CN110428967A - A kind of preparation method and product of ultra-low temperature cold sintered iron base nanocomposite powder core - Google Patents
A kind of preparation method and product of ultra-low temperature cold sintered iron base nanocomposite powder core Download PDFInfo
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- H—ELECTRICITY
- H01—ELECTRIC ELEMENTS
- H01F—MAGNETS; INDUCTANCES; TRANSFORMERS; SELECTION OF MATERIALS FOR THEIR MAGNETIC PROPERTIES
- H01F1/00—Magnets or magnetic bodies characterised by the magnetic materials therefor; Selection of materials for their magnetic properties
- H01F1/01—Magnets or magnetic bodies characterised by the magnetic materials therefor; Selection of materials for their magnetic properties of inorganic materials
- H01F1/03—Magnets or magnetic bodies characterised by the magnetic materials therefor; Selection of materials for their magnetic properties of inorganic materials characterised by their coercivity
- H01F1/12—Magnets or magnetic bodies characterised by the magnetic materials therefor; Selection of materials for their magnetic properties of inorganic materials characterised by their coercivity of soft-magnetic materials
- H01F1/14—Magnets or magnetic bodies characterised by the magnetic materials therefor; Selection of materials for their magnetic properties of inorganic materials characterised by their coercivity of soft-magnetic materials metals or alloys
- H01F1/147—Alloys characterised by their composition
- H01F1/153—Amorphous metallic alloys, e.g. glassy metals
- H01F1/15383—Applying coatings thereon
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- H—ELECTRICITY
- H01—ELECTRIC ELEMENTS
- H01F—MAGNETS; INDUCTANCES; TRANSFORMERS; SELECTION OF MATERIALS FOR THEIR MAGNETIC PROPERTIES
- H01F41/00—Apparatus or processes specially adapted for manufacturing or assembling magnets, inductances or transformers; Apparatus or processes specially adapted for manufacturing materials characterised by their magnetic properties
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- H—ELECTRICITY
- H01—ELECTRIC ELEMENTS
- H01F—MAGNETS; INDUCTANCES; TRANSFORMERS; SELECTION OF MATERIALS FOR THEIR MAGNETIC PROPERTIES
- H01F41/00—Apparatus or processes specially adapted for manufacturing or assembling magnets, inductances or transformers; Apparatus or processes specially adapted for manufacturing materials characterised by their magnetic properties
- H01F41/02—Apparatus or processes specially adapted for manufacturing or assembling magnets, inductances or transformers; Apparatus or processes specially adapted for manufacturing materials characterised by their magnetic properties for manufacturing cores, coils, or magnets
- H01F41/0206—Manufacturing of magnetic cores by mechanical means
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- H—ELECTRICITY
- H01—ELECTRIC ELEMENTS
- H01F—MAGNETS; INDUCTANCES; TRANSFORMERS; SELECTION OF MATERIALS FOR THEIR MAGNETIC PROPERTIES
- H01F41/00—Apparatus or processes specially adapted for manufacturing or assembling magnets, inductances or transformers; Apparatus or processes specially adapted for manufacturing materials characterised by their magnetic properties
- H01F41/02—Apparatus or processes specially adapted for manufacturing or assembling magnets, inductances or transformers; Apparatus or processes specially adapted for manufacturing materials characterised by their magnetic properties for manufacturing cores, coils, or magnets
- H01F41/0206—Manufacturing of magnetic cores by mechanical means
- H01F41/0246—Manufacturing of magnetic circuits by moulding or by pressing powder
Abstract
The invention discloses the preparation methods and product of a kind of ultra-low temperature cold sintered iron base nanocomposite powder core, ferrite presoma is coated on iron based nano crystal magnetic powder surface first, then it is formed by adding the iron based nano crystal magnetic powder that a certain amount of medium coats ferrite presoma convenient for surface, it is sintered to obtain iron based nano crystal composite magnetic powder core idiosome by low temperature cold at low pressures again, used medium is vapored away simultaneously, eventually by annealing destressing, the iron based nano crystal composite magnetic powder core with higher-density and excellent soft magnet performance is obtained.The present invention solves the problems, such as briquetting pressure height and magnetic property dilution effect two simultaneously, and magnetic conductivity is stablized frequency range and improved to ghz band, so as to meet the fields such as electronic information technology to the application demand of higher working frequency, is suitable for promoting the use of in the art.
Description
Technical field
The invention belongs to powder core technical field, relate to prepare iron based nano crystal under low-pressure, sintering temperature and low
The method of composite magnetic powder core and preparation-obtained iron based nano crystal composite magnetic powder core product.
Background technique
Iron based nano crystal powder core mainly passes through the works such as insulating wrapped, cold moudling and annealing by iron(-)base powder
Skill is made, and is a kind of important soft-magnetic composite material, has good answer in fields such as power inductance, transformer and Switching Power Supplies
Use prospect.
