CN114566372B - Nickel-copper-zinc ferrite magnetic nano shuttle and preparation method thereof - Google Patents
Nickel-copper-zinc ferrite magnetic nano shuttle and preparation method thereof Download PDFInfo
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- 229910001308 Zinc ferrite Inorganic materials 0.000 title claims abstract description 69
- KOMIMHZRQFFCOR-UHFFFAOYSA-N [Ni].[Cu].[Zn] Chemical compound [Ni].[Cu].[Zn] KOMIMHZRQFFCOR-UHFFFAOYSA-N 0.000 title claims abstract description 63
- 238000002360 preparation method Methods 0.000 title claims abstract description 13
- 239000002121 nanofiber Substances 0.000 claims abstract description 55
- 239000002243 precursor Substances 0.000 claims abstract description 43
- 239000011259 mixed solution Substances 0.000 claims abstract description 17
- 239000002245 particle Substances 0.000 claims abstract description 16
- 238000010041 electrostatic spinning Methods 0.000 claims abstract description 14
- 229910052751 metal Inorganic materials 0.000 claims abstract description 13
- 239000002184 metal Substances 0.000 claims abstract description 13
- 150000003839 salts Chemical class 0.000 claims abstract description 12
- 238000000034 method Methods 0.000 claims abstract description 8
- 229920000642 polymer Polymers 0.000 claims abstract description 8
- 239000002904 solvent Substances 0.000 claims abstract description 6
- 229910052742 iron Inorganic materials 0.000 claims abstract description 4
- 229910052759 nickel Inorganic materials 0.000 claims abstract description 4
- ZMXDDKWLCZADIW-UHFFFAOYSA-N N,N-Dimethylformamide Chemical group CN(C)C=O ZMXDDKWLCZADIW-UHFFFAOYSA-N 0.000 claims description 29
- 238000001035 drying Methods 0.000 claims description 14
- 230000005415 magnetization Effects 0.000 claims description 10
- 229920002239 polyacrylonitrile Polymers 0.000 claims description 10
- 238000001354 calcination Methods 0.000 claims description 6
- PXHVJJICTQNCMI-UHFFFAOYSA-N nickel Substances [Ni] PXHVJJICTQNCMI-UHFFFAOYSA-N 0.000 claims description 5
- QTBSBXVTEAMEQO-UHFFFAOYSA-M Acetate Chemical compound CC([O-])=O QTBSBXVTEAMEQO-UHFFFAOYSA-M 0.000 claims description 2
- 239000010949 copper Substances 0.000 claims description 2
- 238000002156 mixing Methods 0.000 claims description 2
- 239000011701 zinc Substances 0.000 claims description 2
- 239000000463 material Substances 0.000 abstract description 4
- 239000006185 dispersion Substances 0.000 abstract description 3
- 238000003860 storage Methods 0.000 abstract description 2
- 230000000052 comparative effect Effects 0.000 description 19
- 229910052782 aluminium Inorganic materials 0.000 description 8
- XAGFODPZIPBFFR-UHFFFAOYSA-N aluminium Chemical compound [Al] XAGFODPZIPBFFR-UHFFFAOYSA-N 0.000 description 8
- 238000005245 sintering Methods 0.000 description 8
- 238000002441 X-ray diffraction Methods 0.000 description 7
- MCDLETWIOVSGJT-UHFFFAOYSA-N acetic acid;iron Chemical compound [Fe].CC(O)=O.CC(O)=O MCDLETWIOVSGJT-UHFFFAOYSA-N 0.000 description 7
- MQRWBMAEBQOWAF-UHFFFAOYSA-N acetic acid;nickel Chemical compound [Ni].CC(O)=O.CC(O)=O MQRWBMAEBQOWAF-UHFFFAOYSA-N 0.000 description 7
- ZOIORXHNWRGPMV-UHFFFAOYSA-N acetic acid;zinc Chemical compound [Zn].CC(O)=O.CC(O)=O ZOIORXHNWRGPMV-UHFFFAOYSA-N 0.000 description 7
- OPQARKPSCNTWTJ-UHFFFAOYSA-L copper(ii) acetate Chemical compound [Cu+2].CC([O-])=O.CC([O-])=O OPQARKPSCNTWTJ-UHFFFAOYSA-L 0.000 description 7
- 239000000835 fiber Substances 0.000 description 7
- 238000003760 magnetic stirring Methods 0.000 description 7
- 229940078494 nickel acetate Drugs 0.000 description 7
- 239000004246 zinc acetate Substances 0.000 description 7
- 238000004090 dissolution Methods 0.000 description 6
- 238000010438 heat treatment Methods 0.000 description 6
- 229910052573 porcelain Inorganic materials 0.000 description 6
- 238000004321 preservation Methods 0.000 description 6
