CN104008844B - Fabrication method of soft magnetic alloy materials - Google Patents
Fabrication method of soft magnetic alloy materials Download PDFInfo
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Abstract
The invention relates to a fabrication method of soft magnetic alloy materials. The fabrication method includes flattening, drying and annealing, and post-treating. The surface of soft magnetic alloy powder is provided with a metal oxide film, so that magnetic loss of the powder is reduced on the premise of not reducing magnetic conductivity of the powder and magnetic performance of the powder is improved. The fabrication method is simple, low in cost, and suitable for large-scale batch production; the soft magnetic alloy materials fabricated can meet the high requirements for high saturation flux density, high magnetic conductivity, low iron loss, high strength and high productivity.
Description
Technical field
The present invention relates to the production method of soft magnetic materials, more particularly to a kind of raising magnetic resistivity is so as to improving magnetic
The preparation processing method of the magnetically soft alloy material of magnetic property.
Background technology
At present, increasingly it is used widely using the contactless IC tag of RFID technique.IC tag receives and dispatches day from read/write
Line sends the electromagnetic wave of preset frequency to aerial coil, thus activates IC tag, then the instruction according to contained by electromagnetic wave, reads
Or the information in write IC chip.
However, with the trend toward miniaturization of electronic equipment, IC tag is equidistant with metallic plate shorter and shorter, due to vortex electricity
Stream and impact of the metal to reflection of electromagnetic wave, the reading/writing distance of IC tag significantly shortens.Insert between label and metallic plate soft
After magnetic alloy composite magnetic sheet, the reading/writing distance that can effectively alleviate the problems referred to above initiation shortens.
In high band(13.56MHz)Under, the main magnetic loss of magnetic piece is the magnetic hystersis loss that magnetic hysteresis current strap is come.And be
Reduction magnetic hystersis loss, the resistivity for improving alloy material is an effective method.After resistivity of material is improved, magnetic hysteresis electric current
Can reduce, so as to reach the purpose for reducing magnetic loss.
Field is manufactured in magnetically soft alloy powder core, alloy magnetic powder resistivity is improved mainly by megohmite insulant and alloy magnetic
Powder mixes to isolate alloy powder, it is to avoid soft-magnetic alloy powder is connected with each other causes loss height, magnetic conductivity fast with frequency increase
Speed declines.Because megohmite insulant itself is without magnetic, therefore the comparision contents of general megohmite insulant are moderate, and usually more than 1%,
Less than 5%.If insulant quality is very little, it is difficult to reach insulation effect;If amount is excessive, powder core magnetic conductivity is caused to lower,
Volume increases.That is, at present powder core prepares addition megohmite insulant, the loss problem of magnetic conductivity is caused to a certain extent;
And due to the restriction of addition, cause insulation to be difficult to sufficient problem to a certain extent, it is difficult to reach lower asking so as to be lost
Topic.
Chinese patent publication No. CN103045943A, date of publication on April 17th, 2013, a kind of entitled anticorrosion soft mag
The smelting process of material, this application case discloses a kind of smelting process of anticorrosion soft mag material, to intermediate frequency furnace or vacuum sense
Answering the ingot casting of the equipment melting such as stove carries out electric slag refusion and smelting, so as to obtain the hot-working blank of high-quality, the slag charge of electroslag remelting
Fill a prescription and be:Calcirm-fluoride:Calcium oxide:Aluminum oxide=65-80:1-5:15-25, using the packing ratio of 0.5-0.6 during remelting.It is not enough
Part is, although the method increase the performance of processability and material, but magnetic piece prepared by the material exists
Under high band, magnetic hystersis loss is serious.
The content of the invention
It is an object of the invention under in order to solve existing high band, the higher defect of the magnetic hystersis loss of magnetic piece and provide
It is a kind of to improve magnetic resistivity so as to improve the preparation processing method of the magnetically soft alloy material of the magnetic property of magnetic.
To achieve these goals, the present invention is employed the following technical solutions:
A kind of preparation processing method of magnetically soft alloy material, the preparation method comprises the steps:
a)Flattening:Magnetically soft alloy material is ground with organic solvent and auxiliary agent, milling time is 2-15 hours, is ground
Filter after the completion of mill, take filter residue standby;Wherein, the mass ratio of magnetically soft alloy material, organic solvent and abrasive media is:1:0.6-
1:5-8;
b)Drying and annealing:By step a)Filter residue and drying 5-12 hour after filtration, is subsequently placed in the kiln of adjustable atmosphere
It is interior, made annealing treatment in protective gas atmosphere, annealing temperature is 400-650 DEG C, annealing time 0.5-2 hours;In temperature
After reaching annealing temperature, weak oxide gas is passed through into kiln carries out oxidation processes, and oxidation treatment time is 5-30min;
c)Post processing:After oxidation processes terminate, protective gas is passed through, continues to be incubated 25-47min, then along with the furnace cooling, system
Obtain the magnetically soft alloy magnetic of high resistivity.
