CN101692365B - Nickel-zinc soft magnetic ferrite material and preparation method thereof - Google Patents

Nickel-zinc soft magnetic ferrite material and preparation method thereof Download PDF

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CN101692365B
CN101692365B CN2009100420971A CN200910042097A CN101692365B CN 101692365 B CN101692365 B CN 101692365B CN 2009100420971 A CN2009100420971 A CN 2009100420971A CN 200910042097 A CN200910042097 A CN 200910042097A CN 101692365 B CN101692365 B CN 101692365B
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soft magnetic
accessory
ferrite material
magnetic ferrite
preparation
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CN101692365A (en
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李刘清
李际勇
王国华
王伯辉
胡满明
龚锋
韦建军
伍俏红
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Guangdong Magsource Electronic Co., Ltd.
Guangdong Fenghua Advanced Tech Holding Co Ltd
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GUANGDONG MAGSOURCE ELECTRONIC CO Ltd
Guangdong Fenghua Advanced Tech Holding Co Ltd
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Abstract

The invention discloses a nickel-zinc soft magnetic ferrite material, comprising the following components in parts by mole: 44-50mol% of Fe2O3, 9-18mol% of ZnO, 25-35mol% of NiO, 5-12mol% of CuO, and 3-10mol% of MgO, and the ferrite material also comprises the following components in parts by weight: 0.002-0.008Wt% of accessory A, 0.001-0.002Wt% of accessory B, 0.001-0.006Wt% of accessory C and 0.0002-0.0008Wt % of accessory D. The accessory A is one or two of Bi2O3, SiO2 and Ta2O5, the accessory B is one or more of TiO2, Co2O3 and Nb2O5, the accessory C is one or more of MoO3, V2O5 and Co3O4, and the accessory D is one or both of BaCo3 and WO3. The obtained nickel-zinc ferrite material has the characteristics of high frequency, high Q, high TC and low temperature coefficient, and meets the needs of high-frequency circuits.

