CN105112982A - Magnetic hole substrate for preparing flaky electromagnetic noise suppression material - Google Patents
Magnetic hole substrate for preparing flaky electromagnetic noise suppression material Download PDFInfo
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- CN105112982A CN105112982A CN201510446009.XA CN201510446009A CN105112982A CN 105112982 A CN105112982 A CN 105112982A CN 201510446009 A CN201510446009 A CN 201510446009A CN 105112982 A CN105112982 A CN 105112982A
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Abstract
The invention provides a magnetic hole substrate for preparing a flaky electromagnetic noise suppression material and a preparation method thereof. The magnetic hole substrate comprises an iron substrate and a porous layer on the iron substrate, wherein the porous layer is to coat ferroferric oxide by carbon having nanoscale holes; the aperture is 50-150 nm; and iron magnetic nanowires are deposited in the holes through an electroplating process as the flaky electromagnetic noise suppression material. The preparation method comprises the following steps: firstly, the anodic oxidation treatment is performed for a clean iron chip; then, the iron chip is dipped in gluconic ethanol solution by 8-12 h for drying; and finally, the iron chip is annealed by 2-4 h at a temperature of 400-600 DEG C in an argon atmosphere. A magnetic material is adopted as a hole substrate material to enhance an iron magnetic coupling effect among the magnetic nanowires deposited in the holes; the magnetic hole substrate is excellent in noise absorption performance; the absorption frequency can reach above 10 GHz; the miniaturization and the integration are easy to be realized; and the demands to electromagnetic noise suppression in high-frequency and wide-frequency band ranges can be satisfied.
Description
Technical field
The invention belongs to electronic technology field, relate to high-frequency electromagnetic compatible technique, be specifically related to substrate of a kind of flaky material for the preparation of transmission line electromagnetic noise suppression and preparation method thereof.
Background technology
Along with the widespread use of high-frequency electron device at daily life, industrial circle and the fast development of high integration large-scale integrated circuit, the electromagnetic noise interference between Circuits System and electron device has become day by day serious problem.Practice shows, the electromagnetic noise that the energy waste utilizing magneticsubstance to produce can suppress transmission line to be launched well.In the frequency band of the basic covering signal frequency range of transmission line, when not using magneticsubstance, the noise harmonic wave in signal is very little by its decrement during transmission line.Use the effect of magneticsubstance not to be insertion loss in order to be increased within the scope of signal passband on the transmission line, but retardance suppresses electromagnetic noise harmonic wave, namely those are higher than the harmonic frequency of meaningful signal frequency.
The principle of work that transmission line electromagnetic noise suppresses is: high-frequency signal will make high-frequency electromagnetic signal decay due to magnetic loss (comprising ferromagnetic resonance absorption loss and high frequency eddy current losses) by during transmission line, and the signal frequency be attenuated and frequency span are subject to characteristic and the size control of magneticthin film.In magnetic loss, ferromagnetic loss is determined by the magnetic loss factor of the specific magnetising moment of magneticthin film, anisotropy, demagnetizing field and magneticthin film, and eddy-current loss then determines primarily of the resistivity of magneticthin film, and the width of working band is determined by ferromagnetic resonance line width.The magneticsubstance majority suppressed for high frequency electromagnetic noise is the compounded noise suppression sheet such as ferrimag and polymkeric substance.Ferrimag film meets the requirement of electronic devices and components developing direction and electromagnetic noise suppression because of its thickness I, can be created on a certain special element of integrated electronic system, also can generate in whole integrated electronic system; And for different service requirementss, film performance can be adjusted by change magneticthin film composition or preparation technology, thus meets controlling consumption of electromagnetic noise.Such electromagnetic noise suppression material is owing to adopting its resistivity of metallicl magnetic material lower, and its anisotropy is little, and ferromagnetic resonance frequency is low, and the blanketing frequency of electromagnetic noise, between MHz ~ GHz, is a kind of good electromagnetic noise suppression material.
