The present invention concerns a method for measuring a surface characteristic of a sample, and apparatus for carrying out the method.
There are many applications in industry where it is essential to accurately determine a variety of optical surface characteristics, one such area being that of paper manufacturing. To regulate paper manufacture, the paper must be assessed to determine its surface properties, which usefully include the gloss, surface refractive index and the roughness.
Conventionally, the measurement of surface characteristics has been achieved by the use of a goniometer. A goniophotometer capable of measuring the angular gloss distribution of a sample (Gate & Leaity, 1991; Gate & Parsons, 1983) is shown schematically in
In use the goniometer must scan through a range of angles at a first polarisation, and then scan through the same range of angles at a second orthogonal polarisation. This makes the goniometer extremely time-consuming to use and also introduces the risk of systematic errors if the two scans are not perfectly aligned.
It is an object of the present invention to provide a method and apparatus for measuring surface characteristics of a sample more efficiently and with less chance of alignment errors. This object is achieved by obtaining all the necessary optical information in a single measurement, with no relative movement of the sample and detection apparatus.
In accordance with a first aspect of the present invention there is provided a method for determining a characteristic of a sample as set out in the accompanying claims.
In accordance with a second aspect of the present invention there is provided an apparatus for determining a surface characteristic of a sample as set out in the accompanying claims.
The invention will now be described by way of example with reference to the following figures, in which:
Before describing embodiments of the invention in detail, it is necessary to outline some of the background theory to explain how the surface characteristics of interest are derived. In particular, four such characteristics will be discussed: surface refractive index, gloss, macro-roughness and micro-roughness.
Surface Refractive Index (n):
This is a very sensitive measure of surface composition. With some prior knowledge of the material, it can give important insights into changes and properties at the surface. For example, in coated paper it can be related to particle packing and surface porosity, or in printed surfaces to the ratio of resin/ink pigment at the surface.
The reflectance of light from a perfectly smooth, homogeneous, isotropic and non-absorbing substrate is described by the Fresnel equations for S and P polarised light:
Where
The angle θi is the angle of incidence and n is the refractive index of the reflecting medium. Transmission coefficients are given by
Ts0=1−Rs0 and Tp0=1−Rp0 (4)
Thus light with an incident intensity I0 has reflected intensity R=I0R0. By measuring the ratio Rp0/Rs0, one can deduce the refractive index of the reflecting substrate. By using (1), (2) and (3), one obtains
where
ρ=√{square root over (Rp0/Rs0)} (6)
Therefore it can be seen that in order to determine the surface refractive index, it is necessary to use both S and P polarised light and compare their reflected intensities.
Macro-roughness:
This is roughness on a scale>wavelength of light, and may affect the gloss of the surface depending on the gloss measurement geometry. In the example of coated paper, the macro-roughness is usually dependent on the substrate of the sample, e.g. paper fibre. The macro-roughness is defined here by a facet model, which treats the surface as being made up of a distribution of facets, each of which is assumed to be perfectly smooth, homogeneous, isotropic and non-absorbing and therefore reflects light specularly according to the laws of geometrical optics, e.g. Fresnel's equations and Snell's Law. The distribution in inclination of facets to the surface normal gives rise to an angular distribution of the reflected light.
If the number distribution of facets is described by some function F(θf), where θf is the inclination of the facet from the surface normal, then the intensity reflected in the plane of incidence at some angle θ is described by
Rs(θ)=F(θ−θi)Rs0 (7)
and similarly for Rp, where θf=θ−θi. Normalisation is such that
∫(Rs+Ts)dθ=1 (8)
which implies
∫F(θ)=1 (9)
A Gaussian distribution is a well-studied form for F(θf), and one that works well for many surfaces:
Where it is assumed that the average slope is zero. The parameter Σ is the half-width of the distribution, which will be termed the macro-roughness. The Gaussian distribution will not give a good description of the surface if it contains bumps and pits introducing facets with extreme values of surface slope.
The above theory relates to reflection from a one dimensional surface. In practice of course, real surfaces are two dimensional and the reflection and scattering takes place in three dimensions. A given facet may be described by two angles, θf and φf, being the inclination of the facet normal to the mean surface normal in the plane of reflection and orthogonal to the plane of reflection respectively. The observed angular distribution of light from a facet surface is governed by the facet distribution (eqn. (10)) and the angle of incidence θi according to the laws of geometrical optics.
The macro-roughness Σ is given by the half-width of the angular distribution of the reflected light in the plane of incidence.
Micro-roughness:
This is roughness on a scale≦wavelength of light and strongly affects the gloss of the surface. In paper coating, it is due to mineral particles, and in ink due largely to organic ink pigments. Because both macro and micro-roughness affect gloss, it is important to differentiate between them. They are both important for other material properties, for example the printability of a substrate.
