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Wide-angle X-ray diffraction patterns of single spider-silk fibres of ≤ 5 μm diameter can be obtained at a third-generation synchrotron-radiation source in a few seconds per pattern. This is sufficient to observe the strongest equatorial and first layer line reflections. For higher-resolution structural work, data have to be recorded with cryocooling techniques in order to maintain the crystallinity of the sample for several minutes.
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