SilcoTek CorporationCoatings for inertness and

corrosion resistance

Information, Questions and where coatings are being used

Topics

• Vision• Questions• The process and the coating• Products and Applications• Conclusion/Future Product Development

Vision

• “Easy” Button for customers needing coating– Work together to identify repeat items– Have these items ready for customers to

order– Working with suppliers to figure out a

method for having product ready– Stock, Consignment, Drop shipping, etc.

Questions

• What is the maximum tubing length that you can work with

– Straight lengths: 6 footers (Coat internal & external)

– Coiled tubing: Up to 2000 feet (Coat Internally)– Can coated coil tube be straightened to produce

20’ sticks?

• Is every valve sent to you disassembled?– Yes, the process temperatures would compromise

any lubricants and seals inside of the valves.– Also, to properly clean all the components

Questions

• What is the time frame we can use to give to customers if we send a valve to get treated?– 10 days from the time of receipt– Is there enough demand to predict some repeat

items that can be stocked or consigned?– Can factory hold inventory? We’re trying on our

end.

• Is the process different now with the company name change or is it the same?– Same coatings and people– We will be more flexible now that we’re focused

Questions• What is new with your company since the last time

you visited us?– We’ve become an independent company focused on

coatings– New brand names

• SilcoNert for inertness (1000 and 2000)• Silcolloy for corrosion

– More people, 17 dedicated to customers & coatings

• Are the lubricants replaced after the parts are treated?– No

Questions

• Where do you see industry going with these special materials and processes?– As the need for knowing what’s in streams

increases, there will be more demand• Sulfurs• Mercury• Ammonia• Corrosion• Low level alcohols and other impurities

– More methods specifying need for coatings– Working with suppliers to offer coated products as

stock items– Growing volume of NeSSi systems

Questions

• Are there certain industries that are moving more quickly than others with the sulfinert process?– Refining, the most mature and familiar with the

coating: Rule 1118 coming– Concern for Mercury, gas wells– Power generation growing quickly (coal fired

power plant stack monitoring)– Off shore applications, can we provide the

inertness and corrosion resistance. Need 20’ sticks coated inside and outside

Questions

• Is pressure and temperature affected when the part is treated?– Pressure ratings are still maintained– Maximum temperature rating of coating is

450C.– There are coatings that can be applied for

use up to 600C on stainless

APPLICATION AREAS• SilcoNert: Inertness

(Silcosteel, Sulfinert/Siltek)– Sulfinert = SilcoNert 2000

• Silcolloy: Anti-Corrosion (Silcosteel-CR)

• SilcoKlean: Anti-Coking

(Silcosteel-AC)

• SilcoGuard: Ultra-High

Vacuum (Silcosteel-UHV)

MARKET AREAS

AnalyticalPharmaceuticalEnvironmental

PetrochemicalChemicalProcess

Automotive

Semiconductor/Research

Brand Names

• SilcoNert 2000– Used to be Sulfinert and Siltek

• SilcoNert 1000– Used to be Silcosteel

• Silcolloy 1000– Used to be Silcosteel-CR

Basic Manufacturing Process

• Receive items• Document – digital, customer contact• Clean

– Standard: caustic ultrasonic bath, 2 systems– Custom: solvation via other means

• Chemical Vapor Deposition (CVD) Process– Vacuum– 400ºC– silicon-based deposition

• Clean• Document – digital, customer contact• Pack, ship

Properties

• Max operating temp. – 450C: SilcoNert 2000– 600C: SilcoNert 1000; Silcolloy

• Hardness: Equivalent to stainless steel

• Thickness– SilcoNert 2000: 0.12 microns– Silcolloy 1000: 2 microns

SilcoNert 2000 Properties

• Improves surface inertness by capping active sites.

