CN111777419A - Sintering process of magnetic ferrite core - Google Patents
Sintering process of magnetic ferrite core Download PDFInfo
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Abstract
The invention discloses a sintering process of a magnetic ferrite core, which comprises the following steps: the method comprises the following steps: preparing a sintering liquid: adding phosphoric acid into sodium citrate, then adjusting the pH value of the solution to 4.0-5.0, then adding modified ceramic powder, stirring at the rotation speed of 100-. The magnetic ferrite core is treated by the sintering liquid, the magnetic ferrite core is sent into the sintering liquid in the first step, then is stirred for 15min at the rotating speed of 500r/min, and then is sent into a magnetization tank for magnetization treatment, and the sintering liquid can form stable chemical substances on the surface of the magnetic core material, so that the product performance is more stable.
Description
Technical Field
The invention relates to the technical field of magnetic ferrite cores, in particular to a sintering process of a magnetic ferrite core.
Background
The ferrite core is made of dense and homogeneous non-metallic magnetic material with ceramic structure and low coercive force, and is also called soft magnetic ferrite. It consists of iron oxide (Fe2O3) and one or more oxide or carbonate compounds of other metals (e.g. manganese, zinc, nickel, magnesium). Compared with other types of magnetic materials, the ferrite has the advantages of high magnetic conductivity, high resistance in a wide frequency range, low eddy current loss and the like. These material properties make ferrites ideal for the fabrication of high frequency transformers, wide band transformers, tunable inductors and other high frequency circuits from 10kHz to 50 MHz.
The existing magnetic ferrite core sintering process is more conventional, the performance change of the magnetic material after sintering is not very obvious, and the properties such as strength and the like of the magnetic material cannot be obviously improved, so that further improvement treatment is needed.
Disclosure of Invention
The present invention is directed to a sintering process for magnetic ferrite cores to solve the above-mentioned problems of the prior art.
In order to achieve the purpose, the invention provides the following technical scheme:
the invention provides a sintering process of a magnetic ferrite core, which comprises the following steps:
the method comprises the following steps: preparing a sintering liquid: adding phosphoric acid into sodium citrate, then adjusting the pH value of the solution to 4.0-5.0, then adding modified ceramic powder, stirring at the rotation speed of 100-;
step two, treating the sintering liquid: sending the magnetic ferrite core into the sintering liquid in the first step, stirring for 15-25min at the rotating speed of 500-1000r/min, sending into a magnetization tank for magnetization treatment, and finishing magnetization;
step three, hot pressing treatment: carrying out hot pressing treatment on the magnetic core treated in the step two, wherein the hot pressing pressure is 10-20MPa, the hot pressing temperature is 300-400 ℃, then carrying out heat preservation for 15-25min, and then cooling the temperature to room temperature at the speed of 2 ℃/min;
step four, primary sintering treatment: the magnetic core after the hot pressing treatment is firstly sent into a sintering furnace to be sintered for 10-20min at the temperature of 1000-1500 ℃, and then is naturally cooled to the room temperature;
step five, plasma treatment: the material processed in the step four is sent into a plasma box, the plasma processing power is 500-700W, and the processing time is 15-25 min;
step six, secondary sintering treatment: the material is heated to 600 ℃ at the speed of 2-5 ℃/min, then heat preservation treatment is carried out, then the temperature is raised to 1000 ℃, heat preservation is carried out for 10min, and finally cooling is carried out to the room temperature.
Preferably, the modification method of the modified ceramic powder comprises the following steps: adding the ceramic powder into a magnetic stirrer, adding a zinc chloride pore-forming agent, adding phosphoric acid, stirring at the rotation speed of 500-400 r/min for 15-25min, raising the stirring temperature to 60-100 ℃, adding improved silicon dioxide after stirring, reducing the stirring rotation speed to 200-400r/min, and continuing stirring for 20-30min to obtain the modified ceramic powder.
Preferably, the modifying method of the modified silica is as follows: dispersing silicon dioxide into polyvinyl alcohol solution, then adding montmorillonite, finally adding ammonia water to adjust the pH value to 10-11.0, and then stirring at the rotating speed of 100-200r/min for 15-25 min.
Preferably, the magnetization intensity of the magnetization treatment in the magnetization tank is 2-5BT, and the magnetization time is 10-20 min.
Preferably, the magnetization intensity of the magnetization treatment in the magnetization tank is 3.5BT, and the magnetization time is 15 min.
