CN104496452A - Ferrite preparation method and prepared ferrite thereby - Google Patents
Ferrite preparation method and prepared ferrite thereby Download PDFInfo
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Abstract
The invention discloses a ferrite preparation method and the prepared ferrite thereby. The method comprises the following steps: preparing a ferrite pre-sintering material and performing wet crushing treatment, thereby obtaining ferrite pre-sintering material slurry; drying the ferrite pre-sintering material slurry; performing vibro-milling treatment on the dried ferrite pre-sintering material powder for 20-40 minutes by adopting a vibration mill; performing high speed dispersion treatment on the vibro-milled powder; uniformly mixing the ferrite pre-sintering material powder subjected to high speed dispersion with an adhesive, performing dry pressing in a magnetic field, thereby obtaining the formed ferrite; sintering the formed ferrite, thereby obtaining the high-performance dry pressed and sintered permanent magnetic ferrite. According to the method disclosed by the invention, the density of the formed ferrite can be improved, adhesion among the ferrite particles can be reduced, and the dispersity of the ferrite particles is improved, so that the arrangement degree of the ferrite particles along the easy magnetization direction is improved, and the orientation degree of the particles is greatly improved. Therefore, the magnetic performance of the dry pressed and sintered permanent magnetic ferrite can be greatly improved.
Description
Technical field
The present invention relates to ferrite sintered body field, particularly relate to a kind of ferrite preparation method and prepared ferrite thereof.
Background technology
At present, the forming method of anisotropy sintered permanent ferrite mainly can be divided into wet moulding and dry-press process two kinds.
In wet moulding, owing to there being the existence of the dispersion medium such as water or ethanol, therefore ferrite particle is easy to rotate, ferrite particle is easy to arrange along easy magnetization axis in magnetic field, this can make shaping ferrite obtain higher orientation degree, and therefore the ferrite of wet moulding can obtain higher magnetic property.But wet moulding needs to be discharged to outside die cavity by dispersion medium in extrusion forming process, and therefore productivity is lower; In addition, the requirement of wet moulding to production unit is higher, and production cost is also higher.
In existing dry-press process, dry ferrite powder is directly filled in die cavity, then extrusion forming in magnetic field.Compared with wet moulding, owing to there is no dispersion medium, therefore the friction of ferrite paricles intergranular sharply increases, and there is inevitable adhesion in ferrite particle in drying course, the degree causing ferrite particle to arrange along easy magnetization axis obviously reduces, this can make shaping ferritic orientation degree reduce, and the magnetic property that therefore in prior art, the ferrite of dry-press process obtains is poor.But it is fast that dry-press process has shaping speed, the advantages such as production efficiency is high, and molding device is simple.
As shown in Figure 1, in order to obtain high performance dry-press process sintered permanent ferrite, the method of adding lubricant 2 before the forming in the ferrite powder of drying is mainly adopted in prior art, its concrete technical scheme can be the Chinese patent of CN02803279.9 and CN200710066750.9 with reference to application number, this can reduce the frictional force between ferrite particle 1, improve the mobility of ferrite particle 1, make ferrite particle 1 be easy to arrange along easy magnetization axis in magnetic field.But this method improves limited to ferritic performance.
Summary of the invention
For above-mentioned weak point of the prior art, the invention provides a kind of ferrite preparation method and prepared ferrite thereof, shaping ferritic density can not only be improved, and the adhesion of ferrite paricles intergranular can be reduced, promote the dispersiveness of ferrite paricles intergranular, thus improve the degree of alignment of ferrite particle along easy magnetization axis, the orientation degree of ferrite particle is significantly improved, therefore, it is possible to make the magnetic property of dry-press process sintered permanent ferrite significantly improve.
