Lecture 9: Annealing and Tempering


mathieu.hubert@celsian.nl 36
Introduction – what is tempered glass?

• Tempering of glass is mostly applied to articles with relatively simple


geometries, e.g. windows, windshields…
• The tempering process involves reheating of the glass article to a
critical temperature (typically above 600-650°C) and subsequent
rapid cooling of the surface to create a desired stress profile
within the material
• NB: tempering of the glass is performed on an already well annealed
glass
• The following slides will illustrate the principle of tempering for a flat
glass plate

IMI-NFG Course on Processing of Glass - Lecture 9: Annealing and Tempering


mathieu.hubert@celsian.nl 37
Principle – Tempering of glass

• t 0: Temperature T > Tg

Uniform temperature throughout the sample

NB: The temperature T0 (at t0) should not be too high to avoid
deformation of the glass plate

IMI-NFG Course on Processing of Glass - Lecture 9: Annealing and Tempering


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Principle – Tempering of glass

• t1: surface of the glass piece cooled down rapidly to a T < Tg

Surface temperature below Tg => “frozen”


Core still above Tg, relaxing under viscous flow

Below Tg

Above Tg

Below Tg

At t1: Surface tries to shrink while the inner part acts as a counterforce:
 Surface under tensile stress
 Inner part under compressive stress
IMI-NFG Course on Processing of Glass - Lecture 9: Annealing and Tempering
mathieu.hubert@celsian.nl 39
Principle – Tempering of glass

• t1: surface of the glass piece cooled down rapidly to a T < Tg

Surface temperature below Tg => “frozen”


Core still above Tg, relaxing under viscous flow

Below Tg

Thermal expansion α
Above Tg
αliq (T>Tg) ≈ 3 αsol (T<Tg)

Below Tg

At t1: Surface tries to shrink whileFrom


the R. part“Thermal
Gardon,
inner acts astempering of glass”, in
a counterforce:
“Glass: Science and Technology, Vol.5, Elasticity
 Surface under tensile and stress
Strength in Glasses”, Ed. D. Uhlmann and N.
 Inner part under compressive
Kreidl, Ac. stress
Press, 1980

IMI-NFG Course on Processing of Glass - Lecture 9: Annealing and Tempering


mathieu.hubert@celsian.nl 40
Principle – Tempering of glass

• t1: surface of the glass piece cooled down rapidly to a T < Tg

Surface temperature below Tg => “frozen”


Core still above Tg, relaxing under viscous flow

Below Tg Tensile

Above Tg Compressive

Below Tg Tensile

At t1: Surface tries to shrink while the inner part acts as a counterforce:
 Surface under tensile stress
 Inner part under compressive stress
IMI-NFG Course on Processing of Glass - Lecture 9: Annealing and Tempering
mathieu.hubert@celsian.nl 41
Principle – Tempering of glass

• t2: further cooling, inner part cooled down to a temperature T < Tg

Inner part of the glass piece contracting (“shrinking”)


Surface temperature already “frozen”, shrinking less

“Frozen”

“Shrinking”

“Frozen”

At t2: Inner part tries to shrink while the surface acts as a counterforce:
 Surface under compressive stress
 Inner part under tensile stress
IMI-NFG Course on Processing of Glass - Lecture 9: Annealing and Tempering
mathieu.hubert@celsian.nl 42
Principle – Tempering of glass

• t2: further cooling, inner part cooled down to a temperature T < Tg

Inner part of the glass piece contracting (“shrinking”)


Surface temperature already “frozen”, shrinking less

“Frozen”

“Shrinking”

“Frozen”

At t2: Inner part tries to shrink while the surface acts as a counterforce:
 Surface under compressive stress
 Inner part under tensile stress
IMI-NFG Course on Processing of Glass - Lecture 9: Annealing and Tempering
mathieu.hubert@celsian.nl 43
Principle – Tempering of glass

t1: Surface in tension and core in


compression

t2: Surface in compression and


core in tension

IMI-NFG Course on Processing of Glass - Lecture 9: Annealing and Tempering


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Principle – Tempering of glass

• After further cooling, the glass article is left with a permanent stress
profile with:
 Surface in compressive stress
 Core in tensile stress

• For a crack to propagate from the surface of the glass article, it must
overcome the usable strength of the material + the extra
compressive force at the surface
• For this reason, tempered glass is more resistant to failure than a
glass which is simply annealed (without compressive layer at the
surface)
Picture from: http://www.na.en.sunguardglass.com
IMI-NFG Course on Processing of Glass - Lecture 9: Annealing and Tempering
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Principle – Tempering of glass
Example stress distribution in solar (flat) glass

Source: http://www.cardinalst.com/products/solartemp/
IMI-NFG Course on Processing of Glass - Lecture 9: Annealing and Tempering
mathieu.hubert@celsian.nl 46
Principle – Tempering of glass
Example stress distribution in solar (flat) glass

Source: http://www.cardinalst.com/products/solartemp/
IMI-NFG Course on Processing of Glass - Lecture 9: Annealing and Tempering
mathieu.hubert@celsian.nl 47
Fracture pattern of tempered glass

Source: http://www.graysci.com/chapter-seven/shattering-the-strongest-glass/
IMI-NFG Course on Processing of Glass - Lecture 9: Annealing and Tempering
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Illustration – Prince Rupert’s drops

Taken from: www.bbc.co.uk


IMI-NFG Course on Processing of Glass - Lecture 9: Annealing and Tempering
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Illustration – Prince Rupert’s drops

IMI-NFG Course on Processing of Glass - Lecture 9: Annealing and Tempering


mathieu.hubert@celsian.nl 50
Illustration – Prince Rupert’s drops

• What does it mean?

