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Glass Part 3: New generation of specialty glass for


LCDs and AMOLEDs
B y M aggie Y.M. L ee

As display manufacturers respond to demands for larger screens and higher image
quality, as well as lighter and more portable devices, glass manufacturers have been
optimizing glass composition, properties, and production techniques to meet the electronic manufacturing requirements. Through ion-exchange chemical strengthening,
display covers are stronger and more damage-resistant, while serving multiple user
interface functions.

e continued our coverage on specialty glass for display applications in the January/February issue.1 This article will discuss
ion-exchange chemical strengthening of cover glass for the new
generations of active-matrix liquid crystal and organic light-emitting
diode displays (AMLCDs and AMOLEDs).
In addition to making larger, thinner, and lighter glass for display
panels, glass manufacturers have also focused on techniques to offer
high-quality images on damage-resistant, touch-sensitive screens. Cornings chemically strengthened Gorilla Glass has taken the world by storm

since 2008.2 The next generations Gorilla 2 and Gorilla Glass 3 were
introduced in January 2012 and January 2013, respectively.3,4 Competing
products from other leading glass producers followed in 2011 and 2012,
including Asahis Dragontrail;5 Nippon Electric Glass CX-01, CX-01P, and
CX-01T;6 and Schotts Xensation Cover, Xensation Cover 3D, and Xensation Cover AG (the last in collaboration with Berliner Glas).7,8,9
Combining fanciful product names like Gorilla, Dragontrail, and
Xensation with marketing imageries of pensive simians; fire-dodging,
demonic, flying dragons with glowing eyes and sharp claws; and

Source: Gases & Instrumentation


Figure 1. The compressive stress developed on the surface decreases with depth until it is zero over the depth of the layer. A tensile stress generated in the glass interior balances this stress. Theoretically, as long as the sum of the compressive residual stress and the tensile stress from an
external load is less than zero, mechanical failure cannot occur. CS = compressive stress; CT = central tension; DOL = depth of (compressive) layer

Gases&Instrumentation

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Source: Gases & Instrumentation


Figure 2. Ion exchange process for chemical strengthening of glass. (Left) Glass containing Na+ ions is immersed in a KNO3 bath. (Right) As the
bath containing the glass is heated and then rapidly cooled, the larger K+ ions from the bath replace the smaller Na+ ions in the glass, generating
a compressive stress layer near the glass surface

chiffon-swathed, lithe women leaping in midair; or simply adopting the practical alphanumeric CX-01 with little fanfare, the brands of
new cover glass materials seem to mirror the
demographic profiles across their users.

Low-temperature ion exchange

In our September 2012 newsletter article on


glass production,10 we discussed ion exchange
as a chemical alternative to thermal tempering of glass to create compressive stress on
the surface of thinner glass types, especially
those used as cover glass in electronics, hard
disks, etc. Sodium-containing glass (e.g., soda
lime glass, borosilicate glass, aluminosilicate
glass) is placed in a bath of molten potassium
salt, heated to a temperature below the strain
point of the glass (400600C), and then rapidly cooled. The combination of heat and the
salt prompts the larger potassium atoms to
exchange places with smaller sodium atoms
in the glass. As the surface of the glass gets
crowded, it becomes compressed. After cooling down, the compressive stress generated
on the glass surface, with a balancing tensile
stress in the interior, strengthens the glass sub-

Gases&Instrumentation

stantially. Figure 1 shows the stress distribution


in the glass after ion exchange. Any impact
needs to exceed the built up compressive
stress before cracks can take hold.
In addition to the exchange of Na+ from glass
containing Na2O with K+ in a molten potassium
salt (KNO3 or K2SO4), as shown in Fig. 2, other
alkali salts with an ionic radius larger than the
alkali ion contained in the glass can be used.
In essence, ion-exchange strengthening can
be used for lithium and sodium aluminosilicate
glass compositions based on the exchange of
larger alkali ions (ionic radius: Li+ < Na+ < K+)
for lithium or sodium using nitrate or sulfate
salt baths. The magnitude of the surface compressive stress increases with increasing difference in ionic size. For example, Li+ in lithium
aluminosilicate (LAS) glass can be replaced
with larger Na+ or K+ if the glass is immersed
in a heated sodium or potassium salt bath
(or a mixture of both).11 A mixed salt of KNO3
and a small amount of NaNO3 results in high
compressive stress, primarily owing to the K+
ions, and a low depth of the compressive layer
(DOL), primarily owing to the Na+ ions, in short
process times.12

