CN116375462A - Wide-temperature low-power-consumption manganese-zinc soft magnetic ferrite material and preparation method thereof - Google Patents
Wide-temperature low-power-consumption manganese-zinc soft magnetic ferrite material and preparation method thereof Download PDFInfo
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- CN116375462A CN116375462A CN202310282690.3A CN202310282690A CN116375462A CN 116375462 A CN116375462 A CN 116375462A CN 202310282690 A CN202310282690 A CN 202310282690A CN 116375462 A CN116375462 A CN 116375462A
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- 239000000463 material Substances 0.000 title claims abstract description 50
- 229910000859 α-Fe Inorganic materials 0.000 title claims abstract description 49
- WJZHMLNIAZSFDO-UHFFFAOYSA-N manganese zinc Chemical compound [Mn].[Zn] WJZHMLNIAZSFDO-UHFFFAOYSA-N 0.000 title claims abstract description 16
- 238000002360 preparation method Methods 0.000 title claims abstract description 9
- 239000000654 additive Substances 0.000 claims abstract description 14
- 230000000996 additive effect Effects 0.000 claims abstract description 13
- JEIPFZHSYJVQDO-UHFFFAOYSA-N iron(III) oxide Inorganic materials O=[Fe]O[Fe]=O JEIPFZHSYJVQDO-UHFFFAOYSA-N 0.000 claims abstract description 3
- 238000000034 method Methods 0.000 claims description 37
- 238000005245 sintering Methods 0.000 claims description 37
- 239000000843 powder Substances 0.000 claims description 33
- 238000000227 grinding Methods 0.000 claims description 16
- 239000002994 raw material Substances 0.000 claims description 13
- 238000001816 cooling Methods 0.000 claims description 12
- QVGXLLKOCUKJST-UHFFFAOYSA-N atomic oxygen Chemical compound [O] QVGXLLKOCUKJST-UHFFFAOYSA-N 0.000 claims description 10
- 238000002156 mixing Methods 0.000 claims description 10
- 239000001301 oxygen Substances 0.000 claims description 10
- 229910052760 oxygen Inorganic materials 0.000 claims description 10
- 239000002245 particle Substances 0.000 claims description 10
- 229910010413 TiO 2 Inorganic materials 0.000 claims description 9
- 239000007921 spray Substances 0.000 claims description 9
- 229910006404 SnO 2 Inorganic materials 0.000 claims description 8
- 229910000831 Steel Inorganic materials 0.000 claims description 8
- 239000010959 steel Substances 0.000 claims description 8
- 238000005507 spraying Methods 0.000 claims description 7
- 238000006243 chemical reaction Methods 0.000 claims description 6
- 239000004576 sand Substances 0.000 claims description 5
- IJGRMHOSHXDMSA-UHFFFAOYSA-N Atomic nitrogen Chemical compound N#N IJGRMHOSHXDMSA-UHFFFAOYSA-N 0.000 claims description 4
- 239000004372 Polyvinyl alcohol Substances 0.000 claims description 4
- 238000009826 distribution Methods 0.000 claims description 4
- 238000005469 granulation Methods 0.000 claims description 4
- 230000003179 granulation Effects 0.000 claims description 4
- 230000005484 gravity Effects 0.000 claims description 4
- 238000010438 heat treatment Methods 0.000 claims description 4
- 238000003825 pressing Methods 0.000 claims description 4
- 239000002002 slurry Substances 0.000 claims description 4
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims description 4
- 239000002518 antifoaming agent Substances 0.000 claims description 3
- 230000009467 reduction Effects 0.000 claims description 3
- 229910052757 nitrogen Inorganic materials 0.000 claims description 2
- 238000004321 preservation Methods 0.000 claims description 2
- 230000001681 protective effect Effects 0.000 claims description 2
- 238000012360 testing method Methods 0.000 description 29
- 230000008569 process Effects 0.000 description 27
- 238000004519 manufacturing process Methods 0.000 description 26
- ZKATWMILCYLAPD-UHFFFAOYSA-N niobium pentoxide Chemical compound O=[Nb](=O)O[Nb](=O)=O ZKATWMILCYLAPD-UHFFFAOYSA-N 0.000 description 18
- 230000000052 comparative effect Effects 0.000 description 12
- 229910004298 SiO 2 Inorganic materials 0.000 description 11
- 239000013078 crystal Substances 0.000 description 6
- 230000004907 flux Effects 0.000 description 5
- 230000009471 action Effects 0.000 description 3
