CN102329129B - Nickel-copper-zinc ferrite material with high surface resistance for panel display - Google Patents
Nickel-copper-zinc ferrite material with high surface resistance for panel display Download PDFInfo
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- CN102329129B CN102329129B CN 201110166394 CN201110166394A CN102329129B CN 102329129 B CN102329129 B CN 102329129B CN 201110166394 CN201110166394 CN 201110166394 CN 201110166394 A CN201110166394 A CN 201110166394A CN 102329129 B CN102329129 B CN 102329129B
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- nickel
- copper
- ferrite material
- zinc ferrite
- surface resistance
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Abstract
The invention discloses a nickel-copper-zinc ferrite material with high surface resistance for panel display, which is made of primary components and auxiliary components. The primary components consist of the following substances: 49.00-50.00 mol% of Fe2O3 (ferric oxide), 27.50-28.10 mol% of ZnO (zinc oxide), 4.85-4.95 mol% of CuO (cupric oxide) and NiO (nickel oxide) as the rest, and by using the sum of the masses of all the primary components, the auxiliary components comprise 0.01-0.03 wt% of TiO2 (titanium dioxide), 0.01-0.04 wt% of SnO2 (stannic oxide), 0.01-0.04 wt% of V2O5 (vanadium pentoxide) and 0.1-0.5 wt% of ZrO2 (zirconium dioxide). The nickel-copper-zinc ferrite material has the surface resistance which is not less than 320000 megohms, the room-temperature power consumption which is lower than 250 kw/m3, the high-temperature power consumption which is lower than 180 kw/m3 and the room-temperature saturated magnetic flux density which is more than 400 mT.
Description
Technical field
The invention belongs to the technical field of soft magnetic ferrite in the electronic material, relate to specifically a kind of nickel-copper-zinc ferrite material with high surface resistance for panel display.
Background technology
The development of the flat panel display take liquid crystal display as representative has proposed many Secretaries to power ferrite material and magnetic core thereof.Not only require material to possess the required low-power consumption characteristic of common power ferrite material, also require this Ferrite Material to possess high voltage withstanding performance, at present normal operation MnZn power ferrite material.Extra normal development along with large-sized FPD, under the dual promotion that reduces cost and energy-conservation requirement, the designing technique of LCD backlight source inverter has broken through the pattern that a traditional lamp is joined a transformer, develop two lamps rapidly and joined the new model of a transformer, and this new model requires the sheet resistance of inverter core material higher, original MnZn Ferrite Material that usually adopts is because sheet resistance usually about 100k Ω, can not satisfy this requirement.For this reason, need exploitation not only to possess the high saturation magnetic flux density of power ferrite, low-loss general characteristic, also have simultaneously extra high sheet resistance, make transformer under the high output voltage more than the 2000V, also can obtain high reliability, puncture the difficult problem of sparking to solve transformer high-voltage.It has catered to the up-to-date science and technology of flat panel display development on the one hand to the new demand of power ferrite material, has also guided on the other hand the developing direction of this field Ferrite Material.
Summary of the invention
The object of the present invention is to provide a kind of not only have high saturation magnetic flux density, low-loss, also have simultaneously a kind of flat panel display high surface resistance NiZn Ferrite Material of extra high sheet resistance.
For solving the problems of the technologies described above, technical scheme of the present invention is:
A kind of nickel-copper-zinc ferrite material with high surface resistance for panel display is made by principal component and accessory ingredient; Described principal component is comprised of following material: the Fe of 49.00～50.00mol%
2O
3, the CuO of ZnO, 4.85～4.95mol% of 27.50～28.10mol% and the NiO of surplus; Take the quality sum of all principal components as benchmark, described accessory ingredient comprises the TiO of 0.01～0.03wt%
2, the SnO of 0.01～0.04wt%
2, the V of 0.01～0.04wt%
2O
5, the ZrO of 0.1～0.5wt%
2The inventor thinks, accessory ingredient SnO
2And TiO
2After the adding, Sn
4+And Ti
4+Ion dissolves in spinel crystal structure B position, forms Sn
4+-Fe
2+And Ti
4+-Fe
2+Stablize duplet, can effectively suppress Fe
3+With Fe
2+Between electron transition, improve the grain resistance rate (R of material
g); The ZrO that adds
2And V
2O
5Main segregation forms resistive formation at grain boundaries, improves the grain boundary resistance rate (R of material
G.b), and all-in resistance rate R is by grain boundary resistance rate (R
G.b) and grain resistance rate (R
g) form, so SnO
2, TiO
2, ZrO
2And V
2O
5The affiliation that adds make all-in resistance rate (R=R
g+ R
G, b) increase.In addition, because Ti
4+And Sn
4+Ion incorporates in the crystal structure, has formed stable Fe
2+-Sn
4+Duplet has compensated crystal anisotropy constant K, makes the total anisotropy constant K of material trend towards zero, thus so that initial permeability increase.
