Glass Coating TechnFunction and Production of Coatings on Architectural Glass: Basics and overviewology Primer

7/28/2019 Glass Coating TechnFunction and Production of Coatings on Architectural Glass: Basics and overviewology Primer

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Function and Production ofCoatings on

Architectural Glass

Basics and overview

Leybold Optics GmbH, Alzenau, Germany


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Outline

Outline

Type and function of glass coatings

Coating processes

Coating machine


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[ Mio m / year ]

745605485438

387

3.910

4.735

533657

815

3.195

2.473

2.760

1.151 1.278

1.510

1.910

2.365

810738601 667576

4433590

500

1.000

1.500

2.000

2.500

3.000

3.500

4.000

4.500

1989 1994 1999 2004 2009

Miom

Residential

Specialitymarkets

M o t o rvehicles

N o n

residential

T o t a lWorld Flat

Flat Glass demand worldwide


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Low-E demand worldwide

40 5565

110

160

1994 1999 2004 2010 2015

Americas

50110

140

210

320

1994 1999 2004 2010 2015

Europe

1,56

1230

80

1994 1999 2004 2010 2015

Asia

Total World: 1994 91 Mio m / year

1999 171 Mio m / year2004 217 Mio m / year

2010 350 Mio m / year

2015 560 Mio m / year


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Requirements:

Block out solar energy

keep building interiors cool(low ShadingC., low g-value)

Nice appearance

from outside ( flexible a*, b* )

Shading coefficients:

monolithic: 0.22 - 0.5

double: 0.14 - 0.4

Flexible transmittance8% - 50%

High selectivity

Solar Control Layer

Solar-Control Coatings

Single glazing orDouble glazing


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Reflection

Metal layer acts

like a mirror toheat waves

Absorption

Heat will be

dissipated inthe layer

What is a Solar Control Coating?


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GLASS

SS

GLASS

SnO2metalCrN

GLASS

TiN

Standard Solar Control Coatings


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Solar control

GLASS

top coat, e.g. Si3N

4

blocker layer, e.g. CrN

Bottom coat, e.g. Si3N4

Ty 7-50 %

many colours possible (bronce, silver, green, blue, pink,) temper able versions available


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What is a Low-E Coating?

Low-E = Low emissivityReduction of heat loss through a window

by reflection and NOT absorption

Three functions of a window:

Transmitting the visible lightReflecting the heat (mirror for infra red light)

Neutral appearance


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0

10

20

30

40

50

60

70

80

90

100

300,0 800,0 1300,0 1800,0 2300,0

Wavelength [nm]

Transmission/Reflection[%]

Typical spectrum of a Low-E Coating

Transmission T

Reflection Glass side Rglass

Reflection Film Side RFilm


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Low-E is Working as a IR-Mirror

TCO transparent conductive oxides CVD processes / Pyrolytic coatings / hard coatings

ZnO

SnO2:F / ITO / ZnSnO4/...

Thin metal films sputtering of thin Ag, Cu or Au films (~20 nm)

soft coatings


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Characteristics of Low-E Coatings

Parameters of a Low-E coating transmission Ty [%] L*

reflection Ry (glass) [%] L* colors in reflection a*, b*

emissivity [%] Rsq [sq]

mechanical stability Brush-test (washing machine)

chemical stability SO2/ NaCl-spray-test / climate-test stray light loss haze [%]

Parameters of a complete double/triple glazing (IGU)

U-value / g-value / shading factor / shading coefficient

solar heat gain / k-value


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Composition of a soft coated Low-E

Nearly all commercial used sputtered Low-E

are based on thin silver films

Ag has the best thermal and electrical conductivity

Cu is not as noble as silver and the color can not becompensated by the dielectric layers

Au is very expensive


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Structure of Low-E Coatings - Principal Layout

Dielectric Layer 2 nd = 50-150 nm

Ag d = 5-20 nm

Dielectric Layer 1 nd = 50-150 nm

Glass ZnO Ag - ZnO ASAHI 1988Glass ITO Ag - ITO IMI-Layers

GLASS

e.g. {


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Protection of Silver

Sputtering the second dielectric layer in a reactive atmosphere(SnO2) could destroy the silver layer.

