CN108373327B - Nickel-zinc-cerium ferrite soft magnetic material and preparation method thereof - Google Patents
Nickel-zinc-cerium ferrite soft magnetic material and preparation method thereof Download PDFInfo
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Abstract
The invention discloses a nickel-zinc-cerium ferrite soft magnetic material and a preparation method thereof, and the nickel-zinc-cerium ferrite soft magnetic material comprises the following operation steps of 1) Ni according to a stoichiometric ratio0.4Zn0.6‑xCexFe2O4Dissolving corresponding nickel nitrate, zinc nitrate and ferric nitrate in deionized water, and preparing NiZnCe ferrite nano powder according to a Sol-gel self-propagating powder method; 2) adding the NiZnCe ferrite nano powder obtained in the step 1) into a polyvinyl alcohol aqueous solution with the concentration of 6-8% for granulation, pressing the obtained granules into an annular sample, and sintering the annular sample at 950-1100 ℃ for 2-5h to obtain the NiZnCe ferrite soft magnetic material. The technical proposal is that the prepared nickel-zinc-cerium ferrite soft magnetic material is added with Ce3+Ion, Ce3+The radius of the ferrite is larger, the ferrite affects the original ion distribution of the nickel-zinc-cerium ferrite, the grain size of the nickel-zinc-cerium ferrite is refined, the initial permeability can reach 174, the Curie temperature is higher than 330 ℃, and the ferrite has good electromagnetic performance.
Description
Technical Field
The invention relates to the technical field of soft magnetic ferrite materials, in particular to a nickel-zinc-cerium ferrite soft magnetic material and a preparation method thereof.
Background
The soft magnetic ferrite is widely applied to various electronic equipment such as communication, computers, power supplies and the like, is a very important basic functional material in the electronic information industry, and along with the continuous improvement of the precision and the stability of the electronic equipment, most of the current whole machine systems are usually high in assembly density due to small volume requirements, obvious temperature gradient phenomenon exists in the system, and the environmental temperatures of parts at different positions are greatly different, so that higher requirements are provided for the temperature stability of the performance of the ferrite material. The magnetic properties of ferrite materials are not only dependent on the crystal structure, but also influenced by the microscopic morphology and the distribution of magnetic ions in the crystal structure.
The prior NiZn ferrite material has poor temperature stability due to ion distribution, microstructure, crystal defects and other reasons.
Based on the above, a nickel-zinc-cerium ferrite soft magnetic material and a preparation method thereof are researched and designed.
Disclosure of Invention
The technical problem to be solved by the invention is as follows: the technical problems that the temperature stability of the existing ferrite material is poor in the using process, the material is applied to parts, the difference of different temperatures of the parts is large in environmental performance, even the parts cannot be used, and the like are solved.
The invention is realized by the following technical scheme:
a nickel zinc cerium ferrite soft magnetic material has a nominal general formula of Ni0.4Zn0.6-xCexFe2O4Wherein x is more than 0 and less than or equal to 0.20.
A preparation method of a nickel-zinc-cerium ferrite soft magnetic material comprises the following operation steps,
1) preparing NiZnCe ferrite nano powder by a compound containing Ce, Ni, Zn and Fe according to a Sol-gel self-propagating powder method;
2) adding the NiZnCe ferrite nano powder obtained in the step 1) into a polyvinyl alcohol aqueous solution with the concentration of 6-8% for granulation, pressing the obtained granules into an annular sample, and sintering the annular sample at 950-1100 ℃ for 2-5h to obtain the NiZnCe ferrite soft magnetic material.
Wherein, the concrete method for preparing the NiZnCe ferrite nano powder by adopting the Sol-gel self-propagating powder method in the step 1) comprises the following steps: in Ni0.4Zn0.6-xCexFe2O4In deionized water solution, according to the mass ratio of 3: 1 adding citric acid, sealing, and magnetically stirring at 90 ℃ for 3 hours to obtain a brownish green precursor solution; cooling the precursor solution to room temperature, and adjusting the pH value to 7 by using ammonia water; and drying the solution with the pH value of 7 at 95 ℃ to form dry gel, finally generating fluffy tree-like shape from the dry gel through self-propagating combustion, and grinding to obtain the NiZnCe ferrite nano powder.
