CN107117954A - A kind of preparation method of high-performance permanent-magnet ferrite - Google Patents
A kind of preparation method of high-performance permanent-magnet ferrite Download PDFInfo
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- CN107117954A CN107117954A CN201710290210.2A CN201710290210A CN107117954A CN 107117954 A CN107117954 A CN 107117954A CN 201710290210 A CN201710290210 A CN 201710290210A CN 107117954 A CN107117954 A CN 107117954A
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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
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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
- C04B35/622—Forming processes; Processing powders of inorganic compounds preparatory to the manufacturing of ceramic products
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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
- C04B35/622—Forming processes; Processing powders of inorganic compounds preparatory to the manufacturing of ceramic products
- C04B35/64—Burning or sintering processes
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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
- H01F1/12—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
- H01F1/342—Oxides
- H01F1/344—Ferrites, e.g. having a cubic spinel structure (X2+O)(Y23+O3), e.g. magnetite Fe3O4
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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
- 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
- C04B2235/3205—Alkaline earth oxides or oxide forming salts thereof, e.g. beryllium oxide
- C04B2235/3206—Magnesium oxides or oxide-forming salts thereof
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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
- 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
- C04B2235/3205—Alkaline earth oxides or oxide forming salts thereof, e.g. beryllium oxide
- C04B2235/3208—Calcium oxide or oxide-forming salts thereof, e.g. lime
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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
- 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
- C04B2235/3294—Antimony oxides, antimonates, antimonites or oxide forming salts thereof, indium antimonate
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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
- 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
- C04B2235/3418—Silicon oxide, silicic acids, or oxide forming salts thereof, e.g. silica sol, fused silica, silica fume, cristobalite, quartz or flint
Abstract
The invention discloses a kind of preparation method of high-performance permanent-magnet ferrite.It specifically includes following steps：(1) Preburning material：Using market sale Preburning material；(2) ball milling：Weigh Preburning material, addition magnesia or one kind in antimony oxide or two kinds after sintering aid and corresponding additive as carrying out ball milling；(3) it is compressing：It is molded in 8000Oe magnetic fields, briquetting pressure is 3~10MPa, obtains formed body；(4) sinter：0.1~3 hour is incubated at 1000~1100 DEG C, heating rate is 3 DEG C/min；(5) post-process：Grinding, is cleaned, detection.The beneficial effects of the invention are as follows：Ferrite particle is conducive to be sintered at a lower temperature, can to reduce energy consumption cost-effective by reducing sintering temperature, and is conducive to suppressing abnormal grain growth so that homogeneous grain size, keeps magnetic property not reduce.
Description
Technical field
The present invention relates to permanent-magnet ferrite material correlative technology field, a kind of system of high-performance permanent-magnet ferrite is referred in particular to
Preparation Method.
Background technology
M type permanent-magnet ferrites are a kind of oxides with ferrimagnetism, with good magnetic property, and cost performance is protruded,
It is widely used in the fields such as an electric notor, sensor, office equipment, automobile motor, Medical Devices.
Its main development direction is to be introduced into Ca elements on formula completely or partially to replace in hexagonal M type ferrites in recent years
Sr position, while in order to keep crystal structure stable and electricity price balances addition part La and Co oxide, and herein
On the basis of carry out the ions of other elements and replace so that it is different to obtain stable Hxagonal ferrite crystal, bigger magnetocrystalline
Property constant K1 and Geng Gao material saturation magnetization Ms values, while can further be carried by improving the microstructure of sintered body
The magnetic property of high product.However, as patent CN2013107447669.2 etc. is mentioned, preparing permanent-magnet ferrite material often
Need in 1150~1250 DEG C of sintering, be the process of a high energy consumption.It is generally acknowledged that permanent magnetism ferrite sintered body can pass through oxidation
The joint addition control grain size of silicon and calcium oxide, or adjust in some scopes sintering temperature, but only addition oxidation
Calcium, silica can cause remanent magnetism or HCJ to change, and it controls the scope of sintering temperature to be limited.
The content of the invention
The present invention be in order to overcome the shortcomings of to exist in the prior art it is above-mentioned there is provided a kind of even if reduction sintering temperature
The preparation method for the high-performance permanent-magnet ferrite that magnetic property do not reduce can be kept.
To achieve these goals, the present invention uses following technical scheme：
A kind of preparation method of high-performance permanent-magnet ferrite, specifically includes following steps：
(1) Preburning material：Using market sale Preburning material；
(2) ball milling：Weigh Preburning material, addition magnesia or one kind in antimony oxide or two kinds as sintering aid with
And carry out ball milling after corresponding additive；
(3) it is compressing：It is molded in 8000Oe magnetic fields, briquetting pressure is 3~10MPa, obtains formed body；
(4) sinter：0.1~3 hour is incubated at 1000~1100 DEG C, heating rate is 3 DEG C/min；
(5) post-process：Grinding, is cleaned, detection.
The present invention is used as sintering aid by adding the one or two kinds of in low melting point oxide antimony oxide, magnesia,
Ferrite particle is conducive to be sintered at a lower temperature, can to reduce energy consumption cost-effective by reducing sintering temperature, and
And be conducive to suppressing abnormal grain growth so that homogeneous grain size, keep magnetic property not reduce.
