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All sources NASA NTRS DOE OSTI

DOE OSTI2020

Materials Data on HfCl4 by Materials Project

HfCl4 crystallizes in the monoclinic P2/c space group. The structure is one-dimensional and consists of one HfCl4 ribbon oriented in the (1, 0, 0) direction. Hf4+ is bonded to six Cl1- atoms to form edge-sharing HfCl6 octahedra. There are a spread of Hf–Cl bond distances ranging from 2.32–2.66 Å. There are two inequivalent Cl1- sites. In the first Cl1- site, Cl1- is bonded in a water-like geometry to two equivalent Hf4+ atoms. In the second Cl1- site, Cl1- is bonded in a single-bond geometry to one Hf4+ atom.

36 MATERIALS SCIENCE↗

DOE OSTI2020

Synthesis and Flash Sintering of (Hf1-xZrx)B2 Solid Solution Fine Powders

Fine powders of (Hf1-xZrx)B2 solid solution were synthesized by two methods. In the first one, solution-based processing of HfCl4, ZrCl4, sucrose and H3BO3 was carried out followed by heat treatment (e.g., at 1500 °C for 1 h) in Argon to achieve the carbothermal reduction (CTR) reaction to form the boride solid solution. In the second one, called boron hydride reduction (BHR) method, HfCl4, ZrCl4 and NaBH4 were directly mixed in a glove box followed by heat treatment in Argon at elevated temperatures from 700 to 1500 °C. In addition, the powders synthesized via both methods were flash sintered without sample preheating in a homemade setup. The synthesized powders as well as the flash sintered bulk ceramics were characterized using different techniques including XRD, SEM, EDS, TEM, TGA-DSC, and Vickers hardness test to reveal the inter-relationships between starting materials composition, processing conditions, and the resulting materials microstructure and physical/chemical properties.

Belisario, Jose↗

NASA NTRS1976

Development and study of chemical vapor deposited tantalum base alloys

A technique for the chemical vapor deposition of alloys was developed. The process, termed pulsing, involves the periodic injection of reactant gases into a previously-evacuated reaction chamber where they blanket the substrate almost instantaneously. Formation of alternating layers of the alloy components and subsequent homogenization allows the formation of an alloy of uniform composition with the composition being determined by the duration and relative numbers of the various cycles. The technique has been utilized to produce dense alloys of uniform thickness and composition (Ta- 10 wt % W) by depositing alternating layers of Ta and W by the hydrogen reduction of TaCl5 and WCl6. A similar attempt to deposit a Ta - 8 wt % W - 2 wt% Hf alloy was unsuccessful because of the difficulty in reducing HfCl4 at temperatures below those at which gas phase nucleation of Ta and W occurred.

Meier, G. H.↗

NASA NTRS1975

Preparation of tantalum-based alloys by a unique CVD process

The paper describes a sequential pulsing technique for deposition of refractory alloys and evaluates the technique for the deposition of the tantalum-base alloys Ta-10W (Ta-10 st% W) and T-111 (Ta-8 wt% W-2 wt% Hf). The deposition cycle for Ta-10W was chosen as alternate injections of TaCl5 plus hydrogen and WCl6 plus hydrogen. The cycle for T-111 was chosen as injections of TaCl5 plus hydrogen interspersed with injections of WCl6 plus hydrogen. A temperature range of 900-1300 C was chosen for both alloys. The ability of the pulse process to blanket a uniformly heated section of substrate with a mixture of gases, whose composition varies not with position on the substrate but instead with time of residence in the reactor, allows metal of uniform thickness to be deposited. It is shown that Ta and W can be deposited at high temperature with the formation of a dense columnar grain structure, so that the feasibility of preparing uniformly thick deposits of these elements by a 'pulsing' modification of CVD is demonstrated. A similar attempt to deposit T-111 was unsuccessful due to the difficulty in reducing HfCl4.

Bryant, W. A.↗