- 239000003795 chemical substances by application Substances 0.000 description 3
- 239000004615 ingredient Substances 0.000 description 3
- 239000000203 mixture Substances 0.000 description 3
- VTYYLEPIZMXCLO-UHFFFAOYSA-L Calcium carbonate Chemical compound [Ca+2].[O-]C([O-])=O VTYYLEPIZMXCLO-UHFFFAOYSA-L 0.000 description 2
- GWEVSGVZZGPLCZ-UHFFFAOYSA-N Titan oxide Chemical compound O=[Ti]=O GWEVSGVZZGPLCZ-UHFFFAOYSA-N 0.000 description 2
- 230000002159 abnormal effect Effects 0.000 description 2
- 230000009286 beneficial effect Effects 0.000 description 2
- 230000000694 effects Effects 0.000 description 2
- 238000005265 energy consumption Methods 0.000 description 2
- 238000002844 melting Methods 0.000 description 2
- 230000035699 permeability Effects 0.000 description 2
- 230000001737 promoting effect Effects 0.000 description 2
- 229910001289 Manganese-zinc ferrite Inorganic materials 0.000 description 1
- 208000012868 Overgrowth Diseases 0.000 description 1
- 241001465382 Physalis alkekengi Species 0.000 description 1
- 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 description 1
- 230000004075 alteration Effects 0.000 description 1
- 230000008901 benefit Effects 0.000 description 1
- 229910000019 calcium carbonate Inorganic materials 0.000 description 1
- 235000010216 calcium carbonate Nutrition 0.000 description 1
- 239000013530 defoamer Substances 0.000 description 1
- 238000004134 energy conservation Methods 0.000 description 1
- 238000005516 engineering process Methods 0.000 description 1
- 238000009472 formulation Methods 0.000 description 1
- 230000009191 jumping Effects 0.000 description 1
- 239000011159 matrix material Substances 0.000 description 1
- 230000008018 melting Effects 0.000 description 1
- 238000012986 modification Methods 0.000 description 1
- 230000004048 modification Effects 0.000 description 1
- 231100000957 no side effect Toxicity 0.000 description 1
- 239000007858 starting material Substances 0.000 description 1
- 238000006467 substitution reaction Methods 0.000 description 1
- 239000004408 titanium dioxide Substances 0.000 description 1
- 239000011701 zinc Substances 0.000 description 1
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- H01F1/342—Oxides
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Abstract
The invention belongs to the technical field of soft magnetic ferrite materials, and discloses a wide-temperature low-power-consumption manganese zinc soft magnetic ferrite material, which comprises a ferrite material, wherein the ferrite material comprises a main component and an additive, wherein the main component comprises 52.5-54.5 mol% of Fe2O3, 9-12.5 mol% of ZnO and the balance of MnO; the additive comprises V2O5, caCO3, nb2O5, ta2O5, tiO2, snO2 and CoO, and the total additive amount is 5000-8500 ppm based on the total weight of the main components. The wide-temperature low-power-consumption manganese-zinc soft magnetic ferrite material and the preparation method thereof provided by the invention have the characteristics that the produced product has ultralow normal-temperature power consumption and also has lower power consumption at high temperature; the performance requirement of the design of the server power transformer can be better met.
Description
Technical Field
The invention belongs to the technical field of soft magnetic ferrite materials, and particularly relates to a wide-temperature low-power-consumption manganese-zinc soft magnetic ferrite material and a preparation method thereof.
Background
In the situation that the information is deeper and deeper in daily life, various electronic devices, such as televisions, computers, chargers, automobile electronic devices, energy-saving lamps and lanterns, etc., have come into the home, and a great deal of electric energy is consumed by the devices during operation, so that the energy consumption and efficiency of the devices have very important influence on energy conservation and emission reduction, and therefore, it is necessary to reduce the energy consumption of the electronic devices during operation.
