CN115385678A - Soft magnetic manganese-nickel-zinc-copper composite material and preparation method and application thereof - Google Patents
Soft magnetic manganese-nickel-zinc-copper composite material and preparation method and application thereof Download PDFInfo
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- CN115385678A CN115385678A CN202211163672.5A CN202211163672A CN115385678A CN 115385678 A CN115385678 A CN 115385678A CN 202211163672 A CN202211163672 A CN 202211163672A CN 115385678 A CN115385678 A CN 115385678A
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- 239000002131 composite material Substances 0.000 title claims abstract description 67
- HEWIALZDOKKCSI-UHFFFAOYSA-N [Ni].[Zn].[Mn].[Cu] Chemical compound [Ni].[Zn].[Mn].[Cu] HEWIALZDOKKCSI-UHFFFAOYSA-N 0.000 title claims abstract description 59
- 238000002360 preparation method Methods 0.000 title claims abstract description 21
- 238000005245 sintering Methods 0.000 claims abstract description 66
- 239000002994 raw material Substances 0.000 claims abstract description 35
- 239000003795 chemical substances by application Substances 0.000 claims abstract description 26
- 238000000034 method Methods 0.000 claims abstract description 24
- PXHVJJICTQNCMI-UHFFFAOYSA-N nickel Substances [Ni] PXHVJJICTQNCMI-UHFFFAOYSA-N 0.000 claims abstract description 17
- 229910052596 spinel Inorganic materials 0.000 claims abstract description 6
- 239000011029 spinel Substances 0.000 claims abstract description 6
- 229910052720 vanadium Inorganic materials 0.000 claims abstract description 6
- 229910052759 nickel Inorganic materials 0.000 claims abstract description 5
- 239000000463 material Substances 0.000 claims description 75
- 238000002156 mixing Methods 0.000 claims description 48
- 238000000498 ball milling Methods 0.000 claims description 40
- 230000004907 flux Effects 0.000 claims description 31
- 239000011265 semifinished product Substances 0.000 claims description 23
- 239000002245 particle Substances 0.000 claims description 22
- 239000008367 deionised water Substances 0.000 claims description 14
- 229910021641 deionized water Inorganic materials 0.000 claims description 14
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Chemical compound O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims description 14
- -1 polyethylene ethanol Polymers 0.000 claims description 12
- 238000004519 manufacturing process Methods 0.000 claims description 9
- 238000005303 weighing Methods 0.000 claims description 7
- 238000001035 drying Methods 0.000 claims description 5
- 229910015902 Bi 2 O 3 Inorganic materials 0.000 claims description 4
- 238000000748 compression moulding Methods 0.000 claims description 4
- 238000005469 granulation Methods 0.000 claims description 4
- 230000003179 granulation Effects 0.000 claims description 4
- 238000007873 sieving Methods 0.000 claims description 4
- 238000004891 communication Methods 0.000 claims description 3
- 239000004372 Polyvinyl alcohol Substances 0.000 claims description 2
- 229920002451 polyvinyl alcohol Polymers 0.000 claims description 2
- 230000001105 regulatory effect Effects 0.000 abstract description 2
- 230000000052 comparative effect Effects 0.000 description 29
- 229910000859 α-Fe Inorganic materials 0.000 description 22
- XLOMVQKBTHCTTD-UHFFFAOYSA-N Zinc monoxide Chemical compound [Zn]=O XLOMVQKBTHCTTD-UHFFFAOYSA-N 0.000 description 14
- 239000000696 magnetic material Substances 0.000 description 11
- QPLDLSVMHZLSFG-UHFFFAOYSA-N Copper oxide Chemical compound [Cu]=O QPLDLSVMHZLSFG-UHFFFAOYSA-N 0.000 description 9
- 239000011787 zinc oxide Substances 0.000 description 7
- 239000000203 mixture Substances 0.000 description 6
- 230000035699 permeability Effects 0.000 description 6
- 229910003962 NiZn Inorganic materials 0.000 description 5
- XEEYBQQBJWHFJM-UHFFFAOYSA-N iron Substances [Fe] XEEYBQQBJWHFJM-UHFFFAOYSA-N 0.000 description 4
- ZNOKGRXACCSDPY-UHFFFAOYSA-N tungsten trioxide Chemical compound O=[W](=O)=O ZNOKGRXACCSDPY-UHFFFAOYSA-N 0.000 description 4
- UQSXHKLRYXJYBZ-UHFFFAOYSA-N Iron oxide Chemical group [Fe]=O UQSXHKLRYXJYBZ-UHFFFAOYSA-N 0.000 description 3
- KOMIMHZRQFFCOR-UHFFFAOYSA-N [Ni].[Cu].[Zn] Chemical compound [Ni].[Cu].[Zn] KOMIMHZRQFFCOR-UHFFFAOYSA-N 0.000 description 3
- 239000012467 final product Substances 0.000 description 3
- 230000006698 induction Effects 0.000 description 3
- 239000012071 phase Substances 0.000 description 3
- 239000000843 powder Substances 0.000 description 3
- 238000003825 pressing Methods 0.000 description 3
- 239000010409 thin film Substances 0.000 description 3
- YLZOPXRUQYQQID-UHFFFAOYSA-N 3-(2,4,6,7-tetrahydrotriazolo[4,5-c]pyridin-5-yl)-1-[4-[2-[[3-(trifluoromethoxy)phenyl]methylamino]pyrimidin-5-yl]piperazin-1-yl]propan-1-one Chemical compound N1N=NC=2CN(CCC=21)CCC(=O)N1CCN(CC1)C=1C=NC(=NC=1)NCC1=CC(=CC=C1)OC(F)(F)F YLZOPXRUQYQQID-UHFFFAOYSA-N 0.000 description 2
- IJGRMHOSHXDMSA-UHFFFAOYSA-N Atomic nitrogen Chemical compound N#N IJGRMHOSHXDMSA-UHFFFAOYSA-N 0.000 description 2
- 239000005751 Copper oxide Substances 0.000 description 2
- 230000009286 beneficial effect Effects 0.000 description 2
- 229910000431 copper oxide Inorganic materials 0.000 description 2
- 239000013078 crystal Substances 0.000 description 2
- 238000010304 firing Methods 0.000 description 2
- 229910001004 magnetic alloy Inorganic materials 0.000 description 2
- 238000004321 preservation Methods 0.000 description 2
- 239000000126 substance Substances 0.000 description 2
- OHVLMTFVQDZYHP-UHFFFAOYSA-N 1-(2,4,6,7-tetrahydrotriazolo[4,5-c]pyridin-5-yl)-2-[4-[2-[[3-(trifluoromethoxy)phenyl]methylamino]pyrimidin-5-yl]piperazin-1-yl]ethanone Chemical compound N1N=NC=2CN(CCC=21)C(CN1CCN(CC1)C=1C=NC(=NC=1)NCC1=CC(=CC=C1)OC(F)(F)F)=O OHVLMTFVQDZYHP-UHFFFAOYSA-N 0.000 description 1
