Hydrothermal Green Synthesis Research Articles

Green Synthesis of Luminescent Carbon Dots from Ficus benghalensis Aerial Roots for Bioimaging.

In this work, carbon quantum dots (CQDs) were prepared using a one-step hydrothermal green synthesis method from a low-cost and eco-friendly renewable biomass, specifically the Ficus benghalensis aerial roots (FB-AR). For the past two decades, CQDs have been noted for their tunable emission spectrum, quantum yield, biocompatibility, photostability, and unique optoelectronic properties such as photoluminescence (PL), and fluorescence. The synthesized Ficus benghalensis carbon quantum dots (FB-CQDs) were characterized for their physical, structural, and chemical properties using XRD, Raman, HRTEM, XPS, FTIR, TG-DTG, UV-visible, and photoluminance analysis. XPS analysis confirmed the presence of phytoconstituent functionalities and the composition of components. The FB-CQDs, which exhibit long-range emissions, have potential applications in various biological and therapeutic fields. Their bioimaging capability is tested in Escherichia coli bacteria. However, despite their promising characteristics, the FB-CQDs showed no antibacterial inhibition against Escherichia coli and Staphylococcus aureus, likely due to its carbonization temperature.

Hydrothermal Green Synthesis of LaOx‐Modified Pt/C Catalyst for Glycerol‐to‐Glycerate Electrooxidation in Alkaline Medium

AbstractUsing the bromide anion exchange (BAE) green method to obtain carbon‐supported nanoparticles, Pt(LaOx)/C was successfully prepared under mild conditions. This material, containing LaOx species generated in situ during the synthesis, was efficiently used as an anode to perform glycerol oxidation in alkaline medium in batch mode and at room temperature. In a direct alcohol fuel cell (DAFC), this catalyst was able to boost the glycerol‐to‐glycerate conversion with a 49% selectivity and a 28% power density higher than the same system using a BAE‐synthesized Pt/C anode. The increase in catalytic activity may be due to the interaction of LaOx with the Pt active sites, acting as a bifunctional electrode. Furthermore, when used as an anode in an electrolysis setup, the selectivity of glycerol toward glycerate increased up to 67%. In situ FTIR and HPLC analyses confirmed the formation of the value‐added glycerol oxidation products.

Green Synthesis of Various Heteroatom‐doped Carbon Quantum Dots from Urine, Whey, and Their Mixture: The Optimization of Synthesis and Potential Applications

AbstractThe employment of biomass waste for the fabrication of carbon quantum dots (CQDs), as a novel fluorescent material with high photoluminescence (PL) activity, has gained intense interest for the last decade. However, the fabrication of CQD from biomass waste encounters challenges including low fluorescence yield, reproducibility, and stability. Therefore, the novel, simple, flexible fabrication routes for CQDs using biomass waste as a precursor are still essential for practical applications. In this study, we reported the employment of human urine (U), sour whey (W), and their mixture (U/W) as precursors for the hydrothermal green synthesis approach. For all cases, CQDs with an excitation‐dependent emission nature were obtained with a quantum yield (QY) value of 48 %, 28 %, and 39 % for U, W, and U/W, respectively. For each case, doping of various heteroatoms such as N, P, S, etc., in the structure of CQDs contributed PL characteristics with high QY, reasonably low cytotoxicity, and, robust pH and storage stability which indicate their high potential in various biomedical applications such as bioimaging and pH sensors. This study proves the utilization of human urine and whey as the precursors for the fabrication of CQDs through a low‐cost, flexible, and eco‐friendly green synthesis procedure.

Hydrothermal Green Synthesis of Aloe Vera Gel-Biotemplated Iron Oxide Nanoparticles for Robust Photocatalytic Degradation of Methylene Blue, Chromium (VI) Reduction, and Antibacterial Efficacy

Hydrothermal Green Synthesis of Aloe Vera Gel-Biotemplated Iron Oxide Nanoparticles for Robust Photocatalytic Degradation of Methylene Blue, Chromium (VI) Reduction, and Antibacterial Efficacy

Rapid hydrothermal green synthesis of core-shell-shaped NiCo2O4@MoS2/RGO ternary composites for high-performance electrode materials

