CN115010479B - Shrinkage-free nickel-copper-zinc ferrite material and preparation method thereof - Google Patents

Shrinkage-free nickel-copper-zinc ferrite material and preparation method thereof Download PDF

Info

Publication number
CN115010479B
CN115010479B CN202210718958.9A CN202210718958A CN115010479B CN 115010479 B CN115010479 B CN 115010479B CN 202210718958 A CN202210718958 A CN 202210718958A CN 115010479 B CN115010479 B CN 115010479B
Authority
CN
China
Prior art keywords
shrinkage
copper
zinc ferrite
average particle
preparation
Prior art date
Legal status (The legal status is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the status listed.)
Active
Application number
CN202210718958.9A
Other languages
Chinese (zh)
Other versions
CN115010479A (en
Inventor
陈军林
张利康
Current Assignee (The listed assignees may be inaccurate. Google has not performed a legal analysis and makes no representation or warranty as to the accuracy of the list.)
Hengdian Group DMEGC Magnetics Co Ltd
Original Assignee
Hengdian Group DMEGC Magnetics Co Ltd
Priority date (The priority date is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the date listed.)
Filing date
Publication date
Application filed by Hengdian Group DMEGC Magnetics Co Ltd filed Critical Hengdian Group DMEGC Magnetics Co Ltd
Priority to CN202210718958.9A priority Critical patent/CN115010479B/en
Publication of CN115010479A publication Critical patent/CN115010479A/en
Application granted granted Critical
Publication of CN115010479B publication Critical patent/CN115010479B/en
Active legal-status Critical Current
Anticipated expiration legal-status Critical

Links

Classifications

    • 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
    • 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
    • C04B35/622—Forming processes; Processing powders of inorganic compounds preparatory to the manufacturing of ceramic products
    • 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
    • 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
    • C04B2235/00—Aspects relating to ceramic starting mixtures or sintered ceramic products
    • C04B2235/02—Composition of constituents of the starting material or of secondary phases of the final product
    • C04B2235/30—Constituents and secondary phases not being of a fibrous nature
    • C04B2235/32—Metal oxides, mixed metal oxides, or oxide-forming salts thereof, e.g. carbonates, nitrates, (oxy)hydroxides, chlorides
    • C04B2235/3231—Refractory metal oxides, their mixed metal oxides, or oxide-forming salts thereof
    • C04B2235/3239—Vanadium oxides, vanadates or oxide forming salts thereof, e.g. magnesium vanadate
    • 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
    • C04B2235/00—Aspects relating to ceramic starting mixtures or sintered ceramic products
    • C04B2235/02—Composition of constituents of the starting material or of secondary phases of the final product
    • C04B2235/30—Constituents and secondary phases not being of a fibrous nature
    • C04B2235/32—Metal oxides, mixed metal oxides, or oxide-forming salts thereof, e.g. carbonates, nitrates, (oxy)hydroxides, chlorides
    • C04B2235/327—Iron group oxides, their mixed metal oxides, or oxide-forming salts thereof
    • C04B2235/3279—Nickel oxides, nickalates, or oxide-forming salts thereof
    • 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
    • C04B2235/00—Aspects relating to ceramic starting mixtures or sintered ceramic products
    • C04B2235/02—Composition of constituents of the starting material or of secondary phases of the final product
    • C04B2235/30—Constituents and secondary phases not being of a fibrous nature
    • C04B2235/32—Metal oxides, mixed metal oxides, or oxide-forming salts thereof, e.g. carbonates, nitrates, (oxy)hydroxides, chlorides
    • C04B2235/3281—Copper oxides, cuprates or oxide-forming salts thereof, e.g. CuO or Cu2O
    • 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
    • C04B2235/00—Aspects relating to ceramic starting mixtures or sintered ceramic products
    • C04B2235/02—Composition of constituents of the starting material or of secondary phases of the final product
    • C04B2235/30—Constituents and secondary phases not being of a fibrous nature
    • C04B2235/32—Metal oxides, mixed metal oxides, or oxide-forming salts thereof, e.g. carbonates, nitrates, (oxy)hydroxides, chlorides
    • C04B2235/3284—Zinc oxides, zincates, cadmium oxides, cadmiates, mercury oxides, mercurates or oxide forming salts thereof
    • 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
    • C04B2235/00—Aspects relating to ceramic starting mixtures or sintered ceramic products
    • C04B2235/02—Composition of constituents of the starting material or of secondary phases of the final product
    • C04B2235/30—Constituents and secondary phases not being of a fibrous nature
    • C04B2235/32—Metal oxides, mixed metal oxides, or oxide-forming salts thereof, e.g. carbonates, nitrates, (oxy)hydroxides, chlorides
    • C04B2235/3296—Lead oxides, plumbates or oxide forming salts thereof, e.g. silver plumbate
    • 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
    • C04B2235/00—Aspects relating to ceramic starting mixtures or sintered ceramic products
    • C04B2235/02—Composition of constituents of the starting material or of secondary phases of the final product
    • C04B2235/30—Constituents and secondary phases not being of a fibrous nature
    • C04B2235/32—Metal oxides, mixed metal oxides, or oxide-forming salts thereof, e.g. carbonates, nitrates, (oxy)hydroxides, chlorides
    • C04B2235/3298—Bismuth oxides, bismuthates or oxide forming salts thereof, e.g. zinc bismuthate
    • 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
    • C04B2235/00—Aspects relating to ceramic starting mixtures or sintered ceramic products
    • C04B2235/02—Composition of constituents of the starting material or of secondary phases of the final product
    • C04B2235/30—Constituents and secondary phases not being of a fibrous nature
    • C04B2235/34—Non-metal oxides, non-metal mixed oxides, or salts thereof that form the non-metal oxides upon heating, e.g. carbonates, nitrates, (oxy)hydroxides, chlorides
    • C04B2235/3409—Boron oxide, borates, boric acids, or oxide forming salts thereof, e.g. borax
    • 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
    • C04B2235/00—Aspects relating to ceramic starting mixtures or sintered ceramic products
    • C04B2235/02—Composition of constituents of the starting material or of secondary phases of the final product
    • C04B2235/30—Constituents and secondary phases not being of a fibrous nature
    • C04B2235/40—Metallic constituents or additives not added as binding phase
    • C04B2235/405—Iron group metals
    • 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
    • C04B2235/00—Aspects relating to ceramic starting mixtures or sintered ceramic products
    • C04B2235/70—Aspects relating to sintered or melt-casted ceramic products
    • C04B2235/94—Products characterised by their shape
    • 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
    • C04B2235/00—Aspects relating to ceramic starting mixtures or sintered ceramic products
    • C04B2235/70—Aspects relating to sintered or melt-casted ceramic products
    • C04B2235/96—Properties of ceramic products, e.g. mechanical properties such as strength, toughness, wear resistance

