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Abstract Ceramics such as lead zirconate titanate (PZT) tend to dissolve incongruently, and thus pose a challenge in the cold sintering process. Moist lead nitrate has previously been shown to enable a cold sinter‐assisted densification of PZT by a viscous phase sintering mechanism. In this paper, lead acetate trihydrate is demonstrated to lower the required temperature of the cold sintering step to 200°C. This densification process was described as a two‐step process: cold sintering of PZT with lead acetate trihydrate and post‐annealing the as‐cold sintered PZT ceramics. Unlike in the case of lead nitrate, PZT densification with lead acetate trihydrate occurs by a liquid phase assisted sintering mechanism, leading to an as‐cold sintered relative density of 84% at 200°C. After performing a post‐anneal step at 900°C, >97% relative densities were achieved in samples that were cold sintered with lead acetate trihydrate. This step not only densified PZT but also refined the grain boundaries. In the post‐annealed samples, the room‐temperature relative permittivity at 100 Hz was ~1600, slightly higher than that reported in samples that used lead nitrate as a sintering aid; the loss tangent was about 3.8%. For measurements at 10 Hz, the remanent polarization in both cases was ~28 µC/cm2. Both Rayleigh analysis and aging studies showed that a higher irreversible contribution to the permittivity exists in samples that used lead nitrate as a cold sintering aid.
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Densification and Strengthening of Ferrous‐Based Powder Compacts Through Cold Sintering Aided Warm Compaction
Cold sintering of surface‐modified iron compacts results in a co‐continuous phosphate interphase between iron particles that provide both enhanced green strength and green density similar to the process that has been successfully introduced in low‐temperature densification of ceramic materials. Relative density as high as 95% along with transverse rupture strength of ≈ 75 MPa, which is almost six times that of conventional powdered metal iron compact and 2.5 times that of warm compacted controls, is achieved. Dilatometry study at different pressures shows a small but significant improvement in densification process during cold sintering relative to the larger densification of warm compacted control. Strength model based on microstructural analysis as well as in situ diffused reflectance infrared Fourier transform spectroscopy (DRIFTS) experiments reveals the nature of the interphase that imparts the large cohesive strength under the cold sintered assisted warm compaction. The process is conducive to produce iron compacts for green machining. Furthermore, the samples when subjected to high‐temperature sintering yield a fully sintered iron compact with density > 7.2 g cm−3and transverse rupture strength as high as 780 MPa. All in all, there are major new opportunities with the cold sintered assisted warm compaction of powdered metals that will also be discussed.
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- Award ID(s):
- 2134643
- PAR ID:
- 10502862
- Publisher / Repository:
- Wiley
- Date Published:
- Journal Name:
- Advanced Engineering Materials
- Volume:
- 24
- Issue:
- 12
- ISSN:
- 1438-1656
- Page Range / eLocation ID:
- 2200714
- Format(s):
- Medium: X
- Sponsoring Org:
- National Science Foundation
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Accepted Manuscript1.0
- Journal Article:
- https://doi.org/10.1002/adem.202200714
