CN103117146A - High-Curie-temperature low-loss high-strength ferrite magnetic block and preparation method thereof - Google Patents
High-Curie-temperature low-loss high-strength ferrite magnetic block and preparation method thereof Download PDFInfo
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Abstract
The invention discloses a high-Curie-temperature low-loss high-strength ferrite magnetic block and a preparation method thereof and belongs to the technical field of Mn-Zn serial ferrite. Main raw materials include ferric oxide, manganese oxide and zinc oxide, auxiliary raw materials include calcium carbonate, titanium oxide, cobalt oxide, silicon oxide, chromium oxide, niobium oxide, nickle oxide and copper oxide, the ferrite magnetic block is composed of the main raw materials, 55-61mol% of ferric oxide calculated according to Fe2O3, 33-40mol% of manganese oxide calculated according to MnO and 5-10% of zinc oxide calculated according to ZnO, and the adding amount of the auxiliary raw materials relative to the total weight of the main raw materials is 500-3000ppm of CaCO3, 80-3000ppm of TiO2, 50-1200ppm of Co2O3, 20-200ppm of superfine SiO2, 100-1500ppm of Cr2O3, 100-1500ppm of Nb2O5, 600-2000ppm of NiO and 600-2000ppm of CuO. The high-Curie-temperature low-loss high-strength ferrite magnetic block has the advantages that initial magnetic permeability can be lowered to be maintained at 1400+/-25%, power consumption is lower than 550kw/m3 under the condition of 100KHz200mT and at the temperature of 100 DEG C, saturation magnetic flux density at 100 DEG C is larger than 410mT, the Curie temperature is larger than 275 DEG C, and strength of the magnetic block can meet the strength detection standard (F)40N).
Description
Technical field
The invention belongs to Mn-Zn based ferrite technical field, be specifically related to a kind of high-curie temperature low loss and high strength ferrite magnetic patch, and relate to its preparation method.
Background technology
Along with automotive lighting, automobile mounted DC-DC transducer, the fast development of the inverter of LCD and light-emitting diode display, convertible frequency air-conditioner, solar inverter etc., thereby the application surface of power ferrite is significantly expanded, simultaneously the power ferrite in these fields of being applied to be not limited to exemplify proposed more harsh requirement, be embodied in: requiring at high temperature, (80-160 ℃) has higher power conversion efficiency; Requirement possesses high Curie temperature and uses the variations in temperature that conforms; Requirement has the little characteristics of power loss ratio under hot environment, etc.
In recent years, the low energy consumption solar inverter of being released by America and Europe all state has been widely used in high-rating generator and even miniature solar mobile phone charging device, thereby more strict to the ferritic requirement that is applied to this inverter, particularly: Curie temperature needs greater than 275 ℃ lower than the manganese-zinc ferrite of routine to require magnetic permeability, and the power loss when requiring to satisfy 100KHz 200mT and 100 ℃ is less than 550kw/m
3Standard; In the car-mounted device of severe jolt environment or the open-air atmosphere of Climate Anomalies, so such ferrite magnetic patch need possess good intensity due to such ferrite application.In addition, because the ferritic geometry that is applied to inverter generally is solid cuboid or round (the industry custom claims that the ferrite of round is the magnetic cake), the ferrite of this shape exists shaping efficiency low, yielding and cause the low shortcoming of rate of finished products in sintering process for magnet with respect to the transformer of traditional C font, E font or U font, not only affect industrial amplification production, and preparation cost is high, the shortcoming that energy resource consumption is large (because of rate of finished products low due to).