Abstract

The invention relates to a shrinkage-free nickel-copper-zinc ferrite material and a preparation method thereof, wherein the preparation method comprises the following steps: firstly, niO, cuO, znO and Fe in a molar ratio 2 O 3 Mixing the raw materials in a ratio of (0.2:0.22:0.6:0.98), and sequentially performing first ball milling and drying to obtain mixed powder; then presintering the mixed powder to obtain a presintering material; then, mixing the presintered material and the supplementary material, adding an additive, and sequentially performing second ball milling, drying, granulating and compression molding to obtain a green body; the supplementary material comprises elementary iron, niO, cuO and ZnO; and finally, sintering the green body to obtain the shrinkage-free nickel-copper-zinc ferrite material. The non-shrinkage nickel-copper-zinc ferrite material is obtained by the preparation method. The shrinkage-free nickel-copper-zinc ferrite material provided by the invention can realize no shrinkage under low-temperature sintering, and has a uniform and compact structure. The preparation method provided by the invention is simple to operate and can be industrially applied.

Description

Shrinkage-free nickel-copper-zinc ferrite material and preparation method thereof
Technical Field
The invention relates to the technical field of permanent magnetic material ferrite, in particular to a shrinkage-free nickel-copper-zinc ferrite material and a preparation method thereof.
Background
As electronic devices are being developed in the direction of portability, miniaturization, networking, and multimedia, circuit assembly technology is rapidly being developed in the direction of surface mounting technology, and the core basis of such development is electronic materials. The main direction of electronic materials is laminated chip components with monolithic structures, in which chip capacitors and chip resistors are the main stream, and chip inductors are relatively backward. At present, the industrialized production of the laminated inductor is realized, and the co-firing matching of ferrite and silver electrodes is a technical key.
Ferrite materials generally need to meet the following characteristics: easy synthesis, low cost, low sintering temperature (co-firing with silver electrodes) and high performance (high permeability and high resistivity). The existing material for chip inductors is mainly concentrated on NiCuZn ferrite material sintered at low temperature, but the material has large magnetostriction coefficient and is sensitive to stress, the ferrite material can generate 10-15% dimensional shrinkage during sintering, the dimensional dispersion of products is large, and high dimensional accuracy is difficult to realize; in addition, the dimensional shrinkage can generate stress, strain, cracks and the like among different materials, so that the composite of the different materials is difficult to realize; moreover, the stress from the inner conductor and the stress generated at the time of mounting the substrate may also cause deterioration of the magnetic properties of the material.
CN107857581A discloses a low-temperature sintered NiCuZn ferrite material and a preparation method thereof, and a molecular junction of the material obtained by the methodThe structural expression is Ni 0.29-x-y Zn 0.53+x Cu 0.18+y Fe 1.95 O 4 (x=0-0.02; y=0-0.02) while using BBSZ glass, co 2 O 3 、TiO 2 And CaCO (CaCO) 3 As a dopant. Through the optimized design of the material formula and the process and the combination modification of 4 dopants, the low-temperature sintering at 900 ℃ is realized, and the initial permeability mu is taken into consideration i Between 80-96.
CN108503349A discloses a high-magnetic-field-resistant low-temperature sintered NiCuZn ferrite material and a preparation method thereof, wherein the method is based on the formula of the NiCuZn ferrite material and adopts 1 weight percent of Bi at the same time 2 O 3 And 2.5 to 3.5wt% Zn 2 SiO 4 The presintered materials are combined and doped, thereby realizing low-temperature sintering at 900 ℃ and initial permeability mu i Between 65.3 and 70.4.
CN113603472a discloses a preparation method of NiCuZn ferrite based on LTCC technology, which comprises steps of batching, first ball milling, first drying, presintering, doping, second ball milling, seventh drying, granulating, forming, discharging glue, sintering and the like, and comprises the steps of Bi 2 O 3 And Co 2 O 3 The NiCuZn ferrite with high density, small pore and excellent magnetic performance can be obtained by binary doping.
In summary, although many methods for preparing NiCuZn ferrite have been reported in the prior art, there is no effective solution for solving the problem of low-temperature sintering shrinkage of NiCuZn ferrite. Therefore, developing a nickel-copper-zinc ferrite material which is sintered at low temperature and has no shrinkage and a preparation method thereof has important significance for solving the problems of large size dispersion, poor high size precision, low magnetic performance and the like of the ferrite.
Disclosure of Invention
Compared with the prior art, the shrinkage-free nickel-copper-zinc ferrite material provided by the invention has the advantages that no shrinkage can be realized under low-temperature sintering, the microstructure is uniform and compact, the magnetic property is excellent, the preparation method provided by the invention is simple to operate, the cost is low, and the preparation method can be industrially applied.
In order to achieve the aim of the invention, the invention adopts the following technical scheme:
in a first aspect, the present invention provides a method for preparing a shrinkage-free nickel-copper-zinc ferrite material, the method comprising the steps of:
(1) According to the mole ratio of NiO to CuO to ZnO to Fe 2 O 3 Mixing the raw materials in a ratio of (1) =0.2:0.22:0.6:0.98, and then sequentially performing first ball milling and drying to obtain mixed powder;
(2) Presintering the mixed powder obtained in the step (1) to obtain a presintered material;