Pictures © Smarter everyday


IMI-NFG Course on Processing of Glass - Lecture 9: Annealing and Tempering
mathieu.hubert@celsian.nl 51
Illustration – Prince Rupert’s drops

• When damaging the tail => creation of a flaw which propagates to


the core, in tensile stress
• All the strain energy stored in the glass (stress-strain relationship) is
released, leading to the catastrophic failure of the glass article
• This is similar to what is observed in tempered glass

• More on Prince Rupert’s drops? Check out these videos:


 Video “Smarter everyday - Mystery of Prince Rupert's Drop at 130,000 fps”
 Video “Corning- The glass Age, Part 2: Strong, Durable Glass ”
IMI-NFG Course on Processing of Glass - Lecture 9: Annealing and Tempering
mathieu.hubert@celsian.nl 52
Important parameters for glass tempering

• Permanent stress profile generated σp

𝛼. 𝐸. Δ𝑇𝑀𝑆 𝛼. 𝐸 2λ −1
𝜎𝑝 = = 𝑥 (1 + ) 𝑥 𝑇𝐸
1−𝜇 1−𝜇 ℎ𝑑

With:
α = thermal expansion coefficient [K-1]
E = Young’s modulus [MPa]
Glass
characteristics μ = Poisson’s ratio
λ = thermal conductivity [W/m2.K]
h = heat transfer coefficient [W/m2.K]
Process ΔTMS = TM-TS = Temp. middleplane – Temp. surface [K]
related TE = “freezing temperature” ≈ Tg [K]
d = thickness of the glass plate [m]
IMI-NFG Course on Processing of Glass - Lecture 9: Annealing and Tempering
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Thermal history in a tempered glass plate

Temp. midplane

Temp. surface

Adapted from R. Gardon, “Thermal tempering of glass”, in “Glass: Science and Technology, Vol.5, Elasticity and Strength
in Glasses”, Ed. D. Uhlmann and N. Kreidl, Ac. Press, 1980
IMI-NFG Course on Processing of Glass - Lecture 9: Annealing and Tempering
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Effect of glass thickness

• With thicker plates,


higher degrees of
temper achieved
(larger stress profiles)

• Above a certain
temperature, a
plateau is reached

• Below a certain
thickness, tempering
becomes inefficient

From R. Gardon, “Thermal tempering of glass”, in “Glass: Science and Technology, Vol.5, Elasticity and Strength in
Glasses”, Ed. D. Uhlmann and N. Kreidl, Ac. Press, 1980
IMI-NFG Course on Processing of Glass - Lecture 9: Annealing and Tempering
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Effect of temperature and quenching coefficient

From R. Gardon, “Thermal tempering of glass”, in “Glass: Science and Technology, Vol.5, Elasticity and Strength in
Glasses”, Ed. D. Uhlmann and N. Kreidl, Ac. Press, 1980
IMI-NFG Course on Processing of Glass - Lecture 9: Annealing and Tempering
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Examples for a glass plate of thickness = 8mm

• Initial viscosity of the glass ηi = 108 Pa.s

Hmax Initial temp. Ti σmax midplane σmax surface


(W/m2.K) (°C) (MPa) (MPa)
Soda-lime-silicate
α = 9.10-6 K-1
4500 650 105 235
Borosilicate
α = 3.10-6 K-1
>5000 730 32 70

• Initial viscosity of the glass ηi = 109 Pa.s

Hmax Initial temp. Ti σmax midplane σmax surface


(W/m2.K) (°C) (MPa) (MPa)
Soda-lime-silicate
α = 9.10-6 K-1
470 630 65 135
Borosilicate
α = 3.10-6 K-1
1500 680 25 50

IMI-NFG Course on Processing of Glass - Lecture 9: Annealing and Tempering


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Industrial tempering of glass

Illustration of the a glass tempering unit for a soda-lime-silica glass

From: http://us.agc.com

IMI-NFG Course on Processing of Glass - Lecture 9: Annealing and Tempering


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Industrial tempering of glass

Source: http://www.metroglasstech.co.nz/catalogue/038.aspx

IMI-NFG Course on Processing of Glass - Lecture 9: Annealing and Tempering


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Industrial tempering of glass

From P. Boaz “Thin glass processing with radio wave assist”, www.glassonweb.com/articles/article/561/

IMI-NFG Course on Processing of Glass - Lecture 9: Annealing and Tempering


mathieu.hubert@celsian.nl 60
Heat-strengthened vs tempered glass?

