CN117623409A - NiZn ferrite powder and chemical coprecipitation-microwave heat treatment synthesis method thereof - Google Patents
NiZn ferrite powder and chemical coprecipitation-microwave heat treatment synthesis method thereof Download PDFInfo
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- 229910000859 α-Fe Inorganic materials 0.000 title claims abstract description 54
- 229910003962 NiZn Inorganic materials 0.000 title claims abstract description 49
- 238000010438 heat treatment Methods 0.000 title claims abstract description 35
- 239000000843 powder Substances 0.000 title claims abstract description 28
- 239000000126 substance Substances 0.000 title claims abstract description 12
- 238000001308 synthesis method Methods 0.000 title abstract description 5
- 239000011858 nanopowder Substances 0.000 claims abstract description 33
- 229910052751 metal Inorganic materials 0.000 claims abstract description 27
- 239000002184 metal Substances 0.000 claims abstract description 25
- 239000002243 precursor Substances 0.000 claims abstract description 18
- 239000012266 salt solution Substances 0.000 claims abstract description 15
- 238000000227 grinding Methods 0.000 claims abstract description 14
- 238000007873 sieving Methods 0.000 claims abstract description 13
- 239000012716 precipitator Substances 0.000 claims abstract description 12
- 239000000047 product Substances 0.000 claims abstract description 12
- 238000001035 drying Methods 0.000 claims abstract description 10
- 150000003839 salts Chemical class 0.000 claims abstract description 9
- 238000006243 chemical reaction Methods 0.000 claims abstract description 7
- 239000002244 precipitate Substances 0.000 claims abstract description 6
- 239000002994 raw material Substances 0.000 claims abstract description 6
- 238000005303 weighing Methods 0.000 claims abstract description 6
- 230000002194 synthesizing effect Effects 0.000 claims abstract description 5
- 238000000034 method Methods 0.000 claims description 34
- 238000003756 stirring Methods 0.000 claims description 18
- HEMHJVSKTPXQMS-UHFFFAOYSA-M Sodium hydroxide Chemical group [OH-].[Na+] HEMHJVSKTPXQMS-UHFFFAOYSA-M 0.000 claims description 15
- XEEYBQQBJWHFJM-UHFFFAOYSA-N iron Substances [Fe] XEEYBQQBJWHFJM-UHFFFAOYSA-N 0.000 claims description 12
- 229910021645 metal ion Inorganic materials 0.000 claims description 12
- VEQPNABPJHWNSG-UHFFFAOYSA-N Nickel(2+) Chemical compound [Ni+2] VEQPNABPJHWNSG-UHFFFAOYSA-N 0.000 claims description 6
- PTFCDOFLOPIGGS-UHFFFAOYSA-N Zinc dication Chemical compound [Zn+2] PTFCDOFLOPIGGS-UHFFFAOYSA-N 0.000 claims description 6
- 229910052742 iron Inorganic materials 0.000 claims description 6
- -1 iron ions Chemical class 0.000 claims description 6
- 229910001453 nickel ion Inorganic materials 0.000 claims description 6
- KWYUFKZDYYNOTN-UHFFFAOYSA-M Potassium hydroxide Chemical compound [OH-].[K+] KWYUFKZDYYNOTN-UHFFFAOYSA-M 0.000 claims description 5
- 238000004321 preservation Methods 0.000 claims description 4
- 238000000926 separation method Methods 0.000 claims description 4
- 230000035484 reaction time Effects 0.000 claims description 3
- 230000000630 rising effect Effects 0.000 claims description 2
- 238000000967 suction filtration Methods 0.000 claims description 2
- 239000002245 particle Substances 0.000 abstract description 23
- 230000015572 biosynthetic process Effects 0.000 abstract description 9
- 238000003786 synthesis reaction Methods 0.000 abstract description 8
- 239000000243 solution Substances 0.000 description 16
- 239000008367 deionised water Substances 0.000 description 12
- 229910021641 deionized water Inorganic materials 0.000 description 12
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Chemical compound O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 description 12
- 239000000463 material Substances 0.000 description 11
- 238000000975 co-precipitation Methods 0.000 description 10
- 239000012065 filter cake Substances 0.000 description 8
- XIOUDVJTOYVRTB-UHFFFAOYSA-N 1-(1-adamantyl)-3-aminothiourea Chemical compound C1C(C2)CC3CC2CC1(NC(=S)NN)C3 XIOUDVJTOYVRTB-UHFFFAOYSA-N 0.000 description 7