Description

A kind of Ni-Zn soft magnetic ferrite material and preparation method thereof
Technical field
The present invention relates to a kind of soft magnetic ferrite and preparation method thereof, relate in particular to Ni-Zn soft magnetic ferrite material and preparation method thereof.
Background technology
Traditional soft magnetic material; As: MnZn soft magnetic material, nickel zinc soft magnetic material, magnesium zinc soft magnetic material etc. are as a kind of functional material; Every field in national economy has obtained using widely, and development and national economy has been brought into play great progradation, and is closely related with the people's daily life.Along with the develop rapidly of non-crystaline amorphous metal and nanometer crystallographic system soft magnetic material, new challenge has been proposed traditional soft magnetic material in recent years.To this, produce soft magnetic ferrite and not only must improve aspect the material property, but also should improve technology, reduce cost, aspect such as environmental protection makes greater effort, and could adapt to hyundai electronics industrial expansion and needs.And light weight miniaturization along with electronic equipment; Promoted the high speed development of electronic devices and components miniaturizations, chip type, high performance, to the high frequency ferrite material proposed again to reduce the high frequency power consumption requirement, improve series of requirements such as Q value, assurance high frequency characteristics, high-curie temperature, low-temperature coefficient.
One Chinese patent application CN101286397 discloses nickel-zinc-ferrite material and the preparation method that a kind of initial permeability is 40-8+8; Its principal phase is a spinel structure; Comprise Fe2O3, ZnO, MnO, NiO and CoO main the composition, and it is 46mol%～49mol% that its composition content is calculated as Fe2O3 with oxide; ZnO is 2mol%～8mol%; MnO is 0.1mol%～1.0mol%; NiO is 41.7mol%～48mol%; CoO is 0.3mol%～1.5mol%.
Summary of the invention
The technical issues that need to address of the present invention provide a kind ofly to be had high frequency, high Q, high TC, low-temperature coefficient characteristic and can satisfy Ni-Zn soft magnetic ferrite material of high-frequency circuit and preparation method thereof.
The technical problem that the present invention will solve realizes through following technical scheme: a kind of Ni-Zn soft magnetic ferrite material counts by molar iron oxide Fe 2O 344～50mol%, zinc oxide ZnO 9～18mol%, nickel protoxide NiO 25～35mol%, cupric oxide CuO 5～12mol%, magnesia MgO 3～10mol%.
Further: in above-mentioned Ni-Zn soft magnetic ferrite material, by weight, also add the auxiliary material A of 0.002～0.008Wt%, the auxiliary material B of 0.001～0.002Wt%, the auxiliary material C of 0.001～0.006Wt%, the auxiliary material D of 0.0002～0.0008Wt%.Described auxiliary material A is Bi 2O 3, SiO 2, Ta 2O 5In one or both, auxiliary material B is TiO 2, CO 2O 3, Nb 2O 5In one or more, auxiliary material C is MoO 3, V 2O 5, Co 3O 4In one or more, auxiliary material D is one or more mixtures among BaCo3, the WO3.Preferred auxiliary material A is the Bi of 0.006Wt% 2O 3, auxiliary material B is the CO of 0.002Wt% 2O 3, auxiliary material C is the MoO of 0.005Wt% 3, auxiliary material D is the BaCo of 0.002Wt% 3
The present invention also provides the preparation method of above-mentioned Ni-Zn soft magnetic ferrite material; Step is: raw material are handled, batching, ball milling, a drying, beat powder or sieve, pre-burning, second batch, secondary ball milling, redrying, secondary beat powder or sieve; It promptly is with buying the main raw material(s) of returning that raw material granularity is handled; Carry out ball milling in advance like nickel oxide, cupric oxide, descend the step operation again.The said ball milling time is 0.5h, and raw material is fully mixed.The said secondary ball milling time is 1.5h.Described pre-burning condition is in air furnace, and 2 ± 0.2 hours pre-burning time, calcined temperature is 890 ± 10 ℃.Described burning sintering time 3 ± 0.3 hours, 940 ± 20 ℃ of sintering temperatures.
Compared with prior art, the present invention utilizes and is prone in the ferritic structure of NiZn form little crystal grain, is loose structure, and is difficult for forming Fe 2+, very high (ρ>=10 of resistivity 8Ω cm), high-frequency loss is very little, is beneficial to frequency applications.Add small powder and improve the temperature characterisitic scheduling theory, through adjustment main raw material(s) Fe 2O 3, ZnO, NiO, CuO the mol ratio proportioning, suitably increase small powder simultaneously, improve Q value and temperature coefficient.Prepared material is fit to production miniaturization product, and has characteristics such as high frequency, high Q, low-temperature coefficient, high breaking strength.The characteristic of the high frequency that series of products possessed of this material, high Q, high TC, low-temperature coefficient can satisfy the demand of high-frequency circuit; The series of products of this material also possess the high breaking strength characteristic simultaneously; Can improve shockproof, the anti-mechanical damage ability of product, to the shockproof certain guarantee that provides of complete machine.Meet the electronics miniaturization developing direction, its market prospects are wide.The performance of products index is following:
