CN103350225B - The method that magnetic metallic powder rolls flattening - Google Patents
The method that magnetic metallic powder rolls flattening Download PDFInfo
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- CN103350225B CN103350225B CN201310242962.3A CN201310242962A CN103350225B CN 103350225 B CN103350225 B CN 103350225B CN 201310242962 A CN201310242962 A CN 201310242962A CN 103350225 B CN103350225 B CN 103350225B
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Abstract
A kind of method of magnetic metallic powder calendering flattening, the calendering flattening method are：The magnetic metallic powder of preliminary flattening is made in the presence of the grinding pressure of roller rod, shearing force by the method for rod milling, extruding mutually, powder is forced plastic deformation occur, the size of its thickness direction reduces because being squeezed, shearing, and particle is forced to the extension of length and width direction；The overlapping placement multilayer roller rod in rod milling cylinder, when mill tube inwall rotates, under the double action of gravity and frictional force, drives each layer roller rod to rotate successively, is formed to the rolling of magnetic metallic powder, sheared, so as to realize the method rolled to powder.Beneficial effect：The present invention is by the way of rolling, roll, the power that roller rod applies to powder only has grinding pressure and shearing force, rather than impact, either grinding pressure, or shearing force, there is calendering effect to powder, group movement and the impingement phenomenon appearance being similar in high energy ball mill can be avoided, improve the ratio and production efficiency of powder flattening.
Description
Technical field
The present invention relates to a kind of method of magnetic metallic powder calendering flattening processing, the flakey metal of this method manufacture
Soft magnetism micro mist is mainly used in making the magnetic material that flexible electromagnetic interference wave absorbs magnetic sheet, and the flexible magnetic sheet is preferably used in RFID
(radio frequency identification：Radio Frequency Identification) technology electronic tag and EMC (electromagnetic compatibilities:
Electromagnetic Compatibility or EMI are electromagnetism interference:Electromagnetic
) etc. Interference used in.
Background technology
In recent years, Internet of Things upsurge has been started in the whole world.Internet of Things is emerging high-tech industry, is the new of World Economics
Growth point, it is 30 times bigger than internet sales volume of NPD projects.Internet of Things (Internet of Things) passes various information
Feel equipment, such as radio frequency identification (RFID) device, infrared inductor, global positioning system, a variety of devices of laser scanner with mutually
Networking combines, and the huge network formed.The purpose is to allow all articles to be easy to all together with network connection
Identification and management.The basis of Internet of Things is radio frequency identification, and no radio frequency identification is impossible to realize Internet of Things.Carry out radio frequency identification
Most basic condition is exactly that various objects must carry electronic tag (E tag), is just easy to identify.Electronic tag is by coupling element
(containing flexible magnetic sheet), IC chip and antenna composition.Identify that the length of distance depends on the effective depth of antenna.In coupling element
Flexible magnetic sheet can greatly increase the effective depth of antenna, so as to improve the sensitivity of antenna, increase identification distance.Flakey metal
Soft magnetism micro mist is the crucial main material for making flexible magnetic sheet, is new material indispensable, basic in Internet of Things.
With electronics, electric, communication and the rapid development of information industry, with integrated circuit (IC) and large scale integrated circuit
The electronic instrument and electronic equipment being made up of core, while the every field of modern society is widely applied to, also give
People bring the problem of a series of new.Electromagnetic environmental pollution caused by electromagnetic interference oneself turn into after air, water source and discarded object
The fourth-largest environmental pollution afterwards.The Electro Magnetic Compatibility of electronic equipment has become the important technical for being badly in need of solving in countries in the world and asked
Topic.The flexible magnetic sheet that flat soft magnetic metal micro mist makes is the crucial green wood for the emc issue for solving electronic equipment
Material.(Electromagnetic Shielding abbreviation EMS) can be electromagnetically shielded with it, so as to reduce electronic equipment production
Raw interference signal is to space radiation；The electromagnetic interference signal for being also possible to prevent free space enters device interior, disturbs electronics
Equipment normal work；It can also reduce and be disturbed between the level of electronic equipment internal simultaneously.So as to improve the Electro Magnetic Compatibility of electronic equipment.
Magnetic metal particle flattening is set some problems to be present using high energy ball mill at present.First, high energy ball mill makes
It is that point contacts between ball and ball, in the ideal situation, four isodiametric balls only have with being that ball-milling medium is spherical (steel ball etc.)
