CN104599833A - High-toughness rare earth flexible magnetic strip and production method thereof - Google Patents
High-toughness rare earth flexible magnetic strip and production method thereof Download PDFInfo
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Abstract
The invention discloses a high-toughness rare earth flexible magnetic strip and a production method thereof. The high-toughness rare earth flexible magnetic strip comprises the following components: 92wt%-97wt% of NdFeB (neodymium iron boron) alloy magnetic powder, 2-3wt% of binder, and 1-5% of processing additive, wherein the NdFeB alloy magnetic powder contains a Dy (dysprosium) element or a Tb (terbium) element, the binder contains F48 thermosetting novolac epoxy resin, the processing additive adopts a coupling agent, a coating agent, a lubricating agent, a curing agent and a plasticizing agent, the coupling agent contains titanate, and the coating agent contains aromatic dicarboxylic acid with concentration of 0.2wt%. The high-toughness rare earth flexible magnetic strip has the advantages that a production method has simple technology, and the cost is low; for the produced high-toughness rare earth flexible magnetic strip, the mechanical property is high, the toughness is higher, the easiness in cracking and corner explosion is avoided, the large-scale automatic production is realized, and the economic benefit is high.
Description
Technical field
The present invention relates to technical field of magnetic materials, particularly a kind of rare-earth flexible magnetic stripe of high tenacity and production method thereof.
Background technology
Although rare-earth flexible permanent magnetic material comes out, the time is short, output is also less than agglomeration permanent magnetic material, but the advantage had because of it not available for manufacture methods such as sintering, casting, thermal deformation, binding electromagnetic material is made to develop rapidly, having a extensive future in every field, the extremely attention of various countries' Permanent Magnet Material Industry.
Rare-earth flexible permanent magnetic material is important Metallic Functional Materials, utilizes the various physical effects of its power conversion function and magnetic can make the function element of various ways.The rare-earth flexible magnetic stripe made can be widely used in space flight navigation, information electronic, the energy, traffic, communication and Magnetotherapeutic health various fields, particularly, in recent years, stimulate circulation because rare-earth flexible magnetic stripe is distinctive, the health-care effect of the aspect such as improving water flood, market gets more and more to the demand of flexible magnetic strips.
Tension, the bending strength of rareearth magnetic material are all lower, and its fracture toughness 1-2 order of magnitude lower than ordinary metallic material, suitable with the Fracture Toughness of ceramic material.Toughness official post rare earth magnet easily falls limit arrisdefect in the processes such as production, processing, transport, assembling, even ruptures; Poor toughness, also makes toughness of material poor, reduces the anti shock and vibration ability of material, affects material stability in use and fail safe.The permanent magnet of poor toughness not only increases the production cost of rare earth permanent-magnetic material, and seriously constrains the application development of rare earth permanent-magnetic material.
In prior art, improve the fracture toughness of material by adding appropriate fibrous metal silk in magnetic.But experiment shows, the interpolation of iron fiber not only can make the magnetic of magnetic material reduce, and coercive force and squareness can be made to reduce, and add iron fiber without any the effect of increase toughness, make the dynamics of magnetic material decline on the contrary.Prior art also improves the technical scheme of the toughness of NdFeB permanent magnetic material by adding Cu element, but, along with adding of Cu element, the intermetallic compound NdFeCoCu defining triangle state in sintering process enters into crystal boundary, improve the intensity of sintered body, but along with the increase of Cu content, sintered body intermediate cam state increases mutually and causes stress to be concentrated, and then makes the impact toughness decreased of NdFeB permanent magnetic material.
Prior art also teaches and add other metals to improve the method for the toughness of material in rare earth permanent-magnetic material, such as, Chinese invention patent CN1217551A is " a kind of high-performance rare-earth permanent magnet material and preparation method thereof ", is to account for the additive D (D=Al of basic composition total weight 0.05 ~ 2.0%
20
3or TiN) join in R-Fe-M-B alloy powder, mixed-powder is compressing, sintering, heat treatment obtain rare earth permanent-magnetic material containing additive D.This material mainly adopts Al to reduce magnet cost
20
3or the way that TiN adds, although these the two kinds of particles added can replace heavy rare earth element or heavy rare earth element oxide to improve magnet coercive force to a certain extent, but these two kinds of particles all belong to high rigidity, high brittle particle, they add the obdurability that can not improve magnet.