- LDXJRKWFNNFDSA-UHFFFAOYSA-N 2-(2,4,6,7-tetrahydrotriazolo[4,5-c]pyridin-5-yl)-1-[4-[2-[[3-(trifluoromethoxy)phenyl]methylamino]pyrimidin-5-yl]piperazin-1-yl]ethanone Chemical compound C1CN(CC2=NNN=C21)CC(=O)N3CCN(CC3)C4=CN=C(N=C4)NCC5=CC(=CC=C5)OC(F)(F)F LDXJRKWFNNFDSA-UHFFFAOYSA-N 0.000 description 1
- AFCARXCZXQIEQB-UHFFFAOYSA-N N-[3-oxo-3-(2,4,6,7-tetrahydrotriazolo[4,5-c]pyridin-5-yl)propyl]-2-[[3-(trifluoromethoxy)phenyl]methylamino]pyrimidine-5-carboxamide Chemical compound O=C(CCNC(=O)C=1C=NC(=NC=1)NCC1=CC(=CC=C1)OC(F)(F)F)N1CC2=C(CC1)NN=N2 AFCARXCZXQIEQB-UHFFFAOYSA-N 0.000 description 1
- 229910007565 Zn—Cu Inorganic materials 0.000 description 1
- 229910045601 alloy Inorganic materials 0.000 description 1
- 239000000956 alloy Substances 0.000 description 1
- 230000015572 biosynthetic process Effects 0.000 description 1
- 238000006243 chemical reaction Methods 0.000 description 1
- 230000001276 controlling effect Effects 0.000 description 1
- 238000001816 cooling Methods 0.000 description 1
- 239000011162 core material Substances 0.000 description 1
- 239000003814 drug Substances 0.000 description 1
- 230000000694 effects Effects 0.000 description 1
- 238000004134 energy conservation Methods 0.000 description 1
- 238000005265 energy consumption Methods 0.000 description 1
- 239000004615 ingredient Substances 0.000 description 1
- 239000007791 liquid phase Substances 0.000 description 1
- 239000006249 magnetic particle Substances 0.000 description 1
- 230000005415 magnetization Effects 0.000 description 1
- 229910052751 metal Inorganic materials 0.000 description 1
- 239000002184 metal Substances 0.000 description 1
- 239000002114 nanocomposite Substances 0.000 description 1
- 239000002105 nanoparticle Substances 0.000 description 1
- 229910052757 nitrogen Inorganic materials 0.000 description 1
- NDLPOXTZKUMGOV-UHFFFAOYSA-N oxo(oxoferriooxy)iron hydrate Chemical compound O.O=[Fe]O[Fe]=O NDLPOXTZKUMGOV-UHFFFAOYSA-N 0.000 description 1
- 238000007747 plating Methods 0.000 description 1
- 239000000047 product Substances 0.000 description 1
- 238000006467 substitution reaction Methods 0.000 description 1
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- C—CHEMISTRY; METALLURGY
- C04—CEMENTS; CONCRETE; ARTIFICIAL STONE; CERAMICS; REFRACTORIES
- C04B—LIME, MAGNESIA; SLAG; CEMENTS; COMPOSITIONS THEREOF, e.g. MORTARS, CONCRETE OR LIKE BUILDING MATERIALS; ARTIFICIAL STONE; CERAMICS; REFRACTORIES; TREATMENT OF NATURAL STONE
- C04B35/00—Shaped ceramic products characterised by their composition; Ceramics compositions; Processing powders of inorganic compounds preparatory to the manufacturing of ceramic products
- C04B35/01—Shaped ceramic products characterised by their composition; Ceramics compositions; Processing powders of inorganic compounds preparatory to the manufacturing of ceramic products based on oxide ceramics
- C04B35/26—Shaped ceramic products characterised by their composition; Ceramics compositions; Processing powders of inorganic compounds preparatory to the manufacturing of ceramic products based on oxide ceramics based on ferrites
- C04B35/265—Compositions containing one or more ferrites of the group comprising manganese or zinc and one or more ferrites of the group comprising nickel, copper or cobalt
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- C—CHEMISTRY; METALLURGY
- C04—CEMENTS; CONCRETE; ARTIFICIAL STONE; CERAMICS; REFRACTORIES
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- C04B35/00—Shaped ceramic products characterised by their composition; Ceramics compositions; Processing powders of inorganic compounds preparatory to the manufacturing of ceramic products
- C04B35/622—Forming processes; Processing powders of inorganic compounds preparatory to the manufacturing of ceramic products
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- C—CHEMISTRY; METALLURGY
- C04—CEMENTS; CONCRETE; ARTIFICIAL STONE; CERAMICS; REFRACTORIES
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- C04B35/00—Shaped ceramic products characterised by their composition; Ceramics compositions; Processing powders of inorganic compounds preparatory to the manufacturing of ceramic products
- C04B35/622—Forming processes; Processing powders of inorganic compounds preparatory to the manufacturing of ceramic products
- C04B35/64—Burning or sintering processes
-
- 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
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- C04B2235/00—Aspects relating to ceramic starting mixtures or sintered ceramic products
- C04B2235/60—Aspects relating to the preparation, properties or mechanical treatment of green bodies or pre-forms
- C04B2235/602—Making the green bodies or pre-forms by moulding
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- C04B2235/00—Aspects relating to ceramic starting mixtures or sintered ceramic products
- C04B2235/65—Aspects relating to heat treatments of ceramic bodies such as green ceramics or pre-sintered ceramics, e.g. burning, sintering or melting processes
- C04B2235/656—Aspects relating to heat treatments of ceramic bodies such as green ceramics or pre-sintered ceramics, e.g. burning, sintering or melting processes characterised by specific heating conditions during heat treatment
- C04B2235/6567—Treatment time
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- C04B2235/00—Aspects relating to ceramic starting mixtures or sintered ceramic products
- C04B2235/70—Aspects relating to sintered or melt-casted ceramic products
- C04B2235/74—Physical characteristics
- C04B2235/77—Density
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- Power Engineering (AREA)
