CN1749209A - High saturated magnetic flux density and low loss manganese-zinc ferrite material and its preparing method - Google Patents
High saturated magnetic flux density and low loss manganese-zinc ferrite material and its preparing method Download PDFInfo
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- CN1749209A CN1749209A CN 200510060285 CN200510060285A CN1749209A CN 1749209 A CN1749209 A CN 1749209A CN 200510060285 CN200510060285 CN 200510060285 CN 200510060285 A CN200510060285 A CN 200510060285A CN 1749209 A CN1749209 A CN 1749209A
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- 239000000463 material Substances 0.000 title claims abstract description 46
- 230000004907 flux Effects 0.000 title claims abstract description 30
- 238000000034 method Methods 0.000 title claims description 9
- 229910001289 Manganese-zinc ferrite Inorganic materials 0.000 title abstract description 7
- JIYIUPFAJUGHNL-UHFFFAOYSA-N [O--].[O--].[O--].[O--].[O--].[O--].[O--].[O--].[O--].[O--].[O--].[O--].[O--].[O--].[O--].[O--].[O--].[O--].[O--].[O--].[Mn++].[Mn++].[Mn++].[Fe+3].[Fe+3].[Fe+3].[Fe+3].[Fe+3].[Fe+3].[Fe+3].[Fe+3].[Fe+3].[Fe+3].[Zn++].[Zn++] Chemical compound [O--].[O--].[O--].[O--].[O--].[O--].[O--].[O--].[O--].[O--].[O--].[O--].[O--].[O--].[O--].[O--].[O--].[O--].[O--].[O--].[Mn++].[Mn++].[Mn++].[Fe+3].[Fe+3].[Fe+3].[Fe+3].[Fe+3].[Fe+3].[Fe+3].[Fe+3].[Fe+3].[Fe+3].[Zn++].[Zn++] JIYIUPFAJUGHNL-UHFFFAOYSA-N 0.000 title abstract description 6
- 229920006395 saturated elastomer Polymers 0.000 title abstract 2
- 238000005245 sintering Methods 0.000 claims abstract description 47
- 238000002360 preparation method Methods 0.000 claims abstract description 20
- 238000000498 ball milling Methods 0.000 claims abstract description 17
- 229910044991 metal oxide Inorganic materials 0.000 claims abstract description 9
- 150000004706 metal oxides Chemical class 0.000 claims abstract description 9
- 239000000203 mixture Substances 0.000 claims description 41
- 229910000859 α-Fe Inorganic materials 0.000 claims description 35
- 229910004298 SiO 2 Inorganic materials 0.000 claims description 26
- QVGXLLKOCUKJST-UHFFFAOYSA-N atomic oxygen Chemical compound [O] QVGXLLKOCUKJST-UHFFFAOYSA-N 0.000 claims description 15
- 238000001816 cooling Methods 0.000 claims description 15
- 238000000227 grinding Methods 0.000 claims description 15
- 229910052760 oxygen Inorganic materials 0.000 claims description 15
- 239000001301 oxygen Substances 0.000 claims description 15
- 239000007858 starting material Substances 0.000 claims description 15
- 239000002245 particle Substances 0.000 claims description 14
- 239000000843 powder Substances 0.000 claims description 12
- 239000008367 deionised water Substances 0.000 claims description 11
- 229910021641 deionized water Inorganic materials 0.000 claims description 11
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Chemical compound O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims description 11
- 238000009413 insulation Methods 0.000 claims description 10
- 239000004372 Polyvinyl alcohol Substances 0.000 claims description 9
- 229920002451 polyvinyl alcohol Polymers 0.000 claims description 9
- 239000005338 frosted glass Substances 0.000 claims description 7
- 238000007792 addition Methods 0.000 claims description 6
- 229910052751 metal Inorganic materials 0.000 claims description 6
- 230000008569 process Effects 0.000 claims description 6
- 229910052723 transition metal Inorganic materials 0.000 claims description 6
- 150000003624 transition metals Chemical class 0.000 claims description 6
- 229910052742 iron Inorganic materials 0.000 claims description 5
- 238000000465 moulding Methods 0.000 claims description 5
- 239000002002 slurry Substances 0.000 claims description 5
- 150000001875 compounds Chemical class 0.000 claims description 3
- 238000000748 compression moulding Methods 0.000 claims description 3
- 229910052738 indium Inorganic materials 0.000 claims description 3
