CN104862618B - A kind of composite amorphous magnetically soft alloy material and preparation method thereof - Google Patents
A kind of composite amorphous magnetically soft alloy material and preparation method thereof Download PDFInfo
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- CN104862618B CN104862618B CN201510200879.9A CN201510200879A CN104862618B CN 104862618 B CN104862618 B CN 104862618B CN 201510200879 A CN201510200879 A CN 201510200879A CN 104862618 B CN104862618 B CN 104862618B
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Abstract
A kind of composite amorphous magnetically soft alloy material preparation method, the composite amorphous magnetically soft alloy material composition is Fe67Co18Si11B4‑Ni71P29；Its preparation method is as follows：Amorphous soft magnetic ribbon is prepared first, then prepares chemical nickel phosphorus plating plating solution and composite amorphous magnetically soft alloy is prepared using chemical deposition.It is an advantage of the invention that：The present invention passes through composite amorphous magnetically soft alloy superior performance made from chemical deposition：In the range of frequency is 1kHz 1MHz, alternating magnetic field be that initial permeability can improve an order of magnitude under conditions of 0.05A/m, be maintained at 1870 substantially constants constant；Its relaxation frequency and the more former alloy of quality factor are significantly improved.Present invention process is simple and convenient to operate, with low cost, suitable extensive mass industrial production.
Description
Technical field
It is particularly a kind of composite amorphous soft the present invention relates to magnetic function soft magnetic materials and chemical deposited nickel phosphorus technology field
Permalloy material and preparation method thereof.
Background technology
Soft magnetic materials refers to that those have the metallicl magnetic material of low-coercivity, high magnetic permeability, in electric power, electronics and modern times
Have important in new technology and be widely applied.Digital communication technology and the fast development of fiber optic communication, constantly update, eliminate biography
The artificial traffic equipment of system；The various power transformers largely used in the field of communications, majority is operated under low magnetic flux density,
At this moment the magnetic conductivity of material has just played main function.In particular with the development of high frequency technique, to the high frequency characteristics of soft magnetic materials
Propose higher requirement.Magnetic conductivity is one of basic parameter of soft magnetic materials, is primarily referred to as initial permeability μi, it is operating point
Positioned at the permeability of magnetization curve initial part, for the soft magnetic materials applied under low-intensity magnetic field, this is most important property
Can index.But, high-permeability material should also have high quality factor, high relaxation in addition to it should have high initial permeability
Henan frequency etc., and iron nickel system alloy now often have ignored this means suitable while high magnetic permeability is pursued, and can not carry
Other parameters are taken into account while high magnetic permeability, material property is reached a balance well.
The relaxation frequency f of magnetically soft alloy0It is two important parameters of its high frequency performance of evaluation with quality factor q.Higher
Relaxation frequency and larger quality factor illustrate that material has preferable high frequency performance.Under the conditions of alternating magnetic field, it is desirable to
Higher initial permeability under material low frequency can be remained to higher frequency.Therefore, it is possible to first applied to the height under high frequency condition
Beginning magnetic conductivity magnetically soft alloy inherently obtains extensive use.
Chemical plating is the proper method that a kind of wet method prepares soft magnetism coating.Chemical plating compared with mature electroplating industry,
Have the advantages that its is unique:Cheap, preparation method is simple, do not need external power, transmission system and auxiliary electrode, during operation only
Workpiece need to be correctly hung in the plating solution；Coating, can the uniform plating in complicated shape substrate than more uniform；Can be
Plating in non-conductor substrate；By the autocatalytic activity plating of base material, thus adhesion generally to be preferred over plating；Plated layer compact, space
Rate is low.And chemical Ni-P plating has the soft magnet performance that can be compared favourably with plating.
The content of the invention
The purpose of the present invention is for above-mentioned technical Analysis and there is problem there is provided a kind of composite amorphous magnetically soft alloy material
And preparation method thereof, while the composite amorphous magnetically soft alloy material still has high initial permeability at higher frequencies, gather around
There are higher quality factor and relaxation frequency.
