CN101106003A - Mn-Zn ferrite with ultrahigh magnetic conductivity and high Curie temperature and preparation method thereof - Google Patents
Mn-Zn ferrite with ultrahigh magnetic conductivity and high Curie temperature and preparation method thereof Download PDFInfo
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- CN101106003A CN101106003A CNA2006100524089A CN200610052408A CN101106003A CN 101106003 A CN101106003 A CN 101106003A CN A2006100524089 A CNA2006100524089 A CN A2006100524089A CN 200610052408 A CN200610052408 A CN 200610052408A CN 101106003 A CN101106003 A CN 101106003A
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- 229910000859 α-Fe Inorganic materials 0.000 title claims abstract description 41
- 238000002360 preparation method Methods 0.000 title claims abstract description 19
- 239000011701 zinc Substances 0.000 claims abstract description 52
- XLOMVQKBTHCTTD-UHFFFAOYSA-N Zinc monoxide Chemical compound [Zn]=O XLOMVQKBTHCTTD-UHFFFAOYSA-N 0.000 claims abstract description 36
- AMWRITDGCCNYAT-UHFFFAOYSA-L hydroxy(oxo)manganese;manganese Chemical compound [Mn].O[Mn]=O.O[Mn]=O AMWRITDGCCNYAT-UHFFFAOYSA-L 0.000 claims abstract description 18
- 239000011787 zinc oxide Substances 0.000 claims abstract description 18
- UQSXHKLRYXJYBZ-UHFFFAOYSA-N Iron oxide Chemical compound [Fe]=O UQSXHKLRYXJYBZ-UHFFFAOYSA-N 0.000 claims abstract description 17
- 229910000416 bismuth oxide Inorganic materials 0.000 claims abstract description 7
- 229910000476 molybdenum oxide Inorganic materials 0.000 claims abstract description 7
- 229910000484 niobium oxide Inorganic materials 0.000 claims abstract description 7
- URLJKFSTXLNXLG-UHFFFAOYSA-N niobium(5+);oxygen(2-) Chemical compound [O-2].[O-2].[O-2].[O-2].[O-2].[Nb+5].[Nb+5] URLJKFSTXLNXLG-UHFFFAOYSA-N 0.000 claims abstract description 7
- PQQKPALAQIIWST-UHFFFAOYSA-N oxomolybdenum Chemical compound [Mo]=O PQQKPALAQIIWST-UHFFFAOYSA-N 0.000 claims abstract description 7
- TYIXMATWDRGMPF-UHFFFAOYSA-N dibismuth;oxygen(2-) Chemical compound [O-2].[O-2].[O-2].[Bi+3].[Bi+3] TYIXMATWDRGMPF-UHFFFAOYSA-N 0.000 claims abstract description 6
- 238000001816 cooling Methods 0.000 claims description 25
- 238000005245 sintering Methods 0.000 claims description 24
- QVGXLLKOCUKJST-UHFFFAOYSA-N atomic oxygen Chemical compound [O] QVGXLLKOCUKJST-UHFFFAOYSA-N 0.000 claims description 22
- 239000001301 oxygen Substances 0.000 claims description 22
- 229910052760 oxygen Inorganic materials 0.000 claims description 22
- 230000035699 permeability Effects 0.000 claims description 19
- 239000002245 particle Substances 0.000 claims description 15
- 239000000203 mixture Substances 0.000 claims description 13
- 239000000292 calcium oxide Substances 0.000 claims description 10
- ODINCKMPIJJUCX-UHFFFAOYSA-N calcium oxide Inorganic materials [Ca]=O ODINCKMPIJJUCX-UHFFFAOYSA-N 0.000 claims description 10
- 239000004576 sand Substances 0.000 claims description 10
- 238000003801 milling Methods 0.000 claims description 9
- 239000010955 niobium Substances 0.000 claims description 9
- 238000002425 crystallisation Methods 0.000 claims description 7
- 230000008025 crystallization Effects 0.000 claims description 7
- 238000000465 moulding Methods 0.000 claims description 7
- 208000036366 Sensation of pressure Diseases 0.000 claims description 5
- 238000009413 insulation Methods 0.000 claims description 5
- 238000000034 method Methods 0.000 claims description 5
- 230000008569 process Effects 0.000 claims description 5
- 238000001694 spray drying Methods 0.000 claims description 5
- 229910010413 TiO 2 Inorganic materials 0.000 claims description 4
- MCMNRKCIXSYSNV-UHFFFAOYSA-N Zirconium dioxide Chemical compound O=[Zr]=O MCMNRKCIXSYSNV-UHFFFAOYSA-N 0.000 claims description 4
- BRPQOXSCLDDYGP-UHFFFAOYSA-N calcium oxide Chemical compound [O-2].[Ca+2] BRPQOXSCLDDYGP-UHFFFAOYSA-N 0.000 claims description 3
- XHCLAFWTIXFWPH-UHFFFAOYSA-N [O-2].[O-2].[O-2].[O-2].[O-2].[V+5].[V+5] Chemical compound [O-2].[O-2].[O-2].[O-2].[O-2].[V+5].[V+5] XHCLAFWTIXFWPH-UHFFFAOYSA-N 0.000 claims description 2
- 229910000449 hafnium oxide Inorganic materials 0.000 claims description 2
- WIHZLLGSGQNAGK-UHFFFAOYSA-N hafnium(4+);oxygen(2-) Chemical compound [O-2].[O-2].[Hf+4] WIHZLLGSGQNAGK-UHFFFAOYSA-N 0.000 claims description 2
- 229910003437 indium oxide Inorganic materials 0.000 claims description 2
- PJXISJQVUVHSOJ-UHFFFAOYSA-N indium(iii) oxide Chemical compound [O-2].[O-2].[O-2].[In+3].[In+3] PJXISJQVUVHSOJ-UHFFFAOYSA-N 0.000 claims description 2
- 238000002156 mixing Methods 0.000 claims description 2
- BPUBBGLMJRNUCC-UHFFFAOYSA-N oxygen(2-);tantalum(5+) Chemical compound [O-2].[O-2].[O-2].[O-2].[O-2].[Ta+5].[Ta+5] BPUBBGLMJRNUCC-UHFFFAOYSA-N 0.000 claims description 2