- VTYYLEPIZMXCLO-UHFFFAOYSA-L Calcium carbonate Chemical compound [Ca+2].[O-]C([O-])=O VTYYLEPIZMXCLO-UHFFFAOYSA-L 0.000 abstract 2
- VYPSYNLAJGMNEJ-UHFFFAOYSA-N Silicium dioxide Chemical compound O=[Si]=O VYPSYNLAJGMNEJ-UHFFFAOYSA-N 0.000 abstract 2
- VCBRPAWXBLKZEP-UHFFFAOYSA-N [Mn].[Mn].[Zn] Chemical compound [Mn].[Mn].[Zn] VCBRPAWXBLKZEP-UHFFFAOYSA-N 0.000 abstract 1
- 229910000019 calcium carbonate Inorganic materials 0.000 abstract 1
- 235000010216 calcium carbonate Nutrition 0.000 abstract 1
- 229910052681 coesite Inorganic materials 0.000 abstract 1
- 229910052906 cristobalite Inorganic materials 0.000 abstract 1
- 238000009776 industrial production Methods 0.000 abstract 1
- JEIPFZHSYJVQDO-UHFFFAOYSA-N iron(III) oxide Inorganic materials O=[Fe]O[Fe]=O JEIPFZHSYJVQDO-UHFFFAOYSA-N 0.000 abstract 1
- 238000009740 moulding (composite fabrication) Methods 0.000 abstract 1
- 239000000377 silicon dioxide Substances 0.000 abstract 1
- 235000012239 silicon dioxide Nutrition 0.000 abstract 1
- 229910052682 stishovite Inorganic materials 0.000 abstract 1
- 229910052905 tridymite Inorganic materials 0.000 abstract 1
- 239000011701 zinc Substances 0.000 description 10
- 238000012360 testing method Methods 0.000 description 7
- 239000013078 crystal Substances 0.000 description 4
- 230000000694 effects Effects 0.000 description 3
- 239000012535 impurity Substances 0.000 description 3
- 239000000047 product Substances 0.000 description 3
- 229910052596 spinel Inorganic materials 0.000 description 3
- 239000011029 spinel Substances 0.000 description 3
- 229910004762 CaSiO Inorganic materials 0.000 description 2
- 229910006404 SnO 2 Inorganic materials 0.000 description 2
- 229910010413 TiO 2 Inorganic materials 0.000 description 2
- 238000006243 chemical reaction Methods 0.000 description 2
- 238000011161 development Methods 0.000 description 2
- 238000005516 engineering process Methods 0.000 description 2
- 239000011521 glass Substances 0.000 description 2
- WJZHMLNIAZSFDO-UHFFFAOYSA-N manganese zinc Chemical class [Mn].[Zn] WJZHMLNIAZSFDO-UHFFFAOYSA-N 0.000 description 2
- 238000011160 research Methods 0.000 description 2
- 230000002159 abnormal effect Effects 0.000 description 1
- 239000000654 additive Substances 0.000 description 1
- 230000000996 additive effect Effects 0.000 description 1
- 238000005054 agglomeration Methods 0.000 description 1
- 230000002776 aggregation Effects 0.000 description 1
- 238000004891 communication Methods 0.000 description 1
- 238000000354 decomposition reaction Methods 0.000 description 1
- 239000012467 final product Substances 0.000 description 1
- 239000004615 ingredient Substances 0.000 description 1
- 150000002500 ions Chemical class 0.000 description 1
- 238000004519 manufacturing process Methods 0.000 description 1
- 238000012545 processing Methods 0.000 description 1
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- 239000011800 void material Substances 0.000 description 1
- 238000005303 weighing Methods 0.000 description 1
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- Magnetic Ceramics (AREA)
Abstract
The present invention discloses high saturated magnetic flux density and low loss manganese manganese-zinc ferrite material and its preparation process. The manganese-zinc ferrite material contains: Fe2O3 52-54 mol%, MnO 33-40 mol%, ZnO 8-13 mol%, supplementary components CaCO3 100-600 ppm, SiO2 50-300 ppm and other metal oxides. The preparation process includes the steps of: mixing material, pre-sintering, adding supplementary components, secondary ball milling, forming and sintering. The supplementary components are common oxide grains, and this result in easy adding and low cost. The preparation process of the manganese-zinc ferrite material has relatively low pre-sintering and sintering temperature and relaxed requirement on sintering apparatus, may be completed in common vacuum sintering furnace, and easily realized in industrial production.
