We present in-situ stress measurement results for single and multilayer thin-films deposited by magnetron sputtering. In particular, we report on the influence of the material interfaces on the ensuing stress in both the transient and steady-state regimes of film growth. This behavior is used to determine the appropriate thicknesses of the constituent layers that will result in a net tensile stress in multilayers composed of various material combinations. These multilayers can then be used to compensate the compressive integrated stress in single and multilayer EUV and x-ray optical coatings. The use of multilayers to compensate the integrated stress might be advantageous because, unlike single layers of chromium, the roughness is not expected to increase with the total thickness of the multilayer. In this paper, we demonstrate the technique for W/Si and Mo/Si multilayers and discuss its application to other material combinations.
In this work, we describe the development of multilayer coating capabilities of the X-ray astronomy group at NASA Marshall Space Flight Center (MSFC). A DC magnetron sputtering system has been constructed to deposit periodic, depth-graded and aperiodic multilayer coatings on flat silicon and glass substrates of various diameters. The main goal of this new area of research at MSFC is the development of coatings for use on future hard X-ray astronomical telescopes, extending the reflected energy range into the hard X-ray to soft gamma ray band. Descriptions of the system geometry and calibration process as well as initial results from the first few months of deposition and coating recipe optimization are presented.
We have developed an X-ray reflectometer (XRR) system for the characterization of various soft and hard X-ray optic coatings being developed at Marshall Space Flight Center. The XRR system generates X-ray radiation with a highoutput Rigaku rotating anode source (RAS), operational at a voltage range of 5 – 35 kV, a current range of 10-150 mA. A series of precision slits, adjustable down to approximately 25 micrometers, positioned in the beam path limit the extent of the x-ray beam and control the resolution of the XRR measurement while a goniometer consisting of two precision rotary stages controls the angular position of the coating sample and X-ray detector with respect to the beam. With the high count rate capability of the RAS, a very-high-speed silicon drift detector, the Amptek Fast Silicon Drift Detector (SDD), is implemented to achieve good count rate efficiency and improve reflectivity measurements of coatings at larger graze angles. The coating sample can be adjusted using a series of linear and tipping stages to perfectly align the center of the sample with the center of the incident X-ray beam. These stages in conjunction with the goniometer components are integrated through original control software resulting in full automation of the XRR system. We will show some initial XRR measurements of both single and multilayer coatings made with this system. These results and future measurements are used to characterize potential X-ray optic coatings culminating in the production of highly reflective coatings operational at a large range of X-ray energies.
We examine a method for achieving zero intrinsic stress in thin films of iridium, chromium, and nickel deposited by magnetron sputter deposition. The examination of the stress in these materials is motivated by efforts to advance the optical performance of light-weight x-ray space telescopes into the regime of sub-arc second resolution. A characteristic feature of the intrinsic stress behavior in chromium and nickel is their sensitivity to the magnitude and sign of the intrinsic stress with argon gas pressure, including the existence of a critical pressure that results in zero film stress. This critical pressure scales linearly with the film’s density. While the effect of stress reversal with argon pressure has been previously reported by Hoffman and others for nickel and chromium, we have discovered a similar behavior for the intrinsic stress in iridium films. Additionally, we have identified zero stress in iridium shortly after island coalescence in the high adatom mobility growth regime. This feature of film growth is used for achieving a total internal stress of -2.89 MPa for a 15.8 nm thick iridium film with a surface roughness of 5.0 ± 0.5Å based on x-ray reflectivity (XRR) measurement at CuKα. The surface topography was also examined using atomic force microscopy (AFM). The examination of the stress in these films has been performed with a novel in-situ measurement device. The methodology and sensitivity of the in-situ instrument is also described herein.