- 230000001105 regulatory effect Effects 0.000 description 6
- 239000000243 solution Substances 0.000 description 5
- 238000005303 weighing Methods 0.000 description 5
- 230000002776 aggregation Effects 0.000 description 4
- UGKDIUIOSMUOAW-UHFFFAOYSA-N iron nickel Chemical compound [Fe].[Ni] UGKDIUIOSMUOAW-UHFFFAOYSA-N 0.000 description 4
- 238000005054 agglomeration Methods 0.000 description 3
- XEEYBQQBJWHFJM-UHFFFAOYSA-N iron Substances [Fe] XEEYBQQBJWHFJM-UHFFFAOYSA-N 0.000 description 3
- 229920000036 polyvinylpyrrolidone Polymers 0.000 description 3
- 239000001267 polyvinylpyrrolidone Substances 0.000 description 3
- 235000013855 polyvinylpyrrolidone Nutrition 0.000 description 3
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 description 2
- 229910000863 Ferronickel Inorganic materials 0.000 description 2
- 239000003153 chemical reaction reagent Substances 0.000 description 2
- 239000002131 composite material Substances 0.000 description 2
- 238000001523 electrospinning Methods 0.000 description 2
- 238000002474 experimental method Methods 0.000 description 2
- 239000011888 foil Substances 0.000 description 2
- 230000010354 integration Effects 0.000 description 2
- 238000012986 modification Methods 0.000 description 2
- 230000004048 modification Effects 0.000 description 2
- 239000002105 nanoparticle Substances 0.000 description 2
- 229910000859 α-Fe Inorganic materials 0.000 description 2
- CDVAIHNNWWJFJW-UHFFFAOYSA-N 3,5-diethoxycarbonyl-1,4-dihydrocollidine Chemical compound CCOC(=O)C1=C(C)NC(C)=C(C(=O)OCC)C1C CDVAIHNNWWJFJW-UHFFFAOYSA-N 0.000 description 1
- RYGMFSIKBFXOCR-UHFFFAOYSA-N Copper Chemical compound [Cu] RYGMFSIKBFXOCR-UHFFFAOYSA-N 0.000 description 1
- HCHKCACWOHOZIP-UHFFFAOYSA-N Zinc Chemical compound [Zn] HCHKCACWOHOZIP-UHFFFAOYSA-N 0.000 description 1
- 238000004220 aggregation Methods 0.000 description 1
- 238000010276 construction Methods 0.000 description 1
- 229910052802 copper Inorganic materials 0.000 description 1
- 150000001879 copper Chemical class 0.000 description 1
- TVZPLCNGKSPOJA-UHFFFAOYSA-N copper zinc Chemical compound [Cu].[Zn] TVZPLCNGKSPOJA-UHFFFAOYSA-N 0.000 description 1
- LWFZQIXVMAHQKA-UHFFFAOYSA-N copper zinc iron(2+) nickel(2+) oxygen(2-) Chemical compound [O-2].[Fe+2].[Zn+2].[Cu+2].[Ni+2].[O-2].[O-2].[O-2] LWFZQIXVMAHQKA-UHFFFAOYSA-N 0.000 description 1
- 239000013078 crystal Substances 0.000 description 1
- 230000007547 defect Effects 0.000 description 1
- 238000001514 detection method Methods 0.000 description 1
- 239000007788 liquid Substances 0.000 description 1
- 239000000696 magnetic material Substances 0.000 description 1
- 239000012046 mixed solvent Substances 0.000 description 1
- 239000000203 mixture Substances 0.000 description 1
- 150000002815 nickel Chemical class 0.000 description 1
- 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 1
- 238000004626 scanning electron microscopy Methods 0.000 description 1
- 229910052596 spinel Inorganic materials 0.000 description 1
- 239000011029 spinel Substances 0.000 description 1
- 238000003756 stirring Methods 0.000 description 1
- 239000000126 substance Substances 0.000 description 1
- 230000002194 synthesizing effect Effects 0.000 description 1
- 150000003751 zinc Chemical class 0.000 description 1
- 229910052725 zinc Inorganic materials 0.000 description 1
Classifications
-
- H—ELECTRICITY
- H01—ELECTRIC ELEMENTS
- H01F—MAGNETS; INDUCTANCES; TRANSFORMERS; SELECTION OF MATERIALS FOR THEIR MAGNETIC PROPERTIES
- H01F41/00—Apparatus or processes specially adapted for manufacturing or assembling magnets, inductances or transformers; Apparatus or processes specially adapted for manufacturing materials characterised by their magnetic properties