Description
Technical field
The present invention relates to a kind of high saturation magnetic flux density, low loss manganese-zinc ferrite material and preparation method thereof.
Background technology
The ferrite in manganese zinc series material is widely used on the electronics components and parts of communication, robot calculator, televisor and all kinds of digital products etc. at present, is a class soft magnetic ferrite of volume production maximum.Wherein the power Mn-Zn ferrite is again maximum in a ferrite in manganese zinc series classification, and its topmost application is exactly the main-transformer of the various high frequency switch powers of preparation.The main development trend of switch power supply is exactly miniaturization and low-lossization, and this requires should have higher saturation magnetic flux density and lower power consumption as the Mn-Zn ferrite of main-transformer inner magnetic core.
In recent years, digital camera, Digital Video and mobile signal equipment etc. are universal day by day in people's daily life, these equipment all are operated in below 45 ℃ usually, and therefore the optimal working temp that requires inner various electronic devices and components is all below 45 ℃, and wherein switch power supply is no exception.And this just needs the interior MnZn ferrite material of main-transformer of switch power supply to have minimum power consumption about 45 ℃.Therefore exploitation has lowest power consumption and has boundless market application foreground with the Mn-Zn ferrite with high saturation magnetic flux density about 45 ℃.
At present, the temperature range of the lowest power consumption of most power Mn-Zn ferrites is generally in 60～100 ℃, and the power consumption number under the test condition of 100kHz, 200mT is generally greater than 300kW/m
3And, require the power consumption number of Mn-Zn ferrite to be lower than 245kW/m in order to adapt to the development trend of digital equipment
3, in order to achieve this end, some research workers add the ancillary component of nanoscale usually in MnZn ferrite material.Though the ancillary component of nanoscale can reduce the material power consumption preferably, there are unfavorable factors such as easily reunion, material cost height.Therefore seek a kind of need not to add the nanometer ancillary component about 45 ℃, have the lowest power consumption value and power consumption number is lower than 245kW/m
3Have very important significance for expanding the application of Mn-Zn ferrite in the digital equipment field with power MnZn ferrite material with high saturation magnetic flux density and preparation method thereof.
Summary of the invention
The purpose of this invention is to provide a kind of high saturation magnetic flux density, low loss manganese-zinc ferrite material and preparation method thereof.
High saturation magnetic flux density, have the MnZn ferrite material of super low-power consumption about 45 ℃, its principal phase is a spinel structure, and its major ingredient is calculated as follows with oxide form:
Fe
2O
3：52～54mol％；
MnO：33～40mol％；
ZnO：8～13mol％；
Auxiliary composition CaCO
3: 100～600ppm;
SiO
2：50～300ppm；
All the other are the auxiliary composition of metal oxide.
The auxiliary composition of described metal oxide is A
2O
3, wherein A is a trivalent metallic element, at least from Co
3+, Al
3+, Bi
3+Middle selection is a kind of or unite interpolation, and its overall control is at 100～400ppm.
Perhaps be BO
2, wherein B is a tetravalent, at least from Zr
4+, Hf
4+, Ti
4+And Sn
4+Middle selection is a kind of or unite interpolation, and its overall control is at 100～400ppm.
Perhaps be M
2O
5, wherein M is the pentavalent transition metal, at least from V
5+, Nb
5+Middle selection is a kind of or unite interpolation, and its overall control is at 100～400ppm.
Metal oxide is assisted composition A
2O
3, BO
2And M
2O
5Content should meet following formula: 0＜X+Y+Z≤1000ppm, wherein X, Y and Z represent A respectively
2O
3, BO
2And M
2O
5Content.
