From Lab to Industrial: PZT nanoparticles synthesis and process control for application in additive manufacturing
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Lead Zirconate Titanate (PZT) nanoparticles hold many promising current and future applications, such as PZT ink for 3-D printing or seeds for PZT thick films. One common method is hydrothermal growth, in which temperature, duration time, or mineralizer concentrations are optimized to produce PZT nanoparticles with desired morphology, controlled size and size distribution. A modified hydrothermal process is used to fabricate PZT nanoparticles. The novelty is to employ a high ramping rate (e.g., 20˚C/min) to generate abrupt supersaturation so as to promote burst nucleation of PZT nanoparticles as well as a fast cooling rate (e.g., 5˚C/min) with a controlled termination of crystal growth. As a result, PZT nanoparticles with a size distribution ranging from 200 nm to 800 nm are obtained with cubic morphology and good crystallinity. The identification of nanoparticles is confirmed through use of X-ray diffractometer (XRD). XRD patterns are used to compare sample variations in their microstructures such as lattice parameter. A cubic morphology and particle size are also examined via SEM images. The hydrothermal process is further modified with excess lead (from 20% wt. to 80% wt.) to significantly reduce amorphous phase and agglomeration of the PZT nanoparticles. With a modified process, the particle size still remains within the 200 nm to 800 nm. Also, the crystal structures (microstructure) of the samples show little variations. Finally, a semi-continuous hydrothermal manufacturing process was developed to substantially reduce the fabrication time and maintained the same high quality as the nanoparticles prepared in an earlier stage. In this semi-continuous process, a furnace is maintained at the process temperature (200˚C), whereas autoclaves containing PZT sol are placed in and out of the furnace to control the ramp-up and cooling rates. This setup eliminates an extremely time-consuming step of cooling down the furnace, thus saving tremendous amount of process time making fabrication of a large amount of PZT nanoparticles possible.
- Mechanical engineering