CN102995083A - Method for preparing soft-magnetic material iron-nickel alloy array by adopting plating - Google Patents

Method for preparing soft-magnetic material iron-nickel alloy array by adopting plating Download PDF

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CN102995083A
CN102995083A CN201210526589XA CN201210526589A CN102995083A CN 102995083 A CN102995083 A CN 102995083A CN 201210526589X A CN201210526589X A CN 201210526589XA CN 201210526589 A CN201210526589 A CN 201210526589A CN 102995083 A CN102995083 A CN 102995083A
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nickel alloy
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张海霞
李忠亮
孙旭明
郑阳
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Peking University
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Abstract

The invention aims at providing a method for preparing a soft-magnetic material iron-nickel alloy array by adopting plating. The method provided by the invention achieves the optimized alloy proportion by adopting a specific plating solution formula, thereby realizing the best soft magnetism; the method can be used for growing films with a uniform height of 10-50 microns on a seed layer of 0.15 micron and has the advantages of simple process, easiness for implementation, low cost, convenient for experiment process control, self regulation and great flexibility of the plating solution formula, convenient for integration with other processes by being carried out after photoetching, and the like; the manufactured array is positioned in a unit of 2000*2000 microns and is convenient to measure; according to the manufacturing method of the array, the soft magnetism of an iron-nickel alloy material is greatly enhanced, and the magnetism of the iron-nickel alloy material is greatly enhanced by adding nanometer magnetic granules.

Description

A kind of method for preparing soft magnetic materials iron-nickel alloy array of electroplating that adopts
Technical field
The present invention relates to field of semiconductor manufacture, be specifically related to micro-nano processing technique field, relate in particular to a kind of method for preparing soft magnetic materials iron-nickel alloy array of electroplating that adopts.
Background technology
Iron-nickel alloy is a kind of material that possesses good soft magnetic performance, has narrow and thin magnetic hysteresis loop, and residual magnetization and coercive force are all smaller, and initial permeability has a wide range of applications in low-intensity magnetic field and RF application up to more than 100000.Especially as the core material of MEMS inductance, can greatly promote inductance value and quality factor (Q value), so that inductance has good application under RF application.
MEMS (micro electro mechanical system) (MEMS) is a kind of technology of novel multidisciplinary intersection, and it relates to the multiple subjects such as machinery, electronics, chemistry, physics, optics, biology, material.In the nanometer processing device, often need a kind of high performance magneticsubstance of processing as the part of functions material of device, for example core material of MEMS inductance.In the MEMS processing technology, usually can be by vacuum-evaporation (evaporation), sputter (sputtering), the methods such as (electroplating) of plating prepares alloy firm.Vacuum-evaporation refers in vacuum chamber heating thin-film material to be evaporated, and its atom or molecule are overflowed from the surface gasification, forms vapour stream incident and is deposited to method on the solid (substrate).Sputter is a kind of high-energy ion bombardment target, sputters atom or molecule deposition film forming process on anode substrate.For example, the Co-Femetal/native-oxide multilayers:a new directionin soft magnetic thin film design I.Quasi-static properties anddynamic response(IEEE transaction on Magnetics that the people such as G.S.D.Beach delivered in 2005,2005.41 (6): p.2043--2052) (Chinese exercise question: ferro-cobalt and zone of oxidation multilayered structure: the new direction of soft magnetic film the quasi-static characteristics and dynamic response design) did the sputter Study on Preparation of CoFe alloy.Refer to utilize electrolysis principle to electroplate the method for the metal of some special component in some metallic surface and electroplate.Electro-plating method is that than the advantage of front two kinds of methods produced alloy internal stress is less, and manufacturing processed can assign to control the alloy ratio of alloy firm by the one-tenth of adjusting electroplate liquid, thereby improves soft magnetic property.For example, the Microstructure and magnetic properties inarrays of ac electrodeposited Fe x Ni 1-x nanowires induced bythe continuous and pulse electrodeposition that delivered in 2011 of the people such as M.Almasi Kashi.(Applied Physics A:Materials Science ﹠amp; Processing, 2011.102 (3): p.761--764) (Chinese exercise question: the microstructure of the iron-nickel alloy nano wire of employing direct current and pulsed current preparation and the analysis of magnetic, International Periodicals: the Applied Physics wall bulletin) did the experiment of using alumina anode plating preparation iron nickel nano wire.