RGO-based composites possess great potential as materials for supercapacitors owing to their remarkable properties such as high specific surface area and electrical conductivity. Herein, this work presents an investigation on ternary composite electrode materials composed of RGO, NiCo2O4, and MoS2. The chemical insertion method was employed to overcome the issue of RGO layer repacking. By means of a rapid green hydrothermal synthesis approach, conductive MoS2/RGO substrates were successfully fabricated, and subsequently, NiCo2O4@MoS2/RGO core–shell-shaped composites were prepared using the MoS2/RGO substrates. The ternary NiCo2O4@MoS2/RGO composites were composed of uniformly distributed conductive MoS2/RGO substrates embedded with NiCo2O4 core microspheres. Remarkably, the NiCo2O4@MoS2/RGO composites, used as electrode materials in supercapacitors, exhibited an exceptional specific capacitance of 946 F g-1 at 1 A g-1, improved rate capacity, and demonstrated outstanding electrochemical stability while maintaining 87.3 % retention after 5000 consecutive charge–discharge cycles. The exceptional integrated performance of these composites renders them promising electrode materials for electrochemical supercapacitors.

Enhancement of photocatalytic activity of ZnO by ZnMoO4 compositing under visible light via hydrothermal green synthesis

ZnO has excellent photocatalytic activity under UV light, but its photocatalytic activity under visible light is relatively low due to its wide band gap. Modification of ZnO to a composite with ZnMoO4, which has a band gap energy of 2.61 eV, triggers heterojunction photocatalytic reactions under visible light. Here in this research, ZnO-ZnMoO4 nanocomposites have been successfully synthesized using the green synthesis hydrothermal method with Mentha x piperita leaf extract containing alkaloids as a source of weak bases and other secondary metabolites as capping agents. The development of green synthesis methods in this study aims to reduce the use of hazardous and toxic materials. The synthesized photocatalysts have been fully characterized and evidence of increased photocatalytic activity of ZnO/ZnMoO4 composites is based on the degradation of Rhodamine B (RhB) dye in visible light. The results showed that the degradation of RhB by ZnO/ZnMoO4 nanocomposites could reach 83.7%, and this was better than using ZnO which only reached 13.9%.

Colorimetric Freshness Indicator Based on Cellulose Nanocrystal–Silver Nanoparticle Composite for Intelligent Food Packaging

In this study, a colorimetric freshness indicator based on cellulose nanocrystal-silver nanoparticles (CNC-AgNPs) was successfully fabricated to offer a convenient approach for monitoring the quality of packaged food. AgNPs were directly synthesized and embedded in CNC via a one-pot hydrothermal green synthesis, and CNC-AgNP composited indicator films were prepared using a simple casting method. The AgNPs obtained were confirmed by UV-Vis diffuse reflectance spectroscopy and X-ray diffraction. The ability of the as-prepared CNC-AgNP film to indicate food quality was assessed in terms of the intensity of its color change when in contact with spoilage gases from chicken breast. The CNC-AgNP films initially exhibited a yellowish to dark wine-red color depending on the amount of AgNPs involved. They gradually turned colorless and subsequently to metallic grey. This transition is attributed to the reaction of AgNPs and hydrogen sulfide (H2S), which alters the surface plasmon resonance of AgNPs. Consequently, the color change was suitably discernible to the human eye, implying that the CNC-AgNP composite is a highly effective colorimetric freshness indicator. It can potentially serve as an accurate and irreversible food quality indicator in intelligent packaging during distribution or storage of products that emit hydrogen sulfide when deteriorating, such as poultry products or broccoli.

Graphene Quantum Dots – Hydrothermal Green Synthesis, Material Characterization and Prospects for Cervical Cancer Diagnosis Applications: A Review

AbstractGraphene Quantum Dots (GQDs) have attracted significant attention and applications in the field of biosensors, particularly for early detection of cervical cancer, due to their excellent electrochemical, optical, and biocompatibility properties. In this review, recent results on green methods for the synthesis of GQDs as well as their characterization techniques are discussed, with particular emphasis on structural, morphological, elemental, optical, and functional group analysis. In addition, a comprehensive overview of how the electrochemical and biocompatibility properties of GQDs enable their use in the development of sensing elements for biosensing applications is presented. This paper also highlights the most recent developments in the fabrication of GQDs‐based biosensors for cervical cancer detection. Finally, the future prospects are critically discussed to assist researchers in identifying the shortcomings of the existing biosensors and establishing new methods centered on the development of unique, efficient, sensitive and selective GQDs‐based biosensors.

