CN103898574A - Electroplating Fe-Ni alloy magnetic shielding material and preparation method thereof - Google Patents
Electroplating Fe-Ni alloy magnetic shielding material and preparation method thereof Download PDFInfo
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Abstract
An electroplating Fe-Ni alloy magnetic shielding material and a preparation method thereof. The magnetic shielding material is a composite shielding film material comprising a plurality of Cu thin films or Ni thin films and a plurality of Fe-Ni alloy plating layers, wherein the Fe-Ni alloy plating layers have nickel content of 50%-85%. The magnetic shielding material has high saturation magnetization intensity, and low residual magnetization intensity and coercive force, and has certain magnetic shield performance in a low frequency magnetic field and a static magnetic field. The preparation method comprises the following steps: (1) cleaning the surface of a substrate; (2) depositing the Cu thin films or Ni thin films on the substrate; (3) electroplating the substrate in an electroplating liquid for electroplating the Fe-Ni alloy plating layers; (4) placing the substrate electroplated with the Fe-Ni alloy plating layers in a resistance furnace, fast heating temperature to 300 DEG C, insulating under the protection of hydrogen for 4 h, and finally cooling in hydrogen atmosphere with the furnace to carry out a low temperature annealing treatment; and (5) repeating the steps (2)-(4) to obtain the required Fe-Ni alloy magnetic shielding material.
Description
Technical field
The present invention relates to a kind of plating Fe-Ni alloy magnetic shielding material that is applied to low frequency magnetic field and preparation method thereof.
Background technology
Along with the develop rapidly of modern science and technology, electromagenetic wave radiation increases day by day on environment and human lives's impact, and therefore effective shielding electromagnetic wave is carried out the research of broadband electromagnetic shielding material and is of great significance.The electromagnetic-field-shielded technology of high frequency (> 1MHz) is ripe both at home and abroad at present, but shielding is never well solved for low frequency magnetic field.
Iron-based high magnetic permeability soft magnetic materials, as pure iron, siliconized plate, permalloy, nanocrystalline etc. be magnetic field shielding material the most widely at present.But in low-frequency strong magnetic field, the effectiveness of shielding that material produces by eddying effect is little, and a little less than having the diamagnetic saturability of material of high magnetic permeability, under strong magnetic field action, magnetic permeability declines rapidly, causes effectiveness of shielding sharply to reduce.On the other hand, the ferromagnetic material of high magnetic permeability, generally adopts the method for mechanical workout to obtain, and this not only can reduce the magnetic shield performance of material, and energy consumption increase, cost up, cost performance reduce, all limited its application.
Therefore, traditional single soft magnetic materials is difficult to meet the demand of current electromagnetic wave shielding development.Analyze and numerical evaluation by electromagnetic theory, adopt the composite shielding structure of " high resistance magneticsaturation material+high-permeability material ", using material stronger diamagnetic saturability (as 1J50, electrical pure iron etc.) as the stronger external magnetic field of outer screened film shielding, after magneticstrength is attenuated, the high initial magnetoconductivity material (as 1J79,1J85 etc.) by internal layer further shields again, this optimization design can make material all be operated within the scope of the corresponding magneticstrength of maximum permeability, thereby improves the effectiveness of shielding of material monolithic.
Summary of the invention
The object of the present invention is to provide a kind of Fe-Ni alloy magnetic shielding material with composite shielding structure, this magnetic shielding material can overcome the defect that mechanical workout causes material, and has good magnetic property.
Another object of the present invention is to provide a kind of preparation method of described Fe-Ni alloy magnetic shielding material, adopt the method for galvanic deposit, by adjusting electroplating technology, obtain thering is high saturation and magnetic intensity, the composite shielding thin-film material of low-coercivity.
For achieving the above object, the present invention is by the following technical solutions:
A kind of Fe-Ni alloy magnetic shielding material of electroplating, this magnetic shielding material is to comprise some layers of Cu film/or the composite shielding thin-film material of Ni film and some layers of Fe-Ni alloy layer, wherein, in described Fe-Ni alloy layer, nickel content is 50%～85%.
