WO2013108269A1 - Sintered cobalt ferrites composite material with high magnetostriction - Google Patents

Sintered cobalt ferrites composite material with high magnetostriction Download PDF

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Publication number
WO2013108269A1
WO2013108269A1 PCT/IN2013/000029 IN2013000029W WO2013108269A1 WO 2013108269 A1 WO2013108269 A1 WO 2013108269A1 IN 2013000029 W IN2013000029 W IN 2013000029W WO 2013108269 A1 WO2013108269 A1 WO 2013108269A1
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cobalt ferrite
range
powder
sintered
pellets
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French (fr)
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WO2013108269A4 (en
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Alias Joy PATTAYIL
Mohaideen Kamal KHAJA
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Council of Scientific and Industrial Research CSIR
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Council of Scientific and Industrial Research CSIR
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Priority to US14/372,644 priority Critical patent/US9263174B2/en
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Publication of WO2013108269A4 publication Critical patent/WO2013108269A4/en
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Definitions

  • the present invention relates to sintered cobalt ferrite composite material comprising of nano and micron sized powders of cobalt ferrite with high magnetostriction.
  • the present invention further relates to preparation of nano and micron sized powders of cobalt ferrite, in particular, to the auto combustion process using glycine as fuel for preparing nano sized cobalt ferrite powders.
  • Ferromagnetic materials experience a dimensional change when they are subjected to a magnetic field. This phenomenon is called magnetostriction and is attributed to the rotations of small magnetic domains in the materials which are randomly oriented when the material is not exposed to a magnetic field.
  • magnetostrictive effects including the Joule effect (change in length when ferromagnetic rod is placed in longitudinal field) and the Villari effect (change in magnetic condition when a magnetized ferromagnetic rod is subjected to longitudinal stress), can be used for converting electrical power to mechanical power and vice versa.
  • Magnetostrictive smart materials can be used in sensor applications, principally because of the possibility to sense the control signal from a distance and without wires, which is not in the case for piezo-electric ceramics.
  • ferromagnetic materials examples include sensors (U.S. Pat. Nos.4,414,510 and 5,442,966), transducers (U.S. Pat. No.3,753,058), and vibrators (U.S. Pat. No. 4,151 ,432).
  • these composites show linear magnetostrictive strains of magnitude up to 225 ppm with a rate of change of magnetostriction with applied field ( ⁇ /dH) max of 1.3x10 "9 A "1 m under no external load. They also show good corrosion resistance as well as mechanical properties, apart from its low cost. But these metal bonded ferrites are very much susceptible to magnetomechanical hysteresis. Improvements in both magnetostriction and strain derivative of polycrystalline cobalt ferrite have been reported (D.C. Jiles et al. IEEE Trans. Magn. 41, 10 (2005)) as a result of magnetic annealing.
  • the said article discloses synthesis of mono-phase spinel-type ferrites with the G/N ratio less than about 0.5 for the systems including Mg, Mg-Zn, Co, Co-Zn, Ni, Ni-Zn, (Li, Fe), and (Li, Fe)-Zn, and the ratio between 0.3and. 0.5 for Mn, and Mn-Zn systems.
  • TEM describes that the product powder consisted of agglomerates of primary particles with a typical diameter of about 50nm for a G/N ratio of around 0.4.
  • Table 1 of said article discloses saturation magnetization of 79 emu/g and coercive force of 885 Oe measured for CoFe 2 0 4 at the magnetic field of 15 kOe and at room temperature.
  • Cobalt ferrite is known for its high magnetostriction and there have been many attempts to make sintered polycrystalline cobalt ferrite composites with high magnetostriction at very low magnetic fields. So far there have been no studies reported, on the effect of initial particle size and the resulting microstructure of the sintered material on magnetostriction. It is important to understand the effect of processing conditions, especially during sintering, in the case of nanomaterials. From the application point of view it is necessary to have very large magnetostricitive strains at room temperature. Since cobalt ferrite is an ideal material for future magnetostrictive applications because of its low cost, easy processability, etc. It is the object of the present invention to design a material based on cobalt ferrite with high magnetostriction.
  • the present inventor further directed his research to provide improvements of both magnetostriction level and strain derivative of sintered cobalt ferrite composite material derived from nanosized and micron sized powders of cobalt ferrite, which are effective for use as magnetostrictive sensors and actuators.
  • the further subject of the invention is t provide an improved low temperature auto-combustion process for the preparation of nanocrystalline powders.