1, initial permeability μ i:40 ± 25%;
2, quality factor q (7.96MHz) >=100;
3, Curie temperature Tc (℃) >=250;
4, insulation resistance (M Ω) >=500;
5、αμi(-40℃～+85℃)：200+150(10 -6/℃)
Embodiment
Purport of the present invention is to be prone in the ferritic structure of NiZn form little crystal grain through utilizing, and is loose structure, and is difficult for forming Fe 2+, very high (ρ>=10 of resistivity 7Ω cm), high-frequency loss is very little, is beneficial to frequency applications.Add small powder and improve the temperature characterisitic scheduling theory, through adjustment main raw material(s) Fe 2O 3, ZnO, NiO, CuO the mol ratio proportioning, suitably increase small powder simultaneously, improve Q value and temperature coefficient.Below in conjunction with embodiment content of the present invention is done further to detail, mentioned content is not to qualification of the present invention among the embodiment, and each raw-material selection can be suited measures to local conditions and the result is not had substantial effect in the material.
At first; The basic scheme of summary the inventive method: a kind of Ni-Zn soft magnetic ferrite material; Count by molar iron oxide Fe2O3 44～50mol%, zinc oxide ZnO 9～18mol%, nickel protoxide NiO25～35mol%, cupric oxide CuO 5～12mol%, magnesia MgO 3～10mol%.
Embodiment
A kind of preparation method of Ni-Zn soft magnetic ferrite material; Step is: raw material are handled, batching, ball milling, a drying, beat powder or sieve, pre-burning, second batch, secondary ball milling, redrying, secondary beat powder or sieve; Described pre-burning condition is in air furnace; 2 ± 0.2 hours pre-burning time, calcined temperature is 890 ± 10 ℃; Described burning sintering time 3 ± 0.3 hours, 940 ± 20 ℃ of sintering temperatures.In above-mentioned steps, described once batching adds the Fe in described 1～No. 16 material prescription of table 1 2O 3, add described 1～No. 16 material B i of table 1 among the ZnO, NiO, the described second batch of CuO 2O 3, CO 2O 3, MoO3, BaCo 3The performance test parameter of the Ni-Zn soft magnetic ferrite material of last gained is shown in 1～No. 16 material prescription correspondence of table 2.
Table 1: the prescription of Ni-Zn soft magnetic ferrite material
The prescription sequence number Fe 2O 3 (mol％) ZnO (mol％) NiO (mol％) CuO (mol％) Small powder Bi 2O 3 (Wt％) Small powder CO 2O 3 (Wt％) Small powder MoO 3 (Wt％) Small powder BaCo 3 (Wt％) Pre-burning Sintering
1 49.1 16.9 27 7 0.006 0.002 0.005 0.002 890℃ /2hr 940℃ /3hr
2 47.1 16.9 29 7 0.006 0.002 0.005 0.002 890℃ /2hr 940℃ /3hr
3 46.1 16.9 30 7 0.006 0.002 0.005 0.002 890℃ /2hr 940℃ /3hr
4 45.1 16.9 31 7 0.006 0.002 0.005 0.002 890℃ /2hr 940℃ /3hr
5 45.1 16.8 31 7.1 0.006 0.002 0.005 0.002 890℃ /2hr 940℃ /3hr
6 45.1 16.4 31 7.5 0.006 0.002 0.005 0.002 890℃ /2hr 940℃ /3hr
7 45.1 16 31 7.9 0.006 0.002 0.005 0.002 890℃ /2hr 940℃ /3hr
8 45.1 15.8 31 8.1 0.006 0.002 0.005 0.002 890℃ /2hr 940℃ /3hr
9 45.1 15.8 31.2 7.9 0.006 0.002 0.005 0.002 890℃ /2hr 940℃ /3hr
10 45.1 15.8 31.6 7.5 0.006 0.002 0.005 0.002 890℃ /2hr 940℃ /3hr
11 45.1 15.8 32 7.1 0.006 0.002 0.005 0.002 890℃ /2hr 940℃ /3hr
12 45.1 15.8 32.4 6.7 0.006 0.002 0.005 0.002 890℃ /2hr 940℃ /3hr
13 45.1 15.8 32 7.1 0.006 0.002 0.005 0.002 890℃ /2hr 940℃ /3hr
14 45.1 15.8 32 7.1 0.006 0.002 0.005 0.002 890℃ /2hr 940℃ /3hr
15 45.1 15.8 32 7.1 0.006 0.002 0.005 0.002 890℃ /2hr 940℃ /3hr
16 45.1 15.8 32 7.1 0.006 0.002 0.005 0.002 890℃ /2hr 940℃ /3hr
Table 2: the performance parameter of Ni-Zn soft magnetic ferrite material
The prescription sequence number External diameter (mm) Internal diameter (mm) Highly (mm) L(μH) (1KHz) ?Q?(7.96MHz) Insulation resistance (M Ω) Tc (℃) μi aμi(10 -6/℃) (-40℃～+85℃) Test result
1 25.09 15.04 7.46 11.5 ?6.1 ＞500 251 80 400 Generally
2 25.15 15.12 7.43 18.8 ?5.7 ＞500 252 75 390 Generally
3 25.06 15.19 7.52 22.5 ?5.2 ＞500 255 69 380 Generally
4 25.06 15.25 7.62 30 ?4.6 20 260 61 375 Generally
5 25.05 15.04 7.52 14.7 ?4.8 ＞500 255 63 350 Generally
6 25.12 15.13 7.47 16.8 ?5.1 ＞500 256 67 360 Generally
7 25.14 15.12 7.49 18 ?5.2 ＞500 258 68 300 Generally
8 25.21 15.12 7.52 19 ?5.4 ＞500 260 70 270 Generally
9 25.14 15.15 7.48 15.2 ?4.8 ＞500 254 63 250 Generally
10 25.12 15.11 7.49 15.1 ?4.3 ＞500 256 57 230 Generally
11 25.13 15.13 7.50 14.8 ?3.9 ＞500 265 51 202 Good
12 25.18 15.15 7.50 12.4 ?3.2 ＞500 260 42 212 Generally
13 25.13 15.08 7.47 16 ?3.8 ＞500 265 50 195 Generally
14 25.12 15.09 7.49 15.4 ?4 ＞500 270 52 205 Good
15 25.13 15.11 7.52 15.0 ?3.9 ＞500 268 51 205 Good
16 25.12 15.25 7.51 12 ?3.8 ＞500 264 51 203 Good
According to above experimental result; Purpose in conjunction with this research invention; A kind of prescription of the Ni-Zn soft magnetic ferrite material with high frequency, high Q, low-temperature coefficient and preparation method's composition be No. 11 prescriptions preferably; Simultaneously through 13～No. 16 prescriptions to No. 11 prescription repeated authentication of carrying out, prove that the present invention has reliability, repeatability.