• Needed when sulfurs are analyzed in the part-per-million level

• Performance down to 1 part-per-billion of hydrogen sulfide

Coating Capabilities: Substrates

• Tubing:– 0.004” to 0.5” ID– 2000+ ft. continuous lengths

• Complex geometry parts (inside and out)– Fittings, valves, frits– Block manifolds, sample vessels – custom parts

Sizes of reaction chambers• “Standard” vessels:

– 10” diameter cylinder w/ 48” height– 3” diameter cylinder w/ 72” height– 10” diameter cylinder w/ 18” height

• Large processing oven:– 27” diameter x 26” deep– 4’ diameter x 6’ deep

• Walk-in Oven:– 4 feet by 4 feet by 5 feet– 6 feet by 4 feet by 5 feet

Substrates Which Coat Well

• 300 and 400 grade stainless steel

• High carbon steel

• Titanium

• Ceramics

• Borosilicate glass

• Inconel®

• Hastelloy®

Substrates with Issues

• Nickel / Nickel plating• Aluminum*• Monel®• Copper• Brass• Gold and Silver plated components • Chrome Plated components• Magnesium• Elastomers• No Bases!

*heat-dependent

Benefits of coating?

• Reduce loss of active compounds– Saves costs from re-testing

– Avoid false negatives because sulfur compounds can be quickly lost without coatings

– Sample stable from field to lab.

– Immediate response during process changes creates savings when used in feedback / feed forward monitors

SilcoNert 2000 surface improves storage

• Reduces adsorption effects

• Improves analytical reliability

• Faster cycle times and

• increased accuracy – 17ppbv H2S Containment in 500ml Cylinders

00.20.40.60.8

11.21.41.61.8

2

0 1 2 3 6 7

Day

RR

F

(H2S

to

DM

S)

Coated/functionalized steel cylinders

Uncoated steel cylinders

Sulfur Flow-through data

• 100’ 1/8” x .020” tubing• Standard seamless 316L• Electropolished 316L• Sulfinert® coated EP 316L

• 0.5ppmv methylmercaptan in Helium

• SCD detection• Data courtesy of Shell Research

Technology Centre, Amsterdam

Effectiveness of coated transfer systems to reduce hold-up: Methyl Mercaptan

Inertness: Mercury

• Mercury is growing concern in environment:– Coal fired power plants– Natural Gas

• CMMS (Continuous Mercury Monitoring System) manufacturers currently using SilcoTek technology with success to transfer mercury

• Starting to see need from well sampling firms, Halliburton, Schlumberger

Mercury in oil and gas wells

• Mercury in oil and gas wells is common in many geographic areas.

• Mercury in these streams must be monitored to reduce damage to pump vanes and pipeline equipment.

• SilcoNert technology required to eliminate loss of mercury samples during testing.

Mercury Adsorption by Stainless Steel

• 5 µg/m3 Hg Standard (5PPT)

• Spectra Gasses Inc.• 1 Gallon Sample Cylinder 1800psi DOT rated

• Swagelok Corp• NIST Traceable • Nominal Temp. 70°F• Test Cycle Day 0,7,19,50• Direct Interface Gas Sampling• Atomic Absorption Detector• SilcoNert 2000 treated Regulator and Tubing

Mercury 50 Day StabilityChemisorption greatly reduced

Average Mercury Response Comparison of Stainless Steel vs. Silicon Functionalized Surfaces

01234567

0 10 20 30 40 50 60

Days after fill

Ave

rag

e M

ercu

ry

Co

nce

ntr

atio

n (

ug

/m3 )

Untreated cylinders (n=2) Functionalized cylinders (n=2)

Comparison of Hg Stability in 304SS vs.SilcoNert 2000 Coated Cylinders

Test Day Avg response

Loss vs. Day 0

Avg response

Loss vs. Day 0

 304 SS

cylinders   Functionalized  

  ug/m3   Silicon ug/m3  

0 5.65 - 6.45 -

7 3.25 42% 6.1 5%

19 2.05 64% 6 7%

50 1 82% 5.8 10%

Effect of moisture

• Hydrophobic silicon based coatings decrease adsorption of water

• Quicker removal of moisture • Components less susceptible to corrosion• Faster cycle times and increased accuracy

Moisture Data• 1ppm moisture, 0.35slpm• Amount of time to equilibrate a 1ppm moisture

sample through 100 feet of dry tubing:– Commercial Seamless 316L tubing

• 180 minutes (96% equilibrated)– Electropolished Seamless 316L tubing:

• 60 minutes (98% equilibrated)– Functionalized a-silicon coated e-polished

seamless 316L tubing• 30 minutes (98% equilibrated)