Preferably, the heat preservation time of the secondary sintering treatment is 15-25 min.
Preferably, the heat preservation time of the secondary sintering treatment is 20 min.
Preferably, the secondary sintering treatment is cooled to room temperature by immediately cooling to room temperature by water cooling.
Compared with the prior art, the invention has the following beneficial effects:
(1) the magnetic ferrite core is treated by the sintering liquid, the magnetic ferrite core is sent into the sintering liquid in the first step, then is stirred for 15min at the rotating speed of 500r/min, and then is sent into a magnetization tank for magnetization treatment, and the sintering liquid can form stable chemical substances on the surface of the magnetic core material, so that the product performance is more stable.
(2) The hot pressing treatment aims at enabling the product structure to be more compact, so that the material performance is more perfect, and the primary sintering treatment, the plasma treatment and the secondary sintering treatment improve the sintering quality, so that the product performance is improved, and the product strength and other properties can be obviously improved.
(3) The modification method of the modified ceramic powder comprises the following steps: adding ceramic powder into a magnetic stirrer, adding a zinc chloride pore-forming agent, adding phosphoric acid, stirring at the rotating speed of 500r/min for 15min, raising the stirring temperature to 60 ℃, after stirring, adding improved silicon dioxide, reducing the stirring rotating speed to 200r/min, and continuing stirring for 20min to obtain the modified ceramic powder.
Detailed Description
The technical solutions in the embodiments of the present invention are clearly and completely described below with reference to specific embodiments, and it is obvious that the described embodiments are only a part of the embodiments of the present invention, and not all embodiments. All other embodiments, which can be derived by a person skilled in the art from the embodiments given herein without making any creative effort, shall fall within the protection scope of the present invention.
Example 1:
the sintering process of the magnetic ferrite core of the embodiment comprises the following steps:
the method comprises the following steps: preparing a sintering liquid: adding phosphoric acid into sodium citrate, adjusting the pH value of the solution to 4.0, then adding modified ceramic powder, stirring at the rotating speed of 100r/min for 15min, then adding chitosan and talcum powder, continuing stirring at the rotating speed of 500r/min for 15min, and obtaining sintering liquid after stirring;
step two, treating the sintering liquid: sending the magnetic ferrite core into the sintering liquid obtained in the first step, stirring at a rotating speed of 500r/min for 15min, sending into a magnetizing tank for magnetization treatment, and finishing magnetization;
step three, hot pressing treatment: carrying out hot pressing treatment on the magnetic core treated in the step two, wherein the hot pressing pressure is 10MPa, the hot pressing temperature is 300 ℃, then carrying out heat preservation for 15min, and then cooling the temperature to room temperature at the speed of 2 ℃/min;
step four, primary sintering treatment: the magnetic core after the hot pressing treatment is firstly sent into a sintering furnace to be sintered for 10-20min at the temperature of 1000 ℃, and then is naturally cooled to the room temperature;
step five, plasma treatment: feeding the material processed in the step four into a plasma box, wherein the plasma processing power is 500W, and the processing time is 15 min;
step six, secondary sintering treatment: the material is heated to 600 ℃ at the speed of 2 ℃/min, then is subjected to heat preservation treatment, is heated to 1000 ℃, is subjected to heat preservation for 10min, and is cooled to room temperature.
Preferably, the modification method of the modified ceramic powder comprises the following steps: adding ceramic powder into a magnetic stirrer, adding a zinc chloride pore-forming agent, adding phosphoric acid, stirring at the rotating speed of 500r/min for 15min, raising the stirring temperature to 60 ℃, adding improved silicon dioxide after stirring, reducing the stirring rotating speed to 200r/min, and continuing stirring for 20min to obtain the modified ceramic powder.
The method for improving silicon dioxide of this embodiment is: dispersing silicon dioxide into polyvinyl alcohol solution, adding montmorillonite, adding ammonia water to adjust pH to 10, and stirring at 100r/min for 15 min.
The magnetization intensity of the magnetization treatment in the magnetization tank of this example was 2BT, and the magnetization time was 10 min.
The second-stage sintering treatment heat preservation time of the embodiment is 15 min.
The second-stage sintering treatment heat preservation time of the embodiment is 20 min.