- WKMKTIVRRLOHAJ-UHFFFAOYSA-N oxygen(2-);thallium(1+) Chemical compound [O-2].[Tl+].[Tl+] WKMKTIVRRLOHAJ-UHFFFAOYSA-N 0.000 claims description 2
- 229910001936 tantalum oxide Inorganic materials 0.000 claims description 2
- 229910003438 thallium oxide Inorganic materials 0.000 claims description 2
- 229910001935 vanadium oxide Inorganic materials 0.000 claims description 2
- 238000005303 weighing Methods 0.000 claims description 2
- 239000013078 crystal Substances 0.000 abstract description 5
- JKQOBWVOAYFWKG-UHFFFAOYSA-N molybdenum trioxide Inorganic materials O=[Mo](=O)=O JKQOBWVOAYFWKG-UHFFFAOYSA-N 0.000 abstract 1
- ZKATWMILCYLAPD-UHFFFAOYSA-N niobium pentoxide Inorganic materials O=[Nb](=O)O[Nb](=O)=O ZKATWMILCYLAPD-UHFFFAOYSA-N 0.000 abstract 1
- NDLPOXTZKUMGOV-UHFFFAOYSA-N oxo(oxoferriooxy)iron hydrate Chemical compound O.O=[Fe]O[Fe]=O NDLPOXTZKUMGOV-UHFFFAOYSA-N 0.000 abstract 1
- CJJMLLCUQDSZIZ-UHFFFAOYSA-N oxobismuth Chemical compound [Bi]=O CJJMLLCUQDSZIZ-UHFFFAOYSA-N 0.000 abstract 1
- 238000012360 testing method Methods 0.000 description 12
- KBPLFHHGFOOTCA-UHFFFAOYSA-N 1-Octanol Chemical compound CCCCCCCCO KBPLFHHGFOOTCA-UHFFFAOYSA-N 0.000 description 6
- IJGRMHOSHXDMSA-UHFFFAOYSA-N Atomic nitrogen Chemical compound N#N IJGRMHOSHXDMSA-UHFFFAOYSA-N 0.000 description 6
- 238000010438 heat treatment Methods 0.000 description 6
- XEEYBQQBJWHFJM-UHFFFAOYSA-N iron Substances [Fe] XEEYBQQBJWHFJM-UHFFFAOYSA-N 0.000 description 4
- 229910000831 Steel Inorganic materials 0.000 description 3
- 239000000853 adhesive Substances 0.000 description 3
- 230000001070 adhesive effect Effects 0.000 description 3
- 239000013530 defoamer Substances 0.000 description 3
- 239000008367 deionised water Substances 0.000 description 3
- 229910021641 deionized water Inorganic materials 0.000 description 3
- 238000011161 development Methods 0.000 description 3
- 239000002270 dispersing agent Substances 0.000 description 3
- 238000001035 drying Methods 0.000 description 3
- 238000005469 granulation Methods 0.000 description 3
- 230000003179 granulation Effects 0.000 description 3
- 229910052757 nitrogen Inorganic materials 0.000 description 3
- 238000012856 packing Methods 0.000 description 3
- 238000012545 processing Methods 0.000 description 3
- 239000010959 steel Substances 0.000 description 3
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Chemical compound O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 description 3
- 230000008859 change Effects 0.000 description 2
- 238000005516 engineering process Methods 0.000 description 2
- 238000011160 research Methods 0.000 description 2
- 229910001289 Manganese-zinc ferrite Inorganic materials 0.000 description 1
- 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 description 1
- 230000001133 acceleration Effects 0.000 description 1
- 238000004891 communication Methods 0.000 description 1
- 238000012937 correction Methods 0.000 description 1
- 230000002950 deficient Effects 0.000 description 1
- 239000004615 ingredient Substances 0.000 description 1
- 239000000696 magnetic material Substances 0.000 description 1
- WJZHMLNIAZSFDO-UHFFFAOYSA-N manganese zinc Chemical class [Mn].[Zn] WJZHMLNIAZSFDO-UHFFFAOYSA-N 0.000 description 1
- 239000000463 material Substances 0.000 description 1
- 238000002844 melting Methods 0.000 description 1
- 238000012986 modification Methods 0.000 description 1
- 230000004048 modification Effects 0.000 description 1
- 229910052725 zinc Inorganic materials 0.000 description 1
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- Soft Magnetic Materials (AREA)
- Magnetic Ceramics (AREA)
Abstract
The invention provides a Mn-Zn ferrite with high magnetic conductivity and high Curie temperature; the ferrite contains main components including manganese oxide, zinc oxide and iron oxide, and auxiliary components added to the main components; bismuth oxide, molybdenum oxide, and niobium oxide; wherein the main components are as follows: manganese oxide calculated as MnO in an amount of 23 to 27 mol% and zinc oxide calculated as ZnO in an amount of 20 to 26 mol%; the balance of ferric oxide; the auxiliary components comprise the following components: 0 to 0.08 wt% (excluding zero) of Bi2Bismuth oxide calculated as O, 0 to 0.12% by weight (but not including zero) of MoO3Calculated molybdenum oxide and 0.01 to 0.1 wt.% (excluding zero) of Nb2O5Calculated niobium oxide; the crystal grain size of the Mn-Zn ferrite is 50-180 mu m; the initial magnetic conductivity of the Mn-Zn ferrite is 15000-18000 at 25 ℃, 10KHz and 0.25 mT; under the conditions of 100KHz and 0.25mT, the initial magnetic conductivity is 13000-15000, and the Curie temperature is more than or equal to 130 ℃; in addition, the invention provides a preparation method of the Mn-Zn ferrite.