The object of the invention is to be achieved through the following technical solutions:
A kind of ferrite preparation method, comprises the following steps:
Steps A, prepares ferrite prefiring material, and carries out wet crushing process to ferrite prefiring material, until the mean particle size of ferrite prefiring material reaches 0.8 ~ 0.9 micron, thus obtains ferrite prefiring material slip;
Step B, carries out drying and processing to ferrite prefiring material slip, until obtain the ferrite prefiring material xeraphium of water content lower than 0.5wt%;
Step C, adopt vibrating ball mill to carry out vibration process to ferrite prefiring material xeraphium, vibration, after 20 ~ 40 minutes, obtains the ferrite prefiring material powder after vibration;
Step D, carries out high speed dispersion process to the ferrite prefiring material powder after vibration, obtains the ferrite prefiring material powder after high speed dispersion;
Step e, by the ferrite prefiring material powder after high speed dispersion and tackiness agent Homogeneous phase mixing, and is placed in magnetic field and carries out dry-pressing formed, obtain forming iron oxysome;
Step F, sinters forming iron oxysome, and sintering temperature is 1190 ~ 1290 DEG C, at sintering after 1 ~ 3 hour, namely obtains high performance dry-press process sintered permanent ferrite.
Preferably, described ferrite prefiring material contains the Hxagonal ferrite principal phase of A, R, M, Ti and Fe, and meets following general formula: (1-x) AO (x/2) R
2o
3(n-z-y/2) Fe
2o
3zM
2o
3yTiO
2
In formula, A is at least one in Sr element or Ba element; R is the combination of at least one and La element in Y element or rare earth element, or R is only La element; M is the combination of at least one and Co element in Mn element or Zn element, or M is only Co element; X, y, z is according to amount of substance meter 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 steps A comprises the steps:
Steps A 1, prepares ferrite prefiring material according to the component proportion described in the claims 2;
Steps A 2, carries out coarse crushing process to ferrite prefiring material, until the mean particle size of ferrite prefiring material reaches 3.0 ~ 4.0 microns, obtains ferrite prefiring material after coarse crushing;
Steps A 3, adds the SiO accounting for ferrite prefiring material gross weight 0.2% after coarse crushing after coarse crushing in ferrite prefiring material
2with the CaCO accounting for ferrite prefiring material gross weight 1.2% after coarse crushing
3, and wet crushing is carried out in horizontal ball mill, until the mean particle size of ferrite prefiring material reaches 0.8 ~ 0.9 micron, thus obtain ferrite prefiring material slip.
Preferably, after ferrite prefiring material xeraphium being carried out to the vibration process of 30 minutes, obtain the ferrite prefiring material powder after vibration.
Preferably, in step e, described tackiness 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 dispersion, and the consumption of calcium stearate accounts for the ferrite prefiring material powder gross weight 0.25% after high speed dispersion.
Preferably, in step e, the size of forming magnetic field is 8000Oe, and forming pressure is 7MPa.
Preferably, in the process sintered forming iron oxysome, temperature rise rate is 2 DEG C/min, and sintering temperature is 1230 DEG C, at sintering after 2 hours, namely obtains high performance dry-press process sintered permanent ferrite.
Preferably, in step F, after sintering terminates, naturally cool to room temperature, namely obtain high performance dry-press process sintered permanent ferrite.
A kind of ferrite, adopts the preparation method described in technique scheme to be prepared from.
As seen from the above technical solution provided by the invention, the dry-press process Preburning material that the embodiment of the present invention provides and prepared magnet thereof and magnet manufacture method not use only high performance ferrite prefiring material, and between drying and processing and high speed dispersion process, be provided with the step of " adopting vibrating ball mill to carry out vibration process to ferrite prefiring material xeraphium ", this vibration treating processes can reduce the adhesion of ferrite paricles intergranular, promote dispersiveness and the compressibility of ferrite particle, ferrite particle is significantly strengthened along the degree of alignment of easy magnetization axis, this significantly improves the orientation degree of ferrite particle and shaping ferritic density, therefore, it is possible to make the magnetic property of dry-press process sintered permanent ferrite significantly improve.Compared with the preparation method of dry-press process ferrite sintered body of the prior art, the ferrite preparation method that the embodiment of the present invention provides proposes the technical scheme reducing the adhesion of ferrite paricles intergranular, breach lubricant in prior art and limited bottleneck is promoted to ferrite performance, thus the magnetic property of dry-press process sintered permanent ferrite is compared with prior art largely increased.
