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Nanoparticle Synthesis - Science topic

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Good evening everyone
I am working on green synthesis of selenium nanoparticles from leaf extract. The research article mentions that during selenium nanoparticle synthesis, ascorbic acid should be used as a catalyst. so why there is a need to use a catalyst?., and what is the best drying method for synthesized selenium nanoparticles?
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Is a reducing agent or capping agent which makes the material dispersabe in any solution. Ovum drying is ok with mild temperature.
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Does anyone know?
1. Do biosurfactants still have the capacity to reduce surface tension when used as nanoparticle stabilizing agents?
2. When nanoparticles are produced mediated by biosurfactants, are they in the form of liposomes or micelles? by considering several references using the Riverse microemulsion synthesis procedure (water to oil)
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Biosurfactants have the same properties as synthetic ones. They differ only in that they are isolated from substances of animal or plant origin.
1. Biosurfactants can reduce surface tension when used as stabilizing agents for nanoparticles.
2.When nanoparticles are synthesized in water-in-oil microemulsion, they are synthesized in the form of nanoparticles of metals, salts. It is necessary that biosurfactants form stable microemulsions.
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I want to study the opto-structural and magnetic property by XRD,XPS and SEM analysis.
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The co-precipitation route for Chlorine (Cl) doped Copper Oxide Nanoparticles synthesis involves the simultaneous precipitation of copper and chlorine ions from their respective precursor solutions. Copper chloride (CuCl2) and a chloride-containing compound are mixed together in a solvent, followed by the addition of a precipitating agent such as sodium hydroxide (NaOH). This leads to the formation of copper oxide nanoparticles doped with chlorine. The resulting precipitate is then washed, dried, and calcined to obtain the final Chlorine-doped Copper Oxide Nanoparticles.
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I want to prepare a solution of TiCl4 in Millipore water for the Titanium nanoparticle synthesis.
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Perhaps the maths are simple enough: 1 mole TiCl4 means ~ 190 g , so simply dissolving 19 g in 100 ml would do. The problem is, TiCl4 rapidly hydrolyzes to Ti-chloro-Oxyhydroxides and HCl, so the solution cannot be stable at all. I suppose Mahima Yadav is asking for what chemical component to add in which manner and which amount, regarding equilibrium target concentration is required for the purpose. I think such solution is virtually impossible to remain stable at ambient temperature and pressure
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Hi all,
I am currently working on a microfluidic system where two fluids are introduced with adjustable flow rates into a mixing chamber. The purpose of this system is to facilitate nanoparticle synthesis. The construction of the microfluidic part of my system is completed, and I have a working model of the mixing process that does not include the synthesis aspect.
My inquiry centers around whether anyone has expertise in modeling the synthesis that occurs within such a system. Specifically, I am interested in any type of synthesis modeling as my primary goal is to ascertain the feasibility of simulating this process. Additionally, I am curious to learn which physical principles I should take into account when developing my model.
Any guidance or references to relevant literature would be greatly appreciated.
Thank you in advance for your time and assistance.
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I may have some input on this but, as always, there is a lot to understand first: The word "nanoparticles" covers a wide range of materials that can be formed under an even wider range of conditions. Do you have any particlular material in mind and are you thinking about som specific reaction conditions?
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I am working on Chitosan nanoparticle synthesis and characterization. But I can see the nanoparticle aggregate after some time and hence the respective increase in particle size. How to increase the stability, please suggest.
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Stability of chitosan nanoparticle as a colloid is dependent on the electrostatic repulsion between the particles. Since chitin and chitosan are protonated at acidic pH, it will increase the electrostatic replulsion between particle and therefore more stable colloid. So, I recommend you to slightly reduce to pH to approximately 5-6.
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After nanoparticle synthesis using plant source, we need to take the absorbance data to see the high peak. My question is -
Do I need the blank to get the absorbance data or I can get the absorbance data by keeping the nanoparticle solution in different wavelength?
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Dear friend Md. Shoebul Islam
According to the Beer-Lambert law, the absorbance of a solution is proportional to the concentration of the absorbing species in the solution. The blank is used to zero the spectrophotometer before measuring the absorbance of the standard and unknown solutions. Every standard curve is generated using a blank. The blank is some appropriate solution that is assumed to have an absorbance value of zero (8.5: Spectroscopic Characterization of Nanoparticles....). Therefore, it is recommended to use a blank when measuring absorbance data.
I hope this helps! Let me know if you have any other questions.
Source:
(2) What is negative absorbance and why am I getting it?. https://www.researchgate.net/post/What_is_negative_absorbance_and_why_am_I_getting_it.
(4) Solubility of Nanoparticles - Kansas State University. https://www.phys.ksu.edu/reu2016/hbuckner/.
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I would like to synthesize SnO2 nanoparticles from SnCl4. Having problem with ppt washing. Precipitates washing away during cleaning. Please help with expert opinion or suggestions.
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What is your washing media? Water? Try using some organic solvent like alcohol. your unreacted reactant may be soluble in that. Do check if your ppt is also soluble or not?
Also after drying do check the phase purity by XRD or any other analytical method. Hope it works..
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I made HSA nanoparticles by desolvation method. I took 180mg HSA and dissovled it in 4mL of milliQ water (45mg/ml) and then in the protien solution added 2.5mL of ethanol dropwise, then these nanoparticles were stablized by adding EDC (5mg in 0.5ml of milliQ). The solution was left for 3hrs for nanoparticles synthesis under constant stirring at 1250. The nanoparticles size was checked by zeta sizer and the size found to be 64nm. Then i tried to settle down the nanoparticle at 13000rpm for 10 min but I'm not getting pellet. Further I also tried to increase the cetrifugation speed and time still i did not get the pellet. Any suggetion about this query would be appreciated.
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With such a small hydrodynamic diameter (less than 100 nm) you may need more centrifugal force to sediment the nanoparticles. When you say 13000 rpm, you should convert your value to "g", because, depending on the centrifuge, size of rotor, type of rotor (vasculating or fixed) the conversion between rpm and g is different. I would try to centrifuge up to about 20000xg and maybe add NaCl (approx 10 mM if it does not influence the formulation) to improve sedimentation.