Preferably, in step (2), the addition of sintering aid is in below 0.5wt%, and Ball-milling Time is 14~16 small
When, the average-size of particle is 0.8~1.0 μm after ball milling.Due to when adding magnesia or antimony oxide as sintering aid
The consistency increase for promoting magnet is limited, so needing the addition of strict control sintering aid, and is controlled after ball milling
Size is to preferably ensure magnet HCJ.When the particle diameter less than 0.8 μm is more, paramagnetic phenomenon, magnetic can be caused
Performance is reduced；And the shaping degree of orientation is not high when particle is more more than single domain size, cause remanent magnetism relatively low.
Preferably, in step (3), the slurry moisture content obtained after ball milling is 30~40%, is then suppressed
Shaping.If water content necessarily increases molding time higher than more than 40%, operating efficiency is reduced, and blank moisture content rises,
Moisture discharges tearing tendency increase not in time during sintering.
Preferably, in step (4), base substrate being incubated into 1 hour at 200~300 DEG C to remove moisture, then carried out
Sintering.
Preferably, in step (5), it is necessary to which magnet is incubated into 24 hours at 23 DEG C after grinding cleaning, then carrying out
Detection.
The beneficial effects of the invention are as follows：Be conducive to ferrite particle to be sintered at a lower temperature, sintered by reducing
It is cost-effective that temperature can reduce energy consumption, and is conducive to suppressing abnormal grain growth so that homogeneous grain size, keeps magnetic
It can not reduce.
Embodiment
With reference to embodiment, the present invention will be further described.
Embodiment 1：
Commercially available Y30-1 Preburning materials 1Kg is chosen, addition 1g silica, 2.5g calcium carbonate, 1g magnesia and 1g antimony oxides are carried out
Mixing and ball milling, the time is 16 hours, and rotating speed is 30r/min, and the average-size of particle is 0.8 μm.Obtain the slurry of above-mentioned steps
Moisture content is 30~40%, is then molded in 8000Oe magnetic fields, and briquetting pressure is 3~10MPa, obtains a diameter of of formed body
6cm, high 1.5cm.Base substrate is incubated 1 hour at 120 DEG C to remove moisture, then 1 hour is incubated at 1100 DEG C, heating rate
For 3 DEG C/min.Ferrite sintered magnet is obtained, magnet is incubated 24 hours at 23 DEG C after grinding cleaning, magnet magnetic is then measured
Performance.
Comparative example 1：
Commercially available Y30-1 Preburning materials 1Kg is chosen, 1g silica, 2.5g calcium carbonate is added, carries out mixing and ball milling, the time is 16
Hour, rotating speed is 30r/min, and the average-size of particle is 0.8 μm.The slurry moisture content for obtaining above-mentioned steps is 35%, then
It is molded in 8000Oe magnetic fields, briquetting pressure is 5MPa, obtains a diameter of 6cm of formed body, high 1.5cm.By base substrate at 120 DEG C
1 hour is incubated to remove moisture, then 13 hours are incubated at 1220 DEG C, heating rate is 3 DEG C/min.Obtain ferrite sintered
Magnet, is incubated 24 hours at 23 DEG C by magnet after grinding cleaning, then measures magnet magnetic property.
The embodiment 1 of table 1 and the magnet magnetic property of comparative example 1
Table 1 is the magnetic property of embodiment 1 and the gained magnet of comparative example 1.As shown in Table 1 addition 0.1wt% magnesia and
After 0.1wt% antimony oxides, magnet Br slightly has rising, and Hcj rises simultaneously are larger.The method for surveying density with drainage can be measured
The sample rate of embodiment 1 is 5.03g/m3, and the density of the sample of comparative example 1 is 5.0g/m3, this be due to add magnesia and
The progress that can be reacted after antimony oxide under conditions of lower temperature with acceleration of sintering, so as to be conducive to improving the consistency of magnet.
And it is 1.6 μm of average crystalline substances for being greater than embodiment that the average grain size of comparative example 1 is found after to magnet Analysis on Microstructure
1.2 μm of particle size, and this is also the reason for magnet HCJ of embodiment 1 is high compared with comparative example 1.
Embodiment 2：
Commercially available Y30-1 Preburning materials 1Kg is chosen, mixing and ball milling experiment is carried out according to the dispensing of table 2 respectively, the time is 14 hours,
Rotating speed is 30r/min, and the average-size of particle is 1.0 μm.The slurry moisture content for obtaining above-mentioned steps is 30%, Ran Hou
It is molded in 8000Oe magnetic fields, briquetting pressure is 8MPa, obtains a diameter of 6cm of formed body, high 1.5cm.By base substrate in 120 DEG C of guarantors
Warm 1 hour, to remove moisture, is then incubated 1 hour according to sintering temperature in table 2 respectively, and heating rate is 3 DEG C/min.Obtain
Ferrite sintered magnet, 24 hours are incubated after grinding cleaning by magnet at 23 DEG C, then measure magnet magnetic property as shown in table 3.
