CN103693949B - Soft magnetic NiCuZn ferrite material with characteristics of wide temperature range, low temperature coefficient, high frequency and low loss, and preparation method thereof - Google Patents
Soft magnetic NiCuZn ferrite material with characteristics of wide temperature range, low temperature coefficient, high frequency and low loss, and preparation method thereof Download PDFInfo
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Abstract
The present invention discloses a soft magnetic NiCuZn ferrite material with characteristics of wide temperature range, low temperature coefficient, high frequency and low loss, and a preparation method thereof. The soft magnetic NiCuZn ferrite material comprises a main component and a sub-component, wherein the main component comprises 51-59 mol% of Fe2O3, 10-22 mol of NiO, 20-35 mol% of ZnO, and 0.3-8 mol% of CuO, and the sub-component comprises (by the total weight of the main component) two or more than two components selected from 0.05-1.0 wt% of Mn3O4, 0.05-0.9 wt% of SiO2, 0.01-0.5 wt% of Bi2O3, 0.01-0.8 wt% of TiO2, 0.01-0.6 wt% of CaCO3, and 0.01-0.3 wt% of Co2O3. The soft magnetic NiCuZn ferrite material can be used in the wide temperature range of -40 to 120 DEG C, and has characteristics of low temperature coefficient, low magnetic permeability change along with temperature change, and low loss.
Description
Technical field
The present invention relates to a kind of soft magnetism NiCuZn Ferrite Material, particularly one wide temperature low-temperature coefficient high-frequency low-consumption soft magnetism NiCuZn Ferrite Material and preparation method thereof.
Background technology
The crystal of NiCuZn Ferrite Material is porous spinel structure, has following key property: the high frequency characteristics that (1) is excellent; (2) good temperature stability; (3) large non-linear; (4) diversity of filling a prescription; (5) manufacturing process simple and stable.So it is widely used as high frequency antenna, high intermediate frequency inductance core, filter core, transformer and magnetic amplifier magnetic core etc.
High-frequency communication machine LC filter specifications inductance coil has positive temperature coefficient and wants to mate with the negative temperature coefficient that capacitor has, to obtain the temperature coefficient of null value.Change crystal anisotropy to the interdependence of temperature, make μ i value vary with temperature state change, produce that to have low-loss linear---the little temperature coefficient core material of wide temperature, for high-frequency communication machine high performance mini creates advantage.
The Major Difficulties that this material makes is to change crystal anisotropy to the interdependence of temperature, makes wide temperature low-temperature coefficient, low-loss NiZn ferrite.For soft magnetic ferrite, require magnetic conductivity to vary with temperature little, and be very difficult on the occasion of linear change.Only can not meet this requirement by changing main formula and changing process conditions.Also need add appropriate special additive in NiZn ferrite, its domain wall be stablized, thus improves temperature characterisitic.
Summary of the invention
The object of the present invention is to provide a kind of wide temperature low-temperature coefficient high-frequency low-consumption soft magnetism NiCuZn Ferrite Material, can use in the wide temperature range of-40 DEG C ~ 120 DEG C, have low-temperature coefficient, magnetic conductivity varies with temperature little, the feature that loss is low.
Present invention also offers a kind of preparation method of wide temperature low-temperature coefficient high-frequency low-consumption soft magnetism NiCuZn Ferrite Material.
The technical solution adopted for the present invention to solve the technical problems is:
A kind of wide temperature low-temperature coefficient high-frequency low-consumption soft magnetism NiCuZn Ferrite Material, be made up of principal component and accessory ingredient, the content of each component of described principal component is: Fe
2o
3: 51-59 mol%, NiO:10-22mol, ZnO:20-35mol%, CuO:0.3-8mol%; The two or more components of following content are selected from: Mn by the secondary composition of main composition total weight
3o
4: 0.05-1.0wt%, SiO
2: 0.05-0.9wt%, Bi
2o
3: 0.01-0.5 wt%, TiO
2: 0.01-0.8 wt%, CaCO
3: 0.01-0.6 wt%, Co
2o
3: 0.01-0.3wt%.
Inventor is found by a large amount of experimental studies, by the proportioning of the main composition of conservative control, and be equipped with suitable secondary composition, one or more point of secondary of NiO, ZnO, CuO adds simultaneously, just can obtain a kind of use in the wide temperature range of-40 DEG C ~ 120 DEG C, have low-temperature coefficient, magnetic conductivity varies with temperature little, the Ferrite Material of the low feature of loss.