In these devices, the loss of the switching power supply responsible for providing energy conversion has an important effect on the total loss, in general, the switching power supply is designed according to the temperature rise at the time of maximum power output, so that the switching transformer works near the valley point temperature of ferrite power loss, in the actual operation of the electronic device, the environment temperature and the condition of non-full-load operation have an important effect on the temperature rise of the actual operation of the switching power supply, which results in that the ferrite material in the switching power supply does not work in the state of minimum loss, therefore, it is very important to improve the temperature characteristic of ferrite loss, especially the server power supply, the higher requirement is put forth on the normal temperature consumption of ferrite, the conventional ferrite material controls the minimum loss to be about 90-100 ℃, the wide temperature ferrite material which is currently proposed by various manufacturers has the power loss of 350kW/m < 3 > at 25-120 ℃, the minimum power consumption at 100 ℃ is about 290kW/m < 3 >, and the power consumption at normal temperature is generally about 300kW/m < 3 >.
For example, an ultra-wide temperature low-loss high-magnetic flux density MnZn power ferrite with an authorized bulletin number of CN102693807A and a preparation method thereof, and a wide temperature MnZn power ferrite material with an authorized bulletin number of CN103588472A and a manufacturing method thereof, wherein the temperature range of the special attention of the two inventions is 25-140 ℃, and the normal temperature power consumption is generally about 300kW/m 3. The requirements of the server power supply for lower normal-temperature power consumption cannot be better met.
Disclosure of Invention
(one) solving the technical problems
In order to solve the problems in the background technology, the invention provides a wide-temperature low-power-consumption manganese-zinc soft magnetic ferrite material and a preparation method thereof, and the manganese-zinc soft magnetic ferrite material has the characteristics that the produced product has ultralow normal-temperature power consumption and also has lower power consumption at high temperature; the method has the advantage of meeting the performance requirements of the design of the power transformer of the server better.
(II) technical scheme
In order to achieve the above purpose, the present invention provides the following technical solutions: a wide-temperature low-power consumption Mn-Zn soft magnetic ferrite material comprises ferrite material, wherein the ferrite material comprises a main component and additives, and the main component comprises 52.5-54.5 mol% of Fe 2 O 3 ZnO with the content of 9-12.5 mol percent and MnO as the rest;
the additive comprises V 2 O 5 、CaCO 3 、Nb 2 O 5 、Ta 2 O 5 、TiO 2 、SnO 2 CoO, the total additive amount is 5000-8500 ppm based on the total weight of the main component.
The application also provides a preparation method of the wide-temperature low-power-consumption manganese zinc soft magnetic ferrite material, which comprises the following specific operation steps:
s1, mixing raw materials: mixing the main components according to the set proportion, using a conical stirrer for 15 minutes, and then vibrating and grinding through a vibrating and grinding machine to mix 3 raw materials;
s2, clamping pieces: putting the raw materials mixed by vibration grinding into a clamping piece of a clamping piece machine, enabling flaky powder materials which are discharged from the clamping piece machine to enter a 40-mesh vibrating screen, and enabling the screened fine powder materials to enter the clamping piece machine again;
s3, presintering: pre-burning coarse powder passing through a vibrating screen in a rotary kiln;
s4, sand grinding: firstly, mixing pre-sintered powder materials in a vibrating machine by using steel balls with different sizes according to a proportion, performing coarse grinding, and then adding additive combination, pure water, PVA and defoaming agent, and performing sand grinding;
s5, spray granulation: spraying and granulating the sanded slurry in a spraying tower;
s6, forming: pressing the spray granulated powder into green body by using a forming machine, sintering in a bell kiln at 1250-1300 ℃ for 4-8 hours, controlling the oxygen content to 3-4% in the heat preservation stage, and using a balance equation in the cooling stage atmosphere
Setting;
wherein the method comprises the steps of
Is the magnitude of the partial pressure of oxygen;
a, taking 7-8;
b is a constant, taking 14500;
t is the thermodynamic temperature;
in the cooling stage, the oxygen partial pressure in the sintering atmosphere is less than 2%, the rest atmosphere is a protective atmosphere which does not react with the material, and along with the reduction of the temperature, the oxygen partial pressure is smaller; and cooling to obtain the soft magnetic ferrite material.