The insulating wrapped agent of iron based nano crystal powder core mainly has ZrO2、SiO2、B2O3, phosphate (pass through phosphoric acid or phosphatization
Salt passivation generates) etc. the magnetic phase such as non-magnetic phases and Ni nanoparticle Zn ferrite, Nano-MnZn Ferrite.Relative to non magnetic cladding
The influence to powder core magnetic property dilution effect can be effectively reduced in phase, magnetic surrounding phase.However, such powder core is producing at present
There is still a need for additions organic binder (such as epoxy resin, silicone resin) to carry out proof strength in preparation process, while needing
Apply the pressure of up to 1Gpa or more in cold pressing forming process to promote the initial density of powder core (referring to patent application document
CN109273185A, CN106890999A, CN103559974A, CN102744403A): (1) addition of organic binder anti-mistake
To dilute saturation flux density and Effective permeability again, and its low thermal resistance characteristic limits the annealing temperature of powder core, into
And influence removal and suppress brought residual stress, increase powder core magnetic hystersis loss；(2) pressure crosses conference and causes nanocrystalline magnetic
Insulating wrapped damage layer reduce the resistance of powder core, Jin Erzeng so that nanocrystalline magnetic directly contacts (or part contact)
High frequency and the loss with super band are added；High stress can be brought simultaneously, so that powder core is difficult to remove in annealing process, is deteriorated
Magnetic property.These factors also cause the magnetic conductivity of powder core to stablize frequency range lower than 5MHz, to not be able to satisfy electronic information indirectly
Application demand of the fields such as technology to higher working frequency.
Therefore it reduces briquetting pressure in preparation process, reduce magnetic property dilution effect, while improving iron based nano crystal magnetic powder
The performance of core MHz to ghz band is a technical problem to be solved urgently.
Summary of the invention
The purpose of the present invention is intended to for molding existing during above-mentioned prior art preparation iron based nano crystal powder core
The problems such as pressure is high, magnetic property dilution effect, provides that a kind of ultra-low temperature cold sintered iron base is nanocrystalline to meet powder core and its preparation
Method using the medium for being easy to volatilize to reduce magnetic property dilution effect, and reduces briquetting pressure by low-temperature sintering, thus
Obtain the composite magnetic powder core that soft magnet performance is excellent, consistency is high.
Invention thinking of the invention are as follows: coat ferrite presoma on iron based nano crystal magnetic powder surface first, then pass through
A certain amount of mass transfer media is added convenient for the iron based nano crystal magnetic powder molding of surface cladding ferrite presoma, then in lower pressure
It is sintered down to obtain iron based nano crystal composite magnetic powder core idiosome by low temperature cold, while vaporing away used mass transfer media, finally
By making annealing treatment destressing.By low-temperature sintering, the consistency of nano combined powder core can not only be promoted, can also be avoided
Because of the magnetic property dilution effect caused by using organic binder.
Ultra-low temperature cold sintered iron base nanocomposite powder core provided by the invention, is measured by the percentage by weight, component
Include 96%~99.5% nanocrystalline magnetic and 0.5%~6% nanometer ferrite.Provided iron based nano crystal composite magnetic powder
Raw material used in the preparation method of core is calculated according to each component content in the nanocomposite powder core of required preparation.
Ultra-low temperature cold sintered iron base nanocrystalline magnetic core preparation method provided by the present invention the following steps are included:
(1) ferritic presoma is coated on to the surface of nanocrystalline magnetic, the dosage and Nanoscale Iron oxygen of nanocrystalline magnetic
The dosage of body is respectively 96%~99.5% and is 0.5%~6% by weight percentage；
(2) 10%~30% mass transfer media of the iron based nano crystal powder core weight of required preparation is obtained with step (1)
The nanocrystalline magnetic for being coated with nanometer ferrite presoma be uniformly mixed, then by gained mixture in 200~800MPa,
It is sintered 0.5~3h at 100~300 DEG C and obtains iron based nano crystal composite magnetic powder core idiosome；Or
The resulting nanocrystalline magnetic for being coated with nanometer ferrite presoma of step (1) is made in 450~600 DEG C of pretreatments
Ferrite presoma generates ferrite, then by gained pretreatment product and the iron based nano crystal powder core weight of required preparation
10%~30% medium is uniformly mixed, then gained mixture is sintered to 0.5~3h at 200~800MPa, 100~300 DEG C
Obtain iron based nano crystal composite magnetic powder core idiosome；
(3) gained iron based nano crystal composite magnetic powder core idiosome is made annealing treatment in 400~600 DEG C to get iron-based nanometer is arrived
Brilliant composite magnetic powder core.
In step (1), the nanocrystalline magnetic is by iron-based amorphous nanometer crystalline magnetic powder under vacuum conditions in 300~450 DEG C
0.5~2h of heat treatment is produced.The iron-based amorphous nanometer crystalline magnetic powder can be FeSiBNbCu amorphous magnetic powder, FeSiBPCu amorphous magnetic
Powder, FeSiBP amorphous magnetic powder, FeSiBNbCuMo amorphous magnetic powder, FeSiB amorphous magnetic powder, FeSiBC amorphous magnetic powder, FeSiBCoNi
At least one of amorphous magnetic powder and FeSiBPC amorphous magnetic powder.
