CN115862923A - Powder, conductive paste and magnetic device - Google Patents
Powder, conductive paste and magnetic device Download PDFInfo
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- CN115862923A CN115862923A CN202211599131.7A CN202211599131A CN115862923A CN 115862923 A CN115862923 A CN 115862923A CN 202211599131 A CN202211599131 A CN 202211599131A CN 115862923 A CN115862923 A CN 115862923A
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Abstract
The application provides a powder, conductive paste and a magnetic device. The silver powder particle surface is coated with a layer of compact oxide film with non-conductive characteristic and the thickness of 5 nm-50 nm; when the conductive paste is applied to preparation of conductive paste of a magnetic device, silver powder particles and pure silver powder are mixed, and the dense oxide film is arranged between the silver powder particles and the pure silver powder, so that the non-conductive film with smaller thickness can ensure that the silver powder particles and the pure silver powder are electrically conducted and can generate certain resistance value based on the tunnel effect, and therefore, the resistance of a finally formed inner electrode can be adjusted, and the RDC of a product can be adjusted and controlled; in addition, the compact oxide film can isolate the direct contact between silver particles and NiZnCu ferrite in the sintering process, and can reduce Cu separated out from the interface of the inner electrode and the NiZnCu ferrite, thereby relieving the internal stress of the product and being beneficial to improving the impedance and strength of the product.
Description
Technical Field
The application relates to the technical field of materials, in particular to powder, conductive paste and a magnetic device.
Background
At present, magnetic devices such as chip inductors and the like mainly comprise a coil formed by an inner electrode, niZnCu ferrite and an outer electrode. The inner electrode and the ferrite need to be co-fired into a whole. In order to prevent co-firing cracking, a certain proportion of glass powder is usually added into the conductive paste for manufacturing the inner electrode to adjust the shrinkage matching of the silver paste and the ferrite so that the two are combined more tightly. However, this approach is prone to the following problems: 1. the conductivity of the internal electrode is lowered, deteriorating RDC (direct current resistance); 2. the internal electrode and the ferrite are combined more tightly through the inorganic binder, so that the internal stress is overlarge, the ferrite is a stress sensitive material, the inductance and the impedance are reduced due to the overlarge internal stress, and meanwhile, the bending strength of a product is unqualified; 3. the Cu precipitation of the magnet material cannot be improved or even accelerated, which can cause the actual components of the ferrite to deviate from the design so as to directly deteriorate the electromagnetic performance of the product, and moreover, after the Cu precipitation, a denser alloy is generated between the interface of the ferrite and the internal electrode and Ag ions, so that the internal stress is greatly increased.
Currently, manufacturers in the industry provide a method for reducing the co-firing internal stress of the inner electrode and the ferrite, i.e., cu precipitated at the interface between the ferrite and the inner electrode is removed by soaking an acidic complexing agent for a long time, so as to relatively separate the inner electrode and the ferrite. Although this method can effectively improve Cu deposition and improve product resistance, the following problems exist in practical operation: 1. the production period of the product can be prolonged by soaking the complexing agent solution for a long time and then drying; 2. the porosity of the magnet tends to be excessively increased after soaking, which tends to result in a decrease in strength of the product.
Therefore, in the prior art, cu precipitated from the interface of the inner electrode and the ferrite is still difficult to reduce while the RDC of a product is regulated and controlled, and the internal stress is relieved, so that the impedance and the strength are improved.
Disclosure of Invention
In view of this, the application provides a powder, a conductive paste and a magnetic device, which can not only regulate and control the product RDC, but also reduce Cu precipitated from the interface of the inner electrode and the ferrite and relieve the internal stress, thereby improving the impedance and the strength.
The powder material comprises silver powder particles and a compact oxide film coated on the surfaces of the silver powder particles, wherein the compact oxide film has a non-conductive characteristic and is 5 nm-50 nm thick.
Alternatively, the material of the dense oxide film comprises Al 2 O 3 、SiO 2 、TiO 2 、ZrO 2 、ZnO、SnO 2 At least one of (1).
