CN107151136A - A kind of preparation method of high-quality injection strontium ferrite magnetic powder - Google Patents
A kind of preparation method of high-quality injection strontium ferrite magnetic powder Download PDFInfo
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- CN107151136A CN107151136A CN201710348081.8A CN201710348081A CN107151136A CN 107151136 A CN107151136 A CN 107151136A CN 201710348081 A CN201710348081 A CN 201710348081A CN 107151136 A CN107151136 A CN 107151136A
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- magnetic powder
- ferrite magnetic
- strontium ferrite
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- C—CHEMISTRY; METALLURGY
- C04—CEMENTS; CONCRETE; ARTIFICIAL STONE; CERAMICS; REFRACTORIES
- C04B—LIME, MAGNESIA; SLAG; CEMENTS; COMPOSITIONS THEREOF, e.g. MORTARS, CONCRETE OR LIKE BUILDING MATERIALS; ARTIFICIAL STONE; CERAMICS; REFRACTORIES; TREATMENT OF NATURAL STONE
- C04B35/00—Shaped ceramic products characterised by their composition; Ceramics compositions; Processing powders of inorganic compounds preparatory to the manufacturing of ceramic products
- C04B35/01—Shaped ceramic products characterised by their composition; Ceramics compositions; Processing powders of inorganic compounds preparatory to the manufacturing of ceramic products based on oxide ceramics
- C04B35/26—Shaped ceramic products characterised by their composition; Ceramics compositions; Processing powders of inorganic compounds preparatory to the manufacturing of ceramic products based on oxide ceramics based on ferrites
- C04B35/2683—Other ferrites containing alkaline earth metals or lead
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- C—CHEMISTRY; METALLURGY
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- 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
- C04B35/626—Preparing or treating the powders individually or as batches ; preparing or treating macroscopic reinforcing agents for ceramic products, e.g. fibres; mechanical aspects section B
- C04B35/62605—Treating the starting powders individually or as mixtures
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- C04B35/00—Shaped ceramic products characterised by their composition; Ceramics compositions; Processing powders of inorganic compounds preparatory to the manufacturing of ceramic products
- C04B35/622—Forming processes; Processing powders of inorganic compounds preparatory to the manufacturing of ceramic products
- C04B35/626—Preparing or treating the powders individually or as batches ; preparing or treating macroscopic reinforcing agents for ceramic products, e.g. fibres; mechanical aspects section B
- C04B35/63—Preparing or treating the powders individually or as batches ; preparing or treating macroscopic reinforcing agents for ceramic products, e.g. fibres; mechanical aspects section B using additives specially adapted for forming the products, e.g.. binder binders
- C04B35/632—Organic additives
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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
- 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
- H01F1/0302—Magnets or magnetic bodies characterised by the magnetic materials therefor; Selection of materials for their magnetic properties of inorganic materials characterised by their coercivity characterised by unspecified or heterogeneous hardness or specially adapted for magnetic hardness transitions
- H01F1/0311—Compounds
- H01F1/0313—Oxidic compounds
- H01F1/0315—Ferrites
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- 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
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Abstract
The invention discloses a kind of preparation method of high-quality injection strontium ferrite magnetic powder, comprise the following steps：（1）Raw material mixing,（2）Calcination process,（3）Ball mill grinding.The present invention is optimized by the Reasonable adjustment to each process in manufacture craft, the strontium ferrite magnetic powder finally prepared is molded characteristic with good, simultaneously again with good magnetic property, existing strontium ferrite HCJ is improved, the problem of saturation magnetization is weak.
Description
Technical field
The invention belongs to magnetic material processing technique field, and in particular to a kind of high-quality injection strontium ferrite magnetic powder
Preparation method.