Description
Technical field
The present invention relates to a kind of manganese-zinc ferrite and preparation method thereof, relate in particular to Mn-Zn ferrite of a kind of high magnetic permeability, high-curie temperature and preparation method thereof; Belong to the oxidate magnetic material technical field.
Background technology
High speed development along with electronics and information industries such as communication, computer, networks, and electronic devices and components miniaturization and light-weighted development trend, the high-permeability Mn-Zn ferrite can be widely used in magnetic core of transformer, noise filter, local area network (LAN) isolating transformer and digital network magnetic core of transformer, owing to can obviously reduce volume of transformer, reduce the wastage, so its research attention extremely both domestic and external.This Mn-Zn ferrite except magnetic permeability is wanted height, also requires it to have good frequency characteristic, high-curie temperature in actual applications on the market.Comprehensive raising combination property aspect has been transferred in the research in high magnetic permeability field from simple pursuit high magnetic permeability aspect, this is the development trend of current high magnetic conductivity ferrite.On this direction, major company has all made many effort both at home and abroad.TDK company model as Japan is H
5C
3The Mn-Zn ferrite and Japan FDK company model be
2H
15The ferritic magnetic permeability of Mn-Zn at 25 ℃, 10KHz can reach more than 15000 under the condition of 0.25mT, but the ferritic Curie temperature of this Mn-Zn has only about 100 ℃, this Mn-Zn ferrite then can't worked more than 100 ℃, so the ferritic range of application of this Mn-Zn is narrower.
Summary of the invention
The present invention is directed to the existing initial permeability of prior art, defective that Curie temperature is lower provides a kind of superhigh magnetic conductivity that has, Mn-Zn ferrite of high-curie temperature and preparation method thereof.
Above-mentioned technical problem of the present invention is implemented by the following technical programs; A kind of superhigh magnetic conductivity, high-curie temperature Mn-Zn ferrite is characterized in that the main component that this ferrite contains comprises manganese oxide, zinc oxide and iron oxide, contains the auxiliary element that adds in the main component and comprises; Bismuth oxide, molybdenum oxide and niobium oxide;
The component of wherein said main component is: contain 23～27 moles of % the manganese oxide that calculates by MnO, contain the zinc oxide that calculates by ZnO of 20～26 moles of %; All the other are iron oxide; The component of described auxiliary element is: 0～0.08 weight % (but do not comprise zero) presses Bi
2O
3The bismuth oxide that calculates, 0～0.12 weight % (but not comprising zero) press MoO
3Molybdenum oxide that calculates and 0.01～0.1 weight % (but not comprising zero) press Nb
2O
5The niobium oxide that calculates; The ferritic crystallization particle diameter of described Mn-Zn is 50～180 μ m.
Principal component of the present invention be controlled at 23～27 moles of % the manganese oxide that calculates by MnO, contain the zinc oxide that calculates by ZnO of 20～26 moles of %; All the other are in the scope of iron oxide, can improve Curie temperature, make the ferritic Curie temperature of the present invention reach 130 ℃.
Add bismuth oxide in the present invention, molybdenum oxide, niobium oxide, be since these three kinds all be low-melting material, at first can reduce sintering temperature, acceleration of sintering improves sintered density; Next MoO
3Existence can promote moving of grain boundary; At last, Nb
2O
5Existence can be when high temperature sintering crystal grain thinning, prevent the generation of excessive crystal grain, thereby obtain good micro-structural by uniting to add; Thereby can obtain superhigh magnetic conductivity, the crystallization particle diameter is 50～180 μ m, have the Mn-Zn ferrite than high-curie temperature.
In above-mentioned superhigh magnetic conductivity, high-curie temperature Mn-Zn ferrite, also comprise the calcium oxide of 0.005～0.6 weight % in the component of described auxiliary element by CaO calculating; Add calcium oxide and help improving magnetic permeability, reduce the wastage.
In above-mentioned superhigh magnetic conductivity, high-curie temperature Mn-Zn ferrite, also comprise in the component of described auxiliary element 0.04～0.3 weight % by V
2O
5The vanadium oxide that calculates, 0.001～0.3 weight % (but not comprising zero) press ZrO
2Calculate zirconia and 0.01～0.03 weight % press Ta
2O
5Calculate one or more of tantalum oxide; Add above-mentioned auxiliary element and help improving magnetic permeability, reduce the wastage.
In above-mentioned superhigh magnetic conductivity, high-curie temperature Mn-Zn ferrite, also comprise in the component of described auxiliary element 0.01～0.03 weight % by TiO
2The thallium oxide that calculates, 0.02～0.2 weight % press In
2O
3Indium oxide that calculates and 0.01～0.3 weight % press HfO
2One or more of the hafnium oxide that calculates; Add above-mentioned auxiliary element and help improving magnetic permeability, reduce the wastage.
