CN113838656A - Preparation method of flexible bonded neodymium-iron-boron magnet and product and application thereof - Google Patents
Preparation method of flexible bonded neodymium-iron-boron magnet and product and application thereof Download PDFInfo
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- CN113838656A CN113838656A CN202010578220.8A CN202010578220A CN113838656A CN 113838656 A CN113838656 A CN 113838656A CN 202010578220 A CN202010578220 A CN 202010578220A CN 113838656 A CN113838656 A CN 113838656A
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- 229910001172 neodymium magnet Inorganic materials 0.000 title claims abstract description 110
- 238000002360 preparation method Methods 0.000 title claims abstract description 19
- 235000019687 Lamb Nutrition 0.000 claims abstract description 48
- PXHVJJICTQNCMI-UHFFFAOYSA-N Nickel Chemical compound [Ni] PXHVJJICTQNCMI-UHFFFAOYSA-N 0.000 claims description 78
- 239000006247 magnetic powder Substances 0.000 claims description 64
- PNEYBMLMFCGWSK-UHFFFAOYSA-N aluminium oxide Inorganic materials [O-2].[O-2].[O-2].[Al+3].[Al+3] PNEYBMLMFCGWSK-UHFFFAOYSA-N 0.000 claims description 45
- 239000000843 powder Substances 0.000 claims description 42
- 229910052759 nickel Inorganic materials 0.000 claims description 39
- 239000007864 aqueous solution Substances 0.000 claims description 33
- FGDZQCVHDSGLHJ-UHFFFAOYSA-M rubidium chloride Chemical compound [Cl-].[Rb+] FGDZQCVHDSGLHJ-UHFFFAOYSA-M 0.000 claims description 28
- QJVKUMXDEUEQLH-UHFFFAOYSA-N [B].[Fe].[Nd] Chemical compound [B].[Fe].[Nd] QJVKUMXDEUEQLH-UHFFFAOYSA-N 0.000 claims description 25
- 239000007822 coupling agent Substances 0.000 claims description 24
- 239000011259 mixed solution Substances 0.000 claims description 23
- RTAQQCXQSZGOHL-UHFFFAOYSA-N Titanium Chemical compound [Ti] RTAQQCXQSZGOHL-UHFFFAOYSA-N 0.000 claims description 21
- KTWOOEGAPBSYNW-UHFFFAOYSA-N ferrocene Chemical compound [Fe+2].C=1C=C[CH-]C=1.C=1C=C[CH-]C=1 KTWOOEGAPBSYNW-UHFFFAOYSA-N 0.000 claims description 17
- 238000002156 mixing Methods 0.000 claims description 17
- 230000005291 magnetic effect Effects 0.000 claims description 16
- 238000000034 method Methods 0.000 claims description 16
- 238000004381 surface treatment Methods 0.000 claims description 15
- 229940102127 rubidium chloride Drugs 0.000 claims description 14
- 239000004841 bisphenol A epoxy resin Substances 0.000 claims description 13
- 235000003891 ferrous sulphate Nutrition 0.000 claims description 13
- 239000011790 ferrous sulphate Substances 0.000 claims description 13
- BAUYGSIQEAFULO-UHFFFAOYSA-L iron(2+) sulfate (anhydrous) Chemical compound [Fe+2].[O-]S([O-])(=O)=O BAUYGSIQEAFULO-UHFFFAOYSA-L 0.000 claims description 13
- 229910000359 iron(II) sulfate Inorganic materials 0.000 claims description 13
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 claims description 12
- 238000001035 drying Methods 0.000 claims description 12
- 239000002245 particle Substances 0.000 claims description 12
- 239000002244 precipitate Substances 0.000 claims description 12
- 229910000033 sodium borohydride Inorganic materials 0.000 claims description 12
- 239000012279 sodium borohydride Substances 0.000 claims description 12
- 238000003756 stirring Methods 0.000 claims description 12
- 239000000243 solution Substances 0.000 claims description 11
- VQAPWLAUGBBGJI-UHFFFAOYSA-N [B].[Fe].[Rb] Chemical compound [B].[Fe].[Rb] VQAPWLAUGBBGJI-UHFFFAOYSA-N 0.000 claims description 8
- 239000002131 composite material Substances 0.000 claims description 8
- 238000000465 moulding Methods 0.000 claims description 7
- 238000005245 sintering Methods 0.000 claims description 7
- 239000000203 mixture Substances 0.000 claims description 6
- 239000012299 nitrogen atmosphere Substances 0.000 claims description 6
- 239000000725 suspension Substances 0.000 claims description 6
- 238000005406 washing Methods 0.000 claims description 6
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims description 6
- VEXZGXHMUGYJMC-UHFFFAOYSA-N Hydrochloric acid Chemical compound Cl VEXZGXHMUGYJMC-UHFFFAOYSA-N 0.000 claims description 4
- 230000005389 magnetism Effects 0.000 claims description 2
- 239000000463 material Substances 0.000 abstract description 3
- 230000000052 comparative effect Effects 0.000 description 10
- 238000012360 testing method Methods 0.000 description 5
- XEEYBQQBJWHFJM-UHFFFAOYSA-N Iron Chemical compound [Fe] XEEYBQQBJWHFJM-UHFFFAOYSA-N 0.000 description 3
- 238000005260 corrosion Methods 0.000 description 3
- 230000007797 corrosion Effects 0.000 description 3
- 230000007547 defect Effects 0.000 description 3
- 238000005516 engineering process Methods 0.000 description 3
- 230000005284 excitation Effects 0.000 description 3
- 230000001965 increasing effect Effects 0.000 description 3
- -1 iron ions Chemical class 0.000 description 3
- 230000001105 regulatory effect Effects 0.000 description 3
- 239000003822 epoxy resin Substances 0.000 description 2
- 229910052742 iron Inorganic materials 0.000 description 2
- 238000004519 manufacturing process Methods 0.000 description 2
- 229920000647 polyepoxide Polymers 0.000 description 2
- 239000000047 product Substances 0.000 description 2
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- 239000000853 adhesive Substances 0.000 description 1
- 230000001070 adhesive effect Effects 0.000 description 1
- 229910052782 aluminium Inorganic materials 0.000 description 1
- XAGFODPZIPBFFR-UHFFFAOYSA-N aluminium Chemical compound [Al] XAGFODPZIPBFFR-UHFFFAOYSA-N 0.000 description 1
- 238000006243 chemical reaction Methods 0.000 description 1
- 238000010835 comparative analysis Methods 0.000 description 1
- 230000001276 controlling effect Effects 0.000 description 1