Preferably, the bulk density of the mixed material in the step S1 is controlled to be 1.0+/-0.1 g/cm 3 。
Preferably, in the step S3, the presintering temperature is 900-1050 ℃, the presintering time is 40-70 minutes, and the powder is subjected to preliminary chemical reaction to partially generate ferrite.
Preferably, in the step S4, the diameters of the steel balls with different sizes are 25mm and 15mm respectively when the vibrator coarsely grinds, the number ratio of the two is 5:5, the diameters of the steel balls used for sanding are 4.5mm and 6.5mm respectively, and the number ratio of the two is 5:5.
Preferably, the bulk specific gravity of the powder in the step S5 is controlled to be 1.35-1.48 g/cm < 3 >, and the particle distribution is required to be 60-200 meshes and is more than or equal to 85%.
Preferably, in the step S6, pure nitrogen is introduced after 600 ℃ in the heating process, the oxygen content in the furnace is reduced to below 0.05% at about 800 ℃, the heating rate after 1000 ℃ to 1300 ℃ is controlled to be 1.5 to 3.5 ℃/min, and the atmosphere balance equation is that
The value a of (2) is set between 7.65 and 7.95, and the value a at the temperature of 1200 ℃,1100 ℃ and 1000 ℃ is corrected according to the actual atmosphere content of the sintering furnace, the corrected value is within +/-0.03, the cooling rate of 1200 ℃ to 1100 ℃ is controlled between 1.3 ℃ and 2.0 ℃/min, and the temperature is kept for 2 hours
Since Co2+ has positive magnetocrystalline anisotropy constant K1, the ferrite matrix can be compensated, K1 is close to zero in a wide temperature range, the temperature characteristic of the ferrite material is improved, and especially the power consumption at normal temperature is reduced;
the total additive amount is 2000-8500 ppm, and the excessive or the too low additive amount is unfavorable for ferrite materials to form uniform grains, clear grain boundaries and air holesMicrostructure with low rate; siO (SiO) 2 、V 2 O 5 The sintering temperature can be effectively reduced by promoting the growth of crystal grains, but overgrowth of the crystal grains is caused by excessively high addition, so that the sintering density can be reduced, and the power consumption loss and the saturation magnetic flux density are affected; caCO (CaCO) 3 Is intensively distributed on grain boundary and can be combined with SiO 2 The reaction forms a high-resistance grain boundary, so that the eddy current loss of ferrite can be obviously reduced; nb (Nb) 2 O 5 、Ta 2 O 5 Has the function of preventing the growth of the crystal grains, and can avoid the abnormal growth of the crystal grains; tiO (titanium dioxide) 2 、SnO 2 The ferrite can enter a crystal lattice, the content of Fe < 2+ > in the ferrite can be adjusted, electrons are prevented from jumping between Fe < 2+ > and Fe < 3+ >, the resistivity in the crystal lattice is improved, the power loss is improved, meanwhile, the magnetocrystalline anisotropy constant K1 and the magnetostriction coefficient lambda s of the ferrite can be influenced, the valley point temperature can be adjusted, the initial permeability is improved, and the normal-temperature power consumption is reduced;
to form a uniform and dense grain structure, it is necessary to suppress abnormal growth of grains while promoting grain growth, and a high melting point oxide Nb 2 O 5 And Ta 2 O 5 Sum of addition of (C) and low-melting point oxide SiO 2 And V 2 O 5 The ratio of the total addition amount of (2) is controlled to be between 0.03 and 0.1, preferably between 0.03 and 0.06, which can effectively promote the saturation magnetic flux density and improve the power loss at high temperature, and the addition weight ratio of CoO is between 0.25 and 0.75, preferably between 0.35 and 0.55 for improving the power loss in a wide temperature range, because at 100kHz/200mT, the power loss is composed of hysteresis loss and eddy current loss, the hysteresis loss is dominant at low temperature, and the eddy current loss is dominant at high temperature;
to reduce the sintering temperature, siO is added at the same time 2 And V 2 O 5 The total addition amount of the two fluxing agents is 300-1000 ppm, because excessive addition of any one fluxing agent can lead grains to overgrow, but can reduce sintering density, affect power consumption loss and saturation magnetic flux density, but the addition within a certain range has no side effect, and the simultaneous addition of the two fluxing agents can play a role in improving superposition and obviously reduce sinteringThe junction temperature obviously improves the high-temperature performance of the ferrite material, and simultaneously, the saturation magnetic flux density and the initial magnetic permeability are not deteriorated.