(3) Mixing the presintered material and the supplementary material obtained in the step (2), adding an additive, and then sequentially performing second ball milling, drying, granulating and compression molding to obtain a green body;
the supplementary material comprises elementary iron, niO, cuO and ZnO;
(4) And (3) sintering the green body obtained in the step (3) to obtain the shrinkage-free nickel-copper-zinc ferrite material.
The invention can realize the control of the ferrite size change rate by utilizing the oxidation expansion reaction of the metallic iron simple substance (iron powder). In one aspect, the molecular formula of the presintering material is controlled to be Ni 0.2 Cu 0.22 Zn 0.6 Fe 1.96 O x At the same time, the composition of the supplementary material is controlled, and the molecular formula of the product is kept unchanged finally, thereby obtaining Ni 0.2 Cu 0.22 Zn 0.6 Fe 1.96 O x The ferrite material, namely the invention, through controlling the presintering material and the supplementary material, can freely regulate and control the dimensional change from shrinkage to expansion by changing the ratio of the presintering material and the supplementary material, so as to finally realize the dimensional change rate of 0. On the other hand, the metal iron simple substance is accompanied with uneven grain growth under sintering, so the invention also ensures that the low-melting point oxide additive supplies the metal iron simple substance and surrounding oxides with oxygen in the sintering process by controlling the synergistic effect of the metal iron simple substance and the low-melting point oxide additive, thereby further realizing ferrite promotion, ensuring that the ferrite structure is uniform and completeEliminating residual metallic iron.
Preferably, the average particle size of the powder mixture in step (1) is 1.5-1.9. Mu.m, for example, 1.5. Mu.m, 1.6. Mu.m, 1.7. Mu.m, 1.8. Mu.m, or 1.9. Mu.m, but not limited to the values recited, and other values not recited in the numerical range are equally applicable.
Preferably, the drying temperature in step (1) is 150-200deg.C, such as 150 deg.C, 160 deg.C, 170 deg.C, 180 deg.C, 190 deg.C or 200 deg.C, but not limited to the values recited, and other values not recited in the range of values are equally applicable.
Preferably, the temperature of the pre-sintering in the step (2) is 850-1050 ℃, for example, 850 ℃, 900 ℃, 950 ℃, 1000 ℃ or 1050 ℃, but the pre-sintering is not limited to the listed values, and other non-listed values in the numerical range are applicable.
Preferably, the burn-in time is 1.5-2.5h, for example, 1.5h, 1.6h, 1.7h, 1.8h, 1.9h, 2.0h, 2.1h, 2.2h, 2.3h, 2.4h or 2.5h, but not limited to the recited values, and other non-recited values within the range are equally applicable.
Preferably, the volume of the supplement material in the step (3) is 60-65% of the volume of the presintered material, for example, 60%, 61%, 62%, 63%, 64% or 65%, but not limited to the recited values, and other non-recited values in the range are equally applicable.
The invention preferably controls the volume of the supplementary material to be the percentage of the volume of the presintering material, thereby enhancing the magnetism of ferrite while controlling the size change rate.
Preferably, the mole ratio of elemental iron, niO, cuO and ZnO in the supplement is 1.96:0.2:0.22:0.6.
The invention preferably controls the mole ratio of elementary iron, niO, cuO and ZnO to be 1.96:0.2:0.22:0.6 because the combination of the elementary iron and oxygen is controlled, and the components in the supplement are oxidized and expanded into ferrite, specifically as follows, wherein (alpha=0.99-1.49):
(1.96Fe+0.2NiO+0.22CuO+0.6ZnO)+αO 2 →Ni 0.2 Cu 0.22 Zn 0.6 Fe 1.96 O x
preferably, the average particle size of the pre-sintering material in step (3) is 0.8-1.2 μm, for example, 0.8 μm, 0.9 μm, 1.0 μm, 1.1 μm or 1.2 μm, but not limited to the recited values, and other non-recited values within the range of values are equally applicable.
Preferably, the average particle size of the elemental iron in the supplement is 7-9 μm, for example, 7 μm, 7.2 μm, 7.4 μm, 7.6 μm, 7.8 μm, 8 μm, 8.2 μm, 8.4 μm, 8.6 μm, 8.8 μm or 9 μm, but not limited to the recited values, other non-recited values within the range of values are equally applicable.
The invention preferably controls the average grain diameter of the iron simple substance in the supplementary material in a specific range, can control the size change rate and improves the magnetism and the uniformity.
The average particle size of NiO in the supplement is preferably 1-1.4. Mu.m, for example 1 μm, 1.1 μm, 1.2 μm, 1.3 μm or 1.4. Mu.m, but is not limited to the values recited, and other values not recited in the numerical range are equally applicable.
The average particle size of the CuO in the supplement is preferably 0.8-1.2 μm, for example, 0.8 μm, 0.9 μm, 1.0 μm, 1.1 μm or 1.2 μm, but is not limited to the values recited, and other values not recited in the numerical range are equally applicable.
Preferably, the average particle size of the ZnO in the supplement is 0.6-1 μm, for example, 0.6 μm, 0.7 μm, 0.8 μm, 0.9 μm or 1 μm, but not limited to the recited values, other non-recited values within the range of values are equally applicable.
Preferably, the additive of step (3) comprises Bi 2 O 3 、V 2 O 5 、B 2 O 3 Or PbO, wherein the typical but non-limiting combination comprises Bi 2 O 3 And V 2 O 5 V of the combination of (2) 2 O 5 And B 2 O 3 Or V of (2) 2 O 5 、B 2 O 3 And PbO, preferably Bi 2 O 3 And/or PbO.
Preferably, the additive is 0.4-0.6% by mass of the sum of the pre-sintering material and the supplementary material, for example, 0.4%, 0.42%, 0.44%, 0.46%, 0.48%, 0.5%, 0.52%, 0.54%, 0.56%, 0.58% or 0.6%, but not limited to the recited values, and other non-recited values in the numerical range are equally applicable.
The invention preferably controls the quality of the additive in a specific range, and can improve the uniformity and magnetism of ferrite.
Preferably, the average particle diameter after the second ball milling in the step (3) is 0.8-1.2 μm, for example, 0.8 μm, 0.9 μm, 1 μm, 1.1 μm or 1.2 μm, but not limited to the recited values, and other non-recited values in the numerical range are equally applicable.
