Nanofibers New Developments in Filtration

Dr. Andreas Seeberger Mike Harriman

Abb.: 4, FotoNr.: 0606A00011, 1140 : 1 50 µm

NAFA Technical Seminar PhoenixAbb.: 26, FotoNr.: 0606A00035, AZ, 630 : 1 2012 50 µm 9. Symposium Textile Filter in Chemnitz, 2008 IREMA-FILTER and Aeolus Filter Corp.

• German Company • Located in Greensboro, NC • Manufacturer of synthetic filter media • Manufacturer of synthetic filters • Manufacturer of pleated products • Established 1997

Synthetic Filter Media for Automotive HVAC Industry

9. Symposium Textile Filter in Chemnitz, 2008 2 Let´s talk about fibers

What do you think when you hear „nanofibers“ ?

Small ? New technologies ? High performance filters ? Applications ? Use it ?

Today´s objective

Background information on fine and nanofiber filtration Capabilities for current air filtration requirements

9. Symposium Textile Filter in Chemnitz, 2008 3 Outline

History of Nanofibers in Filtration

Technical Characteristics of Nanofibers

Production Technologies

Performance in Filtration Applications

High Efficiency Filtration

Progressive Media Design

Examples

Summary

9. Symposium Textile Filter in Chemnitz, 2008 4 Outline

History of Nanofibers in Filtration

Technical Characteristics of Nanofibers

Production Technologies

Performance in Filtration Applications

High Efficiency Filtration

Progressive Media Design

Examples

Summary

9. Symposium Textile Filter in Chemnitz, 2008 5 A brief overview

The development of fine and nanofibers for filtration

• Conventional and natural man made fibers were > 10 µm

• Development of brought fibers < 10µm

• Microglass nanofibers (0.4 µm) widely available for decades

• Electrospun nanofibers used for 25 years, increasingly for 10-12 years

• Since 2000 nanofibers in focus of intensive research

• Meltspun nanofibers since 2007

• Today: established products, ongoing R&D, new technologies

9. Symposium Textile Filter in Chemnitz, 2008 6 Outline

History of Nanofibers in Filtration

Technical Characteristics of Nanofibers

Production Technologies

Performance in Filtration Applications

High Efficiency Filtration

Progressive Media Design

Examples

Summary

9. Symposium Textile Filter in Chemnitz, 2008 7 Definition of Nanotechnology

Head of a pin -2 1 cm 10 10 (~ 1-2 mm) mm Micro Electro Ant (~ 5 mm) 10-3 1 Mechanical Devices

mm (~ 10-100 μm wide) Milliscale

-4 0,1 mm Dust Mite 10 100 μm (~ 200 Human hair

μm) (~ 60-120 μm wide) -5 0,01 10 mm 10 μm Red blood Red blood cell with Pollen 10-6 grain cells white cell Microscale Visible (~ 2-5 μm) Spectrum 10-7 10 μm 100 nm

Nanofibers 0,01 10-8 DNA μm 10 (~ 20-500 nm) (~ 1-1/2 nm) nm Stacks of clay mineral -9 pletelets, each platelet 10 Abb.: 26, FotoNr.: 0606A00035, 630 : 1 50 µm Nanoscale 1 nm with ~ 1 nm thickness

Carbon Nanotube 5 Atoms of silicon - 10 10 0,1 nm (~ 2 nm diameter) (~ 1nm)

9. Symposium Textile Filter in Chemnitz, 2008 8 Definition of Nanofibers for Filtration

The definition of nanofibers for filtration

Today: Nanotechnology = smaller than 0.1 µm (100 nm) Common in filtration: Fiber diameter < 0.5 µm (500 nm) Former barrier to achieve fiber diameters < 1 µm

Start of „nano“-effects from 500 nm and below

9. Symposium Textile Filter in Chemnitz, 2008 9 Outline

History of Nanofibers in Filtration

Technical Characteristics of Nanofibers

Production Technologies

Performance in Filtration Applications

High Efficiency Filtration

Progressive Media Design

Examples

Summary

9. Symposium Textile Filter in Chemnitz, 2008 10 Production Technologies

Manufacturing Techniques Meltblown

Synthetic Island-In-The-Sea

Centrifuge Spinning Glass Fiber

Wet Laid Microglass Others

9. Symposium Textile Filter in Chemnitz, 2008 11 Glass fibers

Source: Owens9. Symposium Corning Fiberglas Textile Corporation, Filter in Chemnitz, Journal of 2008 the Air Pollution Control Association 1962 12 Wet-laid microglass production

