CN104496452B - A kind of ferrite preparation method and its prepared ferrite - Google Patents

A kind of ferrite preparation method and its prepared ferrite Download PDF

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CN104496452B
CN104496452B CN201410853445.4A CN201410853445A CN104496452B CN 104496452 B CN104496452 B CN 104496452B CN 201410853445 A CN201410853445 A CN 201410853445A CN 104496452 B CN104496452 B CN 104496452B
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ferrite
prefiring material
ferrite prefiring
preparation
vibration
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CN104496452A (en
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刘辉
李炳山
滕阳民
徐文生
魏汉中
王颖泉
全小康
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North Polytron Technologies Inc
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Beikuan Magnetic-Material Science & Technology Co Ltd
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Abstract

The invention discloses a kind of ferrite preparation method and its prepared ferrite, comprise the following steps:Prepare ferrite prefiring material and carry out wet crushing processing, obtain ferrite prefiring material slurry;Drying and processing is carried out to ferrite prefiring material slurry;The vibration carried out using vibrating ball-mill to ferrite prefiring material xeraphium 20~40 minutes is handled;High speed decentralized processing is carried out to the powder after vibration;Ferrite prefiring material powder of the high speed after scattered is uniformly mixed with adhesive, is placed in carrying out in magnetic field dry-pressing formed, shaping ferrite is obtained;Shaping ferrite is sintered, that is, obtains high performance dry-press process sintered permanent ferrite.The present invention can not only improve the ferritic density of shaping, and the adhesion of ferrite paricles intergranular can be reduced, lift the dispersiveness of ferrite particle, ferrite particle is set to be got a promotion along the degree of alignment of direction of easy axis, the degree of orientation of particle is greatly improved, and is greatly improved therefore, it is possible to the magnetic property that makes dry-press process sintered permanent ferrite.

Description

A kind of ferrite preparation method and its prepared ferrite
Technical field
The present invention relates to ferrite sintered body field, more particularly to a kind of ferrite preparation method and its prepared iron oxygen Body.
Background technology
At present, the forming method of anisotropy sintered permanent ferrite can be divided mainly into wet moulding and dry-press process two Kind.
In wet moulding, due to there is the presence of the decentralized media such as water or ethanol, therefore ferrite particle is easy to rotate, iron oxygen Body particle is easy to arrange along direction of easy axis in magnetic field, and this can make the ferrite of shaping obtain the higher degree of orientation, therefore wet The ferrite of method shaping results in higher magnetic property.But, wet moulding needs by scattered to be situated between during extrusion forming Matter is discharged to outside die cavity, therefore productivity ratio is relatively low;In addition, requirement of the wet moulding to production equipment is higher, production cost is also more It is high.
In existing dry-press process, dry ferrite powder is directly filled into die cavity, is then added in magnetic field It is molded.Compared with wet moulding, because the friction of no decentralized medium, therefore ferrite paricles intergranular increased dramatically, and iron oxygen There is inevitable adhesion in drying course in body particle, and the degree for causing ferrite particle to be arranged along direction of easy axis is obvious Reduction, this can reduce the ferritic degree of orientation of shaping, therefore the magnetic that the ferrite of dry-press process is obtained in the prior art Can be poor.But, dry-press process has shaping speed fast, and production efficiency is high, the advantages of former is simple.
As shown in figure 1, in order to obtain high performance dry-press process sintered permanent ferrite, mainly using in the prior art The method for adding lubricant 2 into dry ferrite powder before the forming, its concrete technical scheme is referred to Application No. CN02803279.9 and CN200710066750.9 Chinese patent, this can reduce the frictional force between ferrite particle 1, improve The mobility of ferrite particle 1, makes ferrite particle 1 be easy to arrange along direction of easy axis in magnetic field.But, this method pair Ferritic performance improves limited.
