Technology that is widely used in semiconductor manufacturing has been successfully applied to the accurate, nondestructive, in-line measurement of coatings on medical devices.
By: S. Morris, PhD, Nightingale-EOS Ltd, Wrexham, UK
Conventional methods
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| A magnified image of a stent: a beam profile reflectometry laser spot is aligned, ready to perform a coating thickness and index measurement. |
An increasing range of medical devices use surface coatings. Devices often have complex shapes, which creates a challenge in quality control of such coatings. There is currently no universally accepted method that is accurate, nondestructive and suitable for in-line production measurement of coatings on devices with complex shapes.
As many medical device coatings are transparent, optical methods dominate. There are two broad approaches in use for measuring a coating thickness optically.
| Figure 1: Schematic of a white-light interferometer. |
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Firstly, techniques such as white-light interferometry and confocal microscopy independently image the top surface and buried interface of the coating, inferring thickness from the amount of z-axis translation needed to go from one to the other. Figure 1 illustrates a typical white-light interferometer: light that is reflected from either the surface or the buried interface is made to interfere with light from the same incident ray that has been reflected from a half-silvered beam splitter and a small mirror placed just beneath the main objective lens. The beam splitter just below this mirror forms a reference plane. As the distance between the sample surface and reference plane varies so the spectral composition of the light that returns to the detector changes because of the interference effects.
| Figure 2: Schematic of a confocal microscope. |
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Figure 2 shows a confocal microscope arrangement. The principle here is that when light falling upon the sample surface or buried interface is in focus, then the reflected light is also brought to a focus at the pinhole beneath the detector and, thus, is able to pass through. When the light is out of focus at the surface, it is also out of focus at the pinhole and so is heavily attenuated. By scanning the focus across the surface and moving it down through the coating, a 3-D map of the coating surface and buried substrate can be built up.
Technical limitations
Both of these techniques are really intended as imaging methods rather than coating-thickness measurement techniques. They suffer from at least three serious limitations:
1. throughput is, by necessity, rather slow because of the amount of sample motion involved in taking a measurement
2. they only can be used where the coating thickness exceeds the depth-of-focus of the objective lens since, otherwise, the interfaces cannot be separately resolved
3. it is necessary to multiply the measured z-axis translation by the refractive index of the material to obtain the physical thickness of the coating.
These techniques can provide no information about the refractive index, and therefore must rely on assumed values measured by another technique, usually on bulk samples.
| Figure 3: General behaviour of light on encountering a coated surface. |
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An alternative approach is to intentionally combine light from the two interfaces and look for interference effects in the reflected light. As illustrated in Figure 3, overall surface reflectance is determined by the wavelength of incident light, the coating thickness, and the angle that the light travels relative to the surface. It is also affected by the refractive indices of both the coating and the substrate, and the polarisation of the light. Analysis of reflected light is usually carried out by keeping most of these factors constant and changing one or, at most, two of them in a controlled manner. In spectrophotometry and spectroscopic ellipsometry, the surface is illuminated by white light at a constant angle-of-incidence and the reflectance is measured as a function of wavelength. In the former case (Figure 4), normal-incidence light is used and the intensity of the reflected light is analysed. In the latter (Figure 5), a high angle-of-incidence is used and both intensity and phase are analysed. Even so, for medical device coatings these techniques face two significant problems. The first is that, as they depend on the assumption of a constant angle-of-incidence, it is difficult to align them on samples with complex shapes in such a way that the orientation and hence the angle-of-incidence is reproducible. This is a major source of error.
| Figure 4: Spectrophotometry measures reflectance as a function of wavelength at normal incidence. |
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Secondly, although the techniques offer some capability of measuring the coating refractive index, this is limited by the phenomenon of optical dispersion, namely the variation of refractive index with wavelength. Hence, they must measure not just one value, but as many values as there are wavelengths. This renders it impossible to make a deterministic measurement, as the number of parameters to be measured always exceeds the number of independent data points that can be collected.
In common with these latter techniques, beam profile reflectometry (BPR) works by analysing light reflected from the coated surface. Uniquely, however, it takes a different approach, keeping the wavelength fixed (using laser light) and measuring reflectance as a function of angle.
Beam profile reflectometry
BPR was first introduced by Therma-Wave Inc. in 19921,2 as a technique for measuring thin films on silicon wafers. Prior to the introduction of BPR, measuring reflectance as a function of angle involved complex and expensive hardware arrangements, where both the light source and detector needed to be moved each time a new angle was selected.
| Figure 5: Spectroscopic ellipsometry measures reflectance as a function of wavelength and polarisation at a fixed angle of incidence. |
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As illustrated in Figure 6, BPR overcomes this limitation by using a high-magnification lens to bring a collimated laser beam to a sharp focus. At the focal point, which is typically less than 1 µm across, light falls on the sample with the whole range of different angles-of-incidence through which the lens bends the light to achieve focus. After reflection, the lens recollimates the reflected light and there is a one-to-one correspondence between the physical location of a ray of light within the recollimated beam and the angle at which that ray was reflected from the surface. It is therefore possible to measure reflectance as a function of angle of incidence simultaneously for a wide range of angles (typically, for a ~100× lens, a range of 0–60˚) with a very short data acquisition time using an apparatus with no moving parts.