- RKTYLMNFRDHKIL-UHFFFAOYSA-N copper;5,10,15,20-tetraphenylporphyrin-22,24-diide Chemical compound [Cu+2].C1=CC(C(=C2C=CC([N-]2)=C(C=2C=CC=CC=2)C=2C=CC(N=2)=C(C=2C=CC=CC=2)C2=CC=C3[N-]2)C=2C=CC=CC=2)=NC1=C3C1=CC=CC=C1 RKTYLMNFRDHKIL-UHFFFAOYSA-N 0.000 description 1
- 230000008878 coupling Effects 0.000 description 1
- 238000010168 coupling process Methods 0.000 description 1
- 238000005859 coupling reaction Methods 0.000 description 1
- 239000013078 crystal Substances 0.000 description 1
- 238000001514 detection method Methods 0.000 description 1
- 238000010586 diagram Methods 0.000 description 1
- 239000006185 dispersion Substances 0.000 description 1
- 230000000694 effects Effects 0.000 description 1
- 230000002708 enhancing effect Effects 0.000 description 1
- 238000002474 experimental method Methods 0.000 description 1
- 229960004887 ferric hydroxide Drugs 0.000 description 1
- 239000003302 ferromagnetic material Substances 0.000 description 1
- 239000003292 glue Substances 0.000 description 1
- 239000001257 hydrogen Substances 0.000 description 1
- 229910052739 hydrogen Inorganic materials 0.000 description 1
- 239000012535 impurity Substances 0.000 description 1
- IEECXTSVVFWGSE-UHFFFAOYSA-M iron(3+);oxygen(2-);hydroxide Chemical compound [OH-].[O-2].[Fe+3] IEECXTSVVFWGSE-UHFFFAOYSA-M 0.000 description 1
- 229910052751 metal Inorganic materials 0.000 description 1
- 239000002184 metal Substances 0.000 description 1
- 239000002105 nanoparticle Substances 0.000 description 1
- 238000012545 processing Methods 0.000 description 1
- 238000010298 pulverizing process Methods 0.000 description 1
- 238000011160 research Methods 0.000 description 1
- 229910052701 rubidium Inorganic materials 0.000 description 1
- IGLNJRXAVVLDKE-UHFFFAOYSA-N rubidium atom Chemical compound [Rb] IGLNJRXAVVLDKE-UHFFFAOYSA-N 0.000 description 1
- 239000000126 substance Substances 0.000 description 1
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- H—ELECTRICITY
- H01—ELECTRIC ELEMENTS
- H01F—MAGNETS; INDUCTANCES; TRANSFORMERS; SELECTION OF MATERIALS FOR THEIR MAGNETIC PROPERTIES
- H01F41/00—Apparatus or processes specially adapted for manufacturing or assembling magnets, inductances or transformers; Apparatus or processes specially adapted for manufacturing materials characterised by their magnetic properties
- H01F41/02—Apparatus or processes specially adapted for manufacturing or assembling magnets, inductances or transformers; Apparatus or processes specially adapted for manufacturing materials characterised by their magnetic properties for manufacturing cores, coils, or magnets
- H01F41/0253—Apparatus or processes specially adapted for manufacturing or assembling magnets, inductances or transformers; Apparatus or processes specially adapted for manufacturing materials characterised by their magnetic properties for manufacturing cores, coils, or magnets for manufacturing permanent magnets
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B06—GENERATING OR TRANSMITTING MECHANICAL VIBRATIONS IN GENERAL
- B06B—METHODS OR APPARATUS FOR GENERATING OR TRANSMITTING MECHANICAL VIBRATIONS OF INFRASONIC, SONIC, OR ULTRASONIC FREQUENCY, e.g. FOR PERFORMING MECHANICAL WORK IN GENERAL
- B06B1/00—Methods or apparatus for generating mechanical vibrations of infrasonic, sonic, or ultrasonic frequency
- B06B1/02—Methods or apparatus for generating mechanical vibrations of infrasonic, sonic, or ultrasonic frequency making use of electrical energy
- B06B1/04—Methods or apparatus for generating mechanical vibrations of infrasonic, sonic, or ultrasonic frequency making use of electrical energy operating with electromagnetism
- B06B1/045—Methods or apparatus for generating mechanical vibrations of infrasonic, sonic, or ultrasonic frequency making use of electrical energy operating with electromagnetism using vibrating magnet, armature or coil system
-
- H—ELECTRICITY
- H01—ELECTRIC ELEMENTS
- H01F—MAGNETS; INDUCTANCES; TRANSFORMERS; SELECTION OF MATERIALS FOR THEIR MAGNETIC PROPERTIES
- H01F1/00—Magnets or magnetic bodies characterised by the magnetic materials therefor; Selection of materials for their magnetic properties
- H01F1/01—Magnets or magnetic bodies characterised by the magnetic materials therefor; Selection of materials for their magnetic properties of inorganic materials
- H01F1/03—Magnets or magnetic bodies characterised by the magnetic materials therefor; Selection of materials for their magnetic properties of inorganic materials characterised by their coercivity
- H01F1/032—Magnets or magnetic bodies characterised by the magnetic materials therefor; Selection of materials for their magnetic properties of inorganic materials characterised by their coercivity of hard-magnetic materials
- H01F1/04—Magnets or magnetic bodies characterised by the magnetic materials therefor; Selection of materials for their magnetic properties of inorganic materials characterised by their coercivity of hard-magnetic materials metals or alloys
- H01F1/047—Alloys characterised by their composition
- H01F1/053—Alloys characterised by their composition containing rare earth metals
- H01F1/055—Alloys characterised by their composition containing rare earth metals and magnetic transition metals, e.g. SmCo5
- H01F1/057—Alloys characterised by their composition containing rare earth metals and magnetic transition metals, e.g. SmCo5 and IIIa elements, e.g. Nd2Fe14B
- H01F1/0571—Alloys characterised by their composition containing rare earth metals and magnetic transition metals, e.g. SmCo5 and IIIa elements, e.g. Nd2Fe14B in the form of particles, e.g. rapid quenched powders or ribbon flakes
- H01F1/0575—Alloys characterised by their composition containing rare earth metals and magnetic transition metals, e.g. SmCo5 and IIIa elements, e.g. Nd2Fe14B in the form of particles, e.g. rapid quenched powders or ribbon flakes pressed, sintered or bonded together
