CN1697094A - Ferrite magnet material of manganese-zinc, and Method for preparing high conductive ferrite of manganese-zinc from material - Google Patents
Ferrite magnet material of manganese-zinc, and Method for preparing high conductive ferrite of manganese-zinc from material Download PDFInfo
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- CN1697094A CN1697094A CN 200510040358 CN200510040358A CN1697094A CN 1697094 A CN1697094 A CN 1697094A CN 200510040358 CN200510040358 CN 200510040358 CN 200510040358 A CN200510040358 A CN 200510040358A CN 1697094 A CN1697094 A CN 1697094A
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Abstract
Mixed main material including 51.5-52.8 mol% ferric oxide, 23.3-26.0 mol% manganese oxide, and 22.5-24.0 mol% zinc oxide is processed through shake grinding and pre-burning procedures. Next, auxiliary materials including 500-1000ppm calcium oxide, 300-1500ppm titanium oxide and 100-400ppm bismuth oxide are added to the said processed main material. Then, procedures including sand mill, granulation, body blank and burning are carried out in sequence to produce products. Advantages are: reasonable compounding ratio between main and auxiliary materials provides precondition for producing the disclosed product in high magnetic permeability and low coefficient of specific loss; optimized curve of agglomeration technology prevents oxidation of products, and improves temperature and even atmosphere in kiln. The product shows preferred initial permeability, coefficient of specific loss and coefficient of specific temperature.
Description
Technical field
The present invention relates to a kind of manganese-zinc ferrite magnet material and lead the method for manganese-zinc ferrite with this material preparation height, the magnet material that more particularly relates to the soft magnetism manganese-zinc ferrite is selected and is had the soft magnetism manganese-zinc ferrite product of high magnetic permeability with selected material preparation, belongs to magnetic material and processing technique field.
Background technology
Along with the fast development of information industry (IT), traditional common soft magnetic ferrite can not satisfy the requirement of emerging IT, thereby makes that the manganese-zinc ferrite of high magnetic permeability is paid attention to by industrial circle day by day, and becomes the important component part of IT technology.Because a large amount of all kinds of power transformers that use are operated under the low magnetic flux density mostly in communication field, therefore, if can reasonably select Ferrite Material, just can obtain the ferrite of excellent magnetic permeability, to reduce the coil turn of power transformer, the D.C. resistance that reduces coil by this reaches by its loss that causes; And volume that can littleization transformer makes transformer satisfy light, thin, little and so on requirement.
Owing to require usually for being operated in communication transformer in the broad frequency range that output signal harmonic distortion is little, transmission speed is fast, therefore also require ferrite to have low loss coefficient again; In low-frequency range, require to have good anti-electromagnetic interference performance, so also require ferrite to have excellent anti-electromagnetic interference performance.
Unite in " the hi-tech industrialization key project that country first develops " of issue April 30 in 2004 in National Development and Reform Committee, the Department of Science and Technology, Department of Commerce, the high performance soft magnetic ferrite of low-loss, low harmonics distortion, broad temperature, broadband characteristics is listed in wherein, adapted to the development of communication, electronic applications with this.
For ferrite, China has tame manufacturing enterprise more than 160 approximately so far, but most to produce low and middle-grade ferrite products, for ferritic preparation, adopts vacuum furnace and N mostly
2The protection tunnel cave.Gradually eliminated because vacuum furnace production automation degree is lower, output is not high, quality is unstable.And N
2Though the protection tunnel cave has the advantage that production cost is low, output is high, cooling rate is difficult to control, temperature, blanket of nitrogen lack of homogeneity, therefore, and the initial permeability (μ of prepared soft magnetism manganese-zinc ferrite
i) only in the 5000-8000 level.For μ
i＞10000 ferrite, at present the domestic producer that has only number in the wrong to refer to utilizes top-hat kiln to attempt, but because of this kiln price height, yield poorly, cause the price height of product, thereby can't promote.