Preferably, the loss of the prepared manganese-zinc ferrite material is less than 220kW/m < 3 > at 25 ℃ under the test conditions of 100KHz and 200 mT;
the loss at 100 ℃ is less than 280kW/m < 3 >;
the loss at 140 ℃ is less than 350kW/m < 3 >.
(III) beneficial effects
Compared with the prior art, the invention has the following beneficial effects:
the wide-temperature low-power-consumption manganese-zinc soft magnetic ferrite material and the preparation method thereof provided by the invention have the characteristics that the produced product has ultralow normal-temperature power consumption and also has lower power consumption at high temperature; the performance requirement of the design of the server power transformer can be better met.
Detailed Description
The following description of the technical solutions in the embodiments of the present invention will be clear and complete, and it is obvious that the described embodiments are only some embodiments of the present invention, but not all embodiments. All other embodiments, which can be made by those skilled in the art based on the embodiments of the invention without making any inventive effort, are intended to be within the scope of the invention.
Example 1:
the starting material consisting of 52.5mol% Fe2O3, 35mol% MnO,12.5mol% ZnO was operated as follows:
(1) Mixing the raw materials: mixing the main components according to the set proportion, using a conical stirrer for 15 minutes, and then performing vibration grinding through a vibration grinder to fully mix 3 raw materials, wherein the apparent density is controlled within 1.0+/-0.1 g/cm < 3 >;
(2) Clamping piece: and (3) putting the raw materials mixed by the vibration mill into a clamping piece of a clamping piece machine, enabling flaky powder materials which are discharged from the clamping piece machine to enter a 40-mesh vibration sieve, and enabling the sieved fine powder to enter the clamping piece machine again.
(3) Presintering: coarse powder passing through the vibrating screen enters a rotary kiln for presintering. The presintering temperature is 900-1050 ℃, the presintering time is 40-70 minutes, and the powder is subjected to preliminary chemical reaction to partially generate ferrite;
(4) And (5) sanding: pre-sintered powder is firstly mixed and coarsely ground in a vibrating machine by using steel balls with different sizes according to a proportion to form small particle powder with the average particle size less than or equal to 2.5 mu m, then additive combination, pure water, PVA and defoamer are added, and then sand grinding is carried out, so that the particle size of the powder is kept between 0.7 and 1.2 mu m;
(5) And (3) spray granulation: spraying and granulating the sanded slurry in a spray tower, wherein the loose specific gravity of the powder is controlled to be 1.35-1.48 g/cm < 3 >, and the particle distribution is required to be more than or equal to 85% from 60 meshes to 200 meshes;
(6) Pressing the spray granulated powder into a green body by using a forming machine, controlling the density of the green body within 2.95-3.05g/cm < 3 >, sintering for 4-8 hours in a bell kiln at 1250-1300 ℃, setting the atmosphere of a cooling section by using a balance equation, and cooling to obtain the soft magnetic ferrite material, wherein the soft magnetic ferrite material is tested for power consumption at 25 ℃ and 100 ℃ and 140 ℃ by using a SY-8218 type B-H tester at 100Hz and 200 mT. The formulation and test results are shown in Table 1, and are the same as below.
Example 2:
the formula is as follows: 53.5mol% Fe 2 O 3 35mol% MnO and 11.5mol% ZnO, and the production process, sintering process and test conditions are the same as those of example 1.
Example 3:
the formula is as follows: 54.1mol% Fe 2 O 3 36.9mol% MnO and 9mol% ZnO, and the production process, sintering process and test conditions were the same as those of example 1.
Example 4:
the formula is as follows: 54.5mol% Fe 2 O 3 36mol% MnO and 9.5mol% ZnO, and the production process, sintering process and test conditions were the same as those of example 1. The manufacturing process, sintering process and test conditions were the same as in example 1.