The content of the invention
For above-mentioned weak point of the prior art, the invention provides a kind of ferrite preparation method and its prepared Ferrite, the ferritic density of shaping can not only be improved, and the adhesion of ferrite paricles intergranular can be reduced, lift iron oxygen The intergranular dispersiveness of body, so as to improve degree of alignment of the ferrite particle along direction of easy axis, makes taking for ferrite particle Greatly improve, greatly improved therefore, it is possible to the magnetic property that makes dry-press process sintered permanent ferrite to degree.
The purpose of the present invention is achieved through the following technical solutions:
A kind of ferrite preparation method, comprises the following steps:
Step A, prepares ferrite prefiring material, and carries out wet crushing processing to ferrite prefiring material, until ferrite is pre- The particle mean size of imitation frosted glass reaches 0.8~0.9 micron, so as to obtain ferrite prefiring material slurry;
Step B, drying and processing is carried out to ferrite prefiring material slurry, until obtaining the iron oxygen that water content is less than 0.5wt% Body Preburning material xeraphium;
Step C, is carried out after vibration processing, vibration 20~40 minutes to ferrite prefiring material xeraphium using vibrating ball-mill, obtained Ferrite prefiring material powder after to vibration;
Step D, high speed decentralized processing is carried out to the ferrite prefiring material powder after vibration, obtains the iron oxygen after disperseing at a high speed Body Preburning material powder;
Step E, ferrite prefiring material powder of the high speed after scattered is uniformly mixed with adhesive, is placed in carrying out in magnetic field It is dry-pressing formed, obtain being molded ferrite;
Step F, is sintered to shaping ferrite, and sintering temperature is 1190~1290 DEG C, after sintering 1~3 hour, i.e., Obtain high performance dry-press process sintered permanent ferrite.
Preferably, the ferrite prefiring material contains A, R, M, Ti and Fe Hxagonal ferrite principal phase, and meet as Lower formula:(1-x) AO (x/2) R2O3(n-z-y/2)Fe2O3zM2O3yTiO2
In formula, A is at least one in Sr elements or Ba elements;R is at least one of Y element or rare earth element and La members The combination of element, or R is only La elements;M is the combination of at least one of Mn elements or Zn elements and Co elements, or M is only Co elements;X, y, z is the gauge according to material respectively, meets following condition:0.04≤x≤0.5、0.04≤z≤0.4、0.005 ≤ y≤0.15, and n meets 5.5≤n≤6.0.
Preferably, described step A comprises the following steps:
Step A1, ferrite prefiring material is prepared according to the component proportion described in the claims 2;
Step A2, coarse crushing processing is carried out to ferrite prefiring material, until the particle mean size of ferrite prefiring material reach 3.0~ 4.0 microns, obtain ferrite prefiring material after coarse crushing;
Step A3, to coarse crushing after in ferrite prefiring material addition account for ferrite prefiring material gross weight 0.2% after coarse crushing SiO2With the CaCO for accounting for ferrite prefiring material gross weight 1.2% after coarse crushing3, and wet crushing is carried out in horizontal ball mill, until The particle mean size of ferrite prefiring material reaches 0.8~0.9 micron, so as to obtain ferrite prefiring material slurry.
Preferably, after the vibration processing that 30 minutes are carried out to ferrite prefiring material xeraphium, the ferrite after vibration is obtained Preburning material powder.
Preferably, in step E, described adhesive is camphor and calcium stearate mixture, and the consumption of camphor is accounted at a high speed Ferrite prefiring material powder gross weight 1.0% after scattered, and the ferrite prefiring that the consumption of calcium stearate is accounted for after disperseing at a high speed Feed powder end gross weight 0.25%.
Preferably, in step E, the size of forming magnetic field is 8000Oe, and briquetting pressure is 7MPa.
Preferably, during being sintered to shaping ferrite, heating rate is 2 DEG C/min, and sintering temperature is 1230 DEG C, after sintering 2 hours, that is, obtain high performance dry-press process sintered permanent ferrite.
