CN114085086A - Sintering process of iron-rich ultrahigh Bs material - Google Patents
Sintering process of iron-rich ultrahigh Bs material Download PDFInfo
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- CN114085086A CN114085086A CN202111286806.8A CN202111286806A CN114085086A CN 114085086 A CN114085086 A CN 114085086A CN 202111286806 A CN202111286806 A CN 202111286806A CN 114085086 A CN114085086 A CN 114085086A
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- XEEYBQQBJWHFJM-UHFFFAOYSA-N Iron Chemical compound [Fe] XEEYBQQBJWHFJM-UHFFFAOYSA-N 0.000 title claims abstract description 89
- 238000005245 sintering Methods 0.000 title claims abstract description 57
- 229910052742 iron Inorganic materials 0.000 title claims abstract description 40
- 239000000463 material Substances 0.000 title claims abstract description 37
- 238000000034 method Methods 0.000 title claims abstract description 18
- 239000001301 oxygen Substances 0.000 claims abstract description 62
- 229910052760 oxygen Inorganic materials 0.000 claims abstract description 62
- QVGXLLKOCUKJST-UHFFFAOYSA-N atomic oxygen Chemical compound [O] QVGXLLKOCUKJST-UHFFFAOYSA-N 0.000 claims abstract description 52
- 238000006243 chemical reaction Methods 0.000 claims abstract description 17
- 238000001816 cooling Methods 0.000 claims abstract description 17
- 238000004321 preservation Methods 0.000 claims abstract description 15
- 229910052761 rare earth metal Inorganic materials 0.000 claims abstract description 15
- 238000010438 heat treatment Methods 0.000 claims abstract description 14
- 238000009770 conventional sintering Methods 0.000 claims abstract description 8
- 150000002910 rare earth metals Chemical class 0.000 claims abstract description 8
- 238000003746 solid phase reaction Methods 0.000 claims abstract description 8
- CWYNVVGOOAEACU-UHFFFAOYSA-N Fe2+ Chemical compound [Fe+2] CWYNVVGOOAEACU-UHFFFAOYSA-N 0.000 claims description 21
- 239000003638 chemical reducing agent Substances 0.000 claims description 9
- 239000007789 gas Substances 0.000 claims description 8
- 239000000470 constituent Substances 0.000 claims description 7
- 238000000280 densification Methods 0.000 claims description 7
- 229910052759 nickel Inorganic materials 0.000 claims description 7
- 238000000354 decomposition reaction Methods 0.000 claims description 6
- 239000000853 adhesive Substances 0.000 claims 1
- 230000001070 adhesive effect Effects 0.000 claims 1
- 230000004907 flux Effects 0.000 abstract description 11
- JEIPFZHSYJVQDO-UHFFFAOYSA-N iron(III) oxide Inorganic materials O=[Fe]O[Fe]=O JEIPFZHSYJVQDO-UHFFFAOYSA-N 0.000 abstract description 10
- 229910000859 α-Fe Inorganic materials 0.000 abstract description 7
- 229910001289 Manganese-zinc ferrite Inorganic materials 0.000 abstract description 5
- 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 abstract description 5
- 239000011162 core material Substances 0.000 abstract description 5
- 239000011701 zinc Substances 0.000 abstract description 4
- 230000003197 catalytic effect Effects 0.000 abstract description 2
- 239000011230 binding agent Substances 0.000 description 6
- 238000012360 testing method Methods 0.000 description 3
- VTLYFUHAOXGGBS-UHFFFAOYSA-N Fe3+ Chemical compound [Fe+3] VTLYFUHAOXGGBS-UHFFFAOYSA-N 0.000 description 2
- UQSXHKLRYXJYBZ-UHFFFAOYSA-N Iron oxide Chemical compound [Fe]=O UQSXHKLRYXJYBZ-UHFFFAOYSA-N 0.000 description 2
- 230000006698 induction Effects 0.000 description 2
- 229910052751 metal Inorganic materials 0.000 description 2
- 239000002184 metal Substances 0.000 description 2
- 229910000976 Electrical steel Inorganic materials 0.000 description 1
- 229910045601 alloy Inorganic materials 0.000 description 1
- 239000000956 alloy Substances 0.000 description 1
- 230000002708 enhancing effect Effects 0.000 description 1
- 239000011019 hematite Substances 0.000 description 1
- 229910052595 hematite Inorganic materials 0.000 description 1
- LIKBJVNGSGBSGK-UHFFFAOYSA-N iron(3+);oxygen(2-) Chemical compound [O-2].[O-2].[O-2].[Fe+3].[Fe+3] LIKBJVNGSGBSGK-UHFFFAOYSA-N 0.000 description 1
- 150000002739 metals Chemical class 0.000 description 1
- 239000000203 mixture Substances 0.000 description 1
- 239000012071 phase Substances 0.000 description 1
- 239000011029 spinel Substances 0.000 description 1
- 229910052596 spinel Inorganic materials 0.000 description 1
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Abstract
