CN115716745A - Wide-temperature-range high-permeability manganese-zinc soft magnetic ferrite for automotive electronics and preparation method thereof - Google Patents
Wide-temperature-range high-permeability manganese-zinc soft magnetic ferrite for automotive electronics and preparation method thereof Download PDFInfo
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Abstract
The invention provides a wide-temperature-range high-permeability manganese-zinc soft magnetic ferrite for automotive electronics and a preparation method thereof, and relates to the technical field of magnetic materials. The Mn-Zn soft magnetic ferrite with wide temperature range and high magnetic conductivity for automobile electronics comprises main components and auxiliary components, wherein the main components comprise 48-50mo percent of Fe 2 O 3 10 to 12mol% of ZnO, the balance of Mn 3 O 4 The auxiliary components comprise: 0.2-0.3wt% of CaCO 3 、0.03～0.04wt％S iO 2 、0.02～0.04wt％T iO 2 And 0 to 0.02wt% of Al 2 O 3 (ii) a The preparation method of the manganese-zinc soft magnetic ferrite comprises the following specific steps: the method comprises the following steps: pretreatment: mixing the above Fe in proportion 2 O 3 ZnO and Mn 3 O 4 Putting the mixture into a ball mill for first ball milling processing, and adding equivalent deionized water in the ball milling process. By optimizing the composition proportion and the processing technology, the initial permeability of the material is stabilized above 5500, the temperature stability is high, the permeability change is small when the material is tested under the extreme temperature conditions of minus 50 ℃ and 120 ℃, and the comprehensive performance is very stable.
Description
Technical Field
The invention relates to the technical field of magnetic materials, in particular to a wide-temperature-range high-permeability manganese-zinc soft magnetic ferrite for automotive electronics and a preparation method thereof.
Background
The automobile electronic is a general term for automobile body electronic control devices and vehicle-mounted electronic control devices. The electronic control device for the automobile comprises an engine control system, a chassis control system and an electronic automobile body control system (electronic automobile body ECU). The most important role of automotive electronics is to improve the safety, comfort, economy and entertainment of automobiles. The electric control system is composed of sensors, a microprocessor MPU, an actuator, dozens or even hundreds of electronic components and parts thereof.
The automobile electronic product is an important component on an automobile, has an important effect on improving the comprehensive performance of the automobile, and is an electronic product which is arranged near an engine or in an engine room.
Therefore, we developed a new manganese-zinc soft magnetic ferrite with wide temperature range and high magnetic permeability for automobile electronics and a preparation method thereof.
Disclosure of Invention
Technical problem to be solved
Aiming at the defects of the prior art, the invention provides a wide-temperature-range high-permeability manganese-zinc soft magnetic ferrite for automobile electronics and a preparation method thereof, and solves the problem that most high-permeability materials are difficult to ensure the stability of automobile electronic products, so that the driving safety of automobiles is influenced.
(II) technical scheme
In order to achieve the purpose, the invention is realized by the following technical scheme: the Mn-Zn soft magnetic ferrite with wide temperature range and high magnetic conductivity for automobile electronics contains main component and auxiliary component, and the main component includes Fe content of 48-50mol% 2 O 3 10 to 12mol% of ZnO, the balance being Mn 3 O 4 The auxiliary components comprise: 0.2-0.3wt% of CaCO 3 、0.03～0.04wt％SiO 2 、0.02～0.04wt％TiO 2 And 0 to 0.02wt% of AL 2 O 3 ；
The preparation of the manganese-zinc soft magnetic ferrite comprises the following specific steps:
the method comprises the following steps: pretreatment: mixing the above Fe in proportion 2 O 3 ZnO and Mn 3 O 4 Putting the mixture into a ball mill for primary ball milling, and adding equivalent deionized water in the ball milling process;
step two: pre-burning: pre-drying the mixture prepared in the step one, and then conveying the mixture into a pre-sintering kiln for pre-sintering, wherein the pre-sintering temperature is controlled to be 1000-1100 ℃, and the temperature is kept for 2-3 hours;
step three: adding impurities: mixing CaCO 3 、SiO 2 、TiO 2 And AL 2 O 3 Adding the mixture into the mixture subjected to the pre-sintering in the second step in proportion;
step four: secondary treatment: performing secondary ball milling on the mixed material obtained in the third step, and adding deionized water according to the proportion of 1;
step five: secondary drying: drying the slurry obtained by the treatment in the fourth step to obtain a powdery material;
step six: and (3) pressing and forming: pressing and molding the powdery material by using a product mold;
step seven: sintering and forming: and (3) placing the pressed and molded material in a sintering furnace for sintering, controlling the sintering temperature at 1250-1400 ℃, and preserving heat for 8-10h.
