CN101412622A - High-frequency nickel-copper-zinc ferrite and preparation thereof - Google Patents
High-frequency nickel-copper-zinc ferrite and preparation thereof Download PDFInfo
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- CN101412622A CN101412622A CNA2008101222028A CN200810122202A CN101412622A CN 101412622 A CN101412622 A CN 101412622A CN A2008101222028 A CNA2008101222028 A CN A2008101222028A CN 200810122202 A CN200810122202 A CN 200810122202A CN 101412622 A CN101412622 A CN 101412622A
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- ferrite
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- 229910001308 Zinc ferrite Inorganic materials 0.000 title claims abstract description 27
- KOMIMHZRQFFCOR-UHFFFAOYSA-N [Ni].[Cu].[Zn] Chemical compound [Ni].[Cu].[Zn] KOMIMHZRQFFCOR-UHFFFAOYSA-N 0.000 title claims abstract description 27
- 238000002360 preparation method Methods 0.000 title claims abstract description 17
- VYPSYNLAJGMNEJ-UHFFFAOYSA-N Silicium dioxide Chemical compound O=[Si]=O VYPSYNLAJGMNEJ-UHFFFAOYSA-N 0.000 claims abstract description 43
- 238000005245 sintering Methods 0.000 claims abstract description 30
- 229910000859 α-Fe Inorganic materials 0.000 claims abstract description 15
- 239000000203 mixture Substances 0.000 claims abstract description 11
- 229910000416 bismuth oxide Inorganic materials 0.000 claims abstract description 3
- 229910000428 cobalt oxide Inorganic materials 0.000 claims abstract description 3
- IVMYJDGYRUAWML-UHFFFAOYSA-N cobalt(ii) oxide Chemical compound [Co]=O IVMYJDGYRUAWML-UHFFFAOYSA-N 0.000 claims abstract description 3
- 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 3
- 229910052814 silicon oxide Inorganic materials 0.000 claims abstract description 3
- XLOMVQKBTHCTTD-UHFFFAOYSA-N Zinc monoxide Chemical compound [Zn]=O XLOMVQKBTHCTTD-UHFFFAOYSA-N 0.000 claims abstract 6
- QPLDLSVMHZLSFG-UHFFFAOYSA-N Copper oxide Chemical compound [Cu]=O QPLDLSVMHZLSFG-UHFFFAOYSA-N 0.000 claims abstract 5
- 239000011787 zinc oxide Substances 0.000 claims abstract 3
- UQSXHKLRYXJYBZ-UHFFFAOYSA-N iron oxide Inorganic materials [Fe]=O UQSXHKLRYXJYBZ-UHFFFAOYSA-N 0.000 claims abstract 2
- 229910000480 nickel oxide Inorganic materials 0.000 claims abstract 2
- NDLPOXTZKUMGOV-UHFFFAOYSA-N oxo(oxoferriooxy)iron hydrate Chemical compound O.O=[Fe]O[Fe]=O NDLPOXTZKUMGOV-UHFFFAOYSA-N 0.000 claims abstract 2
- GNRSAWUEBMWBQH-UHFFFAOYSA-N oxonickel Chemical compound [Ni]=O GNRSAWUEBMWBQH-UHFFFAOYSA-N 0.000 claims abstract 2
- 239000000470 constituent Substances 0.000 claims description 35
- 238000002156 mixing Methods 0.000 claims description 27
- 239000002245 particle Substances 0.000 claims description 26
- 238000010298 pulverizing process Methods 0.000 claims description 20
- 229910004298 SiO 2 Inorganic materials 0.000 claims description 16
- 239000000126 substance Substances 0.000 claims description 14
- 238000001816 cooling Methods 0.000 claims description 10
- 238000001035 drying Methods 0.000 claims description 10
- 239000005338 frosted glass Substances 0.000 claims description 10
- 239000003595 mist Substances 0.000 claims description 10
- 238000005507 spraying Methods 0.000 claims description 10
- 239000011236 particulate material Substances 0.000 claims description 4
- 238000005469 granulation Methods 0.000 claims description 2
- 230000003179 granulation Effects 0.000 claims description 2
- 239000004615 ingredient Substances 0.000 claims description 2
- 239000000843 powder Substances 0.000 claims description 2
- 229960004643 cupric oxide Drugs 0.000 claims 1
- 238000000034 method Methods 0.000 abstract description 23
- 230000035699 permeability Effects 0.000 abstract description 12