One-pot hydrothermal green synthesis of Polygala tenuifolia mediated graphene quantum dots for acetylcholine esterase inhibitory activity

The present paper reports the synthesis of Donepezil hydrochloride functionalized Graphene quantum dots (DO-ptGQD) for the cure of Alzheimer disease. Graphene quantum dots were synthesized through root extract of Polygala tenuifolia by using one-pot hydrothermal synthesis method. Using UV/Visible spectroscopy, FTIR, SEM, TEM and XPS methods, the synthesized ptGQD was evaluated. Further the formulated DO-ptGQD was evaluated by SEM, TEM, FTIR, XPS techniques and was further evaluated for the encapsulation study, in-vitro study and various in-vivo models. Through behavioural model (Radial arm maze and Water morris maze assay) the learning and memory ability of the formulations was evaluated and the outcomes indicate that the DO-ptGQD markedly decreases the transmission latency to get in the baited arm in 12.19 ± 0.39 s or to the hidden stage in 15.37 ± 0.45 in 7 days. DO-ptGQD show more percentage inhibition of AchE enzyme that is 86.23 ± 1.28 as likened with the drug and ptGQD. DO-ptGQD considerably increases the protein and glutathione level and decreases the nitric oxide and lipid peroxide level. The Histopathological image indicates that DO-ptGQD treats the disorganization of the cell and show more preservation of small pyramidal cells as compared with the other formulations. In conclusion, DO-ptGQD was safe and effective drug delivery system for the treatment of Alzheimer disease and also the root extract of Polygala tenuifolia provide synergistic effect for the treatment of disease.

Sieving Effect for the Separation of C2 H2 /C2 H4 in an Ultrastable Ultramicroporous Zinc-Organic Framework.

The separation of C2 H2 from C2 H4 is one of the most challenging tasks due to the similarity of their physical properties. In addition, green synthetic protocol and adsorbent's stability are also the major concerns during the separation. Herein, under hydrothermal green synthesis conditions, an ultrastable ultramicroporous Zn-MOF was designed and synthesized with a high yield. The pore diameter of the Zn-MOF is 3.6 Å, which lies in between the diameters of C2 H2 (3.3 Å) and C2 H4 (4.2 Å) molecules, leading to an efficient separation of the C2 H2 /C2 H4 mixtures by the sieving effect. The practical separation performance of C2 H2 /C2 H4 was confirmed by the dynamic breakthrough experiments. Moreover, the high stability enables the adsorption capacity of the Zn-MOF to C2 H2 , which can be maintained under a wide range of pH (1-13). Molecular simulations were also performed to identify the different C2 H2 - and C2 H4 -binding sites in Zn-MOF.

Hydrothermal green synthesis of MoS2 nanosheets for pollution abatement and antifungal applications.

In this study, we report a green synthesis of MoS2 nanosheets (NSs) using a facile hydrothermal technique in the presence of l-cysteine. l-Cysteine can serve as a greener source of sulfur as well as a capping agent to help the growth of MoS2 nanosheets. The prepared materials were characterized by X-ray powder diffraction (XRD), scanning electron microscopy (SEM) with energy dispersive spectroscopy (EDS), electron transmission microscopy (TEM), X-ray photoelectron microscopy (XPS), and Brunauer, Emmett, and Teller (BET) analysis. The results showed that MoS2 NSs are of high crystallinity with a lattice spacing of 0.61 nm. The optical bandgap of MoS2 NSs nanosheets prepared using l-cysteine as a source of sulfur was found to be 1.79 eV. The photocatalytic degradation of MoS2 NSs towards methylene orange (MO) and rhodamine blue (RB) dyes under sunlight was found to be promising for practical applications. The fast kinetics of degradation of MO and RhB was observed over a wide range of pH range. Moreover, MoS2 NSs showed excellent antifungal activities against Trichophyton mentagrophytes and Penicillium chrysogenum fungus.

