CN117809924A - Low-loss nanocrystalline composite material and preparation method and application thereof - Google Patents
Low-loss nanocrystalline composite material and preparation method and application thereof Download PDFInfo
- Publication number
- CN117809924A CN117809924A CN202311760616.4A CN202311760616A CN117809924A CN 117809924 A CN117809924 A CN 117809924A CN 202311760616 A CN202311760616 A CN 202311760616A CN 117809924 A CN117809924 A CN 117809924A
- Authority
- CN
- China
- Prior art keywords
- powder
- nanocrystalline composite
- loss
- insulating layer
- composite material
- Prior art date
- Legal status (The legal status is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the status listed.)
- Pending
Links
- 239000002131 composite material Substances 0.000 title claims abstract description 81
- 238000002360 preparation method Methods 0.000 title abstract description 17
- 229910052751 metal Inorganic materials 0.000 claims abstract description 48
- 239000002184 metal Substances 0.000 claims abstract description 48
- 239000000956 alloy Substances 0.000 claims abstract description 46
- 229910045601 alloy Inorganic materials 0.000 claims abstract description 45
- 238000000034 method Methods 0.000 claims abstract description 16
- 238000003825 pressing Methods 0.000 claims abstract description 10
- 238000002425 crystallisation Methods 0.000 claims abstract description 5
- 230000008025 crystallization Effects 0.000 claims abstract description 5
- 239000000843 powder Substances 0.000 claims description 85
- 239000010410 layer Substances 0.000 claims description 52
- 239000011248 coating agent Substances 0.000 claims description 39
- 238000000576 coating method Methods 0.000 claims description 39
- LYCAIKOWRPUZTN-UHFFFAOYSA-N Ethylene glycol Chemical compound OCCO LYCAIKOWRPUZTN-UHFFFAOYSA-N 0.000 claims description 25
- 229920005989 resin Polymers 0.000 claims description 25
- 239000011347 resin Substances 0.000 claims description 25
- XEEYBQQBJWHFJM-UHFFFAOYSA-N iron Substances [Fe] XEEYBQQBJWHFJM-UHFFFAOYSA-N 0.000 claims description 21
- RYGMFSIKBFXOCR-UHFFFAOYSA-N Copper Chemical compound [Cu] RYGMFSIKBFXOCR-UHFFFAOYSA-N 0.000 claims description 16
- 239000011247 coating layer Substances 0.000 claims description 15
- 238000000137 annealing Methods 0.000 claims description 14
- 229910005347 FeSi Inorganic materials 0.000 claims description 10
- 238000001694 spray drying Methods 0.000 claims description 9
- 238000003723 Smelting Methods 0.000 claims description 8
- 229910002555 FeNi Inorganic materials 0.000 claims description 7
- 238000004519 manufacturing process Methods 0.000 claims description 7
- 238000002156 mixing Methods 0.000 claims description 7
- 238000005303 weighing Methods 0.000 claims description 6
- WGCNASOHLSPBMP-UHFFFAOYSA-N hydroxyacetaldehyde Natural products OCC=O WGCNASOHLSPBMP-UHFFFAOYSA-N 0.000 claims description 5
- 230000001939 inductive effect Effects 0.000 claims description 4
- 239000007788 liquid Substances 0.000 claims description 4
- 239000002159 nanocrystal Substances 0.000 claims description 4
- 239000000463 material Substances 0.000 abstract description 24
- 230000008569 process Effects 0.000 abstract description 7
- 230000000694 effects Effects 0.000 abstract description 4
- 238000000746 purification Methods 0.000 abstract description 2
- 230000000630 rising effect Effects 0.000 abstract description 2
- 238000006243 chemical reaction Methods 0.000 description 24
- 238000005906 dihydroxylation reaction Methods 0.000 description 15
- 239000002245 particle Substances 0.000 description 11
- 230000000052 comparative effect Effects 0.000 description 10
- 239000011541 reaction mixture Substances 0.000 description 9
- 239000002002 slurry Substances 0.000 description 9
- AQRLNPVMDITEJU-UHFFFAOYSA-N triethylsilane Chemical compound CC[SiH](CC)CC AQRLNPVMDITEJU-UHFFFAOYSA-N 0.000 description 8
- 239000003085 diluting agent Substances 0.000 description 7
- 238000000498 ball milling Methods 0.000 description 6
- 238000001816 cooling Methods 0.000 description 6
- 239000010949 copper Substances 0.000 description 6
- 229910052802 copper Inorganic materials 0.000 description 6
- 239000002994 raw material Substances 0.000 description 6
- 239000000203 mixture Substances 0.000 description 5
- 238000004381 surface treatment Methods 0.000 description 5
- VYPSYNLAJGMNEJ-UHFFFAOYSA-N Silicium dioxide Chemical compound O=[Si]=O VYPSYNLAJGMNEJ-UHFFFAOYSA-N 0.000 description 4
- 238000004140 cleaning Methods 0.000 description 4
- 238000005516 engineering process Methods 0.000 description 4
- 238000005259 measurement Methods 0.000 description 4
- 239000002707 nanocrystalline material Substances 0.000 description 4
- TWNQGVIAIRXVLR-UHFFFAOYSA-N oxo(oxoalumanyloxy)alumane Chemical compound O=[Al]O[Al]=O TWNQGVIAIRXVLR-UHFFFAOYSA-N 0.000 description 4
- 229910052814 silicon oxide Inorganic materials 0.000 description 4
- 239000000126 substance Substances 0.000 description 4
- MCULRUJILOGHCJ-UHFFFAOYSA-N triisobutylaluminium Chemical compound CC(C)C[Al](CC(C)C)CC(C)C MCULRUJILOGHCJ-UHFFFAOYSA-N 0.000 description 4