If you can't reach that centrifugal force with your equipment, you can try to purify by ultrafiltration, centrifuging with filters of about 3KDa pore diameter.
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I found some issues trying to clean a micrometric channel made of PDMS. This channel is part of a chip which has been used as a droplet generator before and it's 50 micrometers wide and 25 micrometers deep. Now I use it for Nanoparticle synthesis. I tried using a syringe pump loaded with DI water and it leaves clots of NPs inside of channel, making the chip useless. Do you have any idea which material (Like HCl solution) I should use and how to use it (Ultrasound or pumping)?
Thanks
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Is it possible to recast and replace the PDMS device after a certain length of time?
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Dear beloved scientist.
I have a question regarding ZIF-8 Nanoparticles synthesis. I used Zn(NO3)2.6 H2O as Zn2+ precursor and 1,2-dimethylimidazole (1,2-Dmim) as the Mim source with molar ratio of 1:4. Then they were solved in 50 ml methanol and stirred for 24 h at room temperature. But, after 2- 3 hours, there is no color change in the reaction solution. I use this journal as my reference for synthesis ( ). Is it normal to have no color change after several hours? How the color of the solution of the success reaction of ZIF-8 NPs? Because it's my first time to do this synthesis. Do you have any opinion that can improve my method? Your opinion regarding this matter is very welcomed.
Thank you.
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Saeideh Hosseini Thank you for your answer, I am using 1,2-dimethylimidazole (1,2-Dmim), but the most articles used 2-methylimidazole, and still a few reporting use 1,2-dimethylimidazole (1,2-Dmim) as the starting material to synthesize ZIF-8
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What are the biggest technological challenges in the production of core-shell nanomaterials?
Can you please tell your experience and/or give comments on morphology control, synthesis precision, stability and durability, economic viability, etc.
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The production of core-shell nanomaterials presents several technological challenges, some of which include:
  1. Controlling the morphology: The morphology of the core-shell nanomaterials can have a significant impact on their properties and performance. Achieving precise control over the size, shape, and composition of the core and shell is therefore critical for producing high-quality core-shell nanomaterials.
  2. Achieving synthesis precision: Core-shell nanomaterials can be synthesized using a variety of methods, including chemical vapor deposition, electrospinning, and sol-gel synthesis. However, achieving high levels of synthesis precision can be challenging, particularly when it comes to controlling the thickness and composition of the shell.
  3. Ensuring stability and durability: Core-shell nanomaterials can be prone to degradation or instability, particularly if the shell is not able to protect the core from environmental factors such as moisture, heat, or pH fluctuations. Ensuring the stability and durability of core-shell nanomaterials is therefore critical for their long-term performance and viability.
  4. Addressing economic viability: The production of core-shell nanomaterials can be expensive, particularly if large quantities are required. Finding ways to produce core-shell nanomaterials at a reasonable cost is therefore an important challenge for the field.
My experience with core-shell nanomaterials has primarily been in the area of nanocatalysis, where core-shell nanoparticles are used as catalysts in a variety of chemical reactions. In my experience, controlling the size, shape, and composition of the core and shell is critical for achieving high catalytic activity and selectivity. Additionally, ensuring the stability and durability of the nanoparticles is important for maintaining their performance over multiple catalytic cycles.
In terms of economic viability, finding ways to scale up the production of core-shell nanoparticles while maintaining their quality and performance is a major challenge. This often requires the development of new synthesis methods that are cost-effective and scalable, without compromising on the precision and control needed to produce high-quality core-shell nanomaterials.
Overall, the production of core-shell nanomaterials presents several technological challenges, ranging from controlling the morphology and achieving synthesis precision, to ensuring stability and durability and addressing economic viability. Overcoming these challenges will be critical for the widespread adoption and application of core-shell nanomaterials in various fields, including catalysis, energy storage, and biomedicine.
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Dear researchers,
Is there any method or device like Amicon 0.5ml ultracentrifuge (Its highest cut-off is 100kDa and not good for my purpose) that I could purify my small amount of volume nanoparticles that are conjugated with high MW polymer (more than 400kDa)? I tried 0.5ml ultracentrifugation of 135k*g for 1 hrs but the pellets are not obvious based on a small initial amount of lipid particles that contain nucleic acid.
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Dear all, it is expected that polymer-NPs conjugation have higher spatial dimensions compared to neat polymer chains, so membrane dialysis may exclude the polymer. My Regards
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I am currently working on chitosan nanoparticles synthesis by ionic gelation method. I dissolve chitosan in 1% acetic acid (to make a solution of 1mg/ml) Regarding that I have some queries:
  1. What is the ideal pH for chitosan nanoparticle synthesis?
  2. Can anyone please share a protocol for chitosan nanoparticles synthesis?
  3. How to increase the yield (final amount in milligram) of synthesized chitosan nanoparticles?
  4. Is it necessary to maintain any specific pH (acidic/basic) of the STPP (cross linker) ?
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The optimum pH ranges from 4.6 to 5; in cases of perparation of chitosan nanoparticles its highly recommended to use high purity chitosan, adding TPP at a proper ratio (1:4) and it should be added drop wise to chitosan solution under stirring
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I'm at the end of my preliminary experiment for the synthesis of Hap, but I noticed traces of black ink in my dried hydroxyapatite, I tried to search at which temperature the component in black ink decomposes, but I'm still quite unsure.
Does these traces of "black ink" decomposes when I further calcinate my dried HAp to 900 celsius for 2 hours?
Best Regards
-Flynne
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It is not possible to determine if the traces of "black ink" in your dried hydroxyapatite sample will decompose during calcination at 900 Celsius for 2 hours without more information about the composition of the black ink.
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e.g: nickel nanoparticles by hydrazine
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The amount of reducing agents used for nanoparticle synthesis can usually be calculated by considering the mass balance, which involves taking into account the stoichiometric ratio of reactants, oxidation numbers, and molar masses. Additionally, the amount of reducing agent needed will depend on the size and type of nanoparticle being synthesized.