The applicant has noticed Chinese patent CNl503280A disclosed high frequency fine grain soft magnetic ferrite and production technology thereof, this patent application the effect that will get the phase be to expect a kind of ferrite with high magnetic permeability, high resistivity, low loss characteristic, but do not show the μ that it will obtain
iCan reach the quantizating index of which kind of degree actually, select and the production technology of being instructed and describe the ferritic μ of gained in conjunction with the 5th page of contained technical indicator contrast of its specification from its disclosed material
iCan be greater than 10000.Because the ferrite that this patent will obtain is a power ferrite, so its magnetic permeability is not high (generally at 2000-3000).
The applicant has been also noted that the disclosed manganese-zinc ferrite of Chinese patent CN1192002C, to μ
iThis key technical indexes is gained ground, but its material is 0-30 ℃ of scope, temperature coefficient (α μ) shows as big negative value, magnetic permeability descends with temperature, at 30 ℃-T bigger α μ ℃ is arranged, because, because inductance value has by a relatively large margin variation with temperature, thereby reduced the stability of ferrite work, and then had influence on the quality of complete machine.And, do not disclose specific loss coefficient (tg δ/μ
i) index, make the use value of product can not get embodying, because select for use ferrite to exert an influence to the user of complete machine production.
In order to obtain the manganese-zinc ferrite product of high magnetic permeability, past people is poured into to the Fe as main material the attentiveness of the selection of material often morely
2O
3, MnO, ZnO component rationally/best proportioning on because these main materials have active good, purity is high and particle mean size in the advantage of μ m level, yet to attaching undue importance to one thing to the neglect of the other to some extent as the attention rate of the auxiliary material of additive in the aforementioned main material.In fact, if kind and addition assurance to auxiliary material are improper, then can to such as grain growth speed, burn till (knot) temperature, resistivity, eddy current loss, magnetocrystalline anisotropy constant, magnetic hysteresis loss, magnetic permeability temperature characterisitic and magnetic permeability frequency characteristic and all can bring different effects, can be related to finally that can obtain high performance be high magnetic permeability (μ
i＞10000) and specific loss coefficient (tg δ/μ
i) little ferrite; In addition, for the preparation method of manganese-zinc ferrite, sintering circuit is crucial link, in view of aforesaid N
2The protection tunnel cave has the advantage that the sintering cost is low, output is high, therefore, though at present domesticly mostly adopt it, also has insoluble logical fraud simultaneously, and this logical fraud mainly shows as: the one, and the sintering process curve in the sintering process is difficult to hold; The 2nd, at N
2The temperature descending section of the kiln body of tunnel cave is difficult to control temperature and atmosphere (N in the thorax
2And air) uniformity, thus the goods oxidation can't be prevented.Known to the industry, at 1350～1380 ℃ of these temperature sections of reducing to 1000 ℃, ferrite is oxidation very easily, at present with 1350～1380 ℃ of times of reducing to 1000 ℃ generally at 1～2h, ferritic oxidative phenomena is more serious.Therefore, even it is perfect to ultimate attainment degree to constitute the selection and the proportioning of main and auxiliary raw material of ferrimagnet material, then still be difficult to obtain the gratifying high magnetic permeability of qualification rate, ferrite product that the specific loss coefficient is little.
Summary of the invention
Task of the present invention is to provide a kind of and helps to accelerate grain growth speed, reduce sintering temperature, improve resistivity, reduce eddy current loss and magnetocrystalline anisotropy constant and magnetic hysteresis loss, be beneficial to that to improve magnetic permeability temperature characterisitic and magnetic permeability frequency characteristic, improve using of high frequency performance be to obtain high magnetic permeability and the little manganese-zinc ferrite magnet material of specific loss coefficient.
It is a kind of by ensureing that the height that obtain high magnetic permeability, coefficient of specific loss lead the preparation method of manganese-zinc ferrite with the uniformity of the temperature of improving kiln body temperature descending section and atmosphere in case the generation of oxidation phenomenon is used to the reasonable assurance of sintering process curve and by rational cooling measure that task of the present invention also is to provide.