The operating frequency of modern electronic devices and equipment is more and more higher, therefore needs the electromagnetic noise suppression material that can work in higher frequency (such as 10GHz).At present, electromagnetic noise suppression material adopts electroplating technology to be deposited in hole template mostly, electroplating technology is adopted to have high magnetic resonance frequency at the ferromagnetic nano wire battle array material of the upper deposition of hole template (such as polycarbonate template PC or alumina formwork AAO) and have wideband absorptive character, sourdine based on ferromagnetic nano wire battle array has good noise absorbent performance, absorption frequency can reach more than 20GHz, and easily realizes microminiaturization, integrated.But, due to the hole template that electromagnetic noise suppression material adopts, if polycarbonate template and alumina formwork are non magnetic template, reduce the ferromagnetic coupling effect between the magnetic nanometer that is plated in its hole, reduce the magnetic permeability of material, limit the raising of its squelch performance.
Summary of the invention
The present invention is directed to the defect that background technology exists, propose a kind of magnetic hole substrate for the preparation of sheet electromagnetic noise suppression material and preparation method thereof.Hole in magnetic hole substrate of the present invention is by magnetic oxide---Z 250 (Fe
3o
4) formed, the present invention adopts magneticsubstance as hole substrate material, enhance the ferromagnetic coupling effect between the magnetic nanometer that is deposited in hole, enhance the magnetic permeability of material, if this magnetic nanometer is used for electromagnetic noise suppression, compare the ferromagnetic nano wire battle array in non magnetic hole template, its squelch performance can improve greatly; In addition, due to Fe
3o
4in containing divalence and ferric ion, enhance electronics and move, thus can increase described based on the eddy-current loss in the electromagnetic noise suppression material of ferromagnetic nano wire battle array, improve the electromagnetic noise suppression performance of material further; The electromagnetic noise suppression material being deposited on hole of the present invention on-chip ferromagnetic nano wire battle array has better noise absorbent performance, absorption frequency can reach more than 10GHz, and easily realize microminiaturization, integrated, the demand to electromagnetic noise suppression in high frequency, broad frequency range can be met.
Technical scheme of the present invention is as follows:
A kind of magnetic hole substrate for the preparation of sheet electromagnetic noise suppression material, comprise at the bottom of iron-based and the suprabasil porous layer of iron, described porous layer is the carbon coated ferriferrous oxide with nano level hole, described hole diameter is 50 ~ 150nm, by electroplating technology in described hole deposited iron magnetic nanowires as sheet electromagnetic noise suppression material.
A kind of preparation method of the magnetic hole substrate for the preparation of sheet electromagnetic noise suppression material, first under constant voltage, adopted by the iron plate cleaned up two-probe method to carry out anodic oxidation treatment, then in the ethanolic soln of glucose, 8 ~ 12h is soaked, dry, finally 400 ~ 600 DEG C of annealing 2 ~ 4h in argon gas atmosphere, obtain described magnetic hole substrate.
For the preparation of a preparation method for the magnetic hole substrate of sheet electromagnetic noise suppression material, specifically comprise the following steps:
Step 1: iron plate is cleaned successively in acetone, ethanol and deionized water, dries;
Step 2: the NH adding the 0.5wt% being equivalent to quality of glycol in ethylene glycol
4the deionized water preparation of F and 3wt% obtains electrolytic solution; Then the iron plate that step 1 cleans up is placed in the electrolytic solution of above-mentioned preparation, under constant voltage, adopts two electrodes to carry out anodic oxidation treatment, form the pertusate amorphous ferric oxide of tool on iron plate surface; The condition of described anodic oxidation treatment: temperature is 60 DEG C, oxidization time is 300s, oxidation voltage 30 ~ 90V;
Step 3: the iron plate of the surface band hole ferric oxide obtained after step 2 being processed soaks 8 ~ 12h in the ethanolic soln of glucose, forms the coated ferric oxide of hole carbon on iron plate surface; The solvent of the ethanolic soln of described glucose is ethanol and deionized water, and solute is glucose, and the volume ratio of described ethanol and deionized water is 2:8, and the concentration of described glucose solute is 3mol/L;
Step 4: the iron plate of the coated ferric oxide of surface band hole carbon step 3 obtained dries 1 ~ 3h at 80 ~ 120 DEG C; Then 400 ~ 600 DEG C of annealing 2 ~ 4h in argon gas atmosphere, form hole carbon coated ferriferrous oxide at iron surface, namely obtain magnetic hole substrate of the present invention.