As a kind of improvement of the present invention, take the quality sum of all principal components as benchmark, described accessory ingredient also comprises the SiO of 0.01～0.03wt%
2, 0.01～0.04wt% CaO.The inventor thinks, CaO and SiO
2But the densification degree of adding acceleration of sintering body, improve sintered density, and SiO
2With V
2O
5Cooperative effect is arranged, can form an amount of amount of liquid phase, can not only promote the growth of crystal grain, and in sintering process, help good microstructural formation.
As another kind of improvement the of the present invention, take the quality sum of all principal components as benchmark, described accessory ingredient also comprises the MnO of 0.10～0.65wt%
2The inventor thinks, MnO
2Can enter lattice, regulate magnetic property, improve magnetic permeability, reduce power loss.
The sheet resistance of described nickel-copper-zinc ferrite material with high surface resistance for panel display is not less than 320000M Ω.
Plate of the present invention shows the preparation method with nickel-copper-zinc ferrite material with high surface resistance, adopts the preparation method of this area routine to get final product, and specifically can comprise the steps:
(1) batching: the mole proportioning according to principal component is prepared burden;
(2) ball millings: with the ball grinder wet-milling in ball mill of packing into of above-mentioned principal component.Ball-milling Time is 30～40 minutes, and rotary speed is 400～600r/min;
(3) pre-burning: the powder that ball milling is good is put into resistance furnace and is carried out pre-burning, 800～900 ℃ of calcined temperatures, and temperature retention time is 1～4h;
(4) secondary ball milling and mix accessory ingredient: powder that will be pre-burned and load weighted accessory ingredient are put into ball grinder and are carried out wet-milling, and Ball-milling Time is 2～3h, and rotary speed is 400～600r/min;
(5) granulation: add certain organic solution and the processing of sieving to secondary ball milling with in the powder after mixing accessory ingredient, powder is made circular fine particle;
(6) moulding: use the desktop electric tablet press machine circular fine particle to be pressed into the blank of given shape size;
(7) sintering: blank is put into resistance furnace carry out sintering processes.During sintering, pressed compact is placed on ZrO
2On the load bearing board, sintering temperature is T=1120～1180 ℃.Temperature controlled processes is: during room temperature to 900 ℃, heating rate is per hour 100～120 ℃; 900 ℃ when the T, heating rate is per hour 300～400 ℃; Behind T insulation 2～8h, lower the temperature, rate of temperature fall is per hour 180～300 ℃ in the time of T to 900 ℃, rate of temperature fall is per hour 100～120 ℃ in the time of 900 ℃ to 600 ℃, rate of temperature fall is per hour 100～120 ℃ in the time of 600 ℃ to 250 ℃, and the rate of temperature fall from 250 ℃ to room temperature is per hour 60～100 ℃.
Not only cost is lower for preparation method of the present invention, technique is simple, and the nickel-copper-zinc ferrite material surface resistance of preparing is not less than 320000M Ω; And ought add simultaneously accessory ingredient TiO
2, SnO
2, V
2O
5, ZrO
2, SiO
2, CaO and MnO
2The time, gained nickel-copper-zinc ferrite room temperature power loss is lower than 250kw/m
3, the high temperature power loss is lower than 180kw/m
3, the room temperature saturation flux density is not less than 180 ℃ greater than 400mT, Curie temperature.