In above-mentioned main compositional ranges, work as Fe
2o
3content is less than 51mol%, then can not get desired low-temperature coefficient, if content is greater than 59mol%, then magnetic conductivity is too low; When the content of NiO, ZnO, CuO is greater than capping, easily there is nonmagnetic dephasign, thus reduce magnetic property; And content is less than in limited time lower, be difficult to the effect playing substitutional ion.
The growth behavior that above-mentioned secondary composition mainly changes ferrite crystal grains by solid phase reaction and ferrite effect controls the size of crystal grain, shape and distribution, thus improves the magnetic property of soft magnetic ferrite.When their content is lower than lower limit, do not have and control grain growth and densified effect, the fluctuation of magnetic conductivity in wide temperature range cannot be stablized, when their content is higher than higher limit, then easily cause the misgrowth of crystal grain, magnetic property is worsened, the fluctuation of magnetic conductivity in wide temperature range cannot be stablized.
As preferably, the content of each component of described principal component is: Fe
2o
3: 51-59 mol%, NiO:16-22mol, ZnO:20-35mol%, CuO:0.3-7mol%.
A preparation method for wide temperature low-temperature coefficient high-frequency low-consumption soft magnetism NiCuZn Ferrite Material, comprises the steps:
A, a ball milling: each for principal component component is mixed by proportioning, by the mixture of gained by wet method ball milling, the particle mean size of the particulate material after a ball milling is at 0.8-1.5 μm;
B, pre-burning: the particulate material after a ball milling is carried out pre-burning in atmosphere, calcined temperature controls at 750 DEG C-1050 DEG C, insulation 0.5-4 hour;
C, secondary ball milling: the particulate material after pre-burning is carried out wet method secondary ball milling together with secondary composition, the particle mean size of the particulate material after secondary ball milling is at 0.8-1.2 μm;
D, shaping and sintering: the particulate material after secondary ball milling is dried, add the poly-vinyl alcohol solution of Preburning material weight 11-13wt%, mix rear granulation, compressing, sinter in atmosphere, sintering temperature controls at 940-1300 DEG C, and insulation 2-6 hour, obtains wide temperature low-temperature coefficient high-frequency low-consumption soft magnetism NiCuZn Ferrite Material.
As preferably, the component of described main composition: one or more components in NiO, ZnO, CuO are added at twice.
As preferably, one or more components first times in NiO, ZnO, CuO add when a ball milling, and ratio >=80% of interpolation, second time is added together with accessory ingredient when secondary ball milling.
One or more components in NiO, ZnO, CuO are added at twice, a part can continue the effect playing substitutional ion, another part rests on boundary surfaces, form crystal ingedient, play the effect of flux, prevent crystal grain from growing up further, the fluctuation of magnetic conductivity in wide temperature range can be stablized, reduce the wastage.
As preferably, the concentration of described poly-vinyl alcohol solution is 10-15wt%.
The invention has the beneficial effects as follows: can use in the wide temperature range of-40 DEG C ~ 120 DEG C, have low-temperature coefficient, magnetic conductivity varies with temperature little, the feature that loss is low.
Detailed description of the invention
Below by specific embodiment, technical scheme of the present invention is described in further detail.
In the present invention, if not refer in particular to, the raw material adopted and equipment etc. all can be buied from market or this area is conventional.Method in following embodiment, if no special instructions, is the conventional method of this area.
embodiment 1:
Principal component and accessory ingredient are coordinated with ormal weight according to table 1 Suo Shi.
Preparation method is:
A, a ball milling: each for principal component component mixed by proportioning, by the mixture of gained by wet method ball milling, the particle mean size of the particulate material after a ball milling is at 0.8-1.5 μm.
B, pre-burning: the particulate material after a ball milling is carried out pre-burning in atmosphere, and calcined temperature controls at 750 DEG C DEG C, be incubated 4 hours.
C, secondary ball milling: the particulate material after pre-burning is carried out wet method secondary ball milling together with secondary composition, the particle mean size of the particulate material after secondary ball milling is at 0.8-1.2 μm.
