gary barone, marty higgins, david smith silcotek corporation

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The Characterization of Novel Carboxysilane Depositions on Stainless Steel Substrates for Inertness, Wear Resistance, and Corrosion Resistance Applications. Gary Barone, Marty Higgins, David Smith SilcoTek Corporation. Overview. Use of Coatings Selecting Coatings Coating Materials/Properties - PowerPoint PPT Presentation

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Improving the Release of Moisture from Stainless Steel to Benefit the Reliability and Recovery of Process Analyzers

The Characterization of Novel Carboxysilane Depositions on Stainless Steel Substrates for Inertness, Wear Resistance, and Corrosion Resistance ApplicationsGary Barone, Marty Higgins, David SmithSilcoTek Corporation1OverviewUse of CoatingsSelecting CoatingsCoating Materials/PropertiesDurabilityCorrosion TestingMoisture ResistanceChemical InertnessConclusion

2Enter speaker notes here.

Using CoatingsMost analytical pathways are stainless steelGreat structurallyGood corrosion resistancePoor chemical properties for analytical chemistsCoatings used to improve material properties.Industries are demanding harsher services for silicon coatings (like SilcoNert 2000 (Sulfinert).Carboxysilane coatings (Dursan) more robust.3Factors Contributing to Poor Sampling ReliabilityDurability/Wear CorrosionMoistureDesignChemical & Material Compatibility/InertnessInstrument CompatibilityInstallation

4Selecting CoatingsFluoropolymersVery inertVery corrosion resistantBroad pH applicabilityPoor adhesionPoor wear resistanceGood to 260C

Silicon (SilcoNert 2000)Very inertGreat adhesionNo carryoverGood corrosion resistanceLimited pH rangeSusceptible to steam cleaningPoor wear resistanceGood to 450C5New CoatingCarboxysilane (Dursan)Good inertnessGreat adhesionNo carryoverGood corrosion resistanceBroad pH applicabilitySteam cleaning, no problemGood wear resistanceTested to 450C Still accumulating application data

6Coating/Material Properties PropertySilicon(SilcoNert 2000) Carboxysilane DursanPTFE,PFAMax Temperature450C450C260CMin Temperature-196C-100C-240CLow pH limit000High pH limit71414Thickness0.12um to 0.5um0.5um to 1.0um25umAdhesionVery GoodVery GoodPoorWear resistance90% of Stainless 2 times 316 Stainless10% of SS (est.)Moisture contact72-90104-140125Inertness vs. SSExcellentGoodExcellent7Improving wear resistance & DurabilityEquipment and sample conditions can damage surfaces and increase activity.Valve cycling/purging cause delaminationParticulate in sample streamsAbrasive cleaningExisting coatings Prone to wearEasily damagedResult: Adsorption & loss of sample

8Wear and Friction DataLoad2.0 NDuration20 minSpeed80 rpmRadius3mmRevolutions1,554Ball Diameter6mmBall MaterialSS 440Pin on Disc: ASTM G133Base substrate is mirror-finish SS 316Courtesy of Nanovea Inc.Avg. Coeff. FrictionWear Rate(x10-5mm3/Nm)Uncoated SS0.58913.810Carboxysilane (Dursan)0.3786.129Silicon (SilcoNert 2000)0.714.00

9Pull Strength Measurements

Paints delaminated from the stainless steel

10Pull Strength MeasurementsDursan more slippery difficult to bond adhesive. Adhesive bond failed before coating. Demonstrating reduced friction characteristics.

