CN1182549C - Magnanese-zinc ferrite magnetic core - Google Patents
Magnanese-zinc ferrite magnetic core Download PDFInfo
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- CN1182549C CN1182549C CNB021382808A CN02138280A CN1182549C CN 1182549 C CN1182549 C CN 1182549C CN B021382808 A CNB021382808 A CN B021382808A CN 02138280 A CN02138280 A CN 02138280A CN 1182549 C CN1182549 C CN 1182549C
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Abstract
The present invention relates to a manganese-zinc ferrite magnetic core which belongs to the technical field of oxide magnetic materials. The magnetic core has the main components of 52 to 55 mol % of iron oxide (Fe2 O3, 7 to 12 mol % of zinc oxide (ZnO) and 36 to 38 mol % of manganese oxide (MnO); nanometer material additive components of 0.01 to 0.5 wt% of calcium oxide (CaO) and 0.004 to 0.03 wt% of silicon dioxide (SiO2) are added. Sintered at the temperature between 1150 to 1300 DEG C for 0.5 to 5 hours, the excellent manganese-zinc ferrite magnetic core which has the initial magnetic permeability of 2600 and the resistivity of 15 to 20 omega m in the frequency range of 1.2 MHz and has the advantages of high frequency, higher saturation flux density Bms and low magnetic loss Pcv can be made.
Description
Technical field:
The present invention relates to a kind of manufacture method of manganese-zinc ferrite magnetic core, belong to the oxidate magnetic material technical field.
Background technology:
Along with developing rapidly of the communications field, manganese-zinc ferrite must have special electromagnetism, machinery and thermal property as the transducer in the high frequency technique, transformer and choke Material Used.The FERRITE CORE that is used for Switch Power Transformer, high frequency, the highly effective transformer of frequency below 3 mhz frequencies particularly, requirement has low core loss Pcv and high saturation magnetic flux density Bms more, with microminiaturization and the high efficiency requirement of satisfying present electric equipment.
Before the present invention made, in prior art, application number 00126316.1 proposed a kind of Fe
2O
3, MnO and ZnO basic composition in contain SiO
2, CaO and NiO ferrite, this ferrite also contains Nb
2O
5, ZrO
2, among P and the B one or both or multiple, with above-mentioned material moulded blank sintering 5 hours in the atmosphere of 1300 ℃ and control partial pressure of oxygen, to improve core loss Pcv and saturation flux density Bms.But because NiO content is up to 0.45 weight %, magnetic anisotropy is bigger, and resistivity generally has only between the 6-10 Ω m.For high frequencyization, the high efficiency that realizes transformer, also require further to improve resistivity, and the additive composition that it contained, owing to be the micron order material, so can not fundamentally reach to the optimization on the magnetic material microstructure.
Summary of the invention:
Purpose of the present invention is overcoming above-mentioned weak point, thereby a kind of have high frequency, high saturation magnetic flux density Bms and low magnetic loss Pcv are provided, the manufacture method of the manganese-zinc ferrite magnetic core that requires with the microminiaturization of satisfying present electric equipment and high efficiency.
Main solution of the present invention is achieved in that
Main Ingredients and Appearance of the present invention contains iron oxide: 52-55 mole %, zinc oxide: 7-12 mole %, manganese oxide 36-38 mole %, and adding dispersant, deionized water, adhesive, defoamer, to be mixed and made into particle mean size be the 80-100 micron, carries out pre-burning, dry type or case of wet attrition again and make the powder that particle mean size is the 1.5-2.0 micron; In above-mentioned powder, add the nanometer materials additive, adding dispersant, deionized water, adhesive, defoamer again carries out mixed powder to be broken into particle mean size is the 0.6-1.2 micron, make the particle of 80-200 micron by spray drier, carry out humidification then, to moisture content be the particle of 0.5-1.0 weight %, carry out being after sintering 0.5-5 hour in the atmosphere of moulding, sintering, introducing nitrogen or vacuum control oxygen concentration finished product at last.
Nanometer additive of the present invention mainly comprises silica, calcium oxide or niobium oxide, tantalum oxide, vanadium oxide and zirconic one or more or tin oxide or titanium oxide or phosphorus P or boron.
The dispersant that the present invention adopts is poly-propionic acid, adds fashionablely, with respect to Main Ingredients and Appearance is: 0.4-0.6 weight %.