can be no lack of the technical information that is seen in ferrite and preparation method thereof in disclosed Chinese patent literature, " broad temperature, broadband, high curie point and low loss MnZn ferrite material and preparation method thereof " of typically recommending as Granted publication CN101620908B, pointed out respectively CN10118358A(high saturation magnetic flux density low loss NiMnZn power ferrite material in specification the 0013rd to 0016 hurdle of this patent), CN1749209A(high saturation magnetic flux density low loss MnZn ferrite material and preparation method thereof), the preparation method of CN101004961A(high frequency high power ferrite material) and CN101004962A(high frequency low-loss manganese zine ferrite material preparation method) shortcoming that exists, and cashed objectively the technique effect that its specification the 0021st hurdle refers.But by to the deciphering of the specification of this patent as can be known, its for be that closed magnetic core namely belongs to the closed magnetic core category, thereby do not have referential meaning for Application and preparation in the open circuit magnetic core of aforementioned car-mounted device.
In addition, the technology contents of the raising ferrite Curie temperature that relates in disclosed China and foreign countries' patent and non-patent literature up to now generally concentrates on the component of high magnetic permeability material and explores, namely by regulating raw material ratio and alloy, initial permeability (μ i) is reached 5000-12000, to improve Curie temperature, lose biased but keep expanding under the low-loss condition Curie temperature for the power-type Ferrite Material.
Summary of the invention
Top priority of the present invention is to provide a kind of and helps significantly to reduce initial permeability, be conducive to significantly to reduce power loss, be of value to and obtain rational saturation flux density and the high-curie temperature low loss and high strength ferrite magnetic patch of being convenient to improve Curie temperature and intensity is arranged.
Another task of the present invention is to provide a kind of preparation method of high-curie temperature low loss and high strength ferrite magnetic patch, and the ferrite magnetic patch that is prepared by the method can embody described technique effect comprehensively.
Top priority of the present invention is completed like this, a kind of high-curie temperature low loss and high strength ferrite magnetic patch, comprise primary raw material and auxiliary material, described primary raw material comprises iron oxide, manganese oxide and zinc oxide, described auxiliary material comprises calcium carbonate, titanium oxide, cobalt oxide, silica, chromium oxide, niobium oxide, nickel oxide and cupric oxide, and the component of described primary raw material is: 55-61mol% presses Fe
2O
3The manganese oxide of pressing MnO calculating of the iron oxide that calculates, 33-40mol% and the zinc oxide of pressing ZnO calculating of 5-10mol%; With respect to the total weight of described primary raw material, the addition of described auxiliary material is: CaCO
3: 500-3000ppm, TiO
2: 80-3000ppm, Co
2O
3: 50-1200ppm, ultra-fine SiO
2: 20-200ppm, Cr
2O
3: 100-1500ppm, Nb
2O
5: 100-1500ppm, NiO:600-2000ppm and CuO:600-2000 ppm.
In a specific embodiment of the present invention, the component of described primary raw material is: 55.4mol% presses Fe
2O
3The manganese oxide of pressing MnO calculating of the iron oxide that calculates, 38.25mol% and the zinc oxide of pressing ZnO calculating of 6.35mol%; With respect to the total weight of described primary raw material, the addition of described auxiliary material is: CaCO
3: 500ppm, TiO
2: 300ppm, Co
2O
3: 200ppm, ultra-fine SiO
2: 100ppm, Cr
2O
3: 100ppm, Nb
2O
5: 600ppm, NiO:800ppm and CuO:600 ppm.
In another specific embodiment of the present invention, the component of described primary raw material is: 58.35mol% presses Fe
2O
3The manganese oxide of pressing MnO calculating of the iron oxide that calculates, 34.85mol% and the zinc oxide of pressing ZnO calculating of 6.8mol%; With respect to the total weight of described primary raw material, the addition of described auxiliary material is: CaCO
3: 3000ppm, TiO
2: 80ppm, Co
2O
3: 1200ppm, ultra-fine SiO
2: 200ppm, Cr
2O
3: 800ppm, Nb
2O
5: 100ppm, NiO:2000ppm and CuO:1300 ppm.