From above introduction as can be known, plating is demanded research urgently as a kind of method for preparing alloy of maturation and how realize integrated processing in MEMS.
Summary of the invention
For above-mentioned processing problems for the iron-nickel alloy material, the invention provides a kind of the employing and electroplate the method for preparing soft magnetic materials iron-nickel alloy array, the method is carried out the plating of specific alloy components containing by disposing specific electroplate liquid.Can realize low-stress, high performance soft magnetic film, and be easy to other micro-nano processing technology technique integrated.
The invention provides a kind of the employing and electroplate the method for preparing soft magnetic materials iron-nickel alloy array, comprise the steps: in order
Substrate sputtering seed layer;
Thick resist lithography goes out array pattern;
The preparation electroplate liquid;
Power parameter is set, junction circuit;
Adjusting electroplating time and uniform stirring equipment electroplates;
Remove photoresist material with acetone;
Go Seed Layer with Glacial acetic acid and hydrogen peroxide;
In vacuum chamber, anneal;
The soft magnetic performance of test iron-nickel alloy array
Substrate is silicon chip in the step (a), and Seed Layer is the titanium copper Seed Layer, and wherein titanium thickness 150
Figure BDA00002547015400031
Copper thickness 1500
Figure BDA00002547015400032
The design of array shape display figure and parameter designing in the step (b), array pattern comprises circular array, quadrate array, rectangular array, monoblock is square and monoblock is circular, the photoetching degree of depth is 10-50 μ m; Parameter designing comprises the spacing between array sizes, the array element, also has array pattern to account for the ratio of monoblock figure.
Composition and the concentration of step (c) preparation electroplate liquid comprise: single nickel salt NiSO 46H 2O:187g/L, nickelous chloride NiCl 26H 2O:50g/L, ferrous sulfate FeSO 47H 2O:64g/L, boric acid H 3BO 3: 40g/L, sodium chloride nacl: 20g/L, sodium lauryl sulphate NaC 12H 25SO 4: 0.2g/L), phosphoric acid H 3PO 4: 5g/L, asccharin Saccharin:3.5g/L.
When iron nickel ratio is 7:93, only need to change following two kinds of reagent: single nickel salt NiSO 46H2O:176g/L, ferrous sulfate FeSO 47H2O:18g/L.
When iron nickel ratio is 50:50, only need to change following three kinds of reagent: single nickel salt NiSO 46H 2O:130.9g/L, nickelous chloride NiCl 26H 2O:35g/L, ferrous sulfate FeSO 47H 2O:179.2g/L.
Step (d) power parameter comprises: current density, pulse-repetition, dutycycle, electroplating time, power supply provides pulsed current.
Step (c) is mixed the nano magnetic particle in electroplate liquid, to improve the alloy soft magnetic performance.
Annealing temperature 600-700 ℃ of step (h) reduces internal stress by heat treatment process, promotes the homogeneity of alloy material.
The invention provides a kind of iron-nickel alloy array, is to use the aforesaid method preparation, and its thickness is 10-50 μ m, and saturation induction density is more than the 1T.
The object of the present invention is to provide a kind of electro-plating method of reliable integrated iron-nickel alloy array, the method adopts specific plating solution formula to reach the ratio of optimized alloy, thereby realizes best soft magnetic performance.It is good to grow homogeneity in the Seed Layer of 0.15 μ m, the film of highly homogeneous 10 μ m-50 μ m.And it is simple to have technique, is easy to realize, with low cost, be convenient to control the advantage such as experimentation.Simultaneously plating solution formula can Self-adjustment, has great handiness.After photoetching, be convenient to other techniques integrated.The array of making is convenient to measure in the unit of 2000 μ m*2000 μ m.By the manufacture method of array, the soft magnetic performance of iron-nickel alloy material has obtained great lifting.The simultaneously adding of nano magnetic particle also has larger lifting to the magnetic of material.