The adhesive that the present invention adopts is a polyvinyl alcohol, adds fashionablely, with respect to Main Ingredients and Appearance is: 0.1-1.2 weight %.
The defoamer that the present invention adopts is a n-octyl alcohol, adds fashionablely, with respect to Main Ingredients and Appearance is: 0.1-0.3 weight %.
The deionized water that adopts among the present invention adds fashionablely, with respect to Main Ingredients and Appearance is: 40-150 weight %.
The nanometer materials additive particle size range that the present invention adopts is between 10-500nm.
The present invention can obtain by any one formation of following 1-6.
1. manganese-zinc ferrite magnetic core wherein contains iron oxide, zinc oxide and the manganese oxide of Main Ingredients and Appearance.Press Fe
2O
3, ZnO, MnO be respectively: Fe
2O
3: 52-55 mole %, ZnO:7-12 mole %,, MnO:36-38 mole %.
Contain as nanometer materials additive composition by SiO
2Be calculated as the silica of 0.004-0.03 weight % for benchmark; By CaO is the calcium oxide that benchmark is calculated as 0.01-0.5 weight %.
2. the manganese-zinc ferrite magnetic core in above-mentioned 1, wherein with respect to above-mentioned Main Ingredients and Appearance, as nanometer materials additive composition, further contain niobium oxide, tantalum oxide, vanadium oxide and zirconic a kind of or more than one, press Nb
2O
5: 0.004-0.06 weight %, Ta
2O
5: 0.006-0.10 weight %, V
2O
5: 0.006-0.12 weight %, ZrO
2: 0.004-0.04 weight %.
3. above-mentioned 1 or 2 manganese-zinc ferrite magnetic core wherein with respect to above-mentioned Main Ingredients and Appearance, as nanometer materials additive composition, further contains tin oxide or titanium oxide, presses SnO
2: 0.04-0.4 weight % or TiO
2: 0.04-0.4 weight %.
4. any one manganese-zinc ferrite magnetic core of above-mentioned 1-3, wherein with respect to above-mentioned Main Ingredients and Appearance, as nanometer materials additive composition, further contain nanometer materials as the additive composition: the content by phosphorus P or boron is below the 0.01 weight %.
5. any one manganese-zinc ferrite magnetic core of above-mentioned 1-4 burns till magnetic core into definite shape having the sintering atmosphere of introducing nitrogen or vacuum control oxygen concentration, and becomes described magnetic core between 1150-1300 ℃ in sintering 0.5-5 hour.
6. any one manganese-zinc ferrite magnetic core of above-mentioned 1-5, described magnetic core is 2600 have initial permeability to the frequency range of 1.2 megahertzes, resistivity reaches 15-20 Ω m.
The present invention also has following feature:
Manganese-zinc ferrite magnetic core of the present invention contains by Fe
2O
3For the iron oxide of 52-55 mole %, by ZnO is the zinc oxide of 7-12 mole %, is that the manganese oxide of 36-38 mole % is as Main Ingredients and Appearance by MnO.With respect to above-mentioned Main Ingredients and Appearance, contain nanometer materials additive composition, press SiO
2Silica for 0.004-0.03 weight %; By CaO is the calcium oxide of 0.01-0.5 weight %.Nanometer materials additive particle size range is between 10-500mm.And in its manufacture process, with respect to above-mentioned Main Ingredients and Appearance and nanometer materials additive composition, need add 1. dispersant, as poly-propionic acid is 0.4-0.6 weight %, 2. adhesive is 0.1-1.2 weight %, 3. defoamer as polyvinyl alcohol, as n-octyl alcohol is 0.1-0.3 weight %, and 4. deionized water is 40-150 weight %.
Main Ingredients and Appearance is preferably pressed Fe respectively
2O
3Be the iron oxide of 52-55 mole %, preferably 53-54 mole % is the zinc oxide of 7-12 mole % by ZnO, and preferably 8-11 mole % is the manganese oxide of 36-38 mole % by MnO, preferably 36-37 mole %.
According to manganese-zinc ferrite magnetic core of the present invention, the common nanometer materials additive composition that contains is pressed SiO
2Be the silica of 0.004-0.03 weight %, preferably 0.006-0.02 weight %; By CaO is the calcium oxide of 0.01-0.5 weight %, preferably 0.04-0.08 weight %.SiO
2Be present on the crystal boundary with CaO.
