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the frequency of the alternating electric field. The process of film formation is a two step process involving the coalescence of the powder particles to form a continuous layer, and the levelling of the melted coating to form a smooth film. The main parameters influencing the quality of the film formation are the surface tension of the powder and the melt viscosity, which changes continuously during the film formation process. The Haake Rheometer produces a rheological profile during the cure cycle. Initially the viscosity falls to a minimum level during the melt period. As the curing reaction begins the viscosity increases until it reaches the gel point where the system becomes more solid than liquid and there is almost no film mobility, signifying that film formation has ended. This is followed by the completion of the curing cycle when the film acquires all of its properties. This paper is explicit is detailing the tests that are applied to the laboratory samples and the wave-scan values, both long and short wave, give an indication of the degree of levelling. Higher values indicate worse levelling with pronounced orange peel effect, while lower values show good levelling properties. The results correlate the influence of minimum viscosity, gel times and film appearance. A low viscosity and a longer open time for the melting and flowing of the powder film improves the surface appearance. High ratios of Primid to polyester make the system more reactive with an adverse effect on film flow and appearance. The correct amount of curing agent is a matter of compromise between the film appearance and the optimum mechanical properties. In the examples shown the ratio 95 polyester: 5 Primid offers the best compromise. The DEA kinetic studies are described comprehensively and are proved to be a useful tool to determine the application changes during the curing of any Cray Valley system designed for use with Primid curing agents. This work is of more practical use to the formulator in creating low gloss powder systems based on Primid. In formulating matte powder coatings the most reliable technique has proved to be dry blending of two powder coatings with differing rates of reactivity. It is a peculiarity of Primid cured systems that catalysts have no effect on speeding the rate of reaction, and the reactivity difference has to be obtained by either modifying the end groups of the polyester resins or combining two polyesters with widely differing acid values. A visual assessment of film formation using an optical microscope shows that the melting step proceeds up to 130°C and above this temperature the film becomes completely flat and undisturbed until the crosslinking reaction commences. At this point different degrees of structure are formed on the film surface dependent upon the gap between the reactivity of the two systems. Surface roughness begins about one minute after reaching the isothermal target of 200°C and intensifies during the next ten minutes. Thereafter, no further changes are observed. The tests carried out on the pigmented powder systems can be applied to selection of the dry blend matte systems, for DEA and rheological characterization are especially useful tools for evaluating the curing kinetics. This allows an accurate selection of the two powders involved in the dry blend formulations and good control of gloss and surface appearance can be achieved. Paper entitled “Curing Behaviour and Surface Properties of ß-Hydroxyalkylamides Based Powder Coatings” by researchers from Cray Valley Iberica and a local University, presented at the recent International Waterborne, High Solids and Powder Coatings Symposium, in New Orleans on 2-4 Feb 2005. Bound copies of the symposium papers available from the organizers: The University of Southern Mississippi, Department of Polymer Science, Hattiesburg, Mississippi, MS 39406, USA New dimensions in fluorocarbon powder coatings Fluoropolymers have been in use since the mid sixties as high performance liquid coatings that comply with Florida exposure requirements. These systems were based on PVDF (polyvinylidene difluoride) and have shown outstanding durability after more than 10 years Florida exposure. They do, however, have significant draw backs since they are solvent based and contain high levels of VOCs, require high temperature treatment for proper film formation, their adhesion is rather poor and a primer is needed, the surface is soft and easily marred, and they are expensive not only in material cost but the application may require a four stage process. As powder coatings became accepted as alternatives to the PVDF process, and the quality of performance steadily increased, it was attempted to extend PVDF technology into the realm of powder coatings. Unfortunately, the Kynar based materials still possessed many of the faults of the liquid PVDF systems, requiring very high temperatures for processing (typically around 450°F, or 220°C) and they also require a primer to improve the adhesion. Since they are thermoplastic they are also soft and there are limitations on the level of gloss that can be formulated, and only dull, low gloss surfaces are possible. The cost factor is also considerable in terms of both material and process stages. A paper by Maier of Tiger Drylac describes a new polymer that addresses these shortcomings. It is fundamentally different from existing PVDF materials and is based on FEVE (fluoroethylene vinylether), which has functional groups attached to the polymer backbone making it capable of thermosetting. This material, Lumiflon, gives a harder surface than PVDF; the processing temperatures are lower MAY 2005 3 FOCUS ON POWDER COATINGS

New dimensions in fluorocarbon powder coatings

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Page 1: New dimensions in fluorocarbon powder coatings

the frequency of the alternatingelectric field.