While Schotts Xensation Cover consists of


chemically strengthened, sodium aluminosilicate glass, its Xensation Cover 3D is a chemically strengthened, lithium aluminosilicate
glass to accommodate a lower transformation temperature (Tg = 505C vs. Tg = 615C of
sodium aluminosilicate glass used for Xensation Cover and Cover AG) for more efficient
three-dimensional glass molding and a deeper
compressive stress layer.12
Since ion exchange is based on the diffusion
of ions, the thickness of the compressive layer
can be varied by altering the glass composition, glass thickness, and treatment duration.
Different types of exchanges can be combined:
in a two-step (or double) ion exchange, for
example, type A ions are first exchanged with
type B ions, followed by a second exchange
where type B ions are exchanged with type
C ions; in a three-step exchange, type C ions
can be exchanged to re-introduce type A
ions into the glass surface layer; and so on. In
some cases, the sodium-containing glass is first
immersed in a moderately heated sodium salt
bath to enrich the glass surface with more Na+.
When the glass is then immersed in a heated

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Table 1. Chemical and thermal tempering

Chemical tempering

Thermal
tempering13

Corning24,18

Asahi5,17

Gorilla Glass
Gorilla Glass 2
Gorilla Glass 3

Dragontrail

Nippon
Electric Glass6

Schott7,8,9

CX-01
CX-01P
CX-01T

Xensation
Cover
Xensation
Cover 3D
Xensation
Cover AG

Capable >845 MPa


@20 m

750 MPa @45 m


Capable >850 MPa

Capable >900
MPa

Capable >900 MPa

Capable >700
MPa

0.28-mm substrate
for touch screens

Concore (Ion-exchanged full sheet IOX-FS) for touch


screens and one-glass-solution applications
High (300900 MPa)
Capable 800 MPa
Compressive stress built up in glass
after strengthening

Low (95150 MPa)

1000 MPa @40 m DOL


950 MPa @50 m DOL
950 MPa @ 50 m DOL

Capable >900
MPa

Capable >550 MPa


Thin (10300 m)
Depth of compressive stress layer
(DOL)

Thick (approx.1/6 of
plate thickness)

Capable 40 m
Capable 50 m
Capable 50 m

Capable >90 m

Capable >70 m
Capable >75 m

Capable >50 m
Capable >120 m
Capable >50 m

75 GPa
75 GPa

74 GPa
83 GPa
74 GPa

Up to 40 m for 0.7-mm thick glass


Low
Youngs modulus

High
(approx. 1/2 of the
compressive stress)

71.7 GPa
71.5 GPa
69.3 GPa

74 GPa

71.7 GPa
Time required

Short (510 minutes)

Long (30 minutes to a few hours; up to one week for special applications)
Unlimited except for ultra-thin material
Thickness range: 0.52.0 mm
Sheet size: Available in
GEN 5 (1250 mm 900 mm)
Thickness range: 0.52.0 mm
Thickness range: 0.52.0 mm

Tempered glass thickness and


format

Limited

Thickness range:
0.5>5.0 mm
Sheet size: 1220 740
mm or 48 29

Concore sheet size: up to GEN 6


(up to 1850 mm 1500 mm)

Thickness range: 1.54.2


mm
Sheet size:
300 500 mm
Thickness range: 1.01.2
mm
Sheet size:
400 500 mm
Thickness range: 0.50.7
mm
Sheet size: GEN 5 (1300
1100 mm)

Drawing process

Any

Overflow down-draw (fusion)

Float

Overflow down-draw (fusion)

Float

Float (light polishing


required)

Overflow down-draw (fusion)


Overflow down-draw (fusion)

Glass composition

Most glasses

Aluminosilicate

Aluminosilicate

Alkali- aluminosilicate

Soda lime
(for touch screens only)

Aluminosilicate

Alkali- aluminosilicate

Thickness Range:
0.52.0 mm
Sheet Size:
1150 950 mm
Thickness Range:
0.53.0 mm
Sheet Size:
950 680 mm
575 475 mm
Microfloat
Microfloat
Microfloat

Overflow down-draw

Alkali- aluminosilicate

Alkali- aluminosilicate

Gases&Instrumentation

Roll-out (polishing
required)

Thickness Range:
0.53.0 mm
Sheet Size:
1150 950 mm
575 475 mm

Aluminosilicate

Sodium aluminosilicate
Lithium aluminosilicate
Sodium aluminosilicate

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potassium salt bath, more Na+ are available for
exchange with K+ to generate higher compressive stress after cooling.