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 only to these embodiment.
Embodiment 1
(1) batching: take by weighing respectively purity and be 99.5% Fe
2O
3, purity is that 99.8% NiO, purity are that 99.8% ZnO and purity are 99.7% CuO, four mol ratio is 49.00: 18.05: 28.10: 4.85;
(2) ball millings: be ball according to mass ratio with powder: material: the ratio of water=2: 1: 1 ball grinder of packing into, then wet-milling in ball mill.Ball-milling Time is 35 minutes, and rotary speed is 400r/min;
(3) pre-burning: the powder that ball milling is good is put into resistance furnace and is carried out pre-burning, 900 ℃ of calcined temperatures, and temperature retention time is 1 hour;
(4) secondary ball milling and mix accessory ingredient: take by weighing pre-burned powder (quality is by 100%) and accessory ingredient: chemical pure TiO
2(0.01wt%), SnO
2(0.04wt%), V
2O
5(0.01wt%), ZrO
2(0.1wt%), SiO
2(0.01wt%), CaO (0.04wt%) and MnO
2(0.1wt%) put into ball grinder, the mass percent of secondary composition is the mass content with respect to principal component, then be ball according to total mass ratio: material: the ratio of water=2: 1: 1, add respectively bead, then add entry, stir, and mash, put into ball mill and carry out wet-milling, Ball-milling Time is 3h, and rotary speed is 400r/min;
(5) granulation: the polyvinyl alcohol water solution with 9% (being commonly called as glue) is to mix at 1: 10 according to the quality of glue and the mass ratio of powder, and mechanical agitator stirs, and then sieve (70 mesh sieve) makes circular fine particle with powder;
(6) moulding: use the desktop electric tablet press machine, load 5 * 10
7The pressure compacting powder of Pa, and pressurize 30s after the unloading, use 3 * 10 again
7The pressure of Pa is suppressed powder, finally is pressed into the column type magnet ring blank of Φ 30mm * Φ 25mm * 6mm;
(7) sintering: blank is put into resistance furnace carry out sintering processes.Temperature controlled processes is during sintering: heating rate is 120 ℃/h during room temperature to 900 ℃; Behind 1120 ℃ of insulation 8h, lower the temperature; Rate of temperature fall is 180 ℃/h in the time of 1120 ℃ to 900 ℃; Rate of temperature fall is 100 ℃/h in the time of 900 ℃ to 600 ℃; Rate of temperature fall is 100 ℃/h in the time of 600 ℃ to 250 ℃; Rate of temperature fall from 250 ℃ to room temperature is 80 ℃/h, obtains the nickel-copper-zinc ferrite material after the cooling.
Embodiment 2
(1) batching: take by weighing respectively purity and be 99.6% Fe
2O
3, purity is that 99.7% NiO, purity are that 99.8% ZnO and purity are 99.8% CuO, four mol ratio is 49.50: 17.75: 27.85: 4.90;
(2) ball millings: be ball according to mass ratio with principal component: material: the ratio of water=2: 1: 1 ball grinder of packing into, then wet-milling in ball mill.Ball-milling Time is 30 minutes, and rotary speed is 500r/min;
(3) pre-burning: the powder that ball milling is good is put into resistance furnace and is carried out pre-burning, 800 ℃ of calcined temperatures, and temperature retention time is 4h;
(4) secondary ball milling and mix secondary composition: take by weighing pre-burned powder (by 100%) and secondary composition: chemical pure TiO
2(0.03wt%), SnO
2(0.02wt%), V
2O
5(0.04wt%), ZrO
2(0.4wt%), SiO
2(0.02wt%), CaO (0.02wt%) and MnO
2(0.35wt%) put into ball grinder, the mass percent of secondary composition is the mass content with respect to principal component, is ball according to total mass ratio then: material: the ratio of water=2: 1: 1, add respectively bead, then add entry, stir, and mash, put into ball mill and carry out wet-milling.Ball-milling Time is 2.5h, and rotary speed is 500r/min;