Distributor Web Formation Binder Application Drying

Source: I. Lappas,9. Symposium Filtrex ASIA, Textile New Filter-Delhi in2010 Chemnitz, / / Dynatec 2008 13 Microglass Composition

Composition „E“-Glass „C-Glas“ Binder Systems

Silicon dioxide 52-56 % 60-65 % Latex

Calcium oxide 16-25 % - Melamine

Aluminium oxide 12-16 % 2- 6 % Phenolic

Boron oxide 8-13 % 2- 7 % Epoxy

Sodium and 0- 1 % 8-12 % potassium oxide Mognesium 0- 6 % - oxide Magnesium - 15-20 % oxide and calcium oxide

9. Symposium Textile Filter in Chemnitz, 2008 14 Microglass characteristics

Microglass filter media

• Can have very low fiber diameters (0.3 µm)

• Is available with large variety of filtration characteristics

• Is filter media of choice for high efficiency (HEPA) applications

• Has advantages and disadvantages

(efficiency vs. handling/moisture resistance/shedding

• Is tried to be replaced in increasing number of applications

• Is NOT focus of today´s presentation

9. Symposium Textile Filter in Chemnitz, 2008 15 Polymer Nanofibers

Tissue engineering scaffold Medical prosthesis Adjustable rate Wound dressing Lower stress concentration Better cell attachment Prevents scar Higher fracture strength Contraollable cell directional growth Bacterial shielding

Filter media Heamostatic devices Higher efficiency in fluid Improved adsorption performance

Protective clothing Polymer Optical applications Breathable fabric that blocks chemicals Nanofibers Liquid crystal optical shutters Cosmetics High utilization Electrical conductors Higher transfer rate Ultra small devices

Material reinforcement Drug delivery Sensor devices Higher fracture toughness Increased dissolution rate Higher sensitivity Higher delamination resistance Drug-nanofiber interlace For celd, arteries and veins

16 9. Symposium Textile Filter in Chemnitz, 2008 Island-In-The-Sea

Spinning of bicomponent fibers Island-in-the-sea structure Different geometries Dissolving sea-polymer

Source: Kuraray

Advantages Disadvantages

 Standard spinning processes for bico-fibers Nano-range not easy achievable  Narrow diameter range Solvent use Two-step-process

9. Symposium Textile Filter in Chemnitz, 2008 17 Electrospinning

Advantages Disadvantages

 Fiber diameters as low as 50 nm Low production rate  Various applicable Use of environmentally critical solvents  Homogeneous fiberdiameters Two-step-process Fibers only in layers

9. Symposium Textile Filter in Chemnitz, 2008 18 Meltblown

polymer

hot air hot air polymer Recently increasing R&D activities air air New improvements for finer fiber diameters

spinneret

fibers

Advantages Disadvantages

 High productivity normal operation: fiber diameters of  Solvent free only 1-2 microns  Single step process

9. Symposium Textile Filter in Chemnitz, 2008 19 Outline

History of Nanofibers in Filtration

Technical Characteristics of Nanofibers

Production Technologies

Performance in Filtration Applications

High Efficiency Filtration

Progressive Media Design

Examples

Summary

9. Symposium Textile Filter in Chemnitz, 2008 20 The impact of nanofibers on filtration

η = viscosity

tU0 f   Decreasing pressure drop p  df = diameter of the fiber 2 t = thickness of filter d f

U0 = face velocity of filter Slip Flow Effect α = Volume fraction of fibers in a filter  Kn  fiber volume r    1 porosity f total volume

Increasing collection efficiency

High inner surface area

Improved media design possibilities

More distinct progressivity

9. Symposium Textile Filter in Chemnitz, 2008 21 Filtration Markets for polymeric nanofiber products

HVAC Dust Collection HEPA Filtration

Automotive Vacuum Cleaners

EDM Fuel Filtration

Battery Separator Protective Clothing

9. Symposium Textile Filter in Chemnitz, 2008 22 High Efficiency Synthetic Filter Media

Nanofiber Product Electrete Product

High efficiency products Very low initial resistance

Well balanced pressure drop Mostly medium efficiencies

No or little discharge Strong discharge possible

Very reliable filtration „Insecure“ performance

All hydrophobic synthetic media show electrete effects of different strength Combination of nanofiber and electrete technology Influence of electrete effect only detectable by discharge treatment