- DNIAPMSPPWPWGF-UHFFFAOYSA-N Propylene glycol Chemical compound CC(O)CO DNIAPMSPPWPWGF-UHFFFAOYSA-N 0.000 description 3
- 238000000354 decomposition reaction Methods 0.000 description 3
- 238000007865 diluting Methods 0.000 description 3
- 238000001035 drying Methods 0.000 description 3
- 239000000696 magnetic material Substances 0.000 description 3
- 238000012986 modification Methods 0.000 description 3
- 230000004048 modification Effects 0.000 description 3
- 229920002050 silicone resin Polymers 0.000 description 3
- IJGRMHOSHXDMSA-UHFFFAOYSA-N Atomic nitrogen Chemical compound N#N IJGRMHOSHXDMSA-UHFFFAOYSA-N 0.000 description 2
- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical group [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 description 2
- 239000004593 Epoxy Substances 0.000 description 2
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 description 2
- 238000003917 TEM image Methods 0.000 description 2
- 238000000889 atomisation Methods 0.000 description 2
- 238000010586 diagram Methods 0.000 description 2
- PCHJSUWPFVWCPO-UHFFFAOYSA-N gold Chemical compound [Au] PCHJSUWPFVWCPO-UHFFFAOYSA-N 0.000 description 2
- 239000010931 gold Substances 0.000 description 2
- 229910052737 gold Inorganic materials 0.000 description 2
- 230000001965 increasing effect Effects 0.000 description 2
- 238000002844 melting Methods 0.000 description 2
- 230000008018 melting Effects 0.000 description 2
- 238000012545 processing Methods 0.000 description 2
- 238000012216 screening Methods 0.000 description 2
- 230000009286 beneficial effect Effects 0.000 description 1
- 229910052799 carbon Inorganic materials 0.000 description 1
- 239000003153 chemical reaction reagent Substances 0.000 description 1
- 238000010344 co-firing Methods 0.000 description 1
- 230000006835 compression Effects 0.000 description 1
- 238000007906 compression Methods 0.000 description 1
- 238000011161 development Methods 0.000 description 1
- 238000009826 distribution Methods 0.000 description 1
- 230000004907 flux Effects 0.000 description 1
- 230000014509 gene expression Effects 0.000 description 1
- 229920006015 heat resistant resin Polymers 0.000 description 1
- 238000010438 heat treatment Methods 0.000 description 1
- 230000006872 improvement Effects 0.000 description 1
- 239000004615 ingredient Substances 0.000 description 1
- 229910052742 iron Inorganic materials 0.000 description 1
- 229910001004 magnetic alloy Inorganic materials 0.000 description 1
- 239000011268 mixed slurry Substances 0.000 description 1
- 238000000465 moulding Methods 0.000 description 1
- 229910052757 nitrogen Inorganic materials 0.000 description 1
- 238000011056 performance test Methods 0.000 description 1
- 230000035699 permeability Effects 0.000 description 1
- 230000009467 reduction Effects 0.000 description 1
- 238000005507 spraying Methods 0.000 description 1
- 238000006467 substitution reaction Methods 0.000 description 1
- 238000004804 winding Methods 0.000 description 1
Abstract
The invention relates to the technical field of inductance materials, in particular to a low-loss nanocrystalline composite material, a preparation method and application thereof. The application discloses a low-loss nanocrystalline composite material, which comprises metal coated by an insulating layer and amorphous nano alloy; the thickness of the insulating layer is 30-50nm; the granularity of the nanocrystalline composite material is 20-120 mu m; the granularity of the amorphous nano alloy is 9-40 mu m; according to the nanocrystalline composite material, the problem of hysteresis loss rising caused by pressing can be greatly reduced by reducing the purification temperature of the amorphous nano alloy and utilizing the stress relief effect in the crystallization process.
Description
Technical Field
The invention relates to the technical field of inductance materials, in particular to a low-loss nanocrystalline composite material, a preparation method and application thereof.
Background
With the increasing development of AI technology, the requirements of large models on data processing capability are higher and higher, so that the power density of a power supply is required to be increased gradually, and the improvement of the switching frequency and the increase of current of the power supply are main technical routes of power supply technology selection, wherein the smaller the magnetic loss of an inductance device of the power supply is, the higher the conversion efficiency of the power supply is. High power chips such as GPUs are in urgent need for high energy density low loss inductive devices, which requires that the loss of materials be reduced as much as possible.
In order to obtain a low-loss material, an amorphous or nanocrystalline material, an alloy composite material such as carbonyl iron powder and the like are generally adopted, so that the magnetic loss of the material is reduced while the direct-current bias performance is ensured, but the conventional amorphous nanocrystalline material cannot be annealed at the temperature of more than 400 ℃ because copper wires are contained in the material, so that the power consumption cannot be substantially reduced.
