CN105174935B - A kind of preparation method of rare earth soft magnetic ferrite - Google Patents
A kind of preparation method of rare earth soft magnetic ferrite Download PDFInfo
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Abstract
The invention discloses a kind of preparation method of rare earth soft magnetic ferrite, comprise the following steps：Ferrous nitrate is added after being stirred in glycerine, heating, added after ethylenediamine tetra-acetic acid stirring, pH is to 7 7.5 for regulation, is subsequently added into zinc nitrate, nickel nitrate, yttrium nitrate, manganese nitrate, is incubated, continue to heat up, insulation obtains first material；First material dry, pulverize, then calcined, then washing obtains second material；After second material and titanium oxide, zirconium oxide, vanadium oxide, cobalt oxide, niobium oxide, molybdenum oxide, barium monoxide, chromium oxide, tin oxide, indium oxide, borax, silica, strontium carbonate, absolute ethyl alcohol are mixed, ball milling obtains 3 material；By 3 material it is compressing after, carry out microwave sintering, cooling obtain rare earth soft magnetic ferrite.Gained rare earth soft magnetic ferrite of the invention has high saturated magnetic induction and outstanding initial magnetic permeability, and core loss is low under normal temperature.
Description
Technical field
The present invention relates to soft magnetic ferrite technical field, more particularly to a kind of preparation method of rare earth soft magnetic ferrite.
Background technology
With the fast development of information technology, high frequency is integrated, development trend of the miniaturization as electronic product, grinds
High-performance processed, efficient miniaturization magnetic inductive device turns into the focus of the area research, is used as the core of inductor
Part, the inductance core used in high-frequency circuit mainly has soft magnetic ferrite and metal magnetic powder core.The spy of soft magnetic ferrite
Point is its high resistivity, and vortex infringement is small.
But the extension of the development and application field with electronics industry, requirement to magnetic material also more and more higher, and
The classificating requirement of material property is more refined and specialized, but soft magnetic ferrite of the prior art often permeability and saturation
Magnetic induction intensity is not ideal enough, it is desirable to which the corresponding powder index of product can reach：Saturation induction density is 480mT left at 25 DEG C
The right side, and initial magnetic permeability is 3400 or so, but at present used in material can not ensure to produce the product for meeting this requirement in batches.
The content of the invention
The technical problem existed based on background technology, the present invention proposes a kind of preparation method of rare earth soft magnetic ferrite,
Method is simple, and gained rare earth soft magnetic ferrite has high saturated magnetic induction and outstanding initial magnetic permeability, and under normal temperature
Core loss is low, while can energy-saving and emission-reduction.
A kind of preparation method of rare earth soft magnetic ferrite proposed by the present invention, comprises the following steps：
S1, will ferrous nitrate add glycerine in stir after, heating, add ethylenediamine tetra-acetic acid stirring after, regulation
PH is subsequently added into zinc nitrate, nickel nitrate, yttrium nitrate, manganese nitrate to 7-7.5, insulation, continues to heat up, insulation obtains first material；
S2, first material dry, pulverize, then calcined, then washing obtains second material；
S3, by second material and titanium oxide, zirconium oxide, vanadium oxide, cobalt oxide, niobium oxide, molybdenum oxide, barium monoxide, oxidation
After chromium, tin oxide, indium oxide, borax, silica, strontium carbonate, absolute ethyl alcohol mixing, ball milling obtains 3 material；
S4, by 3 material it is compressing after, carry out microwave sintering, cooling obtain rare earth soft magnetic ferrite.
Preferably, in S1, ferrous nitrate, zinc nitrate, nickel nitrate, yttrium nitrate, manganese nitrate, ethylenediamine tetra-acetic acid and glycerine
Mol ratio is 54-58：18-22：7-10：2-4：25-28：70-80：110-120.
Preferably, in S1, ferrous nitrate is added after being stirred in glycerine, is warming up to 82-86 DEG C, adds ethylenediamine
After tetraacethyl stirring, pH is to 7-7.5 for regulation, is subsequently added into zinc nitrate, nickel nitrate, yttrium nitrate, manganese nitrate, is incubated 1-2h, continues
150-180 DEG C is warming up to, insulation 1-2h obtains first material.
Preferably, in S2, drying temperature is 68-72 DEG C, and drying time is 14-16h.
Preferably, in S2, calcining heat is 800-850 DEG C, and calcination time is 3-4h.
