Effect of Polymer Removal on the Morphology and Phase of the Nanoparticles in All-Inorganic Heterostructures Synthesized via Two-Step Polymer Infiltration

Berman, Diana; Sha, Yuchen; Shevchenko, Elena V.

doi:10.3390/molecules26030679

Cited by 3 publications

(4 citation statements)

References 50 publications

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“…Similarly, in the case of the field-cooled sample, the magnetic moments were aligned at a higher applied field resulting in higher total magnetization at 5 K starting to decrease with heating. These observations are in agreement with previously reported studies on Fe3O4 nanoparticles incorporation in other materials, including ceramic matrices [43].…”

Section: Magnetization Testsupporting

confidence: 94%

Electrospun Fe3O4-PVDF Nanofiber Composite Mats for Cryogenic Magnetic Sensor Applications

2021

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Magnetically responsive, mechanically stable and highly flexible iron (III) oxide-polyvinylidene fluoride (Fe3O4-PVDF) piezoelectric composite fiber mats were fabricated via one step electrospinning method for magnetic sensing at cryogenic temperature. The properties of Fe3O4-PVDF composite fiber mats were characterized using scanning electron microscopy (SEM), differential scanning calorimetry (DSC), X-ray diffraction (XRD), Fourier transform infrared (FT-IR) spectroscopy, d33 and magnetization test. The fiber diameter decreased as the concentration of Fe3O4 increased. The DSC results suggested a decrease in the crystallinity of the composite fiber mats after adding Fe3O4, and the XRD curves identified that the decrease in crystallinity took place in the β crystalline phases of the fibers. FT-IR results further confirmed the reduction of β phases of the composite fiber mats which dropped the piezoelectric response of the fiber mats by 38% for 5% Fe3O4-PVDF than PVDF fiber but still 400% higher than PVDF pellets. The magnetization test advocated a superparamagnetic state of the fiber at room temperature but a ferromagnetic behavior at a lower temperature. The coercivity values of the mats suggested a homogeneous dispersion of the Fe3O4 nanoparticles into the PVDF matrix. Young’s modulus (E) of the fibers remained the same before and after the magnetization test, indicating the mechanical stability of the fiber in the range of 5 K to 300 K. Its mechanical stability, superparamagnetic behavior at room temperature and ferromagnetic at low temperature could open up its application in spintronic devices at cryogenic temperature and cryogenic power electronic devices.

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Section: Magnetization Testsupporting

confidence: 94%

Electrospun Fe3O4-PVDF Nanofiber Composite Mats for Cryogenic Magnetic Sensor Applications

2021

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“…Figure a depicts the major steps involved in porous ZnO coatings via SIS using swollen BCP templates such as (i) deposition of the BCP layer via spin-coating, (ii) swelling of the deposited BCP in ethanol for 1 h at 75 °C, (iii) infiltration of swollen BCP with ZnO precursors by cycling the exposure of template to DEZ and H 2 O, and (iv) formation of all-inorganic porous ZnO by polymer removal. The polymer can be removed by thermal annealing or ozone cleaning . In this study, we implemented ozone cleaning since prepared QCM samples cannot be heated up to 450 °C required for the complete removal of organics.…”

Section: Results and Discussionmentioning

confidence: 99%

“…The polymer can be removed by thermal annealing or ozone cleaning. 33 In this study, we implemented ozone cleaning since prepared QCM samples cannot be heated up to 450 °C required for the complete removal of organics. QCM analysis (Figure 1b) of BCP templates of varied thicknesses spin-coated on the QCM substrates was used to monitor the mass changes introduced during different steps of the synthesis of porous ZnO conformal coatings.…”

Section: Methodsmentioning

confidence: 99%

Swelling-Assisted Sequential Infiltration Synthesis of Nanoporous ZnO Films with Highly Accessible Pores and Their Sensing Potential for Ethanol

