We synthesized ZnO NPs using Zinc Acetate and NaOH using a microwave (800W, 5mins). After some time, should the particles settle? How can be sure that it is in nanosize before we test it for TEM?
After some time, the nanoparticles settle. If you pass a narrow beam of light through a transparent dispersion system, then when directed perpendicular to the beam you will see a cloudy dispersion.
if you want to determine the size of the particles, you could do some dynamic light scattering. The technique is based on the scattering, which Yuri Mirgorod described, and gives you information about the size and size distribution of your particles and sample preparation is simple and can be done quickly.
I did not recommend the DLS method. It requires a device. I recommended simple nephelometry. You can use a cell phone flashlight to do this in the dark.
I also did not write that you suggested the DLS method. I just mentioned, that DLS is also based on light scatteing in a certain anlge, as nephelometry.
However, DLS is truly more complicated due to not just measuring the intensity of the scattered light but also it's autocorrelation function.
Any dispersed system consisting of nanoparticles is unstable thermodynamically (to the aggregation of nanoparticles) and kinetically (to the sedimentation of nanoparticles). Extracts contain large molecules of rutin, tannins, with hydroxyl groups that act as reducing agents. They also promote aggregation. Depending on their concentration, sedimentation will occur slowly or quickly.
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I found a research article that describes the preparation of bare and stabilized zinc oxide nanoparticles (ZnO NPs) using a microwave-assisted method 1. The article does not mention whether the nanoparticles should settle after some time. However, it is possible that the nanoparticles may settle over time due to gravity. The settling rate of the nanoparticles may depend on various factors such as the size and shape of the nanoparticles, the solvent used, and the concentration of the nanoparticles in the solution. If you have more specific information about the preparation of the ZnO NPs, I may be able to provide a more detailed answer.
1: ACS Omega
In a solution containing microwave-assisted synthesized zinc oxide nanoparticles (ZnO NPs), whether the nanoparticles settle over time depends on various factors, including the size of the nanoparticles, the stabilizing agents or surfactants used during synthesis, and the overall colloidal stability of the solution.
Here are some considerations:
Nanoparticle Size:Smaller nanoparticles tend to have higher surface area-to-volume ratios and may exhibit stronger Brownian motion, which can hinder their sedimentation. Larger nanoparticles are more likely to settle due to gravitational forces.
Stabilizing Agents or Surfactants:The choice and concentration of stabilizing agents or surfactants play a crucial role in preventing nanoparticle agglomeration and settling. These agents create a protective layer around the nanoparticles, preventing them from coming into direct contact and agglomerating.
Colloidal Stability:Colloidal stability is essential for the suspension of nanoparticles in a solution. If the electrostatic or steric repulsion between particles is sufficient to overcome gravitational forces, the nanoparticles are less likely to settle. Proper stabilization is particularly important for long-term stability.
Surface Charge:The surface charge of the nanoparticles, determined by the pH of the solution and the surface functional groups, influences their stability. Like charges repel each other, contributing to the stability of the colloidal solution.
Agglomeration State:If the nanoparticles agglomerate or aggregate, they may settle more easily. Agglomeration can occur due to inadequate stabilization or other factors during synthesis.
Solvent Properties:The properties of the solvent, such as viscosity and density, can influence the settling behavior. High viscosity can hinder settling, while a higher density may promote it.
If settling is observed and is undesirable for your application, you can take the following steps:
Optimize Stabilization: Ensure that the stabilizing agents or surfactants are appropriately chosen and optimized for the specific synthesis conditions.
Redispersion: Gentle agitation or sonication can be used to redisperse settled nanoparticles. Sonication helps break up agglomerates and ensures a more uniform distribution.
Surface Modification: Consider modifying the surface of the nanoparticles to enhance their stability in the solution.
pH Adjustment: Adjusting the pH of the solution may influence the surface charge of the nanoparticles and their stability.
It's important to note that the settling behavior of nanoparticles can be complex, and the specific conditions of the synthesis and the solution can significantly impact the outcomes. Experimental testing and optimization are often necessary to achieve the desired stability in nanoparticle suspensions.