CN103824672B - Compound soft magnetic material thin film based on iron-silicon-aluminum soft magnet material and preparation method thereof - Google Patents
Compound soft magnetic material thin film based on iron-silicon-aluminum soft magnet material and preparation method thereof Download PDFInfo
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Abstract
The invention provides a kind of compound soft magnetic material thin film based on iron-silicon-aluminum soft magnet material and preparation method thereof described thin film and include silicon dioxide hardening network structure and the manganese-zinc ferrite soft magnetic powder particles of the dehydration formation of iron-silicon-aluminum soft magnetic powder granule, waterglass, wherein iron-silicon-aluminum soft magnetic powder granule is by manganese-zinc ferrite soft magnetic powder particles insulating wrapped, the silicon dioxide hardening network structure formed by the dehydration of described waterglass between granule is bondd, and forms mechanical strength.This film preparation includes the pretreatment to film substrate iron-silicon-aluminum soft magnetic powder, the insulating wrapped to film substrate manganese-zinc ferrite soft magnetic powder, the low-temperature setting molding with water glass of binder.Present invention manganese-zinc ferrite is as insulating compound, it is possible to the high-gradient magnetism energy of regulation compound soft magnetic material thin film, improves upper operational frequency limit；There is good cohesive force.Energy-saving of the present invention, greenization, processing compatibility is good, can obtain the compound soft magnetic material thin film that comprehensive magnetic can be excellent.
Description
Technical field
The present invention relates to a kind of compound soft magnetic material thin film, specifically, refer to a kind of soft based on ferrum sial
The compound soft magnetic material thin film of magnetic material and the preparation method of low temperature moulding thereof.
Background technology
Mems device integrated in, need to use magnetic material and thin film to realize energy and signal
Change, transmit and store.The miniaturization of electronic component, high frequency, propose higher to magnetic material and thin film
Standard and requirement.This also means that magnetic material and thin film must have low-loss and good frequency stable
Property, just adapt to the application under high frequency condition.Particularly at high frequency miniature inducer manufacture view, in order to obtain
Enough inductance values, compact inductor uses thin magnetic film.Thin magnetic film conventional machining process have screen printing,
Sputtering etc..Screen printing film-forming process to sinter under 1000 degrees Celsius, this and standard IC manufacturing work
Skill and fine process are incompatible.Sputtering moulding process is the longest, and processing cost is high.Substantial amounts of research work
Concentrate on exploitation and composition integrated level height, magnetic electricity performance is excellent, power capacity is big and standard IC manufacturing work
On the magnetoelectronic devices that skill, fine process are compatible.
Soft magnetic materials application in power electronics and development start from the great development epoch of late nineteenth century industry.?
In the manufacture of motor and transformator, magnetic core just employs substantial amounts of soft-magnetic powder.The development of communication technology,
Light current device aspect, needs to use the material of high magnetic permeability.After the technology such as electronic computer rapidly emerge and develop,
Some soft magnetic materials with higher performance are also a dark horse.
Summary of the invention
In order to reduce processing cost, strengthening processing compatibility and improve thin magnetic film performance, the present invention proposes one
Plant compound soft magnetic material thin film based on iron-silicon-aluminum soft magnet material and low temperature moulding preparation method thereof.Prepared by the present invention
Method is compatible with fine process, the low cost of preparation, and the compound soft magnetic material thin film magnetic of preparation can be excellent,
Possess the potentiality of mass production and industrial applications.
For realizing above-mentioned purpose, the technical solution used in the present invention:
According to an aspect of the present invention, it is provided that a kind of compound soft magnetic material thin film based on iron-silicon-aluminum soft magnet material,
Described thin film include iron-silicon-aluminum soft magnetic powder granule, waterglass dehydration formed silicon dioxide hardening network structure with
And manganese-zinc ferrite soft magnetic powder particles, wherein iron-silicon-aluminum soft magnetic powder granule is by manganese-zinc ferrite soft magnetic powder
Grain insulating wrapped, the silicon dioxide hardening network structure formed by the dehydration of described waterglass between granule is bondd,
Form mechanical strength.
Preferably, described iron-silicon-aluminum soft magnetic powder granule has two kinds of granularities, the iron-silicon-aluminum soft magnet powder that wherein granularity is big
End void among particles is mainly by the little iron-silicon-aluminum soft magnetic powder granule of granularity and manganese-zinc ferrite soft magnetic powder
Grain is filled.
Preferably, described manganese-zinc ferrite soft magnetic powder particles granularity is 1～5 micron.