As preferably, described superhigh magnetic conductivity, the ferritic crystallization particle diameter of high-curie temperature Mn-Zn are 60～150 μ m; More preferably; Described superhigh magnetic conductivity, the ferritic crystallization particle diameter of high-curie temperature Mn-Zn are 70～130 μ m.
Mn-Zn ferrite of the present invention is at 25 ℃, 10KHz, and under the condition of 0.25mT, initial permeability is 15000-18000; At 100KHz, under the condition of 0.25mT, initial permeability is 13000-15000, and Curie temperature is more than or equal to 130 ℃.
In addition, the present invention also provides a kind of superhigh magnetic conductivity, the ferritic preparation method of high-curie temperature Mn-Zn, may further comprise the steps:
(1) batching: adopt main component by 23～27 moles of % of component manganese oxide, 20～26 moles of % of zinc oxide, all the other are iron oxide; After weighing, adopt vibratory milling to do and mix;
(2) pre-burning: the above-mentioned composition of doing after mixing is carried out pre-burning, add auxiliary element after the pre-burning, carry out sand milling;
(3) moulding: through the particle that spray drying is made 80～200 μ m that passes through behind the sand milling, be shaped to blank then with definite shape with above-mentioned;
(4) sintering: the blank after the above-mentioned moulding is carried out sintering, temperature controlled processes during sintering is: programming rate is 100～120 ℃/hour during from room temperature to 600 ℃, programming rate is 120～150 ℃/hour during from 600 ℃ to 900 ℃, programming rate is 120～150 ℃/hour from 900 ℃ to 1250 ℃, from 1250 ℃ to 1350 ℃～and 1450 ℃ of programming rates are 300～400 ℃/hour; In 1350 ℃～1450 ℃ insulations cooling after 3～8 hours, from 180～300 ℃/hour of 1350 ℃～1450 ℃ to 1250 ℃ cooling rates, cooling rate is 120～180 ℃/hour from 1250 ℃ to 900 ℃, cooling rate is 100～120 ℃/hour from 900 ℃ to 600 ℃, from 600 ℃～to 60～100 ℃/hour of room temperature cooling rates; Promptly form wideband low-loss high-permeability Mn-Zn ferrite behind the sintering.
Adopt preparation method of the present invention to improve the ferritic density of Mn-Zn, improved the ferritic apparent dimension structure of Mn-Zn, thereby improved the ferritic magnetic permeability of Mn-Zn, reduce the wastage.
In superhigh magnetic conductivity of the present invention, the ferritic preparation method of high-curie temperature Mn-Zn, be 800 ℃～900 ℃ at the calcined temperature described in the step (2), the pre-burning time is 1～3 hour.
In superhigh magnetic conductivity of the present invention, the ferritic preparation method of high-curie temperature Mn-Zn, temperature rise period ℃ is carried out sintering from room temperature to 600 air during sintering in step (4), from 600 to 1250 ℃ are carried out sintering 5%～21% partial pressure of oxygen, from 1250 to 1400 ℃ are carried out sintering the 0.001-5% partial pressure of oxygen; The holding stage partial pressure of oxygen is at 3.8-20%; Temperature-fall period carries out equilibrium oxygen partial pres-sure from 1400 ℃ to 800 ℃, from 800 ℃ to the N of room temperature partial pressure of oxygen below 50PPM
2In carry out.
Therefore the present invention compared with prior art has the following advantages:
(1) controlled the content of principal component in the composition of the present invention, thereby and added in principal component that an amount of special auxiliary element obtains having superhigh magnetic conductivity, the Mn-Zn ferrite of high-curie temperature.
(2) not only cost is lower, technology is simple for preparation method of the present invention; And strict control temperature curve and carry out atmosphere protection, thereby prepare at 25 ℃, 10KHz, under the condition of 0.25mT, initial permeability is 15000-18000; At 100KHz, under the condition of 0.25mT, initial permeability is 13000-15000, and Curie temperature is more than or equal to 130 ℃ Mn-Zn ferrite.
Embodiment
Below be the specific embodiment of the present invention, technical characterictic of the present invention is described further, but the present invention is not limited to these embodiment.
Embodiment 1
With Fe
2O
3(53.5 moles of %), ZnO (21 moles of %) and MnO (25.5 moles of %) prepare burden, mixed 30 minutes by force as main component, vibrate 30 minutes, and the mixture that obtains is put into rotary kiln 800 ℃ of pre-burnings 3 hours.The calcined body of gained adds auxiliary element shown in table 1～3: add the dispersant pla-pcl with respect to the percentage by weight of ferrite composition: 0.3-0.6wt%, deionized water 80-180wt%, adhesive PVA:0.8-1.2wt%, defoamer n-octyl alcohol: 0.1-0.4wt%, steel ball 400-750 wt%; Carried out sand milling 70 minutes in sand mill, the slip particle diameter is controlled at 0.8～1.2 micron, and then, adding PVA therein and becoming average grain diameter by spray drying granulation is the particle of 80～200 μ m; Adopting automatic moulding machine to become the blank external diameter at the pressure compacted under of 7～11Mpa is 25mm, and internal diameter is 15mm, and height is the sample ring of 6-8.5mm; By heating, 1350 ℃ of insulations 8 hours, during sintering at strictness control temperature curve with carry out atmosphere protection, grind packing warehouse-in after processing, cleaning-drying, the test go-on-go at last.