High-temperature ion exchange

In a 2009 article, Matsunami Glass in Japan


described a high-temperature process to
create two layers of ion exchange in a sheet of
cover glass.13 The technique involves immersing aluminosilicate glass containing Na2O or
K2O in lithium salt at a temperature between
the softening and transformation temperatures (600750C). Ion exchange of Na+ or K+
in the glass with Li+ in the salt occurs before
the glass is cooled to room temperature. The
glass surface layer that now contains Li+ has a
lower coefficient of thermal expansion (CTE)
compared to the internal glass that contains
Na++ or K+. The difference in CTEs means that
the interior will try to contract more than the
surface, thus generating compressive stress
on the exterior, which strengthens the glass.14
Since the glass contains Al2O3, -spodumene
(Li2OAl2O34SiO2) or -eucryptite (Li2O
Al2O32SiO2) crystals with very low CTE are also
created. This method therefore leads to two
layers of ion exchange, which generates a crystallized -spodumene/-eucryptite glass layer
on the surface and a second Li-metasilicate
glass layer underneath. As the ion exchange
is carried out above the strain point and the
glass is then annealed, a very high compressive
stress of ~700 MPa forms after cooling and is
efficiently combined with the internal tension
to form a very strong glass.13,14
Glass types that are applicable for this hightemperature treatment contain 5766% SiO2,
13.522% Al2O3, 811% Na2O, and 1013%
Li2O.13 Suitable lithium salts include lithium
halides (such as LiCl and LiBr) and lithium sulfate (including Li2SO4, binary Li2SO4Na2SO4,
and ternary Li2SO4Na2SO4K2SO4). Alternative Na and Ag salts have also been explored.
One drawback of this high-temperature ionexchange technique is that the large difference
in CTE results in sharp stress gradients at the
interface between the two glass compositions,
which can lead to glass deformation.13,14
Using x-ray diffraction analysis of Li-based
ion exchange in sodium aluminosilicate glass,
UK scientists reported that the surface crystallization phase responsible for strength increase
was a low-CTE phase of -spodumene/eucryptite with a measured crystallite size of
235380 . The flexural strength was found to
be proportional to the depth of the crystallized

Gases&Instrumentation

layer, which in turn was proportional to the


square root of the duration of ion-exchange. In
addition, the dependence of strength increase
was shown to be based on the alumina content
of the glass, temperature of treatment, and
duration of treatment.15
Although the ion exchange rate is lower
in low-temperature ion exchange compared
to the high-temperature alternative involving surface crystallization, there is minimal
glass deformation. It is currently the preferred
strengthening method for cover glass used in
mobile electronics.

Alternative ion exchange

Ion exchange has been used as a means of


chemical strengthening since the 1940s and
1950s. Although the exchange of alkali metal
ions (e.g., Na+ in glass for K+ in the medium) is
the most common method, it is not the only
type of exchange. The reactions of alkaline
earth metal ions (e.g., Ca2+ in glass for Pb2+
and Zn2+) and other metal ions (e.g., Cu+/Cu2+
and Ag+ in copper or silver staining of glass)
are also applicable. Dealkalization is based on
the replacement of alkali ions (e.g., Na+) in the
glass with H+ through surface reactions with an
acidgas atmosphere to improve the chemical
resistance.10 It is usually carried out through
the injection of a sulfur- or fluorine/chlorinecontaining gas mixture (e.g., SO2, (NH4)2SO4,
1,1-difluoroethane mixed with air, HCl) for
reactions with sodium from the glass to form
a new composition with a lower CTE, as in the
case of high-temperature ion exchange.14