Magnetic element ion Ce3+Rare earth ion Ce is introduced into the existing NiZn ferrite powder3+Is large in radius and is influenced by space effect, Ce3+Will preferentially enter the octahedral position (position B). Ce3+The 4f electron layer provides an ionic magnetic moment, which is a magnetic ion. Ce3+Entering ferrite crystal lattice, and enhancing the super exchange effect of magnetic ions between tetrahedron (A site) and octahedron (B site) by influencing the original ion distribution of the nickel-zinc-cerium ferrite, thereby improving the Curie temperature of the material.
Adding magnetic element ion Ce3+In the process of preparing NiZn ferrite nano powder, the prepared ferrite nano powder has uniform components, extremely small particle size, large specific surface area and high chemical activity, can obviously reduce the sintering temperature of the material under the condition of not adding additional additives, can refine the microscopic grain size of the ferrite material, improves the compactness and uniformity of the ferrite material, and improves the initial permeability and Curie temperature of the material.
The following table is Ni0.4Zn0.6-xCexFe2O4Ferrite nano-meterPowder grain size (x is different in value):
TABLE 1 Ni0.4Zn0.6-xCexFe2O4Ferrite nanopowder grain size
According to the technical scheme, the NiZnCe ferrite nano powder is sintered at a certain temperature and for a certain time by adopting a solid-phase sintering method, so that the crystal structure of the formed NiZnCe ferrite material is more complete, and Ce ions are distributed more uniformly, the super exchange effect among magnetic ions is improved to a certain extent, and the Curie temperature of the NiZnCe ferrite material is further improved.
The preparation method of the sol-gel self-propagating powder in the technical scheme is combined with a solid-phase sintering method, wherein the sol-gel method is one of the main methods for preparing the nano powder, and the technology forms a metal complex compound by a complexing agent and metal ions and then forms polymer gel by crosslinking. In the gel, Ce ions are uniformly distributed, and in the process of removing the gelling agent through heat treatment, the Ce ions are subjected to oxidation reaction to form the nano oxide material.
The compounds of Ce, Ni, Zn and Fe as raw materials in the invention can be chloride, nitrate, hydroxide, carbonate, organic acid salt or alkoxide, the salts are dissolved in deionized water solution and generate complexation reaction with added citric acid to grow citrate of corresponding metal elements, and the generated citrate is a chelate between metal ions and citrate, so that the stability is high. Ammonia water is introduced into the reaction of the compound containing the metal elements forming the ferrite and citric acid to adjust the pH value to be neutral to alkalescence, so that the acidic compound generated in the reaction process is consumed, and the complete generation reaction of the citric acid complex of metal ions is promoted.
In the technical scheme, the ammonia water is adopted to adjust the pH value, compared with a method for adjusting the pH value by introducing ammonia gas, the method does not need complex ventilation equipment in operation and avoids secondary pollution of the prepared solution caused by the fact that a ventilation pipe enters the solution, reduces the influence of impurities or pollutants on the accuracy of a material formula, further improves the consistency of material performance, and can avoid harm or environmental pollution caused by the volatilized ammonia gas to a human body by introducing the ammonia water.
Further, the solid-phase sintering method in the step 2) comprises the following specific operation steps: adding 6-8% polyvinyl alcohol aqueous solution for granulation to bond the nano powder together, preventing cracking in the forming process, pressing the obtained granules into an annular sample to facilitate measuring the initial permeability of the material, insulating and sintering the annular sample at 950-1100 ℃ for 2-5h to further perform solid phase reaction on the ferrite nano powder, and finally obtaining the NiZnCe ferrite soft magnetic block material.
Further, in order to better implement the present invention, in the step 2), the pressing is specifically performed by pressing the NiZnCe nanoparticles into a ring-shaped sample with a mold under a pressure of 60 MPa.