- H01F41/02—Apparatus or processes specially adapted for manufacturing or assembling magnets, inductances or transformers; Apparatus or processes specially adapted for manufacturing materials characterised by their magnetic properties for manufacturing cores, coils, or magnets
-
- H—ELECTRICITY
- H01—ELECTRIC ELEMENTS
- H01F—MAGNETS; INDUCTANCES; TRANSFORMERS; SELECTION OF MATERIALS FOR THEIR MAGNETIC PROPERTIES
- H01F1/00—Magnets or magnetic bodies characterised by the magnetic materials therefor; Selection of materials for their magnetic properties
- H01F1/01—Magnets or magnetic bodies characterised by the magnetic materials therefor; Selection of materials for their magnetic properties of inorganic materials
- H01F1/03—Magnets or magnetic bodies characterised by the magnetic materials therefor; Selection of materials for their magnetic properties of inorganic materials characterised by their coercivity
- H01F1/12—Magnets or magnetic bodies characterised by the magnetic materials therefor; Selection of materials for their magnetic properties of inorganic materials characterised by their coercivity of soft-magnetic materials
- H01F1/34—Magnets or magnetic bodies characterised by the magnetic materials therefor; Selection of materials for their magnetic properties of inorganic materials characterised by their coercivity of soft-magnetic materials non-metallic substances, e.g. ferrites
- H01F1/342—Oxides
- H01F1/344—Ferrites, e.g. having a cubic spinel structure (X2+O)(Y23+O3), e.g. magnetite Fe3O4
Landscapes
- Engineering & Computer Science (AREA)
- Power Engineering (AREA)
- Manufacturing & Machinery (AREA)
- Chemical & Material Sciences (AREA)
- Dispersion Chemistry (AREA)
- Compounds Of Iron (AREA)
- Soft Magnetic Materials (AREA)
Abstract
The invention relates to the field of material preparation, in particular to a nickel-copper-zinc ferrite magnetic nano shuttle and a preparation method thereof. According to the nickel-copper-zinc ferrite magnetic nano shuttle, a solvent, a high polymer and metal salts containing Ni, zn, cu and Fe are stirred and mixed, electrostatic spinning is carried out by using a mixed solution, precursor nano fibers are obtained, and the precursor nano fibers are dried and then calcined, so that the nickel-copper-zinc ferrite magnetic nano shuttle is obtained. The nickel-copper-zinc ferrite magnetic nano shuttle particles prepared by the method have small size, excellent magnetic performance, higher storage capacity density and easier dispersion of the morphology particles of the shuttle.
Description
Technical Field
The invention relates to the field of material preparation, in particular to a nickel-copper-zinc ferrite magnetic nano shuttle and a preparation method thereof.
Background
With the construction of new power systems, the requirements of sensor core elements on miniaturization, integration and multifunctionality are increasing. Among them, a magnetic material having excellent electromagnetic properties and stable chemical properties is of great importance in high-frequency partial discharge detection applications. Nickel-copper-zinc-iron-oxide phase has a low sintering temperature and excellent magnetic properties, and is therefore often used in high-frequency antennas, electromagnetic shields and laminated inductors. In order to meet the requirement of high integration of electronic devices, modern laminated inductors often require smaller thicknesses, which require nickel-copper-zinc ferrite to have excellent magnetic properties at smaller particle sizes. But in general, the grain size is critical to the magnetic properties of the material, smaller grain sizes will result in more "dead magnetic layer (dead magnetic layer)" due to spin-disturbance. Currently, the existing nickel-copper-zinc ferrite nanofiber prepared by electrostatic spinning is in an amorphous state, has poor crystallinity and poor magnetic properties, and has long fiber length and cannot be uniformly dispersed.