The invention discloses a sintering process of an iron-rich ultrahigh Bs material, which comprises the following steps of 1) carrying out sufficient solid-phase reaction on the iron-rich ultrahigh Bs material at a high-temperature section, and adding higher oxygen content and other parameters; step 2) performing deoxidation reaction on the excessive Fe, and providing low oxygen in a heating section; 3) carrying out a heat preservation section, carrying out catalytic deoxidation reaction, and setting a constant value on the temperature; 4) the cooling section ensures a low-oxygen environment, the cooling section is adjusted according to an atmosphere formula, the oxygen content of the cooling section is lower than that of a conventional sintering process, and the whole sintering density is improved; 5) adding rare earth metal elements and the iron-rich ultrahigh Bs material to sinter, wherein the sintering steps are according to the steps 1) to 4). The excessive Fe2O3 of the manganese-zinc ferrite is fully discharged with oxygen and reduced, the manganese-zinc ferrite sintered body has enough sintering density, Mn-Zn ferrite with high magnetic flux density is obtained, and the saturation magnetic flux density of the magnetic core material is effectively improved.
Description
Technical Field
The invention relates to the field of sintering, in particular to a sintering process of an iron-rich ultrahigh Bs material.
Background
With the widespread use of portable electronic devices, LSI (large scale integrated circuit) in various electronic apparatuses is being highly integrated, multi-functionalized and speeded up, and the power supply system thereof is being developed to be light, thin, small and efficient, and a power transformer is required to be able to carry a larger power density, that is, to further increase the saturation magnetic flux density of the magnetic core material. To meet the above requirements, many manufacturers use magnetic cores made of soft magnetic metals such as silicon steel and amorphous alloys to obtain higher saturation magnetic flux density. However, they have problems such as high cost, low resistance, and inability to be used at high frequencies. In contrast, soft magnetic ferrite has a higher electrical resistance than soft magnetic metal and can be used at high frequencies, and among them, Mn — Zn ferrite has a higher saturation magnetic flux density and is inexpensive and is rapidly gaining popularity. In order to obtain Mn-Zn ferrite with high magnetic flux density, the content of iron oxide in the formula is increased; a suitable sintering process is also required. When the content of Fe2O3 exceeds 60mol%, the ferrite is commonly called iron-rich manganese-zinc ferrite; if there is no proper sintering process, that is, if the spinel reaction in which Fe2O3 is reduced to feo. Fe2O3 during sintering releases oxygen of Fe2O3, and if Fe2O3 is excessive, the release of oxygen becomes insufficient, and Fe2O3 easily remains as heterogeneous phase (hematite), and high magnetic properties cannot be obtained.
In the published document CN 200610051942-a sintering method of MNZN ferrite with high saturation magnetic flux density, a reducing agent is not utilized to deoxidize Fe sufficiently to form ferrous iron, so that the magnetic flux density cannot be guaranteed in the subsequent sintering process.
Disclosure of Invention
In order to solve the problems, the invention discloses a sintering process of an iron-rich ultrahigh Bs material, which is used for improving the saturation magnetic flux density of a magnetic core material.
The technical scheme of the invention is as follows: the sintering process of the iron-rich ultrahigh Bs material comprises the following steps:
step 1) carrying out sufficient solid-phase reaction on the iron-rich super Bs material at a high-temperature stage, and adding higher oxygen content and other parameters to obtain a ferrous sintered body;
step 2) carrying out deoxidation reaction on the Fe greatly excessive in the temperature rise section in the step 1) to form ferrous iron, wherein the low oxygen is provided in the temperature rise section;
step 3) carrying out heat preservation section setting on the iron-rich super Bs material, utilizing a reducing agent to catalyze the deoxidation reaction, carrying out fixed value setting on the temperature, and adjusting the oxygen content and other parameters according to the sintering condition;
step 4), the cooling section ensures a low-oxygen environment, the cooling section is adjusted according to an atmosphere formula, the content of ferrous iron is controlled, the oxygen content is lower than that of a conventional sintering process, and the whole sintering density is improved;
and 5) adding rare earth metal elements and the iron-rich ultrahigh Bs material to sinter, wherein the sintering step is according to the steps 1) to 4).