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- Magnetic Ceramics (AREA)
Abstract
The invention provides a soft magnetic manganese nickel zinc copper composite material and a preparation method and application thereof, wherein the main phase of the soft magnetic manganese nickel zinc copper composite material is in a spinel structure, and the soft magnetic manganese nickel zinc copper composite material comprises a main component and a fluxing agent component; the content of the main components calculated by oxide comprises: fe 2 O 3 :45~50mol%、ZnO:5~25mo1%、CuO:3~20mo1%、MnO 2 1 to 3mo1% and Ni 2 O 3 10-18 mol%; the fluxing agent comprises the following components in percentage by mass of the total mass of the main components: bi 2 O 3 0.01 to 0.5wt% and V 2 O 5 0.01 to 0.4wt percent. The soft magnetic manganese-nickel-zinc-copper composite material has excellent magnetic propertyThe raw material cost is low, the temperature of the pre-sintering treatment and the sintering treatment is low, the energy can be saved, the preparation process can be conveniently regulated, and the method has a large-scale application prospect.
Description
Technical Field
The invention relates to the technical field of soft magnetic ferrite, in particular to a soft magnetic manganese-nickel-zinc-copper composite material and a preparation method and application thereof.
Background
The ferrite magnetic material mainly comprises spinel-type, garnet-type and magnetoplumbite-type polycrystalline and single crystal ferrite materials, has high resistivity, small loss, good dielectric property and frequency characteristic, is an important magnetic functional material, and has wide application in the fields of modern communication, military, electronics, information, chemical industry, biology, medicine and the like.
The soft magnetic MnZn ferrite magnetic material has the characteristics of higher initial permeability mu i, high saturation magnetic induction Bs, high temperature and low loss Pcv and the like, but the surface resistance is much lower than that of the soft magnetic NiZn ferrite magnetic material. The surface resistance of the soft magnetic MnZn ferrite magnetic material is only a few ohms to hundreds of ohms generally, while the surface resistance of the soft magnetic NiZn ferrite magnetic material can reach more than 109 ohms generally, but the initial permeability mui, the saturation magnetic induction Bs, the high-temperature low-loss Pcv and the like of the soft magnetic NiZn ferrite magnetic material are all poorer than the performances of the soft magnetic MnZn ferrite magnetic material.
CN102262950A discloses a nickel-zinc-copper soft magnetic ferrite and a preparation method thereof, the nickel-zinc-copper soft magnetic ferrite comprises a main component and an auxiliary component, the main component is iron oxide, nickel protoxide, zinc oxide, and copper oxide, and is characterized in that the contents of the main components are as follows: 65.05-66.35 wt% of ferric oxide; 20.66-22.20 wt% of zinc oxide; 9.55-10.06 wt% of nickel protoxide; 2.91-3.17 wt% of copper oxide; the accessory ingredient comprises tungsten trioxide, and the content of the tungsten trioxide is 0.003 to 0.03 weight percent. The nickel-zinc-copper soft magnetic ferrite reduces the loss performance of the product on the premise of keeping higher initial permeability and saturation magnetic flux density. But the sintering temperature of the preparation method is higher, and the energy consumption is larger.
CN103632794A discloses a composite soft magnetic material and a method for preparing the same, the composite soft magnetic material is composed of soft magnetic ferrite powder and a soft magnetic alloy thin film, and the soft magnetic alloy thin film is coated on the surface of soft magnetic ferrite particles to form a thin film with the thickness of 0.01 μm to 10 μm. The material obtained by sintering the obtained composite soft magnetic particles not only has higher saturation magnetic induction intensity, but also has higher magnetic conductivity and has the characteristics of soft magnetic ferrite and metal soft magnetic materials. Meanwhile, the material also has good mechanical properties and is mainly applied to the field of medium and high frequency. However, the method actually adopts a chemical plating process, and ferrite is required to be achieved through sintering subsequently, so that the problem that the composite layer is co-fired under an unsuitable condition cannot be avoided.
CN103765524A discloses a magnetic grain boundary engineered ferrite core material comprising a grain component and a nanostructured grain boundary component, the nanostructured grain boundary being insulating and magnetic so as to provide greater continuity of magnetization of the composite material. The grain component has an average grain size of about 0.5 to 50 μm. The grain boundary component has an average grain size of about 1 to 100 nm. The nanostructured magnetic grain boundary material has a magnetic flux density of at least about 250 mT. Nano NiZn ferrite powder and MnZn ferrite powder are mixed and are finally co-fired under the condition of nitrogen after the processes of sieving and the like, but the method cannot avoid the problem that the sintering condition of the MnZn and the NiZn ferrite is not suitable.
In conclusion, in the process of preparing the composite ferrite magnet in the prior art, the problems that the sintering conditions among the components of different composite materials are not appropriate, the sintering temperature is high, and the preparation process is difficult to control reasonably still exist.
