CN117125969A - Iron-deficiency formula soft magnetic manganese zinc ferrite material and preparation method and application thereof - Google Patents
Iron-deficiency formula soft magnetic manganese zinc ferrite material and preparation method and application thereof Download PDFInfo
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- 239000000463 material Substances 0.000 title claims abstract description 98
- 206010022971 Iron Deficiencies Diseases 0.000 title claims abstract description 48
- 229910001289 Manganese-zinc ferrite Inorganic materials 0.000 title claims abstract description 38
- JIYIUPFAJUGHNL-UHFFFAOYSA-N [O--].[O--].[O--].[O--].[O--].[O--].[O--].[O--].[O--].[O--].[O--].[O--].[O--].[O--].[O--].[O--].[O--].[O--].[O--].[O--].[Mn++].[Mn++].[Mn++].[Fe+3].[Fe+3].[Fe+3].[Fe+3].[Fe+3].[Fe+3].[Fe+3].[Fe+3].[Fe+3].[Fe+3].[Zn++].[Zn++] Chemical compound [O--].[O--].[O--].[O--].[O--].[O--].[O--].[O--].[O--].[O--].[O--].[O--].[O--].[O--].[O--].[O--].[O--].[O--].[O--].[O--].[Mn++].[Mn++].[Mn++].[Fe+3].[Fe+3].[Fe+3].[Fe+3].[Fe+3].[Fe+3].[Fe+3].[Fe+3].[Fe+3].[Fe+3].[Zn++].[Zn++] JIYIUPFAJUGHNL-UHFFFAOYSA-N 0.000 title claims abstract description 38
- 238000002360 preparation method Methods 0.000 title claims abstract description 17
- 230000035699 permeability Effects 0.000 claims abstract description 26
- 229910015902 Bi 2 O 3 Inorganic materials 0.000 claims abstract description 7
- XEEYBQQBJWHFJM-UHFFFAOYSA-N iron Substances [Fe] XEEYBQQBJWHFJM-UHFFFAOYSA-N 0.000 claims description 32
- QVGXLLKOCUKJST-UHFFFAOYSA-N atomic oxygen Chemical compound [O] QVGXLLKOCUKJST-UHFFFAOYSA-N 0.000 claims description 22
- 239000001301 oxygen Substances 0.000 claims description 22
- 229910052760 oxygen Inorganic materials 0.000 claims description 22
- 239000000843 powder Substances 0.000 claims description 19
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims description 17
- IJGRMHOSHXDMSA-UHFFFAOYSA-N nitrogen Substances N#N IJGRMHOSHXDMSA-UHFFFAOYSA-N 0.000 claims description 12
- 238000005245 sintering Methods 0.000 claims description 10
- 238000002156 mixing Methods 0.000 claims description 9
- 238000000498 ball milling Methods 0.000 claims description 7
- 229910052757 nitrogen Inorganic materials 0.000 claims description 7
- 230000002950 deficient Effects 0.000 claims description 4
- 229910052742 iron Inorganic materials 0.000 claims description 4
- 238000000034 method Methods 0.000 claims description 4
- QJGQUHMNIGDVPM-UHFFFAOYSA-N nitrogen group Chemical group [N] QJGQUHMNIGDVPM-UHFFFAOYSA-N 0.000 claims description 2
- 238000003825 pressing Methods 0.000 claims description 2
- 238000010304 firing Methods 0.000 claims 1
- 229910000859 α-Fe Inorganic materials 0.000 abstract description 34
- 239000011701 zinc Substances 0.000 abstract description 30
- 230000006698 induction Effects 0.000 abstract description 2
- 239000004615 ingredient Substances 0.000 abstract 1
- 239000000306 component Substances 0.000 description 60
- 239000000203 mixture Substances 0.000 description 16
- 239000004576 sand Substances 0.000 description 15
- 239000002994 raw material Substances 0.000 description 12
- 239000008367 deionised water Substances 0.000 description 10
- 229910021641 deionized water Inorganic materials 0.000 description 10
- 230000000052 comparative effect Effects 0.000 description 7
- 229910001053 Nickel-zinc ferrite Inorganic materials 0.000 description 6
- 238000012360 testing method Methods 0.000 description 6
- 238000007599 discharging Methods 0.000 description 5
- 238000001035 drying Methods 0.000 description 5
- 238000003801 milling Methods 0.000 description 5
- 238000007873 sieving Methods 0.000 description 5
- 238000005303 weighing Methods 0.000 description 5
- 230000004907 flux Effects 0.000 description 3
- 238000009472 formulation Methods 0.000 description 3
- 239000000654 additive Substances 0.000 description 2
- 230000000996 additive effect Effects 0.000 description 2