Further, in the step 1), on the one hand, densification is carried out, on the other hand, slow temperature rise is carried out, the temperature rise speed is 10 ℃/h, the temperature is 760 ℃ -1350 ℃, the oxygen content is 15-21%, and other parameters are f =100-200kHz, Bm =200-400mT, and N =5-13 Ts.
Further, the temperature in the step 2) is 25-380 ℃, and the oxygen content is 0.12-0.50%.
Furthermore, C, H generated by heating and decomposing the PVA binder in the step 3) is used as a main constituent element reducing gas to promote the reduction of ferric iron into ferrous iron in a low-oxygen environment; in order to ensure that the reducing agent can sufficiently catalyze the reduction of the ferrous iron by the ferric iron, the combination of reducing gas and oxygen in the air is avoided and the catalytic effect is reduced under the low-oxygen environment, the constant temperature of the heat preservation section is 1350 ℃, the oxygen content is 0.5-1.10%, and other parameters are f =50-150kHz, Bm =100-300mT and N =4-8 Ts.
Further, the sintered density in the step 4) is 4.93-4.95 kg/m3, and the equilibrium atmosphere formula LgPO2= 4.0447-9738.5/(t + 273).
Further, the rare earth elements in step 5) were C, Ni and Li.
The invention has the advantages that: the excessive Fe2O3 of the manganese-zinc ferrite is fully discharged with oxygen and reduced, the manganese-zinc ferrite sintered body has enough sintering density, Mn-Zn ferrite with high magnetic flux density is obtained, and the saturation magnetic flux density of the magnetic core material is effectively improved.
Detailed Description
For the purpose of enhancing an understanding of the present invention, the following detailed description will describe specific embodiments of the present invention, which are given by way of illustration only and are not intended to limit the scope of the present invention.
The sintering process of the iron-rich ultrahigh Bs material comprises the following steps:
step 1) carrying out sufficient solid-phase reaction on the iron-rich super Bs material in a high-temperature section, on one hand, carrying out densification, on the other hand, slowly heating up, wherein the heating-up speed is 10 ℃/h, the temperature is 760-1350 ℃, the oxygen content is 15-21%, and other parameters are f = 100-;
step 2) carrying out deoxidation reaction on the Fe greatly excessive in the temperature rise section in the step 1) to form ferrous iron, wherein the temperature rise section provides low oxygen, the temperature is 25-380 ℃, and the oxygen content is 0.12-0.50%;
step 3) carrying out heat preservation section setting on the iron-rich super Bs material, catalyzing the deoxidation reaction by using a reducing agent, using C, H generated by volatilization heating decomposition of a PVA binder as a main constituent element reducing gas, setting the constant value of the heat preservation section at 1350 ℃, setting the oxygen content at 0.5-1.10%, setting other parameters at f =50-150kHz, Bm =100-300mT and N =4-8Ts, setting the constant value of the temperature, and adjusting the oxygen content and other parameters according to the sintering condition;
step 4), ensuring a low-oxygen environment in the cooling section, adjusting the cooling section according to an atmosphere formula, balancing the atmosphere formula LgPO2= 4.0447-9738.5/(t + 273), controlling the content of ferrous iron, wherein the oxygen content is lower than that of a conventional sintering process, the sintering density is 4.93-4.95 kg/m3, and the whole sintering density is improved;
and 5) adding rare earth metal elements and the iron-rich ultrahigh Bs material together for sintering, wherein the rare earth elements are C, Ni and Li, and the sintering steps are as per steps 1) to 4).
