研究目的
To investigate the effects of processing conditions on (Ba1-xCax)(Ti0.9Sn0.1)O3 lead-free ceramics for enhancing structural, humidity sensing, and dielectric properties.
研究成果
The processing conditions for high-quality BCTS ceramics were optimized, with single-phase powder obtained at 1200°C calcination and dense ceramics at 1400°C sintering in platinum crucibles. Compositions with x=0.0-0.04 showed orthorhombic-tetragonal phase transition, while x≥0.06 were purely tetragonal. The highest dielectric permittivity (46,515 at 10 kHz) and piezoelectric coefficient (510 pC/N) were achieved at x=0.02. Humidity sensing was poor due to inadequate pore size and surface properties. Using platinum crucibles prevented contamination compared to alumina.
研究不足
The study found poor humidity sensitivity in all compositions, attributed to large pore sizes (>100 nm) and less prone surface atoms for hydroxyl binding. Sintering at 1400°C did not achieve fully dense microstructures for high Ca content, suggesting higher temperatures may be needed. Contamination from alumina crucibles was an issue, requiring careful crucible selection.
1:Experimental Design and Method Selection:
The study used solid-state reaction technique to prepare BCTS ceramics, with variations in Ca content (x=
2:0 to 1). Methods included XRD for phase analysis, SEM-EDS for microstructure and purity, FE-SEM for morphology, HSM for sintering behavior, DTA for thermal analysis, and electrical measurements for dielectric and piezoelectric properties. Sample Selection and Data Sources:
Samples were prepared from ACS grade reagents (BaCO3, CaCO3, TiO2, SnO2) with purity >99%, mixed in stoichiometric proportions.
3:List of Experimental Equipment and Materials:
Equipment included ball mill, muffle furnace (Nabertherm P330), DTA instrument (DTA 404 PC, Netzsch), XRD (Pan'Analytical), SEM (FEI Inspect, Philips 525), EDS (Quanta 400 FEG, Ametek), FE-SEM, HSM, LCR meter (Hioki 3533-01), piezometer, screen-printing setup, and furnaces. Materials included zirconia balls, ethanol, platinum and alumina crucibles, alumina substrates (ADS-96 R, Coors Tek), platinum conductor paste (ESL 5545, Electro-Science), and organic vehicle (Emflow 227, Emca-Remex).
4:Experimental Procedures and Operational Workflow:
Powders were ball-milled for 24h, dried at 80°C, sieved, calcined at 1050°C or 1200°C for 4h, remilled, dried, sieved, pressed into pellets, sintered at 1300°C or 1400°C for 4h. For humidity sensing, powders were screen-printed onto substrates, dried, and heat-treated. Electrical measurements were conducted after poling.
5:4h. For humidity sensing, powders were screen-printed onto substrates, dried, and heat-treated. Electrical measurements were conducted after poling. Data Analysis Methods:
5. Data Analysis Methods: XRD patterns were indexed using X'Pert Highscore software. EDS and SEM images were analyzed for composition and microstructure. Dielectric and piezoelectric data were analyzed using LCR meter and piezometer.
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muffle furnace
P330
Nabertherm
Used for calcining powders at high temperatures.
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differential thermal analyzer
DTA 404 PC
Netzsch
Used for thermal analysis of mixed powders.
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X-ray diffractometer
Pan'Analytical
Used for studying crystal structure and phase formation.
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scanning electron microscope
FEI Inspect
Philips
Used for investigating morphology of sintered ceramics.
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energy-dispersive spectrometer
Quanta 400 FEG
Ametek Processing & Analytical Instruments
Used for detecting impurities in ceramics.
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LCR meter
3533-01
Hioki
Used for measuring dielectric properties and sensor resistance.
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alumina substrate
ADS-96 R
Coors Tek
Used as a substrate for screen-printing humidity sensors.
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platinum conductor paste
ESL 5545
Electro-Science
Used for creating electrodes on substrates.
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organic vehicle
Emflow 227
Emca-Remex products
Used to confer rheological properties to screen-printing inks.
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humidity and temperature probe
DO9406
Delta Ohm
Used for measuring relative humidity and temperature in sensor testing.
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