Furthermore, in order to better realize the invention, the specification of the NiZnCe nanopowder annular sample is phi 12mm multiplied by phi 8mm multiplied by h5 mm.
Further, in order to better implement the present invention, in the step 1), pure Ni (NO) is analyzed by dissolving into deionized water3)2·6H2O，Zn(NO3)2·6H2O，Ce(NO3)3·6H2O and Fe (NO)3)3·9H2O is taken as a raw material and is expressed by a chemical formula of Ni0.4Zn0.6-xCexFe2O4And x is more than 0 and less than or equal to 0.20, and weighing and proportioning.
The invention has the following advantages and beneficial effects:
1) in the technical scheme, the Sol-gel self-propagating powder preparation method is combined with a solid-phase sintering method to prepare the nickel-zinc-cerium ferrite soft magnetic material, and the magnetic Ce ions are used for replacing non-magnetic ions to prepare the soft magnetic ferrite material with excellent electromagnetic performance and extremely high Curie temperature, so that the method has wide application scenes.
2) The Ni-Zn-Ce ferrite soft magnetic material prepared in the technical scheme is added with Ce3+Ion, Ce3+The radius of the NiZn ferrite is larger, the original ion distribution of the NiZn cerium ferrite is influenced, the grain size of the NiZn cerium ferrite is refined, and the NiZn cerium ferrite has good electromagnetic performance.
Drawings
The accompanying drawings, which are included to provide a further understanding of the embodiments of the invention and are incorporated in and constitute a part of this application, illustrate embodiment(s) of the invention and together with the description serve to explain the principles of the invention. In the drawings:
FIG. 1 is an X-ray diffraction pattern of NiZnCe ferrite materials prepared in examples 1-4.
Detailed Description
In order to make the objects, technical solutions and advantages of the present invention more apparent, the present invention is further described in detail below with reference to examples, and the exemplary embodiments and descriptions thereof are only used for explaining the present invention and are not used as limitations of the present invention.
Example 1:
a preparation method of a nickel-zinc-cerium ferrite soft magnetic material comprises the following operation steps:
1) ingredients
To analyze pure Ni (NO)3)2·6H2O，Zn(NO3)2·6H2O，Ce(NO3)3·6H2O and Fe (NO)3)3·9H2O is taken as a raw material and is expressed by a chemical formula of Ni0.4Zn0.55Ce0.05Fe2O4Weighing and proportioning;
2) preparation of
In stoichiometric ratio of Ni0.4Zn0.55Ce0.05Fe2O4Dissolving nitrate in deionized water, and mixingAfter the mixture is dissolved, a solution with the concentration of 0.15mol/L is formed; adding citric acid with the amount ratio of citric acid to nitrate substance being 3 into the prepared solution, then sealing, and magnetically stirring for 3 hours at 90 ℃ to obtain a clear brownish green precursor solution; cooling the precursor solution to room temperature, adding ammonia water into the precursor solution, and adjusting the pH value of the precursor solution to 7; drying the solution with the pH value of 7 at 95 ℃ to form dry gel, finally generating fluffy tree-like shape from the dry gel through self-propagating combustion, and grinding to obtain NiZnCe ferrite nano powder; adding the obtained NiZnCe ferrite nano powder into a polyvinyl alcohol aqueous solution with the concentration of 8 percent for granulation; the resulting pellets were molded into a ring-shaped sample (Φ 12mm × Φ 8mm × h5mm) with a mold under a pressure of 60 MPa; and (3) carrying out heat preservation sintering on the annular sample at 950 ℃ for 5h to obtain the ferrite material.
The general formula of the soft magnetic material of nickel-zinc-cerium ferrite prepared by the embodiment is as follows: ni0.4Zn0.55Ce0.05Fe2O4Wherein x is 0.05.
The curie temperature of the soft magnetic material of nickel-zinc-cerium ferrite prepared by the embodiment is 208 ℃, and the magnetic permeability of the soft magnetic material is 124.