In another specific embodiment of the present invention, the component of described primary raw material is: 57mol% presses Fe
2O
3The manganese oxide of pressing MnO calculating of the iron oxide that calculates, 33mol% and the zinc oxide of pressing ZnO calculating of 10mol%; With respect to the total weight of described primary raw material, the addition of described auxiliary material is: CaCO
3: 1700ppm, TiO
2: 3000ppm, Co
2O
3: 50ppm, ultra-fine SiO
2: 25ppm, Cr
2O
3: 1500ppm, Nb
2O
5: 1500ppm, NiO:600ppm and CuO:2000 ppm.
Another task of the present invention is completed like this, and a kind of preparation method of high-curie temperature low loss and high strength ferrite magnetic patch comprises the following steps:
A) batching drops into primary raw material in mixer after by component iron oxide 55-61mol%, manganese oxide 30-40mol% and zinc oxide 5-10mol% weighing and is dry mixed, and controls the rotating speed that is dry mixed time and mixer, obtains the primary raw material compound;
B) pre-burning and pulverizing, will be by steps A) the primary raw material compound that obtains introduces the pre-burning of electrothermal rotary kiln, and control calcined temperature and time, introduce vibration pulverizing in vibrator after kiln discharge, and the average particulate diameter of the material after vibration frequency, Oscillation Amplitude and the control of controlling vibration grinding time, vibrator are pulverized obtains crushed material;
C) sand milling, will be by step B) crushed material that obtains and the auxiliary material that will take by weight with respect to the total weight of primary raw material be calcium carbonate 500-3000ppm, titanium oxide 80-3000ppm, cobalt oxide 50-1200ppm, superfine silicon dioxide 20-200ppm, chromium oxide 100-1500ppm, niobium oxide 100-1500ppm, nickel oxide 600-2000ppm and cupric oxide 600-2000ppm drop into and add the water sand milling that circulates in sand mill, control the weight ratio of water and material, control the sand milling time, the average particulate diameter of the material after controlling the rotating speed of sand mill and controlling sand milling, obtain slip,
D) preparation granulation slurry, will be by step C) slip that obtains introduces with in the slurry-mixing tank of blender and add polyvinyl alcohol water solution to stir, control mixing time, the rotating speed of controlling blender, control polyvinyl alcohol water solution join the amount in slip and control the mass percent concentration of polyvinyl alcohol, obtain granulation slurry;
E) mist projection granulating and base will be by step D) in the granulation slurry that obtains carry out mist projection granulating, obtain particulate material, particulate material is pressed into magnetic patch, obtain the magnetic patch base substrate, and control the density of magnetic patch base substrate;
F) sintering; will be by step e) pack into material alms bowl or load bearing board and introduce the kiln sintering of the magnetic patch base substrate that obtains; in sintering process; heating rate from room temperature to 750 ℃ is 60 ℃/h; be 170 ℃/h from the heating rates of 750 ℃ to 1100 ℃; then the heating rate with 140 ℃/h is warming up to 1300-1380 ℃; and be incubated in the time of 1300-1380 ℃; oxygen content when controlling temperature retention time and controlling insulation; insulation is cooling in protective atmosphere after finishing; kiln discharge obtains high-curie temperature low loss and high strength ferrite magnetic patch.
In another specific embodiment of the present invention, steps A) it is that the time of being dry mixed is controlled to be 15-30min that the control described in is dry mixed the time, and the rotating speed of described control mixer is that rotating speed is controlled to be 35-40n/min.。
Also have a specific embodiment of the present invention, step B) described in control calcined temperature and time be that calcined temperature is controlled to be 850-910 ℃, the pre-burning time is controlled to be 50-70min; Described control vibration grinding time is that the vibration grinding time is controlled to be 20-30min, the vibration frequency of described control vibrator is that vibration frequency is controlled to be 20-50 time/min, described control Oscillation Amplitude is that Oscillation Amplitude is controlled to be 3-5 ㎜,, the average particulate diameter of the material after described control is pulverized is that average particulate diameter is controlled to be 0.85-1.25 μ m.
