CN1400192A - Mn-Zn ferrite - Google Patents
Mn-Zn ferrite Download PDFInfo
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- CN1400192A CN1400192A CN 02138177 CN02138177A CN1400192A CN 1400192 A CN1400192 A CN 1400192A CN 02138177 CN02138177 CN 02138177 CN 02138177 A CN02138177 A CN 02138177A CN 1400192 A CN1400192 A CN 1400192A
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Abstract
The present invention relates to a kind of Mn-Zn ferrite, belonging to the field of oxide magnetic material technology, its main components are: Fe2O3 49-58 mole%, MnO 21-31 mole % and ZnO 15-26 mole%, and the additive component is added, they can be made into ring magnetic core whose mean grain size is 20-80 micrometer, outer diameter is 25 millimeter, inner diameter is 15 millimeter and height is 5 millimeter. In the frequency range of 1K-150 KHz its magnetic conductivity can be up to high level more than 12000, when it is used for making transformer, the number of turns can be reduced, said transformer can be miniaturized, specially, the transformer with high-frequency characteristics can be obtained in the digital transmission system of ISDN and ADSL, etc. and low volume distribution can be implemented, and the signal can be accurately transmitted.
Description
Technical field:
The present invention relates to a kind of ferrite in manganese zinc series, belong to the oxidate magnetic material technical field.
Technical background:
Before the present invention makes, number of patent application: 98800266.3 provide and are containing the main component manganese oxide, zinc oxide and ferric oxide, the silicon-dioxide of additive component: 50-150ppm, the calcium oxide of 50-500ppm, the bismuth oxide of 50-400ppm, in the sintered type oxidate magnetic material of the molybdenum oxide of 50-400ppm, initial permeability under 10kHz is 8500 or bigger in-20-20 ℃ scope, in 20-100 ℃ of scope, be 10000 or bigger, with the sintered compact oxidate magnetic material of above-mentioned materials under 1300-1400 ℃, and be excellent oxidate magnetic material with temperature profile with initial permeability by adding bismuth oxide and molybdenum oxide.Though the magneticsubstance of putting down in writing in this communique is applicable to the pulse transformer (need in the temperature compensation of low temperature in the high temperature range) of the S/T contact interface of ISDN.But can't obtain simultaneously to be used for along with communication high speed, the desired high magnetic permeability characteristic of widebandization.
Summary of the invention:
The objective of the invention is to overcome above-mentioned weak point, thereby provide a kind of being particularly related to can be used for being assembled into as in the pulse transformer (common-mode filter) time, can realize that low capacity distributes, can be in wide cycle band domain transmission signal exactly, and the pulse transformer of S/T contact interface that is used for ISDN is to satisfy the ferrite in manganese zinc series in the temperature compensation of low temperature in the high temperature range.
Main solution of the present invention is achieved in that
Its main component contains ferric oxide: 49-58 mole %, manganese oxide: 21-31 mole %, zinc oxide: 15-26 mole %, add dispersion agent simultaneously: 0.4-0.6 weight %, deionized water: 40-150 weight %, tackiness agent: 0.1-1.2 weight %, defoamer: 0.1-0.3 weight %, in super mixer, mixed 70-80 minute, making mean particle size by spray-drier is the 80-100 micron, moisture content is below 0.1%, and flow angle is less than the particle of 40 degree; 2, adopt rotary kiln to carry out pre-burning, calcined temperature: 800-980 ℃, the pre-burning time: 5 minutes-2 hours; 3, carry out dry type again and pulverize or case of wet attrition 25-35 minute, making mean particle size is the 1.5-2.0 micron; 4, the weight percent by pre-imitation frosted glass adds 0-0.4% additive, dispersion agent: 0.4-0.6 weight %, and tackiness agent: 0.1-1.2 weight %, defoamer: 0.1-0.3 weight % and deionized water: 40-150 weight % mixes; Carried out in planetary ball mill fine grinding 50-70 minute, wearing into mean particle size is the 0.8-1.2 micron; 5, be the 140-160 micron by making mean particle size after the spray-drier drying, and flow angle is less than the particle of 30 degree; 6, heat, batch mixing: water ratio is 0.5-.08wt%; 7, adopt automatic molder to carry out forming and sintering, keeping temperature in the sintering process is 1200-1450 ℃, soaking time is 0.5-10 hour, and the operation of control oxygen concn was set before this temperature keeps operation, and to make the temperature of control oxygen concn operation in this sintering be 900-1200 ℃; Cool off in the atmosphere of control oxygen partial pressure, making median size is the 20-80 micron, and external diameter is that 25 millimeters, internal diameter are 15 millimeters, highly is 5 millimeters toroidal core; 8, grind processing, cleaning-drying, go-no-go, test at last, the packing warehouse-in.