Facile green synthesis of ZnFe2O4/rGO nanohybrids and evaluation of its photocatalytic degradation of organic pollutant, photo antibacterial and cytotoxicity activities

In this work, we report a facile hydrothermal green synthesis of ZnFe2O4/reduced graphene oxide nanohybrids (denoted as G-ZnFe2O4/rGO NHs) in the presence of orange peel extract as natural surfactant. The obtained G-ZnFe2O4/rGO NHs were systematically characterized in detail, and then they were served as photocatalyst for degradation of methylene blue (MB) and in vitro biological applications. Importantly, the as-prepared G-ZnFe2O4/rGO NHs showed best photocatalytic performance (92.4 %) than bare G-ZnFe2O4 toward methylene blue degradation under visible light irradiation. In addition, the photo antibacterial and in-vitro anticancer activity of the resulting nanohybrids were evaluated against Escherichia coli and A549 cell line respectively. Under a simulated visible irradiation for 40 min, the G-ZnFe2O4/rGO NHs exhibited effective antibacterial activity and the bacterial survival was found to be 29.43 ± 4.2 %. The cytotoxic activity of the G-ZnFe2O4/rGO NHs showed significant cytotoxic activity against A549 cell line with an IC50 value of 249.9 μg/mL. The present study clearly suggests that G-ZnFe2O4/rGO NHs have great potential in various tribological applications for saving energy, economic, environmental remediation, and biomedical applications.

Rapid microwave-assisted hydrothermal green synthesis of rGO/NiO nanocomposite for glucose detection in diabetes

Diabetes is one of the fastest growing diseases worldwide that can lead to dangerous complications. Therefore, the demand for the development of optimal glucose sensors has increased for diabetes disease management. In this study, a non-enzymatic glucose sensor based on a reduced graphene oxide and nickel oxide (rGO/NiO) nanocomposite was developed. This novel rGO/NiO nanocomposite was synthesized using a facile and rapid green economic microwave-assisted hydrothermal method in the absence and presence of organic/reducing agents and subcritical water, respectively. The morphology and composition of the as-prepared rGO/NiO nanocomposite were characterized via X-ray diffraction, Fourier transform infrared, energy-dispersive X-ray spectrometry, and field emission scanning electron microscopy. The electrochemical performance of the rGO/NiO-modified electrode was examined by cyclic and square wave voltammetric techniques under optimal conditions. The results indicated that the developed rGO/NiO electrode exhibited a good performance toward glucose detection in 0.1 M NaOH alkaline solution with two linear electrochemical responses to glucose ranging from 20 μM to 80μM and from 1mM to 15 mM. Moreover, the detection limit was 19.35 μM ([S/N] = 3). The fabricated sensor was also investigated for the detection of glucose in the presence of common interfering species. Thus, the sensor exhibited good sensitivity and selectivity and was repeatable, stable, and economical for non-enzymatic glucose detection. Additionally, the proposed sensor was successfully applied for glucose detection in human serum samples with satisfactory recoveries.

Template-free microwave-assisted hydrothermal synthesis of manganese zinc ferrite as a nanofertilizer for squash plant (Cucurbita pepo L)

Manganese, zinc, and iron are the most essential micronutrients required for plant growth and applied as foliar fertilizers. Herein, a simple template-free microwave-assisted hydrothermal green synthesis technique was adapted to produce manganese zinc ferrite nanoparticles (Mn0.5Zn0.5Fe2O4 NPs) at different temperatures (100, 120, 140, 160 and 180 °C). The prepared nanomaterials were employed at different concentrations (0, 10, 20, and 30 ppm) as foliar nanofertilizers during the squash (Cucurbita pepo L) planting process. X-ray diffraction patterns of the prepared nanomaterials confirmed successful production of the nanoferrite material. The prepared nanofertilizers showed type IV adsorption isotherm characteristic for mesoporous materials. FE-SEM and HR-TEM imaging showed that the nanoparticles were cubic shaped and increased in particle size with the increase in microwave temperature during production. The impact of application of the synthesized ferrite nanoparticles on vegetative growth, proximate analysis, minerals content and the yield of squash plant was investigated for two consecutive successful planting seasons. The nanoferrite synthesized at 160 °C and applied to the growing plants at a concentration of 10 ppm gave the highest increase in % yield (49.3 and 52.9%) compared to the untreated squash for the two consecutive seasons, whereas the maximum organic matter content (73.0 and 72.5%) and total energy (260 and 258.3 kcal/g) in squash leaves were obtained in plants treated with 30 ppm ferrite nanoparticles synthesized at 180 °C. On the other hand, the maximum organic matter content (76.6 and 76.3%) and total energy (253.6 and 250.3 kcal/g) in squash fruits were attained with plants supplied by 20 ppm ferrite nanoparticles synthesized at 160 °C. These results indicate that the simple template-free microwave-assisted hydrothermal green synthesis technique for the production of manganese zinc ferrite nanoparticles yields nanoparticles appropriate for use as fertilizer for Cucurbita pepo L.

