A new device for high-temperature in situ GISAXS measurements.

A heating stage originally designed for diffraction experiments is implemented into a Bruker NANOSTAR instrument for in situ grazing incidence small-angle x-ray scattering experiments. A controlled atmosphere is provided by a dome separating the sample environment from the evacuated scattering instrument. This dome is double shelled in order to enable cooling water to flow through it. A mesoporous silica film templated by a self-assembled block copolymer system is investigated in situ during step-wise heating in air. The GISAXS pattern shows the structural development of the ordered lattice of parallel cylindrical pores. The deformation of the elliptical pore-cross section perpendicular to the film surface was studied with increasing temperature. Moreover, the performance of the setup was tested by controlled in situ heating of a copper surface under controlled oxygen containing atmosphere.