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WeekLog | 02

Week 4-5: Experimental Setup & Preliminary Trials

Objectives

During this phase, the goal is to set up the experimental workflow and conduct preliminary trials to ensure a successful in-situ synthesis of Nickel Ferrite (NiFe₂O₄) nanoparticles on textiles.

🧪 Materials & Chemicals

The following reagents will be used for the co-precipitation synthesis of NiFe₂O₄ nanoparticles:

✅ Iron(III) Nitrate Nonahydrate (Fe(NO₃)₃·9H₂O) – Fe³⁺ source
✅ Nickel(II) Nitrate Hexahydrate (Ni(NO₃)₂·6H₂O) – Ni²⁺ source
✅ Hydrazine Hydrate (N₂H₄·H₂O) – Reducing agent
✅ Hexamethylenetetramine (C₆H₁₂N₄) – Complexing agent
✅ Deionized Water (DI H₂O) – Solvent for reaction

📌 References:
- Hebeish et al. (2019) demonstrated Fe₃O₄ nanoparticle synthesis on cotton fabric using a similar in-situ method. (DOI)
- Wang et al. (2018) reported hydrothermal growth of magnetic nanoparticles on textiles. (DOI)

🛠️ Experimental Workflow

1️⃣ Procurement & Preparation

  • Acquire fabrics (cotton, polyester, nylon) and verify suitability for nanoparticle adhesion.
  • Ensure all nanoparticle precursors and reagents are available and correctly stored.
  • Clean glassware and prepare reaction setup (stirring setup, heating source, pH monitoring system).

2️⃣ Pre-Treatment of Fabrics

To improve nanoparticle adhesion and uniform distribution, the fabrics will undergo surface activation:

✅ For Natural Fibers (Cotton, Wool): Acid/Base Pre-Treatment (HCl or NaOH).
✅ For Synthetic Fibers (Polyester, Nylon): Plasma or UV Activation.

📌 Expected Outcome: Enhanced surface roughness and reactivity for better nanoparticle binding.

3️⃣ Small-Scale Synthesis of NiFe₂O₄ Nanoparticles

Chemical Reaction:

[ Fe(NO₃)₃·9H₂O + Ni(NO₃)₂·6H₂O + N₂H₄·H₂O + C₆H₁₂N₄ → NiFe₂O₄ + Byproducts ]

📌 Reference for Co-precipitation Method:
- Ali et al. (2021) reviewed different synthesis routes for magnetic textiles, including co-precipitation. (DOI)

Reaction Conditions:
  • Temperature: 80-90°C
  • pH Control: Adjust pH using NaOH (if needed) to maintain ~10-11
  • Stirring: Continuous stirring to ensure homogeneous nanoparticle formation
  • Reaction Time: 1-2 hours for optimal nanoparticle growth

📌 Methodology:
1. Dissolve Fe(NO₃)₃·9H₂O and Ni(NO₃)₂·6H₂O in DI water under constant stirring.
2. Add hexamethylenetetramine (C₆H₁₂N₄) to act as a stabilizer and complexing agent.
3. Slowly introduce N₂H₄·H₂O (hydrazine hydrate) while maintaining controlled pH and temperature.
4. Continue stirring until a uniform nanoparticle dispersion forms.
5. Filter and wash the precipitate with DI water to remove impurities.

4️⃣ Fabric Coating & Drying

  • Dip-Coating: Immerse the pre-treated fabric in the NiFe₂O₄ solution.
  • Drying Process: Heat at 100°C for 2 hours to ensure proper nanoparticle adhesion.
  • Curing & Fixation: Thermal treatment at 150-180°C for crystallization.

📌 Expected Outcome: Formation of uniform, well-adhered NiFe₂O₄ nanoparticles on the textile surface.

📌 Reference for Coating Process:
- Ghosh & Molla (2021) used a sol-gel approach for fabric functionalization with Fe₃O₄ nanoparticles. (DOI)

5️⃣ Initial Characterization & Analysis

To evaluate the synthesized nanoparticles and their interaction with the fabric, the following tests will be conducted:

✅ Magnetic Response Test: Check fabric’s response to a neodymium magnet.
✅ Surface Morphology: SEM (Scanning Electron Microscopy) to analyze nanoparticle size & distribution.
✅ Adhesion Testing: Rubbing & washing tests to assess durability.
✅ Phase Identification: XRD (X-ray Diffraction) to confirm NiFe₂O₄ crystal structure.

📌 Reference for Testing & Characterization:
- Rahman et al. (2022) demonstrated washing durability and magnetization testing of functional textiles. (DOI)

📌 Next Steps

If preliminary trials are successful, the next phase will involve:
1️⃣ Optimization of synthesis conditions (temperature, pH, reaction time).
2️⃣ Scaling up the process for larger fabric samples.
3️⃣ Further testing & performance evaluations (mechanical strength, electrical conductivity, EMI shielding).

🚀 By the end of this phase, a stable and uniform NiFe₂O₄ magnetic textile should be achieved!

🔗 References

  1. Ali, A., Shaker, K., & Nawaz, H. (2021). Functionalization of textiles with magnetic nanoparticles: A review on methods and applications. Materials Today: Proceedings, 46, 1231–1240. https://doi.org/10.1016/j.matpr.2021.04.162
  2. Rahman, M. M., Islam, M. T., & Haque, P. (2022). Advancements in smart textiles: Magnetic textiles and their applications in wearable technology. Advanced Materials Interfaces, 9(15), 2102418. https://doi.org/10.1002/admi.202102418
  3. Ghosh, S., & Molla, M. R. (2021). Sol–gel synthesis of iron oxide nanoparticles on textiles for electromagnetic shielding. ACS Applied Materials & Interfaces, 13(5), 7894–7903. https://doi.org/10.1021/acsami.0c20528