- SZQUEWJRBJDHSM-UHFFFAOYSA-N iron(3+);trinitrate;nonahydrate Chemical compound O.O.O.O.O.O.O.O.O.[Fe+3].[O-][N+]([O-])=O.[O-][N+]([O-])=O.[O-][N+]([O-])=O SZQUEWJRBJDHSM-UHFFFAOYSA-N 0.000 description 7
- AOPCKOPZYFFEDA-UHFFFAOYSA-N nickel(2+);dinitrate;hexahydrate Chemical compound O.O.O.O.O.O.[Ni+2].[O-][N+]([O-])=O.[O-][N+]([O-])=O AOPCKOPZYFFEDA-UHFFFAOYSA-N 0.000 description 7
- 230000008569 process Effects 0.000 description 7
- PXHVJJICTQNCMI-UHFFFAOYSA-N nickel Substances [Ni] PXHVJJICTQNCMI-UHFFFAOYSA-N 0.000 description 6
- 239000011701 zinc Substances 0.000 description 6
- 230000000052 comparative effect Effects 0.000 description 5
- 238000001354 calcination Methods 0.000 description 4
- 238000009826 distribution Methods 0.000 description 4
- 239000000706 filtrate Substances 0.000 description 4
- 238000001914 filtration Methods 0.000 description 4
- 230000005415 magnetization Effects 0.000 description 4
- 230000007935 neutral effect Effects 0.000 description 4
- 238000002441 X-ray diffraction Methods 0.000 description 3
- 239000012071 phase Substances 0.000 description 3
- 238000000498 ball milling Methods 0.000 description 2
- 238000004140 cleaning Methods 0.000 description 2
- 239000013078 crystal Substances 0.000 description 2
- 238000002955 isolation Methods 0.000 description 2
- 238000004519 manufacturing process Methods 0.000 description 2
- 238000002156 mixing Methods 0.000 description 2
- 238000012986 modification Methods 0.000 description 2
- 230000004048 modification Effects 0.000 description 2
- 238000005457 optimization Methods 0.000 description 2
- 230000035699 permeability Effects 0.000 description 2
- 238000001556 precipitation Methods 0.000 description 2
- 230000001105 regulatory effect Effects 0.000 description 2
- 238000001878 scanning electron micrograph Methods 0.000 description 2
- 238000003746 solid phase reaction Methods 0.000 description 2
- 229910052596 spinel Inorganic materials 0.000 description 2
- 239000011029 spinel Substances 0.000 description 2
- 239000007858 starting material Substances 0.000 description 2
- 238000005406 washing Methods 0.000 description 2
- 229910002651 NO3 Inorganic materials 0.000 description 1
- 230000004913 activation Effects 0.000 description 1
- 230000009286 beneficial effect Effects 0.000 description 1
- 238000009792 diffusion process Methods 0.000 description 1
- 239000012467 final product Substances 0.000 description 1
- 239000012535 impurity Substances 0.000 description 1
- 239000006247 magnetic powder Substances 0.000 description 1
- NHNBFGGVMKEFGY-UHFFFAOYSA-N nitrate group Chemical group [N+](=O)([O-])[O-] NHNBFGGVMKEFGY-UHFFFAOYSA-N 0.000 description 1
- 230000001376 precipitating effect Effects 0.000 description 1
- 238000005245 sintering Methods 0.000 description 1
Classifications
-
- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01G—COMPOUNDS CONTAINING METALS NOT COVERED BY SUBCLASSES C01D OR C01F
- C01G53/00—Compounds of nickel
- C01G53/006—Compounds containing, besides nickel, two or more other elements, with the exception of oxygen or hydrogen
-
- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01P—INDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS
- C01P2002/00—Crystal-structural characteristics
- C01P2002/70—Crystal-structural characteristics defined by measured X-ray, neutron or electron diffraction data
- C01P2002/72—Crystal-structural characteristics defined by measured X-ray, neutron or electron diffraction data by d-values or two theta-values, e.g. as X-ray diagram
-
- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01P—INDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS
- C01P2004/00—Particle morphology
- C01P2004/01—Particle morphology depicted by an image
- C01P2004/03—Particle morphology depicted by an image obtained by SEM
-
- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01P—INDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS
- C01P2004/00—Particle morphology
- C01P2004/30—Particle morphology extending in three dimensions
- C01P2004/32—Spheres
-
- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01P—INDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS
