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Temperature effect on the synthesis of 𝑭𝒆 𝟑 𝑶 𝟒 nano particles
                                                                                            Prasenjit Roy
                                                              EPR Spectroscopy Section, National Physical Laboratory, New Delhi-110012

              𝐹𝑒3 𝑂4 Nano-particles were synthesized at different temperature from 30° to 60° C. Chemical co precipitation method was used in this respect. So particles
              with different size were produced. Later on their structural properties were studied by X-ray diffraction method


Introduction ::
Magnetic fluid or Ferrofluids is a liquid dispersion of magnetic nanoparticles has a potential number of applications in different fields as magnetism, optics, rheology, biophysics, and biomedical. A magnetic
particle with a single magnetic domain is coated or stabilized by surfactant molecules to prevent them from aggregation. Out of the wide variety of Ferrofluids, 𝐹𝑒3 𝑂4 is the most widely used fluid and is the
base of all other application with suitable doping.
In the current work, 𝐹𝑒3 𝑂4 based Ferrofluids was synthesized at different temperature . And the change in their structural properties were studied. For my present work kerosene based oleic acid coated fluid
were synthesized . I have also synthesized water based double coated 𝐹𝑒3 𝑂4 Ferrofluid.


                        Core Shell Structure ::
 The nano sized single domain particles are                          Preperation ::
 coated with surfactant molecules. In case of
                                                                     The process called chemical co-precipitation method. 4.33 g of 𝐹𝑒𝐶𝑙2 . 4𝐻2 𝑂 of 99% purity and 7.15 g of anhydrous 𝐹𝑒𝐶𝑙3 were mixed with water
 polar ferrofluid, as water/alchohol based fluid,
                                                                     to make 100 ml solution. Then both are magnetically stirred till the whole stuff dissolved. Then it is heated at 60 degree Celsius and oleic acid
 there are two layer of surfactants whereas, in
                                                                     were made. When the solution was made. It is kept inside a very precise temperature bath (accurate upto 0.01 K). When the solution reaches the
 non-polar fluid based ferrofluid, only one layer of
                                                                     temperature of the bath, Ammonium Hydroxide was added drop-wise to it till it reaches a pH level of 9. Finally the precipitation state stirred
 surfactant is present giving it a stronger
                                                                     again very well.
 saturation magnetization.
                                                                                                                    𝐹𝑒𝐶𝑙3 + 𝐹𝑒𝐶𝑙2 + 𝑁𝐻4 𝑂𝐻 + 𝐻2 𝑂 → 𝐹𝑒3 𝑂4 + 𝑁𝐻4 𝐶𝑙
                                                                     Finally this precipitation states is separated magnetically using a bar magnet. When the process is repeated 3-4 times, the precipitation is heated
                                                                     on a hot plate and at last kerosene is added to it accordingly. Later on the colloidal solution is ultrasonicated for getting an equally dispersed
                                                                     phase and finally centrifuged to separate out the larger particles.
                                                                                                                                                                              Future Work::
                                                                                                                                                                              The VSM study of the samples are to be
                                                                        XRD Pattern ::
                                                                                                                                                                              done along with the HRTEM of the
                Non Polar                                                The following XRD pattern was noted using Rigaku made X-ray                                          samples so to find the actual size
                                              Polar                         diffractometer. We can further calculate the strain from the                                      distribution of particle inside the sample.
                                                                                                                     given data. Using the                                    In the later stage, EPR study at different
                                                                                                                        Scherrer equation                                     temperature of them will be studied in
                               Stability ::                                                                               and the formula
                                                                                                                                                   ppf4                       details.

Because there are two opposite forces acting one                                                                              4𝜖𝑠𝑖𝑛𝜃 =
                                                                                                                                                                                  Conclusion ::
against another, the fluid stability is depending                                                                                   0.154
                                                                                                                          𝛽𝑐𝑜𝑠𝜃 −         ,                                       The preparation stage of the
upon the thickness of the surfactant layer and the                                                                                     𝐷
                                                                                                                                                                                  samples were kept same . But
diameter of the particle.                                                                                               we can find out
                                                                                                                                                                                  after the synthesis it was
                                                                                                                          the crystallite                                         observed that the sample
 Attraction




              1. Dispersion          Brownian                                                                               size and the                                          prepared at 50 °𝐶 was most
              Forces ~ 𝑟 −6.         Repulsion                                                                           value of strain.                                         stable . So we can optimized
                                                      Repulsion




                                     ~ KT                                                                                                                                         the sample preparation .
              2. Dipole
              attraction ~ 𝑟 −3.