• Heat-strengthened glass: the cooling process is slower, which


means the compression stress is lower
• In the end, heat-strengthened glass is approximately twice as strong
as annealed glass but less strong than tempered glass

Pictures from: http://educationcenter.ppg.com


IMI-NFG Course on Processing of Glass - Lecture 9: Annealing and Tempering
mathieu.hubert@celsian.nl 61
Heat-strengthened vs tempered glass?

Source: www.chicagowindowexpert.com
IMI-NFG Course on Processing of Glass - Lecture 9: Annealing and Tempering
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Processing of tempered glass

• Tempered glass cannot be cut nor drilled! It would lead to


release of the strain energy and thus catastrophic failure of the glass
• How are the tempered glass articles made (for instance the
windshields?)

http://www.grandsportautobody.com

http://glassdepotny.com
IMI-NFG Course on Processing of Glass - Lecture 9: Annealing and Tempering
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Processing of tempered glass

• Example of fabrication of tempered windshields

The glass is cut and shaped


before tempering

From: www.agc-automotive.com/english/products/temper.html
IMI-NFG Course on Processing of Glass - Lecture 9: Annealing and Tempering
mathieu.hubert@celsian.nl 64
Industrial tempering of glass

Example of a glass tempering furnace

Picture from www.xinology.com/Glass-Processing-Equipments-Supplies-Consumables/glass-


tempering/glass-tempering-furnace/feature/bending-tempering.html
IMI-NFG Course on Processing of Glass - Lecture 9: Annealing and Tempering
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Other technical considerations

• A certain thickness is necessary for obtaining an efficient


strengthening of the glass by tempering
• For thin glass articles with a thickness below 2mm (typically),
thermal tempering becomes much less efficient
• Also, tempering requires a uniform cooling from both sides of the
glass article (e.g. both surfaces of a glass plate)
• It is thus complicated to temper glass articles with complex or
uneven geometries (such as bottles)
• For these types of products, strengthening (when applied) can be
performed using ion-exchange technique (chemical strengthening)

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Chemical strengthening

• Chemical strengthening of glass also relies on the formation of a


compressive stress on the surface, with the core in tensile stress
• The way to achieve this stress profile is however very different (ion-
exchange instead of thermal treatment)
• Chemical strengthening of
glass will be presented by
A. Varshneya in this series
of IMI-NFG lectures

Picture from: R. Gy, “Ion exchange for glass


strengthening “, Materials Science and
Engineering B 149 (2008) 159–165

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Conclusions – 1/2 - Annealing

• Annealing of the glass articles after the forming process is crucial for
relaxing the stresses due to inhomogeneous, rapid cooling
• The annealing consists in reheating the glass above the annealing
temperature and perform a controlled, slow cooling between the
annealing point and the strain point
• The cooling rate between Tanneal and Tstrain is crucial and will depend
on the type of glass (composition) and the type of article produced
(shape, thickness…)
• At industrial scale, annealing is a continuous process, and is
performed in annealing lehrs
• The temperature profile in the lehr should be optimized to obtain a
well-annealed product in the shortest possible time

IMI-NFG Course on Processing of Glass - Lecture 9: Annealing and Tempering


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Conclusions – 2/2 - Tempering

• Tempering of glass is a thermal treatment performed on annealed


glasses to create controlled stresses in the glass
• The glass is reheated at a critical temperature and then rapidly
cooled, leaving the surface in compressive stress and the core in
tensile stress
• Tempered glasses can be 5 times stronger than annealed glass
• If broken, tempered glass will shatter in small fragments (securit glass)
• Tempered glass cannot be cut or drilled, and the glass article must be
shaped before the tempering process
• Tempering is limited to relatively thick products (> 2mm) and
relatively simple geometries (windows, windshields…)

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Home assignment

• A multiple choice questionnaire (MCQ) including questions on


industrial glass annealing and tempering processes is provided with
this lecture

• The MCQ will be available online on IMI’s website

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References and further reading

• “The glass tempering handbook” by Jonathan Barr, available online (free)


at
https://dl.orangedox.com/IOM4ukrFcunESCW2Yh/TheGlassTemperingHa
ndbook.pdf

• Book “Strength of Inorganic Glass”, Ed. C. Kurkjian (Plenum, 1985)

• R. Gardon, “Thermal tempering of glass”, in “Glass: Science and


Technology, Vol.5, Elasticity and Strength in Glasses”, Ed. D. Uhlmann
and N. Kreidl (Academic Press, 1980)

• CelSian’s glass course e-learning trailer:


https://www.youtube.com/watch?v=pID0PYsBIbQ&feature=youtu.be

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Thank you for your attention

Questions ?
Visit us in Eindhoven

Contact me via email:

mathieu.hubert@celsian.nl

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