Preferably, the temperature of the drying in step (3) is 150-200 ℃, for example 150 ℃, 160 ℃, 170 ℃, 180 ℃, 190 ℃ or 200 ℃, but not limited to the values listed, and other values not listed in the range of values are equally applicable.
Preferably, the granulated binder comprises polyvinyl alcohol.
Preferably, the pressure of the press molding is 280-320MPa, for example, 280MPa, 290MPa, 300MPa, 310MPa or 320MPa, but not limited to the values listed, and other values not listed in the numerical range are equally applicable.
Preferably, the sintering temperature in step (4) is 900-920 ℃, and may be 900 ℃, 902 ℃, 904 ℃, 906 ℃, 908 ℃, 910 ℃, 912 ℃, 914 ℃, 916 ℃, 918 ℃, or 920 ℃, for example, but not limited to the recited values, and other values not recited in the numerical range are equally applicable.
Preferably, the sintering time is 5.5-6.5h, for example, 5.5h, 5.6h, 5.7h, 5.8h, 5.9h, 6h, 6.1h, 6.2h, 6.3h, 6.4h or 6.5h, but not limited to the recited values, other non-recited values within the range of values are equally applicable.
As a preferred technical solution of the first aspect of the present invention, the preparation method includes the following steps:
(1) According to the mole ratio of NiO to CuO to ZnO to Fe 2 O 3 Raw materials are mixed in a ratio of =0.2:0.22:0.6:0.98, then subjected to a first ball milling, then dried at 150-200 ℃,obtaining mixed powder, wherein the average grain diameter of the mixed powder is 1.5-1.9 mu m;
(2) Presintering the mixed powder obtained in the step (1) for 1.5-2.5 hours at 850-1050 ℃ to obtain a presintering material;
(3) Mixing the pre-sintering material and the supplementary material obtained in the step (2), wherein the volume of the supplementary material is 60-65% of that of the pre-sintering material, the molar ratio of elementary iron, niO, cuO and ZnO in the supplementary material is 1.96:0.2:0.22:0.6, and then adding additives, and the additives comprise Bi 2 O 3 、V 2 O 5 、B 2 O 3 Or any one or the combination of at least two of PbO, wherein the mass of the additive is 0.4-0.6% of the sum of the mass of the presintered material and the mass of the supplement material, the mixture is subjected to second ball milling until the average particle size is 0.8-1.2 mu m, the mixture is dried at 150-200 ℃, polyvinyl alcohol is added for granulation, and the mixture is subjected to compression molding at 280-320MPa to obtain a green body;
(4) Sintering the green body obtained in the step (3) for 5.5-6.5 hours at 900-920 ℃ to obtain the shrinkage-free nickel-copper-zinc ferrite material.
In the invention, the non-shrink nickel copper zinc ferrite material is subsequently processed into a ring shape
Figure BDA0003709714930000071
Is a circular sample of (a).
In a second aspect, the present invention also provides a non-shrink nickel-copper-zinc ferrite material obtained by the preparation method of the non-shrink nickel-copper-zinc ferrite material according to the first aspect of the present invention, wherein the molecular structural expression of the non-shrink nickel-copper-zinc ferrite material is Ni 0.2 Cu 0.22 Zn 0.6 Fe 1.96 O x Wherein x ranges from 3 to 4.
Where x is in the range of 3 to 4, for example, 3.2, 3.4, 3.6, 3.8 or 4, but is not limited to the values recited, and other values not recited in the range are equally applicable.
The shrinkage-free nickel-copper-zinc ferrite material provided by the invention can control the change rate of the size to be almost 0 during low-temperature sintering by utilizing the oxidation expansion reaction of the metal Fe simple substance, and has uniform and compact microstructure.
Compared with the prior art, the invention has the following beneficial effects:
(1) The preparation method of the shrinkage-free nickel-copper-zinc ferrite material can freely regulate and control the dimensional change from shrinkage to expansion by changing the ratio of the pre-sintering material and the supplementary material, can realize that the ferrite does not shrink under low-temperature sintering, and promotes homogenization and densification of the ferrite.
(2) The shrinkage-free nickel-copper-zinc ferrite material provided by the invention has no dimensional shrinkage under low-temperature sintering, uniform and compact structure, excellent magnetic performance and initial permeability mu i The size change rate can reach more than 525 and more than-0.65 percent.
Detailed Description
The technical scheme of the invention is further described by the following specific embodiments. It will be apparent to those skilled in the art that the examples are merely to aid in understanding the invention and are not to be construed as a specific limitation thereof.
Example 1
The embodiment provides a preparation method of a shrinkage-free nickel-copper-zinc ferrite material, which comprises the following steps:
(1) According to the mole ratio of NiO to CuO to ZnO to Fe 2 O 3 Mixing the raw materials in a ratio of=0.2:0.22:0.6:0.98, then performing first ball milling, and then drying at 175 ℃ to obtain a mixed powder, wherein the average particle size of the mixed powder is 1.7 μm;
(2) Presintering the mixed powder obtained in the step (1) for 2 hours at 950 ℃ to obtain a presintering material;
(3) Mixing the pre-sintering material and the supplementary material obtained in the step (2), wherein the volume of the supplementary material is 62% of that of the pre-sintering material, the molar ratio of the elementary iron, niO, cuO and ZnO in the supplementary material is 1.96:0.2:0.22:0.6, and then adding Bi 2 O 3 An additive, the mass of the additive is 0.5 percent of the sum of the mass of the presintering material and the mass of the supplement material, the average grain diameter of the presintering material is 1 mu m, the average grain diameter of the elementary iron in the supplement material is 8 mu m, the average grain diameter of NiO is 1.2 mu m, the average grain diameter of CuO is 1 mu m, and the average grain diameter of ZnOThe average particle diameter was 0.8. Mu.m;