- H01F1/0578—Alloys characterised by their composition containing rare earth metals and magnetic transition metals, e.g. SmCo5 and IIIa elements, e.g. Nd2Fe14B in the form of particles, e.g. rapid quenched powders or ribbon flakes pressed, sintered or bonded together bonded together
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- Electromagnetism (AREA)
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- Crystallography & Structural Chemistry (AREA)
- Inorganic Chemistry (AREA)
- Manufacturing & Machinery (AREA)
- Hard Magnetic Materials (AREA)
Abstract
The invention discloses a preparation method of a high-temperature-resistant flexible bonded neodymium iron boron magnet, wherein the prepared flexible bonded neodymium iron boron magnet is a high-temperature-resistant high-magnetism permanent magnet material, and the high-temperature-resistant flexible bonded neodymium iron boron magnet is applied to an omnidirectional lamb wave magnetostrictive sensor, wherein the central frequency of the omnidirectional lamb wave magnetostrictive sensor is basically consistent with the designed theoretical central frequency of 340 kHz.
Description
Technical Field
The invention relates to a preparation method of a neodymium iron boron magnet, in particular to a preparation method of a high-temperature-resistant flexible bonding neodymium iron boron magnet, and a product and application thereof.
Background
With the increasingly obvious advantages of the electromagnetic ultrasonic technology, the technology has become a domestic research hotspot, the electromagnetic ultrasonic sensor is used as a core device of the technology, ultrasonic waves are generated by electromagnetic coupling, the detection can be carried out in a high-temperature environment, the structure of the electromagnetic ultrasonic sensor mainly comprises a coil, a magnet and a to-be-tested piece, the manufacturing is simple, and the cost is low.
The flexible bonded neodymium iron boron magnet has the advantages of high cost performance, convenient magnet forming, high processing precision, good toughness and small magnetic deviation. However, the existing flexible bonded neodymium iron boron magnet has the defects of low Curie temperature, poor temperature characteristic, easy pulverization and corrosion, and can meet the requirements of practical application only by adjusting the chemical components and adopting a surface treatment method to improve the magnet.
Disclosure of Invention
One of the purposes of the invention is to provide a preparation method of a flexible bonded neodymium iron boron magnet.
The invention also aims to obtain the prepared permanent magnet material with high temperature resistance and high magnetism of the flexible bonded neodymium iron boron magnet.
The third purpose of the invention is to apply the high-temperature-resistant flexible bonded neodymium iron boron magnet prepared by the invention to an omnidirectional lamb wave magnetostrictive sensor, wherein the central frequency of the omnidirectional lamb wave magnetostrictive sensor is basically consistent with the designed theoretical central frequency of 340 kHz.
The invention provides a preparation method of a high-temperature-resistant flexible bonded neodymium iron boron magnet, which comprises the following steps:
1) mixing a rubidium chloride aqueous solution with the concentration of 0.3-1.5M and a ferrous sulfate aqueous solution with the concentration of 0.5-1.5M to obtain a mixed solution A; then adjusting the pH value of the mixed solution A to 1.5-2.5;
2) slowly adding a sodium borohydride aqueous solution with the concentration of 3-4M into the mixed solution A with the pH adjusted at the temperature of 5-15 ℃ in a nitrogen atmosphere, washing with water to obtain a black precipitate, and sintering the black precipitate at the temperature of 500-750 ℃ to obtain rapidly quenched neodymium-iron-boron magnetic powder;
3) carrying out surface treatment on nano alumina powder by using a titanate coupling agent, and then uniformly mixing the rapidly quenched neodymium-iron-boron magnetic powder, the ferrocene magnetic powder and the bisphenol A epoxy resin in the step 2) with the nano alumina powder subjected to surface treatment by using a large-scale mixer to obtain mixed magnetic powder;
4) and (3) molding the mixed magnetic powder obtained in the step 3) in a composite environment of a temperature field with a constant temperature of 20-200 ℃ and an orientation field with a magnetic field intensity of 0.5-3T to obtain the high-temperature-resistant flexible bonded NdFeB magnet.
The method for preparing the rapidly quenched rubidium-iron-boron magnetic powder is different from the traditional preparation method, the rapidly quenched rubidium-iron-boron magnetic powder is prepared by a solution method, and the method comprises the steps of firstly using a rubidium chloride aqueous solution and a ferrous sulfate aqueous solution, respectively reducing rubidium chloride and ferrous sulfate into metal states of rubidium and iron by using sodium borohydride as reducibility under the pH and temperature of the method, and sintering at the temperature of 500-750 ℃ to obtain the rapidly quenched rubidium-iron-boron magnetic powder. According to the invention, the reaction conditions of high vacuum and high temperature are avoided, the production safety is realized, the average particle size of the obtained rapidly quenched neodymium-iron-boron magnetic powder is small, and the rapidly quenched neodymium-iron-boron magnetic powder can be directly used for preparing the high-temperature-resistant flexible bonded neodymium-iron-boron magnet without carrying out mesh treatment. The preparation method of the rapidly quenched rubidium-iron-boron magnetic powder is simple, easy to prepare, safe and rapid.