Beneficial effect of the present invention is: compare non-magnetic hole substrate, and magnetic hole substrate provided by the invention is prepared sheet electromagnetic noise suppression material tool and had the following advantages:
1, hole magnetic substrate provided by the invention is metallicl magnetic material iron and hole magnetic oxide Fe
3o
4complex body, and hole magnetic oxide Fe
3o
4also have passed through the coated process of carbon, add its electroconductibility, like this, when the later stage, ferromagnetic nano wire was prepared in plating, without the need to electrode layer need be prepared by sputtering technology as in non-magnetic hole polycarbonate template or alumina formwork, simplify preparation technology, reduce preparation cost.
2, the component of magnetic hole substrate of the present invention is magnetic oxide---Z 250 (Fe
3o
4), the present invention adopts magneticsubstance as hole mould material, enhance the ferromagnetic coupling effect between the magnetic nanometer that is deposited in hole, the magnetic permeability of electromagnetic noise suppression material can be strengthened, if this magnetic nanometer is used for electromagnetic noise suppression, compare the ferromagnetic nano wire battle array in non magnetic hole template, its squelch performance can improve greatly; In addition, due to Fe
3o
4in containing divalence and ferric ion, enhance electronics and move, thus can increase described based on the eddy-current loss in the electromagnetic noise suppression material of ferromagnetic nano wire battle array, improve the electromagnetic noise suppression performance of material further; The electromagnetic noise suppression material being deposited on hole of the present invention on-chip ferromagnetic nano wire battle array has better noise absorbent performance, absorption frequency can reach more than 10GHz, and easily realize microminiaturization, integrated, the demand to electromagnetic noise suppression in high frequency, broad frequency range can be met.
Accompanying drawing explanation
Fig. 1 is the process flow sheet of preparation magnetic hole substrate provided by the invention;
Fig. 2 be the hole substrate of carbon coated and non-carbon coated annealed after XRD figure spectrum, wherein, (a) be the hole substrate of non-carbon coated annealed after XRD figure compose; XRD figure spectrum after b hole substrate that () is carbon coated is annealed;
Fig. 3 is the SEM figure of the magnetic hole substrate surface that the embodiment of the present invention 1 obtains.
Embodiment
For the preparation of a preparation method for the magnetic hole substrate of sheet electromagnetic noise suppression material, its technical process as shown in Figure 1, specifically comprises the following steps:
Step 1: be 0.2mm by thickness, purity is iron plate each ultrasonic cleaning 10min in acetone, ethanol and deionized water successively of 99.9%, naturally dries;
Step 2: the iron plate after step 1 being cleaned adopts two-probe method to carry out anodic oxidation treatment under constant voltage condition, forms the amorphous ferric oxide of hole on iron plate surface; The electrolytic solution that described anodic oxidation adopts is: purity be 99.5% ethylene glycol solution, purity be 96% ammonium fluoride and resistivity be greater than the mixed solution of the deionized water composition of 18.2M Ω .cm; The compound method of electrolytic solution is: the resistivity of the ammonium fluoride (96% purity) adding the 0.5wt% being equivalent to ethylene glycol solution quality in ethylene glycol solution (99.5% purity) successively and the 3wt% being equivalent to ethylene glycol solution quality is greater than the deionized water of 18.2M Ω .cm, mix, obtain electrolytic solution; Described anodised condition: temperature is 60 DEG C, oxidization time is 300s, and oxidation voltage is 30 ~ 90V;
Step 3: surface step 2 obtained is that the iron plate of the amorphous ferric oxide of hole soaks 8 ~ 12h in the aqueous ethanolic solution of glucose, forms the coated ferric oxide of hole carbon on iron plate surface; The compound method of the aqueous ethanolic solution of described glucose is: the glucose adding 0.3mol in every 100mL aqueous ethanolic solution, and described 100mL aqueous ethanolic solution is that 80mL deionized water and 20mL ethanol are mixed to get;
Step 4: surface step 3 obtained is iron plate 80 ~ 120 DEG C of baking 1 ~ 3h in vacuum drying oven of the coated ferric oxide of hole carbon; Then anneal at 400 ~ 600 DEG C of temperature 2 ~ 4h in argon gas (Ar) atmosphere, forms hole carbon coated ferriferrous oxide, namely obtain magnetic hole substrate of the present invention at iron surface.