- C01P2004/00—Particle morphology
- C01P2004/51—Particles with a specific particle size distribution
-
- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01P—INDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS
- C01P2004/00—Particle morphology
- C01P2004/60—Particles characterised by their size
- C01P2004/64—Nanometer sized, i.e. from 1-100 nanometer
-
- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01P—INDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS
- C01P2006/00—Physical properties of inorganic compounds
- C01P2006/42—Magnetic properties
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- Chemical & Material Sciences (AREA)
- Organic Chemistry (AREA)
- Inorganic Chemistry (AREA)
- Compounds Of Iron (AREA)
- Soft Magnetic Materials (AREA)
- Inorganic Compounds Of Heavy Metals (AREA)
Abstract
The invention discloses NiZn ferrite powder and a chemical coprecipitation-microwave heat treatment synthesis method thereof, comprising the following steps: (1) Weighing soluble metal salt raw materials according to the stoichiometric ratio of each component in the NiZn ferrite, and preparing mixed metal salt solution; (2) Adding the mixed metal salt solution in the step (1) into a precipitator, and separating after reaction to obtain a precipitate; (3) Drying the precipitate in the step (2) to constant weight, grinding and sieving to obtain precursor powder; (4) And (3) carrying out microwave heat treatment on the precursor powder obtained in the step (3), and grinding and sieving the heat treated product to obtain the NiZn ferrite nano powder. According to the invention, a microwave treatment is adopted to construct an environment for synthesizing a target phase and rapidly growing particles, so that one-step generation and rapid synthesis of a target product are promoted, the NiZn ferrite nano powder with high magnetic conductivity is obtained, and adhesion caused by conventional heat treatment of the particles is avoided.
Description
Technical Field
The invention relates to a magnetic functional material, in particular to NiZn ferrite powder and a chemical coprecipitation-microwave heat treatment synthesis method thereof.
Background
The spinel type NiZn ferrite with soft magnetic property has the advantages of light weight, thin material, capability of being processed into various shapes according to requirements, and the like, so that the spinel type NiZn ferrite has great advantages in the field of high-frequency materials, has higher magnetic permeability and lower coercive force, and is often used as a raw material for manufacturing the NFC magnetic isolation sheet applied to 13.56 MHz.
The method commonly used for synthesizing NiZn ferrite nano powder is a solid phase reaction method, which generally takes oxide as a starting material, and the target product is synthesized by ball milling and mixing. The problem is that the loss of materials and the introduction of impurities in the ball milling process often lead to the deviation of two-phase components of the final product, and in addition, the heat treatment synthesis process is limited by the uniformity of the mixed materials, so that the magnetic powder with good magnetic permeability and coercivity is difficult to obtain.
In order to solve the problems caused by the solid phase reaction method, researchers have developed a coprecipitation method, which generally uses soluble metal salts as raw materials, uses a precipitant to perform a coprecipitation reaction to obtain a precursor, and finally obtains ferrite powder through drying, grinding and high-temperature sintering. However, in the heat treatment process, the high-temperature environment for a long time promotes the formation of phases and simultaneously promotes the inter-particle diffusion, so that particles are adhered.
Disclosure of Invention
Aiming at the problem of particle adhesion caused by a traditional heat treatment method in the process of synthesizing NiZn ferrite powder by a coprecipitation method, the invention provides the NiZn ferrite powder and a chemical coprecipitation-microwave heat treatment synthesis method thereof.
