CN101607816A - Nickel ferrite for radio frequency range and preparation method thereof - Google Patents

Nickel ferrite for radio frequency range and preparation method thereof Download PDF

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CN101607816A
CN101607816A CNA2009101007134A CN200910100713A CN101607816A CN 101607816 A CN101607816 A CN 101607816A CN A2009101007134 A CNA2009101007134 A CN A2009101007134A CN 200910100713 A CN200910100713 A CN 200910100713A CN 101607816 A CN101607816 A CN 101607816A
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principal constituent
radio frequency
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ferrite
oxide
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CN101607816B (en
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张瑞标
王勤峰
邵峰
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TDG Holding Co Ltd
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TDG Holding Co Ltd
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Abstract

Nickel ferrite for radio frequency range and preparation method thereof the invention belongs to nickel series soft magnetic ferrite technical field, is specifically related to the low magnetic permeability Ni ferrite that a kind of radio band is suitable for.This ferritic principal constituent is ferric oxide, nickel oxide, and minor component comprises cobalt oxide, manganese oxide and vanadium oxide, adopts the conventional ceramic technique preparation.Nickel ferrite for radio frequency range of the present invention has low-down initial permeability, good radio frequency loss performance, broad frequency domain characteristic, high Curie temperature, is applicable to radio band communication class electronic devices and components.