The weight ratio of the control water more of the present invention and in specific embodiment, step C) and material is that the weight ratio with water and material is controlled to be 1.8-2: 1; The described control sand milling time is that the time is controlled to be 60-80min; The rotating speed of described control sand mill is that rotating speed is controlled to be 40-50n/min; The average particulate diameter of the material after described control sand milling is that average particulate diameter is controlled to be 0.75-1.15 μ m.
In of the present invention and then specific embodiment, step D) the control mixing time described in and the rotating speed of blender are that mixing time is controlled to be 120-180min, and the rotating speed of blender is controlled to be 8-12n/min; It is the amount in slip of joining to be controlled to be the 6-9% of slip weight that described control polyvinyl alcohol water solution joins amount in slip; The mass percent concentration of described control polyvinyl alcohol water solution is that mass percent concentration is controlled to be 10-14%.
The density of the control magnetic patch base substrate of the present invention again more and in specific embodiment, step e) is that density is controlled to be 2.8-3.2 g/cm
3Step F) the control temperature retention time described in is that temperature retention time is controlled to be 4-6h, and protective atmosphere is nitrogen protection atmosphere, and described control oxygen content is that oxygen content is controlled to be 4.5-5.5%
Technical scheme provided by the invention is because the composition of primary raw material and auxiliary material is selected and reasonable mixture ratio, so initial permeability can be down to and remain on 1400 ± 25%, and the power consumption when 100KHz 200mT and temperature are 100 ℃ is less than 550kw/m
3, 100 ℃ of saturation flux densities are greater than 410mT, and Curie temperature is greater than 275 ℃, and magnetic patch intensity can satisfy intensity detection standard (F〉40N).
Embodiment
Embodiment 1:
A) batching, primary raw material is dropped in mixer after weighing respectively by component iron oxide 55.4mol%, manganese oxide 38.25mol% and zinc oxide 6.35mol% mix, the rotating speed of mixer is 40n/min, incorporation time is 15min, obtain the primary raw material compound, the iron oxide described in this step is for pressing Fe
2O
3The iron oxide that calculates, and the preferred Fe that uses by the purity of Chinese Shanghai Baoshan Iron and Steel Group Co production and sales 〉=99.3%
2O
3, described manganese oxide is for pressing Mn
3O
4The manganese oxide that calculates, and preferably use the trade mark of Hunan China Hunan of provinceing Jin Rui Science and Technology Ltd. sale to be the Mn of CR-06
3O
4, its purity Mn% 〉=71%, the zinc oxide that described zinc oxide calculates for pressing ZnO, and the preferred ZnO that uses by the chemical plant production and sales of Chinese Shanghai capital, its weight percent content ZnO% 〉=99.7%;
B) pre-burning and pulverizing, will be by steps A) the primary raw material compound that obtains introduces in the electrothermal rotary kiln and at 910 ℃ of lower pre-burning 50min, introduce vibration pulverizing in vibrator after kiln discharge, the vibration frequency of vibrator is 50 times/min, Oscillation Amplitude is 3 ㎜, the vibration grinding time is 25min, and the material after vibration is pulverized is that the average particulate diameter of crushed material is 0.85-1 μ m, obtains crushed material;
C) sand milling will be by step B) crushed material that obtains and the auxiliary material that will take by weight with respect to the total weight of primary raw material be calcium carbonate (CaCO
3) 500ppm, titanium oxide (TiO
2) 300ppm, cobalt oxide (Co
2O
3) 200ppm, superfine silicon dioxide (SiO
2) 100ppm, chromium oxide (Cr
2O
3) 100ppm, niobium oxide (Nb
2O
5) 600ppm, nickel oxide (NiO) 800ppm and cupric oxide (CuO) 600ppm drop into and add water and the appropriate dispersant sand milling that circulates in sand mill, the time of sand milling is 60min, the rotating speed of sand mill is 50n/min, described water is that the weight ratio of pure water and water and material is controlled to be 2: 1, the average particulate diameter of the material after sand milling (also can be described as average diameter of particles) is 0.75-0.85 μ m, obtains slip;
