Measurement and Effects of Paper Coating Structure R.W. Wygant, Ph.D.

Coated Paper Analysis Work Group Leader ECC International Technology Center Sandersville, Georgia 31082 U.S.A. *Introduction The paper industry is continuously improving coating quality and printability to meet higher consumer standards. One key to improving coating quality is to empirically characterize coating structure to determine the factors influencing quality. The technologies used to characterize paper coating structure are evolving rapidly. These technologies are discussed here in the context of measurement of the physical and optical properties of coating surface and bulk structure and the influences of these properties on various end use performance attributes. The premise of this discussion is that techniques discussed are applicable to coated papers, and not necessarily to paper coating formulations or basestocks prior to the coating operation. This is a testing situation frequently faced by the paper industry and its suppliers. The goal of this chapter is to briefly familiarize the reader with the wide variety of testing techniques available for characterizing paper coating structures and the influences these structures may have on the performance of papers. An effort has been made to provide a sizable bibliography so that the interested reader may easily pursue more in-depth discussions of these techniques. Some of the references are primary references for particular testing techniques while others show interesting applications of those techniques. *Surface Structure **Topographical Mapping There are many ways to acquire topographical maps of paper surfaces. The most common involve scanning a surface with some type of sensing mechanism. Different types of sensors include diamond styli, a variety of optical sensors, confocal microscopes and atomic force microscopes. Each of these types of sensors has particular advantages and disadvantages. A different type of topographical measurement that has recently been applied to coated paper surfaces involves optical interferometry. Rather than scanning a probe over the surface, this technique images a relatively large area with coherent light. Through lightwave interference phenomena, this technique is able to map the topography of the entire area. Yet another technique is stereoscopy, employing optical or electron microscope images made at different viewing angles. /1--9/ ***Stylus profilometry. Stylus profilometry involves moving a stylus across a surface while measuring the vertical

deflection of the stylus. This technique can provide excellent vertical resolution, on the order of a nanometer. However, the lateral resolution is typically on the order of 10 microns for paper applications. This is because of the need to prevent damage to the paper surface. With a spring loaded finite force on the stylus tip, as the stylus tip radius decreases, the pressure under the tip increases. Most styli are manufactured with an included angle of 90 degrees, so that the maximum slope that can be measured is 45 degrees. There is also a finite physical inertia of the stylus mechanism. This results in the need to allow the stylus to come to an equilibrium after lateral movement before a vertical deflection measurement can be reliably performed. If one can live with relatively slow scanning speeds, this technique can provide very good topographical maps of fiber-sized and larger features on paper. Figure 1 shows a false color height map of a 1 mm2 topographical image of a double coated SBS board acquired using an ECC Paperscape diamond stylus profilometer. Although this board has been double coated, fiber affects on topography are clearly visible. <Figure 1. Diamond Stylus Profilometer 1 mm2 Topographical Image of Double Coated SBS Board.> ***Optical profilometry. Optical profilometry is similar to stylus profilometry in that a sensing head is scanned across a surface. While vertical resolution is similar to that of stylus profilometry, lateral resolution, limited by the wave nature of light, can be on the order of one micron. There is no physical contact between the sensor and the surface, so there is no possibility of damage to the specimen. This allows more rapid scanning of surfaces. There are several different types of optical profilometer sensors. Most of these do have limitations on the maximum slope angle that can be measured because of design geometries. At too high a slope angle, the light reflected from the surface will fall outside of the acceptance aperture of the sensing head. In general, optical profilometers provide faster scanning and higher resolution than stylus profilometers. However, they still lack sufficient lateral resolution to image paper coating pigments. ***Confocal microscopy. Confocal microscopy provides a special case of optical profilometry wherein the theoretical lateral resolution limit is approximately the wavelength over square root two. This is achieved by imaging a pinhole onto the surface of interest, and re-imaging that spot onto a detector aperture. While this technique allows the resolution of coarser paper coating pigments, many pigments are too fine to be resolved or imaged. A significant drawback of these devices is cost. The imaging technique involved results in low optical throughput, so that high intensity light sources are required. These are typically argon or xenon ion lasers, which alone can be more expensive than other profilometers. In addition, the optical systems required are of high complexity and expense. Two particular advantages are the ability to do both fluorescence imaging and volume imaging. If a fluorescent ink is used, for example, high resolution maps of the lay of the ink can be obtained. The ability to do volume imaging is unique and can of tremendous benefit in some applications. However, the high optical scatter designed into most paper coatings makes this technique less than ideal for volume imaging of paper coatings.