Disclosure of Invention
In order to solve the technical problems, the invention provides the soft magnetic manganese nickel zinc copper composite material and the preparation method and the application thereof, the main component and the fluxing agent component with specific contents are adopted, the raw material cost can be saved, the sintering treatment temperature can be effectively reduced, the energy is saved, and the obtained soft magnetic manganese nickel zinc copper composite material has better magnetic performance and wide application prospect.
In order to achieve the purpose, the invention adopts the following technical scheme:
in a first aspect, the present invention provides a soft magnetic manganese nickel zinc copper composite material, the main phase of which is a spinel structure, the soft magnetic manganese nickel zinc copper composite material comprising a main component and a flux component;
the content of the main components calculated by oxide comprises: fe 2 O 3 :45~50mol%、ZnO:5~25mo1%、CuO:3~20mo1%、MnO 2 1 to 3mo1% and Ni 2 O 3 :10~18mol%;
The fluxing agent comprises the following components in percentage by mass of the total mass of the main components: bi 2 O 3 0.01-0.5 wt% and V 2 O 5 :0.01~0.4wt%。
The soft part of the inventionThe main phase of the magnetic manganese-nickel-zinc-copper composite material is in a spinel structure, the grain size is within the range of 2-4 mu m, and the main components contain CuO and MnO with specific contents 2 Replace part of Ni 2 O 3 ,Ni 2 O 3 The content of (A) is only 10-18 mol%, thus greatly reducing the cost of raw materials. In the present invention, bi of a specific content is used 2 O 3 And V 2 O 5 Added jointly as a fluxing agent, because only V 2 O 5 As a flux, the high-frequency characteristics of the soft magnetic manganese-nickel-zinc-copper composite material can be improved, but the quality factor of a low frequency band is reduced; and only Bi 2 O 3 The flux is opposite to the flux, is beneficial to improving the low-frequency band loss of the soft magnetic manganese-nickel-zinc-copper composite material, but can reduce the quality factor of the high-frequency band. Thus, bi 2 O 3 And V 2 O 5 The combined addition ensures that the high-frequency and low-frequency loss of the soft magnetic manganese-nickel-zinc-copper composite material is greatly improved, and the soft magnetic manganese-nickel-zinc-copper composite material has better frequency characteristic; but also can effectively reduce the temperature of sintering treatment and save energy.
The content of the main components in the invention calculated by oxide comprises: fe 2 O 3 45 to 50mol%, for example, 40mol%, 42mol%, 45mol%, 47mol%, 48mol%, or 50mol% or the like is possible, but the numerical values are not limited to those listed, and other numerical values not listed in the numerical range are also applicable.
ZnO of 5 to 25mo1% may be, for example, 5mol%, 7mol%, 10mol%, 15mol%, 20mol%, or 25mol%, but is not limited to the above-mentioned values, and other values not shown in the above-mentioned numerical range are also applicable.
CuO of 3 to 20mo1% may be, for example, 3mol%, 5mol%, 8mol%, 10mol%, 15mol% or 20mol%, but is not limited to the above-mentioned numerical values, and other numerical values not shown in the numerical value range are also applicable.
MnO 2 The amount of 1 to 3mo1% may be, for example, 1mol%, 1.3mol%, 1.5mol%, 2mol%, 2.5mol% or 3mol%, but is not limited to the above-mentioned values, and other values not shown in the above-mentioned numerical range are also applicable.
Ni 2 O 3 The amount of 10 to 18mol% may be, for example, 10mol%, 12mol%, 14mol%, 15mol%, 17mol% or 18mol%, but is not limited to the above-mentioned values, and other values not shown in the above-mentioned range are also applicable.
In a second aspect, the present invention also provides a method for preparing the soft magnetic manganese-nickel-zinc-copper composite material according to the first aspect, wherein the method comprises the following steps:
(1) Weighing raw materials according to the formula of the main components, and performing first ball milling mixing to obtain a mixed material;
(2) After the mixed material is dried, presintering treatment at the temperature of 720-780 ℃ is carried out to obtain presintered material;
(3) Mixing the pre-sintered material and a fluxing agent raw material weighed according to a fluxing agent component formula, and performing second ball milling mixing to obtain a semi-finished product material;
(4) And drying the semi-finished product material, mixing the semi-finished product material with polyethylene ethanol, and sequentially carrying out sieving granulation, compression molding and sintering treatment at the temperature of 950-1000 ℃ to obtain the soft magnetic manganese-nickel-zinc-copper composite material.
The temperature of the presintering treatment in the preparation method of the soft magnetic manganese-nickel-zinc-copper composite material is 720-780 ℃, and CuO in the main component can be mixed with Fe 2 O 3 Formation of CuFe 2 O 4 So that the spinel ferrite can be formed at a very low temperature, and the subsequent sintering temperature can be effectively reduced; and the temperature of the pre-sintering treatment and the sintering treatment is lower, so that a large amount of energy is saved, the design requirement on sintering equipment is low, and the production cost of the soft magnetic manganese-nickel-zinc-copper composite material is further reduced. Compared with the existing soft magnetic material, the soft magnetic manganese nickel zinc copper composite material prepared by the preparation method has better magnetic property and can better meet the market demand.
The temperature of the pre-firing treatment in the present invention is 720 to 780 ℃, and for example, 720 ℃, 730 ℃, 750 ℃, 760 ℃, 770 ℃, 780 ℃ and the like are possible, but the temperature is not limited to the values listed, and other values not listed in the numerical range are also applicable.
The temperature of the sintering treatment is 950 to 1000 ℃, and may be, for example, 950 ℃, 960 ℃, 970 ℃, 980 ℃, 990 ℃ or 1000 ℃, but is not limited to the values listed, and other values not listed in the numerical range are also applicable.
Preferably, deionized water with the same mass as that of the main component raw materials is added in the first ball-milling mixing in the step (1).