D) preparation granulation slurry, will be by step C) slip that obtains introduces with in the slurry-mixing tank of blender and to add 6% and mass percent concentration of slip weight be that 14% polyvinyl alcohol (PVA) aqueous solution stirs, mixing time is 180min, the rotating speed of blender is 8n/min, obtains granulation slurry;
E) mist projection granulating and base will be by step D) in the granulation slurry that obtains carry out mist projection granulating, obtaining water content is that 0.35-0.55wt%, apparent density are 1.36-1.66 g/cm
3And angle of repose is the particulate material of≤30 °, particulate material is introduced the magnetic patch blank forming machine that mould is housed be pressed into magnetic patch, and obtaining density is 2.8g/cm
3The magnetic patch base substrate;
F) sintering, will be by step e) pack into material alms bowl or be stacked and placed on load bearing board (the present embodiment is selected the latter) and introduce the kiln sintering in stacked mode of the magnetic patch base substrate that obtains, in sintering process, warm area from room temperature to 750 ℃ is the furnace heating-up section or claims heating zone, in this heating rate intensification of section with 60 ℃/h that heat up, be the binder removal section or claim the binder removal district from the warm areas of 750 ℃ to 1100 ℃, heat up at the heating rate of this binder removal section with 170 ℃/h, be the sintering zone from the warm areas of 1100 ℃ to 1380 ℃, rise to 1380 ℃ and this 1380 ℃ under be incubated 4h with the heating rate of 140 ℃/h from 1100 ℃ in this sintering zone, kiln oxygen content (also can claim oxygen content) when insulation is controlled to be 4.5%, insulation cooling in nitrogen protection atmosphere after finishing (the industry custom claims under balanced atmosphere cooling), kiln discharge, obtain high-curie temperature low loss and high strength ferrite magnetic patch.
Because magnetic patch is not closed magnetic core, thereby can't carry out separately electric performance test, so the present embodiment is that the magnet ring of corresponding acquisition is tested, its performance index are by shown in following subordinate list.
Embodiment 2:
Only with steps A) in primary raw material component change as follows: iron oxide 58.35mol%, manganese oxide 34.85mol% and zinc oxide 6.8mol% change respectively rotating speed and the incorporation time of mixer into 35n/min and 30min; Only with step B) in calcined temperature change 850 ℃ into, the pre-burning time changes 70min into, changes the vibration frequency of vibrator into 20 times/min, Oscillation Amplitude changes 5 ㎜ into, the average particulate diameter of crushed material changes 0.95-1.05 μ m into; Only with step C) in auxiliary material change into respect to the total weight of primary raw material: calcium carbonate (CaCO
3) 3000ppm, titanium oxide (TiO
2) 80ppm, cobalt oxide (Co
2O
3) 1200ppm, superfine silicon dioxide (SiO
2) 200ppm, chromium oxide (Cr
2O
3) 800ppm, niobium oxide (Nb
2O
5) 100ppm, nickel oxide (NiO) 2000ppm and cupric oxide (CuO) 1300ppm, change the weight ratio of water and material into 1.9: 1, change the sand milling time into 80min, changing the rotating speed of sand mill into 40n/min, is that average diameter of particles changes 1-1.15 μ m into the average particulate diameter of the material after sand milling; With step D) in the addition of polyvinyl alcohol (PVA) aqueous solution change 9% of slip weight into, and change the mass percent concentration of polyvinyl alcohol water solution into 10%, change mixing time into 120min, change the rotating speed of blender into 12n/min; With step e) in the density of magnetic patch base substrate change 3.2g/cm into
3With step F) in holding temperature change 1300 ℃ into, the temperature retention time under 1300 ℃ changes 6h into, changes the kiln oxygen content in when insulation into 5%.All the other are all with the description to embodiment 1.