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Explanation.
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Colour of NPs is due to surface plasmon, but the colour of semiconductor is due to change of band gap.
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PVP behaves as a capping agent in the synthesis of Ag nanoparticles.
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May i ask you how you prepare the silver nanoparticles?
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For Example, 1 At% / 1 Wt% / 1 mol% of Zn doped in TiO2.
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Hii,
You can estimate the amount of doping via four methods. 1. Go for EDS mapping 2. ICPMS 3. XRF 4. Rietveld refinement of X-ray data. Through occupancies yiou can get your values in at%. However, in refinement intially you have to chose the theoretical value of doping concentrations. After refinement you will get the values. EDS-mapping sometimes gives lesser concentration and so don't believe on EDS results too much. Better will be go for ICPMS and Rietveld refinement.
You can have a look at my papers. I have calculated through Refinement of X-ray data.
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In order to synthesize silver nanoparticles with specific shapes such as triangular or decahedron, we usually add capping agents such as PVP or citrate to the solution. for higher concentration solution the amount of these organic compounds should be increased inevitably. After drying one droplet of the final solution, thick layer of organic materials covers the nanoparticles (as shown in the attached figure).
I have seen that in many papers people suggest using "dialysis bag" or "centrifuge tube with filtration membrane" but both of these techniques may destroy unstable nanoparticles (specially triangular shaped N.Ps). Do you have any suggestion for getting rid of any organic materials form the final solution with out sacrificing the nanoparticles?
(Actually, what I am looking for is removing the excess organic materials from the solutions and not the ones capping on the surface of the Nanoparticle)
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Mohammadreza Khodabakhsh The stability of the system is a function both of the particles (chemistry, charge, etc) and the continuous phase (pH, polyvalent ions, surfactants, stabilizers, admixtures etc) make up. Note also with 'Ag nanoparticles that the surface is invariably oxide (Ag2O) and not metal (Ag0). It's the silver oxide that has some solubility and the Ag+ ion is the bactericide. The organic constituents may be preventing or delaying such oxidation. See, for example, this webinar (registration required):
Silver colloids and invisible ink
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I synthesize mesoporous silica nanoparticles, then the glassware has a white residue in its walls, so how can I eliminate this residue?
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William Alejandro Talavera-Pech If the glassware has been leached (and this is the cause of the frosting/residue) by use of alkali (for example) then it is not possible to recover it. You'll need new glassware.
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Looking forward to the dynamics of plasma - electric field distribution.
and evaluating the forces in plasma - PCVD- nano particle distribution.
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You can reconstruct you reactor geometry with an FEM software, e.g. Comsol, in order to get this information. Colleagues from our institutedid that e.g. in this work for an MW+DC plasma (see fig. 6):
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I used an initiator for polymerization of a monomer, is it possible to use the same initiator for the same monomer to synthesize polymer nanoparticles?
regards
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Dear all, both strategies are used, but for sure not the same results, i.e., NPs features will not be the same. Please have a look at the following document. My Regards
10.1016/j.progpolymsci.2011.01.001
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Hello, I'm working on interactions of some inorganic metals/compounds with some protein of interest. Here the ligand are in nanoparticle form. So as for ligand preparation for docking these need to be in nanoscale range, is there any procedure for preparing it ?
Please suggest some user friendly software other than Vesta if possible!
Thanks in advance.
Regards,
Vinay
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Mohammad Kooti Sir, Thanks for your interest. Actually here the metal compounds that are needed to be converted to nanoparticles will be later subjected to molecular docking analysis with the protein of interest that's why I'm referring to them as ligands. Please guide how to use vesta for such conversion.
Regards,
Vinay.
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The fate of nanodrugs / nanoparticles in vivo draws a lot of attention, and many studies label fluorescent of nanodrugs / nanoparticles in order to disclose their distribution in vivo.
- What are its advantages and disadvantages ?
- Is it a reliable tool ?
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The study of the interaction of nanoparticles (NPs) with proteins is of great importance due to its relevance in several fields including nano-biosafety, nano-bioscience, nano-biomedicine, and nano-biotechnology. an introduction and a discussion of merits of fluorescent NPs compared to molecular fluorophores, labels and probes, the article assesses the kinds and specific features of nanomaterials often used in bioimaging. These include fluorescently doped silicas and sol–gels, hydrophilic polymers (hydrogels), hydrophobic organic polymers, semiconducting polymer dots, quantum dots, carbon dots, other carbonaceous nanomaterials, upconversion NPs, noble metal NPs (mainly gold and silver), various other nanomaterials, and dendrimers. Another section covers coatings and methods for surface modification of NPs..
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Please treatment would you recommend for my mortar and pestle as well as the magnetic stirrer that got stained (with black) after using them for magnetic nanoparticles synthesis?
Thank you
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Dear Abraham,
Keep ceramic morter and pestle dipped in dilute HCl for more time and then ultrasonicate it.
For magnetic stirrer, it's coil should not get damaged. So it would be better if you wrap the magnetic stirrer with Aluminium foil always. Hence staining problem can be avoided.
To remove present staining, try acetone.
Thanks.
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I am currently working on Janus nanoparticles synthesis. I have been tried to wash the colloidosomes with chloroform several times by stirring and centrifugation, and even tried chloroform followed by recrystallization in cold methanol, unfortunately I could not obtain the Janus nanoparticles meanwhile the SEM pictures clearly show the nanoparticles onto the wax surface. Could someone providing me with any suggestions?
Kind regards,
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Dear Alain Pierre Tchameni, what is the name of the wax ? Try to solubilize the wax in an appropriate solvents such as acetone and high carbon alkanes, providing the NPs are not affected. Please check the following links. My Regards
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Dear Everyone. I am trying to do the high yield synthesis from ascorbate and copper salt, according to the similar procedures from the literature (0.18M copper ions) I now tried PVA up to 2%, Tween 20 up to 10%, both, none, dropwise addition of ascorbate, burst addition of ascorbate, nitrogen, air atmosphere, temperatures 50, 60, 90 centigrade. I followed a couple of similar syntheses from the literature, nothing works. All the time instead of suspension I get a salmon-colored precipitate that for sure is not a dozen nanometer copper. What do I do wrong?