(5) granulation: the polyvinyl alcohol water solution with 9% (being commonly called as glue) is to mix at 1: 10 according to the quality of glue and the mass ratio of powder, and mechanical agitator stirs, and then sieve (70 mesh sieve) makes circular fine particle with powder;
(6) moulding: use the desktop electric tablet press machine, load 5 * 10
7The pressure compacting powder of Pa, and pressurize 30s after the unloading, use 3 * 10 again
7The pressure of Pa is suppressed powder, finally is pressed into the column type magnet ring blank of Φ 30mm * Φ 25mm * 6mm;
(7) sintering: blank is put into resistance furnace carry out sintering processes.Temperature controlled processes is during sintering: heating rate is 100 ℃/h during room temperature to 900 ℃; 900 ℃ to 1140 ℃ heating rates are 350 ℃/h; Behind 1140 ℃ of insulation 5h, lower the temperature; Rate of temperature fall is 250 ℃/h in the time of 1140 ℃ to 900 ℃; Rate of temperature fall is 110 ℃/h in the time of 900 ℃ to 600 ℃; Rate of temperature fall is 110 ℃/h in the time of 600 ℃ to 250 ℃; Rate of temperature fall from 250 ℃ to room temperature is 60 ℃/h, obtains the nickel-copper-zinc ferrite material after the cooling.
Embodiment 3
(1) batching: take by weighing respectively purity and be 99.3% Fe
2O
3, purity is that 99.6% NiO, purity are that 99.7% ZnO and purity are 99.8% CuO, four mol ratio is 50.00: 17.55: 27.50: 4.95;
(2) ball millings: be ball according to mass ratio with powder: material: the ratio of water=2: 1: 1 ball grinder of packing into, then wet-milling in ball mill.Ball-milling Time is 40 minutes, and rotary speed is 600r/min;
(3) pre-burning: the powder that ball milling is good is put into resistance furnace and is carried out pre-burning, 850 ℃ of calcined temperatures, and temperature retention time is 3h;
(4) secondary ball milling and mix secondary composition: take by weighing pre-burned powder (by 100%) and secondary composition: chemical pure TiO
2(0.02wt%), SnO
2(0.01wt%), V
2O
5(0.03wt%), ZrO
2(0.5wt%), SiO
2(0.03wt%), CaO (0.01wt%) and MnO
2(0.65wt%) put into ball grinder, the mass percent of secondary composition is the mass content with respect to principal component, is ball according to total mass ratio then: material: the ratio of water=2: 1: 1, add respectively bead, then add entry, stir, and mash, put into ball mill and carry out wet-milling.Ball-milling Time is 2h, and rotary speed is 600r/min;
(5) granulation: the polyvinyl alcohol water solution with 9% (being commonly called as glue) is to mix at 1: 10 according to the quality of glue and the mass ratio of powder, and mechanical agitator stirs, and then sieve (70 mesh sieve) makes circular fine particle with powder;
(6) moulding: use the desktop electric tablet press machine, load 5 * 10
7The pressure compacting powder of Pa, and pressurize 30s after the unloading, use 3 * 10 again
7The pressure of Pa is suppressed powder, finally is pressed into the magnet ring blank of Φ 25mm * Φ 15mm * 5mm;
(7) sintering: blank is put into resistance furnace carry out sintering processes.Temperature controlled processes is during sintering: heating rate is 110 ℃/h during room temperature to 900 ℃; 900 ℃ to 1180 ℃ heating rates are 400 ℃/h; Behind 1180 ℃ of insulation 2h, lower the temperature; Rate of temperature fall is 300 ℃/h in the time of 1180 ℃ to 900 ℃; Rate of temperature fall is 120 ℃/h in the time of 900 ℃ to 600 ℃; Rate of temperature fall is 120 ℃/h in the time of 600 ℃ to 250 ℃; Rate of temperature fall from 250 ℃ to room temperature is 100 ℃/h, obtains the nickel-copper-zinc ferrite material after the cooling.