Protecting the silver allows a following reactive process and might improveadhesion.

D2 nd = 50 - 150 nm

Blocker metallic/suboxide d = 0,5 5 nm

Ag d = 5 - 20 nm

D1 nd = 50 - 150 nmGLASS


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Protection of Silver on Both Sides

The first blocker might improve adhesion.

For temperable systems the first blocker protects the silver of diffusingoxygen and sodium.

Both blockers induce stress to the silver layer to avoid agglomeration duringthe heat treatment.

D2 nd = 50 - 150 nm

B2 d = 0,5 5 nm

Ag d = 5 - 20 nmB1 d = 0,5 5 nmD1 nd = 50 - 150 nm

GLASS


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Better Growth of the Silver Film

The growth of the silver layer is depending on the surface and on thesputtering process. The growth has several steps:

cluster island formation percolation homogenous film

A seed layer can improve the properties of the silver film.ZnO is a well known seed layer.

D2 nd = 50 - 150 nmB2 d = 0,5 - 5 nm

Ag d = 5 - 20 nmSeed d = 3 - 15 nmD1 nd = 50 - 150 nm

GLASS


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Splitting one or both dielectric layers gain better optical appearance.

Different materials with different refractive indices led to more neutralcolors and less loss in reflection.

Additionally some materials have a better adhesion to the next neighbor.

Some dielectric layers are able to improve the protection of silver or can

work as top layers.

D2_2 nd = 50 - 150 nmD2_1 nd = 50 - 150 nm

B2 d = 0,5 5 nm

Ag d = 5 - 20 nmSeed d = 3 15 nm

D1_2 nd = 50 - 150 nm

D1_1 nd = 50 - 150 nm

Improvement of Optical Appearance

GLASS


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Splitting one or both blocker layers could gain better mechanical andchemical resistance of the coating, especially for temperable products.

One blocker is catching the oxygen, the other one improves the adhesionor works as a seed layer for the silver (NiCr-ZnO-Ag-NiCrOx).

D2

B2_2B2_1

AgB1_2 or SeedB1_1D1

Improvement of Stability

GLASS


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The coating is sometimes covered with a very hard layer to obtain a scratchresistance surface. This function is very often combined with the seconddielectric layer D2. Typical materials: Si3N4, SiC or TiO2.

Sometimes temperable coatings are temporary covered with Graphite (C) toprotect the coating before tempering. During the heating process the carbon

will be burned.

Top layerD2

B2_2B2_1

AgB1_2 or seedB1_1D1

Scratch Resistance

GLASS


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Deposition conditions

A sputtered film has severalstages. Thin films are typically

more or less amorphous.

After several atom layers aformation of small crystals begin.The sputtering conditionsinfluence the density and thegrain size in a film.

Sometimes the film is split byan other material to avoid the

formation of crystalline grains.


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Addition of Ag Layers Sharpens SolarTransmission Cut Off

Increasing SelectivityIncreasing Number of

Ag-Layers (0-3)

solar

vis

T

TS=

Comparison of Single-, Double-, and Triple Low-E


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Outline

Coating process


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How to produce such Coatings?

Coating Requirements:

Thin layers (5-100nm) and multiple layers

Optical layers with good uniformity

human eye is the standard (d 2%) Adhesion and corrosion

(Coatings have to survive 20years of usage)

Production Requirements:

Substrate sizes: Jumbo: 6,0x3,2m2 // US: 100x166

Glass thickness: 2mm up to 15mm (varies..)