The electrostatic spinning is a simple method for synthesizing a one-dimensional nanofiber structure, the stoichiometric proportion of the method is easy to control, the method is also suitable for macro preparation, and the preparation of nanofiber materials with different appearances can be realized by adjusting parameters such as solvents, polymers, solutes and the like in an electrospinning solution. The electrostatic spinning can keep the original shape and prevent the agglomeration of nano particles in the subsequent calcination process, thereby being hopeful to realize the preparation of nano nickel-copper-zinc ferrite particles with excellent magnetic properties and uniform dispersion.
Disclosure of Invention
Therefore, the technical problem to be solved by the invention is to overcome the defects of large size, poor magnetic performance and easy aggregation of nickel-copper-zinc ferrite nano particles in the prior art, thereby providing the nickel-copper-zinc ferrite magnetic nano shuttle and the preparation method thereof.
The preparation method of the nickel-copper-zinc ferrite magnetic nano shuttle comprises the following steps: mixing a solvent, a high molecular polymer and metal salts containing Ni, zn, cu and Fe, carrying out electrostatic spinning by using a mixed solution to obtain precursor nanofibers, drying the precursor nanofibers, and calcining the precursor nanofibers to obtain the nickel-copper-zinc ferrite magnetic nano shuttle;
in the mixed solution, the concentration of the nickel salt is as follows: 0.12 to 0.19mol/L; the concentration of the zinc salt is as follows: 0.25 to 0.38mol/L; the concentration of the copper salt is as follows: 0.05 to 0.08mol/L; the concentration of the ferric salt is as follows: 0.81 to 1.23mol/L.
Preferably, the metal salt is a metal acetate.
Preferably, the concentration of the high molecular polymer is: 0.08 g/mL-0.13 g/mL.
Preferably, the solvent is dimethylformamide;
and/or the high molecular polymer is polyacrylonitrile.
Preferably, the parameters of the electrospinning include: the voltage is 15-20 kV, the pushing speed is 0.7-1.2 mL/h, and the distance between the needle head and the collector is 12-16 cm.
Preferably, the drying conditions include: the drying temperature is 40-100 ℃ and the drying time is 12-24 h.
Preferably, the calcining conditions include: preserving heat for 1.5-2.5 h at 500-900 ℃.
The invention also protects the nickel-copper-zinc ferrite magnetic nano shuttle prepared by the method, and the particle size of the nickel-copper-zinc ferrite magnetic nano shuttle is 50-500 nm.
Preferably, the grain size of the nickel-copper-zinc ferrite magnetic nano shuttle is 50 nm-80 nm.
Preferably, the saturation magnetization intensity of the nickel-copper-zinc ferrite magnetic nano shuttle is 40 emu/g-80 emu/g;
and/or the residual magnetization is 10 emu/g-45 emu/g;
and/or, the coercive force is 0.5kOe to 1.0kOe.
The technical scheme of the invention has the following advantages:
1. the nickel-copper-zinc ferrite magnetic nano shuttle particles obtained by improving the concentration of the metal salt are small in size, have excellent magnetic properties, can provide higher storage capacity density, and meanwhile, the morphology particles of the shuttle show dispersed nano shuttle morphology.
2. The nickel-copper-zinc ferrite magnetic nano shuttle with excellent magnetic performance is obtained by adjusting the concentration of metal salt and proper sintering temperature.
Drawings
In order to more clearly illustrate the embodiments of the present invention or the technical solutions in the prior art, the drawings that are needed in the description of the embodiments or the prior art will be briefly described, and it is obvious that the drawings in the description below are some embodiments of the present invention, and other drawings can be obtained according to the drawings without inventive effort for a person skilled in the art.
FIG. 1 precursor nanofibers containing nickel, copper, zinc, iron prepared in example 1.
FIG. 2 shows the morphology of the nickel-copper-zinc ferrite magnetic nano-shuttle prepared in example 1.
Figure 3 XRD pattern of nickel copper zinc ferrite magnetic nano-shuttle prepared in example 1.
Fig. 4 hysteresis loop of nickel-copper-zinc ferrite magnetic nano shuttle prepared in example 1.