Accompanying drawing explanation
In order to be illustrated more clearly in the technical scheme of the embodiment of the present invention, below the accompanying drawing used required in describing embodiment is briefly described, apparently, accompanying drawing in the following describes is only some embodiments of the present invention, for those of ordinary skill in the art, under the prerequisite not paying creative work, other accompanying drawings can also be obtained according to these accompanying drawings.
Fig. 1 improves the principle schematic of magnetic powder particle along easy magnetization axis degree of alignment in existing dry pressuring forming process.
Fig. 2 improves the principle schematic of magnetic powder particle along easy magnetization axis degree of alignment in the embodiment of the present invention.
The process that Fig. 3 provides for the embodiment of the present invention and obtain the XRD figure spectrum of magnet without vibration machining.
Embodiment
Be clearly and completely described the technical scheme in the embodiment of the present invention below in conjunction with accompanying drawing, obviously, described embodiment is only the present invention's part embodiment, instead of whole embodiments.Based on embodiments of the invention, those of ordinary skill in the art, not making the every other embodiment obtained under creative work prerequisite, belong to protection scope of the present invention.
The ferrite preparation method provided the embodiment of the present invention below and prepared ferrite thereof are described in detail.
A kind of ferrite preparation method, it specifically can comprise the following steps:
Steps A, prepares ferrite prefiring material, and carries out wet crushing process to ferrite prefiring material, until the mean particle size of ferrite prefiring material reaches 0.8 ~ 0.9 micron, thus obtains ferrite prefiring material slip.
Wherein, described ferrite prefiring material contains the Hxagonal ferrite principal phase of A, R, M, Ti and Fe, and meets following general formula: (1-x) AO (x/2) R
2o
3(n-z-y/2) Fe
2o
3zM
2o
3yTiO
2; In formula, A is at least one in Sr element or Ba element; R is the combination of at least one and La element in Y element or rare earth element, or R is only La element; M is the combination of at least one and Co element in Mn element or Zn element, or M is only Co element; X, y, z is according to amount of substance meter 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.Prepare burden according to said components, and sinter at 1160 ~ 1260 DEG C, high performance ferrite prefiring material can be obtained.This ferrite prefiring material has high-performance, and the magnetic property of prepared dry-press process sintered permanent ferrite can be made significantly to improve.In actual applications, this steps A specifically comprises the steps:
Steps A 1, prepares ferrite prefiring material according to the component proportion of ferrite prefiring material described in technique scheme.
Steps A 2, carries out coarse crushing process to ferrite prefiring material, until the mean particle size of ferrite prefiring material reaches 3.0 ~ 5.0 microns, obtains ferrite prefiring material after coarse crushing.In actual applications, dry grinder of the prior art can be adopted to carry out coarse crushing process to ferrite prefiring material.
Steps A 3, adds the SiO accounting for ferrite prefiring material gross weight 0.2% after coarse crushing after coarse crushing in ferrite prefiring material
2with the CaCO accounting for ferrite prefiring material gross weight 1.2% after coarse crushing
3, and wet crushing is carried out in horizontal ball mill, until the mean particle size of ferrite prefiring material reaches 0.8 ~ 0.9 micron, thus obtain ferrite prefiring material slip.
Step B, carries out drying and processing to ferrite prefiring material slip, until obtain the ferrite prefiring material xeraphium of water content lower than 0.5wt%.
Wherein, bake out temperature is preferably 140 DEG C, and the constant temperature drying time is preferably 2 hours, until obtain the ferrite prefiring material xeraphium of water content lower than 0.5wt%.
Step C, adopt vibrating ball mill to carry out vibration process to ferrite prefiring material xeraphium, vibration, after 20 ~ 40 minutes, obtains the ferrite prefiring material powder after vibration.
