A furnace with rotating load frame for in situ high temperature deformation and creep experiments in a neutron diffraction beam line

Abstract

A resistive furnace combined with a load frame was built that allows for in situ neutron diffraction studies of high temperature deformation, in particular, creep. A maximum force of 2700 N can be applied at temperatures up to 1000 °C. A load control mode permits studies of, e.g., creep or phase transformations under applied uni-axial stress. In position control, a range of high temperature deformation experiments can be achieved. The examined specimen can be rotated up to 80° around the vertical compression axis allowing texture measurements in the neutron time-of-flight diffractometer HIPPO (High Pressure - Preferred Orientation). We present results from the successful commissioning, deforming a Zr-2.5 wt.% Nb cylinder at 975 °C. The device is now available for the user program of the HIPPO diffractometer at the LANSCE (Los Alamos Neutron Science Center) user facility.

High-temperature neutron diffraction and first-principles study of temperature-dependent crystal structures and atomic vibrations in Ti3AlC2, Ti2AlC, and Ti5Al2C3

“…The HTND experiments were conducted on the HighPressure Preferred Orientation (HIPPO) neutron diffractometer [31][32][33] at the Lujan Neutron Scattering Center, Los Alamos National Laboratory. For both the multiphase Ti-Al-C sample and Ti 3 AlC 2 , bulk samples were placed in a vanadium, V, holder (9 mm diameter, 0.15 mm wall thickness), mounted in an ILL-type high-temperature vacuum furnace with a V setup, and heated at a rate of 20…”

Distinct Recrystallization Pathways in a Cold-Rolled Al-2%Mg Alloy Evidenced by In-Situ Neutron Diffraction

“…The present study was focused on the neutron diffraction measurements of an Al alloy containing 2% Mg, in order to determine the kinetics of recrystallization by ex situ and in-situ annealing. The experiments were conducted on two time-of-flight (TOF) neutron diffraction instruments: the engineering diffractometer (VULCAN) at Oak Ridge National Laboratory (ORNL, Oak Ridge, TN, USA) [39], and at the high-pressure-preferential orientation (HIPPO) at Los Alamos National Laboratory (LANL, Los Alamos, NM, USA) [40][41][42]. The detailed analysis included the texture characterizations of DF and RCX along with developing a new method for texture decomposition.…”

“…Given the fact that optical microscopy showed a fully recrystallized structure after annealing for 20 min at 360 • C, the in-situ isothermal annealing treatments were performed in the temperature range from 250 to 360 • C, and the annealing times from 20 to 210 min. The in-situ isochronal annealing was performed at two TOF neutron diffractometers, HIPPO and VULCAN, for two heating rates with nominal values of 2 • C/min and 7 • C/min, and in the temperature span from room temperature to 400 • C. HIPPO is a TOF instrument dedicated for texture measurements [40][41][42][43][44][45][46], while at VULCAN engineering diffractometer, the texture characterizations and the corresponding data analysis were developed as a complementary capability [47,48].…”

An experimental system for high temperature X-ray diffraction studies with in situ mechanical loading

“…When these studies are conducted with thermal and/or mechanical loads applied in situ, processing and operating conditions can be mimicked and the material response can be probed in real time. [1][2][3][4][5] These experiments paint a clearer picture of the microscale material response than more traditional diffractionbased residual stress studies which provide aggregate averaged lattice strain information, often near the surface of the sample. 6 Lattice strain data measured in these experiments can be used to both validate and calibrate predictive, high fidelity material models.…”