In order to achieve the above purpose, the present invention provides a method for synthesizing NiZn ferrite nano powder by chemical coprecipitation-microwave heat treatment process, comprising the following steps:
(1) Weighing soluble metal salt raw materials according to the stoichiometric ratio of each component in the NiZn ferrite, and preparing mixed metal salt solution;
(2) Adding the mixed metal salt solution in the step (1) into a precipitator, and separating after reaction to obtain a precipitate;
(3) Drying the precipitate in the step (2) to constant weight, grinding and sieving to obtain precursor powder;
(4) And (3) carrying out microwave heat treatment on the precursor powder obtained in the step (3), and grinding and sieving the heat treated product to obtain the NiZn ferrite nano powder.
In the technical scheme, a soluble metal salt is taken as a starting material to prepare a starting metal solution; adopting a precipitator to realize metal ion coprecipitation to obtain a precursor with uniformly dispersed metal elements; and then, carrying out microwave heat treatment to obtain the NiZn ferrite nano powder. The precipitant ensures that the metal elements are distributed in the precursor powder to be uniform in height; the system calcining temperature is regulated, microwave treatment is adopted to replace traditional heat treatment, a target phase synthesis and particle rapid growth environment is constructed, one-step generation and rapid synthesis of a target product are promoted, the particle structure of the target product is regulated and controlled, the NiZn ferrite nano powder with high magnetic conductivity is obtained, and adhesion caused by traditional heat treatment of particles is avoided. In addition, the target product generated by adopting the microwave heat treatment method has small crystal grains and good consistency.
The soluble metal salt is preferably nitrate.
Preferably, in the step (1), the concentration of nickel ions in the mixed metal salt solution is 0.125-0.25 mol/L, the concentration of zinc ions is 0.125-0.25 mol/L, and the concentration of iron ions is 0.5-1 mol/L.
Preferably, in the step (2), the precipitant is sodium hydroxide or potassium hydroxide solution, and the concentration is 4.8-5.0 mol/L.
In the technical scheme, the concentration of the metal ions and the precipitant is proper, so that the precipitation reaction can be orderly carried out.
Further preferably, the amount of the precipitant is 20% -50% excess of the sum of the amounts of the precipitated metal ion species.
In the above technical solution, the excessive precipitant can enable the metal ions to be sufficiently precipitated so that the target product can be obtained later.
Preferably, in the step (2), the adding speed of the mixed metal salt solution is 40-50 ml/s, and the reaction time is 2-3 h.
In the above technical scheme, the proper adding speed and the sufficient reaction time are both used for sufficiently precipitating the metal ions.
Preferably, in step (2), the separation is performed by suction filtration.
Preferably, in the step (2), the mixed metal salt solution in the step (1) is added into the precipitant under the stirring condition, and separation is performed after the stirring reaction, wherein the stirring speed is 500-600 rpm.
Preferably, in the step (3), the temperature of the drying is 80-120 ℃.
Preferably, in the step (4), the conditions of the microwave heat treatment are as follows: the temperature rising rate is 75-80 ℃/min, the heat preservation temperature is 700-900 ℃, and the heat preservation time is 20-30 min.
The second aspect of the invention provides NiZn ferrite nano powder synthesized by the method.
Through the technical scheme, the invention has the following beneficial effects:
the invention combines the uniform mixing of the chemical coprecipitation metal ions and the control of the growth of the crystal by microwave heat treatment, and realizes the precise synthesis of the NiZn ferrite nano powder and the control of the grain structure by the technical means of temperature regulation, the optimization of the precipitant, the replacement of the traditional heat treatment by the microwave heat treatment and the like. Has the following advantages:
1. the invention combines chemical coprecipitation and microwave heat treatment technology, and solves the problems of accurate synthesis of NiZn ferrite nano powder and control of particle structure;
2. the invention designs the method which uses soluble metal salt as the initial raw material, and realizes the effective control of the consistency and uniformity of metal ion precipitation in the coprecipitation process through temperature adjustment, precipitant optimization and dosage control, so as to obtain precursor powder for further synthesis;
3. according to the invention, a microwave heat treatment method is used for replacing a traditional heat treatment method, and the characteristic of microwave rapid heating is utilized, so that the activation energy of particles is improved, the rapid growth of the particles is promoted, and the synthesis efficiency of NiZn ferrite nano powder is greatly improved;
4. the method has the advantages of simple and easy process, short time consumption, high single-time yield and easy industrialization, and meets the requirement of large amount of powder for manufacturing the NFC magnetic isolation sheet.