Wherein, vibration process is carried out to ferrite prefiring material xeraphium, preferably vibration 30 minutes, the ferrite prefiring material powder after vibration can be obtained.
Step D, carries out high speed dispersion process to the ferrite prefiring material powder after vibration, obtains the ferrite prefiring material powder after high speed dispersion.
Wherein, high speed dispersion process can adopt the process of prior art high speed dispersion machine, and high speed disintegrator similar with high speed dispersor principle of work in prior art also can be adopted to process.
Step e, by the ferrite prefiring material powder after high speed dispersion and tackiness agent Homogeneous phase mixing, and is placed in magnetic field and carries out dry-pressing formed, obtain forming iron oxysome.
Wherein, described tackiness agent is camphor and calcium stearate mixture, and the consumption of camphor accounts for 1.0% of the ferrite prefiring material powder gross weight after high speed dispersion, and the consumption of calcium stearate accounts for 0.25% of the ferrite prefiring material powder gross weight after high speed dispersion; The size of forming magnetic field is 8000Oe, and forming pressure is 7MPa.
Step F, sinters forming iron oxysome, and sintering temperature is 1190 ~ 1290 DEG C, at sintering after 1 ~ 3 hour, namely obtains high performance dry-press process sintered permanent ferrite.
Wherein, in the process sintered forming iron oxysome, temperature rise rate is preferably 2 DEG C/min, sintering temperature is preferably 1230 DEG C, and preferably terminate sintering after 2 hours at sintering, then naturally cool to room temperature, namely obtain high performance dry-press process sintered permanent ferrite.
Further, this ferrite preparation method improves the magnetic property of dry-press process sintered permanent ferrite mainly through following two aspects: first, this ferrite preparation method have employed high performance ferrite prefiring material, thus the magnetic property of prepared dry-press process sintered permanent ferrite can be made to be largely increased.Second, the step that this ferrite preparation method is provided with between drying and processing and high speed dispersion process " adopting vibrating ball mill to carry out vibration process to ferrite prefiring material xeraphium ", and this vibration treating processes can reduce the adhesion of ferrite paricles intergranular, promote dispersiveness and the compressibility of ferrite particle, ferrite particle is significantly strengthened along the degree of alignment of easy magnetization axis, this significantly improves the orientation degree of ferrite particle and shaping ferritic density, therefore, it is possible to make the magnetic property of dry-press process sintered permanent ferrite significantly improve; Its concrete principle can be as shown in Figure 2, before vibration process process, ferrite particle a and ferrite particle b is sticked together, the easy magnetization axis of ferrite particle a is α, the easy magnetization axis of ferrite particle is β, therefore ferrite particle a and ferrite particle b is very low along the degree of alignment of easy magnetization axis, and in vibration process treating processes, ferrite particle a and ferrite particle b adhesion are shaken out, ferrite particle disperses, and therefore the degree of alignment along easy magnetization axis of ferrite particle is improved.
It should be noted that, compared with the preparation method of dry-press process ferrite sintered body of the prior art, the ferrite preparation method that the embodiment of the present invention provides proposes the technical scheme reducing the adhesion of ferrite paricles intergranular, breach lubricant in prior art and limited bottleneck is promoted to ferrite performance, thus the magnetic property of dry-press process sintered permanent ferrite is compared with prior art largely increased.
A kind of ferrite, adopts the ferrite preparation method described in technique scheme to be prepared from.
In order to the technique effect more clearly showing technical scheme provided by the present invention and produce, with several specific embodiment, ferrite preparation method provided by the present invention and prepared ferrite thereof are described in detail below.
Embodiment one
A kind of ferrite, adopt following ferrite preparation method to be prepared from, its concrete steps comprise:
Steps A 1 ', prepares ferrite prefiring material according to the component proportion of following ferrite prefiring material.