9. Symposium Textile Filter in Chemnitz, 2008 23 Approach of IREMA and AEOLUS: Integrated Nanofiber Technology

 Integration of polymer nanofibers into nonwoven material

 Inline Process

 Solvent free fabrication of fibers with different diameters

 Task specific fiber diameters for filtration

 Gradient control of nanofiber distribution Patented Technology

Enhanced filtration performance

One-layer pleatable filter material

Unmixed Material

9. Symposium Textile Filter in Chemnitz, 2008 24 Integrated Nanofiber Technology for improved filter media

Developing of new synthetic filter media

•Higher mechanical efficiencies •Higher capacities •Low pressure drops

Nanofiber products not only for high efficiency filtration, but also for basic fine dust filtration and even prefiltration applications !

9. Symposium Textile Filter in Chemnitz, 2008 25 Fine dust filtration for Merv 13-A applications – Discharge Treatments

Objects

• Investigate influence of electrostatic charges • Inactivation by impinging particles • Long term stability / natural decay rate • Efficiency prediction in real applications

Investigations on filter Treatment methods discharge treatments • Superfine KCl • Nordtest / SINTEF • Isopropyl alcohol (IPA) • ASHRAE research projects RP 1189/1190 • Soot • EUROVENT 2004 round robin test • Detergents • R&D of filter companies  Still lack of information/transparency

9. Symposium Textile Filter in Chemnitz, 2008 26 Fine dust filtration for Merv 13-A applications – Filter Media

Fine dust filter media IFN 80 – showing full potential of nanotechnology !

Mechanical protection

Nanofiber zone

Transition region

Stabilisation zone

9. Symposium Textile Filter in Chemnitz, 2008 27 Comparison of treatments for synthetic filter media

prEN779:2010 ASHRAE 52.2 Diesel soot Appendix J

• Isopropyl alcohol • Conditioning step: • Diesel soot (IPA)treatment to nanoparticles superfine KCl simulate discharge treatment to effects (sub 0.1 µ) investigate effects • Minimum DEHS • Loading until on efficiency efficiencies must be minimum efficiency • sub 0.1 µm particles reached (0.4 µ): (0.4 µ KCl) is reached F7: 35 % F8: 55 % F9: 70 %

Independent Testing

9. Symposium Textile Filter in Chemnitz, 2008 28 EN779: F7 panel filter with integrated nanofibers

100 prEN779:2010 90 80 F7 filter class • Isopropyl alcohol 70 (IPA) treatment to 60 simulate discharge 50 Efficiency DEHS [%] effects 40 untreated • Minimum DEHS

30 DEHS Efficiency [%] Efficiency DEHS efficiencies must [%] Efficiency DEHS Efficiency DEHS [%] 20 be reached (0.4 µ): completelyEfficiency immersed DEHS [%] in 10 untreated F7: 35 % IPA and dried for 24 h 0 0,1 1 10 Particle Size [µm]

EN779:2010 test of panel filter with IREMA IFN80 nanofiber media

Cond.: 593x593x95 mm, EN779 standard test, 3400 m3 h-1

9. Symposium Textile Filter in Chemnitz, 2008 29 Ashrae 52.2: Merv 13 panel filter with integrated nanofibers

100 ASHRAE 52.2 Standard 90 80 • KCl efficiency 70 Efficiency DEHS [%] untreated 60 50 Efficiency DEHS [%] 40 discharged by IPA Efficiency [%] Efficiency 30 20 Efficiency KCl [%] 10 untreated 0 0,1 1 10 Particle Size [µm]

Ashrae 52.2 test of panel filter with IFN80 nanofiber media

Cond.: 593x593x95 mm, Ashrae Dust, 3350 m3 h-1

9. Symposium Textile Filter in Chemnitz, 2008 30 Ashrae conditioning characteristics

Peak at 40 nm

30000 KCl conditioning aerosol

25000

20000

15000 Counts 10000

5000

0 0,001 0,01 0,1 1 Particle Size [µm]

Average number distribution of ambient Particle size distribution at Ashrae 52.2 air particles from the Pittsburgh Air conditioning step Quality Study (PAQS)