Description

Nickel ferrite for radio frequency range and preparation method thereof
Technical field
The invention belongs to nickel series soft magnetic ferrite technical field, be specifically related to a kind of low-down initial permeability, good radio frequency loss performance, broad frequency domain characteristic, high Curie temperature, Ni ferrite that radio frequency is suitable for and preparation method thereof.
Background technology
Ferrite Material is having application very widely aspect the electronicss such as communication, digital electric, household electrical appliance.The nickel based ferrite has very large application market as a ferritic main series because of it has good radio-frequency performance in the communication class device.Particularly in the continuous development of the electron device in radio-frequency communication field, the demand of such Ferrite Material is vigorous day by day.
The radio frequency Ni ferrite has low-down initial permeability, good radio frequency loss performance, broad frequency domain characteristic, high characteristics such as Curie temperature.The radio frequency Ni ferrite in signal of communication electron-like device mainly as being widely used of aspects such as radio frequency inductive, impedance transformer, impedance matching box and anti-electromagnetic interference, of a great variety, the huge market demand.
Summary of the invention
The purpose of this invention is to provide a kind of nickel ferrite for radio frequency range, this ferrite has following excellent comprehensive performance: low-down initial permeability, good radio frequency loss performance, broad frequency domain characteristic, high characteristics such as Curie temperature can be good at satisfying radio band electronic devices and components performance demands; The preparation method of this nickel ferrite for radio frequency range is proposed simultaneously.
The cardinal principle of technical solution problem of the present invention is: adopt Fe 2O 3Molar content is 55%~65%, and all the other are the prescription of NiO, adds Co in minor component 2O 3Reduce the radio band relative loss factor factor and initial permeability, in minor component, add Mn 3O 4Promote resistivity of material, in minor component, add V 2O 5Reduce sintering temperature, adjust material microstructure, obtain good material behavior by production technique.
The technical solution adopted in the present invention is: a kind of nickel ferrite for radio frequency range, and this ferrite comprises principal constituent and minor component, principal constituent is: ferric oxide, nickel oxide is characterized in that described principal constituent is as follows in the content of standard substance separately:
Fe 2O 3:55mol%~65mol%,
NiO:45mol%~35mol%;
Described minor component comprises cobalt oxide, manganese oxide, vanadium oxide, described relatively principal constituent total amount, and described minor component is with its standard substance Co separately 2O 3, Mn 3O 4, V 2O 5The total content of meter is 1wt%~3wt%.
Described relatively principal constituent total amount, described minor component is with its standard substance Co separately 2O 3, Mn 3O 4, V 2O 5The content of meter is respectively: Co 2O 3: 0.5wt%~0.8wt%, Mn 3O 4: 0.5wt%~2.5wt%, V 2O 5: 0~1wt%.
Nickel ferrite for radio frequency range of the present invention adopts the manufacture method of conventional oxide method, and concrete steps are as follows successively:
(1) mix: by the principal constituent proportion ingredient, carry out wet-mixed together, mixing time is 30~60 minutes; Described principal constituent in the content of standard substance separately is: Fe 2O 3: 55mol%~65mol%, NiO:45mol%~35mol%;
(2) pre-burning: carry out pre-burning with adding in the rotary kiln after the principal constituent slip spraying drying, calcined temperature is controlled at 900 ℃~1000 ℃, and the pre-burning time is 20~40 minutes;
(3) pulverize: will go up and carry out wet pulverization after adding minor component in the pre-imitation frosted glass of principal constituent that the step pre-burning obtains, the pulverizing time is 120~180 minutes, pulverizes back slip particle diameter and is controlled at 1.5 μ m~2.0 μ m; Described minor component comprises cobalt oxide, manganese oxide, vanadium oxide, described relatively principal constituent total amount, and described minor component is with its standard substance Co separately 2O 3, Mn 3O 4, V 2O 5The total content of meter is 1wt%~3wt%;
(4) granulation: the slip in the last step adds 1.5%PVA, adopts mist projection granulating, obtains particulate material;
(5) compacting: the particulate material that will go up the step adopts the powder former compacting to obtain blank, and the pressed density of blank is controlled at 3.0 ± 0.2g/cm 3
(6) sintering: will go up blank sintering in air atmosphere that the step obtains, sintering temperature is controlled at 1100 ℃~1200 ℃, is incubated 3 hours and carries out sintering, makes described Ni ferrite goods through cooling again.