***Scanning probe microscopy. Scanning probe microscopy offers the highest resolution available for studying paper coating surfaces, on the order of a nanometer. This technique can provide excellent imagery of even the finest paper coating pigments, inks, binders and polymeric additives. Scanning probe microscopy is a relatively new field in which technical advances and new probe designs are appearing on a frequent basis. Scanning tunneling and atomic force microscopy (AFM) are the best known examples of this instrument type. Newer modes of operation of atomic force microscopes can provide lateral force (friction) and mechanical property (elasticity) maps. Near field scanning optical microscopy is becoming more widely known. Other probe types in various stages of development include magnetic field sensors and chemical sensors for a variety of different species. The common theme among all of these instruments is exceptionally high spatial resolution obtained with piezoelectric scan transducers. These devices provide spatial movements accurate to the order of an angstrom. The current technological drive is for the development of micro-sensors to complement this high resolution spatial positioning ability. Figure 2 shows an illuminated view of a 10 mm square (100 mm2) AFM topographical image acquired from the same double coated SBS board sample shown in Figure 1. However, in this figure the visible detail is related entirely to the coating formulation. Kaolin platelets, needle shaped PCC and in some places amorphous blobs of latex binder are the dominant features. Figures 1 and 2 illustrate the importance of understanding surface topography over a broad range of scales. <Figure 2. Atomic Force Microscope 100 mm2 Topographical Image of Double Coated SBS Board.> ***Optical Interferometry Optical interferometry for topographical mapping is a technique that has been applied to optically smooth surfaces for many years. Only since the late 1980's has this technique been applied to optically rough surfaces, including coated paper. This technique is noncontact, can capture data for an entire area at one time and can be used for dynamic deformation analysis. Resolution can be easily varied, from the lower limit of around the wavelength of light to an upper limit defined by optical system apertures, which can be ten centimeters or larger. ***Stereoscopy Stereoscopy implies the use of stereo, or binocular, images to derive height information. Either optical or electron microscope images can be used. Thus, the range of resolution is quite wide, from perhaps several tens of nanometers up to centimeters. This technique does require significant computational resources, however these are now commonly available. Modern analysis algorithms have significantly improved both the speed and accuracy of this technique, making it a much more viable option then it was in past decades. **Air Flow Roughness

There are several instruments available that can provide average surface roughness measurements using air flow techniques. Examples of these include the Parker Print-Surf, Bekk, Bendtson and Sheffield devices. Newer brands employ the same measurement geometries with significantly greater ease of use achieved using modern electronics. These devices typically measure the air flow between the paper surface and a metal edge pressed against the surface. The geometry, applied pressures and backing material vary between devices and even between procedures on the same device. While some of these devices can be calibrated to provide measurements in RMS micron roughness, for example, the size of features they measure is dependent upon the device geometry. There is also the possibility that this type of measurement can be influenced by the porosity of the coating layer itself, with air flowing inside the coating layer as well as between the coating and the measurement head. The major advantage of these types of measurements is that they can be performed very quickly, making them ideal for production environments. /10--13/ **Coefficient of Friction The coefficient of friction of a paper surface can be affected by both the topography and chemistry of the surface. Topography can affect friction on both microscopic and macroscopic scales. Stick-slip phenomena can occur in relation to features varying in size from formation (mm -- cm) to coating pigment organization (< micron). Traditional macroscopic techniques for friction measurement include inclined plane for static friction and level plane for static and dynamic friction. New atomic force microscopy techniques are capable of measuring frictional forces on a nanometer scale. For most paper surfaces, it might be safe to assume that an increase or decrease in friction may be due to an increase or decrease in roughness. However, for very smooth surfaces friction may increase as roughness decreases due to increasing contact area. /14-15/ **Optical Imagery Optical imagery can be employed for studying paper surfaces on scales ranging from the macroscopic down to the order of a micron. Macrophotography can be employed to measure of latex binder migration, for example. A sample must be illuminated with the appropriate ultraviolet wavelength to be absorbed by latex carbon double bonds. The subsequent decrease in local UV reflectivity can be photographed with a suitable panchromatic film. The uniformity of the latex concentration at the coating surface can then be found from such images. Quantitative determination of latex concentrations requires careful calibration with calibrants of known concentration. Fluorescence microscopy can be performed using a suitably equipped microscope. Mercury arc lamps and long-wavelength pass mirrors can be used to direct the excitation light to the sample while preventing that wavelength from reaching the detector. This technique is useful for gauging the depth of penetration of fluorescently labeled fluids into paper coating layers. This can be done using physical cross sections of embedded paper samples. Embedding media must be carefully chosen to minimize dissolution of the fluorephore into the media. Examples of