Example 1
Step 1) carrying out sufficient solid-phase reaction on the iron-rich super Bs material at a high-temperature section, on one hand, carrying out densification, on the other hand, slowly heating up, wherein the heating up speed is 10 ℃/h, the temperature is 760 ℃, the oxygen content is 15%, and other parameters are f =100kHz, Bm =200mT and N =5Ts, so as to obtain a sintered body of ferrous iron;
step 2) performing deoxidation reaction on the Fe greatly excessive in the temperature rise section in the step 1) to form ferrous iron, wherein the temperature rise section provides low oxygen, the temperature is 25 ℃, and the oxygen content is 0.12 percent;
step 3) setting a heat preservation section of the iron-rich super Bs material, catalyzing the deoxidation reaction by using a reducing agent, setting the temperature by using C, H generated by volatilization heating decomposition of a PVA binder as a main constituent element reducing gas, setting the constant value of the heat preservation section to 1350 ℃, setting the oxygen content to 0.5 percent, setting other parameters to f =50kHz, Bm =100mT and N =4Ts, and adjusting the oxygen content and other parameters according to the sintering condition;
step 4), ensuring a low-oxygen environment in the cooling section, adjusting the cooling section according to an atmosphere formula, controlling the content of ferrous iron by a balanced atmosphere formula LgPO2= 4.0447-9738.5/(50 + 273), wherein the oxygen content is lower than that of a conventional sintering process, the sintering density is 4.93kg/m3, and the whole sintering density is improved;
and 5) adding rare earth metal elements and the iron-rich ultrahigh Bs material together for sintering, wherein the rare earth elements are C, Ni and Li, and the sintering steps are as per steps 1) to 4).
Example 2
Step 1) carrying out sufficient solid-phase reaction on the iron-rich ultra Bs material at a high-temperature section, on one hand, carrying out densification, on the other hand, slowly heating up, wherein the heating-up speed is 10 ℃/h, the temperature is 800 ℃, the oxygen content is 17%, and other parameters are f =120kHz, Bm =250mT and N =8Ts, so as to obtain a sintered body of divalent iron;
step 2) carrying out deoxidation reaction on the Fe greatly excessive in the temperature rise section in the step 1) to form ferrous iron, wherein the temperature rise section provides low oxygen, the temperature is 80 ℃, and the oxygen content is 0.30%;
step 3) carrying out heat preservation section setting on the iron-rich super Bs material, catalyzing the deoxidation reaction by using a reducing agent, using C, H generated by volatilization heating decomposition of a PVA binder as a main constituent element reducing gas, setting the constant value of the heat preservation section at 1350 ℃, setting the oxygen content at 0.8 percent and setting other parameters at f =80kHz, Bm =150mT and N =5Ts, setting the constant value of the temperature, and adjusting the oxygen content and other parameters according to the sintering condition;
step 4), ensuring a low-oxygen environment in the cooling section, adjusting the cooling section according to an atmosphere formula, controlling the content of ferrous iron by a balanced atmosphere formula LgPO2= 4.0447-9738.5/(80 + 273), wherein the oxygen content is lower than that of a conventional sintering process, the sintering density is 4.93kg/m3, and the whole sintering density is improved;
and 5) adding rare earth metal elements and the iron-rich ultrahigh Bs material together for sintering, wherein the rare earth elements are C, Ni and Li, and the sintering steps are as per steps 1) to 4).
Example 3
Step 1) carrying out sufficient solid-phase reaction on the iron-rich super Bs material at a high-temperature section, on one hand, carrying out densification, on the other hand, slowly heating up, wherein the heating-up speed is 10 ℃/h, the temperature is 1000 ℃, the oxygen content is 15-21%, and other parameters are f =180kHz, Bm =300mT and N =8Ts, so as to obtain a ferrous sintered body;
step 2) carrying out deoxidation reaction on the Fe greatly excessive in the temperature rise section in the step 1) to form ferrous iron, wherein the temperature rise section provides low oxygen, the temperature is 200 ℃, and the oxygen content is 0.4%;
step 3) carrying out heat preservation section setting on the iron-rich super Bs material, catalyzing the deoxidation reaction by using a reducing agent, using C, H generated by volatilization heating decomposition of a PVA binder as a main constituent element reducing gas, setting the constant value of the heat preservation section at 1350 ℃, setting the oxygen content at 0.80 percent and setting the other parameters at f =100kHz, Bm =200mT and N =7Ts, setting the constant value of the temperature, and adjusting the oxygen content and other parameters according to the sintering condition;
step 4), ensuring a low-oxygen environment in the cooling section, adjusting the cooling section according to an atmosphere formula, controlling the content of ferrous iron by a balanced atmosphere formula LgPO2= 4.0447-9738.5/(100 + 273), wherein the oxygen content is lower than that of a conventional sintering process, the sintering density is 4.94kg/m3, and the whole sintering density is improved;
and 5) adding rare earth metal elements and the iron-rich ultrahigh Bs material together for sintering, wherein the rare earth elements are C, Ni and Li, and the sintering steps are as per steps 1) to 4).
