CN101593590B - Method for preparing warm compaction molding phenolic resin bonded Nd-Fe-B magnet - Google Patents
Method for preparing warm compaction molding phenolic resin bonded Nd-Fe-B magnet Download PDFInfo
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- CN101593590B CN101593590B CN2009100615607A CN200910061560A CN101593590B CN 101593590 B CN101593590 B CN 101593590B CN 2009100615607 A CN2009100615607 A CN 2009100615607A CN 200910061560 A CN200910061560 A CN 200910061560A CN 101593590 B CN101593590 B CN 101593590B
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Abstract
The invention discloses a method for preparing a warm compaction molding phenolic resin bonded Nd-Fe-B magnet, which solves the problem of serious oxidation of magnets caused by needing a solidification treatment working procedure during the preparation of the prior phenolic resin bonded Nd-Fe-B magnets to simplify preparation technology for the phenolic resin bonded Nd-Fe-B magnets and improve magnetic properties of the phenolic resin bonded Nd-Fe-B magnets. The method comprises the steps of surface modification treatment, molding as well as surface treatment and magnetism charging. The density of the phenolic resin bonded isotropical Nd-Fe-B magnet (the content of a phenolic resin is 3.0 percent by weight) is 6.12 g/cm<3>, the remanence is 0.683 T, the intrinsic coercive force is 730 kA/m, and the magnetic energy product is 78.2 kJ/m<3>; the performance of the magnet is higher than that of the magnetic of the prior preparation method; moreover, the preparation method is simple, has economical implementation, is easy to realize industrialized mass production, and has good promotion and application prospect.
Description
Technical field
The invention belongs to the preparation method of binding Nd-Fe-B permanent magnetic material, be specifically related to the preparation method of a kind of warm compaction molding phenolic resin bonded isotropism Nd-Fe-B (neodymium iron boron) magnet.
Background technology
The bonded Nd-Fe-B permanent magnetic material is a kind of novel permanent magnetic composite material that developed recently gets up; Be widely used in fields such as information, automobile, sound system, control system, measuring instrument, office automation and household electrical appliance, and the demand in the whole world is also in continuous increase.The moulding process of bonded Nd-Fe-B magnet mainly contains four kinds: compression molding, injection moulding, calendering formation and extrusion modling; Wherein the performance of compression molding bonded Nd-Fe-B magnet is the highest in four kinds of forming methods; Its output is also maximum, and the injection moulding bonded Nd-Fe-B magnet can prepare complex-shaped small-sized magnet, is easy to realize clean moulding and batch automatic production; At present, have only compression molding and injection moulding in suitability for industrialized production, to obtain practical application.
The bonded Nd-Fe-B magnet of compression molding mainly adopts epoxy resin, nylon, phenolic resins to make binding agent, with magnetic mixing compression moulding.The epoxy resin price is higher, and serviceability temperature is low, and wet and heat ageing resistant property is poor, and toughness is not high, makes the thermal endurance of its preparation magnet relatively poor; The water absorption of nylon is bigger, and dimensional stability is poor slightly, makes the density of its preparation magnet lower, and the performance in the use is stable inadequately; Characteristics such as phenolic resins is compared with epoxy resin, nylon, has cheap, high calorific intensity, and processing performance is good, the Nd-Fe-B magnet of making binding agent of it is more competitive at cost and aspect of performance.
Domestic and international research mainly concentrates on nylon and epoxy bond Nd-Fe-B magnet at present; Like " Mechanical properties of Nylonbonded Nd-Fe-B permanent magents " such as Monika G.Garrel, Albert J.Shih; See " Journal of Mgnetism andMgenetic Materials "; 2003,257:32-43; Zhou Weina, Li Wenxue etc. " technological factor is to the influence of NdFeB bonded permanent magnet magnetic property " see " electronic component and material ", 2006,2:31-34.In recent years, the research of phenolic resin bonded Nd-Fe-B magnet also there was a spot of report, Ru Huangli, Zheng Yini etc. " research of NdFeB/ phenolic resins in-situ composite " see " material engineering ", 2005,12:17-20; Yang Xiaoping, Bai Shuxin etc. " heat-resistant bonded neodymium iron boron magnetic body research " see " magnetic material and device ", 2006,8:55-58.At present, phenolic resin bonded Nd-Fe-B magnet prepares all needs the cured operation in the process, and curing time is long more, and the oxidation of magnet is serious more, and therefore, the magnetic property of magnet is lower.
