3 Introductory Fluoropolymer Coating Formulations

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1 3 Introductory Fluoropolymer Coating Formulations 3.1 Introduction While there are relatively few commercial fluoropolymers, there are thousands of fluoropolymer paint formulations. Previous volumes of this series have dealt with the details of each of the polymers (see Ch. 2, Refs. 1 and 25). The same approach is not practical in this work. Instead, overall technology is discussed and the differences between various formulations must be discussed with the respective manufacturers. Nearly all fluoropolymer coatings come in two forms. They are either dry powders or liquids. This book does not cover laminates (where a film is glued to a surface) or exotic approaches like gas or plasma phase reactions, and depositions. A basic understanding of paint formulation technology would facilitate understanding fluoropolymers coatings. This chapter provides a general overview and details follow in later chapters. 3.2 Components of Paint The components of paint generally include the following: Binder Solvents (except for dry powder coatings) Pigments and fillers Additives Coatings and paints always have what formulators call a binder. A binder is generally a polymeric material that is solid, or becomes solid, and forms the paint film. The polymeric material generally is classified as thermoset or thermoplastic. Thermoplastic coatings typically melt when reheated, whereas thermosets undergo a chemical reaction during curing that prevents remelting. Unless the coating is a dry powder, the binder is in a liquid called the solvent or carrier. Common binders found in household products include materials like acrylics, alkyds, epoxies, or urethanes. Fluoropolymers are usually binders, though they can also be thought of as fillers or additives in some applications. The binder is dissolved, dispersed, or suspended in the solvent. The solvent is usually a mixture. It liquefies the other paint components allowing them to spread out over the substrate being coated. Water is considered an important solvent. Several terms are common in the paint industry. These include medium, vehicle, and carrier. The generally accepted definitions are as follows: Vehicle is the liquid portion of paint. The vehicle is composed mainly of solvents, resins, and oils. Carrier usually refers to the solvent. Medium is the continuous phase in which the pigment is dispersed; it is synonymous with vehicle. Pigments and fillers are small particles added to paints to impart color, affect physical properties such as hardness or abrasion resistance or affect corrosion resistance. Pigments can also be used to influence viscosity, cost, adhesion, moisture permeability, gloss, abrasion resistance, electrical and thermal conductivity, and other properties. Additives are chemicals added to paints, usually in small amounts to achieve specific effects or solve specific problems. These include: 1. Surfactants, which help stabilize dispersions 2. Viscosity agents 3. Defoamers 4. Surface modifiers 5. Stabilizers 6. Wetting agents 7. Catalysts 8. Others discussed in Ch Important Properties of Liquid Coatings A number of important properties describe liquid coatings. Sometimes these properties are part of

2 38 FLUORINATED COATINGS AND FINISHES HANDBOOK the specifications of the coating. Often they are not, but none-the-less are important to know, particularly when problems arise. surface. This creates a velocity gradient, which is called the shear rate: Rheology/Viscosity Eq. (3.2) dv D = = dx v x Viscosity in its simplest definition is the resistance of a liquid to flow or, as the American Heritage Dictionary puts it, The degree to which a fluid resists flow under applied force. The viscosity is usually a specification. It is frequently reported as a single measurement such as: cps (measured by Brookfield Viscometer at 25 C, #2 spindle at 20 RPM). At first glance, a specification such as this might imply that the viscosity is a single measurement of a coating. If one looks closely the information in the parentheses, then the implication is that the viscosity depends exactly on how it is measured. The 25 C in the specification implies that the viscosity is a function of temperature, which it is. The Brookfield Viscometer is the instrument used to measure the viscosity, and its inclusion in the specification implies that the viscosity also depends on how it is measured. The Brookfield viscosity measurement is described in more detail in Ch. 13 Measurment of Coating Performance. Finally, the #2 spindle at 20 RPM defines two of the variables one can control on the Brookfield Viscometer. The spindles of a Brookfield are different designs and each has a different surface area. The more area in contact with the liquid and with the spindle, the more force will be required to turn it. The ratio of that force to the area is called the shear stress : Eq. (3.1) F t = A where: F = Force (dynes) A = Area (cm 2 ) t = Shear stress (dynes/cm 2 ) The 20 RPM defines the rotational speed or velocity. The liquids being moved against this surface include not only the liquid that is in direct contact with the spindle, but also the liquid near its where: D = Shear rate (sec -1 ) v = Shear velocity (cm/sec) x = Thickness (cm) The viscosity is defined as Eq. (3.3) h = t D where: t = Shear stress (dynes/cm 2 ) from Eq. (3.1) D = Shear rate (sec -1 ) h = Viscosity (poise = dyne-sec/cm 2 ) The main point here is that the viscosity depends upon the shear rate and stress applied by the measuring device and the temperature at which the measurement is made. This also implies that the viscosity will change depending upon how the coating is applied. Therein lies a key to using and understanding coatings. The viscosity varies with how the coating is used. Actually, viscosity also affects how coatings are manufactured, how they are stored, how they are prepared for use, and how long their shelf life is. The study of viscosity as a function of shear applied to the coating is called rheology. A test instrument called a Rotoviscometer can make these measurements quickly. This work will not go into deep detail on the physics and chemistry of rheology. Many texts develop the theory, measurement, and interpretation of rheology. [1] An ideal liquid might have a viscosity that is independent of temperature, shear, and time. Some materials approach this ideal. The ideal is called Newtonian Flow. Figure 3.1 shows the viscosity