The temperature curve of embodiment 1:
Heating process:
Programming rate from room temperature to 600 ℃: 100 ℃/hour;
Programming rate from 600 ℃ to 900 ℃: 120 ℃/hour;
Programming rate from 900 ℃ to 1250 ℃: 150 ℃/hour;
Programming rate from 1250 ℃ to 1350 ℃: 300 ℃/hour;
Temperature keeps operation:
Kept 8 hours at 1350 ℃;
Cooling process
Cooling rate from 1350 ℃ to 1250 ℃: 180 ℃/hour;
Cooling rate from 1250 ℃ to 900 ℃: 120 ℃/hour;
Cooling rate from 900 ℃ to 600 ℃: 100 ℃/hour;
Cooling rate from 600 ℃ to room temperature: 60 ℃/hour;
The atmosphere protection of embodiment 1
Temperature rise period:
Atmosphere protection from room temperature to 600 ℃: carry out the air;
Atmosphere protection from 600 ℃ to 1250 ℃: 21% partial pressure of oxygen;
Atmosphere protection from 1250 ℃ to 1350 ℃: 5% partial pressure of oxygen;
Holding stage is 20% partial pressure of oxygen;
Temperature-fall period: from 1350 ℃ to 800 ℃ atmosphere protection: equilibrium oxygen partial pres-sure;
Atmosphere protection from 800 ℃ to room temperature: carry out the nitrogen below the 50PPM.；
Respectively at 10KHz, 0.25mT at 100KHz, tests μ under the 0.25mT after coming out of the stove
i, it is as shown in table 1 to survey Curie temperature Tc. test result simultaneously:
Three kinds of auxiliary elements are to the influence of magnetic property among table 1: the embodiment 1
| Auxiliary element (wt%) | μ i | Tc | ||||
| Bi 2O 3 | MoO 3 | Nb 2O 5 | 10KHz | 100KHz | ||
| Sample 1 | 0.01 | 0.02 | 0.01 | 16500 | 13000 | 131 |
| Sample 2 | 0.02 | 0.08 | 0.01 | 15500 | 13500 | 130.5 |
| Sample 3 | 0.03 | 0.02 | 0 | 14500 | 13000 | 130 |
| Sample 4 | 0.02 | 0.05 | 0.015 | 17000 | 14500 | 131 |
| Sample 5 | 0.08 | 0.01 | 0.01 | 16000 | 13500 | 132 |
| Sample 6 | 0.035 | 0.03 | 0.015 | 16500 | 14000 | 132 |
| Sample 7 * | 0.05 | 0.015 | 0 | 13000 | 9000 | 132 |
| Sample 8 * | 0.05 | 0.03 | 0.08 | 17000 | 13500 | 130 |
| Sample 9 * | 0.01 | 0.12 | 0 | 13500 | 10500 | 131 |
| Sample 10 * | 0.01 | 0.02 | 0.1 | 17500 | 13000 | 132 |
In the composition of above-mentioned ferrite in manganese zinc series, main component contains the Bi that calculates by weight 400ppm as auxiliary element relatively
2O
3, 600ppm MoO
3, 500ppm Nb
2O
5, it is as shown in table 2 to contain auxiliary element simultaneously, obtains sample 11～16 according to above-mentioned preparation method, and the average diameter of sample crystal grain is 50～180 μ m.
Following four kinds of auxiliary elements are to the influence of ferrite performance among table 2: the embodiment 1
| Auxiliary element content (weight %) | μ i | Tc(℃) | |||||
| CaO | V 2O 5 | ZrO 2 | Ta 2O 5 | 10KHz | 100KHz | ||
| Sample 11 | 0.005 | 0.30 | 0.3 | 0 | 16000 | 14000 | 130.5 |
| Sample 12 | 0.015 | 0.18 | 0.12 | 0 | 16500 | 14500 | 131 |
| Sample 13 | 0.12 | 0.08 | 0.008 | 0.01 | 17000 | 15000 | 132 |
| Sample 14 | 0.6 | 0 | 0.006 | 0.02 | 17500 | 15000 | 131 |
| Sample 15 | 0.048 | 0.12 | 0.004 | 0.02 | 18000 | 15000 | 132 |
| Sample 16 | 0.36 | 0.08 | 0 | 0.03 | 16500 | 14500 | 131 |
By the result of table 2 CaO as can be seen, V
2O
5, ZrO
2And Ta
2O
5Interpolation can improve ferritic magnetic permeability of Mn-Zn and Curie temperature.
In the ferritic composition of above-mentioned Mn-Zn, main component contains the Bi that calculates by weight 300ppm as auxiliary element relatively
2O
3, 500ppm MoO
3, 600ppm Nb
2O
5, contain the CaO of accessory ingredient 150ppm, the V of 200ppm simultaneously
2O
5, 500ppm ZrO
2, 600ppm Ta
2O
5As shown in table 3 with a certain amount of following auxiliary element, obtain sample 17～22 according to above-mentioned preparation method, the average diameter of sample crystal grain is 60～150 μ m.