Drawings
FIG. 1 is an X-ray diffraction pattern of NiZn ferrite nano-powder synthesized in example 1 of the present invention;
FIG. 2 is a scanning electron microscope photograph of NiZn ferrite nano powder synthesized in example 1 of the present invention;
FIG. 3 is a graph showing the particle size distribution of NiZn ferrite nano powder synthesized in example 1 of the present invention;
FIG. 4 is a VSM curve of NiZn ferrite nano powder synthesized in example 1 of the present invention;
FIG. 5 is an X-ray diffraction pattern of the NiZn ferrite nano-powder synthesized in example 2 of the present invention;
FIG. 6 is a scanning electron microscope photograph of NiZn ferrite nano powder synthesized in example 2 of the present invention;
FIG. 7 is a graph showing the particle size distribution of NiZn ferrite nano powder synthesized in example 2 of the present invention;
FIG. 8 is a VSM curve of NiZn ferrite nano powder synthesized in example 2 of the present invention;
FIG. 9 is an X-ray diffraction pattern of the NiZn ferrite nano-powder synthesized in example 3 of the present invention;
FIG. 10 is a scanning electron microscope photograph of NiZn ferrite nano powder synthesized in example 3 of the present invention;
FIG. 11 is a graph showing the particle size distribution of NiZn ferrite nano powder synthesized in example 3 of the present invention;
FIG. 12 is a VSM curve of NiZn ferrite nano powder synthesized in example 3 of the present invention;
FIG. 13 is a scanning electron micrograph of the NiZn ferrite nano powder synthesized in the comparative example;
FIG. 14 is a graph showing the particle size distribution of the NiZn ferrite nano-powder synthesized in the comparative example;
FIG. 15 is a VSM curve of the NiZn ferrite nano-powder synthesized in the comparative example.
Detailed Description
The following describes specific embodiments of the present invention in detail with reference to examples. It should be understood that the detailed description and specific examples, while indicating and illustrating the invention, are not intended to limit the invention.
Example 1:
(1) According to Ni 0.5 Zn 0.5 Fe 2 O 4 Weighing nickel nitrate hexahydrate, zinc nitrate hexahydrate and ferric nitrate nonahydrate according to stoichiometric ratio, dissolving the nickel nitrate hexahydrate, the zinc nitrate hexahydrate and the ferric nitrate nonahydrate in deionized water, stirring and dissolving the materials until the materials are clear and transparent to obtain a mixed metal salt solution, wherein the concentration of nickel ions is 0.125 mol/L, the concentration of zinc ions is 0.125 mol/L, and the concentration of iron ions is 0.5 mol/L;
(2) Adding deionized water into sodium hydroxide serving as a precipitator to prepare a precipitator solution with the concentration of 4.8 mol/L;
(3) Rapidly adding the initial metal ion solution obtained in the step (1) into the precipitant solution obtained in the step (2) under the condition of rapid stirring, wherein the adding speed is controlled at 40 ml/s;
(4) Stirring and reacting for 2 hours, filtering and separating, and cleaning with deionized water until the filtrate is neutral to obtain a filter cake;
(5) The obtained filter cake is subjected to 80 o C, drying to constant weight, grinding and sieving to obtain precursor powder;
(6) Performing microwave heat treatment on the obtained precursor powder, calcining at 700 ℃ under microwave power of 6000W for 20min, grinding and sieving the heat treated product to obtain Ni 0.5 Zn 0.5 Fe 2 O 4 Ferrite powder.
The NiZn ferrite nano powder synthesized by adopting the chemical coprecipitation microwave heat treatment method has good crystallinity (shown in figure 1). The synthesized sample particles were spherical in shape from the sem photograph of fig. 2, with a particle size of about 60 nm and a standard deviation of 25nm (as shown in fig. 3). From the hysteresis loop of the sample, the hysteresis loop has small surrounding area, the hysteresis loss of the NiZn ferrite synthesized on the surface is small, the saturation magnetization of the sample is 60.2 emu/g, the coercivity is 25 Oe, and the NiZn ferrite has good magnetic performance (shown in figure 4).