- 238000004891 communication Methods 0.000 abstract description 8
- 238000004519 manufacturing process Methods 0.000 abstract description 8
- 206010022971 Iron Deficiencies Diseases 0.000 abstract description 4
- 238000005265 energy consumption Methods 0.000 abstract description 4
- 150000002815 nickel Chemical class 0.000 abstract description 3
- 239000005751 Copper oxide Substances 0.000 abstract 1
- 238000001354 calcination Methods 0.000 abstract 1
- 229910000431 copper oxide Inorganic materials 0.000 abstract 1
- 238000009472 formulation Methods 0.000 abstract 1
- 230000005389 magnetism Effects 0.000 abstract 1
- 239000004576 sand Substances 0.000 description 40
- 239000011162 core material Substances 0.000 description 29
- XEEYBQQBJWHFJM-UHFFFAOYSA-N iron Substances [Fe] XEEYBQQBJWHFJM-UHFFFAOYSA-N 0.000 description 18
- 238000003801 milling Methods 0.000 description 16
- 239000000463 material Substances 0.000 description 15
- PXHVJJICTQNCMI-UHFFFAOYSA-N Nickel Chemical compound [Ni] PXHVJJICTQNCMI-UHFFFAOYSA-N 0.000 description 12
- 230000000052 comparative effect Effects 0.000 description 9
- 239000003795 chemical substances by application Substances 0.000 description 8
- 230000002596 correlated effect Effects 0.000 description 8
- 239000013530 defoamer Substances 0.000 description 8
- 239000006185 dispersion Substances 0.000 description 8
- 238000000227 grinding Methods 0.000 description 8
- 238000000465 moulding Methods 0.000 description 8
- 238000002791 soaking Methods 0.000 description 8
- 239000007921 spray Substances 0.000 description 8
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 description 8
- 238000005303 weighing Methods 0.000 description 8
- 229910052759 nickel Inorganic materials 0.000 description 6
- 239000013078 crystal Substances 0.000 description 5
- 238000010586 diagram Methods 0.000 description 3
- 229910052742 iron Inorganic materials 0.000 description 3
- 238000009766 low-temperature sintering Methods 0.000 description 2
- 239000011148 porous material Substances 0.000 description 2
- HCHKCACWOHOZIP-UHFFFAOYSA-N Zinc Chemical compound [Zn] HCHKCACWOHOZIP-UHFFFAOYSA-N 0.000 description 1
- 229910045601 alloy Inorganic materials 0.000 description 1
- 239000000956 alloy Substances 0.000 description 1
- 238000005516 engineering process Methods 0.000 description 1
- 230000006698 induction Effects 0.000 description 1
- 238000005457 optimization Methods 0.000 description 1
- 230000000630 rising effect Effects 0.000 description 1
- 230000008054 signal transmission Effects 0.000 description 1
- 229910052725 zinc Inorganic materials 0.000 description 1
- 239000011701 zinc Substances 0.000 description 1
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Abstract
The invention relates to a high frequency nickel-copper-zinc ferrite and a method for preparing the same, which belong to the technical field of nickel series soft magnetism ferrite. The main components of the ferrite are ferric oxide, nickel oxide, zinc oxide, and copper oxide, the accessory components comprise cobalt oxide, bismuth oxide, and silicon oxide, and the ferrite is prepared by an oxide method. The invention adopts an iron deficiency formulation, a low calcination temperature, and a low sintering temperature so that the prepared high frequency nickel-copper-zinc ferrite has good performances of low initial permeability, low relative dissipation factor between 50MHz and 200MHz, and high Curie temperature, and can better satisfy the use requirement of communication electronic parts and components; besides, the preparation process is stable, and the production process has low energy consumption.