Description of drawings
By reading the detailed description that non-limiting example is done of doing with reference to the following drawings, it is more obvious that other features, objects and advantages of the present invention will become, and same or analogous Reference numeral represents same or analogous parts in the accompanying drawing.
Figure l is the flow chart of steps that the present invention adopts the embodiment of the method for electroplating preparation iron-nickel alloy array;
Fig. 2-Fig. 5 is the electron scanning micrograph of the iron-nickel alloy array surface of use the method for the invention preparation, wherein Fig. 2 is the orthographic plan of circular array, Fig. 3 is the orthographic plan of rectangular array, and Fig. 4 is the cross-sectional view of circular array, and Fig. 5 is the larger configuration of surface figure of magnification;
Fig. 6 is the equipment drawing of the electroplanting device that adopts of the present invention;
Fig. 7 is the EDX composition analysis result of iron nickel (20:80) the alloy array of use the method for the invention preparation;
Fig. 8 is the EDX composition analysis result of iron nickel (7:93) the alloy array of use the method for the invention preparation;
Fig. 9 is the magnetic test result of iron nickel (20:80) alloy of use the method for the invention preparation;
Figure 10 is the magnetic test result of iron nickel (7:93) alloy of use the method for the invention preparation.
Embodiment
For above-mentioned purpose of the present invention, feature and advantage can be become apparent more, below in conjunction with the drawings and specific embodiments the embodiment of the invention is described in further detail.
The below describes embodiments of the invention in detail, and the example of described embodiment is shown in the drawings, and wherein identical or similar label represents identical or similar element or the element with identical or similar functions from start to finish.Be exemplary below by the embodiment that is described with reference to the drawings, only be used for explaining the present invention, and can not be interpreted as limitation of the present invention.
Embodiment one:
With reference to Fig. 1, Fig. 1 is that a kind of employing of the present invention electroplated the method for preparing soft magnetic materials iron-nickel alloy array, and the flow chart of steps of embodiment comprises the steps:
Step S1 adopts the method splash-proofing sputtering metal Ti150 of sputter at the silicon chip in (110) crystal orientation of cleaning
Figure BDA00002547015400061
Metal Cu1500
Figure BDA00002547015400062
Step S2 drips photoresist material at silicon chip surface first, spares in advance glue 60s with the speed of 540r/s first, then carries out the formal even glue 180s of 1500r/s, guarantees that photoresist material evenly is coated with out at silicon chip surface.125s, afterwards taking-up expose under lithography machine.Under 80 ℃, dry by the fire film 210s.Then develop, soak 120s in the developing solution.Guarantee development effect at microscopically.
Step S3 is at first measured the configuration that a certain amount of deionized water carries out electroplate liquid.(introducing the configuration of electroplate liquid here as an example of 1L example).Pour deionized water into tank.Get an amount of medicine with projection electronic weighing and pour tank into.Selecting iron nickel ratio is after the electroplate liquid of 20:80 adds all medicines, tank to be put into 60 ℃ of water-baths, and use glass stick to stir the help agent dissolves.Candidate agent dissolves fully, uses the PH test paper to measure pH value and also can adjust electroplate liquid pH value to 4.0 by adding sodium hydroxide or sulfuric acid.
Step S4, according to the area conversion supply current size that needs on the silicon chip are electroplated figure, supply current=current density * electroplates graphics area.The present invention adopts the current density of 4ASD, so can calculate by electroplating graphics area the size of the supply current that needs setting.Here be assumed to be 80mA.Setting dutycycle is 50%, forward conduction time 1ms, and forward turn-off time 1ms, forward current 2ms, reversible circulation 0 is so just set 0-80mA, dutycycle 50%, the pulsed current of frequency 500Hz.