In step (1), the nanometer ferrite is Ni nanoparticle Zn ferrite or Nano-MnZn Ferrite.It can be by molten
Nanometer ferrite presoma is coated on nanocrystalline magnetic surface by glue-gel method, hydro-thermal method or coprecipitation.In the present invention, receive
The brilliant magnetic powder surface cladding ferrite presoma of rice can carry out in the following manner: disperse the first inorganic salts, for nanocrystalline magnetic
In two inorganic salts and the solution of molysite mixing, after mixing evenly, the pH value of mixed liquor is adjusted to 9~12, is further continued for stirring evenly,
It stands under 40~80 DEG C of water bath conditions to collosol state later, gained sol product is then dried to gel state.
First inorganic salts are nickel salt or manganese salt, such as nickel/manganese chlorate or nitrate；Second inorganic salts are zinc salt, example
Such as zinc chloride or zinc nitrate；The molysite is iron chloride or ferric nitrate；Metal member in first inorganic salts and the second inorganic salts
The ratio between amount of substance of element is (2~8): (8~2)；The amount of the substance of ferro element and the second inorganic salts and first in the molysite
The ratio of the sum of amount of substance of other metallic elements is 2:1 in inorganic salts.
In step (2), regardless of which kind of implementation, the mass transfer media is mainly used for the mass transport process in low temperature cold sintering
It can be water, ammonium hydroxide, acetic acid or acetic acid etc. to obtain fine and close idiosome.The difference of two kinds of implementations is: realizing first
It is first to be sintered to obtain fine and close iron based nano crystal composite magnetic powder core idiosome by low temperature cold under the conditions of certain pressure in mode,
Then it is handled by post annealed, ferrite presoma is converted to ferrite, and then obtains iron based nano crystal composite magnetic powder core；In
It in second of implementation, first passes through and the nanocrystalline magnetic for being coated with nanometer ferrite presoma is pre-processed, make iron oxygen
Body presoma is converted to ferrite, then the iron based nano crystal for being sintered to obtain densification by low temperature cold under the conditions of certain pressure is compound
Powder core idiosome handles de-stress by post annealed, and then obtains iron based nano crystal composite magnetic powder core.No matter which kind of mode,
Sample formation pressure is down to 200MPa in such a way that low temperature cold is sintered, highdensity nanometer can be prepared at this pressure
Composite magnetic powder core, so as to avoid because of briquetting pressure height caused by powder core insulating coating be easily destroyed, make powder core
Resistance reduces, and then increases high frequency and be difficult to the problem of removing with super band loss and stress.It has been investigated that passing through the first
Implementation, since the annealing temperature needed for reducing the ferritic temperature of generation simultaneously is lower, obtained iron-based nanometer
The soft magnet performance of brilliant composite magnetic powder core is excellent；By second of implementation, the magnetic conductivity cutoff frequency of material can be greatly improved
Rate, to meet the requirement of high band electronic information technology.In the second implementation, to being coated with nanometer ferrite forerunner
The pretreatment of the nanocrystalline magnetic of body can use vacuum heat treatment, can also use normative heat treatment, and pretreatment time is general
For 0.5~2h.
In step (3), iron based nano crystal composite magnetic powder core idiosome is made annealing treatment residual brought by compacting to remove
Residue stress, annealing can use vacuum heat treatment, can also use normative heat treatment, and the annealing time is generally 0.5
~2h.
The iron based nano crystal composite magnetic powder core product prepared by the above method, consistency with higher, higher magnetic
Conductance and extremely low magnetic powder core loss, at the same by magnetic conductivity stablize frequency range improve to ghz band, and its KHz to ghz band all
With excellent soft magnet performance.
Compared with prior art, the invention has the following advantages:
1, the present invention first coats ferrite presoma on iron based nano crystal magnetic powder surface, then by passing through at low pressures
Low-temperature sintering obtains nano combined powder core idiosome, and last annealed processing is prepared that consistency is higher, soft magnet performance is excellent
Iron based nano crystal composite magnetic powder core.
2, the present invention can make to form institute in nano combined powder core idiosome by carrying out low-temperature sintering in forming process
To 200MPa, the powder core insulating coating caused by can be avoided because of briquetting pressure height is easily destroyed, makes for the pressure reduction needed
Powder core resistance reduces, and then increases high frequency and be difficult to the problem of removing with super band loss and stress.
3, the present invention uses the water, ammonium hydroxide, acetic acid or the acetic acid that are easy to volatilize as medium, to avoid because using organic viscous
Tie magnetic property dilution effect caused by agent.
4, iron based nano crystal composite magnetic powder core product prepared by the present invention, consistency with higher and excellent soft magnetism
Can, and magnetic conductivity is stablized frequency range and is improved to ghz band, so as to meet the fields such as electronic information technology to higher working frequency
Application demand, be suitable in the art promote the use of.
Detailed description of the invention
Fig. 1 is the X-ray diffraction test result of iron based nano crystal composite magnetic powder core prepared by the present invention.
Fig. 2 is the scanning electron microscope (SEM) photograph of iron based nano crystal composite magnetic powder core prepared by the present invention.
Fig. 3 is the magnetic conductivity test result of iron based nano crystal composite magnetic powder core prepared by the present invention.
Fig. 4 is iron based nano crystal composite magnetic powder core loss test result prepared by the present invention.