Description
Technical field
The invention belongs to nickel series soft magnetic ferrite technical field, be specifically related to nickel-copper-zinc ferrite that a kind of low-temperature sintering, low initial permeability, low high-frequency loss, high-curie temperature, high frequency be 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 high frequency performance in the communication class device.Along with electron device constantly develops to direction microminiaturized, portability, the nickel series ferrite material also develops towards high frequency direction; Particularly in the application of communication field.
High frequency nickel based ferrite has low initial permeability, high characteristics such as Curie temperature, good frequency characteristic, high resistance and low-loss.High frequency nickel based ferrite in signal of communication electron-like device mainly as being widely used of aspects such as impedance transformer, impedance matching box and anti-electromagnetic interference, of a great variety, the huge market demand.
Conventional high frequency nickel based ferrite generally adopts Fe
2O
3Molar content surpasses the principal constituent prescription of 50% rich iron, and its sintering temperature of nickel based ferrite that adopts this class prescription is generally more than 1200 ℃.Because the sintering temperature height of material, the energy consumption of production process is very high, and is simultaneously also higher for the requirement of production unit sintering kiln.
Summary of the invention
At the technical shortcoming of existing high frequency nickel based ferrite, the purpose of this invention is to provide a kind of high-frequency nickel-copper-zinc ferrite, this ferrite has following excellent comprehensive performance: under the low-temperature sintering condition, low initial permeability, the low high band relative loss factor factor, high Curie temperature can better meet the over-all properties requirement of class signal electronic devices and components to high frequencyization, miniaturization development.
The cardinal principle of technical solution problem of the present invention is: adopt Fe
2O
3Molar content is less than 50% iron deficiency prescription, adds CuO and reduce pre-burning and sintering temperature in principal constituent, adds Co in minor component
2O
3Reduce the high band relative loss factor factor and initial permeability, in minor component, add Bi
2O
3Reduce sintering temperature, in minor component, add SiO
2Optimize the crystal grain vesicular structure, adjust material microstructure, obtain good material behavior by production technique.
The technical solution adopted in the present invention is: high-frequency nickel-copper-zinc ferrite comprises principal constituent and minor component, and principal constituent is respectively: Fe
2O
3, NiO, ZnO, CuO, described principal constituent is as follows in the content of standard substance separately:
Fe
2O
3：47.5mol％～48.5mol％，
NiO：38mol％～40mol％，
ZnO：6mol％～8mol％，
CuO：3mol％～4mol％；
Described minor component comprises cobalt oxide, bismuth oxide, silicon oxide, described relatively principal constituent total amount, and described minor component is with its standard substance Co separately
2O
3, Bi
2O
3, SiO
2The total content of meter is 5.6wt%～7.8wt%.Co wherein
2O
3Add the relative loss factor factor that can be good at reducing 50MHz～200MHz, Bi
2O
3Can greatly reduce final sintering temperature, SiO
2Adding can optimize the microtexture of material.
With respect to described principal constituent total amount, described minor component is with its standard substance Co separately
2O
3, Bi
2O
3, SiO
2The content of meter is respectively (wt%): Co
2O
3: 0.6～0.8, Bi
2O
3: 2.5～3.5, SiO
2: 2.5～3.5.
The preparation method of high-frequency nickel-copper-zinc ferrite of the present invention adopts the 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
(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 800 ℃～900 ℃, 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 1.0 μ m～1.5 μ m;
(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 ± 0.2) g/cm
3
(6) sintering: will go up blank sintering in air atmosphere that the step compacting obtains, sintering temperature is controlled at 950 ℃～1000 ℃, is incubated 3 hours and carries out sintering, promptly gets described high-frequency nickel-copper-zinc ferrite goods through cooling again.
The temperature of pre-burning is at 800 ℃～900 ℃ in the manufacture method of the present invention, and 1000 ℃～1050 ℃ calcined temperatures with respect to rich iron formula have reduced about 200 ℃; Sintering temperature is at 950 ℃～1000 ℃, and 1200 ℃～1250 ℃ sintering temperature of relative rich iron formula has reduced about 250 ℃.The production technique of high-frequency nickel-copper-zinc ferrite of the present invention has low pre-burning and sintering temperature, has reduced the production energy consumption of product effectively.