Manganese provided by the present invention, Mn-Zn ferrite magnet material, the primary raw material that contains comprises iron oxide, manganese oxide and zinc oxide, being used for of containing adds the auxiliary material that main material goes to and comprises calcium oxide, titanium oxide, bismuth oxide, and the component of primary raw material is: contain 51.5～52.8mol% by Fe
2O
3The manganese oxide of pressing MnO calculating of the iron oxide that calculates, 23.3～26.0mol%, the zinc oxide of pressing ZnO calculating of 22.5～24.0mol%; The component of auxiliary material is: the TiO that presses that presses calcium oxide that CaO calculates and 300～1500ppm of 500～1000ppm
2The titanium oxide that calculates and 100～400ppm press Bi
2O
3The bismuth oxide that calculates.
Manganese-zinc ferrite magnet material of the present invention, the component of described primary raw material is: contain 52.2～52.8mol% by Fe
2O
3The manganese oxide of pressing MnO calculating of the iron oxide that calculates, 24.0～25.0mol%, the zinc oxide of pressing ZnO calculating of 22.8～23.2mol%; The component of described auxiliary material is: the TiO that presses that presses calcium oxide that CaO calculates and 600ppm of 500ppm
2Titanium oxide that calculates and 300ppm press Bi
2O
3The bismuth oxide that calculates.
The above-mentioned manganese-zinc ferrite magnet material of usefulness provided by the present invention prepares the high method of leading manganese-zinc ferrite: earlier mixing mutually by the main material after component oxysome iron 51.5～52.8mol%, manganese oxide 23.2～26.0mol%, the zinc oxide 22.5～24.0mol% weighing, after vibration, deliver to pre-burning, pre-burning finishes the back adding and carries out sand milling by the auxiliary material after component calcium oxide 500～1000ppm, titanium oxide 300～1500ppm, the bismuth oxide 100～400ppm weighing, granulation and make blank behind sand milling is sent blank into N
2The protection tunnel cave burns till; wherein: the programming rate during in room temperature～600 ℃ is 60 ℃/h; programming rate more than 600 ℃ the time is 200 ℃/h; be incubated during to 1350 ℃～1400 ℃; after insulation finishes; the kiln bore temperature that makes kiln body temperature descending section in any one mode in water-cooled or circulation air blast cooling fast cooling to 1000 ℃ in 35～45 minutes is cooled to room temperature then naturally, and kiln discharge is led the manganese-zinc ferrite finished product after mill processing obtains height.
The present invention prepares the method that height is led manganese-zinc ferrite, described main material after the weighing is mixed mutually, and its incorporation time is 55～65 minutes, and hybrid mode is that dry type is mixed.
The present invention prepares the method that height is led manganese-zinc ferrite, and described vibration is vibratory milling, and the time is 0.5～0.7h.
The present invention prepares the method that height is led manganese-zinc ferrite, and described pre-burning is electric rotary kiln pre-burning, and calcined temperature is 930～980 ℃, and the pre-burning time is 110～130 minutes.
The present invention prepares the method that height is led manganese-zinc ferrite, and the time of described sand milling is 110～130 minutes, and material: the sand milling ball: the ratio of water is 1: 1: 0.6, average particle size behind the sand milling＜1 μ m.
The present invention prepares the method that height is led manganese-zinc ferrite, and described granulation is a mist projection granulating, adds 10% polyvinyl alcohol (PVA) aqueous solution before the spraying.
The present invention prepares the method that height is led manganese-zinc ferrite, and 1380～1400 ℃ of the holding temperatures of described insulation, temperature retention time are 3.8～4.2h.
The present invention prepares the method that height is led manganese-zinc ferrite, and described fast cooling is at pure N
2Middle fast cooling, the temperature fall time of fast cooling is 40 minutes.