Preferably, in S3, second material and titanium oxide, zirconium oxide, vanadium oxide, cobalt oxide, niobium oxide, molybdenum oxide, oxidation
Barium, chromium oxide, tin oxide, indium oxide, borax, silica, strontium carbonate, the weight ratio of absolute ethyl alcohol are 100：2-5：7-10：
2.8-4.6：3-6：0.2-0.6：3-8：1-2：0.5-0.8：2-4：0.2-0.4：10-12：8-10：0.3-0.6：20-25.
Preferably, in S3, Ball-milling Time is 8-10h.
Preferably, in S4, compressing pressure is 1-2MPa, and the compressing time is 2-4min.
Preferably, in S4, the frequency of microwave sintering is 1600-1800MHz.
Preferably, in S4, microwave sintering concrete operations are as follows：650-680 is warming up to using 0.6-0.7kW microwave power
DEG C, then 980-100 DEG C is warming up to using 1.2-1.5kW microwave power, then it is warming up to using 1.8-2kW microwave power
1200-1250℃。
The present invention is dissolved in glycerine using ferrous nitrate, zinc nitrate, nickel nitrate, yttrium nitrate, manganese nitrate to be formed after solution, then
Ethylenediamine tetra-acetic acid is added, each cation forms complex compound by carrying out complexing with ethylenediamine tetra-acetic acid, and then heating makes second two
Amine tetraacethyl and glycerine occur fat polymerization and react to form polymer, and each cation can be uniformly distributed in the polymer, then lead to
Cross calcining and remove the oxide powders such as polymer formation iron oxide, zinc oxide, its crystal grain is uniform, permeability is high, impedance is high, has
Good microstructure, and higher sintered density is obtained, so that high saturation induction density is obtained, while oxidation can be improved
The reactivity of powder；Add titanium oxide, zirconium oxide, vanadium oxide, cobalt oxide, niobium oxide, molybdenum oxide, barium monoxide, oxidation
Chromium, tin oxide, indium oxide, borax, silica, strontium carbonate carry out wet-milling, not only reduce the particle diameter of each oxide powder, moreover it is possible to carry
High each oxide powder activity, it is easy to follow-up sintering；Restriction compressing time and pressure, are easy into base substrate after compacting
Type, is easy to sintering, and microwave sintering is penetrated inside ferrite by electromagnetic field radiation, and ferrite integrally occurs dielectric loss and risen
Temperature, each several part temperature difference is small, and microwave sintering is that ferrite Fast Sintering is fine and close, obtains fine and close, uniform tissue, and material is micro-
Structure is improved, and performance is more excellent, and microwave sintering energy consumption is low, efficiency high, than conventional sintering energy-conservation 80%；Wherein oxygen
Change titanium, zirconium oxide and ferrite to coordinate, ferritic mass transfer and sintering can be promoted, accelerate grain growth, improve rising for product
Beginning magnetic conductivity, can also effectively reduce core loss, vanadium oxide, cobalt oxide, niobium oxide, molybdenum oxide, barium monoxide, chromium oxide, oxidation
Tin, indium oxide and ferrite are used cooperatively, further reduction core loss of the present invention, while the original such as borax, silica, strontium carbonate
Material, changes the microstructure of the present invention, reduces crystallite dimension, improve resistivity.
Brief description of the drawings
Fig. 1 is a kind of schematic flow sheet of the preparation method of rare earth soft magnetic ferrite proposed by the present invention.
Embodiment
As shown in figure 1, Fig. 1 is a kind of schematic flow sheet of the preparation method of rare earth soft magnetic ferrite proposed by the present invention.
A kind of reference picture 1, preparation method of rare earth soft magnetic ferrite proposed by the present invention, comprises the following steps：
S1, will ferrous nitrate add glycerine in stir after, heating, add ethylenediamine tetra-acetic acid stirring after, regulation
PH is subsequently added into zinc nitrate, nickel nitrate, yttrium nitrate, manganese nitrate to 7-7.5, insulation, continues to heat up, insulation obtains first material；
S2, first material dry, pulverize, then calcined, then washing obtains second material；
S3, by second material and titanium oxide, zirconium oxide, vanadium oxide, cobalt oxide, niobium oxide, molybdenum oxide, barium monoxide, oxidation
After chromium, tin oxide, indium oxide, borax, silica, strontium carbonate, absolute ethyl alcohol mixing, ball milling obtains 3 material；
S4, by 3 material it is compressing after, carry out microwave sintering, cooling obtain rare earth soft magnetic ferrite.
Below, technical scheme is described in detail by specific embodiment.