Preferably, in step F, after sintering terminates, room temperature is naturally cooled to, that is, obtains high performance dry-press process and burns Tie permanent-magnet ferrite.
A kind of ferrite, is prepared from using the preparation method described in above-mentioned technical proposal.
As seen from the above technical solution provided by the invention, the dry-press process pre-burning that the embodiment of the present invention is provided Material and its prepared magnet and magnet manufacture method not use only high performance ferrite prefiring material, and in drying and processing The step of " vibration processing has been carried out to ferrite prefiring material xeraphium using vibrating ball-mill " being provided between high speed decentralized processing, This vibration processing procedure can reduce the adhesion of ferrite paricles intergranular, lift the dispersiveness and compressibility of ferrite particle, Degree of alignment of the ferrite particle along direction of easy axis is set significantly to be strengthened, the degree of orientation of ferrite particle greatly improved in this And it is molded ferritic density, greatly improved therefore, it is possible to the magnetic property that makes dry-press process sintered permanent ferrite.With it is existing The preparation method of dry-press process ferrite sintered body in technology is compared, and the ferrite preparation method that the embodiment of the present invention is provided is carried Go out the technical scheme for reducing ferrite paricles intergranular adhesion, breach lubricant in the prior art limited to ferrite performance lifting Bottleneck so that the magnetic property of dry-press process sintered permanent ferrite is largely increased compared with prior art.
Brief description of the drawings
Technical scheme in order to illustrate more clearly the embodiments of the present invention, below will be to that will use needed for embodiment description Accompanying drawing be briefly described, it should be apparent that, drawings in the following description are only some embodiments of the present invention, for this For the those of ordinary skill in field, on the premise of not paying creative work, other can also be obtained according to these accompanying drawings Accompanying drawing.
Fig. 1 is principle schematic of the raising magnetic powder particle along direction of easy axis degree of alignment in existing dry pressuring forming process.
Fig. 2 is principle schematic of the raising magnetic powder particle along direction of easy axis degree of alignment in the embodiment of the present invention.
Fig. 3 is the XRD spectrum provided in an embodiment of the present invention passed through and obtained magnet is processed without vibration.
Embodiment
The technical scheme in the embodiment of the present invention is clearly and completely described below in conjunction with the accompanying drawings, it is clear that described Embodiment be only a part of embodiment of the invention, rather than whole embodiment.Based on embodiments of the invention, this area The every other embodiment that those of ordinary skill is obtained under the premise of creative work is not made, belongs to the guarantor of the present invention Protect scope.
The ferrite preparation method and its prepared ferrite provided below the embodiment of the present invention is retouched in detail State.
A kind of ferrite preparation method, it specifically may comprise steps of:
Step A, prepares ferrite prefiring material, and carries out wet crushing processing to ferrite prefiring material, until ferrite is pre- The particle mean size of imitation frosted glass reaches 0.8~0.9 micron, so as to obtain ferrite prefiring material slurry.
Wherein, described ferrite prefiring material contains A, R, M, Ti and Fe Hxagonal ferrite principal phase, and meet as Lower formula:(1-x) AO (x/2) R2O3(n-z-y/2)Fe2O3zM2O3yTiO2;In formula, A be in Sr elements or Ba elements at least It is a kind of;R is the combination of at least one of Y element or rare earth element and La elements, or R is only La elements;M is Mn elements or Zn The combination of at least one of element and Co elements, or M are only Co elements;X, y, z is the gauge according to material respectively, is met such as Lower condition:0.04≤x≤0.5,0.04≤z≤0.4,0.005≤y≤0.15, and n meets 5.5≤n≤6.0.According to above-mentioned group Divide and carry out dispensing, and sintered at 1160~1260 DEG C, you can obtain high performance ferrite prefiring material.The ferrite prefiring material It with high-performance, can greatly improve the magnetic property of prepared dry-press process sintered permanent ferrite.In actual applications, Step A specifically includes following steps:
Step A1, ferrite prefiring material is prepared according to the component proportion of ferrite prefiring material described in above-mentioned technical proposal.