Specific embodiment
Clear, complete description is carried out below with reference to technical solution of the attached drawing to various embodiments of the present invention, it is clear that is retouched
Stating embodiment is only a part of the embodiments of the present invention, instead of all the embodiments.Based on the embodiments of the present invention, originally
Field those of ordinary skill obtained all other embodiment without making creative work, belongs to this hair
Bright protected range.
Examples 1 to 5
The preparation method of ultra-low temperature cold sintered iron base composite magnetic powder core provided by embodiment 1-5 the following steps are included:
(1) FeSiBPCu amorphous and nanocrystalline soft magnetic alloy powder is received in 350 DEG C of heat treatment 1h formation under vacuum conditions
The brilliant magnetic powder of rice.According to the iron based nano crystal composite magnetic powder core constituent content of preparation needed for table 1, chlorination is dispersed by nanocrystalline magnetic
In the solution of nickel, zinc chloride and iron chloride (molar ratio of Ni, Zn, Fe element is 0.5:0.5:2), after mixing evenly, ammonia is utilized
Water adjusts the pH value of mixed liquor to 10, is further continued for stirring 0.5h, 2h is stood under 65 DEG C of water bath conditions later forms mixed liquor
Then gained sol product is dried 4h to gel state by collosol state.
(2) 15% ammonium hydroxide of the iron based nano crystal powder core weight of required preparation is coated with what step (1) obtained
The nanocrystalline magnetic of NiZn ferrite presoma is uniformly mixed, and is then put into mold, applies the pressure of 500MPa, In to mold
Iron based nano crystal composite magnetic powder core idiosome is formed in 150 DEG C of cold sintering 2h under the pressure.
(3) gained iron based nano crystal composite magnetic powder core idiosome is answered in 400 DEG C of annealing 2h to get to iron based nano crystal
Close powder core product.
1 iron based nano crystal composite magnetic powder core component ratio (by weight percentage) of table
| Embodiment 1 | Embodiment 2 | Embodiment 3 | Embodiment 4 | Embodiment 5 | |
| FeSiBPCu | 99.5% | 99.0% | 97.0% | 96.0% | 94.0% |
| Ni nanoparticle Zn ferrite | 0.5% | 1.0% | 3.0% | 4.0% | 6.0% |
Embodiment 6~10
The preparation method of ultra-low temperature cold sintered iron base composite magnetic powder core provided by embodiment 6-10 the following steps are included:
(1) by Fe73.5Si13.5B9Nb3Cu1Amorphous and nanocrystalline soft magnetic alloy powder is heat-treated in 450 DEG C under vacuum conditions
1h forms nanocrystalline magnetic.According to the iron based nano crystal composite magnetic powder core constituent content of preparation needed for table 2, by nanocrystalline magnetic point
(molar ratio of Ni, Zn, Fe element is 0.5:0.5:2) is dissipated in the solution of nickel chloride, zinc chloride and iron chloride, is stirred evenly
Afterwards, the pH value of mixed liquor is adjusted using ammonium hydroxide to 10, is further continued for stirring 0.5h, 2h is stood under 65 DEG C of water bath conditions later makes to mix
Liquid forms collosol state, and gained sol product is then dried 4h to gel state.
(2) 15% water of the iron based nano crystal powder core weight of required preparation is coated with what step (1) obtained
The nanocrystalline magnetic of NiZn ferrite presoma is uniformly mixed, and is then put into mold, applies the pressure of 300MPa, In to mold
Iron based nano crystal composite magnetic powder core idiosome is formed in 150 DEG C of cold sintering 1h under the pressure.
(3) gained iron based nano crystal composite magnetic powder core idiosome is answered in 450 DEG C of annealing 1h to get to iron based nano crystal
Close powder core product.
2 iron based nano crystal composite magnetic powder core component ratio (by weight percentage) of table
| Embodiment 6 | Embodiment 7 | Embodiment 8 | Embodiment 9 | Embodiment 10 | |
| Fe73.5Si13.5B9Nb3Cu1Magnetic powder | 99.5% | 99.0% | 97.0% | 96.0% | 94.0% |
| Ni nanoparticle Zn ferrite | 0.5% | 1.0% | 3.0% | 4.0% | 6.0% |
Embodiment 11~15
The preparation method of ultra-low temperature cold sintered iron base composite magnetic powder core provided by embodiment 11-15 the following steps are included:
(1) by Fe73.5Si13.5B9Nb3Cu1Amorphous and nanocrystalline soft magnetic alloy powder is heat-treated in 350 DEG C under vacuum conditions
1h forms nanocrystalline magnetic.According to the iron based nano crystal composite magnetic powder core constituent content of preparation needed for table 3, by nanocrystalline magnetic point
(molar ratio of Ni, Zn, Fe element is 0.5:0.5:2) is dissipated in the solution of nickel chloride, zinc chloride and iron chloride, is stirred evenly
Afterwards, the pH value of mixed liquor is adjusted using ammonium hydroxide to 10, is further continued for stirring 0.5h, 2h is stood under 65 DEG C of water bath conditions later makes to mix
It closes liquid and forms collosol state, gained sol product is then dried into 4h to gel state.
