CN110372363A - A kind of soft magnetic ferrites with low sintering temperature material and preparation method thereof - Google Patents
A kind of soft magnetic ferrites with low sintering temperature material and preparation method thereof Download PDFInfo
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- 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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- 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
- H01F1/36—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 in the form of particles
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- C04B2235/32—Metal oxides, mixed metal oxides, or oxide-forming salts thereof, e.g. carbonates, nitrates, (oxy)hydroxides, chlorides
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- C04B2235/32—Metal oxides, mixed metal oxides, or oxide-forming salts thereof, e.g. carbonates, nitrates, (oxy)hydroxides, chlorides
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Abstract
The invention discloses a kind of soft magnetic ferrites with low sintering temperature materials and preparation method thereof, belong to electronic information function material and device arts；The present invention is formed using the oxide of iron nickel zinc copper as main component, CBS glass is sintering aid, is prepared using solid reaction process, by ball milling, drying, pre-burning, the processes such as secondary ball milling, is dried, is pulverized and sieved and prepare.The invention has the characteristics that low sintering temperature, higher self-resonant frequency, quality factor are high and impedance is high, can be used for making spike magnetic bead, and chip inductor solves the problems, such as that magnet cannot fine cofiring with silver electrode.
Description
Technical field
The invention belongs to electronic information function material and device arts, and in particular to be a kind of there is sintering temperature
The soft magnetic ferrite and preparation method thereof for the features such as low, higher self-resonant frequency, quality factor are high and impedance is high.It can use
In production spike magnetic bead, chip inductor solves the problems, such as that magnet and silver electrode cannot fine cofirings.
Background technique
Domestic and international low-temperature sintered lamellar formula inductance soft magnetic ferrite is at present with FeNiCuZn and FeMgCuZn
Based on two kinds of materials, because generally can be all added in the formulation design in 900 DEG C or so and fine silver inner conductor matching co-firing knot
Sintering aid in varying numbers, and the most commonly used sintering aid is exactly Bi2O3。
(1) add Bi2O3Help the working principle of burning: because of Bi2O3Fusing point it is very low, start to melt at 730 DEG C, after fusing
Bi2O3Ferrite Material is wrapped up, transition liquid-phase is formed, to promote the growth of Ferrite Material crystal grain.
(2) add Bi2O3Help the internal structure of burning: Bi2O3It is in a liquid state in sintering process, during which, by surrounding ferrite crystal grains
It is wrapped up, and multiple little crystal grains is made to be merged into a big crystal grain.After cooling, Bi2O3 solidification, as between crystal grain and crystal grain
Filling owner's wrappage, exist at the grain boundary.
(3) add Bi2O3Purposes: first is that in a manner of transiting liquid phase sintering, promote grain growth, make the burning of Ferrite Material
Junction temperature drops to 900 DEG C from 960 DEG C or more hereinafter, reaching low sintering purpose；Bi2O3After cooling down and solidifying, in crystal grain
Play bonding and solidification crystal grain between crystal grain, material porcelain body intensity and bulk density is made to reach design requirement.
Add Bi2O3Although low in cost, good cooling effect, easy to operate；But Bi2O3Big on the influence of material electromagnetic performance,
It is be easy to cause abnormal grain growth, and Bi is heavy metal element, it is fewer and fewer to be used.
The transition temperature (Tg) of CBS glass is 590 DEG C, and temperature is increased to an apparent peak occur at 680 DEG C, shows this
Temperature is the softening point of CBS glass, can be used as ferritic sintering aid.
Summary of the invention
The object of the present invention is to provide one kind, and with sintering temperature, low, higher self-resonant frequency, quality factor are high and hinder
The soft magnetic ferrite and preparation method thereof of the features such as anti-high.
The present invention solve the technical problem the technical solution adopted is as follows:
A kind of low-temperature sintering iron nickel zinc copper soft magnetic ferrite, by main crystal phase material and sintering aid material through ball milling mixing, pre-
It burns, adulterate ball milling, filters pressing drying is made.