Step A2, coarse crushing processing is carried out to ferrite prefiring material, until the particle mean size of ferrite prefiring material reach 3.0~ 5.0 microns, obtain ferrite prefiring material after coarse crushing.In actual applications, can be using dry mill of the prior art to iron oxygen Body Preburning material carries out coarse crushing processing.
Step A3, to coarse crushing after in ferrite prefiring material addition account for ferrite prefiring material gross weight 0.2% after coarse crushing SiO2With the CaCO for accounting for ferrite prefiring material gross weight 1.2% after coarse crushing3, and wet crushing is carried out in horizontal ball mill, until The particle mean size of ferrite prefiring material reaches 0.8~0.9 micron, so as to obtain ferrite prefiring material slurry.
Step B, drying and processing is carried out to ferrite prefiring material slurry, until obtaining the iron oxygen that water content is less than 0.5wt% Body Preburning material xeraphium.
Wherein, drying temperature is preferably 140 DEG C, and the constant temperature drying time is preferably 2 hours, is less than until obtaining water content 0.5wt% ferrite prefiring material xeraphium.
Step C, is carried out after vibration processing, vibration 20~40 minutes to ferrite prefiring material xeraphium using vibrating ball-mill, obtained Ferrite prefiring material powder after to vibration.
Wherein, vibration processing, preferably vibration 30 minutes, you can obtain after vibration are carried out to ferrite prefiring material xeraphium Ferrite prefiring material powder.
Step D, high speed decentralized processing is carried out to the ferrite prefiring material powder after vibration, obtains the iron oxygen after disperseing at a high speed Body Preburning material powder.
Wherein, high speed decentralized processing can be handled using high speed dispersor in the prior art, it would however also be possible to employ prior art In the high speed disintegrator similar with high speed dispersor operation principle handle.
Step E, ferrite prefiring material powder of the high speed after scattered is uniformly mixed with adhesive, is placed in carrying out in magnetic field It is dry-pressing formed, obtain being molded ferrite.
Wherein, described adhesive is camphor and calcium stearate mixture, and the consumption of camphor accounts for the ferrite after high speed is disperseed The 1.0% of Preburning material powder gross weight, and the ferrite prefiring material powder gross weight that the consumption of calcium stearate is accounted for after disperseing at a high speed 0.25%;The size of forming magnetic field is 8000Oe, and briquetting pressure is 7MPa.
Step F, is sintered to shaping ferrite, and sintering temperature is 1190~1290 DEG C, after sintering 1~3 hour, i.e., Obtain high performance dry-press process sintered permanent ferrite.
Wherein, during being sintered to shaping ferrite, heating rate is preferably 2 DEG C/min, and sintering temperature is most It is 1230 DEG C well, and preferably terminates sintering after sintering 2 hours, then naturally cool to room temperature, that is, obtains high performance dry method Forming and sintering permanent-magnet ferrite.
Further, the ferrite preparation method mainly improves dry-press process sintered permanent by following two aspects The magnetic property of oxysome:First, the ferrite preparation method employs high performance ferrite prefiring material, prepared so as to make The magnetic property of dry-press process sintered permanent ferrite be largely increased.Second, the ferrite preparation method is in drying and processing The step of " vibration processing has been carried out to ferrite prefiring material xeraphium using vibrating ball-mill " being provided between high speed decentralized processing, And this vibration processing procedure can reduce the adhesion of ferrite paricles intergranular, the dispersed and compressible of ferrite particle is lifted Property, degree of alignment of the ferrite particle along direction of easy axis is significantly strengthened, taking for ferrite particle greatly improved in this To spending and be molded ferritic density, greatly improved therefore, it is possible to the magnetic property that makes dry-press process sintered permanent ferrite;Its Concrete principle can with as shown in Fig. 2 vibration processing processing before, ferrite particle a is sticked together with ferrite particle b, Ferrite particle a direction of easy axis is α, and the direction of easy axis of ferrite particle is β, therefore ferrite particle a and ferrite Degree of alignment of the particle b along direction of easy axis is very low, and in vibration processing processing procedure, ferrite particle a and ferrite paricles Grain b adhesions are shaken out, and ferrite particle disperses, therefore ferrite particle is improved along the degree of alignment of direction of easy axis.
