CN107946012A - A kind of composite magnetic material and preparation method thereof - Google Patents
A kind of composite magnetic material and preparation method thereof Download PDFInfo
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- CN107946012A CN107946012A CN201711157851.7A CN201711157851A CN107946012A CN 107946012 A CN107946012 A CN 107946012A CN 201711157851 A CN201711157851 A CN 201711157851A CN 107946012 A CN107946012 A CN 107946012A
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- 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
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- H—ELECTRICITY
- H01—ELECTRIC ELEMENTS
- H01F—MAGNETS; INDUCTANCES; TRANSFORMERS; SELECTION OF MATERIALS FOR THEIR MAGNETIC PROPERTIES
- H01F41/00—Apparatus or processes specially adapted for manufacturing or assembling magnets, inductances or transformers; Apparatus or processes specially adapted for manufacturing materials characterised by their magnetic properties
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Abstract
The invention discloses a kind of preparation method of composite magnetic material, iron ammonium sulfate, manganese chloride, potassium niobate, tantalic acid magnesium and ethylenediamine tetra-acetic acid are mixed, it is 6.2 6.8 to adjust ph value of mixture, and magnetic agitation reacts 30 50min at 50 70 DEG C of temperature；Above-mentioned products therefrom is put into drying box dry removing solvent；Then in Muffle furnace is put into, under the protection of inert gas, in 200 250 DEG C of 15 25min of roasting of temperature, A material are obtained；Manganese dioxide, zinc oxide and ferroso-ferric oxide are mixed, and add absolute ethyl alcohol, rise temperature to 80 90 DEG C of 35 45min of back flow reaction；After through drying, in 300 400 DEG C roast 20 30min after obtain B material；By A material and B material mixing, the composite magnetic material is can obtain after ball milling, compacting.
Description
Technical field
The invention belongs to field of electronic materials, more particularly to a kind of composite magnetic material and preparation method thereof.
Background technology
Composite material is artificial with different physics and chemical property, the material warp of different shape by two or more
A kind of heterogeneous material with excellent performance made of combination process.Similarly, composite magnetic be by two or more not
Connatural magnetic component is combined, and has the no excellent magnetic performance of single magnetic component, thus is widely used.
Composite magnetic is the important foundation functional material of electronics industry, and emerging multifunctional material, is being calculated
There is important application in the daily necessities such as the industrial circles such as machine, communication, automobile, aerospace and military project and household electrical appliance
Prospect, such as Telecommunication Transformers, inductor, cathode-ray tube, microwave device and magnetics information-recording material.With science and technology
Fast development, new requirement is constantly proposed to the performance of composite magnetic, while also have to its demand and significantly carry
It is high.Preparing the routine techniques of composite magnetic has radio-frequency sputtering technology, sol-gel technique and the multistep co-precipitation+machinery compound
Technology etc..Equipment needed for radio-frequency sputtering technology is expensive；Sol-gel technique takes, and organic matter decomposes generation in high-temperature roasting
Pernicious gas；Multistep co-precipitation+machinery complex technique complex process takes.With the extensive use of magnetic material, to magnetic material
The requirement of material also just it is higher and higher, but existing magnetic material in coercivity, saturation induction density, Effective permeability etc. still
There are larger deficiency.
The content of the invention
For the deficiency of above-mentioned magnetic material in the prior art, the object of the present invention is to provide a kind of composite magnetic material
And preparation method thereof, the magnetic material of excellent performance is prepared with relatively simple production technology.
To realize that the object of the invention technical solution is as follows：
A kind of preparation method of composite magnetic material, includes the following steps：
S1：By 3-8 parts of iron ammonium sulfate, 2-5 parts of manganese chloride, 7-10 parts of potassium niobate, 4-9 parts of tantalic acid magnesium and ethylenediamine tetra-acetic acid
10-15 parts of mixing, adjustings ph value of mixture is 6.2-6.8, and magnetic agitation reacts 30-50min at 50-70 DEG C of temperature；
S2：Products therefrom in step S1 is put into drying box dry removing solvent；Then in Muffle furnace is put into, in indifferent gas
Under the protection of body, in 200-250 DEG C of roasting 15-25min of temperature, A material are obtained；
S3：By 2-6 parts of 4-8 parts of manganese dioxide, 3-7 parts of zinc oxide and ferroso-ferric oxide mixing, and add absolute ethyl alcohol 20-25
Part, rise temperature to 80-90 DEG C of back flow reaction 35-45min；Obtained after through drying, after 300-400 DEG C of roasting 20-30min
B expects；
S4：By B material mixing in A material in step S2 and step S3, the composite magnetic material is can obtain after ball milling, compacting.