Background technology
Magnetic material, usually said magnetic material refers to ferromagnetic substance, is ancient and the quite varied function of purposes
Material, and the magnetic of material was just recognized and applied by people before 3000, such as ancient Chinese native magnet
It is used as compass.Modem magnetic materials have been widely used among our life, for example, permanent-magnet material is used as into motor, should
For the core material in transformer, the magneto-optic disk used as memory, computer magnetic recording floppy disk etc..Ferrite permanent-magnet
Material is one kind of permanent-magnet material, and it is with BaFe12O19Phase, SrFe12O19The permanent magnetism material based on solid solution is mutually obtained with them
Material.A large amount of strategic materials such as nickel, cobalt have not only been saved in its appearance, and are hard magnetic material in high band, the portion of such as television set
During part, microwave and the applications of other national defence devices etc. opens new approach.Ferrite Material serves not only as telecommunication
Phonographic recorder, microphone, sound pick-up, telephone set and various instrument, the magnet of machinery in device, and in pollution processing, doctor
Also it is widely applied in terms of student's thing and typographical display, strontium ferrite is one kind in ferrite.Sol-gel process is
Now prepare one of conventional method of strontium ferrite magnetic powder, current the method has that product magnetic property is relatively low, processing temperature is high, make
The problem of using poor quality.
The content of the invention
The purpose of the present invention is that there is provided a kind of preparation of high-quality injection strontium ferrite magnetic powder the problem of being directed to existing
Method.
The present invention is achieved by the following technical solutions：
A kind of preparation method of high-quality injection strontium ferrite magnetic powder, comprises the following steps：
（1）Raw material is mixed：
A. first strontium carbonate and ferric crystals are mixed, the mol ratio of strontium and iron is 1 in strontium carbonate and ferric nitrate after mixing：
12 ~ 13, nitric acid, 7 ~ 9 times of the deionized water of 1 ~ 1.2 times of strontium carbonate and ferric crystals gross mass are then added, is stirred continuously
It is standby that mixture A is obtained after 30 ~ 40min of processing；
B. to operation a obtained by mixture A in add its gross mass 3 ~ 5% the sodium of diethylene triamine pentamethylene phosphonic five, 0.1 ~
0.3% ethylenediamine tetra-acetic acid, 0.2 ~ 0.5% sodium tartrate, the three of 0.1 ~ 0.15% oxidation second secretarys, are stirred continuously processing uniform
Afterwards, then adjust overall pH value for 6.5 ~ 7.0 mixture B it is standby；
（2）Calcination process：
By step（1）The mixture B of gained is put into roaster, and heating keeps the temperature in roaster to be 800 ~ 850 DEG C, continues
Heat 1 ~ 1.5h, electron beam irradiation processing during which carried out to mixture B simultaneously, after the completion of take out, after filtration drying half
Finished product strontium ferrite magnetic powder is standby；
（3）Ball mill grinding：
By step（2）Semi-finished product strontium ferrite magnetic powder after processing, which is put into planetary ball mill, carries out ball-milling treatment, wherein ball
Grinding media is taking-up drying finished product strontium ferrite magnetic powder after ethanol, 30 ~ 35min of ball milling.
Further, step（2）Described in electron beam irradiation processing when close rate be 0.4 ~ 0.6kGy/min.
Further, step（3）Described in ball milling after drying temperature control be 75 ~ 80 DEG C.
The present invention with the addition of the sodium of diethylene triamine pentamethylene phosphonic five as main complexing agent, again in raw material manufacturing process
Ethylenediamine tetra-acetic acid and sodium tartrate composition are with the addition of, its common cooperation can effectively improve the anisotropic increasing of strontium ferrite
Plus, the growth of crystal grain in course of reaction is promoted, three oxidation second secretarys of addition can also promote the growth of ferrite particle, can carry again
Compactness during follow-up sintering is risen, magnetic conductivity is improved, mixture has been continuously applied at electron beam irradiation in calcination process
Reason, the surface characteristic of reactant is improved using high energy electron, three oxidation second secretary liquid phase wrapping outside ferrite are improved
Uniformity, at the same can further speed up again, the growth of stable crystal grain, improve overall uniformity and the sphericity of particle, and
Certain catalytic action is served, temperature and duration needed for being calcined is reduced, has saved production cost, finally semi-finished product are entered
Ball mill grinding is gone, using ethanol as ball-milling medium, the primary characteristic of magnetic after ball milling is ensure that well, processing is reduced
The performance loss of production.