FIG. 5 shows the morphology of the nickel-copper-zinc ferrite magnetic nano-shuttle prepared in example 2.
Figure 6 XRD pattern of nickel copper zinc ferrite magnetic nano-shuttle prepared in example 2.
Fig. 7 hysteresis loop of nickel-copper-zinc ferrite magnetic nano shuttle prepared in example 2.
FIG. 8 shows the morphology of the nickel-copper-zinc ferrite magnetic nano-shuttle prepared in example 3.
Figure 9 XRD pattern of nickel copper zinc ferrite magnetic nano-shuttle prepared in example 3.
Fig. 10 shows hysteresis loop of nickel-copper-zinc ferrite magnetic nano shuttle prepared in example 3.
FIG. 11 shows the morphology of the nickel-copper-zinc ferrite magnetic nano-shuttle prepared in example 4.
Figure 12 XRD pattern of nickel copper zinc ferrite magnetic nano-shuttle prepared in example 4.
Fig. 13 shows hysteresis loop of nickel-copper-zinc ferrite magnetic nano shuttle prepared in example 4.
FIG. 14 shows the morphology of the nickel-copper-zinc ferrite magnetic nano-shuttle prepared in example 5.
Figure 15 XRD pattern of nickel copper zinc ferrite magnetic nano-shuttle prepared in example 5.
Fig. 16 hysteresis loop of nickel-copper-zinc ferrite magnetic nano shuttle prepared in example 5.
Fig. 17 is a nickel copper zinc ferrite nanofiber prepared in comparative example 1.
Fig. 18 shows the nickel-copper-zinc ferrite prepared in comparative example 1.
Figure 19 is an XRD pattern of the nickel copper zinc ferrite prepared in comparative example 1.
Detailed Description
The specific experimental procedures or conditions are not noted in the examples and may be followed by the operations or conditions of conventional experimental procedures described in the literature in this field. The reagents or apparatus used were conventional reagent products commercially available without the manufacturer's knowledge.
The polyacrylonitrile used in the invention is purchased from mikrin with the product number P823209.
Example 1
The embodiment provides a nickel-copper-zinc ferrite magnetic nano shuttle, which is prepared by the following steps:
1.5mmol of nickel acetate, 0.6mmol of copper acetate, 3mmol of zinc acetate, 9.8mmol of ferrous acetate and 1g of polyacrylonitrile are taken and added to 10mL of dimethylformamide, and after magnetic stirring until complete dissolution, a homogeneous mixed solution is formed. The mixed solution was then transferred to a syringe with a regulated voltage of 18kV, a collector of oiled paper covered aluminum barrel at a rotational speed of 375r/min, a syringe advance rate of 1mL/h, and a needle to collector distance of 15cm. And after the electrostatic spinning is finished, collecting the precursor nanofiber on oilpaper, wherein the microscopic morphology of the precursor nanofiber is shown in figure 1, and the precursor nanofiber has an unobvious necklace fiber morphology. And (3) drying the precursor nanofiber in a 60 ℃ oven for 20 hours, weighing 200mg, placing in a porcelain boat, sintering at 500 ℃ in air, wherein the heating rate is 2 ℃/min, the heat preservation time is 2 hours, and the obtained nickel-copper-zinc ferrite magnetic nano shuttle has a microscopic morphology shown in figure 2, an XRD diffraction pattern shown in figure 3 and a hysteresis loop shown in figure 4.
Example 2
The embodiment provides a nickel-copper-zinc ferrite magnetic nano shuttle, which is prepared by the following steps:
1.5mmol of nickel acetate, 0.6mmol of copper acetate, 3mmol of zinc acetate, 9.8mmol of ferrous acetate and 1g of polyacrylonitrile are taken and added to 10mL of dimethylformamide, and after magnetic stirring until complete dissolution, a homogeneous mixed solution is formed. The mixed solution was then transferred to a syringe with a regulated voltage of 18kV, a collector of oiled paper covered aluminum barrel at a rotational speed of 375r/min, a syringe advance rate of 1mL/h, and a needle to collector distance of 15cm. And after the electrostatic spinning is finished, collecting the precursor nanofiber on oilpaper, wherein the microscopic morphology of the precursor nanofiber is shown in figure 1, and the precursor nanofiber has an unobvious necklace fiber morphology. And (3) drying the precursor nanofiber in a 60 ℃ oven for 20 hours, weighing 200mg, placing the precursor nanofiber in a porcelain boat, sintering the precursor nanofiber in the air at 600 ℃, wherein the heating rate is 2 ℃/min, and the heat preservation time is 2 hours, so as to obtain the nickel-copper-zinc ferrite magnetic nano shuttle. The microstructure is shown in fig. 5, the XRD diffraction pattern is shown in fig. 6, and the hysteresis loop is shown in fig. 7.