Step S5, the circuit anode adopts clean nickel block, and negative electrode connects silicon chip.Silicon chip need to clash the convenient conduction of electrode leads to client with acetone.Anode and cathode is put into electroplate liquid connect power supply, check whether supply current is correct.Pass into whipping appts, electroplate liquid is kept evenly.Setting the power turn-on time is 2h, and plugged begins to electroplate.
Step S6 sets 670 ℃ of annealing temperatures, and annealing continues 2h.Cool off with the speed of 100 ℃/h afterwards.
Step S7 is immersed in 1min in the acetone soln with silicon chip, treats that the photoresist material on surface is all removed afterwards taking-up.(remove Cu: Glacial acetic acid, hydrogen peroxide and deionized water are according to the mixed solution of the ratio of 1:1:20 to utilize corrosive fluid; Remove Ti: hydrofluoric acid and deionized water are according to the mixed solution of the volume ratio of 1:60) remove Cu, the Ti alloy Seed Layer of silicon chip surface.Silicon chip is fully cleaned in deionized water, and oven dry.
Step S8 utilizes the manual sliver of scribing pen, obtains sample.Sample is carried out the measurement of magnetic hysteresis loop.
With reference to Fig. 2-Fig. 5, Fig. 2-Fig. 5 is the electron scanning micrograph (10 μ m) of the iron-nickel alloy array surface of use the method for the invention preparation.Can find out that from photo the alloy array of electroplating out has good configuration of surface and homogeneity.Surface height difference is no more than 0.5 μ m.Fig. 2, Fig. 3 can find out that array surface form and homogeneity are all relatively good, and can find out that homogeneity is very good under the high multiple amplification from Fig. 5, and as can be seen from Figure 4 the transverse section of array does not have the slight crack flaw, and electroplating effect is good.
With reference to Fig. 7, Fig. 7 is the EDX of iron-nickel alloy (20:80) array that uses the method for the invention preparation figure as a result.Figure has shown that the iron-nickel alloy ratio is 20:80. as a result
With reference to Fig. 9, Fig. 9 is the magnetic test result of the iron-nickel alloy (20:80) of the method for the invention preparation on probation.Can find out that from shape and the coordinate parameters of magnetic hysteresis loop sample presents preferably soft magnetic property.Coercive force is lower, is 1.345Oe, and squareness ratio is 5.59*10-4, and saturation induction density can reach 1T.
Embodiment 2:
With reference to Fig. 1, Fig. 1 is the flow chart of steps that the present invention adopts the embodiment of the method for electroplating preparation iron-nickel alloy array, comprises the steps:
Step S1 adopts the method splash-proofing sputtering metal Ti150 of sputter at the silicon chip in (110) crystal orientation of cleaning
Figure BDA00002547015400081
Metal Cu1500
Figure BDA00002547015400082
Step S2 drips photoresist material at silicon chip surface first, spares in advance glue 60s with the speed of 540r/s first, then carries out the formal even glue 180s of 1500r/s, guarantees that photoresist material evenly is coated with out at silicon chip surface.125s, afterwards taking-up expose under lithography machine.Under 80 ℃, dry by the fire film 210s.Then develop, soak 120s in the developing solution.Guarantee development effect at microscopically.
Step S3 is at first measured the configuration that a certain amount of deionized water carries out electroplate liquid.(introducing the configuration of electroplate liquid here as an example of 1L example).Pour deionized water into tank.Get an amount of medicine with projection electronic weighing and pour tank into.Selecting iron nickel ratio is after the electroplate liquid of 7:93 adds all medicines, tank to be put into 60 ℃ of water-baths, and use glass stick to stir the help agent dissolves.Candidate agent dissolves fully, uses the PH test paper to measure pH value and also can adjust electroplate liquid pH value to 4.0 by adding sodium hydroxide or sulfuric acid.