Wet-Up 50% faster response

Moisture Data (cont)

• Time to dry 100’ tubing wetted with 1ppm of moisture when connected to a dry purge– Commercial Seamless 316L tubing:

• 175 minutes– Electropolished Seamless 316L tubing:

• 65 minutes– Functionalized a-silicon coated e-polished

seamless 316L tubing• 35 minutes

Dry-Down 50% faster response

SilcoNert 2000 Applications• International Society of Beverage

Technologists (ISBT): Fountain Carbon Dioxide Quality Guideline– Sulfurs contaminants

• Rule 1118: Control of Emissions from Refinery Flares– Sulfurs emissions

• Ethylene/Propylene feedstock testing– Sulfurs as catalyst poisons

SilcoNert 2000 Applications• Exhaust gas testing, stack emissions testing

– Ammonia release as a result of injection

• Acid Rain Precursors– NOx and SOx compounds from coal fired plants

• Natural Gas well testing– Mercury and H2S Concentrations

• Clean Air Mercury Rule– Emissions of Mercury from Coal Fired plants

SilcoNert 2000 Applications

• Water quality testing: Headspace + Purge & Trap systems– Moisture release and overall inert pathway

• EPA TO-15 method: Toxic organics– Create overall inert surface in stainless vessels

• Homeland Security– Chemical Warfare Agents– Explosive detection

SilcolloyCorrosion Resistance

• Stainless steel surfaces susceptible to attack from substances such as chlorinated environments and acidic exhaust environments.

• Corrosion resistant deposition is a heavier amorphous silicon layer insoluble in hydrochloric acid and unaffected in salt water environments (marine applications)

Corrosion Resistance studies:

• External Evaluation– Certified corrosion engineers (Matco)– Spectroscopic analysis– Mechanical testing– Electrochemical Cyclic Polarization in neutral,

acidic, alkaline– Atmospheric corrosion

• ASTM moisture condensation• Salt spray ASTM B117

– Stress corrosion cracking (MgCl2; ASTM G36)

ASTM G48 B Data: Pitting and Crevice Corrosion

– 6% Ferric Chloride solution – 72hrs, 20ºC– Gasket wrap

Sample InitialWeight (g)

FinalWeight (g)

WeightLoss (g)

Weight Loss(g/m2)

Silcolloy Sample 17 10.4105 10.3710 0.0395 19

Silcolloy Sample 28 10.1256 10.0743 0.0513 25

Silcolloy Sample 47 10.1263 10.0742 0.0521 25

Bare Sample 27 10.0444 9.5655 0.4789 231

Bare Sample 34 10.1265 9.6923 0.4342 209

Bare Sample 37 10.1007 9.6276 0.4731 228

ASTM G48 B (cont.)

• Bare 316L Stainless Steel coupon (left) showing severe crevice corrosion. Coated coupon shows light pitting

ASTM B117 Data: Salt Spray

• 4000 hour exposure– 100 degree Fahrenheit– 3.5% by weight sodium chloride

• No effect on Silicon coating• Reproduces exposure to marine

environments.• Oil-in-water monitors/produced water

applications

Silcolloy Advantages• Longer Life:

– Extend lifetimes of equipment exposed to corrosive environments

• Low Cost• Protection:

– Protection of high value equipment • Inert:

– Provide enhanced corrosion resistance to analytical equipment

– Maintain inert sample pathway– More inert than Inconel, Hastelloy, or glass. Ideal for

10ppm levels or higher• High Temperature:

– High temperature stability up to 1000c

Silcolloy Applications

• Process streams• Process sampling• Continuous Emissions Monitoring Equipment• Automotive Exhaust• Semiconductor Gas transfer• Fasteners in Marine Environments• Off-shore drilling platform equipment• Produced water management

Conclusions/Future• Continual process improvement and new product

development for coatings:– Improving the hardness of coatings– Improved corrosion resistant coatings– Hydrophobic surfaces for moisture sensitive

applications– Protection of high nickel alloys such as Hastelloy®

and Inconel®– Hydrogen embrittlement resistance. – New generation process systems on line in FY08

• Additional manufacturing capacity– New manufacturing facility!