Methylaluminoxane (MAO) is a key activator for a large section of the industrial production of polyolefins (POs), which are ubiquitous as commodity polymers. Of an annual world volume of 20 MT linear low density polyethylene (LLDPE), approximately 10% is produced via processes that are based on MAO. Despite many efforts, little is known either about the details of MAOs molecular structure or about the quantitative relationship between the MAO structure and its activating efficiency in the PO production process. In general, MAO is used in huge excess, up to 1000:1, rather like a black-box component. Structural analysis by means of real time neutron scattering techniques to resolve details of the microscopic structure is the key to understand basic principles of MAO-activated catalyst systems. We therefore propose a comprehensive and systematic investigation of industrial relevant state-of-the-art MAO solutions by time-resolved SANS experiments to unravel the formation of the active catalyst/activator complex and intermediate structures formed during the initial period of the PO polymerisation process.