Following three kinds of auxiliary elements are to the influence of ferrite performance among table 3: the embodiment 1
| Auxiliary element content (weight %) | μ i | Tc(℃) | ||||
| TiO 2 | In 2O 3 | HfO 2 | 10KHz | 100KHz | ||
| Sample 17 | 0.01 | 0 | 0.3 | 16500 | 14000 | 132 |
| Sample 18 | 0 | 0.2 | 0 | 15500 | 13500 | 132 |
| Sample 19 | 0.01 | 0.02 | 0.08 | 16000 | 14000 | 131 |
| Sample 20 | 0.02 | 0.12 | 0.12 | 16500 | 13500 | 130 |
| Sample 21 | 0 | 0.08 | 0.24 | 17000 | 14000 | 131 |
| Sample 22 | 0.03 | 0 | 0 | 16000 | 13500 | 131.5 |
Embodiment 2
With Fe
2O
3(51 moles of %), ZnO (23 moles of %) and MnO (26 moles of %) prepare burden, mixed 30 minutes by force as main component, vibrate 30 minutes, and the mixture that obtains is put into rotary kiln 850 ℃ of pre-burnings 2 hours.It is as shown in table 4 that the calcined body of gained adds auxiliary element: add the dispersant pla-pcl with respect to the percentage by weight of ferrite composition: 0.3-0.6wt%, deionized water 80-180wt%, adhesive PVA:0.8-1.2wt%, defoamer n-octyl alcohol: 0.1-0.4 wt%, steel ball 400-750wt%; Carried out sand milling 70 minutes in sand mill, the slip particle diameter is controlled at 0.8～1.2 micron, and adding PVA then therein and becoming average grain diameter by spray drying granulation is the particle of 80～200 μ m; Adopting automatic moulding machine to become the blank external diameter at the pressure compacted under of 7～11Mpa is 25mm, and internal diameter is 15mm, and height is the sample ring of 6-8.5mm; By heating, 1400 ℃ of insulations 5 hours, during sintering at strictness control temperature curve with carry out atmosphere protection, grind packing warehouse-in after processing, cleaning-drying, the test go-on-go at last.
The temperature curve of embodiment 2:
Heating process:
Programming rate from room temperature to 600 ℃: 110 ℃/hour;
Programming rate from 600 ℃ to 900 ℃: 140 ℃/hour;
Programming rate from 900 ℃ to 1250 ℃: 160 ℃/hour;
Programming rate from 1250 ℃ to 1400 ℃: 350 ℃/hour;
Temperature keeps operation:
Kept 5 hours at 1400 ℃;
Cooling process
Cooling rate from 1400 ℃ to 1250 ℃: 250 ℃/hour;
Cooling rate from 1250 ℃ to 900 ℃: 150 ℃/hour;
Cooling rate from 900 ℃ to 600 ℃: 110 ℃/hour;
Cooling rate from 600 ℃ to room temperature: 80 ℃/hour;
The atmosphere protection of embodiment 2
Temperature rise period:
Atmosphere protection from room temperature to 600 ℃: carry out the air;
Atmosphere protection from 600 ℃ to 1250 ℃: 10% partial pressure of oxygen;
Atmosphere protection from 1250 ℃ to 1400 ℃: 2% partial pressure of oxygen;
Holding stage is 10% partial pressure of oxygen;
Temperature-fall period
Atmosphere protection from 1400 ℃ to 800 ℃: equilibrium oxygen partial pres-sure;
Atmosphere protection from 800 ℃ to room temperature: carry out the nitrogen below the 50PPM.；
Respectively at 10KHz, 0.25mT at 100KHz, tests μ under the 0.25mT after coming out of the stove
i, it is as shown in table 5 to survey Curie temperature Tc. test result simultaneously
Auxiliary element content in the sample of table 4: embodiment 2
| Auxiliary element content (weight %) | |||||||
| Bi 2O 3 | MoO 3 | Nb 2O 5 | CaO | ZrO 2 | TiO 2 | HfO 2 | |
| Sample 23 | 0.01 | 0.12 | 0.01 | 0.01 | 0.02 | 0.01 | |
| Sample 24 | 0.02 | 0.08 | 0.04 | 0.02 | 0.03 | 0.03 | 0.05 |
| Sample 25 | 0.03 | 0.06 | 0.02 | 0.06 | 0.01 | 0.10 | |
| Sample 26 | 0.05 | 0.01 | 0.06 | 0.03 | 0.20 | 0.20 | |
| Sample 27 | 0.04 | 0.05 | 0.08 | 0.02 | 0.02 | 0.02 | 0.30 |
| Sample 28 | 0.08 | 0.02 | 0.10 | 0.03 | 0.01 | 0.10 | |
For each sample, respectively at 10KHz, 0.25mT, at 100KHz, 0.25mT is test μ down
i, survey Curie temperature Tc simultaneously, the results are shown in table 5.
Magnetic property in the sample of table 5: embodiment 2
| Magnetic permeability | Tc(℃) | ||
| 10kHz | 100kHz | ||
| Sample 23 | 15500 | 13500 | 130.5 |
| Sample 24 | 16000 | 14000 | 131 |
| Sample 25 | 16500 | 13000 | 131.5 |
| Sample 26 | 15500 | 13500 | 131 |
| Sample 27 | 17000 | 14500 | 130.5 |
| Sample 28 | 16500 | 13500 | 131 |
Embodiment 3
With Fe
2O
3(53 moles of %), ZnO (27 moles of %) and MnO (20 moles of %) prepare burden, mixed 30 minutes by force as main component, vibrate 30 minutes, and the mixture that obtains is put into rotary kiln 900 ℃ of pre-burnings 1 hour.It is as shown in table 6 that the calcined body of gained adds auxiliary element: add the dispersant pla-pcl with respect to the percentage by weight of ferrite composition: 0.3-0.6wt%, deionized water 80-180wt%, adhesive PVA:0.8-1.2wt%, defoamer n-octyl alcohol: 0.1-0.4wt%, steel ball 400-750wt%; Carried out sand milling 70 minutes in sand mill, the slip particle diameter is controlled at 0.8～1.2 micron, and adding PVA then therein and becoming average grain diameter by spray drying granulation is the particle of 80～200 μ m; Adopting automatic moulding machine to become the blank external diameter at the pressure compacted under of 7～11Mpa is 25mm, and internal diameter is 15mm, and height is the sample ring of 6-8.5mm; By heating, 1450 ℃ of insulations 3 hours, during sintering at strictness control temperature curve with carry out atmosphere protection, grind packing warehouse-in after processing, cleaning-drying, the test go-on-go at last.