(2) preparation of iron based nano crystal composite magnetic powder core idiosome
NiZn iron is coated with by what 15% water of the iron based nano crystal powder core weight of required preparation and step (1) obtained
The nanocrystalline magnetic of oxysome presoma is uniformly mixed, and is then put into mold, applies the pressure of 300MPa to mold, in the pressure
Under in 150 DEG C of cold sintering 1h form iron based nano crystal composite magnetic powder core idiosome.
(3) gained iron based nano crystal composite magnetic powder core idiosome is answered in 500 DEG C of annealing 1h to get to iron based nano crystal
Close powder core product.
3 iron based nano crystal composite magnetic powder core component ratio (by weight percentage) of table
Embodiment 16~20
The preparation method of ultra-low temperature cold sintered iron base composite magnetic powder core provided by embodiment 16-20 the following steps are included:
(1) FeSiBP amorphous and nanocrystalline soft magnetic alloy powder is received in 350 DEG C of heat treatment 0.5h formation under vacuum conditions
The brilliant magnetic powder of rice.According to the iron based nano crystal composite magnetic powder core constituent content of preparation needed for table 4, chlorination is dispersed by nanocrystalline magnetic
In the solution of nickel, zinc chloride and iron chloride (molar ratio of Ni, Zn, Fe element is 0.5:0.5:2), after mixing evenly, ammonia is utilized
Water adjusts the pH value of mixed liquor to 10, is further continued for stirring 0.5h, 2h is stood under 65 DEG C of water bath conditions later forms mixed liquor
Then gained sol product is dried 4h to gel state by collosol state.
(2) 15% acetic acid of the iron based nano crystal powder core weight of required preparation is coated with what step (1) obtained
The nanocrystalline magnetic of NiZn ferrite presoma is uniformly mixed, and is then put into mold, applies the pressure of 200MPa, In to mold
Iron based nano crystal composite magnetic powder core idiosome is formed in 150 DEG C of cold sintering 1h under the pressure.
(3) gained iron based nano crystal composite magnetic powder core idiosome is answered in 600 DEG C of annealing 1h to get to iron based nano crystal
Close powder core product.
4 iron based nano crystal composite magnetic powder core component ratio (by weight percentage) of table
| Embodiment 16 | Embodiment 17 | Embodiment 18 | Embodiment 19 | Embodiment 20 | |
| FeSiBP amorphous nano-crystalline magnetic powder | 99.5% | 99.0% | 97.0% | 96.0% | 94.0% |
| Ni nanoparticle Zn ferrite | 0.5% | 1.0% | 3.0% | 4.0% | 6.0% |
Embodiment 21~25
The preparation method of ultra-low temperature cold sintered iron base composite magnetic powder core provided by embodiment 21-25 the following steps are included:
(1) FeSiBPC amorphous magnetic powder is formed into nanocrystalline magnetic in 350 DEG C of heat treatment 0.5h under vacuum conditions.According to
The iron based nano crystal composite magnetic powder core constituent content prepared needed for table 5, disperses manganese nitrate, zinc nitrate and nitre for nanocrystalline magnetic
(molar ratio of Mn, Zn, Fe element is 0.5:0.5:2) adjusts mixed liquor using ammonium hydroxide after mixing evenly in the solution of sour iron
PH value is further continued for stirring 0.5h, 4h is stood under 80 DEG C of water bath conditions later makes mixed liquor form collosol state, then to 9.5
Gained sol product is dried into 4h to gel state.
(2) first by the resulting nanocrystalline magnetic for being coated with nanometer ferrite presoma of step (1) in 500 DEG C of pretreatment 1h
Ferrite presoma is set to generate ferrite, then by 10% acetic acid of the iron based nano crystal powder core weight of required preparation and in advance
It handles products therefrom to be uniformly mixed, then put into mold, apply the pressure of 700MPa to mold, at this pressure in 150 DEG C
Cold sintering 1h forms iron based nano crystal composite magnetic powder core idiosome.
(3) by gained iron based nano crystal composite magnetic powder core idiosome in 400 DEG C of annealing 0.5h to get arrive iron based nano crystal
Composite magnetic powder core product.
5 iron based nano crystal composite magnetic powder core component ratio (by weight percentage) of table
| Embodiment 21 | Embodiment 22 | Embodiment 23 | Embodiment 24 | Embodiment 25 | |
| FeSiBPC alloy magnetic powder | 99.5% | 99.0% | 97.0% | 96.0% | 94.0% |
| Nano-MnZn Ferrite | 0.5% | 1.0% | 3.0% | 4.0% | 6.0% |
Embodiment 26~30
The preparation method of ultra-low temperature cold sintered iron base composite magnetic powder core provided by embodiment 26-30 the following steps are included:
(1) by Fe73.5Si13.5B9Nb3Cu1Amorphous magnetic powder forms nanocrystalline magnetic in 350 DEG C of heat treatment 1h under vacuum conditions
Powder.According to the iron based nano crystal composite magnetic powder core constituent content of preparation needed for table 6, nickel chloride, chlorine are dispersed by nanocrystalline magnetic
Change in the solution of zinc and iron chloride (molar ratio of Ni, Zn, Fe element is 0.5:0.5:2), after mixing evenly, is adjusted using ammonium hydroxide
The pH value of mixed liquor is further continued for stirring 0.5h, 2h is stood under 65 DEG C of water bath conditions later makes mixed liquor form sol form to 10
Then gained sol product is dried 4h to gel state by state.