Example 2:
(1) According to Ni 0.5 Zn 0.5 Fe 2 O 4 Weighing nickel nitrate hexahydrate, zinc nitrate hexahydrate and ferric nitrate nonahydrate according to stoichiometric ratio, dissolving the nickel nitrate hexahydrate, the zinc nitrate hexahydrate and the ferric nitrate nonahydrate in deionized water, stirring and dissolving the materials until the materials are clear and transparent to obtain a mixed metal salt solution, wherein the concentration of nickel ions is 0.25 mol/L, the concentration of zinc ions is 0.25 mol/L, and the concentration of iron ions is 1.0 mol/L;
(2) Potassium hydroxide is taken as a precipitator, deionized water is added, and a precipitator solution with the concentration of 5.0 mol/L is prepared;
(3) Rapidly adding the initial metal ion solution obtained in the step (1) into the precipitant solution obtained in the step (2) under the condition of rapid stirring, wherein the adding speed is controlled at 45 ml/second;
(4) Stirring and reacting for 3 hours, filtering and separating, and cleaning with deionized water until the filtrate is neutral to obtain a filter cake;
(5) The obtained filter cake is subjected to 120 o C, drying to constant weight, grinding and sieving to obtain precursor powder;
(6) Performing microwave heat treatment on the obtained precursor powder, calcining at 800 ℃ under microwave power of 6000W for 30min, grinding and sieving the heat treated product to obtain Ni 0.5 Zn 0.5 Fe 2 O 4 Ferrite powder.
The NiZn ferrite nano powder synthesized by adopting the chemical coprecipitation microwave heat treatment method has good crystallinity (shown in figure 5). The synthesized sample particles were spherical in shape as seen from the scanning electron microscope photograph of FIG. 6, and had a particle size of about 64nm and a standard deviation of 45nm (as shown in FIG. 7). From the hysteresis loop of the sample, the hysteresis loop has small surrounding area, the hysteresis loss of the NiZn ferrite synthesized on the surface is small, the saturation magnetization of the sample is 65.9 emu/g, the coercivity is 35.5 Oe, and the NiZn ferrite has good magnetic performance (shown in figure 8).
Example 3:
(1) According to Ni 0.5 Zn 0.5 Fe 2 O 4 Weighing nickel nitrate hexahydrate, zinc nitrate hexahydrate and ferric nitrate nonahydrate according to stoichiometric ratio, dissolving the nickel nitrate hexahydrate, the zinc nitrate hexahydrate and the ferric nitrate nonahydrate in deionized water, stirring and dissolving the materials until the materials are clear and transparent to obtain a mixed metal salt solution, wherein the concentration of nickel ions is 0.125 mol/L, the concentration of zinc ions is 0.125 mol/L, and the concentration of iron ions is 0.5 mol/L;
(2) Adding deionized water into sodium hydroxide serving as a precipitator to prepare a precipitator solution with the concentration of 4.8 mol/L;
(3) Rapidly adding the initial metal ion solution obtained in the step (1) into the precipitant solution under the condition of rapid stirring, wherein the adding speed is controlled at 50 ml/second;
(4) Stirring and reacting for 2.5 hours, filtering and separating, and washing with deionized water until the filtrate is neutral to obtain a filter cake;
(5) The obtained filter cake is subjected to 100 o C, drying to constant weight, grinding and sieving to obtain precursor powder;
(6) And carrying out microwave heat treatment on the obtained precursor powder, calcining at 900 ℃ and microwave power of 6000W for 25min, and grinding and sieving the heat treated product to obtain ferrite powder.
The NiZn ferrite nano powder synthesized by adopting the chemical coprecipitation microwave heat treatment method has good crystallinity (shown in figure 9). The synthesized sample particles were spherical in shape as seen from the scanning electron microscope photograph of fig. 10, and had a particle size of about 75nm and a standard deviation of 55nm (as shown in fig. 11). From the hysteresis loop of the sample, the area surrounded by the hysteresis loop is small, the hysteresis loss of the NiZn ferrite synthesized on the surface is small, the saturation magnetization of the sample is 66.9 emu/g, the coercivity is 29.5 Oe, and the sample has good magnetic performance (shown in figure 12).