As a kind of preferred, the minor component that in the pre-imitation frosted glass of principal constituent, adds in the described pulverising step, described relatively principal constituent total amount is with its standard substance Co separately 2O 3, Mn 3O 4, V 2O 5The content of meter is respectively: Co 2O 3: 0.5wt%~0.8wt%, Mn 3O 4: 0.5wt%~2.5wt%, V 2O 5: 0~1wt%.
Mixing of the minor component of the present invention by rational principal constituent proportioning and optimization is equipped with suitable process conditions, and this ferrite has low-down initial permeability, good radio frequency loss performance, broad frequency domain characteristic, high characteristics such as Curie temperature; Specifically, the initial permeability μ of the nickel ferrite for radio frequency range that makes of the present invention iFor: 10 ± 25% (10kHz, 0.25mT, 25 ℃ ± 3 ℃), the relative loss factor factor t an δ/μ of its radio frequency rate iBe not more than 570 * 10 -6(120MHz, 0.25mT, 25 ℃ ± 3 ℃), Curie temperature is not less than 300 ℃.Ni ferrite of the present invention is superior in the over-all properties of radio band, and performances such as its initial permeability, the relative loss factor factor and Curie temperature can be good at satisfying radio band electronic devices and components performance demands.The relative loss factor factor that particularly 50~500MHz is low can be good at reducing the loss of signal transmission.
The present invention has following characteristics compared with prior art: low-down initial permeability, good radio frequency loss performance, broad frequency domain characteristic, high characteristics such as Curie temperature can be good at satisfying radio band electronic devices and components performance demands.
Embodiment
Embodiment 1
Take by weighing the Fe of 59%mol 2O 3, 41%mol NiO.After above-mentioned principal constituent mixing, add in the sand mill and mix, mixing time 30 minutes is sent into rotary kiln after the spraying drying, pre-burning under 950 ℃ ± 10 ℃ temperature, 30 minutes pre-burning time kind.In pre-imitation frosted glass, add minor component input sand mill subsequently and pulverize, 120 minutes pulverizing time, pulverize back slip particle diameter and be controlled at 1.5~2.0 μ m; Described relatively principal constituent total amount, described minor component in its separately the content of standard substance be respectively (wt%): Co 2O 3: 0.7, Mn 3O 4: 1.5, V 2O 5: 0.05.Need to add pure water 35% in described mixing sand milling and the pulverizing sand grinding process, and dispersion agent and defoamer.The spray tower mist projection granulating obtains the Ni ferrite particle behind the PVA of last adding 1.5% in the sand milling slip.
Get the toroidal core of this particle 2.5 gram moulding compacting Φ 12.7mm * Φ 7.9mm * h6.5mm, pressed density is controlled at 3.0 ± 0.2g/cm 3, in air atmosphere, carry out sintering under 1170 ℃ ± 10 ℃ the temperature condition, soaking time 3 hours, back naturally cooling.
Through the magnetic core of said process preparation, as shown in table 1 with the correlated performance of instrument test magnetic cores such as HP4284ALCR tester, HP4291B radio frequency material instrument, SY8258BH analyser, high cryostat.
Embodiment 2
Get the Fe of 61%mol 2O 3, 39%mol NiO.After above-mentioned principal constituent mixing, add in the sand mill and mix, mixing time 30 minutes is sent into rotary kiln after the spraying drying, pre-burning under 950 ℃ ± 10 ℃ temperature, 30 minutes pre-burning time kind.In pre-imitation frosted glass, add minor component input sand mill subsequently and pulverize, 120 minutes pulverizing time, pulverize back slip particle diameter and be controlled at 1.5~2.0 μ m; Described relatively principal constituent total amount, described minor component in its separately the content of standard substance be respectively (wt%): Co 2O 3: 0.7, Mn 3O 4: 1.5, V 2O 5: 0.05.Need to add pure water 35% in described mixing sand milling and the pulverizing sand grinding process, and dispersion agent and defoamer.The spray tower mist projection granulating obtains the Ni ferrite particle behind the PVA of last adding 1.5% in the sand milling slip.
Get the toroidal core of this particle 2.5 gram moulding compacting Φ 12.7mm * Φ 7.9mm * h6.5mm, pressed density is controlled at 3.0 ± 0.2g/cm 3, in air atmosphere, carry out sintering under 1170 ℃ ± 10 ℃ the temperature condition, soaking time 3 hours, back naturally cooling.
Through the magnetic core of said process preparation, as shown in table 1 with the correlated performance of instrument test magnetic cores such as HP4284A LCR tester, HP4291B radio frequency material instrument, SY8258BH analyser, high cryostat.
Embodiment 3