  • Main object of the present invention is to provide sintered cobalt ferrite composite material derived from nanosized and micron sized powders of cobalt ferrite, which are effective for use as magnetostrictive sensors and actuators.
  • Another object of the present invention is to provide an improved low temperature auto- combustion process for the preparation of nanocrystalline powders.
  • present invention provides sintered cobalt ferrite composite material comprising of nano and/or micron sized powders of cobalt ferrite, wherein the ratio of nano sized powder of cobalt ferrite to the micron sized powder of cobalt ferrite in said composite is in the ratio ranging between 70:30 to 95:5 wherein said composite material having a density in the range of 79-81 % compared to theoretical density and magnetostriction in the range of 340-396 ppm.
  • grain size of the sintered cobalt ferrite composite material is in the range of 1 to 10 ⁇ .
  • particle size of micron sized powder of cobalt ferrite is in the range of 1 to ⁇ .
  • particle size of the nano sized powder of cobalt ferrite powder is in the range 3 to 40 nm.
  • present invention provides a process for preparation of sintered cobalt ferrite composite material and the said process comprising the steps of: a. dissolving cobalt nitrate (Co(N0 3 ) 2 .6H 2 0) and Ferric nitrate (Fe(N0 3 ) 3 .9H 2 0) in the molar ratio ranging between 1 : 1.5 to 1 :2 in minimum amount of distilled water; b. adding glycine solution in minimum amount of water with solution of step (a) wherein the metal ion to glycine is in the molar ratio of 1 : 0.125 to 1 : 1.25 followed by mixing to obtain a uniform solution; c.
  • step (c) evaporating the solution of step (c) on a hot plate at temperature in the range of 180 to 220°C to obtain the thick mass which is burnt spontaneously to obtain nano sized cobalt ferrite powder; d. mixing C0CO3 and Fe 2 0 3 in the molar ratio ranging between 1 : 1.5 to 1 :2 followed by heating at temperature in the range of 900 to 1 100°C for period in the range of 1 1 to 13 hours; e. grinding immediately the mixture as obtained in step (d) followed by heating for period in the range of 23 to 25 hrs at temperature in the range of 900 to 1 100°C; f.
  • step (c) heating the resulting powder at temperature in the rnage of 1000 to 1 100°C for period in the range of 70 to 72 hours with two intermediate grindings to obtain micron sized cobalt ferrite powder; g. mixing nano sized powder of cobalt ferrite as obtained in step (c) and micron sized powder of cobalt ferrite as obtained in step (f) in the ratio ranging between 70:30 to 95:5 to obtain mixture; h. pressing the mixture as obtained in step (g) to obtain pellets; and i. sintering the pellets as obtained in step (h) at a temperature in the range of 1200-1500C °C for period in the range of 5 to 60 minutes to obtain sintered cobalt ferrite composite material.
  • nano sized cobalt ferrite powder and micron sized cobalt ferrite powder further comprising pressing the cobalt ferrite powder in the form of pellets and sintering at a temperature in the range of 1200- 1500°C for 5 to 60 minutes to obtain sintered pellets.
  • sintered pellets of nano sized cobalt ferrite powder and micron sized cobalt ferrite powder has magnetostriction in the range of 200 to 310 ppm and 150-208ppm respectively.
  • nano sized cobalt ferrite powder is prepared by an auto combustion process using glycine as a fuel, characterized in that, the metal ion to glycine is in a molar ratio of 1 :0.125 to 1 : 1.25. '
  • present invention provides a process for preparation of nano sized cobalt ferrite powder comprising dual sintering of nano sized cobalt ferrite powder prepared by auto combustion process, said dual sintering process comprising;
  • Fig. 1 relates to a graph illustrating magnetostriction curves of different samples synthesized by auto-combustion method using different total metal to glycine ratios.
  • Fig. 2 relates to magnitude of magnetostriction curves of best results from the current studies:
  • the present invention provides a sintered cobalt ferrite composite material with high magnetostriction comprising of nano and/or micron sized powders of cobalt ferrite, wherein the ratio of nano sized powder of cobalt ferrite to the micron sized powder of cobalt ferrite in said composite is in the ratio of about 70:30 to 95:5; the composite material having a density in the range of 79-81 % and magnetostriction in the range of 340-396 ppm and maximum value of piezomagnetic coefficient is 1.9xl0 "9 A " 'm.