Embodiment 1
A kind of preparation method of rare earth soft magnetic ferrite proposed by the present invention, comprises the following steps：
S1, it will be warming up to 82 DEG C, add after 54 parts of ferrous nitrates add and stirred in 120 parts of glycerine by molar part
After 80 parts of ethylenediamine tetra-acetic acid stirrings, ammoniacal liquor is added dropwise and adjusts pH to 7,22 parts of zinc nitrates, 7 parts of nickel nitrates, 4 parts of nitric acid are subsequently added into
Yttrium, 25 parts of manganese nitrates, are incubated 2h, are continuously heating to 150 DEG C, insulation 2h obtains first material；
S2, first material dried to 14h, drying temperature is 72 DEG C, is crushed, and then carries out calcining 3h, and then washing is obtained
Second material, calcining heat is 850 DEG C；
S3, by weight by 100 parts of second materials and 2 parts of titanium oxide, 10 parts of zirconium oxides, 2.8 parts of vanadium oxides, 6 parts of oxidations
Cobalt, 0.2 part of niobium oxide, 8 parts of molybdenum oxides, 1 part of barium monoxide, 0.8 part of chromium oxide, 2 parts of tin oxide, 0.4 part of indium oxide, 10 parts of boron
After sand, 10 parts of silica, 0.3 part of strontium carbonate, 25 parts of absolute ethyl alcohol mixing, ball milling 8h obtains 3 material；
S4, by 3 material it is compressing after, compressing pressure is 2MPa, and the compressing time is 2min, is entered
Row microwave sintering, the frequency of microwave sintering is 1800MHz, and 680 DEG C are warming up to using 0.6kW microwave power, then using 1.2kW
Microwave power be warming up to 100 DEG C, be then warming up to 1250 DEG C using 1.8kW microwave power, it is soft that natural cooling obtains rare earth
Magnetic ferrites.
Embodiment 2
A kind of preparation method of rare earth soft magnetic ferrite proposed by the present invention, comprises the following steps：
S1, it will be warming up to 86 DEG C, add after 58 parts of ferrous nitrates add and stirred in 110 parts of glycerine by molar part
After 70 parts of ethylenediamine tetra-acetic acid stirrings, sodium hydroxide solution is added dropwise and adjusts pH to 7.5,18 parts of zinc nitrates, 10 parts of nitre are subsequently added into
Sour nickel, 2 parts of yttrium nitrates, 28 parts of manganese nitrates, are incubated 1h, are continuously heating to 180 DEG C, insulation 1h obtains first material；
S2, first material dried to 16h, drying temperature is 68 DEG C, is crushed, and then carries out calcining 4h, and then washing is obtained
Second material, calcining heat is 800 DEG C；
S3, by weight by 100 parts of second materials and 5 parts of titanium oxide, 7 parts of zirconium oxides, 4.6 parts of vanadium oxides, 3 parts of oxidations
Cobalt, 0.6 part of niobium oxide, 3 parts of molybdenum oxides, 2 parts of barium monoxide, 0.5 part of chromium oxide, 4 parts of tin oxide, 0.2 part of indium oxide, 12 parts of boron
After sand, 8 parts of silica, 0.6 part of strontium carbonate, 20 parts of absolute ethyl alcohol mixing, ball milling 10h obtains 3 material；
S4, by 3 material it is compressing after, compressing pressure is 1MPa, and the compressing time is 4min, is entered
Row microwave sintering, the frequency of microwave sintering is 1600MHz, and 650 DEG C are warming up to using 0.7kW microwave power, then using 1.5kW
Microwave power be warming up to 980 DEG C, be then warming up to 1200 DEG C using 2kW microwave power, natural cooling obtains rare earth soft magnetism
Ferrite.