Summary of the invention
The object of the present invention is to provide a kind of preparation method of warm compaction molding phenolic resin bonded Nd-Fe-B magnet; The existing phenolic resin bonded Nd-Fe-B magnet of solution prepares needs the cured operation to cause the serious problem of magnet oxidation in the process; To simplify the preparation technology of phenolic resin bonded Nd-Fe-B magnet, improve its magnetic property.
The preparation method of warm compaction molding phenolic resin bonded Nd-Fe-B magnet provided by the invention comprises:
The 1st step surface modification treatment step: in concentration is the silane acetone soln of 0.02g/ml～0.025g/ml, add isotropism Nd-Fe-B magnetic; The mass percent of silane and magnetic is 0.5%～1.5%; Vibrate dispersion treatment after the stirring, take out the back oven dry and obtain coupling couplet magnetic;
The 2nd one-step forming step: phenolic resins powder and coupling are joined magnetic mix, the phenolic resins powder is 1.5%～5.0% with the mass percent of coupling couplet magnetic, with the powder mould of packing into; After treating that mold temperature is raised to 160 ℃～200 ℃, under 600Mpa～1200MPa pressure, be pressed, keep the temperature and pressure temperature; Carry out repeatedly release, gas is wherein overflowed, again pressurized treatments; Cooling die to 50 ℃～60 ℃ of demouldings obtain blank then;
The 3rd step surface treatment and the step that magnetizes: blank is carried out surperficial deburring and surface anticorrosion processing, and the finished product magnet is processed in the processing of in magnetic field intensity is the magnetic field of 1.5～5T, magnetizing then.
As improvement project of the present invention, in the said surface modification treatment step, mixing time 20～30min adopts ultrasonic cleaner to vibrate dispersion treatment, and processing time 2～3h is dried 60～80 ℃ of bake out temperatures after 3～5h is left standstill in taking-up in baking oven.In the said forming step, release is pressurizeed again behind pressurize 1～1.5min when compression moulding, repeats 5～8 times.
The present invention adopts the phenolic resin bonded isotropism Nd-Fe-B magnet of warm compaction molding prepared; On the one hand, phenolic resins is a kind of solid powder, and warm compaction molding has solved phenolic resins powder at room temperature compressibility difference and mobile poor problem; The flowability and the compressibility of powder have been improved; Reduced to reach the frictional force between powder and the die wall between the powder, significantly improved the filling behavior of magnetic, improved pressing result; On the other hand; Compression moulding at a certain temperature; Phenolic resins can produce a certain amount of gas in the pressing process; The inner space of magnet also has a spot of gas, and the pressurization once more after each release can be discharged the gas that produce in the magnet previous stage smoothly, avoids the inner gas hole defect that produces of magnet; The 3rd, during warm compaction molding, the heat-insulation pressure keeping stage is equivalent to one-step solidification handles, and phenolic resins is cured reaction under the temperature and pressure temperature, simplified the cured operation of traditional preparation process technology, has reduced the degree of oxidation of magnet, has improved magnetic property.
At present, the optimal performance of the phenolic resin bonded isotropism Nd-Fe-B magnet (phenolic resin content is 3.0wt%) of traditional handicraft preparation is: density 5.66～6.04g/cm
3, remanent magnetism 0.627T, HCJ 656kA/m, magnetic energy product 62.8kJ/m
3The phenolic resin bonded isotropism Nd-Fe-B magnet (phenolic resin content is 3.0wt%) that the present invention is prepared, its density 6.12g/cm
3, remanent magnetism 0.683T, HCJ 730kA/m, magnetic energy product 78.2kJ/m
3Therefore, the performance of the phenolic resin bonded isotropism Nd-Fe-B magnet of warm compaction molding prepared of the present invention is than the height of traditional preparation process method, moreover the preparation method is simple, implements economy, is easy to realize industrialized mass production, has good popularization and application prospect.
Description of drawings
Fig. 1 is the stress-relief process of the pressurization repeatedly sketch map of forming step of the present invention.
