Feasibility studies for high pressure neutron powder diffraction experiments

We recently performed two neutron powder diffraction experiments on very small samples on the High Intensity Powder Diffractometer (HIPD), to determine the feasibility of performing in situ high pressure/high temperature neutron diffraction experiments on HIPD at pressures which would exceed the previous limit of ∼50kbar achievable in a neutron diffraction experiment. The sample, which had been prepared at 65kbar and 1000degC, consisted of a small platinum capsule filled with CaGeO3 perovskite. A diffraction experiment taking ∼8.6hrs at a LANSCE proton beam current of ∼53μA gave peaks of good intensity from both Pt and CaGeO3; we could begin to see them after only 20min if beam time. The second experiment was to test the possibility of diffraction from a high pressure apparatus. We placed in the HIPD sample position the central assembly from a 100kbar octahedral press. Four tungsten carbide anvils and a copper block previously pressed to 65kbar were held in an aluminum frame. The sample consisted of a small bit of nickel foil placed in a 3 mm hole in the copper block. The active sample volume is defined by the gap (∼0.7mm) between the anvils and the length of the sample. A small portion of the copper block is also seen in this arrangement. This is viewed at 90deg 2Θ through a similar gap between the anvils by 4 1/2''x12'' 3He counter tubes. This arrangement simulates the operating conditions of a high pressure run at 100kbar and takes advantage of the fixed instrument geometry possible in time-of-flight neutron diffraction experiments. We obtained a diffraction pattern in ∼7.1hrs and ∼57μA beam current which clearly showed peaks from both copper and nickel with no evidence of diffraction from the anvils or any other part of the assembly. These two experiments clearly demonstrate the feasibility of performing high pressure in situ diffraction experiments in excess of 100kbar on HIPD at LANSCE. (J.P.N.)