Atmospheric Environment 38 (2004) 3275–3284

9. Symposium Textile Filter in Chemnitz, 2008 31 Ashrae 52.2: Merv 13-A panel filter w. integrated nanofibers

100 ASHRAE 52.2 90 Appendix J 80 Efficiency DEHS [%] 70 untreated • Conditioning step: 60 Efficiency DEHS [%] superfine KCl 50 discharged by IPA (sub 0.1 µ) 40 • Loading until [%] Efficiency 30 MERV 13-A Efficiency KCl [%] minimum 20 untreated efficiency (0.4 µ 10 Efficiency KCl [%] KCl) is reached 0 discharged by • No p increase 0,1 1 superfine KCl 10 during loading Particle Size [µm]

Ashrae 52.2 test of panel filter with IFN80 nanofiber media including Appendix J conditioning step

Cond.: 593x593x95 mm, Ashrae Dust, 3350 m3 h-1

9. Symposium Textile Filter in Chemnitz, 2008 32 Variability of Ashrae 52.2 KCl Conditioning

Ashrae 52.2 test of non-electret filters including Appendix J conditioning step in different US laboratories

Air Media (Fall 2008) 12-13

9. Symposium Textile Filter in Chemnitz, 2008 33 Soot loadig: F7 integrated nanofiber media

Peak at 70 nm Measurement of NaCl efficiency 350 100 300 90 250 80 70 200 60 150 50 100 40 Initial Efficiency NaCl

Efficiency [%] Efficiency 30

Particle number [10k] number Particle 50 Initial efficiency KCl 20 Initial efficiency DEHS 0 10 0,01 0 0,1 1 Particle0,1 size [µm] 1 10 Particle size distribution of soot Particle size [µm]

Efficiencies of various aerosols on IREMA IFN80 nanofiber media

Cond.: velocity approx. 0.15 m/s, efficiency measurements with NaCl and soot

9. Symposium Textile Filter in Chemnitz, 2008 34 Soot loadig: F7 integrated nanofiber media

100 90 80 70 60 No efficiency 50 drop during soot 40 loading seen 30 Efficiency NaCl [%] NaCl Efficiency 20 Initial Efficiency (APS) 10 0 +50 Pa soot (APS) 0,01 0,1 1 10

Particle size [µm]

Soot loading on IREMA IFN80 nanofiber media

Cond.: velocity 0.15 m/s, efficiency measurements with NaCl

9. Symposium Textile Filter in Chemnitz, 2008 35 Soot loadig: F7 integrated nanofiber media

100 90 80 70 60 50 40 30 Initial Efficiency (SMPS) Efficiency NaCl [%] NaCl Efficiency 20 Initial Efficiency (APS) 10 +50 Pa soot (SMPS) 0 +50 Pa soot (APS) 0,01 0,1 1 10

Particle size [µm]

Soot loading on IREMA IFN80 nanofiber media

Cond.: measurements at velocity 0.15 m/s, efficiency measurements with NaCl, no merging procedure of SMPS and APS results

9. Symposium Textile Filter in Chemnitz, 2008 36 Evaluation of IFN80 nanofiber media

Nanofibers strongly reduce influence of electrostatics

High mechanical efficiencies

Different discharge treatments successfully passed

No loss of filter class with IPA treatment

Sub 0.1 µm KCl particles seem to have strongest influence

Soot particles virtually have no severe effect

Very reliable filtration results under any conditions!

9. Symposium Textile Filter in Chemnitz, 2008 37 Fine dust filtration for Merv 13-A applications – Filter Media

Saving energy by progressive media design ?

9. Symposium Textile Filter in Chemnitz, 2008 38 Dust holding capacity of micro and nanofiber products

500

400

300

p [Pa] p 200  Media A (Fiberglass) 100 Media B (Synthetic ) Media C (Synthetic Microfiber) 0 0 50 100 150 200

Dust holding capacity [g]

Dust holding capacity of different panel filters

Cond.: 593x593x95 mm, measurement according to EN779 (Standard), 3400 m3 h-1

9. Symposium Textile Filter in Chemnitz, 2008 39 Dust holding capacity of micro and nanofiber products

500

400

300

p [Pa] p 200  Media A (Fiberglass) 100 Media B (Synthetic Microfiber) Media C (Synthetic Microfiber) 0 Media D (Synthetic Nanofiber) 0 50 100 150 200 Dust holding capacity [g]