Example 4
Step 1) carrying out sufficient solid-phase reaction on the iron-rich ultra Bs material at a high-temperature section, on one hand, carrying out densification, on the other hand, slowly heating up, wherein the heating-up speed is 10 ℃/h, the temperature is 1350 ℃, the oxygen content is 21%, and other parameters are f =200kHz, Bm =400mT and N =13Ts, so as to obtain a sintered body of divalent iron;
step 2) carrying out deoxidation reaction on the Fe greatly excessive in the temperature rise section in the step 1) to form ferrous iron, wherein the low oxygen is provided in the temperature rise section, the temperature is 380 ℃, and the oxygen content is 0.50%;
step 3) carrying out heat preservation section setting on the iron-rich super Bs material, catalyzing the deoxidation reaction by using a reducing agent, using C, H generated by volatilization heating decomposition of a PVA binder as a main constituent element reducing gas, setting the constant value of the heat preservation section at 1350 ℃, setting the oxygen content at 1.10 percent and setting other parameters at f =150kHz, Bm =300mT and N =8Ts, setting the constant value of the temperature, and adjusting the oxygen content and other parameters according to the sintering condition;
step 4), ensuring a low-oxygen environment in the cooling section, adjusting the cooling section according to an atmosphere formula, controlling the content of ferrous iron by a balanced atmosphere formula LgPO2= 4.0447-9738.5/(100 + 273), wherein the oxygen content is lower than that of a conventional sintering process, the sintering density is 4.95 kg/m3, and the whole sintering density is improved;
and 5) adding rare earth metal elements and the iron-rich ultrahigh Bs material together for sintering, wherein the rare earth elements are C, Ni and Li, and the sintering steps are as per steps 1) to 4).
The final iron-rich ultra-high Bs material composition, as shown in the table below; wt.%
Pressing the sample ring according to the specification of phi 25mm multiplied by 10mm multiplied by 5mm, sintering according to the sintering process, and then using an E4980A precision LCR meter. At normal temperature, according to the conditions: f =1kHz, I =2mA, N =15Ts, test μ I; using a SY8258 type B-H tester, according to the conditions: f =100kHz, Bm =200mT, N =5Ts testing power consumption at 25-120 ℃; according to the conditions: f =0.05kHz, H =1194A/m Bs at 100 ℃ test 25 ℃;
saturation magnetic induction bs (mt) 590 at 25 ℃; saturation magnetic induction bs (mt) 502 at 100 ℃; in sum, the project has completed the intended goal.
Claims (6)
1. The sintering process of the iron-rich ultrahigh Bs material is characterized by comprising the following steps of:
step 1) carrying out sufficient solid-phase reaction on the iron-rich super Bs material at a high-temperature stage, and adding higher oxygen content and other parameters to obtain a ferrous sintered body;
step 2) carrying out deoxidation reaction on the Fe greatly excessive in the temperature rise section in the step 1) to form ferrous iron, wherein the low oxygen is provided in the temperature rise section;
step 3) carrying out heat preservation section setting on the iron-rich super Bs material, utilizing a reducing agent to catalyze the deoxidation reaction, carrying out fixed value setting on the temperature, and adjusting the oxygen content and other parameters according to the sintering condition;
step 4), the cooling section ensures a low-oxygen environment, the cooling section is adjusted according to an atmosphere formula, the content of ferrous iron is controlled, the oxygen content is lower than that of a conventional sintering process, and the whole sintering density is improved;
and 5) adding rare earth metal elements and the iron-rich ultrahigh Bs material to sinter, wherein the sintering step is according to the steps 1) to 4).
2. The sintering process of the ultra-high Bs material rich in iron as claimed in claim 1, wherein: in the step 1), on the one hand, densification is carried out, on the other hand, slow temperature rise is carried out, the temperature rise speed is 10 ℃/h, the temperature is 760-1350 ℃, the oxygen content is 15-21%, and other parameters are f =100-200kHz, Bm =200-400mT and N =5-13 Ts.