The preparation method's of MnZn ferrite material provided by the invention concrete steps are:
1) starting material mix:
Choose 52～54mol%Fe
2O
3, the MnO of 33～40mol% and 8～13mol% ZnO as starting material, put into ball mill, the deionized water of weight such as adding, ball milling 2～5 hours, the mean particle size of the powder behind the mix grinding is controlled at 0.6～0.8 μ m, SiO
2Content be controlled at below the 30ppm;
2) pre-burning:
The stove pre-burning is put in the material oven dry that mix grinding is good, and calcined temperature is 800～950 ℃, and the pre-burning time is 2～4h;
3) auxiliary composition adds:
Contain 100～600ppm CaCO in the auxiliary composition that adds
3With 50～300ppm SiO
2, and the CaCO that adds
3And SiO
2Weight ratio be 1.5～2.2: 1; Except CaCO
3And SiO
2Outside also select A for use
2O
3, BO
2And M
2O
5Add as the auxiliary composition of oxide compound, wherein at A
2O
3In, A is a trivalent metallic element, at least from Co
3+, Al
3+, Bi
3+Middle selection is a kind of or unite interpolation, and its overall control is at 100～400ppm; At BO
2In, B is a tetravalent, at least from Zr
4+, Hf
4+, Ti
4+And Sn
4+Middle selection is a kind of or unite interpolation, and its overall control is at 100～400ppm; At M
2O
5In, M is the pentavalent transition metal, at least from V
5+, Nb
5+Middle selection is a kind of or unite interpolation, and its overall control is at 100～400ppm, and the summation of three class additions should be less than 1000ppm.
4) secondary ball milling:
Material is put into ball mill, the deionized water of weight such as adding, ball milling 3～6h, the mean particle size that makes pre-imitation frosted glass is 1.0～1.2 μ m;
5) moulding:
With the slurry oven dry, add the polyvinyl alcohol (PVA) of 10wt%, compression moulding;
6) sintering:
Sintering is divided into intensification, insulation and cooling three phases,
Heat up: 1250～1300 ℃ from room temperature to sintering temperature, heat-up rate is 3 ℃/min, and temperature-rise period carries out in air,
Insulation: sintering temperature is 1250～1300 ℃, and sintering time is 3～6h, and the air pressure of sintering process is 1 normal atmosphere, and oxygen level is 3.0～5.0mol%, and all the other are N
2,
Cooling: from 1250～1300 ℃ to 200 ℃ of sintering temperatures, cooling rate is 2 ℃/min, and air pressure is a standard atmospheric pressure, and the oxygen level in the temperature-fall period in the stove should meet following formula:
, PO wherein
2Be the volumn concentration of oxygen, a is a constant, and its value is 4～5, and b is a constant, and its value is 14000～15000; T is the absolute temperature of stove.
The ancillary component that adds in the MnZn ferrite material of the present invention preparation is common oxide particle, need not Nano grade, does not have agglomeration traits, therefore add simple and easy, cost is lower, and this material has the 245kw/m of being lower than at 45 ℃
3Power consumption, in the time of 25 ℃, have saturation magnetic flux density greater than 535mT, therefore be the starting material that a kind of good can being applied to prepares the main-transformer magnetic core in the switch power supply in the various digital products.The preparation method of MnZn ferrite material provided by the invention is simple and easy, and pre-burning and sintering temperature are lower, and is lower to the requirement of agglomerating plant, can realize in common vacuum sintering furnace, therefore is easy to realize industrialization.
Embodiment
The invention provides a kind of high saturation magnetic flux density, about 45 ℃, have MnZn ferrite material of super low-power consumption and preparation method thereof.Add and processing parameter by adjusting main formula and impurity, make the MnZn ferrite material of preparing in the time of 45 ℃, have the 245kw/m of being lower than
3Power consumption, in the time of 25 ℃, have saturation magnetic flux density greater than 535mT.
Above-mentioned has the 245kw/m of being lower than at 45 ℃
3Power consumption, in the time of 25 ℃, have exist in the MnZn ferrite material greater than the saturation magnetic flux density of 535mT spinel mutually with a spot of amorphous glass mutually, and amorphous glass is evenly distributed on the crystal boundary mutually.
Select commercially pure Fe
2O
3, MnO and ZnO be as starting material.Take by weighing various starting material according to the component molecules formula and carry out mix grinding, mix grinding equipment choosing high-energy planetary ball mill machine.In the mix grinding process, the deionized water of weight such as adding, ball milling 2～5 hours requires the mean particle size of the powder behind the mix grinding to be controlled at 0.6～0.8 μ m, SiO
2Content be controlled at below the 30ppm.It is in order to reduce the specific surface area of powder that the mean particle size of the powder behind the mix grinding is controlled at 0.6～0.8 μ m, improves the reactive behavior of powder, make powder can be under lower calcined temperature spinelization fully.And SiO
2Content to be controlled at below the 30ppm be in order to control total SiO of final product
2Content.