Get the Fe of 59%mol 2O 3, 41%mol NiO.After above-mentioned principal constituent mixing, add in the sand mill and mix, mixing time 30 minutes is sent into rotary kiln after the spraying drying, pre-burning under 950 ℃ ± 10 ℃ temperature, 30 minutes pre-burning time kind.In pre-imitation frosted glass, add minor component input sand mill subsequently and pulverize, 120 minutes pulverizing time, pulverize back slip particle diameter and be controlled at 1.5~2.0 μ m; Described relatively principal constituent total amount, described minor component in its separately the content of standard substance be respectively (wt%): Co 2O 3: 0.75, Mn 3O 4: 1.5, V 2O 5: 0.05.Need to add pure water 35% in described mixing sand milling and the pulverizing sand grinding process, and dispersion agent and defoamer.The spray tower mist projection granulating obtains the Ni ferrite particle behind the PVA of last adding 1.5% in the sand milling slip.
Get the toroidal core of this particle 2.5 gram moulding compacting Φ 12.7mm * Φ 7.9mm * h6.5mm, pressed density is controlled at 3.0 ± 0.2g/cm 3, in air atmosphere, carry out sintering under 1170 ℃ ± 10 ℃ the temperature condition, soaking time 3 hours, back naturally cooling.
Through the magnetic core of said process preparation, as shown in table 1 with the correlated performance of instrument test magnetic cores such as HP4284A LCR tester, HP4291B radio frequency material instrument, SY8258BH analyser, high cryostat.
Comparative Examples 1
Get the Fe of 53%mol 2O 3, 47%mol NiO.After above-mentioned principal constituent mixing, add in the sand mill and mix, mixing time 30 minutes is sent into rotary kiln after the spraying drying, pre-burning under 950 ℃ ± 10 ℃ temperature, 30 minutes pre-burning time kind.In pre-imitation frosted glass, add minor component input sand mill subsequently and pulverize, 120 minutes pulverizing time, pulverize back slip particle diameter and be controlled at 1.5~2.0 μ m; Described relatively principal constituent total amount, described minor component in its separately the content of standard substance be respectively (wt%): Co 2O 3: 0.75, Mn 3O 4: 1.5, V 2O 5: 0.05.Need to add pure water 35% in described mixing sand milling and the pulverizing sand grinding process, and dispersion agent and defoamer.The spray tower mist projection granulating obtains the Ni ferrite particle behind the PVA of last adding 1.5% in the sand milling slip.
Get the toroidal core of this particle 2.5 gram moulding compacting Φ 2.7mm * Φ 7.9mm * h6.5mm, pressed density is controlled at 3.0 ± 0.2g/cm 3, in air atmosphere, carry out sintering under 1170 ℃ ± 10 ℃ the temperature condition, soaking time 3 hours, back naturally cooling.
Through the magnetic core of said process preparation, as shown in table 1 with the correlated performance of instrument test magnetic cores such as HP4284A LCR tester, HP4291B radio frequency material instrument, SY8258BH analyser, high cryostat.
Comparative Examples 2
Get the Fe of 53%mol 2O 3, 47%mol NiO.After above-mentioned principal constituent mixing, add in the sand mill and mix, mixing time 30 minutes is sent into rotary kiln after the spraying drying, pre-burning under 950 ℃ ± 10 ℃ temperature, 30 minutes pre-burning time kind.In pre-imitation frosted glass, add minor component input sand mill subsequently and pulverize, 120 minutes pulverizing time, pulverize back slip particle diameter and be controlled at 1.5~2.0 μ m; Described relatively principal constituent total amount, described minor component in its separately the content of standard substance be respectively (wt%): Co 2O 3: 1.0, Mn 3O 4: 1.5, V 2O 5: 0.05.Need to add pure water 35% in described mixing sand milling and the pulverizing sand grinding process, and dispersion agent and defoamer.The spray tower mist projection granulating obtains the Ni ferrite particle behind the PVA of last adding 1.5% in the sand milling slip.
Get the toroidal core of this particle 2.5 gram moulding compacting Φ 12.7mm * Φ 7.9mm * h6.5mm, pressed density is controlled at 3.0 ± 0.2g/cm 3, in air atmosphere, carry out sintering under 1170 ℃ ± 10 ℃ the temperature condition, soaking time 3 hours, back naturally cooling.
Through the magnetic core of said process preparation, as shown in table 1 with the correlated performance of instrument test magnetic cores such as HP4284A LCR tester, HP4291B radio frequency material instrument, SY8258BH analyser, high cryostat.
Embodiment that contrast is above and Comparative Examples are as can be seen, radio frequency Ni ferrite of the present invention has low-down initial permeability, good radio frequency loss performance, broad frequency domain characteristic, high characteristics such as Curie temperature, stable production technique and good performance, the service requirements of satisfying the radio band electronic devices and components that can be good.
Table 1 toroidal core material property of the present invention
Project Initial permeability μ i??10kHz、0.25mT、25℃ Relative loss factor factor t an δ/μ i??120MHz、0.25mT Curie temperature Tc (℃) 10kHz, 0.25mT Saturation induction density Bs (mT) 4000A/m
Embodiment 1 ??10.2 ??530×10 -6 ??>300 ??243
Embodiment 2 ??10.8 ??550×10 -6 ??>300 ??235
Embodiment 3 ??11.5 ??526×10 -6 ??>300 ??231
Comparative Examples 1 ??13.5 ??621×10 -6 ??>300 ??256
Comparative Examples 2 ??6.6 ??1164×10 -6 ??>300 ??157