Optionally, the dense oxide film is coated on the surface of the silver powder particles by an atomic deposition process.
Optionally, the atomic deposition process satisfies at least one of the following characteristics:
the coating source comprises trimethylaluminum, diisopropylaminosilane and TiCl 4 、AlCl 3 、SnCl 4 、Zr(NO 3 ) 4 、Zn(ET) 2 At least one of;
the reaction temperature is between 230 and 280 ℃;
the cleaning gas is inert gas;
the oxygen source comprises O 2 、O 3 Or N 2 At least one of O.
The conductive paste provided by the application comprises the powder material, the pure silver powder and an organic carrier, wherein the organic carrier comprises a solvent and an additive.
Optionally, the pure silver powder has a particle size of 0.5-1.5 μm and a specific surface area of 0.4-0.7 m 2 (ii) a tap density of greater than 4g/ml.
Optionally, the total mass ratio of the pure silver powder to the powder is 75-95%, and the mass ratio of the organic carrier is 5-25%.
Optionally, the additives include resins, thixotropic agents, plasticizers, leveling agents, and defoamers.
Optionally, in the organic vehicle, the mass ratio of the solvent is 30% to 70%, the mass ratio of the resin is 10% to 30%, the mass ratio of the thixotropic agent is 0.5% to 5%, the mass ratio of the plasticizer is 2% to 10%, the mass ratio of the leveling agent is 0.5% to 5%, and the mass ratio of the defoaming agent is 0.1% to 2%.
Optionally, the solvent comprises at least one of ethyl acetate, tributyl citrate, butyl carbitol acetate, ethylene glycol ethyl ether acetate, and butyl carbitol.
Optionally, the resin comprises at least one of ethyl cellulose, methyl cellulose, silicone resin.
Optionally, the thixotropic agent comprises at least one of hydrogenated nettle oil, titanate coupling agent, fumed silica.
Optionally, the plasticizer comprises at least one of dibutyl phthalate, dioctyl phthalate.
Optionally, the leveling agent comprises at least one of polymethylphenylsiloxane, lecithin and acrylate copolymer.
Optionally, the defoamer comprises a non-silicon based defoamer.
The application provides a magnetic device, including ferrite with set up in the internal electrode of ferrite, the internal electrode adopts the electrically conductive thick liquids as above-mentioned arbitrary one to make.
As described above, the dense oxide film is coated on the surface of the silver powder particles, the dense oxide film has a non-conductive characteristic and has a thickness of 5 nm-50 nm, when the powder is applied to conductive paste for preparing a magnetic device, the silver powder particles and the pure silver powder are mixed, and due to the arrangement of the dense oxide film, the non-conductive film with a smaller thickness can enable the silver powder particles and the pure silver powder to be electrically conducted and generate a certain resistance value based on a tunnel effect, so that the resistance of a finally formed inner electrode can be adjusted, and the RDC of a product can be adjusted; moreover, the compact oxide film can isolate the direct contact between silver particles and NiZnCu ferrite in the sintering process, so that Cu separated out from the interface of the inner electrode and the NiZnCu ferrite can be reduced, the internal stress of the product is relieved, and the impedance and the strength of the product are improved.
Drawings
FIG. 1 is a schematic illustration of particles of a powder material provided in an embodiment of the present application;
FIG. 2 is a schematic flow chart of an ALD process provided in an embodiment of the present application;
FIG. 3 is a schematic diagram of a process for preparing an organic vehicle according to an embodiment of the present disclosure;
fig. 4 is a schematic flow chart of a process for preparing conductive paste according to an embodiment of the present disclosure;
FIG. 5 is a schematic view of electron probe microanalysis of control group 1;
FIG. 6 is a schematic diagram of a microscopic analysis of an electron probe provided in example 6 of the present application.