11Challenge of CorrosionSamples can contain corrosives that quickly attack stainless Hydrochloric acid (HCl)Sulfuric acid (H2SO4)SaltwaterPhysical loss of equipment due to corrosionMaintenanceReplacement cyclesCorrosion increases surface activity and particulatesSilicon coatings susceptible to caustics12Acid Corrosion ResistanceASTM G31 Guidelines: 6M HCl; 24hr; 23C316L SSSiliconCarboxysilaneMPY181.984.320.44Improvement Factor over 316L stainless---42411

Photo after 19hrexposureDursan coatedSilcolloy coated13Acid Corrosion ResistanceASTM G315% HF70% Nitric85% Phosphoric25% SulfuricMPY ratefactorMPY ratefactorMPY ratefactorMPY ratefactor316 SS120.00-0.78-0.62-54.64-Carboxysilane80.381.490.107.500.088.005.3610.19Silicon44.262.710.362.140.282.1823.622.3114Exposure to Caustic Base1M KOH; 24hr; 22C ASTM G31316L SSSiliconCarboxysilaneMPY03.400.01Improvement FactorOver SiliconInfiniteDissolution26115Challenges of MoistureBenefits of coating that help release water fasterComponents less susceptible to corrosionFaster cycle times Increased accuracyEliminate moisture/sample interaction

16Impact of MoisturePresence of moisture in sampling system reduced H2S response by 22%: 50ppm sample17Measuring HydrophobicityDI Water304 SSSilcoNert 2000DursanPTFEAdvancing36.087.3105.5125.4Receding5.351.585.384

Kruss K100 TensiometerTesting on304 SS OD tubingDI Water Contact Angle Illustrations (advancing) on flat surfaces:304 SSSilcoNert 2000Dursan18Chemical InertnessStainless Steel:Adsorbs sulfur compoundsCauses loss of mercuryDemonstrates poor transportability (tailing) of polar organics such as alcoholsAdsorbs ammonia

Need coating that is chemically inert for analytical systems19Total Sulfur Recovery 36ppb & 25ppm, 300cc cylinderSS 80% loss in 1 daySilcoNert: 36ppb 99%+ recovery2021Mercury 50 Day Stability

Courtesy of Spectra Gases Inc.21Ammonia Adsorption100PPV, 500sccm, 1.8m tubing, minMeasured PTR-MS signals of ammonia (m17). At t=10min the gas stream was switched in a waythat it passed additionally the different 1.8m long lines. The PFA line seems to be best for Ammonia, whilethe steel line completely adsorbs the 100ppbv of Ammonia in the sample gas for hours. All lines were 1.8 m,not heated (30C), sample gas flow was 500 sccm (std. ml/min) of 100 ppb of ammonia in N2. Courtesy of IONIMED Analytik

22Selecting Coatings FactorFluoropolymersWeightSilicon(SilcoNert )Weight

Carboxysilane(Dursan)Weight

DurabilityPoor wear resistanceFair wear resistanceGood wear resistanceCorrosionExcellentGood Good MoistureExcellentGoodExcellentInertnessExcellentExcellent/ no carryoverGoodChemical / Material CompatibilityPoor adhesion/ Broad pH rangeExcellent adhesionExcellentInstrument CompatibilityGoodGoodExcellentInstallation

260c max450c max450c max23ConclusionAnalytical and Process industries demanding increased performance from coatingCoating selection dictated by application Corrosion resistanceMoisture resistanceInertnessWearBroad spectrum environments and applications may involve a tradeoff in performance. In field applications, carboxysilane coatings (Dursan) may be the best overall performer. 24Chart15.656.45Day 1Day 1Day 2Day 2Day 3Day 3Day 4Day 4Day 5Day 53.256.1Day 7Day 7Day 8Day 8Day 9Day 9Day 10Day 10Day 11Day 11Day 12Day 12Day 13Day 13Day 14Day 14Day 15Day 15Day 16Day 16Day 17Day 17Day 18Day 18Day 19Day 19Day 20Day 20Day 21Day 212.056Day 23Day 23Day 24Day 24Day 25Day 25Day 26Day 26Day 27Day 27Day 28Day 28Day 29Day 29Day 30Day 30Day 31Day 31Day 32Day 32Day 33Day 33Day 34Day 34Day 35Day 35Day 36Day 36Day 37Day 37Day 38Day 38Day 39Day 39Day 40Day 40Day 41Day 41Day 42Day 42Day 43Day 43Day 44Day 44Day 45Day 45Day 46Day 46Day 47Day 47Day 48Day 48Day 49Day 49Day 50Day 5015.8