The present invention has advantages below compared with prior art：
The present invention is optimized by the Reasonable adjustment to each process in manufacture craft, and the strontium ferrite magnetic powder finally prepared has good
Good is molded characteristic, while having good magnetic property again, improves existing strontium ferrite HCJ, saturated magnetization strong
The problem of spending weak.
Embodiment
Embodiment 1
A kind of preparation method of high-quality injection strontium ferrite magnetic powder, comprises the following steps：
（1）Raw material is mixed：
A. first strontium carbonate and ferric crystals are mixed, the mol ratio of strontium and iron is 1 in strontium carbonate and ferric nitrate after mixing：
12, nitric acid, 7 times of the deionized water of 1 times of strontium carbonate and ferric crystals gross mass are then added, processing 30min is stirred continuously
It is standby that mixture A is obtained afterwards；
B. the sodium of diethylene triamine pentamethylene phosphonic five, 0.1% second of its gross mass 3% are added into the mixture A obtained by operation a
Ethylenediamine tetraacetic acid (EDTA), 0.2% sodium tartrate, the three of 0.1% oxidation second secretarys, are stirred continuously after processing uniformly, then adjust overall pH
Be worth for 6.5 ~ 7.0 mixture B it is standby；
（2）Calcination process：
By step（1）The mixture B of gained is put into roaster, and heating keeps the temperature in roaster to be 800 DEG C, continuous heating
Handle 1h, electron beam irradiation processing during which carried out to mixture B simultaneously, after the completion of take out, after filtration drying semi-finished product strontium iron
Oxysome magnetic is standby；
（3）Ball mill grinding：
By step（2）Semi-finished product strontium ferrite magnetic powder after processing, which is put into planetary ball mill, carries out ball-milling treatment, wherein ball
Grinding media is taking-up drying finished product strontium ferrite magnetic powder after ethanol, ball milling 30min.
Further, step（2）Described in electron beam irradiation processing when close rate be 0.4kGy/min.
Further, step（3）Described in ball milling after drying temperature control be 75 DEG C.
Embodiment 2
A kind of preparation method of high-quality injection strontium ferrite magnetic powder, comprises the following steps：
（1）Raw material is mixed：
A. first strontium carbonate and ferric crystals are mixed, the mol ratio of strontium and iron is 1 in strontium carbonate and ferric nitrate after mixing：
12.5, nitric acid, 8 times of the deionized water of 1.1 times of strontium carbonate and ferric crystals gross mass are then added, processing is stirred continuously
Mixture A is obtained after 35min standby；
B. the sodium of diethylene triamine pentamethylene phosphonic five, 0.2% second of its gross mass 4% are added into the mixture A obtained by operation a
Ethylenediamine tetraacetic acid (EDTA), 0.4% sodium tartrate, the three of 0.13% oxidation second secretarys, are stirred continuously after processing uniformly, then adjust overall pH
Be worth for 6.5 ~ 7.0 mixture B it is standby；
（2）Calcination process：
By step（1）The mixture B of gained is put into roaster, and heating keeps the temperature in roaster to be 830 DEG C, continuous heating
Handle 1.2h, electron beam irradiation processing during which carried out to mixture B simultaneously, after the completion of take out, after filtration drying semi-finished product strontium
Ferromagnetic oxide powder is standby；
（3）Ball mill grinding：
By step（2）Semi-finished product strontium ferrite magnetic powder after processing, which is put into planetary ball mill, carries out ball-milling treatment, wherein ball
Grinding media is taking-up drying finished product strontium ferrite magnetic powder after ethanol, ball milling 33min.