Step S4, according to the area conversion supply current size that needs on the silicon chip are electroplated figure, supply current=current density * electroplates graphics area.The present invention adopts the current density of 4ASD, so can calculate by electroplating graphics area the size of the supply current that needs setting.Here be assumed to be 80mA.Setting dutycycle is 50%, forward conduction time 1ms, and forward turn-off time 1ms, forward current 2ms, reversible circulation 0 is so just set 0-80mA, dutycycle 50%, the pulsed current of frequency 500Hz.
Step S5, the circuit anode adopts clean nickel block, and negative electrode connects silicon chip.Silicon chip need to clash the convenient conduction of electrode leads to client with acetone.Anode and cathode is put into electroplate liquid connect power supply, check whether supply current is correct.Pass into whipping appts, electroplate liquid is kept evenly.Setting the power turn-on time is 2h, and plugged begins to electroplate.
Step S6 sets 670 ℃ of annealing temperatures, and annealing continues 2h.Cool off with the speed of 100 ℃/h afterwards.
Step S7 is immersed in 1min in the acetone soln with silicon chip, treats that the photoresist material on surface is all removed afterwards taking-up.(remove Cu: Glacial acetic acid, hydrogen peroxide and deionized water are according to the mixed solution of the ratio of 1:1:20 to utilize corrosive fluid; Remove Ti: hydrofluoric acid and deionized water are according to the mixed solution of the volume ratio of 1:60) remove Cu, the Ti alloy Seed Layer of silicon chip surface.Silicon chip is fully cleaned in deionized water, and oven dry.
Step S8 utilizes the manual sliver of scribing pen, obtains sample.Sample is carried out the measurement of magnetic hysteresis loop.
With reference to Fig. 2-Fig. 5, Fig. 2-Fig. 5 is the electron scanning micrograph (10 μ m) of the iron-nickel alloy array surface of use the method for the invention preparation.Can find out that from photo the alloy array of electroplating out has good configuration of surface and homogeneity.Surface height difference is no more than 0.5 μ m.Fig. 2, Fig. 3 can find out that array surface form and homogeneity are all relatively good, and can find out that homogeneity is very good under the high multiple amplification from Fig. 5, and as can be seen from Figure 4 the transverse section of array does not have the slight crack flaw, and electroplating effect is good.
With reference to Fig. 8, Fig. 8 is the EDX of iron-nickel alloy (7:93) array that uses the method for the invention preparation figure as a result.Figure has shown that the iron-nickel alloy ratio is 7:93 as a result.
With reference to Figure 10, Figure 10 is the magnetic test result of the iron-nickel alloy (7:93) of the method for the invention preparation on probation.Can find out that from shape and the coordinate parameters of magnetic hysteresis loop sample presents preferably soft magnetic property.Coercive force is 29.13Oe, and squareness ratio is 0.13, and saturation induction density can reach 1.25T
Embodiment 3:
With reference to Fig. 1, Fig. 1 is the flow chart of steps that the present invention adopts the embodiment of the method for electroplating preparation iron-nickel alloy array, comprises the steps:
Step S1 adopts the method splash-proofing sputtering metal Ti150 of sputter at the silicon chip in (110) crystal orientation of cleaning Metal Cu1500
Figure BDA00002547015400102
Step S2 drips photoresist material at silicon chip surface first, spares in advance glue 60s with the speed of 540r/s first, then carries out the formal even glue 180s of 1500r/s, guarantees that photoresist material evenly is coated with out at silicon chip surface.125s, afterwards taking-up expose under lithography machine.Under 80 ℃, dry by the fire film 210s.Then develop, soak 120s in the developing solution.Guarantee development effect at microscopically.
