TitleNanoparticle-assisted diffusion brazing of metal microchannel arrays : nanoparticle synthesis, deposition, and characterization
Publication TypeThesis
Year of Publication2012
AuthorsEluri, RT
UniversityOregon State University
CityCorvallis, Or.
Thesis TypeDissertation

Microchannel process technology (MPT) offers several advantages to the field of nanomanufacturing: 1) improved process control over very short time intervals owing to shorter diffusional distances; and 2) reduced reactor size due to high surface area to volume ratios and enhanced heat and mass transfer. The objective of this thesis was to consider how nanomaterials, produced in part using MPT, could be used to solve problems associated with the fabrication of MPT devices. Specifically, many MPT devices are produced using transient liquid-phase brazing involving an electroplated interlayer consisting of a brazing alloy designed for melting temperature suppression. Unfortunately, these alloys can form brittle secondary phases which significantly reduce bond strength. In contrast, prior efforts have shown that it is possible to leverage the size-dependent properties of nanomaterials to suppress brazing temperatures. In this prior work, thin films of off-the-shelf elemental nanoparticles were used as interlayers yielding joints with improved mechanical properties. In the present investigation, efforts have been made to characterize the synthesis and deposition of various elemental nanoparticle suspensions for use in the transient liquid-phase brazing of aluminum and stainless steel. Advances were used to demonstrate the nanoparticle-assisted diffusion brazing of a microchannel array. In the first section, a silver nanoparticle (AgNP) interlayer was produced for the diffusion brazing of heat exchanger aluminum. Efforts are made to examine the effect of braze filler particle size ({\textasciitilde}5 nm and {\textasciitilde}50 nm) and processing parameters (heating rate: 5°C/min and 25°C/min; brazing temperature: 550°C and 570°C) on thin coupons of diffusion-brazed 3003 Al. A tensile strength of 69.7 MPa was achieved for a sample brazed at 570°C for 30 min under 1 MPa with an interlayer thickness of approximately 7 [micrometers]. Further suppression of the brazing temperature to 500°C was achieved by sputtering a 1 [micrometer] thick layer of Cu before depositing a 5 nm thick film of AgNPs resulting in a lap shear strength of 45.3±0.2 MPa. In the middle section of this thesis, several techniques are investigated for the synthesis of sub 10 nm diameter nickel nanoparticles (NiNPs) to be used in the diffusion brazing of 316L stainless steel. The average NiNP size was varied from 9.2 nm to 3.9 nm based on the synthesis technique, solvent and reducing agent used. Conventional wet-chemical synthesis using NiCl2.6H2O in ethylene glycol (solvent) and N2H4.H2O (reducing agent) resulted in the formation of 5.4 ± 0.9 nm NiNPs. Continuous flow synthesis using a microchannel T-mixer (barrel diameter of 521[micrometers]) and a 10 second residence time of reactants in a bath temperature of 130°C resulted in a particle size of with 5.3 ± 1 nm. To make the synthesis safer and less energy intense, microwave heating was used along with less toxic Ni(CH3CO2)2·4H2O (nickel salt), propylene glycol (solvent) and NaPH2O2 (reducing agent) yielding 3.9 ± 0.8 nm diameter NiNPs. For the final section, nickel nanoparticles were synthesized using NiCl2.6H2O (nickel salt), de-ionized water (solvent), NaBH4 (co-reducing agent), N2H4.H2O (reducing agent) and polyvinylpyrolidone (capping agent) yielding 4.2 ± 0.6 nm NiNP. Several deposition techniques were investigated for controlling film thickness and uniformity in the diffusion brazing of 316L stainless steel (SS). Using in-house prepared NiNP and automated dispensing, a hermetic joint up to 70 psi (tested pressure) was obtained in 316L SS substrates under brazing conditions of 800°C, 2 MPa and 30 min. Throughout the course of this thesis, techniques used for characterizing nanoparticles, films and joints included FT-IR, XRD, SEM, TEM, HRTEM, EDS, EPMA, DSC, mass spectrometry, and lap-shear testing.