Preferably, the ball milling time in the first step is controlled to be more than one hour.
Preferably, in the pre-burning process in the second step, nitrogen is introduced after the temperature is kept for 2 hours, and the temperature is kept for one hour under the condition of nitrogen.
Preferably, the time of the second ball milling in the fourth step is controlled to be 1.5-2h.
Preferably, the sintering in the seventh step is divided into three temperature stages, namely a low-temperature waste heat stage, a high-temperature sintering stage and a heat preservation stage.
Preferably, the temperature of the low-temperature waste heat stage is controlled to be 900-1200 ℃, the heating rate is 2.3-2.7 ℃/min, and the time is controlled to be 1-2h; the temperature of the high-temperature sintering stage is controlled to be 1200-1400 ℃, the heating rate is 0.8-0.9 ℃/min, and the time is controlled to be 2-4h; the temperature in the heat preservation stage is continuously controlled at 1300 ℃, and the time is controlled at 2-3h.
Preferably, the sintering further comprises a cooling stage, the time of the cooling stage is controlled to be 1-2h, and a mixed gas of nitrogen and pure oxygen is introduced into the cooling stage in a ratio of 4.
Preferably, the wide-temperature-range high-permeability manganese-zinc soft magnetic ferrite for automobile electronics has a specific temperature coefficient of-0.4-0.45 in the range of-50 ℃ to 120 ℃, and the permeability is stabilized above 5500.
(III) advantageous effects
The invention provides a wide-temperature-range high-permeability manganese-zinc soft magnetic ferrite for automotive electronics and a preparation method thereof. The method has the following beneficial effects:
1. the wide-temperature high-permeability manganese-zinc soft magnetic ferrite for automobile electronics and the preparation method thereof have the advantages that the initial permeability of the material is stabilized above 5500 by optimizing the component proportion and the processing technology, the temperature stability is high, the permeability change is small when the material is tested under the extreme temperature conditions of-50 ℃ and 120 ℃, and the comprehensive performance is very stable.
2. According to the wide-temperature-range high-permeability manganese-zinc soft magnetic ferrite for automobile electronics and the preparation method thereof, the stability of an automobile electronic product can be ensured by the produced manganese-zinc soft magnetic ferrite under the condition of extreme temperature through optimizing the component proportion and the processing technology, so that the driving safety of an automobile is ensured.
Drawings
FIG. 1 is a flow chart of the preparation process of the present invention;
FIG. 2 shows an embodiment a of the present invention F A disparity map of (d);
fig. 3 is a graph showing the change of permeability with temperature of the manganese-zinc soft magnetic ferrite in the example.
Detailed Description
The technical solutions in the embodiments of the present invention will be clearly and completely described below with reference to the drawings in the embodiments of the present invention, and it is obvious that the described embodiments are only a part of the embodiments of the present invention, and not all of the embodiments. All other embodiments, which can be obtained by a person skilled in the art without making any creative effort based on the embodiments in the present invention, belong to the protection scope of the present invention.