Embodiment
Below in conjunction with embodiment the present invention is further specified, in the forming step of following each embodiment, all adopt the stress-relief process of pressurization repeatedly as shown in Figure 1.Among Fig. 1, a representes the pressure process after mould reaches the temperature and pressure temperature, and b representes the heat-insulation pressure keeping process; C representes to be incubated stress-relief process; D representes to be incubated the pressure process again after the release, the heat-insulation pressure keeping process after e representes to pressurize, and f representes release pressure process repeatedly; G representes the heat-insulation pressure keeping process after the last pressurization, and h representes the stress-relief process after the mold cools down.
Embodiment 1:
(1) surface modification treatment step: the silane acetone soln that 1g silane is added preparation 0.02g/ml in the beaker that 50ml acetone is housed; The isotropism Nd-Fe-B magnetic that adds 200g then; This moment, the mass ratio of silane and magnetic was 0.5%, put into ultrasonic cleaner behind the stirring 20min and vibrated dispersion treatment 2h, in baking oven, dried after 3h is left standstill in taking-up; 60 ℃ of bake out temperatures obtain coupling and join magnetic;
(2) forming step: get 1.5g phenolic resins powder and 100g coupling and join magnetic and evenly mix, this moment, the phenolic resins powder was 1.5% with the mass ratio of coupling couplet magnetic, the powder that at every turn the takes by weighing equivalent mould of packing into; After treating that mold temperature is raised to 160 ℃, under the pressure of 600Mpa, be pressed release behind the pressurize 1min; And then being pressurized to 600Mpa again, release again behind the pressurize 1min repeats 5 times repeatedly; Cooling die to the 50 ℃ demoulding then obtains the sample blank;
In the compression moulding process, carry out repeatedly release pressurized treatments again, the gas in the powder is overflowed, the inner formation micropore defective that is difficult for of product can improve performance of products;
(3) surface treatment and the step that magnetizes: sample is carried out surperficial deburring and surface anticorrosion processing, in magnetic field intensity is the magnetic field of 1.5T, magnetize then, process the finished product magnet.
Embodiment 2:
(1) surface modification treatment step: the silane acetone soln that 3g silane is added preparation 0.025g/ml in the beaker that 120ml acetone is housed; The isotropism Nd-Fe-B magnetic that adds 200g then; This moment, the mass ratio of silane and magnetic was 1.5%, put into ultrasonic cleaner behind the stirring 30min and vibrated dispersion treatment 3h, in baking oven, dried after 5h is left standstill in taking-up; 80 ℃ of bake out temperatures obtain coupling and join magnetic;
(2) forming step: get 5.0g phenolic resins powder and 100g coupling and join magnetic and evenly mix, this moment, the phenolic resins powder was 5.0% with the mass ratio of coupling couplet magnetic, the powder that at every turn the takes by weighing equivalent mould of packing into; After treating that mold temperature is raised to 200 ℃, under the pressure of 1200Mpa, be pressed release behind the pressurize 1.5min; And then being pressurized to 1200Mpa again, release again behind the pressurize 1.5min repeats 8 times repeatedly; Cooling die to the 60 ℃ demoulding then obtains the sample blank;
(3) surface treatment and the step that magnetizes: sample is carried out surperficial deburring and surface anticorrosion processing, in magnetic field intensity is the magnetic field of 5.0T, magnetize then, process the finished product magnet.
Embodiment 3:
(1) surface modification treatment step: the silane acetone soln that 2g silane is added preparation 0.0222g/ml in the beaker that 90ml acetone is housed; The isotropism Nd-Fe-B magnetic that adds 200g then; This moment, the mass ratio of silane and magnetic was 1.0%, put into ultrasonic cleaner behind the stirring 25min and vibrated dispersion treatment 2.5h, in baking oven, dried after 4h is left standstill in taking-up; 70 ℃ of bake out temperatures obtain coupling and join magnetic;
(2) forming step: get 4.0g phenolic resins powder and 100g coupling and join magnetic and evenly mix, this moment, the phenolic resins powder was 4.0% with the mass ratio of coupling couplet magnetic, the powder that at every turn the takes by weighing equivalent mould of packing into; After treating that mold temperature is raised to 180 ℃, under the pressure of 1000Mpa, be pressed release behind the pressurize 1.2min; And then being pressurized to 1000Mpa again, release again behind the pressurize 1.2min repeats 6 times repeatedly; Cooling die to the 55 ℃ demoulding then obtains the sample blank;
(3) surface treatment and the step that magnetizes: sample is carried out surperficial deburring and surface anticorrosion processing, in magnetic field intensity is the magnetic field of 2.5T, magnetize then, process the finished product magnet.