The determination of micro-roughness here uses the analysis of Beckmann and Spizzichino (1963) for scattering from rough surfaces which gives a general solution valid for a wide range of roughness under the Kirchoff approximation.
The most important case of a random rough surface is the Gaussian distribution of surface heights z, defined such that the mean height <z>=0 and the distribution of z is given by
where σ is the standard deviation (and is also coincidentally equal to the rms value of surface roughness). The surface is described also by an autocorrelation function, which provides information about the density of surface irregularities:
C(τ)=e−r
where τ is the distance between two points and T the correlation distance, the separation for which C(τ) drops to the value 1/e.
The general (1-D) solution for the scattered intensity is
Note M(θi,θ)=<ρρ*> in Beckmann's notation, which gives the mean intensity scattered at an angle θ from the surface where the angle of incidence was θi and where
L is the length of the surface being examined. The principal limit on the realm of validity of the above equation is that the radius of curvature of the surface roughness features is large compared with the wavelength of light, expressed formally as
4πrc cos α>>λ (17)
where rc is the radius of curvature and α the local angle of incidence. In addition it is required that L>>T and L>>λ.
As a general result, the reflectance into the specular direction is modified by a factor (Beckmann and Spizzichino 1963), giving:
M(θi,θl)=exp−(4πσ cos θl/λ)2=R/R0 (18)
Where θi is the angle of incidence, λ is the wavelength of the incident light, σ is the micro-roughness parameter and R0 is the specular reflection from an optically smooth surface of the same refractive index at the given angle of incidence.
The Beckmann model relates to a perfectly conducting rough plane, however Gate (1973) and Hensler (1992) found that the model as applied to specular reflection of dielectrics appeared valid and gave useful insights into surface micro-roughness, yielding fair correlation with roughness measured by other techniques.
Looking at eqn. (18), it can be seen that there are therefore several ways of determining micro-roughness. For example, measurements of the reflected intensity can be taken for more than one angle of incidence using the same wavelength. Alternatively, measurements of the reflected intensity can be taken for different wavelengths at the same angle of incidence.
Separating Micro- and Macro-roughness:
It has been seen that macro-roughness produces a bell-shaped intensity distribution centred on the specular angle. If micro-roughness is now also considered, it has been found that it has the effect of reducing the overall reflectance of the surface leading to a decrease in the measured intensity. It also shifts the centroid of the distribution toward higher angles, away from the specular angle. However, the width of the reflection image is not greatly affected by slight-moderate micro-roughness. For typical coated papers, experimentation has shown that σ is commonly in the range 0.1 to 0.3 μm, while Σ is commonly in the range 1°-3°. The differences between papers are likely to be such that at this level the width of the reflected image can reasonably be taken as a first approximation to the macro-roughness. Furthermore, the area (reflectance) under the reflected image is related almost linearly to the micro-roughness σ. This permits a further method for the determination of micro-roughness, by measuring the total reflectance or area (Aobs) under the reflection image and comparing it to a calculated total reflectance or area (Acalc) under the image produced by reflection from a smooth standard surface of known refractive index, such as highly polished glass. The ratio of Acalc/Aobs can then be related to σ, e.g. by using eqn. (18). This technique will be further explained later.
Gloss:
The gloss of a surface may be defined in a number of ways (e.g. Tappi T480, DIN 54502 standards). Effectively it is a measure of the reflectance of a surface relative to some standard, but the measurement must also be defined in terms of wavelength measurement geometry, and in particular in terms of the acceptance angle of the detector. A general definition for gloss may be given (as a percentage) by
where the integral is of reflectance over some particular solid angle. Note that R=0.5 (Rp+Rs), while R0 is the reflectance of a perfectly smooth standard material of given refractive index.
To determine all of the surface refractive index, gloss, macro-roughness and micro-roughness parameters with one instrument in one static measurement step, it is necessary to provide an instrument that can supply illuminating beams of collimated light of S and P polarisation at the same wavelength and angle of incidence, and a further beam of either polarisation at either a different wavelength or a different angle of incidence, together with a detector capable of angularly resolved intensity measurement.
The phase modulated light is then passed through a sheet polariser 8 to ensure plane polarisation in a fixed direction such that the plane of polarisation is perpendicular to the sample surface, i.e. P-polarisation. The plane polarised light then passes through a switchable polarising means, in this case a liquid crystal variable retarder 9. By applying a suitable AC voltage signal to the liquid crystal retarder, the plane of polarisation may be made to switch through 90° so that the plane of polarisation is parallel to the sample surface, i.e. S-polarisation.