Described Cu film/or the thickness of Ni film be 1～3 μ m.The thickness of described Fe-Ni alloy layer is relevant with shield effectiveness, can suitably adjust according to required in practical application.
A preparation method for described plating Fe-Ni alloy magnetic shielding material, the method comprises the following steps:
(1) alloy matrix aluminum is carried out to oil removal treatment, and remove the oxide compound of matrix surface;
(2) on alloy matrix aluminum, deposit Cu film/or Ni film;
(3) alloy matrix aluminum is put into electroplate liquid, Cu film/or Ni film on electroplate Fe-Ni alloy layer, negative electrode is 2024 aluminium alloys, anode is the Rhometal that nickel, iron weight ratio are 6: 1, adopt constant voltage galvanic deposit, power supply is DC control current and power supply, and galvanic current cathode current density is 1～4A/dm
2; 50～55 ℃ of heating in water bath;
(4) alloy matrix aluminum that is coated with Fe-Ni alloy layer is placed in to resistance furnace, be rapidly heated to 300 ℃, under hydrogen shield, be incubated 4h, finally under hydrogen atmosphere, furnace cooling carries out low-temperature annealing processing, and Fe-Ni alloy layer is carried out to oil removal treatment after washing;
(5) then repeating step (2)～(4) obtain required Fe-Ni alloy magnetic shielding material.
In described step (1), described oil removal treatment adopts ultrasonic technique or alkali liquor oil removing, and processing condition adopt already known processes condition.Alloy matrix aluminum is carried out to oil removal treatment after washing, then this alloy matrix aluminum is put into pH=10～13, the alkali lye of 60 ℃ is processed 10～15s after washing, removes the oxide compound (Al of aluminium film surface
2o
3), the treatment time is unsuitable long, otherwise easily dissolves aluminium alloy matrix surface, then washes with 50% salpeter solution, then washes with water.
In described step (2), Cu film or the deposition of Ni film on matrix are mainly electroplating pretreatment process, electroplate each time before Fe-Ni alloy layer and need to deposit one deck Cu film/or Ni film at matrix surface, play surface activation.Particularly, alloy matrix aluminum is put into zincate solution and process 45s, after washing, with 50% salpeter solution pickling stripping zinc, after washing, again alloy matrix aluminum is put into zincate solution and process 15s, make its surface replacement one deck zinc; Then alloy matrix aluminum is put into the heavy copper solutions of alkalescence or nickel-plating liquid and processed, make its surface uniform and plate one deck Cu film/or Ni film.In the time of deposition Ni film, alloy matrix aluminum can be put into 80 ℃ of nickel-plating liquids and process 30min, make its surface uniform and plate layer of Ni film.
In aforesaid method, the component content of described electroplate liquid is: single nickel salt 60～200g/L, ferrous sulfate 20g/L, sodium-chlor 30g/L, boric acid 40g/L, Trisodium Citrate 20g/L, asccharin 3g/L, benzene sulfinic acid sodium salt 0.3g/L, Sodium dodecylbenzene sulfonate 0.1g/L.In electroplating process, the pH value of controlling this electroplate liquid is 3.2～3.8 (regulating with dilute sulphuric acid).
The invention has the advantages that:
Plating Fe-Ni alloy magnetic shielding material of the present invention adopts the composite shielding structure of " high resistance magneticsaturation material+high-permeability material ", there is higher saturation magnetization, low residual magnetization and coercive force, in low frequency magnetic field and static magnetic field, there is certain magnetic shielding usefulness.
Accompanying drawing explanation
Fig. 1 electroplates Fe-Ni in embodiment 1
80the SEM figure of (Ni content accounts for 79%) alloy layer.
Fig. 2 electroplates Fe-Ni in the embodiment 1 that utilizes NIM-2000S soft magnetism direct current measurement instrument to record
80the magnetic hysteresis loop of (Ni content accounts for 79%) alloy layer.
Fig. 3 is the effectiveness of shielding of electroplating individual layer Fe-Ni alloy layer (Ni content accounts for 79%) low frequency magnetic field in embodiment 1.
Fig. 4 is the effectiveness of shielding of electroplating individual layer Fe-Ni alloy layer (Ni content accounts for 52%) low frequency magnetic field in embodiment 2.