The copper-magnetic cofiring inductance technology is a new product technology which is developed recently, and is formed by pressing soft magnetic alloy materials and copper wires, and the magnetic loss is reduced by eliminating high-voltage lattice distortion of FeSiAl, feNi and other materials at about 700 ℃, but the loss is not obviously reduced due to the severe increase of eddy current loss caused by local failure of a coating layer on the surface of the material due to high temperature.
Therefore, the current material system realizes the effect of annealing with copper wires together to eliminate the loss increase caused by stress, and is a current technical difficulty.
Therefore, the application provides a low-loss nanocrystalline composite material, and a preparation method and application thereof.
Disclosure of Invention
According to the low-loss nanocrystalline composite material, the preparation method and the application thereof, the hysteresis loss rising problem caused by pressing can be greatly reduced by reducing the purification temperature of amorphous nano alloy and utilizing the stress relief effect in the crystallization process of the nanocrystalline composite material; meanwhile, the nanocrystalline composite material can be made of various coating materials and heat-resistant resins, so that the failure of the insulating coating layers on the surfaces of copper wires and particles is prevented, and the nanocrystalline composite material has excellent saturation characteristics and low magnetic loss.
The aim of the invention is achieved by the following technical scheme:
the first object of the present application is to provide a low-loss nanocrystalline composite material, comprising an insulating layer-coated metal, and an amorphous nanocrystalline alloy;
the thickness of the insulating layer is 30-50nm;
the granularity of the nanocrystalline composite material is 20-120 mu m;
the granularity of the amorphous nano alloy is 9-40 mu m.
Preferably, the amorphous nano alloy comprises the following chemical components in percentage by weight: 78-84% of Fe, 7.5-9.0% of Co, 4.5-5.5% of P, 0.8-1.5% of B, 0.4-1.0% of C, 1.5-2.0% of Si, 1.3-2.0% of Nb and 0.5-1.0% of Sn.
Preferably, the crystallization temperature of the amorphous nano alloy is less than 350 ℃.
Preferably, the nanocrystalline composite material has a loss of 1200-1400mW/cm at 1MHz//50mT 3 The inductance can be maintained at 70% or more of the inductance value without applying a DC magnetic field at the applied DC magnetic field strength of 240 Oe.
Preferably, the metal in the metal coated by the insulating layer comprises one or more of FeSi powder, feSiAl powder, feSiCr powder and FeNi powder.
The second object of the present application is to provide a method for preparing the nanocrystalline composite material, which comprises the following steps:
smelting and atomizing to obtain amorphous nano alloy;
preparing metal powder coated by an insulating layer;
weighing 2-7 parts of amorphous nano alloy, 7-12 parts of metal powder coated by an insulating layer and 1-2.5 parts of resin, mixing, and then performing spray drying to obtain the nano crystal composite material.
Preferably, the process for preparing the insulating layer coated metal powder comprises the following steps:
selecting one or more of FeSi powder, feSiAl powder, feSiCr powder and FeNi powder, mixing with carbonyl iron powder, and reacting with glycol; adding a coating liquid to carry out multiple coating; forming a multi-layer coating to form an inorganic composite coating layer; and (3) controlling the granularity of the powder to be 1-7 mu m through a classifier after coating, and preparing the metal powder coated with the insulating layer.
Preferably, the smelting temperature is 1380-1450 ℃.
A third object of the present application is to provide an application of a low-loss nanocrystalline composite, which is applied to the preparation of an inductance device.
Preferably, the nanocrystalline composite is applied to a method for manufacturing an inductance device, comprising the steps of: pressing the nanocrystalline composite material and the copper wire to form an inductance blank; and (3) annealing the inductor blank at 300-350 ℃ to form an annealed blank.
The beneficial effects of this application are:
1. according to the nanocrystalline composite material, the nanocrystalline composite material is obtained under the low-temperature annealing condition by adopting amorphous nano alloy with a certain content, and the stress annealing temperature can be reduced to below 350 ℃;
2. the nanocrystalline composite material removes stress by using the crystallization process of the amorphous nano alloy, and simultaneously, the saturation current of the nanocrystalline composite material is superior to that of the existing material system by using the combination of different materials;
3. according to the nanocrystalline composite material, the surface of the high-saturation magnetic flux material such as carbonyl iron powder is coated with the material with excellent toughness and temperature resistance exceeding 400 ℃, so that the surface insulating layer is not damaged by pressing and annealing treatment, and the lower eddy current loss is maintained;
4. the nanocrystalline composite material has excellent loss characteristics, and the loss of the nanocrystalline composite material at 1MHz//50mT is 1200-1400mW/cm 3 The direct current superposition performance is excellent, the inductance can be kept at more than 70% of the inductance value without applying a direct current magnetic field under the condition that the intensity of an external direct current magnetic field is 240Oe, and the direct current superposition device can be used for preparing various different power inductance devices with higher requirements on efficiency and has higher application value.
Drawings
The invention will be further described with reference to the drawings and examples.