(2) first by the resulting nanocrystalline magnetic for being coated with nanometer ferrite presoma of step (1) in 550 DEG C of pretreatment 1h
Ferrite presoma is set to generate ferrite, then by 15% water of the iron based nano crystal powder core weight of required preparation and pre- place
It manages products therefrom to be uniformly mixed, then put into mold, apply the pressure of 300MPa to mold, it is cold in 150 DEG C at this pressure
Sintering 1h forms iron based nano crystal composite magnetic powder core idiosome.
(3) gained iron based nano crystal composite magnetic powder core idiosome is answered in 450 DEG C of annealing 1h to get to iron based nano crystal
Close powder core product.
6 iron based nano crystal composite magnetic powder core component ratio (by weight percentage) of table
| Embodiment 26 | Embodiment 27 | Embodiment 28 | Embodiment 29 | Embodiment 30 | |
| Fe73.5Si13.5B9Nb3Cu1Magnetic powder | 99.5% | 99.0% | 97.0% | 96.0% | 94.0% |
| Ni nanoparticle Zn ferrite | 0.5% | 1.0% | 3.0% | 4.0% | 6.0% |
Embodiment 31~35
The preparation method of ultra-low temperature cold sintered iron base composite magnetic powder core provided by embodiment 31-35 the following steps are included:
(1) by Fe73.5Si13.5B9Nb3Cu1Amorphous magnetic powder forms nanocrystalline magnetic in 350 DEG C of heat treatment 1h under vacuum conditions
Powder.According to the iron based nano crystal composite magnetic powder core constituent content of preparation needed for table 7, nickel chloride, chlorine are dispersed by nanocrystalline magnetic
Change in the solution of zinc and iron chloride (molar ratio of Ni, Zn, Fe element is 0.5:0.5:2), after mixing evenly, is adjusted using ammonium hydroxide
The pH value of mixed liquor is further continued for stirring 0.5h, 2h is stood under 65 DEG C of water bath conditions later makes mixed liquor form sol form to 10
Then gained sol product is dried 4h to gel state by state.
(2) first by the resulting nanocrystalline magnetic for being coated with nanometer ferrite presoma of step (1) in 550 DEG C of pretreatment 1h
Ferrite presoma is set to generate ferrite, then by 15% water of the iron based nano crystal powder core weight of required preparation and pre- place
It manages products therefrom to be uniformly mixed, then put into mold, apply the pressure of 300MPa to mold, it is cold in 150 DEG C at this pressure
Sintering 1h forms iron based nano crystal composite magnetic powder core idiosome.
(3) gained iron based nano crystal composite magnetic powder core idiosome is answered in 500 DEG C of annealing 1h to get to iron based nano crystal
Close powder core product.
7 iron based nano crystal composite magnetic powder core component ratio (by weight percentage) of table
| Embodiment 31 | Embodiment 32 | Embodiment 33 | Embodiment 34 | Embodiment 35 | |
| Fe73.5Si13.5B9Nb3Cu1Magnetic powder | 99.5% | 99.0% | 97.0% | 96.0% | 94.0% |
| Ni nanoparticle Zn ferrite | 0.5% | 1.0% | 3.0% | 4.0% | 6.0% |
Embodiment 36~40
The preparation method of ultra-low temperature cold sintered iron base composite magnetic powder core provided by embodiment 36-40 the following steps are included:
(1) FeSiBNbCuMo amorphous magnetic powder is formed into nanocrystalline magnetic in 350 DEG C of heat treatment 1h under vacuum conditions.It presses
According to the iron based nano crystal composite magnetic powder core constituent content of preparation needed for table 8, by nanocrystalline magnetic be scattered in manganese nitrate, zinc nitrate and
(molar ratio of Mn, Zn, Fe element is 0.5:0.5:2) adjusts mixed liquor using ammonium hydroxide after mixing evenly in the solution of ferric nitrate
PH value to 10.5, be further continued for stirring 0.5h, 2h is stood under 65 DEG C of water bath conditions later makes mixed liquor form collosol state, so
Gained sol product is dried into 4h to gel state afterwards.
(2) preparation of iron based nano crystal composite magnetic powder core idiosome
First the resulting nanocrystalline magnetic for being coated with nanometer ferrite presoma of step (1) is made in 550 DEG C of pretreatment 1h
Ferrite presoma generates ferrite, then by 10% acetic acid of the iron based nano crystal powder core weight of required preparation and pre- place
It manages products therefrom to be uniformly mixed, then put into mold, apply the pressure of 600MPa to mold, it is cold in 300 DEG C at this pressure
Sintering 1h forms iron based nano crystal composite magnetic powder core idiosome.
(3) gained iron based nano crystal composite magnetic powder core idiosome is answered in 450 DEG C of annealing 2h to get to iron based nano crystal
Close powder core product.