Yearly throughput: 1.0 Mio m2 up to 10 Mio. m2

Costs: Cost of Ownership and First Investment

Large Area Sputtering within an In-Line Systemis the common solution


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Characteristics:

source is distributed over a certain area

moderate heat impact on the substrate

medium deposition rate

high uniformity coatings

metal and dielectric layers possible

Sputtering: Plasma Process


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Principle Of DC - Diode Sputter Process

Ar+

Ar+

Ar+

Ar+

5000 V

Cathode (watercooled)GroundShield

Target

Substrates

Sputtered

Atoms

Electron In duced

SecondaryEmission

Ion Induced

ScondaryEmission

+

Ano de

Primary

Electrones

Los t

Ions

Sputtering Process


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Principle Of DC - magnetron Sputter Process

Ar+

Ar+

Ar+

Ar

Ar+

Ar+

600 V

N NSS

Cathode (wate rcooled)GroundShield

Target

Substrates

MagneticField

High Density

Plasma

Electron Induced

SecondaryEmissio n

Ion Induced

ScondaryEmission

Primary

Electrones

Lost

Ions

Ar. Pressure

5x10 mbar-3

+

Anode

Magnetron Sputtering


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A sputtering environment comprises

What do we need?

Chamber (vacuum tight)Vacuum system:

pumps, valves,pressure gauges

Substrate and transport system

Sputtering source:cathode, anode,

target, power supply,cooling system,control loop,

Constant plasma:gas inlet and distribution,control loopmeasurement equipment

HMI, maintenance, data storage, etc..


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Outline

Coating Machine


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Transfer1Buffer1Entrance

Sputter1 Sputter x / Proces Area10 Compartments per Sputter Chamber

ExitBuffer2Transfer2

Top View Apollon


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Top View of Complete Coater

Glas

sflow

Bring the substrate from atmosphere to process condition Pressure adaption

Continuous substrate flow

E l f


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Example for an vacuum system

Pump layout for a 5 chamber coater

WAU 2001

SV 630F

L1 B1

100 TMP (tbd)

8 x RA 7001

1x RA 3001

SP 630F

Transfer T1 Process Z (partly)Entrance L1 Buffer B1

2 stages @ B1

RA 7001

RA 3001

2 x SV 630F

2 stages

RAV 8000

RAV 4000

SV 630F

C l ti E l 60 d


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Cycle time: Example 60 seconds

Step1: Glass through L1

L1 B1

V1 V2 V3

F1

L1 B1

V1 V2 V3

F1

Action

Entrance L1 time a

p(L1)

[mbar]

p(B1)

[mbar] Pumps

Open VL1 2,0 1000

Glass m oving into L1 6,0

Close V1 2,0 1000 L0

Pum p tim e L1 33,5 32 L1Open V2 2,0 18,0 18,0 L1+B1

Pum p down during L1+B1

Glass m oving from L1 to B1 6,0 L1+B1

Close V2 2,0 1,1 1,1 L1+B1

Venting L1 5,0 1000

SPS reaction tim e 1,5

Sum 60,0

Cycle time Example 60 seconds


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Action

Buffer chamber B1 p(B1) p(T1)

Open V2 2,0 18,0 18,0 L1+B1

Pump down during L1+B1

Glass moving L1 to B1 6,0 L1+B1

Close V2 2,0 1,1 1,1 L1+B1pump down 38,5 0,015 0,015 B1

open V3 2,0 0,005 6x TMP's

Glass moving B1-T1 6,0

close V3 2,0

SPS reaction time 1,5

Sum 60,0

Step2: Glass through B1

L1 B1

V1 V2 V3

F1

L1 B1

V1 V2 V3

F1

Cycle time: Example 60 seconds

Cycle time: Pump Down Diagram


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Cycle time: Pump Down Diagram

32 mbar

18 mbar 2,90 mbar1,05 mbar

3,510-2 mbar1,5 10-2 mbar

Time [s]

pressu

re[mbar]

Pump down L1 Pump down L1+B1 Pump down B1

System A: 4x (rotary vane pumps + roots blower)System B: 6x (rotary vane pumps + roots blower)