Containing a kind of of additive component or two kinds among the present invention is respectively: phosphorus: 0.0003-0.005 weight %, boron: 0.0003-0.005 weight %.
One or more that contain additive component among the present invention are respectively: bismuth oxide: 0.005-0.1 weight %, Indium sesquioxide: 0.005-0.12 weight %, vanadium oxide: 0.005-0.10 weight %, molybdenum oxide: 0.005-0.12 weight %, niobium oxides: 0.03-0.06 weight %, hafnia: 0.003-0.06 weight %, tantalum oxide: 0.003-0.06 weight %, zirconium white: 0.003-0.06 weight %, calcium oxide: 0.005-0.08 weight %, silicon-dioxide: 0.005-0.015 weight %, phosphorus: 0.0003-0.005 weight %, boron: 0.0003-0.005 weight %.
The present invention obtains by following any one formation 1.-7..1. a kind of ferrite in manganese zinc series wherein contains ferric oxide, manganese oxide and the zinc oxide of main component.Be converted into Fe
2O
3, MnO, ZnO be respectively: Fe
2O
3: 49-58 mole %, MnO:21-31 mole %, ZnO:15-26 mole %.Contain as additive component and be the phosphorus of 0.0003-0.005 weight %, be boron a kind of of 0.0003-0.005 weight % or two kinds by B that by P average crystal grain directly is the 20-80 micron.2. above-mentioned ferrite in manganese zinc series in 1. wherein with respect to above-mentioned main component, as additive component, further contains a kind of of bismuth oxide, Indium sesquioxide, vanadium oxide or more than one, presses Bi
2O
3: 0.005-0.1 weight %, In
2O
3: 0.005-0.12 weight %, V
2O
5: the 3. 1. above-mentioned or ferrite in manganese zinc series 2. of 0.005-0.10 weight %., wherein with respect to above-mentioned main component, as additive component, further contain by MoO
3: the molybdenum oxide composition of 0.005-0.12 weight %.4. 1. above-mentioned-3. any one ferrite in manganese zinc series, wherein as additive component further contain niobium oxides, hafnia, tantalum oxide, zirconic one or more, be respectively by Nb
2O
5: 0.003-0.06 weight %, HfO
2: 0.003-0.06 weight %, Ta
2O
5: 0.003-0.06 weight %, ZrO
2: 0.003-0.06 weight %.5. 1. above-mentioned-4. any one ferrite in manganese zinc series, wherein further containing by CaO is the calcium oxide of 0.005-0.08 weight %.6. 1. above-mentioned-5. any one ferrite in manganese zinc series, wherein the magnetic permeability of 1kHz-150kHz be 12000 or more than, the initial permeability under 10kHz is 9500 or bigger in-20-20 ℃ scope, is 11000 or bigger in 20-100 ℃ of scope.
Concrete enforcement of the present invention is described in detail.
Ferrite in manganese zinc series of the present invention contains by Fe
2O
3Being the ferric oxide of 49-58 mole %, is the manganese oxide of 21-31 mole % by MnO, is that the zinc oxide of 15-26 mole % is as main component by ZnO.Containing by P is the phosphorus of 0.0003-0.005 weight %, by the boron that B is 0.0003-0.005 weight %, presses Bi
2O
3For the bismuth oxide of 0.005-0.1 weight %, press In
2O
3For the Indium sesquioxide of 0.005-0.12 weight %, press V
2O
5For one or more of the vanadium oxide of 0.005-0.10 weight % as additive component, average crystal grain is the 20-80 micron.And make in the process at it, with respect to above-mentioned main component and additive component, need add 1. dispersion agent, as poly-propionic acid 0.4-0.6 weight %, 2. tackiness agent is as polyvinyl alcohol 0.1-1.2 weight %, 3. defoamer is as n-Octanol 0.1-0.3 weight %, 4. deionized water 40-150 weight %.