In the preparation process of the rapidly quenched rubidium-iron-boron magnetic powder, if the pH value of the mixed solution A is too high, iron ions in ferrous sulfate can react with hydroxyl ions to obtain ferric hydroxide, impurities in the obtained rapidly quenched neodymium-iron-boron magnetic powder are increased, if the pH value of the mixed solution A is too low, sodium borohydride can react with hydrogen ions, and the ferrous sulfate aqueous solution and the rubidium chloride aqueous solution cannot be completely reduced by the sodium borohydride. Therefore, the pH value of the mixed solution A, the volume of the rubidium chloride aqueous solution, the ferrous sulfate aqueous solution and the sodium borohydride aqueous solution are regulated, so that the obtained rapidly quenched rubidium-iron-boron magnetic powder is small in average particle size, high in purity and capable of being further directly used for preparing the high-temperature-resistant flexible bonded neodymium-iron-boron magnet.
Meanwhile, the coupling agent, the ferrocene magnetic powder and the nano-alumina are introduced, so that the element collocation in the obtained high-temperature-resistant flexible bonded neodymium iron boron magnet is optimized, and the high-temperature resistance of the flexible bonded neodymium iron boron magnet is obviously improved. The nano alumina powder subjected to surface treatment by the titanate coupling agent is added, so that the dispersion is excellent, the nano alumina powder is dispersed in a grain boundary phase of the neodymium iron boron magnet and exists in a tetragonal crystal structure, and the high temperature resistance of the flexible bonded neodymium iron boron magnet is obviously improved. Meanwhile, the flexible bonded NdFeB magnet is high in stability and small in vibration when rotating at a high speed in a driver, so that the prepared flexible bonded NdFeB magnet is better applied to an omnidirectional lamb wave magnetostrictive sensor. In addition, the nano particles have the function of enhancing and toughening, so that the mechanical strength of the bonded neodymium iron boron magnet can be improved, and the purpose of reducing the fracture of the magnet in the subsequent process and transportation process is achieved.
Finally, the mixed magnetic powder in the step 3) is molded in a composite environment of a temperature field and a phase taking field, so that the defects of poor temperature resistance and poor corrosion resistance of the bonded neodymium iron boron magnet material are overcome, the application range of the bondable neodymium iron boron is expanded, the defect of low use temperature of the bonded neodymium iron boron magnet can be overcome, the bonded neodymium iron boron magnet is better suitable for an omnidirectional lamb wave magnetostrictive sensor, and the central frequency of the omnidirectional lamb wave magnetostrictive sensor is basically consistent with the designed theoretical central frequency of 340 kHz.
As an embodiment, the volume of the aqueous solution of rubidium chloride in step 1): the volume of the ferrous sulfate aqueous solution is 1: 4-1: 6; volume of the rubidium chloride aqueous solution in step 1): the volume of the sodium borohydride aqueous solution is 1: 5-1: 9.
In one embodiment, the pH of the mixed solution A is adjusted to 1.5 to 2.5 in step 1) by using a 1M hydrochloric acid solution.
As an implementation mode, the average grain size of the rapidly quenched rubidium-iron-boron magnetic powder in the step 2) is 75-250 meshes. As an implementation mode, the step 3) of carrying out surface treatment on the nano-alumina powder by using the titanate coupling agent comprises the steps of drying the nano-alumina powder at 60-90 ℃, then putting the dried nano-alumina powder into an ethanol solution, stirring to obtain a suspension of the nano-alumina powder, then adding the titanate coupling agent, stirring and drying, wherein the particle size of the nano-alumina powder is 40-60 mu m.
As an embodiment, the rapidly quenched neodymium-iron-boron magnetic powder is 80-90 parts, the ferrocene magnetic powder is 0.2-5 parts, the titanate coupling agent is 0.5-5 parts, the bisphenol A epoxy resin is 5-8 parts, and the nano alumina powder is 0.5-2 parts.
As an implementation mode, the rapidly quenched neodymium-iron-boron magnetic powder is 85 parts, the ferrocene magnetic powder is 2 parts, the titanate coupling agent is 5 parts, the bisphenol A epoxy resin is 6 parts, and the nano alumina powder is 2 parts.
According to the invention, the ferrocene magnetic powder is introduced, so that the structural state of the magnetic field between the obtained high-temperature-resistant flexible bonded neodymium iron boron magnets is changed, the magnetic performance of the magnets at high temperature is greatly improved, and the corrosion resistance of the magnets is improved.
As an implementation mode, in step 3), firstly, mixing nano alumina powder subjected to surface treatment by a titanate coupling agent with rapidly quenched neodymium iron boron magnetic powder to obtain a mixture B, then, dispersing the mixture B by using a high-power ultrasonic generator, and then, uniformly mixing the dispersed mixture B, ferrocene magnetic powder and bisphenol a epoxy resin by using a large-scale mixer to obtain mixed magnetic powder.
The invention provides a high-temperature-resistant flexible bonded neodymium iron boron magnet which is prepared by the preparation method.
The invention relates to an omnidirectional lamb wave magnetostrictive sensor, which comprises the following components: the high-temperature-resistant flexible bonding neodymium iron boron magnet comprises a Printed Circuit Board (PCB) coil 1, a high-temperature-resistant flexible bonding neodymium iron boron magnet 2, a round nickel sheet 3, a PCB coil 1, the high-temperature-resistant flexible bonding neodymium iron boron magnet 2, the round nickel sheet 3 and centroids of the three coincide in the vertical direction, the PCB coil 1 is arranged on the round nickel sheet 3, and the high-temperature-resistant flexible bonding neodymium iron boron magnet 2 is arranged at a certain height above the PCB coil 1; the center frequency of the omnidirectional lamb wave magnetostrictive sensor is 330-340 kHz.