FIG. 1 is a process flow diagram of a method for preparing a low-loss nanocrystalline composite as described herein;
FIG. 2 is a cross-sectional TEM image of carbonyl iron powder coating material of example 2 of the present application;
FIG. 3 is a cross-sectional TEM image of carbonyl iron powder coating material of comparative example 2 of the present application;
fig. 4 is a schematic structural diagram of an inductor blank formed by pressing the nanocrystalline composite material and copper wire described in the present application.
Detailed Description
The invention will be further illustrated by the following examples, which are not intended to limit the scope of the invention, in order to facilitate the understanding of those skilled in the art.
As used herein, "and/or" includes any and all combinations of one or more of the associated listed items. The terminology used herein is for the purpose of describing particular embodiments only and is not intended to be limiting of the invention. As used herein, the singular forms "a", "an", and "the" are intended to include the plural forms as well, unless the context clearly indicates otherwise. It will be further understood that the terms "comprises" and/or "comprising," when used in this specification, specify the presence of stated features, integers, steps, operations, elements, and/or components, but do not preclude the presence or addition of one or more other features, integers, steps, operations, elements, components, and/or groups thereof.
Unless defined otherwise, all terms (including technical and scientific terms) used herein have the same meaning as commonly understood by one of ordinary skill in the art to which this invention belongs. It will be further understood that terms, such as those defined in commonly used dictionaries, should be interpreted as having a meaning that is consistent with their meaning in the context of the relevant art and will not be interpreted in an idealized or overly formal sense unless expressly so defined herein.
The exemplary invention described herein may suitably lack any one or more of the element limitations not specifically disclosed herein. Thus, the terms "comprising," "including," "containing," and the like are to be construed broadly and without limitation. In addition, the term expressions which have been employed herein are used as terms of description and not of limitation, and there is no intention in the use of such terms of description not including any equivalents of the features shown and described, but rather, in accordance with the claims, various modifications are possible within the scope of the invention. Thus, while the invention has been specifically disclosed by preferred embodiments and optional features, modification of the invention disclosed herein may be resorted to by those skilled in the art, and such modifications and variations are considered to be within the scope of this invention.
The raw materials or reagents used in the examples and comparative examples of the present invention were purchased from mainstream commercial manufacturers, and were of analytically pure grade that could be conventionally obtained without any particular limitation, as long as they were capable of achieving the intended effects. The instruments used in this example are all purchased from major market manufacturers and are not particularly limited as long as they can function as intended. No particular technique or condition is identified in this example, which is performed according to techniques or conditions described in the literature in this field or according to product specifications.
The inventor finds that after the alloy soft magnetic material is pressed into a product, a pure metal system is usually adopted for high-temperature annealing or an amorphous nanocrystalline system is compounded with a gold system for low-pressure forming, so that the problem of loss reduction is solved, but the annealing at the temperature of more than 600 ℃ is easy to cause short circuit and other problems due to failure of a coating layer on the surface of a copper wire, and the powder coating layer is easy to fail at the temperature of more than 600 ℃ and also easy to cause severe rise of eddy current loss; the amorphous nanocrystalline system is compounded with a gold system, and the problem that hysteresis loss rise and loss increase easily occur due to compression cannot be completely removed due to low curing temperature in low-pressure molding.
The invention provides a low-loss nanocrystalline composite material which comprises the following raw materials in parts by weight:
2-7 parts of amorphous nano alloy
7-12 parts of metal coated by insulating layer
1-2.5 parts of resin;
the amorphous nano alloy comprises the following chemical components in percentage by weight: 78-84% of Fe, 7.5-9.0% of Co, 4.0-5.5% of P, 0.8-1.5% of B, 0.4-1.0% of C, 1.5-2.0% of Si, 1.3-2.0% of Nb and 0.5-1.0% of Sn; the weight parts of the specific amorphous nano alloy can be 2 parts, 3 parts, 4 parts, 5 parts, 6 parts and 7 parts; the weight parts of the metal coated by the specific insulating layer can be 7 parts, 8 parts, 9 parts, 10 parts, 11 parts and 12 parts; the weight parts of the resin may be 1 part, 1.5 parts, 2 parts, 2.5 parts. The weight proportion of the amorphous nano alloy, the metal coated by the insulating layer and the resin can be combined in the weight proportion range, for example, 2 parts of the amorphous nano alloy, 7 parts of the metal coated by the insulating layer and 1 part of the resin are selected; or 7 parts of amorphous nano alloy, 12 parts of metal coated by an insulating layer and 2.5 parts of resin are selected; or 4 parts of amorphous nano alloy, 10 parts of metal coated by an insulating layer and 2 parts of resin are selected; 2 parts of amorphous nano alloy, 12 parts of metal coated by an insulating layer and 1.5 parts of resin are selected; or 7 parts of amorphous nano alloy, 7 parts of metal coated by an insulating layer and 2.5 parts of resin are selected.
In some specific embodiments, the low-loss nanocrystalline composite finished product comprises an insulating layer-clad metal, an amorphous nanocrystalline alloy, and a resin layer; the thickness of the insulating layer is 30-50nm; the granularity of the nanocrystalline composite material is 20-120 mu m; the granularity of the amorphous nano alloy is 9-40 mu m. The loss of the nanocrystalline composite material finished product at 1MHz//50mT is 1200-1400mW/cm 3 The inductance can be maintained at 70% or more of the inductance value without applying a DC magnetic field at the applied DC magnetic field strength of 240 Oe.