Temperature range during pre-burning is 800～950 ℃, requires the starting material complete reaction to form unicuspid spar phase after pre-burning, and lower calcined temperature helps in promoting follow-up sintering reaction, and this helps to reduce sintering temperature.And number of research projects has also shown, reduces the appearance that sintering temperature can effectively suppress abnormal grain, reduces the void content of crystal grain inside, and this has important effect for the power consumption that improves saturation magnetic flux density, reduction material.
Select CaCO
3And SiO
2As additive, unite interpolation, be in order to reduce the eddy-current loss of Mn-Zn ferrite.The loss of Mn-Zn ferrite can be divided into this three class of magnetic hysteresis loss, eddy-current loss and residual loss, wherein the power Mn-Zn ferrite under working conditions generally based on magnetic hysteresis loss and eddy-current loss.Because CaCO
3And SiO
2Can react, on crystal boundary, form the CaSiO of glassy phase
3, and the CaSiO of glassy phase
3Have very high resistivity, thereby improved the resistance of MnZn ferrite material, reduced eddy-current loss.In order to make CaCO
3And SiO
2Can react more completely, require CaCO
3And SiO
2Weight percent be controlled at 1.5～2.2: 1.But CaCO
3And SiO
2Addition unsuitable too much, otherwise will cause that crystal grain is grown up unusually, disadvantageous effect such as non magnetic mutually too much.
Except CaCO
3And SiO
2Outside also select A for use
2O
3, BO
2And M
2O
5Add as auxiliary composition, wherein A is a trivalent metallic element, at least from Co
3+, Al
3+, Bi
3+In select a kind of or unite interpolation; B is a tetravalent, at least from Zr
4+, Hf
4+, Ti
4+And Sn
4+In select a kind of or unite interpolation; M is the pentavalent transition metal, at least from V
5+, Nb
5+Middle selection is a kind of or unite interpolation, and the summation of three kinds of additions should be less than 1000ppm.The main purpose that these three kinds of ionic add is to regulate the Fe in the material
2+And Fe
3+Proportionlity, simultaneously high valence ion also can by and Fe
2+Form stable electron pair, reduce Fe
2+And Fe
3+Between electronics move more, improved the resistance of Ferrite Material, thereby reduced the magnetic hysteresis loss and the eddy-current loss of Mn-Zn ferrite.But three kinds of ionic additions must be controlled in the 1000ppm, otherwise will cause non magnetic phase go out disadvantageous effects such as item, spinel phase decomposition.
Provided by the invention have the 245kw/m of being lower than at 45 ℃
3Power consumption, the MnZn ferrite material and the preparation process that have in the time of 25 ℃ greater than the saturation magnetic flux density of 535mT specify as follows:
1) starting material mix:
Choose 52～54mol%Fe
2O
3, the MnO of 33～40mol% and 8～13mol% ZnO as starting material, put into ball mill, the deionized water of weight such as adding, ball milling 2～5 hours, the mean particle size of the powder behind the mix grinding is controlled at 0.6～0.8 μ m, SiO
2Content be controlled at below the 30ppm;
2) pre-burning:
The stove pre-burning is put in the material oven dry that mix grinding is good, and calcined temperature is 800～950 ℃, and the pre-burning time is 2～4h:
3) auxiliary composition adds:
Contain 100～600ppm CaCO in the auxiliary composition that adds
3With 50～300ppm SiO
2, and the CaCO that adds
3And SiO
2Weight ratio be 1.5～2.2: 1; Except CaCO
3And SiO
2Outside also select A for use
2O
3, BO
2And M
2O
5Add as the auxiliary composition of oxide compound, wherein at A
2O
3In, A is a trivalent metallic element, at least from Co
3+, Al
3+, Bi
3+Middle selection is a kind of or unite interpolation, and its overall control is at 100～400ppm; At BO
2In, B is a tetravalent, at least from Zr
4+, Hf
4+, Ti
4+And Sn
4+Middle selection is a kind of or unite interpolation, and its overall control is at 100～400ppm; At M
2O
5In, M is the pentavalent transition metal, at least from V
5+, Nb
5+Middle selection is a kind of or unite interpolation, and its overall control is at 100～400ppm, and the summation of three class additions should be less than 1000ppm.