The invention bonds the round nickel sheet 3 on the surface of the board structure by epoxy resin glue, arranges the PCB coil 1 and the high temperature resistant flexible bonding neodymium iron boron magnet 2 on the PCB coil in sequence, ensures that the centroids of the PCB coil 1, the high temperature resistant flexible bonding neodymium iron boron magnet 2 and the round nickel sheet 3 are superposed in the vertical direction, increases the distance of the PCB coil by the high temperature resistant flexible bonding neodymium iron boron magnet 2, magnetic field components are generated around the circular nickel sheet 3, the directions of the magnetic field components are mainly distributed along the radial direction, the bias static magnetic field generated by the high-temperature resistant flexible bonded neodymium iron boron magnet 2 and the dynamic magnetic field generated by the electrified PCB coil 1 both generate magnetic field components along the radial direction, and based on the magnetostrictive effect, the circular nickel sheet 3 made of ferromagnetic materials generates tensile deformation to drive the plate structure to generate deformation and vibration, so that omnidirectional lamb waves are excited in the plate structure.
As an embodiment, the distance between the bottom surface of the high-temperature resistant flexible bonding neodymium iron boron magnet 2 and the surface of the PCB coil 1 is increased by the high-temperature resistant flexible bonding neodymium iron boron magnet 2 and is within a range of 11-15 mm.
In the invention, the outer diameter D of the circular nickel sheet 3 is 24mm, the outer diameter of the PCB coil is 21mm, the inner diameter of the PCB coil is 12mm, the diameter of the coil is 0.2mm, the wire spacing is 0.2mm, and the thickness of the nickel sheet is 0.1 mm. See fig. 1.
In the present invention, the magnet size is such that diameter x thickness =12 x 5 (unit: mm) provides a radially biased static magnetic field by controlling the distance. The theoretical center frequency of the omnidirectional lamb wave magnetostrictive sensor designed by the invention is 340 kHz.
The working temperature of the omnidirectional lamb wave magnetostrictive sensor is 300-500 ℃.
Drawings
FIG. 1: the structure and working schematic diagram of the omnidirectional lamb wave magnetostrictive transducer; 1-PCB coil; 2-high temperature resistant flexible bonding neodymium iron boron magnet; 3-round nickel sheet.
Detailed Description
The following specific examples describe the present invention in detail, however, the present invention is not limited to the following examples.
The frequency characteristic test of the omnidirectional lamb wave magnetostrictive sensor comprises the following steps: according to selected parameters, determining an omnidirectional lamb wave magnetostrictive sensor structure, designing the omnidirectional lamb wave magnetostrictive sensor with the theoretical center frequency of 340kHz, bonding a circular nickel sheet on the surface of an aluminum plate through epoxy resin adhesive, placing a high-temperature-resistant flexible bonding neodymium-iron-boron magnet and a PCB coil on the sensor, carrying out experiments in an one-excitation-one-receiving mode, wherein the distance between an excitation signal and a receiving signal is 300mm, the frequency of the excitation signal is 5-cycle sine waves modulated by a Hanning window, increasing the excitation frequency from 250 kHz to 500kHz by a step length of 10 kHz, extracting So modes including peak values in all frequency receiving signals, and obtaining the frequency characteristic of the omnidirectional lamb wave magnetostrictive sensor through curve fitting.
Example 1:
a preparation method of a high-temperature-resistant flexible bonded neodymium iron boron magnet comprises the following steps:
1) mixing 2L of 0.3M (M, i.e. mol/L, the same applies below) rubidium chloride aqueous solution and 4L of 0.5M ferrous sulfate aqueous solution to obtain a mixed solution A; then adjusting the pH value of the mixed solution A to 1.5;
2) slowly adding 10L of 3M sodium borohydride aqueous solution into the mixed solution A with the regulated pH value at the temperature of 5 ℃ in the nitrogen atmosphere, washing with water to obtain black precipitate, and sintering the black precipitate at 500 ℃ to obtain the rapidly quenched neodymium-iron-boron magnetic powder with the average particle size of 75 meshes;
3) drying 2 parts of nano alumina powder at 60 ℃, then placing the dried nano alumina powder into an ethanol solution, stirring to obtain a suspension of the nano alumina powder, then adding 1 part of titanate coupling agent, stirring and drying, wherein the particle size of the nano alumina powder is 40 mu m, and then uniformly mixing 84 parts of rapidly quenched neodymium-iron-boron magnetic powder, 5 parts of ferrocene magnetic powder, 8 parts of bisphenol A epoxy resin and the nano alumina powder subjected to surface treatment by the titanate coupling agent in the step 2) by using a large-scale mixer to obtain mixed magnetic powder;
4) and (3) molding the mixed magnetic powder obtained in the step 3) in a composite environment of a temperature field with a constant temperature of 20 ℃ and an orientation field with a magnetic field intensity of 0.5T to obtain the high-temperature-resistant flexible bonded NdFeB magnet.
The high temperature resistant flexible bonded neodymium iron boron magnet described in example 1 was applied to the omnidirectional lamb wave magnetostrictive sensor described in this invention: the omnidirectional lamb wave magnetostrictive sensor comprises a Printed Circuit Board (PCB) coil 1, a high-temperature-resistant flexible bonding neodymium iron boron magnet 2 prepared in the embodiment, a circular nickel sheet 3, the PCB coil 1, the high-temperature-resistant flexible bonding neodymium iron boron magnet 2 prepared in the embodiment and the circular nickel sheet 3, wherein centroids of the three are overlapped in the vertical direction, the PCB coil 1 is arranged on the circular nickel sheet 3, and the high-temperature-resistant flexible bonding neodymium iron boron magnet 2 prepared in the embodiment is arranged 11 mm above the PCB coil 1; the outer diameter D of the circular nickel sheet 3 is 24mm, the outer diameter of the PCB coil is 21mm, the inner diameter of the PCB coil is 12mm, the diameter of the coil is 0.2mm, the line spacing is 0.2mm, and the thickness of the nickel sheet is 0.1 mm; the size of the high-temperature-resistant flexible bonded neodymium iron boron magnet 2 prepared by the embodiment is 12mm in diameter and 5mm in thickness. The operating temperature of the omnidirectional lamb wave magnetostrictive sensor of the embodiment is 300 ℃. The frequency characteristic test of the omnidirectional lamb wave magnetostrictive sensor in this embodiment was performed, and the center frequency of the omnidirectional lamb wave magnetostrictive sensor was 330 kHz.