According to a further aspect in the invention, it is provided that a kind of compound soft magnetic material thin film based on iron-silicon-aluminum soft magnet material
Preparation method, the method selects the iron-silicon-aluminum soft magnetic powder of high magnetic permeability as the base of compound soft magnetic material thin film
Material, with the manganese-zinc ferrite soft magnetic powder of high resistivity as the insulating compound of cladding ferrum sial granule, adds water glass
Three, as binding agent, according to the magnetic property requirements of required thin film, is carried out proportioning according to quality, passes through ball by glass
Grind abundant batch mixing, in clean substrate of glass make film coating, after in baking oven oven drying at low temperature to be solidified into
Type, thus it is prepared for a kind of compound soft magnetic material thin film based on iron-silicon-aluminum soft magnet material.
Described preparation method, comprises the following steps:
The first step: iron-silicon-aluminum soft magnetic powder is carried out the pretreatment of ball milling refinement, abundant ball milling, sieves and obtain two
Plant or the iron-silicon-aluminum soft magnetic powder of two or more different grain size specification.
Second step: manganese-zinc ferrite soft magnetic powder is carried out the pretreatment of ball milling refinement, abundant ball milling, obtains grain
Degree is the manganese-zinc ferrite soft magnetic powder of 1～5 micron.
3rd step: according to the magnetic property requirements of required compound soft magnetic material thin film, by ferrum sial different for granularity
Soft magnetic powder and manganese-zinc ferrite soft magnetic powder and water for industrial use glass carry out proportioning according to the quality set, will be mixed
The abundant batch mixing of compound；According to ball milling frequency, typically mixing time is controlled more than 15 minutes, preferably 15～35
Minute.
4th step: in clean substrate of glass, uniformly coats the batch mixing that the 3rd step obtains, after completing coating
Being positioned in baking oven, programming rate is 5～10 DEG C/min, and under 200～240 degrees Celsius be incubated 2 hours with
On fully solidify, after cool to room temperature with the furnace, thus obtain composite soft-magnetic based on iron-silicon-aluminum soft magnet material
Material film.
In said method of the present invention, iron-silicon-aluminum soft magnetic powder carrying out ball milling thinning preprocess, ferrum sial granule has
There is the granularity that two or more are different；Ball milling is carried out thin as the Mn-Zn soft magnetic ferrite powder of insulating compound
Changing pretreatment, granularity is 1～5 micron.
The present invention first passes through the pretreatment that iron-silicon-aluminum soft magnetic powder and ferroxcube magnetic powder carry out ball milling refinement,
Obtain specific varigrained soft magnetic powder.With the iron-silicon-aluminum soft magnetic powder of high magnetic permeability as composite soft-magnetic material
The base material of material thin film, with the manganese-zinc ferrite soft magnetic powder insulating wrapped ferrum sial powder particle of high resistivity.?
In the preparation of compound soft magnetic material thin film, do not select the magnetic powder of Monosized powder, select that there is varigrained magnetic powder
Proportioning.According to the magnetic property requirements of required compound soft magnetic material thin film, add waterglass as binding agent, according to
Extra fine quality carries out proportioning, by the abundant batch mixing of ball mill, makes film coating in clean substrate of glass,
After in baking oven oven drying at low temperature with curing molding, thus be prepared for a kind of based on iron-silicon-aluminum soft magnet material compound soft
Magnetic material film.The technological process of this preparation method is simple, and cost is relatively low, is expected to be used for mass and industrialization
Produce.
Compared with prior art, the method have the advantages that the manganese-zinc ferrite using high resistivity is soft
Magnetic powder is as insulating compound, it is possible to the high-gradient magnetism energy of regulation compound soft magnetic material thin film, improves in operating frequency
Limit, expands range；Binding agent is made with waterglass, can be with low-temperature setting molding.The preparation method of the present invention
Energy-saving, greenization, processing compatibility is good, compatible with fine process and integrated circuit fabrication process.
Accompanying drawing explanation
By the detailed description non-limiting example made with reference to the following drawings of reading, its of the present invention
Its feature, purpose and advantage will become more apparent upon:
Fig. 1 is compound soft magnetic material film profile structure chart prepared by one embodiment of the invention.
In figure: the little granule of iron-silicon-aluminum soft magnetic powder 1, iron-silicon-aluminum soft magnetic powder bulky grain 2, manganese-zinc ferrite are soft
Magnetic powder granule 3, silicon dioxide hardening network structure 4.
Detailed description of the invention
Elaborating embodiments of the invention below, the present embodiment is under premised on technical solution of the present invention
Implement, give detailed embodiment and concrete operating process, but protection scope of the present invention does not limits
In following embodiment.