4) secondary ball milling:
Material is put into ball mill, the deionized water of weight such as adding, ball milling 3～6h, the mean particle size that makes pre-imitation frosted glass is 1.0～1.2 μ m;
5) moulding:
With the slurry oven dry, add the polyvinyl alcohol (PVA) of 10wt%, compression moulding;
6) sintering:
Sintering is divided into intensification, insulation and cooling three phases,
Heat up: 1250～1300 ℃ from room temperature to sintering temperature, heat-up rate is 3 ℃/min, and temperature-rise period carries out in air,
Insulation: sintering temperature is 1250～1300 ℃, and sintering time is 3～6h, and the air pressure of sintering process is 1 normal atmosphere, and oxygen level is 3.0～5.0mol%, and all the other are N
2,
Cooling: from 1250～1300 ℃ to 200 ℃ of sintering temperatures, cooling rate is 2 ℃/min, and air pressure is a standard atmospheric pressure, and the oxygen level in the temperature-fall period in the stove should meet following formula:
, PO wherein
2Be the volumn concentration of oxygen, a is a constant, and its value is 4～5, and b is a constant, and its value is 14000～15000; T is the absolute temperature of stove.
Power MnZn ferrite material by the inventive method preparation can have the 245kw/m of being lower than in the time of 45 ℃
3Power consumption, in the time of 25 ℃, have saturation magnetic flux density greater than 535mT.Preparation method provided by the invention has lower pre-burning and sintering temperature, and the ancillary component of interpolation is the coventional type particle, greatly reduces preparation cost, has simplified preparation technology.The high saturation magnetic flux density of preparing at last, the MnZn ferrite material that has super low-power consumption in the time of 45 ℃ are the good starting material of the main-transformer magnetic core in the switch power supply in the various digital products of preparation.
Embodiment 1:
1) starting material mix:
Choose 54mol%Fe
2O
3, the MnO of 33mol% and 13mol% ZnO as starting material, put into ball mill, the deionized water of weight such as adding, ball milling 2h, the mean particle size of the powder after requiring mix grinding good is controlled at 0.8 μ m, SiO
2Content be controlled at about 25ppm.
2) pre-burning:
The stove pre-burning is put in the material oven dry that mix grinding is good, and calcined temperature is 950 ℃, and the pre-burning time is 3h.
3) impurity adds:
Add ancillary component in pre-burned powder, these ancillary components comprise:
Table 1
| Numbering | CaCO 3 (ppm) | SiO 2 (ppm) | Co 2O 3 (ppm) | Bi 2O 3 (ppm) | Al 2O 3(ppm) | ZrO 2 (ppm) | HfO 2 (ppm) | TiO 2 (ppm) | SnO 2 (ppm) | V 2O 5 (ppm) | Nb 2O 5 (ppm) |
| 1 | 100 | 50 | 200 | 100 | 100 | 100 | 100 | 100 | 100 | 100 | 100 |
| 2 | 600 | 300 | 100 | 0 | 0 | 100 | 0 | 0 | 0 | 200 | 200 |
| 3 | 600 | 300 | 400 | 0 | 0 | 100 | 0 | 0 | 100 | 0 | 100 |
4) secondary ball milling:
The pre-imitation frosted glass that has added ancillary component is put into ball mill, the deionized water of weight such as adding, ball milling 3h, the mean particle size that makes pre-imitation frosted glass is 1.2 μ m.
5) moulding:
With the slurry oven dry, add the polyvinyl alcohol (PVA) of 10wt%, be pressed into external diameter: 29.5mm, internal diameter: 12.2mm and height: 4.5mm's is ring-like.
6) sintering:
Sintering is divided into intensification, insulation and cooling three phases.
Heat up: 1300 ℃ from room temperature to sintering temperature, heat-up rate is 3 ℃/min, and temperature-rise period carries out in air.
Insulation: sintering temperature is 1300 ℃, and sintering time is 3h, and the air pressure of sintering process is 1 normal atmosphere, and oxygen level is 5mol%, and all the other are N
2
Cooling: from 1300 ℃ to 200 ℃ of sintering temperatures, cooling rate is 2 ℃/min, and air pressure is a standard atmospheric pressure, and the oxygen level in the temperature-fall period in the stove meets following formula:
, PO wherein
2For volumn concentration, the T of oxygen is the absolute temperature of stove.