Optimizing the benefits of


chemical strengthening

While chemical strengthening is the current


technique of choice for thinner glass, not all
types of glass are suitable for the process owing
to the time and temperature required for ion
exchange. Obviously, glasses with low or zero
alkali content are not suitable for ion exchange.
As tin acts as a block to ion exchange, the
side of float glass that was directly above the
molten tin bath during forming is believed to
undergo less ion exchange than the side that
was in contact with nitrogenhydrogen.16
Some glass types can form significantly
thicker layers of surface compressive stress
than others.13 Soda lime glass, for example,
cannot form the deep compressive stress layer
(DOL <40 m for standard soda lime glass) that
is required for cover glass because of rapid
stress relaxation despite the high alkali con-

tent.14 Soda lime glass needs to be 5-mm thick


to reach the same load-to-failure offered by
Gorilla Glass with a thickness of only 0.7 mm.
This means a larger television with a soda lime
screen can weigh 1015 kg more than one
made with Gorilla Glass.17 Gorilla Glass 2 has
a >25% higher load-to-failure after abrasion
treatment compared to Gorilla Glass of the
same thickness Alternately, Gorilla Glass 2 can
be up to 20% thinner than Gorilla Glass, but
just as tough. While Gorilla Glass 3 has a modified glass composition for enhanced scratch
resistance, reduced scratch visibility, and better
retained strength once a scratch occurs, it is
still a chemically strengthened alkali-aluminosilicate (Na2OAl2O3SiO2, K2OAl2O3SiO2,
or Li2OAl2O3SiO2) glass. The Knoop (microindentation) hardness of the glass is related to
the mole fractions of the primary oxides, but
the introduction of other oxides (e.g., MgO,
CaO, BaO, ZrO2, SrO) and additives can alter
the fracture threshold.
Although Asahis 0.28-mm soda lime float
glass substrates for touch screens can be
chemically strengthened,18 they are not suited
for use as cover glass. Aluminosilicate glass
has larger openings on the surface than soda
lime glass, which allow the K+ ions to penetrate
deeper into the glass and create a deeper
compression layer. The aluminum content
also increases the hardness of the glass after
strengthening. In 2012, Corning introduced
full sheet ion-exchanged (IOX-FS Concore)
glasses for integrated-touch or one-glasssolution applications; Concore is a fusiondrawn aluminosilicate glass that is chemically
strengthened and has indiumtinoxide (ITO)
sensor patterning underneath.19 As shown in
Table 1, most displays in the market use chemically tempered covers made of aluminosilicate
glass, which are several times more resistant to
surface damage and critical stress than similarly strengthened soda lime glass. In addition,
the images have higher visual quality and the
screens offer improved touch sensitivity than
soda lime screens.
At the Society for Information Display International Symposium in June 2012, scientists at
Asahi Glass presented their study to develop
guidelines and parameters for ideal chemical
strengthening. Using glass samples immersed
in molten KNO3, NaNO3, and KNO3 mixed salt
at 400450C for 612 h, they determined that
the samples were optimally strengthened
when the compressive stress was maximized
and the depth of the compressive layer was

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ARTICLE
kept in the 2030 m range (to maintain low
central tension in the glass interior low and to
prevent strength degradation). Asahis newly
developed glass can acquire compressive
stress of 1000 MPa at a DOL of over 30 m in
the laboratory.20

Laser cutting of chemically


strengthened glass

Traditionally, glass must be cut to size prior


to thermal or chemical tempering because the
added strength vanishes within a small region
of the cut. The cut edge is weakened and the
glass sheet can break or shatter easily. Laser
cutting and scribing technologies have been
developed at Corning and Asahi to cut chemically strengthened glass (e.g., ion-exchanged
full sheets) with a very deep compressive stress
layer.21,22 At Corning, a small artificial flaw with
a depth that is larger than the DOL is first introduced on the glass surface or at the edge of the
glass. Heat from a CO2 laser is used to generate
a transient tensile stress (~100 MPa on borosilicate glass, for example) and propagate a
crack initiated from the flaw along the cutting
path, while a water or mist jet; air convection;
or a jet of compressed nitrogen, helium, or
similar gas is used for cooling. The method
enables debris-free separation of the glass with
high edge strength and without spontaneous
shattering.23,24
Manufacturers of touch panels are increasingly placing the touch sensor directly on
the chemically-strengthened cover glass
instead of laminating a separate touch panel
structure to the cover glass. Until recently,
non-strengthened glass substrates were first
cut and finished to shape before they were
treated with ion exchange. The touch sensors
were then patterned separately onto each
individual panel component. With progressively integrated touch functions and the trend
towards the adoption of the one-glass solution, it is much more economical to pattern
multiple touch sensors onto a single GEN 5
or GEN 6 (1300 mm 1100 mm or 1850 mm
1500 mm) sheet of chemically strengthened
soda lime, borosilicate, aluminoborosilicate, or
aluminosilicate glass such as IOX-FS Concore.
These ion-exchanged glass sheets can vary in
thickness from 0.5 to 1.5 mm and have multiple
touch-screen ITO films applied on one side.
An ion-exchanged glass sheet with the touchscreen films is then separated into multiple
pieces via laser full separation, laser scribeand-break, mechanical scribe-and-break, or