Hydrothermal green synthesis of magnetic Fe3O4-carbon dots by lemon and grape fruit extracts and as a photoluminescence sensor for detecting of E. coli bacteria

The aim of this work is preparing of a photoluminescence nanostructures for rapid detection of bacterial pathogens. Firstly, carbon dots (CDs) were synthesized by grape fruit, lemon, turmeric extracts and hydrothermal method. Then Fe3O4 (magnetite) nanoparticles was achieved using these bio-compatible capping agents. Finally, magnetite-carbon dots were synthesized as a novel magnetic and photoluminescence nanocomposite. X-ray diffraction (XRD) confirms the crystallinity and phase of the products, scanning electron microscopy (SEM) and transmission electron microscopy (TEM) investigate the morphology, shape and size of the magnetite, carbon dot and nanocomposites. Fourier transform infrared (FT-IR) spectroscopy shows the purity of the nanostructures. Ultraviolet-visible (UV–Vis) absorption and photo-luminescence (PL) spectroscopy show suitable photo-luminescence under ultraviolet irradiation. Vibrating sample magnetometer (VSM) shows super paramagnetic property of the product. Interestingly carbon dots were used as a non-toxic photoluminescence sensor for detecting of Escherichia coli (E. coli) bacteria. Results show quenching of photoluminescence of the CDs nanocomposite by increasing amount of E. coli bacteria.

Hydrothermal green synthesis and photocatalytic activity of magnetic CoFe2O4–carbon quantum dots nanocomposite by turmeric precursor

In this work firstly carbon quantum dots were prepared by using turmeric as a green starting materials. Hydrothermal method was used as an effective method for preparation of product with preferential growth. Finally, CoFe2O4 and magnetic cobalt ferrite–carbon nanocomposite were synthesized. To the best of our knowledge, this is the first work that carbon quantum dots were prepared form biocompatible and cost effective turmeric precursor. The effects of time and temperature on the morphology and particle size were investigated. Nanostructures were characterized by X-ray diffraction, scanning electron microscopy, transmission electron microscopy, Fourier transform infrared spectroscopy, ultra violet–visible absorption and photo-luminescence spectroscopy. The prepared product show suitable photo-luminescence under ultraviolet irradiation. Vibrating sample magnetometer shows ferromagnetic property of the both CoFe2O4 and cobalt ferrite–carbon nanocomposite. Photocatalyst property of the magnetic nanocomposite was investigated by degradation of three azo dyes (acid black 24, acid brown 14 and acid red 1) under ultra violet irradiation. The results confirm that green synthesized nanocomposites show applicable photoluminescence and photocatalyst properties.

Hydrothermal green synthesis of gold nanoparticles using mushroom (Agaricus bisporus) extract: physico-chemical characteristics and antifungal activity studies

AbstractEdible mushroom (Agaricus bisporus) extract was used to synthesize gold nanoparticles (AuNPs) through hydrothermal process (at a pressure of 15 psi and a temperature of 121°C for 15 min). Response surface methodology was applied to monitor the influence of the synthesis parameters, namely: the mushroom extract concentration (1–9 gr DP/100 ml distilled water) and the amount of HAuCL4·3H2O solution (8–12 ml) on the particle size and concentration of fabricated AuNPs. The obtained results demonstrated that while the main and quadratic terms of the synthesis parameters had significant (p<0.05) effects on the response variables, their interactions had insignificant effect on them. The results indicated that spherical synthesized AuNPs using 10 ml of HAuCl4·3H2O solution (1 mm) and 1 ml of mushroom extract with concentration of 5 gr DP/100 ml had mean particle size (25 nm) and maximum concentration (534 ppm) and stability (zeta potential of –45.8 mV). The results revealed that mushroom extract could act as both reducing and stabilizing agents due to its bioactive compounds. Fourier-transform infrared analysis showed that polyols and carbonyl groups in mushroom extract had strong effects on formation of stable AuNPs. The fabricated AuNPs exhibited high antifungal activity againstAspergillus flavusas compared to theAspergillus terreus.