Untreated cylinders (n=2)Functionalized cylinders (n=2)Days after fillAverage Mercury Concentration (ug/m3)Average Mercury Response Comparison of Stainless Steel vs. Silicon Functionalized Surfaces

Sheet1Untreated cylinders (n=2)Functionalized cylinders (n=2)Day 05.656.45Day 1Day 2Day 3Day 4Day 5Day 63.256.1Day 7Day 8Day 9Day 10Day 11Day 12Day 13Day 14Day 15Day 16Day 17Day 18Day 19Day 20Day 21Day 222.056Day 23Day 24Day 25Day 26Day 27Day 28Day 29Day 30Day 31Day 32Day 33Day 34Day 35Day 36Day 37Day 38Day 39Day 40Day 41Day 42Day 43Day 44Day 45Day 46Day 47Day 48Day 49Day 50Day 5115.8Day 52Day 53Day 54Day 55Day 56

Sheet100000000000000000000000000000000000000000000000000000000000000000000000000000000000000000000000000000000

Untreated cylinders (n=2)Functionalized cylinders (n=2)Days after fillAverage Mercury Concentration (ug/m3)Figure 4: Average Mercury Response Comparison of Stainless Steel vs. Silicon Functionalized Surfaces

Sheet2Table 3. Tabulated response comparison: 316SS vs. Functionalized sample cylindersTest DayAvg responseLoss vs. day 0Avg responseLoss vs. day 0316 ss cylindersFunctionalizedLR #Cylinder #Manu. DateHydro DatePressureCyl CodePassivatedRequestedAnalyzedDate Analyzedug/m3Silicon ug/m3248876BA-61321475 psigNAir5 ug/m3n5.75.7 ug/m33/8/0705.65-6.45-248876BA-61321325 psig5 ug/m3n3.33.3 ug/m33/15/0773.2542%6.15%248876BA-61321225 psig5 ug/m3n2.22.2 ug/m33/29/07192.0564%67%248876BA-61321125 psig5 ug/m3n1.31.3 ug/m34/27/0750182%5.810%LR #Cylinder #Manu. DateHydro DatePressureCyl CodePassivatedRequestedAnalyzedDate Analyzed248877BA-61291275 psigNAir5 ug/m3n5.65.6 ug/m33/8/07248877BA-61291125 psig5 ug/m3n3.23.2 ug/m33/15/07248877BA-61291000 psig5 ug/m3n1.91.9 ug/m33/29/07248877BA-6129900 psig5 ug/m3n0.70.7 ug/m34/27/07LR #Cylinder #Manu. DateHydro DatePressureCyl CodePassivatedRequestedAnalyzedDate Analyzed248875BA-61141575 psigNSiltek/Air5 ug/m3n6.46.4 ug/m33/8/07248875BA-61141475 psig5 ug/m3n66.0 ug/m33/15/07248875BA-61141325 psig5 ug/m3n5.95.9 ug/m33/29/07248875BA-61141250 psig5 ug/m3n5.75.7 ug/m34/27/07248875BA-61141200 psig5 ug/m3n5.75.7 ug/m35/24/07LR #Cylinder #Manu. DateHydro DatePressureCyl CodePassivatedRequestedAnalyzedDate Analyzed248878BA-61351175 psigNSiltek/Air5 ug/m3n6.56.5 ug/m33/8/07248878BA-61351075 psig5 ug/m3n6.26.2 ug/m33/15/07248878BA-6135975 psig5 ug/m3n6.16.1 ug/m33/29/07248878BA-6135925 psig5 ug/m3n5.95.9 ug/m34/27/07248878BA-6135800 psig5 ug/m3n5.95.9 ug/m35/24/07

Sheet3