  • the sintered cobalt ferrite composite material has a grain size of 8 ⁇ . High magnetostriction of the cobalt ferrite composite of the current invention is observed at applied magnetic field of 800kA/m.
  • the present invention provides cobalt ferrite composite material derived from nariocrystalline powders obtained by low temperature auto combustion process using glycine as fuel in variable ratios of glycine to metal ion.
  • the invention provides a ceramic process to obtain micron sized particles of cobalt ferrites.
  • the invention further relates to dual sintering of nanosized particle of cobalt ferrite obtained from auto combustion process.
  • the present invention provides a process for the preparation of sintered cobalt ferrite composite material comprising; a. Mixing nano sized powder of cobalt ferrite in amount in the range of 70% to 95% and micron sized powder of cobalt ferrite in an amount in the range of 30% to 5% in an agate mortar; b. Pressing the above mixture in the form of pellets; and c. Sintering the pellets of step (b) at a temperature in the range of 1200- 1500 °C for 10 minutes to obtain the desired composite.
  • the magnitude of magnetostriction of sintered cobalt ferrite composites obtained by mixing different ratios of nanosized and micron sized cobalt ferrite are given in examples.
  • the nanosized cobalt ferrite powder used in the composite is prepared by low temperature auto combustion process using glycine as fuel, using variable molar ratio of glycine to metal ion to control the morphology and obtain the desired porous structure and grain size, which forms another preferred embodiment of the current invention.
  • the micron sized cobalt ferrite powder used in the composite is prepared by any of the following processes: i. Ceramic process; ii. Co-precipitation process; iii. Citrate process; iv. Autocombustion process.
  • the present invention relates to an improved auto combustion process using glycine as a fuel to obtain nano sized cobalt ferrite powder.
  • the auto combustion method is very useful for synthesizing homogeneous materials at very low temperatures. This process has several advantages than the other methods of synthesis. It ensures the mixing of metal ions at a molecular level thereby leading to homogeneous powders. Also, shorter reaction times, low temperatures involved, large scale synthesis, high phase purity, fine particle nature of the products obtained, are some of the salient features of this method.
  • the amino acid, glycine plays two important roles in the synthesis. Firstly it forms a complex with metal ions involved, acting as a bidentate ligand.
  • the different end groups i.e., the carboxylic group and amino group can be utilized for complex formation.
  • the zwitter ionic character of glycine allows effective complexation with metal ions of varying ionic size. Also, it enhances the solubility of metal ions thereby avoiding selective precipitation when water is evaporated.
  • the main controllable processing variable is the glycine-to-nitrate ratio, which affects the flame temperature, product morphology and particle size of the resultant product.
  • the invention provides auto combustion using variable molar ratio of glycine to metal ion to control the morphology and obtain the desired porous structure and grain size.
  • the auto combustion process uses glycine as a fuel, where the metal ion to glycine is in a molar ratio of 1 :0.125 to 1 : 1.25 to obtain nanocrystalline cobalt ferrite powder.
  • the auto combustion process for the preparation of nanocrystalline cobalt ferrites comprises: i. dissolving cobalt nitrate, Co(N0 3 ) 2 .6H 2 0, and Ferric nitrate, Fe(N0 3 ) 3 .9H 2 0 in 1 :2 molar ratio, separately, in minimum amount of distilled water; ii. dissolving Glycine separately in minimum amount of distilled water followed by adding to the solution of step (i), wherein the metal ion (Co 2+ and Fe 3+ ) to glycine is in the molar ratio of 1 : 0.125 to 1 : 1.25; iii. mixing the solutions of step (i) and (ii) to obtain a homogenous solution; iv. evaporating the mixed solution of step (iii) on a hot plate (200°C) to obtain the thick mass which is burnt spontaneously to give cobalt ferrite powder.
  • the different sized cobalt ferrite powders obtained from above are pressed into form of pellets and sintered at 1450°C for 10 min. All the pellets are sintered under identical conditions, with a heating rate of 5°C and cooling rate of 20°C.
  • the nanocrystalline cobalt ferrite powder has a particle size in the range 2-40 nm and the sintered pellets have magnetostriction in the range of 200-310 ppm.
  • the highest value of magnetostriction almost 31 Oppm is obtained from the sample 5D on application of low magnetic field of 500kA/m.
  • phase purity of the samples is confirmed by X-ray diffraction studies.