fluids that can be studied in this way include inks, varnishes and fountain solutions. /16--19/ **Contact Angle Analysis ***Fluid droplet. /20,21/ Fluid droplets can be imaged as they impinge upon solid surfaces. Various recording techniques can be employed, including high framing rate photography and video recording, direct digitization of a video signal or even realtime digital analysis. High speed movies can be analyzed by hand or automatically analyzed by computer. Different types of analysis have been employed, from measuring the contact angle and volume of droplets deposited with near zero momenta, to measurements of the maximum spreading of droplets impinging on surfaces with well-controlled momenta. The particular advantage of this type of measurement is that the dynamic interactions (wetting, imbibition, elastic deformation) between fluids and surfaces can be characterized on time scales relevant to industrial processes such as printing or paper coating. ***Immersion and extraction. In this technique, a solid sample is quasi-statically immersed then extracted from a fluid of interest. The sample is typically hung from a transducer that records the forces acting on the sample. These forces include gravitational and buoyant forces, as well as the attractive or repulsive forces between the solid sample and the fluid. For porous samples, the immersion and extraction cycle must be repeated until a stable hysteresis curve is obtained. This technique can provide data on attractive or repulsive forces between fluids and solids, even for porous samples. **Optical Properties ***TAPPI Gloss. The TAPPI glossmeter is an instrument universally used in North America. Similar instrumentation is used globally by the paper industry, both in laboratories and for online process control. The measurement principle involves shining a near-collimated light beam on a surface and measuring the intensity of light reflected into a specific aperture. Near grazing incidence angles (75 from the surface normal) are used for most types of paper. The 75 TAPPI geometry is used with an 11.4 degree acceptance aperture for detection of the gloss signal. It is common to use more normally incident light (20 from the normal) for printed paper or very smooth paper. The TAPPI 20 uses a 5 acceptance aperture. A grazing incidence light beam will spread less than a beam with incidence near the normal. This fact, combined with the different detector apertures for the two TAPPI instruments, makes the 75 instrument suitable for relatively rough surfaces and the 20 instrument suitable for much smoother surfaces. The choice of incidence angle and detector aperture should be chosen so that the specularly reflected beam is only partially captured by the measurement aperture. Surface roughness variations, leading to variations in the width of the specularly reflected beam, will then change

the intensity of light falling into the sensing aperture. /22--25/ ***Goniophotometry. In goniophotometry, the distribution of light intensity reflected from a surface is measured with high angular resolution. The width of a specularly reflected light beam can thus be measured with high accuracy. The width of the reflected beam is calculated either as a full width at half maximum, for example, or as the standard deviation of the angular distribution of reflected optical intensity, which is approximately Gaussian. This angular distribution is caused by the deviation of microscopic surface facets from the macroscopic plane of the surface. An example of such a facet is the face of a kaolin platelet at the surface of a paper coating layer. These facets are too small to be resolved with the unaided eye, but are responsible for the apparent glossiness of a surface. The lower the width of the goniophotometer curves the glossier the appearance of the surface. Figure 3 illustrates the facet angle model, showing how the Gaussian reflection peak arises from the Gaussian distribution of facet angles. Figure 4 shows how this relates to the visual perception of the sharpness of gloss. <Figure 3. Facet Angle Model Explanation of Goniophotometer Peak Formation.> <Figure 4. Visual Perception of Goniophotometer Peak Width.> This measurement differs from TAPPI standard gloss measurements in that the angles resolved are closer to those resolved by the human eye (< 1) and the spot size at a 75 incidence angle is approximately 1 x 3 mm (dependent upon the light source used). This type of device may also be used to measure the effective index of refraction of a surface. This is done by finding the ratio of intensities for light polarized parallel and perpendicular to the plane of incidence. The index of refraction is then found using the Fresnel equations. For coatings with equal solid phase indices of refraction, differences in the effective indices of refraction are indicative of differences in the void volume at the coating surface. Although goniophotometry can be used to measure the effective index of refraction of a surface, peak width measurements are independent of the refractive index. This is in contrast to gloss measurements. Gloss measurements of printed surfaces are strongly influenced by the high index of refraction of inks and are thus almost always greater in value than measurements done of unprinted surfaces. However, goniophotometric measurements show that printed surfaces are frequently rougher than unprinted surfaces, and this increased roughness can be seen./26--31/ ***Specular reflectance uniformity. Several different strategies have been employed for the measurement of specular reflectance, or gloss, uniformity. The Tobias Mottle Tester was originally designed to measure print density mottle using a drum scanner and densitometer sensor head. Gloss mottle can be measured with this device by replacing the densitometer head with a specular reflectance measurement head. Another technique for imaging gloss mottle involves illuminating a sample with a large area