The first embodiment is as follows:
this example provides a wide temperature range high permeability Mn-Zn soft magnetic ferrite for automotive electronics, comprising a main component and an auxiliary component, the main component comprising 48mol% Fe 2 O 3 10mol% of ZnO, the remainder being Mn 3 O 4 The auxiliary components comprise: 0.2wt% of CaCO 3 、0.03wt％SiO 2 And 0.02wt% of TiO 2 ；
The preparation of the manganese-zinc soft magnetic ferrite comprises the following specific steps:
the method comprises the following steps: pretreatment: mixing the above Fe in proportion 2 O 3 ZnO and Mn 3 O 4 Putting the mixture into a ball mill for first ball milling processing, adding equivalent deionized water in the ball milling process, and controlling the ball milling time to be more than one hour;
step two: pre-burning: pre-drying the mixture prepared in the first step, sending the mixture into a pre-burning kiln for pre-burning after drying, controlling the pre-burning temperature at 1000-1100 ℃, preserving heat for 2-3 hours, introducing nitrogen after preserving heat for 2 hours, and preserving heat for one hour under the condition of nitrogen;
step three: impurity addition: mixing CaCO 3 、SiO 2 、TiO 2 And AL 2 O 3 Adding the mixture into the mixture subjected to the pre-sintering in the second step in proportion;
step four: secondary treatment: performing secondary ball milling on the mixed material obtained in the third step, adding deionized water according to the proportion of 1;
step five: secondary drying: drying the slurry obtained by the treatment in the fourth step to obtain a powdery material;
step six: and (3) pressing and forming: pressing and molding the powdery material by using a product mold;
step seven: sintering and forming: placing the pressed and molded material in a sintering furnace for sintering, controlling the sintering temperature at 1250-1400 ℃, and preserving heat for 8-10h;
the sintering is divided into three temperature stages, namely a low-temperature waste heat stage, a high-temperature sintering stage and a heat preservation stage, wherein the temperature of the low-temperature waste heat stage is controlled to be 900-1200 ℃, the heating rate is 2.3-2.7 ℃/min, and the time is controlled to be 1-2h; the temperature of the high-temperature sintering stage is controlled to be 1200-1400 ℃, the heating rate is 0.8-0.9 ℃/min, and the time is controlled to be 2-4h; the temperature of the heat preservation stage is continuously controlled at 1300 ℃, and the time is controlled at 2-3h;
the sintering also comprises a cooling stage, the time of the cooling stage is controlled for 1-2h, and mixed gas of nitrogen and pure oxygen is introduced into the cooling stage in a ratio of 4.
Example two:
this example provides a wide temperature range high permeability Mn-Zn soft magnetic ferrite for automotive electronics, comprising a main component and an auxiliary component, the main component comprising 49mol% Fe 2 O 3 11mol% of ZnO, the rest is Mn 3 O 4 The auxiliary components comprise: 0.25wt.% CaCO 3 、0.035wt％SiO 2 And 0.01wt% of TiO 2 ；
The preparation of the manganese-zinc soft magnetic ferrite comprises the following specific steps:
the method comprises the following steps: pretreatment: mixing the above Fe in proportion 2 O 3 ZnO and Mn 3 O 4 Putting the mixture into a ball mill for first ball milling processing, adding equivalent deionized water in the ball milling process, and controlling the ball milling time to be more than one hour;
step two: pre-burning: pre-drying the mixture prepared in the first step, sending the mixture into a pre-burning kiln for pre-burning after drying, controlling the pre-burning temperature at 1000-1100 ℃, preserving heat for 2-3 hours, introducing nitrogen after preserving heat for 2 hours, and preserving heat for one hour under the condition of nitrogen;
step three: impurity addition: mixing CaCO 3 、SiO 2 、TiO 2 And AL 2 O 3 Adding the mixture into the mixture subjected to the pre-sintering in the second step in proportion;
step four: secondary treatment: performing secondary ball milling on the mixed material obtained in the third step, adding deionized water according to the proportion of 1;
step five: secondary drying: drying the slurry obtained by the treatment in the fourth step to obtain a powdery material;
step six: and (3) pressing and forming: pressing and molding the powdery material by using a product mold;
step seven: sintering and forming: placing the pressed and molded material in a sintering furnace for sintering, controlling the sintering temperature at 1250-1400 ℃, and preserving heat for 8-10h;
the sintering is divided into three temperature stages, namely a low-temperature waste heat stage, a high-temperature sintering stage and a heat preservation stage, wherein the temperature of the low-temperature waste heat stage is controlled to be 900-1200 ℃, the heating rate is 2.3-2.7 ℃/min, and the time is controlled to be 1-2h; the temperature of the high-temperature sintering stage is controlled to be 1200-1400 ℃, the heating rate is 0.8 ℃/min-0.9 ℃/min, and the time is controlled to be 2-4h; the temperature of the heat preservation stage is continuously controlled at 1300 ℃, and the time is controlled at 2-3h;
the sintering also comprises a cooling stage, the time of the cooling stage is controlled for 1-2h, and mixed gas of nitrogen and pure oxygen is introduced into the cooling stage in a ratio of 4.