  • the crystalline size of the cobalt ferrite powder obtained by auto combustion process and the Magnetostriction, which is the relative change in the length of the sample in an applied magnetic field, measured on the sintered pellets at room temperature using strain gauge, are described in Table 6 below.
  • the magnetostriction curves of the different sintered samples are shown in Fig. 1.
  • the magnitude of the maximum magnetostriction in the direction of the applied field for the different samples is compared in Table 6.
  • the highest magnetostriction is obtained for the sample synthesized by lowest value of glycine used as a fuel, i.e., Sample 5A to Sample 5D.
  • the auto combustion process of the current invention uses lysine as a fuel.
  • lysine a fuel.
  • stoichiometric amounts of Cobalt nitrate, Co(N0 3 ) 2 .6H 2 0, and Ferric nitrate, Fe(N0 3 ) 3 .9H 2 0 in the 1 :2 molar ratio are dissolved in minimum amount of distilled water, separately.
  • Various amounts of lysine (corresponding to different metal to lysine ratios) are also dissolved separately in minimum amount of distilled water. All the three solutions are mixed. The mixed solution is evaporated on a hot plate. After evaporation of water, the resulting thick mass is burnt spontaneously to obtain the cobalt ferrite powder.
  • Example 1 Preparation of nanocrystalline cobalt ferrite powder (Sample 5A)
  • the cobalt ferrite powder is further pressed into form of pellets and sintered at 1450°C for 10 minutes and cooled to 30°C to obtain sintered pellets of CoFe 2 0 4 .
  • Example 2 Preparation of nanocrystalline cobalt ferrite powder (Sample 5B)
  • the cobalt ferrite powder is further pressed into form of pellets and sintered at 1450°C for 10 minutes and cooled to 30° C to obtain sintered pellets of CoFe 2 0 4 .
  • Example 3 Preparation of nanocrystalline cobalt ferrite powder (Sample 5C)
  • Example 4 Preparation of nanocrystalline cobalt ferrite powder (Sample 5D)
  • the cobalt ferrite powder is further pressed into form of pellets and sintered at 1450°C for 10 min and cooled to 30° C to obtain sintered pellets of CoFe 2 0 4 .
  • Example 5 Preparation of nanocrystalline cobalt ferrite powder (Sample 5J)
  • the cobalt ferrite powder is further pressed into form of pellets and sintered at 1450 °C for 10 minutes and cooled to 30°C to obtain sintered pellets of CoFe 2 0 4 .
  • Example 7 Preparation of sample 1 by ceramic method at different sintering temperature
  • Stoichiometric amounts of C0CO3 and Fe 2 0 3 (in the molar ratio 1 : 1) are weighed and mixed together.
  • the mixture is first heated at 1000°C for 12 hours, cooled to 30°C and further heated for 24 hours at the same temperature after an intermediate grinding.
  • the resulting CoFe 2 0 4 powder ( ⁇ ⁇ ) is further heated at 1 100°C for 72 hours with two intermediate grindings.
  • Sample 1 is then pressed into the form of pellets and then sintered at different temperatures.
  • the magnetostriction is measured on the sintered pellets at room temperature as a function of applied field using strain gages.
  • the variation of the maximum magnetostriction as a function sintering temperature is shown in Table 8.
  • the magnetostriction is largest for the sample sintered at 1400 °C for 10 min and then decreases to lower values when sintering temperature is again increased and decreased from that particular temperature.
  • Cobalt and iron nitrates are taken in the stoichiometric ratio (1 :2 molar ratio) and dissolved in distilled water. 20% of KOH solution is added drop wise to this solution under constant magnetic stirring. A precipitate formed is filtered and washed several times with distilled water until the pH is around 7. The precipitate is dried overnight in an oven at 100°C which is eventually converted to a black powder of cobalt ferrite (5nm).
  • Sample 2 is pressed into the form of pellets and then sintered at different temperatures.
  • the magnetostriction is measured on the sintered pellets at room temperature as a function of applied field using strain gages.
  • the variation of the maximum magnetostriction as a function of temperature is shown in Table 9 for the sintered products obtained by coprecipitation method.
  • Example 9 Preparation of sample 3 by Citrate method
  • Stoichiometric amounts of cobalt and iron nitrates (1 :2 molar ratio) are dissolved in distilled water.
  • Water solution of citric acid is added to the metal ion solution keeping the metal to citric acid ratio as 1 :2.
  • the solution was evaporated on a water bath and finally a thick gel was formed.