Wherein: the main crystal phase material is Fe2O3Mass percent be 50~70%, NiO mass percent be 20~
30%, ZnO mass percent are that 5~15%, CuO mass percent is 2~10%；The sintering aid is CaO-B2O3-SiO2
(CBS) glass, mass percent are 0.1~2%.
Molar ratio in the main crystal phase material between Fe, Ni, Zn, Cu is 1-x-y-z:x:y:z, and x is 0.2~0.4, y
It is 0.1~0.3 for 0.1~0.3, z.
The doping sintering aid material is CBS glass, and mass percent is 0.2~3%.
A kind of preparation method of soft magnetic ferrite, includes the following steps:
(1), prepared by main crystal phase material, weighs Fe in molar ratio2O3, NiO, ZnO, CuO, in material: ball: the ratio 1:2:0.8 of water
Ball milling is carried out, after filters pressing drying, pre-burning under the conditions of 870/4H.
(2), the main crystal phase material after pre-burning adds sintering aid material C BS glass in the ratio of 1:0.2~3% after crushing,
Secondary ball milling is carried out by the condition of step 1, then filters pressing drying pulverizes and sieves.
Soft magnetic ferrite of the invention at being grouped as are as follows: Fe1-x-y-zNixZnyCuz, wherein x is 0.2~0.4, y
It is 0.1~0.3 for 0.1~0.3, z.
The crucial group that the present invention forms soft magnetic ferrite becomes Fe1-x-y-zNixZnyCuz, in formula components containing iron,
Nickel, zinc, copper and calcium, boron, element silicon, raw material Fe, Ni, Zn, Cu, Ca, B, the Si for preparing this soft magnetic ferrite are to contain
The oxide of these elements.Wherein, doped chemical calcium borosilicate is the ingredient in order to form CBS glass.
Primary focus of the invention is the component prescription of soft magnetic ferrite, can be according to need in actual application
Synthetic method and production technology are adjusted accordingly, flexibility is big.It is solidifying that solid reaction process, colloidal sol-can be used in synthetic method
Glue method, coprecipitation, the synthetic method of vapour deposition process or other ceramic materials are realized.The present invention, which selects, is suitable for the big life of industry
The solid reaction process of production, being conducive to production cost reduces.
The detection of soft magnetic ferrite characteristic of the invention is to use to be pressed into annulus, and high temperature sintering passes around enamel-cover copper
Line measures the characterisitic parameter of magnet ring with HP4291B impedance analyzer.
The characteristic and Heterosis of soft magnetic ferrite of the present invention exist: 1. material composition is simple, raw material ratio
It is relatively abundant, it is environmental-friendly；2. calcined temperature is lower in preparation process, production cost is reduced；3. material firing temperature is low, be conducive to
Silver electrode cofiring；4. the quality factor of adjustable magnetic element, suitable high frequency is answered by the content of copper in modifying ingredients composition
Use occasion.
The electrical property of soft magnetic ferrite of the present invention can realize following parameter request: initial permeability μ0=25 ± 2, product
Prime factor >=180.
The invention has the beneficial effects that: preparation method simple process, it is easy to accomplish, the sintering temperature of material is reduced,
It is able to satisfy the requirement with silver electrode cofiring.
The contents of the present invention are further described with the following Examples.Following embodiment only meets the technology of the present invention
Several examples of content do not illustrate that present invention is limited only to contents described in following examples.The ingredient that focuses on of the invention is matched
Side, the raw material, process and step can be adjusted correspondingly according to actual production conditions, and flexibility is big.
Specific embodiment
The present invention uses the Fe of purity assay2O3, NiO, ZnO, CuO be raw material prepare principal crystalline phase, with purity be it is analytically pure
CaCO3、H3BO3、SiO2CBS glass is prepared, is doped, specific embodiment is as follows:
Ingredient is weighed by table 1, mixture is put into stirring-type ball grinder, by pellet water quality ratio 1:2:0.8, ball milling 2~6
Hour, revolving speed is 260 revs/min.Granularity is controlled in D50Within=1.2 μm, by the material filters pressing that ball milling is mixed, it is put in 100 DEG C of bakings
Case drying, smashes it through 40 meshes, and 870 DEG C/4H condition pre-burning is pressed in chamber type electric resistance furnace, it is spare to smash it through 40 meshes；It presses
Ratio in table 1 adds sintering aid CBS, carries out secondary ball milling, filters pressing, drying, smashes it through 80 meshes, PVA is added to be granulated, and uses
Handpress 20MPa forms outer diameter Φ 20.0mm, internal diameter Φ 10.0mm, the annulus of thickness 2mm.Green compact sample is placed in sintering furnace
In, it under the conditions of 900 DEG C/5H, sinters magnet ring sample into, passes around 10 circle of 0.5mm enamel covered wire, pass through HP4291B impedance analyzer
Sample is tested for the property.