Example 2:
a preparation method of a nickel-zinc-cerium ferrite soft magnetic material comprises the following operation steps:
1) ingredients
To analyze pure Ni (NO)3)2·6H2O，Zn(NO3)2·6H2O，Ce(NO3)3·6H2O and Fe (NO)3)3·9H2O is taken as a raw material and is expressed by a chemical formula of Ni0.4Zn0.50Ce0.10Fe2O4Weighing and proportioning;
2) preparation of
In stoichiometric ratio of Ni0.4Zn0.50Ce0.10Fe2O4Dissolving nitrate in a certain amount of deionized water, and then fully mixing and dissolving to form a solution with the concentration of 0.15 mol/L; adding citric acid to the prepared solution at a citric acid to nitrate substance ratio of 3, sealing, and magnetically treating at 90 deg.CStirring for 3 hours to obtain a clear brown green precursor solution; cooling the precursor solution to room temperature, adding ammonia water into the precursor solution, and adjusting the pH value of the precursor solution to 7; drying the solution with the pH value of 7 at 95 ℃ to form dry gel, finally generating fluffy tree-like shape from the dry gel through self-propagating combustion, and grinding to obtain NiZnCe ferrite nano powder; adding the obtained nano powder into a 7% polyvinyl alcohol aqueous solution for granulation; the resulting pellets were molded into a ring-shaped sample (Φ 12mm × Φ 8mm × h5mm) with a mold under a pressure of 60 MPa; and (3) carrying out heat preservation sintering on the annular sample at 1100 ℃ for 3h to obtain the ferrite material.
The general formula of the soft magnetic material of nickel-zinc-cerium ferrite prepared by the embodiment is as follows: ni0.4Zn0.50Ce0.10Fe2O4Wherein x is 0.10.
The curie temperature of the soft magnetic material of nickel-zinc-cerium ferrite prepared by the embodiment is 238 ℃, and the magnetic permeability is 140.
Example 3:
a preparation method of a nickel-zinc-cerium ferrite soft magnetic material comprises the following operation steps:
1) ingredients
To analyze pure Ni (NO)3)2·6H2O，Zn(NO3)2·6H2O，Ce(NO3)3·6H2O and Fe (NO)3)3·9H2O is taken as a raw material and is expressed by a chemical formula of Ni0.4Zn0.45Ce0.15Fe2O4Weighing and proportioning;
2) preparation:
in stoichiometric ratio of Ni0.4Zn0.45Ce0.15Fe2O4Dissolving nitrate in a certain amount of deionized water, and then fully mixing and dissolving to form a solution with the concentration of 0.15 mol/L; adding citric acid with the amount ratio of citric acid to nitrate substance being 3 into the prepared solution, then sealing, and magnetically stirring for 3 hours at 90 ℃ to obtain a clear brownish green precursor solution; cooling the precursor solution to room temperature, adding ammonia water into the precursor solution, and adjusting the pH value of the precursor solution to 7; the solution with pH value of 7 is processed at 95 DEG CDrying to form dry gel, finally generating fluffy tree-like shape from the dry gel through self-propagating combustion, and obtaining NiZnCe ferrite nano powder after crushing; adding the obtained nano powder into a polyvinyl alcohol aqueous solution with the concentration of 6% for granulation; and pressing the obtained granules by using a mould under the pressure of 60MPa to prepare an annular sample (with the specification of phi 12mm multiplied by phi 8mm multiplied by h5mm), and carrying out heat preservation and sintering on the annular sample at the temperature of 1000 ℃ for 2-5h to obtain the ferrite material.
The general formula of the soft magnetic material of nickel-zinc-cerium ferrite prepared by the embodiment is as follows: ni0.4Zn0.45Ce0.15Fe2O4Wherein x is 0.15.
The chemical formula of the soft magnetic Ni-Zn-Ce ferrite material prepared by the embodiment is Ni0.4Zn0.45Ce0.15Fe2O4The Curie temperature is 290 ℃ and the magnetic permeability is 149.