collimated light beam and placing an imaging device in the specular reflection path. This technique can yield high spatial resolution. However, there can be spatial variation in the gloss angles measured. Other proprietary devices are based upon x-y sample scanning and tightly focused light beams. These devices yield high spatial and intensity resolution with optical geometries that are position invariant. However, this type of measurement involves complex optical systems and is relatively slow. Measurements of visual sensitivity to print density mottle have indicated that the smallest feature sizes that can be perceived are on the order of half a millimeter. However, due to the much higher contrast, it is probable that gloss mottle features an order of magnitude smaller can be visually perceived, on the order of 50 microns. /32--39/ *Bulk Structure **Mercury Porosimetry Mercury porosimetry is one of the most widely used techniques for measuring pore size distributions of paper coatings. The measurement principle in mercury porosimetry involves immersing a sample in mercury and measuring the volume of mercury that intrudes the sample as the pressure is increased. Mercury does not wet the surfaces of paper components, so all void intrusion is forced by the applied pressure. At any particular pressure, there is a minimum void dimension that will be intruded. Thus, it is possible to determine the distribution of void sizes in a sample by increasing the pressure in discrete steps. Particular problems with mercury porosimetry are system and sample elasticity and the possibility of narrow necked, or bottle shaped, voids. System elasticity can, in principle, be determined and corrected. However, this correction is difficult and rare in practice. Sample elasticity will vary, but can be partially corrected for on theoretical bases. It is generally not possible to identify narrow necked voids. Such voids will not be intruded until the applied pressure forces the mercury through the neck. The analysis will then erroneously indicate that there is a void volume that has a minimum dimension equal to the neck minimum dimension. When examining mercury porosimeter data derived from coated paper samples, there is a tendency to assume that a calculated mean pore radius for a sample is indicative of a characteristic pore size within the coating. Unfortunately, the mean pore radius for a coated paper sample is typically influenced more by the larger basestock pores and the system and sample elasticities than by the small pores within the coating layer. However, there are typically identifiable peaks in the pore size spectra of coated papers in the neighborhood of 50 to 100 nanometer pore radius. The peak position on the pore radius axis and the volume represented by the peak both appear to vary logically with alterations to samples. /40--42/ Figure 5 two sets of mercury porosimeter pore size spectra. These are only partial spectra, showing only coating pores rather than the entire spectra including basestock porosity. Each set

consists of two separate scans performed on identical paper samples, showing that the measurement has good reproducibility. The two scan sets are from paper coated with different coatings on the same basestock. Although the Fine #1 Kaolin coating has greater total pore volume, the larger pores produced by the Engineered Kaolin create greater optical scatter and thus better opacity and brightness. <Figure 5. Mercury Porosimeter Coating Pore Spectra Produced Using Different Coating Pigments.> **Fluid Imbibition Dynamic fluid imbibition measurements have been made in a few different ways, with the hope of predicting or explaining print density, print mottle, fountain solution interference and glueability. Capillary suction testing involves filling a capillary tube with a fluid of interest and bringing the end of the capillary into contact with a paper surface. Fluid drawn from the tube into the paper is measured against time, and the paper area wetted is also easily measured. An enhancement of this is to scan the capillary across the paper surface to detect nonuniformity in the absorption. Care must be taken to insure that the end of the capillary tube has a diameter narrow enough to resolve absorptivity features of interest, for example, on the order of half a millimeter for print mottle. This is because the fluid will tend to form a film between the end of the tube and the paper surface, so that lateral resolution is defined by the outer tube diameter rather than the inner diameter. Absorption of impinging fluid droplets can also be measured using image sequences from dynamic fluid droplet contact angle analysis equipment. /43--45/ **Air Permeability There are several different devices used to measure the flow of air through a paper sheet. Examples of these include the Parker Print-Surf, Gurley porometers and the Sheffield device. Low pressure Gurley instruments are generally not suitable for coated papers due to extremely long measurement times. Air permeability measurements can provide information about the relative porosities of different sheets. If two different coatings on the same basestock have different air permeabilities, it is possibly due to structural differences within the coating layers. It should be noted that, due to the low viscosity of air, these measurements are related more to total pore volume and pore connectivity than to pore size. /46--49/ **Staining There is a wide variety of staining techniques that can be used to help characterize the structure of paper coatings. Osmium and iodine can be use to stain latex and starch binders, respectively. Microscopic electron or optical imagery can then show the spatial distribution of these coating components. Other common techniques include Croda red wipe and K&N staining. These are thought to help show the structure and porosity of coatings through the strength of the staining. Coatings that are more open will imbibe greater amounts of the stain, resulting in a greater color or brightness change. Local variation in the stain density may be predictive of some types of print mottle. Varying the length of time that coatings undergo staining can show qualitative