Wherein, ferrite prefiring material contains the Hxagonal ferrite principal phase of A, R, M, Ti and Fe, and meets following general formula: (1-x) AO (x/2) R
2o
3(n-z-y/2) Fe
2o
3zM
2o
3yTiO
2; In formula, A adopts Sr element; R adopts La element; M adopts Co element; X, y, z is according to amount of substance meter respectively, meets following condition: x=0.2, y=0.01, z=0.1, and n=5.87.
Steps A 2 ', adopts dry grinder to carry out coarse crushing process to ferrite prefiring material, until the mean particle size of ferrite prefiring material reaches 3.0 ~ 5.0 microns after pulverizing, namely obtains ferrite prefiring material after coarse crushing.
Steps A 3 ', gets ferrite prefiring material 300g after above-mentioned coarse crushing, and in ferrite prefiring material after this coarse crushing, add the SiO accounting for ferrite prefiring material gross weight 0.2% after coarse crushing
2with the CaCO accounting for ferrite prefiring material gross weight 1.2% after coarse crushing
3, and wet crushing is carried out in horizontal ball mill, after broken 9.5 hours, the mean particle size of ferrite prefiring material reaches 0.85 micron, and specific surface area is 6.06cm
2/ g, thus obtain the ferrite prefiring material slip after wet crushing.
Step B ', carries out drying and processing to ferrite prefiring material slip, and bake out temperature is 140 DEG C, and constant temperature drying, after 2 hours, obtains the ferrite prefiring material xeraphium of water content lower than 0.5wt%.
Step C ', adopt vibrating ball mill to carry out vibration process to ferrite prefiring material xeraphium, vibration, after 30 minutes, obtains the ferrite prefiring material powder after vibration; The mean particle size of the ferrite prefiring material powder after this vibration is 0.82 micron, and specific surface area is 6.68cm
2/ g.
Step D ', adopts high speed dispersor to carry out 1 high speed dispersion process to the ferrite prefiring material powder after vibration, obtains the ferrite prefiring material powder after high speed dispersion.
Step e ', to in the ferrite prefiring material powder after high speed dispersion, add the calcium stearate of the camphor of ferrite prefiring material powder gross weight 1.0% after accounting for high speed dispersion and the ferrite prefiring material powder gross weight 0.25% after accounting for high speed dispersion, and carry out high-speed mixing, mixture is mixed; Being placed in magnetic field again carries out dry-pressing formed, and the size of forming magnetic field is 8000Oe, and forming pressure is 7MPa, thus can obtain forming iron oxysome; This shaping ferritic diameter is 33mm, is highly 12mm.
Step F ', sinter forming iron oxysome, temperature rise rate is 2 DEG C/min, and sintering temperature is 1230 DEG C, has sintered, naturally cool to room temperature at this temperature after 2 hours, namely obtains high performance dry-press process sintered permanent ferrite.
Further, measure the orientation degree of the dry-press process sintered permanent ferrite that embodiment 1 finally obtains, its concrete magnet XRD figure spectrum can be as shown in Figure 3.Simultaneously, mill processing is carried out to the upper and lower surface of the dry-press process sintered permanent ferrite that embodiment 1 finally obtains, and to this ferritic residual magnetic induction intensity (Br), coercive force (Hcb), HCJ (Hcj), maximum magnetic energy product (BH) max, the performance perameters such as magnet density (ρ) are measured, and its specific performance data are as shown in table 1.
Comparative example 1
A kind of ferrite, have employed molecule is SrFe
11.8o
19traditional Strontium ferrite powder, remaining preparation process is all identical with embodiment 1, and also to obtained ferritic residual magnetic induction intensity (Br), coercive force (Hcb), HCJ (Hcj), maximum magnetic energy product (BH) max, magnet, the performance perameters such as magnet density (ρ) are measured, and its specific performance data are also as shown in table 1.