- 239000003153 chemical reaction reagent Substances 0.000 description 2
- 230000007547 defect Effects 0.000 description 2
- 238000005469 granulation Methods 0.000 description 2
- 230000003179 granulation Effects 0.000 description 2
- 230000004048 modification Effects 0.000 description 2
- 238000012986 modification Methods 0.000 description 2
- 238000000465 moulding Methods 0.000 description 2
- 230000009286 beneficial effect Effects 0.000 description 1
- 239000008358 core component Substances 0.000 description 1
- 238000001514 detection method Methods 0.000 description 1
- 238000011161 development Methods 0.000 description 1
- 239000012776 electronic material Substances 0.000 description 1
- 230000006872 improvement Effects 0.000 description 1
- 239000007788 liquid Substances 0.000 description 1
- QELJHCBNGDEXLD-UHFFFAOYSA-N nickel zinc Chemical compound [Ni].[Zn] QELJHCBNGDEXLD-UHFFFAOYSA-N 0.000 description 1
- 230000001105 regulatory effect Effects 0.000 description 1
- 238000011160 research Methods 0.000 description 1
Classifications
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- C—CHEMISTRY; METALLURGY
- C04—CEMENTS; CONCRETE; ARTIFICIAL STONE; CERAMICS; REFRACTORIES
- C04B—LIME, MAGNESIA; SLAG; CEMENTS; COMPOSITIONS THEREOF, e.g. MORTARS, CONCRETE OR LIKE BUILDING MATERIALS; ARTIFICIAL STONE; CERAMICS; REFRACTORIES; TREATMENT OF NATURAL STONE
- C04B35/00—Shaped ceramic products characterised by their composition; Ceramics compositions; Processing powders of inorganic compounds preparatory to the manufacturing of ceramic products
- C04B35/01—Shaped ceramic products characterised by their composition; Ceramics compositions; Processing powders of inorganic compounds preparatory to the manufacturing of ceramic products based on oxide ceramics
- C04B35/26—Shaped ceramic products characterised by their composition; Ceramics compositions; Processing powders of inorganic compounds preparatory to the manufacturing of ceramic products based on oxide ceramics based on ferrites
- C04B35/2658—Other ferrites containing manganese or zinc, e.g. Mn-Zn ferrites
-
- H—ELECTRICITY
- H01—ELECTRIC ELEMENTS
- H01F—MAGNETS; INDUCTANCES; TRANSFORMERS; SELECTION OF MATERIALS FOR THEIR MAGNETIC PROPERTIES
- H01F1/00—Magnets or magnetic bodies characterised by the magnetic materials therefor; Selection of materials for their magnetic properties
- H01F1/01—Magnets or magnetic bodies characterised by the magnetic materials therefor; Selection of materials for their magnetic properties of inorganic materials
- H01F1/03—Magnets or magnetic bodies characterised by the magnetic materials therefor; Selection of materials for their magnetic properties of inorganic materials characterised by their coercivity
- H01F1/12—Magnets or magnetic bodies characterised by the magnetic materials therefor; Selection of materials for their magnetic properties of inorganic materials characterised by their coercivity of soft-magnetic materials
- H01F1/34—Magnets or magnetic bodies characterised by the magnetic materials therefor; Selection of materials for their magnetic properties of inorganic materials characterised by their coercivity of soft-magnetic materials non-metallic substances, e.g. ferrites
- H01F1/342—Oxides
- H01F1/344—Ferrites, e.g. having a cubic spinel structure (X2+O)(Y23+O3), e.g. magnetite Fe3O4
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- Engineering & Computer Science (AREA)
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- Ceramic Engineering (AREA)
- Manufacturing & Machinery (AREA)
- Materials Engineering (AREA)
- Structural Engineering (AREA)
- Organic Chemistry (AREA)
- Dispersion Chemistry (AREA)
- Power Engineering (AREA)
- Soft Magnetic Materials (AREA)
- Magnetic Ceramics (AREA)
Abstract