Each embodiment results of performance analysis is listed in table 1, and μ i is initial permeability, and Pcv is power loss, and Bs is saturation flux density, and Tc is Curie temperature.For convenient relatively, with the 6H40 (PC44 that is equivalent to TDK) of JSF company as a comparison case, the data that under equal conditions record are given in table 1 in the lump.As can be seen from Table 1, NiZn soft magnetic ferrite of the present invention has high sheet resistance, can be used for being higher than the fields such as inverter of 2000V such as the big screen LCD panel with output voltage, needn't worry again when making device miniaturization that insulation distance between terminal and magnetic core is too little and the danger that occurs to puncture.
The performance evaluation of table 1 nickel-copper-zinc ferrite of the present invention and Comparative Examples
Above-described embodiment does not limit the present invention in any way, and every employing is equal to replaces or technical scheme that the mode of equivalent transformation obtains all drops on protection scope of the present invention.
Claims (4)
1. a nickel-copper-zinc ferrite material with high surface resistance for panel display is characterized in that, is made by principal component and accessory ingredient;
Described principal component is comprised of following material: the Fe of 49.00 ~ 50.00mol%
2O
3, the CuO of ZnO, 4.85 ~ 4.95mol% of 27.50 ~ 28.10mol% and the NiO of surplus;
Take the quality sum of all principal components as benchmark, described accessory ingredient comprises the TiO of 0.01 ~ 0.03wt%
2, the SnO of 0.01 ~ 0.04wt%
2, the V of 0.01 ~ 0.04wt%
2O
5, the ZrO of 0.1 ~ 0.5wt%
2
2. nickel-copper-zinc ferrite material with high surface resistance for panel display as claimed in claim 1 is characterized in that, take the quality sum of all principal components as benchmark, described accessory ingredient also comprises the SiO of 0.01 ~ 0.03wt%
2, 0.01 ~ 0.04wt% CaO.
3. nickel-copper-zinc ferrite material with high surface resistance for panel display as claimed in claim 1 or 2 is characterized in that, take the quality sum of all principal components as benchmark, described accessory ingredient also comprises the MnO of 0.10 ~ 0.65wt%
2
4. nickel-copper-zinc ferrite material with high surface resistance for panel display as claimed in claim 1 or 2 is characterized in that, its sheet resistance is not less than 320000M Ω.
Priority Applications (1)
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|---|---|---|---|
| CN 201110166394 CN102329129B (en) | 2011-06-20 | 2011-06-20 | Nickel-copper-zinc ferrite material with high surface resistance for panel display |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN 201110166394 CN102329129B (en) | 2011-06-20 | 2011-06-20 | Nickel-copper-zinc ferrite material with high surface resistance for panel display |
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| CN102329129A CN102329129A (en) | 2012-01-25 |
| CN102329129B true CN102329129B (en) | 2013-03-20 |
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| CN107032777A (en) * | 2017-04-01 | 2017-08-11 | 沅陵辰州磁电高科有限公司 | A kind of high magnetic permeability Ni-Zn soft magnetic ferrite material and preparation method thereof |
| JP2022148515A (en) * | 2021-03-24 | 2022-10-06 | Tdk株式会社 | Ferrite composition and electronic component |
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| Publication number | Priority date | Publication date | Assignee | Title |
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| JPH0630297B2 (en) * | 1988-02-03 | 1994-04-20 | ティーディーケイ株式会社 | Ferrite sintered body and chip parts |
| JP2002198212A (en) * | 2000-12-27 | 2002-07-12 | Fdk Corp | Low-loss oxide magnetic material |
| JP2002246221A (en) * | 2001-02-16 | 2002-08-30 | Nec Tokin Corp | Low loss oxide magnetic material |
| JP4576727B2 (en) * | 2001-02-23 | 2010-11-10 | 株式会社村田製作所 | Oxide magnetic ceramic composition and inductor component using the same |
| CN100558674C (en) * | 2005-07-07 | 2009-11-11 | 横店集团东磁有限公司 | Wide temperature, low-temperature coefficient, high magnetic permeability NiZn Ferrite Material and preparation method thereof |
| CN100589215C (en) * | 2007-12-29 | 2010-02-10 | 电子科技大学 | NiZn series ferrite material and preparing method thereof |
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