Use the SY-8232BH analyser to measure its power consumption number and saturation magnetic flux density on the sample ring that sinters, test result is shown in shown in the following table:
Table 2:
| Numbering | 45 ℃ of power consumption (kW/m 3) test condition: 100kHz, 200mT | 25 ℃ of saturation magnetic flux densities (mT) test condition: 1194A/m, 50Hz |
| 1 | 244 | 542 |
| 2 | 243 | 543 |
| 3 | 241 | 545 |
From the result that measures as can be seen, the sample ring of preparing all has little 245kW/m under 45 ℃ condition
3The super low-power consumption value, and the saturation magnetic flux density in the time of 25 ℃ all up to 535mT more than, so these materials can be good at satisfying the performance requriements of household digital equipment to magnetic core in the inner switch power supply main-transformer.
Embodiment 2:
1) starting material mix:
Choose 52mol%Fe
2O
3, the MnO of 40mol% and 8mol%ZnO be as starting material, puts into ball mill, the deionized water of weight such as adding, ball milling 5h, the mean particle size of the powder after requiring mix grinding good is controlled at 0.6 μ m, SiO
2Content be controlled at about 30ppm.
2) pre-burning:
The stove pre-burning is put in the material oven dry that mix grinding is good, and calcined temperature is 800 ℃, and the pre-burning time is 3h.
3) impurity adds:
Add ancillary component in pre-burned powder, these ancillary components comprise:
Table 3:
| Numbering | CaCO 3 (ppm) | SiO 2 (ppm) | Co 2O 3 (ppm) | Bi 2O 3 (ppm) | Al 2O 3 (ppm) | ZrO 2 (ppm) | HfO 2 (ppm) | TiO 2 (ppm) | SnO 2 (ppm) | V 2O 5 (ppm) | Nb 2O 5 (ppm) |
| 4 | 300 | 200 | 200 | 200 | 0 | 100 | 100 | 100 | 0 | 100 | 0 |
| 5 | 330 | 150 | 0 | 200 | 0 | 100 | 100 | 100 | 0 | 100 | 100 |
| 6 | 330 | 150 | 100 | 0 | 200 | 100 | 100 | 0 | 100 | 0 | 100 |
4) secondary ball milling:
The pre-imitation frosted glass that has added ancillary component is put into ball mill, the deionized water of weight such as adding, ball milling 6h, the mean particle size that makes pre-imitation frosted glass is 1.0 μ m.
5) moulding:
With the slurry oven dry, add the polyvinyl alcohol (PVA) of 10wt%, be pressed into external diameter: 29.5mm, internal diameter: 12.2mm and height: 4.5mm's is ring-like.
6) sintering:
Sintering is divided into intensification, insulation and cooling three phases.
Heat up: 1250 ℃ from room temperature to sintering temperature, heat-up rate is 3 ℃/min, and temperature-rise period carries out in air.
Insulation: sintering temperature is 1250 ℃, and sintering time is 6h, and the air pressure of sintering process is 1 normal atmosphere, and oxygen level is 3.0mol%, and all the other are N
2
Cooling: from 1250 ℃ to 200 ℃ of sintering temperatures, cooling rate is 2 ℃/min, and air pressure is a standard atmospheric pressure, and the oxygen level in the temperature-fall period in the stove meets following formula:
, PO wherein
2For volumn concentration, the T of oxygen is the absolute temperature of stove.
Use the SY-8232BH analyser to measure its power consumption number and saturation magnetic flux density on the sample ring that sinters, test result is shown in shown in the following table:
Table 4:
| Numbering | 45 ℃ of power consumption (kW/m 3) test condition: 100kHz, 200mT | 25 ℃ of saturation magnetic flux densities (mT) test condition: 1194A/m, 50Hz |
| 4 | 240 | 536 |
| 5 | 239 | 537 |
| 6 | 235 | 535 |
From the result that measures as can be seen, the sample ring of preparing all has little 245kW/m under 45 ℃ condition
3The super low-power consumption value, and the saturation magnetic flux density in the time of 25 ℃ all up to 535mT more than, so these materials can be good at satisfying the performance requriements of household digital equipment to magnetic core in the inner switch power supply main-transformer.
Claims (7)
1. a high saturation magnetic flux density, super low-power consumption MnZn ferrite material is characterized in that,
Fe
2O
3：52～54mol％；
MnO：33～40mol％；
ZnO：8～13mol％；
Auxiliary composition CaCO
3: 100～600ppm;
SiO
2：50～300ppm；
All the other are the auxiliary composition of metal oxide.