Preferably, the first ball milling mix has a rotation speed of 300 to 330r/min, such as 300r/min, 302r/min, 305r/min, 310r/min, 320r/min, or 330r/min, but not limited to the values listed, and other values not listed in this range are also applicable.
Preferably, the first ball milling mixture has a ball ratio of 1 (6 to 6.5), which can be, for example, 1.
Preferably, the first ball milling mixing time is 2 to 4 hours, for example, 2 hours, 2.3 hours, 2.5 hours, 3 hours, 3.5 hours, or 4 hours, but not limited to the recited values, and other values not recited in the range of the values are also applicable.
Preferably, the time of the pre-firing treatment is 2 to 4 hours, and may be, for example, 2 hours, 2.3 hours, 2.5 hours, 3 hours, 3.5 hours, or 4 hours, but is not limited to the values listed, and other values not listed in the range of the values are also applicable.
Preferably, the atmosphere of the pre-sintering treatment is air, and the pre-sintering material is cooled along with the furnace after the pre-sintering treatment.
After the pre-sintering treatment is finished, the mixed materials are completely reacted to generate spinel structure crystals, and other impure phases do not exist.
Preferably, bi in the flux component in the step (3) 2 O 3 The average particle size of (A) is 59 to 65nm, and examples thereof include 59nm, 60nm, 61nm, 62nm, 64nm and 65nm, but the average particle size is not limited to the above-mentioned values, and other values not shown in the above-mentioned range are also applicable.
Preferably, V in the flux component 2 O 5 Average particle ofThe degree is 80 to 86nm, and may be, for example, 80nm, 81nm, 82nm, 84nm, 85nm or 86nm, but is not limited to the values listed, and other values not listed in the numerical range are also applicable.
Bi in the flux component of the present invention 2 O 3 And V 2 O 5 The nano-composite material has small average particle size, is nano-sized, has large specific surface area and quite high surface energy, can form a liquid phase at very low temperature, promotes sintering, and effectively reduces the temperature of subsequent sintering treatment.
Preferably, deionized water equal to the total mass of the pre-sintering material and the raw materials of the fluxing agent is added into the second ball-milling mixing in the step (3).
Preferably, the rotation speed of the second ball milling mixing is 300 to 330r/min, such as 300r/min, 302r/min, 305r/min, 310r/min, 320r/min or 330r/min, but not limited to the values listed, and other values not listed in the range of the values are also applicable.
Preferably, the second ball-milling mixture has a ball ratio of 1 (6 to 6.5), which can be, for example, 1.
Preferably, the time for the second ball milling mixing is 3 to 15 hours, for example, 3 hours, 5 hours, 8 hours, 10 hours, 12 hours, or 15 hours, etc., but is not limited to the recited values, and other values not recited in the range of the values are also applicable.
Preferably, the mean particle size of the semifinished product mass is <0.8 μm, and may be, for example, 0.79 μm, 0.75 μm, 0.7 μm, 0.6 μm, 0.5 μm or 0.3 μm, but is not limited to the values listed, and other values not listed in this range are equally applicable.
The invention preferably selects the semi-finished product material with the average particle size of less than 0.8 mu m and large specific surface area, greatly improves the reaction activity of the semi-finished product material and further reduces the sintering treatment temperature.
Preferably, the amount of the polyvinyl alcohol added in step (4) is 8 to 15wt% of the semi-finished product, such as 8wt%, 9wt%, 10wt%, 12wt%, 14wt% or 15wt%, but not limited to the recited values, and other values not recited in the range of the recited values are also applicable.
Preferably, the heat preservation time of the sintering treatment is 6 to 8 hours, for example, 6 hours, 6.5 hours, 7 hours, 7.5 hours, 7.8 hours, 8 hours, etc., but the heat preservation time is not limited to the recited values, and other values not recited in the range of the values are also applicable.
Preferably, the atmosphere of the sintering treatment is air, and the sintering treatment is followed by furnace cooling.
As a preferred technical scheme of the invention, the preparation method comprises the following steps:
(1) Weighing raw materials according to the formula of the main components, and carrying out first ball milling and mixing for 2-4 h at the rotating speed of 300-330 r/min and the material-ball ratio of 1 (6-6.5) to obtain a mixed material; deionized water with the same mass as the main component raw materials is added into the first ball-milling mixing;
(2) After the mixed material is dried, presintering at the temperature of 720-780 ℃ for 2-4 h to obtain a presintered material; the atmosphere of the pre-burning treatment is air, and the pre-burning materials are cooled along with the furnace after the pre-burning treatment;
(3) Mixing the pre-sintered material and flux raw materials weighed according to the flux component formula, and carrying out second ball milling mixing for 3-15 h at the rotating speed of 300-330 r/min and the material-ball ratio of 1 (6-6.5) to obtain the average particle size<0.8 μm of semi-finished material; bi in the flux component 2 O 3 The average particle size of (B) is 59-65 nm; v in the flux component 2 O 5 The average particle size of (A) is 80-86 nm; adding deionized water with the mass equal to the total mass of the pre-sintering material and the fluxing agent raw material into the second ball milling mixing;
(4) After the semi-finished product material is dried, mixing the semi-finished product material with polyethylene ethanol, and sequentially carrying out sieving granulation, compression molding and sintering treatment at 950-1000 ℃ for 6-8 h to obtain the soft magnetic manganese nickel zinc copper composite material; the addition amount of the polyethylene ethanol is 8-15 wt% of the semi-finished product material; the atmosphere of the sintering treatment is air, and the sintering treatment is carried out and then is cooled along with the furnace.
In a third aspect, the invention also provides the use of the soft magnetic manganese nickel zinc copper composite material as described in the first aspect in the field of electronic communication.