Example 2:
the sintering process of the magnetic ferrite core of the embodiment comprises the following steps:
the method comprises the following steps: preparing a sintering liquid: adding phosphoric acid into sodium citrate, adjusting the pH value of the solution to 4.0, then adding modified ceramic powder, stirring at the rotating speed of 200r/min for 25min, then adding chitosan and talcum powder, continuing stirring for 25min at the stirring rotating speed of 1000r/min, and obtaining sintering liquid after stirring;
step two, treating the sintering liquid: sending the magnetic ferrite core into the sintering liquid obtained in the first step, stirring at the rotating speed of 1000r/min for 25min, sending into a magnetizing tank for magnetization treatment, and finishing magnetization;
step three, hot pressing treatment: carrying out hot pressing treatment on the magnetic core treated in the step two, wherein the hot pressing pressure is 20MPa, the hot pressing temperature is 400 ℃, then carrying out heat preservation for 25min, and then cooling the temperature to room temperature at the speed of 2 ℃/min;
step four, primary sintering treatment: the magnetic core after the hot pressing treatment is firstly sent into a sintering furnace to be sintered for 20min at the temperature of 1500 ℃, and then is naturally cooled to the room temperature;
step five, plasma treatment: feeding the material processed in the step four into a plasma box, wherein the plasma processing power is 700W, and the processing time is 25 min;
step six, secondary sintering treatment: the material is heated to 600 ℃ at the speed of 5 ℃/min, then is subjected to heat preservation treatment, is heated to 1000 ℃, is subjected to heat preservation for 10min, and is cooled to room temperature.
Preferably, the modification method of the modified ceramic powder comprises the following steps: adding ceramic powder into a magnetic stirrer, adding a zinc chloride pore-forming agent, adding phosphoric acid, stirring at the rotating speed of 1000r/min for 25min, increasing the stirring temperature to 100 ℃, adding improved silicon dioxide after stirring, reducing the stirring rotating speed to 400r/min, and continuing stirring for 30min to obtain the modified ceramic powder.
The method for improving silicon dioxide of this embodiment is: dispersing silicon dioxide into polyvinyl alcohol solution, adding montmorillonite, adding ammonia water to adjust pH to 11.0, and stirring at a rotation speed of 200r/min for 25 min.
The magnetization intensity of the magnetization treatment in the magnetization tank of this example was 5BT, and the magnetization time was 20 min.
The second-stage sintering treatment heat preservation time of the embodiment is 25 min.
The method for cooling the secondary sintering treatment to room temperature in this embodiment is to immediately cool the secondary sintering treatment to room temperature by means of water cooling.
Example 3:
the sintering process of the magnetic ferrite core of the embodiment comprises the following steps:
the method comprises the following steps: preparing a sintering liquid: adding phosphoric acid into sodium citrate, adjusting the pH value of the solution to 4.5, then adding modified ceramic powder, stirring at the rotating speed of 150r/min for 20min, then adding chitosan and talcum powder, continuing stirring for 20min at the stirring rotating speed of 750r/min, and obtaining sintering liquid after stirring;
step two, treating the sintering liquid: sending the magnetic ferrite core into the sintering liquid obtained in the first step, stirring at a rotating speed of 750r/min for 20min, sending into a magnetizing tank for magnetization treatment, and finishing magnetization;
step three, hot pressing treatment: carrying out hot pressing treatment on the magnetic core treated in the step two, wherein the hot pressing pressure is 15MPa, the hot pressing temperature is 350 ℃, then keeping the temperature for 20min, and then reducing the temperature to room temperature at the speed of 2 ℃/min;
step four, primary sintering treatment: the magnetic core after the hot pressing treatment is firstly sent into a sintering furnace to be sintered for 15min at 1250 ℃, and then is naturally cooled to room temperature;
step five, plasma treatment: feeding the material processed in the step four into a plasma box, wherein the plasma processing power is 600W, and the processing time is 20 min;
step six, secondary sintering treatment: the material is heated to 600 ℃ at the speed of 3.5 ℃/min, then heat preservation treatment is carried out, then the temperature is raised to 1000 ℃, heat preservation is carried out for 10min, and finally cooling is carried out to the room temperature.
Preferably, the modification method of the modified ceramic powder comprises the following steps: adding ceramic powder into a magnetic stirrer, adding a zinc chloride pore-forming agent, adding phosphoric acid, stirring at the rotating speed of 750r/min for 20min, increasing the stirring temperature to 80 ℃, adding improved silicon dioxide after stirring, reducing the stirring rotating speed to 300r/min, and continuing stirring for 25min to obtain the modified ceramic powder.