Detailed Description
In order to solve the above problems in the prior art, the present application provides a powder, a conductive paste, and a magnetic device. The three protection subjects are based on the same conception, the principles for solving the problems are basically the same or similar, the implementation modes of the protection subjects can be referred to each other, and repeated parts are not described again.
In order to make the objects, technical solutions and advantages of the present application more apparent, the technical solutions of the present application will be described below with reference to specific embodiments and accompanying drawings. It should be apparent that the embodiments described below are only a part of the embodiments of the present application, and not all embodiments. In the following embodiments and technical features thereof, all of which are described below may be combined with each other without conflict, and also belong to the technical solutions of the present application.
In the description of the embodiments of the present application, the terms "center", "longitudinal", "lateral", "length", "width", "thickness", "upper", "lower", "front", "rear", "left", "right", "vertical", "horizontal", "top", "bottom", "inner", "outer", "clockwise", "counterclockwise", etc. indicate orientations or positional relationships based on the orientations or positional relationships shown in the drawings, and are only used for convenience of describing technical solutions of the respective embodiments, but do not indicate or imply that the devices or elements must have specific orientations, be constructed and operated in specific orientations, and are not to be construed as limiting the present application.
As shown in FIG. 1, the examples of the present application provide a schematic illustration of the particles of a powder material. The powder (particle) 1 comprises silver particles 11 and a dense oxide film 12 coated on the surfaces of the silver particles 11, wherein the dense oxide film 12 can be made of an insulating material and has a non-conductive characteristic, and the thickness of the dense oxide film 12 is between 5nm and 50nm, so that the thickness of the dense oxide film is smaller.
When the powder material 1 is applied to the preparation of conductive paste of a magnetic device, for example, the silver powder particles 11 and pure silver powder can be mixed in an organic carrier, and the dense oxide film 12 is arranged between the silver powder particles and the pure silver powder, so that the non-conductive film 12 with smaller thickness can lead the silver powder particles 11 and the pure silver powder to be electrically conducted and generate certain resistance value based on the tunnel effect, and the resistance of the finally formed inner electrode can be adjusted, thereby regulating and controlling the RDC of a product; in addition, the silver powder particles 11 can be isolated from being directly contacted with the NiZnCu ferrite in the sintering process through the compact oxide film 12, so that Cu separated out from the interface of the inner electrode and the NiZnCu ferrite can be reduced, the internal stress of the product is relieved, and the impedance and the strength of the product are improved.
It should be noted that, in the product obtained after sintering, the dense oxide film 12 becomes molten and flows during sintering, and finally at least one of the following conditions occurs in the product obtained after sintering: 1. the NiZnCu ferrite is arranged on the interface of the inner electrode and the NiZnCu ferrite; 2. still remain between the silver powder particles 11 and the pure silver powder; 3. and a part is absorbed by the NiZnCu ferrite.
The manner of coating the dense oxide film 12 may be determined according to the material compatibility.
For example, materials of dense oxide thin film 12 include, but are not limited to, al 2 O 3 、SiO 2 、TiO 2 、ZrO 2 、ZnO、SnO 2 At least one of (1). The embodiment of the present application is preferable to ZnO because ZnO belongs to one of the manufacturing materials of the NiZnCu ferrite, and the ZnO can be absorbed by the NiZnCu ferrite without rapidly deteriorating the permeability of the product in the subsequent sintering process for manufacturing the magnetic device.
For the dense oxide thin film 12 of the material, the atomic deposition (ALD) process is preferably adopted to coat the surface of the silver powder particles 11 with the dense oxide thin film 12, the thickness of the dense oxide thin film 12 obtained by the ALD process is more uniform, the film formation on the surface of the silver powder particles 11 is more uniform, and the thickness can be controlled through the cycle number, i.e., the thickness of the dense oxide thin film 12 is easy to control and the thickness precision is better.