Preferably, 6 parts of iron ammonium sulfate described in step S1,4 parts of manganese chloride, 8 parts of potassium niobate, 7 parts of tantalic acid magnesium and second two
The 12 parts of mixing of amine tetraacethyl.
Preferably, it is 6.5 that ph value of mixture is adjusted in step S1, the magnetic agitation reaction 45min at 65 DEG C of temperature.
Preferably, temperature dry in step S2 is 120 DEG C, and inert gas is nitrogen or argon gas；In 230 DEG C of roastings of temperature
20min。
Preferably, 4 parts of 6 parts of manganese dioxide, 5 parts of zinc oxide and ferroso-ferric oxide mixing in step S3, add absolute ethyl alcohol
20-25 parts；Temperature is raised to 85 DEG C of back flow reaction 40min；26min is roasted in 350 DEG C.
Preferably, ball milling condition is described in step S4：Rotational speed of ball-mill 400-600r/min, Ball-milling Time 1-2h；Compacting
Pressure is 10-15MPa.
Preferably, the rotational speed of ball-mill 550r/min, Ball-milling Time 1.5h；Pressing pressure 12MPa.
Compared with prior art, the present invention its advantage is：
The preparation method of a kind of composite magnetic material of the present invention, with iron ammonium sulfate, manganese chloride, potassium niobate and tantalic acid magnesium
A material are prepared；B material are prepared with manganese dioxide, zinc oxide and ferroso-ferric oxide；It will be obtained after A material and B pellets mill, compacting
To composite magnetic material.By the coercivity of the invention that composite magnetic material is prepared, saturation induction density and have
Effect magnetic conductivity improves a lot.
Embodiment
The present invention is further illustrated with reference to embodiments.
Embodiment 1
S1：10 parts of 3 parts of iron ammonium sulfate, 2 parts of manganese chloride, 10 parts of potassium niobate, 9 parts of tantalic acid magnesium and ethylenediamine tetra-acetic acid are mixed,
It is 6.2 to adjust ph value of mixture, and magnetic agitation reacts 30min under temperature 50 C；
S2：Products therefrom in step S1 is put into 120 DEG C of dry removing solvents in drying box；Then in Muffle furnace is put into,
Under the protection of inert nitrogen gas, in 200 DEG C of roasting 15min of temperature, A material are obtained；
S3：By 2 parts of 4 parts of manganese dioxide, 3 parts of zinc oxide and ferroso-ferric oxide mixing, and 20 parts of absolute ethyl alcohol is added, raise temperature
To 80 DEG C of back flow reaction 45min；After through drying, in 300 DEG C roast 20min after obtain B material；
S4：By in step S2 A material and step S3 in B material mixing, under rotating speed 400r/min ball milling 1h, after 10MPa is suppressed i.e.
It can obtain the composite magnetic material.
Embodiment 2
S1：By 15 parts of 8 parts of iron ammonium sulfate, 5 parts of manganese chloride, 7 parts of potassium niobate, 4 parts of tantalic acid magnesium and ethylenediamine tetra-acetic acid mixing, adjust
It is 6.8 to save ph value of mixture, and magnetic agitation reacts 50min under temperature 70 C；
S2：Products therefrom in step S1 is put into 120 DEG C of dry removing solvents in drying box；Then in Muffle furnace is put into,
Under the protection of inert nitrogen gas, in 250 DEG C of roasting 25min of temperature, A material are obtained；
S3：By 6 parts of 8 parts of manganese dioxide, 7 parts of zinc oxide and ferroso-ferric oxide mixing, and 25 parts of absolute ethyl alcohol is added, raise temperature
To 90 DEG C of back flow reaction 35min；After through drying, in 400 DEG C roast 30min after obtain B material；
S4：By in step S2 A material and step S3 in B material mixing, under rotating speed 600r/min ball milling 2h, after 15MPa is suppressed i.e.