Four contact points, if being wherein only possible to 8 contact points of appearance comprising one and their just tangent beads.But this ideal
The probability that state occurs is very small, in addition high energy ball mill use is equal diameter ball, that is to say, that most 4 shocks of four balls
Point.Secondly, in high energy ball mill, the motion of ball and particle is divided into two kinds of irregular movement and group movement.Group movement base
Shock of the ball to material is not present in sheet, even if all very limited with the presence of extruding force, the dynamics of extruding force.Only irregular
During motion, shock and shearing force of the ball to material just occurs, sees Fig. 4 a.Irregular movement is uncontrollable with group movement
, in two kinds of motions, typically based on group movement.In impact and shearing force, impact is more than shearing force.Flat
Change initial stage, sufficiently large impact is than wanting.In the flattening later stage, shearing force contributes to the thickness of flakelike powder to reduce, but
When impact exceedes the ability to bear of thin slice, it is possible to cause thin slice to crush, so as to reduce flat rate.
The content of the invention
A kind of weakness that the present invention is used in metal magnetic flaky process for high energy ball mill, there is provided magnetic metal powder
The method of end calendering flattening, flat (in length and breadth) ratio of magnetic metallic powder is further improved, flakey micro mist is reached average
0.1 μm~1.0 μm of thickness, aspect ratio 150~1500, average grain diameter be 30 μm~100 μm pattern, size requirement.
Technical scheme：A kind of method of magnetic metallic powder calendering flattening, the calendering flattening method are：Pass through rod
The method of mill, make the magnetic metallic powder of preliminary flattening in the presence of the grinding pressure of roller rod, shearing force, mutually extruding, by force
There is plastic deformation (Fig. 2) in urgent powder, and the size of its thickness direction reduces because being squeezed, shearing, and particle is forced to length and width side
To extension；The overlapping placement multilayer roller rod in rod milling cylinder, when mill tube inwall rotates, under the double action of gravity and frictional force,
Drive each layer roller rod to rotate successively, formed to the rolling of magnetic metallic powder, sheared, so as to realize the side rolled to powder
Method.It is linear contact lay between roller rod, a contact line is formed between two roller rods, there are infinite multiple points on this line, sees Fig. 1 a.
, can be roller rod enlarged diameter in order to increase the dynamics for rolling, rolling.If using ball milling, only one contacts between two balls
Point, the ball used is bigger, and contact point is fewer.In order to increase contact point, high energy ball mill can only use bead (such as Ф 4.8mm, Ф
6.35mm ball).Using bead, must just there is high movement velocity, to form enough impulsive forces.Secondly, high energy ball mill
Obtain enough impulsive forces, it is necessary to have powerful and quick mixing power, this power will make considerable part material and spherical
Into group movement, due to the presence of group movement, make the flattening efficiency of magnetic reduce, see Fig. 4.Roller rod motion is to certain height
Degree, apex roller rod will slide to be passed through as lower roller rod, material between roller rod, and powder is pressed because being rolled, being sheared
Prolong, in the absence of group movement.
Sliding between mill tube wall and roller rod, roller rod and roller rod be present, from lower roller rod to apex roller rod, roller rod rotation linear speed
Degree declines with the increase of the number of plies.Because the floating velocity of the different particle of granule size is different, therefore, the material of small grain size
The upper strata of liquid level is always suspended in, bulky grain is then in lower floor or bottom, and then, bulky grain is by weight (upper strata roller rod weight
Power is superimposed) and quickly roll, and the grinding pressure that the particle for being in top is subject to is small, and rolling speed is slow.On the other hand, with
The reduction of grain thickness and the increase of length and width size, in length and breadth bigger powder due to the resistance of motion it is larger without free settling, it is more
Be suspended at the middle and upper levels, therefore, the powder that aspect ratio is less or granularity is larger be always subjected to it is larger roll, shearing force, and indulge
The horizontal less powder of bigger or granularity be always subjected to it is less roll, shearing force.However, high energy ball mill or planetary mill
Machine is then different, the speed all maintained like from beginning to end, material powder, the powder of preliminary flattening, close to finished product requirement
Powder, the impact being subject to is essentially identical, inevitably cause part flattening powder crush.
Grinding pressure between adjacent layer roller rod be present, shearing force be present between same layer adjacent roller rod, see Fig. 1 b.Therefore, no
Pipe is grinding pressure, or shearing force, there is calendering effect to powder, but high energy ball mill is then different, is by impact and cuts
Shear force makes powder extend, and shock can make flakelike powder extend, but it can also be made broken, sees Fig. 5.Contacted with each other at four
An outer and their tangent pony roll rods can be placed among big roller rod, to increase contact line, improves and rolls efficiency, and high energy
Ball mill then can not.In order to improve the benefit and quality of calendering flattening, the roller rod case hardness is more than HRc50, and quenching is deep
Spend more than 1.0mm；Surface roughness is Ra0.10~Ra0.50；The axiality of outer should be less than 0.01mm.