The detailed implementation stages of an ALD process can be seen from the prior art. In the embodiment of the present application, the parameters in each implementation stage are adaptively set, so that the dense oxide thin film 12 with good compactness, good coating uniformity, and good thickness uniformity can be obtained. See the following:
the silver powder particles coated with the dense oxide film are mixed with pure silver powder (for example, the pure silver powder not coated with the dense oxide film can be traditional pure silver powder or pure silver powder adopting the characteristic parameters described below in the application), and the obtained mixed powder is called silver powder. Referring to fig. 2, in order to prepare the silver powder particles coated with the dense oxide film, the provided pure silver powder is first subjected to a pretreatment stage, for example, baking is continuously performed for 2 to 6 hours at a temperature of 90 to 120 ℃; then proceeding ALD cycle, the reaction temperature can be between 230-280 deg.C, first feeding coating source, including but not limited to trimethyl aluminum, diisopropyl amino silane, tiCl 4 、AlCl 3 、SnCl 4 、Zr(NO 3 ) 4 、Zn(ET) 2 At least one of; followed by the introduction of a purge gas, such as an inert gas, preferably nitrogen; then introducing a source of oxygen, the source of oxygen comprising O 2 、O 3 Or N 2 At least one of O; and finally introducing cleaning gas to obtain the dried powder.
Of course, the embodiment of the present application may also adopt a process such as Physical Vacuum Deposition (PVD), chemical Vacuum Deposition (CVD), etc. to obtain the dense oxide thin film 12 with the aforementioned thickness.
The embodiment of the application also provides a conductive paste, which comprises the powder prepared as described above, pure silver powder and an organic vehicle, wherein the organic vehicle comprises a solvent and an additive.
The characteristic parameters of the pure silver powder and the silver powder particles can be completely the same or different. For example, in a practical scenario, grains of pure silver powderThe diameter can be between 0.5 and 1.5 mu m, and the specific surface area can be between 0.4 and 0.7m 2 The tap density may be greater than 4g/ml.
Solvents include, but are not limited to, at least one of ethyl acetate, tributyl citrate, butyl carbitol acetate, ethylene glycol ethyl ether acetate, and butyl carbitol.
Additives include, but are not limited to, resins, thixotropic agents, plasticizers, leveling agents, and defoamers. The function of these components in the conductive paste can be found in the prior art and will not be described herein.
The resin includes but is not limited to at least one of ethyl cellulose, methyl cellulose, silicone resin.
The thixotropic agent includes, but is not limited to, at least one of hydrogenated nettle oil, titanate coupling agent, fumed silica.
Plasticizers include, but are not limited to, at least one of dibutyl phthalate, dioctyl phthalate.
The leveling agent includes, but is not limited to, at least one of polymethylphenylsiloxane, lecithin, and acrylate copolymer.
Defoamers include, but are not limited to, non-silicon based defoamers.
Referring to fig. 3, the process of preparing the organic vehicle in the examples of the present application is exemplified as follows:
firstly, mixing and stirring a solvent and resin uniformly, for example, mechanically stirring and dissolving the solvent and the resin uniformly in a water bath environment at 50-120 ℃, and cooling to room temperature; then, mixing the thixotropic agent, the plasticizer, the leveling agent and the defoaming agent with the solvent and the resin which are uniformly stirred, and uniformly stirring; thereby obtaining the organic vehicle.
The proportions of the above components in the process of preparing the organic vehicle may be determined according to the actual desired adaptability. For example, the mass ratio of the solvent is 30 to 70%, the mass ratio of the resin is 10 to 30%, the mass ratio of the thixotropic agent is 0.5 to 5%, the mass ratio of the plasticizer is 2 to 10%, the mass ratio of the leveling agent is 0.5 to 5%, and the mass ratio of the defoaming agent is 0.1 to 2%.
Similarly, the proportion of the pure silver powder to the powder is also the same. For example, as shown in fig. 4, the pure silver powder and the powder are mixed according to a mixing ratio of 75-95% by mass and 5-25% by mass of the organic carrier, and the mixture is added into a homogenizer for corresponding treatment, and then is subjected to three-roll grinding for uniform and fine particle treatment, and then a series of treatments such as vacuum defoaming and the like, so as to obtain the required conductive paste.