Main component preferably is respectively by Fe
2O
3Be the ferric oxide of 49-58 mole %, preferably 51.5-54.5 mole % is the manganese oxide of 21-31 mole % by MnO, and preferably 23.5-28 mole % is the zinc oxide of 15-26 mole % by ZnO, preferably about 18-24 mole %.
Usually also can contain calcium oxide and silicon-dioxide as additive component according to ferrite in manganese zinc series of the present invention.The content of calcium oxide preferably is calculated as 0.005-0.08 weight % by CaO, particularly preferably is 0.01-0.03 weight %, presses SiO
2Be 0.005-0.015 weight %.CaO and SiO
2Usually be present in the boundary.
In addition, the ferrite in manganese zinc series of this invention preferably contains one or more in bismuth oxide, Indium sesquioxide, vanadium oxide, the molybdenum oxide.The total content of these compositions is preferably pressed Bi
2O
3, In
2O
3, V
2O
5, MoO
3Be about 0-0.4 weight % Deng calculating.
Bismuth oxide composition, molybdenum oxide composition, particularly molybdenum oxide composition, the part of when sintering, can evaporating or distil, at this moment, the bismuth oxide in the ferrite and the content of molybdenum oxide can be inconsistent with add-on.The content that is preferred bismuth oxide is by Bi
2O
3About the 40-100 weight % for add-on, the content of molybdenum oxide is pressed MoO
3About 10-100 weight %, particularly contain 10-50 weight % for add-on.
In the ferrite in manganese zinc series of the present invention, as additive component can preferably contain niobium oxides, hafnia, tantalum oxide, zirconic one or more, press Nb respectively
2O
5, HfO
2, Ta
2O
5, ZrO
2For: Nb
2O
5: 0.003-0.06 weight %, preferred 0.005-0.04 weight %, preferred especially 0.008-0.025 weight %, HfO
2: 0.003-0.06 weight %, preferred 0.005-0.04 weight %, preferred especially 0.01-0.03 weight %, Ta
2O
5: 0.003-0.06 weight %, preferred 0.008-0.05 weight %, preferred especially 0.015-0.03 weight %, ZrO
2: 0.003-0.06 weight %, preferred 0.01-0.05 weight %, preferred especially 0.02-0.04 weight %.
By these additive component elements, can increase substantially the particularly magnetic permeability of high frequency number.In these elements, preferred especially zirconium white, two kinds of hafnia or above and usefulness, and ratio is arbitrarily.
According to average crystal grain of the present invention 20-80 micron preferably, more preferably the 20-60 micron particularly preferably is the 30-50 micron.At average crystal grain too greatly or too hour, the broadband properties of initial permeability can worsen.Average crystal grain can be after with optics observation by microscope acid corrosion high polishing surface, and the mean diameter of the circle that is converted to from poly grains is measured.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 component.As required,, can add lime carbonate etc. and become the compound or the calcium oxide of calcium oxide, and become the compound of silicon oxide or silicon oxide etc. by sintering by sintering as the additive component raw material.But these additive components can add by the final above-mentioned amount ratio of forming of magneticsubstance.
Description of drawings:
Fig. 1 is manufacture craft of the present invention (process flow sheet):
The used stove of sintering of the present invention can be the tunnel like continuous oven, also can be a batch stove.Atmosphere during sintering can be adjusted according to the theory of balance oxygen partial pressure, carries out sintering in the nitrogen atmosphere particularly preferably in the control oxygen partial pressure.
Embodiment:
Represent specific embodiments of the invention below, further describe the present invention.