  • This precursor is dried in an oven at 100 °C and the dried precursor is calcined at 500°C for 4 hours to get the cobalt ferrite powder (15nm).
  • the corresponding powders are pelletized and sintered at different temperatures.
  • the magnetostriction is measured on the sintered pellets at room temperature as a function of applied field using strain gages.
  • the variation of the maximum magnetostriction as a function temperature is shown in Table 10 for the sintered products obtained by citrate method. Table 10
  • Example 10 Preparation of cobalt ferrite composite of nanosized powder (5D) obtained by example 4 and micron sized powder sample 1 obtained by example 6
  • Composites are prepared by mixing different ratios of the nanosized (3nm) cobalt ferrite (Sample 5D), prepared by combustion method, and micron sized ( ⁇ ⁇ ) powder (Sample 1), prepared by ceramic method, in an agate mortar. All the samples are pressed in the form of pellets and sintered at 1400 °C for 10 minutes. All the pellets are sintered under identical, conditions, with a heating rate of 5°C and cooling rate of 20 °C. The magnetostriction is measured on the sintered pellets at room temperature as a function of applied field using strain gages. The magnetostriction values of cobalt ferrite composites are shown in Table 1.
  • Example 11 Preparation of cobalt ferrite composite of nanosized powder (5D) obtained by example 4 and (5J) obtained by example 5
  • Composites are prepared by mixing the ratios of 80% Sample 5D and 20%Sample 5J in an agate mortar. The samples are pressed in the form of pellets and sintered at different temperatures 1450 and 1400 °C for 10 minutes, with a heating rate of 5 °C and cooling rate of 20 °C. The magnetostriction is measured on the sintered pellets at room temperature as a function of applied field using strain gages. The magnetostriction values of cobalt ferrite composites are shown in Table 2.
  • Example 12 Preparation of cobalt ferrite composite of nanosized powder (5 A) obtained by example 1 and (5J) obtained by example 5
  • Composites are prepared by mixing different ratios of Sample 5A and Sample 5J in an agate mortar. The samples are pressed into form of pellets and sintered at 1450°C for 10 minutes. All the pellets are sintered under identical conditions, with a heating rate of 5°C and cooling rate of 20°C. The magnetostriction is measured on the sintered pellets at room temperature as a function of applied field using strain gages. The magnetostriction values of cobalt ferrite composites are shown in Table3.
  • Example 13 Preparation of cobalt ferrite composite of nanosized powder (5A) obtained by example 1, (5J) obtained by example 5 and sample 1 obtained by example 6
  • Cobalt ferrite composites are prepared by the composition of three different particle sizes of mainly the nanosized cobalt ferrite (Sample 5D and Sample 5J), prepared by auto combustion method, and micron sized powder (Sample 1), prepared by ceramic method, in an agate mortar. All the samples are pressed in the form of pellets and sintered at 1450°C for 10 minutes. All the pellets are sintered under identical conditions, with a heating rate of 5°C and cooling rate of 20°C. The magnetostriction is measured on the sintered pellets at room temperature as a function of applied field using strain gages. The magnetostriction value of cobalt ferrite composites are shown in Table 4.
  • EXAMPLE 14 DUAL SINTERING PROCESS (Sample DS) provide examples for different DS samples as mentioned in table 11
  • the present invention provides a dual sintering of nanosized particle of cobalt ferrite obtained from the auto combustion method using glycine as a fuel.
  • Metal ion to glycine in the ratio of 1 : 0.25 is subjected to auto combustion followed by cold uniaxial pressing to form the pellets.
  • Pellets are sintered at a higher temperature in the range of 1 100- 1500°C, cooled and heated at a lower temperature in the range of 1000-1400°C for a period of lOmin- 60hrs to achieve densification without grain growth.
  • the so obtained sintered cobalt ferrite composites exhibit magnetostriction of -331 ppm.
  • Table 11 lists the Magnitude of magnetostriction of the samples formed by two-step sintering experiments.
  • sintered cobalt ferrite composites derived from nano and micron sized crystalline cobalt ferrite powders exhibit improved microstructure, stable grain size while continuous increase in density unlike in normal sintering, improved magnetic properties, porosity, etc. as compared to materials sintered from bulk counter parts.
  • the improved auto combustion process using variable molar ratio of glycine as fuel provides nanocrystalline cobalt ferrite powders which after sintering exhibit high magnetostriction.

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