differences in absorptivity between papers. A major advantage of these types of techniques is that they can be done with simple equipment, yet yield data in good agreement with more complex techniques such as mercury porosimetry. /50,51/ **Brightness, Color and Opacity The brightness, color and opacity of papers are all affected both globally and locally by coating structure. Addition of structuring pigments or chemicals can enhance coating optical scatter, providing higher brightness as well as greater whiteness and opacity. Local coatweight variations can greatly influence the uniformity of these attributes. There are a number of standardized techniques available for measuring these optical properties. Preferences between types of instruments vary with both application and geography. /52--60/ **Transmitted Light Imaging Transmitted light imaging can be performed in a variety of ways. Pinhole source and detector scanners can be used, as can light tables or suitably equipped microscopes. Both the basestock and the coating contribute significantly to optical absorption and scatter. It is difficult at best to separate the two influences. Even if an uncoated basestock sample is available for characterization, it is probable that the coating operation itself will alter the properties of the basestock. It is possible to compare different coatings on the same basestock, as long as coatweight effects are taken into account. /61/ **Coating Burnout Imaging A technique that is in some ways similar to transmitted light imaging is coating burnout imaging. This technique allows measurement of the lateral variation of coating properties. Using this technique with uncalendered sheets gives an indication of coating mass distribution. Comparison of the burnout brightness distribution of calendered to uncalendered sheets provides an indication of the porosity distribution of the calendered sheet. /62/ **Transmitted Electron Imaging An advantage of using electrons (or beta rays) rather than photons in transmission imaging is that electrons are more strongly influenced by the coating than the basestock. This is due to the higher average atomic weight of inorganic pigments in comparison to the predominately carbon basestock. Heavier atoms have denser electron clouds, and thus interact more strongly with beamed electrons. Thus, a transmitted electron image will give a more accurate picture of coatweight distribution than a transmitted light image. /63/ **Kubelka-Munk Theory Kubelka-Munk theory can be used to deduce information about relative pigment packing efficiency within coatings. It is sometimes naively assumed that pigment scatter is an intrinsic property, and that the scatter of pigment mixtures can be calculated as linear combinations of the