As it is shown in figure 1, the present embodiment includes: the little granule of iron-silicon-aluminum soft magnetic powder 1, iron-silicon-aluminum soft magnetic powder are big
Granule 2, manganese-zinc ferrite soft magnetic powder particles 3, silicon dioxide hardening network structure 4.Use manganese-zinc ferrite
Soft magnetic powder particles 3 is coated on iron-silicon-aluminum soft magnetic powder granule 1,2 surface as insulating compound, logical between granule
Cross silicon dioxide hardening network structure 4 to bond.Space between iron-silicon-aluminum soft magnetic powder bulky grain 2 is mainly by ferrum
The little granule of silicon-aluminum soft magnet powder 1 and manganese-zinc ferrite soft magnetic powder particles 3 are filled.
In the present embodiment, the mesh number of the little granule of described iron-silicon-aluminum soft magnetic powder 1 is 600～800 mesh, and ferrum sial is soft
The mesh number of magnetic powder bulky grain 2 is 300～400 mesh, and the granularity of manganese-zinc ferrite soft magnetic powder particles 3 is 1～5
Micron.
Above-mentioned iron-silicon-aluminum soft magnetic powder granule is effectively coated with by manganese-zinc ferrite soft magnetic powder particles, magnetic powder particle
It is distributed in silicon dioxide hardening network structure, has obtained compound soft magnetic material based on iron-silicon-aluminum soft magnet material thin
Film.Specifically can be prepared by the following preparation method:
1, select 15g iron-silicon-aluminum soft magnetic powder, put into ball grinder, and put into 8 big steel balls, 6 little steel
Ball, uses omnidirectional planetary ball mill ball milling, and frequency configuration is 40Hz, and Ball-milling Time 4h～5h sieves
Iron-silicon-aluminum soft magnetic powder to 400 mesh.
2, select 10g iron-silicon-aluminum soft magnetic powder, put into ball grinder, and put into 15 big steel balls, 8 little steel
Ball, uses omnidirectional planetary ball mill ball milling, and frequency configuration is 50Hz, and Ball-milling Time 8h～9h sieves
Iron-silicon-aluminum soft magnetic powder to 800 mesh.
3, select 5g manganese-zinc ferrite soft magnetic powder, put into ball grinder, and put into 15 big steel balls, 8
Small ball, uses omnidirectional planetary ball mill ball milling, and frequency configuration is 50Hz, Ball-milling Time 2h～3h, mistake
Sieve obtains the manganese-zinc ferrite soft magnetic powder that granularity is 1～5 micron.
4, the waterglass selecting modulus to be 3.5 is as binding agent, draws 9～11g with test tube.
5, by the 400 mesh iron-silicon-aluminum soft magnetic powders of 15g, the iron-silicon-aluminum soft magnetic powder of 800 mesh of 10g, 5g
Granularity 1～the manganese-zinc ferrite soft magnetic powder of 5 microns and 9～11g waterglass be mixed into ball grinder, and put into 8
Individual big steel ball, 6 small balls, frequency configuration is 40Hz, and abundant batch mixing took out after 30 minutes.
6, in clean substrate of glass, the material of mixing is evenly applied in substrate of glass, controls thickness
The most uniformly, the thickness of film is 1～2 millimeter.
7, by coated thin film as in baking oven, programming rate is 5 DEG C/min, and at 200 degrees celsius
Be incubated 2 hours fully to solidify, after cool to room temperature with the furnace.
8, utilize mechanical means to carry out grinding so as to get film thickness uniformly, smooth surface, thus obtain
Compound soft magnetic material thin film based on iron-silicon-aluminum soft magnet material.
The present embodiment is simple in technological process, on the basis of cost is the highest, use manganese-zinc ferrite cook insulating compound,
Waterglass makees binding agent, is prepared for composite soft-magnetic material based on iron-silicon-aluminum soft magnet material by the method for low temperature moulding
Material thin film, had both improved the high-gradient magnetism energy of compound soft magnetic material thin film, in turn ensure that good processing compatibility.
It is pointed out that above-described embodiment is one embodiment of the invention, it is also possible to change soft magnetic powder
The granularity of grain and proportioning, all can realize the purpose of the present invention.
The low temperature moulding preparation method of the compound soft magnetic material thin film of this disclosure of the invention, processing compatibility is good, with micro-
Fining-off technique and integrated circuit fabrication process are compatible.With manganese-zinc ferrite as insulating compound, it is possible to regulation is compound
The high-gradient magnetism energy of soft magnetic material thin film, improves upper operational frequency limit.Waterglass has good aqueous solubility and gluing
Performance, low cost, is a kind of environmentally friendly inorganic binder, the silicon dioxide hardening network knot that dehydration is formed
Structure has good cohesive force.The preparation method energy-saving of the present invention, greenization, processing compatibility is good, permissible
Obtain the compound soft magnetic material thin film that comprehensive magnetic can be excellent, be expected to realize commercial application.
Above examples describe advantages of the present invention and processing method, skilled person will appreciate that of the industry,
Without departing from the spirit and scope, the present invention also has various improvement and optimization, these improve and
Optimizing both falls within scope of the claimed invention, and claimed scope is by appending claims
And equivalent defines.