The process of film formation isa two step process involving thecoalescence of the powderparticles to form a continuouslayer, and the levelling of themelted coating to form a smoothfilm. The main parametersinfluencing the quality of the filmformation are the surface tensionof the powder and the meltviscosity, which changescontinuously during the filmformation process. The HaakeRheometer produces a rheologicalprofile during the cure cycle.Initially the viscosity falls to aminimum level during the meltperiod. As the curing reactionbegins the viscosity increasesuntil it reaches the gel pointwhere the system becomes moresolid than liquid and there isalmost no film mobility, signifyingthat film formation has ended.This is followed by the completionof the curing cycle when the filmacquires all of its properties.

This paper is explicit isdetailing the tests that are appliedto the laboratory samples and thewave-scan values, both long andshort wave, give an indication ofthe degree of levelling. Highervalues indicate worse levellingwith pronounced orange peeleffect, while lower values showgood levelling properties. Theresults correlate the influence ofminimum viscosity, gel times andfilm appearance. A low viscosityand a longer open time for themelting and flowing of the powderfilm improves the surfaceappearance. High ratios of Primidto polyester make the systemmore reactive with an adverseeffect on film flow and appearance.The correct amount of curingagent is a matter of compromisebetween the film appearance andthe optimum mechanicalproperties. In the examples shownthe ratio 95 polyester: 5 Primidoffers the best compromise. TheDEA kinetic studies are describedcomprehensively and are provedto be a useful tool to determinethe application changes during the

curing of any Cray Valley systemdesigned for use with Primidcuring agents.

This work is of more practicaluse to the formulator in creatinglow gloss powder systems basedon Primid. In formulating mattepowder coatings the most reliabletechnique has proved to be dryblending of two powder coatingswith differing rates of reactivity. Itis a peculiarity of Primid curedsystems that catalysts have noeffect on speeding the rate ofreaction, and the reactivitydifference has to be obtained byeither modifying the end groupsof the polyester resins orcombining two polyesters withwidely differing acid values.

A visual assessment of filmformation using an opticalmicroscope shows that themelting step proceeds up to130°C and above this temperaturethe film becomes completely flatand undisturbed until thecrosslinking reaction commences.At this point different degrees ofstructure are formed on the filmsurface dependent upon the gapbetween the reactivity of the twosystems. Surface roughnessbegins about one minute afterreaching the isothermal target of200°C and intensifies during thenext ten minutes. Thereafter, nofurther changes are observed.

The tests carried out on thepigmented powder systems canbe applied to selection of the dryblend matte systems, for DEAand rheological characterizationare especially useful tools forevaluating the curing kinetics.This allows an accurate selectionof the two powders involved inthe dry blend formulations andgood control of gloss and surfaceappearance can be achieved.

Paper entitled “Curing Behaviour and SurfaceProperties of ß-Hydroxyalkylamides BasedPowder Coatings” by researchers from CrayValley Iberica and a local University,presented at the recent InternationalWaterborne, High Solids and PowderCoatings Symposium, in New Orleans on 2-4Feb 2005. Bound copies of the symposiumpapers available from the organizers: TheUniversity of Southern Mississippi,Department of Polymer Science, Hattiesburg,Mississippi, MS 39406, USA

New dimensions in fluorocarbonpowder coatings

Fluoropolymers have been in usesince the mid sixties as highperformance liquid coatings thatcomply with Florida exposurerequirements. These systemswere based on PVDF(polyvinylidene difluoride) andhave shown outstanding durabilityafter more than 10 years Floridaexposure. They do, however,have significant draw backs sincethey are solvent based andcontain high levels of VOCs,require high temperature treatmentfor proper film formation, theiradhesion is rather poor and aprimer is needed, the surface issoft and easily marred, and theyare expensive not only in materialcost but the application mayrequire a four stage process.

As powder coatings becameaccepted as alternatives to thePVDF process, and the quality ofperformance steadily increased, itwas attempted to extend PVDFtechnology into the realm ofpowder coatings. Unfortunately,the Kynar based materials stillpossessed many of the faults ofthe liquid PVDF systems,requiring very high temperaturesfor processing (typically around450°F, or 220°C) and they alsorequire a primer to improve theadhesion. Since they arethermoplastic they are also softand there are limitations on thelevel of gloss that can beformulated, and only dull, lowgloss surfaces are possible. Thecost factor is also considerable interms of both material andprocess stages.

A paper by Maier of TigerDrylac describes a new polymerthat addresses theseshortcomings. It is fundamentallydifferent from existing PVDFmaterials and is based on FEVE(fluoroethylene vinylether), whichhas functional groups attached tothe polymer backbone making itcapable of thermosetting. Thismaterial, Lumiflon, gives a hardersurface than PVDF; theprocessing temperatures are lower

MAY 2005 3

F O C U S O N P O W D E R C O A T I N G S

Page 2: New dimensions in fluorocarbon powder coatings

than PVDF; adhesion is improvedto the point where a primer is nolonger necessary; and high glosssurfaces up to 80 at 60° can beformulated. The cost is lowersince only a one step process isneeded and the weatheringproperties are comparable toPVDF performance.