Table 1:
As can be seen from Table 1: compared with the traditional Strontium ferrite powder adopted in comparative example 1, ferrite prefiring material in embodiment 1 can make final obtained ferritic residual magnetic induction intensity and coercive force be largely increased, visible, select the high performance ferrite Preburning material in embodiment 1, the magnetic property of prepared dry-press process sintered permanent ferrite can be made to be largely increased, thus to obtain the inaccessiable dry-pressing performance of traditional Strontium ferrite powder.
Comparative example 2
A kind of ferrite, have employed the ferrite prefiring material identical with embodiment 1, the step of " adopting vibrating ball mill to carry out vibration process to ferrite prefiring material xeraphium " is there is not in its preparation process, all the other steps are substantially the same manner as Example 1, namely the dry powder of ferrite prefiring material carries out vibration process, but directly carries out high speed dispersion process.
Particularly, measure the orientation degree of the dry-press process sintered permanent ferrite that comparative example 2 finally obtains, its concrete magnet XRD figure spectrum can be as shown in Figure 3.Simultaneously, mill processing is carried out to the upper and lower surface of the dry-press process sintered permanent ferrite that comparative example 2 finally obtains, and to this ferritic residual magnetic induction intensity (Br), coercive force (Hcb), HCJ (Hcj), maximum magnetic energy product (BH) max, the performance perameters such as magnet density (ρ) are measured, and its specific performance data are as shown in table 2.
As seen from Figure 3: with in comparative example 2 without compared with the obtained permanent-magnet ferrite of vibration machining, in embodiment 1 through the obtained permanent-magnet ferrite of vibration machining in (004), (006), the crystal face intensity at (0014) place significantly improves, and obviously reduce in the crystal face intensity at (107) place, and background is smooth.According to orientation degree calculation formula: orientation degree=∑ (00l)/∑ (hkl) is known, the orientation degree through vibration processing is higher than the orientation degree of processing without vibration certainly.Visible, really can be opened the adhesion of ferrite paricles intergranular by vibration process, improve the dispersiveness of ferrite particle, ferrite particle be obtained along the degree that easy magnetization axis arranges significantly higher, thus improve orientation degree.
Table 2:
As can be seen from Table 2: the dry-press process sintered permanent ferrite that embodiment 1 finally obtains has higher magnetic property, visible, ferrite particle, through vibration processing treatment, improves orientation degree, the density of magnet also significantly improves, thus obtains more excellent performance.
Embodiment 2
One group of ferrite, all have employed the ferrite prefiring material identical with embodiment 1, its preparation process is substantially the same manner as Example 1, its special feature is: in steps A 3 ', carrying out the wet-curshed broken time in horizontal ball mill is respectively 4.5 hours, 7 hours, 9.5 hours, 12 hours, 16.5 hours, thus broken after the mean particle size of ferrite prefiring material correspond to 1.2 microns, 0.95 micron, 0.82 micron, 0.7 micron, 0.6 micron.
Particularly, mill processing is carried out to the upper and lower surface of the dry-press process sintered permanent ferrite that enforcement 2 finally obtains, and the performance perameters such as this ferritic residual magnetic induction intensity (Br), coercive force (Hcb), HCJ (Hcj), maximum magnetic energy product (BH) max, magnet density (ρ) and formed body yield rate are measured, its specific performance data are as shown in table 3; In table 3, formed body yield rate often presses the salable product number of 20 pieces to calculate.
Table 3:
As can be seen from Table 3, after wet crushing, the mean particle size of ferrite prefiring material is thinner, then obtained ferritic magnetic property is higher, but after the mean particle size of ferrite prefiring material is lower than 0.8 micron, the yield rate of formed body can sharply decline, this is because the mean particle size of ferrite prefiring material is thinner, specific surface area is larger, the specific surface field of ferrite particle is stronger, and the gas of absorption is more, causes formed body intensity low, easy cracking, thus cannot carry out scale production.After the mean particle size of ferrite prefiring material is greater than 0.9 micron, although formed body yield rate is fine, magnetic property declines very fast, cannot meet performance requriements.Comprehensive these two aspects problem, in the embodiment of the present invention, after wet crushing, the mean particle size of ferrite prefiring material is preferably between 0.8 ~ 0.9 micron.
