Lecture09 - Hubert - Annealing and Tempering
Lecture09 - Hubert - Annealing and Tempering
Lecture09 - Hubert - Annealing and Tempering
Spring 2015
(available online www.lehigh.edu/imi)
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
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
Crystal Glass
(e.g. quartz) (e.g. silica glass)
• 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)
• 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
IMI-NFG Course on Processing of Glass - Lecture 9: Annealing and Tempering
mathieu.hubert@celsian.nl 7
Annealing point and stress point
1 Pa.s = 10 Poise
= Tg
Working range
Melting range
• 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,…)
Source: Eurotherm
Source: Eurotherm
Annealing Lehr
Spouts
Source: http://www.britannica.com
Controlled temperature profile
IMI-NFG Course on Processing of Glass - Lecture 9: Annealing and Tempering
mathieu.hubert@celsian.nl 15
Industrial annealing Lehr
Source: http://newhudson.com/
IMI-NFG Course on Processing of Glass - Lecture 9: Annealing and Tempering
mathieu.hubert@celsian.nl 16
Industrial annealing Lehr
Annealing point
Strain point
1 2 3 4
Annealing point
Strain point
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
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)
Characteristic dimension “d ”
Shape factor “b ”
1
h ≤ [K/s]
0.8x106 .𝑑 2 .𝑏
Example: annealing curve for tube glass, 10 cm diam. & 1 cm wall thickness
Temp.
Source: Eurotherm
Time
Example of polariscope
http://www.vision-systems.com
• t 0: Temperature T > Tg
NB: The temperature T0 (at t0) should not be too high to avoid
deformation of the glass plate
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
Below Tg
Thermal expansion α
Above Tg
αliq (T>Tg) ≈ 3 αsol (T<Tg)
Below Tg
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
“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
“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
• 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
mathieu.hubert@celsian.nl 45
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
mathieu.hubert@celsian.nl 48
Illustration – Prince Rupert’s drops
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
mathieu.hubert@celsian.nl 53
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
mathieu.hubert@celsian.nl 54
Effect of glass thickness
• 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
mathieu.hubert@celsian.nl 55
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
mathieu.hubert@celsian.nl 56
Examples for a glass plate of thickness = 8mm
From: http://us.agc.com
Source: http://www.metroglasstech.co.nz/catalogue/038.aspx
From P. Boaz “Thin glass processing with radio wave assist”, www.glassonweb.com/articles/article/561/
Source: www.chicagowindowexpert.com
IMI-NFG Course on Processing of Glass - Lecture 9: Annealing and Tempering
mathieu.hubert@celsian.nl 62
Processing of tempered glass
http://www.grandsportautobody.com
http://glassdepotny.com
IMI-NFG Course on Processing of Glass - Lecture 9: Annealing and Tempering
mathieu.hubert@celsian.nl 63
Processing of tempered glass
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
• 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
Questions ?
Visit us in Eindhoven
mathieu.hubert@celsian.nl