C3 International, LLC

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C3 International, LLC
Molecular Infusion Surface Treatment (MIST)

• Technology Overview

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C3 International

• Founded in 1999 to commercialize diffused oxide
  nano-films
• Headquarters Alpharetta, GA (Atlanta)
• Oak Ridge National Labs (ORNL) Partnership
• Winner, 2006 RD 100 Award
• Provide Services and Products
• Revolutionary Nanometer-Scale Surface Treatment
  Technology
• Ultra-thin films of chosen elements and oxides
• Molecular Infusion Surface Treatment (M.I.S.T.)
• Contract treatment services and OEM Licensing

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C3 Molecular Infusion Surface Treatment

• Oxide nanoparticles can provide superior
  mechanical and chemical performance in surface
  treatment applications
• Attachment method of oxides in ultra-thin films
  has been elusive
• Diffusion process for various elements (oxides
  and metals) was discovered in Russian research
  laboratories circa 1995
• Technology was acquired by U.S. group and has
  been developed into a viable commercial process

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Nano-scale for IC Industry

• Materials science being driven by integrated
  circuit industry
• Technical advances expand into other industries

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C3 Nano-scale Thin Films
100 to 500 nanometers (.1micron to .5
microns)
C3
Ultra -Thin Film
40 to 50 nanometers (.04 to .05 microns)
C3
Infusion Layer
Substrate Material

• Substrates of
• Metals
• Carbides
• Ceramics
• Cermets
• Single Crystals
• Non-Organic Material

• The C3 process results in a conformal surface
  treatment diffused into substrate
• Thicknesses of thin film 0.1 micron to 0.5
  micron (100 nm 0.1 µm)
• Infusion layer produces a alloy layer firmly
  attached to substrate 50 nm deep

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Infused Thin Films

• Superior adhesion possible
• with forced-diffusion into
• substrate inner-granular boundaries
• Nano-scale thin film becomes
• locked to host material
• During mechanical or chemical attack, residual
  effects remain
• If thin film is worn away, substrate retains
  performance characteristics
• A result of the inner-granular diffusion alloy
  layer
• Opens possibility of downgrading a tools
  substrate and upgrading the wearing surface only
• Put investment into the surface, not the core of
  the tool

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Comparison Surface Treatment Methods
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M.I.S.T. Process Attributes

• Wide variety of elements can be applied to
  metals, ceramics, etc.
• Zirconium Oxide, Cerium Oxide currently in wide
  application
• Choose from 57 elements for various effects
• Ultra-thin film adhered to substrate
• Flexible in nature
• Conforms to surface (surface finish lt16 Ra is
  preferred)
• No thermal coef. of expansion issues (CTE)
• Infused to substrate superior adhesion
• Lubrication
• Solid state lubricant
• Porosity can be added as holding sites
• for liquid lubricants
• Surface Protection
• Corrosion protection
• Environmental Boundary Coating
• Thermal property tuning (emissivity,
  transmissivity)

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Infused Nano-Film Characteristics

• M.I.S.T. process produces fine-grain size
• ORNL X-Ray diffraction study shows grain size to
  average 3 nm

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ORNL Material Analysis

• Zirconium Oxide (Zirconia) version of C3 M.I.S.T.
  process analyzed on
• 304 Stainless coupons
• Sputter profiles measured the interface formed
  between the substrate and thin film
• Ultra-thin film diffused into substrate
• Approximately 48 nm depth of Zirconia into
  substrate
• Multiple applications of the C3 process built up
  a 250 nm thin film
• Final diffused nano-film can be described as an
  oxycarbide

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SEM and Auger Analysis
ZrFeO
ZrCO
SEM

• M.I.S.T. process on SS 304
• Sequence of SEMs and Auger maps taken during a
  sputter profile
• As the coating is removed the underlying
  substrate is revealed
• Zrred
• Oblue
• Cgreen

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C3 Competitive Technologies
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Nano-film Diffusion Process
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Corrosion Resistance

• Aqua Regia Test
• Sample exposed to specific volume of 3 parts HCL
  to 1 part HNO3 for 1 hour

MIST 1000 Treatment
MIST 5000 Treatment
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Corrosion Resistance

• High Temperature Salt Spray Test
• Samples heated to 1652F in air, then sprayed
  with 10 salt water solution for 1 hour. Test
  recommended by Alberta Research Council.