It should be noted that compared with the preparation method of dry-press process ferrite sintered body of the prior art, the present invention is real Apply the ferrite preparation method that example provided and propose the technical scheme for reducing ferrite paricles intergranular adhesion, breach prior art Middle lubricant lifts limited bottleneck to ferrite performance so that the magnetic property of dry-press process sintered permanent ferrite with it is existing Technology is compared and is largely increased.
A kind of ferrite, is prepared from using the ferrite preparation method described in above-mentioned technical proposal.
In order to more clearly from show technical scheme provided by the present invention and produced technique effect, below with several Ferrite preparation method provided by the present invention and its prepared ferrite are described in detail individual specific embodiment.
Embodiment one
A kind of ferrite, is prepared from, its specific steps includes using following ferrite preparation method:
Step A1 ', ferrite prefiring material is prepared according to the component proportion of following ferrite prefiring materials.
Wherein, ferrite prefiring material contains A, R, M, Ti and Fe Hxagonal ferrite principal phase, and meets below formula: (1-x) AO (x/2) R2O3(n-z-y/2)Fe2O3zM2O3yTiO2;In formula, A uses Sr elements;R uses La elements;M uses Co Element;X, y, z is the gauge according to material respectively, meets following condition:X=0.2, y=0.01, z=0.1, and n=5.87.
Step A2 ', coarse crushing processing is carried out using dry mill to ferrite prefiring material, until ferrite prefiring material after crushing Particle mean size reaches 3.0~5.0 microns, that is, obtains ferrite prefiring material after coarse crushing.
Step A3 ', takes ferrite prefiring material 300g after above-mentioned coarse crushing, and adds and account for into ferrite prefiring material after the coarse crushing The SiO of ferrite prefiring material gross weight 0.2% after coarse crushing2With the CaCO for accounting for ferrite prefiring material gross weight 1.2% after coarse crushing3, and Wet crushing is carried out in horizontal ball mill, after crushing 9.5 hours, the particle mean size of ferrite prefiring material reaches 0.85 micron, Specific surface area is 6.06cm2/ g, so as to obtain the ferrite prefiring material slurry after wet crushing.
Step B ', drying and processing is carried out to ferrite prefiring material slurry, and drying temperature is 140 DEG C, constant temperature drying 2 hours Afterwards, the ferrite prefiring material xeraphium that water content is less than 0.5wt% is obtained.
Step C ', is carried out after vibration processing, vibration 30 minutes to ferrite prefiring material xeraphium using vibrating ball-mill, is shaken Ferrite prefiring material powder after mill;The particle mean size of ferrite prefiring material powder after the vibration is 0.82 micron, compares surface Product is 6.68cm2/g。
Step D ', carries out 1 high speed decentralized processing to the ferrite prefiring material powder after vibration using high speed dispersor, obtains To ferrite prefiring material powder of the high speed after scattered.
Step E ', into ferrite prefiring material powder of the high speed after scattered, the ferrite prefiring that addition is accounted for after disperseing at a high speed The camphor of feed powder end gross weight 1.0% and the stearic acid of the ferrite prefiring material powder gross weight 0.25% accounted for after disperseing at a high speed Calcium, and mixed at high speed is carried out, it is well mixed mixture;It is placed in again in magnetic field and carries out dry-pressing formed, the size of forming magnetic field For 8000Oe, briquetting pressure is 7MPa, so as to can obtain forming iron oxysome;The ferritic a diameter of 33mm of the shaping, height For 12mm.