The temperature curve of embodiment 2:
Heating process:
Programming rate from room temperature to 600 ℃: 120 ℃/hour;
Programming rate from 600 ℃ to 900 ℃: 150 ℃/hour;
Programming rate from 900 ℃ to 1250 ℃: 180 ℃/hour;
Programming rate from 1250 ℃ to 1450 ℃: 400 ℃/hour;
Temperature keeps operation:
Kept 3 hours at 1450 ℃;
Cooling process
Cooling rate from 1450 ℃ to 1250 ℃: 300 ℃/hour;
Cooling rate from 1250 ℃ to 900 ℃: 180 ℃/hour;
Cooling rate from 900 ℃ to 600 ℃: 120 ℃/hour;
Cooling rate from 600 ℃ to room temperature: 100 ℃/hour;
The atmosphere protection of embodiment 2
Temperature rise period:
Atmosphere protection from room temperature to 600 ℃: carry out the air;
Atmosphere protection from 600 ℃ to 1250 ℃: 5% partial pressure of oxygen;
Atmosphere protection from 1250 ℃ to 1450 ℃: 0.1% partial pressure of oxygen;
Holding stage is 3.8% partial pressure of oxygen;
Temperature-fall period
Atmosphere protection from 1450 ℃ to 800 ℃: equilibrium oxygen partial pres-sure;
Atmosphere protection from 800 ℃ to room temperature: carry out the nitrogen below the 50PPM.；
Respectively at 10KHz, 0.25mT at 100KHz, tests μ under the 0.25mT after coming out of the stove
i, it is as shown in table 7 to survey Curie temperature Tc. test result simultaneously
Auxiliary element content in the sample of table 6: embodiment 3
| Auxiliary element content (weight %) | |||||||
| Bi 2O 3 | MoO 3 | Nb 2O 5 | CaO | V 2O 5 | Ta 2O 5 | In 2O 3 | |
| Sample 23 | 0.02 | 0.10 | 0.02 | 0.04 | 0.01 | 0.18 | |
| Sample 24 | 0.01 | 0.12 | 0.05 | 0.01 | 0.02 | ||
| Sample 25 | 0.04 | 0.08 | 0.01 | 0.03 | 0.08 | 0.03 | 0.10 |
| Sample 26 | 0.03 | 0.06 | 0.03 | 0.05 | 0.10 | 0.30 | |
| Sample 27 | 0.06 | 0.02 | 0.07 | 0.20 | 0.02 | 0.01 | |
| Sample 28 | 0.05 | 0.01 | 0.08 | 0.02 | 0.30 | 0.01 | 0.05 |
For each sample, respectively at 10KHz, 0.25mT, at 100KHz, 0.25mT is test μ down
i, survey Curie temperature Tc simultaneously, the results are shown in table 7.
Magnetic property in the sample of table 7: embodiment 3
| Magnetic permeability | Tc(℃) | ||
| 10kHz | 100kHz | ||
| Sample 23 | 16000 | 14000 | 131 |
| Sample 24 | 15500 | 13500 | 132 |
| Sample 25 | 17000 | 14000 | 130.5 |
| Sample 26 | 17500 | 14500 | 130 |
| Sample 27 | 16500 | 13500 | 131 |
| Sample 28 | 16000 | 13000 | 132 |
Embodiment 4
Component in the table 8 is prepared burden as main component, and relative main component contains as auxiliary element to be calculated by weight promptly: Bi
2O
3(0.02wt%), MoO
3(0.02wt%), Nb
2O
5(0.15wt%), then change Fe
2O
3, MnO, ZnO, the ratio between the three is prepared the Mn-Zn ferrite with the preparation method identical with embodiment 2, respectively at 10KHz, 0.25mT, at 100KHz, 0.25mT is test μ down
i, survey Curie temperature Tc simultaneously, the results are shown in table 8:
The magnetic property of the change sample of three kinds of principal component components among table 8: the embodiment 4
| Main component | μ i | Tc | ||||
| Fe 2O 3 | MnO | ZnO | 10KHz | 100KHz | ||
| Sample 29 | 53.5 | 21.5 | 26 | 17000 | 14500 | 131 |
| Sample 30 | 54 | 22 | 24 | 15500 | 13500 | 133 |
| Sample 31 | 53 | 21.5 | 26.5 | 17500 | 14500 | 130 |
| Sample 32 | 53.5 | 23 | 23.5 | 15600 | 13200 | 132 |
| Sample 33 | 53.2 | 22.5 | 24.4 | 16000 | 14200 | 130 |
Specific embodiment described in the present invention only is that the present invention's spirit is illustrated.The technical staff of the technical field of the invention can make various modifications or replenishes or adopt similar mode to substitute described specific embodiment, but can't depart from spirit of the present invention or surmount the defined scope of appended claims.
Although the present invention has been made detailed explanation and has quoted some instantiations as proof, to those skilled in the art, only otherwise leave that the spirit and scope of the present invention can be done various variations or correction is obvious.