Example 4:
a preparation method of a nickel-zinc-cerium ferrite soft magnetic material comprises the following operation steps:
1) ingredients
To analyze pure Ni (NO)3)2·6H2O，Zn(NO3)2·6H2O，Ce(NO3)3·6H2O and Fe (NO)3)3·9H2O is taken as a raw material and is expressed by a chemical formula of Ni0.4Zn0.40Ce0.20Fe2O4Weighing and proportioning;
2) preparation of
In stoichiometric ratio of Ni0.4Zn0.40Ce0.20Fe2O4Dissolving nitrate in a certain amount of deionized water, and then fully mixing and dissolving to form a solution with the concentration of 0.15 mol/L; adding citric acid with the amount ratio of citric acid to nitrate substance being 3 into the prepared solution, then sealing, and magnetically stirring for 3 hours at 90 ℃ to obtain a clear brownish green precursor solution; cooling the precursor solution to room temperature, adding ammonia water into the precursor solution, and adjusting the pH value of the precursor solution to 7; drying the solution with the pH value of 7 at the temperature of 95 ℃ to form dry gel, and finally generating the awning by the self-propagating combustion of the dry gelPine tree shape, grinding to obtain NiZnCe ferrite nano powder; adding the obtained nano powder into 7.5 percent polyvinyl alcohol aqueous solution for granulation; pressing the obtained pellets into an annular sample (with the specification of phi 12mm multiplied by phi 8mm multiplied by h5mm) by a die under the pressure of 60 MPa; and (3) carrying out heat preservation sintering on the annular sample at 1050 ℃ for 3h to obtain the ferrite material.
The chemical formula of the soft magnetic material of nickel-zinc-cerium ferrite prepared by the embodiment is as follows: ni0.4Zn0.40Ce0.20Fe2O4Where x is 0.20, its curie temperature is 331 ℃, and its magnetic permeability is 174.
The NiZnCe ferrite material prepared in the embodiment is sintered for 3 hours at 1050 ℃, and a curve for measuring the change of the magnetic permeability of the ferrite material along with the temperature is shown in figure 1. When the Ce content is 0.20, the initial permeability is 174, and the Curie temperature is more than 330 ℃.
Examples 1-4 the chemical formula of the NiZnCe soft magnetic ferrite material prepared in the examples is Ni0.4Zn0.6-xCexFe2O4Wherein x is more than 0 and less than or equal to 0.20, the magnetic permeability of the material is 124-174, and the Curie temperature is 238-331 ℃.
Comparative example 1:
a preparation method of a nickel-zinc-cerium ferrite soft magnetic material comprises the following operation steps:
1) ingredients
To analyze pure Ni (NO)3)2·6H2O，Zn(NO3)2·6H2O，Ce(NO3)3·6H2O and Fe (NO)3)3·9H2O is taken as a raw material and is expressed by a chemical formula of Ni0.4Zn0.6Fe2O4Weighing and proportioning;
2) preparation of
In stoichiometric ratio of Ni0.4Zn0.6Fe2O4Dissolving nitrate in deionized water, mixing and dissolving to obtain the product with concentration of 0.15 mol.L-1The solution of (1); adding citric acid to the prepared solution at a citric acid to nitrate substance ratio of 3, sealing, and magnetically treating at 90 deg.CStirring for 3 hours to obtain a clear brown green precursor solution; cooling the precursor solution to room temperature, adding ammonia water into the precursor solution, and adjusting the pH value of the precursor solution to 7; drying the solution with the pH value of 7 at 95 ℃ to form dry gel, finally generating fluffy tree-like shape from the dry gel through self-propagating combustion, and grinding to obtain NiZnCe ferrite nano powder;
and adding the obtained NiZnCe ferrite nano powder into a polyvinyl alcohol aqueous solution with the concentration of 6% for granulation, pressing the obtained granules into an annular sample by using a mould under the pressure of 60MPa, and carrying out heat preservation and sintering on the annular sample at 950 ℃ for 2h to obtain the ferrite material.