Thanks a lot for all the hints
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Slow addition with continuous stirring (magnetic stirring) is required.
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In nanoparticles synthesis, reducing agents change metal into its zero oxidation state,which form cluster with other atoms and then coated with capping agent, why necessary to change metal into zero oxidation states, which force responsible to form clusters?
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thnx for your reply. but i already synthesized the gold clusters stabilized by two thiol ligands . However, when using the same reducing agent NaBH4 with increasing its molar ratio to the gold ions in solution , it results in increasing the intensity of specific band in ints spectrum. my question is what possible reactions might happen caused by NaBH4 more than reducing gold ions to form clusters??
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I am preparing nano ferrites by using microwave hydrothermal method to get the precipitation. We are adding NaOH with maintaining pH, I would like to ask what is the main role of pH?
Does it affect particle size of material? How?
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At higher pH, the surface of the adsorbent is negatively charged. This results in greater attraction for the complex positively charged cations in solution hence, the adsorption increases with increase in pH . This helps to migrated cations between voids due to ionic radius. Hence, it is used to increase their magnetic properties, well-ordered crystallite size and crystallinity
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Hello!
Ive never made micelles before, but I gave it a go today and now I have some questions. I am generating thin films using my polymer solubilized in chloroform, evaporating in a rotovap, and then resolubilizing in water followed by 30 min of sonication. I currently (very sadly) do not have access to DLS, I am thinking about getting the Lens3 from Tosoh and analyzing my particles using MALS very soon, until then I dont have any physical characterization assays setup. As a very general description of my molecule, I have conjugated a hydrophobic molecule onto a cationic/hydrophilic polymer
1. What size flask is appropriate for 2mgs of polymer? I tried 100mL, 250mL, and 1L. the 1L sized flask was a bit cumbersome to do the hydration in and the thin films from the 100 or 250 mL flask dont look that thin
2. How quickly do I add water to the solution? Dropwise or all at once?
3. Should i start sonicating the micelles as they rehydrate? Should I rehydrate and then wait and then sonicate?
4. Does adding salt to micelles during hydration or after hydration change particle size?
5. How stable are cationic micelles in general in water or buffer? Hours? Days Weeks? The paper im referencing has no stability data
6. Are there any solvents that are not acceptable for forming thin films/micelles? Variants of my polymer are soluble in ethanol but not in chloroform so can I use ethanol instead?
Im still going through all the literature to find answers to some of my more basic questions, but any useful papers you can recommend would be very much appreciated and a big time saver for me!
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Micelle forming ability is dependent to your polymer physicochemical properties. Polymer charge and net charge in solution is important. Also HlB is a important parameter.
Furthermore you can use hhydrophobic fluorescence probes such as pyrene for study of micelles in your study. Block copolymers also without charge may generate micelle or reverse micelles in solution.
A book entitled as micelles , monolayers and biomembrane from M.N. jones is useful.
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Which one is better?
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Dear all, for each type of nanocarrier there are various possibilities of drug encapsulation. The following attached chapter gives a brief review of some nanocarriers and the encapsulation methods. My Regards
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At the first 1 g of HIPS polystyrene thermoplastic polymer was mixed with 10 cc of toluene solution for 1 hour and a half using a magnetic stirrer.
The resulting solution was mixed with 0.2 g of hydrophobic sio2 nanoparticles for 1 hour using a magnetic stirrer.
The solution obtained from the previous step was dispersed under ultrasonic bath ( 5 x 100 second cycles )
Then polydimethylsiloxane Silgar 184 was mixed in a ratio of 10: 1 with the solution obtained in the previous step for 30 minutes.
And then 500 seconds (5x100) again with ultrasonic.
The resulting solution was immersed twice as a coating on aluminum substrates, wood and glass slides.
After 24 hours, the coating was dried in the oven for 30 minutes at 100 degrees
The contact angle of the water drop was 118 degrees (without polydimethylsiloxane) if the contact angle with polydimethylsiloxane was expected to increase but decreased to 100 degrees.
Is there a mistake in the protocol?
Is there a problem with the time it takes to put it in the oven?
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Dear Alireza Taheri, please refer to the following documents for better understanding of the contribution of both: PDMS and SiO2, to the contact angle changes. My Regards
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I have synthesized Magnetite Nanoparticles using Cyanobacterial Polysaccharide crystals and as the nanoparticles are not dissolved, I am not able to proceed with my work . Can any one help me in dissolving the MNPs.
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If possible, please let me know which solvent had worked with you ??
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nanoparticles synthesis and applications
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Hello,
Yes, the physical characteristics of amorphous and crystalline TiO2 and ZnO differ slightly, and this influences their performance. Some of the differences found are conductivity, electrical resistance, and some other microstructural characteristics.
For instance, amorphous TiO2 is typically thought to have no photocatalytic properties because the imperfections in the crystal structure can act as recombination centers. However, recent research has found that amorphous TiO2 created via the atomic layer deposition approach can have some photocatalytic activity.
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Stocks of KHP near me ran out due to pandemic and it would take months to arrive if I order overseas. Is it really necessary to standardize them in this type of research? If not, can you please share me an article about it? i would gladly accept your answers
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Dear Paulette Sofia Laurente, one aspect is to be considered as it may affect the dissociation and reactivity of the precursors. This is the so called 'dilution effect'. For example, if using 1 N and 10N NaOH, you add 10 times volume more of water when using 1N compared to 10N, to reach the same pH. The situation becomes more drastic if a surfactant or a capping agent are used, they are more sensitive to concentration (dilution). My Regards
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How the the defects like oxygen vacancies and structure distortion from its original, un saturated bonds. particularly in Ferrites (Ni, Zn ferrites) can effect lattice parameter?.