The collimated light then passes through apertures 10, 11 whose diameters define a particular area of illumination on the sample. The light is reflected by a fixed plane mirror 12 such that the first beam is incident onto the surface of sample 13 at an angle of around 75° to the surface normal and the second beam is incident at an angle of around 73°. Light scattered from the sample surface within approximately ±10° is collected by a second fixed plane mirror 14 and directed onto a lens assembly 15. An imaging detector 16 is placed at the back focal point of the lens assembly such that the angle of the incoming light with respect to the optical axis is mapped to a given position on the detector.
The imaging detector 16 is for example a charge coupled device (CCD) or complementary metal oxide semiconductor (CMOS) camera, which can record an intensity angular distribution image of the scattered light, such that the intensity in a given image pixel can be related to the intensity scattered by surface facets at a given (θ,φ) orientation. Using a static imaging detector is more efficient than using a goniometer which has a small acceptance angle and must be moved round to obtain various angular intensity measurements. The exposure time of the image of scattered light must be sufficiently long to ensure that speckle effects are substantially removed by time averaging.
In use, the reflectometer is operated as follows. Firstly, the first laser source 1 is used to produce a collimated beam, which is passed through phase modulating beam expander 3, 5a, 6. The phase modulated light is then polarised by the sheet polariser 8 to confer P-polarisation. The polarised light illuminates the surface of sample 13 at an angle of 75°. The scattered light forms an image (a) which is measured at the detector 16. Secondly, using the same laser source, the liquid crystal retarder is switched to change the plane of polarisation to produce S-polarised light. The scattered light then forms image (b) which is measured at detector 16. Thirdly, the laser source 1 is turned off, and the second laser 2 is used instead. The light is passed through phase modulating beam expander 4, 5b, 7. The phase modulated light may be polarised with either P or S polarisation, it is not important which is used. This beam illuminates the sample surface at an angle of 73°, and the scattered light forms an image (c) which is measured at detector 16.
The ratio of image intensity in images (a) and (b) gives Rp/Rs which is used with equations (5) and (6) to calculate the refractive index. In general the incident intensities of the various lasers are not the same, but the relative intensities are measured and used to adjust the value of Rp/Rs accordingly. When calculating the refractive index, the angle of incidence used should not equal the Brewster angle.
The intensity in images (a) and (b) may be integrated over a given solid angular range and used with equation (19) to calculate the gloss according to any definition so long as the acceptance angle does not exceed ±10°.
The intensity distribution through the centre of the reflection image in the θ and φ directions is calculated by averaging a number of tracks and the half width half maximum (HWHM) obtained for the θ direction by calculating the standard deviation of intensity about the centroid. This procedure gives the macro-roughness Σ as defined by eqn. (10). The complete observed angular distribution of scattered light may be transformed into a distribution of facet angles for graphical display or calculation of other statistics by knowledge of the system geometry and geometrical optics.
With this apparatus, the micro-roughness can be determined by two methods:
In practice, measuring at the specular angle alone is not particularly useful owing to the noise in the imaging detector. Either an area must be integrated, or repeat measurements taken (or both).
or
As an alternative to using two beams of the same wavelength but different illuminating angles, it is possible to utilise two beams arranged at the same illuminating angle but with different wavelengths. Such an arrangement is shown in
In use, this arrangement of reflectometer is operated as follows. Firstly, the first laser source 21 is used to produce a collimated beam which is passed through phase modulating beam expander 23, 25, 27. This beam is polarised by the sheet polariser 30 to confer P-polarisation. The polarised light illuminates the surface of sample 33 at an angle of 75°. The scattered light forms an image (a) which is measured at the detector 37. Secondly, using the same laser source, the liquid crystal retarder is switched to change the plane of polarisation to produce S-polarised light. The scattered light then forms image (b) which is measured at detector 37. Thirdly, the laser source 21 is turned off, and the second laser 22, which has a different wavelength, is used instead. This produces a collimated beam which is phase modulated by phase modulating beam expander 24, 26, 28. The beam may be polarised with either P or S polarisation depending on the switching state of the liquid crystal retarder. It is not important which polarisation direction is used. The beam illuminates the sample surface at an angle of 75°, and the scattered light forms an image (c) which is measured, time-averaged, at detector 37.
The refractive index, gloss and macro-roughness are then determined in exactly the same manner as for the first embodiment, as images (a) and (b) correspond in both cases.
The micro-roughness may be determined in two ways:
The arrangement shown in
An alternative arrangement using light of two wavelengths is shown in
The use of three lasers, without polarisation switching, allows simultaneous imaging to be achieved. Such an arrangement is shown in
A further embodiment of the invention is shown in
The effect of the beam separating polariser 71 is shown in more detail in
As in the embodiment of
The macroroughness (expressed as the standard deviation of scattered intensity about the specular angle, as described earlier) is obtained from the standard deviation of the angular distribution of the forward scattered light as measured on the imaging detector 97. The refractive index and microroughness may then be calculated using the intensity of the scattered light as described previously. A potential problem with the imaging detector for measuring specularly reflecting samples is that a very small intense spot may be formed on the image which gives poor measurement statistics. The photodiode 99 is not limited in this respect and is therefore appropriate for measuring the intensity for specularly reflecting samples. With proper calibration, the photometric measurements may be made using both imaging and photodiode detectors.