The invention discloses an iron-deficiency formula soft magnetic manganese zinc ferrite material, a preparation method and application thereof. The iron-deficiency soft magnetic manganese zinc ferrite material comprises main components and auxiliary components, wherein the main components comprise the following components in percentage by mole: fe (Fe) 2 O 3 43.5 to 48.5mol percent, 30 to 35mol percent of MnO and the balance of ZnO; the minor ingredients comprise the following components: caCO (CaCO) 3 、CuO、ZrO 2 、Bi 2 O 3 And MoO 3 . The iron-deficiency soft magnetic Mn-Zn ferrite material of the invention has low mole percent (less than 50%) of Fe 2 O 3 The magnetic permeability cutoff frequency of the Mn-Zn ferrite material is improved by matching with MnO and ZnO as main components so as to improve the attenuation of the magnetic permeability in a high frequency band; simultaneously combined with CaCO 3 、CuO、ZrO 2 、Bi 2 O 3 、MoO 3 To promote grain growth and improve Mn-Zn ferriteThe magnetic permeability of the material is ensured to have higher saturation magnetic induction intensity and higher Curie temperature.
Description
Technical Field
The invention relates to the technical field of electronic materials, in particular to an iron-deficiency soft magnetic manganese zinc ferrite material, a preparation method and application thereof.
Background
With the continuous development of the electronic industry, the performance requirements on electronic components are also increasing. Ferrite cores are also being used as one of the core components of electronic components, and their electromagnetic performance index is being improved and optimized continuously. The high-permeability Mn-Zn ferrite material is widely applied to pulse transformers in the fields of electromagnetic interference noise (EMI) resistance, ISDN, LAN, WAN, automobile electronics and the like because of high initial permeability and low loss; however, the magnetic cores in these fields are limited by the cutoff frequency of the high permeability material itself, and generally operate under low frequency and weak field conditions, which is difficult to be applied to high frequency environments. The existing ferrite core in the high-frequency environment generally adopts nickel-zinc ferrite material, but the cost of the nickel-zinc ferrite material is relatively high, and the initial permeability and the Curie temperature of the nickel-zinc ferrite material are low.
In order to solve the problem of low magnetic permeability of nickel-zinc ferrite materials, nickel-zinc ferrite materials are continuously improved to improve the magnetic permeability. For example, the prior art discloses a high-permeability broadband high-impedance nickel-zinc soft magnetic ferrite material, which comprises a main material and an additive, wherein the main material comprises the following components in percentage by mole: fe (Fe) 2 O 3 45-55 mol%, znO 25-35 mol%, niO 10-20 mol% and CuO 5-10 mol%, and the additive comprises the following components in percentage by mol: mgO 0.5-5 mol%, co 2 O 3 0.5 to 9.5mol percent of CaCO 30.5 to 5mol percent, and the content of ZnO in the main material is improved and Fe is regulated and controlled 2 O 3 The molar ratio of the ferrite to ZnO is matched with CuO to improve the magnetic permeability of the ferrite, but the magnetic permeability only reaches 952-968, and the magnetic permeability needs to be further improved.
Disclosure of Invention
The invention aims to overcome the defects and defects that the existing high-permeability manganese-zinc ferrite material cannot be applied to high frequency bands and the permeability of broadband high-impedance nickel-zinc ferrite material is poor, and provides an iron-deficiency soft magnetic manganese-zinc ferrite material.
The invention further aims to provide a preparation method of the iron-deficiency soft magnetic manganese zinc ferrite material.
The invention also aims to provide the application of the iron-deficiency soft magnetic manganese zinc ferrite material in the preparation of electronic components.
It is a further object of the present invention to provide a pulse transformer.