The each group distribution ratio of 2 embodiment of table 2
The magnet magnetic property of 3 embodiment of table 2
Table 3 is the magnetic property of the gained magnet of embodiment 2.Understood by table 2, table 3 with magnesia or antimony oxide addition
Change, corresponding optimal sintering temperature can change, while the magnetic property of magnet is not less than the magnet magnetic of comparative example 1
Energy.Downward trend after first rising is presented with the addition increase magnet Br of magnesia or antimony oxide, this is due to work as to add
Plus magnesia or antimony oxide are limited as the consistency increase for promoting magnet during sintering aid, when addition magnesia or
Antimony content is aoxidized to the consistency of magnet during 0.3wt% not in increase, simultaneously because under the increase magnet Br of non-magnetic phase slightly has
Drop.Due to the reduction of sintering temperature, the crystallite dimension of magnet is relatively small, so higher Hcj can be kept.
Claims (5)
1. a kind of preparation method of high-performance permanent-magnet ferrite, it is characterized in that, specifically include following steps：
(1) Preburning material：Using market sale Preburning material；
(2) ball milling：Weigh Preburning material, addition magnesia or one kind in antimony oxide or two kinds are used as sintering aid and phase
Ball milling is carried out after the additive answered；
(3) it is compressing：It is molded in 8000Oe magnetic fields, briquetting pressure is 3~10MPa, obtains formed body；
(4) sinter：0.1~3 hour is incubated at 1000~1100 DEG C, heating rate is 3 DEG C/min；
(5) post-process：Grinding, is cleaned, detection.
2. a kind of preparation method of high-performance permanent-magnet ferrite according to claim 1, it is characterized in that, in step (2),
The addition of sintering aid is 14~16 hours in below 0.5wt%, Ball-milling Time, and the average-size of particle is 0.8 after ball milling
~1.0 μm.
3. a kind of preparation method of high-performance permanent-magnet ferrite according to claim 1 or 2, it is characterized in that, in step (3)
In, the slurry moisture content obtained after ball milling is 30~40%, is then pressed.
4. a kind of preparation method of high-performance permanent-magnet ferrite according to claim 3, it is characterized in that, in step (4),
Base substrate is incubated 1 hour at 200~300 DEG C to remove moisture, is then sintered.
5. a kind of preparation method of high-performance permanent-magnet ferrite according to claim 1, it is characterized in that, in step (5),
, it is necessary to which magnet is incubated into 24 hours at 23 DEG C after grinding cleaning, then detected.
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| Application Number | Priority Date | Filing Date | Title |
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| CN201710290210.2A CN107117954A (en) | 2017-04-27 | 2017-04-27 | A kind of preparation method of high-performance permanent-magnet ferrite |
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| CN201710290210.2A CN107117954A (en) | 2017-04-27 | 2017-04-27 | A kind of preparation method of high-performance permanent-magnet ferrite |
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Cited By (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN107564652A (en) * | 2017-09-15 | 2018-01-09 | 安徽信息工程学院 | A kind of inorganic composite materials IV for permanent-magnet material and preparation method thereof |
| CN108892489A (en) * | 2018-06-25 | 2018-11-27 | 河津市锦浩特种陶瓷有限公司 | Easy fired high alumina ceramic and preparation method thereof |
| CN109836148A (en) * | 2019-02-22 | 2019-06-04 | 横店集团东磁股份有限公司 | One kind is without La, Co element permanent-magnet ferrite material and preparation method thereof |
Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| JPH06151151A (en) * | 1992-11-06 | 1994-05-31 | Kawasaki Steel Corp | Mn-zn type ferrite |
| CN102311260A (en) * | 2011-08-08 | 2012-01-11 | 中国地质大学（北京） | Novel MnZn-doped ferrite material and preparation method thereof |
| CN106145917A (en) * | 2016-06-23 | 2016-11-23 | 南京航空航天大学 | A kind of coercitive secondary of permanently magnetic strontium ferrite that improves is combined adding method |
-
2017
- 2017-04-27 CN CN201710290210.2A patent/CN107117954A/en active Pending
Patent Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| JPH06151151A (en) * | 1992-11-06 | 1994-05-31 | Kawasaki Steel Corp | Mn-zn type ferrite |
| CN102311260A (en) * | 2011-08-08 | 2012-01-11 | 中国地质大学（北京） | Novel MnZn-doped ferrite material and preparation method thereof |
| CN106145917A (en) * | 2016-06-23 | 2016-11-23 | 南京航空航天大学 | A kind of coercitive secondary of permanently magnetic strontium ferrite that improves is combined adding method |
Cited By (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN107564652A (en) * | 2017-09-15 | 2018-01-09 | 安徽信息工程学院 | A kind of inorganic composite materials IV for permanent-magnet material and preparation method thereof |
| CN108892489A (en) * | 2018-06-25 | 2018-11-27 | 河津市锦浩特种陶瓷有限公司 | Easy fired high alumina ceramic and preparation method thereof |
| CN109836148A (en) * | 2019-02-22 | 2019-06-04 | 横店集团东磁股份有限公司 | One kind is without La, Co element permanent-magnet ferrite material and preparation method thereof |
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