Manganese-zinc ferrite material provided by the present invention and lead the method for manganese-zinc ferrite and the distinctive points of prior art is: 1, main and auxiliary reasonable raw material proportioning with this material preparation height, especially the selection of auxiliary material helps to accelerate grain growth speed, reduces sintering temperature, improves resistivity, reduces eddy current loss and magnetocrystalline anisotropy constant and magnetic hysteresis loss, improve magnetic permeability temperature, frequency characteristic, improve high frequency performance, for the manganese-zinc ferrite product that obtains high magnetic permeability and coefficient of specific loss provides precondition; 2. to firing process: optimized good sintering process curve, avoid goods oxidation to occur with fast cooling and improve ferritic performance at kiln body temperature descending section, fast cooling can improve temperature, atmosphere evenness in the kiln body, improves the consistency of ferrite product; 3. the height of gained is led the initial permeability μ of manganese-zinc ferrite product
i(f:10KHZ) more than 12000, specific loss coefficient tg δ/μ
i＜3.4 * 10
-6, than temperature coefficient-40～120 ℃ of scopes be on the occasion of, α μ is 0-2 in 20～70 ℃ of scopes, has improved magnetic permeability-temperature characterisitic.
Description of drawings
Figure 1 shows that the present invention is used for adding to auxiliary material that main material goes to improving the curve synoptic diagram of magnetic permeability-temperature characterisitic.
Figure 2 shows that the present invention is used for adding to auxiliary material that main material goes to improving the curve synoptic diagram of magnetic permeability-frequency characteristic.
Figure 3 shows that temperature curve, oxygen content curve synoptic diagram in the sintering circuit of the present invention.
Figure 4 shows that N
2The kiln body temperature descending section of protection tunnel cave imposes water-cooled schematic perspective view.
Figure 5 shows that N
2The kiln body temperature descending section air blast cooling schematic cross-section but that circulates of protection tunnel cave.
Fig. 6 is a process chart of the present invention.
Embodiment
Embodiment 1:
Be the component that optimizes that main material thousand formulas that drop into that iron oxide 52.2mol%, manganese oxide 25mol%, zinc oxide 22.8mol% are converted into after the percentage by weight weighing are mixed the mixing of machine through 1h by force earlier, send into vibrator vibration 0.6h after the mixing and obtain fine powder material, the fine powder material that vibration is thin is delivered to electric rotary kiln pre-burning, calcined temperature is that 950 ℃, time are 2h, and it is CaO 0.05WT%, TiO that the cooling back adds the component that optimizes
20.06wt%, Bi
2O
3Auxiliary material after the 0.03wt% weighing, send into sand mill sand milling 2h, in sand grinding process, the control material: ball: the ratio of water is 1: 1: 0.6, and the granularity of the material behind the sand milling then adopts spray drying device that the slip of sand milling gained is made particle below 1 μ m, it is mist projection granulating, add 10% the PVA aqueous solution of feeding before the spraying, the requirement of particle is: water content 0.15-0.25%, particle size distribution 100-200 μ m account for 75%, flow angle 26-35 °, loose specific weight 1.35～1.45g/cm
3, adopt the full automatic press that is equipped with sintered-carbide die to be pressed into required blank then, the briquetting pressure of press is 1.2-1.5T/cm
2, blank density 2.9-3.2g/cm
3, dimensional tolerance ± 0.1mm, then blank is sent into N again
2The protection tunnel cave burns till, and the temperature section from room temperature～600 ℃ heats up with the programming rate of 60 ℃/h, from 600 ℃ temperature section, heats up with the programming rate of 200 ℃/h, and insulation 4h when reaching 1380 ℃ is after the insulation end, at pure N