The above object of the present invention is achieved by the following technical scheme:
the invention provides an iron-deficiency soft magnetic manganese zinc ferrite material, which comprises a main component and an auxiliary component, wherein the main component comprises the following components in percentage by mole:
Fe 2 O 3 43.5 to 48.5mol percent, 30 to 35mol percent of MnO and the balance of ZnO;
the auxiliary components comprise the following components in percentage by weight relative to the total weight of the main components:
CaCO 3 0.3 to 0.7 weight percent, 0.2 to 0.4 weight percent of CuO and ZrO 2 0 to 0.08 weight percent of Bi 2 O 3 0.03 to 0.1 weight percent of MoO 3 0.03 to 0.1wt%.
The inventors found through research that Fe in Mn-Zn ferrite material 2 O 3 When the mole percentage content of the magnetic permeability is reduced to below 50%, the cutoff frequency of the magnetic permeability can be obviously improved, so that the attenuation of the magnetic permeability in a high frequency band is improved; at the same time combine CaCO with specific content 3 And ZrO(s) 2 The temperature coefficient of the Mn-Zn ferrite material can be reduced, the grain boundary resistivity can be increased, the loss of the Mn-Zn ferrite material can be reduced, the grain growth can be uniform, and the electrical characteristics of the Mn-Zn ferrite material can be further improved.
Preferably, the main component comprises Fe in mole percent 2 O 3 46.5 to 47.9mol percent, 31.8 to 33.7mol percent of MnO and the balance of ZnO.
Specifically, the main components may be: fe (Fe) 2 O 3 46.5mol%, mnO 33.7mol% and ZnO in balance; or Fe (Fe) 2 O 3 47.0mol%, mnO 32.7mol% and ZnO in balance; or Fe (Fe) 2 O 3 47.3mol%, mnO 32.3mol% and ZnO in balance; or Fe (Fe) 2 O 3 47.90mol%, mnO 31.8mol% and ZnO in balance.
Specifically, the iron-deficiency soft magnetic manganese zinc ferrite material has 1MHz impedance Z which is more than or equal to 20Ω,25MHz impedance Z which is more than or equal to 80Ω, and 100MHz impedance Z which is more than or equal to 150Ω at 25 ℃, and the test conditions are H25 15 x 8, 1Ts phi 0.5mm L=160 mm.
Specifically, the initial magnetic permeability mu i of the iron-deficiency formula soft magnetic manganese zinc ferrite material is more than or equal to 3000 under the conditions of 5 ℃,10 KHz and 0.05V; the density rho of the soft magnetic Mn-Zn ferrite material of the iron-deficiency formula is more than or equal to 4.9g/cm 3 Curie temperature Tc>130 ℃; the saturation magnetic flux density Bs of the iron-deficiency formula soft magnetic manganese zinc ferrite material at 25 ℃ is more than or equal to 400mT.
The invention also provides a preparation method of the iron-deficiency soft magnetic manganese zinc ferrite material, which comprises the following steps:
s1, proportioning the content of the main components, and uniformly mixing;
s2, placing the mixed main components in the S1 into a presintering furnace for presintering treatment to form presintering materials;
s3, mixing the presintered material in the S2 with the auxiliary components, adding water at the same time, and performing secondary ball milling to obtain ground powder with the granularity of 1.00-1.40 mu m;
s4, granulating and pressing the fine powder in the S3 to obtain the product with the density of 3.00-3.05 g/cm 3 Is a green body of (c);
s5, sintering the green body in the S4 in an atmosphere furnace at 1250-1350 ℃ to obtain the iron-deficiency soft magnetic manganese zinc ferrite material.
Preferably, the temperature of the pre-sintering treatment in S2 is 850-950 ℃ and the time is 2.5-3.5 h.
Specifically, the oxygen partial pressure in the sintering atmosphere in S5 is 2.0% -4.5%, and the balance is nitrogen partial pressure.
The application of the iron-deficiency soft magnetic manganese zinc ferrite material in the preparation of electronic components is also within the protection scope of the invention.
The invention also protects a pulse transformer prepared from the iron-deficiency soft magnetic manganese zinc ferrite material.