MIST 1000 Treatment
MIST 5000 Treatment
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Micro Welding

• When exposed to molten metal, micro welding
  occurs in tool steels, stainless steels, etc.
• This also applies to machining operations where
  micro-welding is one failure mechanism in metal
  cutting tools
• Metal forming operations can experience micro
  welding in high stress areas

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Case Study Molten Aluminum Attack
Thermocouple Sheath Test 1010 steel exposed to
molten/liquid aluminum
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Case Study Wallace Dunker Test

• Case Western Reserve University trial using
  Wallace Dunker Test

• Test blocks made from test steel sized 2 x 2 x 7
  inch rectangular shape
• 1.5 inch diameter hole in the center for internal
  water cooling
• Four corners with 0.010 inch radius intensifies
  the predominately uniaxial stresses
• Test produces considerable constraint and high
  thermal fluctuations during immersion and removal
  from the aluminum 380 alloy bath (1350F)
• Specimen is immersed for 12 seconds
• Specimen then removed from the bath for
• 24 seconds to produce the thermal cycle
• Outer surface of the specimen sprayed with
• water-base lubricant prior to dunking
• Water flows through the central hole at
• a constant rate of four gallons per minute
• C3 treated test block ran for 15,000 cycles
• Ni-based super alloy performance unsatisfactory

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Case Study Ladle Durability

• Aluminum Foundry Ladles
• Casting ladles made from 440 SS
• Ceramic paint applied at start of each shift
  after cleaning
• Standard 1200 pours to failure
• MIST process applied to identical ladle
• Treated ladle lasted 52,125 pours

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Case Study Core Pins

• Die Cast core pins
• H13 Steel in low pressure operation
• MIST process results in 7X life over Nitrided
  pins
• (See graph at right)
• Untreated pin (top photo, below) shows typical
  aluminum soldering after 3,500 cycles
• Treated pin (bottom photo) lasts 200,000 cycles
  w/o soldering

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Case Study Intricate Die Molds

• Complex auto transmission valve body die casting
• H13 die with heat treatment Nitriding
• 383 Aluminum pour _at_ 1250F
• 8000 part limit before intense soldering occurs
• C3 M.I.S.T. process applied to untreated mold
• After 27,000 parts mold fails due to fin fracture
  unrelated to surface treatment

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Case Study Shot Sleeves

• High pressure die casting shot sleeves
• H13 construction with water cooling circuits
• Molten Aluminum _at_ 1150-130F temperatures
• 4.0 ID size
• Graphite bead lube between shots
• Normal life 20,000 cycles to tool failure
• C3 treated shot sleeves last 98,000 cycles
• Beryllium plunger tips last longer when used with
  C3
• treated sleeves
• Standard life with untreated sleeves 7,200
  shots
• Tip life when operated in treated sleeves
  12,500 shots
• Coefficient of friction reduced between tip and
  sleeve with infused nano-film of ZrO2

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Case Study Metal Forming

• Infused nano-films of Zirconia extend metal
  forming tool life
• Stamping
• Forging
• Also applicable to punches and extruders
• Extends life of shearing blades
• Reduces need for coolants
• Surface finish of stamped parts
• is improved

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Case Study Metal Cutting Tools

• Infused nano-film of ZrO2 extends
  cutting tool life
• Near-diamond hardness in nano-film and substrate
  surface
• Tool life and/or cutting speed improved
• Surface finish of machined part is improved
• Synergistic with coolants and cutting fluids

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C3 Process Critical Applications Benefits

• Gun Barrel Program
• High temperature rise in short time frame
• High rate of mechanical wear at high T
• Exposure to caustic chemicals at high T
• Close dimensional tolerances
• Hazardous material electroplating currently used
  (hard chrome plating)
• Performance is key
• Lubricity of C3 film improves range lethality
• Greater rounds per minute possible for longer
  durations
• Extended time between replacement

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C3 Process Friction Reduction

• Bearing Steel Wear Friction Test

Two bearing steel coupons were tested. The coupon
coated with the C3 infused thin film gave a 10
reduction in the coefficient of friction and
provided an 80 reduction in wear rate as
compared to the standard steel coupon. All tests
run using reference test oil.
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C3 Process Provides Multiple Benefits

• C3 Process addresses multiple areas of concern
• Can withstand extremely high temperature rise
  rates
• 4500ºF in 100 milliseconds
• Infusion into grain boundaries provides alloying
  strength
• Zirconia infusion provides high wear hardness
• Zirconia is second only to industrial diamonds in
  hardness
• Zirconia infusion provides inert barrier to
  caustic chemicals
• Nano-scale film does not cause dimensional change
• Application process is quick, with no HazMat
  issues
• Carrier fluid classification similar to kerosene
• No large capital investment needed
• Well-suited to licensing to manufacturers

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C3 Process Catalytic Surfaces

• C3 infused surface treatment can make surfaces
  chemically active
• CeO2 coating prevents carbon deposits
• CeO2 plus other elements increase surface
  activity (Platinum, etc.)
• Turbine engine combustion chambers
• Automotive engine combustion chambers
• MEMS engine combustion rate
• Diesel Particulate Filters
• Oil Refinery Piping systems
• Extends process pipe life by 600
• Jet/Turbine engine fuel injector nozzles
• Reduces internal coking

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C3 International, LLC

• 1370 E Union Hill Industrial Court
• Alpharetta, GA 30004
• Phone [phone] Fax [phone]
• www.c3international.com