Claims (12)
1. a superhigh magnetic conductivity, high-curie temperature Mn-Zn ferrite is characterized in that the main component that this ferrite contains comprises manganese oxide, zinc oxide and iron oxide, contains the auxiliary element that adds in the main component and comprises; Bismuth oxide, molybdenum oxide and niobium oxide;
The component of wherein said main component is: contain 23～27 moles of % the manganese oxide that calculates by MnO, contain the zinc oxide that calculates by ZnO of 20～26 moles of %; All the other are iron oxide; The component of described auxiliary element is: 0～0.08 weight % (but do not comprise zero) presses Bi
2O
3The bismuth oxide that calculates, 0～0.12 weight % (but not comprising zero) press MoO
3Molybdenum oxide that calculates and 0.01～0.1 weight % (but not comprising zero) press Nb
2O
5The niobium oxide that calculates; The ferritic crystallization particle diameter of described Mn-Zn is 50～180 μ m.
2. a kind of superhigh magnetic conductivity according to claim 1, high-curie temperature Mn-Zn ferrite is characterized in that also comprising in the component of described auxiliary element the calcium oxide that calculates by CaO of 0.005～0.6 weight %.
3. a kind of superhigh magnetic conductivity according to claim 1, high-curie temperature Mn-Zn ferrite, it is characterized in that also comprising in the component of described auxiliary element 0.04～0.3 weight % by V
2O
5The vanadium oxide that calculates, 0.001～0.3 weight % (but not comprising zero) press ZrO
2Calculate zirconia and 0.01～0.03 weight % press Ta
2O
5Calculate one or more of tantalum oxide.
4. a kind of superhigh magnetic conductivity according to claim 1, high-curie temperature Mn-Zn ferrite, it is characterized in that also comprising in the component of described auxiliary element 0.01～0.03 weight % by TiO
2The thallium oxide that calculates, 0.02～0.2 weight % press In
2O
3Indium oxide that calculates and 0.01～0.3 weight % press HfO
2One or more of the hafnium oxide that calculates.
5. a kind of superhigh magnetic conductivity according to claim 1, high-curie temperature Mn-Zn ferrite is characterized in that the ferritic crystallization particle diameter of described Mn-Zn is 60～150 μ m.
6. a kind of superhigh magnetic conductivity according to claim 1, high-curie temperature Mn-Zn ferrite is characterized in that the ferritic crystallization particle diameter of described Mn-Zn is 70～130 μ m.
7. according to the described a kind of superhigh magnetic conductivity of claim 1～6, high-curie temperature Mn-Zn ferrite, it is characterized in that this Mn-Zn ferrite at 25 ℃, 10KHz, under the condition of 0.25mT, initial permeability is 15000-18000; At 100KHz, under the condition of 0.25mT, initial permeability is 13000-15000, and Curie temperature is more than or equal to 130 ℃.
8. a superhigh magnetic conductivity, the ferritic preparation method of high-curie temperature Mn-Zn may further comprise the steps:
(1) batching: adopt main component by 23～27 moles of % of component manganese oxide, 20～26 moles of % of zinc oxide, all the other are iron oxide; After weighing, adopt vibratory milling to do and mix;
(2) pre-burning: the above-mentioned composition of doing after mixing is carried out pre-burning, add auxiliary element after the pre-burning, carry out sand milling;
(3) moulding: through the particle that spray drying is made 80～200 μ m that passes through behind the sand milling, be shaped to blank then with definite shape with above-mentioned;
(4) sintering: the blank after the above-mentioned moulding is carried out sintering, temperature controlled processes during sintering is: programming rate is 100～120 ℃/hour during from room temperature to 600 ℃, programming rate is 120～150 ℃/hour during from 600 ℃ to 900 ℃, programming rate is 120～150 ℃/hour from 900 ℃ to 1250 ℃, from 1250 ℃ to 1350 ℃～and 1450 ℃ of programming rates are 300～400 ℃/hour; In 1350 ℃～1450 ℃ insulations cooling after 3～8 hours, from 180～300 ℃/hour of 1350 ℃～1450 ℃ to 1250 ℃ cooling rates, cooling rate is 120～180 ℃/hour from 1250 ℃ to 900 ℃, cooling rate is 100～120 ℃/hour from 900 ℃ to 600 ℃, from 600 ℃～to 60～100 ℃/hour of room temperature cooling rates; Promptly form wideband low-loss high-permeability Mn-Zn ferrite behind the sintering.
9. a kind of superhigh magnetic conductivity according to claim 8, the ferritic preparation method of high-curie temperature Mn-Zn is characterized in that the calcined temperature described in the step (2) is 800 ℃～900 ℃, and the pre-burning time is 1～3 hour.
10. according to Claim 8 or 9 described a kind of superhigh magnetic conductivities, the ferritic preparation method of high-curie temperature Mn-Zn, the temperature rise period ℃ is carried out sintering from room temperature to 600 when it is characterized in that in the step (4) sintering air, from 600 to 1250 ℃ are carried out sintering 5%～21% partial pressure of oxygen, from 1250 to 1400 ℃ are carried out sintering the 0.001-5% partial pressure of oxygen.
11. the holding stage partial pressure of oxygen is at 3.8-20% when according to Claim 8 or 9 described a kind of superhigh magnetic conductivities, the ferritic preparation method of high-curie temperature Mn-Zn, it is characterized in that in the step (4) sintering.
12. according to Claim 8 or 9 described a kind of superhigh magnetic conductivities, the ferritic preparation method of high-curie temperature Mn-Zn, temperature-fall period carries out equilibrium oxygen partial pres-sure from 1400 ℃ to 800 ℃ when it is characterized in that in the step (4) sintering, from 800 ℃ to the N of room temperature partial pressure of oxygen below 50PPM
2In carry out.
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