then carrying out second ball milling until the average grain diameter is 1 mu m, drying at 175 ℃, adding polyvinyl alcohol for granulating, and carrying out compression molding at 300MPa to obtain a green body;
(4) And (3) sintering the green body obtained in the step (3) for 6 hours at the temperature of 910 ℃ to obtain the shrinkage-free nickel-copper-zinc ferrite material.
The embodiment also provides a non-shrinkage nickel-copper-zinc ferrite material obtained by the preparation method, wherein the molecular structural expression of the non-shrinkage nickel-copper-zinc ferrite material is Ni 0.2 Cu 0.22 Zn 0.6 Fe 1.96 O 4 。
Example 2
The embodiment provides a preparation method of a shrinkage-free nickel-copper-zinc ferrite material, which comprises the following steps:
(1) According to the mole ratio of NiO to CuO to ZnO to Fe 2 O 3 Mixing the raw materials in a ratio of=0.2:0.22:0.6:0.98, then performing first ball milling, and then drying at 150 ℃ to obtain a mixed powder, wherein the average particle size of the mixed powder is 1.9 μm;
(2) Presintering the mixed powder obtained in the step (1) for 2.5 hours at 850 ℃ to obtain a presintering material;
(3) Mixing the pre-sintering material and the supplementary material obtained in the step (2), wherein the volume of the supplementary material is 60% of that of the pre-sintering material, the molar ratio of the elementary iron, niO, cuO and ZnO in the supplementary material is 1.96:0.2:0.22:0.6, and then adding Bi 2 O 3 And V 2 O 5 The mass of the additive is 0.6% of the sum of the mass of the presintering material and the mass of the supplementary material, the average particle size of the presintering material is 0.8 mu m, the average particle size of the elementary iron in the supplementary material is 9 mu m, the average particle size of NiO is 1 mu m, the average particle size of CuO is 1.2 mu m, and the average particle size of ZnO is 0.6 mu m;
performing second ball milling until the average grain diameter is 0.8 mu m, drying at 150 ℃, adding polyvinyl alcohol for granulating, and performing compression molding at 320MPa to obtain a green body;
(4) Sintering the green body obtained in the step (3) for 6.5 hours at 900 ℃ to obtain the shrinkage-free nickel-copper-zinc ferrite material.
The embodiment also provides a non-shrinkage nickel-copper-zinc ferrite material obtained by the preparation method, wherein the molecular structural expression of the non-shrinkage nickel-copper-zinc ferrite material is Ni 0.2 Cu 0.22 Zn 0.6 Fe 1.96 O 4 。
Example 3
The embodiment provides a preparation method of a shrinkage-free nickel-copper-zinc ferrite material, which comprises the following steps:
(1) According to the mole ratio of NiO to CuO to ZnO to Fe 2 O 3 Mixing the raw materials in a ratio of=0.2:0.22:0.6:0.98, then performing first ball milling, and then drying at 200 ℃ to obtain mixed powder, wherein the average particle size of the mixed powder is 1.5 μm;
(2) Presintering the mixed powder obtained in the step (1) for 1.5 hours at 1050 ℃ to obtain a presintering material;
(3) Mixing the presintering material and the supplementary material obtained in the step (2), wherein the volume of the supplementary material is 65% of that of the presintering material, the molar ratio of the elementary iron, niO, cuO and ZnO in the supplementary material is 1.96:0.2:0.22:0.6, and then adding B 2 O 3 And a PbO additive, wherein the mass of the additive is 0.4 percent of the sum of the mass of the presintering material and the mass of the supplementary material, the average particle size of the presintering material is 1.2 mu m, the average particle size of the elementary iron in the supplementary material is 7 mu m, the average particle size of NiO is 1.4 mu m, the average particle size of CuO is 0.8 mu m, and the average particle size of ZnO is 1 mu m;
then carrying out second ball milling until the average grain diameter is 1.2 mu m, drying at 200 ℃, adding polyvinyl alcohol for granulating, and carrying out compression molding at 280MPa to obtain a green body;
(4) Sintering the green body obtained in the step (3) for 5.5 hours at the temperature of 920 ℃ to obtain the shrinkage-free nickel-copper-zinc ferrite material.
The embodiment also provides a non-shrinkage nickel-copper-zinc ferrite material obtained by the preparation method, wherein the molecular structural expression of the non-shrinkage nickel-copper-zinc ferrite material is Ni 0.2 Cu 0.22 Zn 0.6 Fe 1.96 O 4 。
Example 4
This example provides a method of preparing a shrink-free nickel copper zinc ferrite material that differs from example 1 only in that the volume of the supplement is 50% of the volume of the pre-sinter.
Example 5
This example provides a method of preparing a shrink-free nickel copper zinc ferrite material that differs from example 1 only in that the volume of the supplement is 70% of the volume of the pre-sinter.
Example 6
This example provides a method for preparing a shrinkage-free nickel copper zinc ferrite material, which differs from example 1 only in that the average particle size of the elemental iron in the supplement is 6 μm.
Example 7
This example provides a method for preparing a shrinkage-free nickel copper zinc ferrite material, which differs from example 1 only in that the average particle size of the elemental iron in the supplement is 10 μm.
Example 8
This example provides a method of preparing a shrink-free nickel copper zinc ferrite material that differs from example 1 only in that the mass of the additive is 0.2% of the sum of the mass of the pre-sinter and the supplement.
Example 9
This example provides a method of preparing a shrink-free nickel copper zinc ferrite material that differs from example 1 only in that the mass of the additive is 0.8% of the sum of the mass of the pre-sinter and the make-up.
Comparative example 1
This comparative example provides a method for preparing a shrinkage-free nickel copper zinc ferrite material, which differs from example 1 only in that Bi is not added 2 O 3 。
Comparative example 2