In some specific embodiments, the metal in the metal coated by the insulating layer is carbonyl iron powder and one or more of FeSi powder, fesai powder, feSiCr powder, feNi powder. The thickness of the insulating layer is 30-50nm.
In some specific embodiments, the resin (the resin forming the resin layer) is an epoxy modified silicone resin, requiring a decomposition temperature greater than 500 ℃. For example, the epoxy modified silicone resin adopts KR311 which is believed to be more chemical, the decomposition temperature of the resin is more than 500 ℃ (other types of resins such as silicone resins with decomposition temperature of more than 500 ℃ can be adopted), and the resin is prevented from being invalid in the heat treatment process of the product, so that the strength of the product is prevented from being deteriorated.
On the other hand, the preparation method of the low-loss nanocrystalline composite material comprises the following steps:
smelting and atomizing to obtain amorphous nano alloy;
preparing metal powder coated by an insulating layer;
weighing 2-7 parts of amorphous nano alloy, 7-12 parts of metal powder coated by an insulating layer and 1-2.5 parts of resin, mixing, and then performing spray drying to obtain the nano crystal composite material.
The specific process is as follows:
(1) Preparation of materials
Preparing raw materials containing corresponding chemical components according to the weight parts of the amorphous nano alloy;
(2) Smelting atomization
The raw materials of the amorphous nano alloy in the step (1) are subjected to vacuum melting, molten slurry is formed by melting at 1380-1450 ℃, and the molten slurry is subjected to atomization cooling and drying to obtain the amorphous nano alloy;
(3) Screening is carried out
The dried amorphous nano alloy is distributed into amorphous nano alloy with the granularity of 9-40 mu m by a classifier;
(4) Surface treatment
Selecting one or more of FeSi powder, feSiAl powder, feSiCr powder and FeNi powder, mixing with carbonyl iron powder, and reacting with glycol; adding a coating liquid to carry out multiple coating; forming a multi-layer coating to form an inorganic composite coating layer; controlling the granularity of the powder to be 1-7 mu m through a classifier after coating to form metal powder coated by an insulating layer;
(5) Grading of products
Weighing 2-7 parts of amorphous nano alloy, 7-12 parts of metal powder coated by an insulating layer and 1-2.5 parts of resin, diluting into mixed slurry by a diluent, performing wet ball milling and dispersing, performing spray drying, grading by grading equipment, controlling the particle size of particles to be 20-120 mu m, and grading to obtain the nano-crystalline composite material.
In some specific embodiments, in step (4), carbonyl iron powder and one or more of FeSi powder, fesai powder, feSiCr powder, feNi powder are added to ethylene glycol and reacted at 120-150 ℃ for 3-5 hours.
In some specific embodiments, in step (4), the coating reaction is performed with a dehydroxylation reaction mixture obtained by a glycol dehydroxylation reaction, and a coating liquid containing an oxide.
In some specific embodiments, in step (5), the diluent is at least one of ethanol, propylene glycol.
The application of the low-loss nanocrystalline composite material is that the nanocrystalline composite material is applied to the preparation of an inductance device.
In some specific embodiments, the nanocrystalline composite is applied to a method of making an inductive device, comprising the steps of: pressing the nanocrystalline composite material with copper wires through a press to form an inductance blank; annealing the inductor blank at 300-350 ℃ to form an annealed blank; and (5) processing the annealed blank to obtain a copper wire terminal structure, and tinning the surface of the copper wire terminal to obtain the inductance device.
The technical solutions of the present application are illustrated by the following detailed experimental examples, examples and comparative examples:
experimental example
A method for preparing a low-loss nanocrystalline composite material shown in fig. 1, which comprises the following steps:
1) And (3) batching: weighing and proportioning Fe, co, P, B, C, si, nb, sn serving as a raw material according to the formula shown in Table 1;
2) Smelting and atomizing: smelting the ingredients in the step 1) in vacuum to form metal slurry at 1380-1450 ℃, atomizing and cooling the slurry to form metal powder with the granularity of 1-70 mu m, and drying the metal powder with nitrogen to obtain metal powder;
3) And (3) screening: the dried powder was subjected to controlled distribution of powder particle size into 9-40 μm amorphous nano alloy powder (no annealing treatment at this time, the material was in an amorphous state) by a classifier to obtain amorphous nano alloy 1, amorphous nano alloy 2, amorphous nano alloy 3 as described in table 1.