Embodiment 1
With Fe
2O
3(53.5 moles of %), MnO (26 moles of %) and ZnO (20.5 moles of %) as major ingredient, add dispersion agent simultaneously: poly-propionic acid: 0.5 weight %, defoamer: n-Octanol: 0.2 weight %, deionized water 95 weight %.After their are mixed, add tackiness agent: polyvinyl alcohol: 0.8 weight % solution, in super mixer, mixed 70-80 minute, making mean particle size by spray-drier is 100 microns, moisture content is below 0.1%, and flow angle less than 40 degree particle; In rotary kiln, carry out pre-burning, calcined temperature: 800-980 ℃, the pre-burning time: 5 minutes-2 hours; 3, carry out dry type again and pulverize or case of wet attrition 25-35 minute, making mean particle size is the 1.5-2.0 micron; Add the additive composition: calcium oxide (CaO): 0.02 weight %, silicon-dioxide (SiO
2): 0.01 weight %, niobium oxides (Nb
2O
5): 0.03 weight %, tantalum oxide (Ta
2O
5): 0.03 weight %, zirconium white (ZrO
2): 0.04 weight %, hafnia (HfO
2): 0.04 weight %, above-mentioned CaO and SiO
2Final composition for magneticsubstance.Add deionized water 95 weight %, dispersion agent when adding additive component again: poly-propionic acid: 0.5 weight %, defoamer: n-Octanol: 0.2 weight %, tackiness agent: polyvinyl alcohol: 0.8 weight % solution mixes, be placed on and carry out fine grinding 50-70 minute in the planetary ball mill, grinding mean particle size is the 0.8-1.2 micron; Solid content is more than 60%, and viscosity is 250-350cps; By making the particle that mean particle size is the 140-160 micron after the spray-drier drying, and flow angle is less than the particles of 30 degree; Carry out humidification, batch mixing, water ratio is 0.5-0.8wt%; Adopt automatic molder to form sintering, be pressed into 100 in sample.It is to be warming up to 900 ℃ in the atmosphere more than 20% that these molding blanks are placed on oxygen concentration, in being 0.5% nitrogen atmosphere, oxygen concentration is warming up to 1200 ℃ then, be 1200-1450 ℃ of maintenance steady temperature 1-8 hour in the atmosphere 20% or more at last, carry out sintering in oxygen concentration.Cool off in the atmosphere of control oxygen partial pressure, obtaining median size is the 20-80 micron, 25 millimeters of external diameters, and 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 ℃ heat-up rate: 60 ℃/hour
Heat-up rate from 400 ℃ to 900 ℃: 300 ℃/hour
Heat-up rate from 900 ℃ to 1200 ℃: 150 ℃/hour
From 1200 to 1400 ℃ heat-up rate: 120 ℃/hour
The insulation operation
Kept 5 hours at 1400 ℃
Cooling process
Cooling rate from 1400 ℃ to 1100 ℃: 100 ℃/hour
1100 ℃ of cooling rates: 250 ℃/hour to normal temperature
When the product of measuring embodiment and comparative example by fluorescent X-ray is formed at last, as main component CaO, SiO
2, Nb
2O
5, Ta
2O
5, ZrO
2And HfO
2Form corresponding substantially with raw material.
Measure resulting each toroidal core under the frequency of magnetic permeability, median size and the 10kHz of 25 ℃ of following 10kHz, 150kHz, the Schwellenwert of μ i in-20-20 ℃ scope, the Schwellenwert of μ i in 20-100 ℃ of scope.The mensuration of magnetic permeability adopts electric impedance analyzer. the results are shown in table 1
Table 1
*) represent outside the scope of the present invention.
By the visible effect of the present invention of the result shown in the table 1.It is the sample (the sample 1-7 of expression formula) that median size of the present invention is adjusted to the 43-141 micron, magnetic permeability under 10kHz and existing (the sample 8-10 of table 1) are much bigger, particularly the magnetic permeability more than the 150kHz is very big compared with the existing, under the frequency of 10kHz, the Schwellenwert of μ i is also much bigger compared with the existing in-20-20 ℃ scope.In this embodiment, particle diameter greater than the crystallization of 30-60 micron more than 80 volume %.