When the beam profile is viewed after reflection from a coated surface, a characteristic bull’s-eye pattern is seen because of the pattern of light and dark fringes that form as a result of the interference between rays as shown earlier in Figure 3. The amplitude of the fringes depends only on the refractive indices of the materials in the film stack. The period of the fringes is determined by the coating thickness. It is therefore possible to decouple the effects of thickness and refractive index and measure the two classes of parameter independently.
It can also be seen from Figure 6 that the beam profile differs slightly depending on whether the cross-section is viewed horizontally or vertically. This is because of the dependence of the sample reflectance on the polarisation of the incident light: the reflectance differs slightly for the two cases of s and p polarisation, where the ‘plane of incidence’ is respectively perpendicular and parallel to the polarisation. For unstrained films, both s and p signals contain essentially the same data; if the film is strained, as is often the case for polymer or diamond-like carbon films, then the two diverge. This is because of strain-induced birefringence, which causes the p-polarised light to experience a slightly different refractive index from the s-polarised light. Because BPR measures both the s and p polarised components independently, it is able to quantify this refractive index difference and so measure the strain in the coating as well as the other parameters.
| Figure 6: Schematic representation of a beam profile reflectometry system. |
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Because all these measurements take place at a single wavelength, determined by the laser source employed, there is no need to take account of optical dispersion. This means that for each material in the film stack there is only one value of refractive index to find (or, at most, two in the case of a birefringent film), and yet there are hundreds of independent data points in the raw data. This data richness enables direct, deterministic measurements of refractive index to be made, in contrast with spectral techniques, which must rely on models and assumptions to account for the effects of dispersion.
In the simple case shown in Figure 6, the sample is flat and aligned at right angles to the lens axis, leading to the simple and symmetrical fringe pattern shown. However, where the sample is misaligned relative to the lens axis, the fringe pattern shows characteristic distortion, enabling the misalignment to be identified and quantified. It is possible to model this distorted fringe pattern taking full account of the misalignment, in effect allowing the sample’s orientation to be measured along with the coating properties.
| Figure 7: Results obtained from an evaluation on curved samples performed at the UK National Physical Laboratory. |
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Where the surface is not only misaligned but also curved, there are further effects that need to be accounted for and to which, again, BPR is uniquely sensitive. Further details of the analysis involved are given elsewhere3, but Figure 7 gives an indication of the resulting capability of BPR by showing results obtained over a range of samples with different coating thicknesses and curvatures, up to an extreme case of 15-µm films deposited on 50-µm-diam wires. Extremely high (better than 99%) correlation was obtained relative to destructive measurements carried out by the UK’s National Physical Laboratory4.
Medtech manufacturing applications
The ability to measure the combination of coating thickness, refractive index and strain on actual devices in a production environment offers many benefits, particularly in light of US FDA’s Process Analytical Technology (PAT) initiative that seeks to promote greater use of in-line and on-device process quality control5. Efforts to characterise coatings on devices hitherto have focused on measuring thickness, while assuming a refractive index value for the coating material based on off-line measurements of bulk samples. However, the refractive indices of device coatings can vary significantly as a result of deposition conditions or deliberate variation of the coating composition. For example, the refractive index of metal oxide coatings depends strongly on their density; the refractive index of drug-eluting polymer coatings depends on the embedded drug concentration. Without the ability to measure refractive index, variations in these process conditions could go undetected or be wrongly diagnosed as variations in just the thickness of the coating. BPR’s ability to measure both thickness and index in tandem can help to ensure that numerous different types of process excursion can be flagged up when they happen and then be correctly diagnosed.
The semiconductor industry has led the way in adopting in-line process control technologies to maximise yield and productivity in high-volume manufacturing. The medical device industry, on the other hand, has tended to lag behind in this respect. It is believed that adopting semiconductor industry practices and technologies such as BPR could result in significant improvements in device yield and factory productivity. In turn, that would increase profitability for medical device manufacturers.
References
1. Rosencwaig A., et al., “Beam profile reflectometry: A new technique for dielectric film measurements,” Appl. Phys. Lett. 60, 1301-1303 (1992).
2. Fanton J. T., et al., “Multiparameter measurements of thin films using beam-profile reflectometry,” J. Appl. Phys. 73, 7035-7040 (1993).
3. Morris, S.J., “A laser reflectometry technique for on-device coating thickness measurements,” Proc. SPIE, Vol. 7556, 75560M (2010).
4. Brice L., et al., “Measurement of single and multi layer film coatings for medical implants,” National Physical Laboratory report ENG10, October 2008.
Stephen Morris, PhD,
is Managing Director, at Nightingale-EOS Ltd, Unit 2, Bryn Estyn Business Centre, Bryn Estyn Road, Wrexham LL13 9TY, UK
tel. +44 1978 351 711
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