Further, step（2）Described in electron beam irradiation processing when close rate be 0.5kGy/min.
Further, step（3）Described in ball milling after drying temperature control be 77 DEG C.
Embodiment 3
A kind of preparation method of high-quality injection strontium ferrite magnetic powder, comprises the following steps：
（1）Raw material is mixed：
A. first strontium carbonate and ferric crystals are mixed, the mol ratio of strontium and iron is 1 in strontium carbonate and ferric nitrate after mixing：
13, nitric acid, 9 times of the deionized water of 1.2 times of strontium carbonate and ferric crystals gross mass are then added, processing is stirred continuously
Mixture A is obtained after 40min standby；
B. the sodium of diethylene triamine pentamethylene phosphonic five, 0.3% second of its gross mass 5% are added into the mixture A obtained by operation a
Ethylenediamine tetraacetic acid (EDTA), 0.5% sodium tartrate, the three of 0.15% oxidation second secretarys, are stirred continuously after processing uniformly, then adjust overall pH
Be worth for 6.5 ~ 7.0 mixture B it is standby；
（2）Calcination process：
By step（1）The mixture B of gained is put into roaster, and heating keeps the temperature in roaster to be 850 DEG C, continuous heating
Handle 1.5h, electron beam irradiation processing during which carried out to mixture B simultaneously, after the completion of take out, after filtration drying semi-finished product strontium
Ferromagnetic oxide powder is standby；
（3）Ball mill grinding：
By step（2）Semi-finished product strontium ferrite magnetic powder after processing, which is put into planetary ball mill, carries out ball-milling treatment, wherein ball
Grinding media is taking-up drying finished product strontium ferrite magnetic powder after ethanol, ball milling 35min.
Further, step（2）Described in electron beam irradiation processing when close rate be 0.6kGy/min.
Further, step（3）Described in ball milling after drying temperature control be 80 DEG C.
Comparative example 1
This comparative example 1 compared with Example 2, in step（1）Without ethylenediamine tetra-acetic acid and wine in raw material married operation b
Stone acid sodium composition, method and step all same in addition.
Comparative example 2
This comparative example 2 compared with Example 2, in step（2）Handled in calcination process without electron beam irradiation, in addition
Method and step all same.
Comparative example 3
This comparative example 3 compared with Example 2, in step（1）Without ethylenediamine tetra-acetic acid and wine in raw material married operation b
Stone acid sodium composition, while in step（2）Handled in calcination process without electron beam irradiation, method and step in addition is homogeneous
Together.
In order to contrast effect of the present invention, to above-described embodiment 2, comparative example 1, comparative example 2, comparative example 3
Strontium ferrite magnetic powder made from described method carries out performance test, and specific correction data is as shown in table 1 below：
Table 1
| Remanent magnetism Br（Gs） | HCJ Hcj（Oe） | Curie temperature（℃） | |
| Embodiment 2 | 3910 | 4.7×104 | 821 |
| Comparative example 1 | 3640 | 4.3×104 | 768 |
| Comparative example 2 | 3580 | 4.0×104 | 735 |
| Comparative example 3 | 3260 | 3.6×104 | 680 |
Preparation method of the present invention can effectively improve the synthesis of magnetic and use characteristic it can be seen from upper table 1, improve it and use
Value, is that material base has been established in the manufacture of more quality product.