Claims (3)

1. a Ni-Zn soft magnetic ferrite material is characterized in that: count by molar iron oxide Fe 2O 344～50mol%, zinc oxide ZnO 9～18mol%, nickel protoxide NiO 25～35mol%, cupric oxide CuO 5～12mol%, magnesia MgO 3～10mol%;
By weight, the Bi that also adds 0.006wt% 2O 3, 0.002wt% Co 2O 3, 0.005wt% MoO 3, 0.002wt% BaCO 3
2. the preparation method of the said Ni-Zn soft magnetic ferrite material of claim 1; Step is: raw material are handled, batching, ball milling, a drying, beat powder or sieve, pre-burning, second batch, secondary ball milling, redrying, secondary beat powder or sieve; It is characterized in that: the said ball milling time is 0.5h, and raw material is fully mixed; The said secondary ball milling time is 1.5h; Described pre-burning condition is in air furnace, and 2 ± 0.2 hours pre-burning time, calcined temperature is 890 ± 10 ℃; Sintering time 3 ± 0.3 hours, 940 ± 20 ℃ of sintering temperatures.
3. preparation method according to claim 2 is characterized in that: described second batch is the Bi that in the pre-burning material, adds 0.006wt% 2O 3, 0.002wt% Co 2O 3, 0.005wt% MoO 3, 0.002wt% BaCO 3
CN2009100420971A 2009-08-21 2009-08-21 Nickel-zinc soft magnetic ferrite material and preparation method thereof Expired - Fee Related CN101692365B (en)

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CN101891456B (en) * 2010-06-22 2013-06-05 广东风华高新科技股份有限公司 High rupture strength nickel-zinc soft magnetic ferrite material and preparation method thereof
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CN102424570A (en) * 2011-09-01 2012-04-25 上海大学 Preparation method of NiFe2O4 magnetic material
CN103396110A (en) * 2013-08-06 2013-11-20 深圳先进技术研究院 Barium titanate-nickel zinc ferrite composite ceramic material and preparation method thereof
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CN104496445A (en) * 2014-09-30 2015-04-08 横店集团东磁股份有限公司 Soft-magnetic magnetostrictive ferrite material and manufacturing method thereof
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CN106431378A (en) * 2016-08-31 2017-02-22 中山市华佑磁芯材料有限公司 Formula of high-frequency lead-free ferrite material
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CN108774056B (en) * 2018-06-14 2021-04-20 横店集团东磁股份有限公司 NiZn ferrite magnetic sheet and preparation method and application thereof
CN111933376A (en) * 2020-06-29 2020-11-13 洛阳中赫非晶科技有限公司 Formula for ferrite magnetic core
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