Comparative example 1:
the formula is as follows: 54.4mol% Fe 2 O 3 23.1mol% MnO,17.6mol% ZnO, manufacturing process, sintering process and test stripThe piece is the same as in example 1. The manufacturing process, sintering process and test conditions were the same as in example 1.
Comparative example 2:
the formula is as follows: 56.2mol% Fe 2 O 3 33.9mol% MnO and 9.9mol% ZnO, and the production process, sintering process and test conditions were the same as those of example 1. The manufacturing process, sintering process and test conditions were the same as in example 1.
Comparative example 3:
the formula is as follows: 53.5mol% Fe 2 O 3 31.2mol% MnO and 15.3mol% ZnO, and the production process, sintering process and test conditions are the same as those of example 1. The manufacturing process, sintering process and test conditions were the same as in example 1.
Comparative example 4:
fe with the formula of 51.0mol percent 2 O 3 39.5mol% MnO and 9.5mol% ZnO, and the production process, sintering process and test conditions were the same as those of example 1. The manufacturing process, sintering process and test conditions are the same as those of example 1
Comparative example 5:
the formula is as follows: 52.0mol% Fe 2 O 3 34.9mol% MnO and 13.1mol% ZnO, and the production process, sintering process and test conditions were the same as those of example 1. The manufacturing process, sintering process and test conditions were the same as in example 1.
Comparative example 6:
the formula is as follows: 54.2mol% Fe 2 O 3 37mol% MnO and 8.8mol% ZnO, and the production process, sintering process and test conditions are the same as those of example 1. The manufacturing process, sintering process and test conditions were the same as in example 1.
TABLE 1
Example 5:
will consist of 52.5mol% Fe 2 O 3 35.0mol percent of MnO and 12.5mol percent of ZnO, and the raw materials are prepared according to the following steps:
(1) Mixing the raw materials: mixing the main components according to the set proportion, using a conical stirrer for 15 minutes, and then performing vibration grinding through a vibration grinder to fully mix 3 raw materials, wherein the apparent density is controlled within 1.0+/-0.1 g/cm < 3 >;
(2) Clamping piece: and (3) putting the raw materials mixed by the vibration mill into a clamping piece of a clamping piece machine, enabling flaky powder materials which are discharged from the clamping piece machine to enter a 40-mesh vibration sieve, and enabling the sieved fine powder to enter the clamping piece machine again.
(3) Presintering: coarse powder passing through the vibrating screen enters a rotary kiln for presintering. The presintering temperature is 900-1050 ℃, the presintering time is 40-70 minutes, and the powder is subjected to preliminary chemical reaction to partially generate ferrite;
(4) And (5) sanding: firstly, pre-sintered powder is mixed and coarsely ground in a vibrating machine by using steel balls with different sizes according to a proportion to form small particle powder with average particle size less than or equal to 2.5um, and then auxiliary components (ppm) are added into the pre-sintered material by taking the mass of the pre-sintered powder as a reference: 400ppm CaCO3, 3500ppm Co 2 O 3 500ppm TiO 2 300ppm Nb2O5, 300ppm V 2 O 5 Adding pure water, PVA and defoaming agent, and then sanding to keep the particle size of the powder between 0.7 and 1.2 mu m;
(5) And (3) spray granulation: spraying and granulating the sanded slurry in a spraying tower, and controlling the loose specific gravity of the powder;
at 1.35-1.48 g/cm3, the particle distribution is required to be more than or equal to 85% from 60 meshes to 200 meshes;
(6) Pressing the spray granulated powder into a green body by using a forming machine, controlling the density of the green body within 2.95-3.05g/cm < 3 >, sintering for 4-8 hours in a bell kiln at 1250-1300 ℃, setting the atmosphere of a cooling section by using a balance equation, cooling to obtain the soft magnetic ferrite material, and testing the power consumption at 25 ℃ and 100 ℃ and 140 ℃ by using a SY-8218 type B-H tester at 100Hz and 200mT, wherein the auxiliary components and the test results are shown in Table 2 and are the same as below.