Based on the proportion of the components, the RDC of the finally prepared magnetic device can be well regulated and controlled; the Cu separated out from the interface of the inner electrode and the NiZnCu ferrite can be well reduced, and the method has a good effect on relieving the internal stress of the product so as to improve the impedance and strength of the product.
The embodiment of the application also provides a magnetic device. The magnetic device comprises ferrite and internal electrodes arranged in the ferrite, wherein the internal electrodes are made of the conductive paste according to any one of the embodiments.
It should be understood that the magnetic device is a complete device, such as an inductor, with known structural designs for corresponding magnetic devices, including but not limited to structural elements that do not create technical inconsistencies with the inventive principles of the present application. For example, also an outer electrode. The function and position of these structural elements can be found in the prior art. Only the portions of the ferrite and the inner electrode are described, and the description of the other components is omitted.
The present application is further illustrated by the following more specific examples.
The components and the proportion ratio of the organic carrier are shown in the following table 1:
TABLE 1
The electrical standard of the magnetic device product is as follows: z =470 ± 25% Ω; RDC (Max) =1300m Ω; and (4) randomly testing 50 bending resistances of 2mm, and determining that the product is qualified if no appearance crack is generated after all tests.
Criterion for Cu deposition: grinding a magnetic device product to expose an inner electrode structure of the magnetic device product, and then carrying out ion grinding treatment; then selecting a region containing the inner electrode and NiZnCu ferrite, carrying out an EPMA (electronic probe) test, and representing the distribution of Cu and Ag elements; if the Cu element exhibits aggregation at the interface between the internal electrode and the ferrite, interfacial Cu precipitation is considered to be present.
In light of the foregoing material components and proportioning ratios, the following provides 3 control groups of the prior art, and 7 examples prepared based on the technology of the present application, and the specific parameters and test results are shown in the following tables 2 and 3:
TABLE 2
TABLE 3
As can be seen from tables 2 and 3 above, there is almost no or very little Cu precipitation at the interface between the internal electrode and the NiZnCu ferrite of the magnetic device of the present application; in addition, please refer to fig. 5 and fig. 6, wherein fig. 5 is a schematic diagram of an electron probe microanalysis of the control group 1, and fig. 6 is a schematic diagram of an electron probe microanalysis provided in example 6 of the present application; the electron probe microscopic analysis schematic diagram is mainly used for describing element distribution, and can also visually display that almost no Cu is precipitated on the interface between the internal electrode of the magnetic device and the NiZnCu ferrite. Therefore, the internal stress of the magnetic device product is reduced, the impedance is greatly improved compared with that of a comparison group, for example, the impedance can be improved by 25% through embodiment 6 of the magnetic device compared with that of the comparison group, and the bending strength is also obviously improved. Compared with a control group, the product has no holes or gaps inside, no subsequent risk and no increase of production cost. In addition, the RDC of the magnetic devices prepared using the silver powders and silver pastes disclosed herein are within the specification, as compared to the control (i.e., the internal electrode made using conventional silver pastes without the silver powder described herein).
It should be understood that the above-mentioned embodiments are only some examples of the present application, and not intended to limit the scope of the present application, and all structural equivalents made by those skilled in the art using the contents of the present specification and the accompanying drawings are also included in the scope of the present application.
Although the terms "first, second, etc. are used herein to describe various information, such information should not be limited to these terms. These terms are only used to distinguish one type of information from another. In addition, the singular forms "a", "an" and "the" are intended to include the plural forms as well. The terms "or" and/or "are to be construed as inclusive or meaning any one or any combination. An exception to this definition will occur only when a combination of elements, functions, steps or operations are inherently mutually exclusive in some way.
Claims (10)
1. The powder is characterized by comprising silver powder particles and a dense oxide film coated on the surfaces of the silver powder particles, wherein the dense oxide film has a non-conductive characteristic and is 5 nm-50 nm thick.
