CN116477934B - Preparation process of nickel-zinc ferrite core - Google Patents

Preparation process of nickel-zinc ferrite core Download PDF

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CN116477934B
CN116477934B CN202310555013.4A CN202310555013A CN116477934B CN 116477934 B CN116477934 B CN 116477934B CN 202310555013 A CN202310555013 A CN 202310555013A CN 116477934 B CN116477934 B CN 116477934B
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CN116477934A (en
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林致婷
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Sumeier Magnetic Electronics Huizhou Co ltd
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Abstract

The invention relates to a preparation process of a nickel-zinc ferrite core, which comprises the following steps: grinding the main material; a first granulation step: adding a strengthening solution into the main material powder, and granulating to obtain first particles; a first pressing step: pressing the first primary particles into a first blank; presintering: preliminary firing is carried out on the first blank at the temperature of 920-960 ℃ for 6-10 hours to obtain a prefabricated blank; and (3) crushing and grinding the prefabricated blank: crushing and grinding the prefabricated blank to obtain prefabricated powder; and a second granulation step: adding an auxiliary agent solution into the prefabricated powder, and granulating to obtain second granules; a second particle improvement step: adding an improvement liquid into the second particles to infiltrate and encapsulate the second particles; and a second pressing step: pressing the reinforced second particles into a second blank; firing: the second blank is subjected to a multi-stage firing process.