Example 2:
a preparation method of a high-temperature-resistant flexible bonded neodymium iron boron magnet comprises the following steps:
1) mixing 2L of 1.5M rubidium chloride aqueous solution and 12L of 1.5M ferrous sulfate aqueous solution to obtain a mixed solution A; then adjusting the pH value of the mixed solution A to 2.5;
2) slowly adding 18L of sodium borohydride aqueous solution with the concentration of 4M into the mixed solution A with the regulated pH value in the nitrogen atmosphere at the temperature of 15 ℃, washing with water to obtain black precipitate, and sintering the black precipitate at 750 ℃ to obtain the rapidly quenched neodymium iron boron magnetic powder with the average particle size of 250 meshes;
3) drying 2 parts of nano alumina powder at 90 ℃, then placing the dried nano alumina powder into an ethanol solution, stirring to obtain a suspension of the nano alumina powder, then adding 5 parts of titanate coupling agent, stirring and drying, wherein the particle size of the nano alumina powder is 60 microns, and then uniformly mixing 87 parts of rapidly quenched neodymium iron boron magnetic powder, 1 part of ferrocene magnetic powder, 5 parts of bisphenol A epoxy resin and the nano alumina powder subjected to surface treatment by the titanate coupling agent in the step 2) by using a large-scale mixer to obtain mixed magnetic powder;
4) and (3) molding the mixed magnetic powder obtained in the step 3) in a composite environment of a temperature field with a constant temperature of 200 ℃ and an orientation field with a magnetic field intensity of 3T to obtain the high-temperature-resistant flexible bonded neodymium iron boron magnet.
The high temperature resistant flexible bonded neodymium iron boron magnet described in embodiment 2 is applied to the omnidirectional lamb wave magnetostrictive sensor described in the present invention: the omnidirectional lamb wave magnetostrictive sensor comprises a Printed Circuit Board (PCB) coil 1, a high-temperature-resistant flexible bonding neodymium iron boron magnet 2 prepared in the embodiment, a circular nickel sheet 3, the PCB coil 1, the high-temperature-resistant flexible bonding neodymium iron boron magnet 2 prepared in the embodiment and the circular nickel sheet 3, wherein centroids of the three are overlapped in the vertical direction, the PCB coil 1 is arranged on the circular nickel sheet 3, and the high-temperature-resistant flexible bonding neodymium iron boron magnet 2 prepared in the embodiment is arranged at a position 15mm above the PCB coil 1; the outer diameter D of the circular nickel sheet 3 is 24mm, the outer diameter of the PCB coil is 21mm, the inner diameter of the PCB coil is 12mm, the diameter of the coil is 0.2mm, the line spacing is 0.2mm, and the thickness of the nickel sheet is 0.1 mm; the size of the high-temperature-resistant flexible bonded neodymium iron boron magnet 2 prepared by the embodiment is 12mm in diameter and 5mm in thickness. The operating temperature of the omnidirectional lamb wave magnetostrictive sensor of the present embodiment is 500 ℃. The frequency characteristic test of the omnidirectional lamb wave magnetostrictive sensor in this embodiment was performed, and the center frequency of the omnidirectional lamb wave magnetostrictive sensor was 335 kHz.
Example 3:
a preparation method of a high-temperature-resistant flexible bonded neodymium iron boron magnet comprises the following steps:
1) mixing 2L of 1.5M rubidium chloride aqueous solution and 10L of 1.5M ferrous sulfate aqueous solution to obtain a mixed solution A; then adjusting the pH value of the mixed solution A to 2.0;
2) slowly adding 14L of 3M sodium borohydride aqueous solution into the mixed solution A with the adjusted pH value at the temperature of 10 ℃ in a nitrogen atmosphere, washing with water to obtain black precipitate, and sintering the black precipitate at 650 ℃ to obtain the rapidly quenched neodymium-iron-boron magnetic powder with the average particle size of 120 meshes;
3) drying 2 parts of nano alumina powder at 80 ℃, then placing the dried nano alumina powder into an ethanol solution, stirring to obtain a suspension of the nano alumina powder, then adding 5 parts of titanate coupling agent, stirring and drying, wherein the particle size of the nano alumina powder is 50 microns, and then uniformly mixing 85 parts of rapidly quenched neodymium-iron-boron magnetic powder, 2 parts of ferrocene magnetic powder, 6 parts of bisphenol A epoxy resin and the nano alumina powder subjected to surface treatment by the titanate coupling agent in the step 2) by using a large-scale mixer to obtain mixed magnetic powder;
4) and (3) molding the mixed magnetic powder obtained in the step 3) in a composite environment of a temperature field with a constant temperature of 100 ℃ and an orientation field with a magnetic field intensity of 2T to obtain the high-temperature-resistant flexible bonded neodymium iron boron magnet.