D, shaping and sintering: the particulate material after secondary ball milling is dried, the concentration adding Preburning material weight 11wt% is the poly-vinyl alcohol solution of 15wt%, mix rear mist projection granulating, the pressure in 7MPa makes type, and compact dimensions is external diameter 25mm, internal diameter 15mm, is highly the annular solid of 7mm.Sinter in atmosphere, sintering temperature controls at 940 DEG C, is incubated 6 hours, obtains toroidal core.
Wherein, NiO adds at twice, and first time adds when a ball milling, and the ratio of interpolation is 80%, and remainder second time is added together with accessory ingredient when secondary ball milling.
To toroidal core, measure (1) relative temperature coefficient (α μ r), (2) initial permeability when 1KHz (μ i), (3) quality factor Q value when 1MHz, the higher loss of Q value is lower.
The mensuration of above-mentioned (1) ~ (3) is carried out according to following main points:
(1) relative temperature coefficient (α μ r) and (2) initial permeability when 1KHz (μ i) are be wound around 20 circle coils on toroidal core after, measure inductance value etc. by HP4284A instrument, obtain-40 DEG C ~ 120 DEG C relative temperature coefficient (α μ r) and at KHz time initial permeability (μ i).
Relative temperature coefficient (α μ r) is the changing value of the initial permeability represented between the temperature of 2, such as temperature T
1time initial permeability with μ i
1expression, temperature T
2time initial permeability with μ i
2during expression, at temperature range T
1~ T
2α μ r can be represented by following formula:
αμr=（μi
2－μi
1)/μi
1 2(T
2-T
1)
(3) the Q value when 1MHz
After toroidal core is wound around 20 circle coils, be determined at the Q value under 1MHz frequency by HP4284A instrument.
The results are shown in following table 1.
embodiment 2:
Principal component and accessory ingredient are coordinated with ormal weight according to table 2 Suo Shi.
Preparation method is:
A, a ball milling: each for principal component component mixed by proportioning, by the mixture of gained by wet method ball milling, the particle mean size of the particulate material after a ball milling is at 0.8-1.5 μm.
B, pre-burning: the particulate material after a ball milling is carried out pre-burning in atmosphere, calcined temperature controls at 1050 DEG C, is incubated 0.5 hour.
C, secondary ball milling: the particulate material after pre-burning is carried out wet method secondary ball milling together with secondary composition, the particle mean size of the particulate material after secondary ball milling is at 0.8-1.2 μm.
D, shaping and sintering: the particulate material after secondary ball milling is dried, the concentration adding Preburning material weight 13wt% is the poly-vinyl alcohol solution of 10wt%, mix rear mist projection granulating, the pressure in 7MPa makes type, and compact dimensions is external diameter 25mm, internal diameter 15mm, is highly the annular solid of 7mm.Sinter in atmosphere, sintering temperature controls at 1300 DEG C, is incubated 2 hours, obtains toroidal core.
Wherein, NiO, ZnO add at twice, and first time adds when a ball milling, and the ratio of interpolation is 90%, and remainder second time is added together with accessory ingredient when secondary ball milling.
To toroidal core, measure (1) relative temperature coefficient (α μ r), (2) initial permeability when 1KHz (μ i), (3) Q value when 1MHz.
The mensuration of above-mentioned (1) ~ (3) is carried out according to following main points:
(1) relative temperature coefficient (α μ r) and (2) initial permeability when 1KHz (μ i) are be wound around 20 circle coils on toroidal core after, measure inductance value etc. by HP4284A instrument, obtain-40 DEG C ~ 120 DEG C relative temperature coefficient (α μ r) and at KHz time initial permeability (μ i).
Relative temperature coefficient (α μ r) is the changing value of the initial permeability represented between the temperature of 2, such as temperature T
1time initial permeability with μ i
1expression, temperature T
2time initial permeability with μ i
2during expression, at temperature range T
1~ T
2α μ r can be represented by following formula:
αμr=（μi
2－μi
1)/μi
1 2(T
2-T
1)
(3) the Q value when 1MHz
After toroidal core is wound around 20 circle coils, be determined at the Q value under 1MHz frequency by HP4284A instrument.
The results are shown in following table 2.
embodiment 3:
Principal component and accessory ingredient are coordinated with ormal weight according to table 3 Suo Shi.