Example 3
The embodiment provides a nickel-copper-zinc ferrite magnetic nano shuttle, which is prepared by the following steps:
1.5mmol of nickel acetate, 0.6mmol of copper acetate, 3mmol of zinc acetate, 9.8mmol of ferrous acetate and 1g of polyacrylonitrile are taken and added to 10mL of dimethylformamide, and after magnetic stirring until complete dissolution, a homogeneous mixed solution is formed. The mixed solution was then transferred to a syringe with a regulated voltage of 18kV, a collector of oiled paper covered aluminum barrel at a rotational speed of 375r/min, a syringe advance rate of 1mL/h, and a needle to collector distance of 15cm. And after the electrostatic spinning is finished, collecting the precursor nanofiber on oilpaper, wherein the microscopic morphology of the precursor nanofiber is shown in figure 1, and the precursor nanofiber has an unobvious necklace fiber morphology. Drying the precursor nanofiber in a 60 ℃ oven for 20 hours, weighing 200mg, placing the precursor nanofiber in a porcelain boat, sintering at 700 ℃ in air, wherein the heating rate is 2 ℃/min, the heat preservation time is 2 hours, and the obtained nickel-copper-zinc ferrite magnetic nano shuttle has a microscopic morphology shown in figure 8, an XRD diffraction pattern shown in figure 9 and a hysteresis loop shown in figure 10.
Example 4
The embodiment provides a nickel-copper-zinc ferrite magnetic nano shuttle, which is prepared by the following steps:
1.5mmol of nickel acetate, 0.6mmol of copper acetate, 3mmol of zinc acetate, 9.8mmol of ferrous acetate and 1g of polyacrylonitrile are taken and added to 10mL of dimethylformamide, and after magnetic stirring until complete dissolution, a homogeneous mixed solution is formed. The mixed solution was then transferred to a syringe with a regulated voltage of 18kV, a collector of oiled paper covered aluminum barrel at a rotational speed of 375r/min, a syringe advance rate of 1mL/h, and a needle to collector distance of 15cm. And after the electrostatic spinning is finished, collecting the precursor nanofiber on oilpaper, wherein the microscopic morphology of the precursor nanofiber is shown in figure 1, and the precursor nanofiber has an unobvious necklace fiber morphology. And (3) drying the precursor nanofiber in a 60 ℃ oven for 20 hours, weighing 200mg, placing in a porcelain boat, sintering at 800 ℃ in air, wherein the heating rate is 2 ℃/min, the heat preservation time is 2 hours, and the obtained nickel-copper-zinc ferrite magnetic nano shuttle has a microscopic morphology shown in figure 11, an XRD diffraction pattern shown in figure 12 and a hysteresis loop shown in figure 13.
Example 5
The embodiment provides a nickel-copper-zinc ferrite magnetic nano shuttle, which is prepared by the following steps:
1.5mmol of nickel acetate, 0.6mmol of copper acetate, 3mmol of zinc acetate, 9.8mmol of ferrous acetate and 1g of polyacrylonitrile are taken and added to 10mL of dimethylformamide, and after magnetic stirring until complete dissolution, a homogeneous mixed solution is formed. The mixed solution was then transferred to a syringe with a regulated voltage of 18kV, a collector of oiled paper covered aluminum barrel at a rotational speed of 375r/min, a syringe advance rate of 1mL/h, and a needle to collector distance of 15cm. And after the electrostatic spinning is finished, collecting the precursor nanofiber on oilpaper, wherein the microscopic morphology of the precursor nanofiber is shown in figure 1, and the precursor nanofiber has an unobvious necklace fiber morphology. Drying the precursor nanofiber in a 60 ℃ oven for 20 hours, weighing 200mg, placing the precursor nanofiber in a porcelain boat, sintering the precursor nanofiber in the air at 900 ℃, wherein the heating rate is 2 ℃/min, the heat preservation time is 2 hours, and the obtained nickel-copper-zinc ferrite magnetic nano shuttle has a microscopic morphology shown in fig. 14, an XRD diffraction pattern shown in fig. 15 and a hysteresis loop shown in fig. 16.