Compared with the prior art, the invention has at least the following beneficial effects:
(1) The soft magnetic manganese-nickel-zinc-copper composite material provided by the invention has excellent magnetic property, the initial magnetic conductivity can reach more than 800, and the density can reach 5.05kg/m 3 Above, the specific temperature coefficient is lower than 7.0 x 10 in the temperature range of-20 to 65 DEG C -6 (ii) a At a frequency of 100kHz, the specific loss factor is lower than 10 multiplied by 10 -6 (ii) a Under the test magnetic field of 4000A/m, the saturation magnetic flux density can reach more than 420 mT; curie temperature can reach over 160 ℃;
(2) The preparation method of the soft magnetic manganese-nickel-zinc-copper composite material provided by the invention has the advantages of low raw material cost, lower temperature of pre-sintering treatment and sintering treatment, energy conservation, convenience in regulating and controlling the preparation process, and large-scale industrial popularization and application prospect.
Detailed Description
For the purpose of facilitating an understanding of the present invention, the present invention will now be described by way of examples. It should be understood by those skilled in the art that the examples are only for the understanding of the present invention and should not be construed as the specific limitations of the present invention.
The present invention is described in further detail below. The following examples are merely illustrative of the present invention and do not represent or limit the scope of the claims, which are defined by the appended claims.
Example 1
The embodiment provides a preparation method of a soft magnetic manganese-nickel-zinc-copper composite material, which comprises the following steps:
(1) Weighing the raw materials according to the formula of the main component, 50mol% of Fe 2 O 3 、22mo1%ZnO、14.5mo1%CuO、1.5mo1%MnO 2 And 12mol% of Ni 2 O 3 Carrying out first ball milling and mixing for 3h at the rotating speed of 300r/min and the material-ball ratio of 1; deionized water with the same mass as the main component raw materials is added into the first ball-milling mixing;
(2) After the mixed material is dried, presintering at 780 ℃ for 3 hours to obtain a presintered material; the atmosphere of the pre-burning treatment is air, and the pre-burning materials are cooled along with the furnace after the pre-burning treatment;
(3) Mixing the pre-sintered material with a fluxing agent raw material weighed according to a fluxing agent component formula, and carrying out second ball milling mixing for 12 hours at a rotating speed of 300r/min and a material-ball ratio of 1<0.8 μm of semi-finished material; the fluxing agent comprises the following components in percentage by mass of the total mass of the main components: bi 2 O 3 0.13wt% and V 2 O 5 0.18wt%; bi in the flux component 2 O 3 Has an average particle size of 65nm; v in the flux component 2 O 5 Has an average particle size of 82nm; adding deionized water with the mass equal to the total mass of the pre-sintering material and the fluxing agent raw material into the second ball milling mixing;
(4) Drying the semi-finished product material, mixing with polyethylene ethanol, sequentially granulating by a 45-mesh sample sieve, and pressing to obtain the final productPlacing the sample ring into a box-type furnace, and sintering at 965 ℃ for 6 hours to obtain the soft magnetic manganese-nickel-zinc-copper composite material; the addition amount of the polyethylene ethanol is 10wt% of the semi-finished product material; the atmosphere of the sintering treatment is air, and the sintering treatment is carried out and then is cooled along with the furnace.
Example 2
The embodiment provides a preparation method of a soft magnetic manganese-nickel-zinc-copper composite material, which comprises the following steps:
(1) Weighing the raw materials according to the formula of the main component, 49mol% of Fe 2 O 3 、23mo1%ZnO、15mo1%CuO、3mo1%MnO 2 And 10mol% of Ni 2 O 3 Performing first ball milling and mixing for 3 hours at a rotating speed of 310r/min and a material-to-ball ratio of 1.3 to obtain a mixed material; deionized water with the same mass as the main component raw materials is added into the first ball-milling mixture;
(2) After the mixed material is dried, pre-sintering treatment is carried out for 3 hours at the temperature of 740 ℃ to obtain a pre-sintered material; the atmosphere of the pre-burning treatment is air, and the pre-burning materials are cooled along with the furnace after the pre-burning treatment;
(3) Mixing the pre-sintered material with a fluxing agent raw material weighed according to a fluxing agent component formula, and carrying out second ball milling mixing for 10 hours at the rotating speed of 320r/min and the material-ball ratio of 1<0.8 μm of semi-finished material; the fluxing agent comprises the following components in percentage by mass of the total mass of the main components: bi 2 O 3 0.10wt% and V 2 O 5 0.12wt%; bi in the flux component 2 O 3 Has an average particle size of 60nm; v in the flux component 2 O 5 Has an average particle size of 80nm; adding deionized water with the same total mass as the raw materials of the pre-sintering material and the fluxing agent into the second ball-milling mixture;
(4) Drying the semi-finished product material, mixing with polyethylene ethanol, sequentially granulating by a 45-mesh sample sieve, and pressing to obtain the final productPlacing the sample ring into a box furnace, and sintering at 950 ℃ for 6 hours to obtain the soft magnetic manganese nickel zinc copper composite material; the addition amount of the polyethylene ethanol is 10wt% of the semi-finished product material; the atmosphere of the sintering treatment is air, and the sintering treatment is carried out and then is cooled along with the furnace.
Example 3
The embodiment provides a preparation method of a soft magnetic manganese-nickel-zinc-copper composite material, which comprises the following steps:
(1) Weighing the raw materials according to the formula of the main component, 45mol percent Fe 2 O 3 、25mo1%ZnO、13mo1%CuO、2mo1%MnO 2 And 15mol% of Ni 2 O 3 Carrying out first ball milling and mixing for 3h at the rotating speed of 330r/min and the material-ball ratio of 1; deionized water with the same mass as the main component raw materials is added into the first ball-milling mixture;
(2) After the mixed material is dried, pre-sintering treatment is carried out for 3 hours at the temperature of 780 ℃ to obtain a pre-sintered material; the atmosphere of the pre-burning treatment is air, and the pre-burning materials are cooled along with the furnace after the pre-burning treatment;
(3) Mixing the pre-sintered material with flux raw materials weighed according to the flux component formulaAnd (3) carrying out second ball milling and mixing for 15 hours at the rotating speed of 305r/min and the material-ball ratio of 1<0.8 μm of semi-finished material; the fluxing agent comprises the following components in percentage by mass of the total mass of the main components: bi 2 O 3 0.20wt% and V 2 O 5 0.28wt%; bi in the flux component 2 O 3 Has an average particle size of 59nm; v in the flux component 2 O 5 Has an average particle size of 86nm; adding deionized water with the mass equal to the total mass of the pre-sintering material and the fluxing agent raw material into the second ball milling mixing;
(4) Drying the semi-finished product material, mixing with polyethylene ethanol, sequentially granulating by a 45-mesh sample sieve, and pressing to obtain the final productPlacing the sample ring into a box-type furnace, and sintering at 1000 ℃ for 6 hours to obtain the soft magnetic manganese-nickel-zinc-copper composite material; the addition amount of the polyethylene ethanol is 10wt% of the semi-finished product material; the atmosphere of the sintering treatment is air, and the sintering treatment is carried out and then the furnace is cooled.