4) Surface treatment: carbonyl iron powder with granularity of 1-12 mu m is selected; selecting one or more of FeSi powder, feSiAl powder, feSiCr powder and FeNi powder; at least one of FeSi powder, feSiAl powder, feSiCr powder and FeNi powder is subjected to dehydroxylation reaction with ethylene glycol and then is combined with the surface of carbonyl iron powder to form a carbon chain, the other end of the carbon chain and oxide are then formed into an insulating coating layer, and a 30-50nm inorganic composite coating layer is formed through multilayer coating; controlling the granularity of the powder to be 1-7 mu m through a classifier after coating to form metal powder coated by an insulating layer;
the specific process is as follows: carbonyl iron powder with granularity of 1-12 mu m is selected; selecting second powder with granularity of 1-12 μm (the second powder is at least one of FeSi powder, feSiAl powder, feSiCr powder and FeNi powder); the feeding weight ratio of the carbonyl iron powder to the second powder is 3:1;
uniformly mixing carbonyl iron powder and second powder, adding glycol, and carrying out dehydroxylation reaction for 3-5 hours at 120-150 ℃; after the reaction is finished, cooling to room temperature, performing surface cleaning to obtain a dehydroxylation reaction mixture, and performing a coating reaction on the dehydroxylation reaction mixture and a coating solution (triisobutylaluminum or triethylsilane) containing oxide (aluminum oxide or silicon oxide) at 80-120 ℃ to obtain metal coated by an insulating layer after the reaction is finished; multiple coating reactions can be carried out according to actual needs; forming an inorganic composite coating layer of 30-50nm through multi-layer coating; controlling the granularity of the powder to be 1-7 mu m through a classifier after coating to form metal powder coated by an insulating layer;
5) Grading: weighing d parts of amorphous nano alloy powder, e parts of insulating layer coated metal powder and f parts of resin, wherein d is 2-7 parts, e is 7-12 parts, f is 1-2.5 parts, and the specific parts are as shown in table 2, diluting into slurry by a diluent, performing wet ball milling and dispersing, spray drying, grading by grading equipment, controlling the particle size of particles to be 20-120 mu m, and grading to obtain a final nano crystal composite material;
the preparation method of the power inductor composed of the low-loss nanocrystalline composite material shown in fig. 4 comprises the following specific steps:
(1) Pressing the main powder through a press and a copper wire to form an inductance blank;
(2) Annealing the inductor blank at 300-350 ℃ to form an annealed blank;
(3) Spraying resin on the surface of the annealed blank, drying, and exposing the bottom copper wire terminal structure through laser burning;
(4) Tinning the surface of the copper wire terminal to obtain a power inductor;
the electromagnetic performance of the power inductor was tested by LCR and the material loss was tested by BH analyzer, wherein the material loss was tested by magnetic loop winding of the inductor under the same pressing and annealing conditions, wherein the magnetic loop had a size of 8mm outside diameter, 5mm inside diameter, 2mm height, and the performance results are shown in table 3.
Example 1-example 6, amorphous nanoalloy 1, amorphous nanoalloy 2, amorphous nanoalloy 3 were prepared with reference to the preparation method of the amorphous nanoalloy of experimental example and the amorphous nanoalloy composition of table 1; example 1-example 6 referring again to the preparation method of the low-loss nanocrystalline composite material of experimental example and the raw material composition of experimental example of table 2, nanocrystalline composite materials were prepared, and corresponding performance tests were performed and recorded in table 3.
Comparative example 1
A preparation method of a nanocrystalline composite material comprises the following steps:
1) Surface treatment: feSiAl powder (14 parts) with granularity of 1-12 mu m is selected, ethylene glycol is added, and dehydroxylation reaction is carried out for 3-5 hours at 120-150 ℃; after the reaction is finished, cooling to room temperature, performing surface cleaning to obtain a dehydroxylation reaction mixture, and performing a coating reaction on the dehydroxylation reaction mixture and a coating solution (triisobutylaluminum or triethylsilane) containing oxide (aluminum oxide or silicon oxide) at 80-120 ℃ to obtain metal coated by an insulating layer after the reaction is finished; multiple coating reactions can be carried out according to actual needs; forming an inorganic composite coating layer of 30-50nm through multi-layer coating; controlling the granularity of the powder to be 1-7 mu m through a classifier after coating to form metal powder coated by an insulating layer;
2) Grading: 14 parts of insulating layer coated metal powder and 2.5 parts of resin; specific parts are shown in table 2; diluting into slurry by a diluent, performing wet ball milling and dispersing, performing spray drying, grading by a grading device, controlling the particle size of particles to be 20-120 mu m, and grading to obtain a final nanocrystalline composite material; the nanocrystalline composite material was prepared, and the corresponding performance measurements were performed and recorded in table 3.
Comparative example 2
A preparation method of a nanocrystalline composite material comprises the following steps:
1) Surface treatment: selecting FeSiBNBCu powder (2 parts) with granularity of 1-12 mu m, selecting carbonyl iron powder (12 parts) with granularity of 1-12 mu m, adding ethylene glycol, and carrying out dehydroxylation reaction for 3-5 hours at 120-150 ℃; after the reaction is finished, cooling to room temperature, performing surface cleaning to obtain a dehydroxylation reaction mixture, and performing a coating reaction on the dehydroxylation reaction mixture and a coating solution (triisobutylaluminum or triethylsilane) containing oxide (aluminum oxide or silicon oxide) at 80-120 ℃ to obtain metal coated by an insulating layer after the reaction is finished; multiple coating reactions can be carried out according to actual needs; forming an inorganic composite coating layer of 30-50nm through multi-layer coating; controlling the granularity of the powder to be 1-7 mu m through a classifier after coating to form metal powder coated by an insulating layer;
2) Grading: 14 parts of insulating layer coated metal powder and 2.5 parts of resin; the specific parts are shown in table 2, the mixture is diluted into slurry by a diluent, then wet ball milling and dispersing are carried out, spray drying is carried out, classification is carried out by a classification device, the particle size is controlled to be 20-120 mu m, and the final nanocrystalline composite material is obtained after classification; the nanocrystalline composite material was prepared, and the corresponding performance measurements were performed and recorded in table 3.