The magnetic metallic powder includes：Pure iron (Fe) powder, iron silicon (Fe-Si) series alloy powder, iron sial (Fe-Si-
Al) series alloy powder, iron silicochromium (Fe-Si-Cr) series alloy powder, ferronickel system (permalloy and iron nickel molybdenum Fe-Ni, Fe-Ni-
Mo) alloy powder, iron Cobalt (Fe-Co) series alloy powder, magnetic stainless steel (Fe-Si-Cr-Al) series alloy powder, iron copper silicon
(Fe-Si-B-Cu-Nb) series alloy powder, iron silicon boron Fe-Si-B) series alloy powder, iron silicochromium nickel (Fe-Si-Cr-Ni) system
Alloy powder, iron sial nickel chromium triangle (Fe-Si-Al-Ni-Cr) series alloy powder, iron silicon Cobalt boron (Fe-Si-Co-B) are alloyed powder
End, and Fe-based amorphous alloy, iron-nickel-based amorphous alloy, Cobalt Fe-based amorphous alloys, iron-based alloy nano-powder.
According to the situation of powder flattening, take classification to process, use different roller rod diameters and different rod milling linear speeds
Degree processing.Classification processing can divide two level, can also divide three-level, even level Four.
Preference, two-stage rod milling, including first order rod milling and second level rod milling.
Beneficial effect：For the present invention by the way of rolling, roll, the power that roller rod applies to powder only has grinding pressure and shearing
Power, therefore, either grinding pressure, or shearing force, there is calendering effect to powder, can avoid being similar in high energy ball mill
Group movement and excessive impact, improve the ratio and production efficiency of powder flattening.
Brief description of the drawings
Fig. 1 be with the present invention compared with high energy ball mill in the motion state schematic diagram of material and ball；
Fig. 2 is roller rod of the present invention to the rolling of material, shears schematic diagram；
Fig. 3 is present invention process flow chart；
Fig. 4 is rod milling campaign schematic diagram of the present invention；
Fig. 5 be in high energy ball mill compared with the present invention ball to the crush force schematic diagram of material；
Fig. 6 is raw material of the present invention, i.e., the SEM of the powder morphology of preliminary flattening is processed through upper process
Photo；
Fig. 7 is the electron scanning micrograph of the powder morphology after first order rod milling of the present invention；
Fig. 8 is the electron scanning micrograph of the powder morphology after second level rod milling of the present invention.
Embodiment
In order that the object, technical solutions and advantages of the present invention are clearer, the preferred embodiments of the present invention are entered below
The detailed description of row.
As explained above, according to the present invention it is possible to by block, spherical, ellipsoid, and it is other irregular
Shape pure iron (Fe) powder, iron silicon (Fe-Si) series alloy powder, iron sial (Fe-Si-Al) series alloy powder, iron silicochromium
(Fe-Si-Cr) series alloy powder, ferronickel system (permalloy and iron nickel molybdenum Fe-Ni, Fe-Ni-Mo)) alloy powder, iron cobalt
(Fe-Co) series alloy powder, magnetic stainless steel (Fe-Si-Cr-Al) series alloy powder, iron copper silicon (Fe-Si-B-Cu-Nb) system close
Bronze end, iron silicon boron Fe-Si-B) series alloy powder, iron silicochromium nickel (Fe-Si-Cr-Ni) series alloy powder, iron sial nickel chromium triangle
(Fe-Si-Al-Ni-Cr) series alloy powder, iron silicon cobalt boron (Fe-Si-Co-B) series alloy powder, and Fe-based amorphous alloy,
The powder such as iron-nickel-based amorphous alloy, ferro-cobalt base noncrystal alloy, iron-base nanometer crystal alloy.These through preliminary flattening processing after,
Average thickness is processed into as 0.1 μm~1.0 μm with the present invention again, and aspect ratio 150~1500, average grain diameter is 30 μm~100
μm squamose metal soft magnetic micro powder.
Flattening flow process chart is shown in Fig. 3.Calendering flattening work flow includes first order rod milling and second level rod milling.
The metal soft magnetic alloy material powder of various different chemical compositions, crystalline condition and different-shape first passes around stone roller
Pressure, punching press, make its preliminary flattening.By rolling, punching press, the stereoscan photograph of the powder of preliminary flattening is shown in Fig. 6.
The present invention is the method by rod milling, preliminary flattening metal soft magnetic alloy powder is existed in linear velocity poor
In the presence of the grinding pressure of different roller rod, shearing force, extruding, forces powder plastic deformation occur, the chi of its thickness direction mutually
Very little to reduce because of extruding, particle is forced to the extension of length and width direction.That is, roll, shearing force generates calendering effect.
During first order rod milling, also should according to metal dust number, decentralized medium ratio etc., select frotton diameter big
It is small, to provide corresponding calendering dynamics, and the linear velocity of suitable frotton rotation is selected, quickly roll repeatedly.Through
The stereoscan photograph for the powder crossed after first order rod milling, calendering is shown in Fig. 7.