Step S3 is at first measured the configuration that a certain amount of deionized water carries out electroplate liquid.(introducing the configuration of electroplate liquid here as an example of 1L example).Pour deionized water into tank.Get an amount of medicine with projection electronic weighing and pour tank into.Selecting iron nickel ratio is after the electroplate liquid of 20:80 adds all medicines, tank to be put into 60 ℃ of water-baths, and use glass stick to stir the help agent dissolves.Add magnetic nanoparticle Fe 3O 4, stir electroplate liquid.Candidate agent and magnetic nanoparticle dissolve fully and evenly after, use the PH test paper to measure pH value and can adjust electroplate liquid pH value to 4.0 by adding sodium hydroxide or sulfuric acid.
Step S4, according to the area conversion supply current size that needs on the silicon chip are electroplated figure, supply current=current density * electroplates graphics area.The present invention adopts the current density of 4ASD, so can calculate by electroplating graphics area the size of the supply current that needs setting.Here be assumed to be 80mA.Setting dutycycle is 50%, forward conduction time 1ms, and forward turn-off time 1ms, forward current 2ms, reversible circulation 0 is so just set 0-80mA, dutycycle 50%, the pulsed current of frequency 500Hz.
Step S5, the circuit anode adopts clean nickel block, and negative electrode connects silicon chip.Silicon chip need to clash the convenient conduction of electrode leads to client with acetone.Anode and cathode is put into electroplate liquid connect power supply, check whether supply current is correct.Pass into whipping appts, electroplate liquid is kept evenly.Setting the power turn-on time is 2h, and plugged begins to electroplate.
Step S6 sets 670 ℃ of annealing temperatures, and annealing continues 2h.Cool off with the speed of 100 ℃/h afterwards.
Step S7 is immersed in 1min in the acetone soln with silicon chip, treats that the photoresist material on surface is all removed afterwards taking-up.(remove Cu: Glacial acetic acid, hydrogen peroxide and deionized water are according to the mixed solution of the ratio of 1:1:20 to utilize corrosive fluid; Remove Ti: hydrofluoric acid and deionized water are according to the mixed solution of the volume ratio of 1:60) remove Cu, the Ti alloy Seed Layer of silicon chip surface.Silicon chip is fully cleaned in deionized water, and oven dry.
Step S8 utilizes the manual sliver of scribing pen, obtains sample.Sample is carried out the measurement of magnetic hysteresis loop.
With reference to Fig. 2-Fig. 5, Fig. 2-Fig. 5 is the electron scanning micrograph (10 μ m) of the iron-nickel alloy array surface of use the method for the invention preparation.Can find out that from photo the alloy array of electroplating out has good configuration of surface and homogeneity.Surface height difference is no more than 0.5 μ m.Fig. 2, Fig. 3 can find out that array surface form and homogeneity are all relatively good, and can find out that homogeneity is very good under the high multiple amplification from Fig. 5, and as can be seen from Figure 4 the transverse section of array does not have the slight crack flaw, and electroplating effect is good.
With reference to Fig. 7, Fig. 7 is the EDX of the iron-nickel alloy array that uses the method for the invention preparation figure as a result.Figure has shown that the iron-nickel alloy ratio is 20:80 as a result.
With reference to Fig. 9, Fig. 9 is the magnetic test result of the iron-nickel alloy (20:80) of the method for the invention preparation on probation.Can find out that from shape and the coordinate parameters of magnetic hysteresis loop sample presents preferably soft magnetic property.Coercive force is lower, is 1.345Oe, and squareness ratio is 5.59*10-4, and saturation induction density can reach 1T.
Above-described specific embodiment further describes purpose of the present invention, technical scheme and beneficial effect.Will be appreciated that above said content is the specific embodiment of the present invention only, is not limited to the present invention.All within essence of the present invention and ultimate principle, any modification of making, be equal to replacement, improvement etc., all should be included within protection scope of the present invention.
Although describe in detail about example embodiment and advantage thereof, be to be understood that in the situation of the protection domain that does not break away from the restriction of spirit of the present invention and claims, can carry out various variations, substitutions and modifications to these embodiment.For other examples, when those of ordinary skill in the art should understand easily within keeping protection domain of the present invention, the order of processing step can change.