Claims (3)
1. a kind of preparation method of high-quality injection strontium ferrite magnetic powder, it is characterised in that comprise the following steps：
（1）Raw material is mixed：
A. first strontium carbonate and ferric crystals are mixed, the mol ratio of strontium and iron is 1 in strontium carbonate and ferric nitrate after mixing：
12 ~ 13, nitric acid, 7 ~ 9 times of the deionized water of 1 ~ 1.2 times of strontium carbonate and ferric crystals gross mass are then added, is stirred continuously
It is standby that mixture A is obtained after 30 ~ 40min of processing；
B. to operation a obtained by mixture A in add its gross mass 3 ~ 5% the sodium of diethylene triamine pentamethylene phosphonic five, 0.1 ~
0.3% ethylenediamine tetra-acetic acid, 0.2 ~ 0.5% sodium tartrate, the three of 0.1 ~ 0.15% oxidation second secretarys, are stirred continuously processing uniform
Afterwards, then adjust overall pH value for 6.5 ~ 7.0 mixture B it is standby；
（2）Calcination process：
By step（1）The mixture B of gained is put into roaster, and heating keeps the temperature in roaster to be 800 ~ 850 DEG C, continues
Heat 1 ~ 1.5h, electron beam irradiation processing during which carried out to mixture B simultaneously, after the completion of take out, after filtration drying half
Finished product strontium ferrite magnetic powder is standby；
（3）Ball mill grinding：
By step（2）Semi-finished product strontium ferrite magnetic powder after processing, which is put into planetary ball mill, carries out ball-milling treatment, wherein ball
Grinding media is taking-up drying finished product strontium ferrite magnetic powder after ethanol, 30 ~ 35min of ball milling.
2. a kind of preparation method of high-quality injection strontium ferrite magnetic powder according to claim 1, it is characterised in that step
Suddenly（2）Described in electron beam irradiation processing when close rate be 0.4 ~ 0.6kGy/min.
3. a kind of preparation method of high-quality injection strontium ferrite magnetic powder according to claim 1, it is characterised in that step
Suddenly（3）Described in ball milling after drying temperature control be 75 ~ 80 DEG C.
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Citations (6)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| JP2006225601A (en) * | 2005-02-21 | 2006-08-31 | Uchiyama Mfg Corp | Magnetic rubber composition, and molding method thereof using it |
| CN101004961A (en) * | 2006-12-11 | 2007-07-25 | 电子科技大学 | Process for preparing high frequency high power ferrite material |
| CN101913854A (en) * | 2010-08-18 | 2010-12-15 | 重庆大学 | Preparation method of nanometer strontium ferrite magnetic powder |
| CN102732397A (en) * | 2011-04-02 | 2012-10-17 | 上海制皂有限公司 | Boric acid decontamination soap |
| US20130256584A1 (en) * | 2012-03-30 | 2013-10-03 | Fujifilm Corporation | Hexagonal strontium ferrite magnetic powder and method of manufacturing the same, and magnetic recording medium and method of manufacturing the same |
| US20150187380A1 (en) * | 2013-12-27 | 2015-07-02 | Fujifilm Corporation | Magnetic powder for magnetic recording, magnetic recording medium, and method of manufacturing magnetic powder for magnetic recording |
-
2017
- 2017-05-17 CN CN201710348081.8A patent/CN107151136A/en active Pending
Patent Citations (6)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| JP2006225601A (en) * | 2005-02-21 | 2006-08-31 | Uchiyama Mfg Corp | Magnetic rubber composition, and molding method thereof using it |
| CN101004961A (en) * | 2006-12-11 | 2007-07-25 | 电子科技大学 | Process for preparing high frequency high power ferrite material |
| CN101913854A (en) * | 2010-08-18 | 2010-12-15 | 重庆大学 | Preparation method of nanometer strontium ferrite magnetic powder |
| CN102732397A (en) * | 2011-04-02 | 2012-10-17 | 上海制皂有限公司 | Boric acid decontamination soap |
| US20130256584A1 (en) * | 2012-03-30 | 2013-10-03 | Fujifilm Corporation | Hexagonal strontium ferrite magnetic powder and method of manufacturing the same, and magnetic recording medium and method of manufacturing the same |
| US20150187380A1 (en) * | 2013-12-27 | 2015-07-02 | Fujifilm Corporation | Magnetic powder for magnetic recording, magnetic recording medium, and method of manufacturing magnetic powder for magnetic recording |
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