Embodiment 3:
Only with steps A) in the primary raw material component more intend as follows: iron oxide 57mol%, manganese oxide 33mol% and zinc oxide 10mol% change respectively rotating speed and the incorporation time of mixer into 37n/min and 20min; Only with step B) in calcined temperature change 880 ℃ into, the pre-burning time changes 60min into, changes the vibration frequency of vibrator into 35 times/min, Oscillation Amplitude changes 4 ㎜ into, the average particulate diameter of crushed material changes 1-1.2 μ m into; Only with step C) in the total weight of the corresponding primary raw material of auxiliary material change into: calcium carbonate (CaCO
3) 1700ppm, titanium oxide (TiO
2) 3000ppm, cobalt oxide (Co
2O
3) 50ppm, superfine silicon dioxide (SiO
2) 25ppm, chromium oxide (Cr
2O
3) 1500ppm, niobium oxide (Nb
2O
5) 1500ppm, nickel oxide (NiO) 600ppm and cupric oxide (CuO) 2000ppm, change the weight ratio of water and material into 1.8: 1, change the sand milling time into 70min, changing the rotating speed of sand mill into 45n/min, is that average diameter of particles changes into less than 1.15 μ m with the average particulate diameter of the material after sand milling; With step D) in the addition of polyvinyl alcohol (PVA) aqueous solution change 8% of slip weight into, and change the mass percent concentration of polyvinyl alcohol water solution into 12%, change mixing time into 150min, change the rotating speed of blender into 10n/min; With step e) in the density of magnetic patch base substrate change 3g/cm into
3With step F) in holding temperature change 1340 ℃ into, the temperature retention time under 1340 ℃ changes 5h into, changes the kiln oxygen content in when insulation into 5.5%.All the other are all with the description to embodiment 1.
Technique effect shown in subordinate list below the high-curie temperature low loss and high strength ferrite magnetic patch that is obtained by above-described embodiment 1 to 3 has after tested with the form of magnet ring.
By above-mentioned subordinate list as seen, high-curie temperature low loss and high strength ferrite magnetic patch of the present invention has lower initial permeability (1400 ± 25%), and 100 ℃ of power consumptions less than 550kw/m
3, 100 ℃ of saturation flux densities are greater than 410mT, and Curie temperature is greater than 275 ℃.
Above-mentioned test instrument used is the instruments such as the U.S.'s 2330 power consumption testers, HP4284 inductance instrument, HP42841A direct current magnetic power source, SJK-5KV electric vertical magnetic core intensity of pressure test machine, insulating box and resistivity tester.
In addition, adopt mechanical strength test pushing force machine to test its mechanical strength and can satisfy F the 40N standard, meet the vehicle electronics product requirement fully.
In sum, the present invention is by rational main raw materials in proportion, increases the iron oxide ratio reducing initial permeability, and optimizes as the auxiliary material, particularly inventive application NiO and CuO of the doping system part as system's doping, by increasing CaCO
3Doping improves the product mechanical strength, reduces simultaneously the particulate material activity, indirectly improves product strength after sintering.In addition, average grain diameter to the material after sand milling is controlled, and improves the particulate material apparent density, forms evenly, high conformity and without the microstructure of abnormal crystal grain, be aided with simultaneously preferred sintering process atmosphere, temperature curve sintering, form that the porosity is low, high density, without the ferrite of out-phase.