Hydrothermal green synthesis of silver nanoparticles using Pelargonium/Geranium leaf extract and evaluation of their antifungal activity

Abstract Silver nanoparticles (AgNPs) were synthesized using Pelargonium/Geranium leaf extract via a hydrothermal method. The effects of the Pelargonium/Geranium leaf extract concentration (PLEC) and the amount of 1 mm AgNO3 solution on the center of the broad emission peak (λmax) and the color of the synthesized AgNP solution were investigated by using response surface methodology. The main reducing and stabilizing compounds of Pelargonium/Geranium leaf extract were identified by Fourier transform-infrared and gas chromatography. Spherical AgNPs with an average size of 29 nm were successfully fabricated at the optimal synthesis conditions using 9.8 ml of 1 mm AgNO3 solution and 0.1 ml of 0.62 g/100 ml PLEC. AgNPs were determined to have a polydispersity index value of 0.413 and a ζ potential of +0.6 mV. The antifungal activity of fabricated AgNPs was tested against Aspergillus flavus and Aspergillus terreus, and found to posses a significant inhibitory effect against these microorganisms.

One-step hydrothermal green synthesis of silver nanoparticle-carbon nanotube reduced-graphene oxide composite and its application as hydrogen peroxide sensor

A novel sensing composite of silver nanoparticles (AgNPs)-reduced graphene oxide (rGO)-carbon nanotube (MWCNT) was successfully synthesized by a simple one-step hydrothermal method without reducing agent. Mild reduction of GO was carried out under hydrothermal condition. While most conventional approaches make use of multistep chemical methods wherein strong reducing agents, such as hydrazine, hydroquinone, and sodium borohydride are employed, our method provides the notable advantage of a single-step reaction without employing any toxic solvent or reducing agent by providing a novel green synthetic route to produce the nanocomposites of rGO, carbon nanotube and silver. The results of X-ray diffraction (XRD) and Fourier-transform infrared transmission spectroscopy (FT-IR) confirmed the simultaneous formation of silver nanoparticles in the GO and MWCNT matrix. Field emission scanning electron microscope (FESEM) images and transmission electron microscopy (TEM) showed uniform distribution of nanometer-sized silver nanoparticles and narrow-sized MWCNT on GO sheets, which was achieved using silver ammonia complex as the precursor, instead of the commonly used silver nitrate. The composite exhibited excellent electrocatalytic activity for the reduction of H2O2 with a fast amperometric response time less than 3s. The electrocatalytic activity for the reduction was strongly affected by the concentration of silver ammonia solution in the nanocomposites, with the best electrocatalytic activity observed for the composite of 6:1 volume ratios of MWCNT–GO (3:1, v/v) to Ag(NH3)2OH (0.04M). The corresponding calibration curve for the current response showed a linear detection range of 0.1–100mM (R2=0. 9985), while the limit of detection was estimated to be 0.9μM.

Microwave‐Assisted Hydrothermal Green Synthesis of Analcime Icositetrahedra: Insight into Intermediates Formed in the Reversed Crystal Growth Process

AbstractThis contribution reports new details that we have observed in the early stages of the reversed crystal growth of zeolite analcime icositetrahedra synthesized by a facile microwave‐assisted hydrothermal method in the presence of sodium carboxymethyl cellulose (CMC) as a green template. The detailed time‐dependent evolution of the crystallization and the morphology of the crystals were elucidated by X‐ray diffraction (XRD) and field emission scanning electron microscopy (FE‐SEM) analysis. Under microwave irradiation and in the viscous environment provided by CMC, some kinetically controlled stages provided new information about the early stages of analcime crystal growth; hollow microsphere thin‐shell nanoplatelets and nanorods orderly fill the core, and this creates a thick core. The influence of parameters such as CMC concentration, microwave irradiation time, and hydrothermal reaction time on the crystallinity, size, and morphology of the analcime crystals was thoroughly investigated. Perfect large analcime icositetrahedra were obtained only at CMC concentrations and long microwave irradiation times. Moreover, the employment of acid‐treated seeds led to the formation of analcime nanocrystals of 60 ± 20 nm accompanied by the retained ANA parent. Our results suggest that these newly revealed orientations of the precursors could shed light on the early stages of reversed crystal growth of other zeolites and microstructured materials in the field of materials science and crystal engineering.