Fig. 5 is the effectiveness of shielding of two-layer plating Fe-Ni alloy layer (Ni content accounts for 84% and 56%) low frequency magnetic field in embodiment 3.
Embodiment
Below by specific embodiment, the present invention will be further described.
Electroplate FeNi
80alloy layer, adopts Copper Foil (0.3mm is thick) substrate.
Operational path is: oil removing-washing-pickling-washing-mono-time zincate solution-washing-pickling-washing-secondary soaking zinc-washing-plating FeNi
80alloy layer-washing.In this operational path, oil removing is alkaline degreasing, and that pickling is used is 50%HNO
3solution, corresponding processing condition are undertaken by existing technique.
The electroplate liquid proportioning of electroplating Fe-Ni alloy layer is as follows: single nickel salt 200g/L, ferrous sulfate 20g/L, sodium-chlor 30g/L, boric acid 40g/L, Trisodium Citrate 20g/L, asccharin 3g/L, benzene sulfinic acid sodium salt 0.3g/L, Sodium dodecylbenzene sulfonate 0.1g/L.Negative electrode is Copper Foil (0.3mm is thick), and anode is the Rhometal that nickel, iron weight ratio are 6: 1.Adopt constant voltage galvanic deposit, power supply is DC control current and power supply, and galvanic current cathode current density is 4A/dm
2; 55 ℃ of heating in water bath; Control the pH value of electroplate liquid and be 3.2～3.8 (regulating with dilute sulphuric acid).Electroplate 2h; then the alloy matrix aluminum that is coated with Fe-Ni alloy layer is placed in to resistance furnace; be rapidly heated to 300 ℃; under hydrogen shield, be incubated 4h; finally under hydrogen atmosphere, furnace cooling carries out low-temperature annealing processing; and Fe-Ni alloy layer is carried out to oil removal treatment after washing, and obtaining Ni content and be 79% Fe-Ni alloy layer, the thickness of this coating is about 300 μ m.
Adopt NIM-2000S soft magnetism direct current measurement instrument to record and electroplate FeNi
80the magnetic hysteresis loop of alloy layer; Sample is attached on the plastics tubing of Φ 32 × 450mm, adopts Helmholtz coil method magnetic field shielding effect test; Adopt ICP test Coating composition.Fig. 1 is FeNi
80the SEM figure of alloy layer microscopic appearance and diffraction pattern, thin-film material is made up of the crystal grain of nano-scale.Fig. 2 is for electroplating FeNi
80the magnetic hysteresis loop of alloy layer, the sample Bs value recording is 7780Gs, Hc value is 142.9A/m.Illustrate that Fe-Ni alloy layer prepared by the present embodiment has higher saturation magnetization and lower coercive force.Fig. 3 is for electroplating FeNi
80the magnetic field shielding usefulness of alloy layer, test frequency 10～500kHz, initial field intensity is 2.3Gs.As can be seen from the figure electroplate FeNi
80alloy layer has reached good shield effectiveness at high frequency region, more than 10kHz reaches 35dB.
Embodiment 2
Electroplate FeNi
50alloy layer, Copper Foil (0.3mm is thick) substrate
Operational path: oil removing-washing-pickling-washing-mono-time zincate solution-washing-pickling-washing-secondary soaking zinc-washing-plating Fe-Ni alloy layer-washing.In this operational path, oil removing is alkaline degreasing, and that pickling is used is 50%HNO
3solution, corresponding processing condition are undertaken by existing technique.
The electroplate liquid proportioning of electroplating Fe-Ni alloy layer is as follows: single nickel salt 60g/L (electroplates FeNi
50), ferrous sulfate 20g/L, sodium-chlor 30g/L, boric acid 40g/L, Trisodium Citrate 20g/L, asccharin 3g/L, benzene sulfinic acid sodium salt 0.3g/L, Sodium dodecylbenzene sulfonate 0.1g/L.Negative electrode is Copper Foil (0.3mm is thick), and anode is the Rhometal that ferronickel ratio is 6: 1.Adopt constant voltage galvanic deposit, power supply is DC control current and power supply, and galvanic current cathode current density is 1A/dm
2; 55 ℃ of heating in water bath; The pH value of controlling electroplate liquid (regulates with dilute sulphuric acid) 3.2～3.8.Electroplate 2h; then the alloy matrix aluminum that is coated with Fe-Ni alloy layer is placed in to resistance furnace; be rapidly heated to 300 ℃; under hydrogen shield, be incubated 4h; finally under hydrogen atmosphere, furnace cooling carries out low-temperature annealing processing; and Fe-Ni alloy layer is carried out to oil removal treatment after washing, and obtaining Ni content and be 52% Fe-Ni alloy layer, the thickness of this coating is about 300 μ m.