Compared with the prior art, the invention has the beneficial effects that:
the iron-deficiency soft magnetic Mn-Zn ferrite material of the invention has low mole percent (less than 50%) of Fe 2 O 3 The magnetic permeability cutoff frequency of the Mn-Zn ferrite material is improved by matching with MnO and ZnO as main components so as to improve the attenuation of the magnetic permeability in a high frequency band; simultaneously combined with CaCO 3 、CuO、ZrO 2 、Bi 2 O 3 、MoO 3 So as to promote grain growth, improve the magnetic permeability of the Mn-Zn ferrite material and ensure that the Mn-Zn ferrite material has higher saturation induction intensity and higher Curie temperature.
Detailed Description
The invention will be further described with reference to the following specific embodiments, but the examples are not intended to limit the invention in any way. Raw materials reagents used in the examples of the present invention are conventionally purchased raw materials reagents unless otherwise specified.
Example 1
An iron-deficiency formula soft magnetic Mn-Zn ferrite material comprises the following main components in percentage by weight: fe (Fe) 2 O 3 46.5mo1%; mnO is 33.4 mol 1%; znO was 20.1% at 1%; the composition also comprises the following auxiliary components relative to the total weight of the main components: caCO (CaCO) 3 0.55wt% of CuO, 0.25wt% of ZrO 2 0.04wt%, bi 2 O 3 0.04wt%, moO 3 0.04wt%.
The soft magnetic manganese zinc ferrite material with the iron-deficiency formula can be prepared by the following preparation method:
s1, weighing main component raw materials, placing the main component raw materials into a sand mill, adding deionized water in a certain proportion for mixing and crushing, operating the planetary ball mill for 30 minutes, and drying water at 180 ℃ after discharging;
s2, firstly, sieving the dried powder with a 40-mesh screen, then placing the powder into a presintering furnace, and then preserving heat for 2.5 hours at 880 ℃ to perform presintering treatment to form presintering materials;
s3, adding auxiliary components into the presintered material, putting the presintered material into a sand mill, adding deionized water for secondary sand milling, wherein the planetary ball milling time is 80 minutes, and the granularity of the powder is controlled to be 1.00-1.40 mu m;
s4, manually granulating in a laboratory and then forming a phi 25.00 multiplied by 15.00 multiplied by 7.50mm standard sample ring, wherein the density of the green body of the sample ring is 3.10g/cm 3 Left and right;
s5, in the atmosphere of oxygen and nitrogen with a certain proportion, the temperature is kept for 6 hours at 1320 ℃, the oxygen partial pressure during sintering is 3.5 percent, and the mixture is cooled to the room temperature under the control of proper oxygen partial pressure (the oxygen partial pressure defaults to the routine industry).
Example 2
An iron-deficiency formula soft magnetic Mn-Zn ferrite material comprises the following main components in percentage by weight: fe (Fe) 2 O 3 46.5mo1%; mnO 33.7mol 1%; znO was 19.8 mol 1%; the composition also comprises the following auxiliary components relative to the total weight of the main components: caCO (CaCO) 3 0.55wt% of CuO, 0.25wt% of ZrO 2 0.04wt%, bi 2 O 3 0.04wt%, moO 3 0.04wt%.
The soft magnetic manganese zinc ferrite material with the iron-deficiency formula can be prepared by the following preparation method:
s1, weighing main component raw materials, placing the main component raw materials into a sand mill, adding deionized water in a certain proportion for mixing and crushing, operating the planetary ball mill for 30 minutes, and drying water at 180 ℃ after discharging;
s2, firstly, sieving the dried powder with a 40-mesh screen, then placing the powder into a presintering furnace, and then preserving heat for 2.5 hours at 880 ℃ to perform presintering treatment to form presintering materials;
s3, adding auxiliary components into the presintered material, putting the presintered material into a sand mill, adding deionized water for secondary sand milling, wherein the planetary ball milling time is 80 minutes, and the granularity of the powder is controlled to be 1.00-1.40 mu m;
s4, manually granulating in a laboratory and then forming a phi 25.00 multiplied by 15.00 multiplied by 7.50mm standard sample ring, wherein the density of the green body of the sample ring is 3.10g/cm 3 Left and right;
s5, in the atmosphere of oxygen and nitrogen with a certain proportion, the temperature is kept for 6 hours at 1320 ℃, the oxygen partial pressure during sintering is 3.5 percent, and the mixture is cooled to the room temperature under the control of proper oxygen partial pressure (the oxygen partial pressure defaults to the routine industry).