Embodiment 3
A kind of preparation method of rare earth soft magnetic ferrite proposed by the present invention, comprises the following steps：
S1, it will be warming up to 85 DEG C, add after 56 parts of ferrous nitrates add and stirred in 112 parts of glycerine by molar part
After the stirring of 74 parts of ethylenediamine tetra-acetic acids, ammoniacal liquor is added dropwise and adjusts pH to 7.4, be subsequently added into 19 parts of zinc nitrates, 9 parts of nickel nitrates, 2.6 parts
Yttrium nitrate, 27 parts of manganese nitrates, are incubated 1.5h, are continuously heating to 170 DEG C, insulation 1.4h obtains first material；
S2, first material dried to 15.6h, drying temperature is 69 DEG C, is crushed, and then carries out calcining 3.6h, then washes
Second material is obtained, calcining heat is 820 DEG C；
S3, by weight by 100 parts of second materials and 4 parts of titanium oxide, 8 parts of zirconium oxides, 4 parts of vanadium oxides, 4 parts of cobalt oxides,
0.5 part of niobium oxide, 4 parts of molybdenum oxides, 1.8 parts of barium monoxide, 0.6 part of chromium oxide, 3.4 parts of tin oxide, 0.2 part of indium oxide, 11.2 parts
After borax, 8.5 parts of silica, 0.5 part of strontium carbonate, 22 parts of absolute ethyl alcohol mixing, ball milling 9.4h obtains 3 material；
S4, by 3 material it is compressing after, compressing pressure is 1.6MPa, and the compressing time is
3.5min, carries out microwave sintering, the frequency of microwave sintering is 1650MHz, and 660 DEG C are warming up to using 0.68kW microwave power,
985 DEG C are warming up to using 1.4kW microwave power again, 1220 DEG C, natural cooling are then warming up to using 1.9kW microwave power
Obtain rare earth soft magnetic ferrite.
Embodiment 4
A kind of preparation method of rare earth soft magnetic ferrite proposed by the present invention, comprises the following steps：
S1, it will be warming up to 83 DEG C, add after 55 parts of ferrous nitrates add and stirred in 118 parts of glycerine by molar part
After 78 parts of ethylenediamine tetra-acetic acid stirrings, sodium hydroxide solution is added dropwise and adjusts pH to 7.2,21 parts of zinc nitrates, 8 parts of nitric acid are subsequently added into
Nickel, 3.4 parts of yttrium nitrates, 26 parts of manganese nitrates, are incubated 1.8h, are continuously heating to 160 DEG C, insulation 1.6h obtains first material；
S2, first material dried to 14.6h, drying temperature is 71 DEG C, is crushed, and then carries out calcining 3.3h, then washes
Second material is obtained, calcining heat is 840 DEG C；
S3, by weight by 100 parts of second materials and 3 parts of titanium oxide, 9 parts of zirconium oxides, 3 parts of vanadium oxides, 5 parts of cobalt oxides,
0.3 part of niobium oxide, 6 parts of molybdenum oxides, 1.6 parts of barium monoxide, 0.7 part of chromium oxide, 2.6 parts of tin oxide, 0.4 part of indium oxide, 10.6 parts
After borax, 9.3 parts of silica, 0.4 part of strontium carbonate, 24 parts of absolute ethyl alcohol mixing, ball milling 8.6h obtains 3 material；
S4, by 3 material it is compressing after, compressing pressure is 1.8MPa, and the compressing time is
2.5min, carries out microwave sintering, the frequency of microwave sintering is 1750MHz, and 670 DEG C are warming up to using 0.62kW microwave power,
995 DEG C are warming up to using 1.3kW microwave power again, then 1240 DEG C are warming up to using 1.83kW microwave power, it is naturally cold
But rare earth soft magnetic ferrite is obtained.
Embodiment 5
A kind of preparation method of rare earth soft magnetic ferrite proposed by the present invention, comprises the following steps：
S1, by molar part 84 DEG C will be warming up to, then add after 55.5 parts of ferrous nitrates add and stirred in 115 parts of glycerine
Enter after 76 parts of ethylenediamine tetra-acetic acid stirrings, ammoniacal liquor is added dropwise and adjusts pH to 7.3,20 parts of zinc nitrates, 8.5 parts of nickel nitrates, 3 are subsequently added into
Part yttrium nitrate, 26.5 parts of manganese nitrates, are incubated 1.6h, are continuously heating to 165 DEG C, insulation 1.5h obtains first material；
S2, first material dried to 15h, drying temperature is 70 DEG C, is crushed, and then carries out calcining 3.5h, then washes
To second material, calcining heat is 830 DEG C；
S3, by weight by 100 parts of second materials and 3.4 parts of titanium oxide, 8.6 parts of zirconium oxides, 3.4 parts of vanadium oxides, 4.5 parts
Cobalt oxide, 0.4 part of niobium oxide, 5 parts of molybdenum oxides, 1.7 parts of barium monoxide, 0.65 part of chromium oxide, 3 parts of tin oxide, 0.3 part of indium oxide,
After 11 parts of boraxs, 9 parts of silica, 0.45 part of strontium carbonate, 23 parts of absolute ethyl alcohol mixing, ball milling 9h obtains 3 material；
S4, by 3 material it is compressing after, compressing pressure is 1.7MPa, and the compressing time is 3min,
Microwave sintering is carried out, the frequency of microwave sintering is 1700MHz, is warming up to 665 DEG C using 0.65kW microwave power, then use
1.35kW microwave power is warming up to 990 DEG C, is then warming up to 1230 DEG C using 1.85kW microwave power, natural cooling is obtained
Rare earth soft magnetic ferrite.