Comparative example 3
A preparation method of a nanocrystalline composite material comprises the following steps:
1) Surface treatment: selecting FeSiBNBCu powder (2 parts) with granularity of 1-12 mu m, selecting carbonyl iron powder (12 parts) with granularity of 1-12 mu m, adding ethylene glycol, and carrying out dehydroxylation reaction for 3-5 hours at 120-150 ℃; after the reaction is finished, cooling to room temperature, performing surface cleaning to obtain a dehydroxylation reaction mixture, and performing a coating reaction on the dehydroxylation reaction mixture and a coating solution (triisobutylaluminum or triethylsilane) containing oxide (aluminum oxide or silicon oxide) at 80-120 ℃ to obtain metal coated by an insulating layer after the reaction is finished; multiple coating reactions can be carried out according to actual needs; forming an inorganic composite coating layer of 30-50nm through multi-layer coating; controlling the granularity of the powder to be 1-7 mu m through a classifier after coating to form metal powder coated by an insulating layer;
2) Grading: 14 parts of insulating layer coated metal powder and 2.5 parts of resin; the specific parts are shown in table 2, the mixture is diluted into slurry by a diluent, then wet ball milling and dispersing are carried out, spray drying is carried out, classification is carried out by a classification device, the particle size is controlled to be 20-120 mu m, and the final nanocrystalline composite material is obtained after classification; the nanocrystalline composite material was prepared, and the corresponding performance measurements were performed and recorded in table 3.
Comparative example 3
A preparation method of a nanocrystalline composite material comprises the following steps:
1) Grading: 14 parts of amorphous nano alloy 1 (as shown in table 1), 1 part of resin; the specific parts are shown in table 2, the mixture is diluted into slurry by a diluent, then wet ball milling and dispersing are carried out, spray drying is carried out, classification is carried out by a classification device, the particle size is controlled to be 20-120 mu m, and the final nanocrystalline composite material is obtained after classification; the nanocrystalline composite material was prepared, and the corresponding performance measurements were performed and recorded in table 3.
TABLE 1
TABLE 2
TABLE 3 Table 3
Examples 1-6 herein, which can anneal with copper wire at 300℃and have low magnetic loss (1200-1400mW/cm 3 ) The inductance energy of the applied direct current magnetic field strength 240Oe is kept above 70% of the inductance value of the direct current magnetic field which is not applied, and the magnetic material is suitable for being applied to magnetic materials required by power inductance devices.
In the comparative example 1, the traditional FeSiAl system and copper wires are adopted for high-temperature co-firing, the material has lower DC resistance, and the material has higher loss caused by low resistivity and higher short-circuit risk;
in comparative example 2, the conventional nanocrystalline material and carbonyl iron powder are adopted for grading, so that high-temperature annealing cannot be used, the residual stress of the material is large, and the loss is high;
in comparative example 3, only the nanocrystalline material of the present invention was used, and the material could not be crystallized without annealing at 300 ℃, resulting in higher loss and lower permeability.
As can be seen from fig. 2 and 3, the uniform coating layer formed in fig. 2 is more uniform and denser than the conventional coating layer formed in fig. 3. Therefore, the low-loss nanocrystalline composite materials prepared in examples 1-6 have the advantages of being not easy to damage under high pressure and high temperature, and therefore, the high resistivity is maintained.
The above embodiments are preferred embodiments of the present invention, and besides, the present invention may be implemented in other ways, and any obvious substitution is within the scope of the present invention without departing from the concept of the present invention.
Claims (10)
1. The low-loss nanocrystalline composite material is characterized by comprising metal coated by an insulating layer and amorphous nano alloy;
the thickness of the insulating layer is 30-50nm;
the granularity of the nanocrystalline composite material is 20-120 mu m;
the granularity of the amorphous nano alloy is 9-40 mu m.
2. The low-loss nanocrystalline composite according to claim 1, wherein the amorphous nanocrystalline alloy comprises, in weight percent: 78-84% of Fe, 7.5-9.0% of Co, 4.5-5.5% of P, 0.8-1.5% of B, 0.4-1.0% of C, 1.5-2.0% of Si, 1.3-2.0% of Nb and 0.5-1.0% of Sn.
3. The low-loss nanocrystalline composite according to claim 1, wherein the amorphous nanocrystalline alloy has a crystallization temperature < 350 ℃.
4. The low loss nanocrystalline composite according to claim 1, wherein the nanocrystalline composite has a loss of 1200-1400mW/cm at 1MHz//50mT 3 The inductance can be maintained at 70% or more of the inductance value without applying a DC magnetic field at the applied DC magnetic field strength of 240 Oe.
5. The nanocrystalline composite according to claim 1, wherein the metal in the metal covered by the insulating layer comprises one or more of FeSi powder, fesai powder, feSiCr powder, feNi powder.