In addition, prior art also improves the fracture toughness of material by two alloyage, but the complex process of the method and limited to the toughness improvement effect of material.
For this reason, rare-earth flexible magnetic stripe and the production method thereof of developing a kind of new high tenacity is needed.
Summary of the invention
The technical problem that the invention solves is: the limited and complex process of modified effect in rare earth permanent-magnetic material poor toughness of the prior art, toughening modifying process.For this reason, the present invention proposes a kind of rare-earth flexible magnetic stripe and production method thereof of high tenacity, can eliminate one or more problems that restriction and defect due to prior art cause fully.
Additional advantages of the present invention, object and characteristic, a part will be elucidated in the following description, and another part for those of ordinary skill in the art by being obvious to the investigation of explanation below or acquiring from enforcement of the present invention.Can realize and obtain the object of the invention and advantage by the structure pointed out especially in the specification of word and claims and accompanying drawing.
The invention provides a kind of production method of rare-earth flexible magnetic stripe of high tenacity, said method comprising the steps of:
Step 1, adds Dy element or Tb element in NdFeB, forms NdFeB alloy;
Step 2, preparation average grain diameter is the NdFeB alloy powder of 3-4 μm; Concrete, first utilize Quench belt-rejecting technology to prepare NdFeB alloy sheet, then obtain NdFeB alloy powder through broken, grinding;
Step 3, utilize coupling agent and coating agent to carry out surface treatment to NdFeB alloy powder, described coupling agent is titanate esters, and described coating agent is aromatic dicarboxylic acid; Specifically comprise: be the titanate esters toluene solution of 0.1wt% by NdFeB alloy powder and concentration, concentration is that the aromatic dicarboxylic acid of 0.2wt% mixes, and stirs half an hours with magnetic stirring apparatus with 400 revs/min at 100 DEG C;
Step 4, in masticator, by the NdFeB alloy powder after surface treatment and binding agent and processing aid evenly mixing, melting temperature is 90-110 DEG C, and mixing time is 10-15 minute, and wherein said binding agent is F48 thermosetting phenolic epoxy resin;
Step 5, is rolled into mixing uniform material the sheet material that thickness is 2-3mm;
Step 6, carries out fragmentation by sheet material in disintegrating machine, obtains the pellet by 12 object screen clothes;
Step 7, by extruder by pellet extrusion molding, obtains rare-earth flexible magnetic stripe, wherein, applies the alignment magnetic field of 1.5T in extrusion molding process.
Preferably, described Dy element or the weight percent content of Tb element in NdFeB alloy are respectively 6% and 4%.
Preferably, in step 2, by the method that hydrogen is broken, NdFeB alloy sheet is broken.
Preferably, the method for described grinding is airflow milling or ball milling.
Preferably, the processing aid in step 4 is lubricant, curing agent, plasticizer.
Preferably, described lubricant is polyvinyl butyral resin, and described curing agent is m-phenylene diamine (MPD), and described plasticizer is phthalate compound or epoxy compounds.
Present invention also offers a kind of rare-earth flexible magnetic stripe of high tenacity, the component of the rare-earth flexible magnetic stripe of described high tenacity comprises: NdFeB alloy magnetic powder 92wt%-97wt%, binding agent 2-3wt%, processing aid 1-5wt%, wherein, described NdFeB alloy magnetic powder comprises Dy element or Tb element, described binding agent is F48 thermosetting phenolic epoxy resin, described processing aid is coupling agent, coating agent, lubricant, curing agent and plasticizer, described coupling agent is titanate esters, the aromatic dicarboxylic acid of described coating agent to be concentration be 0.2wt%.
Preferably, described Dy element or the weight percent content of Tb element in NdFeB alloy are respectively 6% and 4%.
Preferably, described lubricant is polyvinyl butyral resin, and described curing agent is m-phenylene diamine (MPD), and described plasticizer is phthalate compound or epoxy compounds.
The rare-earth flexible magnetic stripe production method technique of high tenacity provided by the invention is simple, and cost is low, and the rare-earth flexible magnetic stripe good mechanical property produced, has very high toughness, and not easy to crack and quick-fried angle, can realize large-scale automated production, high financial profit.