Claims (10)
1. high-curie temperature low loss and high strength ferrite magnetic patch, it is characterized in that comprising primary raw material and auxiliary material, described primary raw material comprises iron oxide, manganese oxide and zinc oxide, described auxiliary material comprises calcium carbonate, titanium oxide, cobalt oxide, silica, chromium oxide, niobium oxide, nickel oxide and cupric oxide, and the component of described primary raw material is: 55-61mol% presses Fe
2O
3The manganese oxide of pressing MnO calculating of the iron oxide that calculates, 33-40mol% and the zinc oxide of pressing ZnO calculating of 5-10mol%; With respect to the total weight of described primary raw material, the addition of described auxiliary material is: CaCO
3: 500-3000ppm, TiO
2: 80-3000ppm, Co
2O
3: 50-1200ppm, ultra-fine SiO
2: 20-200ppm, Cr
2O
3: 100-1500ppm, Nb
2O
5: 100-1500ppm, NiO:600-2000ppm and CuO:600-2000 ppm.
2. high-curie temperature low loss and high strength ferrite magnetic patch according to claim 1 is characterized in that the component of described primary raw material is: 55.4mol% presses Fe
2O
3The manganese oxide of pressing MnO calculating of the iron oxide that calculates, 38.25mol% and the zinc oxide of pressing ZnO calculating of 6.35mol%; With respect to the total weight of described primary raw material, the addition of described auxiliary material is: CaCO
3: 500ppm, TiO
2: 300ppm, Co
2O
3: 200ppm, ultra-fine SiO
2: 100ppm, Cr
2O
3: 100ppm, Nb
2O
5: 600ppm, NiO:800ppm and CuO:600 ppm.
3. high-curie temperature low loss and high strength ferrite magnetic patch according to claim 1 is characterized in that the component of described primary raw material is: 58.35mol% presses Fe
2O
3The manganese oxide of pressing MnO calculating of the iron oxide that calculates, 34.85mol% and the zinc oxide of pressing ZnO calculating of 6.8mol%; With respect to the total weight of described primary raw material, the addition of described auxiliary material is: CaCO
3: 3000ppm, TiO
2: 80ppm, Co
2O
3: 1200ppm, ultra-fine SiO
2: 200ppm, Cr
2O
3: 800ppm, Nb
2O
5: 100ppm, NiO:2000ppm and CuO:1300 ppm.
4. high-curie temperature low loss and high strength ferrite magnetic patch according to claim 1 is characterized in that the component of described primary raw material is: 57mol% presses Fe
2O
3The manganese oxide of pressing MnO calculating of the iron oxide that calculates, 33mol% and the zinc oxide of pressing ZnO calculating of 10mol%; With respect to the total weight of described primary raw material, the addition of described auxiliary material is: CaCO
3: 1700ppm, TiO
2: 3000ppm, Co
2O
3: 50ppm, ultra-fine SiO
2: 25ppm, Cr
2O
3: 1500ppm, Nb
2O
5: 1500ppm, NiO:600ppm and CuO:2000 ppm.
5. the preparation method of a high-curie temperature low loss and high strength ferrite magnetic patch as claimed in claim 1 is characterized in that comprising the following steps:
A) batching drops into primary raw material in mixer after by component iron oxide 55-61mol%, manganese oxide 30-40mol% and zinc oxide 5-10mol% weighing and is dry mixed, and controls the rotating speed that is dry mixed time and mixer, obtains the primary raw material compound;
B) pre-burning and pulverizing, will be by steps A) the primary raw material compound that obtains introduces the pre-burning of electrothermal rotary kiln, and control calcined temperature and time, introduce vibration pulverizing in vibrator after kiln discharge, and the average particulate diameter of the material after vibration frequency, Oscillation Amplitude and the control of controlling vibration grinding time, vibrator are pulverized obtains crushed material;
C) sand milling, will be by step B) crushed material that obtains and the auxiliary material that will take by weight with respect to the total weight of primary raw material be calcium carbonate 500-3000ppm, titanium oxide 80-3000ppm, cobalt oxide 50-1200ppm, superfine silicon dioxide 20-200ppm, chromium oxide 100-1500ppm, niobium oxide 100-1500ppm, nickel oxide 600-2000ppm and cupric oxide 600-2000ppm drop into and add the water sand milling that circulates in sand mill, control the weight ratio of water and material, control the sand milling time, the average particulate diameter of the material after controlling the rotating speed of sand mill and controlling sand milling, obtain slip,