The high temperature resistant flexible bonded neodymium iron boron magnet described in embodiment 3 is applied to the omnidirectional lamb wave magnetostrictive sensor described in the present invention: the omnidirectional lamb wave magnetostrictive sensor comprises a Printed Circuit Board (PCB) coil 1, a high-temperature-resistant flexible bonding neodymium iron boron magnet 2 prepared in the embodiment, a circular nickel sheet 3, the PCB coil 1, the high-temperature-resistant flexible bonding neodymium iron boron magnet 2 prepared in the embodiment and the circular nickel sheet 3, wherein centroids of the three are overlapped in the vertical direction, the PCB coil 1 is arranged on the circular nickel sheet 3, and the flexible bonding neodymium iron boron magnet 22 prepared in the embodiment is arranged 12mm above the PCB coil 1; the outer diameter D of the circular nickel sheet 3 is 24mm, the outer diameter of the PCB coil is 21mm, the inner diameter of the PCB coil is 12mm, the diameter of the coil is 0.2mm, the line spacing is 0.2mm, and the thickness of the nickel sheet is 0.1 mm; the size of the high-temperature-resistant flexible bonded neodymium iron boron magnet 2 prepared by the embodiment is 12mm in diameter and 5mm in thickness. The operating temperature of the omni-directional lamb wave magnetostrictive sensor in the embodiment is 500 ℃. The frequency characteristic test was performed on the omnidirectional lamb wave magnetostrictive sensor described in this embodiment, and the center frequency of the obtained omnidirectional lamb wave magnetostrictive sensor was 340 kHz.
Comparative example 1:
a preparation method of a high-temperature-resistant flexible bonded neodymium iron boron magnet comprises the following steps:
1) drying 2 parts of nano alumina powder at 80 ℃, then placing the dried nano alumina powder into an ethanol solution, stirring to obtain a suspension of the nano alumina powder, then adding 5 parts of titanate coupling agent, stirring and drying, wherein the particle size of the nano alumina powder is 50 microns, and then uniformly mixing 85 parts of rapidly quenched neodymium iron boron magnetic powder (Zhejiang Kogyo Co., Ltd.), 2 parts of ferrocene magnetic powder, 6 parts of bisphenol A epoxy resin and the nano alumina powder subjected to surface treatment by the titanate coupling agent by using a large-scale mixer to obtain mixed magnetic powder;
2) and (3) molding the mixed magnetic powder obtained in the step 2) in a composite environment of a temperature field with a constant temperature of 100 ℃ and an orientation field with a magnetic field intensity of 2T to obtain the high-temperature-resistant flexible bonded neodymium iron boron magnet.
The high temperature resistant flexible bonded neodymium iron boron magnet described in comparative example 1 was applied to the omnidirectional lamb wave magnetostrictive sensor described in the present invention: the omnidirectional lamb wave magnetostrictive sensor comprises a Printed Circuit Board (PCB) coil 1, a high-temperature-resistant flexible bonding neodymium iron boron magnet 2 prepared in the embodiment, a circular nickel sheet 3, the PCB coil 1, the high-temperature-resistant flexible bonding neodymium iron boron magnet 2 prepared in the embodiment and the circular nickel sheet 3, wherein centroids of the three are overlapped in the vertical direction, the PCB coil 1 is arranged on the circular nickel sheet 3, and the high-temperature-resistant flexible bonding neodymium iron boron magnet 2 prepared in the embodiment is arranged 12mm above the PCB coil 1; the outer diameter D of the circular nickel sheet 3 is 24mm, the outer diameter of the PCB coil is 21mm, the inner diameter of the PCB coil is 12mm, the diameter of the coil is 0.2mm, the line spacing is 0.2mm, and the thickness of the nickel sheet is 0.1 mm; the size of the high-temperature-resistant flexible bonded neodymium iron boron magnet 2 prepared by the embodiment is 12mm in diameter and 5mm in thickness. The operating temperature of the omni-directional lamb wave magnetostrictive sensor of this comparative example was 500 ℃. The frequency characteristic test was performed on the omnidirectional lamb wave magnetostrictive sensor described in this embodiment, and the center frequency of the obtained omnidirectional lamb wave magnetostrictive sensor was 280 kHz.
Comparative example 2:
a preparation method of a flexible bonded neodymium iron boron magnet comprises the following steps:
1) mixing 2L of 1.5M rubidium chloride aqueous solution and 10L of 1.5M ferrous sulfate aqueous solution to obtain a mixed solution A; then adjusting the pH value of the mixed solution A to 2.0;
2) slowly adding 14L of 3M sodium borohydride aqueous solution into the mixed solution A with the adjusted pH value at the temperature of 10 ℃ in a nitrogen atmosphere, washing with water to obtain black precipitate, and sintering the black precipitate at 650 ℃ to obtain the rapidly quenched neodymium-iron-boron magnetic powder with the average particle size of 120 meshes;
3) then uniformly mixing 85 parts of the rapidly quenched neodymium iron boron magnetic powder in the step 2), 2 parts of ferrocene magnetic powder and 6 parts of bisphenol A epoxy resin by using a large-scale mixer to obtain mixed magnetic powder;
4) and (3) molding the mixed magnetic powder obtained in the step 3) in a composite environment of a temperature field with a constant temperature of 100 ℃ and an orientation field with a magnetic field intensity of 2T to obtain the flexible bonded neodymium iron boron magnet.
The high temperature resistant flexible bonded neodymium iron boron magnet described in comparative example 2 was applied to the omnidirectional lamb wave magnetostrictive sensor described in the present invention: the omnidirectional lamb wave magnetostrictive sensor comprises a Printed Circuit Board (PCB) coil 1, a high-temperature-resistant flexible bonding neodymium iron boron magnet 2 prepared in the embodiment, a circular nickel sheet 3, the PCB coil 1, the high-temperature-resistant flexible bonding neodymium iron boron magnet 2 prepared in the embodiment and the circular nickel sheet 3, wherein centroids of the three are overlapped in the vertical direction, the PCB coil 1 is arranged on the circular nickel sheet 3, and the high-temperature-resistant flexible bonding neodymium iron boron magnet 2 prepared in the embodiment is arranged 12mm above the PCB coil 1; the outer diameter D of the circular nickel sheet 3 is 24mm, the outer diameter of the PCB coil is 21mm, the inner diameter of the PCB coil is 12mm, the diameter of the coil is 0.2mm, the line spacing is 0.2mm, and the thickness of the nickel sheet is 0.1 mm; the size of the high-temperature-resistant flexible bonded neodymium iron boron magnet 2 prepared by the embodiment is 12mm in diameter and 5mm in thickness. The omnidirectional lamb wave magnetostrictive sensor of this comparative example has a center frequency of 20kHz at an operating temperature of 500 c.
