研究目的
To develop a simple and reliable method for quantifying hexagonal boron nitride (h-BN) impurities in boron nitride nanotubes (BNNTs) using FTIR spectroscopy, enabling better purification and study of BNNTs.
研究成果
The study successfully demonstrates a simple FTIR-based method for quantifying h-BN impurities in BNNTs using an internal standard spiking technique. This enables accurate assessment of BNNT purity, which is crucial for advancing BNNT applications in composites and other technologies. The enrichment methods show promise but require further optimization. Future work should focus on improving synthesis and purification processes to produce high-purity BNNTs at larger scales.
研究不足
The method may not be effective for samples with high oxide content due to overlapping FTIR absorptions. The enrichment methods are not fully optimized and could damage BNNTs over time, especially with alcohols and water present. The technique relies on the availability of high-purity h-BN standards.
1：Experimental Design and Method Selection:
The study uses FTIR spectroscopy to analyze mixed h-BN/BNNT samples, employing an internal standard 'spiking' technique with pure nanoscale h-BN. Two enrichment methods—sonication-assisted isovolumetric filtration (SAIF) and surfactant wrapping with centrifugation—are tested to remove h-BN from BNNTs.
2：Sample Selection and Data Sources:
Samples include as-received BNNTs from commercial sources (BNNT, Llc and BNNano), high-purity nanoscale h-BN (Sigma Aldrich), and various processed samples.
3：List of Experimental Equipment and Materials:
Equipment includes a Thermo Scientific Nicolet iS50 FT-IR spectrometer, TA Instruments Q5000 TGA, Bruker D2 PHASER XRD, tip-probe ultrasonicator, tube furnace, vacuum filtration apparatus, and centrifuges. Materials include BNNTs, h-BN, methanol, dimethylformamide (DMF), acetone, surfactants (Triton X-100, Span 20, Tween 20), and deionized water.
4：Experimental Procedures and Operational Workflow:
Steps involve oxidation of BNNTs at 800°C to remove amorphous impurities, washing with water, dispersion in solvents, sonication, filtration or centrifugation for enrichment, and FTIR analysis. For spiking, known amounts of h-BN are added to BNNT samples, dried, and analyzed.
5：Data Analysis Methods:
FTIR peak ratios (R/TO) are measured and used in linear regression to quantify h-BN content. XRD and TGA are used for complementary analysis.
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FT-IR Spectrometer
Nicolet iS50
Thermo Scientific
Used for Fourier Transform Infrared spectroscopy to analyze BNNT and h-BN samples, measuring peak ratios for quantification.
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XRD
D2 PHASER
Bruker
Used for powder X-ray diffraction to analyze crystal structure of BNNT and h-BN samples.
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TGA
Q5000
TA Instruments
Used for thermogravimetric analysis to observe mass changes during heating of BNNT samples in air.
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Tube Furnace
Lindeberg Blue M
Used for high-temperature oxidation of BNNT samples at 800°C in air.
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Ultrasonicator
Used for tip-probe sonication to disperse BNNT and h-BN samples in solvents.
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Centrifuge
Used for centrifugation in surfactant wrapping method to separate BNNTs and h-BN.
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Vacuum Filtration Apparatus
Used for filtration processes, including SAIF, to separate BNNTs and h-BN.
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h-BN
< 150 nm particle size
Sigma Aldrich
Used as an internal standard for spiking in FTIR quantification.
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BNNTs
BNNT, Llc and BNNano
Primary material studied, as-received and processed for impurity quantification.
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Surfactants
Triton X-100, Span 20, Tween 20
Used in surfactant wrapping method to disperse and separate BNNTs and h-BN.
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Solvents
Methanol, DMF, Acetone
Fisher Scientific
Used for dispersion and washing of BNNT samples.
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