Comparative example 1
This comparative example provides a production method of a soft magnetic manganese nickel zinc copper composite material, which except for the step (1), was as follows by dividing 10mol% of Ni 2 O 3 The procedure of example 2 was repeated except that 7mol% was used instead.
Comparative example 2
This comparative example provides a production method of a soft magnetic manganese-nickel-zinc-copper composite material, which except for step (1), was characterized by dividing 10mol% of Ni 2 O 3 The procedure of example 2 was repeated except that 20mol% was replaced.
Comparative example 3
This comparative example provides a production method of a soft magnetic manganese nickel zinc copper composite material, which was conducted except that 0.1wt% of Bi was conducted in step (3) 2 O 3 The procedure of example 2 was repeated except that 0.001wt% was used instead.
Comparative example 4
The present comparative example provides a method for preparing a soft magnetic manganese-nickel-zinc-copper composite material, the method comprising the steps of(3)0.1wt%Bi 2 O 3 The procedure of example 2 was repeated except that 0.6wt% was used instead.
Comparative example 5
This comparative example provides a production method of a soft magnetic manganese nickel zinc copper composite material, which except for step (3) 0.12wt% of 2 O 5 The procedure of example 2 was repeated except that 0.0001wt% was used instead.
Comparative example 6
This comparative example provides a production method of a soft magnetic manganese nickel zinc copper composite material, which except for step (3) 0.12wt% of 2 O 5 The procedure of example 2 was repeated except that 0.6% by weight was used instead.
Comparative example 7
This comparative example provides a method for preparing a soft magnetic manganese nickel zinc copper composite material, which is the same as that of example 2 except that the sintering temperature in step (4) was changed from 950 ℃ to 900 ℃.
Comparative example 8
This comparative example provides a method for preparing a soft magnetic manganese nickel zinc copper composite material, which is the same as that of example 2 except that the sintering temperature of 950 c in step (4) was replaced with 1100 c.
The soft magnetic manganese nickel zinc copper composite material sample rings obtained in the above examples and comparative examples were subjected to magnetic property test on an Hp4284A impedance analyzer, the test frequency of initial permeability was 10KHz, the test temperature range of specific temperature coefficient was-20 to 65 ℃, the test frequency of Q value and specific loss coefficient was 100KHz, the saturation magnetic flux density Bs was measured under a magnetic field of 4000A/m, the density of the soft magnetic manganese nickel zinc copper composite material was measured by a buoyancy method, and the results are shown in table 1.
TABLE 1
As can be seen from table 1:
(1) It can be seen from the comprehensive examples 1-3 that the soft magnetic manganese nickel zinc copper composite material prepared by the preparation method of the soft magnetic manganese nickel zinc copper composite material provided by the invention has excellent magnetic performance, the initial magnetic permeability can reach more than 800, and the density can reach 5.05kg/m 3 Above, in the temperature range of-20 to 65 ℃, the specific temperature coefficient is lower than 7.0 multiplied by 10 -6 (ii) a At a frequency of 100kHz, the specific loss factor is lower than 10 multiplied by 10 -6 (ii) a Under the test magnetic field of 4000A/m, the saturation magnetic flux density can reach more than 420 mT; curie temperature can reach over 160 ℃; the quality factor can reach more than 85;
(2) As can be seen by combining example 2 with comparative examples 1 to 2, ni in comparative example 1 2 O 3 Is lower in mole percentage than in comparative example 2 2 O 3 The mole percentage content of the Ni-Zn-Cu alloy is higher, the initial magnetic permeability, the specific temperature coefficient, the specific loss coefficient, the saturation magnetic flux density and the quality factor of the obtained soft magnetic manganese-nickel-zinc-copper composite material are all greatly reduced, and the Ni in the comparative example 2 2 O 3 The molar percentage content of the raw materials is higher, and the cost of the raw materials is also higher; it is thus shown that the present invention defines Ni 2 O 3 The molar percentage of the soft magnetic manganese-nickel-zinc-copper composite material is in a specific range, so that the prepared soft magnetic manganese-nickel-zinc-copper composite material has excellent magnetic performance, and the cost of raw materials can be reduced;
(3) As can be seen by combining example 2 with comparative examples 3 to 6, bi in comparative example 3 2 O 3 Is lower in mol% than in comparative example 4 2 O 3 Is higher in mol% than in comparative example 5, V 2 O 5 In lower mole percent, comparative example 6, V 2 O 5 The molar percentage content of the composite material is higher, and the magnetic performance and quality factors of the finally prepared soft magnetic manganese-nickel-zinc-copper composite material are greatly reduced; it is thus shown that the present invention is limited to the use of a specific molar percentage of Bi 2 O 3 And V 2 O 5 As a fluxing agent, the soft magnetic manganese nickel zinc copper composite material with excellent magnetic property can be obtained;
(4) It can be seen from the combination of the embodiment 2 and the comparative examples 7 to 8 that the sintering temperature in the comparative example 7 is low, and the magnetic property of the prepared soft magnetic manganese nickel zinc copper composite material is greatly reduced; the temperature of the sintering treatment in the comparative example 8 is higher, which not only wastes a large amount of energy, but also has higher design requirements on sintering equipment, further increases the production cost of the soft magnetic manganese nickel zinc copper composite material, and the magnetic performance of the obtained soft magnetic manganese nickel zinc copper composite material is poorer than that of the embodiment 2; therefore, the invention only needs to carry out sintering treatment in a specific lower temperature range, and the soft magnetic manganese nickel zinc copper composite material with excellent magnetic property can be obtained.