Concept of the Machine


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Entrance Chamber 01



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Single Compartment View

Entrance Chamber

Entry/Exit Chambers


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Entry/Exit Chambers

Sputter Compartments / Drive system


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Sputter Compartments / Drive system

Full protection against heat and dust

Entrance & Exit Chambers


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Entrance & Exit Chambers

Optional hydraulic lid

Buffer Chamber


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Buffer Chamber

Shown here with optional hydraulic lid

Transfer

Transfer

Buffer

Transfer Chamber


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Transfer Chamber

Chamber toa) build up the continuous substrate flowb) adapt the pressure to process conditions

Speed Matching and Differential Pumping

Flow Schematic


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Flow Schematic

Entry Buffer Transfer

Discontinuous loading

decreasing pressure increasing pressure

Pressure adaption

Glass catch up

Continuous glasstransport

Process area

Process chambers with identicalmultipurpose processcompartments (standard: 10)

Process ExitBufferTransfer

Coater-Layout: SLE Example


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y p

2 2 2 3 3 3 3 3 3 2 1 2 2 1 1 2 2 1 1 2 2 1 2 2 2 2 2 2 2 2 2 2

Transfer 1 Transfer 2

TiO2 TiO2 TiO2 ZnO Ag NiCr Si3N4 Si3N4 Si3N4

1 2 3 4 5 6 7 8 9 10 11 12 13 14 15 16 17 18 19 20 21 22 23 24 25 26 27 28 29 30

AC AC AC AC DC DC AC AC AC150kW 150kW 150kW 150kW 30kW 60kW 150kW 150kW 150kW

Layer-Stack TiO2 TiO2 TiO2 ZnO Ag NiCr Si3N4 Si3N4 Si3N4

1 1 1

Apollon

The layer stack terminates the sequence of the processesand their configuration inside the coater.

Type of process: metal, saturated or transitionLayer thickness, deposition rate, throughput, production speed

Cross talk of the processes, gas separation factors

Gas Separation with tunnel only


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p y

Pumping Sputter Process to both sides via half compartments

GasSeparationProcess A Process B

SPP P P

( ) ( )[ ]

( ) ( )[ ]BpBpApAp

GSF01

01

=

Sputter Section with gas separation


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p g p

Pumping Sputter Process to both sides via half compartments

Process A: Oxide Process B: Nitride

S S PPP P

Gas

Separation

( ) ( )[ ]

( ) ( )[ ]BpBp

ApApGSF

01

01

=

Example for Apollon configurations by LO


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Virtually any coater configuration is possible and can be adjusted tocustomer needs

A few examples of coater configurations :

5.53300 x 7000SuperJumbo

4.53210 x 6100Jumbo

single silver low E,

double silver low E,solar control,temperable low E &solar control,transparentconductive oxides,

1.52540 x 3660US

Estimated Pricein 2008 [M] *

Product rangesAnnual

productivity[Mm] *

Glassdimensions

[mm]Format

*The pricing and the productivity inevitably depends upon the exact scope of the coaters configuration.

Top View of Apollon


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Glas

sflow

Realize the sputtering process for the moving substratesDifferent conditions (Pressure / Gas Mix)

Different materials

Different thicknesses

Process Chamber


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Empty open chamber

Process Chamber


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1st compartment with pump lid

Process Chamber


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Configuring the Machine 2


Compartment 2 and 3 filled with rotatable cathodes

Process Chamber


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Further population of the chamber

Process Chamber


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All 10 compartments closed



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View on the shield covered rollers

What Fits in a Process Chamber?


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10 compartment chamber - module

Longitudinal Cross Section

Sputter Compartment


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Cross section view with an installed Rotatable Cathode

Sputter Compartment


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Exemplary set up with Twin Rotatable

Documents

Glass Coating TechnFunction and Production of Coatings on Architectural Glass: Basics and overviewology Primer