According to manganese-zinc ferrite magnetic core of the present invention also can contain usually nanometer materials additive composition niobium oxide, tantalum oxide, vanadium oxide, zirconic one or more.With respect to above-mentioned Main Ingredients and Appearance, press Nb respectively
2O
5, Ta
2O
5, V
2O
5, ZrO
2For: Nb
2O
5: 0.004-0.06 weight %, preferred 0.01-0.04 weight %; Ta
2O
5: 0.006-0.10 weight %, preferred 0.02-0.05 weight %; V
2O
5: 0.006-0.12 weight %, preferred 0.02-0.05 weight %; ZrO
2: 0.004-0.04 weight %, preferred 0.01-0.03 weight %.
By these nanometer materials additive elements, can increase substantially high frequency particularly and count the above magnetic permeability of 1MHz.In these elements, preferred especially niobium oxide, two kinds of zirconias or above and usefulness, and ratio is arbitrarily.
In addition, in manganese-zinc ferrite magnetic core of the present invention, as the additive composition preferably nano material press SnO
2Be the tin oxide of 0.04-0.4 weight %, preferred 0.1-0.3 weight % or TiO
2Be the titanium oxide of 0.04-0.4 weight %, preferred 0.1-0.3 weight %.
In manganese-zinc ferrite magnetic core of the present invention, as the preferred nano material of additive composition, be below the 0.01 weight % by the content of phosphorus P or boron, preferred 0.001-0.005 weight %.
Thus, can present following actual effect.
Can be 2600 have initial permeability to the frequency range of 1.2 megahertzes, resistivity reaches 15-20 Ω m, and provides loss the very little and MnZn of high saturation magnetic flux density Bms (Mn-Zn) ferrite more at the high frequency transformer of approximate 100 ℃ of uses with magnetic core.
Make the ferrite in manganese zinc series of this invention, at first, adopt the mixture of iron oxide composition, manganese oxide composition and zinc oxide composition usually as Main Ingredients and Appearance.As required,, can add calcium carbonate etc. and become the compound or the calcium oxide of calcium oxide, and become the compound of silica or silica etc. by sintering by sintering as nanometer materials additive composition raw material.But these nanometer materials additive compositions can add by the final above-mentioned amount ratio of forming of magnetic material.
Compared with the prior art the present invention has the following advantages:
The formula materials convenient sources of the present invention's combination; Manufacture craft is simple; Can make a kind of is 2600 have initial permeability to the frequency range of 1.2 megahertzes, and resistivity reaches 15-20 Ω m, has high frequency, the excellent manganese-zinc ferrite magnetic core of high saturation magnetic flux density Bms and low magnetic loss Pcv.
Description of drawings:
Accompanying drawing 1 is manufacture craft of the present invention (process chart).
The used stove of sintering of the present invention can be the tunnel type continuous oven, also can be a batch stove.Atmosphere during sintering can be adjusted according to the theory of balance oxygen partial pressure, but carries out sintering in the nitrogen particularly preferably in the control oxygen partial pressure.
Embodiment:
Following the present invention will be described in further detail in conjunction with specific embodiments.
Embodiment 1
With Fe
2O
3(53.5 moles of %), ZnO (9.5 moles of %) and MnO (37 moles of %) prepare burden as main component, add dispersant simultaneously: poly-propionic acid 0.5 weight %, defoamer: n-octyl alcohol 0.2 weight %, deionized water 95 weight %, after their mixing, add adhesive: polyvinyl alcohol 0.8 weight % solution, in super mixer, mixed 70-80 minute, be made for average grain diameter by spray drier and be about 100 microns, moisture content is below 0.1 weight %, and flow angle is less than the particle of 40 degree; Be placed on rotary kiln and carry out pre-burning, 925 ℃ of calcined temperatures, pre-burning 1.5-2.0 hour; Carried out dry type or case of wet attrition 25-35 minute, and made the powder that average grain diameter is the 1.5-2.0 micron; Add the nanometer materials additive: calcium oxide (CaO): 0.06 weight %, silicon dioxide (SiO
2): 0.015 weight %.Above-mentioned CaO and SiO
2Final composition for magnetic material.Nanometer materials additive particle size range is between 10-500mm.When adding nanometer materials additive composition, add deionized water 50 weight %, dispersant again: poly-propionic acid 0.5 weight %, defoamer: n-octyl alcohol 0.2 weight %, adhesive: polyvinyl alcohol 0.8 weight % solution, be placed in the sand mill mix, fine grinding 50-70 minute, wearing into particle mean size is the 0.8-1.0 micron; Solid content is more than 60%, and viscosity is the slurry of 250-350CPS; Adopt spray drier to make the particle of about 80-200 micron, and flow angle is less than the particle of 30 degree; Mix, humidification, to moisture content be 0.5-0.8 weight %; The employing automatic moulding machine forms, and is pressed into 100 in sample.These molding blanks were placed in the atmosphere of 1240 ℃ of temperature and control partial pressure of oxygen sintering 3 hours, and cooled off in the atmosphere of control oxygen partial pressure then, obtain 25 millimeters of external diameters, 15 millimeters of internal diameters highly are 5 millimeters toroidal core.