D) preparation granulation slurry, will be by step C) slip that obtains introduces with in the slurry-mixing tank of blender and add polyvinyl alcohol water solution to stir, control mixing time, the rotating speed of controlling blender, control polyvinyl alcohol water solution join the amount in slip and control the mass percent concentration of polyvinyl alcohol, obtain granulation slurry;
E) mist projection granulating and base will be by step D) in the granulation slurry that obtains carry out mist projection granulating, obtain particulate material, particulate material is pressed into magnetic patch, obtain the magnetic patch base substrate, and control the density of magnetic patch base substrate;
F) sintering; will be by step e) pack into material alms bowl or load bearing board and introduce the kiln sintering of the magnetic patch base substrate that obtains; in sintering process; heating rate from room temperature to 750 ℃ is 60 ℃/h; be 170 ℃/h from the heating rates of 750 ℃ to 1100 ℃; then the heating rate with 140 ℃/h is warming up to 1300-1380 ℃; and be incubated in the time of 1300-1380 ℃; oxygen content when controlling temperature retention time and controlling insulation; insulation is cooling in protective atmosphere after finishing; kiln discharge obtains high-curie temperature low loss and high strength ferrite magnetic patch.
6. the preparation method of high-curie temperature low loss and high strength ferrite magnetic patch according to claim 5, it is characterized in that steps A) described in control to be dry mixed the time be that the time of being dry mixed is controlled to be 15-30min, the rotating speed of described control mixer is that rotating speed is controlled to be 35-40n/min.。
7. the preparation method of high-curie temperature low loss and high strength ferrite magnetic patch according to claim 5, it is characterized in that step B) described in control calcined temperature and time be that calcined temperature is controlled to be 850-910 ℃, the pre-burning time is controlled to be 50-70min; Described control vibration grinding time is that the vibration grinding time is controlled to be 20-30min, the vibration frequency of described control vibrator is that vibration frequency is controlled to be 20-50 time/min, described control Oscillation Amplitude is that Oscillation Amplitude is controlled to be 3-5 ㎜,, the average particulate diameter of the material after described control is pulverized is that average particulate diameter is controlled to be 0.85-1.25 μ m.
8. the preparation method of high-curie temperature low loss and high strength ferrite magnetic patch according to claim 5, is characterized in that step C) described in control water and the weight ratio of material be that weight ratio with water and material is controlled to be 1.8-2: 1; The described control sand milling time is that the time is controlled to be 60-80min; The rotating speed of described control sand mill is that rotating speed is controlled to be 40-50n/min; The average particulate diameter of the material after described control sand milling is that average particulate diameter is controlled to be 0.75-1.15 μ m.
9. the preparation method of high-curie temperature low loss and high strength ferrite magnetic patch according to claim 5, it is characterized in that step D) described in the control mixing time and the rotating speed of blender be that mixing time is controlled to be 120-180min, the rotating speed of blender is controlled to be 8-12n/min; It is the amount in slip of joining to be controlled to be the 6-9% of slip weight that described control polyvinyl alcohol water solution joins amount in slip; The mass percent concentration of described control polyvinyl alcohol water solution is that mass percent concentration is controlled to be 10-14%.
10. the preparation method of high-curie temperature low loss and high strength ferrite magnetic patch according to claim 5, is characterized in that step e) described in the density of control magnetic patch base substrate be that density is controlled to be 2.8-3.2 g/cm
3Step F) the control temperature retention time described in is that temperature retention time is controlled to be 4-6h, and protective atmosphere is nitrogen protection atmosphere, and described control oxygen content is that oxygen content is controlled to be 4.5-5.5%.
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