The method for improving silicon dioxide of this embodiment is: dispersing silicon dioxide into polyvinyl alcohol solution, adding montmorillonite, adding ammonia water to adjust pH to 10.5, and stirring at 150r/min for 20 min.
The magnetization intensity of the magnetization treatment in the magnetization tank of this example was 3.5BT, and the magnetization time was 15 min.
The second-stage sintering treatment heat preservation time of the embodiment is 20 min.
The method for cooling the secondary sintering treatment to room temperature in this embodiment is to immediately cool the secondary sintering treatment to room temperature by means of water cooling.
Comparative example 1:
the materials and preparation process are basically the same as those of example 3, except that the materials which are conventional in the market are adopted.
It will be evident to those skilled in the art that the invention is not limited to the details of the foregoing illustrative embodiments, and that the present invention may be embodied in other specific forms without departing from the spirit or essential attributes thereof. The present embodiments are therefore to be considered in all respects as illustrative and not restrictive, the scope of the invention being indicated by the appended claims rather than by the foregoing description, and all changes which come within the meaning and range of equivalency of the claims are therefore intended to be embraced therein.
Furthermore, it should be understood that although the present description refers to embodiments, not every embodiment may contain only a single embodiment, and such description is for clarity only, and those skilled in the art should integrate the description, and the embodiments may be combined as appropriate to form other embodiments understood by those skilled in the art.
Claims (8)
1. A sintering process of a magnetic ferrite core is characterized by comprising the following steps:
the method comprises the following steps: preparing a sintering liquid: adding phosphoric acid into sodium citrate, then adjusting the pH value of the solution to 4.0-5.0, then adding modified ceramic powder, stirring at the rotation speed of 100-;
step two, treating the sintering liquid: sending the magnetic ferrite core into the sintering liquid in the first step, stirring for 15-25min at the rotating speed of 500-1000r/min, sending into a magnetization tank for magnetization treatment, and finishing magnetization;
step three, hot pressing treatment: carrying out hot pressing treatment on the magnetic core treated in the step two, wherein the hot pressing pressure is 10-20MPa, the hot pressing temperature is 300-400 ℃, then carrying out heat preservation for 15-25min, and then cooling the temperature to room temperature at the speed of 2 ℃/min;
step four, primary sintering treatment: the magnetic core after the hot pressing treatment is firstly sent into a sintering furnace to be sintered for 10-20min at the temperature of 1000-1500 ℃, and then is naturally cooled to the room temperature;
step five, plasma treatment: the material processed in the step four is sent into a plasma box, the plasma processing power is 500-700W, and the processing time is 15-25 min;
step six, secondary sintering treatment: the material is heated to 600 ℃ at the speed of 2-5 ℃/min, then heat preservation treatment is carried out, then the temperature is raised to 1000 ℃, heat preservation is carried out for 10min, and finally cooling is carried out to the room temperature.
2. The sintering process of a magnetic ferrite core according to claim 1, wherein the modification method of the modified ceramic powder is: adding the ceramic powder into a magnetic stirrer, adding a zinc chloride pore-forming agent, adding phosphoric acid, stirring at the rotation speed of 500-400 r/min for 15-25min, raising the stirring temperature to 60-100 ℃, adding improved silicon dioxide after stirring, reducing the stirring rotation speed to 200-400r/min, and continuing stirring for 20-30min to obtain the modified ceramic powder.
3. A process for sintering a magnetic ferrite core as claimed in claim 2, wherein said modified silica is modified by: dispersing silicon dioxide into polyvinyl alcohol solution, then adding montmorillonite, finally adding ammonia water to adjust the pH value to 10-11.0, and then stirring at the rotating speed of 100-200r/min for 15-25 min.
4. A process for sintering a magnetic ferrite core according to claim 1, wherein the magnetization of said magnetization tank is 2-5BT for 10-20 min.
5. A sintering process of a magnetic ferrite core according to claim 4, characterized in that the magnetization intensity of the magnetization treatment in the magnetization tank is 3.5BT and the magnetization time is 15 min.
6. A process for sintering a magnetic ferrite core according to claim 1, wherein said secondary sintering treatment is carried out for a holding time of 15-25 min.
7. A process according to claim 6, wherein said secondary sintering is carried out for a holding time of 20 min.
8. A process of sintering a magnetic ferrite core as claimed in claim 1, wherein said secondary sintering treatment is carried out by cooling to room temperature immediately by water cooling.
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