The specific embodiment of the invention is shown in Table 2 at porcelain density, magnetic conductivity, Q value result in detail.
The percentage of raw material in each example of table 1.
The properties of sample of each example of table 2.
Claims (4)
1. a kind of soft magnetic ferrites with low sintering temperature material, by main crystal phase material and sintering aid material through ball milling mixing, pre-burning, doping
Ball milling, filters pressing drying are made；Wherein: the main crystal phase material is Fe2O3Mass percent is 50~70%, NiO mass percent
It is 5~15%, CuO mass percent for 20~30%, ZnO mass percent is 2~10%；The sintering aid is CaO-B2O3-
SiO2(CBS) glass, mass percent are 0.1~2%.
2. the soft magnetic ferrite according to claim 1, which is characterized in that Fe, Ni in the main crystal phase material, Zn,
Molar ratio between Cu is 1-x-y-z:x:y:z, and it be 0.1~0.3, z is 0.1~0.3 that x, which is 0.2~0.4, y,.
3. the soft magnetic ferrite according to claim 1, which is characterized in that the doping sintering aid material is CBS glass
Glass, mass percent are 0.2~3%.
4. a kind of preparation method of soft magnetic ferrite includes the following steps: prepared by main crystal phase material, weighs in molar ratio
Fe2O3, NiO, ZnO, CuO, in material: ball: the ratio 1:2:0.8 of water carries out ball milling, pre- under the conditions of 870/4H after filters pressing drying
It burns；Main crystal phase material after pre-burning adds sintering aid material C BS glass in the ratio of 1:0.2~3% after crushing, by step 1
Condition carry out secondary ball milling, filters pressing drying, then pulverize and sieve.
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Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN110372364A (en) * | 2019-06-15 | 2019-10-25 | 山东格仑特电动科技有限公司 | A kind of copper-based soft magnetic ferrite of low-temperature sintering iron nickel zinc and preparation method thereof |
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| JPH0891917A (en) * | 1994-09-19 | 1996-04-09 | Matsushita Electric Ind Co Ltd | Ferrite material and its production |
| US5853608A (en) * | 1996-11-30 | 1998-12-29 | Samsung Electro-Mechanics Co., Ltd. | Low temperature sintering radio frequency soft ferrite material, and method for manufacturing a wire coiling inductor core using such material |
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2019
- 2019-06-13 CN CN201910509638.0A patent/CN110372363A/en active Pending
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| JPH0891917A (en) * | 1994-09-19 | 1996-04-09 | Matsushita Electric Ind Co Ltd | Ferrite material and its production |
| US5853608A (en) * | 1996-11-30 | 1998-12-29 | Samsung Electro-Mechanics Co., Ltd. | Low temperature sintering radio frequency soft ferrite material, and method for manufacturing a wire coiling inductor core using such material |
| CN1591707A (en) * | 2003-08-26 | 2005-03-09 | 奇力新电子股份有限公司 | Lead-free flux composition for low-temp sintering Ni Zn ferrimagnet |
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| Title |
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| YUNYAN WANG ET AL.: "Effect of CaO–B2O3–SiO2 glass on the magnetic and dielectric properties of NiCuZn ferrites", 《JOURNAL OF MAGNETISM AND MAGNETIC MATERIALS》 * |
Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN110372364A (en) * | 2019-06-15 | 2019-10-25 | 山东格仑特电动科技有限公司 | A kind of copper-based soft magnetic ferrite of low-temperature sintering iron nickel zinc and preparation method thereof |
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