研究目的
To develop a high-efficiency synthesis method for high-performance K0.5Na0.5NbO3 ceramics using mechanochemical activation-assisted process, reducing synthesis time and improving electrical properties compared to conventional methods.
研究成果
The mechanochemical activation-assisted method successfully synthesized high-performance KNN ceramics with significantly reduced synthesis time (100 min vs. 6-24 h) and improved electrical properties, including high energy storage density (Wtol=1.612 J/cm3, Wrec=0.431 J/cm3) and dielectric breakdown strength (110 kV/cm). The method offers advantages in efficiency and property enhancement, making it promising for KNN-based ceramic preparation.
研究不足
The study is limited to KNN ceramics and may not generalize to other materials. High-energy ball milling can lead to particle agglomeration and impurity phases with prolonged milling times, affecting density and properties. The method requires optimization of milling parameters to avoid excessive heating and ensure reproducibility. External factors like sample thickness and electrode configuration could influence dielectric breakdown strength measurements.
1:Experimental Design and Method Selection:
The study employed a mechanochemical activation-assisted route to synthesize KNN ceramics, involving high-energy ball milling to reduce particle size and enhance reaction kinetics, followed by calcination and sintering. This method was chosen to overcome limitations of conventional solid-state reactions, such as long milling times and high volatility of alkali elements.
2:Sample Selection and Data Sources:
Raw materials included K2CO3, Na2CO3, and Nb2O5 powders (purity 99.99%) from Sinopharm Chemical Reagent Co., Ltd. Samples were prepared with varying milling times (20-360 min) and compared to a control sample (CKNN) made by conventional method with 24 h milling.
3:99%) from Sinopharm Chemical Reagent Co., Ltd. Samples were prepared with varying milling times (20-360 min) and compared to a control sample (CKNN) made by conventional method with 24 h milling. List of Experimental Equipment and Materials:
3. List of Experimental Equipment and Materials: Equipment included a Fritsch Vario-Planetary Mill (pulverisette P7?) for ball milling, zirconia vial/ball set, freeze dryer for drying, calcination furnace, cold isostatic press, sintering furnace in sealed alumina crucible, laser particle size analyzer (Model BI-90Plus, Brookhaven), Field Transmission Electron Microscopy (FTEM; Tecnai G2 F20, FEI), X-ray diffractometer (XRD, Philips), Raman spectrophotometer (in Via Reflex, Renishaw), Field Scanning Electron Microscopy (FE-SEM; SU-8020, Hitachi), LCR meter (TH2818; Tonghui), and ferroelectric analyzer (TF-2000; Aix ACCT). Materials were the chemical reagents mentioned.
4:Experimental Procedures and Operational Workflow:
Powders were weighed stoichiometrically, blended in hyperpure water, and subjected to high-energy ball milling with specific parameters (speed 300/600 rpm, ball-to-powder ratio 8:1, reverse directions every 2 min with 8 min rest). The slurry was freeze-dried, calcined at 700°C or 850°C for 9 h, ball-milled again, dried, pressed into pellets at 200 MPa, and sintered at 1120-1140°C for 2 h. Characterization involved particle size analysis, TEM, XRD, Raman spectroscopy, SEM, dielectric measurements, and ferroelectric property measurements.
5:Data Analysis Methods:
Data were analyzed using software for particle size distribution (nano measurer), XRD peak fitting, Raman spectrum fitting, and calculations for energy storage density (Wtol, Wrec, Wloss) from P-E hysteresis loops using integrals.
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Field Transmission Electron Microscopy
Tecnai G2 F20
FEI
Exhibited morphologies of the particles.
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Field Scanning Electron Microscopy
SU-8020
Hitachi
Observed surface and section morphologies of the samples.
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Planetary Mill
pulverisette P7
Fritsch
Used for high-energy ball milling to reduce particle size and activate mechanochemical reactions.
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Laser Particle Size Analyzer
BI-90Plus
Brookhaven
Analyzed particle size distribution of the powders.
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X-ray Diffractometer
Philips
Investigated phase structure of powders using Cu-Kα radiation.
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Raman Spectrophotometer
in Via Reflex
Renishaw
Performed Raman spectroscopy in the range 0-1000 nm.
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LCR Meter
TH2818
Tonghui
Carried out dielectric measurements at 1 kHz-200 kHz.
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Ferroelectric Analyzer
TF-2000
Aix ACCT
Measured ferroelectric properties, including P-E hysteresis loops.
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