3 3 INTRODUCTORY FLUOROPOLYMER COATING FORMULATIONS 39 versus shear rate of a Newtonian fluid. Solvents and water are nearly Newtonian. Most coatings exhibit viscosity change with shear change. There are many practical reasons for making coatings behave in this manner. For instance, nearly everyone is familiar with house paint. It has very high viscosity as it sits undisturbed in a can. That is high viscosity at a low shear rate. However, when it is rolled or brushed, the shear rate becomes high. The viscosity drops dramatically. This allows the paint to flow out and level well on a wall or ceiling. Then after it is applied and the shear is removed the viscosity rises dramatically preventing or at least minimizing which keeps the paint from dripping or running. This type of viscosity behavior is called shear-thinning or pseudoplastic. Figure 3.2 shows the viscosity versus shear relationships of two coatings. Coating B shows a linear relationship while A shows a more non-linear change. Both are considered pseudoplastic. The opposite of pseudoplastic flow is dilatant flow or shear-thickening. Figure 3.3 shows dilatant behavior. Dilatant coatings are rare. Thixotropic flow is a special case of shear-thinning behavior. A thixotropic coating thins with shear, but its viscosity does not return to the original value after the shear is removed. There is time dependence. Often with enough time, the viscosity will recover. Figure 3.4 shows a thixotropic coating and what is referred to as a thixotropic loop. The arrows indicate how the experiment was run. Starting from low shear, shear is gradually increased. Then, gradually the shear is removed. This type of behavior is sometimes designed into coatings with additives (discussed in Ch.7). It can be used to minimize settling in a coating formulation, increasing the time a coating can be stored. To give a feeling for the magnitude of the shear forces, several processes and their shears rates are given in Table 3.1. There are many ways to measure or estimate viscosity (discussed in Ch. 13). Some are easier than others. Some have more variability than others. Many plants and paint shops use a cup method which times how long it takes for a given volume of coating to drain through a hole of specific size. This work will not deal with all of these tests, but Table 3.2 allows estimation and conversion between some common devices. Figure 3.1 Newtonian flow. Figure 3.2 Pseudoplastic flow.

4 40 FLUORINATED COATINGS AND FINISHES HANDBOOK Figure 3.3 Dilatant flow. Figure 3.4 Thixotropic flow. Table 3.1 Approximate Shear Ranges for Common Coating Processes Process Shear Range, sec 1 Sagging Leveling Dipping Flow Coating Pumping Mixing Dispersion Spraying Roller Coating Brushing

5 Table 3.2 Viscosity Conversion Chart [2] Poise cp #7 #10 #1 #2 #3 #4 Holdt Bubble Litho. Krebs Units, KU Seybolt Univ., SSU A A A A A B C D E E G H I J K L M N O #1, #2, #3, #4, #5, Sears, (Cont d.) 41

6 Table 3.2 (Cont d.) 42 Poise cp #7 #10 #1 #2 #3 #4 Holdt Bubble Litho P Q R S T U V W X Krebs Units, KU Seybolt Univ., SSU Y #1, #2, #3, #4, #5, Sears, (Cont d.)

7 Table 3.2 (Cont d.) Poise cp #7 #10 #1 #2 #3 #4 Holdt Bubble Litho. Krebs Units, KU Seybolt Univ., SSU #1, #2, #3, #4, #5, Sears, Z Z Z Z Z Z Z

8 44 FLUORINATED COATINGS AND FINISHES HANDBOOK Weight Solids, Volume Solids Users of coatings need to know how much a given volume of coating they need for their particular coating job. This information is important not only in determining how much to buy, but also how much it costs if they are a processor, a seller, or a distributor of coated items. Two measures are typically reported by coatings manufacturers. Weight solids is frequently a specification and is quite easy to measure. It is simply what is left of the paint on the surface after the volatiles have evaporated during the curing. The American Society for Testing and Materials (ASTM) test for this determination is D Standard Test Methods for Nonvolatile Content of Varnishes. This measure is not directly useful to a paint user. He needs to know the cured coating density to calculate how much dried paint he has. Volume solids is a more useful measure than weight percent solids. It is the volume of the solid materials left after a gallon of paint s volatile components are removed. With this number on hand, one can easily calculate how much surface area can be painted with a gallon of a particular coating. Eq. (3.4) 1604 S E C = I A where: C = Square feet of substrate covered per gallon of paint S = Percent volume solids E = Transfer efficiency I = Dry film thickness of the paint in mils A = Part area to be coated in square feet Volume solids is more difficult to measure. The procedure is described by ASTM D , which is the Standard Test Method for Volume Nonvolatile Matter in Clear or Pigmented Coatings. Typically, weight solids is measured and reported as a specified factor. Volume solids, or coverage, is reported but it is generally not measured. It is usually calculated based on the prescribed mixture of the raw materials using their densities. The underlining assumption is that there are no chemical reactions or unusual interactions. This is sometimes incorrect. The ingredients all can affect the coating properties. The next several chapters (Chs. 4 7) look in more detail at each of the components of a fluorinated coating. REFERENCES 1. Patton, T. C., Paint Flow and Pigment Dispersion: A Rheological Approach to Coating and Ink Technology, John Wiley & Sons, New York (Apr 1979) 2. Viscosity conversion chart based on charts widely available from multiple sources including, Fine Woodworking, online extra to Vol. 169 (Mar 2004)

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