component pigments. However, this is not so, as scatter depends intricately upon the environment in which a pigment particle is immersed. It is not difficult to produce pigment mixtures that pack either better or worse than the individual components. These will yield scatter coefficients below or above those predicted by linear combination calculations. Thus, if a coating formulation produces a scatter higher or lower than expected, it may be deduced that the coating has a different porous structure than its components would have alone. Differences could be either in the total pore volume or in the average pore radius. /64/ **Physical Cross Sectioning Physical cross sectioning provides some of the best information obtainable about the internal structure of paper coatings. However, it can be highly labor intensive. Typically, a paper sample is embedded in a hard, penetrating media such as epoxy or acrylic to minimize sample deformation during microtoming or grinding. The embedding medium should be chosen based upon the sample type. Thick samples such as boards with multiple heavy coating layers require the use of a low viscosity, slow curing epoxy. Samples with components that may diffuse into the medium require a rapid curing medium such as an acrylic. Alternatively, it is possible to obtain relatively high quality cross sections using freeze fracture techniques. This can be done by freezing the specimen with liquid nitrogen, for example, then fracturing with a knife edge. Such cross sections are typically suitable for electron microscopy. However, the unpolished roughness of such sections may be great enough to exceed the limited depth of field of most optical microscopes. When scanning electron microscopy is used to image a sample, the solid block is usually used. A transmission electron microscope requires the use of thin sections. An optical microscope can be used with either thin sections or a block. However, if optical fluorescence imaging is employed, a thin section must be used to avoid fluorescence from within the bulk of a sample. Optical microscopes have sufficient resolution to measure coating thickness or the roughness at the top of the coating or at the coating/basestock interface. Optical fluorescence imaging techniques can be used to gauge the penetration of fluorescent penetrant fluids, and stains can be used to measure the distribution of starch, for example. Electron microscopy offers higher resolution so that multiple coating layers can sometimes be distinguished by differences in pigment particle size. Elemental mapping may also be carried out, for example to identify the location of osmium labeled latex. Cross sectional examination can reveal many different structural features of paper coatings, for example, the coating thickness distribution. The shape of this distribution can show differences in the tendencies of coatings to penetrate the basestock. These can be seen by comparing the maximum depth of penetration and the skew of the distribution. The mean coating thickness, combined with knowledge of the coatweight, yields the bulk of the coating. Coating bulk relates to optical scatter, and can be influenced by coating formulation, application and finishing. The roughness of the top of the coating layer can be compared to that of the bottom of the coating (the top of the basestock) to find a smoothing index, which is dependent on the coating formulation and application as well as the basestock itself. On multiply coated grades, the

tendency towards delamination between layers can sometimes be compared. /65--68/ Figure 6 shows an optical micrograph of a double coated board cross section. This image was acquired using reflected light. Note that the two coating layers are easily differentiated due to a gross difference in the brightness of the pigments in the two layers. A significant amount of coating pigment can also be seen to have penetrated below the top fibers of the basestock. <Figure 6. Optical Micrograph of a Double Coated Board Cross Section.> **Neutron Scattering Neutron scattering can be used to deduce information about the structure within paper coatings. With proper choices of neutron energy and grazing incidence angle, it is possible to determine the average alignment of clay platelets in a coating layer, for example, as well as the variation in the alignment. The great disadvantage of this technique is that there are very few facilities worldwide in which this type of experiment can be conducted. /69/ **X-ray Diffraction X-ray diffraction measurements can be used to measure the degree of alignment of kaolin particles. By slow and careful measurement of the shape of the primary kaolin diffraction peak, an alignment index can be found. However, this technique requires that the detector be held motionless for lengthy periods as various angles in order to measure the peak shape with sufficient accuracy. Some X-ray diffractometers insist on continuously scanning the detector and thus are not suitable for this technique. An advantage of this technique over neutron scattering is that suitable X-ray diffractometers are readily available. /70, 71/ *Effects of Coating Structure **Brightness, Opacity and Color Coating structure can affect measurements of sheet brightness, color and opacity in several ways. Brightness meters that employ directional lighting (GE geometry) have greater sensitivity to surface finish than diffuse (ISO geometry) instruments. Thus, changes in sheet gloss will affect GE brightness readings more than ISO readings. The primary influence of coating structure on these measurements is through optical scatter. Optical scatter has a linear dependence on coating void volume, that is, if you double the void volume (without affecting void size) you can expect the scatter to double. The dependence of scatter on void size is highly nonlinear. If you double the size of voids, the scatter could quadruple, for example. This is due to the wave nature of light. There will be an optimum void size, on the order of half a wavelength, that will give greater scatter than larger or smaller voids. **Sheet Gloss

Sheet gloss is primarily dependent upon the surface structure of coating. measurement can be responsive to a broad bandwidth of feature sizes. This include features from the microscopic, on the order of 100 nm or less, all macroscopic features approaching the size of the area illuminated on the sheet. bandwidth affecting different glossmeter geometries will vary somewhat.