Comparative example
(1) According to Ni 0.5 Zn 0.5 Fe 2 O 4 The stoichiometric ratio of the nickel nitrate hexahydrate, the zinc nitrate hexahydrate and the ferric nitrate nonahydrate are weighed and dissolved in deionized water, and the mixed metal salt is obtained after stirring and dissolving until the mixed metal salt is clear and transparentA solution, wherein the concentration of nickel ions is 0.125 mol/L, the concentration of zinc ions is 0.125 mol/L, and the concentration of iron ions is 0.5 mol/L;
(2) Adding deionized water into sodium hydroxide serving as a precipitator to prepare a precipitator solution with the concentration of 4.8 mol/L;
(3) Rapidly adding the initial metal ion solution obtained in the step (1) into the precipitant solution under the condition of rapid stirring, wherein the adding speed is controlled at 50 ml/second;
(4) Stirring and reacting for 2.5 hours, filtering and separating, and washing with deionized water until the filtrate is neutral to obtain a filter cake;
(5) The obtained filter cake is subjected to 100 o C, drying to constant weight, grinding and sieving to obtain precursor powder;
(6) Performing heat treatment on the obtained precursor powder 800 o And C, heat treatment is carried out for 2 hours, so as to obtain ferrite powder.
The crystallinity of the NiZn ferrite nano powder synthesized in the comparative example is poor. The synthesized sample particles were spherical in shape from the scanning electron micrograph of FIG. 13, had a particle size of about 89nm, a standard deviation of 112nm (as shown in FIG. 14), and had poor uniformity. As shown in FIG. 15, the saturation magnetization of the sample was 58emu/g, and the magnetic properties of the sample were inferior to those of the example.
The preferred embodiments of the present invention have been described in detail above with reference to the examples, but the present invention is not limited to the specific details of the above embodiments, and various simple modifications can be made to the technical solutions of the present invention within the scope of the technical concept of the present invention, and all the simple modifications belong to the protection scope of the present invention.
In addition, the specific features described in the above embodiments may be combined in any suitable manner, and in order to avoid unnecessary repetition, various possible combinations are not described further.
Moreover, any combination of the various embodiments of the invention can be made without departing from the spirit of the invention, which should also be considered as disclosed herein.
Claims (10)
1. The method for synthesizing NiZn ferrite nano powder by using a chemical coprecipitation-microwave heat treatment method is characterized by comprising the following steps of:
(1) Weighing soluble metal salt raw materials according to the stoichiometric ratio of each component in the NiZn ferrite, and preparing mixed metal salt solution;
(2) Adding the mixed metal salt solution in the step (1) into a precipitator, and separating after reaction to obtain a precipitate;
(3) Drying the precipitate in the step (2) to constant weight, grinding and sieving to obtain precursor powder;
(4) And (3) carrying out microwave heat treatment on the precursor powder obtained in the step (3), and grinding and sieving the heat treated product to obtain the NiZn ferrite nano powder.
2. The method according to claim 1, wherein in the step (1), the concentration of nickel ions in the mixed metal salt solution is 0.125-0.25 mol/L, the concentration of zinc ions is 0.125-0.25 mol/L, and the concentration of iron ions is 0.5-1 mol/L.
3. The method of claim 1, wherein in the step (2), the precipitant is sodium hydroxide or potassium hydroxide solution, and the concentration is 4.8-5.0 mol/L.
4. A method according to claim 3, wherein the precipitant is used in an amount of 20% -50% excess of the sum of the amounts of metal ion species precipitated.
5. The method according to claim 1, wherein in the step (2), the addition rate of the mixed metal salt solution is 40-50 ml/s, and the reaction time is 2-3 hours.
6. The method of claim 1, wherein in step (2), the separation is performed by suction filtration.
7. The method according to claim 1, wherein in the step (2), the mixed metal salt solution in the step (1) is added to the precipitant under stirring, and separation is performed after stirring reaction, wherein the stirring speed is 500-600 rpm.
8. The method according to claim 1, wherein in the step (3), the temperature of the drying is 80-120 ℃.
9. The method of claim 1, wherein in step (4), the conditions of the microwave heat treatment are: the temperature rising rate is 75-80 ℃/min, the heat preservation temperature is 700-900 ℃, and the heat preservation time is 20-30 min.
10. A NiZn ferrite nano powder synthesized by the method of any one of claims 1 to 9.
Priority Applications (1)
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