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Lattice parameter of which one is high : Bulk and Nanomaterils?
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Hello everyone,
I hope you are doing well in this pandemic.
Currently, I am doing PhD in powder metallurgy. I am in the stage of submission, so looking for a postdoc. But, I am a little bit confused about the selection of the topic. I have worked on metal matrix composites, polymer matrix composites, and nanoparticles synthesis during my M.Tech and PhD. I have published papers in all three areas. Can anyone suggest which topic will be better for me (in terms of future scope, novelty)? I am looking for your valuable suggestions.
Thank you
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Dear Naveen kumar
Firstly congratulations for phd work.
For postdoctoral, you need to do valuable litterateur survey. It will give right direction for your future.
All the best ...
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It is hard to find any reference related with gold nanoparticle synthesis using plant extracts that were extracted using ethanol solvent and has weight concentration (m/v) as one of its optimizing parameters aside from other parameters such as temperature, pH, HAuCl4 concentration (mM). I need the weight concentrations parameter for me to refer to and use in my current work for a research project in Masters's.
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THANK YOU EVERY ONE
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Hi community,
I am currently looking into strategies to reliably and robustly generate, preferably in the direction of minimum 50 mg total metal quantity per batch, colloidal bimetallic Janus NPs. While I have come across a variety of options lately (see the references at the end of the question description), there may be some expert advice out there that could point me at important considerations that I have previously not thought of (so I am more asking for directions, rather than a chewed out protocol).
I decided on a simple starting point and created spherical Au NPs around 10-20 nm in diameter as a seed (and reference) material for further ' bimetallization'. These were prepared by the established citrate-reduction method. Then I would like to perform a second step in which I grow the metal of lesser nobility on the Au seed surface. For a metal like Ag, that step seems rather simple as the metal precursor is added with additional reductant and stirred/refluxed for minutes to an hour to complete the process (e.g. [1] or [2]). In combination with Cu, there are also several reported methods (e.g. [3] or [4]), though these two in particular use inert atmosphere to effect the synthesis, which I think should not have to be a necessity to prepare AuCu NPs in general (and would make reproducibility labile I think). Metals such as Ni, Co, and even Fe can be made into a Janus NP with Au (e.g. [5] and [6]). However, I am avoiding a one-pot method to co-reduce the noble and non-noble metal concomitantly, as I would like to exert more control on i) NP size by first establishing the seed size, and ii) its growth mode on the seed by varying e.g. ligand/surfactant concentration (though this reasoning may not be entirely grounded for going with a two-step process).
Any suggestions would be helpful.
References:
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I'm trying to understand exactly what you want to make and achieve.
I worked on bimetallic (PdAu and PdAg) systems in the 1970's during my Ph.D. Are you looking for mixed systems or true alloys? The latter have particular effects (e.g. maximum at ~ Pd60Au40 in diene hydrogenation activity). Such nano systems will need stabilization - mine were stabilized on 'inert' supports to preserve the 'nanoness' (average particle size by number on the support ~ 10 nm). You state that you want to make 50 mg of material. This will have to remain in colloidal suspension or be sterically stabilized on a support - there are no free, independent, discrete particles < 100 nm in a powder. See (registration required):
Dispersion and nanotechnology
Note that in all applications, the surface is critical. I assume you have XPS to look at this - in a mixture the surface and bulk compositions cannot be the same and the surface will be enriched in air through chemisorption induced segregation. I think that you'll have real understanding issues without XPS or Auger to look at surface composition and oxidation states. You say 'several reported methods (e.g. [3] or [4]), though these two in particular use inert atmosphere to effect the synthesis. I think should not have to be a necessity to prepare AuCu' Elements will be found in the fully oxidized state on the surfaces in air or in the presence of oxygen containing systems (water in particular) - we found gold in the +3 oxidation state and so-called 'silver' nanoparticles are 100% oxide on the surface (i.e. all Ag in the +1 oxidation state). Only with extensive Ar+ etching could one get to Ag0 metal well below the surface.
So, a lot to think about. Size is controlled by a number of parameters:
  • Small size is favored by low concentrations of metal precursors
  • Reduction mechanisms are important - I would avoid borohydride reduction like the plague. All gets contaminated with intractable boron. The Turkevich citrate reduction that you mention is widely used. I favored 5 or 10% hydrazine hydrate reduction of metal precursors as well as H2 (also removes/reduces surface oxide). With the latter one needs to understand hydride formation in systems, in particular those containing Pd. TPR (Temperature Programmed Reduction) was very useful in this regard and I was privileged to work with John Jenkins, the inventor of the technique
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I have been synthesizing albumin nanoparticles for about 5 months. But for the last 1 month, I have been having trouble with nanoparticle synthesis. I can precipitate nanoparticles in 1 of the 5-6 experiments I have done. Suspecting that the BSA was broken, we ordered a new one and the result did not change. What could be the problem?
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Dear Cansu Akyol, what about the stability of the ionic liquid used? Please additional details are needed. My Regards
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hi I'm currently trying to synthesize nanoparticles SnO2 by co-precipitation method. From the XRD result, it appears that SnO2 have been detected. But when I tried to check the optical band gap with tauc plot method, the optical band gap was far below 3.6 eV (which is the bulk SnO2 optical band gap). Is there any explanation what causes this? (the absorption curve in the attachment)
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Actually, as Sina Safavi wrote, the band gap of nanomaterials is different than the bulk equivalents. However, due to the reduction of atoms amount in the nanomaterial there are less energy levels that are available, and the band gap, with reduction of the size of nanoparticles, is most often increasing. But I think you should check the XRD diffractograms more thoroughly. Maybe you have some defects or nonstoichiometric phase in your material which can cause the band gap narrowing. Sometimes it can be only a small shift in XRD pattern. And there is strong possibility that you did not obtain perfect crystals via co-precipitation method. And it is also important for what kind of band gap you have applied the Tauc plot (the direct or indirect one).
All the best with your research.