In the technical program, magnetically soft alloy material is carried out into flaky process primarily to improving magnetic conductivity, soft magnetism
Alloy material diminishes through grinding thickness, by the D0 in material3Superstructure is changed into the phase structure of α-Fe, the crystalline size of material
Reduce, so that the magnetic conductivity of the magnetically soft alloy material of unit mass is improved;And grind after made annealing treatment, be in order to
So that D03Superstructure is reappeared, and degree of order ratio is higher without the material of milled processed, can effectively improve magnetically soft alloy material
Saturation magnetization, while reduce coercivity;Weak oxide gas is passed through during annealing, is in order in soft magnetism
Alloy material surface produces layer of oxide layer, so as to improve the resistivity of material, because surface has a floor height resistivity, cladding
Sufficient metal oxide thin deielectric-coating, so while possessing low magnetic loss, magnetic conductivity declines less.
Preferably, the magnetically soft alloy material is iron sial, iron nickel molybdenum, iron silicochromium, iron silicon, iron tantnickel and with the addition of
One or more in phosphorus or boron doped above-mentioned alloy material, organic solvent is in ethanol, acetone, toluene, dimethylbenzene
Plant or several, auxiliary agent is coupling agent and CNT or the mixture of Graphene.In the technical program, CNT or graphite
The addition of alkene so that further increase magnetic conductivity.
Preferably, 0-0.8% of the addition of auxiliary agent for magnetically soft alloy material quality, coupling agent and CNT or stone
The mass ratio of black alkene is 1:0.01-0.05.
Preferably, step b)In the weak oxide gas that is passed through for air, vapor, vapor and air gaseous mixture
One kind in body.
Preferably, weak oxide gas accounts for the 4-20% of protective gas volume, at normal temperatures relative humidity is vapor
95-100%。
Preferably, the temperature of filter residue and drying is 50-80 DEG C.
Preferably, the mass ratio of magnetically soft alloy material, organic solvent and abrasive media is:1:0.6-0.7:5-6.At this
In technical scheme, solvent ratios are too high and the too low treatment effeciency that can all reduce flattening of abrasive media ratio, and solvent ratios
Too low and abrasive media ratio is too high so that the control of flattening magnetically soft alloy magnetic pattern is relatively difficult.
Preferably, weak oxide gas accounts for the 4-10% of protective gas volume.
Preferably, step a)The equipment of middle grinding is in sand mill, ball mill, rod mill, machinery mill, planetary mills
Kind.
Preferably, magnetically soft alloy material thickness≤1 micron obtained after flaky process, average diameter is that 30-50 is micro-
Rice.
The invention has the beneficial effects as follows:
1)The present invention is not by magnetically soft alloy magnetic surface production metal-oxide film, reducing magnetic magnetic conductivity
Under the premise of reduce magnetic magnetic loss, so as to improve the magnetic property of magnetic;
2)The preparation method of the present invention is simple, with low cost, is adapted to large-scale batch production;
3)Magnetically soft alloy material prepared by the present invention can at a high level meet high saturation magnetic flux density, high magnetic permeability, low
Iron loss, high intensity and large-duty demand.
Specific embodiment
Below by way of specific embodiment, the present invention will be further explained:
In the present invention, if not refering in particular to, the raw material for being adopted is commercially available or commonly used in the art, following enforcements
Method in example, if no special instructions, is the conventional method of this area.
Embodiment 1
A kind of preparation processing method of magnetically soft alloy material, the preparation method comprises the steps:
a)Flattening:Weigh 500 grams of FeSiAl magnetics to be put in planet grinding jar, the inside there are 3000 grams of Φ 5.6mm carbon steel
Ball, adds 300 grams of absolute ethyl alcohols, stirs 3 hours in the case where rotating speed is 30Hz;
b)Drying and annealing:After stirring terminates, organic solvent is filtered to remove, then filter residue is put into baking oven and is dried at 80 DEG C;
Drying time is 12 hours, and dried filter residue is put in tube furnace, and 550 DEG C are warming up under nitrogen protection, and in furnace temperature 5 are stablized
After minute, air is mixed into, air accounts for 10% of nitrogen volume in stove, maintains 30 minutes;
c)Post processing:Then atmosphere is reverted to into full nitrogen protection, then is incubated 25 minutes;Anneal after terminating in nitrogen atmosphere
Allow tube furnace along with the furnace cooling under protection.So as to prepare the magnetically soft alloy magnetic of high resistivity.