Comparative example 1
The comparative example provides a nickel-copper-zinc ferrite, which is prepared by the following steps:
1.5mmol of nickel acetate, 0.6mmol of copper acetate, 3mmol of zinc acetate, 9.8mmol of ferrous acetate and 1g of polyacrylonitrile are taken and added to 15mL of dimethylformamide, and after magnetic stirring until complete dissolution, a homogeneous mixed solution is formed. The mixed solution was then transferred to a syringe with a regulated voltage of 18kV, a collector of oiled paper covered aluminum barrel at a rotational speed of 375r/min, a syringe advance rate of 1mL/h, and a needle to collector distance of 15cm. After the electrostatic spinning is finished, the precursor nanofiber can be collected on oilpaper, the microscopic morphology of the precursor nanofiber is shown in fig. 17, 200mg of the precursor nanofiber is weighed after the precursor nanofiber is dried in a 60 ℃ oven for 20 hours, the precursor nanofiber is placed in a porcelain boat, 900 ℃ sintering is carried out in air, the heating rate is 2 ℃/min, the heat preservation time is 2 hours, the microscopic morphology is shown in fig. 18, the agglomeration phenomenon is obvious, the nano shuttle morphology is not shown, and the XRD diffraction pattern of the precursor nanofiber is shown in fig. 19.
Comparative example 2
The comparative example provides a copper zinc ferrite magnetic nanofiber, which is prepared by the following steps:
1.5mmol of nickel acetate, 0.6mmol of copper acetate, 3mmol of zinc acetate, 9.8mmol of ferrous acetate and 1g of polyacrylonitrile are taken and added to 5mL of dimethylformamide, and a completely uniform liquid cannot be obtained by magnetic stirring, so that the subsequent steps cannot be carried out.
Comparative example 3
The comparative example provides a ferronickel composite oxide nanofiber, which is prepared by the following steps:
1g of polyvinylpyrrolidone (PVP) was added to a mixed solvent of 10mL of ethanol and 3mL of DMF and stirred at room temperature for 30min until PVP was completely dissolved, and the solution was colorless and transparent. Under stirring, 0.5mmol of nickel nitrate hexahydrate and 1mmol of ferric acetylacetonate are added in sequence, and the mixture is stirred at room temperature for 12 hours to obtain a uniform solution. Pouring the solution into a 5mL syringe, wherein the inner diameter of a needle is 0.41mm, an aluminum foil is used as a cathode receiving plate, collecting nanofiber products, the distance between the aluminum foil and the two electrode plates of the needle is 22cm, applying voltage of 23kV, the temperature of 25 ℃ and the humidity of 20%, then carrying out electrostatic spinning, and obtaining nanofiber precursors on the receiving plate after 25 hours. And (3) drying the nanofiber precursor at 70 ℃ for 24 hours, and calcining the obtained dried nanofiber precursor at 550 ℃ for 3 hours in an air atmosphere to obtain the ferronickel composite oxide nanofiber.
Experimental example 1:
the nickel copper zinc ferrite magnetic nano shuttle obtained in examples 1 to 5 and the nickel copper zinc ferrite obtained in comparative example 1 and the nickel iron composite oxide nanofiber obtained in comparative example 3 were collected by using a scanning electron microscope to obtain the corresponding average particle sizes, and experimental results are shown in table 1.
TABLE 1 mean particle size of Nickel copper Zinc ferrite
The particle size was obtained by scanning electron microscopy, and since the particle size was difficult to observe in the image of example 1, example 1 did not have this value, and the nickel-iron composite oxide nanofiber obtained in comparative example 3 did not have the corresponding particle size due to the fiber morphology.
Experimental example 2:
XRD patterns of the nickel copper zinc ferrite magnetic nano-shuttles obtained in examples 1 to 5 and the nickel copper zinc ferrite obtained in comparative example 1 and the nickel iron composite oxide nanofiber obtained in comparative example 3 were collected using an X-ray diffractometer, corresponding to standard spinel ferrite diffraction peaks, according to the Shelle formulaThe grain sizes of the nickel copper zinc ferrite magnetic nano-shuttles obtained in examples 1 to 5 and the nickel copper zinc ferrites obtained in comparative examples 1 to 3 were calculated as shown in table 2.