Pleshek

Tran

et al. 2021

ACS Appl. Mater. Interfaces

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Here, we report a swelling-assisted sequential infiltration synthesis (SIS) approach for the design of highly porous zinc oxide (ZnO) films by infiltration of block copolymer templates such as polystyrene-block-polyvinyl pyridine with inorganic precursors followed by UV ozone-assisted removal of the polymer template. We show that porous ZnO coatings with the thickness in the range between 140 and 420 nm can be obtained using only five cycles of SIS. The pores in ZnO fabricated via swelling-assisted SIS are highly accessible, and up to 98% of pores are available for solvent penetration. The XPS data indicate that the surface of nanoporous ZnO films is terminated with −OH groups. Density functional theory calculations show a lower energy barrier for ethanol-induced release of the oxygen restricted depletion layer in the case of the presence of −OH groups at the ZnO surface, and hence, it can lead to higher sensitivity in sensing of ethanol. We monitored the response of ZnO porous coatings with different thicknesses and porosities to ethanol vapors using combined mass-based and chemiresistive approaches at room temperature and 90 °C. The porous ZnO conformal coatings reveal a promising sensitivity toward detection of ethanol at low temperatures. Our results suggest the excellent potential of the SIS approach for the design of conformal ZnO coatings with controlled porosity, thickness, and composition that can be adapted for sensing applications.

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“…The infiltration of polymer templates with alumina precursors was performed using a SIS method that has been described earlier. ,− A GEMStar thermal atomic layer deposition (ALD) system was used for the process for convenience, though we note that our process is not an ALD process (deposition rates are much higher and the deposition is not atomic layer-by-layer) and could be carried out in other appropriately configured chemical vapor deposition systems as well. TMA and H 2 O were used as gas-phase precursors.…”

Section: Methodsmentioning

confidence: 99%

Porous but Mechanically Robust All-Inorganic Antireflective Coatings Synthesized using Polymers of Intrinsic Microporosity

Zhang

Omotosho

et al. 2022

ACS Nano

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Here, we introduce polymer of intrinsic microporosity 1 (PIM-1) to design single-layer and multilayered all-inorganic antireflective coatings (ARCs) with excellent mechanical properties. Using PIM-1 as a template in sequential infiltration synthesis (SIS), we can fabricate highly uniform, mechanically stable conformal coatings of AlO x with porosities of ∼50% and a refractive index of 1.41 compared to 1.76 for nonporous AlO x that is perfectly suited for substrates commonly used in high-end optical systems or touch screens (e.g., sapphire, conductive glass, bendable glass, etc.). We show that such films can be used as a single-layer ARC capable of reduction of the Fresnel reflections of sapphire to as low as 0.1% at 500 nm being deposited only on one side of the substrate. We also demonstrate that deposition of the second layer with higher porosity using block copolymers enables the design of graded-index double-layered coatings. AlO x structures with just two layers and a total thickness of less than 200 nm are capable of reduction of Fresnel reflections under normal illumination to below 0.5% in a broad spectral range with 0.1% reflection at 700 nm. Additionally, and most importantly, we show that highly porous single-layer and graded-index double-layered ARCs are characterized by high hardness and scratch resistivity. The hardness and the maximum reached load were 7.5 GPa and 13 mN with a scratch depth of about 130 nm, respectively, that is very promising for the structures consisting of two porous AlO x layers with 50% and 85% porosities, correspondingly. Such mechanical properties of coatings can also allow their application as protective layers for other optical coatings.

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Effect of Polymer Removal on the Morphology and Phase of the Nanoparticles in All-Inorganic Heterostructures Synthesized via Two-Step Polymer Infiltration

Cited by 3 publications

References 50 publications

Electrospun Fe3O4-PVDF Nanofiber Composite Mats for Cryogenic Magnetic Sensor Applications

Electrospun Fe3O4-PVDF Nanofiber Composite Mats for Cryogenic Magnetic Sensor Applications

Swelling-Assisted Sequential Infiltration Synthesis of Nanoporous ZnO Films with Highly Accessible Pores and Their Sensing Potential for Ethanol

Porous but Mechanically Robust All-Inorganic Antireflective Coatings Synthesized using Polymers of Intrinsic Microporosity

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