2Accelerating the cooling of kiln body with the circulation air blast cooling in the atmosphere, specifically is to adopt by shown in Figure 5 being located at from N
2The blower fan with pressurization 5 that source 4 leads on the pipeline 6 of kiln thorax 3 improves the N that enters into kiln thorax 3
2Pressure, be implemented in the temperature that makes in 40 minutes in the kiln thorax 3 and reduce to 1000 ℃ fast from 1380 ℃, and can make temperature, atmosphere (N in the kiln thorax 3
2And air) is evenly distributed.Venthole 7 among Fig. 5 is in order to draw the pore of gas; If with water cooling mode, be laid in position, kiln body temperature descending section 1 both sides and cold water be generally normal temperature corresponding to conveying in the water pipe 2 of kiln thorax 3 by shown in Figure 4 so, the temperature of kiln thorax 3 that makes insulation of furnace wall section 1 (length of this soaking zone generally accounts for about 2 meters in whole tunnel cave) was reduced to 1000 ℃ fast from 1380 ℃ in 40 minutes, this cooling method can guarantee that temperature, the atmosphere in the kiln thorax 3 is even.As soon as after the temperature of kiln thorax 3 reduces to 1000 ℃, then return to the state that naturally cools to room temperature, that is to say after 1000 ℃, need not artificially cool off kiln thorax 3 with blower fan 5 or cooling water again.Wait to burn till part and in balanced atmosphere, be cooled to kiln discharge after the room temperature,, obtain initial permeability μ through mill processing or according to after need making mirror finish
i＞12300, specific loss coefficient tg δ/μ
i=3.0 * 10
-6(f:10kHZ), saturation flux density BS＞400mT, Curie temperature Tc (℃)＞120 ℃ height leads the manganese-zinc ferrite finished product.
The sintering process curve of present embodiment is by shown in Figure 3, and among the figure, solid line is a temperature curve, and dotted line is the oxygen content curve, and P represents oxygen content in 600～1380 ℃ of kilns of temperature-rise period, and t represents temperature-fall period 1380-1000 ℃ temperature fall time; Can promote rapid grain growth as the calcium oxide (CaO) that adds the auxiliary material that goes in the main material in the present embodiment, help reducing firing temperature, during high temperature, its compound is separated out in the grain boundary mutually with other, resistivity be can improve, eddy current loss, titanium oxide (TiO reduced
2) adding help improving material resistivity, make magnetocrystalline anisotropy constant K1-0 (reduce to zero), reduce magnetic hysteresis loss, improve magnetic permeability-temperature characterisitic and magnetic permeability-frequency characteristic, bismuth oxide (Bi
2O
3) adding can promote grain growth, help the high frequency performance that improves magnetic permeability value, reduce the wastage, improve material.Effect as these auxiliary materials can be disclosed by Fig. 1, Fig. 2.Chain-dotted line among Fig. 1 represents to add the magnetic permeability-temperature characteristics behind the auxiliary material, and solid line represents not add the magnetic permeability-temperature characteristics of auxiliary material; Chain-dotted line among Fig. 2 represents to add the magnetic permeability-frequency characteristics behind the auxiliary material, and solid line represents not add the magnetic permeability-frequency characteristics of auxiliary material.
Embodiment 2:
Only iron oxide, manganese oxide, the zinc oxide of main material component are changed into Fe respectively
2O
352.2mol%, MnO24.6mol%, ZnO23.2mol%, the initial permeability μ of resulting finished iron oxygen iron
i=13400, specific loss coefficient tg δ/μ
i=3 * 10
-6(f:10kHZ), all the other are all with embodiment 1.
Embodiment 3:
Only iron oxide, manganese oxide, the zinc oxide of main material component are changed into Fe respectively
2O
352.8mol%, MnO24.0mol%, ZnO23.2mol%, the initial permeability μ of resulting finished iron oxygen iron
i=12800, specific loss coefficient tg δ/μ
i=2.8 * 10
-6(f:10kHZ), all the other are all with embodiment 1.