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In nanoparticles synthesis the use of hydroalcohol solvent in soxhlet extraction is correct or not... and I need article reference for this.
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I have synthesized NiO nano particle. And they shown change in properties when we goes from bulk to nano regime. In bulk regime shown transition metal oxide but in nano regime shown semiconductor. Why this properties will be changed? I want to know the exact reason. Please explain it in details.
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Quantum confinement effect is the main reason. Quantum size effects result from reduction in the dimensionality of the material below a certain initial value that leads to changes in the electronic structure. So optical and structural properties are get changed.
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In one reaction, cyanamide and 1,6-diaminohexan were used to link one compound with the NH2 functional group and the other with the COOH. I do not understand exactly the role and function of cyanamide and 1,6-diaminohexan. Can anyone help me?
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Faezeh Mohammadi Please read the following book (chapter 3; link provided below) for detailed explanation of the proposed mechanisms of action.
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I tried to synthesize samarium nanoparticles using curcumin. I used samarium nitrate as a processor and curcumin as a reducing agent. I put the solution of samarium nitrate and curcumin on a magnetic stirrer at 80 ° C for 4 hours. But after centrifugation, I got a small amount of precipitate and could not dry it.
I also put samarium nitrate and curcumin solution in an incubator shaker overnight. No precipitate is formed after centrifugation.
Should I use another substance (eg samarium chloride or samarium oxide) instead of samarium nitrate?
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You need to check the molar concentrations/dilution of your synthesis. No precipitate/precipitate is not the sign for synthesis, instead, the color change is. Your time, temperature also need variations, Curcumin can work but, if for your applications, the use of Curcuma sp. plant extract, can be a feasible choice. Check few references for the Sm- nitrate-based NPs synthesis.
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volume ratio of Nickel acetate and Tannic acid?
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Dear Anju Joseph P.S. Please e.g. have a look at the following useful articles in which particularly the tannic acid-mediated synthesis of NiO nanoparticles is reported:
1. Tannic acid mediated synthesis of nanostructured NiO and SnO2 for catalytic degradation of methylene blue
2. Recent Advances in the Synthesis and Stabilization of Nickel and Nickel Oxide Nanoparticles: A Green Adeptness
Both articles can be freely downloaded as pdf files.
Good luck with you research and best wishes! 👍
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I have heard, that larger the ligands, more better the core shell structures due to the packing of the which in turn results in a decrease in the density of ligands on the surface of the NP.
Is is true? How branching affects the formation of core shell?
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Dear Anchal Yadav many thanks indeed for your interesting technical question. The proper choice of ligands plays a very important role in the design and property control of nanoparticles. For an excellent overview of this field please have a look at the following review article entitled:
The Role of Ligands in the Chemical Synthesis and Applications of Inorganic Nanoparticles
Fortunately this valuable article is freely available as public full text on RG. Moreover, it comprises a list of 600+ references to original research articles in this rapidly expanding field.
In this context please also see the following potentially useful articles:
Effects of Branched Ligands on the Structure and Stability of Monolayers on Gold Nanoparticles
and
PEG-stabilized core-shell nanoparticles: impact of linear versus dendritic polymer shell architecture on colloidal properties and the reversibility of temperature-induced aggregation
Please note that this is just a small selection of relevant articles in this area. I suggest that you also use the "Search" function of RG to find and access other useful research articles related to your subject.
Good luck with you research! 👍
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I am trying to find the reduction potential of long chain primary alkylamines, in particulcar Dodecylamine and Oleylamine.
What it could be?
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Dear Anchal Yadav many thanks for your interesting technical question. I assume that this question is difficult to answer. Quite often such basic data of known compounds have never been studied due to the lack of general interest. Editors of scientific journals always want exciting novel findings. Thus there is little change today too have a manuscript accepted in which you studied the reduction potentials of a series of known long-chain alkyl amines. In fact , I did a SciFinder search for the term "reduction potential of long chain primary alkylamines" and found only 1 (!) reference:
Computational investigation of the control of the thermodynamics and microkinetics of the reductive amination reaction by solvent coordination and a co-catalyst
Even in this case I assume that the article is of little or no use to you. I assume, that the perhaps only potentially useful source for such kind of information is the "CRC Handbook of Chemistry and Physics". Try to get hold of a copy of this book in your university library. Chances are that you can find the date there.
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Hello,
During the synthesis of nanoparticles, many at times a particular pH value is optimum for that process.
I am confused as to whether the pH needs to be adjusted during the reaction while mixing the precursors, or after mixing the precursors (followed by continued stirring for a certain period of time).
Does it depend on the reaction or is there a preferred way?
I am asking this as I have found both of the above mentioned approaches in papers.
For example for the synthesis of covellite copper sulide (CuS) nanoparticles:
  1. https://linkinghub.elsevier.com/retrieve/pii/S2352507X15300159
  2. https://linkinghub.elsevier.com/retrieve/pii/S0254058419308272
Thank you
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Dear all, if the pH has an additional role besides reduction, for exemple in the solubilization of precursors and surfactant/caping agents performance, then it should be adjusted first. Otherwise it is optional. My Regards
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They need to be agglomerate free. They can be in any aqueous or alcohol solution. These are commercially available, but the vendors generally don't tell you how it is done.
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Please i still want more clarity on synthesis of silver nanoparticles. I tried different parameters like changing concentration of plant extract, for silver nitrate and so on. I observed color change from green to dark brown but yet there is nor SPR at 420. My peak is now at 345. Is it possible that my plant extract cannot reduce silver nitrate or what is the justification? Or maybe the problem could be silver nitrate?
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Dear Mariah Muhongo
Please find and read a very useful article in this regard with the title “Green synthesis and characterization of silver nanoparticles using Cydonia oblong seed extract”. They have developed not only their own technique but have also discissed about the prone and con of the previous techniques.
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I have encountered some studies doing this through some calculations involving FWHM values of PL bands but I couldn't figure that out. I am calculating radii by using the effective mass approximation. EMA predicts radii through bandgap energy, therefore, the output is unrealistically precise and doesn't have any error function. One of the reviewers especially asked for the size distribution calculation from the FWHM value of the PL band.