Mixing of the minor component of the present invention by rational principal constituent proportioning and optimization, be equipped with suitable process conditions, made the tiny homogeneous of microcosmic crystal grain, cavernous ambrose alloy zinc body oxysome under the condition of sintering temperature and low, this ferrite has low initial permeability, the low high band relative loss factor factor and high Curie temperature; Specifically, the initial permeability μ of the nickel-copper-zinc ferrite that makes of the present invention
iFor: 15 ± 25% (10kHz, 0.25mT, 25 ℃ ± 3 ℃), its high-frequency relative loss factor factor t an δ/μ
iBe not more than 780 * 10
-6(120MHz, 0.25mT, 25 ℃ ± 3 ℃), Curie temperature is not less than 300 ℃.High frequency low permeability nickel-copper-zinc ferrite of the present invention is superior in the over-all properties of high band, and performances such as its initial permeability, the relative loss factor factor and Curie temperature can be good at satisfying the service requirements of communication class electronic devices and components.The relative loss factor factor that particularly 50MHz～200MHz is low can reduce the loss of signal transmission well.
The present invention adopts iron deficiency prescription, low calcined temperature, sintering temperature and low to prepare high-frequency nickel-copper-zinc ferrite, have following characteristics compared with prior art: prepared high-frequency nickel-copper-zinc ferrite has low initial permeability, the relative loss factor factor that 50MHz～200MHz is low, high good performances such as Curie temperature, can satisfy the service requirements of communication class electronic devices and components well; And stable preparation process, the production process energy consumption reduces.
Description of drawings
Fig. 1 is the SEM micro-structure diagram of the prepared magnetic core of embodiment 1.
Fig. 2 is the SEM micro-structure diagram of the prepared magnetic core of Comparative Examples 2.
Embodiment
Take by weighing the Fe of 48%mol
2O
3, the ZnO of NiO, 8%mol of 40%mol and the CuO of 4%mol.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 830 ℃ ± 10 ℃ temperature, 30 minutes pre-burning time kind.In pre-imitation frosted glass, add minor component input sand mill subsequently and pulverize, 150 minutes pulverizing time, pulverize back slip particle diameter and be controlled at 1.0 μ m～1.5 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, Bi
2O
3: 2.5, SiO
2: 2.5.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 nickel-copper-zinc ferrite particle behind the PVA of last adding 1.5% in the sand milling slip.
Get the toroidal core of this particle 2.4 gram moulding compacting Φ 12.7mm * Φ 7.9mm * 6.5mm, pressed density is controlled at (3.0 ± 0.2) g/cm
3, in air atmosphere, carry out sintering under 970 ℃ ± 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, SY8258 BH analyser, high cryostat.Fig. 1 is the microtexture SEM figure of the magnetic core of present embodiment 1 preparation, and crystal grain is little and even as can be seen, pore many and even, is typical vesicular structure.
Embodiment 2
Take by weighing the Fe of 48.2%mol
2O
3, the ZnO of NiO, 8%mol of 39.8%mol and the CuO of 4%mol.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 830 ℃ ± 10 ℃ temperature, 30 minutes pre-burning time kind.In pre-imitation frosted glass, add minor component input sand mill subsequently and pulverize, 150 minutes pulverizing time, pulverize back slip particle diameter and be controlled at 1.0 μ m～1.5 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, Bi
2O
3: 2.5, SiO
2: 2.5.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 nickel-copper-zinc ferrite particle behind the PVA of last adding 1.5% in the sand milling slip.
Get the toroidal core of this particle 2.4 gram moulding compacting Φ 12.7mm * Φ 7.9mm * 6.5mm, pressed density is controlled at (3.0 ± 0.2) g/cm
3, in air atmosphere, carry out sintering under 970 ℃ ± 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, SY8258 BH analyser, high cryostat.
Take by weighing the Fe of 48.4%mol
2O
3, the ZnO of NiO, 8%mol of 39.6%mol and the CuO of 4%mol.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 830 ℃ ± 10 ℃ temperature, 30 minutes pre-burning time kind.In pre-imitation frosted glass, add minor component input sand mill subsequently and pulverize, 150 minutes pulverizing time, pulverize back slip particle diameter and be controlled at 1.0 μ m～1.5 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, Bi
2O
3: 2.5, SiO
2: 2.5.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 nickel-copper-zinc ferrite particle behind the PVA of last adding 1.5% in the sand milling slip.