Example three:
this example provides a wide temperature range high permeability Mn-Zn soft magnetic ferrite for automotive electronics, comprising a main component comprising 50mol% Fe and an auxiliary component 2 O 3 12mol% of ZnO and the balance of Mn 3 O 4 The auxiliary components comprise: 0.3wt.% of CaCO 3 、0.04wt％SiO 2 And 0.02wt% of TiO 2 ；
The preparation of the manganese-zinc soft magnetic ferrite comprises the following specific steps:
the method comprises the following steps: pretreatment: mixing the above Fe in proportion 2 O 3 ZnO and Mn 3 O 4 Putting the mixture into a ball mill for first ball milling processing, adding equivalent deionized water in the ball milling process, and controlling the ball milling time to be more than one hour;
step two: pre-burning: pre-drying the mixture prepared in the first step, sending the mixture into a pre-burning kiln for pre-burning after drying, controlling the pre-burning temperature at 1000-1100 ℃, preserving heat for 2-3 hours, introducing nitrogen after preserving heat for 2 hours, and preserving heat for one hour under the condition of nitrogen;
step three: adding impurities: mixing CaCO 3 、SiO 2 、TiO 2 And AL 2 O 3 Adding the mixture into the mixture subjected to the pre-sintering in the second step in proportion;
step four: secondary treatment: performing secondary ball milling on the mixed material obtained in the third step, adding deionized water according to the proportion of 1;
step five: and (3) secondary drying: drying the slurry obtained by the treatment in the fourth step to obtain a powdery material;
step six: and (3) pressing and forming: pressing and molding the powdery material by using a product mold;
step seven: sintering and forming: placing the pressed and molded material in a sintering furnace for sintering, controlling the sintering temperature at 1250-1400 ℃, and preserving heat for 8-10h;
the sintering is divided into three temperature stages, namely a low-temperature waste heat stage, a high-temperature sintering stage and a heat preservation stage, wherein the temperature of the low-temperature waste heat stage is controlled to be 900-1200 ℃, the heating rate is 2.3-2.7 ℃/min, and the time is controlled to be 1-2h; the temperature of the high-temperature sintering stage is controlled to be 1200-1400 ℃, the heating rate is 0.8-0.9 ℃/min, and the time is controlled to be 2-4h; the temperature of the heat preservation stage is continuously controlled at 1300 ℃, and the time is controlled at 2-3h;
the sintering also comprises a cooling stage, the time of the cooling stage is controlled to be 1-2h, and mixed gas of nitrogen and pure oxygen is introduced into the cooling stage in a ratio of 4.
The results of the temperature permeability tests on the three example sintered samples are shown in the following table:
the embodiment shows that the composition proportion and the processing technology of the invention have obvious optimization effect on the material, the initial permeability is stable above 5500, the temperature stability is high, the permeability change is not large under the test of extreme temperature conditions of minus 50 ℃ and 120 ℃, and the comprehensive performance is very stable.
Although embodiments of the present invention have been shown and described, it will be appreciated by those skilled in the art that changes, modifications, substitutions and alterations can be made in these embodiments without departing from the principles and spirit of the invention, the scope of which is defined in the appended claims and their equivalents.