Example 6:
CaCO with 200ppm auxiliary component 3 4500ppm Co 2 O 3 1500ppm TiO 2 200ppm Nb2O5. 900ppm V 2 O 5 Ta of 100ppm 2 O 5 1000ppm SnO 2 100ppm of SiO 2 The manufacturing process, sintering process and test conditions were the same as in example 5.
Example 7:
CaCO with auxiliary component changed to 500ppm 3 5500ppm Co 2 O 3 300ppm Nb2O5, 350ppm V 2 O 5 Ta of 300ppm 2 O 5 500ppm SnO 2 50ppm of SiO 2 The manufacturing process, sintering process and test conditions were the same as in example 5.
Example 8:
auxiliary ingredient was changed to 600ppm CaCO 3 4000ppm Co 2 O 3 500ppm TiO 2 250ppm Nb2O5, 400ppm V 2 O 5 Ta of 250ppm 2 O 5 500ppm SnO 2 100ppm of SiO 2 The manufacturing process, sintering process and test conditions were the same as in example 5.
Comparative example 7:
CaCO with auxiliary component changed to 400ppm 3 Co of 2000ppm 2 O 3 1000ppm TiO 2 250ppm Nb2O5, 100ppm SiO 2 The manufacturing process, sintering process and test conditions were the same as in example 5.
Comparative example 8:
CaCO with auxiliary component changed to 300ppm 3 5000ppm Co 2 O 3 1000ppm TiO 2 V at 100ppm 2 O 5 Ta of 250ppm 2 O 5 1500ppm SnO 2 50ppm of SiO 2 The manufacturing process, sintering process and test conditions were the same as in example 5.
Comparative example 9:
CaCO with auxiliary component changed to 350ppm 3 1000ppm Co 2 O 3 100ppm Nb2O5. Ta of 100ppm 2 O 5 V of 150ppm 2 O 5 20ppm of SiO 2 The manufacturing process, sintering process and test conditions were the same as in example 5.
Comparative example 10:
auxiliary ingredient was changed to 550ppm CaCO 3 3000ppm Co 2 O 3 500ppm Nb2O5. Ta of 550ppm 2 O 5 500ppm SnO 2 V at 250ppm 2 O 5 30ppm of SiO 2 The manufacturing process, sintering process and test conditions were the same as in example 5.
Comparative example 11:
auxiliary ingredient was changed to 600ppm CaCO 3 5000ppm Co 2 O 3 550ppm Nb2O5. 1500ppm TiO 2 Ta of 500ppm 2 O 5 SnO of 1000ppm 2 900ppm V 2 O 5 150ppm of SiO 2 The manufacturing process, sintering process and test conditions were the same as in example 5.
Comparative example 12:
CaCO with auxiliary component changed to 350ppm 3 4000ppm Co 2 O 3 250ppm Nb2O5. 2000ppm TiO 2 Ta of 150ppm 2 O 5 SnO of 1500ppm 2 800ppm V 2 O 5 250ppm of SiO 2 The manufacturing process, sintering process and test conditions were the same as in example 5.
TABLE 2
It is noted that relational terms such as first and second, and the like are used solely to distinguish one entity or action from another entity or action without necessarily requiring or implying any actual such relationship or order between such entities or actions. Moreover, the terms "comprises," "comprising," or any other variation thereof, are intended to cover a non-exclusive inclusion, such that a process, method, article, or apparatus that comprises a list of elements does not include only those elements but may include other elements not expressly listed or inherent to such process, method, article, or apparatus.
Although embodiments of the present invention have been shown and described, it will be understood by those skilled in the art that various changes, modifications, substitutions and alterations can be made therein without departing from the principles and spirit of the invention, the scope of which is defined in the appended claims and their equivalents.
Claims (7)
1. A wide-temperature low-power consumption manganese zinc soft magnetic ferrite material is characterized in that: the ferrite material comprises a main component and an additive, wherein the main component comprises 52.5-54.5 mol% of Fe2O3, 9-12.5 mol% of ZnO and the balance of MnO;
the additive comprises V 2 O 5 、CaCO 3 、Nb 2 O 5 、Ta 2 O 5 、TiO 2 、SnO 2 CoO, the total additive amount is 5000-8500 ppm based on the total weight of the main component.