                                                                     Prasenjit Roy is thankful to Dr. R. P. Pant for guiding him , Mr. Mahesh Chand for viscosity data and CSIR for providing fellowship.

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Roy-document-2

  • 1. Temperature effect on the synthesis of 𝑭𝒆 𝟑 𝑶 𝟒 nano particles Prasenjit Roy EPR Spectroscopy Section, National Physical Laboratory, New Delhi-110012 𝐹𝑒3 𝑂4 Nano-particles were synthesized at different temperature from 30° to 60° C. Chemical co precipitation method was used in this respect. So particles with different size were produced. Later on their structural properties were studied by X-ray diffraction method Introduction :: Magnetic fluid or Ferrofluids is a liquid dispersion of magnetic nanoparticles has a potential number of applications in different fields as magnetism, optics, rheology, biophysics, and biomedical. A magnetic particle with a single magnetic domain is coated or stabilized by surfactant molecules to prevent them from aggregation. Out of the wide variety of Ferrofluids, 𝐹𝑒3 𝑂4 is the most widely used fluid and is the base of all other application with suitable doping. In the current work, 𝐹𝑒3 𝑂4 based Ferrofluids was synthesized at different temperature . And the change in their structural properties were studied. For my present work kerosene based oleic acid coated fluid were synthesized . I have also synthesized water based double coated 𝐹𝑒3 𝑂4 Ferrofluid. Core Shell Structure :: The nano sized single domain particles are Preperation :: coated with surfactant molecules. In case of The process called chemical co-precipitation method. 4.33 g of 𝐹𝑒𝐶𝑙2 . 4𝐻2 𝑂 of 99% purity and 7.15 g of anhydrous 𝐹𝑒𝐶𝑙3 were mixed with water polar ferrofluid, as water/alchohol based fluid, to make 100 ml solution. Then both are magnetically stirred till the whole stuff dissolved. Then it is heated at 60 degree Celsius and oleic acid there are two layer of surfactants whereas, in were made. When the solution was made. It is kept inside a very precise temperature bath (accurate upto 0.01 K). When the solution reaches the non-polar fluid based ferrofluid, only one layer of temperature of the bath, Ammonium Hydroxide was added drop-wise to it till it reaches a pH level of 9. Finally the precipitation state stirred surfactant is present giving it a stronger again very well. saturation magnetization. 𝐹𝑒𝐶𝑙3 + 𝐹𝑒𝐶𝑙2 + 𝑁𝐻4 𝑂𝐻 + 𝐻2 𝑂 → 𝐹𝑒3 𝑂4 + 𝑁𝐻4 𝐶𝑙 Finally this precipitation states is separated magnetically using a bar magnet. When the process is repeated 3-4 times, the precipitation is heated on a hot plate and at last kerosene is added to it accordingly. Later on the colloidal solution is ultrasonicated for getting an equally dispersed phase and finally centrifuged to separate out the larger particles. Future Work:: The VSM study of the samples are to be XRD Pattern :: done along with the HRTEM of the Non Polar The following XRD pattern was noted using Rigaku made X-ray samples so to find the actual size Polar diffractometer. We can further calculate the strain from the distribution of particle inside the sample. given data. Using the In the later stage, EPR study at different Scherrer equation temperature of them will be studied in Stability :: and the formula ppf4 details. Because there are two opposite forces acting one 4𝜖𝑠𝑖𝑛𝜃 = Conclusion :: against another, the fluid stability is depending 0.154 𝛽𝑐𝑜𝑠𝜃 − , The preparation stage of the upon the thickness of the surfactant layer and the 𝐷 samples were kept same . But diameter of the particle. we can find out after the synthesis it was the crystallite observed that the sample Attraction 1. Dispersion Brownian size and the prepared at 50 °𝐶 was most Forces ~ 𝑟 −6. Repulsion value of strain. stable . So we can optimized Repulsion ~ KT the sample preparation . 2. Dipole attraction ~ 𝑟 −3. Prasenjit Roy is thankful to Dr. R. P. Pant for guiding him , Mr. Mahesh Chand for viscosity data and CSIR for providing fellowship.