The comparative example provides a preparation method of a non-shrink nickel copper zinc ferrite material, which is different from example 1 only in that no supplementary material is added, additives are directly added into the pre-sintered material, and then the pre-sintered material is subjected to second ball milling, drying, granulation and compression molding to obtain a green compact, and then the non-shrink nickel copper zinc ferrite material is obtained through sintering.
Comparative example 3
This comparative example provides a method of preparing a shrinkage-free nickel copper zinc ferrite material, which differs from example 1 only in that the pre-firing material is added with the additive and then mixed with the supplemental material.
Initial permeability μ of the non-shrink Nickel copper Zinc ferrite materials prepared in examples 1-9 and comparative examples 1-3 using an Agilent E4980A LCR tester i The measurement was performed, and the results are shown in table 1.
The change rate of the shrinkage-free nickel-copper-zinc ferrite materials prepared in examples 1 to 9 and comparative examples 1 to 3 was measured by: the green body was heated at 5 ℃/min by a thermo-mechanical analysis device (TMA) measurement, and the dimensional change rate= (outer diameter of sintered body-outer diameter of green body)/outer diameter of green body, the sintered body was the produced shrink-free nickel copper zinc ferrite material, and the results are shown in table 1.
TABLE 1
μ i Initial permeability Dimensional change rate/%
Example 1 550 -0.4％
Example 2 548 -0.42％
Example 3 543 -0.48％
Example 4 539 -0.53％
Example 5 536 -0.56％
Example 6 534 -0.59％
Example 7 530 -0.60％
Example 8 528 -0.62％
Example 9 525 -0.65％
Comparative example 1 413 -0.7％
Comparative example 2 406 -0.73％
Comparative example 3 397 -0.75％
From table 1, the following points can be seen:
(1) As can be seen from the data of examples 1-9, the non-shrinkage nickel-copper-zinc ferrite material provided by the invention has excellent magnetic properties, almost has no shrinkage under low-temperature sintering, and has an initial magnetic permeability of more than 525% and a dimensional change rate of more than-0.65%.
(2) As can be seen from a combination of the data from examples 1 and examples 4-5, the volume of the supplement in example 1 was 62% of the volume of the pre-sintered material, as compared to 50% and 70% of the initial permeability μ in example 1 in examples 4-5, respectively i 550, the dimensional change rate is-0.4%, and the initial permeability in examples 4-5 is lower than that in example 1, and the dimensional change rate in examples 4-5 is lower than that in example 1, so that the invention preferably controls the volume of the supplement material to the volume of the presintered material to be in a specific range, thereby improving the magnetic property of ferrite and reducing shrinkage.
(3) As can be seen from a combination of the data of examples 1 and examples 6 to 7, the average particle diameter of the elemental iron in the supplement of example 1 was 8. Mu.m, compared with the initial permeability. Mu.m, of examples 6 to 7 of 6 μm and 10. Mu.m, respectively, in example 1 i 550, the dimensional change rate is-0.4%, and the initial permeability in examples 6-7 is lower than that in example 1, and the dimensional change rate in examples 6-7 is lower than that in example 1, so that the invention preferably controls the average grain size of the elementary iron in the supplement to be in a specific range, thereby improving the magnetic property of ferrite and reducing shrinkage.
(4) As can be seen from a combination of the data of examples 1 and examples 8-9, the mass of the additive in example 1 is 0.5% of the sum of the mass of the pre-sinter and the supplement, compared to 0.2% and 0.8% of the initial permeability μ in example 1, respectively, in examples 8-9 i 550, the dimensional change rate is-0.4%, and the initial permeability in examples 8-9 is lower than that in example 1, and the dimensional change rate in examples 8-9 is lower than that in example 1, so that the invention preferably controls the percentage of the mass of the additive to the sum of the mass of the presintered material and the mass of the supplement material in a specific range, thereby improving the magnetic property of the ferrite and reducing shrinkage.
(5) As can be seen from a combination of the data of comparative example 1 and comparative examples 1-2, comparative example 1 differs from example 1 only in that Bi was not added 2 O 3 Comparative example 2 differs from example 1 only in that no supplement is added, the initial permeability μ in example 1 i 550, the dimensional change rate is-0.4%, and the initial permeability in comparative examples 1-2 is lower than that in example 1, and the dimensional change rate in comparative examples 1-2 is lower than that in example 1, so that the preparation method provided by the invention can improve the magnetic property of ferrite and reduce shrinkage.
(6) From a combination of the data of comparative example 1 and comparative example 3, it can be seen that comparative example 3 differs from example 1 only in that the additive is added to the pre-sintered material and then mixed with the supplement, and that the initial permeability and dimensional change rate of comparative example 3 are smaller than those of example 1, and thus, the shrinkage can be reduced while improving the magnetic properties of ferrite by adding the additive to the pre-sintered material and then mixing with the supplement.
In conclusion, the shrinkage-free nickel-copper-zinc ferrite material provided by the invention has no dimensional shrinkage under low-temperature sintering, uniform and compact structure and excellent magnetic property, and the preparation method provided by the invention is simple to operate and can be industrially applied.
The applicant declares that the above is only a specific embodiment of the present invention, but the scope of the present invention is not limited thereto, and it should be apparent to those skilled in the art that any changes or substitutions that are easily conceivable within the technical scope of the present invention disclosed by the present invention fall within the scope of the present invention and the disclosure.