Description

Preparation process of nickel-zinc ferrite core
Technical Field
The invention relates to the field of ferrite core manufacturing, in particular to a preparation process of a nickel-zinc ferrite core.
Background
Ferrite core is a high frequency magnetic conduction material, mainly used as high frequency transformer, high frequency magnetic ring, etc. ferrite core is used to increase magnetic permeability and improve inductance quality. Ferrite cores are made of dense and homogeneous ceramic-structured nonmetallic magnetic materials, and have low coercivity, also known as soft magnetic ferrites. It consists of iron oxide and one or more other metal oxide or carbonate compounds. The ferrite raw material is pressed, sintered at high temperature and finally machined to form a finished magnetic core meeting application requirements, and compared with other types of magnetic materials, the ferrite has the advantages of high magnetic permeability, high resistance, small eddy current loss and the like in a wide frequency range.
However, nickel zinc ferrite has been increasingly emphasized in recent years due to its characteristics of high frequency, wide frequency band, high impedance, and low loss, and has become the most widely used soft magnetic ferrite material in the high frequency range (1 to 100 MHz). However, the traditional nickel-zinc ferrite core has complex preparation process, and the prepared nickel-zinc ferrite core has lower structural strength and can not meet the high-strength requirement of the nickel-zinc ferrite core in the market.
Disclosure of Invention
Based on the above, it is necessary to provide a preparation process of a nickel-zinc ferrite core, aiming at the technical problems that the traditional preparation process of the nickel-zinc ferrite core is complex, the structure strength of the prepared nickel-zinc ferrite core is low, and the high strength requirement of the nickel-zinc ferrite core on the market cannot be met.
A process for preparing a nickel zinc ferrite core, the process comprising the steps of:
grinding the main material: ball milling the main material to obtain main material powder; the main material comprises the following components in parts by mass: 45 to 55 parts of Fe 2O3, 20 to 28 parts of NiO and 20 to 28 parts of ZnO;
A first granulation step: adding a strengthening solution into the main material powder, and granulating to obtain first particles; the strengthening solution comprises 0.1 to 0.3mol/L FeCL 3, 0.1 to 0.3mol/L ZnCL 2 and 0.4 to 0.8mol/L NiCL 2;
a first pressing step: pressing the first primary particles into a first blank;
Presintering: preliminary firing is carried out on the first blank at the temperature of 920-960 ℃ for 6-10 hours to obtain a prefabricated blank;
and (3) crushing and grinding the prefabricated blank: crushing and grinding the prefabricated blank to obtain prefabricated powder;
And a second granulation step: adding an auxiliary agent solution into the prefabricated powder, and granulating to obtain second granules; the auxiliary agent solution comprises the following components in parts by mass: 2 to 5 parts of adhesive, 0.2 to 0.5 part of dispersing agent, 0.1 to 0.3 part of defoaming agent, 0.5 to 1 part of coupling agent and the balance of water;
A second particle improvement step: adding an improvement liquid into the second particles to infiltrate and encapsulate the second particles; the improvement liquid comprises the following components in parts by mass: 8 to 12 parts of nano silicon dioxide, 6 to 8 parts of nano aluminum oxide, 6 to 10 parts of calcium carbonate powder, 4 to 6 parts of vanadium pentoxide powder, 6 to 10 parts of niobium pentoxide powder, 8 to 10 parts of bismuth trioxide powder and the balance of water;
And a second pressing step: pressing the reinforced second particles into a second blank;
Firing: and carrying out multi-stage firing treatment on the second blank to obtain the finished nickel-zinc ferrite core.
In one embodiment, in the main material grinding step, the main material further includes CuO 0.2 parts to 0.5 parts.
In one embodiment, in the first granulation step, the mass ratio of the main material powder and the strengthening solution is 1:1.2 to 1:1.
In one embodiment, in the second granulation step, the mass ratio of the pre-powder and the adjuvant solution is from 1:1.4 to 1:1.2.
In one embodiment, in the second granulation step, the binder includes the following components in parts by mass: 20 to 40 parts of polyvinyl alcohol, 20 to 30 parts of polyvinyl acetate, 10 to 30 parts of oxymethylsilane and 10 to 20 parts of polyethylene glycol.
In one embodiment, in the second granulation step, the dispersant is a polyethylene wax.
In one embodiment, in the second granulation step, the defoamer is polydimethylsiloxane.
In one embodiment, in the second particle strengthening improvement step, the mass ratio of the improvement liquid to the second particles is 1:8 to 1:5.
In one embodiment, in the firing step, the first firing stage: heating the second blank to 300-400 ℃ and keeping the second blank for 2-3 hours; a second firing stage: heating the second blank to 800-900 ℃ and keeping for 1-2 hours; and a third firing stage: the second blank is first heated to 1100 to 1200 degrees celsius for 3 to 4 hours.
In one embodiment, the ramp rate is 70 degrees celsius per minute to 100 degrees celsius per minute.
The preparation process steps of the nickel-zinc ferrite core are concise and exquisite, the operation is easy, each step is carefully and finely carried out, the prepared nickel-zinc ferrite core has high structural strength and good thermal stability, and the high-strength requirement of the nickel-zinc ferrite core on the market is met.
Drawings
FIG. 1 is a schematic flow chart of a process for preparing a nickel zinc ferrite core according to an embodiment.
Detailed Description
The present invention will be described in further detail with reference to the drawings and examples, in order to make the objects, technical solutions and advantages of the present invention more apparent. It should be understood that the specific embodiments described herein are for purposes of illustration only and are not intended to limit the scope of the invention.
Referring to fig. 1, the invention provides a preparation process of a nickel-zinc ferrite core, which comprises the following steps:
Step 101: grinding the main material: ball milling the main material to obtain main material powder; the main material comprises the following components in parts by mass: 45 to 55 parts of Fe 2O3, 20 to 28 parts of NiO and 20 to 28 parts of ZnO.
Specifically, performing ball milling treatment on the main material to obtain main material powder; the main material comprises the following components in parts by mass: 45 to 55 parts of Fe 2O3, 20 to 28 parts of NiO and 20 to 28 parts of ZnO. In this embodiment, the main material further includes CuO 0.2 to 0.5 parts.