Embodiment 2:
Weigh 500 grams of FeSiCr magnetics to be put in planet grinding jar, the inside there are 2500 grams of Φ 5.6mm and Φ 3.1mm ratios to be
1:1 carbon steel ball, adds 350 grams of acetone and auxiliary agent, and auxiliary agent is 0.495 gram of titanate coupling agent and 0.005 gram of CNT
Mixture, rotating speed be 30Hz under stir 3 hours, stirring terminate after, most of organic solvent is filtered to remove, then by filter residue
It is put into baking oven to be dried at 60 DEG C, drying time is 5 hours, and dried filter residue is put in tube furnace, is risen under nitrogen protection
Temperature after furnace temperature stablizes 5 minutes, is passed through the vapor of steam evaporator generation to 600 DEG C, controls mixed gas normal temperature phase pair
Humidity is 100%, and duration of ventilation is 10 minutes, then atmosphere is reverted to into full nitrogen protection, then is incubated 47 minutes, and annealing terminates
Tube furnace along with the furnace cooling is allowed under nitrogen atmosphere protection afterwards, so as to prepare the magnetically soft alloy magnetic of high resistivity.
Embodiment 3:
Weigh 1000 grams of FeNiMo magnetics to be put in sand mill, it is 1 that the inside there are 8000 grams of Φ 5.6mm and Φ 3.1mm ratios:
1 carbon steel ball, adds 700 grams of absolute ethyl alcohols, stirs 15 hours in the case where rotating speed is for 150 revs/min, after stirring terminates, crosses and filters
Most of organic solvent is removed, then filter residue is put into baking oven and is dried 8 hours at 80 DEG C, and dried filter residue is put in clock hood type furnace,
500 DEG C are warming up under nitrogen protection, after furnace temperature stablizes 5 minutes, are passed through the vapor and air of steam evaporator generation,
It is 95% to control mixed gas normal temperature relative humidity, and volume of air ratio is 4%, and duration of ventilation is 10 minutes, then recovers atmosphere
For the protection of full nitrogen, then 45 minutes are incubated, annealing allows tube furnace along with the furnace cooling under nitrogen atmosphere protection after terminating, so as to prepare
Obtain the magnetically soft alloy magnetic of high resistivity.
Embodiment 4:
Weigh 300 grams of FeSi magnetics to be put in planet grinding jar, there is the zirconium ball of 1500 grams of Φ 5.6mm the inside, add 200 gram third
Ketone and auxiliary agent, auxiliary agent is 2.427 grams of titanate coupling agent and 0.073 gram of Graphene, and in the case where rotating speed is 30Hz, stirring 2.5 is little
When, after stirring terminates, most of organic solvent is filtered to remove, then filter residue is put into baking oven and is dried at 60 DEG C, and drying time is 4
Hour, dried filter residue is put in tube furnace, and 400 DEG C are warming up under nitrogen protection, after furnace temperature stablizes 5 minutes, is passed through
Vapor and air that steam evaporator is generated, it is 100% to control mixed gas oxygen concentration for normal temperature relative humidity, air
Volume ratio is 15%, and duration of ventilation is 8 minutes, then atmosphere is reverted to into full nitrogen protection, then is incubated 47 minutes, and annealing terminates
Tube furnace along with the furnace cooling is allowed under nitrogen atmosphere protection afterwards, so as to prepare the magnetically soft alloy magnetic of high resistivity.
Embodiment 5:
Weigh 300 grams of FeSiNi magnetics to be put in rod milling tank, there is the rod iron of 2400 grams of Φ 5mm the inside, add 200 grams of toluene
And auxiliary agent, auxiliary agent is 3.7 grams of titanate coupling agent and 0.3 gram of CNT, is stirred 10 hours in the case where rotating speed is 30Hz, is stirred
After mixing end, filter and remove most of organic solvent, then filter residue is put into baking oven and is dried at 60 DEG C, drying time is 4 hours,
Dried feed is put in tube furnace, and 450 DEG C are warming up under nitrogen protection, after furnace temperature stablizes 5 minutes, is passed through air, air body
Than being 20%, duration of ventilation is 25 minutes to product, then atmosphere is reverted to into full nitrogen protection, then is incubated 40 minutes, after annealing terminates
Tube furnace along with the furnace cooling is allowed under nitrogen atmosphere protection, so as to prepare the magnetically soft alloy magnetic of high resistivity.