Wherein the specifications of the annular sample obtained by pressing are phi 12mm multiplied by phi 8mm multiplied by h5 mm.
The general formula of the soft magnetic material of nickel-zinc-cerium ferrite prepared in the embodiment is as follows: ni0.4Zn0.6Fe2O4Wherein x is 0.00.
The curie temperature of the soft magnetic material of nickel-zinc-cerium ferrite prepared in the example is 187 ℃, and the magnetic permeability of the soft magnetic material is 120.
Examples 1-4 in comparison with comparative examples, examples 1-4 were prepared by adding Ce3+The method has the advantages of influencing the original ion distribution of the nickel-zinc-cerium ferrite, changing the grain diameter of the nickel-zinc-cerium ferrite and enhancing the Curie temperature and the magnetic conductivity of the soft magnetic material of the nickel-zinc-cerium ferrite.
The nickel-zinc-cerium ferrite soft magnetic material prepared in the embodiments 1 to 4 is applied to the production of electronic products, the temperature stability of the performance of the ferrite material is not affected by the internal temperature gradient of the electronic products, and the temperature of parts at different positions is greatly improved.
The above-mentioned embodiments are intended to illustrate the objects, technical solutions and advantages of the present invention in further detail, and it should be understood that the above-mentioned embodiments are merely exemplary embodiments of the present invention, and are not intended to limit the scope of the present invention, and any modifications, equivalent substitutions, improvements and the like made within the spirit and principle of the present invention should be included in the scope of the present invention.
Claims (4)
1. A preparation method of a nickel-zinc-cerium ferrite soft magnetic material is characterized by comprising the following operation steps,
1) preparing NiZnCe ferrite nano powder by a compound containing Ce, Ni, Zn and Fe according to a Sol-gel self-propagating powder method;
2) preparing the NiZnCe ferrite nano powder obtained in the step 1) into a NiZnCe ferrite soft magnetic material according to a solid-phase sintering method;
the nominal general formula of the nickel-zinc-cerium ferrite soft magnetic material is Ni0.4Zn0.6-xCexFe2O4Wherein x is more than 0 and less than or equal to 0.20;
in the step 1), the raw material is dissolved in deionized water to analyze pure Ni (NO)3)2·6H2O，Zn(NO3)2·6H2O，Ce(NO3)3·6H2O and Fe (NO)3)3·9H2O is taken as a raw material and is expressed by a chemical formula of Ni0.4Zn0.6-xCexFe2O4，0＜xWeighing and proportioning at most 0.20;
the solid-phase sintering method in the step 2) comprises the following specific operation steps: adding 6-8% polyvinyl alcohol aqueous solution for granulation, pressing the obtained granules into an annular sample, and sintering the annular sample at 950-1100 ℃ for 2-5h to obtain the NiZnCe ferrite soft magnetic material.
2. The method for preparing the nickel-zinc-cerium ferrite soft magnetic material according to claim 1, wherein the specific method for preparing the NiZnCe ferrite nano powder by adopting the Sol-gel self-propagating powder method in the step 1) comprises the following steps: in Ni0.4Zn x0.6-Ce x Fe2O4In deionized water solution, according to the mass ratio of 3: 1 adding citric acid, sealing, and magnetically stirring at 90 ℃ for 3 hours to obtain a brownish green precursor solution; cooling the precursor solution to room temperature, and adjusting the pH value to 7 by using ammonia water; drying the solution with the pH value of 7 at 95 ℃ to form dry gel, and finally, enabling the dry gel to generate fluffiness through self-propagating combustionAnd grinding the mixture to obtain NiZnCe ferrite nano powder.
3. The method for preparing a ni-zn-ce-ferrite soft magnetic material according to claim 1, wherein in the step 2), the pressing is performed by pressing the NiZnCe nano-particles into a ring sample with a die under a pressure of 60 MPa.
4. The method for preparing a nickel-zinc-cerium ferrite soft magnetic material according to claim 1, wherein the NiZnCe nanopowder annular sample has the specification of phi 12mm x phi 8mm x h5 mm.
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