This type of bandwidth can the way up to Of course, the

Theoretically, sheet gloss should also be responsive to the effective index of refraction of a surface. It is the index of refraction of a surface that determines the reflectivity of that surface. The index of refraction depends on both void volume and the material present in the coating. However, most pigments and binders have very similar indices of refraction, between 1.5 and 1.6. Titanium dioxides do have much higher indices of refraction, 2.5 for anatase and 2.9 for rutile. Increasing levels of TiO2 should increase the index of refraction (if roughness is constant) and reflectivity and thus the gloss of a surface. In the same way, increasing the void volume (with air's n 1) should decrease the index of refraction and thus the gloss./72/ **Print Gloss Print gloss and delta gloss are strongly affected by both the surface and the bulk structure of coatings. Of course, the strongest influence on print gloss is the sheet gloss. Print gloss is also affected by pore radius and by microscopic surface topography. Interestingly, the fact that sheet gloss and microscopic topography both influence print gloss independently suggests that the micro-topography influences print gloss in a different way than it influences sheet gloss. The effect of pore radius on print gloss is possibly through both capillary pressure and phase separation. Smaller pores have higher capillary pressure and thus greater suction pulling the ink from the paper surface. Inks are typically multiphase systems composed of pigments, resins and solvents. It has been hypothesized that fine pores could pull the solvent from the full ink and thus set ink more rapidly than large pores. It has also been theorized that surface pores are of greater importance than bulk pores. However, neither of these ideas seems to have been proven quantitatively. Sheet gloss is influenced by a broad bandwidth of roughness from the microscopic to the macroscopic. Yet, print and delta gloss are influenced by microscopic topography independently of sheet gloss. The reason for this is that the ink layer is capable of hiding a significant amount of microscopic roughness. This mechanism is independent of the influence of microtopography on sheet gloss./73--77/ **Print Mottle Print mottle is a general term that describes an uneven appearance of color density or gloss of a halftone or a solid print area. It is most visible in uniform color areas where the surface fails to absorb ink evenly due to basestock formation or coat weight variations. Coated boards sometimes show mottling because of rough surface topography. Poor basestock formation can lead to print mottle through nonuniform compression during calendering, resulting in variation in coating layer densification. Sheets that contain binder migration, coat weight variations, inferior

coating profile and heterogeneous pigment blending can all cause mottle formation on the printed sheet. Several ink stain test methods work well in predicting print mottle. K&N ink and Croda Red Wipe are frequently used in the mills and paper testing laboratories. Print mottle can be measured many ways. Popular techniques include programmable scanning densitometry and digital image analysis. Densitometer heads typically have sensing heads with lateral resolution on the order of a millimeter, which is too large to resolve the finest features to which the visual system is responsive. These systems can usually be programmed to measure the variability in many different print areas. Image analysis systems can have pixel sizes on the order of tens of microns, easily exceeding human visual resolution. General mottle analysis systems typically assume that input images are supposed to represent single tones, and that any variation is representative of error in the print process. Either solid tones should be used, or halftone dots should be unresolved or digitally filtered out. The mean intensity and standard deviation yield the contrast of the mottle, which can be calculated as the ratio of the standard deviation to the mean. The contrast is probably the single strongest influence on the visual perception of mottle. However, the lateral size of features, and lateral periodic variations in the density also contribute to visual perception. The lateral size of random features can be found by calculating the autocorrelation length along the intensity surface. The worst (most strongly perceived) feature size is about 1 or 2 millimeters, with the strength of perception dropping off for very small or very large features. Many organic visual systems (specifically including mammalian vision) are hardwired to respond to periodic features, which can be measured digitally using frequency transforms, such as the Fourier or wavelet transforms. Frequency domain power spectra should be weighted against a visual response function to determine the visibility of mottle features. A halftone print, for example, takes advantage of the averaging functions in the visual system to produce apparently continuous color variations. Other types of texture analysis, co-occurrence matrices for example, can also be used to predict the strength of perception of print mottle./78-88/ **Offset Halftone Dot Fidelity. The fidelity of halftone dot reproduction can be influenced by coatweight as well as coating structure. LWC coatings, for example, frequently leave partially exposed wood fibers that can cause ink to wick. It should be expected that variation in coating structure will influence dot size, with more closed, impermeable areas allowing dots to spread more. Variability in dot size and shape can make process print colors appear muddy and washed out. Measurement of halftone dot size and shape can be done routinely with microscope-based image analysis systems. Full color systems can sometimes analyze overprinted dots using color thresholding techniques. Many dots should be analyzed from multiple sheets of particular paper samples to account for both large and small scale variations in the papers. There will usually be strong overlaps in the populations of dot sizes and shapes among different paper samples. However, if sufficient numbers of dots are measured the means of these populations can usually be statistically differentiated. /89/ Figure 7 shows an optical micrograph of offset halftone dots from a fleshtone area of a print. Note that with a full color image analysis system it was possible to identify a dot of one color