Performance test is carried out to the gained high saturated magnetic induction high permeability soft magnetic ferrite of embodiment 5, from ZP45
As a control group, wherein the detection temperature of saturation induction density and core loss is 25 DEG C to material；Its result is as follows：
As seen from the above table：Initial magnetic permeability, saturation induction density and the normal temperature core loss of the present invention is superior to existing
Technology, meets actual product requirement.
The foregoing is only a preferred embodiment of the present invention, but protection scope of the present invention be not limited thereto,
Any one skilled in the art the invention discloses technical scope in, technique according to the invention scheme and its
Inventive concept is subject to equivalent substitution or change, should all be included within the scope of the present invention.
Claims (8)
1. a kind of preparation method of rare earth soft magnetic ferrite, it is characterised in that comprise the following steps：
S1, will ferrous nitrate add glycerine in stir after, heating, add ethylenediamine tetra-acetic acid stirring after, regulation pH to
7-7.5, is subsequently added into zinc nitrate, nickel nitrate, yttrium nitrate, manganese nitrate, insulation, continues to heat up, insulation obtains first material, nitric acid
Ferrous iron, zinc nitrate, nickel nitrate, yttrium nitrate, manganese nitrate, the mol ratio of ethylenediamine tetra-acetic acid and glycerine are 54-58：18-22：7-
10：2-4：25-28：70-80：110-120；
S2, first material dry, pulverize, then calcined, then washing obtains second material；
S3, by second material and titanium oxide, zirconium oxide, vanadium oxide, cobalt oxide, niobium oxide, molybdenum oxide, barium monoxide, chromium oxide, oxygen
Change after tin, indium oxide, borax, silica, strontium carbonate, absolute ethyl alcohol mixing, ball milling obtains 3 material, second material and oxidation
Titanium, zirconium oxide, vanadium oxide, cobalt oxide, niobium oxide, molybdenum oxide, barium monoxide, chromium oxide, tin oxide, indium oxide, borax, oxidation
Silicon, strontium carbonate, the weight ratio of absolute ethyl alcohol are 100：2-5：7-10：2.8-4.6：3-6：0.2-0.6：3-8：1-2：0.5-0.8：
2-4：0.2-0.4：10-12：8-10：0.3-0.6：20-25；
S4, by 3 material it is compressing after, carry out microwave sintering, cooling obtain rare earth soft magnetic ferrite.
2. the preparation method of rare earth soft magnetic ferrite according to claim 1, it is characterised in that in S1, by ferrous nitrate plus
Enter after being stirred in glycerine, be warming up to 82-86 DEG C, add after ethylenediamine tetra-acetic acid stirring, adjust pH to 7-7.5, then
Zinc nitrate, nickel nitrate, yttrium nitrate, manganese nitrate are added, 1-2h is incubated, 150-180 DEG C is continuously heating to, insulation 1-2h obtains first
Material.
3. the preparation method of rare earth soft magnetic ferrite according to claim 1 or claim 2, it is characterised in that in S2, drying temperature is
68-72 DEG C, drying time is 14-16h.
4. the preparation method of rare earth soft magnetic ferrite according to claim 1 or claim 2, it is characterised in that in S2, calcining heat is
800-850 DEG C, calcination time is 3-4h.
5. the preparation method of rare earth soft magnetic ferrite according to claim 1 or claim 2, it is characterised in that in S3, Ball-milling Time is
8-10h。
6. the preparation method of rare earth soft magnetic ferrite according to claim 1 or claim 2, it is characterised in that compressing in S4
Pressure is 1-2MPa, and the compressing time is 2-4min.
7. the preparation method of rare earth soft magnetic ferrite according to claim 1 or claim 2, it is characterised in that in S4, microwave sintering
Frequency is 1600-1800MHz.
8. the preparation method of rare earth soft magnetic ferrite according to claim 1 or claim 2, it is characterised in that in S4, microwave sintering tool
Gymnastics is made as follows：650-680 DEG C is warming up to using 0.6-0.7kW microwave power, then using 1.2-1.5kW microwave power liter
Then temperature is warming up to 1200-1250 DEG C to 980-100 DEG C using 1.8-2kW microwave power.
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