Preparation method is:
A, a ball milling: each for principal component component mixed by proportioning, by the mixture of gained by wet method ball milling, the particle mean size of the particulate material after a ball milling is at 0.8-1.5 μm.
B, pre-burning: the particulate material after a ball milling is carried out pre-burning in atmosphere, calcined temperature controls at 910 DEG C, is incubated 2.5 hours.
C, secondary ball milling: the particulate material after pre-burning is carried out wet method secondary ball milling together with secondary composition, the particle mean size of the particulate material after secondary ball milling is at 0.8-1.2 μm.
D, shaping and sintering: the particulate material after secondary ball milling is dried, the concentration adding Preburning material weight 12wt% is the poly-vinyl alcohol solution of 12wt%, mix rear mist projection granulating, the pressure in 7MPa makes type, and compact dimensions is external diameter 25mm, internal diameter 15mm, is highly the annular solid of 7mm.Sinter in atmosphere, sintering temperature controls at 1100 DEG C, is incubated 3 hours, obtains toroidal core.
Wherein, NiO, ZnO, CuO add at twice, and first time adds when a ball milling, and the ratio of interpolation is 95%, and remainder second time is added together with accessory ingredient when secondary ball milling.
To toroidal core, measure (1) relative temperature coefficient (α μ r), (2) initial permeability when 1KHz (μ i), (3) Q value when 1MHz.
The mensuration of above-mentioned (1) ~ (3) is carried out according to following main points:
(1) relative temperature coefficient (α μ r) and (2) initial permeability when 1KHz (μ i) are be wound around 20 circle coils on toroidal core after, measure inductance value etc. by HP4284A instrument, obtain-40 DEG C ~ 120 DEG C relative temperature coefficient (α μ r) and at KHz time initial permeability (μ i).
Relative temperature coefficient (α μ r) is the changing value of the initial permeability represented between the temperature of 2, such as temperature T
1time initial permeability with μ i
1expression, temperature T
2time initial permeability with μ i
2during expression, at temperature range T
1~ T
2α μ r can be represented by following formula:
αμr=（μi
2－μi
1)/μi
1 2(T
2-T
1)
(3) the Q value when 1MHz
After toroidal core is wound around 20 circle coils, be determined at the Q value under 1MHz frequency by HP4284A instrument.
The results are shown in following table 3.
From table 1-table 3, the present invention is by reasonably controlling the proportioning of main composition, and be equipped with suitable secondary composition, one or more point of secondary of NiO, ZnO, CuO adds simultaneously, just can obtain a kind of use in the wide temperature range of-40 DEG C ~ 120 DEG C, have low-temperature coefficient, magnetic conductivity varies with temperature little, the Ferrite Material of the low feature of loss.
Above-described embodiment is one of the present invention preferably scheme, not does any pro forma restriction to the present invention, also has other variant and remodeling under the prerequisite not exceeding the technical scheme described in claim.
Claims (1)
1. a wide temperature low-temperature coefficient high-frequency low-consumption soft magnetism NiCuZn Ferrite Material, is made up of principal component and accessory ingredient, it is characterized in that: the content of each component of described principal component is: Fe
2o
3: 51-59 mol%, NiO:16-22mol%, ZnO:20-35mol%, CuO:0.3-7mol%; The two or more components of following content are selected from: Mn by the secondary composition of main composition total weight
3o
4: 0.05-1.0wt%, SiO
2: 0.05-0.9wt%, Bi
2o
3: 0.01-0.5wt%, TiO
2: 0.01-0.8 wt%, CaCO
3: 0.01-0.6 wt%, Co
2o
3: 0.01-0.3wt%;
The preparation method of described wide temperature low-temperature coefficient high-frequency low-consumption soft magnetism NiCuZn Ferrite Material comprises the steps:
A, a ball milling: each for principal component component is mixed by proportioning, by the mixture of gained by wet method ball milling, the particle mean size of the particulate material after a ball milling is at 0.8-1.5 μm;
B, pre-burning: the particulate material after a ball milling is carried out pre-burning in atmosphere, calcined temperature controls at 750 DEG C-1050 DEG C, insulation 0.5-4 hour;
C, secondary ball milling: the particulate material after pre-burning is carried out wet method secondary ball milling together with secondary composition, the particle mean size of the particulate material after secondary ball milling is at 0.8-1.2 μm;
D, shaping and sintering: the particulate material after secondary ball milling is dried, add the poly-vinyl alcohol solution of Preburning material weight 11-13wt%, mix rear granulation, compressing, sinter in atmosphere, sintering temperature controls at 940-1300 DEG C, and insulation 2-6 hour, obtains wide temperature low-temperature coefficient high-frequency low-consumption soft magnetism NiCuZn Ferrite Material;
The component of described main composition: one or more components in NiO, ZnO, CuO are added at twice; One or more component first times in NiO, ZnO, CuO add when a ball milling, ratio >=80% of interpolation, and second time is added together with accessory ingredient when secondary ball milling; The concentration of described poly-vinyl alcohol solution is 10-15wt%.