Sample is attached on the plastics tubing of Φ 32 × 450mm, adopts Helmholtz coil method magnetic field shielding effect test.Adopt ICP test Coating composition.Fig. 4 is for electroplating FeNi
50the low frequency magnetic field effectiveness of shielding of alloy layer, test frequency 10～500kHz, initial field intensity is 2.3Gs.As can be seen from the figure electroplate FeNi
50alloy layer has reached good shield effectiveness at high frequency region, but presents rapid downtrending at low frequency region (below 100kHz).
Embodiment 3
Electroplate FeNi
50/ FeNi
80double-layer alloy coating, alloy matrix aluminum
Operational path: oil removing-washing-alkali lye-pickling-washing-mono-time zincate solution-washing-pickling-washing-secondary soaking zinc-washing-chemical nickel plating-plating FeNi
80alloy layer-washing-thermal treatment-oil removing-washing-copper facing-plating FeNi
50alloy layer-washing.
In above-mentioned route, alkali lye is caustic alkali, removes the oxide compound (Al of aluminium film surface
2o
3).Treatment time is unsuitable long, otherwise easy dissolved aluminum matrix surface; That pickling is used is 50%HNO
3solution, chemical nickel plating is alloy matrix aluminum to be put into 80 ℃ of nickel-plating liquids process 30min, makes its surface uniform and plates one deck nickel.The electroplate liquid proportioning of electroplating Fe-Ni alloy layer is as follows: single nickel salt 200g/L (electroplates FeNi
80) or 60g/L (plating FeNi
50), ferrous sulfate 20g/L, sodium-chlor 30g/L, boric acid 40g/L, Trisodium Citrate 20g/L, asccharin 3g/L, benzene sulfinic acid sodium salt 0.3g/L, Sodium dodecylbenzene sulfonate 0.1g/L.Alloy matrix aluminum, anode is the Rhometal that ferronickel ratio is 6: 1.Adopt constant voltage galvanic deposit, power supply is DC control current and power supply, and galvanic current cathode current density is 2A/dm
2; 55 ℃ of heating in water bath; The pH value of controlling electroplate liquid (regulates with dilute sulphuric acid) 3.2～3.8.
Sample is put into Fe-Ni
80in electroplate liquid, prepare the first layer FeNi
80alloy layer; electroplating time is 4h; then the alloy matrix aluminum that is coated with Fe-Ni alloy layer is placed in to resistance furnace; be rapidly heated to 300 ℃, under hydrogen shield, be incubated 4h, finally under hydrogen atmosphere, furnace cooling carries out low-temperature annealing processing; and Fe-Ni alloy layer is carried out to oil removal treatment after washing; obtain Ni content and be 84% Fe-Ni alloy layer, then sample is put into the heavy copper solutions of alkalescence and processed 20min, make its surface uniform deposition one deck copper film.Again sample is put into Fe-Ni
50in electroplate liquid, prepare second layer FeNi
50alloy layer, electroplating time is 4h, obtains Ni content and be 56% second layer Fe-Ni alloy layer.After plating, the total thickness of sample coating is about 300 μ m.
Sample is attached on the plastics tubing of Φ 32 × 450mm, adopts Helmholtz coil method magnetic field shielding effect test; Adopt ICP test Coating composition.Fig. 4 is for electroplating FeNi
50/ FeNi
80the low frequency magnetic field effectiveness of shielding of double-layer alloy coating, test frequency is 10～500kHz, initial field intensity is 2.3Gs.As can be seen from the figure electroplate FeNi
50/ FeNi
80double-layer alloy coating has reached good shield effectiveness at high frequency region, and is better than the FeNi of identical thickness of coating at low frequency region
80alloy layer and FeNi
50the magnetic shielding usefulness of alloy layer.Under the static magnetic field of 1Gs, record double-deck Fe-Ni alloy composite coating and can reach 36.6dB, show that this matrix material has good shielding in of magnetostatic field effect.