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There is Scherrer's equation for X-ray diffraction analysis of nanocrystals, which lets calculate average size of them from FWHM of X-ray peak. But I don't listen about similar calculation for PL spectra. Of course, the PL peak position depends on Eg, and Eg is a function of nanocrystal size. So, your calculations of radii by using the effective mass approximation looks quite reasonable, I believe.
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Hello, I am creating Nickel nanoparticles and I am always creating a black precipitate. I either use NiCl2/NiSO4 with citrate or PEG in water/Ethanol. My reducing agent is NaBH4. No matter what combination or slight molar changes I do, I always get a black precipitates forming. Sometimes they're a fine mist that settles after or large chunks. If anyone has any experience with this, please let me know. Thank you in advance.
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Dear All,
Based on my experience, I would be inclined to say that the reaction product is agglomerates of nickel oxides. If the reduction of the salt with borohydride is not carried out in a deoxygenated argon atmosphere, nanoxides are always formed, even if there is still a reducing agent in the reaction solution.
Of course, I agree with the previous speakers that the product must be isolated and identified.
Good luck!
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I recently found a publication that states extruded nanoparticles of roughly 120nm with +/- 1.21nm. This converts to a PDI of roughly 0.00011. Is this reliable? Or even possible?
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The PDI reported in the Zetasizer software comes from the normalized second order term of the cumulant fitting. Assuming a Gaussian distribution the relation PDI = (sigma/peak mean)^2 holds.
The calculation is well-described in the international standards. For example ISO22412:2020 and ASTM E2490-09 (15).
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I have seen 'n' of papers talking about deposition of semiconductor shells on metal surfaces. However, there is a very limited literature about the deposition of metal shells on semiconductor nanocrystal. Why is it hard to achieve a full or complete shell on semiconductor?
Please pour your suggestions.
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I have chemically synthesized silver nanoparticle to combat microbes on wound site. I have used many methods of synthesis, but I found minimal field of silver NP product.I am getting whitish precipitate if I target high yield using sodium borohydride and ethanol.
Is there any method that give high yield silver nanoparticles. I would also like to know the post processing steps after AgNP synthesis(drying, finding collidal NP concentration,resuspension), as many articles won't report those steps.
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Dear Hari Prasath Nagaiah, many investigations witness precipitation is the best choice for high yield and easy synthesis technique. Please check the following documents and links. My Regards
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hello
I am trying to synthesize CS NPs by ionic gelation method using TPP but I can not get PDI under 0.3. what am I doing wrong? here is my method till here.
my sizes are good and under 300 nm mostly. even though I use filtering (0.22 nm filters) and sonication and centrifuge. and I dilute my sample before testing for getting a more transparent solution.
the Conc of my LMW CS is 1 mg/ml (solvent 10 cc acid acetic 0.1 %) and Conc of TPP is 0.5 mg/ml (solvent 10 cc deionized water).
I let the CS to dissolve overnight on the heater stirrer with temperature 30-40 C. the next dey I have a transparent CS solution. after dissolving the TPP by stirring for about 10-30 min at RT, I add TPP dropwise to the stirring CS solution. I used syringes sometimes but the rate of adding was too rapid I think and by using burette I could control the rate but I think it was still high and with bigger drops. all of TPP solution will drop in about 4 min into the CS solution. how should I add TPP? with such rate and what equipment? after adding TPP, I let the solution to stirr for 1 h in RT in 7000 rpm trying to have a balanced stirr. and then I centrifuge for 5 min, 6000 rpm, after that filtration and sonication for about 2 min.
so now here is my QAs:
1. is there a special environment to work in to be sure that I am avoiding external Contaminations?
2.how should I add TPP? syringes? special made burette?
3.how can I control the rate of adding TPP? and how many drops per min?
4.is the rate of stirring(7000 rpm) while adding the TPP ok?
any suggestion will do
thank you
sorry for the long description
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You may use an infusion pump for controlled addition at a programmable rate.
Filtering out is not a solution to getting the desired particle sizes. By doing so you are just removing the undesired part of the sample, not the root cause.
Probe sanitation is also a good option but that comes with the associated drawback of metal from the probe contaminating your sample and you may find a grey precipitate at the bottom of your sample after you centrifuge it .
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In my laboratory, I have an analog centrifuge (does not show real RPM value). Its' brochure indicates the range is 300-3000 RPM. The regulator is marked from 1 to 10. Is there any way to determine the RPM in this model since it has no digital screen to show the RPM?
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I am confused. A centrifuge separates particles of different sizes, shapes, and densities. It does not synthesize nanoparticles. So, what is the role of the centrifuge in your work? To remove extraneous larger material retaining the nanoparticles in suspension? Concentrating the nanoparticles into a lower layer?
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As it is well known fact that nano-particles can easily aggregate during nucleation/ synthesis part due to high surface energy..by reading literature, I came to know that surfactants can help to prevent this but is there any other method by which we can prevent aggregation of nano-particles without using chemical surfactants?.. Thank you in advance for your valueable time, suggestions and help. ..
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Dear all, a lot of work is done on the powerfull effect of ultrasound and microwaves on nanoparticles aggregation control, so may be this is usefull to investigate in your work. My Regards
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What should be the optimum concentration or volume of acetic acid for chitosan nanoparticles synthesis?
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You should see as much as possible the previous references
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Has anyone synthesised water soluble Fe3O4 magnetic nanoparticles? Or Fe3O4 particles with an aminosylane cover?
if so, which method did you use?
Another question: it is described in literature (J. Phys. Chem. B 2005, 109, 3879-3885) that Fe3O4 magnetic particles form a colloidal solution and remain dispersed in the fluid even in the presence of the external field. does this means that the particles do not react to the magnetic field?
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I am probably late in answering your question. I recommend that you look at our article on the preparation and study of magnetic nanoparticles.
If you have an article ready, I invite you to be published in a special collection of the journal Nanochemistry.