Comparative analysis of examples:
as can be seen from example 3 and comparative example 1, the flexible bonded ndfeb magnet prepared by the solution method of the present invention matched the theoretical center frequency of 340kHz of the isotropic lamb wave magnetostrictive sensor.
In comparative example 1, the difference between the center frequency of the flexible bonded neodymium iron boron magnet prepared without using the solution method and applied to the omnidirectional lamb wave magnetostrictive sensor and the theoretical center frequency of the omnidirectional lamb wave magnetostrictive sensor is larger.
From the embodiment 3 and the comparative example 2, it can be known that the high-temperature-resistant flexible bonded neodymium iron boron magnet prepared by introducing the coupling agent, the ferrocene magnetic powder and the nano alumina can be better applied to the omnidirectional lamb wave magnetostrictive sensor. The high-temperature-resistant flexible bonded neodymium iron boron magnet prepared by the invention can work at a high temperature of 500 ℃, when the high-temperature-resistant flexible bonded neodymium iron boron magnet is applied to an omnidirectional lamb wave magnetostrictive sensor, the obtained central frequency is basically consistent with the designed theoretical central frequency, a coupling agent, ferrocene magnetic powder and nano-alumina are not introduced in a comparative example 2, and when the flexible bonded neodymium iron boron magnet obtained by the traditional preparation method is applied to the omnidirectional lamb wave magnetostrictive sensor, the central frequency is only 20kHz at a working temperature of 500 ℃, which is obviously lower than that of the high-temperature-resistant flexible bonded neodymium iron boron magnet.
Claims (10)
1. A preparation method of a flexible bonded neodymium iron boron magnet comprises the following steps:
mixing a rubidium chloride aqueous solution with the concentration of 0.3-1.5M and a ferrous sulfate aqueous solution with the concentration of 0.5-1.5M to obtain a mixed solution A; then adjusting the pH value of the mixed solution A to 1.5-2.5;
slowly adding a sodium borohydride aqueous solution with the concentration of 3-4M into the mixed solution A with the pH adjusted at the temperature of 5-15 ℃ in a nitrogen atmosphere, washing with water to obtain a black precipitate, and sintering the black precipitate at the temperature of 500-750 ℃ to obtain rapidly quenched neodymium-iron-boron magnetic powder;
carrying out surface treatment on nano alumina powder by using a titanate coupling agent, and then uniformly mixing the rapidly quenched neodymium-iron-boron magnetic powder, the ferrocene magnetic powder and the bisphenol A epoxy resin in the step 2) with the nano alumina powder subjected to surface treatment by using a large-scale mixer to obtain mixed magnetic powder;
and (3) molding the mixed magnetic powder obtained in the step 3) in a composite environment of a temperature field with a constant temperature of 20-200 ℃ and an orientation field with a magnetic field intensity of 0.5-3T to obtain the high-temperature-resistant flexible bonded NdFeB magnet.
2. The method of claim 1, wherein: volume of the rubidium chloride aqueous solution in step 1): the volume of the ferrous sulfate aqueous solution is 1: 4-1: 6; volume of the rubidium chloride aqueous solution in step 1): the volume of the sodium borohydride aqueous solution is 1: 5-1: 9.
3. The method of claim 1, wherein: step 1) adjusting the pH value of the mixed solution A to 1.5-2.5 by using 1M hydrochloric acid solution.
4. The method of claim 1, wherein: the average particle size of the rapidly quenched rubidium-iron-boron magnetic powder in the step 2) is 75-250 meshes.
5. The method of claim 1, wherein: and 3) carrying out surface treatment on the nano-alumina powder by using a titanate coupling agent, wherein the surface treatment comprises the steps of drying the nano-alumina powder at 60-90 ℃, then putting the dried nano-alumina powder into an ethanol solution, stirring to obtain a suspension of the nano-alumina powder, then adding the titanate coupling agent, stirring and drying, and the granularity of the nano-alumina powder is 40-60 mu m.
6. The method of claim 1, wherein: 80-90 parts of rapidly quenched neodymium iron boron magnetic powder, 0.2-5 parts of ferrocene magnetic powder, 0.5-5 parts of titanate coupling agent, 5-8 parts of bisphenol A epoxy resin and 0.5-2 parts of nano alumina powder.
7. The method of claim 1, wherein: 85 parts of rapidly quenched neodymium iron boron magnetic powder, 2 parts of ferrocene magnetic powder, 5 parts of titanate coupling agent, 6 parts of bisphenol A epoxy resin and 2 parts of nano alumina powder.
8. The method of claim 1, wherein: and 3) mixing the nano-alumina powder subjected to surface treatment by the titanate coupling agent with the rapidly quenched neodymium-iron-boron magnetic powder to obtain a mixture B, then dispersing the mixture B by using a high-power ultrasonic generator, and then uniformly mixing the dispersed mixture B, the ferrocene magnetic powder and the bisphenol A epoxy resin by using a large-scale mixer to obtain mixed magnetic powder.
9. A high-temperature-resistant flexible bonded NdFeB magnet prepared by the preparation method of any one of claims 1 to 8.
10. An omnidirectional lamb wave magnetostrictive sensor: including printed circuit board PCB coil 1, high temperature resistant flexible bonding neodymium iron boron magnetism body 2 of claim 9, circular nickel piece 3, characterized by: the PCB coil 1, the high-temperature-resistant flexible bonded neodymium iron boron magnet 2 and the round nickel sheet 3 are overlapped in the vertical direction, the PCB coil 1 is arranged on the round nickel sheet 3, and the high-temperature-resistant flexible bonded neodymium iron boron magnet 2 is arranged at a certain height above the PCB coil 1; the center frequency of the omnidirectional lamb wave magnetostrictive sensor is 330-340 kHz.
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| JP2000034502A (en) * | 1998-07-17 | 2000-02-02 | Sumitomo Metal Mining Co Ltd | Alloy powder for neodymium-iron-boron bonded magnet |
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