The preparation method of a kind of magnetic hole substrate for the preparation of sheet electromagnetic noise suppression material provided by the invention, on the adjustment formula of electrolytic solution and the basis of anode oxidation process (temperature, oxidization time), the size of iron plate surface apertures can be adjusted by oxidation voltage.
Embodiment 1
For the preparation of a preparation method for the magnetic hole substrate of sheet electromagnetic noise suppression material, specifically comprise the following steps:
Step 1: be 0.2mm by thickness, purity be 99.9% iron plate each ultrasonic cleaning 10 minutes in acetone, dehydrated alcohol and deionized water successively, take out nature and dry;
Step 2: the resistivity of the ammonium fluoride (96% purity) adding the 0.5wt% being equivalent to quality of glycol in ethylene glycol (99.5% purity) successively and the 3wt% being equivalent to quality of glycol is greater than the deionized water of 18.2M Ω .cm, mix, preparation obtains anodised electrolytic solution;
Step 3: the glucose adding 0.3mol in 100mL aqueous ethanolic solution (80mL deionized water and the mixing of 20mL ethanol), preparation obtains carbon covering liquid;
Step 4: the iron plate after step 1 being cleaned adopts two-probe method to carry out anodic oxidation treatment under constant voltage condition: using the iron plate after step 1 is cleaned as anode, platinum electrode is parallel with iron plate staggered relatively as negative electrode, composition electrode system, the distance between negative electrode and anode is 2.5cm; Then the electrode system that the iron plate assembled and platinized platinum form is put into the electrolytic solution that step 2 is prepared, oxidation voltage is adjusted to 60V, temperature of reaction controls at 60 DEG C, through the anodic oxidation treatment of 300 seconds, obtains the complex body of iron and the amorphous ferric oxide of hole;
Step 5: soak 12h in the carbon covering liquid that the complex body of iron step 4 obtained and the amorphous ferric oxide of hole is prepared in step 3, form the complex body of iron and the coated amorphous ferric oxide of hole carbon;
Step 6: complex body 100 DEG C of baking 1h in vacuum drying oven of the iron that step 5 is obtained and the coated amorphous ferric oxide of hole carbon; Then 500 DEG C of annealing 3 hours in argon gas (Ar) atmosphere, forms hole carbon coated ferriferrous oxide at iron surface, namely obtains magnetic hole substrate of the present invention.
In order to verify the magnetic substrate adopting the inventive method can obtain hole carbon coated ferriferrous oxide, the sample obtained through step 1-4 directly being carried out step 6 and processes, the sample A obtained; Compare with the sample B obtained through entire protocol 1-6.To the diffractogram that sample A and sample B obtains as shown in Figure 2 through X-ray diffractometer (XRD) analysis.As can be known from Fig. 2, what formed through the sample B of entire protocol 1-6 is Z 250 phase, and the sample A lacking step 5 is formed is ferric oxide phase.
Fig. 3 is the surface topography map of the magnetic hole substrate that the embodiment of the present invention 1 obtains; As shown in Figure 3, embodiment 1 successfully prepares magnetic hole substrate, and iron plate surface is the hole formed by carbon coated ferriferrous oxide, and the aperture of described hole is about 100nm.