Step F ', is sintered to shaping ferrite, and heating rate is 2 DEG C/min, and sintering temperature is 1230 DEG C, herein Temperature sinters completion after 2 hours, naturally cool to room temperature, that is, obtains high performance dry-press process sintered permanent ferrite.
Further, measurement embodiment 1 institute it is final made from dry-press process sintered permanent ferrite the degree of orientation, its is specific Magnet XRD spectrum can be as shown in Figure 3.Meanwhile, to embodiment 1 final obtained dry-press process sintered permanent ferrite Upper and lower surface carries out mill processing, and to ferritic residual magnetic induction intensity (Br), coercivity (Hcb), the HCJ (Hcj), maximum magnetic energy product (BH) max, the performance parameter such as magnet density (ρ) is measured, its specific performance data such as institute of table 1 Show.
Comparative example 1
A kind of ferrite, employs molecule for SrFe11.8O19Traditional Strontium ferrite powder, remaining preparation process is equal It is same as Example 1, and also to obtained ferritic residual magnetic induction intensity (Br), coercivity (Hcb), HCJ (Hcj), maximum magnetic energy product (BH) max, magnet, the performance parameter such as magnet density (ρ) is measured, and its specific performance data is also such as Shown in table 1.
Table 1:
As can be seen from Table 1:Compared with the traditional Strontium ferrite powder used in comparative example 1, the iron in embodiment 1 Ferrite prefiring material can make final obtained ferritic residual magnetic induction intensity and coercivity be largely increased, it is seen then that select High performance ferrite Preburning material in embodiment 1, can obtain the magnetic property of prepared dry-press process sintered permanent ferrite To greatly improving, so as to obtain the inaccessiable dry-pressing performance of traditional Strontium ferrite powder institute.
Comparative example 2
A kind of ferrite, employs ferrite prefiring material same as Example 1, is not present and " uses in its preparation process Vibrating ball-mill carries out vibration processing to ferrite prefiring material xeraphium " the step of, remaining step is substantially the same manner as Example 1, i.e. iron Ferrite prefiring material dries powder and carries out vibration processing, but directly carries out high speed decentralized processing.
Specifically, measurement comparative example 2 institute it is final made from dry-press process sintered permanent ferrite the degree of orientation, its is specific Magnet XRD spectrum can be as shown in Figure 3.Meanwhile, above and below obtained dry-press process sintered permanent ferrite final to comparative example 2 Surface carries out mill processing, and to the ferritic residual magnetic induction intensity (Br), coercivity (Hcb), HCJ (Hcj), most Big magnetic energy product (BH) max, the performance parameter such as magnet density (ρ) is measured, and its specific performance data is as shown in table 2.
As seen from Figure 3:Compared with processing obtained permanent-magnet ferrite without vibration in comparative example 2, embodiment 1 Crystal face intensity of the obtained permanent-magnet ferrite of middle process vibration processing at (004), (006), (0014) place is significantly improved, and (107) the crystal face intensity at place is substantially reduced, and background is smooth.According to degree of orientation computing formula:The degree of orientation=∑ (00l)/∑ (hkl) understand, the degree of orientation processed by vibration is higher than the degree of orientation processed without vibration certainly.It can be seen that, pass through vibration Processing can actually open the adhesion of ferrite paricles intergranular, improve the dispersiveness of ferrite particle so that ferrite particle is along easily The degree of direction of magnetization arrangement obtains significantly higher, so as to improve the degree of orientation.
Table 2:
As can be seen from Table 2:Embodiment 1 final obtained dry-press process sintered permanent ferrite there is higher magnetic Performance, it is seen then that ferrite particle passes through vibration working process, the degree of orientation is improved, the density of magnet is also significantly improved, so as to obtain Obtained more excellent performance.