Example 3
An iron-deficiency formula soft magnetic Mn-Zn ferrite material comprises the following main components in percentage by weight: fe (Fe) 2 O 3 47.0 m.o 1%; mnO is 33.5mo1%; znO is 19.5mo1%; the composition also comprises the following auxiliary components relative to the total weight of the main components: caCO (CaCO) 3 0.55wt% of CuO, 0.25wt% of ZrO 2 0.04wt%, bi 2 O 3 0.04wt%, moO 3 0.04wt%.
The soft magnetic manganese zinc ferrite material with the iron-deficiency formula can be prepared by the following preparation method:
s1, weighing main component raw materials, placing the main component raw materials into a sand mill, adding deionized water in a certain proportion for mixing and crushing, operating the planetary ball mill for 30 minutes, and drying water at 180 ℃ after discharging;
s2, firstly, sieving the dried powder with a 40-mesh screen, then placing the powder into a presintering furnace, and then preserving heat for 2.5 hours at 880 ℃ to perform presintering treatment to form presintering materials;
s3, adding auxiliary components into the presintered material, putting the presintered material into a sand mill, adding deionized water for secondary sand milling, wherein the planetary ball milling time is 80 minutes, and the granularity of the powder is controlled to be 1.00-1.40 mu m;
s4, manual granulation in a laboratory and then moldingStandard sample ring, sample ring green density of 3.10g/cm 3 Left and right;
s5, in the atmosphere of oxygen and nitrogen with a certain proportion, the temperature is kept for 6 hours at 1320 ℃, the oxygen partial pressure during sintering is 3.5 percent, and the mixture is cooled to the room temperature under the control of proper oxygen partial pressure (the oxygen partial pressure defaults to the routine industry).
Example 4
An iron-deficiency formula soft magnetic Mn-Zn ferrite material comprises the following main components in percentage by weight: fe (Fe) 2 O 3 47.2mo1%; mnO is 33.5mo1%; znO was 19.3 mol 1%; the composition also comprises the following auxiliary components relative to the total weight of the main components: caCO (CaCO) 3 0.55wt% of CuO, 0.25wt% of ZrO 2 0.04wt%, bi 2 O 3 0.04wt%, moO 3 0.04wt%.
The soft magnetic manganese zinc ferrite material with the iron-deficiency formula can be prepared by the following preparation method:
s1, weighing main component raw materials, placing the main component raw materials into a sand mill, adding deionized water in a certain proportion for mixing and crushing, operating the planetary ball mill for 30 minutes, and drying water at 180 ℃ after discharging;
s2, firstly, sieving the dried powder with a 40-mesh screen, then placing the powder into a presintering furnace, and then preserving heat for 2.5 hours at 880 ℃ to perform presintering treatment to form presintering materials;
s3, adding auxiliary components into the presintered material, putting the presintered material into a sand mill, adding deionized water for secondary sand milling, wherein the planetary ball milling time is 80 minutes, and the granularity of the powder is controlled to be 1.00-1.40 mu m;
s4, manual granulation in a laboratory and then moldingStandard sample ring, sample ring green density of 3.10g/cm 3 Left and right;
s5, in the atmosphere of oxygen and nitrogen with a certain proportion, the temperature is kept for 6 hours at 1320 ℃, the oxygen partial pressure during sintering is 3.5 percent, and the mixture is cooled to the room temperature under the control of proper oxygen partial pressure (the oxygen partial pressure defaults to the routine industry).
Example 5
An iron-deficiency formula soft magnetic Mn-Zn ferrite material comprises the following main components in percentage by weight: fe (Fe) 2 O 3 47.2mo1%; mnO is 33.5mo1%; znO was 19.3 mol 1%; the composition also comprises the following auxiliary components relative to the total weight of the main components: caCO (CaCO) 3 0.55wt% of CuO, 0.50wt% of ZrO 2 0.04wt%, bi 2 O 3 0.04wt%, moO 3 0.04wt%.