even though it overlaid a dot of another color. <Figure 7. Offset Halftone Dots, with One Dot Digitally Identified.> **Blister Resistance Blistering occurs in the drying ovens of heatset offset printing presses. As the paper is heated to set the ink, moisture in the basestock will evaporate. If the vapor can not easily escape through the coating layer, internal pressure can build up to the point that the paper literally explodes. It is intuitively obvious that more open coating structures should have greater resistance to blistering. Measurements of air permeability should correlate well to blister resistance./90/ **Glueability and Surface Strength There are several different glues used in the packaging industry. However, many board producers rely upon K&N ink brightness loss as a measure of glueability. Absorption of K&N ink can be related to coating pore size and volume. Use of engineered pigments to open up the coating structure can enhance K&N ink absorption as well as surface strength as measured by laboratory picking. However, these types of pigments also have lower surface area than more traditional pigments. Thus, it is debatable whether the added pick strength and glueability are due to the more porous structure or the lower binder demand, and thus greater strength, of coatings produced with engineered pigments./77/ **Rotogravure Printability The most common rotogravure printability measure is that of the prevalence of missing dots. A common measure is the distance to the twentieth missing dot on an IGT Heliotest print. This measurement is typically performed by a technician, hunched over a workbench and rapidly becoming nearsighted. More modern methodologies employ digital image analysis with automatic sample and camera positioning. Dot identification algorithms can be based on thresholding techniques, or can discern the spatial distribution pattern of dots using local intensity minima hunting operators. Advantages of digital systems include machine objectivity, the ability to measure larger sample sets more quickly and ability to find the percentage of missing dots as well as the adjacency number. The adjacency number is the average number of missing dots in a group, and has been claimed to be more closely related to visual perception of quality than the percentage of missing dots. Regardless of how missing dots are measured, they are generally due to poor contact between the paper and the printing roll. Poor contact may be blamed on surface roughness. However, the dynamic, compressed roughness of the paper in the printing nip may not be similar to the uncompressed roughness. Thus, it is common to measure the compressibility of rotogravure papers. Measurements of dot fidelity and print density uniformity can be applied to rotogravure prints as easily as to offset prints. However, a characteristic of rotogravure printing is the desirability of the ink forming a continuous film of varying thickness, rather than offset printing's varying halftone dot sizes. Thus a measure of ink film continuity is also useful. A typical measure is the

ink density at which a film looses its continuity, lower being better./91,92/ Figure 8 shows an IGT laboratory rotogravure print of well separated dots suitable for missing dot counting. Figure 9 shows a Diamond International laboratory roto print of a specific tonal density at which the continuous ink film has begun to break up. In some areas of this image there appears to be a continuous ink film while in other areas discrete dots are visible. <Figure 8. Laboratory Rotogravure Print of Dots Suitable for Missing Dot Counting.> <Figure 9. Laboratory Rotogravure Print of Tone Where Continuous Ink Film Breaks Up.> **Inkjet Printability The wide variety of physical processes employed in different types of nonimpact printing require an equally broad range of coating structures. Highly fluid ink jet inks will tend to wick along exposed fibers. Thus, measures of dot fidelity and edge sharpness along solidly printed areas become important. These can quantify the ability of the coating structure to localize the large volumes of ink typically used in this printing method. Thermal prints, from facsimile machines for example, are dependent upon the thermal diffusion properties of coatings, as well as the smoothness to insure good thermal contact. Color laser printability is also dependent upon thermal properties of coated sheets that may have to withstand multiple toner fusion processes. /93,94/ Figure 10 shows an image of inkjet print dots printed on a premium coated inkjet paper. Note the poor shape of these dots. This is due in part to the lateral motion of the inkjet printhead as it is ejecting dots toward the surface. However, the paper coating can have a significant influence on the shape and size of inkjet dots. <Figure 10. Inkjet Print Dots.> *Conclusions There are many techniques available for studying paper coating surfaces, structures and printability. Some have been in use for decades, others are in various stages of development or deployment. Perhaps the greatest challenge lies in finding the right technique to employ in attacking a particular problem. A primary goal of this paper was to provide a resource for researchers to be able to identify the appropriate techniques for their problems. Interested readers should consult the references before making any decisions about the applicability of particular methods. *References **Surface Physical and Optical Properties 1. Thomas, T.R., "Characterization of Surface Roughness," Precision Engineering, 3(2):97

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