Embodiment 2
One group of ferrite, employs ferrite prefiring material same as Example 1, its preparation process and the base of embodiment 1 This is identical, and its special feature is:It is respectively 4.5 small that the wet-curshed broken time is carried out in step A3 ', in horizontal ball mill When, 7 hours, 9.5 hours, 12 hours, 16.5 hours so that after broken the particle mean size of ferrite prefiring material to correspond to 1.2 micro- Rice, 0.95 micron, 0.82 micron, 0.7 micron, 0.6 micron.
Specifically, mill processing is carried out to the upper and lower surface for implementing 2 final obtained dry-press process sintered permanent ferrites, and To the ferritic residual magnetic induction intensity (Br), coercivity (Hcb), HCJ (Hcj), maximum magnetic energy product (BH) max, magnetic The performance parameters such as volume density (ρ) and formed body yield rate are measured, and its specific performance data is as shown in table 3;In table 3, into Type body yield rate is calculated with the certified products number of every 20 pieces of pressure.
Table 3:
From table 3 it is observed that after wet crushing, the particle mean size of ferrite prefiring material is thinner, then obtained ferrite Magnetic property it is higher, but after the particle mean size of ferrite prefiring material is less than 0.8 micron, the yield rate of formed body can drastically under Drop, because the particle mean size of ferrite prefiring material is thinner, specific surface area is bigger, and the ratio surface field of ferrite particle is stronger, The gas of absorption is more, causes formed body low intensity, easily cracking, thus can not carry out large-scale production.Work as ferrite prefiring material Particle mean size be more than after 0.9 micron, although formed body yield rate very well, but magnetic property decline it is very fast, it is impossible to meeting performance will Ask.In comprehensive these two aspects problem, the embodiment of the present invention, after wet crushing, the particle mean size of ferrite prefiring material is preferably 0.8 Between~0.9 micron.
Embodiment 3
One group of ferrite, employs ferrite prefiring material same as Example 1, its preparation process and the base of embodiment 1 This is identical, and its special feature is:In step C ', vibration time of vibration processing is respectively 0 minute, 10 minutes, 20 minutes, 30 Minute, 60 minutes, 120 minutes.
Specifically, mill processing is carried out to the upper and lower surface for implementing 3 final obtained dry-press process sintered permanent ferrites, and To the ferritic residual magnetic induction intensity (Br), coercivity (Hcb), HCJ (Hcj), maximum magnetic energy product (BH) max, magnetic The performance parameters such as volume density (ρ) and formed body yield rate are measured, and its specific performance data is as shown in table 4;In table 4, into Type body yield rate is calculated with the certified products number of every 20 pieces of pressure.
Table 4:
As can be seen from Table 4, with the increase of vibration time, magnetic property Br present ascendant trend, magnet density also with Increase, because with the increase of vibration time, the degree that the adhesion of ferrite paricles intergranular is opened is higher, ferrite The degree that particle is arranged along direction of easy axis is higher, and the degree of orientation and shaping volume density of ferrite particle are higher, thus magnetic Ascendant trend is presented in performance.But, vibration process time is long, causes specific surface area to increase, the ratio surface field of ferrite particle Enhancing, the gas of absorption is more, causes formed body intensity to decrease, yield rate has declined.Comprehensive these two aspects problem, this In inventive embodiments, the vibration time is preferably 30 minutes.
As fully visible, the embodiment of the present invention can not only improve the ferritic density of shaping, and can reduce ferrite Intergranular adhesion, lifts the dispersiveness of ferrite paricles intergranular, so as to improve arrangement of the ferrite particle along direction of easy axis Degree, greatly improves the degree of orientation of ferrite particle, therefore, it is possible to make the magnetic property of dry-press process sintered permanent ferrite big Width is improved.
The foregoing is intended to be a preferred embodiment of the present invention, but protection scope of the present invention is not limited thereto, Any one skilled in the art the invention discloses technical scope in, the change or replacement that can be readily occurred in, It should all be included within the scope of the present invention.Therefore, protection scope of the present invention should be with the protection model of claims Enclose and be defined.