Accompanying drawing explanation
Fig. 1 be according to the embodiment of the present invention, the flow chart of the production method of the rare-earth flexible magnetic stripe of high tenacity.
Embodiment
With reference to the accompanying drawings the present invention is described more fully, exemplary embodiment of the present invention is wherein described.
Inventor is on the basis of actual production in conjunction with a large amount of experimental study work, find the toughness of rare-earth flexible magnetic stripe and the composition of material, the auxiliary agent of the size of particle and interpolation has relation closely, for this reason, the present invention improves emphatically the toughness of rare-earth flexible magnetic stripe by above-mentioned several aspect.
The present invention proposes a kind of production method of rare-earth flexible magnetic stripe of high tenacity, rareearth magnetic material of the present invention adopts NdFeB, said method comprising the steps of:
Step 1, adds additional elements in NdFeB, forms NdFeB alloy;
Preferably, described additional elements is Dy element or Tb element, and described Dy element or the weight percent content of Tb element in NdFeB alloy are respectively 6% and 4%.
NdFeB magnet mainly contains in 3 and forms phase: the matrix phase Nd of (1) polygonal shape
2fe
14b, it is Magnetic Phase, is intermetallic compound, is anisotropy tetragonal structure; (2) rich neodymium phase, generally exist with 3 kinds of existence forms: the first is embedded in the rich neodymium phase of the borderline bulk of principal phase, the second is that continuous distribution hands over the rich neodymium phase of the lamelliform at corner place in grain boundary and crystal boundary, and the third is the rich neodymium phase of the disperse being distributed in main phase grain inside.(3) boron-rich phase, is often present on crystal boundary with isolated block (angle) shape or graininess.This structure of alloy contributes to the magnetic behavior improving magnet, but but there is negative effect to terms of mechanics, the relative crystal grain of rich neodymium wherein mainly plays the isolated effect of magnetic, the magnetic property of NdFeB permanent magnetic material can be improved, but the hardness of rich neodymium phase is lower, micro-crack is expanded relatively easily wherein, and these laminar rich neodymiums are the major reason making NdFeB permanent magnetic material produce grain boundary fracture mutually.Therefore in NdFeB permanent magnetic material, add suitable element, improve the composition and structure of rich neodymium phase, improve the intensity of rich neodymium phase, thus the mechanical property of NdFeB permanent magnetic material can be improved.
The present invention, by a large amount of experiments, when finding that the content in described NdFeB alloy is 4% when Dy element or Tb element, can significantly improve the toughness of magnet.Interpolation Dy element or Tb element can significantly improve the toughness of NdFeB permanent magnetic material, are because interpolation Dy element or Tb element improve the crystal boundary micro-structural of material, enhance local bond strength.
Step 2, preparation NdFeB alloy powder;
Concrete, first utilize Quench belt-rejecting technology to prepare NdFeB alloy sheet, then obtain NdFeB alloy powder through broken, grinding.
Preferably, the present invention is broken by NdFeB alloy sheet, concrete by the method that hydrogen is broken, to prepare NdFeB alloy sheet loads in hydrogen crushing furnace, after vacuumizing, be filled with high-purity hydrogen, under 0.02-1.2Mpa hydrogen pressure, inhale hydrogen 0.5-5h, hear the cracker of alloy, can detect that the temperature of container is in continuous rising simultaneously, this forms hydride volumetric expansion after RE permanent magnetic alloy inhales hydrogen and bursts, then dehydrogenase 12-10h at 450-650 DEG C, obtains flour.
In the present invention, the flour after described grinding is broken by hydrogen is broken further, thus completes the pulverizing process of alloy.The method of described grinding is airflow milling or ball milling.The present invention preferably adopts airflow milling.The method of airflow milling powder is conventionally known to one of skill in the art, and powder particle is accelerated to supersonic speed for utilizing air-flow by it, makes it mutually head-on collision and broken.Along with the increase of airflow milling granularity of magnet powder, magnet bending strength obviously reduces, and when granularity reduces, the magnetic property of magnet just weakens, and considers, and the average grain diameter of magnetic of the present invention is 3-4 μm.