Get the toroidal core of this particle 2.4 gram moulding compacting Φ 12.7mm * Φ 7.9mm * 6.5mm, pressed density is controlled at (3.0 ± 0.2) g/cm
3, in air atmosphere, carry out sintering under 970 ℃ ± 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 4
Take by weighing the Fe of 48.2%mol
2O
3, the ZnO of NiO, 8%mol of 39.8%mol and the CuO of 4%mol.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 830 ℃ ± 10 ℃ temperature, 30 minutes pre-burning time kind.In pre-imitation frosted glass, add minor component input sand mill subsequently and pulverize, 150 minutes pulverizing time, pulverize back slip particle diameter and be controlled at 1.0 μ m～1.5 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, Bi
2O
3: 2, SiO
2: 2.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 nickel-copper-zinc ferrite particle behind the PVA of last adding 1.5% in the sand milling slip.
Get the toroidal core of this particle 2.4 gram moulding compacting Φ 12.7mm * Φ 7.9mm * 6.5mm, pressed density is controlled at (3.0 ± 0.2) g/cm
3, in air atmosphere, carry out sintering under 970 ℃ ± 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, SY8258 BH analyser, high cryostat.
Embodiment 5
Take by weighing the Fe of 48.2%mol
2O
3, the ZnO of NiO, 8%mol of 39.8%mol and the CuO of 4%mol.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 830 ℃ ± 10 ℃ temperature, 30 minutes pre-burning time kind.In pre-imitation frosted glass, add minor component input sand mill subsequently and pulverize, 150 minutes pulverizing time, pulverize back slip particle diameter and be controlled at 1.0 μ m～1.5 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: 0.8, Bi
2O
3: 3, SiO
2: 3.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 nickel-copper-zinc ferrite particle behind the PVA of last adding 1.5% in the sand milling slip.
Get the toroidal core of this particle 2.4 gram moulding compacting Φ 12.7mm * Φ 7.9mm * 6.5mm, pressed density is controlled at (3.0 ± 0.2) g/cm
3, carry out sintering under 970 ℃ ± 10 ℃ the temperature condition in the air atmosphere, 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, SY8258 BH analyser, high cryostat.
Comparative Examples 1
Take by weighing the Fe of 48.2%mol
2O
3, the ZnO of NiO, 8%mol of 39.8%mol and the CuO of 4%mol.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 830 ℃ ± 10 ℃ temperature, 30 minutes pre-burning time kind.In pre-imitation frosted glass, add minor component input sand mill subsequently and pulverize, 150 minutes pulverizing time, pulverize back slip particle diameter and be controlled at 1.0 μ m～1.5 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: 0.4, Bi
2O
3: 2.5, SiO
2: 2.5.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 nickel-copper-zinc ferrite particle behind the PVA of last adding 1.5% in the sand milling slip.
Get the toroidal core of this particle 2.4 gram moulding compacting Φ 12.7mm * Φ 7.9mm * 6.5mm, pressed density is controlled at (3.0 ± 0.2) g/cm
3, carry out sintering under 970 ℃ ± 10 ℃ the temperature condition in the air atmosphere, 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, SY8258 BH analyser, high cryostat.
Comparative Examples 2
Take by weighing the Fe of 48.2%mol
2O
3, the ZnO of NiO, 8%mol of 39.8%mol and the CuO of 4%mol.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 830 ℃ ± 10 ℃ temperature, 30 minutes pre-burning time kind.In pre-imitation frosted glass, add minor component input sand mill subsequently and pulverize, 150 minutes pulverizing time, pulverize back slip particle diameter and be controlled at 1.0 μ m～1.5 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, Bi
2O
3: 2.5, SiO
2: 2.5.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 nickel-copper-zinc ferrite particle behind the PVA of last adding 1.5% in the sand milling slip.