Describe above-mentioned said temperature curve below in detail.
The temperature curve of embodiment
Heating process
Real temperature is to 400 ℃ programming rate: 60 ℃/hour
Programming rate from 400 ℃ to 900 ℃: 300 ℃/hour
Programming rate from 900 ℃ to 1240 ℃: 150 ℃/hour
The insulation operation
Kept 3 hours at 1240 ℃
Cooling process
Cooling rate from 1240 ℃ to 1100 ℃: 100 ℃/hour
1100 ℃ of cooling rates: 250 ℃/hour to normal temperature
When the product of measuring embodiment by fluorescent X-ray is formed at last, as composition CaO, SiO
2, Nb
2O
5, Ta
2O
5, V
2O
5And ZrO
2Form corresponding substantially with raw material.
Measure initial permeability, resistivity, core loss Pcv and the saturation flux density Bms of resulting each toroidal core at 25 ℃ of following 100kHz, 1.2MHz.The mensuration of magnetic permeability adopts electric impedance analyzer; Each sample is applied in the sinusoidal current magnetic field of 100kHz and 200mT (maximum), under 100 ℃, measures core loss and saturation flux density with B-H magnetic hysteresis loop tester, the results are shown in table 1
Table 1
| Sample 5 | 18 | 2750 | 2700 | 244 | 424 |
| Sample 6 | 19.5 | 2650 | 2700 | 249 | 420 |
| Sample 7 | 20.5 | 2750 | 2800 | 258 | 426 |
By the visible effect of the present invention of the result shown in the table 1.Be the sample (the sample 1-7 in the table 1) that resistivity of the present invention is adjusted to 15.5-20.5 Ω m, the initial permeability under 1.2MHz is more much bigger than initial permeability 1800 left and right sides of prior art.In this embodiment, resistivity greater than 15 Ω m more than 80%.
[embodiment 2]
In the composition of the manganese-zinc ferrite magnetic core of embodiment 1, main component is removed as the nanometer materials additive component and is contained CaCO relatively
3And SiO
2, also contain Nb
2O
5, Ta
2O
5, V
2O
5And ZrO
2Adopt the manufacture method of embodiment 1, obtain sample 8-20.Estimate each sample of gained similarly to Example 1.The results are shown in table 2
Table 2
[embodiment 3]
In the composition of the manganese-zinc ferrite magnetic core of embodiment 1, main component is removed as additive component and is contained CaCO relatively
3And SiO
2, also contain nano material: SnO
2Or TiO
2, the manufacture method of employing embodiment 1 obtains sample 21-26; P or B obtain sample 27 and 32.Estimate each sample of gained similarly to Example 1.The results are shown in table 3
Table 3
[embodiment 4]
In manganese-zinc ferrite magnetic core of the present invention is formed, contain Fe
2O
3(52 moles of %), ZnO (12 moles of %) and MnO (36 moles of %) prepare burden as main component, and main component is removed as the nanometer materials additive component and contained CaO and SiO relatively
2, also contain Nb
2O
5, Ta
2O
5, V
2O
5And ZrO
2, the manufacture method of employing embodiment 1 obtains sample 33-45.Estimate each sample of gained similarly to Example 1.Estimate each sample of gained similarly to Example 1.The results are shown in table 4
Table 4
| Sample 43 | 0 | 0 | 0 | 0.01 | 2600 | 2600 | 254 | 418 |
| Sample 44 | 0 | 0 | 0 | 0.02 | 2500 | 2600 | 253 | 420 |
| Sample 45 | 0 | 0 | 0 | 0.03 | 2600 | 2600 | 249 | 422 |
[embodiment 5]
In manganese-zinc ferrite magnetic core of the present invention is formed, contain Fe
2O
3(55 moles of %), ZnO (7 moles of %) and MnO (38 moles of %) prepare burden as main component, and main component is removed and contained CaO and SiO as the nanometer materials additive component relatively
2, also contain SnO
2Or TiO
2, the manufacture method of employing embodiment 1 obtains sample 46-51; Contain P or B and obtain sample 52 and 57.Estimate each sample of gained similarly to Example 1.The results are shown in table 5
Table 5
Claims (10)