8 iron based nano crystal composite magnetic powder core component ratio (by weight percentage) of table
| Embodiment 36 | Embodiment 37 | Embodiment 38 | Embodiment 39 | Embodiment 40 | |
| FeSiBNbCuMo alloy powder | 99.5% | 99.0% | 97.0% | 96.0% | 94.0% |
| Nanometer ferrite | 0.5% | 1.0% | 3.0% | 4.0% | 6.0% |
Embodiment 41~45
The preparation method of ultra-low temperature cold sintered iron base composite magnetic powder core provided by embodiment 41-45 the following steps are included:
(1) by Fe73.5Si13.5B9Nb3Cu1Amorphous magnetic powder forms nanocrystalline magnetic in 300 DEG C of heat treatment 2h under vacuum conditions
Powder.According to the iron based nano crystal composite magnetic powder core constituent content of preparation needed for table 9, nickel chloride, chlorine are dispersed by nanocrystalline magnetic
Change in the solution of zinc and iron chloride (molar ratio of Ni, Zn, Fe element is 0.5:0.5:2), after mixing evenly, is adjusted using ammonium hydroxide
The pH value of mixed liquor is further continued for stirring 0.5h, 2h is stood under 65 DEG C of water bath conditions later makes mixed liquor form sol form to 9
Then gained sol product is dried 4h to gel state by state.
(2) first by the resulting nanocrystalline magnetic for being coated with nanometer ferrite presoma of step (1) in 450 DEG C of pretreatment 2h
Ferrite presoma is set to generate ferrite, then by 15% water of the iron based nano crystal powder core weight of required preparation and pre- place
It manages products therefrom to be uniformly mixed, then put into mold, apply the pressure of 800MPa to mold, it is cold in 100 DEG C at this pressure
Sintering 3h forms iron based nano crystal composite magnetic powder core idiosome.
(3) gained iron based nano crystal composite magnetic powder core idiosome is answered in 450 DEG C of annealing 1h to get to iron based nano crystal
Close powder core product.
9 iron based nano crystal composite magnetic powder core component ratio (by weight percentage) of table
Embodiment 46~50
The preparation method of ultra-low temperature cold sintered iron base composite magnetic powder core provided by embodiment 46-50 the following steps are included:
(1) by Fe73.5Si13.5B9Nb3Cu1Amorphous magnetic powder forms nanocrystalline magnetic in 350 DEG C of heat treatment 1h under vacuum conditions
Powder.According to the iron based nano crystal composite magnetic powder core constituent content of preparation needed for table 10, nickel chloride, chlorine are dispersed by nanocrystalline magnetic
Change in the solution of zinc and iron chloride (molar ratio of Ni, Zn, Fe element is 0.5:0.5:2), after mixing evenly, is adjusted using ammonium hydroxide
The pH value of mixed liquor is further continued for stirring 0.5h, 2h is stood under 65 DEG C of water bath conditions later makes mixed liquor form sol form to 12
Then gained sol product is dried 4h to gel state by state.
(2) first by the resulting nanocrystalline magnetic for being coated with nanometer ferrite presoma of step (1) in 550 DEG C of pretreatment 1h
Ferrite presoma is set to generate ferrite, then by 15% ammonium hydroxide of the iron based nano crystal powder core weight of required preparation and in advance
It handles products therefrom to be uniformly mixed, then put into mold, apply the pressure of 300MPa to mold, at this pressure in 300 DEG C
Cold sintering 0.5h is to form fine and close iron based nano crystal composite magnetic powder core idiosome.
(3) by gained iron based nano crystal composite magnetic powder core idiosome in 600 DEG C of annealing 0.5h to get arrive iron based nano crystal
Composite magnetic powder core product.
10 iron based nano crystal composite magnetic powder core component ratio (by weight percentage) of table
Pattern, soft magnetism and mechanical property point are carried out to the amorphous nano-crystalline composite magnetic powder core of above-mentioned section Example preparation
Analysis:
X-ray diffraction is carried out to iron based nano crystal composite magnetic powder core prepared by embodiment 7, embodiment 12 and embodiment 32
Test analysis, analysis result is as shown in Figure 1, it can be seen from the figure that the prepared iron based nano crystal magnetic coated through ferrite
Powder core contains a-Fe, NiZn ferrite and a small amount of a-Fe2O3Phase.
Electronic Speculum test is scanned to iron based nano crystal composite magnetic powder core prepared by embodiment 12, as a result as shown in Figure 2.From
It can be seen that the iron based nano crystal composite magnetic powder core compact structure being prepared by the method for the invention, while magnetic powder quilt in figure
Nanometer particle size glass uniformly coats, so that magnetic conductivity and mechanical strength greatly improved, while magnetic loss and coercive is greatly reduced
Power.
11 the results are shown in Table to the soft magnet performance analysis of embodiment 6-15,26-35.
11 iron based nano crystal composite magnetic powder core component ratio (by weight percentage) of table
Note: 1, above-mentioned magnetic conductivity is to pass through impedance analyzer (E4991B) to prepared iron based nano crystal composite magnetic powder core
It is tested, is obtained by obtained magnetic conductivity real part with frequency variation curve, as shown in figure 3, taking the corresponding magnetic conductance of 10MHz here
Rate real part is as Effective permeability.
2, above-mentioned magnetic powder core loss is under the conditions of 50m and 100mT respectively by soft magnetic materials dynamic measurement device
(MATS-3000SA) it is tested, is obtained by obtained magnetic powder core loss with frequency variation curve, as shown in figure 4, taking here
(50mT, 100KHz) and (100mT, 50KHz) corresponding magnetic powder core loss.