Get the toroidal core of this particle 2.4 gram moulding compacting Φ 12.7mm * Φ 7.9mm * 6.5mm, pressed density is controlled at (3.0 ± 0.2) g/cm
3, carry out sintering under 1060 ℃ ± 10 ℃ the temperature condition in the air atmosphere, 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, SY8258 BH analyser, high cryostat.Fig. 2 is the microtexture SEM figure of the prepared magnetic core of this Comparative Examples 2, and crystal grain is thick, not of uniform size as can be seen, the intragranular pore is more.Comparison diagram 1 as can be seen because the rising of sintering temperature, crystal grain is grown up unusually, microtexture is relatively poor, influences the electrical specification of material.
Comparative Examples 3
Take by weighing the Fe of 48.2%mol
2O
3, the ZnO of NiO, 8%mol of 39.8%mol and the CuO of 4%mol.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 1000 ℃ ± 10 ℃ temperature, 30 minutes pre-burning time kind.In pre-imitation frosted glass, add minor component input sand mill subsequently and pulverize, 150 minutes pulverizing time, pulverize back slip particle diameter and be controlled at 1.0 μ m～1.5 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, Bi
2O
3: 2.5, SiO
2: 2.5.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 nickel-copper-zinc ferrite particle behind the PVA of last adding 1.5% in the sand milling slip.
Get the toroidal core of this particle 2.4 gram moulding compacting Φ 12.7mm * Φ 7.9mm * 6.5mm, pressed density is controlled at (3.0 ± 0.2) g/cm
3, carry out sintering under 970 ℃ ± 10 ℃ the temperature condition in the air atmosphere, 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, SY8258 BH analyser, high cryostat.
Embodiment that contrast is above and Comparative Examples are as can be seen, the present invention adopts the high-frequency nickel-copper-zinc ferrite of iron deficiency prescription, low calcined temperature, sintering temperature and low preparation, have low initial permeability, the relative loss factor factor that 120MHz is low, high good performances such as Curie temperature, can satisfy the service requirements of communication class electronic devices and components well.
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/ |
| Embodiment | ||||
| 1 | 15.5 | 586×10 -6 | >300 | 261 |
| Embodiment 2 | 15.6 | 644×10 -6 | >300 | 267 |
| |
14.5 | 518×10 -6 | >300 | 268 |
| Embodiment 4 | 15.5 | 614×10 -6 | >300 | 268 |
| Embodiment 5 | 15.2 | 578×10 -6 | >300 | 266 |
| Comparative Examples 1 | 45.2 | 2427×10 -6 | >300 | 324 |
| Comparative Examples 2 | 35.7 | 1659×10 -6 | >300 | 284 |
| Comparative Examples 3 | 15.6 | 1235×10 -6 | >300 | 284 |
Claims (3)
1, a kind of high-frequency nickel-copper-zinc ferrite, this ferrite comprises principal constituent and minor component, principal constituent is: ferric oxide, nickel oxide, zinc oxide, cupric oxide is characterized in that described principal constituent is as follows in the content of standard substance separately:
Fe
2O
3：47.5mol％～48.5mol％
NiO：38mol％～40mol％
ZnO：6mol％～8mol％
CuO：3mol％～4mol％
Minor component comprises cobalt oxide, bismuth oxide, silicon oxide, described relatively principal constituent total amount, and described minor component is with its standard substance Co separately
2O
3, Bi
2O
3, SiO
2The total content of meter is 5.6wt%～7.8wt%.
2, high-frequency nickel-copper-zinc ferrite according to claim 1 is characterized in that: described relatively principal constituent total amount, described minor component is with its standard substance Co separately
2O
3, Bi
2O
3, SiO
2The content of meter is respectively (wt%): Co
2O
3: 0.6～0.8, Bi
2O
3: 2.5～3.5, SiO
2: 2.5～3.5.
3, the preparation method of high-frequency nickel-copper-zinc ferrite 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;
(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 800 ℃～900 ℃, 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 1.0 μ m～1.5 μ m;
(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 ± 0.2) g/cm
3
(6) sintering: will go up blank sintering in air atmosphere that the step obtains, sintering temperature is controlled at 950 ℃～1000 ℃, is incubated 3 hours and carries out sintering, promptly gets described high-frequency nickel-copper-zinc ferrite goods through cooling again.
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