Embodiment 2
In the composition of ferrite in manganese zinc series, contain Fe
2O
3(50 moles of %), MnO (22 moles of %), ZnO (16 moles of %) are as main component, and main component is removed as additive component and contained CaO and SiO relatively
2, also contain Bi
2O
3, MoO
3Making method with among the P employing embodiment 1 makes sample 11-16; Contain Bi
2O
3Obtain sample 17 and 18 with P, only contain P and obtain sample 19.Sample 20-22 makes Bi as a comparison
2O
3, MoO
3Prepare outside above-mentioned scope with the add-on of P.
Estimate each sample of gained similarly to Example 1.The results are shown in one table 2 is arranged
Table 2
| Sample 12 | ????0.03 | ????0.04 | ??0.0015 | ??16100 | ??14100 | ????12500 | ??15800 |
| Sample 13 | ????0.03 | ????0.04 | ??0.0025 | ??16000 | ??14000 | ????12700 | ??15900 |
| Sample 14 | ????0.04 | ????0.04 | ??0.0015 | ??16800 | ??13800 | ????13000 | ??16500 |
| Sample 15 | ????0.03 | ????0.06 | ??16400 | ??14100 | ????12500 | ??16100 | |
| Sample 16 | ????0.06 | ????0.08 | ??0.001 | ??15000 | ??14400 | ????12200 | ??14900 |
| Sample 17 | ????0.03 | ????0 | ??0.0015 | ??16300 | ??13100 | ????13000 | ??16000 |
| Sample 18 | ????0.06 | ????0 | ??0.0015 | ??15900 | ??12700 | ????12800 | ??15700 |
| Sample 19 | ????0 | ????0 | ??0.0015 | ??14700 | ??13900 | ????12300 | ??14500 |
| Sample 20 | ????0 | ????0 | ??0.0060 | ??13900 | ??7180 | ????7100 | ??13500 |
| Sample 21 | ????0.03 | ????0.04 | ??0.0060 | ??12700 | ??7000 | ????7400 | ??12600 |
| Sample 22 | ????0.12 | ????0.10 | ??0.0015 | ??14300 | ??8200 | ????7200 | ??13900 |
*) be illustrated in outside scope of the present invention and the preferable range.
Embodiment 3
In the composition of ferrite in manganese zinc series, contain Fe
2O
3(55 moles of %), MnO (25 moles of %), ZnO (18 moles of %) are main component, and main component is removed as additive component and contained CaO and SiO relatively
2, also contain In
2O
3, MoO
3The method that adopts embodiment 1 to make with P makes sample 23-28; Contain In
2O
3Obtain sample 29 and 30 with P, only contain P and obtain sample 31.Sample 32-34 makes In as a comparison
2O
3, MoO
3Prepare outside above-mentioned scope with the add-on of P.
Estimate each sample of gained similarly to Example 1.The results are shown in one table 3 is arranged
Table 3
*) be illustrated in outside scope of the present invention and the preferable range.
Embodiment 4
In the composition of ferrite in manganese zinc series, contain Fe
2O
3(49 moles of %), MnO (21 moles of %), ZnO (15 moles of %) are main component, and main component is removed as additive component and contained CaCO relatively
3And SiO
2, also contain V
2O
5, MoO
3Adopt the making method of embodiment 1 to obtain sample 35-40 with P; Contain V
2O
5Obtain sample 41 and 42 with B, only contain B and obtain sample 43.Sample 44-46 makes V as a comparison
2O
5, MoO
3Prepare outside above-mentioned scope with the add-on of B.
Estimate each sample of gained similarly to Example 1.The results are shown in one table 4 is arranged
Table 4
*) be illustrated in outside scope of the present invention and the preferable range.
Embodiment 5
In the composition of ferrite in manganese zinc series, contain Fe
2O
3(58 moles of %), MnO (31 moles of %), ZnO (26 moles of %) are main component, and main component is removed as additive component and contained CaCO relatively
3And SiO
2, Bi
2O
3Or In
2O
3Or V
2O
5, MoO
3Further contain ZrO with P or B
2, Ta
2O
5, HfO
2, Nb
2O
5The making method of employing embodiment 1 makes and obtains sample 47-50, sample 51 and 53, and to sample 54-56, sample 57-59.Comparative sample 60 is that add-on does not prepare at above-mentioned additive component.