In addition, range of application of the present invention is not limited to technique, mechanism, manufacturing, material composition, means, method and the step of the specific embodiment of describing in the specification sheets.From disclosure of the present invention, to easily understand as those of ordinary skill in the art, for the technique, mechanism, manufacturing, material composition, means, method or the step that have existed or be about to later on develop at present, wherein they carry out identical function or the identical result of acquisition cardinal principle of corresponding embodiment cardinal principle who describes with the present invention, can use them according to the present invention.Therefore, claims of the present invention are intended to these technique, mechanism, manufacturing, material composition, means, method or step are included in its protection domain.

Claims (10)

1. a method that adopts plating to prepare soft magnetic materials iron-nickel alloy array is characterized in that comprising the steps: in order
(a) sputtering seed layer in the substrate;
(b) thick resist lithography goes out array pattern;
(c) preparation electroplate liquid;
(d) power parameter is set, junction circuit;
(e) adjusting electroplating time and uniform stirring equipment electroplates;
(f) remove photoresist material with acetone;
(g) go Seed Layer with Glacial acetic acid and hydrogen peroxide;
(h) in vacuum chamber, anneal;
(i) soft magnetic performance of test iron-nickel alloy array.
2. method according to claim 1 is characterized in that:
Substrate is silicon chip in the step (a), and Seed Layer is the titanium copper Seed Layer, and wherein titanium thickness 150
Figure FDA00002547015300011
Copper thickness 1500
Figure FDA00002547015300012
3. method according to claim 1 is characterized in that:
The design of array shape display figure and parameter designing in the step (b), array pattern comprises circular array, quadrate array, rectangular array, monoblock is square and monoblock is circular, the photoetching degree of depth is 10-50 μ m; Parameter designing comprises the spacing between array sizes, the array element, and array pattern accounts for the ratio of monoblock figure.
4. method according to claim 1 is characterized in that:
Composition and the concentration of step (c) preparation electroplate liquid comprise: single nickel salt NiSO 46H 2O:187g/L, nickelous chloride NiCl 26H 2O:50g/L, ferrous sulfate FeSO 47H 2O:64g/L, boric acid H 3BO 3: 40g/L, sodium chloride nacl: 20g/L, sodium lauryl sulphate NaC 12H 25SO 4: 0.2g/L, phosphoric acid H 3PO 4: 5g/L, asccharin Saccharin:3.5g/L.
5. method according to claim 4 is characterized in that:
When iron nickel ratio is 7:93, only need to change following two kinds of reagent: single nickel salt NiSO 46H2O:176g/L, ferrous sulfate FeSO 47H2O:18g/L.
6. method according to claim 4 is characterized in that:
When iron nickel ratio is 50:50, only need to change following three kinds of reagent: single nickel salt NiSO 46H 2O:130.9g/L, nickelous chloride NiCl 26H 2O:35g/L, ferrous sulfate FeSO 47H 2O:179.2g/L.
7. method according to claim 1 is characterized in that:
Step (d) power parameter comprises: current density, pulse-repetition, dutycycle, electroplating time, power supply provides pulsed current.
8. method according to claim 1 is characterized in that:
Step (c) is mixed the nano magnetic particle in electroplate liquid, to improve the alloy soft magnetic performance.
9. method according to claim 1 is characterized in that:
Annealing temperature 600-700 ℃ of step (h) reduces internal stress by heat treatment process, promotes the homogeneity of alloy material.
10. soft magnetic materials iron-nickel alloy array is characterized in that: right to use requires the method preparation of one of 1-9, and its thickness is 10-50 μ m, and saturation induction density is more than the 1T.
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CN103866364A (en) * 2014-03-06 2014-06-18 天津大学 Preparation method of iron-nickel alloy magnetic layer on surface of stainless steel fiber
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
CN108732863A (en) * 2018-05-24 2018-11-02 南方科技大学 A kind of flexible nano impression block and preparation method thereof

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