As can be seen from Table 11, through the invention provided by preparation method, even if briquetting pressure is down to~
200MPa, obtained iron based nano crystal composite magnetic powder core still have higher consistency, higher magnetic conductivity and extremely low magnetic powder
Core loss.Magnetic conductivity is stablized frequency range simultaneously and improved to ghz band by the present invention.It is worth noting that, the iron based nano crystal is compound
Powder core shows excellent soft magnet performance in kHz to ghz band.
Claims (10)
1. a kind of preparation method of ultra-low temperature cold sintered iron base nanocomposite powder core, it is characterised in that the following steps are included:
(1) ferritic presoma is coated on to the surface of nanocrystalline magnetic, the dosage of nanocrystalline magnetic and nanometer ferrite
Dosage is respectively 96%~99.5% and is 0.5%~6% by weight percentage；
(2) packet for obtaining 10%~30% mass transfer media of the iron based nano crystal powder core weight of required preparation and step (1)
Be covered with nanometer ferrite presoma nanocrystalline magnetic be uniformly mixed, then by gained mixture in 200~800MPa, 100~
It is sintered 0.5~3h at 300 DEG C and obtains iron based nano crystal composite magnetic powder core idiosome；Or
The resulting nanocrystalline magnetic for being coated with nanometer ferrite presoma of step (1) is made into iron oxygen in 450~600 DEG C of pretreatments
Body presoma generates ferrite, then by gained pretreatment product and the 10% of the iron based nano crystal powder core weight of required preparation
~30% medium is uniformly mixed, and then gained mixture is sintered 0.5~3h at 200~800MPa, 100~300 DEG C and obtained
Iron based nano crystal composite magnetic powder core idiosome；
(3) gained iron based nano crystal composite magnetic powder core idiosome is answered in 400~600 DEG C of annealings to get to iron based nano crystal
Close powder core.
2. the preparation method of ultra-low temperature cold sintered iron base nanocomposite powder core according to claim 1, it is characterised in that
The nanocrystalline magnetic is produced in 300~450 DEG C of 0.5~2h of heat treatment under vacuum conditions by iron-based amorphous nanometer crystalline magnetic powder.
3. the preparation method of ultra-low temperature cold sintered iron base nanocomposite powder core according to claim 2, it is characterised in that
The iron-based amorphous nanometer crystalline magnetic powder be FeSiBNbCu amorphous magnetic powder, FeSiBPCu amorphous magnetic powder, FeSiBP amorphous magnetic powder,
FeSiBNbCuMo amorphous magnetic powder, FeSiB amorphous magnetic powder, FeSiBC amorphous magnetic powder, FeSiBCoNi amorphous magnetic powder and FeSiBPC are non-
At least one of brilliant magnetic powder.
4. the preparation method of the according to claim 1 or 2 or 3 ultra-low temperature cold sintered iron base nanocomposite powder cores, special
Sign is that the nanometer ferrite is Ni nanoparticle Zn ferrite or Nano-MnZn Ferrite.
5. the preparation method of the according to claim 1 or 2 or 3 ultra-low temperature cold sintered iron base nanocomposite powder cores, special
Sign is that nanometer ferrite presoma is coated on nanocrystalline magnetic surface by sol-gel method, hydro-thermal method or coprecipitation.
6. the preparation method of ultra-low temperature cold sintered iron base nanocomposite powder core according to claim 5, it is characterised in that
Nanocrystalline magnetic surface cladding ferrite presoma carries out in the following manner: dispersing the first inorganic salts, for nanocrystalline magnetic
In the mixed solution of two inorganic salts and molysite, after mixing evenly, the pH value of mixed liquor is adjusted to 9~12, is further continued for stirring evenly,
It stands under 40~80 DEG C of water bath conditions to collosol state later, gained sol product is then dried to gel state；
First inorganic salts are nickel salt or manganese salt, and second inorganic salts are zinc salt；In first inorganic salts and the second inorganic salts
The ratio between amount of substance of metallic element is (2~8): (8~2)；The amount of the substance of ferro element and the second inorganic salts in the molysite
Ratio with the sum of amount of substance of other metallic elements in the first inorganic salts is 2:1.
7. the preparation method of the according to claim 1 or 2 or 3 ultra-low temperature cold sintered iron base nanocomposite powder cores, special
Sign is that the mass transfer media is deionized water, ammonium hydroxide, acetic acid or acetic acid.
8. the preparation method of the according to claim 1 or 2 or 3 ultra-low temperature cold sintered iron base nanocomposite powder cores, special
Sign is in step (2), in the second implementation, to the pre- place for the nanocrystalline magnetic for being coated with nanometer ferrite presoma
The reason time is 0.5~2h.
9. the preparation method of the according to claim 1 or 2 or 3 ultra-low temperature cold sintered iron base nanocomposite powder cores, special
Sign is in step (3) that the annealing time to iron based nano crystal composite magnetic powder core idiosome is 0.5~2h.
10. the iron based nano crystal composite magnetic powder core product of claim 1 to 9 any claim the method preparation.
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