Claims (8)

1. a kind of ferrite preparation method, it is characterised in that comprise the following steps:
Step A, prepares ferrite prefiring material, and carries out wet crushing processing to ferrite prefiring material, until ferrite prefiring material Particle mean size reach 0.8~0.9 micron, so as to obtain ferrite prefiring material slurry;
Step B, drying and processing is carried out to ferrite prefiring material slurry, until it is pre- to obtain ferrite of the water content less than 0.5wt% Imitation frosted glass xeraphium;
Step C, is carried out after vibration processing, vibration 20~40 minutes to ferrite prefiring material xeraphium using vibrating ball-mill, is shaken Ferrite prefiring material powder after mill;
Step D, high speed decentralized processing is carried out to the ferrite prefiring material powder after vibration, obtains the ferrite after disperseing at a high speed pre- Imitation frosted glass powder;
Step E, ferrite prefiring material powder of the high speed after scattered is uniformly mixed with adhesive, is placed in magnetic field carrying out dry-pressing Shaping, obtains being molded ferrite;
Step F, is sintered to shaping ferrite, and sintering temperature is 1190~1290 DEG C, after sintering 1~3 hour, that is, is obtained High performance dry-press process sintered permanent ferrite;
The ferrite prefiring material contains A, R, M, Ti and Fe Hxagonal ferrite principal phase, and meets below formula:
(1-x) AO (x/2) R2O3(n-z-y/2)Fe2O3zM2O3 yTiO2
In formula, A is at least one in Sr elements or Ba elements;R is La elements;M is at least one of Mn elements or Zn elements With the combination of Co elements, or M is only Co elements;X, y, z is the gauge according to material respectively, meets following condition:0.04≤x ≤ 0.5,0.04≤z≤0.4,0.005≤y≤0.15, and n meets 5.5≤n≤6.0.
2. preparation method according to claim 1, it is characterised in that described step A comprises the following steps:
Step A1, ferrite prefiring material is prepared according to the component proportion described in the claims 1;
Step A2, coarse crushing processing is carried out to ferrite prefiring material, until the particle mean size of ferrite prefiring material reaches 3.0~4.0 Micron, obtains ferrite prefiring material after coarse crushing;
Step A3, to coarse crushing after in ferrite prefiring material addition account for the SiO of ferrite prefiring material gross weight 0.2% after coarse crushing2With account for The CaCO of ferrite prefiring material gross weight 1.2% after coarse crushing3, and wet crushing is carried out in horizontal ball mill, until ferrite The particle mean size of Preburning material reaches 0.8~0.9 micron, so as to obtain ferrite prefiring material slurry.
3. preparation method according to any one of claim 1 to 2, it is characterised in that to ferrite prefiring material xeraphium After the vibration processing for carrying out 30 minutes, the ferrite prefiring material powder after vibration is obtained.
4. preparation method according to any one of claim 1 to 2, it is characterised in that in step E, described bonding Agent is camphor and calcium stearate mixture, and the consumption of camphor accounts for the ferrite prefiring material powder gross weight 1.0% after high speed is disperseed, And the ferrite prefiring material powder gross weight 0.25% that the consumption of calcium stearate is accounted for after disperseing at a high speed.
5. preparation method according to any one of claim 1 to 2, it is characterised in that in step E, forming magnetic field Size is 8000 Oe, and briquetting pressure is 7MPa.
6. preparation method according to any one of claim 1 to 2, it is characterised in that burnt to shaping ferrite During knot, heating rate is 2 DEG C/min, and sintering temperature is 1230 DEG C, after sintering 2 hours, that is, obtains high performance dry Method forming and sintering permanent-magnet ferrite.
7. preparation method according to any one of claim 1 to 2, it is characterised in that in step F, when sintering terminates Afterwards, room temperature is naturally cooled to, that is, obtains high performance dry-press process sintered permanent ferrite.
8. a kind of ferrite, it is characterised in that using the preparation method preparation any one of the claims 1 to 7 Into.
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