The applicant declares that the above description is only a specific embodiment of the present invention, but the scope of the present invention is not limited thereto, and it should be understood by those skilled in the art that any changes or substitutions that can be easily conceived by those skilled in the art within the technical scope of the present invention disclosed herein fall within the scope and disclosure of the present invention.
Claims (10)
1. The soft magnetic manganese nickel zinc copper composite material is characterized in that the main phase of the soft magnetic manganese nickel zinc copper composite material is in a spinel structure, and the soft magnetic manganese nickel zinc copper composite material comprises a main component and a fluxing agent component;
the content of the main components calculated by oxide comprises: fe 2 O 3 :45~50mol%、ZnO:5~25mo1%、CuO:3~20mo1%、MnO 2 1-3 mo1% and Ni 2 O 3 :10~18mol%;
The fluxing agent comprises the following components in percentage by mass of the total mass of the main components: bi 2 O 3 0.01 to 0.5wt% and V 2 O 5 :0.01~0.4wt%。
2. A method for preparing a soft magnetic manganese nickel zinc copper composite material according to claim 1, characterized in that the method comprises the following steps:
(1) Weighing raw materials according to the formula of the main components, and performing first ball milling mixing to obtain a mixed material;
(2) After the mixed material is dried, pre-burning treatment is carried out at the temperature of 720-780 ℃ to obtain a pre-burned material;
(3) Mixing the pre-sintered material and a fluxing agent raw material weighed according to a fluxing agent component formula, and performing second ball milling mixing to obtain a semi-finished product material;
(4) And drying the semi-finished product material, mixing the dried semi-finished product material with polyethylene ethanol, and sequentially performing screen granulation, compression molding and sintering treatment at the temperature of 950-1000 ℃ to obtain the soft magnetic manganese nickel zinc copper composite material.
3. The preparation method according to claim 2, characterized in that deionized water with the same mass as that of the main component raw materials is added in the first ball-milling mixing in the step (1);
preferably, the rotating speed of the first ball milling mixing is 300-330 r/min;
preferably, the ratio of the first ball milling and mixing material balls is 1 (6-6.5);
preferably, the time for the first ball milling mixing is 2 to 4 hours.
4. The preparation method according to claim 2 or 3, wherein the pre-burning treatment in the step (2) is performed for 2 to 4 hours;
preferably, the atmosphere of the pre-sintering treatment is air, and the pre-sintering material is cooled along with the furnace after the pre-sintering treatment.
5. The method according to any one of claims 2 to 4, wherein Bi in the flux component in the step (3) is Bi 2 O 3 The average particle size of (B) is 59-65 nm;
preferably, V in the flux component 2 O 5 Has an average particle size of 80 to 86nm.
6. The preparation method according to any one of claims 2 to 5, characterized in that deionized water equal to the total mass of the pre-sintering material and the raw materials of the fluxing agent is added in the second ball-milling mixing in the step (3);
preferably, the rotating speed of the second ball milling mixing is 300-330 r/min;
preferably, the ratio of the material balls of the second ball-milling mixing is 1 (6-6.5);
preferably, the time for the second ball milling and mixing is 3-15 h;
preferably, the mean particle size of the semi-finished product mass is <0.8 μm.
7. The process according to any one of claims 2 to 6, wherein the amount of the polyvinyl alcohol added in step (4) is 8 to 15wt% of the semi-finished material.
8. The production method according to any one of claims 2 to 7, wherein the heat-retaining time for the sintering treatment in step (4) is 6 to 8 hours;
preferably, the atmosphere of the sintering treatment is air, and the furnace is cooled after the sintering treatment.
9. The production method according to any one of claims 2 to 8, characterized by comprising the steps of:
(1) Weighing the raw materials according to the formula of the main component, and carrying out first ball milling and mixing for 2-4 h at the rotating speed of 300-330 r/min and the material-ball ratio of 1 (6-6.5) to obtain a mixed material; deionized water with the same mass as the main component raw materials is added into the first ball-milling mixing;
(2) After the mixed material is dried, pre-sintering treatment is carried out for 2-4 h at the temperature of 720-780 ℃ to obtain a pre-sintered material; the atmosphere of the pre-burning treatment is air, and the pre-burning materials are cooled along with the furnace after the pre-burning treatment;
(3) Mixing the pre-sintered material and flux raw materials weighed according to the flux component formula, and performing second ball milling and mixing for 3-15 h at the rotating speed of 300-330 r/min and the material-ball ratio of 1 (6-6.5) to obtain the average particle size<0.8 μm of semi-finished material; bi in the flux component 2 O 3 The average particle size of (B) is 59-65 nm; v in the flux component 2 O 5 The average particle size of (a) is 80-86 nm; adding deionized water with the mass equal to the total mass of the pre-sintering material and the fluxing agent raw material into the second ball milling mixing;
(4) After the semi-finished product material is dried, mixing the semi-finished product material with polyethylene ethanol, and sequentially carrying out sieving granulation, compression molding and sintering treatment at the temperature of 950-1000 ℃ for 6-8 h to obtain the soft magnetic manganese-nickel-zinc-copper composite material; the addition amount of the polyethylene ethanol is 8-15 wt% of the semi-finished product material; the atmosphere of the sintering treatment is air, and the sintering treatment is carried out and then the furnace is cooled.
10. Use of the soft magnetic manganese nickel zinc copper composite material according to claim 1 in the field of electronic communications.
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