Claims (8)
1. A wide-temperature-range high-permeability manganese-zinc soft magnetic ferrite for automobile electronics is characterized in that: the Mn-Zn soft magnetic ferrite comprises a main component and an auxiliary component, the main component comprising 48 to 50mol% Fe 2 O 3 10 to 12mol% of ZnO, the balance being Mn 3 O 4 The auxiliary components comprise: 0.2-0.3wt% of CaCO 3 、0.03～0.04wt％SiO 2 、0.02～0.04wt％TiO 2 And 0 to 0.02wt% of Al 2 O 3 ；
The preparation method of the manganese-zinc soft magnetic ferrite comprises the following specific steps:
the method comprises the following steps: pretreatment: mixing the above Fe in proportion 2 O 3 ZnO and Mn 3 O 4 Putting the mixture into a ball mill for primary ball milling, and adding equivalent deionized water in the ball milling process;
step two: pre-burning: pre-drying the mixture prepared in the step one, and then conveying the mixture into a pre-sintering kiln for pre-sintering, wherein the pre-sintering temperature is controlled to be 1000-1100 ℃, and the temperature is kept for 2-3 hours;
step three: adding impurities: mixing CaCO 3 、SiO 2 、TiO 2 And AL 2 O 3 Adding the mixture into the mixture subjected to the pre-sintering in the second step in proportion;
step four: and (3) secondary treatment: performing secondary ball milling on the mixed material obtained in the third step, and adding deionized water according to the proportion of 1;
step five: secondary drying: drying the slurry obtained by the treatment in the fourth step to obtain a powdery material;
step six: and (3) pressing and forming: pressing and molding the powdery material by using a product mold;
step seven: sintering and forming: and (3) placing the pressed and molded material in a sintering furnace for sintering, controlling the sintering temperature at 1250-1400 ℃, and preserving heat for 8-10h.
2. The wide-temperature-range high-permeability manganese-zinc soft magnetic ferrite for automotive electronics according to claim 1, characterized in that: in the step one, the ball milling time is controlled to be more than one hour.
3. The wide-temperature high-permeability manganese-zinc soft magnetic ferrite for automotive electronics according to claim 1, characterized in that: and in the pre-sintering process in the second step, nitrogen is introduced after the temperature is kept for 2 hours, and the temperature is kept for one hour under the condition of nitrogen.
4. The wide-temperature high-permeability manganese-zinc soft magnetic ferrite for automotive electronics according to claim 1, characterized in that: in the fourth step, the time of the secondary ball milling is controlled to be 1.5-2h.
5. The wide-temperature high-permeability manganese-zinc soft magnetic ferrite for automotive electronics according to claim 1, characterized in that: and the sintering in the seventh step is divided into three temperature stages, namely a low-temperature waste heat stage, a high-temperature sintering stage and a heat preservation stage.
6. The wide-temperature-range high-permeability manganese-zinc soft magnetic ferrite for automotive electronics according to claim 5, characterized in that: the temperature of the low-temperature waste heat stage is controlled to be 900-1200 ℃, the heating rate is 2.3-2.7 ℃/min, and the time is controlled to be 1-2h; the temperature of the high-temperature sintering stage is controlled to be 1200-1400 ℃, the heating rate is 0.8 ℃/min-0.9 ℃/min, and the time is controlled to be 2-4h; the temperature of the heat preservation stage is continuously controlled at 1300 ℃ and the time is controlled at 2-3h.
7. The wide-temperature-range high-permeability manganese-zinc soft magnetic ferrite for automotive electronics according to claim 5, characterized in that: the sintering process also comprises a cooling stage, wherein the time of the cooling stage is controlled for 1-2h, and mixed gas of nitrogen and pure oxygen is introduced into the cooling stage in a ratio of 4.
8. The wide-temperature high-permeability manganese-zinc soft magnetic ferrite for automotive electronics according to claim 1, characterized in that: the wide-temperature-range high-permeability manganese-zinc soft magnetic ferrite for automobile electronics has a specific temperature coefficient of-0.4-0.45 within the range of-50-120 ℃ and a stable permeability of over 5500.
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