Claims (5)
1. a compound soft magnetic material thin film based on iron-silicon-aluminum soft magnet material, it is characterised in that include that ferrum sial is soft
The silicon dioxide hardening network structure of magnetic powder granule, waterglass dehydration formation and manganese-zinc ferrite soft magnetic powder
Granule, wherein iron-silicon-aluminum soft magnetic powder granule is by manganese-zinc ferrite soft magnetic powder particles insulating wrapped, between granule
The silicon dioxide hardening network structure formed by the dehydration of described waterglass is bondd, and forms mechanical strength；
Described iron-silicon-aluminum soft magnetic powder granule has two kinds of granularities, iron-silicon-aluminum soft magnetic powder granule all quilts of two kinds of granularities
Manganese-zinc ferrite soft magnetic powder particles insulating wrapped, the iron-silicon-aluminum soft magnetic powder void among particles that wherein granularity is big
The iron-silicon-aluminum soft magnetic powder granule little by granularity and manganese-zinc ferrite soft magnetic powder particles are filled；Described ferrum sial is soft
Magnetic powder short grained mesh number is 600～800 mesh, and iron-silicon-aluminum soft magnetic powder oarse-grained mesh number is 300～400
Mesh, the granularity of manganese-zinc ferrite soft magnetic powder particles is 1～5 micron.
2. the system of a compound soft magnetic material thin film based on iron-silicon-aluminum soft magnet material according to claim 1
Preparation Method, it is characterised in that comprise the following steps:
The first step: iron-silicon-aluminum soft magnetic powder is carried out the pretreatment of ball milling refinement, abundant ball milling, sieves and obtain two
Plant or the iron-silicon-aluminum soft magnetic powder of two or more different grain size specification；
Second step: manganese-zinc ferrite soft magnetic powder is carried out the pretreatment of ball milling refinement, abundant ball milling, obtains grain
Degree is the manganese-zinc ferrite soft magnetic powder of 1～5 micron；
3rd step: according to the magnetic property requirements of required composite soft-magnetic thin film, by iron-silicon-aluminum soft magnets different for granularity
Powder and manganese-zinc ferrite soft magnetic powder and water for industrial use glass carry out proportioning, by mixture according to the quality set
Fully batch mixing；
4th step: in clean substrate of glass, uniformly coats the batch mixing that the 3rd step obtains, after completing coating,
Being positioned in baking oven, programming rate is 5～10 DEG C/min, and under 200～240 degrees Celsius be incubated 2 hours with
On fully solidify, after cool to room temperature with the furnace, thus obtain composite soft-magnetic based on iron-silicon-aluminum soft magnet material
Material film.
The preparation side of compound soft magnetic material thin film based on iron-silicon-aluminum soft magnet material the most according to claim 2
Method, is characterized in that: iron-silicon-aluminum soft magnetic powder carries out ball milling thinning preprocess, ferrum sial granule have two kinds or
Two or more different granularities, the wherein grain of the fineness ratio ferrum sial powder particle of manganese-zinc ferrite powder granule
Degree is little, and manganese-zinc ferrite soft magnetic powder particles granularity is 1～5 micron.
The preparation side of compound soft magnetic material thin film based on iron-silicon-aluminum soft magnet material the most according to claim 3
Method, is characterized in that: the Mn-Zn soft magnetic ferrite powder as insulating compound carries out ball milling thinning preprocess, particle
Degree is 1～5 micron, and the network structure formed by the hardening of waterglass low temperature dewatering between granule is bondd.
5. according to the compound soft magnetic material thin film based on iron-silicon-aluminum soft magnet material described in any one of claim 2-4
Preparation method, it is characterized in that: in the 3rd step, mixing time controlled more than 15 minutes.
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| CN106158340B (en) * | 2016-08-10 | 2018-02-27 | 华南理工大学 | A kind of Fe Si Al powder core toroidal magnets and preparation method thereof |
| JP6237853B1 (en) * | 2016-09-30 | 2017-11-29 | Tdk株式会社 | Soft magnetic alloy |
| CN109192432A (en) * | 2018-08-31 | 2019-01-11 | 周晓东 | A kind of preparation method of compound structure type soft magnetic materials |
| CN109688780B (en) * | 2019-01-22 | 2020-05-12 | 西华大学 | Fe-Si-Al electromagnetic wave absorbent and preparation method thereof |
| CN112094114A (en) * | 2020-09-25 | 2020-12-18 | 麦格磁电科技（珠海）有限公司 | Manganese-zinc ferrite composite material and preparation method thereof |
| CN113223845B (en) * | 2021-04-25 | 2022-11-18 | 宁波中科毕普拉斯新材料科技有限公司 | Insulating coating method of soft magnetic alloy powder |
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