Technical scheme：
A kind of composite amorphous magnetically soft alloy material, composition is Fe67Co18Si11B4-Ni71P29。
A kind of preparation method of the composite amorphous magnetically soft alloy material, step is as follows：
1) preparation of master alloy ingot
Fe, Co, Si, B raw material that purity is not less than 99.9% are chosen respectively, and dispensing is carried out according to element mass percent,
Fe is smelted into vaccum sensitive stove67Co18Si11B4Master alloy ingot, control is weightless to be no more than 5%；
2)Fe67Co18Si11B4The preparation of amorphous alloy ribbon
Fe is prepared using single roller melt rotation quick quenching technique in an atmosphere67Co18Si11B4Amorphous soft magnetic ribbon sample, it is non-
The width of brilliant strip is that 22mm, thickness are 25.2 μm；
3)Fe67Co18Si11B4The pretreatment of amorphous alloy ribbon
Under the conditions of room temperature and outer ultrasonic ripple, above-mentioned amorphous thin ribbon is placed in ethanol solution and soaks 20min, taken out
The oxide of three greasy dirts to remove surface, the impurity of absorption and surface porosity is eluted with deionized water afterwards；
4) preparation of chemical nickel plating phosphor bath
Chemical nickel plating phosphor bath is to be dissolved in distilled by nickel sulfate, sodium hypophosphite, sodium citrate, lactic acid and anhydrous sodium acetate
The concentration of each component is in the mixed liquor that water is made, mixed liquor：Nickel sulfate 25g/L, sodium hypophosphite 40g/L, sodium citrate
10g/L, lactic acid 15ml/L, anhydrous sodium acetate 30g/L, mixed liquor are 4.4-4.6 by adding natrium carbonicum calcinatum to adjust pH value；
5)Fe67Co18Si11B4-Ni71P29The preparation of composite soft magnetic alloy material
In Fe67Co18Si11B4Ni is carried out on amorphous soft-magnetic alloy71P29Magnetospheric deposition, method is as follows：Will be by pre- place
The amorphous thin ribbon of reason is placed in the chemical nickel plating phosphor bath of preparation, the plating 10min under 86-88 DEG C of temperature, stirring condition, is taken out
Eluted three times with deionized water afterwards, natural air drying, Fe is made67Co18Si11B4-Ni71P29Composite amorphous magnetically soft alloy.
The advantages of the present invention are：
Superior using composite amorphous magnetically soft alloy high frequency performance made from chemical deposition, its relaxation frequency is up to
5.11MHz；Its quality factor is 12 under conditions of 1MHz；Magnetic field is 0.05A/m's in the range of frequency is 1kHz-1MHz
Under the conditions of initial permeability to be maintained at 1870 substantially constants constant；Present invention process is simple and convenient to operate, with low cost, is adapted to
Extensive mass industrial production.
Embodiment
Embodiment：
A kind of preparation method of composite amorphous magnetically soft alloy material, the composite amorphous magnetically soft alloy material composition is
Fe67Co18Si11B4-Ni71P29, prepared using chemical deposition, step is as follows：
1) preparation of master alloy ingot
Fe, Co, Si, B raw material that purity is 99.95% are chosen respectively, dispensing are carried out according to element mass percent, true
Fe is smelted into empty induction furnace67Co18Si11B4Master alloy ingot, it is 4% to control weightless；
2)Fe67Co18Si11B4The preparation of amorphous alloy ribbon
Fe is prepared using single roller melt rotation quick quenching technique in an atmosphere67Co18Si11B4Amorphous soft magnetic ribbon sample, it is non-
The width of brilliant strip is that 22mm, thickness are 25.2 μm；
3)Fe67Co18Si11B4The pretreatment of amorphous alloy ribbon
Under the conditions of room temperature and outer ultrasonic ripple, above-mentioned amorphous thin ribbon is placed in ethanol solution and soaks 20min, taken out
The oxide of three greasy dirts to remove surface, the impurity of absorption and surface porosity is eluted with deionized water afterwards；
4) preparation of chemical nickel plating phosphor bath
Chemical nickel plating phosphor bath is to be dissolved in distilled by nickel sulfate, sodium hypophosphite, sodium citrate, lactic acid and anhydrous sodium acetate
The concentration of each component is in the mixed liquor that water is made, mixed liquor：Nickel sulfate 25g/L, sodium hypophosphite 40g/L, sodium citrate
10g/L, lactic acid 15ml/L, anhydrous sodium acetate 30g/L, mixed liquor are 4.4-4.6 by adding natrium carbonicum calcinatum to adjust pH value；
5)Fe67Co18Si11B4-Ni71P29The preparation of composite soft magnetic alloy material
In Fe67Co18Si11B4Ni is carried out on amorphous soft-magnetic alloy71P29Magnetospheric deposition, method is as follows：Will be by pre- place
The amorphous thin ribbon of reason is placed in the chemical nickel plating phosphor bath of preparation, the plating 10min under 86 DEG C of temperature, stirring conditions, after taking-up
Eluted three times with deionized water, natural air drying, Fe is made67Co18Si11B4-Ni71P29Composite amorphous magnetically soft alloy, it is non-after plating
The thickness of brilliant strip is 26.7 μm.