Before use the reflectometer is calibrated using a highly polished glass of known refractive index. Measuring this sample gives the intensities in the various measurements states corresponding to known refractive index and zero microroughness. This calibration eliminates the need to know precisely the reflection and transmission characteristics of the various optical components in the system.
With this embodiment, the sample is illuminated with P-polarised polychromatic light and an image is obtained which is separated into red, green and blue (RGB) intensities by the colour imaging device 118. The colour imaging device 118 uses filters to separate the colour components of the beam, and the R, G and B are hence wavebands determined by the camera characteristics. The polarisation is rotated to give S polarised light with respect to the surface and a second RGB image obtained. A refractive index is calculated for each colour (wavelength average) from the S and P intensities using procedures described for previous embodiments.
The relative intensities of the incident S and P light in each colour waveband is previously determined by measuring the reflection of a highly glossy material of known refractive index and dispersion. This calibration measurement also allows the relative intensity of R, G and B light in the incident beam to be determined, and the total intensity in each colour band to be determined.
The micro-roughness is obtained by comparing the intensity of colour pairs R-B, G-B and G-R for a given polarisation and using the method for determination by two wavelengths (described with reference to
In the calculation of refractive index and micro-roughness, intensities are used which are averaged over a wavelength interval defined by the colour discrimination characteristics of the imaging device. Both refractive index and micro-roughness vary with wavelength. In the absence of high absorption, changes to refractive index may not be large, and the refractive index obtained for a given colour interval is an average defined by the transmission characteristic of the filter used in the imaging device for the given colour, i.e. determined by the average reflectance over the given wavelength interval. Similarly micro-roughness will be an average based upon wavelength averaged reflectance values.
The macro-roughness is determined directly from the image of reflected light on the detector for each of R, G and B and at the two polarisation states.
A value for the gloss at each of the colours R, G and B is determined as described with reference to previous embodiments.
The colour shift relative to the colour at the specular angle is determined as a function of angle about the specular angle. RGB colour as measured may be converted to other colour representations; for example CIE L*a*b* according to well-known procedures. This parameter is of interest for special effects pigments.
In each embodiment described, a supplementary converging lens may be inserted with its front focal point at or near to the centre of the illuminated area on the sample. This lens produces an image of the sample surface, and in the case of specularly reflecting materials, effectively spreads the reflected beam over a larger area on the imaging detector. The low-angle image of the surface can be useful in some circumstances, presenting an impression of the spatial distribution of roughness features. For specularly reflecting samples, it is advantageous to spread the reflected beam over a large number of pixels on the imaging detector to obtain better intensity statistics. Other possibilities for achieving a spread of the reflected beam will be obvious to those skilled in the optical arts, including for example inserting a diverging lens immediately before the imaging lens assembly, or modifying that assembly directly.
In all embodiments, before measurements are made it is necessary to calibrate the system in some way to define the various incident intensities. This calibration is readily done using a highly polished glass plate of known refractive index. During operation of the instrument it may be desirable to continue to monitor the absolute and relative intensities of the various light sources, in a position after the phase modulating beam expander, but before the sample. By measuring the incident intensities in this way, it is possible to correct calibrated intensities according to any variations in light source output over a period of time. Ways of monitoring incident light will be apparent to those skilled in the art. For example, in
Although the invention has been described with reference to the embodiments above, there are many other modifications and alternatives possible within the scope of the claims. It is envisaged that the invention will be of particular application in the paper industry, to determine paper surface characteristics, although the invention is not limited to this field. It is not necessary to use lasers for the sample illumination, any collimated light source of suitable intensity could be used, for example filtered LEDs. In this case it would be unnecessary to use a phase modulating beam expander, as the light from an LED is substantially incoherent. Any type of switchable polariser could be used in place of the liquid crystal retarder. The surface characteristics may be mapped to the surface by repeating the measurements at a variety of points on the surface, and there may be adjustable mounting means for the sample to enable this to be done with the minimum of disruption to the apparatus. The wavelengths and angles of incidence quoted are exemplary only, and any suitable values may be selected for these depending on application and equipment available etc. The phase modulating beam expander used may comprise any suitable apparatus, for example a reflection diffuser may be used.
Number | Date | Country | Kind |
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0309690.6 | Apr 2003 | GB | national |
Filing Document | Filing Date | Country | Kind | 371c Date |
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PCT/GB04/01634 | 4/15/2004 | WO | 1/9/2007 |