The new alternative to PVDF isclaimed to meet all of therequirements of AAMA 2605-02,which can also be met by speciallyformulated polyester powdercoatings, although the UVresistance is said to be significantlybetter. It is not intended that thiscoating is meant to compete withpolyester powder technology, butas an improvement to both liquidand solid Kynar technology.

The Lumiflon coatings arethermosetting and the crosslinkingagents are blocked isocyanatesgiving rise to volatile componentssuch as caprolactam. Work isprogressing to eliminate all VOCcomponents and futuredevelopments could allow theformulation of emission freepowder systems. There is aproblem with the choice ofpigments due to the extremedurability requirements and thedull earth colours of inorganicpigments are most suitable tomeet durability standards.

The flexibility of the Lumiflonpolymer is limited and postforming operations could causecracking that can lead tocorrosion problems. Nevertheless,this new product offers anattractive alternative to existingPVDF powder systems at lowercost whilst retaining equivalentUV resistance and durability.

Paper entitled “Producing Highly DurableSubstrates in New Dimensions with a New,Easy to Handle Fluorine Carbon Powder” byBurkhard Maier of Tiger Drylac Inc, USAoffered for presentation at the cancelledSymposium scheduled for 12-14 Apr inHannover, Germany. Copies of the paperscan be downloaded at http://www.coatings.de

Innovative maintenance service forpowder production machinery

Powder coatings manufacturers inEurope are currently under

pressure to meet the diverseneeds of a market that hasbecome fragmented by customerdemands for special colours, thetechnical demands of runningTGIC-free products to replace theolder established products, andthey also have to face additionalcompetitive pressures as moreproducers enter the market. It isbelieved that modern powdercoating production plants are onlyrunning at 50-60% efficiency,because of the maintenancedemands and the increased downtime between production batches.Modern equipment is now gearedto increased production rates withhigher work loads placed on theessential machinery andbreakdowns can occur morefrequently, particularly whenregular maintenance proceduresare sidelined to meet productiondemands. When breakdowns dooccur there is reluctance on thepart of the machinery suppliers toretrofit upgrades to an older line,preferring instead to supply costlynew equipment, which producersmay not be able to afford intoday’s economic climate. Theneed for rationalization ofproduction lines has, in manycases, reduced the in-house skillsto maintain and repair worn ordamaged machinery.

A new company has now beenset up to service the EuropeanPowder Coatings industry, andoffers to relieve this burden. Thecompany, Xtrutech, is based inthe UK, but is now in the processof setting up offices in Germanyand Italy to offer their expertise tothe whole European powdercoatings industry. It is theirintention to serve the industry byoffering more than just spareparts or servicing of machinery.Engineers can be sent to clientsto replace, upgrade and retro-fitparts and service machinery toallow powder producers toupgrade their equipment ifrequired. One unique facet ofXtrutech’s service is the ability totake parts from one machine anddesign an imitation that fits theinternal geometry of another

machine. They can take the bestdesign features of severalextruder manufacturers andincorporate them into onemachine.

Recently, Xtrutech installed anew design replacement clamshellbarrel for an 80mm twin screwextruder in the UK. This provideda cost saving and many technicaladvantages over the old stylebarrel, giving improvedperformance, better wear andchemical resistance.

The new service from Xtrutech is describedin an article entitled “Compounding theProblem” published in PPCJ Polymers, Paint,Colour Journal, Feb 2005, 195 (4485), 36-38

Improving antimicrobial coatings

Powder coatings with anti-microbial properties weredeveloped by BioCote in the midnineties and have since becomea profitable niche outlet for thespecialist powder coatingsproducer. In the early days, theanti-microbial agent was a blendof organic materials, or even asingle organic compound;incorporated as a solid material,at the hot melt blending stage ofmanufacture. It was later foundthat the silver ion was a moreeffective anti-microbial, particularlywhen the silver ions are carriedin the lattice of a zeolite material.Silver is attractive as an anti-microbial material because it hasa low or non-existent cytotoxicity,and it is widely approved for avariety of applications in themedical and food industries.Recently an article by MichaelWagener of Bio-gate describes analternative to the use of silverions carried in a zeolite. This newtechnique is based uponnanoparticles of pure metallicsilver. The anti-microbial activityof metallic silver depends stronglyon the surface area of the silverand, in this respect silvernanoparticles give a strong anti-microbial effect at lowconcentrations.

Using an inert gas evaporationand condensation process, highpurity silver (99.96%) is

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