2. A preparation method of a wide-temperature low-power-consumption manganese-zinc soft magnetic ferrite material is characterized by comprising the following steps: the specific operation steps are as follows:
s1, mixing raw materials: mixing the main components according to the set proportion, using a conical stirrer for 15 minutes, and then vibrating and grinding through a vibrating and grinding machine to mix 3 raw materials;
s2, clamping pieces: putting the raw materials mixed by vibration grinding into a clamping piece of a clamping piece machine, enabling flaky powder materials which are discharged from the clamping piece machine to enter a 40-mesh vibrating screen, and enabling the screened fine powder materials to enter the clamping piece machine again;
s3, presintering: pre-burning coarse powder passing through a vibrating screen in a rotary kiln;
s4, sand grinding: firstly, mixing pre-sintered powder materials in a vibrating machine by using steel balls with different sizes according to a proportion, performing coarse grinding, and then adding additive combination, pure water, PVA and defoaming agent, and performing sand grinding;
s5, spray granulation: spraying and granulating the sanded slurry in a spraying tower;
s6, forming: pressing the spray granulated powder into green body by using a forming machine, sintering in a bell kiln at 1250-1300 ℃ for 4-8 hours, controlling the oxygen content to 3-4% in the heat preservation stage, and using a balance equation in the cooling stage atmosphere
Setting;
wherein the method comprises the steps of
Is the magnitude of the partial pressure of oxygen;
a, taking 7-8;
b is a constant, taking 14500;
t is the thermodynamic temperature;
in the cooling stage, the oxygen partial pressure in the sintering atmosphere is less than 2%, the rest atmosphere is a protective atmosphere which does not react with the material, and along with the reduction of the temperature, the oxygen partial pressure is smaller; and cooling to obtain the soft magnetic ferrite material.
3. The method for preparing the wide-temperature low-power-consumption manganese-zinc soft magnetic ferrite material according to claim 1, which is characterized by comprising the following steps: the bulk density of the mixed material in the step S1 is controlled to be 1.0+/-0.1 g/cm 3 。
4. The method for preparing the wide-temperature low-power-consumption manganese-zinc soft magnetic ferrite material according to claim 1, which is characterized by comprising the following steps: and in the step S3, the presintering temperature is 900-1050 ℃, the presintering time is 40-70 minutes, and the powder is subjected to preliminary chemical reaction to partially generate ferrite.
5. The method for preparing the wide-temperature low-power-consumption manganese-zinc soft magnetic ferrite material according to claim 1, which is characterized by comprising the following steps: in the step S4, the diameters of steel balls with different sizes are 25mm and 15mm respectively in rough grinding of the vibrator, the number ratio of the two is 5:5, the diameters of steel balls used in sanding are 4.5mm and 6.5mm respectively, and the number ratio of the two is 5:5.
6. The method for preparing the wide-temperature low-power-consumption manganese-zinc soft magnetic ferrite material according to claim 1, which is characterized by comprising the following steps: in the step S5, the loose specific gravity of the powder is controlled to be 1.35-1.48 g/cm < 3 >, and the particle distribution is required to be 60-200 meshes and is more than or equal to 85%.
7. The method for preparing the wide-temperature low-power-consumption manganese-zinc soft magnetic ferrite material according to claim 1, which is characterized by comprising the following steps: in the step S6, pure nitrogen is introduced after 600 ℃ in the heating process, the oxygen content in the furnace is reduced to below 0.05% at about 800 ℃, the heating rate after 1000 ℃ to 1300 ℃ is controlled to be 1.5 to 3.5 ℃/min, and the temperature is controlled in an atmosphere balance equation
The value a of (2) is set between 7.65 and 7.95, and the value a at the temperature of 1200 ℃ and the temperature of 1100 ℃ and the temperature of 1000 ℃ is corrected according to the actual atmosphere content of the sintering furnace, the corrected value is within +/-0.03, the cooling rate of 1200 ℃ to 1100 ℃ is controlled between 1.3 ℃ and 2.0 ℃/min, and the temperature is kept for 2 hours.
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