CN116477934A - Preparation process of nickel-zinc ferrite core - Google Patents
Preparation process of nickel-zinc ferrite core Download PDFInfo
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- CN116477934A CN116477934A CN202310555013.4A CN202310555013A CN116477934A CN 116477934 A CN116477934 A CN 116477934A CN 202310555013 A CN202310555013 A CN 202310555013A CN 116477934 A CN116477934 A CN 116477934A
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- 229910001053 Nickel-zinc ferrite Inorganic materials 0.000 title claims abstract description 30
- 238000002360 preparation method Methods 0.000 title abstract description 10
- 239000000843 powder Substances 0.000 claims abstract description 45
- 239000000463 material Substances 0.000 claims abstract description 29
- 238000010304 firing Methods 0.000 claims abstract description 27
- 239000002245 particle Substances 0.000 claims abstract description 27
- 238000005469 granulation Methods 0.000 claims abstract description 19
- 230000003179 granulation Effects 0.000 claims abstract description 19
- 230000006872 improvement Effects 0.000 claims abstract description 16
- 238000003825 pressing Methods 0.000 claims abstract description 15
- 238000000227 grinding Methods 0.000 claims abstract description 14
- 238000000034 method Methods 0.000 claims abstract description 14
- 230000008569 process Effects 0.000 claims abstract description 14
- 238000005728 strengthening Methods 0.000 claims abstract description 14
- 239000007788 liquid Substances 0.000 claims abstract description 13
- 239000012752 auxiliary agent Substances 0.000 claims abstract description 9
- 239000008187 granular material Substances 0.000 claims abstract description 5
- 239000011164 primary particle Substances 0.000 claims abstract description 5
- VTYYLEPIZMXCLO-UHFFFAOYSA-L Calcium carbonate Chemical compound [Ca+2].[O-]C([O-])=O VTYYLEPIZMXCLO-UHFFFAOYSA-L 0.000 claims description 8
- VYPSYNLAJGMNEJ-UHFFFAOYSA-N Silicium dioxide Chemical compound O=[Si]=O VYPSYNLAJGMNEJ-UHFFFAOYSA-N 0.000 claims description 8
- GNTDGMZSJNCJKK-UHFFFAOYSA-N divanadium pentaoxide Chemical compound O=[V](=O)O[V](=O)=O GNTDGMZSJNCJKK-UHFFFAOYSA-N 0.000 claims description 8
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims description 8
- 239000002270 dispersing agent Substances 0.000 claims description 7
- 238000010438 heat treatment Methods 0.000 claims description 6
- -1 polyethylene Polymers 0.000 claims description 6
- 239000002518 antifoaming agent Substances 0.000 claims description 5
- PNEYBMLMFCGWSK-UHFFFAOYSA-N Alumina Chemical compound [O-2].[O-2].[O-2].[Al+3].[Al+3] PNEYBMLMFCGWSK-UHFFFAOYSA-N 0.000 claims description 4
- 239000000853 adhesive Substances 0.000 claims description 4
- 230000001070 adhesive effect Effects 0.000 claims description 4
- 238000000498 ball milling Methods 0.000 claims description 4
- WMWLMWRWZQELOS-UHFFFAOYSA-N bismuth(III) oxide Inorganic materials O=[Bi]O[Bi]=O WMWLMWRWZQELOS-UHFFFAOYSA-N 0.000 claims description 4
- 229910000019 calcium carbonate Inorganic materials 0.000 claims description 4
- 239000007822 coupling agent Substances 0.000 claims description 4
- 238000004519 manufacturing process Methods 0.000 claims description 4
- 239000005543 nano-size silicon particle Substances 0.000 claims description 4
- ZKATWMILCYLAPD-UHFFFAOYSA-N niobium pentoxide Inorganic materials O=[Nb](=O)O[Nb](=O)=O ZKATWMILCYLAPD-UHFFFAOYSA-N 0.000 claims description 4
- URLJKFSTXLNXLG-UHFFFAOYSA-N niobium(5+);oxygen(2-) Chemical compound [O-2].[O-2].[O-2].[O-2].[O-2].[Nb+5].[Nb+5] URLJKFSTXLNXLG-UHFFFAOYSA-N 0.000 claims description 4
- 235000012239 silicon dioxide Nutrition 0.000 claims description 4
- QBUKAFSEUHGMMX-MTJSOVHGSA-N (5z)-5-[[3-(1-hydroxyethyl)thiophen-2-yl]methylidene]-10-methoxy-2,2,4-trimethyl-1h-chromeno[3,4-f]quinolin-9-ol Chemical compound C1=CC=2NC(C)(C)C=C(C)C=2C2=C1C=1C(OC)=C(O)C=CC=1O\C2=C/C=1SC=CC=1C(C)O QBUKAFSEUHGMMX-MTJSOVHGSA-N 0.000 claims description 3
- 239000004698 Polyethylene Substances 0.000 claims description 3
- 239000002202 Polyethylene glycol Substances 0.000 claims description 3
- 239000004372 Polyvinyl alcohol Substances 0.000 claims description 3
- 239000011230 binding agent Substances 0.000 claims description 3
- 239000004205 dimethyl polysiloxane Substances 0.000 claims description 3
- 229920000435 poly(dimethylsiloxane) Polymers 0.000 claims description 3
- 229920000573 polyethylene Polymers 0.000 claims description 3
- 229920001223 polyethylene glycol Polymers 0.000 claims description 3
- 229920002689 polyvinyl acetate Polymers 0.000 claims description 3
- 239000011118 polyvinyl acetate Substances 0.000 claims description 3
- 229920002451 polyvinyl alcohol Polymers 0.000 claims description 3