Claims (19)

1. The preparation method of the shrinkage-free nickel-copper-zinc ferrite material is characterized by comprising the following steps of:
(1) According to the mole ratio of NiO to CuO to ZnO to Fe 2 O 3 Mixing the raw materials in a ratio of (1) =0.2:0.22:0.6:0.98, and then sequentially performing first ball milling and drying to obtain mixed powder;
(2) Presintering the mixed powder obtained in the step (1) to obtain a presintered material;
(3) Mixing the pre-firing material and the supplementary material obtained in the step (2), and then adding additives, wherein the additives comprise Bi 2 O 3 、V 2 O 5 、B 2 O 3 Or any one or the combination of at least two of PbO, wherein the mass of the additive is 0.4-0.6% of the sum of the mass of the presintered material and the mass of the supplement material, and then the mixture is subjected to second ball milling, drying, granulating and press forming in sequence to obtain a green body;
the supplementary material comprises elementary iron, niO, cuO and ZnO;
the volume of the supplementary material is 60-65% of the volume of the presintered material;
the mol ratio of the elementary iron, niO, cuO and ZnO in the supplement is 1.96:0.2:0.22:0.6;
(4) And (3) sintering the green body obtained in the step (3) to obtain the shrinkage-free nickel-copper-zinc ferrite material.
2. The process according to claim 1, wherein the average particle size of the powder mixture in step (1) is 1.5 to 1.9. Mu.m.
3. The method of claim 1, wherein the drying in step (1) is performed at a temperature of 150-200 ℃.
4. The method of claim 1, wherein the pre-firing in step (2) is performed at a temperature of 850-1050 ℃.
5. The method of claim 1, wherein the pre-firing time is 1.5-2.5 hours.
6. The method according to claim 1, wherein the average particle size of the pre-firing material in the step (3) is 0.8 to 1.2 μm.
7. The method according to claim 1, wherein the average particle size of the elemental iron in the supplement is 7-9 μm.
8. The preparation method according to claim 1, wherein the average particle size of NiO in the supplement is 1-1.4 μm.
9. The preparation method according to claim 1, wherein the average particle diameter of CuO in the supplement is 0.8 to 1.2 μm.
10. The method according to claim 1, wherein the average particle size of ZnO in the supplement is 0.6-1 μm.
11. The method according to claim 1, wherein the additive in the step (3) is Bi 2 O 3 And/or PbO.
12. The method according to claim 1, wherein the average particle diameter after the second ball milling in the step (3) is 0.8 to 1.2. Mu.m.
13. The method of claim 1, wherein the drying in step (3) is performed at a temperature of 150-200 ℃.
14. The method of claim 1, wherein the granulated binder comprises polyvinyl alcohol.
15. The method according to claim 1, wherein the pressure of the press molding is 280 to 320MPa.
16. The method of claim 1, wherein the sintering temperature in step (4) is 900-920 ℃.
17. The method of claim 1, wherein the sintering time is 5.5 to 6.5 hours.
18. The preparation method according to claim 1, characterized in that the preparation method comprises the steps of:
(1) According to the mole ratio of NiO to CuO to ZnO to Fe 2 O 3 Mixing raw materials in a ratio of (1) =0.2:0.22:0.6:0.98, performing first ball milling, and drying at 150-200 ℃ to obtain mixed powder, wherein the average particle size of the mixed powder is 1.5-1.9 mu m;
(2) Presintering the mixed powder obtained in the step (1) for 1.5-2.5 hours at 850-1050 ℃ to obtain a presintering material;
(3) Mixing the pre-sintering material and the supplementary material obtained in the step (2), wherein the volume of the supplementary material is 60-65% of that of the pre-sintering material, the molar ratio of elementary iron, niO, cuO and ZnO in the supplementary material is 1.96:0.2:0.22:0.6, and then adding additives, and the additives comprise Bi 2 O 3 、V 2 O 5 、B 2 O 3 Or any one or the combination of at least two of PbO, wherein the mass of the additive is 0.4-0.6% of the sum of the mass of the presintered material and the mass of the supplement material, the mixture is subjected to second ball milling until the average particle size is 0.8-1.2 mu m, the mixture is dried at 150-200 ℃, polyvinyl alcohol is added for granulation, and the mixture is subjected to compression molding at 280-320MPa to obtain a green body;
(4) Sintering the green body obtained in the step (3) for 5.5-6.5 hours at 900-920 ℃ to obtain the shrinkage-free nickel-copper-zinc ferrite material.
19. A non-shrink nickel copper zinc ferrite material obtained by the method of any one of claims 1 to 18, characterized in that the molecular structure of the non-shrink nickel copper zinc ferrite materialThe expression is Ni 0.2 Cu 0.22 Zn 0.6 Fe 1.96 O x Wherein x ranges from 3 to 4.
CN202210718958.9A 2022-06-23 2022-06-23 Shrinkage-free nickel-copper-zinc ferrite material and preparation method thereof Active CN115010479B (en)