Estimate each sample of gained similarly to Example 1.The results are shown in one table 5 is arranged
Table 5
*) be illustrated in outside the scope of the present invention.
Compared with the prior art the present invention has the following advantages:
The magnetic conductivity of the present invention in the 1k-150kHz frequency range also can reach the high level more than 12000, as transformer the time, can reduce the coiling number, make the transformer miniaturization, particularly can obtain in the digital transmission system of ISDN and ADSL etc. the transformer of performance high frequency characteristics, can realize that low capacity distributes, can be in wide cycle band domain signal transmission exactly, simultaneously, can obtain again at low temperature excellent temperature compensation characteristic in the high temperature range.
Claims (6)
1, a kind of ferrite in manganese zinc series, it is characterized in that: 1, its main component contains ferric oxide: 49-58 mole %, manganese oxide: 21-31 mole %, zinc oxide: 15-26 mole %, add dispersion agent simultaneously: 0.4-0.6 weight %, deionized water: 40-150 weight %, tackiness agent: 0.1-1.2 weight %, defoamer: 0.1-0.3 weight %, in super mixer, mixed 70-80 minute, making mean particle size by spray-drier is the 80-100 micron, moisture content is below 0.1%, and flow angle is less than the particle of 40 degree; 2, adopt rotary kiln to carry out pre-burning, calcined temperature: 800-980 ℃, the pre-burning time: 5 minutes-2 hours; 3, carry out dry type again and pulverize or case of wet attrition 25-35 minute, making mean particle size is the 1.5-2.0 micron; 4, the weight percent by pre-imitation frosted glass adds 0-0.4% additive, dispersion agent: 0.4-0.6 weight %, tackiness agent: 0.1-1.2 weight %, defoamer: 0.1-0.3 weight % and deionized water: 40-150 weight % mixes; Carried out in planetary ball mill fine grinding 50-70 minute, wearing into mean particle size is the 0.8-1.2 micron; 5, be the 140-160 micron by making mean particle size after the spray-drier drying, and flow angle is less than the particle of 30 degree; 6, heat, batch mixing: water ratio is 0.5-08wt%; 7, adopt automatic molder to carry out forming and sintering, keeping temperature in the sintering process is 1200-1450 ℃, soaking time is 0.5-10 hour, and the operation of control oxygen concn was set before this temperature keeps operation, and to make the temperature of control oxygen concn operation in this sintering be 900-1200 ℃; Cool off in the atmosphere of control oxygen partial pressure, making median size is the 20-80 micron, and external diameter is 15 millimeters of 25 millimeters, internal diameter, highly is 5 millimeters toroidal core.
2, a kind of ferrite in manganese zinc series according to claim 1 is characterized in that described dispersion agent is poly-propionic acid.
3, a kind of ferrite in manganese zinc series according to claim 1 is characterized in that described tackiness agent is a polyvinyl alcohol.
4, a kind of ferrite in manganese zinc series according to claim 1 is characterized in that described defoamer is a n-Octanol.
5, a kind of ferrite in manganese zinc series according to claim 1, it is characterized in that below adopting one or more of described additive component, be respectively: bismuth oxide: 0.005-0.1 weight %, Indium sesquioxide: 0.005-0.12 weight %, vanadium oxide: 0.005-0.10 weight %, molybdenum oxide: 0.005-0.12 weight %, niobium oxides: 0.03-0.06 weight %, hafnia: 0.003-0.06 weight %, tantalum oxide: 0.003-0.06 weight %, zirconium white: 0.003-0.06 hangs down and measures %, calcium oxide: 0.005-0.08 weight %, silicon-dioxide: 0.005-0.015 weight %, phosphorus: 0.0003-0.005 weight %, boron: 0.0003-0.005 weight %.
6, a kind of ferrite in manganese zinc series according to claim 1 is characterized in that described additive component contains phosphorus: 0.0003-0.005 weight %, boron: 0.0003-0.005 weight % a kind of or two kinds.
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|---|---|---|---|
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