Step 102: a first granulation step: adding strengthening solution into the main material powder, and granulating to obtain first particles. The strengthening solution comprises 0.1 to 0.3mol/L FeCL 3, 0.1 to 0.3mol/L ZnCL 2, and 0.4 to 0.8mol/L NiCL 2.
Specifically, the primary particles are obtained by adding a strengthening solution into the primary powder and granulating the mixture. The strengthening solution comprises 0.1 to 0.3mol/L FeCL 3, 0.1 to 0.3mol/L ZnCL 2, and 0.4 to 0.8mol/L NiCL 2. In this embodiment, the mass ratio of the main material powder to the strengthening solution is 1:1.2 to 1:1.
Step 103: a first pressing step: the first secondary particles are pressed into a first blank.
Specifically, the first primary particles are pressed into a first billet using a powder forming machine.
Step 104: presintering: and (3) performing primary firing on the first blank at 920-960 ℃ for 6-10 hours to obtain a prefabricated blank.
Specifically, the first blank is subjected to preliminary firing at 920-960 ℃ for 6-10 hours to obtain a prefabricated blank. The temperature rising speed in the primary firing process is 70-100 ℃ per minute.
Step 105: and (3) crushing and grinding the prefabricated blank: and crushing and grinding the prefabricated blank to obtain prefabricated powder.
Specifically, the prefabricated blank is crushed by a crusher, and then the crushed prefabricated blank is ground by a ball mill to obtain prefabricated powder.
Step 106: and a second granulation step: adding the auxiliary agent solution into the prefabricated powder, and granulating to obtain second granules. The auxiliary agent solution comprises the following components in parts by mass: 2 to 5 parts of adhesive, 0.2 to 0.5 part of dispersing agent, 0.1 to 0.3 part of defoaming agent, 0.5 to 1 part of coupling agent and the balance of water.
Specifically, the secondary particles are obtained by adding an auxiliary agent solution into the prefabricated powder and granulating. The auxiliary agent solution comprises the following components in parts by mass: 2 to 5 parts of adhesive, 0.2 to 0.5 part of dispersing agent, 0.1 to 0.3 part of defoaming agent, 0.5 to 1 part of coupling agent and the balance of water. In this example, the mass ratio of the preformed powder to the adjuvant solution is 1:1.4 to 1:1.2. In this embodiment, in the second granulation step, the binder includes the following components in parts by mass: 20 to 40 parts of polyvinyl alcohol, 20 to 30 parts of polyvinyl acetate, 10 to 30 parts of oxymethylsilane and 10 to 20 parts of polyethylene glycol; to increase the adhesion between the components in the preformed powder and thereby increase the structural strength and structural stability of the finished product. Further, the dispersing agent is polyethylene wax to increase the mixing uniformity of the components in the preformed powder. The defoamer is polydimethylsiloxane so as to reduce foam generated in the stirring and mixing process.
Step 107: a second particle improvement step: the modifying liquid is added to the second particles to wet-pack the second particles. The improvement liquid comprises the following components in parts by mass: 8 to 12 parts of nano silicon dioxide, 6 to 8 parts of nano aluminum oxide, 6 to 10 parts of calcium carbonate powder, 4 to 6 parts of vanadium pentoxide powder, 6 to 10 parts of niobium pentoxide powder, 8 to 10 parts of bismuth trioxide powder and the balance of water.
Specifically, the modifying liquid is added to the second particles to wet-pack the second particles. The improvement liquid comprises the following components in parts by mass: 8 to 12 parts of nano silicon dioxide, 6 to 8 parts of nano aluminum oxide, 6 to 10 parts of calcium carbonate powder, 4 to 6 parts of vanadium pentoxide powder, 6 to 10 parts of niobium pentoxide powder, 8 to 10 parts of bismuth trioxide powder and the balance of water. In this embodiment, the mass ratio of the improving liquid to the second particles is 1:8 to 1:5. the improvement liquid can improve the structural strength and the thermal stability of the finished product.
Step 108: and a second pressing step: and pressing the reinforced second particles into a second blank.
Specifically, the reinforced second granules are pressed into a second blank by a powder forming machine.
Step 109: firing: and carrying out multi-stage firing treatment on the second blank to obtain the finished nickel-zinc ferrite core.
Specifically, the second blank is subjected to multi-stage firing treatment to obtain the finished nickel-zinc ferrite core. In this embodiment, in the firing step, the first firing stage: heating the second blank to 300-400 ℃ and keeping the second blank for 2-3 hours; a second firing stage: heating the second blank to 800-900 ℃ and keeping for 1-2 hours; and a third firing stage: the second blank is first heated to 1100 to 1200 degrees celsius for 3 to 4 hours. In this embodiment, the temperature rise rate is 70 degrees celsius per minute to 100 degrees celsius per minute.
Experimental tests were performed on 100 finished nickel zinc ferrite cores. Conditions of the experiment: testing the initial permeability mu i of the finished nickel-zinc ferrite core at the turn number of N=20Ts; testing the Curie temperature Tc of the finished nickel-zinc ferrite core; and testing the saturation induction Bs of the finished nickel-zinc ferrite core.
The data obtained are as follows:
Project Results Evaluation
μi 190 To 220 Good quality
Tc(℃) 370 To 380 Good quality
Bs(25℃) 220 To 240 Good quality
Intensity (Mpa) 280 To 320 Good quality
The preparation process steps of the nickel-zinc ferrite core are concise and exquisite, the operation is easy, each step is carefully and finely carried out, the prepared nickel-zinc ferrite core has high structural strength and good thermal stability, and the high-strength requirement of the nickel-zinc ferrite core on the market is met.
The technical features of the above embodiments may be arbitrarily combined, and all possible combinations of the technical features in the above embodiments are not described for brevity of description, however, as long as there is no contradiction between the combinations of the technical features, they should be considered as the scope of the description.
The above examples illustrate only a few embodiments of the invention, which are described in detail and are not to be construed as limiting the scope of the invention. It should be noted that it will be apparent to those skilled in the art that several variations and modifications can be made without departing from the spirit of the invention, which are all within the scope of the invention. Accordingly, the scope of protection of the present invention is to be determined by the appended claims.