The soft magnetic manganese zinc ferrite material with the iron-deficiency formula can be prepared by the following preparation method:
s1, weighing main component raw materials, placing the main component raw materials into a sand mill, adding deionized water in a certain proportion for mixing and crushing, operating the planetary ball mill for 30 minutes, and drying water at 180 ℃ after discharging;
s2, firstly, sieving the dried powder with a 40-mesh screen, then placing the powder into a presintering furnace, and then preserving heat for 2.5 hours at 880 ℃ to perform presintering treatment to form presintering materials;
s3, adding auxiliary components into the presintered material, putting the presintered material into a sand mill, adding deionized water for secondary sand milling, wherein the planetary ball milling time is 80 minutes, and the granularity of the powder is controlled to be 1.00-1.40 mu m;
s4, manually granulating in a laboratory and then forming a phi 25.00 multiplied by 15.00 multiplied by 7.50mm standard sample ring, wherein the density of the green body of the sample ring is 3.10g/cm 3 Left and right;
s5, in the atmosphere of oxygen and nitrogen with a certain proportion, the temperature is kept for 6 hours at 1320 ℃, the oxygen partial pressure during sintering is 3.5 percent, and the mixture is cooled to the room temperature under the control of proper oxygen partial pressure (the oxygen partial pressure defaults to the routine industry).
Example 6
An iron-deficiency formula soft magnetic Mn-Zn ferrite material comprises the following main components in percentage by weight: fe (Fe) 2 O 3 43.5mo1%; mnO is 35mo1%; znO is 21.5mo1%; the composition also comprises the following auxiliary components relative to the total weight of the main components: caCO (CaCO) 3 0.1wt% of CuO, 0.4wt% of ZrO 2 0.08wt%, bi 2 O 3 0.1wt%, moO 3 0.1wt%.
The preparation method of the soft magnetic Mn-Zn ferrite material with the iron deficiency formula is the same as that of the example 1.
Comparative example 1
An iron-deficiency formula soft magnetic Mn-Zn ferrite material comprises the following main components in percentage by weight: fe (Fe) 2 O 3 40mo1%; mnO is 33.4 mol 1%; znO was 26.6mo1%; the composition also comprises the following auxiliary components relative to the total weight of the main components: caCO (CaCO) 3 0.55wt% of CuO, 0.25wt% of ZrO 2 0.04wt％，Bi 2 O 3 0.04wt%, moO 3 0.04wt%.
The preparation method of the soft magnetic Mn-Zn ferrite material with the iron deficiency formula is the same as that of the example 1.
Comparative example 2
A soft magnetic Mn-Zn ferrite material comprises the following componentsThe main components of the content are as follows: fe (Fe) 2 O 3 50mo1%; mnO is 33.4 mol 1%; znO was 16.6 mol 1%; the composition also comprises the following auxiliary components relative to the total weight of the main components: caCO (CaCO) 3 0.55wt% of CuO, 0.25wt% of ZrO 2 0.04wt％，Bi 2 O 3 0.04wt%, moO 3 0.04wt%.
The preparation method of the soft magnetic Mn-Zn ferrite material with the iron deficiency formula is the same as that of the example 1.
Result detection
(1) The iron-deficiency formulation soft magnetic manganese zinc ferrite materials of examples 1 to 6 and comparative examples 1 to 2 were subjected to density test by a liquid discharge method while the curie temperature, initial permeability and saturation magnetic flux density thereof were measured, and specific test results are shown in table 1.
TABLE 1 Curie temperature, density, initial permeability, and saturation magnetic flux Density of iron-deficiency formulated Soft magnetic manganese Zinc ferrite materials in examples 1-6 and comparative examples 1-2
(2) The iron-deficient formulation soft magnetic manganese zinc ferrite materials of examples 1 to 6 and comparative examples 1 to 2 were subjected to impedance testing using an HP4192A meter (test coil:10 Ts), the specific test results are shown in table 2:
table 2 resistance under different conditions of the iron deficiency formulation soft magnetic manganese zinc ferrite materials of examples 1 to 6 and comparative examples 1 to 2
As can be seen from the data in tables 1 and 2, the Curie temperature of the iron-deficiency soft magnetic Mn-Zn ferrite material of the invention reaches 102-134 ℃, the initial magnetic permeability mu i reaches 3007-3892, and meanwhile, the Z under the condition of 100Mhz is 238-278 omega, so that the iron-deficiency soft magnetic Mn-Zn ferrite material not only has excellent initial magnetic permeability, but also can be applied to high frequency bands, and has obvious advantages compared with the existing Mn-Zn ferrite material and nickel-Zn ferrite material.