Embodiment 6:
Weigh 150 grams of FeSiAl and 150 gram of FeNiMo magnetics to be put in planet grinding jar, the inside has 1500 grams of Φ 5.6mm's
Carbon steel ball, adds 240 grams of dimethylbenzene, stirs 2 hours in the case where rotating speed is 30Hz, and after stirring terminates, being filtered to remove major part has
Machine solvent, then filter residue be put into baking oven at 50 DEG C be dried 6 hours, dried feed is put in tube furnace, is heated up under nitrogen protection
To 580 DEG C, after furnace temperature stablizes 5 minutes, the vapor and air of steam evaporator generation are passed through, control mixed gas oxygen
It is 100% that concentration is normal temperature relative humidity, and volume of air ratio is 10%, and duration of ventilation is 10 minutes, then reverts to atmosphere entirely
Nitrogen is protected, then is incubated 45 minutes, and annealing allows tube furnace along with the furnace cooling under nitrogen atmosphere protection after terminating, so as to prepare
The magnetically soft alloy magnetic of high resistivity.
Comparative example 1:
Weigh 500 grams of FeSiAl magnetics to be put in planet grinding jar, the inside there are 3000 grams of Φ 5.6mm carbon steel balls, add 300
Gram absolute ethyl alcohol, stirs 2 hours in the case where rotating speed is 30Hz, after stirring terminates, by screen cloth most of organic solvent is tentatively removed,
It is then placed in baking oven to be dried at 80 DEG C, drying time is 12 hours, and dried feed is put in tube furnace, is heated up under nitrogen protection
To 550 DEG C, 1 hour is incubated, insulation allows tube furnace along with the furnace cooling after terminating under nitrogen atmosphere protection.
Magnetically soft alloy magnetic and 10% aqueous polyurethane prepared by embodiment 1-6 and comparative example 1 is diluted using ethanol, and is added
Enter titante coupling agent(The 1% of magnetic quality)With deaeration agent(Add the 0.1% of ethanol volume), the stirring mixing in mixer
15 minutes, then the wet film that thickness is 0.3mm is coated on PET basement membranes with spreader, be put into baking oven dry at 80 DEG C 5 hours with
Organic solvent is removed, after peeling off above-mentioned institute's made membrane, 5 film stacks are added carries out hot-pressing processing, and pressure is 15MPa, and the time is same
For 2 minutes, temperature was 150 DEG C.The magnetic sheet that hot-pressing processing is obtained carries out rushing ring, and the size of ring is Φ 14X Φ 8.5mm, Ran Houyong
Agilent 4991A materials/electric impedance analyzer is tested, and obtains complex permeability at 13.56 mhz.
Table 1, embodiment 1-6 and comparative example 1 prepare the magnetic conductivity of magnetic sheet
Sequence number | μ′ | μ″ | Q | μ′Q |
Embodiment 1 | 47.8 | 1.3 | 36.8 | 1759 |
Embodiment 2 | 50.3 | 0.87 | 57.8 | 2908 |
Embodiment 3 | 72.3 | 2.5 | 28.9 | 2091 |
Embodiment 4 | 42.3 | 0.81 | 52.2 | 2208 |
Embodiment 5 | 51.6 | 1.5 | 34.4 | 1775 |
Embodiment 6 | 57.9 | 1.4 | 41.4 | 2397 |
Comparative example 1 | 52.4 | 4.2 | 12.5 | 655 |
Q(μ′/μ″)Quality factor:The magnetic loss of the higher explanation material of its value is less.μ′Q:Affect RFID tag application magnetic sheet
Reading/writing distance afterwards.
The present invention by magnetically soft alloy magnetic surface production metal-oxide film, before magnetic magnetic conductivity is not reduced
Putting reduces the magnetic loss of magnetic, so as to improve the magnetic property of magnetic.
Embodiment described above is a kind of preferred version of the present invention, and any pro forma limit is not made to the present invention
System, also has other variants and remodeling on the premise of without departing from the technical scheme described in claim.
Claims (1)
1. the preparation processing method of a kind of magnetically soft alloy material, it is characterised in that prepare processing method and comprise the following steps:Weigh
500 grams of FeSiCr magnetics are put in planet grinding jar, and it is 1 that there are 2500 grams of Φ 5.6mm and Φ 3.1mm ratios the inside:1 carbon steel
Ball, adds 350 grams of acetone and auxiliary agent, and auxiliary agent is the mixture of 0.495 gram of titanate coupling agent and 0.005 gram of CNT,
Rotating speed is to stir 3 hours under 30Hz, after stirring terminates, is filtered to remove most of organic solvent, then filter residue is put into into baking oven and is existed
It is dried at 60 DEG C, drying time is 5 hours, and dried filter residue is put in tube furnace, and 600 DEG C are warming up under nitrogen protection,
After furnace temperature stablizes 5 minutes, the vapor of steam evaporator generation is passed through, controlling mixed gas normal temperature relative humidity is
100%, duration of ventilation is 10 minutes, then atmosphere is reverted to into full nitrogen protection, then is incubated 47 minutes, is annealed after terminating in nitrogen
Tube furnace along with the furnace cooling is allowed under gas atmosphere protection, so as to prepare the magnetically soft alloy magnetic of high resistivity.
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