Step 3, carries out surface treatment to NdFeB alloy powder;
Concrete, the present invention utilizes coupling agent and coating agent to carry out surface treatment to NdFeB alloy powder.
Coupling agent is in the preparation technology of magnet must be indispensable, therefore magnetic is hydrophilic, and general binding agent is oil loving, the effect of coupling agent is linked together at magnetic and binding agent, thus enhance the affinity of magnetic and interlaminar resin, improve the overlay capacity of magnetic surface resin, thus improve magnetic property.In order to make coupling agent be uniformly dispersed in magnetic, the present invention is by the organic solution of coupling agent and magnetic mixing, and as preferably, the present invention selects titanate coupling agent, selects toluene solution that dissolubility is good as solvent.If use excessive titanate coupling agent process magnetic, the adhesion between magnetic and binding agent can be reduced, thus affect the humidification of magnetic in bonded permanent magnet, cause the toughness of magnet to reduce.For this reason, inventor is through a large amount of experiments, and choosing coupling agent is titanate coupling agent, and titanate coupling agent organic solution is: titanate coupling agent concentration is the toluene solution of 0.1wt%.
In addition, the rare-earth flexible magnetic stripe border of making, is easy to get rusty, and therefore, also adds the aromatic dicarboxylic acid that may be applied to various ring as coating agent, prevent rare-earth flexible magnetic stripe from getting rusty when carrying out surface treatment to NdFeB alloy powder.As preferably, aromatic dicarboxylic acid is the mixture of phthalic acid or M-phthalic acid or said two devices.
Step 3 specifically comprises: be the titanate coupling agent toluene solution of 0.1wt% by NdFeB alloy powder and concentration, concentration is that the aromatic dicarboxylic acid of 0.2wt% mixes, and stirs half an hours with magnetic stirring apparatus with 400 revs/min at 100 DEG C.
By carrying out surface treatment to NdFeB alloy powder, forming one deck organic protective film on magnetic surface, not only increasing the oxidation resistance of magnetic itself, also add the adhesion of magnetic and binding agent, effectively can improve the toughness of magnet.
Step 4, in masticator, by the NdFeB alloy powder after surface treatment and binding agent and processing aid evenly mixing, melting temperature is 90-110 DEG C, and mixing time is 10-15 minute;
Consider from the angle of mechanical property, should choose the binding agent that epoxide number is high, for this reason, the present invention chooses F48 thermosetting phenolic epoxy resin as binding agent, with the toughness of enhancing magnet.The consumption of binding agent is very few, and the compression strength of magnet can be caused low; The consumption of bonding is too much, and the overall plasticity of magnet can be caused to increase.Consider the impact of binding agent on the magnetic property of magnet and mechanical strength two aspect, the consumption of the binding agent that the present invention selects is 2-3wt%.
What processing aid of the present invention adopted is lubricant, curing agent and plasticizer.
The lubricant that prior art adopts can produce adverse influence to the mechanical property of magnet, and in order to overcome this problem, the present invention selects and can form the polyvinyl butyral resin of good adhesive as lubricant with resin complex.Adopt polyvinyl butyral resin process, the compression strength of magnet can be improved, and raise along with increasing of polyvinyl butyral resin addition.This is because polyvinyl butyral resin coordinates with F48 thermosetting phenolic resin, the adhesivity that energy forming property is good, increases the node in binding agent network structure when bonded permanent magnet solidifies, and adhesion strength enhancing causes the compression strength of magnet to increase.
The curing agent that the present invention selects is m-phenylene diamine (MPD), and plasticizer is phthalate compound or epoxy compounds.
Step 5, is rolled into mixing uniform material the sheet material that thickness is 2-3mm;
Step 6, carries out fragmentation by sheet material in disintegrating machine, obtains the pellet by 12 object screen clothes;
Step 7, by extruder by pellet extrusion molding, obtains rare-earth flexible magnetic stripe, wherein, applies the alignment magnetic field of 1.5T in extrusion molding process.