- 229910000859 α-Fe Inorganic materials 0.000 description 8
- 238000012360 testing method Methods 0.000 description 4
- XEEYBQQBJWHFJM-UHFFFAOYSA-N iron Substances [Fe] XEEYBQQBJWHFJM-UHFFFAOYSA-N 0.000 description 3
- 230000035699 permeability Effects 0.000 description 3
- UQSXHKLRYXJYBZ-UHFFFAOYSA-N Iron oxide Chemical compound [Fe]=O UQSXHKLRYXJYBZ-UHFFFAOYSA-N 0.000 description 2
- 239000002671 adjuvant Substances 0.000 description 2
- 239000013530 defoamer Substances 0.000 description 2
- 239000000696 magnetic material Substances 0.000 description 2
- 238000002156 mixing Methods 0.000 description 2
- 239000011163 secondary particle Substances 0.000 description 2
- 150000004649 carbonic acid derivatives Chemical class 0.000 description 1
- 238000011156 evaluation Methods 0.000 description 1
- 238000002474 experimental method Methods 0.000 description 1
- 239000006260 foam Substances 0.000 description 1
- 230000006698 induction Effects 0.000 description 1
- 229910044991 metal oxide Inorganic materials 0.000 description 1
- 150000004706 metal oxides Chemical class 0.000 description 1
- 239000000203 mixture Substances 0.000 description 1
- 238000012986 modification Methods 0.000 description 1
- 230000004048 modification Effects 0.000 description 1
- 239000002994 raw material Substances 0.000 description 1
- 230000000630 rising effect Effects 0.000 description 1
- 238000003756 stirring Methods 0.000 description 1
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- C04B35/26—Shaped ceramic products characterised by their composition; Ceramics compositions; Processing powders of inorganic compounds preparatory to the manufacturing of ceramic products based on oxide ceramics based on ferrites
- C04B35/2608—Compositions containing one or more ferrites of the group comprising manganese, zinc, nickel, copper or cobalt and one or more ferrites of the group comprising rare earth metals, alkali metals, alkaline earth metals or lead
- C04B35/2633—Compositions containing one or more ferrites of the group comprising manganese, zinc, nickel, copper or cobalt and one or more ferrites of the group comprising rare earth metals, alkali metals, alkaline earth metals or lead containing barium, strontium or calcium
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- H01F1/34—Magnets or magnetic bodies characterised by the magnetic materials therefor; Selection of materials for their magnetic properties of inorganic materials characterised by their coercivity of soft-magnetic materials non-metallic substances, e.g. ferrites
- H01F1/342—Oxides
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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
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: fe (Fe) 2 O 3 45 to 55 parts, 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 0.1mol/L to 0.3mol/L FeCL 3 ZnCL of 0.1mol/L to 0.3mol/L 2 NiCL of 0.4mol/L to 0.8mol/L 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: fe (Fe) 2 O 3 45 to 55 parts of NiO20 to 28 parts of ZnO 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: fe (Fe) 2 O 3 45 to 55 parts, 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 0.1mol/L to 0.3mol/L FeCL 3 ZnCL of 0.1mol/L to 0.3mol/L 2 NiCL of 0.4mol/L to 0.8mol/L 2 。
Specifically, the primary particles are obtained by adding a strengthening solution into the primary powder and granulating the mixture. The strengthening solution comprises 0.1mol/L to 0.3mol/L FeCL 3 ZnCL of 0.1mol/L to 0.3mol/L 2 NiCL of 0.4mol/L to 0.8mol/L 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 (10)
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: 345 to 55 parts of Fe2O, 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 FeCL3, 0.1 to 0.3mol/L ZnCL2 and 0.4 to 0.8mol/L NiCL2;
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.
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 first granulation step, the mass ratio of the main charge powder and the strengthening solution is 1:1.2 to 1:1.
4. 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.
5. 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.
6. The process according to claim 1, characterized in that in the second granulation step, the dispersant is a polyethylene wax.
7. The process according to claim 1, characterized in that in the second granulation step, the antifoaming agent is polydimethylsiloxane.
8. The process according to claim 1, wherein in the second particle strengthening improvement step, the mass ratio of the improvement liquid to the second particles is from 1:8 to 1:5.
9. 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.
10. The process of claim 9, wherein the ramp rate is from 70 degrees celsius per minute to 100 degrees celsius per minute.
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