Priority Applications (1)

Application Number Priority Date Filing Date Title
CN202210718958.9A CN115010479B (en) 2022-06-23 2022-06-23 Shrinkage-free nickel-copper-zinc ferrite material and preparation method thereof

Applications Claiming Priority (1)

Application Number Priority Date Filing Date Title
CN202210718958.9A CN115010479B (en) 2022-06-23 2022-06-23 Shrinkage-free nickel-copper-zinc ferrite material and preparation method thereof

Publications (2)

Publication Number Publication Date
CN115010479A CN115010479A (en) 2022-09-06
CN115010479B true CN115010479B (en) 2023-06-30

Family

ID=83077680

Family Applications (1)

Application Number Title Priority Date Filing Date
CN202210718958.9A Active CN115010479B (en) 2022-06-23 2022-06-23 Shrinkage-free nickel-copper-zinc ferrite material and preparation method thereof

Country Status (1)

Country Link
CN (1) CN115010479B (en)

Families Citing this family (2)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN117735970A (en) * 2022-09-14 2024-03-22 华为技术有限公司 Filling agent of packaging material, preparation method of filling agent, magnetic plastic packaging material and packaging device
CN115448373B (en) * 2022-10-20 2024-03-05 横店集团东磁股份有限公司 Preparation method of manganese ferrite material

Citations (1)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
GB201302979D0 (en) * 2013-02-20 2013-04-03 Siemens Plc Methods and apparatus for compensating for drift in magnetic field strength in superconducting magnets

Family Cites Families (15)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
USRE32714E (en) * 1984-09-25 1988-07-19 North Carolina State University Method of producing high performance permanent magnets
JP2812152B2 (en) * 1992-11-25 1998-10-22 松下電器産業株式会社 Magnetic body and method of manufacturing the same
US5518641A (en) * 1992-11-25 1996-05-21 Matsushita Electric Industrial Co., Ltd. Magnetic material and manufacturing method thereof
JP2950117B2 (en) * 1993-10-19 1999-09-20 松下電器産業株式会社 Magnetic body and method of manufacturing the same
JP3391108B2 (en) * 1993-10-19 2003-03-31 松下電器産業株式会社 Magnetic body and method of manufacturing the same
JPH0971455A (en) * 1995-09-04 1997-03-18 Matsushita Electric Ind Co Ltd Ferrite material and its production
KR100222757B1 (en) * 1996-11-30 1999-10-01 이형도 A soft magnetic material for inductor and a method for manufacturing therewith
JP3635016B2 (en) * 2000-08-21 2005-03-30 Ｔｄｋ株式会社 Ferrite material
CN101206941A (en) * 2006-12-21 2008-06-25 横店集团东磁股份有限公司 Method of preparing high magnetoconductivity low temperature co-baking NiCuZn ferrite
JP2012180258A (en) * 2011-03-03 2012-09-20 Tdk Corp MnZn-BASED FERRITE POWDER, MnZn-BASED FERRITE GRANULES, METHOD OF MANUFACTURING MnZn-BASED FERRITE CORE AND MnZn-BASED FERRITE CORE
CN102557605A (en) * 2012-03-09 2012-07-11 深圳顺络电子股份有限公司 Preparation method of low-temperature sintered Ni-Zn-Cu soft magnetic ferrite material
CN104761250A (en) * 2015-01-29 2015-07-08 横店集团东磁股份有限公司 Low temperature sintered nickel-copper-zinc soft-magnetic ferrite material and preparation method thereof
JP6540977B1 (en) * 2018-01-17 2019-07-10 Tdk株式会社 Ferrite sintered body and electronic component using the same
CN111205075B (en) * 2019-10-23 2021-04-20 横店集团东磁股份有限公司 Nickel-zinc ferrite material and preparation method thereof
CN113534027B (en) * 2021-06-23 2024-03-22 麦格磁电科技（珠海）有限公司 Magnetization testing method and method for preparing soft magnetic ferrite by using same

Patent Citations (1)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
GB201302979D0 (en) * 2013-02-20 2013-04-03 Siemens Plc Methods and apparatus for compensating for drift in magnetic field strength in superconducting magnets

Also Published As

Publication number Publication date
CN115010479A (en) 2022-09-06

Similar Documents

Publication Publication Date Title
CN115010479B (en) Shrinkage-free nickel-copper-zinc ferrite material and preparation method thereof
KR100349003B1 (en) Method for the Preparation of Soft Magnetic Ferrite Powder and Method for the Production of Laminated Chip Inductor
CN101388268B (en) High magnetic conductive low temperature sintered NiCuZn ferrite material
CN1637962A (en) Composite sintered magnetic material, its manufacturing method, and magnetic element using composite sintered magnetic material
CN108706968B (en) Low-temperature sintered direct-current bias resistant NiCuZn ferrite and preparation method thereof
CN109231967B (en) Bi2O3-B2O3Binary system microwave dielectric ceramic material and preparation method thereof
CN105523750A (en) Photosensitive nano ceramic material and preparation method thereof
CN112830775A (en) Low-dielectric-constant microwave dielectric ceramic and preparation method thereof
CN110483032B (en) Low-temperature sintered YIG ferrite based on LTCC technology and preparation method thereof
CN101172853A (en) Porcelain material for temperature stabilization X9R type multilayer ceramic capacitor and method for producing the same
KR100567632B1 (en) Dielectric compositions for firing at low temperatures and electronic parts
CN112010650A (en) Low-temperature sintered high-quality factor microwave dielectric ceramic and preparation method thereof
CN114133231A (en) Nickel-zinc ferrite material and method for producing same
KR100907455B1 (en) Low temperature sintering nano-glass and manufacturing method the same
JP3735228B2 (en) Method for producing soft magnetic ferrite powder and method for producing multilayer chip inductor
US6068786A (en) Low-fire ferrite composition and a process for manufacturing ceramic articles using the said composition
CN110418774B (en) Ni-based ferrite sintered body, coil component, and method for producing Ni-based ferrite sintered body
JP6967418B2 (en) Magnetic materials and laminated chip parts
JP2008137873A (en) Dielectric ceramic composition and ceramic electronic component
JP3909366B2 (en) Low dielectric constant porcelain composition and method for producing substrate for electronic circuit using the porcelain composition
JP4766339B2 (en) Sintered ferrite and manufacturing method thereof
JP2762531B2 (en) Ferrite magnetic body and method of manufacturing the same
CN112479697B (en) MnZn ferrite material with low temperature coefficient and low loss at high frequency and preparation method thereof
KR100279373B1 (en) Manufacturing method of soft magnetic ferrite
US6251299B1 (en) Magnetic material, inductance element using the same and manufacturing method thereof

Legal Events

Date Code Title Description
PB01 Publication
PB01 Publication
SE01 Entry into force of request for substantive examination
SE01 Entry into force of request for substantive examination
GR01 Patent grant
GR01 Patent grant