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How can i synthesize silver nanoparticle?
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Be aware that in the presence of air or water you’re synthesizing silver oxide Ag2O, not Ag metal, at least on the top 10 - 15 atomic layers on the surface.
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Why agglomeration occurs during aliginate nanoparticles synthesis.
How agglomeration can be avoided in aliginate nanoparticles synthesis
Can someone define detailed protocol with precautionary measures
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please try to optimum the ratio between your factors, also the pH is so important, secondly make sure there are different grade of alginate.
on the other side, aggumulation happens through repulsion or using big amount of cacl2 with another positive polymer. the pKa of alginate is 3.4 to 4.4.
I have already summarized all formulation factors to obtaine the optimal formulation in this article:
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Could somebody please share some references that compares these two parameters in terms of particle size and morphology. Also, could tuning the concentration of iron salts or the addition rate of the alkaline have a similar effect in changing particle size and morphology?
Thanks
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Hello,
I am trying to form a pellet of PMMA particles. I have tried centrifuging for 1 hour at 26000 RPM (highest the centrifuge I have will go) but the particles do not form a pellet they just clump/form strands thoughout the liquid.
I have also tried in a 1.5mL eppendorf (narrower tube) only going to 15000RPM max speed for 1 hour but the particles form a layer at the top.
Not sure if these particles are impossible to form a pellet or if there is anything else I can do?!
I have about 20% particles to water ratio and am using a 1mL volume in a centrifuge vial that is quite high diameter (compared to eppendorf) at around 1cm diameter.
Thank you.
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Dear all, if I understood well the question, you want to coarsening the nanoparticles, if so, you didn't need centrifuge, just search for 'induction of Oswald Ripenning', you will find different techniques to provoke nanoparticles agglomeration to peletets. My Regards
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DEAR ALL MEMBERS, I am Ph D and have research experience in Nanotechnology specifically focusing Nanoparticles synthesis using plant source, biopolymer, and characterization for antimicrobial, antioxidants, anticancer and wound healing applications. I also studied nanoparticle DNA toxicity and Nanoparticles toxicity to various organs in Zebrafish. I Need suggesting what other areas experience in nanotechnology will help to to broaden my expertise that will helpful to build my research and post doctorate career. Thank in advance
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Since your research is close to molecular biology, you should be interested in the problem of water thin films 2-6 nm in biological structures. Apparently, it is associated with the transmission of information in the human body and various diseases. For example, why does COVID-19 "dock" to the cell and binds to it. This interaction is regulated by water. It is necessary to trick the virus through water and no vaccinations will be needed. Watch the beginning of this research.
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Hello everyone,
I want to know whole chemistry behind synthesis of boron nanoparticle via chemical and biogenic methods. Focussing on why naked boron is not used as I have seen in papers, boron is complexed with some other material like Ag/Zn metal or any other polymer or salt. ALso I want to know the reaction mechanism of Boron nanoparticle synthesis via both biogenic & chemical synthesis approach.
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In generall SDS is an insulator due to its long alkyl chain and hence it prevents the electron transport.
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I looked at your articles. You work with hydrophobic double bond polymers. If you receive polymers by emulsion polymerization in the presence of SDS, then the surfactant will not get into the polymer and will not be an alloying additive. It will dissolve in water.
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Hi, I'm trying a procedure to synthesis nano ZIF-90 in water for specific application, but there is some problem. pxrd pattern for as-synthesized MOF is not completely compatible with charactristic XRD pattern of ZIF-90, in terms of tetha. on the other side, as article indicated, i choose 1 to 40 ratio of zinc acetate to 2-imidazole carboxaldehyde to obtain particles with the scale of 100 nm, but led to really low yield, there is not another way to reach nanosize ZIF-90? I appreciate if anyone has the same experience and could help me.
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Naeimeh Hassanzadeh Goji Anytime. I did not also find the hydrate structure. Maybe it hasn't been reported, yet. You can give it a trial. Good Luck!
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mandatory work need to be carried out
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Zeta potential measurement is essential for your nanoparticles. Nanoparticles exhibit hydrodynamic interfacial double layer consisting of dispersion medium and the dispersed particle. So the value gives you insight into the possibility of aggregation of the particles due to van der Waal inter-particle attraction.
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I am very much confused, may be i have no knowledge regarding this issue.
We claim that in nanoparticle synthesis, the particles are pristine but when we go with the FTIR analysis of the samples, we detect the functional groups or biomolecules of the chemicals we used during the synthesis. If our samples still have the functional groups of the chemicals used during the synthesis how we still claim the purity of our nanoparticles?
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Dear all, if you are using bifunctional or multifunctional reactants, there will be always remaining unreacted functions at the surface. What is the intensity of these functions? Have you done any quantitative analysis? Be sure that you have particles and the concentration is correspending to either the surface or the bulk of particles. My Regards
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I want to know the factors affecting scale up and is kinetic data a parameter in that?
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I would suggest performing incremental reactions to ensure the safety.
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If it possibility to take Metal doped nano SnO2.  Please guide me for measurements
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Yes, we have synthesized the SnO2 nanoparticles by chemical co-precipitation method. we have made the FL life time measurement to study effect solvents and calcination temperature on life time of carriers of synthesized sample. Refer our article "Strctural and Optical properties of Zirconium Oxide nanopaticles : effect of calcination temperature " which we have published recently in Nano Express. We will publish articles on life measurement on SnO2 nanoparticles soon.
Best of luck.
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Hello,
I have to explain why the first UV-vis spectra's peak is near 530 nm (purple color) and when I did a repetition it showed the peak near 600 nm (violet color). I know that violet color and the peak near 600 nm shows the agglomeration of the particles, but I need a scientific explanation. Thank you very much for the help!
I'm adding some key points below:
  • This is a green gold nanoparticles synthesis from banana peels with chloroauric acid.
  • SEM photos for (peak 530 nm) showed the particles size ~45 nm, spherical shape. I don't have SEM results for the repetition (peak 600 nm).
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