Claims (4)
1. electroplate Fe-Ni alloy magnetic shielding material for one kind, it is characterized in that, this magnetic shielding material is to comprise some layers of Cu film/or the composite shielding thin-film material of Ni film and some layers of Fe-Ni alloy layer, and wherein, in described Fe-Ni alloy layer, nickel content is 50%～85%.
2. plating Fe-Ni alloy magnetic shielding material according to claim 1, is characterized in that, described Cu film/or the thickness of Ni film be 1～3 μ m.
3. a preparation method for plating Fe-Ni alloy magnetic shielding material claimed in claim 1, is characterized in that, the method comprises the following steps:
(1) alloy matrix aluminum is carried out to oil removal treatment, and remove the oxide compound of matrix surface;
(2) on alloy matrix aluminum, deposit Cu film/or Ni film;
(3) alloy matrix aluminum is put into electroplate liquid, Cu film/or Ni film on electroplate Fe-Ni alloy layer, negative electrode is 2024 aluminium alloys, anode is the Rhometal that nickel, iron weight ratio are 6: 1, adopt constant voltage galvanic deposit, power supply is DC control current and power supply, and galvanic current cathode current density is 1～4A/dm
2; 50～55 ℃ of heating in water bath;
(4) alloy matrix aluminum that is coated with Fe-Ni alloy layer is placed in to resistance furnace, be rapidly heated to 300 ℃, under hydrogen shield, be incubated 4h, finally under hydrogen atmosphere, furnace cooling carries out low-temperature annealing processing, and Fe-Ni alloy layer is carried out to oil removal treatment after washing;
(5) repeating step (2)～(4) obtain required Fe-Ni alloy magnetic shielding material.
4. the preparation method of plating Fe-Ni alloy magnetic shielding material according to claim 3, it is characterized in that, the component content of described electroplate liquid is: single nickel salt 60～200g/L, ferrous sulfate 20g/L, sodium-chlor 30g/L, boric acid 40g/L, Trisodium Citrate 20g/L, asccharin 3g/L, benzene sulfinic acid sodium salt 0.3g/L, Sodium dodecylbenzene sulfonate 0.1g/L, the pH value of controlling this electroplate liquid is 3.2～3.8.
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| CN108796587A (en) * | 2017-05-02 | 2018-11-13 | 贵州理工学院 | A kind of continuous method and device for preparing high-silicon steel thin strip |
| CN108930053A (en) * | 2018-08-22 | 2018-12-04 | 哈尔滨工业大学 | A kind of preparation method of aluminum-based layered shielding material |
| CN109065360A (en) * | 2018-08-22 | 2018-12-21 | 哈尔滨工业大学 | A kind of preparation method of the electro-deposition permalloy film on aluminum matrix composite |
| CN110149790A (en) * | 2019-05-31 | 2019-08-20 | 厦门大学 | Graphene electromagnetic shielding film and preparation method thereof |
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| CN114318445A (en) * | 2021-12-24 | 2022-04-12 | 珠海多创科技有限公司 | Composite magnetic gathering film |
| CN115213396A (en) * | 2022-08-16 | 2022-10-21 | 湖南金天铝业高科技股份有限公司 | Electromagnetic shielding material and preparation method thereof |
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| CN105780068A (en) * | 2014-12-16 | 2016-07-20 | 北京有色金属研究总院 | Single-pulse electrodeposition method for Ni-Fe alloy magnetic coatings |
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| CN111304653A (en) * | 2020-04-01 | 2020-06-19 | 哈尔滨工业大学（威海） | Multi-frequency band electromagnetic wave shielding composite film layer and preparation method and application thereof |
| CN114318445A (en) * | 2021-12-24 | 2022-04-12 | 珠海多创科技有限公司 | Composite magnetic gathering film |
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Application publication date: 20140702 |