Gases&Instrumentation

acid etching.
With laser and traditional cutting techniques,
the cut edge of an individual glass plate after
separation was not exposed to ion exchange
and is therefore subject to damage and possible delayed failure (fatigue). Although the
edge can be protected by a coating after
separation, it does not protect the glass from
damage incurred by user handling. An additional strengthening process can provide compression on the edge or edges of glass plates
for both damage and fatigue resistance after
they are separated from the ion-exchanged
mother glass sheet.25
The laser-cut edges of a plate can be
strengthened locally by ion exchange using
an alkali salt containing alkali metal ions larger
than the exchangeable alkali metal ions in the
glass. The plate has two chemically strengthened faces and one or more exposed edges
that are not chemically strengthened, which
provide fresh material for ion exchange. An
edge of the cut sensor plate is inserted in a
bath of molten alkali metal salt (e.g., KNO3 for
exchanging with Na+ or Li+1 ions in the glass)
at a temperature between 400 and 600C for
1060 min.25 Alternately, the edges of the individual plate can be coated with a paste, such
as one consisting of KNO3, clay, and water. The
edge or edges with the K-containing medium
are then locally heated by convection, induction, laser, or microwave radiation at temperatures between 330500C for 10 min to 7 h.25
Since touch sensor functions are sensitive
to high temperatures, the ITO touch pattern
films should not be subjected to temperatures
above 200C. During the edge strengthening
process, both planar surfaces of the glass are
kept at a temperature of <200C by continuously passing a cooling gas (air, CO2, N2, or
another inert gas) across the surfaces.25 At
the end of the treatment, the strengthened
plates are washed to remove the ion-exchange
medium. A compressive stress in the range of
180600 MPa and DOL of 4050 m can be
obtained at each of the edges.25

Plasma treatment of glass


before and after chemical
strengthening

Innovations on chemical strengthening of


display glass are not limited to the biggest
manufacturers. At Taiwan-based Applied
Vacuum Coating Technologies, for example,
plasma technology is used to bolster ionexchanged soda lime glass, borosilicate glass,

and aluminosilicate glass for anti-reflective


touch screens.26 Unless glass sheets are processed for strengthening immediately after
production, they can be contaminated by
ambient particles or oxidized by oxygen in
the atmosphere during storage. As a result,
the pores of the glass plate in different areas
can have different sizes and depths, and the
distribution of the pores can vary significantly.
Subsequent chemical strengthening of stored
glass plates can lead to uneven distribution of
compressive stress, thus compromising the
strengthening effect. To enhance the chemicalstrengthening performance, a plasma-treating
process is first performed on a glass plate with
a thickness of 0.25.0 mm to reduce variations
in the average size, density, depth, and relief of
pores in different areas of the surface.26
The high-temperature plasma treating process is performed at 5002000 W under a low
pressure of 0.53 mTorr. The plasma gas used
can be air, Ar, N2, He, O2, H2, or a combination of these gases, supplied at a flow rate of
10200 sccm.26 The process leads to a smaller
surface porous variation on the glass surface,
thus eliminating any uneven distribution of
stress so that chemical strengthening can
be performed evenly on the glass sheet. The
strengthened, ion-exchanged layer has a thickness in the 5100 m range.26
The same plasma treating process can be
performed after chemical strengthening to
facilitate the removal of the potassium nitrate
crystals that were formed unevenly on the
surface of the glass plate, thus reducing the
surface pore variation and bonding the melted
network crosslinking structure on the surface
of the glass plate to further strengthen the
glass plate.26
In our next installments of this series, we will
investigate the development of float glass, downdrawn glass, and alkali-free glass for AMLCD
substrates. Advances in these technologies have
enabled reduction in density and thickness of
glass panels, as well as increases in thermal and
chemical resistance of the glass against aggressive processing environments for the growth of
amorphous silicon, low-temperature polysilicon,
and metal oxide thin-film transistors. The emergence of ultra-slim glass also offers the possibility
of bendable glass for roll-to-toll processing and
flexible electronics.
MAGGIE LEE can be reached at mlee @
gasesmag . com

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ARTICLE
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