Present invention also offers a kind of rare-earth flexible magnetic stripe of high tenacity, this magnetic stripe method above-mentioned according to the present invention is made, concrete, the component of the rare-earth flexible magnetic stripe of described high tenacity comprises: NdFeB alloy magnetic powder 92wt%-97wt%, binding agent 2-3wt%, processing aid 1-5wt%, wherein, described NdFeB alloy magnetic powder comprises Dy element or Tb element, described binding agent is F48 thermosetting phenolic epoxy resin, described processing aid is coupling agent, coating agent, lubricant, curing agent and plasticizer, described coupling agent is titanate esters, described coating agent is aromatic dicarboxylic acid.
Above content is only preferred embodiment of the present invention, and for those of ordinary skill in the art, according to thought of the present invention, all will change in specific embodiments and applications, this description should not be construed as limitation of the present invention.
Claims (9)
1. a production method for the rare-earth flexible magnetic stripe of high tenacity, is characterized in that, said method comprising the steps of:
Step 1, adds Dy element or Tb element in NdFeB, forms NdFeB alloy;
Step 2, preparation average grain diameter is the NdFeB alloy powder of 3-4 μm; Concrete, first utilize Quench belt-rejecting technology to prepare NdFeB alloy sheet, then obtain NdFeB alloy powder through broken, grinding;
Step 3, utilize coupling agent and coating agent to carry out surface treatment to NdFeB alloy powder, described coupling agent is titanate esters, and described coating agent is aromatic dicarboxylic acid; Specifically comprise: be the titanate esters toluene solution of 0.1wt% by NdFeB alloy powder and concentration, concentration is that the aromatic dicarboxylic acid of 0.2wt% mixes, and stirs half an hours with magnetic stirring apparatus with 400 revs/min at 100 DEG C;
Step 4, in masticator, by the NdFeB alloy powder after surface treatment and binding agent and processing aid evenly mixing, melting temperature is 90-110 DEG C, and mixing time is 10-15 minute, and wherein said binding agent is F48 thermosetting phenolic epoxy resin;
Step 5, is rolled into mixing uniform material the sheet material that thickness is 2-3mm;
Step 6, carries out fragmentation by sheet material in disintegrating machine, obtains the pellet by 12 object screen clothes;
Step 7, by extruder by pellet extrusion molding, obtains rare-earth flexible magnetic stripe, wherein, applies the alignment magnetic field of 1.5T in extrusion molding process.
2. the production method of the rare-earth flexible magnetic stripe of high tenacity according to claim 1, is characterized in that, described Dy element or the weight percent content of Tb element in NdFeB alloy are respectively 6% and 4%.
3. the production method of the rare-earth flexible magnetic stripe of high tenacity according to claim 1, is characterized in that, in step 2, the method broken by hydrogen is broken by NdFeB alloy sheet.
4. the production method of the rare-earth flexible magnetic stripe of high tenacity according to claim 1, is characterized in that, the method for described grinding is airflow milling or ball milling.
5. the production method of the rare-earth flexible magnetic stripe of high tenacity according to claim 1, is characterized in that, the processing aid in step 4 is lubricant, curing agent, plasticizer.
6. the production method of the rare-earth flexible magnetic stripe of high tenacity according to claim 5, is characterized in that, described lubricant is polyvinyl butyral resin, and described curing agent is m-phenylene diamine (MPD), and described plasticizer is phthalate compound or epoxy compounds.
7. the rare-earth flexible magnetic stripe of a high tenacity, it is characterized in that, the component of the rare-earth flexible magnetic stripe of described high tenacity comprises: NdFeB alloy magnetic powder 92wt%-97wt%, binding agent 2-3wt%, processing aid 1-5wt%, wherein, described NdFeB alloy magnetic powder comprises Dy element or Tb element, described binding agent is F48 thermosetting phenolic epoxy resin, described processing aid is coupling agent, coating agent, lubricant, curing agent and plasticizer, described coupling agent is titanate esters, the aromatic dicarboxylic acid of described coating agent to be concentration be 0.2wt%.
8. the rare-earth flexible magnetic stripe of high tenacity according to claim 7, is characterized in that, described Dy element or the weight percent content of Tb element in NdFeB alloy are respectively 6% and 4%.
9. the rare-earth flexible magnetic stripe of high tenacity according to claim 7, is characterized in that, described lubricant is polyvinyl butyral resin, and described curing agent is m-phenylene diamine (MPD), and described plasticizer is phthalate compound or epoxy compounds.
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