It can obtain the composite magnetic material.
Embodiment 3
S1：By 14 parts of 5 parts of iron ammonium sulfate, 3 parts of manganese chloride, 9 parts of potassium niobate, 8 parts of tantalic acid magnesium and ethylenediamine tetra-acetic acid mixing, adjust
It is 6.5 to save ph value of mixture, the magnetic agitation reaction 35min at 55 DEG C of temperature；
S2：Products therefrom in step S1 is put into 120 DEG C of dry removing solvents in drying box；Then in Muffle furnace is put into,
Under the protection of inert gas argon gas, in 220 DEG C of roasting 17min of temperature, A material are obtained；
S3：By 5 parts of 5 parts of manganese dioxide, 6 parts of zinc oxide and ferroso-ferric oxide mixing, and 24 parts of absolute ethyl alcohol is added, raise temperature
To 88 DEG C of back flow reaction 40min；After through drying, in 350 DEG C roast 22min after obtain B material；
S4：By in step S2 A material and step S3 in B material mixing, under rotating speed 500r/min ball milling 1.5h, after 12MPa is suppressed
It can obtain the composite magnetic material.
Embodiment 4
S1：By 12 parts of 7 parts of iron ammonium sulfate, 5 parts of manganese chloride, 7 parts of potassium niobate, 5 parts of tantalic acid magnesium and ethylenediamine tetra-acetic acid mixing, adjust
It is 6.3 to save ph value of mixture, the magnetic agitation reaction 45min at 65 DEG C of temperature；
S2：Products therefrom in step S1 is put into 120 DEG C of dry removing solvents in drying box；Then in Muffle furnace is put into,
Under the protection of inert gas argon gas, in 230 DEG C of roasting 22min of temperature, A material are obtained；
S3：By 3 parts of 7 parts of manganese dioxide, 3 parts of zinc oxide and ferroso-ferric oxide mixing, and 21 parts of absolute ethyl alcohol is added, raise temperature
To 83 DEG C of back flow reaction 37min；After through drying, in 380 DEG C roast 27min after obtain B material；
S4：By in step S2 A material and step S3 in B material mixing, under rotating speed 550r/min ball milling 2h, after 14MPa is suppressed i.e.
It can obtain the composite magnetic material.
Embodiment 5
S1：By 12 parts of 6 parts of iron ammonium sulfate, 4 parts of manganese chloride, 8 parts of potassium niobate, 7 parts of tantalic acid magnesium and ethylenediamine tetra-acetic acid mixing, adjust
It is 6.5 to save ph value of mixture, the magnetic agitation reaction 45min at 65 DEG C of temperature；
S2：Products therefrom in step S1 is put into 120 DEG C of dry removing solvents in drying box；Then in Muffle furnace is put into,
Under the protection of inert nitrogen gas, in 230 DEG C of roasting 20min of temperature, A material are obtained；
S3：By 4 parts of 6 parts of manganese dioxide, 5 parts of zinc oxide and ferroso-ferric oxide mixing, and 25 parts of absolute ethyl alcohol is added, raise temperature
To 85 DEG C of back flow reaction 40min；After through drying, in 350 DEG C roast 26min after obtain B material；
S4：By in step S2 A material and step S3 in B material mixing, under rotating speed 550r/min ball milling 1.5h, after 12MPa is suppressed
It can obtain the composite magnetic material.
After testing, the performance of composite magnetic material is as follows described in each embodiment：
| Experiment | Coercivity（A/m） | Saturation induction density/T | Effective permeability 1KHz |
| Embodiment 1 | 0.12 | 0.9 | 68850 |
| Embodiment 2 | 0.15 | 1.2 | 71020 |
| Embodiment 3 | 0.19 | 1.1 | 67000 |
| Embodiment 4 | 0.17 | 1.3 | 69500 |
| Embodiment 5 | 0.21 | 1.5 | 72000 |
The invention is not restricted to embodiment here, those skilled in the art disclose according to the present invention, do not depart from scope
The improvement and modification made all should be within protection scope of the present invention.