TABLE 2 grain size of Nickel copper Zinc ferrite
The nickel-iron composite oxide nanofiber obtained in comparative example 3 was in an amorphous state, and had no corresponding grain size.
Experimental example 3:
the hysteresis loops of the nickel copper zinc ferrite magnetic nano-shuttles obtained in examples 1 to 5 and the nickel copper zinc ferrite obtained in comparative example 1 were measured within.+ -.70 kOe using the MPMS-required VSM-094 magnetic test system to obtain saturation magnetization, residual magnetization and coercive force, and the magnetic properties were not examined since the agglomeration phenomenon of the particles of comparative example 1 was remarkable and the morphology was changed, and the magnetic properties were not examined since comparative example 3 had no corresponding crystal grains and particle sizes, as shown in Table 3.
TABLE 3 saturation magnetization, residual magnetization and coercivity results
| Saturation magnetization emu/g | Residual magnetization emu/g | Coercivity kOe | |
| Example 1 | 51.17 | 14.58 | 0.797 |
| Example 2 | 59.67 | 25.72 | 0.734 |
| Example 3 | 60.42 | 28.93 | 0.755 |
| Example 4 | 65.59 | 33.59 | 0.804 |
| Example 5 | 68.07 | 34.64 | 0.670 |
As can be seen from the table, the nickel-copper-zinc ferrite magnetic nano shuttle prepared by the method has small particle size, uniform dispersion and good magnetic property.
It is apparent that the above examples are given by way of illustration only and are not limiting of the embodiments. Other variations or modifications of the above teachings will be apparent to those of ordinary skill in the art. It is not necessary here nor is it exhaustive of all embodiments. While still being apparent from variations or modifications that may be made by those skilled in the art are within the scope of the invention.
Claims (5)
1. The preparation method of the nickel-copper-zinc ferrite magnetic nano shuttle is characterized by comprising the following steps of: mixing a solvent, a high molecular polymer and metal salts containing Ni, zn, cu and Fe, carrying out electrostatic spinning by using a mixed solution to obtain precursor nanofibers, drying the precursor nanofibers, and calcining the precursor nanofibers to obtain the nickel-copper-zinc ferrite magnetic nano shuttle;
in the mixed solution, the concentration of the metal salt containing Ni is as follows: 0.12 to 0.19mol/L; the concentration of the Zn-containing metal salt is: 0.25 to 0.38mol/L; the concentration of the Cu-containing metal salt is: 0.05 to 0.08mol/L; the concentration of the Fe-containing metal salt is: 0.81 to 1.23mol/L; the metal salt is metal acetate; the concentration of the high molecular polymer is as follows: 0.08 g/mL-0.13 g/mL;
the solvent is dimethylformamide; the high molecular polymer is polyacrylonitrile;
the parameters of the electrostatic spinning include: the voltage is 15-20 kV, the propulsion rate is 0.7-1.2 mL/h, and the distance between the needle head and the collector is 12-16 cm;
the calcination conditions include: preserving heat for 1.5-2.5 h at 500-900 ℃.
2. The method for preparing a nickel copper zinc ferrite magnetic nano-shuttle according to claim 1, wherein the drying conditions include: the drying temperature is 40-100 ℃ and the drying time is 12-24 h.
3. A nickel-copper-zinc-ferrite magnetic nano-shuttle prepared by the preparation method according to any one of claims 1 to 2, wherein the particle size of the nickel-copper-zinc-ferrite magnetic nano-shuttle is 50nm to 500nm.
4. The nickel-copper-zinc-ferrite magnetic nano-shuttle according to claim 3, wherein the grain size of the nickel-copper-zinc-ferrite magnetic nano-shuttle is 50nm to 80nm.
5. The nickel-copper-zinc-ferrite magnetic nano-shuttle according to claim 3 or 4, wherein the saturation magnetization of the nickel-copper-zinc-ferrite magnetic nano-shuttle is 40emu/g to 80emu/g;
and/or the residual magnetization is 10 emu/g-45 emu/g;
and/or, the coercive force is 0.5kOe to 1.0kOe.
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