6. The method for preparing a nanocrystalline composite according to any one of claims 1 to 5, comprising the steps of:
smelting and atomizing to obtain amorphous nano alloy;
preparing metal powder coated by an insulating layer;
weighing 2-7 parts of amorphous nano alloy, 7-12 parts of metal powder coated by an insulating layer and 1-2.5 parts of resin, mixing, and then performing spray drying to obtain the nano crystal composite material.
7. The method of claim 6, wherein the process for preparing the insulating layer coated metal powder comprises:
selecting one or more of FeSi powder, feSiAl powder, feSiCr powder and FeNi powder, mixing with carbonyl iron powder, and reacting with glycol; adding a coating liquid to carry out multiple coating; forming a multi-layer coating to form an inorganic composite coating layer; and (3) controlling the granularity of the powder to be 1-7 mu m through a classifier after coating, and preparing the metal powder coated with the insulating layer.
8. The method according to claim 6, wherein the smelting temperature is 1380-1450 ℃.
9. Use of a low-loss nanocrystalline composite, characterized in that the nanocrystalline composite according to any one of claims 1 to 5 or the nanocrystalline composite produced by the production method according to any one of claims 6 to 8 is applied to the production of an inductive component.
10. The use according to claim 9, characterized in that the nanocrystalline composite is applied to a method for producing an inductive device, comprising the steps of: pressing the nanocrystalline composite material and the copper wire to form an inductance blank; and (3) annealing the inductor blank at 300-350 ℃ to form an annealed blank.
Priority Applications (1)
Application Number | Priority Date | Filing Date | Title |
---|---|---|---|
CN202311760616.4A CN117809924A (en) | 2023-12-18 | 2023-12-18 | Low-loss nanocrystalline composite material and preparation method and application thereof |
Applications Claiming Priority (1)
Application Number | Priority Date | Filing Date | Title |
---|---|---|---|
CN202311760616.4A CN117809924A (en) | 2023-12-18 | 2023-12-18 | Low-loss nanocrystalline composite material and preparation method and application thereof |
Publications (1)
Publication Number | Publication Date |
---|---|
CN117809924A true CN117809924A (en) | 2024-04-02 |
Family
ID=90429308
Family Applications (1)
Application Number | Title | Priority Date | Filing Date |
---|---|---|---|
CN202311760616.4A Pending CN117809924A (en) | 2023-12-18 | 2023-12-18 | Low-loss nanocrystalline composite material and preparation method and application thereof |
Country Status (1)
Country | Link |
---|---|
CN (1) | CN117809924A (en) |
-
2023
- 2023-12-18 CN CN202311760616.4A patent/CN117809924A/en active Pending
Similar Documents
Publication | Publication Date | Title |
---|---|---|
CN104505209B (en) | A kind of soft magnetic metal composite core and preparation method thereof | |
CN106158340B (en) | A kind of Fe Si Al powder core toroidal magnets and preparation method thereof | |
CN112530655B (en) | Low-power-consumption soft magnetic alloy material and preparation method and application thereof | |
WO2014116004A1 (en) | Method for manufacturing fe-based amorphous metal powder and method for manufacturing amorphous soft magnetic cores using same | |
CN103730224A (en) | Preparation method for iron-based amorphous magnetic powder core with ultrahigh magnetic conductivity | |
CN113012886B (en) | High-resistance direct-current-superposition low-power-consumption integrally-formed inductance material and preparation method thereof | |
CN111451515B (en) | Low-power-consumption soft magnetic alloy material, preparation method thereof and electronic device | |
CN112509777A (en) | Soft magnetic alloy material and preparation method and application thereof | |
CN103745791A (en) | Production method of ultrahigh magnetic permeability of iron-based nanocrystalline magnetic powder core | |
CN107119174B (en) | Annealing method for improving DC bias performance of Fe-Si-Al soft magnetic powder core | |
CN113380483B (en) | Composite soft magnetic material and preparation method thereof | |
US6621399B2 (en) | Powder core and high-frequency reactor using the same | |
CN113223844A (en) | Powder coating method | |
EP3605567B1 (en) | Powder magnetic core with attached terminals and method for manufacturing the same | |
CN117809924A (en) | Low-loss nanocrystalline composite material and preparation method and application thereof | |
CN113223845B (en) | Insulating coating method of soft magnetic alloy powder | |
CN114133231A (en) | Nickel-zinc ferrite material and method for producing same | |
US6788185B2 (en) | Powder core and high-frequency reactor using the same | |
CN111383810A (en) | Preparation method of amorphous alloy magnetic powder core | |
KR100835886B1 (en) | Method of manufacturing high current smd inductor by using new type inner coil | |
CN115475935B (en) | Preparation method of iron-based soft magnetic composite powder and iron-based soft magnetic composite powder | |
CN116013678B (en) | Preparation method of low-loss ferrosilicon magnetic powder core material | |
CN115490507B (en) | Broadband high-strength heat shock-resistant nickel-zinc ferrite core and preparation method thereof | |
CN113539663B (en) | Soft magnetic composite material and preparation method and application thereof | |
JP2003188009A (en) | Compound magnetic material |
Legal Events
Date | Code | Title | Description |
---|---|---|---|
PB01 | Publication | ||
PB01 | Publication | ||
SE01 | Entry into force of request for substantive examination |