The present invention not only is confined to above-mentioned embodiment; Persons skilled in the art are according to content disclosed by the invention; Can adopt other multiple embodiment embodiment of the present invention, therefore, every employing mentality of designing of the present invention; Do some simple designs that change or change, all fall into the scope of the present invention's protection.
Claims (2)
1. the preparation method of a warm compaction molding phenolic resin bonded Nd-Fe-B magnet comprises:
The 1st step surface modification treatment step: in concentration is the silane acetone soln of 0.02g/ml～0.025g/ml, add isotropism Nd-Fe-B magnetic; The mass percent of silane and magnetic is 0.5%～1.5%; Vibrate dispersion treatment after the stirring, take out the back oven dry and obtain coupling couplet magnetic;
The 2nd one-step forming step: phenolic resins powder and coupling are joined magnetic mix, the phenolic resins powder is 1.5%～5.0% with the mass percent of coupling couplet magnetic, with the powder mould of packing into; After treating that mold temperature is raised to 160 ℃～200 ℃, under 600Mpa～1200MPa pressure, be pressed, keep the temperature and pressure temperature; Carry out repeatedly release, gas is wherein overflowed, again pressurized treatments; Cooling die to 50 ℃～60 ℃ of demouldings obtain blank then; Release is pressurizeed again behind pressurize 1～1.5min when compression moulding, repeats 5～8 times;
The 3rd step surface treatment and the step that magnetizes: blank is carried out surperficial deburring and surface anticorrosion processing, and the finished product magnet is processed in the processing of in magnetic field intensity is the magnetic field of 1.5～5T, magnetizing then.
2. preparation method as claimed in claim 1 is characterized in that:
In the said surface modification treatment step, mixing time 20～30min adopts ultrasonic cleaner to vibrate dispersion treatment, and processing time 2～3h is dried 60～80 ℃ of bake out temperatures after 3～5h is left standstill in taking-up in baking oven.
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| CN102314986A (en) * | 2011-05-19 | 2012-01-11 | 浙江科达磁电有限公司 | Ferrum-silicon alloy magnetic powder core and manufacturing method thereof |
| CN102360661A (en) * | 2011-05-19 | 2012-02-22 | 浙江科达磁电有限公司 | Iron-silicon alloy soft magnetic material with permeability mu of 75 and manufacturing method thereof |
| CN104174843A (en) * | 2014-08-11 | 2014-12-03 | 北京京磁强磁材料有限公司 | Oriented compression moulding method for sintered NdFeB |
| JP6274068B2 (en) * | 2014-10-03 | 2018-02-07 | トヨタ自動車株式会社 | Rare earth magnet manufacturing method |
| CN109524233B (en) * | 2018-12-29 | 2021-01-15 | 陈亮 | Magnet material mixing and bonding process |
| CN109767905B (en) * | 2018-12-29 | 2021-01-15 | 陈亮 | Magnet material hot press molding process |
Citations (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| JP2004349337A (en) * | 2003-05-20 | 2004-12-09 | Aichi Steel Works Ltd | Method of manufacturing bond magnet |
| CN101028652A (en) * | 2007-01-12 | 2007-09-05 | 北京科技大学 | Magnetic-field temperature-pressure formation |
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| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| JP2004349337A (en) * | 2003-05-20 | 2004-12-09 | Aichi Steel Works Ltd | Method of manufacturing bond magnet |
| CN101028652A (en) * | 2007-01-12 | 2007-09-05 | 北京科技大学 | Magnetic-field temperature-pressure formation |
Non-Patent Citations (2)
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| 李军.高性价比的模压粘结钕铁硼永磁体制备.《中国优秀硕士论文电子期刊网》.2004, * |
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