Dust holding capacity of different panel filters

Cond.: 593x593x95 mm, measurement according to EN 779 (Standard), 3400 m3 h-1

9. Symposium Textile Filter in Chemnitz, 2008 40 Energy demand and lifetime costs

Q p t Annual costs (operation and service) E = 1000  700

650

] € E Energy demand [kWh] 600 Q Flow rate [m3 s-1] p Pressure drop [Pa] 550 t Time [h]

 Fan efficiency [-] [ costs Total 500 Total costs F7 450 Assumptions: Total costs IFN 80 400 Dust concentration: 1 g Ashrae/day Flow rate: 3400 m3 h-1 0 50 100 150 200 Energy costs: 0,15 €/kWh Operation time [d] Cost per filter: 60 €/filter Labour costs: 15 €/change

Annual Energy costs: Total costs:

Media C: 390,59 € 705,25 € Media D: 335,93 € (- 14,0 %) 562,17 € (-20,3%)

9. Symposium Textile Filter in Chemnitz, 2008 41 Nanofiber filtration for Merv 13-A applications – Filter Media

Nanofiber filter media – Washable mini pleats?

9. Symposium Textile Filter in Chemnitz, 2008 42 Nanofiber filtration for Merv 13-A applications – Washable Filter Media

100.0

75.0

50.0

25.0

Important0.3 - 0.5 µm! Efficiency Efficiency NaCl @ 500fpm 0.5-1.0 µm • Mechanical 0.0 protection of New Filter Loaded Filter 1st Washing 2nd Washing 3rd Washing nanofibers Efficiency measurements after several dust loading and washing procedures • Sufficient nanofiber Cond.: 24 x 24 x 4, 2000 cfm, ISO fine dust, washing with clear water concentraiton

9. Symposium Textile Filter in Chemnitz, 2008 43 Nanofiber filtration for Merv 13-A applications – Washable Filter Media

2.0 1.8 New Filter 1.6 Loaded Filter 1.4 1st Washing 1.2 2nd Washing 1.0 3rd Washing 0.8 0.6 0.4

Pressure Drop [inch PressureDrop [inch w.g.] 0.2 0.0 100 300 500 700 Air Flow [fpm]

Resistance measurements after several dust loading and washing procedures

Cond.: 24 x 24 x 4, 2000 cfm, ISO fine dust, washing with clear water

9. Symposium Textile Filter in Chemnitz, 2008 44 Other examples I: nanofiber filter media for high efficiency filters

High efficiency filters up to 95 DOP

•Increased nanofiber density •Coarse fibers only for stabilization •Very good mechanical stability

9. Symposium Textile Filter in Chemnitz, 2008 45 Other examples II: nanofiber filter media for prefilters ?!

0.40 350

0.35 Pressure Drop DHC 300 - 35% + 69% 0.30 250 0.25 200 0.20 150 0.15 100 0.10

0.05 50 AshraeDHC Dust @ 1.8''

Initial Resistance Resistance Initial inch w.g.@ 500fpm 0.00 0 Standard Nanofiber Standard Nanofiber

Improvement of prefilter (MERV10) by innovative media design using nanofibers

Cond.: 24 x 24 x 4, 2000 cfm, ASHRAE 52.2 and EN779 tests

9. Symposium Textile Filter in Chemnitz, 2008 46 Outline

History of Nanofibers in Filtration

Technical Characteristics of Nanofibers

Production Technologies

Performance in Filtration Applications

High Efficiency Filtration

Progressive Media Design

Examples

Summary

9. Symposium Textile Filter in Chemnitz, 2008 47 Summary and Outlook

HVAC: Nanofibers / Electrostatics / Energy Efficiency

• Push back of electrostatics by nanofibers • Washability of filters possible if nanofibers protected and mechanically stable • Improved progressivity by nanofibers for higher DHC • Enhanced energy efficieny • High and low efficiency filters with nanofibers possible

9. Symposium Textile Filter in Chemnitz, 2008 48 Nanofiber filter media - beyond filtration…

Department of Applied Art

University of Applied Science Zwickau

9. Symposium Textile Filter in Chemnitz, 2008 49

Thank you !

9. Symposium Textile Filter in Chemnitz, 2008 50