In order to verify magnetic hole substrate deposition magnetic nanometer that the present invention the obtains performance as electromagnetic noise suppression material.The magnetic hole substrate obtained in the present invention, the hole Al with same thickness and hole size
2o
3template splash-proofing sputtering metal layers of copper, as after electrode, under same electroplating technology, deposits pure cobalt nanowire, then adopts the test of standard electric magnetic noise rejection testing method.Test result is as follows: its loss of noise sheet adopting hole magnetic substrate of the present invention to prepare reaches maximum close to 88% at 22 ~ 27GHz, and adopts hole Al
2o
3it is then nearly 70% that its loss of noise sheet of Template preparation reaches maximum at 22 ~ 27GHz, and its drain performance increases nearly 25%.
Embodiment 2
Being distinguished as of the present embodiment and embodiment 1: the oxidation voltage in step 4 is 30V, and all the other steps are identical with embodiment 1.
After tested, the aperture of magnetic hole substrate surface hole that embodiment 2 obtains is about 50nm.
Embodiment 3
Being distinguished as of the present embodiment and embodiment 1: the oxidation voltage in step 4 is 50V, and all the other steps are identical with embodiment 1.
After tested, the aperture of magnetic hole substrate surface hole that embodiment 3 obtains is about 80nm.
Embodiment 4
Being distinguished as of the present embodiment and embodiment 1: the oxidation voltage in step 4 is 90V, and all the other steps are identical with embodiment 1.
After tested, the aperture of magnetic hole substrate surface hole that embodiment 4 obtains is about 125nm.
Claims (3)
1., for the preparation of a magnetic hole substrate for sheet electromagnetic noise suppression material, comprise at the bottom of iron-based and the suprabasil porous layer of iron, described porous layer is the carbon coated ferriferrous oxide with nano level hole, and described hole diameter is 50 ~ 150nm.
2. the preparation method for the preparation of the magnetic hole substrate of sheet electromagnetic noise suppression material, first under constant voltage, adopted by the iron plate cleaned up two-probe method to carry out anodic oxidation treatment, then in the ethanolic soln of glucose, 8 ~ 12h is soaked, dry, finally 400 ~ 600 DEG C of annealing 2 ~ 4h in argon gas atmosphere, obtain described magnetic hole substrate.
3., for the preparation of a preparation method for the magnetic hole substrate of sheet electromagnetic noise suppression material, specifically comprise the following steps:
Step 1: iron plate is cleaned successively in acetone, ethanol and deionized water, dries;
Step 2: the NH adding the 0.5wt% being equivalent to quality of glycol in ethylene glycol
4the deionized water preparation of F and 3wt% obtains electrolytic solution; Then the iron plate that step 1 cleans up is placed in the electrolytic solution of above-mentioned preparation, under constant voltage, adopts two electrodes to carry out anodic oxidation treatment, form the pertusate amorphous ferric oxide of tool on iron plate surface; The condition of described anodic oxidation treatment: temperature is 60 DEG C, oxidization time is 300s, oxidation voltage 30 ~ 90V;
Step 3: the iron plate of the surface band hole ferric oxide obtained after step 2 being processed soaks 8 ~ 12h in the ethanolic soln of glucose, forms the coated ferric oxide of hole carbon on iron plate surface; The solvent of the ethanolic soln of described glucose is ethanol and deionized water, and solute is glucose, and the volume ratio of described ethanol and deionized water is 2:8, and the concentration of described glucose solute is 3mol/L;
Step 4: the iron plate of the coated ferric oxide of surface band hole carbon step 3 obtained dries 1 ~ 3h at 80 ~ 120 DEG C; Then 400 ~ 600 DEG C of annealing 2 ~ 4h in argon gas atmosphere, form hole carbon coated ferriferrous oxide at iron surface, namely obtain magnetic hole substrate of the present invention.
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-
2015
- 2015-07-27 CN CN201510446009.XA patent/CN105112982B/en not_active Expired - Fee Related
Patent Citations (6)
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| JP2006291256A (en) * | 2005-04-07 | 2006-10-26 | Jfe Steel Kk | Method for manufacturing black steel sheet superior in electromagnetic-wave-shielding property and corrosion resistance |
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| L.HUANG ET AL: "Carbon innercoated ordered porous TiO2 as anode materials for lithium-ion batteries", 《IONICS》 * |
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