2. The powder batch of claim 1, wherein the material of the dense oxide film comprises Al 2 O 3 、SiO 2 、TiO 2 、ZrO 2 、ZnO、SnO 2 At least one of (1).
3. The powder lot according to claim 1 or 2, wherein the dense oxide film is coated on the surface of the silver powder particles by an atomic deposition process.
4. The powder batch of claim 3, wherein the atomic deposition process satisfies at least one of the following characteristics:
the coating source comprises trimethylaluminum, diisopropylaminosilane and TiCl 4 、AlCl 3 、SnCl 4 、Zr(NO 3 ) 4 、Zn(ET) 2 At least one of;
the reaction temperature is between 230 and 280 ℃;
the cleaning gas is inert gas;
the oxygen source comprises O 2 、O 3 Or N 2 At least one of O.
5. An electroconductive paste comprising the powder material according to any one of claims 1 to 4, a pure silver powder, and an organic vehicle, wherein the organic vehicle comprises a solvent and an additive.
6. The conductive paste according to claim 5, wherein the pure silver powder has a particle size of 0.5 to 1.5 μm and a specific surface area of 0.4 to 0.7m 2 (ii) a tap density of greater than 4g/ml.
7. The conductive paste according to claim 5 or 6, wherein the total mass ratio of the pure silver powder and the powder is 75% to 95%, and the mass ratio of the organic vehicle is 5% to 25%.
8. The conductive paste as claimed in claim 5, wherein the additives include a resin, a thixotropic agent, a plasticizer, a leveling agent, and an antifoaming agent; in the organic carrier, the mass ratio of the solvent is 30-70%, the mass ratio of the resin is 10-30%, the mass ratio of the thixotropic agent is 0.5-5%, the mass ratio of the plasticizer is 2-10%, the mass ratio of the leveling agent is 0.5-5%, and the mass ratio of the defoaming agent is 0.1-2%.
9. The conductive paste according to claim 8,
the solvent comprises at least one of ethyl acetate, tributyl citrate, butyl carbitol acetate, ethylene glycol ethyl ether acetate and butyl carbitol;
the resin comprises at least one of ethyl cellulose, methyl cellulose and organic silicon resin;
the thixotropic agent comprises at least one of hydrogenated nettle oil, titanate coupling agent and fumed silica;
the plasticizer comprises at least one of dibutyl phthalate and dioctyl phthalate;
the leveling agent comprises at least one of polymethylphenylsiloxane, lecithin and acrylate copolymer;
the defoaming agent includes a non-silicon type defoaming agent.
10. A magnetic device comprising a ferrite and internal electrodes provided in the ferrite, the internal electrodes being made of the conductive paste according to any one of claims 5 to 9.
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| Application Number | Priority Date | Filing Date | Title |
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| CN202211599131.7A CN115862923A (en) | 2022-12-12 | 2022-12-12 | Powder, conductive paste and magnetic device |
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| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN202211599131.7A CN115862923A (en) | 2022-12-12 | 2022-12-12 | Powder, conductive paste and magnetic device |
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| CN115862923A true CN115862923A (en) | 2023-03-28 |
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| CN114360767A (en) * | 2021-12-31 | 2022-04-15 | 广东南海启明光大科技有限公司 | Solar cell positive electrode silver paste with excellent printing performance and preparation method thereof |
| CN115359947A (en) * | 2022-09-13 | 2022-11-18 | 浙江旭达电子有限公司 | Preparation method of inner electrode silver paste for chip ZnO piezoresistor |
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| CN1369883A (en) * | 2001-02-05 | 2002-09-18 | 日本碍子株式会社 | Electronic assembly and mfg. method thereof |
| JP2006108399A (en) * | 2004-10-06 | 2006-04-20 | Kyoto Elex Kk | Conductive paste for forming conductive section for ferrite multilayer circuit board and ferrite multilayer circuit board using conductive paste |
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