Adhesives of aquatic organisms are of high scientific interest with a view to biomimicry. The visualization of their fine-structure, however, is difficult due to the fragility of the extracellular matrix (ECM). Care must be taken in its preparation for high-resolution SEM. Relating matrix structures to substrate properties demands a high throughput of samples for reliable comparisons. In order to acquaint ourselves with a suitable method we found an easy way to manage the critical steps of preparation for SEM. We show that thin layers of proteinaceous matrix can be satisfactorily prepared by combining freeze-drying and sputtering in a conventional sputter coater after one-step fixation (2.5% glutaraldehyde). The results were superior to CPD.