2. a kind of high saturation magnetic flux density according to claim 1, super low-power consumption MnZn ferrite material is characterized in that, the auxiliary composition of described metal oxide is A
2O
3, wherein A is a trivalent metallic element, at least from Co
3+, Al
3+, Bi
3+Middle selection is a kind of or unite interpolation, and its overall control is at 100～400ppm.
3. a kind of high saturation magnetic flux density according to claim 1, super low-power consumption MnZn ferrite material is characterized in that, the auxiliary composition of described metal oxide is BO
2, wherein B is a tetravalent, at least from Zr
4+, Hf
4+, Ti
4+And Sn
4+Middle selection is a kind of or unite interpolation, and its overall control is at 100～400ppm.
4. a kind of high saturation magnetic flux density according to claim 1, super low-power consumption MnZn ferrite material is characterized in that, the auxiliary composition of described metal oxide is M
2O
5, wherein M is the pentavalent transition metal, at least from V
5+, Nb
5+Middle selection is a kind of or unite interpolation, and its overall control is at 100～400ppm.
5. a kind of high saturation magnetic flux density according to claim 1, super low-power consumption MnZn ferrite material is characterized in that, described metal oxide is assisted composition A
2O
3, BO
2And M
2O
5Content should meet following formula: 0＜X+Y+Z≤1000ppm, wherein X, Y and Z represent A respectively
2O
3, BO
2And M
2O
5Content.
6. the preparation method of a high saturation magnetic flux density as claimed in claim 1, super low-power consumption MnZn ferrite material is characterized in that the step of method is:
1) starting material mix:
Choose 52～54mol%Fe
2O
3, the MnO of 33～40mol% and 8～13mol% ZnO as starting material, put into ball mill, the deionized water of weight such as adding, ball milling 2～5 hours, the mean particle size of the powder behind the mix grinding is controlled at 0.6～0.8 μ m, SiO
2Content be controlled at below the 30ppm;
2) pre-burning:
The stove pre-burning is put in the material oven dry that mix grinding is good, and calcined temperature is 800～950 ℃, and the pre-burning time is 2～4h;
3) auxiliary composition adds:
Contain 100～600ppm CaCO in the auxiliary composition that adds
3With 50～300ppm SiO
2, and the CaCO that adds
3And SiO
2Weight ratio be 1.5～2.2: 1;
4) secondary ball milling:
Material is put into ball mill, the deionized water of weight such as adding, ball milling 3～6h, the mean particle size that makes pre-imitation frosted glass is 1.0～1.2 μ m;
5) moulding:
With the slurry oven dry, add the polyvinyl alcohol of 10wt%, compression moulding;
6) sintering:
Sintering is divided into intensification, insulation and cooling three phases,
Heat up: 1250～1300 ℃ from room temperature to sintering temperature, heat-up rate is 3 ℃/min, and temperature-rise period carries out in air,
Insulation: sintering temperature is 1250～1300 ℃, and sintering time is 3～6h, and the air pressure of sintering process is 1 normal atmosphere, and oxygen level is 3.0～5.0mol%, and all the other are N
2,
Cooling: from 1250～1300 ℃ to 200 ℃ of sintering temperatures, cooling rate is 2 ℃/min, and air pressure is a standard atmospheric pressure, and the oxygen level in the temperature-fall period in the stove should meet following formula:
PO wherein
2Be the volumn concentration of oxygen, a is a constant, and its value is 4～5, and b is a constant, and its value is 14000～15000; T is the absolute temperature of stove.
7. the preparation method of a kind of high saturation magnetic flux density according to claim 6, super low-power consumption MnZn ferrite material is characterized in that, the auxiliary composition of described step 3) adds: except CaCO
3And SiO
2Outside also select A for use
2O
3, BO
2And M
2O
5Add as the auxiliary composition of oxide compound, wherein at A
2O
3In, A is a trivalent metallic element, at least from Co
3+, Al
3+, Bi
3+Middle selection is a kind of or unite interpolation, and its overall control is at 100～400ppm; At BO
2In, B is a tetravalent, at least from Zr
4+, Hf
4+, Ti
4+And Sn
4+Middle selection is a kind of or unite interpolation, and its overall control is at 100～400ppm; At M
2O
5In, M is the pentavalent transition metal, at least from V
5+, Nb
5+Middle selection is a kind of or unite interpolation, and its overall control is at 100～400ppm, and the summation of three class additions should be less than 1000ppm.
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