Claims (4)

1. nickel ferrite for radio frequency range, this ferrite comprises principal constituent and minor component, principal constituent is: ferric oxide, nickel oxide is characterized in that described principal constituent is as follows in the content of standard substance separately:
Fe 2O 3:55mol%~65mol%
NiO:45mol%~35mol%
Described minor component comprises cobalt oxide, manganese oxide, vanadium oxide, described relatively principal constituent total amount, and described minor component is with its standard substance Co separately 2O 3, Mn 3O 4, V 2O 5The total content of meter is 1wt%~3wt%.
2. nickel ferrite for radio frequency range as claimed in claim 1 is characterized in that: described relatively principal constituent total amount, described minor component is with its standard substance Co separately 2O 3, Mn 3O 4, V 2O 5The content of meter is respectively: Co 2O 3: 0.5wt%~0.8wt%, Mn 3O 4: 0.5wt%~2.5wt%, V 2O 5: 0~1wt%.
3. the preparation method of nickel ferrite for radio frequency range as claimed in claim 1 or 2 is characterized in that concrete steps are as follows successively:
(1) mix: by claim 1 principal constituent proportion ingredient, carry out wet-mixed together, mixing time is 30~60 minutes; Described principal constituent in the content of standard substance separately is: Fe 2O 3: 55mol%~65mol%, NiO:45mol%~35mol%;
(2) pre-burning: carry out pre-burning with adding in the rotary kiln after the principal constituent slip spraying drying, calcined temperature is controlled at 900 ℃~1000 ℃, and the pre-burning time is 20~40 minutes;
(3) pulverize: will go up and carry out wet pulverization after adding minor component in the pre-imitation frosted glass of principal constituent that the step pre-burning obtains, the pulverizing time is 120~180 minutes, pulverizes back slip particle diameter and is controlled at 1.5 μ m~2.0 μ m; Described minor component comprises cobalt oxide, manganese oxide, vanadium oxide, described relatively principal constituent total amount, and described minor component is with its standard substance Co separately 2O 3, Mn 3O 4, V 2O 5The total content of meter is 1wt%~3wt%;
(4) granulation: the slip in the last step adds 1.5%PVA, adopts mist projection granulating, obtains particulate material;
(5) compacting: the particulate material that will go up the step adopts the powder former compacting to obtain blank, and the pressed density of blank is controlled at 3.0 ± 0.2g/cm 3
(6) sintering: will go up blank sintering in air atmosphere that the step obtains, sintering temperature is controlled at 1100 ℃~1200 ℃, is incubated 3 hours and carries out sintering, makes described Ni ferrite goods through cooling again.
4. the preparation method of nickel ferrite for radio frequency range as claimed in claim 3 is characterized in that: the minor component that adds in the pre-imitation frosted glass of principal constituent in the described pulverising step, described relatively principal constituent total amount is with its standard substance Co separately 2O 3, Mn 3O 4, V 2O 5The content of meter is respectively: Co 2O 3: 0.5wt%~0.8wt%, Mn 3O 4: 0.5wt%~2.5wt%, V 2O 5: 0~1wt%.
CN200910100713A 2009-07-15 2009-07-15 Nickel ferrite for radio frequency range and preparation method thereof Active CN101607816B (en)

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Cited By (2)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN105272195A (en) * 2015-11-23 2016-01-27 杭州电子科技大学 NiZn series ferrite wave-absorbing material core and manufacturing method thereof
CN112441828A (en) * 2020-12-08 2021-03-05 江门安磁电子有限公司 Ferrite material and preparation method thereof

Family Cites Families (3)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN1222487C (en) * 2002-07-05 2005-10-12 邓廷成 High-conductive nickel-zinc ferrite and preparing process thereof
JP2006160584A (en) * 2004-12-10 2006-06-22 Sumida Corporation Ni-Zn-BASED FERRITE COMPOSITION AND ANTENNA COIL
CN101412622A (en) * 2008-10-31 2009-04-22 天通控股股份有限公司 High-frequency nickel-copper-zinc ferrite and preparation thereof

Cited By (2)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN105272195A (en) * 2015-11-23 2016-01-27 杭州电子科技大学 NiZn series ferrite wave-absorbing material core and manufacturing method thereof
CN112441828A (en) * 2020-12-08 2021-03-05 江门安磁电子有限公司 Ferrite material and preparation method thereof

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