The desirable physical property that the iron oxygen iron product that the foregoing description is obtained is shown after tested is by shown in the following table:
Claims (10)
1, a kind of manganese, Mn-Zn ferrite magnet material, it is characterized in that the primary raw material that contains comprises iron oxide, manganese oxide and zinc oxide, being used for of containing adds the auxiliary material that main material goes to and comprises calcium oxide, titanium oxide, bismuth oxide, and the component of primary raw material is: contain 51.5～52.8mol% by Fe
2O
3The manganese oxide of pressing MnO calculating of the iron oxide that calculates, 23.3～26.0mol%, the zinc oxide of pressing ZnO calculating of 22.5～24.0mol%; The component of auxiliary material is: the TiO that presses that presses calcium oxide that CaO calculates and 300～1500ppm of 500～1000ppm
2The titanium oxide that calculates and 100～400ppm press Bi
2O
3The bismuth oxide that calculates.
2, manganese-zinc ferrite magnet material according to claim 1 is characterized in that the component of described primary raw material is: contain 52.2～52.8mol% by Fe
2O
3The manganese oxide of pressing MnO calculating of the iron oxide that calculates, 24.0～25.0mol%, the zinc oxide of pressing ZnO calculating of 22.8～23.2mol%; The component of described auxiliary material is: the TiO that presses that presses calcium oxide that CaO calculates and 600ppm of 500ppm
2Titanium oxide that calculates and 300ppm press Bi
2O
3The bismuth oxide that calculates.
3, a kind of manganese-zinc ferrite magnet material as claimed in claim 1 prepares the high method of manganese-zinc ferrite of leading, it is characterized in that earlier mixing mutually by the main material after component oxysome iron 51.5～52.8mol%, manganese oxide 23.2～26.0mol%, the zinc oxide 22.5～24.0mol% weighing, after vibration, deliver to pre-burning, pre-burning finishes the back adding and carries out sand milling by the auxiliary material after component calcium oxide 500～1000ppm, titanium oxide 300～1500ppm, the bismuth oxide 100～400ppm weighing, granulation and make blank behind sand milling is sent blank into N
2The protection tunnel cave burns till; wherein: the programming rate during in room temperature～600 ℃ is 60 ℃/h; programming rate more than 600 ℃ the time is 200 ℃/h; be incubated during to 1350 ℃～1400 ℃; after insulation finishes; the kiln bore temperature that makes kiln body temperature descending section in any one mode in water-cooled or circulation air blast cooling fast cooling to 1000 ℃ in 35～45 minutes is cooled to room temperature then naturally, and kiln discharge is led the manganese-zinc ferrite finished product after mill processing obtains height.
4, highly lead the method for manganese-zinc ferrite described the preparation according to claim described 3, it is characterized in that described main material after the weighing being mixed mutually, its incorporation time is 55～65 minutes, and hybrid mode is to mix in formula.
5, lead the method for manganese-zinc ferrite according to the claim described 3 described height that prepare, it is characterized in that described vibration is vibratory milling, the time is 0.5～0.7h.
6, lead the method for manganese-zinc ferrite according to the claim described 3 described height that prepare, it is characterized in that described pre-burning is electric rotary kiln pre-burning, calcined temperature is 930～980 ℃, and the pre-burning time is 110～130 minutes.
7, lead the method for manganese-zinc ferrite according to the claim described 3 described height that prepare, the time that it is characterized in that described sand milling is 110～130 minutes, and material: the sand milling ball: the ratio of water is 1: 1: 0.6, average particle size behind the sand milling＜1 μ m.
8, highly lead the method for manganese-zinc ferrite described the preparation according to claim described 3, it is characterized in that described granulation is a mist projection granulating, add 10% polyvinyl alcohol (PVA) aqueous solution of feeding before the spraying.
9, highly lead the method for manganese-zinc ferrite described the preparation according to claim described 3, it is characterized in that 1380～1400 ℃ of the holding temperatures of described insulation, temperature retention time is 3.8～4.2h.
10, lead the method for manganese-zinc ferrite according to the claim described 3 described height that prepare, it is characterized in that described fast cooling is at pure N
2Middle fast cooling, the time of fast cooling is 40 minutes.
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