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| CN104193314A (en) * | 2014-08-14 | 2014-12-10 | 蕲春县蕊源电子有限公司 | High-permeability soft magnetic ferrite material and preparation method thereof |
| CN104291802A (en) * | 2014-09-01 | 2015-01-21 | 湖南创一电子科技有限公司 | High performance soft magnetic composite Ni-Zn ferrite material |
| JP5999278B1 (en) * | 2015-04-02 | 2016-09-28 | Tdk株式会社 | Composite ferrite composition and electronic component |
| CN104844184A (en) * | 2015-04-27 | 2015-08-19 | 厦门大学 | Near field communication magnetic sheet with low magnetic permeability and temperature coefficient and preparation method thereof |
| CN105036724B (en) * | 2015-07-15 | 2017-05-31 | 深圳顺络电子股份有限公司 | A kind of NiCuZn Ferrite Materials and preparation method, Stacked magnetic bead |
| CN105529127A (en) * | 2016-03-08 | 2016-04-27 | 佛山市川东磁电股份有限公司 | Integral magnetic core for magneto-dependent sensor and manufacturing method of integral magnetic core for magneto-dependent sensor |
| CN106431377A (en) * | 2016-08-31 | 2017-02-22 | 中山市华佑磁芯材料有限公司 | Formula of anti-stress material with high magnetic permittivity and low temperature coefficient |
| CN107857581B (en) * | 2017-10-18 | 2021-02-05 | 电子科技大学 | Low-temperature sintered NiCuZn ferrite material and preparation method thereof |
| CN109320229A (en) * | 2018-11-01 | 2019-02-12 | 沅陵辰州磁电高科有限公司 | Nickel zinc soft magnet material |
| CN111205075B (en) * | 2019-10-23 | 2021-04-20 | 横店集团东磁股份有限公司 | Nickel-zinc ferrite material and preparation method thereof |
| CN115838282A (en) * | 2022-10-20 | 2023-03-24 | 上海华源磁业股份有限公司 | Preparation method of high-frequency low-loss ferrite material |
| CN115745591A (en) * | 2022-11-25 | 2023-03-07 | 国网辽宁省电力有限公司沈阳供电公司 | High-frequency current sensor NiCuZn soft magnetic ferrite material for partial discharge monitoring and preparation method thereof |
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| JP5224495B2 (en) * | 2006-08-23 | 2013-07-03 | Ｆｄｋ株式会社 | Manufacturing method of high frequency ferrite |
| CN101409123B (en) * | 2008-07-25 | 2011-03-23 | 深圳振华富电子有限公司 | Soft magnetic ferrite inductor manufacturing technology |
| CN101692365B (en) * | 2009-08-21 | 2012-05-30 | 广东肇庆微硕电子有限公司 | Nickel-zinc soft magnetic ferrite material and preparation method thereof |
| WO2012151714A1 (en) * | 2011-05-09 | 2012-11-15 | 临沂中瑞电子有限公司 | Nicuzn ferrite material with high magnetic conductivity |
| CN102557605A (en) * | 2012-03-09 | 2012-07-11 | 深圳顺络电子股份有限公司 | Preparation method of low-temperature sintered Ni-Zn-Cu soft magnetic ferrite material |
| CN102807361B (en) * | 2012-07-03 | 2014-10-22 | 天通控股股份有限公司 | Nickel-zinc ferrite material for wireless signal sensing, sheet core and preparation method thereof |
| CN103382106A (en) * | 2013-06-27 | 2013-11-06 | 电子科技大学 | High-conductive and high-loss NiCuZn ferrite material, magnetic sheets and preparation method thereof |
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