Table 1 is Fe67Co18Si11B4Amorphous soft-magnetic alloy and Fe67Co18Si11B4-Ni71P29Composite soft magnetic alloy in frequency
It is initial permeability μ, relaxation frequency f under the conditions of 0.05A/m for 1kHz magnetic fields0, and the quality factor q under the conditions of 1MHz.
Table 1
Claims (2)
1. a kind of composite amorphous magnetically soft alloy material, it is characterised in that：Composition is Fe67Co18Si11B4-Ni71P29。
2. a kind of preparation method of composite amorphous magnetically soft alloy material as claimed in claim 1, it is characterised in that step is as follows：
1) preparation of master alloy ingot
Fe, Co, Si, B raw material that purity is not less than 99.9% are chosen respectively, dispensing are carried out according to element mass percent, true
Fe is smelted into empty induction furnace67Co18Si11B4Master alloy ingot, control is weightless to be no more than 5%；
2)Fe67Co18Si11B4The preparation of amorphous alloy ribbon
Fe is prepared using single roller melt rotation quick quenching technique in an atmosphere67Co18Si11B4Amorphous soft magnetic ribbon sample, amorphous is thin
The width of band is that 22mm, thickness are 25.2 μm；
3)Fe67Co18Si11B4The pretreatment of amorphous alloy ribbon
Under the conditions of room temperature and outer ultrasonic ripple, above-mentioned amorphous thin ribbon is placed in ethanol solution and soaks 20min, is used after taking-up
Deionized water elutes the oxide of three greasy dirts to remove surface, the impurity of absorption and surface porosity；
4) preparation of chemical nickel plating phosphor bath
Chemical nickel plating phosphor bath is to be dissolved in aquae destillata system by nickel sulfate, sodium hypophosphite, sodium citrate, lactic acid and anhydrous sodium acetate
Into mixed liquor, the concentration of each component is in mixed liquor：Nickel sulfate 25g/L, sodium hypophosphite 40g/L, sodium citrate 10g/L,
Lactic acid 15ml/L, anhydrous sodium acetate 30g/L, mixed liquor are 4.4-4.6 by adding natrium carbonicum calcinatum to adjust pH value；
5)Fe67Co18Si11B4-Ni71P29The preparation of composite soft magnetic alloy material
In Fe67Co18Si11B4Ni is carried out on amorphous soft-magnetic alloy71P29Magnetospheric deposition, method is as follows：By by pretreatment
Amorphous thin ribbon is placed in the chemical nickel plating phosphor bath of preparation, is used under 86-88 DEG C of temperature, stirring condition after plating 10min, taking-up
Deionized water is eluted three times, natural air drying, and Fe is made67Co18Si1B14-Ni71P29Composite amorphous magnetically soft alloy.
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Family Cites Families (6)
| Publication number | Priority date | Publication date | Assignee | Title |
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| JP2710938B2 (en) * | 1987-12-11 | 1998-02-10 | 日立金属株式会社 | High saturation magnetic flux density soft magnetic alloy |
| CN1150349C (en) * | 2001-09-29 | 2004-05-19 | 中国科学院金属研究所 | Method of supersonic chemical plating nickel phosphorus of powder metallurgy material |
| JP4044531B2 (en) * | 2004-03-10 | 2008-02-06 | 独立行政法人科学技術振興機構 | Ultra high strength Fe-Co based bulk metallic glass alloy |
| JP5645108B2 (en) * | 2010-07-14 | 2014-12-24 | 日立金属株式会社 | Amorphous alloy ribbon and magnetic component having amorphous alloy ribbon |
| CN102568745B (en) * | 2011-12-14 | 2014-04-02 | 同济大学 | Electro-deposition preparation method for Fe-Co soft magnetic film |
| CN103632794B (en) * | 2012-08-28 | 2017-04-12 | 有研稀土新材料股份有限公司 | Composite soft magnetic material and method for preparing material |
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