Embodiment 3
One group of ferrite, all have employed the ferrite prefiring material identical with embodiment 1, its preparation process is substantially the same manner as Example 1, and its special feature is: in step C ', and the vibration time of vibration process is respectively 0 minute, 10 minutes, 20 minutes, 30 minutes, 60 minutes, 120 minutes.
Particularly, mill processing is carried out to the upper and lower surface of the dry-press process sintered permanent ferrite that enforcement 3 finally obtains, and the performance perameters such as this ferritic residual magnetic induction intensity (Br), coercive force (Hcb), HCJ (Hcj), maximum magnetic energy product (BH) max, magnet density (ρ) and formed body yield rate are measured, its specific performance data are as shown in table 4; In table 4, formed body yield rate often presses the salable product number of 20 pieces to calculate.
Table 4:
As can be seen from Table 4, along with the increase of vibration time, magnetic property Br presents ascendant trend, magnet density is also along with increase, this is because along with the increase of vibration time, the degree that the adhesion of ferrite paricles intergranular is opened is higher, and the degree that ferrite particle arranges along easy magnetization axis is higher, orientation degree and the formed body density of ferrite particle are higher, and thus magnetic property presents ascendant trend.But vibration is long for process period, cause specific surface area to increase, the specific surface field of ferrite particle strengthens, and the gas of absorption is more, and cause formed body intensity to decrease, yield rate declines to some extent.Comprehensive these two aspects problem, in the embodiment of the present invention, the vibration time is preferably 30 minutes.
As fully visible, the embodiment of the present invention can not only improve shaping ferritic density, and the adhesion of ferrite paricles intergranular can be reduced, promote the dispersiveness of ferrite paricles intergranular, thus improve the degree of alignment of ferrite particle along easy magnetization axis, the orientation degree of ferrite particle is significantly improved, therefore, it is possible to make the magnetic property of dry-press process sintered permanent ferrite significantly improve.
The above; be only the present invention's preferably embodiment, but protection scope of the present invention is not limited thereto, is anyly familiar with those skilled in the art in the technical scope that the present invention discloses; the change that can expect easily or replacement, all should be encompassed within protection scope of the present invention.Therefore, protection scope of the present invention should be as the criterion with the protection domain of claims.
Claims (9)
1. a ferrite preparation method, is characterized in that, comprises the following steps:
Steps A, prepares ferrite prefiring material, and carries out wet crushing process to ferrite prefiring material, until the mean particle size of ferrite prefiring material reaches 0.8 ~ 0.9 micron, thus obtains ferrite prefiring material slip;
Step B, carries out drying and processing to ferrite prefiring material slip, until obtain the ferrite prefiring material xeraphium of water content lower than 0.5wt%;
Step C, adopt vibrating ball mill to carry out vibration process to ferrite prefiring material xeraphium, vibration, after 20 ~ 40 minutes, obtains the ferrite prefiring material powder after vibration;
Step D, carries out high speed dispersion process to the ferrite prefiring material powder after vibration, obtains the ferrite prefiring material powder after high speed dispersion;
Step e, by the ferrite prefiring material powder after high speed dispersion and tackiness agent Homogeneous phase mixing, and is placed in magnetic field and carries out dry-pressing formed, obtain forming iron oxysome;
Step F, sinters forming iron oxysome, and sintering temperature is 1190 ~ 1290 DEG C, at sintering after 1 ~ 3 hour, namely obtains high performance dry-press process sintered permanent ferrite.
2. preparation method according to claim 1, is characterized in that, described ferrite prefiring material contains the Hxagonal ferrite principal phase of A, R, M, Ti and Fe, and meets following general formula:
(1－x)AO(x/2)R
2O
3(n-z-y/2)Fe
2O
3zM
2O
3yTiO
2
In formula, A is at least one in Sr element or Ba element; R is the combination of at least one and La element in Y element or rare earth element, or R is only La element; M is the combination of at least one and Co element in Mn element or Zn element, or M is only Co element; X, y, z is according to amount of substance meter 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.