3. The sintering process of the ultra-high Bs material rich in iron as claimed in claim 1, wherein: the temperature in the step 2) is 25-380 ℃, and the oxygen content is 0.12-0.50%.
4. The sintering process of the ultra-high Bs material rich in iron as claimed in claim 1, wherein: c, H generated by the heating decomposition of the PVA adhesive is used as main constituent reducing gas in the step 3), the constant value temperature of the heat preservation section is 1350 ℃, the oxygen content is 0.5-1.10%, and other parameters are f =50-150kHz, Bm =100-300mT and N =4-8 Ts.
5. The sintering process of the ultra-high Bs material rich in iron as claimed in claim 1, wherein: the sintering density in the step 4) is 4.93-4.95 kg/m3, and the equilibrium atmosphere formula LgPO2= 4.0447-9738.5/(t + 273).
6. The sintering process of the ultra-high Bs material rich in iron as claimed in claim 1, wherein: the rare earth elements in the step 5) are C, Ni and Li.
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Citations (8)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| GB1004748A (en) * | 1963-08-05 | 1965-09-15 | Philips Electronic Associated | Improvements in methods of manufacturing sintered ferrite bodies |
| JPH06333726A (en) * | 1993-05-21 | 1994-12-02 | Minebea Co Ltd | Manufacture of high-density mn-zn ferrite |
| CN1890197A (en) * | 2003-12-24 | 2007-01-03 | 日立金属株式会社 | Ferrite sintered compact and method for producing the same, and electronic parts using the same |
| CN101090016A (en) * | 2006-06-14 | 2007-12-19 | 横店集团东磁有限公司 | Sintering method of high saturation magnetic flux density MnZn ferrite |
| JP2008214161A (en) * | 2007-03-07 | 2008-09-18 | Hitachi Metals Ltd | Ni BASED SPINEL FERRITE SINTERED COMPACT AND METHOD FOR PRODUCING THE SAME |
| JP2012180258A (en) * | 2011-03-03 | 2012-09-20 | Tdk Corp | MnZn-BASED FERRITE POWDER, MnZn-BASED FERRITE GRANULES, METHOD OF MANUFACTURING MnZn-BASED FERRITE CORE AND MnZn-BASED FERRITE CORE |
| CN103467106A (en) * | 2013-09-03 | 2013-12-25 | 宝钢磁业（江苏）有限公司 | Sintering process of ferrite with high magnetic permeability |
| CN103570363A (en) * | 2013-11-13 | 2014-02-12 | 宝钢磁业（江苏）有限公司 | High-performance power manganese zinc ferrite sintering process |
-
2021
- 2021-11-02 CN CN202111286806.8A patent/CN114085086A/en active Pending
Patent Citations (8)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| GB1004748A (en) * | 1963-08-05 | 1965-09-15 | Philips Electronic Associated | Improvements in methods of manufacturing sintered ferrite bodies |
| JPH06333726A (en) * | 1993-05-21 | 1994-12-02 | Minebea Co Ltd | Manufacture of high-density mn-zn ferrite |
| CN1890197A (en) * | 2003-12-24 | 2007-01-03 | 日立金属株式会社 | Ferrite sintered compact and method for producing the same, and electronic parts using the same |
| CN101090016A (en) * | 2006-06-14 | 2007-12-19 | 横店集团东磁有限公司 | Sintering method of high saturation magnetic flux density MnZn ferrite |
| JP2008214161A (en) * | 2007-03-07 | 2008-09-18 | Hitachi Metals Ltd | Ni BASED SPINEL FERRITE SINTERED COMPACT AND METHOD FOR PRODUCING THE SAME |
| JP2012180258A (en) * | 2011-03-03 | 2012-09-20 | Tdk Corp | MnZn-BASED FERRITE POWDER, MnZn-BASED FERRITE GRANULES, METHOD OF MANUFACTURING MnZn-BASED FERRITE CORE AND MnZn-BASED FERRITE CORE |
| CN103467106A (en) * | 2013-09-03 | 2013-12-25 | 宝钢磁业（江苏）有限公司 | Sintering process of ferrite with high magnetic permeability |
| CN103570363A (en) * | 2013-11-13 | 2014-02-12 | 宝钢磁业（江苏）有限公司 | High-performance power manganese zinc ferrite sintering process |
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