1. the manufacture method of a manganese-zinc ferrite magnetic core, it is characterized in that Main Ingredients and Appearance contains iron oxide: 52-55 mole %, zinc oxide: 7-12 mole %, manganese oxide 36-38 mole %, and adding dispersant, deionized water, adhesive, defoamer, to be mixed and made into particle mean size be the 80-100 micron, moisture content carries out pre-burning, dry type or case of wet attrition again and makes the powder that particle mean size is the 1.5-2.0 micron below 0.1 weight %; In above-mentioned powder, add the nanometer materials additive, adding dispersant, deionized water, adhesive, defoamer again carries out mixed powder to be broken into particle mean size is the 0.6-1.2 micron, make the particle of 80-200 micron by spray drier, carry out humidification then, to moisture content be the particle of 0.5-1.0 weight %, carry out moulding at last, introduce in the atmosphere of nitrogen or vacuum control oxygen concentration and be finished product after sintering 0.5-5 hour.
2, the manufacture method of a kind of manganese-zinc ferrite magnetic core according to claim 1 is characterized in that described dispersant is poly-propionic acid, adds fashionablely, with respect to Main Ingredients and Appearance is: 0.4-0.6 weight %.
3. the manufacture method of a kind of manganese-zinc ferrite magnetic core according to claim 1 is characterized in that described adhesive is a polyvinyl alcohol, adds fashionablely, with respect to Main Ingredients and Appearance is: 0.1-1.2 weight %.
4. the manufacture method of a kind of manganese-zinc ferrite magnetic core according to claim 1 is characterized in that described defoamer is a n-octyl alcohol, adds fashionablely, with respect to Main Ingredients and Appearance is: 0.1-0.3 weight %.
5. the manufacture method of a kind of manganese-zinc ferrite magnetic core according to claim 1 is characterized in that described nanometer materials additive particle size range is between 10-500nm.
6. the manufacture method of a kind of manganese-zinc ferrite magnetic core according to claim 1 is characterized in that described nanometer materials additive is silica, calcium oxide or niobium oxide, tantalum oxide, vanadium oxide and zirconic one or more or tin oxide or titanium oxide or phosphorus P or boron.
7. according to the manufacture method of claim 1 or 6 described a kind of manganese-zinc ferrite magnetic cores, it is characterized in that described silica content is 0.004-0.03 weight %, calcium oxide content is 0.01-0.5 weight %.
8. according to the manufacture method of claim 1 or 6 described a kind of manganese-zinc ferrite magnetic cores, it is characterized in that described niobium oxide content is 0.004-0.06 weight %, tantalum oxide content is 0.006-0.1.0 weight %, vanadium oxide content is 0.006-0.12 weight %, and zirconic content is 0.004-0.04 weight %.
9. according to the manufacture method of claim 1 or 6 described a kind of manganese-zinc ferrite magnetic cores, it is characterized in that described tin oxide content is 0.04-0.4 weight %, titanium oxide content is 0.04-0.4 weight %.
10. according to the manufacture method of claim 1 or 6 described a kind of manganese-zinc ferrite magnetic cores, the content that it is characterized in that described phosphorus P or boron is below the 0.01 weight %.
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Assignee: Wuxi Spinel Magnetics Co., Ltd. Assignor: Wuxi Jingshi Magnetic Electronic Device Co., Ltd. Contract fulfillment period: 2008.5.14 to 2018.5.14 contract change Contract record no.: 2008320000024 Denomination of invention: Manganese-zinc ferrite magnetic core mfg. method Granted publication date: 20041229 License type: Exclusive license Record date: 2008.5.21 |
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Free format text: EXCLUSIVE LICENCE; TIME LIMIT OF IMPLEMENTING CONTACT: 2008.5.14 TO 2018.5.14 Name of requester: NONE WUXI SIBEIER MAGNETIC MATERIALS CO., LTD. Effective date: 20080521 |