3. preparation method according to claim 2, is characterized in that, described steps A comprises the steps:
Steps A 1, prepares ferrite prefiring material according to the component proportion described in the claims 2;
Steps A 2, carries out coarse crushing process to ferrite prefiring material, until the mean particle size of ferrite prefiring material reaches 3.0 ~ 4.0 microns, obtains ferrite prefiring material after coarse crushing;
Steps A 3, adds the SiO accounting for ferrite prefiring material gross weight 0.2% after coarse crushing after coarse crushing in ferrite prefiring material
2with the CaCO accounting for ferrite prefiring material gross weight 1.2% after coarse crushing
3, and wet crushing is carried out in horizontal ball mill, until the mean particle size of ferrite prefiring material reaches 0.8 ~ 0.9 micron, thus obtain ferrite prefiring material slip.
4. preparation method according to any one of claim 1 to 3, is characterized in that, after ferrite prefiring material xeraphium being carried out to the vibration process of 30 minutes, obtains the ferrite prefiring material powder after vibration.
5. preparation method according to any one of claim 1 to 3, it is characterized in that, in step e, described tackiness agent is camphor and calcium stearate mixture, the consumption of camphor accounts for the ferrite prefiring material powder gross weight 1.0% after high speed dispersion, and the consumption of calcium stearate accounts for the ferrite prefiring material powder gross weight 0.25% after high speed dispersion.
6. preparation method according to any one of claim 1 to 3, is characterized in that, in step e, the size of forming magnetic field is 8000 Oe, and forming pressure is 7MPa.
7. preparation method according to any one of claim 1 to 3, is characterized in that, in the process sintered forming iron oxysome, temperature rise rate is 2 DEG C/min, sintering temperature is 1230 DEG C, at sintering after 2 hours, namely obtains high performance dry-press process sintered permanent ferrite.
8. preparation method according to any one of claim 1 to 3, is characterized in that, in step F, after sintering terminates, naturally cools to room temperature, namely obtains high performance dry-press process sintered permanent ferrite.
9. a ferrite, is characterized in that, adopts the preparation method according to any one of the claims 1 to 8 to be prepared from.
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| CN104876563A (en) * | 2015-04-23 | 2015-09-02 | 程凯芬 | Ferrite magnetic-isolating material |
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| CN112530654A (en) * | 2020-12-04 | 2021-03-19 | 安徽中马磁能科技股份有限公司 | Sintered permanent magnetic ferrite and molding method thereof |
| CN112908676A (en) * | 2021-02-05 | 2021-06-04 | 浙江安特磁材股份有限公司 | Permanent magnetic ferrite magnetic powder for dry pressing molding and preparation method thereof |
| CN113213907A (en) * | 2021-06-24 | 2021-08-06 | 横店集团东磁股份有限公司 | Composite ferrite material and preparation method and application thereof |
| CN114643120A (en) * | 2022-02-23 | 2022-06-21 | 北矿磁材（阜阳）有限公司 | Method for manufacturing dry-pressed anisotropic sintered magnetic powder |
| CN115448715A (en) * | 2022-07-25 | 2022-12-09 | 矿冶科技集团有限公司 | Method for manufacturing dry-pressed sintered ferrite permanent magnet material |
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| CN115448715A (en) * | 2022-07-25 | 2022-12-09 | 矿冶科技集团有限公司 | Method for manufacturing dry-pressed sintered ferrite permanent magnet material |
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Address after: 100160 Beijing Fengtai District South Fourth Ring West Road 188 18 District 23 Building 4 Floor Patentee after: North Polytron Technologies Inc Address before: 102600 No. 22, East Beixing Road, Daxing District, Beijing Patentee before: Beikuan Magnetic-material Science & Technology Co., Ltd. |