Claims (8)

1. A process for preparing a nickel zinc ferrite core, the process comprising the steps of:
grinding the main material: ball milling the main material to obtain main material powder; the main material comprises the following components in parts by mass: 45 to 55 parts of Fe 2O3, 20 to 28 parts of NiO and 20 to 28 parts of ZnO;
A first granulation step: adding a strengthening solution into the main material powder, and granulating to obtain first particles; the strengthening solution comprises 0.1 to 0.3mol/L FeCL 3, 0.1 to 0.3mol/L ZnCL 2 and 0.4 to 0.8mol/L NiCL 2; the mass ratio of the main material powder to the strengthening solution is 1:1.2-1:1;
a first pressing step: pressing the first primary particles into a first blank;
Presintering: preliminary firing is carried out on the first blank at the temperature of 920-960 ℃ for 6-10 hours to obtain a prefabricated blank;
and (3) crushing and grinding the prefabricated blank: crushing and grinding the prefabricated blank to obtain prefabricated powder;
And a second granulation step: adding an auxiliary agent solution into the prefabricated powder, and granulating to obtain second granules; the auxiliary agent solution comprises the following components in parts by mass: 2 to 5 parts of adhesive, 0.2 to 0.5 part of dispersing agent, 0.1 to 0.3 part of defoaming agent, 0.5 to 1 part of coupling agent and the balance of water;
A second particle improvement step: adding an improvement liquid into the second particles to infiltrate and encapsulate the second particles; the improvement liquid comprises the following components in parts by mass: 8 to 12 parts of nano silicon dioxide, 6 to 8 parts of nano aluminum oxide, 6 to 10 parts of calcium carbonate powder, 4 to 6 parts of vanadium pentoxide powder, 6 to 10 parts of niobium pentoxide powder, 8 to 10 parts of bismuth trioxide powder and the balance of water; the mass ratio of the improving liquid to the second particles is 1:8 to 1:5, a step of;
And a second pressing step: pressing the reinforced second particles into a second blank;
Firing: and carrying out multi-stage firing treatment on the second blank to obtain the finished nickel-zinc ferrite core.
2. The process according to claim 1, wherein in the main material grinding step, the main material further comprises CuO 0.2 parts to 0.5 parts.
3. The process according to claim 1, characterized in that in the second granulation step the mass ratio of the preformed powder and the auxiliary solution is between 1:1.4 and 1:1.2.
4. The process according to claim 1, characterized in that in the second granulation step, the binder comprises the following components in parts by mass: 20 to 40 parts of polyvinyl alcohol, 20 to 30 parts of polyvinyl acetate, 10 to 30 parts of oxymethylsilane and 10 to 20 parts of polyethylene glycol.
5. The process according to claim 1, characterized in that in the second granulation step, the dispersant is a polyethylene wax.
6. The process according to claim 1, characterized in that in the second granulation step, the antifoaming agent is polydimethylsiloxane.
7. The process of claim 1, wherein in the firing step, the first firing stage: heating the second blank to 300-400 ℃ and keeping the second blank for 2-3 hours; a second firing stage: heating the second blank to 800-900 ℃ and keeping for 1-2 hours; and a third firing stage: the second blank is first heated to 1100 to 1200 degrees celsius for 3 to 4 hours.
8. The process of claim 7, wherein the ramp rate is from 70 degrees celsius per minute to 100 degrees celsius per minute.
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