Claims (7)
1. a kind of preparation method of composite magnetic material, it is characterised in that include the following steps：
S1：By 3-8 parts of iron ammonium sulfate, 2-5 parts of manganese chloride, 7-10 parts of potassium niobate, 4-9 parts of tantalic acid magnesium and ethylenediamine tetra-acetic acid
10-15 parts of mixing, adjustings ph value of mixture is 6.2-6.8, and magnetic agitation reacts 30-50min at 50-70 DEG C of temperature；
S2：Products therefrom in step S1 is put into drying box dry removing solvent；Then in Muffle furnace is put into, in indifferent gas
Under the protection of body, in 200-250 DEG C of roasting 15-25min of temperature, A material are obtained；
S3：By 2-6 parts of 4-8 parts of manganese dioxide, 3-7 parts of zinc oxide and ferroso-ferric oxide mixing, and add absolute ethyl alcohol 20-25
Part, rise temperature to 80-90 DEG C of back flow reaction 35-45min；Obtained after through drying, after 300-400 DEG C of roasting 20-30min
B expects；
S4：By B material mixing in A material in step S2 and step S3, the composite magnetic material is can obtain after ball milling, compacting.
2. the preparation method of a kind of composite magnetic material according to claim 1, it is characterised in that described in step S1
12 parts of 6 parts of iron ammonium sulfate, 4 parts of manganese chloride, 8 parts of potassium niobate, 7 parts of tantalic acid magnesium and ethylenediamine tetra-acetic acid mixing.
3. the preparation method of a kind of composite magnetic material according to claim 1, it is characterised in that adjusted in step S1
Ph value of mixture is 6.5, the magnetic agitation reaction 45min at 65 DEG C of temperature.
4. the preparation method of a kind of composite magnetic material according to claim 1, it is characterised in that dry in step S2
Temperature be 120 DEG C, inert gas is nitrogen or argon gas；In 230 DEG C of roasting 20min of temperature.
A kind of 5. preparation method of composite magnetic material according to claim 1, it is characterised in that dioxy in step S3
Change 4 parts of 6 parts of manganese, 5 parts of zinc oxide and ferroso-ferric oxide mixing, add 20-25 parts of absolute ethyl alcohol；It is anti-to 85 DEG C of reflux to raise temperature
Answer 40min；26min is roasted in 350 DEG C.
6. the preparation method of a kind of composite magnetic material according to claim 1, it is characterised in that described in step S4
Ball milling condition is：Rotational speed of ball-mill 400-600r/min, Ball-milling Time 1-2h；Pressing pressure is 10-15MPa.
A kind of 7. preparation method of composite magnetic material according to claim 6, it is characterised in that the rotational speed of ball-mill
550r/min, Ball-milling Time 1.5h；Pressing pressure 12MPa.
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Citations (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1111800A (en) * | 1994-03-30 | 1995-11-15 | 高桥靖典 | Material for permanent magnet production method thereof and permanent magnet |
| JPH10279312A (en) * | 1997-03-31 | 1998-10-20 | Tdk Corp | Spinel type ferrite |
| CN101409122A (en) * | 2008-08-05 | 2009-04-15 | 中钢集团安徽天源科技股份有限公司 | High-performance permanent ferrite and dyadic manufacturing method thereof |
| CN102731079A (en) * | 2012-07-02 | 2012-10-17 | 河北工业大学 | Method for preparing MnZn ferrite |
-
2017
- 2017-11-20 CN CN201711157851.7A patent/CN107946012A/en active Pending
Patent Citations (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1111800A (en) * | 1994-03-30 | 1995-11-15 | 高桥靖典 | Material for permanent magnet production method thereof and permanent magnet |
| JPH10279312A (en) * | 1997-03-31 | 1998-10-20 | Tdk Corp | Spinel type ferrite |
| CN101409122A (en) * | 2008-08-05 | 2009-04-15 | 中钢集团安徽天源科技股份有限公司 | High-performance permanent ferrite and dyadic manufacturing method thereof |
| CN102731079A (en) * | 2012-07-02 | 2012-10-17 | 河北工业大学 | Method for preparing MnZn ferrite |
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Application publication date: 20180420 |