During the rod milling of the second level, the frotton of minor diameter should be selected, the ratio of decentralized medium and magnetic should also increase, with less
Calendering force, the thickness of powder is reached pre-provisioning request, and be unlikely to broken.Powder after second level rod milling, calendering
Stereoscan photograph is shown in Fig. 8..
Powder after second level rod milling, calendering has been semi-finished product.
Embodiment 1
The commercially available 400 mesh permalloy powder produced using aeroponics makees raw material, and has been subjected to that process rolls, punching press adds
Work, the stereoscan photograph of the powder of preliminary flattening are shown in Fig. 6
Make decentralized medium with ethanol, the volume ratio of decentralized medium and alloyed powder is 6:1, antirust, lubricant quantity are metal
0.2% (mass ratio) of powder.Using Ф 80mm, Ф 30mm and Ф 12mm roller rod, the quantity ratio about 20 of large, medium and small rod：
5：1, the ratio of roller rod and alloyed powder is 10:1 (mass ratio).The linear velocity of rod milling top tank structure is 200 ms/min.Continuous calendering 30
After hour, sampling.The stereoscan photograph of sample is shown in Fig. 7.
And then, rod milling is continued using spillikin.The volume ratio of decentralized medium and alloyed powder is 8:1, antirust, the ratio of lubricant
Example is constant.Using Ф 16mm and Ф 6mm roller rod, the quantity ratio about 4 of large and small rod:1, the ratio of roller rod and alloyed powder is 12:
1 (mass ratio).The linear velocity of rod milling top tank structure is 100 ms/min.After continuous calendering 30 hours, sampling.The ESEM of sample
Photo is shown in Fig. 8.The pattern of sample is flakey, and its average thickness is 0.66 μm, in length and breadth about 450.Use laser particle analyzer
Measurement, average grain diameter are 60 μm.
Claims (4)
- A kind of 1. method of magnetic metallic powder calendering flattening, it is characterised in that：It is described calendering flattening method be：Pass through rod The method of mill makes the magnetic metallic powder of preliminary flattening in the presence of the grinding pressure of roller rod, shearing force, and extruding, is forced mutually There is plastic deformation in powder, and the size of its thickness direction reduces because being squeezed, shearing, and particle is forced to the extension of length and width direction； Overlapping placement multilayer roller rod, when mill tube inwall rotates, under the double action of gravity and frictional force, drives successively in rod milling cylinder The rotation of each layer roller rod, formed to the rolling of magnetic metallic powder, sheared, so as to realize the method rolled to powder；Sliding between mill tube inwall and roller rod, roller rod and roller rod be present, with the increase of the number of plies, from lower roller rod to apex roller rod Rotary speed be sequentially reduced；Between same layer adjacent roller rod contact site rotation it is in opposite direction, powder is sheared； The direction of contact site rotation between adjacent layer roller rod is identical, powder is extruded, extruding and shearing can be played to powder The calendering effect at end；An outer and their tangent pony roll rods are placed among the big roller rod that four contact with each other, to improve Efficiency；The magnetic metallic powder includes：Pure iron powder, iron Si system alloy powder, iron sial series alloy powder, iron silicochromium system close Bronze end, ferronickel series alloy powder, iron Co-based alloy powder, magnetic stainless steel series alloy powder, iron Si-Cu-based alloy powder, iron Silicon boron based alloy powder, iron silicochromium nickel system alloy powder, iron sial Nimonic powder, iron silicon cobalt boron based alloy powder, with And Fe-based amorphous alloy, iron-nickel-based amorphous alloy, ferro-cobalt base noncrystal alloy, iron-based alloy nano-powder.
- 2. the method for magnetic metallic powder calendering flattening according to claim 1, it is characterised in that：The table of the roller rod Surface hardness is more than HRc50, more than depth of quenching 1.0mm；Surface roughness is Ra0.10~Ra0.50；The axiality of outer should be small In 0.01mm.
- 3. the method for the magnetic metallic powder calendering flattening according to any one of claim 1-2, it is characterised in that：Root According to the situation of powder flattening, take classification to process, carried out using different roller rod diameters from different rod milling linear velocities Processing.
- 4. the method for magnetic metallic powder calendering flattening according to claim 3, it is characterised in that：Described rod milling is extremely Include two-stage, i.e. first order rod milling and second level rod milling less, in particular cases, three-level, even level Four rod milling can be carried out.
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Address after: Henan Bridge, Yangtze East Road, Sanmao Street, Yangzhong City, Zhenjiang City, Jiangsu Province Patentee after: Jiangsu Bona Electromagnetic New Materials Co., Ltd. Address before: 212200 Henan Bridge, Yangtze East Road, Sanmao Street, Yangzhong City, Zhenjiang City, Jiangsu Province Patentee before: Zhenjiang Baona Electromagnetic New Material Co., Ltd. |