As can be seen from comparative examples 1 and 2, when Fe in the main component of the soft magnetic Mn-Zn ferrite material 2 O 3 When the content of (2) is too low, although the application frequency band can be widened and the initial magnetic permeability can be improved to a certain extent, the Curie temperature can be reduced sharply; fe in main component of soft magnetic Mn-Zn ferrite material 2 O 3 When the content of (c) is too high, the initial permeability is low and cannot be applied to a high frequency band, although the curie temperature is high.
It is to be understood that the above examples of the present invention are provided by way of illustration only and not by way of limitation of the embodiments of the present invention. Other variations or modifications of the above teachings will be apparent to those of ordinary skill in the art. It is not necessary here nor is it exhaustive of all embodiments. Any modification, equivalent replacement, improvement, etc. which come within the spirit and principles of the invention are desired to be protected by the following claims.
Claims (10)
1. The iron-deficiency soft magnetic manganese zinc ferrite material comprises a main component and an auxiliary component, and is characterized by comprising the following components in percentage by mole:
Fe 2 O 3 43.5 to 48.5mol percent, 30 to 35mol percent of MnO and the balance of ZnO;
the auxiliary components comprise the following components in percentage by weight relative to the total weight of the main components:
CaCO 3 0.3 to 0.7 weight percent, 0.2 to 0.4 weight percent of CuO and ZrO 2 0 to 0.08 weight percent of Bi 2 O 3 0.03 to 0.1 weight percent of MoO 3 0.03 to 0.1wt%.
2. The iron-deficient soft magnetic manganese-zinc ferrite material according to claim 1, wherein the main component comprises Fe in mole percent 2 O 3 46.5 to47.9mol%, mnO 31.8-33.7 mol% and ZnO in balance.
3. The iron-deficiency type soft magnetic manganese zinc ferrite material according to claim 1, wherein the iron-deficiency type soft magnetic manganese zinc ferrite material has an impedance Z of 1MHz of 20 Ω or more, an impedance Z of 25MHz of 80 Ω or more, and an impedance Z of 100MHz of 150 Ω or more at 25 ℃.
4. The iron-deficiency soft magnetic manganese zinc ferrite material according to claim 3, wherein the initial magnetic permeability mui of the iron-deficiency soft magnetic manganese zinc ferrite material is more than or equal to 3000 under the conditions of 25 ℃,10 KHz and 0.05V.
5. The iron-deficiency soft magnetic manganese zinc ferrite material according to claim 1, wherein the density ρ of the iron-deficiency soft magnetic manganese zinc ferrite material is not less than 4.9g/cm 3 。
6. A method for preparing the iron-deficiency soft magnetic manganese zinc ferrite material according to any one of claims 1 to 5, which is characterized by comprising the following steps:
s1, proportioning the content of the main components, and uniformly mixing;
s2, placing the mixed main components in the S1 into a presintering furnace for presintering treatment to form presintering materials;
s3, mixing the presintered material in the S2 with the auxiliary components, adding water at the same time, and performing secondary ball milling to obtain ground powder with the granularity of 1.00-1.40 mu m;
s4, granulating and pressing the fine powder in the S3 to obtain the product with the density of 3.00-3.05 g/cm 3 Is a green body of (c);
s5, sintering the green body in the S4 in an atmosphere furnace at 1250-1350 ℃ to obtain the iron-deficiency soft magnetic manganese zinc ferrite material.
7. The method according to claim 6, wherein the temperature of the pre-firing treatment in S2 is 850 to 950 ℃ for 2.5 to 3.5 hours.
8. The method according to claim 6, wherein the partial pressure of oxygen in the sintering atmosphere in S5 is 2.0% to 4.5%, and the balance is nitrogen partial pressure.
9. Use of the iron-deficient soft magnetic manganese zinc ferrite material according to any one of claims 1 to 5 in the preparation of electronic components.
10. A pulse transformer comprising the iron-deficient soft magnetic manganese zinc ferrite material of any one of claims 1 to 5.
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